#============================================================================= 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 ; '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 # 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 ; ; _audit_creation_method 'spawned by CRYSTALS (Betteridge et al., 2003)' #=============================================================================== # 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_C17H11N5Pb1S2 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C17 H11 N5 Pb1 S2' _chemical_formula_moiety 'C17 H11 N5 Pb1 S2' _chemical_compound_source ? _chemical_formula_weight 556.64 #============================================================= # 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 16.122(8) _cell_length_b 10.856(5) _cell_length_c 10.082(5) _cell_angle_alpha 90 _cell_angle_beta 94.22(3) _cell_angle_gamma 90 _cell_volume 1759.7(15) _cell_formula_units_Z 4 _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 '?' _exptl_crystal_size_min ? _exptl_crystal_size_mid ? _exptl_crystal_size_max ? _exptl_crystal_density_diffrn 2.101 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 9.834 # 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_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 45620 _reflns_number_total 6875 _diffrn_reflns_av_R_equivalents 0.050 # Number of reflections without Friedels Law is 12356 # Number of reflections with Friedels Law is 6875 # Theoretical number of reflections is about 7104 _diffrn_reflns_theta_min 2.264 _diffrn_reflns_theta_max 44.591 _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.417 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 #========================================================================== # 8. REFINEMENT DATA _reflns_limit_h_min -31 _reflns_limit_h_max 31 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.25 _refine_diff_density_max 2.80 # 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 4215 _refine_ls_number_restraints 4 _refine_ls_number_parameters 118 _oxford_refine_ls_R_factor_ref 0.0341 _refine_ls_wR_factor_ref 0.0283 _refine_ls_goodness_of_fit_ref 1.0747 _refine_ls_shift/su_max 0.0002908 _refine_ls_shift/su_mean 0.0000179 # The values computed from all data _oxford_reflns_number_all 6875 _refine_ls_R_factor_all 0.0680 _refine_ls_wR_factor_all 0.0676 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4644 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_gt 0.0307 # 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: 0.396 0.558 0.377 0.176 0.408E-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 '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 0.5000 0.154297(14) 0.7500 0.0333 1.0000 Uani S T . . . . S1 S 0.35084(7) 0.19418(11) 0.90363(11) 0.0619 1.0000 Uani . . . . . . N1 N 0.4144(4) 0.0628(4) 1.1273(4) 0.0888 1.0000 Uani . . . . . . N2 N 0.41403(16) 0.2616(2) 0.5503(2) 0.0361 1.0000 Uani . . . . . . N3 N 0.5000 0.3915(3) 0.7500 0.0296 1.0000 Uani S T . . . . C1 C 0.3894(3) 0.1173(3) 1.0342(4) 0.0522 1.0000 Uani . . . . . . C2 C 0.3735(2) 0.1973(3) 0.4520(3) 0.0439 1.0000 Uani . . . . . . C3 C 0.3151(2) 0.2488(3) 0.3612(3) 0.0489 1.0000 Uani . . . . . . C4 C 0.2956(2) 0.3723(3) 0.3750(4) 0.0517 1.0000 Uani . . . . . . C5 C 0.3375(2) 0.4405(3) 0.4753(3) 0.0466 1.0000 Uani . . . . . . C6 C 0.39810(18) 0.3833(2) 0.5595(3) 0.0336 1.0000 Uani . . . . . . C7 C 0.45042(17) 0.4547(2) 0.6603(2) 0.0314 1.0000 Uani . . . . . . C8 C 0.4495(2) 0.5841(2) 0.6573(3) 0.0397 1.0000 Uani . . . . . . C9 C 0.500000(7) 0.6477(4) 0.750000(7) 0.0423 1.0000 Uani S T . . . . H21 H 0.3861 0.1123 0.4443 0.058(5) 1.0000 Uiso R . . . . . H31 H 0.2891 0.2009 0.2910 0.063(5) 1.0000 Uiso R . . . . . H41 H 0.2538 0.4097 0.3170 0.066(5) 1.0000 Uiso R . . . . . H51 H 0.3250 0.5251 0.4869 0.061(5) 1.0000 Uiso R . . . . . H81 H 0.4137 0.6256 0.5928 0.053(5) 1.0000 Uiso R . . . . . H91 H 0.5000 0.7352 0.7500 0.055(5) 1.0000 Uiso RS . . . . . 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 0.04522(8) 0.02282(5) 0.03078(6) 0.0000 -0.00372(5) 0.0000 S1 0.0643(6) 0.0607(6) 0.0579(5) -0.0027(4) -0.0150(5) 0.0039(5) N1 0.154(4) 0.049(2) 0.059(2) 0.0014(17) -0.017(3) 0.003(2) N2 0.0435(13) 0.0279(9) 0.0358(11) 0.0013(8) -0.0033(9) -0.0016(9) N3 0.0352(15) 0.0236(11) 0.0299(13) 0.0000 0.0006(11) 0.0000 C1 0.068(2) 0.0331(14) 0.0547(19) -0.0107(13) -0.0007(17) -0.0038(14) C2 0.0550(18) 0.0332(12) 0.0419(15) -0.0020(11) -0.0065(13) -0.0062(12) C3 0.0532(19) 0.0490(18) 0.0426(16) 0.0013(13) -0.0093(13) -0.0089(15) C4 0.0503(18) 0.051(2) 0.0505(17) 0.0048(14) -0.0149(14) 0.0030(14) C5 0.0507(18) 0.0384(14) 0.0485(17) 0.0036(12) -0.0096(14) 0.0061(13) C6 0.0378(13) 0.0296(11) 0.0333(12) 0.0031(9) 0.0013(10) -0.0007(9) C7 0.0383(13) 0.0251(9) 0.0307(11) 0.0012(8) 0.0023(9) 0.0008(9) C8 0.0535(17) 0.0254(10) 0.0395(14) 0.0050(9) -0.0009(12) 0.0035(11) C9 0.060(2) 0.0212(13) 0.046(2) 0.0000 0.0060(18) 0.0000 _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.04885(4) 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 . N2 6_656 2.631(3) yes Pb1 . S1 6_656 2.9862(18) yes Pb1 . S1 . 2.9862(18) yes Pb1 . N2 . 2.631(3) yes Pb1 . N3 . 2.575(3) yes S1 . C1 . 1.642(4) yes N1 . C1 . 1.156(5) yes N2 . C2 . 1.342(4) yes N2 . C6 . 1.350(4) yes N3 . C7 6_656 1.350(3) yes N3 . C7 . 1.350(3) yes C2 . C3 . 1.383(5) yes C2 . H21 . 0.950 no C3 . C4 . 1.386(5) yes C3 . H31 . 0.950 no C4 . C5 . 1.388(5) yes C4 . H41 . 0.950 no C5 . C6 . 1.392(4) yes C5 . H51 . 0.950 no C6 . C7 . 1.489(4) yes C7 . C8 . 1.405(4) yes C8 . C9 . 1.379(4) yes C8 . H81 . 0.950 no C9 . H91 . 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 N2 6_656 Pb1 . S1 6_656 86.20(8) yes N2 6_656 Pb1 . S1 . 86.43(7) yes S1 6_656 Pb1 . S1 . 163.33(5) yes N2 6_656 Pb1 . N2 . 127.43(10) yes S1 6_656 Pb1 . N2 . 86.43(8) yes S1 . Pb1 . N2 . 86.20(7) yes N2 6_656 Pb1 . N3 . 63.71(6) yes S1 6_656 Pb1 . N3 . 81.66(4) yes S1 . Pb1 . N3 . 81.66(4) yes N2 . Pb1 . N3 . 63.71(6) yes Pb1 . S1 . C1 . 94.01(16) yes Pb1 . N2 . C2 . 122.36(19) yes Pb1 . N2 . C6 . 118.21(18) yes C2 . N2 . C6 . 118.4(3) yes Pb1 . N3 . C7 6_656 120.55(15) yes Pb1 . N3 . C7 . 120.55(15) yes C7 6_656 N3 . C7 . 118.9(3) yes S1 . C1 . N1 . 178.1(5) yes N2 . C2 . C3 . 123.3(3) yes N2 . C2 . H21 . 118.0 no C3 . C2 . H21 . 118.6 no C2 . C3 . C4 . 118.2(3) yes C2 . C3 . H31 . 120.9 no C4 . C3 . H31 . 120.9 no C3 . C4 . C5 . 119.1(3) yes C3 . C4 . H41 . 120.5 no C5 . C4 . H41 . 120.4 no C4 . C5 . C6 . 119.3(3) yes C4 . C5 . H51 . 120.5 no C6 . C5 . H51 . 120.2 no C5 . C6 . N2 . 121.5(3) yes C5 . C6 . C7 . 121.3(3) yes N2 . C6 . C7 . 117.1(2) yes C6 . C7 . N3 . 118.0(2) yes C6 . C7 . C8 . 120.1(2) yes N3 . C7 . C8 . 121.8(3) yes C7 . C8 . C9 . 118.8(3) yes C7 . C8 . H81 . 119.6 no C9 . C8 . H81 . 121.6 no C8 . C9 . C8 6_656 119.9(4) yes C8 . C9 . H91 . 120.0 no C8 6_656 C9 . H91 . 120.0 no data_C17H11N5O1Pb1S2 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C17 H11 N5 O1 Pb1 S2' _chemical_formula_moiety 'C17 H11 N5 O1 Pb1 S2' _chemical_compound_source ? _chemical_formula_weight 572.64 #============================================================= # 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 8.7387(2) _cell_length_b 10.3631(3) _cell_length_c 11.7559(3) _cell_angle_alpha 94.5700(10) _cell_angle_beta 103.6630(10) _cell_angle_gamma 114.6460(10) _cell_volume 920.91(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 '?' _exptl_crystal_size_min ? _exptl_crystal_size_mid ? _exptl_crystal_size_max ? _exptl_crystal_density_diffrn 2.065 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 9.403 # 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_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 41104 _reflns_number_total 9068 _diffrn_reflns_av_R_equivalents 0.027 # Number of reflections without Friedels Law is 12217 # Number of reflections with Friedels Law is 9068 # Theoretical number of reflections is about 9316 _diffrn_reflns_theta_min 1.820 _diffrn_reflns_theta_max 36.927 _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.110 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 #========================================================================== # 8. REFINEMENT DATA _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.84 _refine_diff_density_max 2.00 # 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 7825 _refine_ls_number_restraints 0 _refine_ls_number_parameters 236 _oxford_refine_ls_R_factor_ref 0.0245 _refine_ls_wR_factor_ref 0.0229 _refine_ls_goodness_of_fit_ref 1.0728 _refine_ls_shift/su_max 0.0025182 _refine_ls_shift/su_mean 0.0000409 # The values computed from all data _oxford_reflns_number_all 9068 _refine_ls_R_factor_all 0.0317 _refine_ls_wR_factor_all 0.0307 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7995 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_gt 0.0231 # 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: 0.445 0.629 0.452 0.223 0.771E-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 '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 0.953306(11) 0.882786(8) 0.262291(7) 0.0279 1.0000 Uani . . . . . . S1 S 0.98145(12) 0.80552(8) -0.16845(6) 0.0518 1.0000 Uani . . . . . . S2 S 0.87046(9) 0.79247(7) 0.50365(6) 0.0429 1.0000 Uani . . . . . . N1 N 0.9668(5) 0.8215(3) 0.0642(2) 0.0634 1.0000 Uani . . . . . . N2 N 1.2303(3) 0.9002(3) 0.6197(3) 0.0518 1.0000 Uani . . . . . . N3 N 1.1559(2) 0.76631(19) 0.31512(19) 0.0347 1.0000 Uani . . . . . . N4 N 0.8007(2) 0.61505(17) 0.23463(15) 0.0282 1.0000 Uani . . . . . . N5 N 0.6302(3) 0.7695(2) 0.1560(2) 0.0390 1.0000 Uani . . . . . . C1 C 0.9745(3) 0.8190(2) -0.0322(2) 0.0352 1.0000 Uani . . . . . . C2 C 1.0811(3) 0.8548(2) 0.5702(2) 0.0359 1.0000 Uani . . . . . . C3 C 1.3311(3) 0.8474(3) 0.3537(3) 0.0449 1.0000 Uani . . . . . . C4 C 1.4459(3) 0.7944(3) 0.4043(3) 0.0509 1.0000 Uani . . . . . . C5 C 1.3756(4) 0.6525(4) 0.4164(4) 0.0591 1.0000 Uani . . . . . . C6 C 1.1947(3) 0.5665(3) 0.3771(3) 0.0493 1.0000 Uani . . . . . . C7 C 1.0874(3) 0.6275(2) 0.3261(2) 0.0316 1.0000 Uani . . . . . . C8 C 0.8917(3) 0.5446(2) 0.28168(19) 0.0293 1.0000 Uani . . . . . . C9 C 0.8087(3) 0.4011(2) 0.2911(2) 0.0395 1.0000 Uani . . . . . . C10 C 0.6249(3) 0.3269(2) 0.2509(3) 0.0448 1.0000 Uani . . . . . . C11 C 0.5306(3) 0.3993(2) 0.2031(3) 0.0442 1.0000 Uani . . . . . . C12 C 0.6230(3) 0.5431(2) 0.1956(2) 0.0320 1.0000 Uani . . . . . . C13 C 0.5302(3) 0.6271(2) 0.1451(2) 0.0339 1.0000 Uani . . . . . . C14 C 0.3498(3) 0.5644(3) 0.0884(3) 0.0503 1.0000 Uani . . . . . . C15 C 0.2742(4) 0.6514(4) 0.0442(3) 0.0598 1.0000 Uani . . . . . . C16 C 0.3779(4) 0.7974(4) 0.0568(3) 0.0559 1.0000 Uani . . . . . . C17 C 0.5561(4) 0.8526(3) 0.1134(3) 0.0497 1.0000 Uani . . . . . . O1 O 0.5367(3) 0.1880(2) 0.2582(3) 0.0697 1.0000 Uani . . . . . . H11 H 0.6187 0.1536 0.2926 0.091(4) 1.0000 Uiso R . . . . . H31 H 1.3779 0.9457 0.3455 0.062(4) 1.0000 Uiso R . . . . . H41 H 1.5697 0.8541 0.4299 0.069(4) 1.0000 Uiso R . . . . . H51 H 1.4509 0.6129 0.4524 0.078(4) 1.0000 Uiso R . . . . . H61 H 1.1446 0.4679 0.3844 0.067(4) 1.0000 Uiso R . . . . . H91 H 0.8758 0.3536 0.3245 0.056(4) 1.0000 Uiso R . . . . . H111 H 0.4054 0.3516 0.1761 0.061(4) 1.0000 Uiso R . . . . . H141 H 0.2793 0.4634 0.0803 0.068(4) 1.0000 Uiso R . . . . . H151 H 0.1510 0.6102 0.0054 0.079(4) 1.0000 Uiso R . . . . . H161 H 0.3282 0.8586 0.0276 0.074(4) 1.0000 Uiso R . . . . . H171 H 0.6294 0.9531 0.1217 0.067(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 0.03206(4) 0.02049(3) 0.02868(3) 0.00606(2) 0.00953(2) 0.00918(2) S1 0.0806(5) 0.0437(3) 0.0375(3) 0.0132(2) 0.0287(3) 0.0270(3) S2 0.0433(3) 0.0424(3) 0.0386(3) 0.0088(2) 0.0120(2) 0.0153(2) N1 0.095(2) 0.0604(16) 0.0452(13) 0.0157(11) 0.0357(14) 0.0358(16) N2 0.0499(13) 0.0441(12) 0.0638(15) 0.0221(11) 0.0178(11) 0.0210(10) N3 0.0299(8) 0.0252(7) 0.0461(10) 0.0101(7) 0.0120(7) 0.0087(6) N4 0.0287(7) 0.0213(6) 0.0321(7) 0.0045(5) 0.0087(6) 0.0091(5) N5 0.0346(9) 0.0304(8) 0.0504(11) 0.0114(8) 0.0092(8) 0.0144(7) C1 0.0404(10) 0.0308(9) 0.0366(10) 0.0088(7) 0.0156(8) 0.0157(8) C2 0.0474(12) 0.0293(9) 0.0366(10) 0.0121(7) 0.0172(9) 0.0192(8) C3 0.0314(10) 0.0322(10) 0.0625(15) 0.0122(10) 0.0155(10) 0.0051(8) C4 0.0268(9) 0.0448(13) 0.0715(18) 0.0138(12) 0.0111(10) 0.0086(9) C5 0.0313(11) 0.0485(15) 0.091(2) 0.0205(15) 0.0079(13) 0.0166(10) C6 0.0326(10) 0.0338(10) 0.0784(19) 0.0174(11) 0.0111(11) 0.0138(9) C7 0.0287(8) 0.0250(8) 0.0400(10) 0.0078(7) 0.0117(7) 0.0101(6) C8 0.0285(8) 0.0211(7) 0.0368(9) 0.0070(6) 0.0109(7) 0.0091(6) C9 0.0316(9) 0.0243(8) 0.0587(14) 0.0143(8) 0.0107(9) 0.0093(7) C10 0.0325(10) 0.0251(8) 0.0708(17) 0.0169(10) 0.0129(10) 0.0077(7) C11 0.0296(9) 0.0277(9) 0.0665(16) 0.0141(10) 0.0082(10) 0.0071(7) C12 0.0290(8) 0.0259(8) 0.0372(9) 0.0055(7) 0.0079(7) 0.0100(6) C13 0.0319(9) 0.0301(9) 0.0379(10) 0.0073(7) 0.0084(7) 0.0132(7) C14 0.0341(11) 0.0377(12) 0.0683(18) 0.0114(11) 0.0035(11) 0.0122(9) C15 0.0352(12) 0.0579(17) 0.079(2) 0.0199(15) 0.0027(13) 0.0206(12) C16 0.0471(14) 0.0547(16) 0.074(2) 0.0256(15) 0.0124(13) 0.0310(13) C17 0.0445(13) 0.0386(12) 0.0690(18) 0.0211(12) 0.0128(12) 0.0219(10) O1 0.0355(9) 0.0322(9) 0.127(2) 0.0347(12) 0.0110(11) 0.0059(7) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.13721(8) 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 . S2 . 3.2061(6) yes Pb1 . N1 . 2.407(3) yes Pb1 . N3 . 2.5222(19) yes Pb1 . N4 . 2.4795(16) yes Pb1 . N5 . 2.499(2) yes S1 . C1 . 1.614(2) yes S2 . C2 . 1.632(3) yes N1 . C1 . 1.150(3) yes N2 . C2 . 1.161(4) yes N3 . C3 . 1.339(3) yes N3 . C7 . 1.339(3) yes N4 . C8 . 1.347(3) yes N4 . C12 . 1.349(3) yes N5 . C13 . 1.341(3) yes N5 . C17 . 1.339(3) yes C3 . C4 . 1.376(4) yes C3 . H31 . 0.950 no C4 . C5 . 1.371(4) yes C4 . H41 . 0.950 no C5 . C6 . 1.386(4) yes C5 . H51 . 0.950 no C6 . C7 . 1.388(3) yes C6 . H61 . 0.950 no C7 . C8 . 1.489(3) yes C8 . C9 . 1.384(3) yes C9 . C10 . 1.396(3) yes C9 . H91 . 0.950 no C10 . C11 . 1.387(4) yes C10 . O1 . 1.341(3) yes C11 . C12 . 1.389(3) yes C11 . H111 . 0.950 no C12 . C13 . 1.487(3) yes C13 . C14 . 1.390(3) yes C14 . C15 . 1.389(4) yes C14 . H141 . 0.950 no C15 . C16 . 1.375(5) yes C15 . H151 . 0.950 no C16 . C17 . 1.379(4) yes C16 . H161 . 0.950 no C17 . H171 . 0.950 no O1 . H11 . 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 S2 . Pb1 . N1 . 151.00(7) yes S2 . Pb1 . N3 . 81.64(5) yes N1 . Pb1 . N3 . 82.22(10) yes S2 . Pb1 . N4 . 69.97(4) yes N1 . Pb1 . N4 . 81.44(8) yes N3 . Pb1 . N4 . 65.43(6) yes S2 . Pb1 . N5 . 90.05(5) yes N1 . Pb1 . N5 . 82.06(10) yes N3 . Pb1 . N5 . 129.84(6) yes N4 . Pb1 . N5 . 65.26(6) yes Pb1 . S2 . C2 . 90.08(8) yes Pb1 . N1 . C1 . 166.2(3) yes Pb1 . N3 . C3 . 120.54(16) yes Pb1 . N3 . C7 . 118.94(14) yes C3 . N3 . C7 . 119.3(2) yes Pb1 . N4 . C8 . 119.38(12) yes Pb1 . N4 . C12 . 120.42(13) yes C8 . N4 . C12 . 118.77(16) yes Pb1 . N5 . C13 . 120.32(15) yes Pb1 . N5 . C17 . 119.61(17) yes C13 . N5 . C17 . 120.0(2) yes S1 . C1 . N1 . 176.7(2) yes S2 . C2 . N2 . 178.5(2) yes N3 . C3 . C4 . 122.9(2) yes N3 . C3 . H31 . 118.4 no C4 . C3 . H31 . 118.7 no C3 . C4 . C5 . 117.8(2) yes C3 . C4 . H41 . 121.0 no C5 . C4 . H41 . 121.2 no C4 . C5 . C6 . 120.4(3) yes C4 . C5 . H51 . 120.0 no C6 . C5 . H51 . 119.6 no C5 . C6 . C7 . 118.5(2) yes C5 . C6 . H61 . 121.1 no C7 . C6 . H61 . 120.4 no C6 . C7 . N3 . 121.1(2) yes C6 . C7 . C8 . 122.67(19) yes N3 . C7 . C8 . 116.20(18) yes C7 . C8 . N4 . 117.59(16) yes C7 . C8 . C9 . 120.35(19) yes N4 . C8 . C9 . 122.05(19) yes C8 . C9 . C10 . 119.1(2) yes C8 . C9 . H91 . 120.5 no C10 . C9 . H91 . 120.4 no C9 . C10 . C11 . 119.0(2) yes C9 . C10 . O1 . 121.9(2) yes C11 . C10 . O1 . 119.0(2) yes C10 . C11 . C12 . 118.7(2) yes C10 . C11 . H111 . 120.7 no C12 . C11 . H111 . 120.7 no C11 . C12 . N4 . 122.4(2) yes C11 . C12 . C13 . 121.45(19) yes N4 . C12 . C13 . 116.15(17) yes C12 . C13 . N5 . 116.49(19) yes C12 . C13 . C14 . 123.1(2) yes N5 . C13 . C14 . 120.5(2) yes C13 . C14 . C15 . 119.1(3) yes C13 . C14 . H141 . 120.3 no C15 . C14 . H141 . 120.6 no C14 . C15 . C16 . 119.9(3) yes C14 . C15 . H151 . 120.2 no C16 . C15 . H151 . 120.0 no C15 . C16 . C17 . 118.1(3) yes C15 . C16 . H161 . 120.9 no C17 . C16 . H161 . 121.0 no C16 . C17 . N5 . 122.5(3) yes C16 . C17 . H171 . 118.9 no N5 . C17 . H171 . 118.7 no C10 . O1 . H11 . 109.2 no data_C17H10N5Cl1Pb1S2 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C17 H10 Cl1 N5 Pb1 S2' _chemical_formula_moiety 'C17 H10 Cl1 N5 Pb1 S2' _chemical_compound_source ? _chemical_formula_weight 591.08 #============================================================= # 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 8.7523(13) _cell_length_b 9.9505(14) _cell_length_c 11.5875(17) _cell_angle_alpha 78.608(2) _cell_angle_beta 79.574(2) _cell_angle_gamma 69.777(2) _cell_volume 921.3(2) _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 '?' _exptl_crystal_size_min ? _exptl_crystal_size_mid ? _exptl_crystal_size_max ? _exptl_crystal_density_diffrn 2.131 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 9.539 # 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_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 13683 _reflns_number_total 3702 _diffrn_reflns_av_R_equivalents 0.177 # Number of reflections without Friedels Law is 5797 # Number of reflections with Friedels Law is 3702 # Theoretical number of reflections is about 3716 _diffrn_reflns_theta_min 1.806 _diffrn_reflns_theta_max 26.239 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 0.216 _diffrn_measured_fraction_theta_full NaN _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 #========================================================================== # 8. REFINEMENT DATA _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min -11 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _oxford_diffrn_Wilson_B_factor 2.14 _oxford_diffrn_Wilson_scale 14.11 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -3.06 _refine_diff_density_max 2.43 # 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 3624 _refine_ls_number_restraints 0 _refine_ls_number_parameters 236 _oxford_refine_ls_R_factor_ref 0.0347 _refine_ls_wR_factor_ref 0.0379 _refine_ls_goodness_of_fit_ref 1.0687 _refine_ls_shift/su_max 0.0008454 _refine_ls_shift/su_mean 0.0000140 # The values computed from all data _oxford_reflns_number_all 3702 _refine_ls_R_factor_all 0.0353 _refine_ls_wR_factor_all 0.0385 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3639 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_gt 0.0380 # 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: 1.40 1.47 1.32 0.449 0.311 ; #========================================================== # 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 0.436935(17) 0.121795(15) 0.278237(13) 0.0256 1.0000 Uani . . . . . . Cl1 Cl 0.2062(2) 0.87640(15) 0.2071(2) 0.0736 1.0000 Uani . . . . . . S1 S 0.29791(17) 0.17948(15) -0.15051(11) 0.0416 1.0000 Uani . . . . . . S2 S 0.4490(2) 0.22353(18) 0.50701(13) 0.0505 1.0000 Uani . . . . . . N1 N 0.3592(8) 0.1795(6) 0.0760(5) 0.0560 1.0000 Uani . . . . . . N2 N 0.2019(8) 0.1064(7) 0.6123(5) 0.0615 1.0000 Uani . . . . . . N3 N 0.1286(5) 0.2497(4) 0.3306(4) 0.0339 1.0000 Uani . . . . . . N4 N 0.3436(5) 0.3957(4) 0.2382(3) 0.0288 1.0000 Uani . . . . . . N5 N 0.6562(5) 0.2292(4) 0.1779(4) 0.0335 1.0000 Uani . . . . . . C1 C 0.3359(6) 0.1754(5) -0.0175(4) 0.0337 1.0000 Uani . . . . . . C2 C 0.3027(6) 0.1560(6) 0.5684(4) 0.0390 1.0000 Uani . . . . . . C3 C 0.0272(7) 0.1737(6) 0.3745(5) 0.0424 1.0000 Uani . . . . . . C4 C -0.1359(7) 0.2344(7) 0.4159(6) 0.0502 1.0000 Uani . . . . . . C5 C -0.1941(7) 0.3833(8) 0.4122(7) 0.0590 1.0000 Uani . . . . . . C6 C -0.0921(7) 0.4635(7) 0.3678(6) 0.0510 1.0000 Uani . . . . . . C7 C 0.0713(6) 0.3949(5) 0.3260(4) 0.0325 1.0000 Uani . . . . . . C8 C 0.1887(5) 0.4748(5) 0.2758(4) 0.0310 1.0000 Uani . . . . . . C9 C 0.1417(6) 0.6245(6) 0.2686(5) 0.0417 1.0000 Uani . . . . . . C10 C 0.2567(7) 0.6901(5) 0.2216(6) 0.0454 1.0000 Uani . . . . . . C11 C 0.4166(7) 0.6110(6) 0.1838(6) 0.0453 1.0000 Uani . . . . . . C12 C 0.4531(6) 0.4630(5) 0.1924(5) 0.0336 1.0000 Uani . . . . . . C13 C 0.6224(6) 0.3719(5) 0.1493(4) 0.0324 1.0000 Uani . . . . . . C14 C 0.7352(7) 0.4320(6) 0.0817(6) 0.0504 1.0000 Uani . . . . . . C15 C 0.8903(7) 0.3403(7) 0.0441(7) 0.0551 1.0000 Uani . . . . . . C16 C 0.9244(7) 0.1948(6) 0.0747(6) 0.0494 1.0000 Uani . . . . . . C17 C 0.8057(6) 0.1416(6) 0.1422(6) 0.0441 1.0000 Uani . . . . . . H31 H 0.0700 0.0717 0.3764 0.050(6) 1.0000 Uiso R . . . . . H41 H -0.2046 0.1764 0.4465 0.059(6) 1.0000 Uiso R . . . . . H51 H -0.3055 0.4295 0.4404 0.069(6) 1.0000 Uiso R . . . . . H61 H -0.1316 0.5657 0.3649 0.061(6) 1.0000 Uiso R . . . . . H91 H 0.0330 0.6791 0.2959 0.050(6) 1.0000 Uiso R . . . . . H111 H 0.4974 0.6567 0.1527 0.053(6) 1.0000 Uiso R . . . . . H141 H 0.7093 0.5341 0.0628 0.059(6) 1.0000 Uiso R . . . . . H151 H 0.9699 0.3794 -0.0032 0.066(6) 1.0000 Uiso R . . . . . H161 H 1.0292 0.1307 0.0499 0.057(6) 1.0000 Uiso R . . . . . H171 H 0.8295 0.0399 0.1637 0.052(6) 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 0.02330(11) 0.02371(11) 0.02841(12) -0.00503(7) -0.00222(7) -0.00564(7) Cl1 0.0551(9) 0.0241(6) 0.1336(17) -0.0196(8) 0.0007(10) -0.0044(6) S1 0.0462(7) 0.0469(7) 0.0352(6) -0.0123(5) -0.0088(5) -0.0139(6) S2 0.0506(8) 0.0601(9) 0.0431(7) -0.0143(6) -0.0038(6) -0.0181(7) N1 0.070(4) 0.059(3) 0.041(3) -0.011(2) -0.019(2) -0.015(3) N2 0.062(3) 0.078(4) 0.046(3) -0.008(3) -0.005(2) -0.026(3) N3 0.0273(19) 0.034(2) 0.039(2) -0.0107(16) -0.0019(15) -0.0061(15) N4 0.0244(17) 0.0252(17) 0.0350(19) -0.0092(14) -0.0045(14) -0.0028(14) N5 0.0240(18) 0.0282(18) 0.046(2) -0.0072(16) -0.0023(16) -0.0054(15) C1 0.034(2) 0.030(2) 0.038(3) -0.0064(18) -0.0029(19) -0.0113(18) C2 0.036(3) 0.040(3) 0.032(2) -0.010(2) -0.0063(19) 0.003(2) C3 0.040(3) 0.039(3) 0.050(3) -0.011(2) -0.002(2) -0.014(2) C4 0.037(3) 0.059(3) 0.061(4) -0.013(3) 0.003(2) -0.025(3) C5 0.027(3) 0.060(4) 0.083(5) -0.017(3) 0.007(3) -0.009(2) C6 0.029(3) 0.042(3) 0.076(4) -0.017(3) 0.004(3) -0.004(2) C7 0.026(2) 0.035(2) 0.034(2) -0.0081(18) -0.0040(17) -0.0054(18) C8 0.023(2) 0.032(2) 0.034(2) -0.0079(17) -0.0047(17) -0.0024(17) C9 0.029(2) 0.035(2) 0.056(3) -0.015(2) -0.002(2) -0.0008(19) C10 0.041(3) 0.023(2) 0.069(4) -0.013(2) -0.004(2) -0.004(2) C11 0.034(3) 0.030(2) 0.069(4) -0.010(2) -0.001(2) -0.008(2) C12 0.025(2) 0.030(2) 0.044(3) -0.0102(19) -0.0025(18) -0.0047(17) C13 0.027(2) 0.029(2) 0.039(2) -0.0093(18) -0.0027(18) -0.0058(17) C14 0.038(3) 0.032(2) 0.073(4) -0.007(2) 0.009(3) -0.011(2) C15 0.037(3) 0.044(3) 0.079(4) -0.011(3) 0.012(3) -0.015(2) C16 0.033(3) 0.041(3) 0.067(4) -0.016(3) 0.008(2) -0.007(2) C17 0.029(2) 0.029(2) 0.068(4) -0.012(2) 0.002(2) -0.0036(19) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.4003(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 Pb1 . S2 . 3.0494(15) yes Pb1 . N1 . 2.462(5) yes Pb1 . N3 . 2.571(4) yes Pb1 . N4 . 2.532(4) yes Pb1 . N5 . 2.510(4) yes Cl1 . C10 . 1.731(5) yes S1 . C1 . 1.624(5) yes S2 . C2 . 1.635(6) yes N1 . C1 . 1.149(7) yes N2 . C2 . 1.149(8) yes N3 . C3 . 1.329(7) yes N3 . C7 . 1.349(6) yes N4 . C8 . 1.353(6) yes N4 . C12 . 1.330(6) yes N5 . C13 . 1.331(6) yes N5 . C17 . 1.342(6) yes C3 . C4 . 1.380(8) yes C3 . H31 . 0.950 no C4 . C5 . 1.384(9) yes C4 . H41 . 0.950 no C5 . C6 . 1.365(9) yes C5 . H51 . 0.950 no C6 . C7 . 1.397(7) yes C6 . H61 . 0.950 no C7 . C8 . 1.481(7) yes C8 . C9 . 1.391(7) yes C9 . C10 . 1.361(8) yes C9 . H91 . 0.950 no C10 . C11 . 1.386(8) yes C11 . C12 . 1.382(7) yes C11 . H111 . 0.950 no C12 . C13 . 1.500(6) yes C13 . C14 . 1.375(7) yes C14 . C15 . 1.396(8) yes C14 . H141 . 0.950 no C15 . C16 . 1.360(9) yes C15 . H151 . 0.950 no C16 . C17 . 1.376(8) yes C16 . H161 . 0.950 no C17 . H171 . 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 S2 . Pb1 . N1 . 149.37(14) yes S2 . Pb1 . N3 . 81.05(10) yes N1 . Pb1 . N3 . 82.21(17) yes S2 . Pb1 . N4 . 73.51(9) yes N1 . Pb1 . N4 . 76.14(16) yes N3 . Pb1 . N4 . 64.15(13) yes S2 . Pb1 . N5 . 88.96(10) yes N1 . Pb1 . N5 . 81.95(18) yes N3 . Pb1 . N5 . 129.03(13) yes N4 . Pb1 . N5 . 65.08(12) yes Pb1 . S2 . C2 . 87.55(18) yes Pb1 . N1 . C1 . 165.6(5) yes Pb1 . N3 . C3 . 120.7(3) yes Pb1 . N3 . C7 . 119.8(3) yes C3 . N3 . C7 . 119.1(4) yes Pb1 . N4 . C8 . 121.0(3) yes Pb1 . N4 . C12 . 119.4(3) yes C8 . N4 . C12 . 119.1(4) yes Pb1 . N5 . C13 . 120.9(3) yes Pb1 . N5 . C17 . 119.5(3) yes C13 . N5 . C17 . 119.2(4) yes S1 . C1 . N1 . 176.7(5) yes S2 . C2 . N2 . 178.8(5) yes N3 . C3 . C4 . 123.9(5) yes N3 . C3 . H31 . 117.7 no C4 . C3 . H31 . 118.5 no C3 . C4 . C5 . 117.0(5) yes C3 . C4 . H41 . 121.4 no C5 . C4 . H41 . 121.7 no C4 . C5 . C6 . 120.2(5) yes C4 . C5 . H51 . 119.8 no C6 . C5 . H51 . 120.0 no C5 . C6 . C7 . 119.8(5) yes C5 . C6 . H61 . 120.5 no C7 . C6 . H61 . 119.8 no C6 . C7 . N3 . 120.1(5) yes C6 . C7 . C8 . 122.8(5) yes N3 . C7 . C8 . 117.0(4) yes C7 . C8 . N4 . 117.1(4) yes C7 . C8 . C9 . 121.3(4) yes N4 . C8 . C9 . 121.7(4) yes C8 . C9 . C10 . 117.8(4) yes C8 . C9 . H91 . 121.1 no C10 . C9 . H91 . 121.1 no Cl1 . C10 . C9 . 120.4(4) yes Cl1 . C10 . C11 . 118.1(4) yes C9 . C10 . C11 . 121.5(5) yes C10 . C11 . C12 . 117.2(5) yes C10 . C11 . H111 . 121.4 no C12 . C11 . H111 . 121.4 no C11 . C12 . N4 . 122.7(4) yes C11 . C12 . C13 . 119.8(4) yes N4 . C12 . C13 . 117.5(4) yes C12 . C13 . N5 . 116.3(4) yes C12 . C13 . C14 . 121.9(4) yes N5 . C13 . C14 . 121.8(4) yes C13 . C14 . C15 . 118.8(5) yes C13 . C14 . H141 . 120.6 no C15 . C14 . H141 . 120.6 no C14 . C15 . C16 . 119.1(5) yes C14 . C15 . H151 . 120.3 no C16 . C15 . H151 . 120.7 no C15 . C16 . C17 . 119.2(5) yes C15 . C16 . H161 . 120.2 no C17 . C16 . H161 . 120.5 no C16 . C17 . N5 . 121.9(5) yes C16 . C17 . H171 . 119.3 no N5 . C17 . H171 . 118.8 no data_C17H10Br1N5Pb1S2 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C17 H10 Br1 N5 Pb1 S2' _chemical_formula_moiety 'C17 H10 Br1 N5 Pb1 S2' _chemical_compound_source ? _chemical_formula_weight 635.54 #============================================================= # 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 7.6556(5) _cell_length_b 8.1769(5) _cell_length_c 16.6410(9) _cell_angle_alpha 88.064(2) _cell_angle_beta 79.197(2) _cell_angle_gamma 66.386(2) _cell_volume 936.58(10) _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 '?' _exptl_crystal_size_min ? _exptl_crystal_size_mid ? _exptl_crystal_size_max ? _exptl_crystal_density_diffrn 2.253 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 22.196 # 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_type 'Unknown' _diffrn_measurement_device 'Serial' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _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 7135 _reflns_number_total 2889 _diffrn_reflns_av_R_equivalents 0.040 # Number of reflections without Friedels Law is 3422 # Number of reflections with Friedels Law is 2889 # Theoretical number of reflections is about 3170 _diffrn_reflns_theta_min 2.706 _diffrn_reflns_theta_max 64.774 _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 29.796 _diffrn_measured_fraction_theta_full 0.942 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 #========================================================================== # 8. REFINEMENT DATA _reflns_limit_h_min -8 _reflns_limit_h_max 8 _reflns_limit_k_min -9 _reflns_limit_k_max 9 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -3.48 _refine_diff_density_max 3.33 # 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 2516 _refine_ls_number_restraints 0 _refine_ls_number_parameters 236 _oxford_refine_ls_R_factor_ref 0.0634 _refine_ls_wR_factor_ref 0.0706 _refine_ls_goodness_of_fit_ref 0.9125 _refine_ls_shift/su_max 0.0001534 _refine_ls_shift/su_mean 0.0000055 # The values computed from all data _oxford_reflns_number_all 2520 _refine_ls_R_factor_all 0.0638 _refine_ls_wR_factor_all 0.0708 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2520 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_gt 0.0708 # 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: 1.33 1.86 1.11 0.469 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 '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 0.08480(6) 0.63661(5) 0.14212(2) 0.0402 1.0000 Uani . . . . . . Br1 Br 0.2613(3) 0.9955(3) 0.48657(8) 0.0788 1.0000 Uani . . . . . . S1 S -0.1822(8) 0.5364(7) 0.4169(3) 0.0898 1.0000 Uani . . . . . . S2 S 0.7390(5) 0.7077(5) 0.0115(2) 0.0625 1.0000 Uani . . . . . . N1 N -0.2007(19) 0.6809(15) 0.2629(9) 0.0663 1.0000 Uani . . . . . . N2 N 0.3894(19) 0.690(2) 0.0844(8) 0.0733 1.0000 Uani . . . . . . N3 N -0.0469(13) 0.9687(12) 0.1529(5) 0.0398 1.0000 Uani . . . . . . N4 N 0.1588(13) 0.7573(13) 0.2596(5) 0.0398 1.0000 Uani . . . . . . N5 N 0.2952(14) 0.4045(13) 0.2253(6) 0.0472 1.0000 Uani . . . . . . C1 C -0.1950(18) 0.6248(17) 0.3275(9) 0.0533 1.0000 Uani . . . . . . C2 C 0.528(2) 0.7044(16) 0.0561(7) 0.0513 1.0000 Uani . . . . . . C3 C -0.1483(19) 1.0668(15) 0.0964(7) 0.0446 1.0000 Uani . . . . . . C4 C -0.2230(18) 1.2474(17) 0.1001(7) 0.0482 1.0000 Uani . . . . . . C5 C -0.1972(19) 1.3364(16) 0.1627(8) 0.0494 1.0000 Uani . . . . . . C6 C -0.0943(18) 1.2372(16) 0.2207(8) 0.0486 1.0000 Uani . . . . . . C7 C -0.0220(16) 1.0513(14) 0.2139(6) 0.0394 1.0000 Uani . . . . . . C8 C 0.0853(16) 0.9362(15) 0.2741(6) 0.0384 1.0000 Uani . . . . . . C9 C 0.1115(19) 1.0106(18) 0.3430(7) 0.0492 1.0000 Uani . . . . . . C10 C 0.2181(19) 0.896(2) 0.3958(7) 0.0557 1.0000 Uani . . . . . . C11 C 0.2915(17) 0.7164(19) 0.3823(7) 0.0488 1.0000 Uani . . . . . . C12 C 0.2597(16) 0.6454(17) 0.3124(7) 0.0460 1.0000 Uani . . . . . . C13 C 0.3370(17) 0.4523(17) 0.2918(7) 0.0474 1.0000 Uani . . . . . . C14 C 0.446(2) 0.3247(18) 0.3420(8) 0.0578 1.0000 Uani . . . . . . C15 C 0.514(2) 0.1486(19) 0.3180(10) 0.0657 1.0000 Uani . . . . . . C16 C 0.479(2) 0.098(2) 0.2479(10) 0.0659 1.0000 Uani . . . . . . C17 C 0.3632(19) 0.2320(17) 0.2026(9) 0.0541 1.0000 Uani . . . . . . H31 H -0.1609 1.0065 0.0514 0.065(15) 1.0000 Uiso R . . . . . H41 H -0.3014 1.3146 0.0627 0.066(15) 1.0000 Uiso R . . . . . H51 H -0.2404 1.4628 0.1640 0.068(15) 1.0000 Uiso R . . . . . H61 H -0.0768 1.2952 0.2651 0.072(15) 1.0000 Uiso R . . . . . H91 H 0.0608 1.1367 0.3518 0.067(15) 1.0000 Uiso R . . . . . H111 H 0.3661 0.6377 0.4181 0.074(15) 1.0000 Uiso R . . . . . H141 H 0.4773 0.3595 0.3893 0.082(15) 1.0000 Uiso R . . . . . H151 H 0.5839 0.0612 0.3524 0.090(15) 1.0000 Uiso R . . . . . H161 H 0.5353 -0.0236 0.2290 0.090(15) 1.0000 Uiso R . . . . . H171 H 0.3274 0.1997 0.1559 0.083(15) 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 0.0406(3) 0.0396(3) 0.0384(3) 0.00110(18) -0.01351(19) -0.0114(2) Br1 0.0847(11) 0.1320(16) 0.0420(7) -0.0040(8) -0.0226(7) -0.0613(11) S1 0.098(3) 0.116(4) 0.0503(19) -0.002(2) -0.0156(19) -0.037(3) S2 0.062(2) 0.074(2) 0.0609(18) 0.0039(16) -0.0171(15) -0.0349(18) N1 0.069(8) 0.045(6) 0.087(9) 0.004(6) -0.032(7) -0.018(6) N2 0.056(7) 0.102(10) 0.065(7) 0.002(7) -0.006(6) -0.038(7) N3 0.044(5) 0.038(5) 0.035(4) 0.002(3) -0.009(4) -0.013(4) N4 0.035(5) 0.051(5) 0.036(4) 0.003(4) -0.013(4) -0.017(4) N5 0.041(5) 0.053(6) 0.045(5) 0.017(4) -0.013(4) -0.016(5) C1 0.041(6) 0.051(7) 0.069(8) -0.007(6) -0.008(6) -0.020(5) C2 0.056(8) 0.048(7) 0.045(6) 0.005(5) -0.024(6) -0.011(6) C3 0.061(7) 0.038(6) 0.038(5) 0.001(4) -0.015(5) -0.020(5) C4 0.051(7) 0.062(8) 0.040(5) 0.009(5) -0.020(5) -0.026(6) C5 0.054(7) 0.037(6) 0.057(7) -0.003(5) -0.018(5) -0.015(5) C6 0.051(7) 0.052(7) 0.050(6) 0.009(5) -0.017(5) -0.026(6) C7 0.043(6) 0.040(6) 0.038(5) 0.007(4) -0.009(4) -0.019(5) C8 0.040(6) 0.047(6) 0.033(5) 0.005(4) -0.008(4) -0.022(5) C9 0.057(7) 0.064(8) 0.036(5) 0.000(5) -0.005(5) -0.034(6) C10 0.052(7) 0.097(11) 0.032(5) 0.012(6) -0.018(5) -0.040(8) C11 0.039(6) 0.072(9) 0.039(5) 0.011(5) -0.018(5) -0.023(6) C12 0.037(6) 0.061(8) 0.040(5) 0.007(5) -0.007(4) -0.020(5) C13 0.042(6) 0.052(7) 0.040(5) 0.011(5) -0.010(5) -0.009(5) C14 0.056(7) 0.058(8) 0.054(7) 0.020(6) -0.026(6) -0.011(6) C15 0.059(8) 0.055(8) 0.070(9) 0.031(7) -0.023(7) -0.008(7) C16 0.050(7) 0.066(9) 0.075(9) 0.021(7) -0.008(7) -0.019(7) C17 0.043(6) 0.048(7) 0.064(7) 0.011(6) -0.014(5) -0.010(5) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.1169(4) 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 . 2.591(15) yes Pb1 . N2 . 2.550(13) yes Pb1 . N3 . 2.489(9) yes Pb1 . N4 . 2.471(9) yes Pb1 . N5 . 2.514(9) yes Br1 . C10 . 1.883(13) yes S1 . C1 . 1.635(16) yes S2 . C2 . 1.653(15) yes N1 . C1 . 1.156(18) yes N2 . C2 . 1.130(18) yes N3 . C3 . 1.362(15) yes N3 . C7 . 1.321(14) yes N4 . C8 . 1.352(15) yes N4 . C12 . 1.357(14) yes N5 . C13 . 1.320(17) yes N5 . C17 . 1.333(17) yes C3 . C4 . 1.352(17) yes C3 . H31 . 0.950 no C4 . C5 . 1.377(17) yes C4 . H41 . 0.950 no C5 . C6 . 1.389(17) yes C5 . H51 . 0.950 no C6 . C7 . 1.394(17) yes C6 . H61 . 0.950 no C7 . C8 . 1.480(15) yes C8 . C9 . 1.399(16) yes C9 . C10 . 1.386(18) yes C9 . H91 . 0.950 no C10 . C11 . 1.35(2) yes C11 . C12 . 1.420(18) yes C11 . H111 . 0.950 no C12 . C13 . 1.474(18) yes C13 . C14 . 1.408(15) yes C14 . C15 . 1.36(2) yes C14 . H141 . 0.950 no C15 . C16 . 1.36(2) yes C15 . H151 . 0.950 no C16 . C17 . 1.403(19) yes C16 . H161 . 0.950 no C17 . H171 . 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 N1 . Pb1 . N2 . 148.3(4) yes N1 . Pb1 . N3 . 83.3(3) yes N2 . Pb1 . N3 . 79.1(4) yes N1 . Pb1 . N4 . 74.0(3) yes N2 . Pb1 . N4 . 74.8(4) yes N3 . Pb1 . N4 . 65.9(3) yes N1 . Pb1 . N5 . 86.5(3) yes N2 . Pb1 . N5 . 85.5(4) yes N3 . Pb1 . N5 . 131.0(3) yes N4 . Pb1 . N5 . 65.2(3) yes Pb1 . N1 . C1 . 128.5(10) yes Pb1 . N2 . C2 . 175.8(13) yes Pb1 . N3 . C3 . 120.0(7) yes Pb1 . N3 . C7 . 120.5(7) yes C3 . N3 . C7 . 119.5(9) yes Pb1 . N4 . C8 . 119.2(6) yes Pb1 . N4 . C12 . 120.4(8) yes C8 . N4 . C12 . 120.2(10) yes Pb1 . N5 . C13 . 120.4(8) yes Pb1 . N5 . C17 . 119.8(8) yes C13 . N5 . C17 . 119.8(10) yes S1 . C1 . N1 . 177.4(12) yes S2 . C2 . N2 . 175.2(14) yes N3 . C3 . C4 . 121.9(11) yes N3 . C3 . H31 . 119.0 no C4 . C3 . H31 . 119.0 no C3 . C4 . C5 . 119.6(11) yes C3 . C4 . H41 . 121.2 no C5 . C4 . H41 . 119.0 no C4 . C5 . C6 . 118.8(11) yes C4 . C5 . H51 . 120.7 no C6 . C5 . H51 . 120.4 no C5 . C6 . C7 . 119.0(11) yes C5 . C6 . H61 . 120.5 no C7 . C6 . H61 . 120.6 no C6 . C7 . N3 . 121.3(10) yes C6 . C7 . C8 . 122.3(10) yes N3 . C7 . C8 . 116.5(9) yes C7 . C8 . N4 . 117.7(9) yes C7 . C8 . C9 . 120.9(11) yes N4 . C8 . C9 . 121.4(10) yes C8 . C9 . C10 . 118.1(12) yes C8 . C9 . H91 . 120.3 no C10 . C9 . H91 . 121.7 no Br1 . C10 . C9 . 118.2(11) yes Br1 . C10 . C11 . 120.6(9) yes C9 . C10 . C11 . 121.2(11) yes C10 . C11 . C12 . 119.2(10) yes C10 . C11 . H111 . 121.2 no C12 . C11 . H111 . 119.6 no C11 . C12 . N4 . 119.9(11) yes C11 . C12 . C13 . 123.1(10) yes N4 . C12 . C13 . 116.9(11) yes C12 . C13 . N5 . 116.8(10) yes C12 . C13 . C14 . 121.6(12) yes N5 . C13 . C14 . 121.5(12) yes C13 . C14 . C15 . 118.0(14) yes C13 . C14 . H141 . 121.4 no C15 . C14 . H141 . 120.5 no C14 . C15 . C16 . 120.9(12) yes C14 . C15 . H151 . 118.6 no C16 . C15 . H151 . 120.4 no C15 . C16 . C17 . 118.0(15) yes C15 . C16 . H161 . 120.9 no C17 . C16 . H161 . 121.0 no C16 . C17 . N5 . 121.6(14) yes C16 . C17 . H171 . 119.7 no N5 . C17 . H171 . 118.7 no data_C45H39N12O15Pb3 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C22.50 H19.50 N6 O7.50 Pb1.50' _chemical_formula_moiety 'C22.50 H19.50 N6 O7.50 Pb1.50' _chemical_compound_source ? _chemical_formula_weight 804.74 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting 'hexagonal' _symmetry_space_group_name_H-M 'P 63/m ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x-y,x,z+1/2' '-x+y,-x,-z+1/2' '-y,x-y,z' 'y,-x+y,-z' '-x,-y,z+1/2' 'x,y,-z+1/2' '-x+y,-x,z' 'x-y,x,-z' 'y,-x+y,z+1/2' '-y,x-y,-z+1/2' _cell_length_a 13.1063(2) _cell_length_b 13.1063(2) _cell_length_c 15.9383(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2371.01(4) _cell_formula_units_Z 4 _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 '?' _exptl_crystal_size_min ? _exptl_crystal_size_mid ? _exptl_crystal_size_max ? _exptl_crystal_density_diffrn 2.254 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1518 _exptl_absorpt_coefficient_mu 10.710 #============================================================================= # 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 88387 _reflns_number_total 4202 _diffrn_reflns_av_R_equivalents 0.080 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 4202 # Theoretical number of reflections is about 8171 _diffrn_reflns_theta_min 1.794 _diffrn_reflns_theta_max 37.235 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 37.235 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 #========================================================================== # 8. REFINEMENT DATA _reflns_limit_h_min -18 _reflns_limit_h_max 0 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom,iterative # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -2.89 _refine_diff_density_max 3.57 # 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>3.0\s(I) _refine_ls_number_reflns 3126 _refine_ls_number_restraints 0 _refine_ls_number_parameters 1 _oxford_refine_ls_R_factor_ref 0.0371 _refine_ls_wR_factor_ref 0.0425 _refine_ls_goodness_of_fit_ref 0.7026 _refine_ls_shift/su_max 0.0000309 _refine_ls_shift/su_mean 0.0000309 # The values computed with all filters except I/sigma _oxford_reflns_number_all 4193 _refine_ls_R_factor_all 0.0637 _refine_ls_wR_factor_all 0.0920 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3370 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_gt 0.0501 # 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 noref #undef, noref, refall, # refxyz, refU, constr or mixed # WARNING. The IUCr will not accept pure Unit Weights for F-squared refinements _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Quasi-Unit weights W = 1.0 or 1./4Fsq ; #========================================================== # 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 0.2476 0.0877 0.2500 0.0193 1.0000 Uani . . . . . . H32 H 0.1417 -0.2080 0.2500 0.0500 1.0000 Uiso . . . . . . N1 N 0.3494 0.1288 0.3949 0.0256 1.0000 Uani . . . . . . O2 O 0.3135 0.2913 0.2500 0.0321 1.0000 Uani . . . . . . H31 H 0.2551 -0.1794 0.2500 0.0500 1.0000 Uiso . . . . . . N2 N 0.0000 0.0000 0.1361 0.0274 0.9990 Uani . . . . . . O3 O 0.2230 -0.1335 0.2500 0.0375 1.0000 Uani . . . . . . H21 H 0.2715 0.3237 0.2500 0.0153 1.0000 Uiso . . . . . . N3 N 0.3333 -0.3333 0.2500 0.0392 1.0020 Uani . . . . . . O4 O 0.0397 -0.0680 0.1387 0.0487 1.0000 Uani . . . . . . N5 N 0.4526 0.1184 0.2500 0.0202 1.0000 Uani . . . . . . C9 C 0.3041 0.1497 0.4642 0.0311 1.0000 Uani . . . . . . H91 H 0.2328 0.1486 0.4599 0.0500 1.0000 Uiso . . . . . . O O 0.3830 -0.2214 0.2500 0.0714 1.0000 Uani . . . . . . C C 0.4984 0.1061 0.3223 0.0222 1.0000 Uani . . . . . . C10 C 0.5853 0.0756 0.3246 0.0281 1.0000 Uani . . . . . . H101 H 0.6143 0.0670 0.3757 0.0500 1.0000 Uiso . . . . . . C11 C 0.4288 0.3710 0.2500 0.0253 1.0000 Uani . . . . . . C12 C 0.4521 0.1281 0.4008 0.0222 1.0000 Uani . . . . . . C13 C 0.5097 0.1498 0.4781 0.0364 1.0000 Uani . . . . . . H131 H 0.5805 0.1497 0.4820 0.0500 1.0000 Uiso . . . . . . C14 C 0.3592 0.1728 0.5417 0.0350 1.0000 Uani . . . . . . H141 H 0.3266 0.1889 0.5881 0.0500 1.0000 Uiso . . . . . . C15 C 0.4622 0.1713 0.5486 0.0392 1.0000 Uani . . . . . . H151 H 0.5000 0.1847 0.6002 0.0500 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 Pb1 0.0132 0.0202 0.0234 0.0000 0.0000 0.0076 N1 0.0221 0.0304 0.0260 -0.0006 0.0011 0.0145 O2 0.0175 0.0221 0.0520 0.0000 0.0000 0.0064 N2 0.0273 0.0273 0.0276 0.0000 0.0000 0.0136 O3 0.0343 0.0241 0.0492 0.0000 0.0000 0.0110 N3 0.0346 0.0346 0.0485 0.0000 0.0000 0.0173 O4 0.0400 0.0339 0.0809 -0.0133 -0.0075 0.0251 N5 0.0172 0.0289 0.0202 0.0000 0.0000 0.0157 C9 0.0272 0.0395 0.0292 -0.0024 0.0027 0.0187 O 0.0541 0.0381 0.1212 0.0000 0.0000 0.0225 C 0.0170 0.0273 0.0231 0.0001 -0.0016 0.0117 C10 0.0232 0.0354 0.0319 0.0027 -0.0025 0.0193 C11 0.0161 0.0110 0.0461 0.0000 0.0000 0.0047 C12 0.0175 0.0256 0.0233 0.0014 -0.0006 0.0106 C13 0.0296 0.0578 0.0276 -0.0011 -0.0059 0.0262 C14 0.0358 0.0431 0.0237 -0.0004 0.0039 0.0181 C15 0.0382 0.0479 0.0275 0.0004 -0.0048 0.0185 _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.21403(16) 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 8_555 2.586 yes Pb1 . N1 . 2.586 yes Pb1 . O2 . 2.359 yes Pb1 . O3 . 2.752 yes Pb1 . N5 . 2.509 yes H32 . O3 . 1.024 no N1 . C9 . 1.345 yes N1 . C12 . 1.354 yes O2 . H21 . 0.847 no O2 . C11 . 1.340 yes H31 . O3 . 0.890 no N2 . O4 9_555 1.237 yes N2 . O4 5_555 1.237 yes N2 . O4 . 1.237 yes N3 . O0 12_545 1.273 yes N3 . O0 9_655 1.273 yes N3 . O0 . 1.273 yes N5 . C0 8_555 1.346 yes N5 . C0 . 1.346 yes C9 . H91 . 0.930 no C9 . C14 . 1.386 yes C0 . C10 . 1.384 yes C0 . C12 . 1.480 yes C10 . C11 5_655 1.388 yes C10 . H101 . 0.930 no C12 . C13 . 1.398 yes C13 . H131 . 0.930 no C13 . C15 . 1.380 yes C14 . H141 . 0.930 no C14 . C15 . 1.365 yes C15 . H151 . 0.930 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 8_555 Pb1 . N1 . 126.588 yes N1 8_555 Pb1 . O2 . 84.558 yes N1 . Pb1 . O2 . 84.558 yes N1 8_555 Pb1 . O3 . 89.787 yes N1 . Pb1 . O3 . 89.787 yes O2 . Pb1 . O3 . 167.344 yes N1 8_555 Pb1 . N5 . 64.364 yes N1 . Pb1 . N5 . 64.364 yes O2 . Pb1 . N5 . 93.518 yes O3 . Pb1 . N5 . 73.825 yes Pb1 . N1 . C9 . 122.792 yes Pb1 . N1 . C12 . 118.113 yes C9 . N1 . C12 . 119.092 yes Pb1 . O2 . H21 . 127.3 no Pb1 . O2 . C11 . 120.964 yes H21 . O2 . C11 . 111.8 no O4 9_555 N2 . O4 5_555 119.890 yes O4 9_555 N2 . O4 . 119.890 yes O4 5_555 N2 . O4 . 119.890 yes H32 . O3 . H31 . 88.5 no H32 . O3 . Pb1 . 121.5 no H31 . O3 . Pb1 . 150.0 no O0 12_545 N3 . O0 9_655 120.000 yes O0 12_545 N3 . O0 . 120.000 yes O0 9_655 N3 . O0 . 120.000 yes Pb1 . N5 . C0 8_555 119.103 yes Pb1 . N5 . C0 . 119.103 yes C0 8_555 N5 . C0 . 117.835 yes N1 . C9 . H91 . 118.6 no N1 . C9 . C14 . 122.772 yes H91 . C9 . C14 . 118.6 no N5 . C0 . C10 . 122.518 yes N5 . C0 . C12 . 116.711 yes C10 . C0 . C12 . 120.769 yes C11 5_655 C10 . C0 . 119.642 yes C11 5_655 C10 . H101 . 120.2 no C0 . C10 . H101 . 120.2 no C10 4_665 C11 . C10 9_665 117.720 yes C10 4_665 C11 . O2 . 121.133 yes C10 9_665 C11 . O2 . 121.133 yes C0 . C12 . N1 . 116.670 yes C0 . C12 . C13 . 123.461 yes N1 . C12 . C13 . 119.857 yes C12 . C13 . H131 . 119.8 no C12 . C13 . C15 . 120.360 yes H131 . C13 . C15 . 119.8 no C9 . C14 . H141 . 120.7 no C9 . C14 . C15 . 118.659 yes H141 . C14 . C15 . 120.7 no C13 . C15 . C14 . 119.238 yes C13 . C15 . H151 . 120.4 no C14 . C15 . H151 . 120.4 no