#============================================================================= data_global #============================================================================= # 1. SUBMISSION DETAILS _publ_contact_author_name 'Daniel B. Leznoff' _publ_contact_author_address ; Leznoff, Daniel B. Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; _publ_contact_author_phone '+1-778-782-4887' _publ_contact_author_fax '+1-778-782-3765' _publ_contact_author_email 'dleznoff@sfu.ca' _publ_requested_journal 'Inorg. Chem.' #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; INSERT TITLE ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Kobayashi, Masayuki ' ; Department of Chemistry Faculty of Science, Kyushu University Hakozaki 6-10-1, Higashi-ku, Fukuoka 812-8581, Japan ; 'Savard, Didier' ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; 'Geisheimer, Andrew R.' ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; 'Sakai, Ken ' ; Department of Chemistry Faculty of Science, Kyushu University Hakozaki 6-10-1, Higashi-ku, Fukuoka 812-8581, Japan ; 'Leznoff, Daniel B.' ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; ## -------------------REFERENCES ----------------------## _publ_section_references ; International Tables for X-ray Crystallography, Vol. IV, (1974) Kynoch Press, Birmingham, England. Johnson, C.K., (1976) ORTEP - A Fortran Thermal Ellipsoid Plot Program, Technical Report ORNL-5138, Oak Ridge National Lab., U.S.A. Le Page, Y., (1988) J. Appl. Cryst., 21, 983-984. Le Page, Y. and Gabe, E.J., (1979) J. Appl. Cryst., 12, 464-466. # CRYSTALS # Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. # Extinction correction # Larson, A.C. (1970), Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294 #ORTEP-3 version 1.073 # Farrugia, L.J., (1997) J. Appl. Cryst. 30, 565. # SIR92 # Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_C50H40Co2N16O2Pt2S8 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_moiety ? _chemical_formula_sum 'C25 H20 Co N8 O Pt S4' _chemical_formula_weight 830.75 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' #------------------------------------------------ _cell_length_a 16.613(6) _cell_length_b 11.492(4) _cell_length_c 17.209(6) _cell_angle_alpha 90.00 _cell_angle_beta 118.188(5) _cell_angle_gamma 90.00 _cell_volume 2895.8(17) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 5.722 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4564 _exptl_absorpt_correction_T_max 0.7950 _exptl_absorpt_process_details ? #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15431 _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_sigmaI/netI 0.1128 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.90 _reflns_number_total 6612 _reflns_number_gt 4514 _reflns_threshold_expression >2sigma(I) _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.955 #========================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+28.2129P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6612 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1141 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.1492 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 3.933 _refine_diff_density_min -2.664 _refine_diff_density_rms 0.246 #========================================================== # 9. General computing _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.89788(3) 0.32271(3) 1.04420(2) 0.02086(13) Uani 1 1 d . . . Co2 Co 0.91906(10) 0.10465(11) 0.73616(8) 0.0191(3) Uani 1 1 d . . . S1 S 0.8994(2) 0.4087(2) 0.92344(17) 0.0256(6) Uani 1 1 d . . . S2 S 0.9128(2) 0.1364(2) 0.99987(15) 0.0237(6) Uani 1 1 d . . . S3 S 0.8956(2) 0.2632(3) 1.17236(17) 0.0303(7) Uani 1 1 d . . . S4 S 0.8944(2) 0.5163(2) 1.0829(2) 0.0351(7) Uani 1 1 d . . . N2 N 0.9844(6) -0.0070(7) 0.8445(5) 0.022(2) Uani 1 1 d . . . N7 N 0.7874(6) 0.0866(7) 0.7280(5) 0.0171(18) Uani 1 1 d . . . N6 N 0.9176(6) -0.0325(8) 0.6528(5) 0.022(2) Uani 1 1 d . . . N8 N 0.8348(7) 0.2177(7) 0.6294(5) 0.021(2) Uani 1 1 d . . . N5 N 1.0398(7) 0.1353(8) 0.7288(5) 0.027(2) Uani 1 1 d . . . N1 N 0.9382(7) 0.2430(8) 0.8258(5) 0.027(2) Uani 1 1 d . . . C23 C 0.8024(9) 0.3489(10) 0.5095(7) 0.032(3) Uani 1 1 d . . . H23 H 0.8228 0.3909 0.4760 0.038 Uiso 1 1 calc R . . C20 C 0.7486(8) 0.2269(9) 0.6145(6) 0.021(2) Uani 1 1 d . . . C24 C 0.8621(9) 0.2773(9) 0.5788(7) 0.028(3) Uani 1 1 d . . . H24 H 0.9225 0.2708 0.5901 0.033 Uiso 1 1 calc R . . C21 C 0.6850(9) 0.2957(9) 0.5438(7) 0.030(3) Uani 1 1 d . . . H21 H 0.6243 0.3006 0.5320 0.036 Uiso 1 1 calc R . . C1 C 0.9225(8) 0.3077(9) 0.8667(6) 0.024(2) Uani 1 1 d . . . C19 C 0.7246(8) 0.1644(8) 0.6764(6) 0.023(2) Uani 1 1 d . . . C18 C 0.6463(8) 0.1839(9) 0.6822(7) 0.027(2) Uani 1 1 d . . . H18 H 0.6043 0.2394 0.6465 0.033 Uiso 1 1 calc R . . C16 C 0.6938(8) 0.0374(10) 0.7945(7) 0.028(3) Uani 1 1 d . . . H16 H 0.6841 -0.0076 0.8342 0.034 Uiso 1 1 calc R . . C9 C 1.0572(8) 0.0613(10) 0.6784(6) 0.026(3) Uani 1 1 d . . . C17 C 0.6301(9) 0.1197(10) 0.7424(7) 0.029(3) Uani 1 1 d . . . H17 H 0.5774 0.1320 0.7474 0.035 Uiso 1 1 calc R . . C13 C 0.8585(9) -0.2065(10) 0.5658(7) 0.036(3) Uani 1 1 d . . . H13 H 0.8142 -0.2644 0.5434 0.044 Uiso 1 1 calc R . . C10 C 0.9895(9) -0.0333(10) 0.6355(6) 0.031(3) Uani 1 1 d . . . C14 C 0.8539(9) -0.1159(9) 0.6190(7) 0.028(3) Uani 1 1 d . . . H14 H 0.8049 -0.1141 0.6310 0.034 Uiso 1 1 calc R . . C5 C 1.0992(9) 0.2199(11) 0.7700(7) 0.036(3) Uani 1 1 d . . . H5 H 1.0861 0.2718 0.8041 0.043 Uiso 1 1 calc R . . C6 C 1.1801(10) 0.2358(12) 0.7653(8) 0.044(4) Uani 1 1 d . . . H6 H 1.2205 0.2956 0.7957 0.053 Uiso 1 1 calc R . . C8 C 1.1367(10) 0.0723(12) 0.6706(8) 0.040(3) Uani 1 1 d . . . H8 H 1.1483 0.0203 0.6356 0.048 Uiso 1 1 calc R . . C22 C 0.7154(10) 0.3551(10) 0.4930(7) 0.037(3) Uani 1 1 d . . . H22 H 0.6745 0.4004 0.4462 0.045 Uiso 1 1 calc R . . C11 C 0.9966(10) -0.1204(12) 0.5824(7) 0.040(3) Uani 1 1 d . . . H11 H 1.0455 -0.1201 0.5702 0.048 Uiso 1 1 calc R . . C12 C 0.9324(11) -0.2053(11) 0.5485(8) 0.042(4) Uani 1 1 d . . . H12 H 0.9378 -0.2632 0.5134 0.051 Uiso 1 1 calc R . . C15 C 0.7720(8) 0.0238(9) 0.7862(6) 0.024(2) Uani 1 1 d . . . H15 H 0.8154 -0.0304 0.8217 0.028 Uiso 1 1 calc R . . C2 C 1.0285(8) -0.0634(9) 0.9069(7) 0.024(2) Uani 1 1 d . . . C3 C 0.8175(10) 0.1560(11) 1.1415(7) 0.038(3) Uani 1 1 d . . . C4 C 0.7912(10) 0.5346(10) 1.0688(7) 0.034(3) Uani 1 1 d . . . N4 N 0.7164(8) 0.5596(9) 1.0583(7) 0.038(3) Uani 1 1 d . . . N3 N 0.7618(11) 0.0852(10) 1.1236(8) 0.063(4) Uani 1 1 d . . . C7 C 1.1973(10) 0.1588(13) 0.7137(9) 0.050(4) Uani 1 1 d . . . H7 H 1.2502 0.1659 0.7083 0.060 Uiso 1 1 calc R . . O1 O 0.9470(13) 0.5672(11) 0.4216(8) 0.107(6) Uani 1 1 d . . . H1 H 0.9937 0.5487 0.4661 0.160 Uiso 1 1 calc R . . C25 C 0.936(2) 0.493(2) 0.3478(18) 0.165(14) Uani 1 1 d . . . H25A H 0.8741 0.4975 0.3014 0.247 Uiso 1 1 calc R . . H25B H 0.9496 0.4134 0.3677 0.247 Uiso 1 1 calc R . . H25C H 0.9768 0.5179 0.3263 0.247 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0262(2) 0.0157(2) 0.01816(18) -0.00141(16) 0.00843(15) 0.0041(2) Co2 0.0232(8) 0.0160(7) 0.0172(6) 0.0025(5) 0.0089(6) 0.0031(6) S1 0.0357(18) 0.0143(13) 0.0275(13) 0.0024(10) 0.0154(12) 0.0046(13) S2 0.0383(18) 0.0147(12) 0.0155(11) 0.0004(9) 0.0106(11) 0.0042(12) S3 0.0317(18) 0.0381(17) 0.0221(13) -0.0023(11) 0.0135(12) 0.0023(14) S4 0.046(2) 0.0180(15) 0.0485(18) -0.0079(12) 0.0280(16) -0.0005(14) N2 0.027(6) 0.018(5) 0.021(4) 0.002(3) 0.011(4) 0.004(4) N7 0.015(5) 0.009(4) 0.021(4) -0.003(3) 0.003(3) -0.004(4) N6 0.023(5) 0.024(5) 0.018(4) 0.006(3) 0.009(4) 0.013(4) N8 0.031(6) 0.007(4) 0.021(4) 0.001(3) 0.009(4) 0.005(4) N5 0.028(6) 0.033(5) 0.018(4) 0.005(4) 0.011(4) -0.003(5) N1 0.045(7) 0.020(5) 0.015(4) -0.004(3) 0.014(4) -0.005(5) C23 0.041(8) 0.035(7) 0.021(5) 0.001(4) 0.015(5) 0.003(6) C20 0.025(7) 0.022(5) 0.012(4) -0.006(4) 0.004(4) -0.001(5) C24 0.038(8) 0.027(6) 0.022(5) -0.002(4) 0.017(5) 0.001(5) C21 0.032(7) 0.023(6) 0.028(6) -0.003(4) 0.009(5) 0.006(5) C1 0.029(6) 0.022(6) 0.017(5) 0.005(4) 0.008(4) -0.005(5) C19 0.034(7) 0.011(5) 0.019(5) -0.006(4) 0.008(4) -0.006(5) C18 0.030(7) 0.016(5) 0.031(5) -0.005(5) 0.011(5) -0.002(6) C16 0.029(7) 0.033(6) 0.024(5) -0.011(5) 0.013(5) -0.008(6) C9 0.020(6) 0.037(7) 0.018(5) 0.012(4) 0.006(4) 0.008(5) C17 0.029(7) 0.027(6) 0.032(6) -0.009(5) 0.016(5) 0.002(6) C13 0.050(9) 0.028(7) 0.020(5) -0.001(4) 0.008(5) 0.007(6) C10 0.050(9) 0.026(6) 0.018(5) 0.011(4) 0.017(5) 0.020(6) C14 0.038(8) 0.017(6) 0.023(5) 0.004(4) 0.009(5) 0.006(5) C5 0.032(8) 0.048(8) 0.030(6) 0.007(5) 0.016(5) 0.005(6) C6 0.048(9) 0.053(9) 0.039(7) 0.001(6) 0.027(7) -0.024(7) C8 0.046(9) 0.048(8) 0.046(7) 0.004(6) 0.037(7) 0.004(7) C22 0.062(10) 0.022(6) 0.025(6) 0.007(4) 0.018(6) 0.015(6) C11 0.047(9) 0.049(8) 0.025(6) 0.005(6) 0.018(6) 0.017(7) C12 0.065(10) 0.036(8) 0.030(6) 0.002(5) 0.025(7) 0.018(7) C15 0.029(7) 0.017(5) 0.019(5) -0.002(4) 0.007(4) -0.001(5) C2 0.035(7) 0.022(6) 0.026(5) -0.002(4) 0.024(5) -0.004(5) C3 0.062(10) 0.036(8) 0.028(6) -0.002(5) 0.032(6) -0.002(7) C4 0.055(10) 0.023(6) 0.031(6) -0.004(5) 0.028(6) -0.019(6) N4 0.037(7) 0.040(7) 0.039(6) 0.005(5) 0.019(5) 0.007(6) N3 0.116(13) 0.037(7) 0.050(7) -0.008(6) 0.050(8) -0.027(8) C7 0.040(9) 0.064(10) 0.056(8) 0.014(7) 0.032(7) -0.008(8) O1 0.212(19) 0.054(8) 0.069(8) -0.011(7) 0.078(10) 0.022(9) C25 0.20(3) 0.078(18) 0.15(3) -0.005(17) 0.02(2) -0.01(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 S1 2.312(3) . ? Pt1 S2 2.325(3) . ? Pt1 S3 2.327(3) . ? Pt1 S4 2.330(3) . ? Co2 N5 2.098(10) . ? Co2 N2 2.095(8) . ? Co2 N6 2.124(8) . ? Co2 N1 2.133(8) . ? Co2 N7 2.135(9) . ? Co2 N8 2.143(8) . ? S1 C1 1.673(11) . ? S2 C2 1.659(11) 3_757 ? S3 C3 1.682(15) . ? S4 C4 1.628(15) . ? N2 C2 1.168(13) . ? N7 C19 1.342(13) . ? N7 C15 1.354(13) . ? N6 C14 1.340(14) . ? N6 C10 1.361(15) . ? N8 C20 1.334(14) . ? N8 C24 1.344(13) . ? N5 C5 1.327(16) . ? N5 C9 1.341(14) . ? N1 C1 1.136(13) . ? C23 C22 1.338(18) . ? C23 C24 1.401(16) . ? C23 H23 0.9300 . ? C20 C21 1.417(15) . ? C20 C19 1.486(15) . ? C24 H24 0.9300 . ? C21 C22 1.379(17) . ? C21 H21 0.9300 . ? C19 C18 1.370(16) . ? C18 C17 1.398(15) . ? C18 H18 0.9300 . ? C16 C17 1.386(16) . ? C16 C15 1.382(16) . ? C16 H16 0.9300 . ? C9 C8 1.396(17) . ? C9 C10 1.487(17) . ? C17 H17 0.9300 . ? C13 C12 1.395(19) . ? C13 C14 1.411(15) . ? C13 H13 0.9300 . ? C10 C11 1.397(15) . ? C14 H14 0.9300 . ? C5 C6 1.397(18) . ? C5 H5 0.9300 . ? C6 C7 1.376(19) . ? C6 H6 0.9300 . ? C8 C7 1.358(19) . ? C8 H8 0.9300 . ? C22 H22 0.9300 . ? C11 C12 1.357(19) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C15 H15 0.9300 . ? C2 S2 1.659(11) 3_757 ? C3 N3 1.160(17) . ? C4 N4 1.203(16) . ? C7 H7 0.9300 . ? O1 C25 1.47(3) . ? O1 H1 0.8200 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Pt1 S2 92.89(9) . . ? S1 Pt1 S3 171.79(10) . . ? S2 Pt1 S3 95.30(10) . . ? S1 Pt1 S4 82.03(10) . . ? S2 Pt1 S4 173.51(11) . . ? S3 Pt1 S4 89.76(11) . . ? N5 Co2 N2 92.8(4) . . ? N5 Co2 N6 77.9(4) . . ? N2 Co2 N6 89.0(3) . . ? N5 Co2 N1 95.7(4) . . ? N2 Co2 N1 88.6(3) . . ? N6 Co2 N1 173.0(4) . . ? N5 Co2 N7 172.4(3) . . ? N2 Co2 N7 94.8(3) . . ? N6 Co2 N7 101.5(3) . . ? N1 Co2 N7 85.3(3) . . ? N5 Co2 N8 95.9(3) . . ? N2 Co2 N8 171.2(4) . . ? N6 Co2 N8 94.4(3) . . ? N1 Co2 N8 89.0(3) . . ? N7 Co2 N8 76.6(3) . . ? C1 S1 Pt1 109.3(3) . . ? C2 S2 Pt1 104.7(4) 3_757 . ? C3 S3 Pt1 105.7(4) . . ? C4 S4 Pt1 104.3(4) . . ? C2 N2 Co2 173.4(9) . . ? C19 N7 C15 119.1(9) . . ? C19 N7 Co2 115.5(7) . . ? C15 N7 Co2 123.3(7) . . ? C14 N6 C10 119.7(10) . . ? C14 N6 Co2 125.3(7) . . ? C10 N6 Co2 115.0(7) . . ? C20 N8 C24 119.7(9) . . ? C20 N8 Co2 114.8(7) . . ? C24 N8 Co2 125.5(8) . . ? C5 N5 C9 118.5(10) . . ? C5 N5 Co2 125.5(8) . . ? C9 N5 Co2 116.0(8) . . ? C1 N1 Co2 159.6(10) . . ? C22 C23 C24 118.1(11) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? N8 C20 C21 120.5(10) . . ? N8 C20 C19 116.8(9) . . ? C21 C20 C19 122.7(11) . . ? N8 C24 C23 122.0(12) . . ? N8 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? C22 C21 C20 118.1(12) . . ? C22 C21 H21 120.9 . . ? C20 C21 H21 120.9 . . ? N1 C1 S1 176.9(9) . . ? N7 C19 C18 121.9(10) . . ? N7 C19 C20 114.1(10) . . ? C18 C19 C20 124.0(10) . . ? C19 C18 C17 119.4(11) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C17 C16 C15 118.6(11) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? N5 C9 C8 120.6(11) . . ? N5 C9 C10 116.2(10) . . ? C8 C9 C10 123.2(11) . . ? C16 C17 C18 118.9(11) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C12 C13 C14 117.1(12) . . ? C12 C13 H13 121.5 . . ? C14 C13 H13 121.5 . . ? N6 C10 C11 120.2(12) . . ? N6 C10 C9 115.0(9) . . ? C11 C10 C9 124.8(12) . . ? N6 C14 C13 122.3(12) . . ? N6 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? N5 C5 C6 123.9(12) . . ? N5 C5 H5 118.1 . . ? C6 C5 H5 118.1 . . ? C7 C6 C5 116.9(13) . . ? C7 C6 H6 121.5 . . ? C5 C6 H6 121.5 . . ? C7 C8 C9 120.3(12) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C23 C22 C21 121.5(11) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C12 C11 C10 120.3(13) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 120.5(11) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? N7 C15 C16 122.1(10) . . ? N7 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? N2 C2 S2 174.8(10) . 3_757 ? N3 C3 S3 175.7(11) . . ? N4 C4 S4 173.6(11) . . ? C8 C7 C6 119.8(13) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C25 O1 H1 109.5 . . ? O1 C25 H25A 109.5 . . ? O1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? data_C50H40Cu2N16O2Pt2S8 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C50 H40 Cu2 N16 O2 Pt2 S8' _chemical_formula_moiety 'C50 H40 Cu2 N16 O2 Pt2 S8' _chemical_formula_weight 1670.77 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' #------------------------------------------------ _cell_length_a 16.597(3) _cell_length_b 11.502(2) _cell_length_c 16.941(3) _cell_angle_alpha 90 _cell_angle_beta 116.685(2) _cell_angle_gamma 90 _cell_volume 2889.7(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6367 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.83 _cell_measurement_temperature 100 _exptl_crystal_description 'plate' _exptl_crystal_colour 'green' _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 1.920 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1620 _exptl_absorpt_coefficient_mu 5.896 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device 'Unknown' _diffrn_measurement_device_type 'Serial' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 16579 _reflns_number_total 6670 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_theta_min 1.427 _diffrn_reflns_theta_max 27.946 _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.990 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -21 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 22 #========================================================================== # 8. REFINEMENT DATA _atom_sites_solution_primary direct #heavy,direct,difmap,geom _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.78 _refine_diff_density_max 5.66 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 5206 _refine_ls_number_restraints 2 _refine_ls_number_parameters 357 _oxford_refine_ls_R_factor_ref 0.0458 _refine_ls_wR_factor_ref 0.0628 _refine_ls_goodness_of_fit_ref 1.1927 _refine_ls_shift/su_max 0.002745 _oxford_reflns_number_all 6670 _refine_ls_R_factor_all 0.0626 _refine_ls_wR_factor_all 0.0748 _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5412 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_gt 0.0648 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Pt1 Pt 0.398142(17) 0.33033(2) 1.044124(18) 0.0237 1.0000 Uani . . . . . . . Cu1 Cu 0.41251(5) 0.11054(8) 0.72791(5) 0.0220 1.0000 Uani . . . . . . . S1 S 0.39976(13) 0.41115(17) 0.91995(13) 0.0305 1.0000 Uani . . . . . . . S2 S 0.40578(15) 0.14232(17) 0.99876(13) 0.0329 1.0000 Uani . . . . . . . S3 S 0.39680(14) 0.2767(2) 1.17551(13) 0.0352 1.0000 Uani . . . . . . . S4 S 0.39523(13) 0.52531(17) 1.08129(16) 0.0353 1.0000 Uani . . . . . . . O11 O 0.0761(12) 0.0649(12) 0.0904(10) 0.0566 0.536(15) Uani D . P . 1 . . O12 O 0.0250(13) 0.0644(14) 0.0598(11) 0.0566 0.464(15) Uani D . P . 2 . . N1 N 0.4359(4) 0.2407(6) 0.8207(4) 0.0272 1.0000 Uani . . . . . . . N2 N 0.5202(4) 0.0184(6) 1.1516(4) 0.0304 1.0000 Uani . . . . . . . N3 N 0.2725(8) 0.0929(8) 1.1381(6) 0.0726 1.0000 Uani . . . . . . . N4 N 0.2183(5) 0.5667(7) 1.0614(5) 0.0419 1.0000 Uani . . . . . . . N5 N 0.2888(4) 0.0960(5) 0.7235(4) 0.0239 1.0000 Uani . . . . . . . N6 N 0.3319(4) 0.2350(6) 0.6217(4) 0.0280 1.0000 Uani . . . . . . . N7 N 0.5297(4) 0.1348(6) 0.7233(4) 0.0270 1.0000 Uani . . . . . . . N8 N 0.4087(4) -0.0295(6) 0.6506(4) 0.0279 1.0000 Uani . . . . . . . C1 C 0.4215(5) 0.3068(7) 0.8625(5) 0.0250 1.0000 Uani . . . . . . . C2 C 0.4741(5) 0.0722(6) 1.0914(5) 0.0250 1.0000 Uani . . . . . . . C3 C 0.3259(7) 0.1662(8) 1.1521(6) 0.0403 1.0000 Uani . . . . . . . C4 C 0.2895(6) 0.5433(7) 1.0704(5) 0.0311 1.0000 Uani . . . . . . . C5 C 0.2749(5) 0.0336(7) 0.7831(5) 0.0286 1.0000 Uani . . . . . . . C6 C 0.1962(5) 0.0434(7) 0.7939(5) 0.0332 1.0000 Uani . . . . . . . C7 C 0.1316(5) 0.1235(8) 0.7409(6) 0.0338 1.0000 Uani . . . . . . . C8 C 0.1457(5) 0.1875(7) 0.6793(6) 0.0309 1.0000 Uani . . . . . . . C9 C 0.2249(5) 0.1734(6) 0.6705(5) 0.0260 1.0000 Uani . . . . . . . C10 C 0.2459(5) 0.2392(6) 0.6077(5) 0.0252 1.0000 Uani . . . . . . . C11 C 0.1812(6) 0.3056(7) 0.5379(5) 0.0357 1.0000 Uani . . . . . . . C12 C 0.2078(6) 0.3671(8) 0.4850(6) 0.0420 1.0000 Uani . . . . . . . C13 C 0.2979(6) 0.3652(8) 0.5006(6) 0.0408 1.0000 Uani . . . . . . . C14 C 0.3567(6) 0.2953(8) 0.5688(6) 0.0395 1.0000 Uani . . . . . . . C15 C 0.5883(6) 0.2205(8) 0.7651(6) 0.0354 1.0000 Uani . . . . . . . C16 C 0.6682(6) 0.2323(9) 0.7580(6) 0.0436 1.0000 Uani . . . . . . . C17 C 0.6863(6) 0.1528(9) 0.7071(7) 0.0485 1.0000 Uani . . . . . . . C18 C 0.6271(6) 0.0672(8) 0.6647(6) 0.0415 1.0000 Uani . . . . . . . C19 C 0.5481(5) 0.0578(8) 0.6742(5) 0.0321 1.0000 Uani . . . . . . . C20 C 0.4801(5) -0.0338(7) 0.6323(5) 0.0314 1.0000 Uani . . . . . . . C21 C 0.4887(6) -0.1238(8) 0.5809(6) 0.0397 1.0000 Uani . . . . . . . C22 C 0.4224(7) -0.2076(9) 0.5472(6) 0.0482 1.0000 Uani . . . . . . . C23 C 0.3485(7) -0.2018(9) 0.5659(6) 0.0457 1.0000 Uani . . . . . . . C24 C 0.3459(6) -0.1104(8) 0.6180(5) 0.0373 1.0000 Uani . . . . . . . C251 C 0.0711(17) -0.0048(19) 0.1590(12) 0.0544 0.536(15) Uani D . P . 1 . . C252 C 0.0627(19) -0.017(2) 0.1319(14) 0.0544 0.464(15) Uani D . P . 2 . . H11 H 0.1348 0.0739 0.1044 0.0712 0.536(15) Uiso R . P . 1 . . H12 H -0.0084 0.0231 0.0107 0.0692 0.464(15) Uiso R . P . 2 . . H51 H 0.3202 -0.0194 0.8195 0.0331 1.0000 Uiso R . . . . . . H61 H 0.1872 -0.0029 0.8358 0.0409 1.0000 Uiso R . . . . . . H71 H 0.0780 0.1341 0.7471 0.0410 1.0000 Uiso R . . . . . . H81 H 0.1013 0.2415 0.6427 0.0360 1.0000 Uiso R . . . . . . H111 H 0.1202 0.3074 0.5280 0.0401 1.0000 Uiso R . . . . . . H121 H 0.1649 0.4115 0.4374 0.0469 1.0000 Uiso R . . . . . . H131 H 0.3180 0.4101 0.4658 0.0499 1.0000 Uiso R . . . . . . H141 H 0.4175 0.2900 0.5783 0.0488 1.0000 Uiso R . . . . . . H151 H 0.5750 0.2742 0.8002 0.0457 1.0000 Uiso R . . . . . . H161 H 0.7092 0.2935 0.7874 0.0548 1.0000 Uiso R . . . . . . H171 H 0.7408 0.1584 0.7019 0.0634 1.0000 Uiso R . . . . . . H181 H 0.6391 0.0136 0.6286 0.0563 1.0000 Uiso R . . . . . . H211 H 0.5397 -0.1272 0.5695 0.0479 1.0000 Uiso R . . . . . . H221 H 0.4268 -0.2686 0.5116 0.0564 1.0000 Uiso R . . . . . . H231 H 0.3019 -0.2584 0.5437 0.0498 1.0000 Uiso R . . . . . . H241 H 0.2959 -0.1057 0.6310 0.0416 1.0000 Uiso R . . . . . . H2511 H 0.1020 0.0343 0.2140 0.0678 0.536(15) Uiso R . P . 1 . . H2512 H 0.0989 -0.0779 0.1618 0.0678 0.536(15) Uiso R . P . 1 . . H2513 H 0.0100 -0.0166 0.1470 0.0678 0.536(15) Uiso R . P . 1 . . H2521 H 0.0970 0.0246 0.1849 0.0678 0.464(15) Uiso R . P . 2 . . H2522 H 0.1003 -0.0730 0.1232 0.0678 0.464(15) Uiso R . P . 2 . . H2523 H 0.0143 -0.0560 0.1362 0.0678 0.464(15) Uiso R . P . 2 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02295(16) 0.02092(16) 0.02812(17) -0.00386(12) 0.01231(11) 0.00102(11) Cu1 0.0214(4) 0.0254(5) 0.0210(4) 0.0000(4) 0.0109(3) 0.0046(3) S1 0.0348(10) 0.0224(9) 0.0375(11) 0.0028(8) 0.0192(8) 0.0050(8) S2 0.0544(12) 0.0206(9) 0.0233(9) -0.0009(7) 0.0172(9) 0.0039(8) S3 0.0383(11) 0.0391(12) 0.0330(10) -0.0080(9) 0.0201(9) -0.0029(9) S4 0.0353(10) 0.0238(10) 0.0561(13) -0.0112(9) 0.0288(10) -0.0063(8) O11 0.056(3) 0.056(3) 0.056(3) -0.004(3) 0.023(3) -0.004(3) O12 0.056(3) 0.056(3) 0.056(3) -0.004(3) 0.023(3) -0.004(3) N1 0.032(3) 0.027(3) 0.026(3) 0.001(3) 0.016(3) -0.002(3) N2 0.028(3) 0.031(4) 0.033(4) -0.006(3) 0.014(3) 0.001(3) N3 0.127(9) 0.049(6) 0.070(6) -0.017(5) 0.069(6) -0.043(6) N4 0.036(4) 0.041(4) 0.060(5) 0.010(4) 0.031(4) 0.012(3) N5 0.018(3) 0.023(3) 0.025(3) -0.006(3) 0.004(2) -0.001(2) N6 0.030(3) 0.028(4) 0.026(3) -0.007(3) 0.013(3) 0.002(3) N7 0.029(3) 0.029(3) 0.026(3) 0.009(3) 0.015(3) 0.008(3) N8 0.024(3) 0.033(4) 0.023(3) 0.008(3) 0.008(2) 0.008(3) C1 0.024(3) 0.026(4) 0.022(4) 0.009(3) 0.008(3) -0.002(3) C2 0.027(4) 0.026(4) 0.025(4) -0.008(3) 0.014(3) 0.001(3) C3 0.063(6) 0.033(5) 0.040(5) 0.003(4) 0.037(5) 0.006(4) C4 0.054(5) 0.020(4) 0.027(4) -0.002(3) 0.025(4) -0.003(3) C5 0.025(4) 0.031(4) 0.027(4) -0.004(3) 0.009(3) 0.001(3) C6 0.035(4) 0.033(4) 0.035(4) -0.010(4) 0.018(3) -0.005(3) C7 0.023(4) 0.034(4) 0.045(5) -0.010(4) 0.016(3) 0.000(3) C8 0.024(4) 0.026(4) 0.040(4) -0.005(3) 0.012(3) 0.006(3) C9 0.023(3) 0.019(4) 0.029(4) -0.012(3) 0.005(3) -0.002(3) C10 0.029(4) 0.020(4) 0.025(4) -0.006(3) 0.010(3) 0.004(3) C11 0.035(4) 0.028(4) 0.037(5) -0.003(3) 0.010(4) 0.011(3) C12 0.057(6) 0.028(4) 0.032(5) 0.001(4) 0.012(4) 0.012(4) C13 0.059(6) 0.038(5) 0.027(4) -0.002(4) 0.021(4) 0.004(4) C14 0.041(5) 0.047(5) 0.034(4) -0.005(4) 0.020(4) 0.002(4) C15 0.040(4) 0.033(5) 0.041(5) 0.000(4) 0.026(4) -0.003(4) C16 0.037(5) 0.050(6) 0.050(5) -0.001(5) 0.026(4) -0.007(4) C17 0.033(4) 0.061(7) 0.065(6) 0.014(5) 0.033(4) 0.005(4) C18 0.042(5) 0.048(6) 0.051(5) 0.004(4) 0.036(4) 0.006(4) C19 0.034(4) 0.039(5) 0.031(4) 0.011(4) 0.022(3) 0.011(3) C20 0.034(4) 0.034(4) 0.027(4) 0.006(3) 0.014(3) 0.014(3) C21 0.043(5) 0.045(5) 0.032(4) 0.001(4) 0.017(4) 0.013(4) C22 0.068(6) 0.038(5) 0.035(5) 0.000(4) 0.020(5) 0.019(5) C23 0.044(5) 0.045(5) 0.037(5) 0.006(4) 0.007(4) 0.000(4) C24 0.037(4) 0.039(5) 0.028(4) 0.010(4) 0.008(3) 0.013(4) C251 0.053(3) 0.053(3) 0.053(3) -0.007(3) 0.020(3) -0.007(3) C252 0.053(3) 0.053(3) 0.053(3) -0.007(3) 0.020(3) -0.007(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . S1 . 2.311(2) yes Pt1 . S2 . 2.318(2) yes Pt1 . S3 . 2.320(2) yes Pt1 . S4 . 2.336(2) yes Cu1 . N2 2_657 2.359(7) yes Cu1 . N1 . 2.078(7) yes Cu1 . N5 . 2.028(6) yes Cu1 . N6 . 2.216(6) yes Cu1 . N7 . 2.000(6) yes Cu1 . N8 . 2.059(7) yes Cu1 . C19 . 2.846(7) yes Cu1 . C20 . 2.875(8) yes S1 . C1 . 1.684(8) yes S2 . C2 . 1.673(8) yes S3 . C3 . 1.655(10) yes S4 . C4 . 1.692(9) yes O11 . C251 . 1.446(9) yes O11 . H11 . 0.900 no O12 . C252 . 1.443(9) yes O12 . H12 . 0.900 no N1 . C1 . 1.134(10) yes N2 . C2 . 1.144(9) yes N3 . C3 . 1.168(12) yes N4 . C4 . 1.154(10) yes N5 . C5 . 1.340(10) yes N5 . C9 . 1.368(9) yes N6 . C10 . 1.337(9) yes N6 . C14 . 1.338(11) yes N7 . C15 . 1.342(11) yes N7 . C19 . 1.342(10) yes N8 . C20 . 1.353(10) yes N8 . C24 . 1.319(11) yes C5 . C6 . 1.403(11) yes C5 . H51 . 0.950 no C6 . C7 . 1.393(12) yes C6 . H61 . 0.950 no C7 . C8 . 1.380(12) yes C7 . H71 . 0.950 no C8 . C9 . 1.397(11) yes C8 . H81 . 0.950 no C9 . C10 . 1.471(11) yes C10 . C11 . 1.412(10) yes C11 . C12 . 1.361(13) yes C11 . H111 . 0.950 no C12 . C13 . 1.397(13) yes C12 . H121 . 0.950 no C13 . C14 . 1.387(12) yes C13 . H131 . 0.950 no C14 . H141 . 0.950 no C15 . C16 . 1.390(11) yes C15 . H151 . 0.950 no C16 . C17 . 1.380(14) yes C16 . H161 . 0.950 no C17 . C18 . 1.348(13) yes C17 . H171 . 0.950 no C18 . C19 . 1.395(11) yes C18 . H181 . 0.950 no C19 . C20 . 1.473(12) yes C20 . C21 . 1.401(12) yes C21 . C22 . 1.379(15) yes C21 . H211 . 0.950 no C22 . C23 . 1.399(15) yes C22 . H221 . 0.950 no C23 . C24 . 1.386(14) yes C23 . H231 . 0.950 no C24 . H241 . 0.950 no C251 . H2511 . 0.950 no C251 . H2512 . 0.950 no C251 . H2513 . 0.950 no C252 . H2521 . 0.950 no C252 . H2522 . 0.950 no C252 . H2523 . 0.950 no H12 . H12 2_555 0.764 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 . Pt1 . S2 . 92.79(7) yes S1 . Pt1 . S3 . 171.71(7) yes S2 . Pt1 . S3 . 95.48(8) yes S1 . Pt1 . S4 . 82.49(8) yes S2 . Pt1 . S4 . 174.99(7) yes S3 . Pt1 . S4 . 89.22(8) yes N2 2_657 Cu1 . N1 . 86.7(2) yes N2 2_657 Cu1 . N5 . 93.3(2) yes N1 . Cu1 . N5 . 85.9(2) yes N2 2_657 Cu1 . N6 . 170.7(2) yes N1 . Cu1 . N6 . 89.3(2) yes N5 . Cu1 . N6 . 77.9(2) yes N2 2_657 Cu1 . N7 . 91.7(2) yes N1 . Cu1 . N7 . 94.2(3) yes N5 . Cu1 . N7 . 174.9(2) yes N6 . Cu1 . N7 . 97.0(2) yes N2 2_657 Cu1 . N8 . 85.8(2) yes N1 . Cu1 . N8 . 170.8(2) yes N5 . Cu1 . N8 . 99.8(2) yes N6 . Cu1 . N8 . 98.9(2) yes N7 . Cu1 . N8 . 80.6(3) yes N2 2_657 Cu1 . C19 . 90.4(2) yes N1 . Cu1 . C19 . 119.3(2) yes N5 . Cu1 . C19 . 154.7(2) yes N6 . Cu1 . C19 . 98.9(2) yes N7 . Cu1 . C19 . 25.2(3) yes N2 2_657 Cu1 . C20 . 88.4(2) yes N1 . Cu1 . C20 . 148.7(2) yes N5 . Cu1 . C20 . 125.2(2) yes N6 . Cu1 . C20 . 99.3(2) yes N7 . Cu1 . C20 . 55.0(3) yes N8 . Cu1 . C19 . 55.4(2) yes N8 . Cu1 . C20 . 25.6(2) yes C19 . Cu1 . C20 . 29.8(2) yes Pt1 . S1 . C1 . 109.5(3) yes Pt1 . S2 . C2 . 104.7(3) yes Pt1 . S3 . C3 . 106.6(3) yes Pt1 . S4 . C4 . 103.5(3) yes C251 . O11 . H11 . 107.4 no C252 . O12 . H12 . 107.0 no Cu1 . N1 . C1 . 159.2(6) yes Cu1 2_657 N2 . C2 . 168.3(6) yes Cu1 . N5 . C5 . 122.1(5) yes Cu1 . N5 . C9 . 116.4(5) yes C5 . N5 . C9 . 119.8(6) yes Cu1 . N6 . C10 . 112.0(5) yes Cu1 . N6 . C14 . 128.6(5) yes C10 . N6 . C14 . 119.1(7) yes Cu1 . N7 . C15 . 124.7(5) yes Cu1 . N7 . C19 . 115.4(5) yes C15 . N7 . C19 . 119.9(7) yes Cu1 . N8 . C20 . 113.2(5) yes Cu1 . N8 . C24 . 127.6(6) yes C20 . N8 . C24 . 119.2(7) yes S1 . C1 . N1 . 176.5(7) yes S2 . C2 . N2 . 175.8(7) yes S3 . C3 . N3 . 175.1(9) yes S4 . C4 . N4 . 173.4(7) yes N5 . C5 . C6 . 122.8(7) yes N5 . C5 . H51 . 118.6 no C6 . C5 . H51 . 118.6 no C5 . C6 . C7 . 117.4(8) yes C5 . C6 . H61 . 121.3 no C7 . C6 . H61 . 121.3 no C6 . C7 . C8 . 119.9(7) yes C6 . C7 . H71 . 120.1 no C8 . C7 . H71 . 120.1 no C7 . C8 . C9 . 120.3(7) yes C7 . C8 . H81 . 119.8 no C9 . C8 . H81 . 119.8 no C8 . C9 . N5 . 119.7(7) yes C8 . C9 . C10 . 123.9(7) yes N5 . C9 . C10 . 116.3(6) yes C9 . C10 . N6 . 115.7(6) yes C9 . C10 . C11 . 123.1(7) yes N6 . C10 . C11 . 121.2(7) yes C10 . C11 . C12 . 118.9(8) yes C10 . C11 . H111 . 120.6 no C12 . C11 . H111 . 120.6 no C11 . C12 . C13 . 120.2(8) yes C11 . C12 . H121 . 119.9 no C13 . C12 . H121 . 119.9 no C12 . C13 . C14 . 117.4(9) yes C12 . C13 . H131 . 121.3 no C14 . C13 . H131 . 121.3 no C13 . C14 . N6 . 123.1(8) yes C13 . C14 . H141 . 118.4 no N6 . C14 . H141 . 118.5 no N7 . C15 . C16 . 121.4(8) yes N7 . C15 . H151 . 119.3 no C16 . C15 . H151 . 119.3 no C15 . C16 . C17 . 118.2(9) yes C15 . C16 . H161 . 120.9 no C17 . C16 . H161 . 120.9 no C16 . C17 . C18 . 120.5(8) yes C16 . C17 . H171 . 119.8 no C18 . C17 . H171 . 119.7 no C17 . C18 . C19 . 119.5(9) yes C17 . C18 . H181 . 120.3 no C19 . C18 . H181 . 120.3 no C18 . C19 . N7 . 120.6(8) yes C18 . C19 . Cu1 . 160.0(7) yes N7 . C19 . Cu1 . 39.4(4) yes C18 . C19 . C20 . 123.8(8) yes N7 . C19 . C20 . 115.6(7) yes Cu1 . C19 . C20 . 76.2(4) yes C19 . C20 . N8 . 115.1(7) yes C19 . C20 . Cu1 . 74.0(4) yes N8 . C20 . Cu1 . 41.2(4) yes C19 . C20 . C21 . 123.9(8) yes N8 . C20 . C21 . 120.9(8) yes Cu1 . C20 . C21 . 162.1(7) yes C20 . C21 . C22 . 119.2(9) yes C20 . C21 . H211 . 120.4 no C22 . C21 . H211 . 120.4 no C21 . C22 . C23 . 119.4(9) yes C21 . C22 . H221 . 120.3 no C23 . C22 . H221 . 120.3 no C22 . C23 . C24 . 117.5(9) yes C22 . C23 . H231 . 121.2 no C24 . C23 . H231 . 121.3 no C23 . C24 . N8 . 123.8(9) yes C23 . C24 . H241 . 118.1 no N8 . C24 . H241 . 118.1 no O11 . C251 . H2511 . 108.9 no O11 . C251 . H2512 . 109.2 no H2511 . C251 . H2512 . 109.5 no O11 . C251 . H2513 . 110.3 no H2511 . C251 . H2513 . 109.5 no H2512 . C251 . H2513 . 109.5 no O12 . C252 . H2521 . 108.5 no O12 . C252 . H2522 . 111.8 no H2521 . C252 . H2522 . 109.5 no O12 . C252 . H2523 . 108.0 no H2521 . C252 . H2523 . 109.5 no H2522 . C252 . H2523 . 109.5 no H12 2_555 H12 . O12 . 126.9 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag O11 . H11 . N3 1_554 179 0.90 2.10 3.002(15) yes O12 . H12 . O11 2_555 179 0.90 1.87 2.769(15) yes O12 . H12 . O12 2_555 156 0.90 1.49 2.340(15) yes O12 . H12 . C251 2_555 147 0.90 2.59 3.383(15) yes O12 . H12 . C252 2_555 145 0.90 2.17 2.952(15) yes C5 . H51 . N2 2_657 126 0.95 2.47 3.126(15) yes C14 . H141 . O12 4_555 133 0.95 2.57 3.288(15) yes C18 . H181 . N4 4_554 156 0.95 2.28 3.178(15) yes C22 . H221 . O11 3_545 175 0.95 2.57 3.513(15) yes C22 . H221 . O12 3_545 168 0.95 2.58 3.515(15) yes data_C46H32Cu2N14PtS6 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_moiety ? _chemical_formula_sum 'C46 H32 Cu2 N14 Pt S6' _chemical_formula_weight 1295.39 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' #------------------------------------------------ _cell_length_a 9.0049(13) _cell_length_b 11.9725(17) _cell_length_c 12.6910(18) _cell_angle_alpha 68.519(2) _cell_angle_beta 87.540(2) _cell_angle_gamma 70.532(2) _cell_volume 1195.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173 _cell_measurement_reflns_used 7994 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.93 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 638 _exptl_absorpt_coefficient_mu 4.113 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5572 _exptl_absorpt_correction_T_max 0.8495 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13782 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.93 _reflns_number_total 10520 _reflns_number_gt 9688 _reflns_threshold_expression >2sigma(I) _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 27.93 _diffrn_measured_fraction_theta_full 0.960 #========================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.7501P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.18(3) _refine_ls_number_reflns 10520 _refine_ls_number_parameters 622 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0620 _refine_ls_wR_factor_gt 0.0602 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.108 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.094 #========================================================== # 9. General computing _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.86382(8) 0.23775(6) 0.28453(5) 0.01708(4) Uani 1 1 d . . . Cu2 Cu 0.78953(10) 0.88501(8) 0.97986(7) 0.0170(3) Uani 1 1 d . . . Cu1 Cu -0.06155(10) 0.59029(8) 0.58923(7) 0.0166(3) Uani 1 1 d . . . S4 S 0.9809(3) 0.2115(2) 0.1241(2) 0.0246(5) Uani 1 1 d . . . S2 S 0.7469(3) 0.2647(2) 0.4447(2) 0.0252(5) Uani 1 1 d . . . N13 N 0.8647(9) 0.7070(7) 1.0942(6) 0.0183(15) Uani 1 1 d . . . C37 C 0.9939(11) 0.6162(8) 1.0848(8) 0.025(2) Uani 1 1 d . . . H37 H 1.0456 0.6356 1.0170 0.030 Uiso 1 1 calc R . . C39 C 0.9768(11) 0.4736(9) 1.2693(8) 0.029(2) Uani 1 1 d . . . H39 H 1.0158 0.3935 1.3307 0.035 Uiso 1 1 calc R . . C41 C 0.7893(10) 0.6850(8) 1.1881(7) 0.0187(18) Uani 1 1 d . . . C40 C 0.8447(11) 0.5669(8) 1.2788(8) 0.0217(19) Uani 1 1 d . . . H40 H 0.7913 0.5515 1.3461 0.026 Uiso 1 1 calc R . . C38 C 1.0561(11) 0.4957(9) 1.1683(8) 0.025(2) Uani 1 1 d . . . H38 H 1.1461 0.4317 1.1588 0.030 Uiso 1 1 calc R . . N8 N 0.0949(8) 0.5727(6) 0.4636(6) 0.0136(14) Uani 1 1 d . . . C16 C 0.2147(10) 0.4686(8) 0.4655(7) 0.0194(18) Uani 1 1 d . . . H16 H 0.2272 0.3898 0.5264 0.023 Uiso 1 1 calc R . . C15 C 0.3209(11) 0.4703(9) 0.3833(8) 0.025(2) Uani 1 1 d . . . H15 H 0.4040 0.3948 0.3868 0.030 Uiso 1 1 calc R . . C13 C 0.1805(11) 0.6936(9) 0.2919(7) 0.0213(19) Uani 1 1 d . . . H13 H 0.1667 0.7739 0.2328 0.026 Uiso 1 1 calc R . . C12 C 0.0757(10) 0.6851(8) 0.3763(6) 0.0170(17) Uani 1 1 d . . . S1 S 1.0812(3) 0.0586(2) 0.3871(2) 0.0257(5) Uani 1 1 d . . . S3 S 0.6466(3) 0.4166(2) 0.1822(2) 0.0243(5) Uani 1 1 d . . . C4 C 0.8770(11) 0.3364(9) 0.0069(8) 0.0240(19) Uani 1 1 d . . . N4 N 0.8181(10) 0.4188(8) -0.0753(7) 0.035(2) Uani 1 1 d . . . N5 N -0.2703(9) 0.5732(7) 0.5766(6) 0.0239(17) Uani 1 1 d . . . C5 C -0.4083(10) 0.6045(7) 0.5702(7) 0.0159(17) Uani 1 1 d . . . C21 C 0.1432(10) 0.5227(8) 0.7861(7) 0.0168(17) Uani 1 1 d . . . C17 C 0.0468(10) 0.7437(8) 0.7000(7) 0.0212(19) Uani 1 1 d . . . H17 H -0.0207 0.8192 0.6431 0.025 Uiso 1 1 calc R . . C22 C 0.1324(9) 0.4026(8) 0.7871(7) 0.0175(17) Uani 1 1 d . . . C24 C 0.1850(11) 0.1773(9) 0.8658(8) 0.028(2) Uani 1 1 d . . . H24 H 0.2348 0.0954 0.9229 0.034 Uiso 1 1 calc R . . C23 C 0.2078(10) 0.2822(8) 0.8722(7) 0.0203(19) Uani 1 1 d . . . H23 H 0.2736 0.2737 0.9332 0.024 Uiso 1 1 calc R . . N10 N 0.0375(9) 0.4139(7) 0.7018(6) 0.0174(15) Uani 1 1 d . . . N9 N 0.0477(8) 0.6294(6) 0.7045(6) 0.0167(15) Uani 1 1 d . . . N6 N 1.0001(9) 0.9022(7) 0.9937(7) 0.0229(17) Uani 1 1 d . . . N12 N 0.6902(9) 1.0617(7) 0.8689(6) 0.0181(15) Uani 1 1 d . . . N11 N 0.6784(8) 0.8474(7) 0.8643(6) 0.0176(15) Uani 1 1 d . . . C31 C 0.5832(10) 0.9541(8) 0.7827(7) 0.0181(18) Uani 1 1 d . . . C30 C 0.4819(10) 0.9495(8) 0.7068(7) 0.0197(18) Uani 1 1 d . . . H30 H 0.4119 1.0259 0.6522 0.024 Uiso 1 1 calc R . . C32 C 0.5948(10) 1.0765(8) 0.7809(7) 0.0168(17) Uani 1 1 d . . . C36 C 0.7112(10) 1.1670(8) 0.8729(7) 0.0224(19) Uani 1 1 d . . . H36 H 0.7777 1.1578 0.9338 0.027 Uiso 1 1 calc R . . C27 C 0.6787(10) 0.7336(8) 0.8690(7) 0.0204(18) Uani 1 1 d . . . H27 H 0.7458 0.6586 0.9267 0.025 Uiso 1 1 calc R . . C6 C 1.1372(11) 0.8694(8) 0.9996(7) 0.0194(18) Uani 1 1 d . . . C1 C 1.1875(12) 0.1273(10) 0.4319(9) 0.033(2) Uani 1 1 d . . . C25 C 0.0895(11) 0.1906(8) 0.7765(8) 0.024(2) Uani 1 1 d . . . H25 H 0.0752 0.1182 0.7700 0.029 Uiso 1 1 calc R . . C26 C 0.0156(10) 0.3111(8) 0.6973(7) 0.0229(19) Uani 1 1 d . . . H26 H -0.0533 0.3213 0.6373 0.027 Uiso 1 1 calc R . . C14 C 0.3005(11) 0.5902(9) 0.2929(7) 0.0227(19) Uani 1 1 d . . . H14 H 0.3707 0.5965 0.2346 0.027 Uiso 1 1 calc R . . C3 C 0.5369(11) 0.3510(8) 0.1359(7) 0.0244(19) Uani 1 1 d . . . C11 C -0.0639(9) 0.7942(8) 0.3778(7) 0.0150(16) Uani 1 1 d . . . C29 C 0.4844(11) 0.8283(8) 0.7121(7) 0.025(2) Uani 1 1 d . . . H29 H 0.4174 0.8219 0.6604 0.030 Uiso 1 1 calc R . . C28 C 0.5859(11) 0.7208(9) 0.7935(8) 0.025(2) Uani 1 1 d . . . H28 H 0.5921 0.6384 0.7978 0.030 Uiso 1 1 calc R . . C35 C 0.6385(11) 1.2882(8) 0.7909(8) 0.025(2) Uani 1 1 d . . . H35 H 0.6554 1.3605 0.7956 0.030 Uiso 1 1 calc R . . C33 C 0.5198(10) 1.1927(8) 0.6972(7) 0.0213(19) Uani 1 1 d . . . H33 H 0.4544 1.1993 0.6369 0.026 Uiso 1 1 calc R . . C18 C 0.1429(11) 0.7539(9) 0.7774(8) 0.024(2) Uani 1 1 d . . . H18 H 0.1384 0.8349 0.7759 0.028 Uiso 1 1 calc R . . C19 C 0.2456(10) 0.6410(9) 0.8567(7) 0.026(2) Uani 1 1 d . . . H19 H 0.3166 0.6452 0.9072 0.031 Uiso 1 1 calc R . . C20 C 0.2459(11) 0.5267(9) 0.8629(8) 0.024(2) Uani 1 1 d . . . H20 H 0.3144 0.4503 0.9183 0.028 Uiso 1 1 calc R . . C42 C 0.6505(10) 0.7922(8) 1.1918(7) 0.0174(17) Uani 1 1 d . . . C46 C 0.5118(9) 1.0078(8) 1.1040(7) 0.0194(18) Uani 1 1 d . . . H46 H 0.4981 1.0873 1.0438 0.023 Uiso 1 1 calc R . . C43 C 0.5499(11) 0.7802(9) 1.2769(7) 0.0218(19) Uani 1 1 d . . . H43 H 0.5649 0.7002 1.3368 0.026 Uiso 1 1 calc R . . N14 N 0.6313(9) 0.9046(7) 1.1052(6) 0.0191(16) Uani 1 1 d . . . N7 N -0.1394(9) 0.7685(7) 0.4752(6) 0.0205(16) Uani 1 1 d . . . N1 N 1.2715(12) 0.1660(8) 0.4638(8) 0.047(3) Uani 1 1 d . . . N3 N 0.4596(10) 0.3079(8) 0.1037(8) 0.039(2) Uani 1 1 d . . . S5 S -0.6013(3) 0.6499(2) 0.5605(2) 0.0213(5) Uani 1 1 d . . . S6 S 1.3288(3) 0.8256(2) 1.0090(2) 0.0209(5) Uani 1 1 d . . . C10 C -0.1204(11) 0.9115(8) 0.2884(7) 0.0217(19) Uani 1 1 d . . . H10 H -0.0680 0.9276 0.2207 0.026 Uiso 1 1 calc R . . C9 C -0.2548(10) 1.0053(8) 0.2991(7) 0.0229(19) Uani 1 1 d . . . H9 H -0.2964 1.0859 0.2385 0.027 Uiso 1 1 calc R . . C7 C -0.2672(10) 0.8626(9) 0.4836(9) 0.028(2) Uani 1 1 d . . . H7 H -0.3188 0.8473 0.5517 0.034 Uiso 1 1 calc R . . C8 C -0.3249(11) 0.9797(8) 0.3968(9) 0.032(2) Uani 1 1 d . . . H8 H -0.4155 1.0436 0.4057 0.038 Uiso 1 1 calc R . . C45 C 0.4072(10) 1.0030(9) 1.1877(7) 0.0215(19) Uani 1 1 d . . . H45 H 0.3248 1.0785 1.1850 0.026 Uiso 1 1 calc R . . C44 C 0.4226(11) 0.8917(9) 1.2719(8) 0.028(2) Uani 1 1 d . . . H44 H 0.3492 0.8871 1.3281 0.033 Uiso 1 1 calc R . . C2 C 0.8487(11) 0.1397(9) 0.5600(8) 0.0222(19) Uani 1 1 d . . . C34 C 0.5407(10) 1.3016(8) 0.7018(7) 0.0219(19) Uani 1 1 d . . . H34 H 0.4890 1.3833 0.6450 0.026 Uiso 1 1 calc R . . N2 N 0.9132(10) 0.0577(8) 0.6448(8) 0.034(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01665(7) 0.01831(7) 0.01877(7) -0.00915(5) 0.00314(5) -0.00674(5) Cu2 0.0191(7) 0.0145(7) 0.0155(6) -0.0024(5) -0.0003(5) -0.0067(6) Cu1 0.0159(7) 0.0147(7) 0.0170(7) -0.0023(5) 0.0017(5) -0.0065(6) S4 0.0238(13) 0.0265(13) 0.0207(12) -0.0114(10) 0.0067(10) -0.0029(10) S2 0.0257(13) 0.0234(13) 0.0195(12) -0.0064(10) 0.0024(10) -0.0017(10) N13 0.018(4) 0.016(4) 0.019(4) -0.003(3) 0.000(3) -0.007(3) C37 0.025(5) 0.021(5) 0.023(5) -0.002(4) 0.005(4) -0.009(4) C39 0.033(5) 0.016(4) 0.039(5) -0.002(4) -0.015(4) -0.016(4) C41 0.027(5) 0.016(4) 0.012(4) 0.003(3) -0.010(3) -0.013(4) C40 0.026(5) 0.020(4) 0.026(5) -0.009(4) 0.000(4) -0.015(4) C38 0.026(5) 0.024(5) 0.033(5) -0.018(4) 0.004(4) -0.010(4) N8 0.009(3) 0.012(3) 0.017(3) -0.006(3) -0.002(3) 0.001(3) C16 0.024(5) 0.019(4) 0.017(4) -0.003(3) -0.001(3) -0.012(4) C15 0.023(5) 0.021(5) 0.030(5) -0.008(4) 0.000(4) -0.007(4) C13 0.027(5) 0.029(5) 0.014(4) -0.006(4) 0.007(3) -0.019(4) C12 0.027(5) 0.018(4) 0.007(3) 0.001(3) -0.005(3) -0.014(4) S1 0.0233(13) 0.0237(13) 0.0258(12) -0.0106(10) 0.0020(10) -0.0011(10) S3 0.0264(13) 0.0211(12) 0.0226(12) -0.0078(10) -0.0007(10) -0.0045(10) C4 0.021(5) 0.024(5) 0.028(5) -0.013(4) 0.005(4) -0.006(4) N4 0.040(5) 0.031(5) 0.018(4) -0.004(4) 0.009(4) 0.001(4) N5 0.025(4) 0.023(4) 0.021(4) -0.004(3) 0.003(3) -0.010(3) C5 0.022(5) 0.013(4) 0.013(4) -0.005(3) 0.003(3) -0.006(3) C21 0.020(4) 0.020(4) 0.016(4) -0.012(4) 0.008(3) -0.008(4) C17 0.025(5) 0.017(4) 0.025(5) -0.011(4) 0.013(4) -0.009(4) C22 0.013(4) 0.016(4) 0.013(4) 0.004(3) 0.005(3) -0.003(3) C24 0.024(5) 0.018(4) 0.029(5) 0.004(4) 0.006(4) -0.005(4) C23 0.024(5) 0.018(4) 0.016(4) -0.002(3) 0.002(4) -0.010(4) N10 0.021(4) 0.017(4) 0.016(3) -0.003(3) 0.002(3) -0.012(3) N9 0.020(4) 0.014(3) 0.012(3) -0.001(3) 0.003(3) -0.005(3) N6 0.019(4) 0.022(4) 0.029(4) -0.007(3) 0.000(3) -0.011(3) N12 0.018(4) 0.014(4) 0.018(4) -0.004(3) 0.003(3) -0.005(3) N11 0.018(4) 0.020(4) 0.022(4) -0.011(3) 0.007(3) -0.010(3) C31 0.014(4) 0.020(4) 0.017(4) -0.002(3) 0.003(3) -0.007(4) C30 0.020(5) 0.023(5) 0.017(4) -0.008(4) 0.003(3) -0.009(4) C32 0.018(4) 0.018(4) 0.021(4) -0.013(3) 0.005(3) -0.009(3) C36 0.025(5) 0.025(5) 0.031(5) -0.019(4) 0.007(4) -0.016(4) C27 0.020(4) 0.022(5) 0.019(4) -0.006(4) 0.002(3) -0.009(4) C6 0.029(5) 0.020(4) 0.015(4) -0.004(3) 0.003(3) -0.018(4) C1 0.022(5) 0.025(5) 0.037(6) -0.001(4) 0.002(4) 0.000(4) C25 0.025(5) 0.017(4) 0.035(5) -0.014(4) 0.006(4) -0.009(4) C26 0.026(5) 0.021(4) 0.016(4) 0.003(3) -0.001(3) -0.012(4) C14 0.024(4) 0.036(5) 0.013(4) -0.007(3) 0.005(3) -0.019(4) C3 0.027(5) 0.017(4) 0.020(4) -0.002(4) -0.006(4) -0.001(4) C11 0.013(4) 0.019(4) 0.020(4) -0.013(3) 0.004(3) -0.008(3) C29 0.042(5) 0.028(4) 0.020(4) -0.016(4) 0.008(4) -0.025(4) C28 0.033(5) 0.024(5) 0.027(5) -0.013(4) 0.010(4) -0.018(4) C35 0.030(5) 0.017(4) 0.022(4) 0.002(3) 0.005(4) -0.014(4) C33 0.014(4) 0.026(5) 0.021(4) -0.009(4) 0.001(3) -0.002(4) C18 0.027(5) 0.027(5) 0.027(5) -0.019(4) 0.008(4) -0.012(4) C19 0.015(4) 0.038(5) 0.021(4) -0.011(4) 0.003(3) -0.005(4) C20 0.024(5) 0.026(5) 0.020(4) -0.010(4) 0.003(4) -0.007(4) C42 0.011(4) 0.020(4) 0.024(4) -0.013(4) 0.000(3) -0.004(3) C46 0.012(4) 0.021(4) 0.022(4) -0.009(4) -0.004(3) 0.000(3) C43 0.028(5) 0.023(5) 0.018(4) -0.008(4) -0.001(4) -0.012(4) N14 0.024(4) 0.025(4) 0.011(3) -0.003(3) -0.002(3) -0.016(3) N7 0.021(4) 0.017(4) 0.021(4) -0.004(3) -0.002(3) -0.006(3) N1 0.060(7) 0.026(5) 0.044(6) 0.005(4) -0.032(5) -0.016(5) N3 0.034(5) 0.025(4) 0.047(5) 0.000(4) -0.022(4) -0.005(4) S5 0.0185(12) 0.0235(12) 0.0241(12) -0.0096(10) 0.0045(9) -0.0095(10) S6 0.0189(12) 0.0236(12) 0.0234(12) -0.0103(10) 0.0024(9) -0.0095(10) C10 0.031(5) 0.019(4) 0.013(4) 0.003(3) -0.010(3) -0.014(4) C9 0.024(5) 0.016(4) 0.023(4) 0.000(3) -0.012(4) -0.004(3) C7 0.016(5) 0.031(5) 0.040(5) -0.018(4) 0.003(4) -0.008(4) C8 0.019(5) 0.014(4) 0.053(6) -0.005(4) -0.011(4) -0.002(4) C45 0.015(4) 0.030(5) 0.023(4) -0.017(4) 0.003(3) -0.004(4) C44 0.024(5) 0.032(5) 0.034(5) -0.021(4) 0.007(4) -0.010(4) C2 0.023(5) 0.025(5) 0.019(4) -0.011(4) 0.005(4) -0.006(4) C34 0.021(5) 0.020(4) 0.021(4) -0.004(4) 0.002(3) -0.005(4) N2 0.033(5) 0.034(5) 0.035(5) -0.017(4) 0.005(4) -0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 S2 2.327(2) . ? Pt1 S4 2.328(2) . ? Pt1 S3 2.342(2) . ? Pt1 S1 2.346(2) . ? Cu2 N12 1.981(7) . ? Cu2 N13 1.991(7) . ? Cu2 N6 1.996(8) . ? Cu2 N11 2.066(7) . ? Cu2 N14 2.115(7) . ? Cu1 N5 1.977(8) . ? Cu1 N10 1.985(7) . ? Cu1 N7 1.992(7) . ? Cu1 N9 2.063(7) . ? Cu1 N8 2.104(7) . ? S4 C4 1.698(10) . ? S2 C2 1.679(10) . ? N13 C41 1.331(11) . ? N13 C37 1.338(11) . ? C37 C38 1.382(13) . ? C37 H37 0.9500 . ? C39 C40 1.370(13) . ? C39 C38 1.422(13) . ? C39 H39 0.9500 . ? C41 C40 1.401(12) . ? C41 C42 1.476(12) . ? C40 H40 0.9500 . ? C38 H38 0.9500 . ? N8 C16 1.342(10) . ? N8 C12 1.356(10) . ? C16 C15 1.383(12) . ? C16 H16 0.9500 . ? C15 C14 1.431(12) . ? C15 H15 0.9500 . ? C13 C14 1.341(13) . ? C13 C12 1.395(11) . ? C13 H13 0.9500 . ? C12 C11 1.486(12) . ? S1 C1 1.683(12) . ? S3 C3 1.686(10) . ? C4 N4 1.135(12) . ? N5 C5 1.169(11) . ? C5 S5 1.634(9) . ? C21 N9 1.349(11) . ? C21 C20 1.396(12) . ? C21 C22 1.470(12) . ? C17 N9 1.346(11) . ? C17 C18 1.400(12) . ? C17 H17 0.9500 . ? C22 N10 1.347(11) . ? C22 C23 1.406(11) . ? C24 C23 1.369(13) . ? C24 C25 1.382(14) . ? C24 H24 0.9500 . ? C23 H23 0.9500 . ? N10 C26 1.331(11) . ? N6 C6 1.160(11) . ? N12 C36 1.355(10) . ? N12 C32 1.360(11) . ? N11 C27 1.340(11) . ? N11 C31 1.348(11) . ? C31 C30 1.383(12) . ? C31 C32 1.495(11) . ? C30 C29 1.420(11) . ? C30 H30 0.9500 . ? C32 C33 1.368(12) . ? C36 C35 1.391(12) . ? C36 H36 0.9500 . ? C27 C28 1.380(12) . ? C27 H27 0.9500 . ? C6 S6 1.623(9) . ? C1 N1 1.161(13) . ? C25 C26 1.375(12) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C14 H14 0.9500 . ? C3 N3 1.157(12) . ? C11 N7 1.369(10) . ? C11 C10 1.388(12) . ? C29 C28 1.372(13) . ? C29 H29 0.9500 . ? C28 H28 0.9500 . ? C35 C34 1.393(13) . ? C35 H35 0.9500 . ? C33 C34 1.400(12) . ? C33 H33 0.9500 . ? C18 C19 1.394(13) . ? C18 H18 0.9500 . ? C19 C20 1.341(12) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C42 N14 1.352(11) . ? C42 C43 1.377(12) . ? C46 N14 1.336(11) . ? C46 C45 1.387(11) . ? C46 H46 0.9500 . ? C43 C44 1.423(13) . ? C43 H43 0.9500 . ? N7 C7 1.348(11) . ? C10 C9 1.391(13) . ? C10 H10 0.9500 . ? C9 C8 1.346(14) . ? C9 H9 0.9500 . ? C7 C8 1.372(13) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C45 C44 1.335(13) . ? C45 H45 0.9500 . ? C44 H44 0.9500 . ? C2 N2 1.165(12) . ? C34 H34 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Pt1 S4 179.82(12) . . ? S2 Pt1 S3 84.97(8) . . ? S4 Pt1 S3 94.94(9) . . ? S2 Pt1 S1 95.00(9) . . ? S4 Pt1 S1 85.09(8) . . ? S3 Pt1 S1 179.95(16) . . ? N12 Cu2 N13 173.5(3) . . ? N12 Cu2 N6 94.7(3) . . ? N13 Cu2 N6 91.5(3) . . ? N12 Cu2 N11 80.9(3) . . ? N13 Cu2 N11 96.1(3) . . ? N6 Cu2 N11 134.1(3) . . ? N12 Cu2 N14 95.6(3) . . ? N13 Cu2 N14 79.7(3) . . ? N6 Cu2 N14 119.4(3) . . ? N11 Cu2 N14 106.5(3) . . ? N5 Cu1 N10 94.6(3) . . ? N5 Cu1 N7 91.0(3) . . ? N10 Cu1 N7 174.3(3) . . ? N5 Cu1 N9 133.4(3) . . ? N10 Cu1 N9 80.8(3) . . ? N7 Cu1 N9 96.0(3) . . ? N5 Cu1 N8 119.7(3) . . ? N10 Cu1 N8 96.6(3) . . ? N7 Cu1 N8 79.7(3) . . ? N9 Cu1 N8 106.9(3) . . ? C4 S4 Pt1 108.7(3) . . ? C2 S2 Pt1 108.3(3) . . ? C41 N13 C37 120.5(7) . . ? C41 N13 Cu2 116.3(6) . . ? C37 N13 Cu2 122.8(6) . . ? N13 C37 C38 123.6(8) . . ? N13 C37 H37 118.2 . . ? C38 C37 H37 118.2 . . ? C40 C39 C38 120.6(8) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? N13 C41 C40 120.5(8) . . ? N13 C41 C42 116.5(7) . . ? C40 C41 C42 123.0(8) . . ? C39 C40 C41 119.2(9) . . ? C39 C40 H40 120.4 . . ? C41 C40 H40 120.4 . . ? C37 C38 C39 115.7(9) . . ? C37 C38 H38 122.2 . . ? C39 C38 H38 122.2 . . ? C16 N8 C12 118.5(7) . . ? C16 N8 Cu1 128.0(6) . . ? C12 N8 Cu1 113.3(5) . . ? N8 C16 C15 123.3(8) . . ? N8 C16 H16 118.3 . . ? C15 C16 H16 118.3 . . ? C16 C15 C14 117.4(9) . . ? C16 C15 H15 121.3 . . ? C14 C15 H15 121.3 . . ? C14 C13 C12 121.1(8) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? N8 C12 C13 120.9(8) . . ? N8 C12 C11 115.0(7) . . ? C13 C12 C11 124.0(7) . . ? C1 S1 Pt1 100.9(3) . . ? C3 S3 Pt1 102.2(3) . . ? N4 C4 S4 174.8(9) . . ? C5 N5 Cu1 156.6(7) . . ? N5 C5 S5 179.4(9) . . ? N9 C21 C20 122.2(8) . . ? N9 C21 C22 115.1(7) . . ? C20 C21 C22 122.7(8) . . ? N9 C17 C18 121.6(9) . . ? N9 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? N10 C22 C23 120.1(8) . . ? N10 C22 C21 115.6(7) . . ? C23 C22 C21 124.2(8) . . ? C23 C24 C25 120.1(9) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C23 C22 118.9(9) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C26 N10 C22 120.2(7) . . ? C26 N10 Cu1 124.6(6) . . ? C22 N10 Cu1 115.2(6) . . ? C17 N9 C21 118.8(7) . . ? C17 N9 Cu1 128.2(6) . . ? C21 N9 Cu1 112.6(5) . . ? C6 N6 Cu2 155.3(7) . . ? C36 N12 C32 118.1(7) . . ? C36 N12 Cu2 125.5(6) . . ? C32 N12 Cu2 116.4(6) . . ? C27 N11 C31 118.9(7) . . ? C27 N11 Cu2 127.8(6) . . ? C31 N11 Cu2 112.9(6) . . ? N11 C31 C30 121.8(8) . . ? N11 C31 C32 115.4(8) . . ? C30 C31 C32 122.9(8) . . ? C31 C30 C29 118.7(8) . . ? C31 C30 H30 120.7 . . ? C29 C30 H30 120.7 . . ? N12 C32 C33 122.8(8) . . ? N12 C32 C31 113.8(7) . . ? C33 C32 C31 123.3(8) . . ? N12 C36 C35 122.3(8) . . ? N12 C36 H36 118.9 . . ? C35 C36 H36 118.9 . . ? N11 C27 C28 122.8(8) . . ? N11 C27 H27 118.6 . . ? C28 C27 H27 118.6 . . ? N6 C6 S6 178.8(8) . . ? N1 C1 S1 174.4(10) . . ? C26 C25 C24 118.4(8) . . ? C26 C25 H25 120.8 . . ? C24 C25 H25 120.8 . . ? N10 C26 C25 122.2(8) . . ? N10 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C13 C14 C15 118.7(8) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? N3 C3 S3 178.9(9) . . ? N7 C11 C10 121.2(8) . . ? N7 C11 C12 114.2(7) . . ? C10 C11 C12 124.6(8) . . ? C28 C29 C30 118.5(8) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? C29 C28 C27 119.2(8) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C36 C35 C34 118.8(9) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? C32 C33 C34 119.1(8) . . ? C32 C33 H33 120.5 . . ? C34 C33 H33 120.5 . . ? C19 C18 C17 117.7(8) . . ? C19 C18 H18 121.2 . . ? C17 C18 H18 121.2 . . ? C20 C19 C18 121.2(9) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 118.4(9) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 120.8 . . ? N14 C42 C43 122.4(8) . . ? N14 C42 C41 114.3(7) . . ? C43 C42 C41 123.3(8) . . ? N14 C46 C45 122.3(8) . . ? N14 C46 H46 118.8 . . ? C45 C46 H46 118.8 . . ? C42 C43 C44 117.7(8) . . ? C42 C43 H43 121.1 . . ? C44 C43 H43 121.1 . . ? C46 N14 C42 118.4(7) . . ? C46 N14 Cu2 128.9(6) . . ? C42 N14 Cu2 112.5(6) . . ? C7 N7 C11 118.0(8) . . ? C7 N7 Cu1 124.7(6) . . ? C11 N7 Cu1 117.2(6) . . ? C11 C10 C9 119.2(8) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C8 C9 C10 118.8(8) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N7 C7 C8 122.0(9) . . ? N7 C7 H7 119.0 . . ? C8 C7 H7 119.0 . . ? C9 C8 C7 120.9(9) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C44 C45 C46 119.8(9) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C45 C44 C43 119.4(9) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? N2 C2 S2 175.1(9) . . ? C35 C34 C33 118.9(8) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? data_C8H16CuN8PtS4cis #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C8 H16 Cu1 N8 Pt1 S4' _chemical_formula_moiety 'C8 H16 Cu1 N8 Pt1 S4' _chemical_compound_source ? _chemical_formula_weight 611.17 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' #------------------------------------------------ _cell_length_a 11.8764(18) _cell_length_b 11.4014(18) _cell_length_c 14.242(2) _cell_angle_alpha 90 _cell_angle_beta 110.453(2) _cell_angle_gamma 90 _cell_volume 1806.9(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4358 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.49 _cell_measurement_temperature 100 _exptl_crystal_description 'prism' _exptl_crystal_colour 'brown' _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_max 0.09 _exptl_crystal_density_diffrn 2.247 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 9.379 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device 'Unknown' _diffrn_measurement_device_type 'Serial' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 10321 _reflns_number_total 4117 _diffrn_reflns_av_R_equivalents 0.023 # Number of reflections with Friedels Law is 4117 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4155 _diffrn_reflns_theta_min 1.930 _diffrn_reflns_theta_max 27.510 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.959 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #========================================================================== # 8. REFINEMENT DATA _refine_diff_density_min -0.83 _refine_diff_density_max 1.33 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 3060 _refine_ls_number_restraints 0 _refine_ls_number_parameters 202 _oxford_refine_ls_R_factor_ref 0.0245 _refine_ls_wR_factor_ref 0.0258 _refine_ls_goodness_of_fit_ref 1.3251 _refine_ls_shift/su_max 0.002292 _oxford_reflns_number_all 4117 _refine_ls_R_factor_all 0.0402 _refine_ls_wR_factor_all 0.0321 _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3169 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_gt 0.0265 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.01P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Pt1 Pt 0.527485(13) 0.000917(19) 0.697771(10) 0.0137 1.0000 Uani . . . . . . . Cu1 Cu 0.0000 0.0000 0.5000 0.0164 1.0000 Uani S . . . . . . Cu2 Cu 0.5000 0.5000 0.5000 0.0176 1.0000 Uani S . . . . . . S1 S 0.42071(10) 0.17412(10) 0.68643(8) 0.0171 1.0000 Uani . . . . . . . S2 S 0.65209(11) 0.07883(12) 0.62135(9) 0.0260 1.0000 Uani . . . . . . . S3 S 0.63902(10) -0.17213(11) 0.72998(8) 0.0201 1.0000 Uani . . . . . . . S4 S 0.39993(12) -0.07893(12) 0.77437(9) 0.0238 1.0000 Uani . . . . . . . N1 N 0.1833(4) 0.1179(4) 0.5626(3) 0.0236 1.0000 Uani . . . . . . . N2 N 0.5678(4) 0.2955(4) 0.5272(3) 0.0215 1.0000 Uani . . . . . . . N3 N 0.8607(3) -0.1267(3) 0.7045(3) 0.0196 1.0000 Uani . . . . . . . N4 N 0.3833(4) -0.3200(4) 0.7231(3) 0.0258 1.0000 Uani . . . . . . . N5 N 0.0816(3) -0.0986(3) 0.4258(2) 0.0179 1.0000 Uani . . . . . . . N6 N 0.0630(3) -0.1209(3) 0.6098(2) 0.0186 1.0000 Uani . . . . . . . N7 N 0.3455(4) 0.4406(4) 0.3967(3) 0.0228 1.0000 Uani . . . . . . . N8 N 0.4137(4) 0.4712(3) 0.5980(3) 0.0188 1.0000 Uani . . . . . . . C1 C 0.2800(4) 0.1371(4) 0.6128(3) 0.0164 1.0000 Uani . . . . . . . C2 C 0.5960(4) 0.2072(4) 0.5668(3) 0.0178 1.0000 Uani . . . . . . . C3 C 0.7709(4) -0.1443(4) 0.7133(3) 0.0146 1.0000 Uani . . . . . . . C4 C 0.3903(4) -0.2224(5) 0.7427(3) 0.0198 1.0000 Uani . . . . . . . C5 C 0.1534(4) -0.1932(4) 0.4932(3) 0.0235 1.0000 Uani . . . . . . . C6 C 0.0876(4) -0.2288(4) 0.5627(3) 0.0219 1.0000 Uani . . . . . . . C7 C 0.2741(4) 0.3805(4) 0.4493(3) 0.0231 1.0000 Uani . . . . . . . C8 C 0.2856(4) 0.4520(5) 0.5418(3) 0.0248 1.0000 Uani . . . . . . . H53 H 0.2312 -0.1647 0.5312 0.0284 1.0000 Uiso R . . . . . . H54 H 0.1605 -0.2587 0.4545 0.0284 1.0000 Uiso R . . . . . . H63 H 0.1361 -0.2806 0.6127 0.0264 1.0000 Uiso R . . . . . . H64 H 0.0141 -0.2665 0.5256 0.0264 1.0000 Uiso R . . . . . . H73 H 0.3044 0.3036 0.4682 0.0269 1.0000 Uiso R . . . . . . H74 H 0.1922 0.3761 0.4069 0.0269 1.0000 Uiso R . . . . . . H83 H 0.2461 0.5252 0.5225 0.0302 1.0000 Uiso R . . . . . . H84 H 0.2501 0.4107 0.5824 0.0302 1.0000 Uiso R . . . . . . H51 H 0.1324 -0.0516 0.4050 0.0215 1.0000 Uiso R . . . . . . H52 H 0.0240 -0.1324 0.3702 0.0215 1.0000 Uiso R . . . . . . H61 H 0.0058 -0.1359 0.6393 0.0229 1.0000 Uiso R . . . . . . H62 H 0.1333 -0.0940 0.6583 0.0229 1.0000 Uiso R . . . . . . H71 H 0.3019 0.5033 0.3599 0.0264 1.0000 Uiso R . . . . . . H72 H 0.3632 0.3881 0.3538 0.0264 1.0000 Uiso R . . . . . . H81 H 0.3861 0.5375 0.6213 0.0227 1.0000 Uiso R . . . . . . H82 H 0.4517 0.4215 0.6516 0.0227 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.00905(8) 0.01519(9) 0.01626(8) 0.00001(8) 0.00381(6) 0.00073(8) Cu1 0.0135(3) 0.0217(4) 0.0144(3) 0.0012(4) 0.0054(3) 0.0017(4) Cu2 0.0170(4) 0.0201(4) 0.0150(3) 0.0003(4) 0.0050(3) -0.0011(4) S1 0.0098(5) 0.0162(6) 0.0236(5) -0.0031(5) 0.0036(4) 0.0002(5) S2 0.0158(6) 0.0219(7) 0.0462(7) 0.0138(6) 0.0181(6) 0.0072(5) S3 0.0137(6) 0.0183(6) 0.0299(6) 0.0043(5) 0.0094(5) 0.0031(5) S4 0.0240(7) 0.0221(7) 0.0323(6) 0.0032(5) 0.0188(5) 0.0029(6) N1 0.014(2) 0.025(2) 0.029(2) 0.0003(17) 0.0045(17) -0.0003(18) N2 0.020(2) 0.020(2) 0.027(2) 0.0029(17) 0.0119(17) 0.0026(18) N3 0.0110(19) 0.024(2) 0.0236(19) 0.0042(16) 0.0058(16) 0.0063(17) N4 0.024(2) 0.028(3) 0.027(2) -0.0009(19) 0.0113(18) -0.002(2) N5 0.0105(19) 0.025(2) 0.0180(17) -0.0002(16) 0.0046(15) 0.0004(17) N6 0.0098(19) 0.025(2) 0.0215(18) 0.0028(16) 0.0064(15) 0.0036(17) N7 0.026(2) 0.021(2) 0.0196(19) 0.0032(17) 0.0053(17) -0.0001(19) N8 0.018(2) 0.019(2) 0.0209(19) 0.0016(14) 0.0087(16) 0.0056(16) C1 0.015(2) 0.017(3) 0.019(2) -0.0006(17) 0.0082(18) 0.0016(19) C2 0.012(2) 0.022(3) 0.021(2) -0.0025(19) 0.0069(18) -0.001(2) C3 0.011(2) 0.016(2) 0.0152(19) 0.0011(17) 0.0024(17) 0.0063(18) C4 0.010(2) 0.032(3) 0.019(2) 0.006(2) 0.0067(18) 0.002(2) C5 0.018(3) 0.028(3) 0.025(2) 0.001(2) 0.008(2) 0.003(2) C6 0.015(2) 0.025(3) 0.026(2) 0.003(2) 0.007(2) 0.003(2) C7 0.020(3) 0.023(3) 0.025(2) 0.002(2) 0.005(2) 0.000(2) C8 0.019(3) 0.029(3) 0.027(2) 0.002(2) 0.010(2) 0.004(2) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.2057(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . S1 . 2.3218(12) yes Pt1 . S2 . 2.2999(12) yes Pt1 . S3 . 2.3309(12) yes Pt1 . S4 . 2.3385(12) yes Cu1 . N1 2_556 2.447(4) yes Cu1 . N6 2_556 2.022(3) yes Cu1 . N5 2_556 2.009(3) yes Cu1 . N1 . 2.447(4) yes Cu1 . N5 . 2.009(3) yes Cu1 . N6 . 2.022(3) yes Cu2 . N2 2_666 2.453(4) yes Cu2 . N8 2_666 2.027(4) yes Cu2 . N7 2_666 2.026(4) yes Cu2 . N2 . 2.453(4) yes Cu2 . N7 . 2.026(4) yes Cu2 . N8 . 2.027(4) yes S1 . C1 . 1.687(5) yes S2 . C2 . 1.681(5) yes S3 . C3 . 1.693(4) yes S4 . C4 . 1.689(5) yes N1 . C1 . 1.141(6) yes N2 . C2 . 1.145(6) yes N3 . C3 . 1.135(5) yes N4 . C4 . 1.144(6) yes N5 . C5 . 1.496(5) yes N5 . H51 . 0.930 no N5 . H52 . 0.930 no N6 . C6 . 1.479(6) yes N6 . H61 . 0.930 no N6 . H62 . 0.930 no N7 . C7 . 1.481(6) yes N7 . H71 . 0.930 no N7 . H72 . 0.930 no N8 . C8 . 1.468(6) yes N8 . H81 . 0.930 no N8 . H82 . 0.930 no C5 . C6 . 1.515(6) yes C5 . H53 . 0.950 no C5 . H54 . 0.950 no C6 . H63 . 0.950 no C6 . H64 . 0.950 no C7 . C8 . 1.514(6) yes C7 . H73 . 0.950 no C7 . H74 . 0.950 no C8 . H83 . 0.950 no C8 . H84 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 . Pt1 . S2 . 93.71(5) yes S1 . Pt1 . S3 . 173.04(4) yes S2 . Pt1 . S3 . 90.27(4) yes S1 . Pt1 . S4 . 86.36(4) yes S2 . Pt1 . S4 . 179.58(4) yes S3 . Pt1 . S4 . 89.71(4) yes N1 2_556 Cu1 . N6 2_556 92.92(14) yes N1 2_556 Cu1 . N5 2_556 88.14(14) yes N6 2_556 Cu1 . N5 2_556 84.80(14) yes N1 2_556 Cu1 . N1 . 179.995 yes N6 2_556 Cu1 . N1 . 87.08(14) yes N5 2_556 Cu1 . N1 . 91.86(14) yes N1 2_556 Cu1 . N5 . 91.86(14) yes N6 2_556 Cu1 . N5 . 95.20(14) yes N5 2_556 Cu1 . N5 . 179.994 yes N1 . Cu1 . N5 . 88.14(14) yes N1 2_556 Cu1 . N6 . 87.08(14) yes N6 2_556 Cu1 . N6 . 179.994 yes N5 2_556 Cu1 . N6 . 95.20(14) yes N1 . Cu1 . N6 . 92.92(14) yes N5 . Cu1 . N6 . 84.80(14) yes N2 2_666 Cu2 . N8 2_666 87.38(13) yes N2 2_666 Cu2 . N7 2_666 87.76(15) yes N8 2_666 Cu2 . N7 2_666 84.16(15) yes N2 2_666 Cu2 . N2 . 179.995 yes N8 2_666 Cu2 . N2 . 92.62(13) yes N7 2_666 Cu2 . N2 . 92.24(15) yes N2 2_666 Cu2 . N7 . 92.24(15) yes N8 2_666 Cu2 . N7 . 95.84(15) yes N7 2_666 Cu2 . N7 . 179.994 yes N2 . Cu2 . N7 . 87.76(15) yes N2 2_666 Cu2 . N8 . 92.62(13) yes N8 2_666 Cu2 . N8 . 179.994 yes N7 2_666 Cu2 . N8 . 95.84(15) yes N2 . Cu2 . N8 . 87.38(13) yes N7 . Cu2 . N8 . 84.16(15) yes Pt1 . S1 . C1 . 103.21(16) yes Pt1 . S2 . C2 . 109.79(16) yes Pt1 . S3 . C3 . 107.67(16) yes Pt1 . S4 . C4 . 104.29(16) yes Cu1 . N1 . C1 . 154.9(4) yes Cu2 . N2 . C2 . 159.5(3) yes Cu1 . N5 . C5 . 109.7(2) yes Cu1 . N5 . H51 . 109.4 no C5 . N5 . H51 . 109.4 no Cu1 . N5 . H52 . 109.4 no C5 . N5 . H52 . 109.5 no H51 . N5 . H52 . 109.5 no Cu1 . N6 . C6 . 107.1(2) yes Cu1 . N6 . H61 . 110.1 no C6 . N6 . H61 . 110.0 no Cu1 . N6 . H62 . 110.1 no C6 . N6 . H62 . 110.0 no H61 . N6 . H62 . 109.5 no Cu2 . N7 . C7 . 108.7(3) yes Cu2 . N7 . H71 . 109.7 no C7 . N7 . H71 . 109.7 no Cu2 . N7 . H72 . 109.6 no C7 . N7 . H72 . 109.6 no H71 . N7 . H72 . 109.5 no Cu2 . N8 . C8 . 109.0(3) yes Cu2 . N8 . H81 . 116.1 no C8 . N8 . H81 . 83.6 no Cu2 . N8 . H82 . 116.5 no C8 . N8 . H82 . 118.0 no H81 . N8 . H82 . 109.5 no S1 . C1 . N1 . 176.5(4) yes S2 . C2 . N2 . 173.3(4) yes S3 . C3 . N3 . 178.3(4) yes S4 . C4 . N4 . 178.5(4) yes N5 . C5 . C6 . 107.7(4) yes N5 . C5 . H53 . 110.0 no C6 . C5 . H53 . 109.9 no N5 . C5 . H54 . 109.9 no C6 . C5 . H54 . 109.9 no H53 . C5 . H54 . 109.5 no C5 . C6 . N6 . 107.6(4) yes C5 . C6 . H63 . 109.9 no N6 . C6 . H63 . 110.0 no C5 . C6 . H64 . 109.9 no N6 . C6 . H64 . 109.9 no H63 . C6 . H64 . 109.5 no N7 . C7 . C8 . 107.3(4) yes N7 . C7 . H73 . 110.0 no C8 . C7 . H73 . 109.9 no N7 . C7 . H74 . 110.0 no C8 . C7 . H74 . 110.0 no H73 . C7 . H74 . 109.5 no C7 . C8 . N8 . 108.4(4) yes C7 . C8 . H83 . 109.6 no N8 . C8 . H83 . 109.9 no C7 . C8 . H84 . 109.7 no N8 . C8 . H84 . 109.7 no H83 . C8 . H84 . 109.5 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag N5 . H51 . N3 2_656 144 0.93 2.58 3.377(7) yes N5 . H52 . N4 4_444 169 0.93 2.24 3.161(7) yes N5 . H52 . C4 4_444 164 0.93 2.56 3.462(7) yes N6 . H61 . N3 1_455 166 0.93 2.23 3.140(7) yes N7 . H71 . C3 4_454 147 0.93 2.56 3.374(7) yes N8 . H81 . N4 1_565 158 0.93 2.19 3.069(7) yes N8 . H82 . N3 3_656 147 0.93 2.51 3.327(7) yes data_C8H16CuN8PtS4trans #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C8 H24 Cu1 N8 Pt1 S4' _chemical_formula_moiety 'C8 H24 Cu1 N8 Pt1 S4' _chemical_compound_source ? _chemical_formula_weight 619.23 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' #------------------------------------------------ _cell_length_a 6.6261(10) _cell_length_b 8.3050(13) _cell_length_c 8.7992(13) _cell_angle_alpha 112.9030(10) _cell_angle_beta 98.4060(10) _cell_angle_gamma 94.745(2) _cell_volume 436.04(11) _cell_formula_units_Z 1 _cell_measurement_reflns_used 4863 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 26.35 _cell_measurement_temperature 100 _exptl_crystal_description 'prism' _exptl_crystal_colour 'purple' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.14 _exptl_crystal_density_diffrn 2.358 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 299 _exptl_absorpt_coefficient_mu 9.717 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device 'Unknown' _diffrn_measurement_device_type 'Serial' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 5016 _reflns_number_total 2018 _diffrn_reflns_av_R_equivalents 0.014 # Number of reflections with Friedels Law is 2018 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2081 _diffrn_reflns_theta_min 2.562 _diffrn_reflns_theta_max 27.882 _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.094 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _reflns_limit_h_min -8 _reflns_limit_h_max 8 _reflns_limit_k_min -10 _reflns_limit_k_max 10 _reflns_limit_l_min 0 _reflns_limit_l_max 11 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #========================================================================== # 8. REFINEMENT DATA _refine_diff_density_min -0.98 _refine_diff_density_max 0.75 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 2018 _refine_ls_number_restraints 0 _refine_ls_number_parameters 103 _oxford_refine_ls_R_factor_ref 0.0135 _refine_ls_wR_factor_ref 0.0223 _refine_ls_goodness_of_fit_ref 1.6769 _refine_ls_shift/su_max 0.000129 _oxford_reflns_number_all 2018 _refine_ls_R_factor_all 0.0135 _refine_ls_wR_factor_all 0.0223 _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2018 _refine_ls_R_factor_gt 0.0135 _refine_ls_wR_factor_gt 0.0223 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.01P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Pt1 Pt 0.0000 0.0000 -0.5000 0.0125 1.0000 Uani S . . . . . . Cu1 Cu 0.0000 0.5000 0.0000 0.0123 1.0000 Uani S . . . . . . S1 S 0.28741(10) 0.19473(8) -0.48179(8) 0.0165 1.0000 Uani . . . . . . . S2 S 0.16968(10) -0.11670(9) -0.32480(8) 0.0176 1.0000 Uani . . . . . . . N1 N 0.2778(4) 0.4739(3) -0.1692(3) 0.0240 1.0000 Uani . . . . . . . N2 N 0.5724(4) 0.0785(3) -0.1721(3) 0.0208 1.0000 Uani . . . . . . . N5 N 0.0292(3) 0.2631(3) 0.0078(3) 0.0152 1.0000 Uani . . . . . . . N6 N 0.2144(3) 0.5991(3) 0.2137(3) 0.0147 1.0000 Uani . . . . . . . C1 C 0.2764(4) 0.3585(3) -0.2980(3) 0.0162 1.0000 Uani . . . . . . . C2 C 0.4076(4) 0.0020(3) -0.2375(3) 0.0164 1.0000 Uani . . . . . . . C5 C 0.2199(4) 0.2860(4) 0.1309(3) 0.0174 1.0000 Uani . . . . . . . C6 C 0.2338(4) 0.4606(3) 0.2790(3) 0.0165 1.0000 Uani . . . . . . . H53 H 0.0387 0.1811 -0.0980 0.0183 1.0000 Uiso . . . . . . . H54 H -0.0844 0.2236 0.0417 0.0183 1.0000 Uiso . . . . . . . H51 H 0.3371 0.2873 0.0806 0.0222 1.0000 Uiso R . . . . . . H52 H 0.2142 0.1918 0.1666 0.0222 1.0000 Uiso R . . . . . . H63 H 0.1742 0.6968 0.2928 0.0178 1.0000 Uiso . . . . . . . H64 H 0.3406 0.6323 0.1919 0.0178 1.0000 Uiso . . . . . . . H61 H 0.3625 0.4865 0.3538 0.0210 1.0000 Uiso R . . . . . . H62 H 0.1246 0.4547 0.3366 0.0210 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01323(8) 0.01189(8) 0.01032(8) 0.00308(5) 0.00192(5) -0.00118(5) Cu1 0.0119(2) 0.0104(2) 0.0130(2) 0.00419(16) -0.00003(16) 0.00125(16) S1 0.0163(3) 0.0176(3) 0.0140(3) 0.0056(2) 0.0032(2) -0.0019(2) S2 0.0167(3) 0.0173(3) 0.0184(3) 0.0088(3) 0.0001(2) -0.0020(2) N1 0.0176(11) 0.0247(12) 0.0248(12) 0.0041(10) 0.0072(9) 0.0015(9) N2 0.0194(12) 0.0183(11) 0.0250(12) 0.0101(9) 0.0020(9) 0.0020(9) N5 0.0160(10) 0.0122(9) 0.0157(10) 0.0043(8) 0.0022(8) 0.0019(8) N6 0.0137(10) 0.0133(10) 0.0161(10) 0.0063(8) 0.0007(8) -0.0004(8) C1 0.0112(11) 0.0174(12) 0.0213(13) 0.0096(10) 0.0031(9) -0.0002(9) C2 0.0197(13) 0.0137(11) 0.0167(12) 0.0063(9) 0.0050(10) 0.0049(10) C5 0.0174(12) 0.0188(12) 0.0207(13) 0.0121(10) 0.0045(10) 0.0058(10) C6 0.0146(12) 0.0209(13) 0.0158(12) 0.0103(10) 0.0012(9) 0.0010(10) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.6236(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . S1 2_554 2.3383(7) yes Pt1 . S2 2_554 2.3273(7) yes Pt1 . S1 . 2.3383(7) yes Pt1 . S2 . 2.3273(7) yes Cu1 . N1 2_565 2.504(2) yes Cu1 . N5 2_565 2.019(2) yes Cu1 . N6 2_565 2.013(2) yes Cu1 . N1 . 2.504(2) yes Cu1 . N5 . 2.019(2) yes Cu1 . N6 . 2.013(2) yes S1 . C1 . 1.676(3) yes S2 . C2 . 1.687(3) yes N1 . C1 . 1.163(4) yes N2 . C2 . 1.159(4) yes N5 . C5 . 1.485(3) yes N5 . H53 . 0.930 no N5 . H54 . 0.930 no N6 . C6 . 1.479(3) yes N6 . H63 . 0.930 no N6 . H64 . 0.928 no C5 . C6 . 1.511(4) yes C5 . H51 . 0.954 no C5 . H52 . 0.950 no C6 . H61 . 0.950 no C6 . H62 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 2_554 Pt1 . S2 2_554 95.72(3) yes S1 2_554 Pt1 . S1 . 179.995 yes S2 2_554 Pt1 . S1 . 84.28(2) yes S1 2_554 Pt1 . S2 . 84.28(3) yes S2 2_554 Pt1 . S2 . 179.995 yes S1 . Pt1 . S2 . 95.72(3) yes N1 2_565 Cu1 . N5 2_565 91.45(9) yes N1 2_565 Cu1 . N6 2_565 90.28(9) yes N5 2_565 Cu1 . N6 2_565 85.01(9) yes N1 2_565 Cu1 . N1 . 179.995 yes N5 2_565 Cu1 . N1 . 88.55(9) yes N6 2_565 Cu1 . N1 . 89.72(9) yes N1 2_565 Cu1 . N5 . 88.55(9) yes N5 2_565 Cu1 . N5 . 179.994 yes N6 2_565 Cu1 . N5 . 94.99(9) yes N1 . Cu1 . N5 . 91.45(9) yes N1 2_565 Cu1 . N6 . 89.72(9) yes N5 2_565 Cu1 . N6 . 94.99(9) yes N6 2_565 Cu1 . N6 . 179.994 yes N1 . Cu1 . N6 . 90.28(9) yes N5 . Cu1 . N6 . 85.01(9) yes Pt1 . S1 . C1 . 98.28(9) yes Pt1 . S2 . C2 . 108.59(9) yes Cu1 . N1 . C1 . 125.1(2) yes Cu1 . N5 . C5 . 108.06(15) yes Cu1 . N5 . H53 . 109.9 no C5 . N5 . H53 . 109.9 no Cu1 . N5 . H54 . 109.9 no C5 . N5 . H54 . 109.6 no H53 . N5 . H54 . 109.4 no Cu1 . N6 . C6 . 108.51(15) yes Cu1 . N6 . H63 . 109.7 no C6 . N6 . H63 . 109.7 no Cu1 . N6 . H64 . 109.8 no C6 . N6 . H64 . 109.5 no H63 . N6 . H64 . 109.6 no S1 . C1 . N1 . 177.1(2) yes S2 . C2 . N2 . 176.3(2) yes N5 . C5 . C6 . 107.8(2) yes N5 . C5 . H51 . 109.8 no C6 . C5 . H51 . 109.7 no N5 . C5 . H52 . 110.0 no C6 . C5 . H52 . 110.4 no H51 . C5 . H52 . 109.1 no C5 . C6 . N6 . 107.9(2) yes C5 . C6 . H61 . 110.0 no N6 . C6 . H61 . 110.4 no C5 . C6 . H62 . 109.4 no N6 . C6 . H62 . 110.0 no H61 . C6 . H62 . 109.2 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag N6 . H64 . N2 2_665 122 0.93 2.50 3.096(4) yes data_C8H16CuN8PtSe4 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C8 H16 Cu1 N8 Pt1 Se4' _chemical_formula_moiety 'C8 H16 Cu1 N8 Pt1 Se4' _chemical_compound_source ? _chemical_formula_weight 798.74 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' #------------------------------------------------ _cell_length_a 7.1053(14) _cell_length_b 7.8223(16) _cell_length_c 9.423(3) _cell_angle_alpha 109.979(3) _cell_angle_beta 101.138(3) _cell_angle_gamma 103.475(2) _cell_volume 456.85(19) _cell_formula_units_Z 1 _cell_measurement_reflns_used 3893 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.98 _cell_measurement_temperature 100 _exptl_crystal_description 'block' _exptl_crystal_colour 'brown' _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_max 0.15 _exptl_crystal_density_diffrn 2.903 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 363 _exptl_absorpt_coefficient_mu 16.784 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device 'Unknown' _diffrn_measurement_device_type 'Serial' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 5290 _reflns_number_total 2118 _diffrn_reflns_av_R_equivalents 0.034 # Number of reflections with Friedels Law is 2118 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2202 _diffrn_reflns_theta_min 2.410 _diffrn_reflns_theta_max 27.982 _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.744 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _reflns_limit_h_min -9 _reflns_limit_h_max 8 _reflns_limit_k_min -10 _reflns_limit_k_max 9 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #========================================================================== # 8. REFINEMENT DATA _refine_diff_density_min -1.27 _refine_diff_density_max 2.55 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 2010 _refine_ls_number_restraints 0 _refine_ls_number_parameters 104 _oxford_refine_ls_R_factor_ref 0.0219 _refine_ls_wR_factor_ref 0.0296 _refine_ls_goodness_of_fit_ref 0.9936 _refine_ls_shift/su_max 0.000517 # The values computed from all data _oxford_reflns_number_all 2118 _refine_ls_R_factor_all 0.0230 _refine_ls_wR_factor_all 0.0304 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2032 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_gt 0.0299 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Pt1 Pt 0.5000 1.0000 1.0000 0.0133 1.0000 Uani S . . . . . . Cu1 Cu 0.5000 1.0000 0.5000 0.0165 1.0000 Uani S . . . . . . Se1 Se 0.70898(5) 0.80157(5) 0.90836(4) 0.0196 1.0000 Uani . . . . . . . Se2 Se 0.20972(5) 0.72788(5) 0.95469(4) 0.0193 1.0000 Uani . . . . . . . N1 N 0.7988(6) 0.9222(5) 0.6523(4) 0.0296 1.0000 Uani . . . . . . . N2 N 0.2960(5) 0.3619(5) 0.8033(4) 0.0267 1.0000 Uani . . . . . . . N5 N 0.3684(5) 0.7206(4) 0.3522(3) 0.0200 1.0000 Uani . . . . . . . N6 N 0.3044(4) 0.9437(4) 0.6189(3) 0.0152 1.0000 Uani . . . . . . . C1 C 0.7673(5) 0.8805(5) 0.7545(4) 0.0197 1.0000 Uani . . . . . . . C2 C 0.2728(5) 0.5073(5) 0.8631(4) 0.0199 1.0000 Uani . . . . . . . C5 C 0.2632(6) 0.6228(5) 0.4374(5) 0.0246 1.0000 Uani . . . . . . . C6 C 0.1559(5) 0.7500(5) 0.5240(4) 0.0228 1.0000 Uani . . . . . . . H51 H 0.4665 0.6671 0.3235 0.028(4) 1.0000 Uiso R . . . . . . H52 H 0.2758 0.7085 0.2619 0.028(4) 1.0000 Uiso R . . . . . . H53 H 0.3588 0.6031 0.5108 0.031(4) 1.0000 Uiso R . . . . . . H54 H 0.1674 0.5022 0.3643 0.031(4) 1.0000 Uiso R . . . . . . H61 H 0.2371 1.0342 0.6369 0.022(4) 1.0000 Uiso R . . . . . . H62 H 0.3746 0.9489 0.7152 0.022(4) 1.0000 Uiso R . . . . . . H63 H 0.1020 0.6995 0.5914 0.030(4) 1.0000 Uiso R . . . . . . H64 H 0.0490 0.7564 0.4500 0.030(4) 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01620(11) 0.01319(12) 0.01166(11) 0.00510(8) 0.00520(7) 0.00569(8) Cu1 0.0232(3) 0.0109(3) 0.0139(3) 0.0043(2) 0.0085(2) 0.0016(2) Se1 0.02343(19) 0.01721(19) 0.0256(2) 0.01145(16) 0.01386(15) 0.01000(15) Se2 0.01917(18) 0.01533(19) 0.02254(19) 0.00557(15) 0.00866(15) 0.00533(14) N1 0.043(2) 0.033(2) 0.0238(17) 0.0146(15) 0.0156(15) 0.0218(17) N2 0.0277(17) 0.0189(17) 0.0314(18) 0.0072(14) 0.0107(14) 0.0065(13) N5 0.0260(16) 0.0144(15) 0.0184(15) 0.0051(12) 0.0104(12) 0.0039(12) N6 0.0196(14) 0.0130(14) 0.0134(13) 0.0062(11) 0.0058(11) 0.0042(11) C1 0.0220(17) 0.0175(18) 0.0214(17) 0.0053(14) 0.0094(14) 0.0111(14) C2 0.0226(17) 0.0153(18) 0.0200(17) 0.0070(14) 0.0065(14) 0.0030(14) C5 0.0287(19) 0.0136(18) 0.0257(19) 0.0053(15) 0.0115(16) -0.0019(15) C6 0.0203(17) 0.0187(18) 0.0248(19) 0.0059(15) 0.0104(15) -0.0006(14) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.4585(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . Se1 2_677 2.4522(5) yes Pt1 . Se2 2_677 2.4413(5) yes Pt1 . Se1 . 2.4522(5) yes Pt1 . Se2 . 2.4413(5) yes Cu1 . N1 2_676 2.638(4) yes Cu1 . N5 2_676 2.014(3) yes Cu1 . N6 2_676 2.009(3) yes Cu1 . N1 . 2.638(4) yes Cu1 . N5 . 2.014(3) yes Cu1 . N6 . 2.009(3) yes Se1 . C1 . 1.838(4) yes Se2 . C2 . 1.848(4) yes N1 . C1 . 1.161(5) yes N2 . C2 . 1.150(5) yes N5 . C5 . 1.475(4) yes N5 . H51 . 0.930 no N5 . H52 . 0.930 no N6 . C6 . 1.474(4) yes N6 . H61 . 0.930 no N6 . H62 . 0.930 no C5 . C6 . 1.509(5) yes C5 . H53 . 0.950 no C5 . H54 . 0.950 no C6 . H63 . 0.950 no C6 . H64 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Se1 2_677 Pt1 . Se2 2_677 94.56(2) yes Se1 2_677 Pt1 . Se1 . 179.995 yes Se2 2_677 Pt1 . Se1 . 85.44(2) yes Se1 2_677 Pt1 . Se2 . 85.44(2) yes Se2 2_677 Pt1 . Se2 . 179.995 yes Se1 . Pt1 . Se2 . 94.56(2) yes N1 2_676 Cu1 . N5 2_676 91.01(12) yes N1 2_676 Cu1 . N6 2_676 97.37(11) yes N5 2_676 Cu1 . N6 2_676 85.00(12) yes N1 2_676 Cu1 . N1 . 179.996 yes N5 2_676 Cu1 . N1 . 88.99(13) yes N6 2_676 Cu1 . N1 . 82.63(11) yes N1 2_676 Cu1 . N5 . 88.99(12) yes N5 2_676 Cu1 . N5 . 179.994 yes N6 2_676 Cu1 . N5 . 95.00(12) yes N1 . Cu1 . N5 . 91.01(12) yes N1 2_676 Cu1 . N6 . 82.63(11) yes N5 2_676 Cu1 . N6 . 95.00(12) yes N6 2_676 Cu1 . N6 . 179.994 yes N1 . Cu1 . N6 . 97.37(11) yes N5 . Cu1 . N6 . 85.00(12) yes Pt1 . Se1 . C1 . 99.49(11) yes Pt1 . Se2 . C2 . 107.07(11) yes Cu1 . N1 . C1 . 114.4(3) yes Cu1 . N5 . C5 . 107.3(2) yes Cu1 . N5 . H51 . 110.0 no C5 . N5 . H51 . 110.0 no Cu1 . N5 . H52 . 110.0 no C5 . N5 . H52 . 110.0 no H51 . N5 . H52 . 109.5 no Cu1 . N6 . C6 . 109.0(2) yes Cu1 . N6 . H61 . 109.6 no C6 . N6 . H61 . 109.6 no Cu1 . N6 . H62 . 109.6 no C6 . N6 . H62 . 109.6 no H61 . N6 . H62 . 109.5 no Se1 . C1 . N1 . 176.9(3) yes Se2 . C2 . N2 . 174.5(3) yes N5 . C5 . C6 . 107.7(3) yes N5 . C5 . H53 . 109.9 no C6 . C5 . H53 . 109.9 no N5 . C5 . H54 . 109.9 no C6 . C5 . H54 . 109.9 no H53 . C5 . H54 . 109.5 no C5 . C6 . N6 . 108.3(3) yes C5 . C6 . H63 . 109.8 no N6 . C6 . H63 . 109.8 no C5 . C6 . H64 . 109.8 no N6 . C6 . H64 . 109.8 no H63 . C6 . H64 . 109.5 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag N5 . H51 . N2 2_666 152 0.93 2.26 3.110(6) yes N6 . H61 . N2 1_565 140 0.93 2.39 3.158(6) yes data_C8H16N8NiPtS4 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C8 H16 N8 Ni1 Pt1 S4' _chemical_formula_moiety 'C8 H16 N8 Ni1 Pt1 S4' _chemical_compound_source ? _chemical_formula_weight 606.33 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' #------------------------------------------------ _cell_length_a 11.7946(18) _cell_length_b 11.3401(18) _cell_length_c 14.311(2) _cell_angle_alpha 90 _cell_angle_beta 111.943(2) _cell_angle_gamma 90 _cell_volume 1775.5(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6515 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 27.57 _cell_measurement_temperature 100 _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_max 0.14 _exptl_crystal_density_diffrn 2.268 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 9.407 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device 'Unknown' _diffrn_measurement_device_type 'Serial' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 10000 _reflns_number_total 4032 _diffrn_reflns_av_R_equivalents 0.027 # Number of reflections with Friedels Law is 4032 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4117 _diffrn_reflns_theta_min 1.919 _diffrn_reflns_theta_max 27.592 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.765 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #========================================================================== # 8. REFINEMENT DATA _refine_diff_density_min -1.02 _refine_diff_density_max 2.54 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 3669 _refine_ls_number_restraints 0 _refine_ls_number_parameters 197 _oxford_refine_ls_R_factor_ref 0.0243 _refine_ls_wR_factor_ref 0.0323 _refine_ls_goodness_of_fit_ref 1.1182 _refine_ls_shift/su_max 0.001654 # The values computed from all data _oxford_reflns_number_all 4032 _refine_ls_R_factor_all 0.0280 _refine_ls_wR_factor_all 0.0367 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3734 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_gt 0.0328 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration '.' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Pt1 Pt 0.477346(12) 0.514818(13) 0.307416(10) 0.0140 1.0000 Uani . . . . . . . Ni1 Ni 1.0000 0.5000 0.5000 0.0148 1.0000 Uani S . . . . . . Ni2 Ni 0.5000 1.0000 0.5000 0.0159 1.0000 Uani S . . . . . . S1 S 0.59703(8) 0.68211(8) 0.32513(7) 0.0181 1.0000 Uani . . . . . . . S2 S 0.36164(9) 0.59358(9) 0.39186(8) 0.0236 1.0000 Uani . . . . . . . S3 S 0.36441(9) 0.34090(9) 0.27733(8) 0.0227 1.0000 Uani . . . . . . . S4 S 0.58793(10) 0.43522(10) 0.21682(8) 0.0253 1.0000 Uani . . . . . . . N1 N 0.8317(3) 0.5888(3) 0.4336(2) 0.0205 1.0000 Uani . . . . . . . N2 N 0.4381(3) 0.8237(3) 0.4625(2) 0.0191 1.0000 Uani . . . . . . . N3 N 0.1389(3) 0.3787(3) 0.3008(3) 0.0251 1.0000 Uani . . . . . . . N4 N 0.6315(3) 0.1986(4) 0.2840(3) 0.0330 1.0000 Uani . . . . . . . N5 N 1.0769(3) 0.6034(3) 0.4185(2) 0.0189 1.0000 Uani . . . . . . . N6 N 1.0602(3) 0.6370(3) 0.6048(2) 0.0215 1.0000 Uani . . . . . . . N7 N 0.6615(3) 0.9331(3) 0.6069(2) 0.0215 1.0000 Uani . . . . . . . N8 N 0.5968(3) 0.9833(3) 0.4037(3) 0.0200 1.0000 Uani . . . . . . . C2 C 0.4116(3) 0.7297(3) 0.4328(3) 0.0161 1.0000 Uani . . . . . . . C3 C 0.2324(3) 0.3659(3) 0.2942(3) 0.0186 1.0000 Uani . . . . . . . C4 C 0.6141(3) 0.2954(4) 0.2581(3) 0.0225 1.0000 Uani . . . . . . . C5 C 1.1450(4) 0.7017(4) 0.4832(3) 0.0227 1.0000 Uani . . . . . . . C6 C 1.0768(4) 0.7411(4) 0.5492(3) 0.0257 1.0000 Uani . . . . . . . C7 C 0.7343(4) 0.8791(4) 0.5530(3) 0.0268 1.0000 Uani . . . . . . . C8 C 0.7269(4) 0.9590(4) 0.4664(3) 0.0278 1.0000 Uani . . . . . . . C9 C 0.7360(3) 0.6254(3) 0.3894(3) 0.0177 1.0000 Uani . . . . . . . H51 H 1.0140 0.6341 0.3604 0.026(3) 1.0000 Uiso R . . . . . . H52 H 1.1310 0.5568 0.3986 0.026(3) 1.0000 Uiso R . . . . . . H53 H 1.1510 0.7655 0.4422 0.032(3) 1.0000 Uiso R . . . . . . H54 H 1.2247 0.6759 0.5244 0.032(3) 1.0000 Uiso R . . . . . . H61 H 1.1360 0.6164 0.6562 0.029(3) 1.0000 Uiso R . . . . . . H62 H 1.0016 0.6525 0.6341 0.029(3) 1.0000 Uiso R . . . . . . H63 H 1.1224 0.8000 0.5951 0.034(3) 1.0000 Uiso R . . . . . . H64 H 0.9991 0.7719 0.5085 0.034(3) 1.0000 Uiso R . . . . . . H71 H 0.6427 0.8757 0.6472 0.027(3) 1.0000 Uiso R . . . . . . H72 H 0.7069 0.9954 0.6484 0.027(3) 1.0000 Uiso R . . . . . . H73 H 0.7013 0.8040 0.5278 0.034(3) 1.0000 Uiso R . . . . . . H74 H 0.8169 0.8703 0.5977 0.034(3) 1.0000 Uiso R . . . . . . H81 H 0.5904 1.0542 0.3666 0.028(3) 1.0000 Uiso R . . . . . . H82 H 0.5642 0.9197 0.3583 0.028(3) 1.0000 Uiso R . . . . . . H83 H 0.7674 1.0312 0.4923 0.035(3) 1.0000 Uiso R . . . . . . H84 H 0.7653 0.9219 0.4265 0.035(3) 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01355(9) 0.01386(10) 0.01562(9) -0.00004(5) 0.00648(6) 0.00007(5) Ni1 0.0135(3) 0.0192(4) 0.0131(3) -0.0013(2) 0.0066(3) -0.0007(2) Ni2 0.0203(4) 0.0144(3) 0.0147(3) -0.0015(2) 0.0084(3) -0.0016(2) S1 0.0152(4) 0.0156(5) 0.0237(5) 0.0013(4) 0.0076(3) 0.0003(3) S2 0.0229(5) 0.0171(5) 0.0384(6) -0.0081(4) 0.0203(4) -0.0054(4) S3 0.0213(5) 0.0165(5) 0.0347(6) -0.0042(4) 0.0154(4) -0.0023(4) S4 0.0326(5) 0.0234(6) 0.0287(5) -0.0031(4) 0.0218(4) -0.0026(4) N1 0.0148(15) 0.0256(19) 0.0217(17) -0.0005(14) 0.0074(12) 0.0024(13) N2 0.0240(16) 0.0177(18) 0.0203(16) -0.0020(13) 0.0136(13) -0.0014(13) N3 0.0240(17) 0.028(2) 0.0270(19) -0.0048(15) 0.0136(14) -0.0078(15) N4 0.037(2) 0.030(2) 0.034(2) 0.0008(17) 0.0167(17) 0.0050(17) N5 0.0167(15) 0.0243(18) 0.0185(16) -0.0021(13) 0.0099(12) -0.0010(13) N6 0.0185(16) 0.029(2) 0.0211(17) -0.0049(14) 0.0121(13) -0.0051(13) N7 0.0270(17) 0.0186(18) 0.0191(16) -0.0021(13) 0.0088(13) 0.0012(14) N8 0.0265(19) 0.0174(18) 0.0192(17) -0.0009(13) 0.0120(15) -0.0028(13) C2 0.0155(17) 0.017(2) 0.0180(18) 0.0004(15) 0.0091(14) 0.0016(14) C3 0.0223(19) 0.018(2) 0.0154(18) -0.0013(15) 0.0065(14) -0.0033(15) C4 0.0199(19) 0.028(2) 0.020(2) -0.0062(17) 0.0088(15) -0.0020(16) C5 0.025(2) 0.023(2) 0.025(2) -0.0019(17) 0.0149(16) -0.0039(16) C6 0.028(2) 0.025(2) 0.028(2) -0.0047(17) 0.0148(17) -0.0028(17) C7 0.023(2) 0.027(2) 0.030(2) -0.0035(18) 0.0089(17) 0.0025(17) C8 0.029(2) 0.024(2) 0.034(2) -0.0039(19) 0.0170(19) -0.0018(18) C9 0.0208 0.0156 0.0188 -0.0016 0.0099 -0.0029 _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.2133(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . S1 . 2.3213(10) yes Pt1 . S2 . 2.3137(10) yes Pt1 . S3 . 2.3282(10) yes Pt1 . S4 . 2.3368(10) yes Ni1 . N1 2_766 2.109(3) yes Ni1 . N6 2_766 2.090(3) yes Ni1 . N5 2_766 2.085(3) yes Ni1 . N1 . 2.109(3) yes Ni1 . N5 . 2.085(3) yes Ni1 . N6 . 2.090(3) yes Ni2 . N2 2_676 2.127(3) yes Ni2 . N8 2_676 2.102(4) yes Ni2 . N7 2_676 2.089(3) yes Ni2 . N2 . 2.127(3) yes Ni2 . N7 . 2.089(3) yes Ni2 . N8 . 2.102(4) yes S1 . C9 . 1.679(4) yes S2 . C2 . 1.678(4) yes S3 . C3 . 1.686(4) yes S4 . C4 . 1.680(5) yes N1 . C9 . 1.146(5) yes N2 . C2 . 1.147(5) yes N3 . C3 . 1.151(5) yes N4 . C4 . 1.152(6) yes N5 . C5 . 1.479(5) yes N5 . H51 . 0.950 no N5 . H52 . 0.950 no N6 . C6 . 1.477(5) yes N6 . H61 . 0.950 no N6 . H62 . 0.950 no N7 . C7 . 1.484(5) yes N7 . H71 . 0.950 no N7 . H72 . 0.950 no N8 . C8 . 1.486(5) yes N8 . H81 . 0.950 no N8 . H82 . 0.950 no C5 . C6 . 1.519(5) yes C5 . H53 . 0.950 no C5 . H54 . 0.950 no C6 . H63 . 0.950 no C6 . H64 . 0.950 no C7 . C8 . 1.511(6) yes C7 . H73 . 0.950 no C7 . H74 . 0.950 no C8 . H83 . 0.950 no C8 . H84 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 . Pt1 . S2 . 94.63(4) yes S1 . Pt1 . S3 . 174.28(3) yes S2 . Pt1 . S3 . 90.87(4) yes S1 . Pt1 . S4 . 86.19(4) yes S2 . Pt1 . S4 . 177.94(4) yes S3 . Pt1 . S4 . 88.26(4) yes N1 2_766 Ni1 . N6 2_766 88.78(13) yes N1 2_766 Ni1 . N5 2_766 90.71(12) yes N6 2_766 Ni1 . N5 2_766 83.16(12) yes N1 2_766 Ni1 . N1 . 179.995 yes N6 2_766 Ni1 . N1 . 91.22(13) yes N5 2_766 Ni1 . N1 . 89.29(13) yes N1 2_766 Ni1 . N5 . 89.29(12) yes N6 2_766 Ni1 . N5 . 96.84(12) yes N5 2_766 Ni1 . N5 . 179.994 yes N1 . Ni1 . N5 . 90.71(12) yes N1 2_766 Ni1 . N6 . 91.22(13) yes N6 2_766 Ni1 . N6 . 179.995 yes N5 2_766 Ni1 . N6 . 96.84(13) yes N1 . Ni1 . N6 . 88.78(13) yes N5 . Ni1 . N6 . 83.16(13) yes N2 2_676 Ni2 . N8 2_676 88.23(12) yes N2 2_676 Ni2 . N7 2_676 88.65(13) yes N8 2_676 Ni2 . N7 2_676 82.96(13) yes N2 2_676 Ni2 . N2 . 179.995 yes N8 2_676 Ni2 . N2 . 91.77(12) yes N7 2_676 Ni2 . N2 . 91.35(13) yes N2 2_676 Ni2 . N7 . 91.35(13) yes N8 2_676 Ni2 . N7 . 97.04(13) yes N7 2_676 Ni2 . N7 . 179.995 yes N2 . Ni2 . N7 . 88.65(13) yes N2 2_676 Ni2 . N8 . 91.77(12) yes N8 2_676 Ni2 . N8 . 179.995 yes N7 2_676 Ni2 . N8 . 97.04(13) yes N2 . Ni2 . N8 . 88.23(12) yes N7 . Ni2 . N8 . 82.96(13) yes Pt1 . S1 . C9 . 100.13(13) yes Pt1 . S2 . C2 . 109.79(13) yes Pt1 . S3 . C3 . 109.05(14) yes Pt1 . S4 . C4 . 103.71(14) yes Ni1 . N1 . C9 . 171.5(3) yes Ni2 . N2 . C2 . 170.9(3) yes Ni1 . N5 . C5 . 108.8(2) yes Ni1 . N5 . H51 . 109.6 no C5 . N5 . H51 . 109.6 no Ni1 . N5 . H52 . 109.6 no C5 . N5 . H52 . 109.8 no H51 . N5 . H52 . 109.5 no Ni1 . N6 . C6 . 106.6(2) yes Ni1 . N6 . H61 . 110.0 no C6 . N6 . H61 . 109.7 no Ni1 . N6 . H62 . 110.3 no C6 . N6 . H62 . 110.7 no H61 . N6 . H62 . 109.5 no Ni2 . N7 . C7 . 108.4(2) yes Ni2 . N7 . H71 . 109.7 no C7 . N7 . H71 . 110.2 no Ni2 . N7 . H72 . 109.6 no C7 . N7 . H72 . 109.4 no H71 . N7 . H72 . 109.5 no Ni2 . N8 . C8 . 108.2(3) yes Ni2 . N8 . H81 . 109.9 no C8 . N8 . H81 . 110.1 no Ni2 . N8 . H82 . 109.6 no C8 . N8 . H82 . 109.6 no H81 . N8 . H82 . 109.5 no S2 . C2 . N2 . 174.9(3) yes S3 . C3 . N3 . 175.9(4) yes S4 . C4 . N4 . 178.3(4) yes N5 . C5 . C6 . 108.7(3) yes N5 . C5 . H53 . 109.6 no C6 . C5 . H53 . 109.8 no N5 . C5 . H54 . 109.6 no C6 . C5 . H54 . 109.6 no H53 . C5 . H54 . 109.5 no C5 . C6 . N6 . 107.9(3) yes C5 . C6 . H63 . 110.0 no N6 . C6 . H63 . 110.2 no C5 . C6 . H64 . 109.9 no N6 . C6 . H64 . 109.4 no H63 . C6 . H64 . 109.5 no N7 . C7 . C8 . 108.1(3) yes N7 . C7 . H73 . 109.4 no C8 . C7 . H73 . 109.7 no N7 . C7 . H74 . 109.9 no C8 . C7 . H74 . 110.2 no H73 . C7 . H74 . 109.5 no C7 . C8 . N8 . 109.7(3) yes C7 . C8 . H83 . 109.3 no N8 . C8 . H83 . 109.3 no C7 . C8 . H84 . 109.5 no N8 . C8 . H84 . 109.6 no H83 . C8 . H84 . 109.5 no S1 . C9 . N1 . 178.7(4) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag N5 . H51 . N4 3_655 176 0.95 2.26 3.206(6) yes N5 . H51 . C4 3_655 156 0.95 2.57 3.456(6) yes N5 . H52 . N3 1_655 143 0.95 2.48 3.284(6) yes N6 . H62 . N3 2_666 160 0.95 2.21 3.122(6) yes N7 . H72 . C3 4_565 147 0.95 2.54 3.378(6) yes N8 . H81 . N4 1_565 162 0.95 2.18 3.096(6) yes data_C19H11MnN7PtS4 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C19 H11 Mn1 N7 Pt1 S4' _chemical_formula_moiety 'C19 H11 Mn1 N7 Pt1 S4' _chemical_compound_source ? _chemical_formula_weight 715.63 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' #------------------------------------------------ _cell_length_a 9.9635(16) _cell_length_b 13.508(2) _cell_length_c 16.235(3) _cell_angle_alpha 90 _cell_angle_beta 90.776(2) _cell_angle_gamma 90 _cell_volume 2184.8(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7345 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 27.91 _cell_measurement_temperature 100 _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 2.175 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 7.380 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device 'Unknown' _diffrn_measurement_device_type 'Serial' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 12563 _reflns_number_total 5069 _diffrn_reflns_av_R_equivalents 0.023 # Number of reflections with Friedels Law is 5069 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5239 _diffrn_reflns_theta_min 1.961 _diffrn_reflns_theta_max 27.958 _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.721 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #========================================================================== # 8. REFINEMENT DATA _refine_diff_density_min -0.65 _refine_diff_density_max 1.21 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 4527 _refine_ls_number_restraints 0 _refine_ls_number_parameters 289 _oxford_refine_ls_R_factor_ref 0.0245 _refine_ls_wR_factor_ref 0.0338 _refine_ls_goodness_of_fit_ref 1.2249 _refine_ls_shift/su_max 0.002239 # The values computed from all data _oxford_reflns_number_all 5069 _refine_ls_R_factor_all 0.0295 _refine_ls_wR_factor_all 0.0366 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4620 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_gt 0.0344 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Pt1 Pt 0.917761(13) 0.348111(10) 0.312591(8) 0.0131 1.0000 Uani . . . . . . . Mn1 Mn 0.63843(5) 0.74195(4) 0.35283(3) 0.0121 1.0000 Uani . . . . . . . S1 S 0.99230(10) 0.48323(7) 0.38930(7) 0.0210 1.0000 Uani . . . . . . . S2 S 0.76452(10) 0.44461(7) 0.24069(6) 0.0188 1.0000 Uani . . . . . . . S3 S 0.86894(10) 0.20274(7) 0.24213(6) 0.0197 1.0000 Uani . . . . . . . S4 S 1.07750(9) 0.25994(7) 0.39188(6) 0.0159 1.0000 Uani . . . . . . . N1 N 0.7978(3) 0.6356(2) 0.3871(2) 0.0192 1.0000 Uani . . . . . . . N2 N 0.5335(3) 0.3321(2) 0.2009(2) 0.0183 1.0000 Uani . . . . . . . N3 N 0.8614(5) 0.2531(3) 0.0727(2) 0.0380 1.0000 Uani . . . . . . . N4 N 1.2731(3) 0.2350(2) 0.2692(2) 0.0188 1.0000 Uani . . . . . . . N5 N 0.4863(3) 0.6261(2) 0.3848(2) 0.0139 1.0000 Uani . . . . . . . N6 N 0.5588(3) 0.7793(2) 0.47613(19) 0.0128 1.0000 Uani . . . . . . . N7 N 0.7453(3) 0.8781(2) 0.3982(2) 0.0145 1.0000 Uani . . . . . . . C1 C 0.8742(4) 0.5720(3) 0.3853(2) 0.0175 1.0000 Uani . . . . . . . C2 C 0.6321(4) 0.3728(3) 0.2178(2) 0.0158 1.0000 Uani . . . . . . . C3 C 0.8655(4) 0.2355(3) 0.1424(3) 0.0210 1.0000 Uani . . . . . . . C4 C 1.1928(4) 0.2441(3) 0.3189(2) 0.0130 1.0000 Uani . . . . . . . C5 C 0.4625(4) 0.5459(3) 0.3391(2) 0.0171 1.0000 Uani . . . . . . . C6 C 0.3798(4) 0.4690(3) 0.3638(2) 0.0187 1.0000 Uani . . . . . . . C7 C 0.3187(4) 0.4772(3) 0.4404(3) 0.0209 1.0000 Uani . . . . . . . C8 C 0.3410(4) 0.5598(3) 0.4873(2) 0.0173 1.0000 Uani . . . . . . . C9 C 0.4261(4) 0.6345(3) 0.4585(2) 0.0146 1.0000 Uani . . . . . . . C10 C 0.4593(4) 0.7243(3) 0.5070(2) 0.0129 1.0000 Uani . . . . . . . C11 C 0.3955(4) 0.7522(3) 0.5787(2) 0.0183 1.0000 Uani . . . . . . . C12 C 0.4356(4) 0.8379(3) 0.6182(3) 0.0196 1.0000 Uani . . . . . . . C13 C 0.5379(4) 0.8940(3) 0.5854(2) 0.0193 1.0000 Uani . . . . . . . C14 C 0.5974(4) 0.8628(3) 0.5137(2) 0.0128 1.0000 Uani . . . . . . . C15 C 0.7071(4) 0.9184(3) 0.4708(2) 0.0138 1.0000 Uani . . . . . . . C16 C 0.7650(4) 1.0035(3) 0.5020(2) 0.0174 1.0000 Uani . . . . . . . C17 C 0.8658(4) 1.0503(3) 0.4574(3) 0.0211 1.0000 Uani . . . . . . . C18 C 0.9056(4) 1.0092(3) 0.3842(2) 0.0188 1.0000 Uani . . . . . . . C19 C 0.8437(4) 0.9234(3) 0.3570(2) 0.0196 1.0000 Uani . . . . . . . H51 H 0.5038 0.5413 0.2868 0.0232 1.0000 Uiso R . . . . . . H61 H 0.3647 0.4130 0.3295 0.0248 1.0000 Uiso R . . . . . . H71 H 0.2628 0.4255 0.4599 0.0266 1.0000 Uiso R . . . . . . H81 H 0.2988 0.5673 0.5390 0.0227 1.0000 Uiso R . . . . . . H111 H 0.3245 0.7133 0.5999 0.0234 1.0000 Uiso R . . . . . . H121 H 0.3939 0.8576 0.6679 0.0266 1.0000 Uiso R . . . . . . H131 H 0.5664 0.9533 0.6118 0.0254 1.0000 Uiso R . . . . . . H161 H 0.7363 1.0303 0.5529 0.0236 1.0000 Uiso R . . . . . . H171 H 0.9067 1.1092 0.4775 0.0279 1.0000 Uiso R . . . . . . H181 H 0.9744 1.0394 0.3529 0.0246 1.0000 Uiso R . . . . . . H191 H 0.8718 0.8952 0.3065 0.0259 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01087(9) 0.01409(9) 0.01445(9) 0.00067(5) 0.00199(6) 0.00001(5) Mn1 0.0106(3) 0.0118(3) 0.0142(3) 0.0001(2) 0.0028(2) -0.0011(2) S1 0.0159(5) 0.0188(5) 0.0281(5) -0.0050(4) -0.0050(4) 0.0036(4) S2 0.0157(5) 0.0162(4) 0.0244(5) 0.0018(4) -0.0038(4) -0.0007(4) S3 0.0240(5) 0.0151(4) 0.0202(5) 0.0005(4) 0.0006(4) -0.0006(4) S4 0.0159(5) 0.0170(4) 0.0149(4) 0.0007(3) 0.0038(3) 0.0009(3) N1 0.0176(17) 0.0149(15) 0.0251(18) 0.0022(13) -0.0003(14) 0.0000(13) N2 0.0141(16) 0.0218(17) 0.0191(17) -0.0016(13) 0.0014(13) 0.0053(13) N3 0.060(3) 0.027(2) 0.027(2) 0.0020(17) -0.0037(19) -0.005(2) N4 0.0177(17) 0.0200(17) 0.0187(17) -0.0020(13) 0.0001(13) 0.0017(13) N5 0.0103(15) 0.0142(14) 0.0173(16) 0.0021(12) 0.0019(12) 0.0008(12) N6 0.0098(15) 0.0140(14) 0.0147(15) 0.0001(11) -0.0003(11) 0.0016(11) N7 0.0116(15) 0.0143(15) 0.0177(16) -0.0012(12) 0.0011(12) -0.0044(12) C1 0.0169(19) 0.0173(18) 0.0183(19) -0.0005(14) 0.0006(15) -0.0043(15) C2 0.0178(19) 0.0165(17) 0.0133(18) -0.0006(14) 0.0026(15) 0.0042(15) C3 0.022(2) 0.0173(19) 0.024(2) -0.0022(16) -0.0028(16) -0.0016(15) C4 0.0118(17) 0.0109(16) 0.0162(18) 0.0011(13) -0.0017(14) -0.0005(13) C5 0.0166(19) 0.0144(18) 0.0203(19) -0.0009(14) 0.0025(15) 0.0020(15) C6 0.0160(19) 0.0171(19) 0.023(2) -0.0016(15) -0.0001(15) -0.0035(15) C7 0.0129(19) 0.019(2) 0.031(2) 0.0044(16) 0.0009(16) -0.0056(15) C8 0.0126(18) 0.0172(18) 0.0223(19) 0.0032(15) 0.0046(15) -0.0009(14) C9 0.0117(18) 0.0144(17) 0.0179(19) -0.0019(14) 0.0034(15) 0.0025(14) C10 0.0105(17) 0.0134(17) 0.0150(17) 0.0049(13) 0.0006(13) -0.0014(13) C11 0.0131(18) 0.023(2) 0.0196(19) 0.0014(15) 0.0069(15) -0.0016(15) C12 0.018(2) 0.023(2) 0.019(2) -0.0044(15) 0.0057(16) 0.0004(15) C13 0.021(2) 0.0191(19) 0.0182(19) -0.0038(15) 0.0000(16) -0.0011(16) C14 0.0112(17) 0.0112(16) 0.0160(18) 0.0010(13) 0.0013(14) 0.0010(13) C15 0.0112(17) 0.0146(17) 0.0157(18) 0.0031(14) -0.0012(14) 0.0019(13) C16 0.019(2) 0.0168(18) 0.0166(19) -0.0027(14) -0.0001(15) -0.0019(15) C17 0.020(2) 0.0164(18) 0.027(2) -0.0017(16) -0.0026(16) -0.0040(15) C18 0.0144(19) 0.0195(19) 0.023(2) 0.0035(15) 0.0051(15) -0.0051(15) C19 0.019(2) 0.0191(19) 0.021(2) -0.0033(15) 0.0040(16) 0.0000(15) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.2320(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . S1 . 2.3257(10) yes Pt1 . S2 . 2.3118(10) yes Pt1 . S3 . 2.3208(10) yes Pt1 . S4 . 2.3565(10) yes Mn1 . N4 3_755 2.181(3) yes Mn1 . N2 3_655 2.267(4) yes Mn1 . N1 . 2.207(3) yes Mn1 . N5 . 2.244(3) yes Mn1 . N6 . 2.221(3) yes Mn1 . N7 . 2.244(3) yes S1 . C1 . 1.681(4) yes S2 . C2 . 1.676(4) yes S3 . C3 . 1.678(4) yes S4 . C4 . 1.675(4) yes N1 . C1 . 1.148(5) yes N2 . C2 . 1.155(5) yes N3 . C3 . 1.157(5) yes N4 . C4 . 1.151(5) yes N5 . C5 . 1.333(5) yes N5 . C9 . 1.350(5) yes N6 . C10 . 1.342(4) yes N6 . C14 . 1.336(5) yes N7 . C15 . 1.358(5) yes N7 . C19 . 1.342(5) yes C5 . C6 . 1.389(5) yes C5 . H51 . 0.950 no C6 . C7 . 1.395(6) yes C6 . H61 . 0.950 no C7 . C8 . 1.369(6) yes C7 . H71 . 0.950 no C8 . C9 . 1.402(5) yes C8 . H81 . 0.950 no C9 . C10 . 1.481(5) yes C10 . C11 . 1.386(5) yes C11 . C12 . 1.381(5) yes C11 . H111 . 0.950 no C12 . C13 . 1.382(5) yes C12 . H121 . 0.950 no C13 . C14 . 1.380(5) yes C13 . H131 . 0.950 no C14 . C15 . 1.505(5) yes C15 . C16 . 1.379(5) yes C16 . C17 . 1.396(5) yes C16 . H161 . 0.950 no C17 . C18 . 1.376(5) yes C17 . H171 . 0.950 no C18 . C19 . 1.382(5) yes C18 . H181 . 0.950 no C19 . H191 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 . Pt1 . S2 . 91.82(4) yes S1 . Pt1 . S3 . 172.42(4) yes S2 . Pt1 . S3 . 95.49(4) yes S1 . Pt1 . S4 . 84.01(4) yes S2 . Pt1 . S4 . 175.81(3) yes S3 . Pt1 . S4 . 88.69(3) yes N4 3_755 Mn1 . N2 3_655 89.21(13) yes N4 3_755 Mn1 . N1 . 84.42(13) yes N2 3_655 Mn1 . N1 . 169.78(13) yes N4 3_755 Mn1 . N5 . 117.57(12) yes N2 3_655 Mn1 . N5 . 87.37(12) yes N1 . Mn1 . N5 . 88.50(12) yes N4 3_755 Mn1 . N6 . 169.09(12) yes N2 3_655 Mn1 . N6 . 86.97(12) yes N1 . Mn1 . N6 . 100.69(12) yes N5 . Mn1 . N6 . 72.48(11) yes N4 3_755 Mn1 . N7 . 97.91(12) yes N2 3_655 Mn1 . N7 . 92.24(12) yes N1 . Mn1 . N7 . 96.54(12) yes N5 . Mn1 . N7 . 144.51(12) yes N6 . Mn1 . N7 . 72.06(11) yes Pt1 . S1 . C1 . 108.72(14) yes Pt1 . S2 . C2 . 107.36(14) yes Pt1 . S3 . C3 . 104.71(14) yes Pt1 . S4 . C4 . 98.20(13) yes Mn1 . N1 . C1 . 162.8(3) yes Mn1 3_645 N2 . C2 . 169.3(3) yes Mn1 3_745 N4 . C4 . 157.8(3) yes Mn1 . N5 . C5 . 123.6(2) yes Mn1 . N5 . C9 . 117.2(2) yes C5 . N5 . C9 . 118.9(3) yes Mn1 . N6 . C10 . 119.1(2) yes Mn1 . N6 . C14 . 119.9(2) yes C10 . N6 . C14 . 120.5(3) yes Mn1 . N7 . C15 . 118.4(2) yes Mn1 . N7 . C19 . 123.8(3) yes C15 . N7 . C19 . 117.7(3) yes S1 . C1 . N1 . 175.3(4) yes S2 . C2 . N2 . 173.0(4) yes S3 . C3 . N3 . 176.5(4) yes S4 . C4 . N4 . 178.6(3) yes N5 . C5 . C6 . 123.3(3) yes N5 . C5 . H51 . 118.4 no C6 . C5 . H51 . 118.3 no C5 . C6 . C7 . 117.8(4) yes C5 . C6 . H61 . 121.0 no C7 . C6 . H61 . 121.1 no C6 . C7 . C8 . 119.4(3) yes C6 . C7 . H71 . 120.3 no C8 . C7 . H71 . 120.4 no C7 . C8 . C9 . 119.7(3) yes C7 . C8 . H81 . 120.5 no C9 . C8 . H81 . 119.8 no C8 . C9 . N5 . 120.9(3) yes C8 . C9 . C10 . 122.9(3) yes N5 . C9 . C10 . 116.2(3) yes C9 . C10 . N6 . 114.5(3) yes C9 . C10 . C11 . 124.6(3) yes N6 . C10 . C11 . 120.8(3) yes C10 . C11 . C12 . 119.0(4) yes C10 . C11 . H111 . 120.4 no C12 . C11 . H111 . 120.5 no C11 . C12 . C13 . 119.4(4) yes C11 . C12 . H121 . 120.1 no C13 . C12 . H121 . 120.5 no C12 . C13 . C14 . 119.0(4) yes C12 . C13 . H131 . 120.4 no C14 . C13 . H131 . 120.5 no C13 . C14 . N6 . 121.2(3) yes C13 . C14 . C15 . 124.1(3) yes N6 . C14 . C15 . 114.6(3) yes C14 . C15 . N7 . 114.5(3) yes C14 . C15 . C16 . 123.3(3) yes N7 . C15 . C16 . 122.1(3) yes C15 . C16 . C17 . 119.2(4) yes C15 . C16 . H161 . 120.5 no C17 . C16 . H161 . 120.3 no C16 . C17 . C18 . 118.9(4) yes C16 . C17 . H171 . 120.7 no C18 . C17 . H171 . 120.5 no C17 . C18 . C19 . 118.7(4) yes C17 . C18 . H181 . 120.4 no C19 . C18 . H181 . 120.8 no C18 . C19 . N7 . 123.3(4) yes C18 . C19 . H191 . 118.4 no N7 . C19 . H191 . 118.2 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C17 . H171 . N3 4_565 140 0.95 2.46 3.250(5) yes data_C34H22N10MnPtS4 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C22.67 H14.67 Mn0.67 N6.67 Pt0.67 S2.67' _chemical_formula_moiety 'C22.67 H14.67 Mn0.67 N6.67 Pt0.67 S2.67' _chemical_compound_source ? _chemical_formula_weight 632.60 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' #------------------------------------------------ _cell_length_a 19.387(4) _cell_length_b 8.4368(19) _cell_length_c 23.520(5) _cell_angle_alpha 90 _cell_angle_beta 112.315(5) _cell_angle_gamma 90 _cell_volume 3558.8(14) _cell_formula_units_Z 6 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 293 _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_max 0.48 _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1852 _exptl_absorpt_coefficient_mu 4.558 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device_type 'Unknown' _diffrn_measurement_device 'Serial' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 56806 _reflns_number_total 5808 _diffrn_reflns_av_R_equivalents 0.043 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 5808 # Theoretical number of reflections is about 11645 _diffrn_reflns_theta_min 1.135 _diffrn_reflns_theta_max 24.359 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.359 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min -22 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 9 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _oxford_diffrn_Wilson_B_factor 4.66 _oxford_diffrn_Wilson_scale 418.25 _atom_sites_solution_primary Direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap #========================================================================== # 8. REFINEMENT DATA _refine_diff_density_min -0.45 _refine_diff_density_max 1.00 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 3249 _refine_ls_number_restraints 0 _refine_ls_number_parameters 455 _oxford_refine_ls_R_factor_ref 0.0333 _refine_ls_wR_factor_ref 0.0474 _refine_ls_goodness_of_fit_ref 1.2109 _refine_ls_shift/su_max 0.0004811 _refine_ls_shift/su_mean 0.0000274 # The values computed from all data _oxford_reflns_number_all 5808 _refine_ls_R_factor_all 0.0736 _refine_ls_wR_factor_all 0.0929 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3465 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_gt 0.0498 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F) + ( 0.03P)^2^ + 0.00P] ,where P=(max(Fo,0) + 2Fc)/3 ; #========================================================== # 9. General computing _computing_data_collection 'Bruker Apex2' _computing_cell_refinement 'Bruker Apex2' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pt1 Pt 0.5000 0.5000 0.5000 0.0646 1.0000 Uani S . . . . . Pt2 Pt 1.0000 0.0000 1.0000 0.0705 1.0000 Uani S . . . . . Mn3 Mn 0.75472(6) 0.48230(10) 0.75808(4) 0.0556 1.0000 Uani . . . . . . S3 S 0.48870(13) 0.2314(2) 0.47685(13) 0.1147 1.0000 Uani . . . . . . S4 S 1.03881(12) 0.1718(3) 1.08314(9) 0.1097 1.0000 Uani . . . . . . S1 S 0.46289(16) 0.4505(3) 0.58012(11) 0.1160 1.0000 Uani . . . . . . S2 S 1.11652(13) 0.0207(3) 0.99499(11) 0.1127 1.0000 Uani . . . . . . N1 N 0.3962(5) 0.7137(13) 0.6098(4) 0.1561 1.0000 Uani . . . . . . N5 N 0.8750(3) 0.4019(6) 0.7976(3) 0.0596 1.0000 Uani . . . . . . N6 N 0.7854(3) 0.7088(6) 0.7244(2) 0.0548 1.0000 Uani . . . . . . N7 N 0.7256(3) 0.4574(6) 0.6587(2) 0.0574 1.0000 Uani . . . . . . N8 N 0.7008(3) 0.2443(6) 0.7292(2) 0.0560 1.0000 Uani . . . . . . N3 N 0.6573(4) 0.5606(7) 0.7801(3) 0.0596 1.0000 Uani . . . . . . N4 N 0.7906(3) 0.4738(5) 0.8586(2) 0.0586 1.0000 Uani . . . . . . N2 N 0.3571(4) 0.1203(7) 0.4846(3) 0.0840 1.0000 Uani . . . . . . N10 N 0.9282(5) 0.2232(12) 1.1293(4) 0.1479 1.0000 Uani . . . . . . N9 N 1.2256(5) 0.0970(13) 1.1082(4) 0.1528 1.0000 Uani . . . . . . C1 C 0.4253(5) 0.6099(12) 0.5963(4) 0.1088 1.0000 Uani . . . . . . C2 C 0.4099(5) 0.1704(8) 0.4835(3) 0.0668 1.0000 Uani . . . . . . C10 C 0.9715(5) 0.1970(11) 1.1094(4) 0.0990 1.0000 Uani . . . . . . C15 C 0.6758(3) 0.2111(8) 0.6691(3) 0.0580 1.0000 Uani . . . . . . C17 C 0.6670(4) 0.5689(8) 0.8397(3) 0.0565 1.0000 Uani . . . . . . C18 C 0.8150(4) 0.8320(8) 0.7608(3) 0.0676 1.0000 Uani . . . . . . C19 C 0.6979(3) 0.3202(7) 0.6311(3) 0.0534 1.0000 Uani . . . . . . C20 C 0.7786(3) 0.7170(7) 0.6655(3) 0.0492 1.0000 Uani . . . . . . C21 C 0.7489(3) 0.5760(8) 0.6292(3) 0.0550 1.0000 Uani . . . . . . C22 C 0.9760(5) 0.3190(10) 0.8867(4) 0.1010 1.0000 Uani . . . . . . C25 C 0.7148(4) 0.3993(10) 0.5414(3) 0.0770 1.0000 Uani . . . . . . C26 C 0.6925(3) 0.2900(8) 0.5725(3) 0.0698 1.0000 Uani . . . . . . C27 C 0.6319(4) 0.0810(9) 0.6452(4) 0.0787 1.0000 Uani . . . . . . C28 C 0.9062(4) 0.3800(8) 0.8590(3) 0.0648 1.0000 Uani . . . . . . C29 C 0.6834(4) 0.1480(8) 0.7660(3) 0.0716 1.0000 Uani . . . . . . C30 C 0.9142(4) 0.3674(8) 0.7640(3) 0.0743 1.0000 Uani . . . . . . C31 C 0.7984(4) 0.8474(8) 0.6418(3) 0.0717 1.0000 Uani . . . . . . C32 C 0.8306(5) 0.9724(9) 0.6797(5) 0.0829 1.0000 Uani . . . . . . C33 C 0.8323(6) 0.4460(11) 0.9823(4) 0.1159 1.0000 Uani . . . . . . C34 C 0.8590(4) 0.4224(8) 0.8936(3) 0.0630 1.0000 Uani . . . . . . C35 C 0.7426(4) 0.5489(9) 0.5688(3) 0.0720 1.0000 Uani . . . . . . C37 C 0.8398(5) 0.9669(8) 0.7406(4) 0.0811 1.0000 Uani . . . . . . C38 C 1.0154(4) 0.2802(11) 0.8516(4) 0.1128 1.0000 Uani . . . . . . C39 C 0.6146(5) -0.0228(8) 0.6835(4) 0.0914 1.0000 Uani . . . . . . C40 C 0.7418(4) 0.5168(7) 0.8834(3) 0.0622 1.0000 Uani . . . . . . C43 C 0.5920(5) 0.5993(8) 0.7382(3) 0.0701 1.0000 Uani . . . . . . C44 C 0.7609(5) 0.5013(8) 0.9469(3) 0.0908 1.0000 Uani . . . . . . C45 C 0.6123(4) 0.6208(8) 0.8576(3) 0.0786 1.0000 Uani . . . . . . C47 C 0.5454(4) 0.6646(9) 0.8136(4) 0.0875 1.0000 Uani . . . . . . C48 C 0.5350(4) 0.6504(8) 0.7531(3) 0.0813 1.0000 Uani . . . . . . C9 C 1.1777(6) 0.0620(12) 1.0628(4) 0.0981 1.0000 Uani . . . . . . C51 C 0.6409(5) 0.0123(8) 0.7454(4) 0.0787 1.0000 Uani . . . . . . C53 C 0.8811(5) 0.4102(10) 0.9559(3) 0.0946 1.0000 Uani . . . . . . C57 C 0.9854(5) 0.3072(10) 0.7897(4) 0.0938 1.0000 Uani . . . . . . H181 H 0.8202 0.8251 0.8018 0.072(5) 1.0000 Uiso R . . . . . H221 H 0.9969 0.3058 0.9292 0.103(5) 1.0000 Uiso R . . . . . H251 H 0.7126 0.3795 0.5016 0.080(5) 1.0000 Uiso R . . . . . H261 H 0.6732 0.1942 0.5535 0.073(5) 1.0000 Uiso R . . . . . H271 H 0.6142 0.0609 0.6032 0.088(5) 1.0000 Uiso R . . . . . H291 H 0.7001 0.1741 0.8076 0.077(5) 1.0000 Uiso R . . . . . H301 H 0.8935 0.3870 0.7217 0.082(5) 1.0000 Uiso R . . . . . H311 H 0.7906 0.8516 0.6001 0.078(5) 1.0000 Uiso R . . . . . H321 H 0.8471 1.0618 0.6650 0.087(5) 1.0000 Uiso R . . . . . H331 H 0.8457 0.4365 1.0247 0.116(5) 1.0000 Uiso R . . . . . H351 H 0.7576 0.6283 0.5480 0.073(5) 1.0000 Uiso R . . . . . H371 H 0.8606 1.0511 0.7671 0.085(5) 1.0000 Uiso R . . . . . H381 H 1.0625 0.2338 0.8696 0.117(5) 1.0000 Uiso R . . . . . H391 H 0.5841 -0.1110 0.6680 0.092(5) 1.0000 Uiso R . . . . . H431 H 0.5849 0.5908 0.6968 0.076(5) 1.0000 Uiso R . . . . . H441 H 0.7260 0.5270 0.9643 0.097(5) 1.0000 Uiso R . . . . . H451 H 0.6202 0.6266 0.8992 0.084(5) 1.0000 Uiso R . . . . . H471 H 0.5077 0.7037 0.8250 0.094(5) 1.0000 Uiso R . . . . . H481 H 0.4889 0.6760 0.7224 0.089(5) 1.0000 Uiso R . . . . . H511 H 0.6315 -0.0564 0.7729 0.086(5) 1.0000 Uiso R . . . . . H531 H 0.9292 0.3764 0.9802 0.098(5) 1.0000 Uiso R . . . . . H571 H 1.0123 0.2836 0.7653 0.102(5) 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0662(3) 0.0519(2) 0.0645(3) -0.00668(19) 0.0123(2) -0.0055(2) Pt2 0.0606(3) 0.1027(4) 0.0474(3) -0.0042(2) 0.0196(2) 0.0085(2) Mn3 0.0657(7) 0.0597(6) 0.0395(6) -0.0045(4) 0.0177(5) -0.0044(5) S3 0.1146(19) 0.0653(13) 0.184(2) -0.0345(15) 0.0793(18) -0.0192(12) S4 0.0829(16) 0.163(2) 0.0766(15) -0.0426(15) 0.0231(13) 0.0041(15) S1 0.171(3) 0.0897(16) 0.0982(19) -0.0098(14) 0.0638(19) -0.0208(17) S2 0.0739(17) 0.192(3) 0.0773(16) -0.0196(15) 0.0349(14) -0.0017(15) N1 0.169(9) 0.208(10) 0.076(6) -0.042(6) 0.030(5) 0.036(7) N5 0.063(4) 0.060(4) 0.056(4) -0.001(3) 0.022(3) 0.004(3) N6 0.060(4) 0.053(3) 0.050(4) -0.005(3) 0.019(3) -0.006(3) N7 0.060(4) 0.067(4) 0.045(3) -0.003(3) 0.019(3) 0.007(3) N8 0.065(4) 0.057(3) 0.045(3) -0.003(3) 0.021(3) -0.003(3) N3 0.073(5) 0.056(3) 0.051(4) 0.004(3) 0.025(4) 0.007(3) N4 0.063(4) 0.063(4) 0.046(3) 0.001(3) 0.016(3) -0.002(3) N2 0.102(6) 0.081(5) 0.078(5) -0.017(4) 0.043(4) -0.027(4) N10 0.159(8) 0.214(9) 0.087(6) -0.024(6) 0.065(6) 0.039(7) N9 0.098(7) 0.226(10) 0.109(7) 0.007(8) 0.011(6) -0.012(7) C1 0.111(9) 0.147(10) 0.056(6) -0.026(6) 0.018(5) -0.019(7) C2 0.089(7) 0.049(4) 0.056(5) -0.007(3) 0.020(5) -0.009(4) C10 0.104(8) 0.137(8) 0.048(5) -0.006(5) 0.020(5) 0.026(6) C15 0.062(5) 0.058(4) 0.055(5) -0.012(4) 0.024(4) -0.003(4) C17 0.066(6) 0.055(4) 0.050(5) -0.003(4) 0.024(4) -0.001(4) C18 0.078(5) 0.068(5) 0.050(4) -0.006(4) 0.017(4) -0.005(4) C19 0.058(5) 0.058(4) 0.039(4) -0.013(3) 0.013(3) -0.003(3) C20 0.052(4) 0.050(4) 0.045(4) 0.006(3) 0.018(3) 0.001(3) C21 0.052(5) 0.072(4) 0.043(4) 0.009(4) 0.021(4) 0.008(4) C22 0.064(6) 0.160(8) 0.083(6) 0.025(6) 0.032(5) 0.013(6) C25 0.077(6) 0.111(7) 0.039(4) -0.019(5) 0.018(4) 0.003(5) C26 0.069(5) 0.076(5) 0.062(5) -0.013(4) 0.023(4) -0.011(4) C27 0.087(6) 0.079(5) 0.071(5) -0.017(5) 0.032(5) -0.008(5) C28 0.057(5) 0.066(5) 0.064(5) 0.006(4) 0.015(4) 0.004(4) C29 0.086(6) 0.061(5) 0.066(5) -0.005(4) 0.027(4) -0.002(4) C30 0.066(6) 0.083(5) 0.078(6) -0.003(4) 0.031(5) -0.009(4) C31 0.074(6) 0.076(5) 0.061(5) 0.005(4) 0.021(4) 0.001(4) C32 0.082(6) 0.087(7) 0.088(7) 0.026(5) 0.042(6) 0.010(5) C33 0.141(10) 0.156(8) 0.041(5) 0.021(5) 0.024(6) 0.060(7) C34 0.060(6) 0.068(4) 0.052(5) 0.004(4) 0.011(4) 0.009(4) C35 0.067(5) 0.101(6) 0.053(5) 0.013(4) 0.029(4) 0.002(4) C37 0.084(7) 0.057(5) 0.095(7) -0.005(4) 0.027(5) -0.002(4) C38 0.052(6) 0.185(9) 0.099(7) 0.037(7) 0.026(6) 0.026(6) C39 0.115(7) 0.069(5) 0.090(7) -0.022(5) 0.038(6) -0.028(4) C40 0.077(6) 0.068(5) 0.046(4) -0.003(4) 0.028(4) 0.006(4) C43 0.067(6) 0.087(6) 0.050(5) -0.005(4) 0.015(5) -0.001(5) C44 0.107(7) 0.127(7) 0.044(4) 0.003(5) 0.036(5) 0.021(5) C45 0.070(6) 0.108(6) 0.061(5) -0.007(4) 0.027(5) 0.008(5) C47 0.062(6) 0.123(7) 0.081(6) -0.026(5) 0.032(5) 0.005(5) C48 0.065(6) 0.103(6) 0.065(6) -0.017(5) 0.012(5) 0.001(4) C9 0.077(7) 0.140(7) 0.081(7) 0.001(6) 0.033(6) 0.012(6) C51 0.091(6) 0.064(5) 0.087(7) 0.005(4) 0.040(5) -0.004(4) C53 0.096(7) 0.132(7) 0.046(5) 0.014(5) 0.017(5) 0.046(6) C57 0.078(7) 0.126(7) 0.093(7) 0.013(6) 0.050(6) 0.000(5) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.05983(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . S3 2_666 2.322(2) yes Pt1 . S1 2_666 2.296(2) yes Pt1 . S3 . 2.322(2) yes Pt1 . S1 . 2.296(2) yes Pt2 . S4 2_757 2.318(2) yes Pt2 . S2 2_757 2.313(2) yes Pt2 . S4 . 2.318(2) yes Pt2 . S2 . 2.313(2) yes Mn3 . N5 . 2.262(5) yes Mn3 . N6 . 2.234(5) yes Mn3 . N7 . 2.195(5) yes Mn3 . N8 . 2.246(5) yes Mn3 . N3 . 2.239(6) yes Mn3 . N4 . 2.198(5) yes S3 . C2 . 1.675(8) yes S4 . C10 . 1.655(9) yes S1 . C1 . 1.643(11) yes S2 . C9 . 1.623(11) yes N1 . C1 . 1.148(10) yes N5 . C28 . 1.349(7) yes N5 . C30 . 1.319(7) yes N6 . C18 . 1.330(7) yes N6 . C20 . 1.342(7) yes N7 . C19 . 1.336(7) yes N7 . C21 . 1.388(8) yes N8 . C15 . 1.340(7) yes N8 . C29 . 1.320(7) yes N3 . C17 . 1.345(8) yes N3 . C43 . 1.316(8) yes N4 . C34 . 1.340(8) yes N4 . C40 . 1.337(8) yes N2 . C2 . 1.116(7) yes N10 . C10 . 1.129(9) yes N9 . C9 . 1.156(10) yes C15 . C19 . 1.456(8) yes C15 . C27 . 1.371(9) yes C17 . C40 . 1.490(9) yes C17 . C45 . 1.353(8) yes C18 . C37 . 1.389(9) yes C18 . H181 . 0.932 no C19 . C26 . 1.366(8) yes C20 . C21 . 1.451(8) yes C20 . C31 . 1.354(7) yes C21 . C35 . 1.396(9) yes C22 . C28 . 1.360(8) yes C22 . C38 . 1.361(9) yes C22 . H221 . 0.932 no C25 . C26 . 1.345(9) yes C25 . C35 . 1.427(10) yes C25 . H251 . 0.935 no C26 . H261 . 0.931 no C27 . C39 . 1.386(10) yes C27 . H271 . 0.930 no C28 . C34 . 1.482(9) yes C29 . C51 . 1.387(8) yes C29 . H291 . 0.933 no C30 . C57 . 1.377(9) yes C30 . H301 . 0.937 no C31 . C32 . 1.369(9) yes C31 . H311 . 0.935 no C32 . C37 . 1.374(12) yes C32 . H321 . 0.936 no C33 . C44 . 1.397(11) yes C33 . C53 . 1.348(11) yes C33 . H331 . 0.934 no C34 . C53 . 1.366(9) yes C35 . H351 . 0.940 no C37 . H371 . 0.931 no C38 . C57 . 1.366(9) yes C38 . H381 . 0.935 no C39 . C51 . 1.379(11) yes C39 . H391 . 0.934 no C40 . C44 . 1.401(10) yes C43 . C48 . 1.352(8) yes C43 . H431 . 0.933 no C44 . H441 . 0.939 no C45 . C47 . 1.368(8) yes C45 . H451 . 0.934 no C47 . C48 . 1.364(9) yes C47 . H471 . 0.929 no C48 . H481 . 0.935 no C51 . H511 . 0.936 no C53 . H531 . 0.934 no C57 . H571 . 0.932 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S3 2_666 Pt1 . S1 2_666 89.07(9) yes S3 2_666 Pt1 . S3 . 179.995 yes S1 2_666 Pt1 . S3 . 90.93(9) yes S3 2_666 Pt1 . S1 . 90.93(9) yes S1 2_666 Pt1 . S1 . 179.995 yes S3 . Pt1 . S1 . 89.07(9) yes S4 2_757 Pt2 . S2 2_757 89.16(8) yes S4 2_757 Pt2 . S4 . 179.995 yes S2 2_757 Pt2 . S4 . 90.84(8) yes S4 2_757 Pt2 . S2 . 90.84(8) yes S2 2_757 Pt2 . S2 . 179.995 yes S4 . Pt2 . S2 . 89.16(8) yes N5 . Mn3 . N6 . 91.75(18) yes N5 . Mn3 . N7 . 102.5(2) yes N6 . Mn3 . N7 . 72.5(2) yes N5 . Mn3 . N8 . 98.32(18) yes N6 . Mn3 . N8 . 144.5(2) yes N7 . Mn3 . N8 . 72.0(2) yes N5 . Mn3 . N3 . 145.3(2) yes N6 . Mn3 . N3 . 101.01(19) yes N7 . Mn3 . N3 . 112.1(2) yes N8 . Mn3 . N3 . 89.83(19) yes N5 . Mn3 . N4 . 72.1(2) yes N6 . Mn3 . N4 . 113.03(18) yes N7 . Mn3 . N4 . 171.97(19) yes N8 . Mn3 . N4 . 102.50(18) yes N3 . Mn3 . N4 . 73.2(2) yes Pt1 . S3 . C2 . 106.6(2) yes Pt2 . S4 . C10 . 110.2(3) yes Pt1 . S1 . C1 . 110.3(4) yes Pt2 . S2 . C9 . 109.2(3) yes Mn3 . N5 . C28 . 117.0(5) yes Mn3 . N5 . C30 . 123.9(5) yes C28 . N5 . C30 . 119.0(6) yes Mn3 . N6 . C18 . 123.2(4) yes Mn3 . N6 . C20 . 118.3(4) yes C18 . N6 . C20 . 118.3(5) yes Mn3 . N7 . C19 . 119.6(4) yes Mn3 . N7 . C21 . 117.6(4) yes C19 . N7 . C21 . 121.8(5) yes Mn3 . N8 . C15 . 116.5(4) yes Mn3 . N8 . C29 . 123.9(4) yes C15 . N8 . C29 . 118.8(6) yes Mn3 . N3 . C17 . 117.4(5) yes Mn3 . N3 . C43 . 123.8(5) yes C17 . N3 . C43 . 118.8(6) yes Mn3 . N4 . C34 . 120.5(4) yes Mn3 . N4 . C40 . 118.3(5) yes C34 . N4 . C40 . 121.2(6) yes S1 . C1 . N1 . 174.7(11) yes S3 . C2 . N2 . 174.3(7) yes S4 . C10 . N10 . 175.2(10) yes N8 . C15 . C19 . 116.3(6) yes N8 . C15 . C27 . 121.3(6) yes C19 . C15 . C27 . 122.4(6) yes N3 . C17 . C40 . 114.8(6) yes N3 . C17 . C45 . 121.6(7) yes C40 . C17 . C45 . 123.6(7) yes N6 . C18 . C37 . 122.7(7) yes N6 . C18 . H181 . 117.9 no C37 . C18 . H181 . 119.3 no C15 . C19 . N7 . 114.0(6) yes C15 . C19 . C26 . 125.0(6) yes N7 . C19 . C26 . 121.0(6) yes N6 . C20 . C21 . 115.4(5) yes N6 . C20 . C31 . 122.3(6) yes C21 . C20 . C31 . 122.3(6) yes C20 . C21 . N7 . 115.3(6) yes C20 . C21 . C35 . 126.6(6) yes N7 . C21 . C35 . 118.2(6) yes C28 . C22 . C38 . 119.1(8) yes C28 . C22 . H221 . 120.6 no C38 . C22 . H221 . 120.4 no C26 . C25 . C35 . 120.3(6) yes C26 . C25 . H251 . 121.3 no C35 . C25 . H251 . 118.4 no C19 . C26 . C25 . 120.2(7) yes C19 . C26 . H261 . 120.5 no C25 . C26 . H261 . 119.3 no C15 . C27 . C39 . 120.4(7) yes C15 . C27 . H271 . 120.2 no C39 . C27 . H271 . 119.5 no C22 . C28 . N5 . 121.7(7) yes C22 . C28 . C34 . 122.5(7) yes N5 . C28 . C34 . 115.8(7) yes N8 . C29 . C51 . 123.1(7) yes N8 . C29 . H291 . 117.9 no C51 . C29 . H291 . 119.0 no N5 . C30 . C57 . 121.9(7) yes N5 . C30 . H301 . 119.1 no C57 . C30 . H301 . 119.0 no C20 . C31 . C32 . 119.2(7) yes C20 . C31 . H311 . 120.3 no C32 . C31 . H311 . 120.4 no C31 . C32 . C37 . 119.9(7) yes C31 . C32 . H321 . 121.0 no C37 . C32 . H321 . 119.1 no C44 . C33 . C53 . 120.7(8) yes C44 . C33 . H331 . 118.5 no C53 . C33 . H331 . 120.8 no C28 . C34 . N4 . 114.4(6) yes C28 . C34 . C53 . 124.3(7) yes N4 . C34 . C53 . 121.2(7) yes C25 . C35 . C21 . 118.4(6) yes C25 . C35 . H351 . 122.2 no C21 . C35 . H351 . 119.4 no C18 . C37 . C32 . 117.4(7) yes C18 . C37 . H371 . 120.9 no C32 . C37 . H371 . 121.6 no C22 . C38 . C57 . 119.8(8) yes C22 . C38 . H381 . 120.3 no C57 . C38 . H381 . 119.9 no C27 . C39 . C51 . 117.8(7) yes C27 . C39 . H391 . 121.5 no C51 . C39 . H391 . 120.7 no C17 . C40 . N4 . 116.3(6) yes C17 . C40 . C44 . 123.9(7) yes N4 . C40 . C44 . 119.7(7) yes N3 . C43 . C48 . 122.3(7) yes N3 . C43 . H431 . 118.8 no C48 . C43 . H431 . 118.9 no C40 . C44 . C33 . 117.9(7) yes C40 . C44 . H441 . 120.0 no C33 . C44 . H441 . 122.1 no C17 . C45 . C47 . 118.9(7) yes C17 . C45 . H451 . 120.5 no C47 . C45 . H451 . 120.6 no C45 . C47 . C48 . 119.1(7) yes C45 . C47 . H471 . 120.2 no C48 . C47 . H471 . 120.6 no C47 . C48 . C43 . 119.1(7) yes C47 . C48 . H481 . 120.3 no C43 . C48 . H481 . 120.6 no S2 . C9 . N9 . 173.3(10) yes C29 . C51 . C39 . 118.6(7) yes C29 . C51 . H511 . 121.0 no C39 . C51 . H511 . 120.4 no C34 . C53 . C33 . 119.2(8) yes C34 . C53 . H531 . 120.8 no C33 . C53 . H531 . 120.0 no C30 . C57 . C38 . 118.6(8) yes C30 . C57 . H571 . 120.7 no C38 . C57 . H571 . 120.7 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C44 . H441 . N2 3_656 173.6(2) 0.939 2.476 3.411(11) yes C45 . H451 . N2 3_656 175.8(2) 0.934 2.598 3.530(11) yes C48 . H481 . N1 . 154.7(3) 0.935 2.595 3.464(11) yes data_C19H11CoN7PtS4 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_moiety ? _chemical_formula_sum 'C19 H11 Co N7 Pt S4' _chemical_formula_weight 719.61 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' #------------------------------------------------ _cell_length_a 9.3569(17) _cell_length_b 14.609(3) _cell_length_c 16.563(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2264.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 7.296 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3701 _exptl_absorpt_correction_T_max 0.8678 _exptl_absorpt_process_details ? #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12257 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0732 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.87 _reflns_number_total 5134 _reflns_number_gt 4331 _reflns_threshold_expression >2sigma(I) _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.984 #========================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.032(9) _refine_ls_number_reflns 5134 _refine_ls_number_parameters 289 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.0890 _refine_ls_wR_factor_gt 0.0853 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 3.367 _refine_diff_density_min -1.757 _refine_diff_density_rms 0.217 #========================================================== # 9. General computing _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N3 N 0.7390(8) 0.8676(5) 0.6230(5) 0.0268(18) Uani 1 1 d . . . N4 N 0.3176(9) 1.0339(6) 0.2772(5) 0.025(2) Uani 1 1 d . . . C4 C 0.3929(9) 0.9962(6) 0.3204(6) 0.0191(19) Uani 1 1 d . . . Pt1 Pt 0.38903(3) 0.902234(19) 0.49897(3) 0.01957(9) Uani 1 1 d . . . Co1 Co -0.15805(13) 0.96914(8) 0.68407(7) 0.0202(3) Uani 1 1 d . . . S2 S 0.3120(3) 0.86594(17) 0.62868(15) 0.0260(5) Uani 1 1 d . . . S4 S 0.5079(2) 0.94204(18) 0.38119(15) 0.0266(5) Uani 1 1 d . . . C7 C -0.3659(10) 1.2528(7) 0.5786(6) 0.032(2) Uani 1 1 d . . . H7 H -0.4003 1.3079 0.5584 0.038 Uiso 1 1 calc R . . C8 C -0.2590(10) 1.2531(6) 0.6354(6) 0.028(2) Uani 1 1 d . . . H8 H -0.2195 1.3080 0.6532 0.034 Uiso 1 1 calc R . . C6 C -0.4225(10) 1.1715(7) 0.5513(6) 0.026(2) Uani 1 1 d . . . H6 H -0.4964 1.1707 0.5137 0.031 Uiso 1 1 calc R . . N5 N -0.2616(8) 1.0889(5) 0.6380(5) 0.0229(17) Uani 1 1 d . . . C9 C -0.2103(9) 1.1687(7) 0.6664(5) 0.023(2) Uani 1 1 d . . . N7 N -0.0130(8) 0.8994(6) 0.7610(5) 0.0257(18) Uani 1 1 d . . . C5 C -0.3652(9) 1.0902(7) 0.5820(6) 0.029(2) Uani 1 1 d . . . H5 H -0.4004 1.0348 0.5628 0.035 Uiso 1 1 calc R . . C16 C 0.1552(11) 0.9154(7) 0.8682(7) 0.035(3) Uani 1 1 d . . . H16 H 0.2043 0.9528 0.9042 0.041 Uiso 1 1 calc R . . N1 N -0.0084(8) 0.9819(5) 0.5883(5) 0.0268(18) Uani 1 1 d . . . C10 C -0.0968(10) 1.1610(7) 0.7295(6) 0.028(2) Uani 1 1 d . . . C12 C 0.0709(10) 1.2122(7) 0.8262(6) 0.029(2) Uani 1 1 d . . . H12 H 0.1185 1.2598 0.8522 0.035 Uiso 1 1 calc R . . C14 C 0.0345(9) 1.0536(7) 0.8028(6) 0.025(2) Uani 1 1 d . . . C11 C -0.0319(10) 1.2330(7) 0.7695(6) 0.026(2) Uani 1 1 d . . . H11 H -0.0568 1.2933 0.7585 0.032 Uiso 1 1 calc R . . C18 C 0.0998(10) 0.7668(8) 0.8183(7) 0.038(3) Uani 1 1 d . . . H18 H 0.1103 0.7035 0.8198 0.045 Uiso 1 1 calc R . . C15 C 0.0622(10) 0.9531(7) 0.8127(6) 0.024(2) Uani 1 1 d . . . C17 C 0.1744(11) 0.8223(8) 0.8697(7) 0.040(3) Uani 1 1 d . . . H17 H 0.2388 0.7968 0.9061 0.048 Uiso 1 1 calc R . . N6 N -0.0603(9) 1.0737(5) 0.7457(5) 0.0204(17) Uani 1 1 d . . . C13 C 0.1047(10) 1.1242(8) 0.8455(6) 0.032(2) Uani 1 1 d . . . H13 H 0.1717 1.1111 0.8853 0.038 Uiso 1 1 calc R . . C2 C 0.3289(9) 0.9698(7) 0.6702(5) 0.021(2) Uani 1 1 d . . . N2 N 0.3430(11) 1.0412(7) 0.7014(5) 0.031(2) Uani 1 1 d . . . S1 S 0.2121(2) 1.00850(17) 0.47369(13) 0.0248(5) Uani 1 1 d . . . C1 C 0.0823(10) 0.9907(7) 0.5433(6) 0.027(2) Uani 1 1 d . . . C19 C 0.0075(11) 0.8085(7) 0.7635(6) 0.033(2) Uani 1 1 d . . . H19 H -0.0419 0.7718 0.7271 0.039 Uiso 1 1 calc R . . S3 S 0.5601(2) 0.78521(16) 0.5081(2) 0.0307(6) Uani 1 1 d . . . C3 C 0.6641(10) 0.8341(6) 0.5770(6) 0.023(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N3 0.023(4) 0.028(4) 0.029(4) -0.001(4) -0.004(4) 0.006(3) N4 0.019(4) 0.031(5) 0.024(5) 0.001(4) -0.001(4) -0.001(4) C4 0.012(4) 0.017(5) 0.029(5) -0.003(4) 0.000(4) -0.007(4) Pt1 0.02061(13) 0.01844(15) 0.01967(14) -0.0028(2) -0.0049(2) 0.00341(13) Co1 0.0194(6) 0.0209(7) 0.0203(6) -0.0037(5) -0.0011(5) 0.0003(5) S2 0.0320(13) 0.0215(12) 0.0245(12) 0.0022(10) -0.0032(10) 0.0003(10) S4 0.0212(11) 0.0330(14) 0.0256(12) -0.0004(11) -0.0010(10) 0.0064(10) C7 0.032(5) 0.027(6) 0.036(6) 0.007(4) 0.005(4) 0.003(4) C8 0.034(5) 0.018(5) 0.031(6) -0.003(4) 0.005(4) 0.005(4) C6 0.020(5) 0.032(6) 0.026(5) 0.008(4) -0.001(4) -0.001(4) N5 0.025(4) 0.012(4) 0.032(5) -0.003(3) 0.002(3) -0.001(3) C9 0.017(4) 0.034(6) 0.018(5) -0.001(4) 0.014(4) 0.003(4) N7 0.020(4) 0.030(5) 0.027(4) 0.000(4) 0.001(3) 0.004(4) C5 0.024(5) 0.037(6) 0.027(5) -0.004(5) -0.001(4) -0.001(4) C16 0.032(5) 0.036(7) 0.035(6) 0.002(5) -0.012(5) -0.007(5) N1 0.019(4) 0.030(5) 0.031(5) 0.000(4) 0.001(4) 0.006(3) C10 0.025(5) 0.034(6) 0.025(5) -0.006(4) 0.007(4) -0.003(5) C12 0.028(5) 0.029(6) 0.030(5) -0.010(4) 0.009(4) -0.002(4) C14 0.008(4) 0.030(6) 0.038(6) -0.003(5) 0.010(4) -0.001(4) C11 0.030(5) 0.026(6) 0.023(5) -0.009(4) 0.007(4) -0.005(4) C18 0.030(5) 0.030(6) 0.053(7) 0.009(5) -0.003(5) -0.003(5) C15 0.018(4) 0.028(6) 0.026(5) 0.003(4) -0.001(4) -0.002(4) C17 0.024(5) 0.044(8) 0.051(7) 0.011(6) -0.016(5) -0.004(5) N6 0.021(4) 0.017(4) 0.024(4) -0.005(3) -0.001(3) -0.002(3) C13 0.021(5) 0.047(7) 0.028(5) -0.017(5) -0.005(4) 0.000(5) C2 0.014(4) 0.033(6) 0.016(5) 0.001(4) -0.010(4) 0.005(4) N2 0.040(5) 0.034(6) 0.018(5) 0.003(4) -0.001(4) 0.002(5) S1 0.0241(11) 0.0302(14) 0.0202(12) 0.0040(9) 0.0020(8) 0.0076(10) C1 0.030(6) 0.027(6) 0.024(5) -0.007(4) -0.012(4) 0.006(4) C19 0.028(6) 0.038(7) 0.032(6) -0.003(5) -0.001(5) 0.000(5) S3 0.0336(10) 0.0274(12) 0.0311(15) -0.0100(14) -0.0138(13) 0.0100(9) C3 0.028(5) 0.007(5) 0.034(5) -0.002(4) -0.002(4) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N3 C3 1.145(11) . ? N3 Co1 2.037(8) 1_655 ? N4 C4 1.145(12) . ? N4 Co1 2.147(8) 2_574 ? C4 S4 1.672(10) . ? Pt1 S1 2.308(2) . ? Pt1 S4 2.320(3) . ? Pt1 S2 2.327(3) . ? Pt1 S3 2.347(2) . ? Co1 N3 2.037(8) 1_455 ? Co1 N6 2.052(8) . ? Co1 N7 2.122(8) . ? Co1 N1 2.124(8) . ? Co1 N5 2.141(7) . ? Co1 N4 2.147(8) 2_575 ? S2 C2 1.674(11) . ? C7 C8 1.373(14) . ? C7 C6 1.377(14) . ? C7 H7 0.9300 . ? C8 C9 1.412(13) . ? C8 H8 0.9300 . ? C6 C5 1.399(13) . ? C6 H6 0.9300 . ? N5 C5 1.342(12) . ? N5 C9 1.345(12) . ? C9 C10 1.494(13) . ? N7 C19 1.343(13) . ? N7 C15 1.358(12) . ? C5 H5 0.9300 . ? C16 C17 1.372(14) . ? C16 C15 1.380(14) . ? C16 H16 0.9300 . ? N1 C1 1.137(12) . ? C10 N6 1.348(13) . ? C10 C11 1.384(13) . ? C12 C13 1.362(14) . ? C12 C11 1.378(14) . ? C12 H12 0.9300 . ? C14 N6 1.329(12) . ? C14 C13 1.413(13) . ? C14 C15 1.500(14) . ? C11 H11 0.9300 . ? C18 C17 1.369(15) . ? C18 C19 1.393(14) . ? C18 H18 0.9300 . ? C17 H17 0.9300 . ? C13 H13 0.9300 . ? C2 N2 1.171(13) . ? S1 C1 1.695(11) . ? C19 H19 0.9300 . ? S3 C3 1.661(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 N3 Co1 158.6(8) . 1_655 ? C4 N4 Co1 150.1(8) . 2_574 ? N4 C4 S4 177.8(9) . . ? S1 Pt1 S4 91.30(8) . . ? S1 Pt1 S2 95.66(8) . . ? S4 Pt1 S2 169.11(8) . . ? S1 Pt1 S3 172.29(9) . . ? S4 Pt1 S3 84.81(10) . . ? S2 Pt1 S3 89.20(10) . . ? N3 Co1 N6 178.2(3) 1_455 . ? N3 Co1 N7 104.5(3) 1_455 . ? N6 Co1 N7 76.9(3) . . ? N3 Co1 N1 90.3(3) 1_455 . ? N6 Co1 N1 90.7(3) . . ? N7 Co1 N1 93.9(3) . . ? N3 Co1 N5 101.8(3) 1_455 . ? N6 Co1 N5 76.8(3) . . ? N7 Co1 N5 153.6(3) . . ? N1 Co1 N5 87.7(3) . . ? N3 Co1 N4 90.7(3) 1_455 2_575 ? N6 Co1 N4 88.2(3) . 2_575 ? N7 Co1 N4 90.2(3) . 2_575 ? N1 Co1 N4 175.3(3) . 2_575 ? N5 Co1 N4 87.6(3) . 2_575 ? C2 S2 Pt1 98.3(3) . . ? C4 S4 Pt1 108.4(3) . . ? C8 C7 C6 120.6(9) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 118.7(9) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C7 C6 C5 117.7(9) . . ? C7 C6 H6 121.1 . . ? C5 C6 H6 121.1 . . ? C5 N5 C9 119.2(8) . . ? C5 N5 Co1 125.8(6) . . ? C9 N5 Co1 115.0(6) . . ? N5 C9 C8 121.0(9) . . ? N5 C9 C10 115.7(8) . . ? C8 C9 C10 123.3(9) . . ? C19 N7 C15 118.5(9) . . ? C19 N7 Co1 125.8(7) . . ? C15 N7 Co1 115.7(7) . . ? N5 C5 C6 122.7(9) . . ? N5 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C17 C16 C15 119.3(9) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C1 N1 Co1 172.7(8) . . ? N6 C10 C11 120.8(9) . . ? N6 C10 C9 113.0(8) . . ? C11 C10 C9 126.2(10) . . ? C13 C12 C11 121.9(9) . . ? C13 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? N6 C14 C13 120.3(9) . . ? N6 C14 C15 114.2(8) . . ? C13 C14 C15 125.5(9) . . ? C12 C11 C10 117.8(10) . . ? C12 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? C17 C18 C19 117.5(10) . . ? C17 C18 H18 121.2 . . ? C19 C18 H18 121.2 . . ? N7 C15 C16 121.2(9) . . ? N7 C15 C14 114.0(8) . . ? C16 C15 C14 124.9(9) . . ? C18 C17 C16 120.6(10) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C14 N6 C10 121.4(8) . . ? C14 N6 Co1 119.1(6) . . ? C10 N6 Co1 119.5(6) . . ? C12 C13 C14 117.7(10) . . ? C12 C13 H13 121.2 . . ? C14 C13 H13 121.2 . . ? N2 C2 S2 177.8(9) . . ? C1 S1 Pt1 106.7(3) . . ? N1 C1 S1 176.9(9) . . ? N7 C19 C18 122.8(10) . . ? N7 C19 H19 118.6 . . ? C18 C19 H19 118.6 . . ? C3 S3 Pt1 97.5(3) . . ? N3 C3 S3 178.0(9) . . ? data_C10H16CuN6PtS4 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C10 H16 Cu1 N6 Pt1 S4' _chemical_formula_moiety 'C10 H16 Cu1 N6 Pt1 S4' _chemical_compound_source ? _chemical_formula_weight 607.18 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 21 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,y+1/2,-z' #------------------------------------------------ _cell_length_a 8.1693(17) _cell_length_b 10.479(2) _cell_length_c 10.576(2) _cell_angle_alpha 90 _cell_angle_beta 91.237(2) _cell_angle_gamma 90 _cell_volume 905.1(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3492 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.96 _cell_measurement_temperature 100 _exptl_crystal_description 'plate' _exptl_crystal_colour 'green' _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.11 _exptl_crystal_density_diffrn 2.228 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 578 _exptl_absorpt_coefficient_mu 9.358 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device 'Unknown' _diffrn_measurement_device_type 'Serial' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 5181 _reflns_number_total 3181 _diffrn_reflns_av_R_equivalents 0.024 # Number of reflections with Friedels Law is 2207 # Number of reflections without Friedels Law is 3181 # Theoretical number of reflections is about 2177 _diffrn_reflns_theta_min 1.926 _diffrn_reflns_theta_max 27.960 _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.723 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min -13 _reflns_limit_k_max 10 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #========================================================================== # 8. REFINEMENT DATA _refine_diff_density_min -1.11 _refine_diff_density_max 1.40 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 2927 _refine_ls_number_restraints 527 _refine_ls_number_parameters 254 _oxford_refine_ls_R_factor_ref 0.0267 _refine_ls_wR_factor_ref 0.0301 _refine_ls_goodness_of_fit_ref 0.9699 _refine_ls_shift/su_max 2.025573 # The values computed from all data _oxford_reflns_number_all 3181 _refine_ls_R_factor_all 0.0303 _refine_ls_wR_factor_all 0.0311 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2973 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_gt 0.0302 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration 'unk' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.01P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Pt1 Pt -0.04906(3) 0.84299(13) 0.27534(2) 0.0148 1.0000 Uani . . . . . . . Cu1 Cu 0.51606(11) 0.76793(15) 0.70275(8) 0.0156 1.0000 Uani . . . . . . . S1 S 0.23275(19) 0.8490(3) 0.28877(15) 0.0208 1.0000 Uani . . . . . . . S2 S -0.0553(2) 0.6720(2) 0.41586(19) 0.0246 1.0000 Uani . . . . . . . S3 S -0.33165(19) 0.8367(3) 0.24684(15) 0.0214 1.0000 Uani . . . . . . . S4 S -0.0455(3) 0.9898(2) 0.11143(19) 0.0283 1.0000 Uani . . . . . . . N1 N 0.3363(7) 0.8252(7) 0.5438(5) 0.0232 1.0000 Uani . . . . . . . N2 N -0.3204(9) 0.7118(6) 0.5769(7) 0.0213 1.0000 Uani . . . . . . . N3 N -0.4262(7) 1.0939(5) 0.2801(6) 0.0198 1.0000 Uani . . . . . . . N4 N 0.2347(10) 1.1501(7) 0.1248(7) 0.0382 1.0000 Uani . . . . . . . N5 N 0.6270(7) 0.9427(4) 0.7071(4) 0.0233 1.0000 Uani D . . . . . . N6 N 0.3772(6) 0.8271(4) 0.8505(5) 0.0274 1.0000 Uani D . . . . . . C1 C 0.2874(7) 0.8367(9) 0.4430(5) 0.0183 1.0000 Uani . . . . . . . C2 C -0.2134(9) 0.6963(6) 0.5108(7) 0.0187 1.0000 Uani . . . . . . . C3 C -0.3847(9) 0.9885(6) 0.2669(6) 0.0173 1.0000 Uani . . . . . . . C4 C 0.1217(11) 1.0829(7) 0.1245(7) 0.0278 1.0000 Uani . . . . . . . C51 C 0.5212(11) 1.0259(7) 0.7897(7) 0.0343 0.7360(14) Uani D . P . 1 . . C52 C 0.5659(17) 1.0017(17) 0.8285(12) 0.0376 0.2640(14) Uani D . P . 2 . . C61 C 0.4409(11) 0.9591(7) 0.8870(7) 0.0345 0.7360(14) Uani D . P . 1 . . C62 C 0.3969(19) 0.9721(10) 0.831(2) 0.0371 0.2640(14) Uani D . P . 2 . . C71 C 0.6465(13) 0.9988(7) 0.5843(7) 0.0145 0.7360(14) Uani D . P . 1 . . C72 C 0.618(3) 1.0320(15) 0.6047(14) 0.0206 0.2640(14) Uani D . P . 2 . . C81 C 0.7773(11) 0.9473(11) 0.7845(10) 0.0322 0.7360(14) Uani D . P . 1 . . C82 C 0.8010(13) 0.927(2) 0.7463(15) 0.0088 0.2640(14) Uani D . P . 2 . . C91 C 0.2011(9) 0.8492(9) 0.8150(10) 0.0230 0.7360(14) Uani D . P . 1 . . C92 C 0.2022(15) 0.8011(15) 0.811(3) 0.0237 0.2640(14) Uani D . P . 2 . . C101 C 0.3863(13) 0.7367(7) 0.9571(7) 0.0235 0.7360(14) Uani D . P . 1 . . C102 C 0.404(3) 0.7898(18) 0.9812(11) 0.0331 0.2640(14) Uani D . P . 2 . . H511 H 0.5919 1.0860 0.8302 0.0542 0.7360(14) Uiso R . P . 1 . . H512 H 0.4427 1.0698 0.7384 0.0542 0.7360(14) Uiso R . P . 1 . . H521 H 0.5792 1.0918 0.8264 0.0542 0.2640(14) Uiso R . P . 2 . . H522 H 0.6243 0.9679 0.8996 0.0542 0.2640(14) Uiso R . P . 2 . . H611 H 0.5141 0.9491 0.9573 0.0432 0.7360(14) Uiso R . P . 1 . . H612 H 0.3493 1.0084 0.9114 0.0432 0.7360(14) Uiso R . P . 1 . . H621 H 0.3443 1.0177 0.8965 0.0432 0.2640(14) Uiso R . P . 2 . . H622 H 0.3488 0.9947 0.7517 0.0432 0.2640(14) Uiso R . P . 2 . . H711 H 0.7101 0.9435 0.5338 0.0266 0.7360(14) Uiso R . P . 1 . . H712 H 0.7009 1.0784 0.5937 0.0266 0.7360(14) Uiso R . P . 1 . . H713 H 0.5423 1.0117 0.5447 0.0266 0.7360(14) Uiso R . P . 1 . . H721 H 0.6511 0.9909 0.5294 0.0266 0.2640(14) Uiso R . P . 2 . . H722 H 0.6812 1.1073 0.6175 0.0266 0.2640(14) Uiso R . P . 2 . . H723 H 0.5055 1.0538 0.5976 0.0266 0.2640(14) Uiso R . P . 2 . . H811 H 0.8575 0.8969 0.7441 0.0250 0.7360(14) Uiso R . P . 1 . . H812 H 0.8147 1.0329 0.7908 0.0250 0.7360(14) Uiso R . P . 1 . . H813 H 0.7591 0.9145 0.8667 0.0250 0.7360(14) Uiso R . P . 1 . . H821 H 0.8540 0.8868 0.6776 0.0250 0.2640(14) Uiso R . P . 2 . . H822 H 0.8518 1.0062 0.7642 0.0250 0.2640(14) Uiso R . P . 2 . . H823 H 0.8093 0.8732 0.8188 0.0250 0.2640(14) Uiso R . P . 2 . . H911 H 0.1523 0.7705 0.7906 0.0380 0.7360(14) Uiso R . P . 1 . . H912 H 0.1452 0.8834 0.8852 0.0380 0.7360(14) Uiso R . P . 1 . . H913 H 0.1942 0.9076 0.7463 0.0380 0.7360(14) Uiso R . P . 1 . . H921 H 0.1757 0.7134 0.8216 0.0380 0.2640(14) Uiso R . P . 2 . . H922 H 0.1307 0.8516 0.8603 0.0380 0.2640(14) Uiso R . P . 2 . . H923 H 0.1902 0.8238 0.7248 0.0380 0.2640(14) Uiso R . P . 2 . . H1011 H 0.3460 0.6559 0.9302 0.0259 0.7360(14) Uiso R . P . 1 . . H1012 H 0.3231 0.7668 1.0253 0.0259 0.7360(14) Uiso R . P . 1 . . H1013 H 0.4975 0.7287 0.9841 0.0259 0.7360(14) Uiso R . P . 1 . . H1021 H 0.3872 0.7006 0.9901 0.0259 0.2640(14) Uiso R . P . 2 . . H1022 H 0.5089 0.8118 1.0152 0.0259 0.2640(14) Uiso R . P . 2 . . H1023 H 0.3220 0.8347 1.0255 0.0259 0.2640(14) Uiso R . P . 2 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01265(11) 0.01520(9) 0.01659(11) -0.00096(13) 0.00173(8) 0.00124(14) Cu1 0.0181(5) 0.0130(4) 0.0158(4) -0.0020(3) 0.0046(3) -0.0008(3) S1 0.0134(7) 0.0305(9) 0.0185(7) 0.0071(10) 0.0014(6) 0.0018(11) S2 0.0192(10) 0.0219(8) 0.0330(11) 0.0079(7) 0.0113(8) 0.0062(7) S3 0.0145(7) 0.0163(6) 0.0332(8) -0.0037(12) -0.0017(6) 0.0012(12) S4 0.0227(11) 0.0330(9) 0.0294(11) 0.0088(8) 0.0019(8) 0.0024(8) N1 0.026(3) 0.019(3) 0.024(3) -0.004(3) -0.001(2) 0.002(3) N2 0.023(3) 0.018(3) 0.024(3) 0.000(2) 0.012(3) 0.000(3) N3 0.012(3) 0.025(3) 0.022(3) 0.000(2) 0.001(2) 0.002(2) N4 0.036(4) 0.036(3) 0.043(4) 0.006(3) 0.014(3) -0.001(3) N5 0.035(3) 0.012(2) 0.023(3) -0.0009(19) 0.008(2) -0.003(2) N6 0.028(2) 0.019(2) 0.036(2) -0.012(2) 0.013(2) -0.004(3) C1 0.018(3) 0.017(2) 0.020(3) 0.001(4) -0.001(2) 0.006(4) C2 0.018(3) 0.012(3) 0.026(4) 0.004(2) 0.000(3) -0.001(3) C3 0.019(3) 0.021(3) 0.012(3) 0.000(2) 0.004(3) 0.000(3) C4 0.040(4) 0.024(3) 0.020(4) 0.004(3) 0.011(3) 0.012(3) C51 0.049(4) 0.016(3) 0.038(4) -0.002(3) 0.017(4) 0.005(4) C52 0.045(5) 0.030(5) 0.037(6) -0.003(5) 0.007(5) 0.005(5) C61 0.045(4) 0.028(4) 0.031(4) -0.018(3) 0.019(4) -0.007(4) C62 0.041(5) 0.033(5) 0.038(6) -0.013(5) 0.008(5) 0.004(5) C71 0.030(4) -0.006(3) 0.021(4) -0.006(3) 0.003(4) 0.000(3) C72 0.034(5) 0.009(6) 0.019(6) -0.006(6) 0.006(6) 0.008(6) C81 0.042(4) 0.028(4) 0.026(5) -0.002(4) -0.002(4) -0.003(4) C82 0.029(5) -0.002(5) 0.000(6) -0.007(5) 0.001(6) -0.004(5) C91 0.029(4) 0.005(3) 0.036(4) 0.001(4) 0.014(3) 0.001(4) C92 0.026(5) 0.008(6) 0.038(6) -0.012(6) 0.017(6) 0.001(6) C101 0.023(4) 0.030(4) 0.018(4) -0.011(3) 0.005(4) -0.008(4) C102 0.030(5) 0.035(6) 0.035(6) -0.014(6) 0.015(6) -0.008(6) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.4381(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . S1 . 2.3044(17) yes Pt1 . S2 . 2.3293(18) yes Pt1 . S3 . 2.3226(16) yes Pt1 . S4 . 2.3183(19) yes Cu1 . N2 1_655 1.994(7) yes Cu1 . N3 2_546 1.976(6) yes Cu1 . N1 . 2.288(6) yes Cu1 . N5 . 2.044(5) yes Cu1 . N6 . 2.047(5) yes S1 . C1 . 1.687(6) yes S2 . C2 . 1.673(8) yes S3 . C3 . 1.663(7) yes S4 . C4 . 1.682(9) yes N1 . C1 . 1.137(7) yes N2 . C2 . 1.143(9) yes N3 . C3 . 1.165(8) yes N4 . C4 . 1.160(11) yes N5 . C51 . 1.517(7) yes N5 . C71 . 1.437(7) yes N5 . C81 . 1.461(8) yes N6 . C61 . 1.524(7) yes N6 . C91 . 1.497(7) yes N6 . C101 . 1.473(7) yes C51 . C61 . 1.418(7) yes C51 . H511 . 0.950 no C51 . H512 . 0.950 no C52 . C62 . 1.415(9) yes C52 . H521 . 0.950 no C52 . H522 . 0.950 no C61 . H611 . 0.950 no C61 . H612 . 0.950 no C62 . H621 . 0.950 no C62 . H622 . 0.950 no C71 . H711 . 0.950 no C71 . H712 . 0.950 no C71 . H713 . 0.950 no C72 . H721 . 0.950 no C72 . H722 . 0.950 no C72 . H723 . 0.950 no C81 . H811 . 0.950 no C81 . H812 . 0.950 no C81 . H813 . 0.950 no C82 . H821 . 0.950 no C82 . H822 . 0.950 no C82 . H823 . 0.950 no C91 . H911 . 0.950 no C91 . H912 . 0.950 no C91 . H913 . 0.950 no C92 . H921 . 0.950 no C92 . H922 . 0.950 no C92 . H923 . 0.950 no C101 . H1011 . 0.950 no C101 . H1012 . 0.950 no C101 . H1013 . 0.950 no C102 . H1021 . 0.950 no C102 . H1022 . 0.950 no C102 . H1023 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 . Pt1 . S2 . 90.99(8) yes S1 . Pt1 . S3 . 176.08(6) yes S2 . Pt1 . S3 . 91.47(8) yes S1 . Pt1 . S4 . 89.96(8) yes S2 . Pt1 . S4 . 171.25(7) yes S3 . Pt1 . S4 . 87.14(8) yes N2 1_655 Cu1 . N3 2_546 92.6(3) yes N2 1_655 Cu1 . N1 . 90.9(3) yes N3 2_546 Cu1 . N1 . 94.3(2) yes N2 1_655 Cu1 . N5 . 88.6(2) yes N3 2_546 Cu1 . N5 . 172.2(2) yes N1 . Cu1 . N5 . 93.4(2) yes N2 1_655 Cu1 . N6 . 171.5(3) yes N3 2_546 Cu1 . N6 . 89.8(2) yes N1 . Cu1 . N6 . 97.1(2) yes N5 . Cu1 . N6 . 87.9(2) yes Pt1 . S1 . C1 . 107.5(2) yes Pt1 . S2 . C2 . 107.1(2) yes Pt1 . S3 . C3 . 102.6(3) yes Pt1 . S4 . C4 . 110.3(3) yes Cu1 . N1 . C1 . 157.5(6) yes Cu1 1_455 N2 . C2 . 169.2(6) yes Cu1 2_556 N3 . C3 . 174.9(6) yes Cu1 . N5 . C51 . 105.7(5) yes Cu1 . N5 . C71 . 113.8(5) yes C51 . N5 . C71 . 111.153(18) yes Cu1 . N5 . C81 . 114.1(5) yes C51 . N5 . C81 . 98.091(19) yes C71 . N5 . C81 . 112.6(8) yes Cu1 . N6 . C61 . 106.1(4) yes Cu1 . N6 . C91 . 113.6(5) yes C61 . N6 . C91 . 104.12(2) yes Cu1 . N6 . C101 . 111.7(5) yes C61 . N6 . C101 . 112.240(12) yes C91 . N6 . C101 . 108.9(7) yes S1 . C1 . N1 . 174.5(6) yes S2 . C2 . N2 . 179.0(6) yes S3 . C3 . N3 . 178.1(7) yes S4 . C4 . N4 . 175.1(7) yes N5 . C51 . C61 . 114.4(6) yes N5 . C51 . H511 . 107.0 no C61 . C51 . H511 . 106.6 no N5 . C51 . H512 . 109.6 no C61 . C51 . H512 . 109.6 no H511 . C51 . H512 . 109.5 no N5 . C52 . C62 . 105.4(13) yes N5 . C52 . H521 . 110.1 no C62 . C52 . H521 . 109.3 no N5 . C52 . H522 . 110.3 no C62 . C52 . H522 . 112.1 no H521 . C52 . H522 . 109.5 no N6 . C61 . C51 . 115.2(6) yes N6 . C61 . H611 . 107.7 no C51 . C61 . H611 . 109.2 no N6 . C61 . H612 . 107.2 no C51 . C61 . H612 . 108.0 no H611 . C61 . H612 . 109.5 no N6 . C62 . C52 . 108.9(12) yes N6 . C62 . H621 . 110.4 no C52 . C62 . H621 . 111.2 no N6 . C62 . H622 . 108.7 no C52 . C62 . H622 . 108.2 no H621 . C62 . H622 . 109.5 no N5 . C71 . H711 . 109.4 no N5 . C71 . H712 . 109.0 no H711 . C71 . H712 . 109.5 no N5 . C71 . H713 . 110.0 no H711 . C71 . H713 . 109.5 no H712 . C71 . H713 . 109.5 no N5 . C72 . H721 . 109.1 no N5 . C72 . H722 . 114.6 no H721 . C72 . H722 . 109.5 no N5 . C72 . H723 . 104.5 no H721 . C72 . H723 . 109.5 no H722 . C72 . H723 . 109.5 no N5 . C81 . H811 . 108.0 no N5 . C81 . H812 . 109.6 no H811 . C81 . H812 . 109.5 no N5 . C81 . H813 . 110.8 no H811 . C81 . H813 . 109.5 no H812 . C81 . H813 . 109.5 no N5 . C82 . H821 . 106.6 no N5 . C82 . H822 . 111.5 no H821 . C82 . H822 . 109.5 no N5 . C82 . H823 . 110.2 no H821 . C82 . H823 . 109.5 no H822 . C82 . H823 . 109.5 no N6 . C91 . H911 . 109.3 no N6 . C91 . H912 . 109.7 no H911 . C91 . H912 . 109.5 no N6 . C91 . H913 . 109.4 no H911 . C91 . H913 . 109.5 no H912 . C91 . H913 . 109.5 no N6 . C92 . H921 . 111.2 no N6 . C92 . H922 . 109.9 no H921 . C92 . H922 . 109.5 no N6 . C92 . H923 . 107.3 no H921 . C92 . H923 . 109.5 no H922 . C92 . H923 . 109.5 no N6 . C101 . H1011 . 109.4 no N6 . C101 . H1012 . 110.4 no H1011 . C101 . H1012 . 109.5 no N6 . C101 . H1013 . 108.6 no H1011 . C101 . H1013 . 109.5 no H1012 . C101 . H1013 . 109.5 no N6 . C102 . H1021 . 109.9 no N6 . C102 . H1022 . 114.3 no H1021 . C102 . H1022 . 109.5 no N6 . C102 . H1023 . 104.0 no H1021 . C102 . H1023 . 109.5 no H1022 . C102 . H1023 . 109.5 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C72 . H713 . N1 . 128 0.90 2.58 3.217(16) yes C72 . H722 . C1 2_656 145 0.95 2.50 3.326(16) yes C81 . H823 . N4 2_646 153 0.89 2.44 3.261(16) yes C82 . H823 . N4 2_646 139 0.95 2.44 3.217(16) yes C91 . H923 . N1 . 140 0.99 2.28 3.106(16) yes C92 . H923 . N1 . 140 0.95 2.28 3.067(16) yes data_C28H16N8PbPtS4 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_moiety ? _chemical_formula_sum 'C28 H16 N8 Pb Pt S4' _chemical_formula_weight 995.01 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' #------------------------------------------------ _cell_length_a 16.106(7) _cell_length_b 15.435(7) _cell_length_c 13.475(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.184(6) _cell_angle_gamma 90.00 _cell_volume 3217(2) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.054 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 9.862 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2202 _exptl_absorpt_correction_T_max 0.6938 _exptl_absorpt_process_details ? #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8240 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.70 _reflns_number_total 3576 _reflns_number_gt 2766 _reflns_threshold_expression >2sigma(I) _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 27.70 _diffrn_measured_fraction_theta_full 0.948 #========================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3576 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.354 _refine_diff_density_min -3.932 _refine_diff_density_rms 0.257 #========================================================== # 9. General computing _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.5000 0.10909(3) 0.2500 0.01282(12) Uani 1 2 d S . . Pt1 Pt 0.2500 0.2500 0.5000 0.01422(13) Uani 1 2 d S . . S2 S 0.22577(14) 0.13833(15) 0.37942(16) 0.0220(5) Uani 1 1 d . . . S1 S 0.38947(14) 0.20930(16) 0.59045(16) 0.0236(5) Uani 1 1 d . . . N4 N 0.4272(4) 0.1693(5) 0.0682(5) 0.0158(15) Uani 1 1 d . . . C8 C 0.2941(6) 0.4049(6) 0.0379(6) 0.028(2) Uani 1 1 d . . . H8 H 0.2656 0.4578 0.0317 0.034 Uiso 1 1 calc R . . C13 C 0.3950(5) 0.1585(6) -0.1170(6) 0.0209(19) Uani 1 1 d . . . H13 H 0.3988 0.1266 -0.1741 0.025 Uiso 1 1 calc R . . N3 N 0.4062(4) 0.2479(4) 0.2409(5) 0.0134(14) Uani 1 1 d . . . C10 C 0.3836(5) 0.2449(5) 0.0553(6) 0.0140(17) Uani 1 1 d . . . C7 C 0.3737(5) 0.2886(6) 0.1479(6) 0.0157(18) Uani 1 1 d . . . C12 C 0.3540(6) 0.2363(6) -0.1297(6) 0.0192(19) Uani 1 1 d . . . H12 H 0.3314 0.2588 -0.1958 0.023 Uiso 1 1 calc R . . C4 C 0.3525(6) 0.3660(6) 0.3219(7) 0.026(2) Uani 1 1 d . . . H4 H 0.3460 0.3902 0.3825 0.032 Uiso 1 1 calc R . . C3 C 0.3956(5) 0.2866(6) 0.3243(6) 0.0173(18) Uani 1 1 d . . . H3 H 0.4180 0.2597 0.3879 0.021 Uiso 1 1 calc R . . C9 C 0.3014(6) 0.3632(6) -0.0488(6) 0.023(2) Uani 1 1 d . . . H9 H 0.2768 0.3878 -0.1132 0.027 Uiso 1 1 calc R . . C6 C 0.3296(6) 0.3683(6) 0.1372(6) 0.0193(19) Uani 1 1 d . . . C11 C 0.3455(5) 0.2833(6) -0.0424(6) 0.0200(18) Uani 1 1 d . . . C14 C 0.4318(5) 0.1268(6) -0.0162(6) 0.0184(18) Uani 1 1 d . . . H14 H 0.4605 0.0739 -0.0083 0.022 Uiso 1 1 calc R . . C5 C 0.3201(6) 0.4078(6) 0.2286(7) 0.027(2) Uani 1 1 d . . . H5 H 0.2925 0.4611 0.2256 0.032 Uiso 1 1 calc R . . C2 C 0.3224(6) 0.0979(6) 0.3751(6) 0.0191(19) Uani 1 1 d . . . N2 N 0.3847(5) 0.0666(5) 0.3654(5) 0.0220(17) Uani 1 1 d . . . C1 C 0.3814(6) 0.1030(7) 0.6167(6) 0.026(2) Uani 1 1 d . . . N1 N 0.3802(6) 0.0295(6) 0.6372(6) 0.040(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0139(2) 0.0167(2) 0.0079(2) 0.000 0.00327(16) 0.000 Pt1 0.0160(2) 0.0185(3) 0.0091(2) 0.00184(16) 0.00499(18) 0.00237(18) S2 0.0198(11) 0.0248(12) 0.0188(11) -0.0052(9) 0.0011(9) 0.0020(10) S1 0.0177(11) 0.0330(14) 0.0179(11) -0.0029(10) 0.0014(9) 0.0050(10) N4 0.014(3) 0.024(4) 0.011(3) 0.000(3) 0.006(3) -0.001(3) C8 0.030(5) 0.030(6) 0.018(5) -0.003(4) -0.003(4) 0.004(4) C13 0.019(4) 0.028(5) 0.014(4) -0.006(4) 0.002(4) -0.002(4) N3 0.011(3) 0.021(4) 0.008(3) -0.002(3) 0.004(3) -0.001(3) C10 0.015(4) 0.021(5) 0.006(4) 0.001(3) 0.002(3) 0.000(3) C7 0.011(4) 0.021(5) 0.015(4) -0.002(3) 0.003(3) -0.007(4) C12 0.022(4) 0.030(5) 0.003(4) 0.002(3) -0.001(3) -0.003(4) C4 0.031(5) 0.028(6) 0.024(5) -0.006(4) 0.014(4) 0.001(4) C3 0.014(4) 0.025(5) 0.012(4) -0.001(3) 0.003(3) 0.000(4) C9 0.028(5) 0.024(5) 0.014(4) 0.010(4) 0.000(4) 0.003(4) C6 0.022(4) 0.018(5) 0.018(4) 0.005(3) 0.006(4) 0.002(4) C11 0.020(4) 0.026(5) 0.015(4) 0.004(4) 0.006(4) -0.001(4) C14 0.020(4) 0.020(5) 0.015(4) -0.001(3) 0.005(3) 0.003(4) C5 0.030(5) 0.022(5) 0.027(5) 0.001(4) 0.005(4) 0.003(4) C2 0.027(5) 0.021(5) 0.009(4) 0.000(3) 0.005(4) -0.007(4) N2 0.025(4) 0.028(5) 0.016(4) -0.004(3) 0.011(3) 0.001(4) C1 0.029(5) 0.038(6) 0.009(4) -0.004(4) 0.004(4) 0.014(5) N1 0.060(6) 0.035(6) 0.019(4) 0.006(4) 0.003(4) 0.020(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 N4 2.577(6) 2_655 ? Pb1 N4 2.577(6) . ? Pb1 N3 2.605(7) 2_655 ? Pb1 N3 2.605(7) . ? Pt1 S1 2.324(2) . ? Pt1 S1 2.324(2) 7_556 ? Pt1 S2 2.326(2) 7_556 ? Pt1 S2 2.326(2) . ? S2 C2 1.693(9) . ? S1 C1 1.691(11) . ? N4 C14 1.332(10) . ? N4 C10 1.349(10) . ? C8 C9 1.367(12) . ? C8 C6 1.418(12) . ? C8 H8 0.9300 . ? C13 C12 1.357(13) . ? C13 C14 1.409(11) . ? C13 H13 0.9300 . ? N3 C3 1.324(10) . ? N3 C7 1.369(10) . ? C10 C11 1.418(11) . ? C10 C7 1.465(11) . ? C7 C6 1.408(12) . ? C12 C11 1.421(11) . ? C12 H12 0.9300 . ? C4 C5 1.379(12) . ? C4 C3 1.405(12) . ? C4 H4 0.9300 . ? C3 H3 0.9300 . ? C9 C11 1.414(13) . ? C9 H9 0.9300 . ? C6 C5 1.421(12) . ? C14 H14 0.9300 . ? C5 H5 0.9300 . ? C2 N2 1.154(11) . ? C1 N1 1.169(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Pb1 N4 137.7(3) 2_655 . ? N4 Pb1 N3 63.6(2) 2_655 2_655 ? N4 Pb1 N3 81.5(2) . 2_655 ? N4 Pb1 N3 81.5(2) 2_655 . ? N4 Pb1 N3 63.6(2) . . ? N3 Pb1 N3 69.3(3) 2_655 . ? S1 Pt1 S1 180.0 . 7_556 ? S1 Pt1 S2 83.37(8) . 7_556 ? S1 Pt1 S2 96.63(8) 7_556 7_556 ? S1 Pt1 S2 96.63(8) . . ? S1 Pt1 S2 83.37(8) 7_556 . ? S2 Pt1 S2 180.0 7_556 . ? C2 S2 Pt1 108.7(3) . . ? C1 S1 Pt1 104.6(3) . . ? C14 N4 C10 117.9(7) . . ? C14 N4 Pb1 121.0(6) . . ? C10 N4 Pb1 121.1(5) . . ? C9 C8 C6 120.8(9) . . ? C9 C8 H8 119.6 . . ? C6 C8 H8 119.6 . . ? C12 C13 C14 119.2(8) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C3 N3 C7 117.6(7) . . ? C3 N3 Pb1 122.8(5) . . ? C7 N3 Pb1 119.3(5) . . ? N4 C10 C11 123.7(7) . . ? N4 C10 C7 117.7(7) . . ? C11 C10 C7 118.5(7) . . ? N3 C7 C6 123.2(7) . . ? N3 C7 C10 117.7(7) . . ? C6 C7 C10 119.1(7) . . ? C13 C12 C11 120.2(8) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C5 C4 C3 119.2(8) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N3 C3 C4 123.6(8) . . ? N3 C3 H3 118.2 . . ? C4 C3 H3 118.2 . . ? C8 C9 C11 121.3(8) . . ? C8 C9 H9 119.3 . . ? C11 C9 H9 119.3 . . ? C7 C6 C8 120.2(8) . . ? C7 C6 C5 117.4(8) . . ? C8 C6 C5 122.4(8) . . ? C9 C11 C10 120.0(7) . . ? C9 C11 C12 123.9(8) . . ? C10 C11 C12 116.1(8) . . ? N4 C14 C13 122.9(8) . . ? N4 C14 H14 118.5 . . ? C13 C14 H14 118.5 . . ? C4 C5 C6 119.0(8) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? N2 C2 S2 174.5(8) . . ? N1 C1 S1 176.7(9) . . ? data_C16H14N6PbS2 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C16 H14 N6 Pb1 S2' _chemical_formula_moiety 'C16 H14 N6 Pb1 S2' _chemical_compound_source ? _chemical_formula_weight 561.66 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' #------------------------------------------------ _cell_length_a 7.7166(2) _cell_length_b 8.8079(2) _cell_length_c 14.5476(3) _cell_angle_alpha 101.6918(10) _cell_angle_beta 93.0916(10) _cell_angle_gamma 107.2670(10) _cell_volume 917.70(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 293 _exptl_crystal_description ? _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.032 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 9.431 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device_type 'Unknown' _diffrn_measurement_device 'Serial' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 37379 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_theta_min 1.440 _diffrn_reflns_theta_max 41.225 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.560 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 #========================================================================== # 8. REFINEMENT DATA _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min -16 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _oxford_diffrn_Wilson_B_factor 2.23 _oxford_diffrn_Wilson_scale 87.24 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.38 _refine_diff_density_max 2.10 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 9456 _refine_ls_number_restraints 0 _refine_ls_number_parameters 227 _oxford_refine_ls_R_factor_ref 0.0302 _refine_ls_wR_factor_ref 0.0283 _refine_ls_goodness_of_fit_ref 1.0641 _refine_ls_shift/su_max 0.0011257 _refine_ls_shift/su_mean 0.0000249 # The values computed from all data _oxford_reflns_number_all 11997 _refine_ls_R_factor_all 0.0478 _refine_ls_wR_factor_all 0.0374 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9667 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_gt 0.0286 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration '.' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.484 0.627 0.498 0.229 0.113 ; #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pb1 Pb 0.336977(11) 0.513804(9) 0.197517(6) 0.0291 1.0000 Uani . . . . . . S1 S 0.84488(12) 0.86154(10) 0.42098(6) 0.0546 1.0000 Uani . . . . . . S2 S -0.31830(10) 0.49635(13) 0.06033(6) 0.0550 1.0000 Uani . . . . . . N1 N 0.5991(4) 0.5635(3) 0.3231(2) 0.0589 1.0000 Uani . . . . . . N2 N -0.0204(4) 0.4547(5) 0.1572(3) 0.0618 1.0000 Uani . . . . . . N3 N 0.4738(3) 0.8605(3) 0.25402(17) 0.0432 1.0000 Uani . . . . . . N4 N 0.2350(3) 0.6618(3) 0.34537(17) 0.0423 1.0000 Uani . . . . . . N5 N 0.1962(3) 0.3315(3) 0.30595(15) 0.0382 1.0000 Uani . . . . . . N6 N 0.2540(4) 0.1836(3) 0.13263(16) 0.0438 1.0000 Uani . . . . . . C1 C 0.7020(3) 0.6882(3) 0.36285(19) 0.0395 1.0000 Uani . . . . . . C2 C -0.1448(3) 0.4730(3) 0.1178(2) 0.0420 1.0000 Uani . . . . . . C3 C 0.5942(5) 0.9611(4) 0.2136(3) 0.0574 1.0000 Uani . . . . . . C4 C 0.6610(6) 1.1299(5) 0.2500(3) 0.0680 1.0000 Uani . . . . . . C5 C 0.6019(5) 1.1951(4) 0.3314(3) 0.0629 1.0000 Uani . . . . . . C6 C 0.4816(4) 1.0932(3) 0.3748(3) 0.0513 1.0000 Uani . . . . . . C7 C 0.4200(4) 0.9264(3) 0.33434(19) 0.0390 1.0000 Uani . . . . . . C8 C 0.2910(4) 0.8140(3) 0.37988(19) 0.0426 1.0000 Uani . . . . . . C9 C 0.1087(5) 0.5558(4) 0.3938(3) 0.0558 1.0000 Uani . . . . . . C10 C 0.1754(6) 0.4131(4) 0.4006(2) 0.0553 1.0000 Uani . . . . . . C11 C 0.1306(4) 0.1765(3) 0.27941(19) 0.0407 1.0000 Uani . . . . . . C12 C 0.1549(3) 0.0905(3) 0.18607(18) 0.0375 1.0000 Uani . . . . . . C13 C 0.0829(4) -0.0783(3) 0.1571(2) 0.0480 1.0000 Uani . . . . . . C14 C 0.1155(6) -0.1553(4) 0.0706(3) 0.0587 1.0000 Uani . . . . . . C15 C 0.2199(7) -0.0604(4) 0.0158(3) 0.0655 1.0000 Uani . . . . . . C16 C 0.2851(6) 0.1081(4) 0.0490(2) 0.0591 1.0000 Uani . . . . . . H31 H 0.6364 0.9160 0.1594 0.076(4) 1.0000 Uiso R . . . . . H41 H 0.7463 1.1970 0.2192 0.088(4) 1.0000 Uiso R . . . . . H51 H 0.6468 1.3113 0.3590 0.083(4) 1.0000 Uiso R . . . . . H61 H 0.4418 1.1352 0.4336 0.072(4) 1.0000 Uiso R . . . . . H81 H 0.2483 0.8535 0.4340 0.058(4) 1.0000 Uiso R . . . . . H91 H 0.0890 0.6095 0.4574 0.076(4) 1.0000 Uiso R . . . . . H92 H -0.0056 0.5109 0.3526 0.077(4) 1.0000 Uiso R . . . . . H101 H 0.2914 0.4461 0.4401 0.075(4) 1.0000 Uiso R . . . . . H102 H 0.0855 0.3388 0.4300 0.074(4) 1.0000 Uiso R . . . . . H111 H 0.0692 0.1181 0.3225 0.057(4) 1.0000 Uiso R . . . . . H131 H 0.0153 -0.1392 0.1967 0.066(4) 1.0000 Uiso R . . . . . H141 H 0.0669 -0.2699 0.0501 0.078(4) 1.0000 Uiso R . . . . . H151 H 0.2421 -0.1125 -0.0458 0.089(4) 1.0000 Uiso R . . . . . H161 H 0.3560 0.1746 0.0113 0.077(4) 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.02792(3) 0.02671(3) 0.03075(3) 0.00693(2) 0.00454(2) 0.00528(2) S1 0.0503(4) 0.0430(3) 0.0599(4) 0.0051(3) -0.0104(3) 0.0064(3) S2 0.0373(3) 0.0780(5) 0.0562(4) 0.0264(4) 0.0064(3) 0.0205(3) N1 0.0523(14) 0.0401(11) 0.0774(19) 0.0108(12) -0.0136(13) 0.0100(10) N2 0.0412(12) 0.076(2) 0.0729(19) 0.0283(16) -0.0010(12) 0.0192(13) N3 0.0476(11) 0.0384(10) 0.0433(10) 0.0123(8) 0.0069(9) 0.0110(8) N4 0.0485(11) 0.0399(10) 0.0434(10) 0.0114(8) 0.0195(9) 0.0176(8) N5 0.0455(10) 0.0389(9) 0.0361(8) 0.0151(7) 0.0144(7) 0.0163(8) N6 0.0533(12) 0.0320(8) 0.0390(9) 0.0079(7) 0.0105(8) 0.0024(8) C1 0.0348(10) 0.0413(11) 0.0431(11) 0.0111(9) -0.0019(8) 0.0131(8) C2 0.0331(9) 0.0431(12) 0.0497(12) 0.0166(10) 0.0068(9) 0.0075(8) C3 0.0625(18) 0.0533(16) 0.0563(17) 0.0235(14) 0.0134(14) 0.0098(14) C4 0.064(2) 0.0528(17) 0.085(3) 0.0372(18) 0.0043(18) 0.0028(15) C5 0.0627(19) 0.0344(12) 0.089(3) 0.0168(14) -0.0050(18) 0.0121(12) C6 0.0509(14) 0.0353(11) 0.0662(18) 0.0050(11) -0.0037(13) 0.0176(10) C7 0.0415(11) 0.0336(9) 0.0438(11) 0.0086(8) 0.0006(9) 0.0155(8) C8 0.0493(13) 0.0409(11) 0.0420(11) 0.0072(9) 0.0129(10) 0.0212(10) C9 0.0666(18) 0.0479(14) 0.0613(17) 0.0178(13) 0.0395(15) 0.0214(13) C10 0.085(2) 0.0503(15) 0.0416(13) 0.0190(11) 0.0304(14) 0.0288(15) C11 0.0419(11) 0.0393(10) 0.0464(12) 0.0195(9) 0.0133(9) 0.0131(9) C12 0.0363(9) 0.0323(9) 0.0425(11) 0.0136(8) 0.0040(8) 0.0055(7) C13 0.0500(14) 0.0334(10) 0.0557(15) 0.0147(10) 0.0071(11) 0.0027(9) C14 0.071(2) 0.0333(11) 0.0583(17) 0.0053(11) 0.0079(15) 0.0005(12) C15 0.094(3) 0.0384(13) 0.0485(15) 0.0008(11) 0.0203(16) 0.0018(15) C16 0.083(2) 0.0398(12) 0.0435(13) 0.0071(10) 0.0196(14) 0.0023(13) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.17030(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pb1 . N1 . 2.525(3) yes Pb1 . N2 . 2.659(3) yes Pb1 . N3 . 2.845(2) yes Pb1 . N4 . 2.569(2) yes Pb1 . N5 . 2.5342(19) yes Pb1 . N6 . 2.734(2) yes S1 . C1 . 1.625(3) yes S2 . C2 . 1.627(3) yes N1 . C1 . 1.160(4) yes N2 . C2 . 1.159(4) yes N3 . C3 . 1.332(4) yes N3 . C7 . 1.340(4) yes N4 . C8 . 1.263(4) yes N4 . C9 . 1.456(4) yes N5 . C10 . 1.460(3) yes N5 . C11 . 1.274(3) yes N6 . C12 . 1.346(3) yes N6 . C16 . 1.333(4) yes C3 . C4 . 1.398(6) yes C3 . H31 . 0.929 no C4 . C5 . 1.371(7) yes C4 . H41 . 0.943 no C5 . C6 . 1.365(6) yes C5 . H51 . 0.968 no C6 . C7 . 1.391(4) yes C6 . H61 . 0.965 no C7 . C8 . 1.470(4) yes C8 . H81 . 0.913 no C9 . C10 . 1.511(5) yes C9 . H91 . 0.991 no C9 . H92 . 0.966 no C10 . H101 . 0.968 no C10 . H102 . 0.984 no C11 . C12 . 1.466(4) yes C11 . H111 . 0.949 no C12 . C13 . 1.388(4) yes C13 . C14 . 1.377(5) yes C13 . H131 . 0.940 no C14 . C15 . 1.387(5) yes C14 . H141 . 0.943 no C15 . C16 . 1.388(4) yes C15 . H151 . 0.970 no C16 . H161 . 0.957 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Pb1 . N2 . 146.95(12) yes N1 . Pb1 . N3 . 77.07(8) yes N2 . Pb1 . N3 . 103.11(10) yes N1 . Pb1 . N4 . 77.54(10) yes N2 . Pb1 . N4 . 74.27(10) yes N3 . Pb1 . N4 . 60.60(7) yes N1 . Pb1 . N5 . 76.65(9) yes N2 . Pb1 . N5 . 76.26(9) yes N3 . Pb1 . N5 . 123.86(7) yes N4 . Pb1 . N5 . 65.73(7) yes N1 . Pb1 . N6 . 99.49(8) yes N2 . Pb1 . N6 . 84.10(10) yes N3 . Pb1 . N6 . 171.43(7) yes N4 . Pb1 . N6 . 126.71(7) yes N5 . Pb1 . N6 . 61.98(7) yes Pb1 . N1 . C1 . 127.5(2) yes Pb1 . N2 . C2 . 152.1(3) yes Pb1 . N3 . C3 . 127.2(2) yes Pb1 . N3 . C7 . 115.15(17) yes C3 . N3 . C7 . 117.5(3) yes Pb1 . N4 . C8 . 125.58(18) yes Pb1 . N4 . C9 . 115.11(18) yes C8 . N4 . C9 . 119.2(2) yes Pb1 . N5 . C10 . 116.68(17) yes Pb1 . N5 . C11 . 123.51(17) yes C10 . N5 . C11 . 119.5(2) yes Pb1 . N6 . C12 . 116.02(17) yes Pb1 . N6 . C16 . 125.89(18) yes C12 . N6 . C16 . 117.6(2) yes S1 . C1 . N1 . 178.6(3) yes S2 . C2 . N2 . 178.7(3) yes N3 . C3 . C4 . 122.9(4) yes N3 . C3 . H31 . 118.1 no C4 . C3 . H31 . 119.0 no C3 . C4 . C5 . 118.8(3) yes C3 . C4 . H41 . 120.3 no C5 . C4 . H41 . 120.9 no C4 . C5 . C6 . 119.1(3) yes C4 . C5 . H51 . 120.9 no C6 . C5 . H51 . 120.1 no C5 . C6 . C7 . 119.1(3) yes C5 . C6 . H61 . 120.8 no C7 . C6 . H61 . 120.0 no C6 . C7 . N3 . 122.7(3) yes C6 . C7 . C8 . 120.2(3) yes N3 . C7 . C8 . 117.1(2) yes C7 . C8 . N4 . 121.4(2) yes C7 . C8 . H81 . 120.3 no N4 . C8 . H81 . 118.3 no N4 . C9 . C10 . 108.7(2) yes N4 . C9 . H91 . 115.2 no C10 . C9 . H91 . 109.8 no N4 . C9 . H92 . 106.2 no C10 . C9 . H92 . 106.2 no H91 . C9 . H92 . 110.2 no C9 . C10 . N5 . 109.0(2) yes C9 . C10 . H101 . 112.6 no N5 . C10 . H101 . 108.7 no C9 . C10 . H102 . 108.2 no N5 . C10 . H102 . 111.3 no H101 . C10 . H102 . 107.1 no N5 . C11 . C12 . 120.8(2) yes N5 . C11 . H111 . 118.2 no C12 . C11 . H111 . 120.9 no C11 . C12 . N6 . 116.3(2) yes C11 . C12 . C13 . 120.8(2) yes N6 . C12 . C13 . 122.9(3) yes C12 . C13 . C14 . 119.1(3) yes C12 . C13 . H131 . 120.3 no C14 . C13 . H131 . 120.6 no C13 . C14 . C15 . 118.4(3) yes C13 . C14 . H141 . 119.8 no C15 . C14 . H141 . 121.8 no C14 . C15 . C16 . 119.2(3) yes C14 . C15 . H151 . 119.4 no C16 . C15 . H151 . 121.3 no C15 . C16 . N6 . 122.8(3) yes C15 . C16 . H161 . 119.7 no N6 . C16 . H161 . 117.5 no data_C20H20N6PbS2 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_moiety ? _chemical_formula_sum 'C20 H20 N6 Pb S2' _chemical_formula_weight 615.73 #============================================================= # 6. CRYSTAL DATA _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_H-M_alt 'P b c n' _space_group_name_Hall '-P 2n 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' #------------------------------------------------ _cell_length_a 34.1371(19) _cell_length_b 16.4965(9) _cell_length_c 8.0031(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4506.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_F_000 2368 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 7.690 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8157 _diffrn_reflns_av_unetI/netI 0.0375 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.371 _diffrn_reflns_theta_max 26.371 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.965 _diffrn_measured_fraction_theta_full 0.975 _diffrn_reflns_Laue_measured_fraction_max 0.965 _diffrn_reflns_Laue_measured_fraction_full 0.975 _diffrn_reflns_point_group_measured_fraction_max 0.965 _diffrn_reflns_point_group_measured_fraction_full 0.975 #========================================================================== # 8. REFINEMENT DATA _reflns_number_total 4444 _reflns_number_gt 3742 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0892P)^2^+29.4629P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4444 _refine_ls_number_parameters 262 _refine_ls_number_restraints 91 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1538 _refine_ls_wR_factor_gt 0.1458 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 3.916 _refine_diff_density_min -2.408 _refine_diff_density_rms 0.202 #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group PB1 Pb 0.33368(2) 0.73767(2) 0.69874(4) 0.02815(16) Uani 1 1 d . U . . . S1 S 0.27480(11) 0.7746(2) 1.3056(3) 0.0602(8) Uani 1 1 d . U . . . N1 N 0.3204(3) 0.7618(5) 1.0190(11) 0.050(2) Uani 1 1 d . U . . . C1 C 0.3016(3) 0.7680(5) 1.1366(12) 0.037(2) Uani 1 1 d . U . . . N2 N 0.4434(3) 0.8046(8) 0.4234(17) 0.085(3) Uani 1 1 d . U . . . C2 C 0.4189(4) 0.7568(7) 0.4192(14) 0.051(2) Uani 1 1 d . U . . . S2 S 0.38440(9) 0.68717(19) 0.4156(3) 0.0566(7) Uani 1 1 d . U . . . N3 N 0.3550(2) 0.8920(5) 0.7063(10) 0.046(2) Uani 1 1 d . U . . . C3 C 0.3332(3) 0.9528(7) 0.662(2) 0.070(4) Uani 1 1 d . U . . . H3 H 0.308871 0.941826 0.614240 0.084 Uiso 1 1 calc R U . . . N4 N 0.4017(2) 0.7672(4) 0.8085(8) 0.0293(15) Uani 1 1 d . U . . . C4 C 0.3444(5) 1.0350(8) 0.6814(19) 0.081(4) Uani 1 1 d . U . . . H4 H 0.327488 1.077098 0.654229 0.098 Uiso 1 1 calc R U . . . C5 C 0.3804(4) 1.0496(7) 0.7407(18) 0.076(3) Uani 1 1 d . U . . . H5 H 0.389526 1.102674 0.747977 0.091 Uiso 1 1 calc R U . . . N5 N 0.3685(2) 0.6142(4) 0.8209(8) 0.0264(13) Uani 1 1 d . U . . . N6 N 0.3042(2) 0.5888(4) 0.6154(9) 0.0337(15) Uani 1 1 d . U . . . C6 C 0.4036(4) 0.9876(7) 0.7902(16) 0.066(3) Uani 1 1 d . U . . . H6 H 0.427991 0.997814 0.837747 0.079 Uiso 1 1 calc R U . . . C7 C 0.3907(3) 0.9086(5) 0.7694(12) 0.040(2) Uani 1 1 d . U . . . C8 C 0.4141(3) 0.8389(5) 0.8219(12) 0.040(2) Uani 1 1 d . U . . . H8 H 0.438849 0.847754 0.866721 0.048 Uiso 1 1 calc R U . . . C9 C 0.4274(2) 0.6972(5) 0.8499(9) 0.0253(15) Uani 1 1 d . U . . . H9 H 0.437402 0.675084 0.744522 0.030 Uiso 1 1 calc R U . . . C10 C 0.4626(3) 0.7185(6) 0.9583(11) 0.0371(19) Uani 1 1 d . U . . . H10A H 0.479332 0.755917 0.897893 0.045 Uiso 1 1 calc R U . . . H10B H 0.453571 0.745623 1.058693 0.045 Uiso 1 1 calc R U . . . C11 C 0.4862(3) 0.6449(6) 1.0071(12) 0.044(2) Uani 1 1 d . U . . . H11A H 0.506741 0.660987 1.084090 0.053 Uiso 1 1 calc R U . . . H11B H 0.498557 0.622323 0.908387 0.053 Uiso 1 1 calc R U . . . C12 C 0.4605(3) 0.5800(6) 1.0896(11) 0.0391(19) Uani 1 1 d . U . . . H12A H 0.476185 0.532284 1.112463 0.047 Uiso 1 1 calc R U . . . H12B H 0.450597 0.600417 1.195119 0.047 Uiso 1 1 calc R U . . . C13 C 0.4263(3) 0.5570(5) 0.9776(10) 0.0348(18) Uani 1 1 d . U . . . H13A H 0.409992 0.517527 1.034525 0.042 Uiso 1 1 calc R U . . . H13B H 0.436183 0.532105 0.876199 0.042 Uiso 1 1 calc R U . . . C14 C 0.4015(2) 0.6310(4) 0.9321(9) 0.0258(15) Uani 1 1 d . U . . . H14 H 0.390951 0.653480 1.036020 0.031 Uiso 1 1 calc R U . . . C15 C 0.3583(2) 0.5422(5) 0.7831(9) 0.0270(16) Uani 1 1 d . U . . . H15 H 0.372910 0.499079 0.824578 0.032 Uiso 1 1 calc R U . . . C16 C 0.3240(3) 0.5244(5) 0.6760(10) 0.0260(16) Uani 1 1 d . U . . . C17 C 0.3117(3) 0.4458(5) 0.6483(10) 0.0320(17) Uani 1 1 d . U . . . H17 H 0.325145 0.402684 0.696577 0.038 Uiso 1 1 calc R U . . . C18 C 0.2802(3) 0.4319(5) 0.5508(11) 0.0389(19) Uani 1 1 d . U . . . H18 H 0.272215 0.379198 0.527395 0.047 Uiso 1 1 calc R U . . . C19 C 0.2605(3) 0.4964(6) 0.4876(12) 0.0394(19) Uani 1 1 d . U . . . H19 H 0.238579 0.488358 0.420828 0.047 Uiso 1 1 calc R U . . . C20 C 0.2731(3) 0.5735(5) 0.5228(11) 0.0367(18) Uani 1 1 d . U . . . H20 H 0.259094 0.616960 0.479265 0.044 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 PB1 0.0252(3) 0.0272(2) 0.0321(2) -0.00177(10) -0.00165(12) 0.00209(10) S1 0.067(2) 0.0632(18) 0.0503(16) 0.0072(12) 0.0248(14) 0.0217(15) N1 0.055(6) 0.060(5) 0.035(4) -0.003(3) 0.010(4) 0.001(4) C1 0.044(6) 0.027(4) 0.040(4) 0.000(3) 0.007(4) 0.000(3) N2 0.052(7) 0.090(8) 0.113(9) 0.010(7) 0.022(6) -0.008(5) C2 0.041(6) 0.061(6) 0.050(6) 0.014(5) 0.005(5) 0.010(4) S2 0.0537(18) 0.0800(18) 0.0362(12) -0.0170(12) 0.0078(12) -0.0091(13) N3 0.039(5) 0.032(3) 0.069(6) 0.008(3) -0.013(4) -0.002(3) C3 0.053(8) 0.038(5) 0.118(10) 0.014(6) -0.030(7) 0.005(4) N4 0.021(4) 0.032(3) 0.035(4) 0.003(3) -0.001(3) -0.002(2) C4 0.088(9) 0.035(5) 0.121(12) 0.014(6) -0.025(8) 0.012(6) C5 0.097(9) 0.030(5) 0.101(9) 0.001(6) -0.012(8) -0.007(5) N5 0.018(4) 0.032(3) 0.029(3) -0.003(2) -0.001(2) 0.000(2) N6 0.027(4) 0.035(3) 0.039(4) -0.001(3) -0.005(3) -0.001(3) C6 0.063(7) 0.036(5) 0.099(10) -0.001(5) -0.022(6) -0.013(4) C7 0.039(5) 0.034(4) 0.047(5) -0.003(4) -0.001(4) -0.002(3) C8 0.030(5) 0.035(4) 0.054(5) 0.001(4) -0.007(4) -0.004(3) C9 0.023(4) 0.032(4) 0.021(3) 0.002(3) -0.001(3) 0.002(3) C10 0.021(5) 0.049(5) 0.041(5) 0.006(4) -0.010(4) -0.004(3) C11 0.027(5) 0.058(6) 0.047(5) 0.009(4) -0.006(4) 0.008(4) C12 0.031(5) 0.051(5) 0.036(5) 0.006(4) -0.008(4) 0.008(4) C13 0.040(5) 0.032(4) 0.032(4) 0.005(3) -0.003(4) 0.004(3) C14 0.029(4) 0.028(3) 0.020(3) -0.003(3) -0.003(3) 0.004(3) C15 0.025(5) 0.031(4) 0.025(4) 0.000(3) 0.004(3) 0.003(3) C16 0.023(4) 0.026(3) 0.029(4) -0.003(3) 0.008(3) -0.003(3) C17 0.031(5) 0.031(4) 0.034(4) -0.004(3) 0.008(3) -0.004(3) C18 0.042(6) 0.038(4) 0.036(5) -0.008(3) 0.002(4) -0.012(3) C19 0.031(5) 0.055(5) 0.032(4) -0.002(4) 0.002(4) -0.012(4) C20 0.029(5) 0.044(4) 0.037(4) 0.004(4) -0.009(4) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag PB1 N4 2.531(8) . ? PB1 N5 2.554(7) . ? PB1 N1 2.633(9) . ? PB1 N3 2.648(8) . ? PB1 N6 2.736(7) . ? PB1 S2 2.971(3) . ? S1 C1 1.637(10) . ? N1 C1 1.144(13) . ? N2 C2 1.150(15) . ? C2 S2 1.644(13) . ? N3 C3 1.299(13) . ? N3 C7 1.348(13) . ? C3 C4 1.419(18) . ? N4 C8 1.261(11) . ? N4 C9 1.488(10) . ? C4 C5 1.34(2) . ? C5 C6 1.354(17) . ? N5 C15 1.275(10) . ? N5 C14 1.462(10) . ? N6 C20 1.319(11) . ? N6 C16 1.350(11) . ? C6 C7 1.386(13) . ? C7 C8 1.461(13) . ? C9 C10 1.523(11) . ? C9 C14 1.550(10) . ? C10 C11 1.508(12) . ? C11 C12 1.534(13) . ? C12 C13 1.521(12) . ? C13 C14 1.529(10) . ? C15 C16 1.480(12) . ? C16 C17 1.380(11) . ? C17 C18 1.348(12) . ? C18 C19 1.357(13) . ? C19 C20 1.372(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 PB1 N5 66.0(2) . . ? N4 PB1 N1 77.9(3) . . ? N5 PB1 N1 80.1(2) . . ? N4 PB1 N3 63.6(2) . . ? N5 PB1 N3 129.1(2) . . ? N1 PB1 N3 83.1(3) . . ? N4 PB1 N6 126.5(2) . . ? N5 PB1 N6 63.2(2) . . ? N1 PB1 N6 108.0(2) . . ? N3 PB1 N6 165.7(2) . . ? N4 PB1 S2 77.52(17) . . ? N5 PB1 S2 78.28(15) . . ? N1 PB1 S2 152.2(2) . . ? N3 PB1 S2 97.3(2) . . ? N6 PB1 S2 77.10(16) . . ? C1 N1 PB1 155.6(9) . . ? N1 C1 S1 178.7(8) . . ? N2 C2 S2 178.9(12) . . ? C2 S2 PB1 102.0(4) . . ? C3 N3 C7 117.7(9) . . ? C3 N3 PB1 125.3(7) . . ? C7 N3 PB1 116.9(6) . . ? N3 C3 C4 123.5(11) . . ? C8 N4 C9 120.8(8) . . ? C8 N4 PB1 121.1(6) . . ? C9 N4 PB1 118.0(5) . . ? C5 C4 C3 117.5(11) . . ? C4 C5 C6 120.2(11) . . ? C15 N5 C14 122.2(7) . . ? C15 N5 PB1 121.6(5) . . ? C14 N5 PB1 116.1(4) . . ? C20 N6 C16 117.0(7) . . ? C20 N6 PB1 127.2(6) . . ? C16 N6 PB1 115.8(5) . . ? C5 C6 C7 119.3(11) . . ? N3 C7 C6 121.6(9) . . ? N3 C7 C8 116.3(8) . . ? C6 C7 C8 122.1(9) . . ? N4 C8 C7 122.1(9) . . ? N4 C9 C10 114.4(7) . . ? N4 C9 C14 107.8(6) . . ? C10 C9 C14 111.7(6) . . ? C11 C10 C9 112.5(8) . . ? C10 C11 C12 111.6(7) . . ? C13 C12 C11 111.1(7) . . ? C12 C13 C14 111.4(7) . . ? N5 C14 C13 114.8(6) . . ? N5 C14 C9 108.3(6) . . ? C13 C14 C9 110.4(7) . . ? N5 C15 C16 122.6(7) . . ? N6 C16 C17 122.0(8) . . ? N6 C16 C15 116.6(7) . . ? C17 C16 C15 121.3(8) . . ? C18 C17 C16 119.7(8) . . ? C17 C18 C19 118.5(8) . . ? C18 C19 C20 119.7(9) . . ? N6 C20 C19 123.0(8) . . ? data_C22H20N8PbPtS4 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_moiety ? _chemical_formula_sum 'C22 H20 N8 Pb Pt S4' _chemical_formula_weight 926.98 #============================================================= # 6. CRYSTAL DATA _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' #------------------------------------------------ _cell_length_a 8.5760(3) _cell_length_b 16.7744(7) _cell_length_c 18.8088(7) _cell_angle_alpha 90 _cell_angle_beta 95.3290(12) _cell_angle_gamma 90 _cell_volume 2694.09(18) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.285 _exptl_crystal_F_000 1728 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 24.714 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32064 _diffrn_reflns_av_unetI/netI 0.0383 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.537 _diffrn_reflns_theta_max 72.113 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_point_group_measured_fraction_full 0.998 #========================================================================== # 8. REFINEMENT DATA _reflns_number_total 5281 _reflns_number_gt 4931 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2016/4 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+10.3583P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5281 _refine_ls_number_parameters 325 _refine_ls_number_restraints 104 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.459 _refine_diff_density_min -1.576 _refine_diff_density_rms 0.141 #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group PB1 Pb 0.07613(3) 0.78009(2) 0.32897(2) 0.04169(7) Uani 1 1 d . U . . . C1 C -0.3072(7) 0.7085(4) 0.3246(3) 0.0447(12) Uani 1 1 d . U . . . N1 N -0.1838(6) 0.7224(3) 0.3112(3) 0.0542(12) Uani 1 1 d . U . . . S1 S -0.48956(18) 0.68282(11) 0.33993(8) 0.0542(4) Uani 1 1 d . U . . . PT1 Pt -0.50260(3) 0.74485(2) 0.44987(2) 0.04182(8) Uani 1 1 d . U . . . S3 S -0.5203(2) 0.81731(10) 0.55342(8) 0.0566(4) Uani 1 1 d . U . . . C3 C -0.4968(9) 0.7544(5) 0.6237(3) 0.0620(17) Uani 1 1 d . U . . . N3 N -0.4813(10) 0.7188(4) 0.6745(3) 0.081(2) Uani 1 1 d . U . . . S2 S -0.4617(3) 0.62607(11) 0.51047(10) 0.0762(6) Uani 1 1 d . U . . . C2 C -0.3252(10) 0.5770(4) 0.4691(4) 0.0619(16) Uani 1 1 d . U . . . N2 N -0.2299(10) 0.5411(4) 0.4461(4) 0.089(2) Uani 1 1 d . U . . . S4 S -0.5559(2) 0.85930(11) 0.38155(9) 0.0667(5) Uani 1 1 d . U . . . C4 C -0.6464(11) 0.9244(5) 0.4299(4) 0.0689(19) Uani 1 1 d . U . . . N4 N -0.7135(13) 0.9706(5) 0.4571(4) 0.117(3) Uani 1 1 d . U . . . N7 N 0.0756(7) 0.6860(3) 0.4326(2) 0.0510(12) Uani 1 1 d . U . . . C7 C -0.2906(9) 1.0446(4) 0.2959(4) 0.0676(18) Uani 1 1 d . U . . . H7 H -0.348224 1.091642 0.293278 0.081 Uiso 1 1 calc R U . . . N6 N -0.0391(8) 0.8360(3) 0.4347(2) 0.0594(14) Uani 1 1 d . U . . . C6 C -0.2450(9) 1.0095(5) 0.2352(4) 0.0693(19) Uani 1 1 d . U . . . H6 H -0.273647 1.031706 0.190599 0.083 Uiso 1 1 calc R U . . . N5 N -0.1149(6) 0.9065(3) 0.3036(3) 0.0516(11) Uani 1 1 d . U . . . C5 C -0.1572(9) 0.9416(4) 0.2413(4) 0.0642(17) Uani 1 1 d . U . . . H5 H -0.125395 0.918704 0.199979 0.077 Uiso 1 1 calc R U . . . N8 N 0.1464(6) 0.6268(3) 0.3022(2) 0.0458(10) Uani 1 1 d . U . . . C8 C -0.2490(9) 1.0087(4) 0.3608(4) 0.0617(16) Uani 1 1 d . U . . . H8 H -0.278893 1.030875 0.402790 0.074 Uiso 1 1 calc R U . . . C9 C -0.1631(8) 0.9397(4) 0.3626(3) 0.0501(13) Uani 1 1 d . U . . . C10 C -0.1211(9) 0.8988(4) 0.4308(3) 0.0638(18) Uani 1 1 d . U . . . H10 H -0.155882 0.919629 0.472287 0.077 Uiso 1 1 calc R U . . . C11 C 0.0028(19) 0.7949(6) 0.5031(4) 0.139(6) Uani 1 1 d . U . . . H11 H 0.113194 0.810869 0.509286 0.167 Uiso 1 1 calc R U . . . C12 C -0.0479(9) 0.8343(4) 0.5693(3) 0.0633(18) Uani 1 1 d . U . . . H12A H -0.001437 0.887012 0.574121 0.076 Uiso 1 1 calc R U . . . H12B H -0.160773 0.840651 0.564280 0.076 Uiso 1 1 calc R U . . . C13 C -0.001(2) 0.7873(7) 0.6354(4) 0.149(6) Uani 1 1 d . U . . . H13A H 0.095479 0.810392 0.657195 0.178 Uiso 1 1 calc R U . . . H13B H -0.080226 0.796474 0.668088 0.178 Uiso 1 1 calc R U . . . C14 C 0.021(2) 0.7103(6) 0.6327(4) 0.146(6) Uani 1 1 d . U . . . H14A H -0.076775 0.685349 0.642949 0.175 Uiso 1 1 calc R U . . . H14B H 0.097812 0.696827 0.671823 0.175 Uiso 1 1 calc R U . . . C15 C 0.0716(10) 0.6702(4) 0.5665(3) 0.0646(19) Uani 1 1 d . U . . . H15A H 0.024506 0.617658 0.561919 0.077 Uiso 1 1 calc R U . . . H15B H 0.184418 0.663502 0.571850 0.077 Uiso 1 1 calc R U . . . C16 C 0.0253(17) 0.7177(5) 0.4993(4) 0.115(5) Uani 1 1 d . U . . . H16 H -0.084777 0.701357 0.492292 0.138 Uiso 1 1 calc R U . . . C17 C 0.1097(8) 0.6130(4) 0.4264(3) 0.0544(15) Uani 1 1 d . U . . . H17 H 0.107023 0.579817 0.465880 0.065 Uiso 1 1 calc R U . . . C18 C 0.1532(7) 0.5792(4) 0.3592(3) 0.0469(12) Uani 1 1 d . U . . . C19 C 0.2034(10) 0.5016(4) 0.3571(4) 0.069(2) Uani 1 1 d . U . . . H19 H 0.206003 0.469526 0.397494 0.082 Uiso 1 1 calc R U . . . C20 C 0.2500(11) 0.4722(5) 0.2937(4) 0.081(2) Uani 1 1 d . U . . . H20 H 0.284005 0.419733 0.290700 0.098 Uiso 1 1 calc R U . . . C21 C 0.2454(9) 0.5212(4) 0.2355(4) 0.0665(18) Uani 1 1 d . U . . . H21 H 0.277638 0.503094 0.192438 0.080 Uiso 1 1 calc R U . . . C22 C 0.1924(7) 0.5973(4) 0.2420(3) 0.0533(14) Uani 1 1 d . U . . . H22 H 0.188193 0.630273 0.202118 0.064 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 PB1 0.04808(12) 0.04020(12) 0.03768(11) 0.00111(8) 0.00878(9) -0.00612(9) C1 0.051(3) 0.052(3) 0.031(2) -0.005(2) 0.005(2) -0.005(3) N1 0.050(3) 0.064(3) 0.049(3) -0.012(2) 0.009(2) -0.009(2) S1 0.0506(8) 0.0692(10) 0.0432(7) -0.0116(7) 0.0068(6) -0.0135(7) PT1 0.04293(13) 0.04935(15) 0.03392(11) -0.00005(9) 0.00754(9) -0.00483(10) S3 0.0718(10) 0.0570(9) 0.0418(7) -0.0043(6) 0.0085(7) 0.0047(8) C3 0.074(4) 0.078(5) 0.035(3) -0.004(3) 0.010(3) -0.002(4) N3 0.113(6) 0.092(5) 0.037(3) 0.006(3) 0.007(3) -0.005(4) S2 0.1150(16) 0.0602(10) 0.0589(10) 0.0151(8) 0.0367(11) 0.0158(11) C2 0.085(5) 0.050(4) 0.051(3) 0.006(3) 0.009(3) 0.002(3) N2 0.122(6) 0.072(4) 0.075(4) 0.009(3) 0.024(4) 0.031(4) S4 0.0876(12) 0.0629(10) 0.0513(8) 0.0144(7) 0.0162(8) 0.0094(9) C4 0.097(6) 0.057(4) 0.053(4) 0.007(3) 0.005(4) 0.010(4) N4 0.179(10) 0.093(6) 0.082(5) 0.013(4) 0.029(6) 0.054(6) N7 0.075(3) 0.044(2) 0.036(2) 0.0027(19) 0.016(2) 0.012(3) C7 0.071(4) 0.054(4) 0.076(4) 0.016(3) -0.001(4) 0.011(3) N6 0.095(4) 0.048(3) 0.034(2) -0.001(2) -0.001(2) 0.022(3) C6 0.083(5) 0.063(4) 0.060(4) 0.024(3) -0.005(4) 0.000(4) N5 0.067(3) 0.042(2) 0.045(2) 0.004(2) 0.001(2) 0.004(2) C5 0.085(5) 0.061(4) 0.046(3) 0.009(3) 0.005(3) 0.003(3) N8 0.047(2) 0.048(3) 0.043(2) -0.0027(19) 0.005(2) 0.002(2) C8 0.075(4) 0.047(3) 0.063(4) 0.005(3) 0.004(3) 0.011(3) C9 0.061(3) 0.041(3) 0.047(3) 0.003(2) -0.001(3) 0.004(3) C10 0.092(5) 0.057(4) 0.041(3) -0.003(3) 0.001(3) 0.026(4) C11 0.299(17) 0.090(6) 0.027(3) 0.002(3) 0.013(5) 0.112(9) C12 0.086(5) 0.067(4) 0.036(3) -0.012(3) 0.002(3) 0.028(4) C13 0.296(18) 0.117(7) 0.030(3) -0.004(4) 0.005(6) 0.108(10) C14 0.300(19) 0.100(6) 0.045(4) 0.020(4) 0.065(8) 0.076(9) C15 0.102(5) 0.059(4) 0.035(3) 0.006(3) 0.015(3) 0.017(4) C16 0.242(13) 0.070(5) 0.042(3) 0.019(3) 0.059(6) 0.074(7) C17 0.072(4) 0.049(3) 0.044(3) 0.006(2) 0.014(3) 0.012(3) C18 0.052(3) 0.047(3) 0.041(3) -0.001(2) 0.003(2) 0.004(3) C19 0.105(6) 0.049(3) 0.053(3) 0.000(3) 0.011(4) 0.014(4) C20 0.121(7) 0.054(4) 0.070(4) -0.015(3) 0.017(5) 0.015(5) C21 0.084(5) 0.067(4) 0.049(3) -0.021(3) 0.009(3) 0.004(4) C22 0.056(3) 0.064(4) 0.040(3) -0.005(3) 0.002(2) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag PB1 N1 2.425(5) . ? PB1 N6 2.484(5) . ? PB1 N7 2.508(5) . ? PB1 N5 2.695(5) . ? PB1 N8 2.699(5) . ? C1 N1 1.135(8) . ? C1 S1 1.673(6) . ? S1 PT1 2.3268(14) . ? PT1 S2 2.3060(18) . ? PT1 S3 2.3128(15) . ? PT1 S4 2.3316(17) . ? S3 C3 1.688(7) . ? C3 N3 1.124(9) . ? S2 C2 1.679(8) . ? C2 N2 1.134(10) . ? S4 C4 1.660(8) . ? C4 N4 1.117(10) . ? N7 C17 1.266(8) . ? N7 C16 1.465(8) . ? C7 C6 1.373(11) . ? C7 C8 1.379(10) . ? N6 C10 1.265(8) . ? N6 C11 1.474(8) . ? C6 C5 1.365(10) . ? N5 C5 1.331(8) . ? N5 C9 1.341(8) . ? N8 C22 1.328(7) . ? N8 C18 1.334(7) . ? C8 C9 1.370(9) . ? C9 C10 1.470(8) . ? C11 C16 1.312(11) . ? C11 C12 1.510(9) . ? C12 C13 1.495(10) . ? C13 C14 1.305(14) . ? C14 C15 1.514(10) . ? C15 C16 1.516(9) . ? C17 C18 1.466(8) . ? C18 C19 1.372(9) . ? C19 C20 1.384(10) . ? C20 C21 1.367(11) . ? C21 C22 1.364(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 PB1 N6 80.34(19) . . ? N1 PB1 N7 77.75(19) . . ? N6 PB1 N7 65.56(16) . . ? N1 PB1 N5 75.73(18) . . ? N6 PB1 N5 64.18(16) . . ? N7 PB1 N5 126.00(16) . . ? N1 PB1 N8 79.18(17) . . ? N6 PB1 N8 128.40(16) . . ? N7 PB1 N8 64.03(15) . . ? N5 PB1 N8 149.20(15) . . ? N1 C1 S1 175.9(6) . . ? C1 N1 PB1 156.3(5) . . ? C1 S1 PT1 99.27(19) . . ? S2 PT1 S3 93.25(6) . . ? S2 PT1 S1 92.02(7) . . ? S3 PT1 S1 174.73(6) . . ? S2 PT1 S4 175.44(8) . . ? S3 PT1 S4 90.37(6) . . ? S1 PT1 S4 84.35(6) . . ? C3 S3 PT1 108.5(3) . . ? N3 C3 S3 173.3(7) . . ? C2 S2 PT1 106.0(2) . . ? N2 C2 S2 174.7(7) . . ? C4 S4 PT1 108.5(3) . . ? N4 C4 S4 174.0(8) . . ? C17 N7 C16 121.2(5) . . ? C17 N7 PB1 121.4(4) . . ? C16 N7 PB1 117.3(4) . . ? C6 C7 C8 118.6(7) . . ? C10 N6 C11 121.9(6) . . ? C10 N6 PB1 121.9(4) . . ? C11 N6 PB1 116.1(4) . . ? C5 C6 C7 119.1(6) . . ? C5 N5 C9 117.7(6) . . ? C5 N5 PB1 128.0(4) . . ? C9 N5 PB1 114.2(4) . . ? N5 C5 C6 123.1(7) . . ? C22 N8 C18 117.9(5) . . ? C22 N8 PB1 127.1(4) . . ? C18 N8 PB1 114.5(4) . . ? C9 C8 C7 119.0(7) . . ? N5 C9 C8 122.6(6) . . ? N5 C9 C10 117.2(5) . . ? C8 C9 C10 120.2(6) . . ? N6 C10 C9 122.0(6) . . ? C16 C11 N6 116.0(7) . . ? C16 C11 C12 122.1(8) . . ? N6 C11 C12 116.8(6) . . ? C13 C12 C11 112.3(6) . . ? C14 C13 C12 121.2(8) . . ? C13 C14 C15 121.6(8) . . ? C14 C15 C16 112.2(6) . . ? C11 C16 N7 117.5(6) . . ? C11 C16 C15 120.1(7) . . ? N7 C16 C15 116.6(6) . . ? N7 C17 C18 122.2(5) . . ? N8 C18 C19 122.4(6) . . ? N8 C18 C17 117.8(5) . . ? C19 C18 C17 119.8(6) . . ? C18 C19 C20 118.7(7) . . ? C21 C20 C19 119.1(7) . . ? C22 C21 C20 118.4(6) . . ? N8 C22 C21 123.6(6) . . ? data_C17H14N7PbPtS3 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_moiety ? _chemical_formula_sum 'C17 H14 N7 Pb Pt0.50 S3' _chemical_formula_weight 717.27 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' #------------------------------------------------ _cell_length_a 9.3859(9) _cell_length_b 11.3420(12) _cell_length_c 11.5733(12) _cell_angle_alpha 66.628(5) _cell_angle_beta 87.508(6) _cell_angle_gamma 71.190(5) _cell_volume 1065.48(19) _cell_formula_units_Z 2 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.236 _exptl_crystal_F_000 668 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.251 _exptl_crystal_size_mid 0.119 _exptl_crystal_size_min 0.092 _exptl_absorpt_coefficient_mu 11.495 _shelx_estimated_absorpt_T_min 0.160 _shelx_estimated_absorpt_T_max 0.418 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10741 _diffrn_reflns_av_unetI/netI 0.0277 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.074 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.848 _diffrn_measured_fraction_theta_full 0.843 _diffrn_reflns_Laue_measured_fraction_max 0.848 _diffrn_reflns_Laue_measured_fraction_full 0.843 _diffrn_reflns_point_group_measured_fraction_max 0.848 _diffrn_reflns_point_group_measured_fraction_full 0.843 #========================================================================== # 8. REFINEMENT DATA _reflns_number_total 3690 _reflns_number_gt 3190 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2016/4 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1113P)^2^+1.2025P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3690 _refine_ls_number_parameters 259 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.1620 _refine_ls_wR_factor_gt 0.1167 _refine_ls_goodness_of_fit_ref 1.182 _refine_ls_restrained_S_all 1.172 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.166 _refine_diff_density_min -1.585 _refine_diff_density_rms 0.443 #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group PB1 Pb 0.97040(4) 0.09098(3) 0.79197(3) 0.03462(18) Uani 1 1 d . U . . . C1 C 1.1615(15) 0.2169(12) 0.5183(11) 0.046(2) Uani 1 1 d . U . . . N1 N 1.2649(14) 0.2252(13) 0.5517(12) 0.072(3) Uani 1 1 d . U . . . S1 S 0.9928(3) 0.2169(3) 0.4685(3) 0.0502(7) Uani 1 1 d . U . . . PT1 Pt 1.000000 0.000000 0.500000 0.03299(19) Uani 1 2 d S U P . . S2 S 0.7651(4) 0.0893(4) 0.3868(4) 0.0720(11) Uani 1 1 d . U . . . C2 C 0.6829(13) 0.2484(13) 0.3716(11) 0.048(3) Uani 1 1 d . U . . . N2 N 0.6183(13) 0.3580(11) 0.3596(12) 0.066(3) Uani 1 1 d . U . . . S3 S 0.6942(5) 0.3672(4) 0.9968(4) 0.0751(11) Uani 1 1 d . U . . . C3 C 0.7843(13) 0.2260(12) 0.9807(9) 0.045(2) Uani 1 1 d . U . . . N3 N 0.8485(10) 0.1274(8) 0.9723(7) 0.0408(17) Uani 1 1 d . U . . . N4 N 0.8238(11) -0.0822(10) 0.8033(8) 0.0439(18) Uani 1 1 d . U . . . C4 C 0.8831(15) -0.2184(13) 0.8462(11) 0.049(2) Uani 1 1 d . U . . . H4 H 0.981256 -0.261925 0.885627 0.059 Uiso 1 1 calc R U . . . N5 N 0.6973(11) 0.1976(10) 0.7060(8) 0.0419(18) Uani 1 1 d . U . . . C5 C 0.8029(19) -0.2947(15) 0.8335(13) 0.061(3) Uani 1 1 d . U . . . H5 H 0.847035 -0.388957 0.867874 0.074 Uiso 1 1 calc R U . . . N7 N 1.1496(11) 0.2154(9) 0.8414(8) 0.0428(18) Uani 1 1 d . U . . . C7 C 0.5998(18) -0.0952(16) 0.7212(14) 0.070(4) Uani 1 1 d . U . . . H7 H 0.504398 -0.049774 0.676575 0.084 Uiso 1 1 calc R U . . . N6 N 0.8786(11) 0.3488(9) 0.6950(8) 0.0446(18) Uani 1 1 d . U . . . C6 C 0.6577(19) -0.2370(17) 0.7711(16) 0.074(4) Uani 1 1 d . U . . . H6 H 0.603314 -0.289432 0.763408 0.089 Uiso 1 1 calc R U . . . C9 C 0.6226(12) 0.1285(12) 0.6934(10) 0.047(2) Uani 1 1 d . U . . . H9 H 0.524271 0.172939 0.654520 0.056 Uiso 1 1 calc R U . . . C8 C 0.6861(13) -0.0200(13) 0.7382(11) 0.048(2) Uani 1 1 d . U . . . C10 C 0.6266(14) 0.3430(13) 0.6686(12) 0.052(3) Uani 1 1 d . U . . . H10A H 0.590265 0.360349 0.742000 0.062 Uiso 1 1 calc R U . . . H10B H 0.540190 0.376293 0.607548 0.062 Uiso 1 1 calc R U . . . C11 C 0.7326(12) 0.4181(11) 0.6125(10) 0.046(2) Uani 1 1 d . U . . . H11A H 0.689487 0.511145 0.605027 0.056 Uiso 1 1 calc R U . . . H11B H 0.750056 0.420222 0.528567 0.056 Uiso 1 1 calc R U . . . C12 C 0.9499(14) 0.4189(12) 0.7150(11) 0.052(2) Uani 1 1 d . U . . . H12 H 0.905811 0.513154 0.682310 0.062 Uiso 1 1 calc R U . . . C13 C 1.0989(13) 0.3557(11) 0.7878(9) 0.041(2) Uani 1 1 d . U . . . C14 C 1.1818(14) 0.4311(13) 0.7980(12) 0.053(3) Uani 1 1 d . U . . . H14 H 1.143686 0.525714 0.759734 0.063 Uiso 1 1 calc R U . . . C15 C 1.3220(15) 0.3659(15) 0.8653(13) 0.060(3) Uani 1 1 d . U . . . H15 H 1.379099 0.415273 0.875362 0.071 Uiso 1 1 calc R U . . . C16 C 1.3764(14) 0.2245(15) 0.9180(12) 0.057(3) Uani 1 1 d . U . . . H16 H 1.471531 0.176892 0.962739 0.068 Uiso 1 1 calc R U . . . C17 C 1.2822(14) 0.1541(14) 0.9017(12) 0.053(3) Uani 1 1 d . U . . . H17 H 1.318704 0.059409 0.936354 0.063 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 PB1 0.0302(3) 0.0287(3) 0.0373(2) -0.00892(17) -0.00297(16) -0.00502(17) C1 0.052(6) 0.039(6) 0.050(6) -0.017(5) -0.001(5) -0.018(5) N1 0.061(7) 0.065(7) 0.085(8) -0.023(6) -0.016(6) -0.024(6) S1 0.0408(15) 0.0352(13) 0.0669(16) -0.0161(12) -0.0088(12) -0.0067(12) PT1 0.0290(3) 0.0302(3) 0.0323(3) -0.0096(2) -0.0012(2) -0.0038(2) S2 0.049(2) 0.0458(17) 0.111(3) -0.0340(19) -0.0391(19) 0.0058(15) C2 0.033(6) 0.049(6) 0.053(6) -0.019(5) -0.003(4) -0.003(4) N2 0.051(7) 0.041(5) 0.087(7) -0.020(5) -0.004(6) 0.000(5) S3 0.073(3) 0.055(2) 0.094(3) -0.043(2) -0.007(2) -0.0009(18) C3 0.039(6) 0.050(6) 0.036(4) -0.015(4) -0.002(4) -0.003(5) N3 0.048(5) 0.032(4) 0.034(3) -0.006(3) 0.000(3) -0.012(4) N4 0.043(5) 0.044(4) 0.046(4) -0.017(4) -0.001(4) -0.016(4) C4 0.054(7) 0.048(5) 0.056(6) -0.028(5) 0.002(5) -0.021(5) N5 0.037(5) 0.046(4) 0.040(4) -0.020(4) -0.009(3) -0.006(4) C5 0.081(9) 0.050(6) 0.060(7) -0.021(6) 0.007(6) -0.032(6) N7 0.046(5) 0.027(4) 0.047(4) -0.003(3) -0.004(3) -0.016(3) C7 0.069(9) 0.069(7) 0.082(9) -0.027(7) -0.016(7) -0.039(7) N6 0.043(5) 0.034(4) 0.037(4) -0.001(3) -0.004(3) -0.004(4) C6 0.074(9) 0.072(7) 0.093(10) -0.040(8) -0.001(7) -0.038(8) C9 0.034(5) 0.057(5) 0.046(5) -0.018(5) -0.007(4) -0.013(4) C8 0.041(6) 0.054(5) 0.052(6) -0.020(5) 0.004(4) -0.023(5) C10 0.037(6) 0.046(5) 0.053(6) -0.015(5) -0.004(5) 0.003(4) C11 0.038(6) 0.033(4) 0.049(5) -0.010(4) -0.013(4) 0.006(4) C12 0.050(6) 0.037(5) 0.057(6) -0.018(5) -0.009(5) 0.000(4) C13 0.051(6) 0.031(4) 0.038(4) -0.011(4) -0.002(4) -0.014(4) C14 0.047(6) 0.050(6) 0.063(7) -0.023(5) 0.000(5) -0.017(5) C15 0.040(6) 0.068(7) 0.072(8) -0.029(6) 0.009(5) -0.019(6) C16 0.036(6) 0.066(7) 0.063(7) -0.020(6) -0.001(5) -0.017(5) C17 0.039(6) 0.049(6) 0.059(6) -0.013(5) -0.008(5) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag PB1 N3 2.451(8) . ? PB1 N5 2.508(9) . ? PB1 N6 2.531(9) . ? PB1 N4 2.701(9) . ? PB1 N7 2.721(9) . ? C1 N1 1.104(17) . ? C1 S1 1.709(13) . ? S1 PT1 2.317(3) . ? PT1 S2 2.316(3) 2_756 ? PT1 S2 2.316(3) . ? PT1 S1 2.317(3) 2_756 ? S2 C2 1.657(13) . ? C2 N2 1.148(17) . ? S3 C3 1.632(12) . ? C3 N3 1.127(14) . ? N4 C4 1.343(15) . ? N4 C8 1.345(15) . ? C4 C5 1.366(18) . ? N5 C9 1.257(15) . ? N5 C10 1.449(15) . ? C5 C6 1.39(2) . ? N7 C17 1.285(15) . ? N7 C13 1.378(13) . ? C7 C6 1.39(2) . ? C7 C8 1.420(17) . ? N6 C12 1.279(16) . ? N6 C11 1.494(13) . ? C9 C8 1.465(17) . ? C10 C11 1.478(18) . ? C12 C13 1.469(16) . ? C13 C14 1.366(16) . ? C14 C15 1.375(18) . ? C15 C16 1.39(2) . ? C16 C17 1.430(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 PB1 N5 78.5(3) . . ? N3 PB1 N6 81.9(3) . . ? N5 PB1 N6 66.0(3) . . ? N3 PB1 N4 91.4(3) . . ? N5 PB1 N4 63.8(3) . . ? N6 PB1 N4 129.7(3) . . ? N3 PB1 N7 81.9(3) . . ? N5 PB1 N7 127.0(3) . . ? N6 PB1 N7 62.7(3) . . ? N4 PB1 N7 165.1(3) . . ? N1 C1 S1 174.9(13) . . ? C1 S1 PT1 111.9(4) . . ? S2 PT1 S2 180.0 2_756 . ? S2 PT1 S1 90.42(11) 2_756 2_756 ? S2 PT1 S1 89.58(11) . 2_756 ? S2 PT1 S1 89.58(11) 2_756 . ? S2 PT1 S1 90.42(11) . . ? S1 PT1 S1 180.0 2_756 . ? C2 S2 PT1 109.5(4) . . ? N2 C2 S2 176.2(13) . . ? N3 C3 S3 178.3(10) . . ? C3 N3 PB1 129.2(8) . . ? C4 N4 C8 118.4(10) . . ? C4 N4 PB1 126.8(8) . . ? C8 N4 PB1 113.7(7) . . ? N4 C4 C5 121.7(13) . . ? C9 N5 C10 120.1(10) . . ? C9 N5 PB1 121.6(8) . . ? C10 N5 PB1 118.3(8) . . ? C4 C5 C6 122.7(14) . . ? C17 N7 C13 117.7(10) . . ? C17 N7 PB1 125.2(8) . . ? C13 N7 PB1 116.9(7) . . ? C6 C7 C8 120.1(14) . . ? C12 N6 C11 120.4(9) . . ? C12 N6 PB1 123.2(7) . . ? C11 N6 PB1 116.5(7) . . ? C7 C6 C5 115.3(13) . . ? N5 C9 C8 121.9(10) . . ? N4 C8 C7 121.6(12) . . ? N4 C8 C9 117.6(10) . . ? C7 C8 C9 120.7(11) . . ? N5 C10 C11 112.0(10) . . ? C10 C11 N6 109.2(9) . . ? N6 C12 C13 122.3(10) . . ? C14 C13 N7 123.0(11) . . ? C14 C13 C12 122.2(10) . . ? N7 C13 C12 114.8(10) . . ? C13 C14 C15 119.4(12) . . ? C14 C15 C16 118.4(13) . . ? C15 C16 C17 118.3(12) . . ? N7 C17 C16 123.1(12) . . ?