#============================================================================= 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 'Savard, Didier' ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; 'Storr, Tim' ; Department of Chemistry Simon Fraser University Burnaby, British Columbia Canada V5A 1S6 ; '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. # ShelXle # C. B. Hubschle, G. M. Sheldrick, B. Dittrich, J. Appl. Cryst., 44, (2011) 1281-1284. # Extinction correction # Larson, A.C. (1970), Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294 # 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_C26H22Cu2N6O4S2 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C26 H22 Cu2 N6 O4 S2' _chemical_formula_moiety 'C26 H22 Cu2 N6 O4 S2' _chemical_compound_source ? _chemical_formula_weight 673.72 #============================================================= # 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 8.1759(2) _cell_length_b 9.4443(2) _cell_length_c 9.5483(2) _cell_angle_alpha 69.3570(10) _cell_angle_beta 71.4920(10) _cell_angle_gamma 79.6760(10) _cell_volume 652.37(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1420 _cell_measurement_theta_min 5.59 _cell_measurement_theta_max 25.25 _exptl_crystal_description 'Plate' _exptl_crystal_colour 'purple' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.21 _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 342 _exptl_absorpt_coefficient_mu 1.837 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.6750 _exptl_absorpt_correction_T_max 0.7473 _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' #============================================================================= # 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 20762 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_theta_min 2.311 _diffrn_reflns_theta_max 37.305 _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 30.217 _diffrn_measured_fraction_theta_full 0.967 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #========================================================================== # 8. REFINEMENT DATA _reflns_number_total 6468 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -14 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _refine_diff_density_min -0.38 _refine_diff_density_max 0.45 _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 4147 _refine_ls_number_restraints 0 _refine_ls_number_parameters 182 _oxford_refine_ls_R_factor_ref 0.0368 _refine_ls_wR_factor_ref 0.0340 _refine_ls_goodness_of_fit_ref 1.0534 _refine_ls_shift/su_max 0.0013350 _refine_ls_shift/su_mean 0.0000268 # The values computed from all data _oxford_reflns_number_all 6468 _refine_ls_R_factor_all 0.0775 _refine_ls_wR_factor_all 0.0615 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4147 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_gt 0.0340 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # 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: 0.294 0.307 0.229 0.106 0.402E-01 ; #========================================================== # 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 'USER DEFINED DATA RENDERING' #=================================================================== # 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 Cu1 Cu 1.07901(3) 0.34470(2) 0.04635(2) 0.0267 1.0000 Uani . . . . . . S1 S 1.47145(7) 0.36663(6) 0.34202(6) 0.0432 1.0000 Uani . . . . . . N1 N 1.2589(2) 0.3721(2) 0.1626(2) 0.0488 1.0000 Uani . . . . . . N2 N 1.24659(18) 0.20664(14) -0.06761(16) 0.0279 1.0000 Uani . . . . . . N3 N 0.99832(18) 0.14160(15) 0.19838(17) 0.0296 1.0000 Uani . . . . . . C1 C 1.3464(2) 0.37141(19) 0.2361(2) 0.0327 1.0000 Uani . . . . . . C2 C 1.3743(2) 0.2434(2) -0.1977(2) 0.0352 1.0000 Uani . . . . . . C3 C 1.4816(3) 0.1341(2) -0.2592(2) 0.0418 1.0000 Uani . . . . . . C4 C 1.4535(3) -0.0161(2) -0.1860(2) 0.0419 1.0000 Uani . . . . . . C5 C 1.3183(2) -0.05898(18) -0.0481(2) 0.0324 1.0000 Uani . . . . . . C6 C 1.2782(3) -0.21382(19) 0.0403(2) 0.0397 1.0000 Uani . . . . . . C7 C 1.1506(3) -0.24697(19) 0.1753(2) 0.0385 1.0000 Uani . . . . . . C8 C 1.0512(2) -0.12923(18) 0.2359(2) 0.0320 1.0000 Uani . . . . . . C9 C 1.0855(2) 0.02222(16) 0.15036(19) 0.0266 1.0000 Uani . . . . . . C10 C 1.2194(2) 0.05767(17) 0.00712(19) 0.0269 1.0000 Uani . . . . . . C11 C 0.9207(3) -0.1565(2) 0.3773(2) 0.0419 1.0000 Uani . . . . . . C12 C 0.8336(3) -0.0360(2) 0.4243(3) 0.0486 1.0000 Uani . . . . . . C13 C 0.8769(3) 0.1120(2) 0.3325(2) 0.0404 1.0000 Uani . . . . . . O1 O 0.88015(15) 0.46921(12) 0.13123(14) 0.0305 1.0000 Uani . . . . . . O2 O 0.8339(4) 0.4212(3) 0.4539(3) 0.1037 1.0000 Uani . . . . . . H21 H 1.3931 0.3476 -0.2510 0.059(2) 1.0000 Uiso R . . . . . H31 H 1.5740 0.1640 -0.3512 0.067(2) 1.0000 Uiso R . . . . . H41 H 1.5244 -0.0911 -0.2278 0.067(2) 1.0000 Uiso R . . . . . H61 H 1.3427 -0.2936 0.0027 0.064(2) 1.0000 Uiso R . . . . . H71 H 1.1262 -0.3497 0.2313 0.062(2) 1.0000 Uiso R . . . . . H111 H 0.8937 -0.2574 0.4397 0.067(2) 1.0000 Uiso R . . . . . H121 H 0.7436 -0.0525 0.5191 0.074(2) 1.0000 Uiso R . . . . . H131 H 0.8166 0.1942 0.3679 0.065(2) 1.0000 Uiso R . . . . . H11 H 0.7827 0.4315 0.1526 0.067(2) 1.0000 Uiso R . . . . . H221 H 0.7298 0.4831 0.4942 0.067(2) 1.0000 Uiso . . . . . . H222 H 0.8396 0.4582 0.3459 0.051(2) 1.0000 Uiso . . . . . . 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 Cu1 0.02836(9) 0.01809(8) 0.02996(10) -0.00796(6) -0.00541(7) 0.00284(6) S1 0.0396(2) 0.0481(3) 0.0447(3) -0.0132(2) -0.0152(2) -0.0064(2) N1 0.0469(10) 0.0468(10) 0.0631(12) -0.0264(9) -0.0240(9) 0.0053(8) N2 0.0317(6) 0.0209(5) 0.0292(6) -0.0086(5) -0.0064(5) 0.0009(5) N3 0.0300(6) 0.0226(5) 0.0326(7) -0.0091(5) -0.0054(5) 0.0013(5) C1 0.0312(8) 0.0254(7) 0.0397(9) -0.0122(6) -0.0065(7) -0.0002(6) C2 0.0382(9) 0.0267(7) 0.0340(8) -0.0080(6) -0.0041(7) -0.0002(6) C3 0.0469(10) 0.0359(9) 0.0327(9) -0.0116(7) -0.0003(7) 0.0029(8) C4 0.0514(11) 0.0313(8) 0.0377(9) -0.0167(7) -0.0048(8) 0.0084(8) C5 0.0413(9) 0.0236(6) 0.0319(8) -0.0121(6) -0.0098(7) 0.0046(6) C6 0.0532(11) 0.0219(7) 0.0426(10) -0.0140(7) -0.0112(8) 0.0042(7) C7 0.0464(10) 0.0203(6) 0.0471(10) -0.0093(7) -0.0141(8) 0.0007(6) C8 0.0332(8) 0.0223(6) 0.0383(9) -0.0071(6) -0.0102(7) -0.0015(6) C9 0.0274(7) 0.0202(6) 0.0319(7) -0.0082(5) -0.0092(6) 0.0005(5) C10 0.0317(7) 0.0197(5) 0.0298(7) -0.0092(5) -0.0102(6) 0.0024(5) C11 0.0419(10) 0.0269(7) 0.0449(10) -0.0039(7) -0.0024(8) -0.0058(7) C12 0.0451(11) 0.0351(9) 0.0455(11) -0.0068(8) 0.0081(9) -0.0033(8) C13 0.0393(9) 0.0305(8) 0.0404(10) -0.0117(7) 0.0016(7) 0.0024(7) O1 0.0288(5) 0.0209(5) 0.0344(6) -0.0069(4) -0.0032(5) 0.0020(4) O2 0.145(2) 0.1045(19) 0.0670(14) -0.0472(13) -0.0543(15) 0.0633(17) 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 Cu1 . Cu1 2_765 2.9315(4) yes Cu1 . O1 2_765 1.9558(11) yes Cu1 . N1 . 2.1995(19) yes Cu1 . N2 . 2.0433(13) yes Cu1 . N3 . 2.0259(14) yes Cu1 . O1 . 1.9578(11) yes S1 . C1 . 1.636(2) yes N1 . C1 . 1.148(3) yes N2 . C2 . 1.325(2) yes N2 . C10 . 1.357(2) yes N3 . C9 . 1.363(2) yes N3 . C13 . 1.321(2) yes C2 . C3 . 1.399(3) yes C2 . H21 . 0.950 no C3 . C4 . 1.367(3) yes C3 . H31 . 0.950 no C4 . C5 . 1.407(3) yes C4 . H41 . 0.950 no C5 . C6 . 1.444(2) yes C5 . C10 . 1.401(2) yes C6 . C7 . 1.352(3) yes C6 . H61 . 0.950 no C7 . C8 . 1.436(3) yes C7 . H71 . 0.950 no C8 . C9 . 1.402(2) yes C8 . C11 . 1.403(3) yes C9 . C10 . 1.428(2) yes C11 . C12 . 1.368(3) yes C11 . H111 . 0.950 no C12 . C13 . 1.401(3) yes C12 . H121 . 0.950 no C13 . H131 . 0.950 no O1 . H11 . 0.866 no O2 . H221 . 0.993 no O2 . H222 . 0.953 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 Cu1 2_765 Cu1 . O1 2_765 41.52(3) yes Cu1 2_765 Cu1 . N1 . 100.84(5) yes O1 2_765 Cu1 . N1 . 98.00(7) yes Cu1 2_765 Cu1 . N2 . 135.43(4) yes O1 2_765 Cu1 . N2 . 95.50(5) yes N1 . Cu1 . N2 . 95.67(6) yes Cu1 2_765 Cu1 . N3 . 136.00(4) yes O1 2_765 Cu1 . N3 . 164.63(6) yes N1 . Cu1 . N3 . 97.28(7) yes N2 . Cu1 . N3 . 81.26(5) yes Cu1 2_765 Cu1 . O1 . 41.46(3) yes O1 2_765 Cu1 . O1 . 82.98(5) yes N1 . Cu1 . O1 . 98.20(6) yes N2 . Cu1 . O1 . 166.12(5) yes N3 . Cu1 . O1 . 96.54(5) yes Cu1 . N1 . C1 . 172.24(18) yes Cu1 . N2 . C2 . 129.09(11) yes Cu1 . N2 . C10 . 112.45(11) yes C2 . N2 . C10 . 118.45(14) yes Cu1 . N3 . C9 . 112.85(11) yes Cu1 . N3 . C13 . 129.18(12) yes C9 . N3 . C13 . 117.97(15) yes S1 . C1 . N1 . 178.81(17) yes N2 . C2 . C3 . 122.19(17) yes N2 . C2 . H21 . 118.7 no C3 . C2 . H21 . 119.1 no C2 . C3 . C4 . 119.75(18) yes C2 . C3 . H31 . 120.2 no C4 . C3 . H31 . 120.1 no C3 . C4 . C5 . 119.50(16) yes C3 . C4 . H41 . 120.4 no C5 . C4 . H41 . 120.1 no C4 . C5 . C6 . 124.36(16) yes C4 . C5 . C10 . 116.97(16) yes C6 . C5 . C10 . 118.65(16) yes C5 . C6 . C7 . 121.09(16) yes C5 . C6 . H61 . 119.4 no C7 . C6 . H61 . 119.5 no C6 . C7 . C8 . 121.02(16) yes C6 . C7 . H71 . 119.7 no C8 . C7 . H71 . 119.3 no C7 . C8 . C9 . 118.85(17) yes C7 . C8 . C11 . 123.75(16) yes C9 . C8 . C11 . 117.39(16) yes C8 . C9 . N3 . 123.12(16) yes C8 . C9 . C10 . 120.24(14) yes N3 . C9 . C10 . 116.63(14) yes C9 . C10 . C5 . 120.11(14) yes C9 . C10 . N2 . 116.76(13) yes C5 . C10 . N2 . 123.11(16) yes C8 . C11 . C12 . 119.06(17) yes C8 . C11 . H111 . 120.3 no C12 . C11 . H111 . 120.6 no C11 . C12 . C13 . 119.95(19) yes C11 . C12 . H121 . 120.1 no C13 . C12 . H121 . 119.9 no C12 . C13 . N3 . 122.48(17) yes C12 . C13 . H131 . 118.9 no N3 . C13 . H131 . 118.6 no Cu1 . O1 . Cu1 2_765 97.02(5) yes Cu1 . O1 . H11 . 112.5 no Cu1 2_765 O1 . H11 . 115.2 no H221 . O2 . H222 . 99.8 no data_C22H18Cu2N6O3S2 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C22 H18 Cu2 N6 O3 S2' _chemical_formula_moiety 'C22 H18 Cu2 N6 O3 S2' _chemical_compound_source ? _chemical_formula_weight 605.64 #============================================================= # 6. CRYSTAL DATA _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1569(9) _cell_length_b 9.6888(10) _cell_length_c 16.5639(16) _cell_angle_alpha 75.686(4) _cell_angle_beta 83.677(4) _cell_angle_gamma 73.445(4) _cell_volume 1214.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9583 _cell_measurement_theta_min 4.89 _cell_measurement_theta_max 71.65 _exptl_crystal_description 'Plate' _exptl_crystal_colour 'green' _exptl_crystal_size_min 0.13 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.31 _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 4.086 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.4206 _exptl_absorpt_correction_T_max 0.7535 _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device_type 'Unknown' _diffrn_measurement_device 'Serial' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 296(2) _diffrn_reflns_number 11949 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_theta_min 4.889 _diffrn_reflns_theta_max 71.647 _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_full 0.950 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 #========================================================================== # 8. REFINEMENT DATA _reflns_number_total 4325 _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 4325 _refine_ls_number_parameters 322 _refine_ls_number_restraints 95 _refine_ls_wR_factor_ref 0.1733 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 # The values computed from all data _refine_ls_R_factor_all 0.0546 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4002 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_gt 0.1708 _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^)+(0.0936P)^2^+1.7140P] where P=(Fo^2^+2Fc^2^)/3' _refine_diff_density_max 1.627 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.155 #========================================================== # 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 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_publication_material 'SHELXle (Hubschle et al. 2011)' _computing_molecular_graphics 'USER DEFINED DATA RENDERING' #=================================================================== # 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 Cu1 Cu 0.43370(8) 0.45662(7) 0.58539(3) 0.0374(2) Uani 1 1 d . U . . . C1 C 0.1542(6) 0.2761(6) 0.5552(3) 0.0476(10) Uani 1 1 d . U . . . N1 N 0.2336(6) 0.3513(5) 0.5620(3) 0.0591(11) Uani 1 1 d . U . . . O1 O 0.6100(4) 0.3735(4) 0.50923(18) 0.0445(7) Uani 1 1 d . U . . . H1 H 0.5971 0.2950 0.5044 0.28(8) Uiso 1 1 calc DR . . . . S1 S 0.0397(2) 0.1654(2) 0.54787(11) 0.0766(5) Uani 1 1 d . U . . . H2 H 0.693(7) 0.369(7) 0.994(4) 0.044(19) Uiso 1 1 d . . . . . Cu2 Cu 0.55752(7) 0.59302(6) 0.92514(3) 0.0329(2) Uani 1 1 d . U . . . C2 C 0.8380(5) 0.7350(5) 0.9822(2) 0.0403(9) Uani 1 1 d . U . . . N2 N 0.7516(6) 0.6661(6) 0.9718(3) 0.0608(11) Uani 1 1 d . U . . . O2 O 0.6164(5) 0.3890(3) 0.98459(18) 0.0377(7) Uani 1 1 d . U . . . S2 S 0.96031(16) 0.83294(15) 0.99642(9) 0.0552(3) Uani 1 1 d . U . . . N3 N 0.2886(5) 0.5629(4) 0.6696(2) 0.0388(7) Uani 1 1 d . U . . . C3 C 0.1735(6) 0.6933(6) 0.6510(3) 0.0541(12) Uani 1 1 d . U . . . H3 H 0.1600 0.7428 0.5954 0.065 Uiso 1 1 calc R U . . . O3 O 0.6120(8) 0.0757(6) 0.5111(4) 0.1038(18) Uani 1 1 d D . . . . C9 C 0.4938(7) 0.2643(6) 0.8411(3) 0.0513(11) Uani 1 1 d . U . . . H9 H 0.4390 0.2928 0.8890 0.062 Uiso 1 1 calc R U . . . C8 C 0.4449(6) 0.3491(5) 0.7634(2) 0.0390(9) Uani 1 1 d . U . . . C7 C 0.3102(5) 0.4896(5) 0.7503(2) 0.0377(8) Uani 1 1 d . U . . . N6 N 0.6828(4) 0.5612(4) 0.8153(2) 0.0354(7) Uani 1 1 d . U . . . C6 C 0.2115(6) 0.5495(6) 0.8135(3) 0.0500(11) Uani 1 1 d . U . . . H6 H 0.2257 0.4987 0.8689 0.060 Uiso 1 1 calc R U . . . N5 N 0.4482(4) 0.7855(4) 0.8500(2) 0.0361(7) Uani 1 1 d . U . . . C5 C 0.0928(7) 0.6841(7) 0.7937(3) 0.0633(14) Uani 1 1 d . U . . . H5 H 0.0260 0.7252 0.8355 0.076 Uiso 1 1 calc R U . . . N4 N 0.5224(5) 0.3114(4) 0.6925(2) 0.0421(8) Uani 1 1 d . U . . . C4 C 0.0735(7) 0.7574(6) 0.7117(4) 0.0648(14) Uani 1 1 d . U . . . H4 H -0.0058 0.8489 0.6972 0.078 Uiso 1 1 calc R U . . . C10 C 0.6254(8) 0.1365(6) 0.8468(3) 0.0666(14) Uani 1 1 d . U . . . H10 H 0.6603 0.0771 0.8986 0.080 Uiso 1 1 calc R U . . . C11 C 0.7040(8) 0.0983(7) 0.7747(4) 0.0712(16) Uani 1 1 d . U . . . H11 H 0.7940 0.0131 0.7772 0.085 Uiso 1 1 calc R U . . . C12 C 0.6484(7) 0.1872(6) 0.6987(3) 0.0581(12) Uani 1 1 d . U . . . H12 H 0.7005 0.1596 0.6502 0.070 Uiso 1 1 calc R U . . . C13 C 0.3314(6) 0.8976(5) 0.8745(3) 0.0457(10) Uani 1 1 d . U . . . H13 H 0.3019 0.8887 0.9310 0.055 Uiso 1 1 calc R U . . . C14 C 0.2534(7) 1.0254(6) 0.8193(3) 0.0587(13) Uani 1 1 d . U . . . H14 H 0.1714 1.1009 0.8379 0.070 Uiso 1 1 calc R U . . . C15 C 0.2996(8) 1.0387(6) 0.7362(3) 0.0671(15) Uani 1 1 d . U . . . H15 H 0.2494 1.1242 0.6976 0.080 Uiso 1 1 calc R U . . . C16 C 0.4207(7) 0.9249(6) 0.7100(3) 0.0567(12) Uani 1 1 d . U . . . H16 H 0.4530 0.9335 0.6537 0.068 Uiso 1 1 calc R U . . . C17 C 0.4939(6) 0.7980(5) 0.7677(2) 0.0398(9) Uani 1 1 d . U . . . C18 C 0.6274(6) 0.6703(5) 0.7482(2) 0.0394(9) Uani 1 1 d . U . . . C19 C 0.6942(7) 0.6596(6) 0.6682(3) 0.0544(12) Uani 1 1 d . U . . . H19 H 0.6527 0.7347 0.6223 0.065 Uiso 1 1 calc R U . . . C20 C 0.8221(7) 0.5367(7) 0.6581(3) 0.0630(14) Uani 1 1 d . U . . . H20 H 0.8685 0.5279 0.6052 0.076 Uiso 1 1 calc R U . . . C21 C 0.8810(7) 0.4270(6) 0.7268(3) 0.0582(12) Uani 1 1 d . U . . . H21 H 0.9686 0.3437 0.7209 0.070 Uiso 1 1 calc R U . . . C22 C 0.8089(6) 0.4415(5) 0.8045(3) 0.0465(10) Uani 1 1 d . U . . . H22 H 0.8483 0.3666 0.8508 0.056 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 Cu1 0.0441(4) 0.0404(4) 0.0255(3) -0.0088(2) 0.0061(2) -0.0094(3) C1 0.044(3) 0.060(3) 0.034(2) -0.0036(19) -0.0040(18) -0.012(2) N1 0.069(3) 0.067(3) 0.048(2) -0.0096(19) -0.0042(19) -0.030(2) O1 0.0559(19) 0.0441(17) 0.0318(14) -0.0099(12) 0.0114(13) -0.0145(14) S1 0.0721(10) 0.0842(11) 0.0825(10) -0.0058(8) -0.0194(8) -0.0402(9) Cu2 0.0380(4) 0.0335(3) 0.0247(3) -0.0005(2) 0.0010(2) -0.0118(2) C2 0.039(2) 0.051(2) 0.0315(19) -0.0102(17) 0.0021(16) -0.0131(18) N2 0.062(3) 0.084(3) 0.051(2) -0.016(2) -0.0028(19) -0.042(2) O2 0.040(2) 0.0350(15) 0.0318(14) 0.0007(11) 0.0019(13) -0.0087(13) S2 0.0501(7) 0.0548(7) 0.0701(8) -0.0221(6) -0.0040(6) -0.0211(5) N3 0.0439(19) 0.0410(18) 0.0304(16) -0.0114(13) 0.0047(13) -0.0090(14) C3 0.055(3) 0.054(3) 0.043(2) -0.010(2) 0.004(2) 0.000(2) O3 0.129(4) 0.081(3) 0.118(4) -0.048(3) 0.026(4) -0.044(3) C9 0.069(3) 0.051(3) 0.035(2) -0.0086(18) -0.003(2) -0.018(2) C8 0.048(2) 0.044(2) 0.0313(18) -0.0113(16) 0.0019(16) -0.0206(18) C7 0.042(2) 0.047(2) 0.0295(18) -0.0141(16) 0.0044(15) -0.0175(17) N6 0.0387(18) 0.0348(17) 0.0297(15) -0.0013(12) -0.0010(13) -0.0107(13) C6 0.061(3) 0.058(3) 0.035(2) -0.0191(19) 0.0092(19) -0.020(2) N5 0.0429(19) 0.0327(16) 0.0305(16) -0.0012(12) 0.0006(13) -0.0127(14) C5 0.066(3) 0.070(3) 0.054(3) -0.031(3) 0.021(2) -0.012(3) N4 0.049(2) 0.0435(19) 0.0337(17) -0.0116(14) 0.0018(14) -0.0108(15) C4 0.064(3) 0.056(3) 0.061(3) -0.020(2) 0.009(3) 0.005(2) C10 0.087(4) 0.058(3) 0.049(3) -0.001(2) -0.018(3) -0.011(3) C11 0.073(4) 0.057(3) 0.067(3) -0.012(3) -0.014(3) 0.010(3) C12 0.064(3) 0.051(3) 0.051(3) -0.015(2) 0.000(2) 0.001(2) C13 0.057(3) 0.038(2) 0.038(2) -0.0039(17) 0.0044(18) -0.0133(19) C14 0.068(3) 0.042(3) 0.054(3) -0.004(2) 0.001(2) -0.003(2) C15 0.085(4) 0.048(3) 0.048(3) 0.008(2) -0.014(3) 0.002(3) C16 0.075(3) 0.054(3) 0.032(2) 0.0035(18) -0.003(2) -0.013(2) C17 0.047(2) 0.043(2) 0.0301(18) -0.0018(15) -0.0010(16) -0.0185(18) C18 0.042(2) 0.047(2) 0.0283(18) -0.0024(16) 0.0013(15) -0.0177(17) C19 0.062(3) 0.066(3) 0.029(2) -0.0019(19) 0.0062(19) -0.016(2) C20 0.069(3) 0.078(4) 0.034(2) -0.011(2) 0.013(2) -0.014(3) C21 0.056(3) 0.062(3) 0.047(3) -0.013(2) 0.009(2) -0.005(2) C22 0.047(3) 0.043(2) 0.040(2) -0.0036(17) 0.0009(18) -0.0044(18) 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 Cu1 O1 1.937(3) . ? Cu1 O1 1.951(3) 2_666 ? Cu1 N3 2.015(3) . ? Cu1 N4 2.030(4) . ? Cu1 N1 2.267(4) . ? Cu1 Cu1 2.9235(11) 2_666 ? C1 N1 1.135(6) . ? C1 S1 1.642(5) . ? O1 Cu1 1.951(3) 2_666 ? Cu2 O2 1.925(3) . ? Cu2 O2 1.949(3) 2_667 ? Cu2 N5 1.993(3) . ? Cu2 N6 2.035(3) . ? Cu2 N2 2.187(4) . ? Cu2 Cu2 2.9190(10) 2_667 ? C2 N2 1.151(6) . ? C2 S2 1.629(4) . ? O2 Cu2 1.949(3) 2_667 ? N3 C3 1.330(6) . ? N3 C7 1.354(5) . ? C3 C4 1.378(7) . ? C9 C8 1.377(6) . ? C9 C10 1.379(8) . ? C8 N4 1.352(5) . ? C8 C7 1.470(6) . ? C7 C6 1.388(6) . ? N6 C18 1.347(5) . ? N6 C22 1.347(6) . ? C6 C5 1.373(8) . ? N5 C13 1.339(6) . ? N5 C17 1.358(5) . ? C5 C4 1.372(8) . ? N4 C12 1.331(6) . ? C10 C11 1.375(8) . ? C11 C12 1.378(8) . ? C13 C14 1.376(7) . ? C14 C15 1.371(8) . ? C15 C16 1.379(8) . ? C16 C17 1.382(6) . ? C17 C18 1.474(6) . ? C18 C19 1.392(6) . ? C19 C20 1.374(8) . ? C20 C21 1.374(8) . ? C21 C22 1.377(7) . ? 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 O1 Cu1 O1 82.48(15) . 2_666 ? O1 Cu1 N3 167.61(15) . . ? O1 Cu1 N3 95.99(14) 2_666 . ? O1 Cu1 N4 97.92(14) . . ? O1 Cu1 N4 163.66(15) 2_666 . ? N3 Cu1 N4 80.10(14) . . ? O1 Cu1 N1 96.79(16) . . ? O1 Cu1 N1 98.05(15) 2_666 . ? N3 Cu1 N1 95.60(16) . . ? N4 Cu1 N1 98.12(16) . . ? O1 Cu1 Cu1 41.42(10) . 2_666 ? O1 Cu1 Cu1 41.05(9) 2_666 2_666 ? N3 Cu1 Cu1 135.78(11) . 2_666 ? N4 Cu1 Cu1 137.03(11) . 2_666 ? N1 Cu1 Cu1 99.89(11) . 2_666 ? N1 C1 S1 178.5(4) . . ? C1 N1 Cu1 168.1(5) . . ? Cu1 O1 Cu1 97.52(15) . 2_666 ? O2 Cu2 O2 82.23(15) . 2_667 ? O2 Cu2 N5 163.69(15) . . ? O2 Cu2 N5 95.71(14) 2_667 . ? O2 Cu2 N6 97.05(13) . . ? O2 Cu2 N6 162.84(15) 2_667 . ? N5 Cu2 N6 80.14(13) . . ? O2 Cu2 N2 99.10(18) . . ? O2 Cu2 N2 99.99(16) 2_667 . ? N5 Cu2 N2 97.20(17) . . ? N6 Cu2 N2 97.06(15) . . ? O2 Cu2 Cu2 41.42(9) . 2_667 ? O2 Cu2 Cu2 40.81(9) 2_667 2_667 ? N5 Cu2 Cu2 134.39(10) . 2_667 ? N6 Cu2 Cu2 135.97(10) . 2_667 ? N2 Cu2 Cu2 102.72(12) . 2_667 ? N2 C2 S2 179.7(5) . . ? C2 N2 Cu2 163.5(4) . . ? Cu2 O2 Cu2 97.77(15) . 2_667 ? C3 N3 C7 119.8(4) . . ? C3 N3 Cu1 124.9(3) . . ? C7 N3 Cu1 115.3(3) . . ? N3 C3 C4 122.0(5) . . ? C8 C9 C10 118.9(5) . . ? N4 C8 C9 122.1(4) . . ? N4 C8 C7 114.6(4) . . ? C9 C8 C7 123.3(4) . . ? N3 C7 C6 120.2(4) . . ? N3 C7 C8 114.9(3) . . ? C6 C7 C8 124.9(4) . . ? C18 N6 C22 118.9(4) . . ? C18 N6 Cu2 115.0(3) . . ? C22 N6 Cu2 126.1(3) . . ? C5 C6 C7 119.6(5) . . ? C13 N5 C17 119.2(4) . . ? C13 N5 Cu2 125.0(3) . . ? C17 N5 Cu2 115.7(3) . . ? C4 C5 C6 119.4(4) . . ? C12 N4 C8 118.6(4) . . ? C12 N4 Cu1 126.4(3) . . ? C8 N4 Cu1 115.0(3) . . ? C5 C4 C3 119.0(5) . . ? C11 C10 C9 119.0(5) . . ? C10 C11 C12 119.4(5) . . ? N4 C12 C11 122.1(5) . . ? N5 C13 C14 122.6(4) . . ? C15 C14 C13 118.3(5) . . ? C14 C15 C16 119.8(5) . . ? C15 C16 C17 119.7(4) . . ? N5 C17 C16 120.3(4) . . ? N5 C17 C18 114.6(4) . . ? C16 C17 C18 125.0(4) . . ? N6 C18 C19 121.3(4) . . ? N6 C18 C17 114.3(3) . . ? C19 C18 C17 124.4(4) . . ? C20 C19 C18 119.1(4) . . ? C21 C20 C19 119.5(4) . . ? C20 C21 C22 119.2(5) . . ? N6 C22 C21 121.9(4) . . ? data_C28H22Au2Cu2N12O4 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C28 H22 Au2 Cu2 N12 O4' _chemical_formula_moiety 'C28 H22 Au2 Cu2 N12 O4' _chemical_compound_source ? _chemical_formula_weight 1111.62 #============================================================= # 6. CRYSTAL DATA _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.22600(10) _cell_length_b 10.13900(10) _cell_length_c 11.4550(2) _cell_angle_alpha 105.9710(8) _cell_angle_beta 107.1760(8) _cell_angle_gamma 102.4360(8) _cell_volume 830.53(2) _cell_formula_units_Z 1 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 9873 _cell_measurement_theta_min 3.40 _cell_measurement_theta_max 37.32 _exptl_crystal_description 'Block' _exptl_crystal_colour 'blue' _exptl_crystal_size_min 0.28 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_max 0.32 _exptl_crystal_density_diffrn 2.222 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 522 _exptl_absorpt_coefficient_mu 10.121 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.3118 _exptl_absorpt_correction_T_max 0.7474 _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' #============================================================================= # 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 299(2) _diffrn_reflns_number 15717 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_theta_min 1.997 _diffrn_reflns_theta_max 26.372 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 #========================================================================== # 8. REFINEMENT DATA _reflns_number_total 3398 _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 3398 _refine_ls_number_parameters 229 _refine_ls_number_restraints 62 _refine_ls_wR_factor_ref 0.0471 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 # The values computed from all data _refine_ls_R_factor_all 0.0206 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3281 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_gt 0.0467 _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^)+(0.0246P)^2^+0.1383P] where P=(Fo^2^+2Fc^2^)/3' _refine_diff_density_max 0.666 _refine_diff_density_min -1.503 _refine_diff_density_rms 0.185 #========================================================== # 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 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_publication_material 'SHELXle (Hubschle et al. 2011)' _computing_molecular_graphics 'USER DEFINED DATA RENDERING' #=================================================================== # 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 Au1 Au 0.71927(2) 0.22230(2) 0.14478(2) 0.03458(6) Uani 1 1 d . U . . . Cu1 Cu 0.09749(5) 0.59660(4) 0.44748(3) 0.03423(9) Uani 1 1 d . U . . . O1 O -0.1419(3) 0.4939(3) 0.4245(3) 0.0455(5) Uani 1 1 d D U . . . N1 N 0.8435(5) 0.0977(5) 0.3658(4) 0.0622(9) Uani 1 1 d . U . . . C1 C 0.7950(5) 0.1392(4) 0.2836(4) 0.0445(7) Uani 1 1 d . U . . . H1 H -0.240(3) 0.495(5) 0.377(4) 0.09(2) Uiso 1 1 d D . . . . O2 O 0.4996(3) 0.4831(3) 0.2388(3) 0.0549(6) Uani 1 1 d D . . . . N2 N 0.3122(5) 0.0683(4) 0.0799(4) 0.0583(8) Uani 1 1 d . U . . . C2 C 0.4608(5) 0.1267(4) 0.1063(3) 0.0416(7) Uani 1 1 d . U . . . H2 H 0.395(3) 0.434(4) 0.223(5) 0.080(16) Uiso 1 1 d D . . . . N3 N 0.6005(5) 0.3542(5) -0.0696(4) 0.0649(9) Uani 1 1 d . U . . . C3 C 0.6466(5) 0.3079(4) 0.0079(4) 0.0441(7) Uani 1 1 d . U . . . H3 H 0.490(6) 0.537(5) 0.196(5) 0.094(18) Uiso 1 1 d D . . . . N4 N 1.1253(5) 0.3718(4) 0.2101(4) 0.0663(9) Uani 1 1 d . U . . . C4 C 0.9773(5) 0.3172(4) 0.1833(4) 0.0455(7) Uani 1 1 d . U . . . N5 N 0.3481(4) 0.6948(3) 0.4715(3) 0.0352(5) Uani 1 1 d . U . . . C5 C 0.4994(5) 0.6918(4) 0.5543(3) 0.0458(7) Uani 1 1 d . U . . . H5 H 0.4906 0.6371 0.6068 0.055 Uiso 1 1 calc R U . . . N6 N 0.0429(4) 0.6906(3) 0.3166(3) 0.0367(5) Uani 1 1 d . U . . . C6 C 0.6679(5) 0.7661(4) 0.5654(4) 0.0507(8) Uani 1 1 d . U . . . H6 H 0.7705 0.7629 0.6252 0.061 Uiso 1 1 calc R U . . . C7 C 0.6819(5) 0.8451(4) 0.4867(4) 0.0464(7) Uani 1 1 d . U . . . H7 H 0.7941 0.8950 0.4914 0.056 Uiso 1 1 calc R U . . . C8 C 0.5272(4) 0.8490(4) 0.4007(3) 0.0407(7) Uani 1 1 d . U . . . H8 H 0.5338 0.9023 0.3469 0.049 Uiso 1 1 calc R U . . . C9 C 0.3612(4) 0.7727(3) 0.3947(3) 0.0314(5) Uani 1 1 d . U . . . C10 C 0.1877(4) 0.7709(3) 0.3076(3) 0.0321(6) Uani 1 1 d . U . . . C11 C 0.1716(5) 0.8466(4) 0.2230(3) 0.0422(7) Uani 1 1 d . U . . . H11 H 0.2739 0.9032 0.2194 0.051 Uiso 1 1 calc R U . . . C12 C 0.0035(5) 0.8376(4) 0.1445(4) 0.0506(8) Uani 1 1 d . U . . . H12 H -0.0096 0.8873 0.0869 0.061 Uiso 1 1 calc R U . . . C13 C -0.1439(5) 0.7538(5) 0.1529(4) 0.0592(10) Uani 1 1 d . U . . . H13 H -0.2591 0.7455 0.1009 0.071 Uiso 1 1 calc R U . . . C14 C -0.1196(5) 0.6819(5) 0.2394(4) 0.0546(9) Uani 1 1 d D U . . . H14 H -0.2206 0.6249 0.2442 0.065 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 Au1 0.03320(8) 0.03653(8) 0.03582(8) 0.01709(5) 0.01376(5) 0.00858(5) Cu1 0.03084(18) 0.03948(18) 0.04188(19) 0.02668(15) 0.01797(14) 0.00809(14) O1 0.0323(12) 0.0601(14) 0.0594(14) 0.0441(12) 0.0199(10) 0.0116(10) N1 0.063(2) 0.076(2) 0.060(2) 0.0439(18) 0.0231(17) 0.0218(18) C1 0.0441(18) 0.0464(17) 0.0459(18) 0.0214(14) 0.0191(14) 0.0112(14) O2 0.0354(13) 0.0716(16) 0.0705(16) 0.0498(14) 0.0183(11) 0.0129(12) N2 0.0431(18) 0.0621(19) 0.072(2) 0.0345(17) 0.0225(16) 0.0075(15) C2 0.0445(18) 0.0388(15) 0.0432(17) 0.0197(13) 0.0168(14) 0.0103(14) N3 0.058(2) 0.090(3) 0.070(2) 0.055(2) 0.0266(17) 0.0295(19) C3 0.0389(17) 0.0526(18) 0.0492(18) 0.0272(15) 0.0200(14) 0.0148(15) N4 0.0373(17) 0.081(2) 0.082(2) 0.042(2) 0.0201(16) 0.0087(17) C4 0.0408(18) 0.0507(18) 0.0472(18) 0.0256(15) 0.0159(14) 0.0098(15) N5 0.0334(13) 0.0397(12) 0.0388(13) 0.0222(11) 0.0168(10) 0.0093(10) C5 0.0408(17) 0.0576(19) 0.0480(18) 0.0354(16) 0.0147(14) 0.0149(15) N6 0.0317(13) 0.0406(13) 0.0446(14) 0.0253(11) 0.0173(11) 0.0078(10) C6 0.0343(17) 0.065(2) 0.056(2) 0.0322(17) 0.0127(14) 0.0139(15) C7 0.0308(15) 0.0543(18) 0.0545(19) 0.0256(16) 0.0168(14) 0.0060(14) C8 0.0359(16) 0.0461(16) 0.0468(17) 0.0273(14) 0.0186(13) 0.0081(13) C9 0.0325(14) 0.0319(12) 0.0374(14) 0.0182(11) 0.0193(12) 0.0092(11) C10 0.0327(14) 0.0341(13) 0.0346(14) 0.0173(11) 0.0166(11) 0.0085(11) C11 0.0406(17) 0.0485(17) 0.0492(17) 0.0318(15) 0.0210(14) 0.0128(14) C12 0.049(2) 0.063(2) 0.057(2) 0.0411(18) 0.0216(16) 0.0215(17) C13 0.0364(18) 0.081(3) 0.069(2) 0.050(2) 0.0121(16) 0.0167(17) C14 0.0292(16) 0.073(2) 0.071(2) 0.047(2) 0.0164(15) 0.0100(16) 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 Au1 C4 1.990(4) . ? Au1 C2 1.994(4) . ? Au1 C3 1.997(4) . ? Au1 C1 2.001(4) . ? Cu1 O1 1.921(2) . ? Cu1 O1 1.922(2) 2_566 ? Cu1 N6 1.983(3) . ? Cu1 N5 1.987(3) . ? Cu1 Cu1 2.9901(7) 2_566 ? O1 Cu1 1.922(2) 2_566 ? N1 C1 1.136(5) . ? N2 C2 1.144(5) . ? N3 C3 1.122(5) . ? N4 C4 1.131(5) . ? N5 C5 1.336(4) . ? N5 C9 1.346(4) . ? C5 C6 1.378(5) . ? N6 C14 1.336(4) . ? N6 C10 1.340(4) . ? C6 C7 1.373(5) . ? C7 C8 1.377(5) . ? C8 C9 1.389(4) . ? C9 C10 1.473(5) . ? C10 C11 1.386(4) . ? C11 C12 1.377(5) . ? C12 C13 1.368(6) . ? C13 C14 1.376(5) . ? 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 C4 Au1 C2 179.85(12) . . ? C4 Au1 C3 90.39(15) . . ? C2 Au1 C3 89.73(14) . . ? C4 Au1 C1 88.98(15) . . ? C2 Au1 C1 90.90(15) . . ? C3 Au1 C1 179.17(13) . . ? O1 Cu1 O1 77.85(11) . 2_566 ? O1 Cu1 N6 100.24(10) . . ? O1 Cu1 N6 177.74(11) 2_566 . ? O1 Cu1 N5 177.39(10) . . ? O1 Cu1 N5 100.29(10) 2_566 . ? N6 Cu1 N5 81.66(11) . . ? O1 Cu1 Cu1 38.93(7) . 2_566 ? O1 Cu1 Cu1 38.92(7) 2_566 2_566 ? N6 Cu1 Cu1 139.16(8) . 2_566 ? N5 Cu1 Cu1 139.18(8) . 2_566 ? Cu1 O1 Cu1 102.15(11) . 2_566 ? N1 C1 Au1 177.0(4) . . ? N2 C2 Au1 177.4(3) . . ? N3 C3 Au1 177.9(4) . . ? N4 C4 Au1 177.3(4) . . ? C5 N5 C9 118.5(3) . . ? C5 N5 Cu1 127.2(2) . . ? C9 N5 Cu1 114.3(2) . . ? N5 C5 C6 122.8(3) . . ? C14 N6 C10 118.3(3) . . ? C14 N6 Cu1 127.0(2) . . ? C10 N6 Cu1 114.6(2) . . ? C7 C6 C5 118.9(3) . . ? C6 C7 C8 118.9(3) . . ? C7 C8 C9 119.5(3) . . ? N5 C9 C8 121.3(3) . . ? N5 C9 C10 114.7(3) . . ? C8 C9 C10 124.0(3) . . ? N6 C10 C11 121.5(3) . . ? N6 C10 C9 114.7(3) . . ? C11 C10 C9 123.8(3) . . ? C12 C11 C10 119.7(3) . . ? C13 C12 C11 118.6(3) . . ? C12 C13 C14 119.2(3) . . ? N6 C14 C13 122.8(3) . . ? data_C28H18Au2Cu2N12O2 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C28 H18 Au2 Cu2 N12 O2' _chemical_formula_moiety 'C28 H18 Au2 Cu2 N12 O2' _chemical_compound_source ? _chemical_formula_weight 1075.56 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' 'x,-y,z+1/2' '-x,y,-z+1/2' 'x+1/2,-y+1/2,z+1/2' '-x+1/2,y+1/2,-z+1/2' _cell_length_a 22.291(2) _cell_length_b 7.8710(7) _cell_length_c 20.6325(18) _cell_angle_alpha 90 _cell_angle_beta 118.248(4) _cell_angle_gamma 90 _cell_volume 3188.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9872 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 34.18 _exptl_crystal_description 'plate' _exptl_crystal_colour 'purple' _exptl_crystal_size_min 0.030 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_max 0.400 _exptl_crystal_density_diffrn 2.240 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 10.536 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.3725 _exptl_absorpt_correction_T_max 0.7470 _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' #============================================================================= # 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 36888 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_theta_min 2.241 _diffrn_reflns_theta_max 35.363 _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 27.583 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 #========================================================================== # 8. REFINEMENT DATA _reflns_number_total 6548 _reflns_limit_h_min -35 _reflns_limit_h_max 31 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 33 _refine_diff_density_min -0.93 _refine_diff_density_max 1.32 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 4085 _refine_ls_number_restraints 0 _refine_ls_number_parameters 201 _oxford_refine_ls_R_factor_ref 0.0301 _refine_ls_wR_factor_ref 0.0273 _refine_ls_goodness_of_fit_ref 1.0177 _refine_ls_shift/su_max 0.0006898 _refine_ls_shift/su_mean 0.0000209 # The values computed from all data _oxford_reflns_number_all 6548 _refine_ls_R_factor_all 0.0611 _refine_ls_wR_factor_all 0.0595 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4275 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_gt 0.0283 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # 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: 0.320 0.385 0.267 0.128 0.336E-01 ; #========================================================== # 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 'USER DEFINED DATA RENDERING' #=================================================================== # 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 Au1 Au 0.5000 0.82560(3) 0.7500 0.0379 1.0000 Uani S . . . . . Au2 Au 0.5000 1.0000 0.5000 0.0393 1.0000 Uani S . . . . . Cu1 Cu 0.07082(2) 0.98935(6) 0.51550(3) 0.0398 1.0000 Uani . . . . . . N1 N 0.5666(3) 0.5357(6) 0.7029(3) 0.0711 1.0000 Uani . . . . . . N2 N 0.4233(4) 1.1081(7) 0.7868(4) 0.1010 1.0000 Uani . . . . . . N3 N 0.6308(2) 0.7953(6) 0.6060(3) 0.0705 1.0000 Uani . . . . . . N4 N 0.4133(2) 0.8555(7) 0.5710(2) 0.0688 1.0000 Uani . . . . . . N5 N 0.13000(16) 1.0512(5) 0.47073(18) 0.0427 1.0000 Uani . . . . . . N6 N 0.15705(15) 0.8891(4) 0.59115(18) 0.0417 1.0000 Uani . . . . . . C1 C 0.5448(2) 0.6427(6) 0.7214(2) 0.0480 1.0000 Uani . . . . . . C2 C 0.4515(3) 1.0054(6) 0.7746(3) 0.0588 1.0000 Uani . . . . . . C3 C 0.5831(2) 0.8714(6) 0.5699(2) 0.0506 1.0000 Uani . . . . . . C4 C 0.4458(2) 0.9052(6) 0.5461(2) 0.0504 1.0000 Uani . . . . . . C5 C 0.1103(2) 1.1287(7) 0.4063(3) 0.0559 1.0000 Uani . . . . . . C6 C 0.1533(2) 1.1532(7) 0.3762(3) 0.0629 1.0000 Uani . . . . . . C7 C 0.2194(3) 1.0962(8) 0.4149(3) 0.0673 1.0000 Uani . . . . . . C8 C 0.2406(2) 1.0180(7) 0.4821(3) 0.0598 1.0000 Uani . . . . . . C9 C 0.19461(19) 0.9963(5) 0.5085(2) 0.0447 1.0000 Uani . . . . . . C10 C 0.21094(18) 0.9136(6) 0.5793(2) 0.0443 1.0000 Uani . . . . . . C11 C 0.2757(2) 0.8664(8) 0.6316(3) 0.0682 1.0000 Uani . . . . . . C12 C 0.2844(2) 0.7913(9) 0.6955(3) 0.0809 1.0000 Uani . . . . . . C13 C 0.2292(2) 0.7623(7) 0.7063(3) 0.0649 1.0000 Uani . . . . . . C14 C 0.1659(2) 0.8129(6) 0.6526(3) 0.0529 1.0000 Uani . . . . . . O1 O -0.01234(12) 1.0977(4) 0.44694(15) 0.0481 1.0000 Uani . . . . . . H11 H -0.0233 1.0719 0.4032 0.069(5) 1.0000 Uiso R . . . . . H51 H 0.0648 1.1681 0.3802 0.064(5) 1.0000 Uiso R . . . . . H61 H 0.1386 1.2063 0.3313 0.072(5) 1.0000 Uiso R . . . . . H71 H 0.2491 1.1110 0.3953 0.078(5) 1.0000 Uiso R . . . . . H81 H 0.2852 0.9785 0.5094 0.067(5) 1.0000 Uiso R . . . . . H111 H 0.3126 0.8851 0.6228 0.077(5) 1.0000 Uiso R . . . . . H121 H 0.3274 0.7604 0.7315 0.091(5) 1.0000 Uiso R . . . . . H131 H 0.2344 0.7098 0.7492 0.073(5) 1.0000 Uiso R . . . . . H141 H 0.1276 0.7925 0.6588 0.058(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 Au1 0.0397 0.0382 0.0374 0.0000 0.0195 0.0000 Au2 0.0377 0.0438 0.0359 -0.0052 0.0171 -0.0026 Cu1 0.02639(17) 0.0550(3) 0.0372(2) 0.0020(2) 0.01448(17) 0.00101(19) N1 0.079(3) 0.062(3) 0.083(3) -0.010(2) 0.047(3) 0.008(2) N2 0.150(5) 0.075(3) 0.121(5) 0.023(3) 0.099(5) 0.043(4) N3 0.060(2) 0.081(3) 0.068(3) 0.009(2) 0.029(2) 0.015(2) N4 0.060(2) 0.089(3) 0.063(3) 0.009(2) 0.033(2) -0.004(2) N5 0.0343(14) 0.0560(19) 0.0390(17) 0.0013(15) 0.0182(13) -0.0020(14) N6 0.0314(13) 0.0518(19) 0.0420(17) 0.0022(15) 0.0174(13) 0.0024(13) C1 0.0436(19) 0.051(2) 0.050(2) -0.004(2) 0.0228(18) -0.0021(18) C2 0.077(3) 0.054(3) 0.061(3) 0.010(2) 0.045(3) 0.015(2) C3 0.051(2) 0.056(3) 0.048(2) 0.000(2) 0.0270(19) 0.001(2) C4 0.046(2) 0.058(3) 0.047(2) 0.004(2) 0.0219(19) 0.0005(19) C5 0.048(2) 0.071(3) 0.050(2) 0.004(2) 0.024(2) -0.003(2) C6 0.062(3) 0.082(3) 0.048(2) 0.006(3) 0.029(2) -0.008(3) C7 0.063(3) 0.086(4) 0.071(3) -0.002(3) 0.046(3) -0.008(3) C8 0.043(2) 0.082(3) 0.064(3) 0.005(3) 0.033(2) 0.003(2) C9 0.0363(16) 0.055(2) 0.047(2) -0.0056(19) 0.0233(16) -0.0028(17) C10 0.0332(16) 0.055(2) 0.046(2) -0.0038(18) 0.0190(16) 0.0021(16) C11 0.0369(19) 0.101(4) 0.067(3) 0.022(3) 0.024(2) 0.012(2) C12 0.042(2) 0.116(5) 0.073(4) 0.033(4) 0.018(2) 0.023(3) C13 0.054(2) 0.086(4) 0.050(3) 0.027(3) 0.021(2) 0.018(2) C14 0.0441(19) 0.064(3) 0.055(2) 0.011(2) 0.0267(19) 0.010(2) O1 0.0303(11) 0.075(2) 0.0384(14) 0.0057(14) 0.0156(11) 0.0033(13) 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 Au1 . C1 6_656 1.994(4) yes Au1 . C2 6_656 1.987(5) yes Au1 . C1 . 1.994(4) yes Au1 . C2 . 1.987(5) yes Au2 . C4 2_676 2.002(4) yes Au2 . C3 2_676 2.001(5) yes Au2 . C3 . 2.001(5) yes Au2 . C4 . 2.002(4) yes Cu1 . Cu1 2_576 2.9145(9) yes Cu1 . O1 2_576 1.930(3) yes Cu1 . N5 . 1.996(3) yes Cu1 . N6 . 1.978(3) yes Cu1 . C9 . 2.830(4) yes Cu1 . C10 . 2.820(4) yes Cu1 . O1 . 1.919(3) yes N1 . C1 . 1.125(6) yes N2 . C2 . 1.123(6) yes N3 . C3 . 1.139(6) yes N4 . C4 . 1.138(5) yes N5 . C5 . 1.335(6) yes N5 . C9 . 1.344(5) yes N6 . C10 . 1.349(5) yes N6 . C14 . 1.330(5) yes C5 . C6 . 1.382(6) yes C5 . H51 . 0.946 no C6 . C7 . 1.376(7) yes C6 . H61 . 0.923 no C7 . C8 . 1.380(7) yes C7 . H71 . 0.934 no C8 . C9 . 1.381(6) yes C8 . H81 . 0.934 no C9 . C10 . 1.477(6) yes C10 . C11 . 1.383(6) yes C11 . C12 . 1.372(8) yes C11 . H111 . 0.934 no C12 . C13 . 1.371(7) yes C12 . H121 . 0.924 no C13 . C14 . 1.378(6) yes C13 . H131 . 0.932 no C14 . H141 . 0.936 no O1 . H11 . 0.841 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 C1 6_656 Au1 . C2 6_656 177.5(2) yes C1 6_656 Au1 . C1 . 87.5(2) yes C2 6_656 Au1 . C1 . 91.70(18) yes C1 6_656 Au1 . C2 . 91.70(18) yes C2 6_656 Au1 . C2 . 89.2(3) yes C1 . Au1 . C2 . 177.5(2) yes C4 2_676 Au2 . C3 2_676 91.73(18) yes C4 2_676 Au2 . C3 . 88.27(18) yes C3 2_676 Au2 . C3 . 179.994 yes C4 2_676 Au2 . C4 . 179.994 yes C3 2_676 Au2 . C4 . 88.27(18) yes C3 . Au2 . C4 . 91.73(18) yes Cu1 2_576 Cu1 . O1 2_576 40.63(8) yes Cu1 2_576 Cu1 . N5 . 140.26(10) yes O1 2_576 Cu1 . N5 . 172.88(14) yes Cu1 2_576 Cu1 . N6 . 138.01(10) yes O1 2_576 Cu1 . N6 . 97.49(12) yes N5 . Cu1 . N6 . 81.62(13) yes Cu1 2_576 Cu1 . C9 . 165.59(9) yes O1 2_576 Cu1 . C9 . 152.51(12) yes N5 . Cu1 . C9 . 25.60(13) yes N6 . Cu1 . C9 . 56.03(13) yes Cu1 2_576 Cu1 . C10 . 163.77(9) yes O1 2_576 Cu1 . C10 . 123.16(12) yes N5 . Cu1 . C10 . 55.87(13) yes N6 . Cu1 . C10 . 25.78(12) yes C9 . Cu1 . C10 . 30.32(12) yes Cu1 2_576 Cu1 . O1 . 40.92(8) yes O1 2_576 Cu1 . O1 . 81.56(13) yes N5 . Cu1 . O1 . 99.79(13) yes N6 . Cu1 . O1 . 176.14(14) yes C9 . Cu1 . O1 . 125.37(12) yes C10 . Cu1 . O1 . 155.25(12) yes Cu1 . N5 . C5 . 126.5(3) yes Cu1 . N5 . C9 . 114.5(3) yes C5 . N5 . C9 . 118.9(4) yes Cu1 . N6 . C10 . 114.6(3) yes Cu1 . N6 . C14 . 125.6(3) yes C10 . N6 . C14 . 119.6(3) yes Au1 . C1 . N1 . 176.2(4) yes Au1 . C2 . N2 . 178.3(5) yes Au2 . C3 . N3 . 175.8(4) yes Au2 . C4 . N4 . 177.6(4) yes N5 . C5 . C6 . 122.7(4) yes N5 . C5 . H51 . 118.4 no C6 . C5 . H51 . 118.9 no C5 . C6 . C7 . 118.2(5) yes C5 . C6 . H61 . 121.3 no C7 . C6 . H61 . 120.5 no C6 . C7 . C8 . 119.6(4) yes C6 . C7 . H71 . 119.4 no C8 . C7 . H71 . 121.0 no C7 . C8 . C9 . 119.1(4) yes C7 . C8 . H81 . 121.0 no C9 . C8 . H81 . 120.0 no C8 . C9 . N5 . 121.5(4) yes C8 . C9 . Cu1 . 161.1(3) yes N5 . C9 . Cu1 . 39.93(18) yes C8 . C9 . C10 . 124.2(4) yes N5 . C9 . C10 . 114.2(3) yes Cu1 . C9 . C10 . 74.4(2) yes C9 . C10 . N6 . 114.7(3) yes C9 . C10 . Cu1 . 75.2(2) yes N6 . C10 . Cu1 . 39.63(18) yes C9 . C10 . C11 . 124.6(4) yes N6 . C10 . C11 . 120.7(4) yes Cu1 . C10 . C11 . 159.6(3) yes C10 . C11 . C12 . 119.2(4) yes C10 . C11 . H111 . 119.7 no C12 . C11 . H111 . 121.1 no C11 . C12 . C13 . 119.9(4) yes C11 . C12 . H121 . 120.5 no C13 . C12 . H121 . 119.6 no C12 . C13 . C14 . 118.5(5) yes C12 . C13 . H131 . 120.7 no C14 . C13 . H131 . 120.8 no C13 . C14 . N6 . 122.1(4) yes C13 . C14 . H141 . 119.6 no N6 . C14 . H141 . 118.4 no Cu1 2_576 O1 . Cu1 . 98.44(13) yes Cu1 2_576 O1 . H11 . 115.9 no Cu1 . O1 . H11 . 111.9 no data_C16H34Cu2N8O2PtS4 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C16 H34 Cu2 N8 O2 Pt1 S4' _chemical_formula_moiety 'C16 H34 Cu2 N8 O2 Pt1 S4' _chemical_compound_source ? _chemical_formula_weight 820.94 #============================================================= # 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 8.5340(3) _cell_length_b 9.2598(3) _cell_length_c 10.3664(3) _cell_angle_alpha 69.455(2) _cell_angle_beta 68.160(2) _cell_angle_gamma 86.479(2) _cell_volume 709.77(4) _cell_formula_units_Z 1 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 9952 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 32.57 _exptl_crystal_description 'plate' _exptl_crystal_colour 'blue' _exptl_crystal_size_min 0.050 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 1.921 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 402 _exptl_absorpt_coefficient_mu 6.723 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.5514 _exptl_absorpt_correction_T_max 0.7467 _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' #============================================================================= # 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 23251 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_theta_min 2.263 _diffrn_reflns_theta_max 33.948 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.819 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 #========================================================================== # 8. REFINEMENT DATA _reflns_number_total 10328 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -14 _reflns_limit_k_max 14 _reflns_limit_l_min -16 _reflns_limit_l_max 15 _refine_diff_density_min -1.03 _refine_diff_density_max 1.18 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 7660 _refine_ls_number_restraints 0 _refine_ls_number_parameters 152 _oxford_refine_ls_R_factor_ref 0.0390 _refine_ls_wR_factor_ref 0.0356 _refine_ls_goodness_of_fit_ref 1.0919 _refine_ls_shift/su_max 0.0008085 _refine_ls_shift/su_mean 0.0000242 # The values computed from all data _oxford_reflns_number_all 10328 _refine_ls_R_factor_all 0.0587 _refine_ls_wR_factor_all 0.0469 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8116 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_gt 0.0370 _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: 0.510 0.527 0.489 0.242 0.144 ; #========================================================== # 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 'USER DEFINED DATA RENDERING' #=================================================================== # 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 0.0318 1.0000 Uani S . . . . . Cu1 Cu 1.09916(5) 0.89951(4) -0.07908(4) 0.0350 1.0000 Uani . . . . . . S1 S 0.76891(13) 0.52279(12) 0.50055(14) 0.0626 1.0000 Uani . . . . . . S2 S 0.57701(13) 0.71555(13) 0.28384(12) 0.0709 1.0000 Uani . . . . . . N1 N 0.8323(5) 0.2218(5) 0.6530(4) 0.0704 1.0000 Uani . . . . . . N2 N 0.8835(5) 0.6711(4) 0.0800(4) 0.0746 1.0000 Uani . . . . . . N3 N 1.1296(4) 0.8677(3) -0.2717(3) 0.0407 1.0000 Uani . . . . . . N4 N 1.3090(4) 0.7757(3) -0.0790(3) 0.0432 1.0000 Uani . . . . . . C1 C 0.8048(5) 0.3440(5) 0.5927(4) 0.0507 1.0000 Uani . . . . . . C2 C 0.7601(5) 0.6830(4) 0.1679(4) 0.0479 1.0000 Uani . . . . . . C3 C 0.9705(5) 0.8235(5) -0.2769(4) 0.0579 1.0000 Uani . . . . . . C4 C 1.2062(6) 1.0111(5) -0.3997(4) 0.0609 1.0000 Uani . . . . . . C5 C 1.2437(6) 0.7398(5) -0.2756(5) 0.0649 1.0000 Uani . . . . . . C6 C 1.3827(6) 0.7622(6) -0.2286(5) 0.0675 1.0000 Uani . . . . . . C7 C 1.4371(6) 0.8560(5) -0.0593(5) 0.0635 1.0000 Uani . . . . . . C8 C 1.2606(6) 0.6229(5) 0.0392(5) 0.0652 1.0000 Uani . . . . . . O1 O 1.0791(3) 0.9627(3) 0.0828(3) 0.0505 1.0000 Uani . . . . . . H11 H 1.0963 0.9100 0.1592 0.061(4) 1.0000 Uiso R . . . . . H31 H 0.9141 0.7335 -0.1909 0.101(4) 1.0000 Uiso R . . . . . H32 H 0.9933 0.7999 -0.3659 0.081(4) 1.0000 Uiso R . . . . . H33 H 0.8989 0.9097 -0.2776 0.102(4) 1.0000 Uiso R . . . . . H41 H 1.1278 1.0921 -0.3937 0.039(4) 1.0000 Uiso R . . . . . H42 H 1.2268 0.9928 -0.4907 0.097(4) 1.0000 Uiso R . . . . . H43 H 1.3115 1.0428 -0.4017 0.106(4) 1.0000 Uiso R . . . . . H51 H 1.2973 0.7829 -0.3824 0.094(4) 1.0000 Uiso R . . . . . H52 H 1.1847 0.6382 -0.2188 0.119(4) 1.0000 Uiso R . . . . . H61 H 1.4181 0.6601 -0.1934 0.101(4) 1.0000 Uiso R . . . . . H62 H 1.4652 0.8466 -0.3006 0.067(4) 1.0000 Uiso R . . . . . H71 H 1.4678 0.9585 -0.1352 0.069(4) 1.0000 Uiso R . . . . . H72 H 1.5366 0.7988 -0.0705 0.084(4) 1.0000 Uiso R . . . . . H73 H 1.3918 0.8619 0.0388 0.096(4) 1.0000 Uiso R . . . . . H81 H 1.1858 0.5659 0.0227 0.058(4) 1.0000 Uiso R . . . . . H82 H 1.3600 0.5686 0.0413 0.086(4) 1.0000 Uiso R . . . . . H83 H 1.2037 0.6379 0.1311 0.090(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 0.03248(9) 0.03067(9) 0.02821(8) -0.00834(6) -0.00986(6) 0.00781(6) Cu1 0.0469(2) 0.03460(19) 0.02948(17) -0.01565(15) -0.01892(16) 0.01632(16) S1 0.0493(5) 0.0558(6) 0.0779(7) -0.0068(5) -0.0342(5) 0.0022(4) S2 0.0523(6) 0.0630(6) 0.0533(6) 0.0132(5) -0.0060(4) 0.0188(5) N1 0.070(2) 0.082(3) 0.058(2) -0.0183(18) -0.0332(18) 0.037(2) N2 0.077(3) 0.064(2) 0.0487(19) -0.0039(16) -0.0020(18) 0.0053(19) N3 0.0522(16) 0.0434(14) 0.0304(12) -0.0176(11) -0.0167(11) 0.0134(12) N4 0.0495(16) 0.0442(15) 0.0416(14) -0.0188(12) -0.0219(12) 0.0179(12) C1 0.0427(18) 0.073(2) 0.0407(17) -0.0199(17) -0.0216(15) 0.0162(17) C2 0.051(2) 0.0385(17) 0.0397(16) 0.0006(13) -0.0129(15) -0.0059(14) C3 0.067(3) 0.068(3) 0.050(2) -0.0308(19) -0.0260(19) 0.008(2) C4 0.073(3) 0.065(2) 0.0349(17) -0.0103(17) -0.0171(17) 0.003(2) C5 0.087(3) 0.074(3) 0.057(2) -0.046(2) -0.037(2) 0.046(2) C6 0.069(3) 0.094(3) 0.049(2) -0.040(2) -0.0263(19) 0.046(2) C7 0.064(3) 0.061(2) 0.070(3) -0.021(2) -0.035(2) 0.013(2) C8 0.079(3) 0.046(2) 0.068(3) -0.0120(19) -0.034(2) 0.022(2) O1 0.0768(17) 0.0537(14) 0.0424(12) -0.0297(11) -0.0388(12) 0.0390(13) 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_666 2.3198(10) yes Pt1 . S2 2_666 2.3159(9) yes Pt1 . S1 . 2.3198(10) yes Pt1 . S2 . 2.3159(9) yes Cu1 . Cu1 2_775 2.9506(7) yes Cu1 . O1 2_775 1.927(2) yes Cu1 . N2 . 2.521(4) yes Cu1 . N3 . 2.040(3) yes Cu1 . N4 . 2.066(3) yes Cu1 . C5 . 2.807(3) yes Cu1 . C6 . 2.844(4) yes Cu1 . O1 . 1.911(2) yes S1 . C1 . 1.671(4) yes S2 . C2 . 1.666(4) yes N1 . C1 . 1.143(5) yes N2 . C2 . 1.137(5) yes N3 . C3 . 1.466(5) yes N3 . C4 . 1.475(5) yes N3 . C5 . 1.488(4) yes N4 . C6 . 1.488(5) yes N4 . C7 . 1.470(5) yes N4 . C8 . 1.468(5) yes C3 . H31 . 0.964 no C3 . H32 . 0.970 no C3 . H33 . 0.974 no C4 . H41 . 0.977 no C4 . H42 . 0.966 no C4 . H43 . 0.954 no C5 . C6 . 1.489(6) yes C5 . H51 . 0.964 no C5 . H52 . 0.966 no C6 . H61 . 0.961 no C6 . H62 . 0.965 no C7 . H71 . 0.970 no C7 . H72 . 0.964 no C7 . H73 . 0.965 no C8 . H81 . 0.948 no C8 . H82 . 0.963 no C8 . H83 . 0.951 no O1 . H11 . 0.833 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_666 Pt1 . S2 2_666 88.58(4) yes S1 2_666 Pt1 . S1 . 179.995 yes S2 2_666 Pt1 . S1 . 91.42(4) yes S1 2_666 Pt1 . S2 . 91.42(4) yes S2 2_666 Pt1 . S2 . 179.995 yes S1 . Pt1 . S2 . 88.58(4) yes Cu1 2_775 Cu1 . O1 2_775 39.54(7) yes Cu1 2_775 Cu1 . N2 . 93.15(9) yes O1 2_775 Cu1 . N2 . 90.58(13) yes Cu1 2_775 Cu1 . N3 . 135.06(8) yes O1 2_775 Cu1 . N3 . 95.99(10) yes N2 . Cu1 . N3 . 93.46(13) yes Cu1 2_775 Cu1 . N4 . 136.29(8) yes O1 2_775 Cu1 . N4 . 172.68(12) yes N2 . Cu1 . N4 . 95.94(13) yes N3 . Cu1 . N4 . 86.96(11) yes Cu1 2_775 Cu1 . C5 . 165.87(9) yes O1 2_775 Cu1 . C5 . 126.37(11) yes N2 . Cu1 . C5 . 87.46(14) yes N3 . Cu1 . C5 . 30.91(11) yes N4 . Cu1 . C5 . 57.50(12) yes Cu1 2_775 Cu1 . C6 . 160.01(11) yes O1 2_775 Cu1 . C6 . 150.49(11) yes N2 . Cu1 . C6 . 102.32(15) yes N3 . Cu1 . C6 . 57.26(11) yes N4 . Cu1 . C6 . 30.35(11) yes Cu1 2_775 Cu1 . O1 . 39.94(7) yes O1 2_775 Cu1 . O1 . 79.48(10) yes N2 . Cu1 . O1 . 94.28(13) yes N3 . Cu1 . O1 . 171.06(11) yes N4 . Cu1 . O1 . 96.66(10) yes C5 . Cu1 . C6 . 30.56(13) yes C5 . Cu1 . O1 . 154.11(11) yes C6 . Cu1 . O1 . 125.01(12) yes Pt1 . S1 . C1 . 105.14(14) yes Pt1 . S2 . C2 . 106.52(12) yes Cu1 . N2 . C2 . 120.4(3) yes Cu1 . N3 . C3 . 113.4(2) yes Cu1 . N3 . C4 . 110.0(2) yes C3 . N3 . C4 . 107.9(3) yes Cu1 . N3 . C5 . 104.3(2) yes C3 . N3 . C5 . 109.6(3) yes C4 . N3 . C5 . 111.6(3) yes Cu1 . N4 . C6 . 105.1(2) yes Cu1 . N4 . C7 . 112.6(2) yes C6 . N4 . C7 . 108.6(3) yes Cu1 . N4 . C8 . 110.9(2) yes C6 . N4 . C8 . 111.3(3) yes C7 . N4 . C8 . 108.4(3) yes S1 . C1 . N1 . 178.5(4) yes S2 . C2 . N2 . 174.5(3) yes N3 . C3 . H31 . 109.6 no N3 . C3 . H32 . 110.0 no H31 . C3 . H32 . 109.1 no N3 . C3 . H33 . 108.6 no H31 . C3 . H33 . 109.9 no H32 . C3 . H33 . 109.6 no N3 . C4 . H41 . 109.4 no N3 . C4 . H42 . 109.3 no H41 . C4 . H42 . 108.6 no N3 . C4 . H43 . 110.6 no H41 . C4 . H43 . 110.5 no H42 . C4 . H43 . 108.4 no N3 . C5 . Cu1 . 44.75(14) yes N3 . C5 . C6 . 110.3(3) yes Cu1 . C5 . C6 . 76.1(2) yes N3 . C5 . H51 . 92.1 no Cu1 . C5 . H51 . 127.6 no C6 . C5 . H51 . 102.0 no N3 . C5 . H52 . 113.3 no Cu1 . C5 . H52 . 102.0 no C6 . C5 . H52 . 111.6 no H51 . C5 . H52 . 125.5 no C5 . C6 . N4 . 109.5(3) yes C5 . C6 . Cu1 . 73.3(2) yes N4 . C6 . Cu1 . 44.53(14) yes C5 . C6 . H61 . 104.4 no N4 . C6 . H61 . 94.6 no Cu1 . C6 . H61 . 128.7 no C5 . C6 . H62 . 113.7 no N4 . C6 . H62 . 112.7 no Cu1 . C6 . H62 . 106.0 no H61 . C6 . H62 . 120.1 no N4 . C7 . H71 . 109.2 no N4 . C7 . H72 . 109.1 no H71 . C7 . H72 . 108.7 no N4 . C7 . H73 . 109.2 no H71 . C7 . H73 . 111.0 no H72 . C7 . H73 . 109.6 no N4 . C8 . H81 . 109.4 no N4 . C8 . H82 . 110.0 no H81 . C8 . H82 . 110.6 no N4 . C8 . H83 . 107.9 no H81 . C8 . H83 . 109.2 no H82 . C8 . H83 . 109.7 no Cu1 2_775 O1 . Cu1 . 100.52(10) yes Cu1 2_775 O1 . H11 . 124.5 no Cu1 . O1 . H11 . 126.4 no