# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email whuang@nju.edu.cn _publ_contact_author_name 'Wei Huang' _publ_author_name 'Wei Huang' # Attachment '- Sum-rev1.Cif' data_Lsym _database_code_depnum_ccdc_archive 'CCDC 815007' #TrackingRef '- Sum-rev1.Cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 N4 S' _chemical_formula_sum 'C10 H8 N4 S' _chemical_formula_weight 216.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 32 2 1' _symmetry_space_group_name_Hall 'P 32 2"' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' _cell_length_a 7.3135(4) _cell_length_b 7.3135(4) _cell_length_c 16.4964(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 764.14(11) _cell_formula_units_Z 3 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3330 _cell_measurement_theta_min 3.217 _cell_measurement_theta_max 28.092 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 0.287 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9502 _exptl_absorpt_correction_T_max 0.9719 _exptl_absorpt_process_details 'SADABS, BRUKER(2000)' _exptl_special_details ; The structure was solved by direct methods (BRUKER, 2000) and successive difference Fourier syntheses. ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER Smart Apex CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4756 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 28.15 _reflns_number_total 1243 _reflns_number_gt 1201 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (BRUKER 2000)' _computing_structure_solution 'SHELXTL (BRUKER 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+0.0793P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(10) _refine_ls_number_reflns 1243 _refine_ls_number_parameters 69 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0276(2) 0.8655(2) 0.11274(9) 0.0449(3) Uani 1 1 d . . . H1 H -0.1037 0.7660 0.0730 0.054 Uiso 1 1 calc R . . C2 C 0.1725(2) 0.9222(2) 0.13518(8) 0.0352(3) Uani 1 1 d . . . C3 C 0.3556(3) 0.8557(3) 0.02238(9) 0.0518(4) Uani 1 1 d . . . H3 H 0.3481 0.9479 -0.0145 0.062 Uiso 1 1 calc R . . C4 C 0.4118(3) 0.6234(3) 0.07506(8) 0.0454(4) Uani 1 1 d . . . H4 H 0.4524 0.5223 0.0811 0.054 Uiso 1 1 calc R . . C5 C 0.3232(2) 0.6822(2) 0.13402(8) 0.0427(3) Uani 1 1 d . . . H5 H 0.2930 0.6311 0.1868 0.051 Uiso 1 1 calc R . . N1 N 0.28705(18) 0.83223(19) 0.10014(6) 0.0355(3) Uani 1 1 d . . . N2 N 0.4332(2) 0.7339(3) 0.00529(7) 0.0541(4) Uani 1 1 d . . . S1 S -0.12164(7) 1.0000 0.1667 0.0546(2) Uani 1 2 d S . . 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 C1 0.0381(7) 0.0468(8) 0.0514(8) -0.0174(6) -0.0096(6) 0.0225(6) C2 0.0358(7) 0.0370(7) 0.0348(6) -0.0063(5) -0.0023(5) 0.0196(5) C3 0.0690(12) 0.0561(9) 0.0379(7) 0.0081(6) 0.0140(7) 0.0370(9) C4 0.0437(8) 0.0552(9) 0.0472(7) -0.0020(6) 0.0007(6) 0.0322(7) C5 0.0463(7) 0.0562(9) 0.0357(6) 0.0027(6) 0.0007(5) 0.0332(7) N1 0.0366(6) 0.0396(6) 0.0320(5) -0.0027(4) 0.0006(5) 0.0205(5) N2 0.0639(9) 0.0664(9) 0.0423(6) 0.0017(6) 0.0154(6) 0.0403(8) S1 0.0381(2) 0.0611(4) 0.0723(4) -0.0261(3) -0.01303(14) 0.03056(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.3576(19) . ? C1 S1 1.7053(15) . ? C1 H1 0.9300 . ? C2 N1 1.4218(17) . ? C2 C2 1.432(2) 5_675 ? C3 N2 1.304(2) . ? C3 N1 1.3565(17) . ? C3 H3 0.9300 . ? C4 C5 1.3523(19) . ? C4 N2 1.3694(19) . ? C4 H4 0.9300 . ? C5 N1 1.3698(18) . ? C5 H5 0.9300 . ? S1 C1 1.7053(15) 5_675 ? 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 C2 C1 S1 111.44(10) . . ? C2 C1 H1 124.3 . . ? S1 C1 H1 124.3 . . ? C1 C2 N1 122.85(12) . . ? C1 C2 C2 112.33(8) . 5_675 ? N1 C2 C2 124.82(7) . 5_675 ? N2 C3 N1 112.19(14) . . ? N2 C3 H3 123.9 . . ? N1 C3 H3 123.9 . . ? C5 C4 N2 110.41(14) . . ? C5 C4 H4 124.8 . . ? N2 C4 H4 124.8 . . ? C4 C5 N1 106.03(12) . . ? C4 C5 H5 127.0 . . ? N1 C5 H5 127.0 . . ? C3 N1 C5 106.25(12) . . ? C3 N1 C2 126.31(13) . . ? C5 N1 C2 126.84(12) . . ? C3 N2 C4 105.11(12) . . ? C1 S1 C1 92.47(10) 5_675 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.15 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.149 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.044 #===END data_L1 _database_code_depnum_ccdc_archive 'CCDC 815008' #TrackingRef '- Sum-rev1.Cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H5 Br N2 S' _chemical_formula_sum 'C7 H5 Br N2 S' _chemical_formula_weight 229.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.969(3) _cell_length_b 7.073(3) _cell_length_c 9.075(4) _cell_angle_alpha 92.827(5) _cell_angle_beta 106.248(4) _cell_angle_gamma 99.958(6) _cell_volume 420.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1133 _cell_measurement_theta_min 2.939 _cell_measurement_theta_max 27.461 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 224 _exptl_absorpt_coefficient_mu 5.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6313 _exptl_absorpt_correction_T_max 0.6313 _exptl_absorpt_process_details 'SADABS, BRUKER(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2091 _diffrn_reflns_av_R_equivalents 0.1106 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1450 _reflns_number_gt 1158 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (BRUKER 2000)' _computing_structure_solution 'SHELXTL (BRUKER 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1051P)^2^+1.9800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1450 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.1822 _refine_ls_wR_factor_gt 0.1721 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.904 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 1.30679(11) 0.83431(13) 0.29497(12) 0.0761(4) Uani 1 1 d . . . C1 C 0.8182(11) 1.1024(9) 0.1831(9) 0.0521(17) Uani 1 1 d . . . H1 H 0.6797 1.0964 0.1688 0.063 Uiso 1 1 calc R . . C2 C 0.9162(9) 0.9567(8) 0.2272(7) 0.0395(13) Uani 1 1 d . . . C3 C 1.1262(10) 1.0051(9) 0.2396(8) 0.0446(15) Uani 1 1 d . . . C4 C 1.1801(11) 1.1872(10) 0.2049(8) 0.060(2) Uani 1 1 d . . . H4 H 1.3120 1.2435 0.2073 0.071 Uiso 1 1 calc R . . C5 C 0.6701(9) 0.6454(8) 0.1537(8) 0.0421(14) Uani 1 1 d . . . H5 H 0.6226 0.6589 0.0491 0.051 Uiso 1 1 calc R . . C6 C 0.7091(11) 0.5361(10) 0.3729(9) 0.0538(17) Uani 1 1 d . . . H6 H 0.6920 0.4577 0.4493 0.065 Uiso 1 1 calc R . . C7 C 0.8434(11) 0.7049(10) 0.3968(8) 0.0513(16) Uani 1 1 d . . . H7 H 0.9352 0.7617 0.4903 0.062 Uiso 1 1 calc R . . N1 N 0.8182(7) 0.7756(7) 0.2573(6) 0.0374(11) Uani 1 1 d . . . N2 N 0.6021(9) 0.4974(8) 0.2202(7) 0.0532(15) Uani 1 1 d . . . S2 S 0.9806(3) 1.2990(2) 0.1570(3) 0.0654(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0391(5) 0.0871(7) 0.1117(8) 0.0304(5) 0.0283(5) 0.0221(4) C1 0.040(4) 0.044(3) 0.075(5) 0.007(3) 0.020(3) 0.006(3) C2 0.035(3) 0.036(3) 0.046(3) -0.003(2) 0.015(3) -0.002(2) C3 0.034(3) 0.049(3) 0.049(4) -0.001(3) 0.017(3) -0.002(3) C4 0.050(4) 0.059(4) 0.065(5) -0.004(3) 0.030(4) -0.018(3) C5 0.028(3) 0.039(3) 0.053(4) 0.006(3) 0.005(3) -0.001(2) C6 0.052(4) 0.051(4) 0.062(5) 0.020(3) 0.022(4) 0.006(3) C7 0.049(4) 0.055(4) 0.044(4) 0.004(3) 0.009(3) 0.001(3) N1 0.027(2) 0.037(2) 0.048(3) 0.003(2) 0.013(2) 0.0017(19) N2 0.036(3) 0.047(3) 0.069(4) 0.010(3) 0.012(3) -0.005(2) S2 0.0742(14) 0.0392(9) 0.0872(15) 0.0138(9) 0.0339(11) 0.0032(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C3 1.878(7) . ? C1 C2 1.349(10) . ? C1 S2 1.705(7) . ? C1 H1 0.9300 . ? C2 C3 1.415(9) . ? C2 N1 1.421(8) . ? C3 C4 1.356(10) . ? C4 S2 1.680(9) . ? C4 H4 0.9300 . ? C5 N2 1.318(9) . ? C5 N1 1.356(8) . ? C5 H5 0.9300 . ? C6 C7 1.349(10) . ? C6 N2 1.365(10) . ? C6 H6 0.9300 . ? C7 N1 1.361(9) . ? C7 H7 0.9300 . ? 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 C2 C1 S2 111.4(5) . . ? C2 C1 H1 124.3 . . ? S2 C1 H1 124.3 . . ? C1 C2 C3 112.3(6) . . ? C1 C2 N1 123.4(6) . . ? C3 C2 N1 124.2(6) . . ? C4 C3 C2 112.1(7) . . ? C4 C3 Br1 124.3(5) . . ? C2 C3 Br1 123.6(5) . . ? C3 C4 S2 112.0(5) . . ? C3 C4 H4 124.0 . . ? S2 C4 H4 124.0 . . ? N2 C5 N1 111.4(6) . . ? N2 C5 H5 124.3 . . ? N1 C5 H5 124.3 . . ? C7 C6 N2 110.2(6) . . ? C7 C6 H6 124.9 . . ? N2 C6 H6 124.9 . . ? C6 C7 N1 106.6(6) . . ? C6 C7 H7 126.7 . . ? N1 C7 H7 126.7 . . ? C5 N1 C7 106.5(5) . . ? C5 N1 C2 126.4(5) . . ? C7 N1 C2 126.9(5) . . ? C5 N2 C6 105.3(5) . . ? C4 S2 C1 92.1(3) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.046 _refine_diff_density_min -1.414 _refine_diff_density_rms 0.169 #===END data_1 _database_code_depnum_ccdc_archive 'CCDC 815009' #TrackingRef '- Sum-rev1.Cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H54 Cl6 N18 O25 S6 Zn3' _chemical_formula_sum 'C72 H54 Cl6 N18 O25 S6 Zn3' _chemical_formula_weight 2172.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3 c' _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' 'x, x-y, z-1/2' '-x+y, y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' _cell_length_a 23.8364(8) _cell_length_b 23.8364(8) _cell_length_c 26.589(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 13083.2(12) _cell_formula_units_Z 6 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3778 _cell_measurement_theta_min 4.996 _cell_measurement_theta_max 43.160 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6612 _exptl_absorpt_coefficient_mu 1.232 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8764 _exptl_absorpt_correction_T_max 0.8867 _exptl_absorpt_process_details 'SADABS; BRUKER, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21337 _diffrn_reflns_av_R_equivalents 0.0780 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2566 _reflns_number_gt 1733 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (BRUKER 2000)' _computing_structure_solution 'SHELXTL (BRUKER 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2566 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1071 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 1.01624(2) 0.34957(2) -0.0833 0.0468(2) Uani 1 2 d S . . C1 C 0.94962(17) 0.21090(17) -0.05072(12) 0.0523(9) Uani 1 1 d . . . H1 H 0.9325 0.2028 -0.0831 0.063 Uiso 1 1 calc R . . C2 C 0.92785(17) 0.15928(17) -0.01778(13) 0.0516(9) Uani 1 1 d . . . H2 H 0.8963 0.1180 -0.0278 0.062 Uiso 1 1 calc R . . C3 C 0.95370(15) 0.16986(15) 0.03055(11) 0.0399(7) Uani 1 1 d . . . C4 C 1.00108(15) 0.23279(15) 0.04241(11) 0.0402(8) Uani 1 1 d . . . H4 H 1.0201 0.2422 0.0741 0.048 Uiso 1 1 calc R . . C5 C 1.01962(15) 0.28073(16) 0.00739(12) 0.0448(8) Uani 1 1 d . . . H5 H 1.0521 0.3223 0.0160 0.054 Uiso 1 1 calc R . . C6 C 0.92477(16) 0.05714(16) 0.05457(13) 0.0537(9) Uani 1 1 d . . . H6 H 0.9301 0.0459 0.0222 0.064 Uiso 1 1 calc R . . C7 C 0.93233(15) 0.11611(15) 0.06675(12) 0.0434(8) Uani 1 1 d . . . C8 C 0.91979(16) 0.11788(15) 0.11903(12) 0.0416(8) Uani 1 1 d . . . C9 C 0.90388(16) 0.06232(16) 0.14374(13) 0.0523(9) Uani 1 1 d . . . H9 H 0.8939 0.0557 0.1778 0.063 Uiso 1 1 calc R . . C10 C 0.95596(15) 0.20012(16) 0.18555(11) 0.0414(8) Uani 1 1 d . . . H10 H 0.9784 0.1846 0.2041 0.050 Uiso 1 1 calc R . . C11 C 0.91473(16) 0.25787(17) 0.15965(12) 0.0468(8) Uani 1 1 d . . . H11 H 0.9040 0.2903 0.1578 0.056 Uiso 1 1 calc R . . C12 C 0.89675(16) 0.20961(16) 0.12656(12) 0.0457(8) Uani 1 1 d . . . H12 H 0.8715 0.2022 0.0980 0.055 Uiso 1 1 calc R . . Cl1 Cl 0.75485(5) 0.87860(4) 0.18045(3) 0.0548(3) Uani 1 1 d . . . N1 N 0.99357(13) 0.27121(13) -0.03886(9) 0.0447(7) Uani 1 1 d . . . N2 N 0.92314(12) 0.17292(12) 0.14319(9) 0.0387(6) Uani 1 1 d . . . N3 N 0.95220(12) 0.25197(13) 0.19738(9) 0.0418(7) Uani 1 1 d . . . O1 O 0.8142(2) 0.9026(2) 0.20626(19) 0.1512(18) Uani 1 1 d . . . O2 O 0.73749(15) 0.92718(13) 0.17722(11) 0.0822(9) Uani 1 1 d . . . O3 O 0.7598(2) 0.85812(17) 0.13266(11) 0.1231(15) Uani 1 1 d . . . O4 O 0.70878(16) 0.82472(13) 0.20818(10) 0.0859(9) Uani 1 1 d . . . O5 O 0.0000 0.0000 0.2500 0.411(16) Uiso 1 6 d S . . S1 S 0.90449(5) 0.00616(5) 0.10468(4) 0.0662(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0536(3) 0.0536(3) 0.0258(3) 0.00001(12) -0.00001(12) 0.0214(3) C1 0.062(2) 0.056(2) 0.0334(19) -0.0084(17) -0.0094(17) 0.026(2) C2 0.057(2) 0.046(2) 0.040(2) -0.0095(16) -0.0091(17) 0.0172(18) C3 0.0438(19) 0.0421(19) 0.0323(17) -0.0031(14) 0.0015(14) 0.0203(16) C4 0.0416(19) 0.0433(19) 0.0288(17) -0.0021(14) -0.0071(14) 0.0161(16) C5 0.0421(19) 0.046(2) 0.0373(19) -0.0051(15) -0.0057(15) 0.0149(17) C6 0.060(2) 0.047(2) 0.046(2) -0.0072(16) 0.0015(17) 0.0214(19) C7 0.0410(19) 0.0378(19) 0.044(2) -0.0007(15) -0.0006(15) 0.0141(16) C8 0.0437(19) 0.0418(19) 0.0381(19) -0.0022(15) -0.0034(15) 0.0204(16) C9 0.058(2) 0.054(2) 0.044(2) 0.0088(17) 0.0046(17) 0.0276(19) C10 0.048(2) 0.051(2) 0.0282(17) 0.0055(15) 0.0006(14) 0.0266(17) C11 0.053(2) 0.052(2) 0.044(2) 0.0042(17) 0.0000(16) 0.0327(18) C12 0.050(2) 0.053(2) 0.0380(19) 0.0018(16) -0.0063(16) 0.0292(18) Cl1 0.0735(7) 0.0543(6) 0.0454(5) 0.0089(4) 0.0084(5) 0.0386(5) N1 0.0460(16) 0.0511(18) 0.0314(15) -0.0025(13) -0.0011(12) 0.0199(14) N2 0.0411(15) 0.0428(16) 0.0324(14) -0.0003(12) -0.0011(12) 0.0212(13) N3 0.0509(17) 0.0479(17) 0.0291(14) 0.0047(12) 0.0042(12) 0.0266(14) O1 0.100(3) 0.118(3) 0.230(5) -0.020(3) -0.076(3) 0.050(2) O2 0.137(3) 0.0717(18) 0.0712(19) 0.0072(15) 0.0081(18) 0.0766(19) O3 0.253(5) 0.115(3) 0.0503(18) 0.0215(18) 0.055(2) 0.129(3) O4 0.123(2) 0.0616(18) 0.073(2) 0.0250(15) 0.0424(18) 0.0459(18) S1 0.0794(7) 0.0436(6) 0.0732(7) 0.0044(5) 0.0034(5) 0.0291(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N3 1.974(3) 18_554 ? Zn1 N3 1.974(3) 14_644 ? Zn1 N1 2.042(3) . ? Zn1 N1 2.042(3) 10_544 ? C1 N1 1.326(4) . ? C1 C2 1.383(5) . ? C1 H1 0.9300 . ? C2 C3 1.393(4) . ? C2 H2 0.9300 . ? C3 C4 1.390(4) . ? C3 C7 1.475(4) . ? C4 C5 1.365(4) . ? C4 H4 0.9300 . ? C5 N1 1.345(4) . ? C5 H5 0.9300 . ? C6 C7 1.364(4) . ? C6 S1 1.702(4) . ? C6 H6 0.9300 . ? C7 C8 1.427(4) . ? C8 C9 1.352(4) . ? C8 N2 1.426(4) . ? C9 S1 1.700(4) . ? C9 H9 0.9300 . ? C10 N3 1.321(4) . ? C10 N2 1.339(4) . ? C10 H10 0.9300 . ? C11 C12 1.337(4) . ? C11 N3 1.396(4) . ? C11 H11 0.9300 . ? C12 N2 1.381(4) . ? C12 H12 0.9300 . ? Cl1 O3 1.387(3) . ? Cl1 O4 1.410(3) . ? Cl1 O1 1.411(4) . ? Cl1 O2 1.414(3) . ? N3 Zn1 1.974(3) 9_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zn1 N3 120.29(15) 18_554 14_644 ? N3 Zn1 N1 99.47(10) 18_554 . ? N3 Zn1 N1 114.99(11) 14_644 . ? N3 Zn1 N1 114.99(11) 18_554 10_544 ? N3 Zn1 N1 99.48(10) 14_644 10_544 ? N1 Zn1 N1 107.73(15) . 10_544 ? N1 C1 C2 123.8(3) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C1 C2 C3 119.2(3) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 116.9(3) . . ? C4 C3 C7 122.1(3) . . ? C2 C3 C7 121.0(3) . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 123.6(3) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? C7 C6 S1 113.2(3) . . ? C7 C6 H6 123.4 . . ? S1 C6 H6 123.4 . . ? C6 C7 C8 109.9(3) . . ? C6 C7 C3 123.4(3) . . ? C8 C7 C3 126.6(3) . . ? C9 C8 N2 122.8(3) . . ? C9 C8 C7 113.9(3) . . ? N2 C8 C7 123.3(3) . . ? C8 C9 S1 111.5(3) . . ? C8 C9 H9 124.3 . . ? S1 C9 H9 124.3 . . ? N3 C10 N2 110.9(3) . . ? N3 C10 H10 124.5 . . ? N2 C10 H10 124.5 . . ? C12 C11 N3 109.4(3) . . ? C12 C11 H11 125.3 . . ? N3 C11 H11 125.3 . . ? C11 C12 N2 106.4(3) . . ? C11 C12 H12 126.8 . . ? N2 C12 H12 126.8 . . ? O3 Cl1 O4 108.8(2) . . ? O3 Cl1 O1 110.1(3) . . ? O4 Cl1 O1 106.3(2) . . ? O3 Cl1 O2 110.10(19) . . ? O4 Cl1 O2 111.36(18) . . ? O1 Cl1 O2 110.0(2) . . ? C1 N1 C5 116.6(3) . . ? C1 N1 Zn1 123.9(2) . . ? C5 N1 Zn1 119.1(2) . . ? C10 N2 C12 107.7(3) . . ? C10 N2 C8 125.1(3) . . ? C12 N2 C8 127.2(3) . . ? C10 N3 C11 105.6(3) . . ? C10 N3 Zn1 128.5(2) . 9_665 ? C11 N3 Zn1 125.2(2) . 9_665 ? C9 S1 C6 91.56(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -1.2(5) . . . . ? C1 C2 C3 C4 -0.7(5) . . . . ? C1 C2 C3 C7 -179.4(3) . . . . ? C2 C3 C4 C5 0.6(5) . . . . ? C7 C3 C4 C5 179.4(3) . . . . ? C3 C4 C5 N1 1.3(5) . . . . ? S1 C6 C7 C8 -0.9(4) . . . . ? S1 C6 C7 C3 176.2(3) . . . . ? C4 C3 C7 C6 -134.0(4) . . . . ? C2 C3 C7 C6 44.7(5) . . . . ? C4 C3 C7 C8 42.6(5) . . . . ? C2 C3 C7 C8 -138.7(4) . . . . ? C6 C7 C8 C9 0.1(4) . . . . ? C3 C7 C8 C9 -176.9(3) . . . . ? C6 C7 C8 N2 -179.4(3) . . . . ? C3 C7 C8 N2 3.6(5) . . . . ? N2 C8 C9 S1 -179.7(2) . . . . ? C7 C8 C9 S1 0.8(4) . . . . ? N3 C11 C12 N2 -0.3(4) . . . . ? C2 C1 N1 C5 3.0(5) . . . . ? C2 C1 N1 Zn1 -170.6(3) . . . . ? C4 C5 N1 C1 -3.1(5) . . . . ? C4 C5 N1 Zn1 170.9(3) . . . . ? N3 Zn1 N1 C1 145.1(3) 18_554 . . . ? N3 Zn1 N1 C1 -85.0(3) 14_644 . . . ? N1 Zn1 N1 C1 24.9(2) 10_544 . . . ? N3 Zn1 N1 C5 -28.4(2) 18_554 . . . ? N3 Zn1 N1 C5 101.6(2) 14_644 . . . ? N1 Zn1 N1 C5 -148.6(3) 10_544 . . . ? N3 C10 N2 C12 0.2(3) . . . . ? N3 C10 N2 C8 177.2(3) . . . . ? C11 C12 N2 C10 0.0(3) . . . . ? C11 C12 N2 C8 -176.9(3) . . . . ? C9 C8 N2 C10 50.7(5) . . . . ? C7 C8 N2 C10 -129.8(3) . . . . ? C9 C8 N2 C12 -132.8(4) . . . . ? C7 C8 N2 C12 46.6(5) . . . . ? N2 C10 N3 C11 -0.4(3) . . . . ? N2 C10 N3 Zn1 -171.06(19) . . . 9_665 ? C12 C11 N3 C10 0.4(4) . . . . ? C12 C11 N3 Zn1 171.5(2) . . . 9_665 ? C8 C9 S1 C6 -1.1(3) . . . . ? C7 C6 S1 C9 1.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.424 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.063 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 815010' #TrackingRef '- Sum-rev1.Cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 Cd Cl2 N6 S2' _chemical_formula_sum 'C24 H18 Cd Cl2 N6 S2' _chemical_formula_weight 637.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.1844(4) _cell_length_b 9.6968(5) _cell_length_c 15.7097(8) _cell_angle_alpha 90.00 _cell_angle_beta 104.4480(10) _cell_angle_gamma 90.00 _cell_volume 1207.33(11) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3080 _cell_measurement_theta_min 2.491 _cell_measurement_theta_max 28.056 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 1.326 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8571 _exptl_absorpt_correction_T_max 0.8788 _exptl_absorpt_process_details 'SADABS, BRUKER(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5938 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2121 _reflns_number_gt 1793 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (BRUKER 2000)' _computing_structure_solution 'SHELXTL (BRUKER 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0251P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2121 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0490 _refine_ls_wR_factor_gt 0.0473 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 1.0000 0.5000 0.0000 0.03151(9) Uani 1 2 d S . . C1 C 0.7453(3) 0.2791(2) 0.06924(15) 0.0359(6) Uani 1 1 d . . . H1 H 0.6698 0.2824 0.0142 0.043 Uiso 1 1 calc R . . C2 C 0.8554(3) 0.2295(2) 0.20731(16) 0.0408(6) Uani 1 1 d . . . H2 H 0.8728 0.1946 0.2640 0.049 Uiso 1 1 calc R . . C3 C 0.9615(3) 0.3104(2) 0.17574(16) 0.0410(6) Uani 1 1 d . . . H3 H 1.0663 0.3407 0.2082 0.049 Uiso 1 1 calc R . . C4 C 0.5674(3) 0.1343(2) 0.14180(15) 0.0331(5) Uani 1 1 d . . . C5 C 0.4318(3) 0.1985(2) 0.15738(16) 0.0441(6) Uani 1 1 d . . . H5 H 0.4230 0.2934 0.1633 0.053 Uiso 1 1 calc R . . C6 C 0.3958(3) -0.0510(2) 0.14611(17) 0.0391(6) Uani 1 1 d . . . H6 H 0.3595 -0.1421 0.1441 0.047 Uiso 1 1 calc R . . C7 C 0.5497(3) -0.0129(2) 0.13406(15) 0.0316(5) Uani 1 1 d . . . C8 C 0.6678(3) -0.1140(2) 0.11238(14) 0.0294(5) Uani 1 1 d . . . C9 C 0.6352(3) -0.2533(2) 0.11840(17) 0.0416(6) Uani 1 1 d . . . H9 H 0.5460 -0.2815 0.1411 0.050 Uiso 1 1 calc R . . C10 C 0.7334(3) -0.3496(2) 0.09124(18) 0.0487(7) Uani 1 1 d . . . H10 H 0.7059 -0.4421 0.0949 0.058 Uiso 1 1 calc R . . C11 C 0.9024(3) -0.1864(2) 0.05776(17) 0.0435(6) Uani 1 1 d . . . H11 H 0.9967 -0.1617 0.0382 0.052 Uiso 1 1 calc R . . C12 C 0.8093(3) -0.0824(2) 0.08273(18) 0.0442(7) Uani 1 1 d . . . H12 H 0.8414 0.0090 0.0797 0.053 Uiso 1 1 calc R . . Cl1 Cl 1.27203(8) 0.54370(6) 0.12284(4) 0.03926(15) Uani 1 1 d . . . N1 N 0.8925(2) 0.34116(18) 0.08907(13) 0.0358(5) Uani 1 1 d . . . N2 N 0.7173(2) 0.20981(17) 0.13872(12) 0.0316(4) Uani 1 1 d . . . N3 N 0.8661(2) -0.31908(18) 0.05983(13) 0.0356(5) Uani 1 1 d . . . S1 S 0.27856(8) 0.08367(7) 0.16488(5) 0.0530(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03730(15) 0.02424(13) 0.03615(15) -0.00124(10) 0.01512(11) 0.00092(11) C1 0.0460(15) 0.0291(12) 0.0332(14) 0.0009(11) 0.0113(11) -0.0015(11) C2 0.0441(15) 0.0457(15) 0.0332(14) 0.0072(12) 0.0110(12) 0.0005(12) C3 0.0400(14) 0.0430(14) 0.0394(16) 0.0018(12) 0.0090(12) 0.0006(12) C4 0.0380(13) 0.0297(12) 0.0343(14) -0.0002(10) 0.0139(11) 0.0002(11) C5 0.0479(16) 0.0318(13) 0.0571(18) -0.0020(12) 0.0214(13) 0.0082(12) C6 0.0363(14) 0.0334(12) 0.0518(17) -0.0041(12) 0.0188(12) -0.0014(11) C7 0.0336(13) 0.0296(13) 0.0331(13) -0.0005(10) 0.0113(10) 0.0017(10) C8 0.0288(12) 0.0290(12) 0.0317(13) -0.0019(10) 0.0100(10) 0.0010(10) C9 0.0401(15) 0.0310(13) 0.0614(18) 0.0013(12) 0.0272(13) 0.0001(11) C10 0.0505(16) 0.0275(13) 0.075(2) 0.0008(13) 0.0290(15) 0.0013(12) C11 0.0424(15) 0.0352(14) 0.0620(18) -0.0035(12) 0.0302(13) -0.0006(12) C12 0.0489(16) 0.0239(13) 0.0683(19) -0.0049(12) 0.0306(14) -0.0043(11) Cl1 0.0391(3) 0.0381(3) 0.0403(4) -0.0018(3) 0.0094(3) -0.0023(3) N1 0.0442(12) 0.0273(10) 0.0388(12) 0.0017(9) 0.0159(10) 0.0008(9) N2 0.0388(11) 0.0244(10) 0.0340(11) 0.0008(8) 0.0138(9) 0.0011(9) N3 0.0358(11) 0.0291(11) 0.0450(13) -0.0032(9) 0.0158(10) 0.0019(9) S1 0.0403(4) 0.0502(4) 0.0758(6) -0.0066(4) 0.0282(4) 0.0069(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N3 2.3826(17) 1_565 ? Cd1 N3 2.3826(17) 3_755 ? Cd1 N1 2.3914(18) 3_765 ? Cd1 N1 2.3914(18) . ? Cd1 Cl1 2.5916(6) . ? Cd1 Cl1 2.5916(6) 3_765 ? C1 N1 1.313(3) . ? C1 N2 1.349(3) . ? C1 H1 0.9300 . ? C2 C3 1.353(3) . ? C2 N2 1.366(3) . ? C2 H2 0.9300 . ? C3 N1 1.370(3) . ? C3 H3 0.9300 . ? C4 C5 1.347(3) . ? C4 C7 1.437(3) . ? C4 N2 1.440(3) . ? C5 S1 1.703(2) . ? C5 H5 0.9300 . ? C6 C7 1.370(3) . ? C6 S1 1.689(2) . ? C6 H6 0.9300 . ? C7 C8 1.475(3) . ? C8 C9 1.385(3) . ? C8 C12 1.385(3) . ? C9 C10 1.368(3) . ? C9 H9 0.9300 . ? C10 N3 1.334(3) . ? C10 H10 0.9300 . ? C11 N3 1.322(3) . ? C11 C12 1.379(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? N3 Cd1 2.3826(17) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cd1 N3 180.00(8) 1_565 3_755 ? N3 Cd1 N1 91.68(6) 1_565 3_765 ? N3 Cd1 N1 88.32(6) 3_755 3_765 ? N3 Cd1 N1 88.32(6) 1_565 . ? N3 Cd1 N1 91.68(6) 3_755 . ? N1 Cd1 N1 180.00(7) 3_765 . ? N3 Cd1 Cl1 88.86(5) 1_565 . ? N3 Cd1 Cl1 91.14(5) 3_755 . ? N1 Cd1 Cl1 87.55(5) 3_765 . ? N1 Cd1 Cl1 92.45(5) . . ? N3 Cd1 Cl1 91.14(5) 1_565 3_765 ? N3 Cd1 Cl1 88.86(5) 3_755 3_765 ? N1 Cd1 Cl1 92.45(5) 3_765 3_765 ? N1 Cd1 Cl1 87.55(5) . 3_765 ? Cl1 Cd1 Cl1 180.00(3) . 3_765 ? N1 C1 N2 111.6(2) . . ? N1 C1 H1 124.2 . . ? N2 C1 H1 124.2 . . ? C3 C2 N2 105.8(2) . . ? C3 C2 H2 127.1 . . ? N2 C2 H2 127.1 . . ? C2 C3 N1 110.3(2) . . ? C2 C3 H3 124.8 . . ? N1 C3 H3 124.8 . . ? C5 C4 C7 113.9(2) . . ? C5 C4 N2 121.3(2) . . ? C7 C4 N2 124.80(19) . . ? C4 C5 S1 111.40(18) . . ? C4 C5 H5 124.3 . . ? S1 C5 H5 124.3 . . ? C7 C6 S1 113.43(18) . . ? C7 C6 H6 123.3 . . ? S1 C6 H6 123.3 . . ? C6 C7 C4 109.42(19) . . ? C6 C7 C8 122.04(19) . . ? C4 C7 C8 128.47(19) . . ? C9 C8 C12 115.5(2) . . ? C9 C8 C7 118.95(19) . . ? C12 C8 C7 125.6(2) . . ? C10 C9 C8 120.4(2) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? N3 C10 C9 124.0(2) . . ? N3 C10 H10 118.0 . . ? C9 C10 H10 118.0 . . ? N3 C11 C12 124.1(2) . . ? N3 C11 H11 118.0 . . ? C12 C11 H11 118.0 . . ? C11 C12 C8 120.1(2) . . ? C11 C12 H12 119.9 . . ? C8 C12 H12 119.9 . . ? C1 N1 C3 105.19(18) . . ? C1 N1 Cd1 127.33(16) . . ? C3 N1 Cd1 126.95(15) . . ? C1 N2 C2 107.13(19) . . ? C1 N2 C4 126.8(2) . . ? C2 N2 C4 126.06(19) . . ? C11 N3 C10 115.7(2) . . ? C11 N3 Cd1 125.31(15) . 1_545 ? C10 N3 Cd1 118.67(15) . 1_545 ? C6 S1 C5 91.89(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C2 C3 N1 -0.1(3) . . . . ? C7 C4 C5 S1 0.9(3) . . . . ? N2 C4 C5 S1 -175.83(17) . . . . ? S1 C6 C7 C4 0.5(3) . . . . ? S1 C6 C7 C8 -176.85(18) . . . . ? C5 C4 C7 C6 -0.9(3) . . . . ? N2 C4 C7 C6 175.7(2) . . . . ? C5 C4 C7 C8 176.2(2) . . . . ? N2 C4 C7 C8 -7.2(4) . . . . ? C6 C7 C8 C9 -10.7(4) . . . . ? C4 C7 C8 C9 172.5(2) . . . . ? C6 C7 C8 C12 166.8(2) . . . . ? C4 C7 C8 C12 -10.0(4) . . . . ? C12 C8 C9 C10 -3.7(4) . . . . ? C7 C8 C9 C10 174.1(2) . . . . ? C8 C9 C10 N3 1.6(4) . . . . ? N3 C11 C12 C8 0.1(4) . . . . ? C9 C8 C12 C11 2.9(4) . . . . ? C7 C8 C12 C11 -174.7(2) . . . . ? N2 C1 N1 C3 -0.3(2) . . . . ? N2 C1 N1 Cd1 -172.29(13) . . . . ? C2 C3 N1 C1 0.2(3) . . . . ? C2 C3 N1 Cd1 172.27(15) . . . . ? N3 Cd1 N1 C1 87.40(18) 1_565 . . . ? N3 Cd1 N1 C1 -92.60(18) 3_755 . . . ? N1 Cd1 N1 C1 24(100) 3_765 . . . ? Cl1 Cd1 N1 C1 176.18(18) . . . . ? Cl1 Cd1 N1 C1 -3.82(18) 3_765 . . . ? N3 Cd1 N1 C3 -82.96(18) 1_565 . . . ? N3 Cd1 N1 C3 97.04(18) 3_755 . . . ? N1 Cd1 N1 C3 -146(100) 3_765 . . . ? Cl1 Cd1 N1 C3 5.83(18) . . . . ? Cl1 Cd1 N1 C3 -174.17(18) 3_765 . . . ? N1 C1 N2 C2 0.2(3) . . . . ? N1 C1 N2 C4 177.64(19) . . . . ? C3 C2 N2 C1 -0.1(2) . . . . ? C3 C2 N2 C4 -177.52(19) . . . . ? C5 C4 N2 C1 -83.3(3) . . . . ? C7 C4 N2 C1 100.4(3) . . . . ? C5 C4 N2 C2 93.6(3) . . . . ? C7 C4 N2 C2 -82.7(3) . . . . ? C12 C11 N3 C10 -2.3(4) . . . . ? C12 C11 N3 Cd1 171.4(2) . . . 1_545 ? C9 C10 N3 C11 1.5(4) . . . . ? C9 C10 N3 Cd1 -172.7(2) . . . 1_545 ? C7 C6 S1 C5 0.0(2) . . . . ? C4 C5 S1 C6 -0.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.239 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.052 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 815011' #TrackingRef '- Sum-rev1.Cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 N10 O10 S2 Zn' _chemical_formula_sum 'C24 H32 N10 O10 S2 Zn' _chemical_formula_weight 750.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.0358(10) _cell_length_b 15.9866(17) _cell_length_c 12.5425(16) _cell_angle_alpha 90.00 _cell_angle_beta 116.0400(10) _cell_angle_gamma 90.00 _cell_volume 1627.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3007 _cell_measurement_theta_min 2.509 _cell_measurement_theta_max 25.155 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.951 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8944 _exptl_absorpt_correction_T_max 0.9026 _exptl_absorpt_process_details 'SADABS; BRUKER, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8014 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2847 _reflns_number_gt 2284 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (BRUKER 2000)' _computing_structure_solution 'SHELXTL (BRUKER 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2847 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0698 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.5000 0.0000 1.0000 0.03151(11) Uani 1 2 d S . . C1 C 0.6029(2) 0.05223(13) 0.80320(17) 0.0341(5) Uani 1 1 d . . . H1 H 0.7051 0.0274 0.8467 0.041 Uiso 1 1 calc R . . C3 C 0.3581(3) 0.09694(13) 0.74886(19) 0.0410(5) Uani 1 1 d . . . H3 H 0.2572 0.1087 0.7487 0.049 Uiso 1 1 calc R . . C2 C 0.3999(3) 0.11819(14) 0.66167(19) 0.0426(6) Uani 1 1 d . . . H2 H 0.3352 0.1467 0.5920 0.051 Uiso 1 1 calc R . . C5 C 0.6560(2) 0.09490(13) 0.63441(17) 0.0341(5) Uani 1 1 d . . . C4 C 0.7166(3) 0.02737(15) 0.60202(19) 0.0448(6) Uani 1 1 d . . . H4 H 0.6962 -0.0277 0.6153 0.054 Uiso 1 1 calc R . . C7 C 0.8037(3) 0.15964(15) 0.54808(19) 0.0459(6) Uani 1 1 d . . . H7 H 0.8485 0.2027 0.5217 0.055 Uiso 1 1 calc R . . C6 C 0.7054(2) 0.17148(13) 0.60262(17) 0.0340(5) Uani 1 1 d . . . C8 C 0.5969(3) 0.31323(13) 0.54153(19) 0.0379(5) Uani 1 1 d . . . H8 H 0.5759 0.3072 0.4624 0.046 Uiso 1 1 calc R . . C9 C 0.6171(3) 0.36406(15) 0.70411(19) 0.0493(6) Uani 1 1 d . . . H9 H 0.6120 0.4012 0.7594 0.059 Uiso 1 1 calc R . . C10 C 0.6690(3) 0.28484(15) 0.72697(19) 0.0503(6) Uani 1 1 d . . . H10 H 0.7066 0.2575 0.7996 0.060 Uiso 1 1 calc R . . C11 C 0.1013(3) -0.01204(19) 0.8806(3) 0.0725(9) Uani 1 1 d . . . H11A H 0.1057 -0.0277 0.8082 0.109 Uiso 1 1 d R . . H11B H 0.0059 0.0221 0.8627 0.109 Uiso 1 1 d R . . H11C H 0.0947 -0.0614 0.9218 0.109 Uiso 1 1 d R . . C12 C 0.2311(4) 0.17478(18) 0.2280(3) 0.0803(9) Uani 1 1 d . . . H12A H 0.1233 0.1588 0.2178 0.120 Uiso 1 1 d R . . H12B H 0.2679 0.1364 0.1858 0.120 Uiso 1 1 d R . . H12C H 0.2271 0.2303 0.1976 0.120 Uiso 1 1 d R . . N1 N 0.4854(2) 0.05559(10) 0.83779(14) 0.0332(4) Uani 1 1 d . . . N2 N 0.5569(2) 0.08928(10) 0.69664(14) 0.0332(4) Uani 1 1 d . . . N3 N 0.6558(2) 0.25189(10) 0.62236(14) 0.0349(4) Uani 1 1 d . . . N4 N 0.5725(2) 0.38259(10) 0.58696(14) 0.0362(4) Uani 1 1 d . . . N5 N 0.0696(3) 0.22641(17) 0.93444(19) 0.0620(6) Uani 1 1 d . . . O1 O 0.24592(16) 0.03267(10) 0.95408(13) 0.0449(4) Uani 1 1 d . . . H1A H 0.2312 0.0841 0.9349 0.067 Uiso 1 1 d R . . O2 O 0.3397(2) 0.17323(12) 0.34754(18) 0.0821(6) Uani 1 1 d . . . H2A H 0.2948 0.1932 0.3861 0.123 Uiso 1 1 d R . . O3 O 0.1955(2) 0.19827(12) 0.9273(2) 0.0888(7) Uani 1 1 d . . . O4 O -0.0351(2) 0.17783(13) 0.93686(18) 0.0762(6) Uani 1 1 d . . . O5 O 0.0572(2) 0.30282(13) 0.94037(19) 0.0767(6) Uani 1 1 d . . . S1 S 0.83532(8) 0.05626(4) 0.53376(6) 0.05609(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0375(2) 0.0295(2) 0.03162(19) 0.00177(15) 0.01896(15) 0.00019(16) C1 0.0372(12) 0.0325(12) 0.0335(12) 0.0052(10) 0.0164(10) 0.0024(10) C3 0.0407(12) 0.0442(13) 0.0438(13) 0.0064(11) 0.0238(11) 0.0085(11) C2 0.0426(13) 0.0481(14) 0.0391(13) 0.0129(11) 0.0198(11) 0.0112(11) C5 0.0408(12) 0.0364(12) 0.0300(11) 0.0045(9) 0.0201(9) 0.0048(10) C4 0.0611(15) 0.0374(12) 0.0436(13) 0.0051(11) 0.0299(12) 0.0079(11) C7 0.0524(14) 0.0473(14) 0.0480(14) 0.0088(12) 0.0314(12) 0.0027(12) C6 0.0398(12) 0.0332(12) 0.0332(12) 0.0042(10) 0.0198(10) 0.0027(10) C8 0.0527(14) 0.0338(12) 0.0318(12) 0.0037(10) 0.0227(11) 0.0006(11) C9 0.0755(16) 0.0415(14) 0.0320(13) -0.0013(11) 0.0246(12) 0.0062(13) C10 0.0773(17) 0.0441(14) 0.0302(12) 0.0052(11) 0.0243(12) 0.0075(13) C11 0.0422(15) 0.091(2) 0.078(2) -0.0053(17) 0.0199(14) -0.0063(15) C12 0.102(2) 0.0619(19) 0.073(2) -0.0077(17) 0.0351(19) -0.0122(19) N1 0.0395(10) 0.0309(10) 0.0329(9) 0.0021(8) 0.0191(8) 0.0007(8) N2 0.0406(10) 0.0319(9) 0.0324(10) 0.0037(8) 0.0209(8) 0.0007(8) N3 0.0443(10) 0.0317(10) 0.0332(10) 0.0037(8) 0.0211(8) -0.0003(8) N4 0.0450(10) 0.0322(10) 0.0321(10) 0.0010(8) 0.0176(8) 0.0018(8) N5 0.0578(14) 0.0784(18) 0.0570(14) 0.0178(13) 0.0319(12) 0.0226(14) O1 0.0367(8) 0.0480(9) 0.0496(9) 0.0075(8) 0.0187(7) 0.0037(7) O2 0.0890(14) 0.0748(14) 0.0714(14) 0.0015(11) 0.0250(12) 0.0175(12) O3 0.0875(14) 0.0759(14) 0.141(2) 0.0356(13) 0.0854(15) 0.0391(12) O4 0.0666(12) 0.0797(15) 0.0912(15) 0.0173(12) 0.0427(11) 0.0096(11) O5 0.0731(13) 0.0661(14) 0.1032(16) -0.0078(12) 0.0501(12) 0.0131(11) S1 0.0700(4) 0.0580(4) 0.0588(4) 0.0068(3) 0.0453(4) 0.0191(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N4 2.1248(17) 4_566 ? Zn1 N4 2.1248(17) 2_646 ? Zn1 N1 2.1703(16) . ? Zn1 N1 2.1703(16) 3_657 ? Zn1 O1 2.1713(14) . ? Zn1 O1 2.1713(14) 3_657 ? C1 N1 1.313(2) . ? C1 N2 1.350(2) . ? C1 H1 0.9300 . ? C3 C2 1.348(3) . ? C3 N1 1.370(3) . ? C3 H3 0.9300 . ? C2 N2 1.368(2) . ? C2 H2 0.9300 . ? C5 C4 1.351(3) . ? C5 C6 1.419(3) . ? C5 N2 1.426(2) . ? C4 S1 1.704(2) . ? C4 H4 0.9300 . ? C7 C6 1.351(3) . ? C7 S1 1.700(2) . ? C7 H7 0.9300 . ? C6 N3 1.419(2) . ? C8 N4 1.309(3) . ? C8 N3 1.341(2) . ? C8 H8 0.9300 . ? C9 C10 1.337(3) . ? C9 N4 1.374(3) . ? C9 H9 0.9300 . ? C10 N3 1.370(3) . ? C10 H10 0.9300 . ? C11 O1 1.418(3) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9599 . ? C12 O2 1.385(3) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9599 . ? N4 Zn1 2.1248(16) 2_656 ? N5 O5 1.232(3) . ? N5 O4 1.234(3) . ? N5 O3 1.263(2) . ? O1 H1A 0.8500 . ? O2 H2A 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Zn1 N4 180.00(4) 4_566 2_646 ? N4 Zn1 N1 89.87(6) 4_566 . ? N4 Zn1 N1 90.13(6) 2_646 . ? N4 Zn1 N1 90.13(6) 4_566 3_657 ? N4 Zn1 N1 89.87(6) 2_646 3_657 ? N1 Zn1 N1 180.0 . 3_657 ? N4 Zn1 O1 88.59(6) 4_566 . ? N4 Zn1 O1 91.41(6) 2_646 . ? N1 Zn1 O1 91.75(6) . . ? N1 Zn1 O1 88.25(6) 3_657 . ? N4 Zn1 O1 91.41(6) 4_566 3_657 ? N4 Zn1 O1 88.59(6) 2_646 3_657 ? N1 Zn1 O1 88.25(6) . 3_657 ? N1 Zn1 O1 91.75(6) 3_657 3_657 ? O1 Zn1 O1 180.0 . 3_657 ? N1 C1 N2 111.53(18) . . ? N1 C1 H1 124.2 . . ? N2 C1 H1 124.2 . . ? C2 C3 N1 110.40(18) . . ? C2 C3 H3 124.8 . . ? N1 C3 H3 124.8 . . ? C3 C2 N2 105.97(19) . . ? C3 C2 H2 127.0 . . ? N2 C2 H2 127.0 . . ? C4 C5 C6 112.70(18) . . ? C4 C5 N2 123.32(19) . . ? C6 C5 N2 123.96(18) . . ? C5 C4 S1 111.24(17) . . ? C5 C4 H4 124.4 . . ? S1 C4 H4 124.4 . . ? C6 C7 S1 111.59(17) . . ? C6 C7 H7 124.2 . . ? S1 C7 H7 124.2 . . ? C7 C6 N3 122.93(19) . . ? C7 C6 C5 112.27(19) . . ? N3 C6 C5 124.79(17) . . ? N4 C8 N3 112.15(18) . . ? N4 C8 H8 123.9 . . ? N3 C8 H8 123.9 . . ? C10 C9 N4 110.12(19) . . ? C10 C9 H9 124.9 . . ? N4 C9 H9 124.9 . . ? C9 C10 N3 106.50(19) . . ? C9 C10 H10 126.8 . . ? N3 C10 H10 126.8 . . ? O1 C11 H11A 109.7 . . ? O1 C11 H11B 110.0 . . ? H11A C11 H11B 109.5 . . ? O1 C11 H11C 108.8 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O2 C12 H12A 109.6 . . ? O2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O2 C12 H12C 109.4 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 N1 C3 105.19(16) . . ? C1 N1 Zn1 124.59(14) . . ? C3 N1 Zn1 130.16(13) . . ? C1 N2 C2 106.91(16) . . ? C1 N2 C5 125.11(17) . . ? C2 N2 C5 127.97(17) . . ? C8 N3 C10 106.36(17) . . ? C8 N3 C6 125.56(17) . . ? C10 N3 C6 127.91(17) . . ? C8 N4 C9 104.86(18) . . ? C8 N4 Zn1 126.71(14) . 2_656 ? C9 N4 Zn1 128.23(14) . 2_656 ? O5 N5 O4 122.1(2) . . ? O5 N5 O3 117.8(2) . . ? O4 N5 O3 120.1(3) . . ? C11 O1 Zn1 128.08(15) . . ? C11 O1 H1A 108.5 . . ? Zn1 O1 H1A 108.9 . . ? C12 O2 H2A 109.4 . . ? C7 S1 C4 92.20(11) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.278 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.043 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 815012' #TrackingRef '- Sum-rev1.Cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 Cd N10 O10 S2' _chemical_formula_sum 'C24 H32 Cd N10 O10 S2' _chemical_formula_weight 797.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.0887(8) _cell_length_b 16.3768(15) _cell_length_c 12.6796(14) _cell_angle_alpha 90.00 _cell_angle_beta 116.0150(10) _cell_angle_gamma 90.00 _cell_volume 1696.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2028 _cell_measurement_theta_min 2.178 _cell_measurement_theta_max 21.595 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9067 _exptl_absorpt_correction_T_max 0.9214 _exptl_absorpt_process_details 'SADABS, BRUKER(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8477 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2973 _reflns_number_gt 2117 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (BRUKER 2000)' _computing_structure_solution 'SHELXTL (BRUKER 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0178P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2973 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0561 _refine_ls_wR_factor_gt 0.0529 _refine_ls_goodness_of_fit_ref 0.845 _refine_ls_restrained_S_all 0.845 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.0000 0.0000 0.03950(11) Uani 1 2 d S . . C1 C 0.4013(4) 0.05213(17) 0.2079(3) 0.0444(8) Uani 1 1 d . . . H1 H 0.3013 0.0264 0.1652 0.053 Uiso 1 1 calc R . . C3 C 0.6414(4) 0.09916(18) 0.2605(3) 0.0495(8) Uani 1 1 d . . . H3 H 0.7413 0.1120 0.2607 0.059 Uiso 1 1 calc R . . C2 C 0.5974(4) 0.12013(18) 0.3453(3) 0.0516(9) Uani 1 1 d . . . H2 H 0.6594 0.1496 0.4132 0.062 Uiso 1 1 calc R . . C5 C 0.3442(4) 0.09492(18) 0.3723(2) 0.0412(8) Uani 1 1 d . . . C4 C 0.2833(4) 0.02921(19) 0.4046(3) 0.0538(9) Uani 1 1 d . . . H4 H 0.3040 -0.0246 0.3919 0.065 Uiso 1 1 calc R . . C7 C 0.1944(4) 0.15752(19) 0.4558(3) 0.0575(9) Uani 1 1 d . . . H7 H 0.1487 0.1995 0.4811 0.069 Uiso 1 1 calc R . . C6 C 0.2919(4) 0.16923(18) 0.4025(2) 0.0428(8) Uani 1 1 d . . . C8 C 0.4010(4) 0.30853(19) 0.4590(3) 0.0488(8) Uani 1 1 d . . . H8 H 0.4251 0.3035 0.5380 0.059 Uiso 1 1 calc R . . C9 C 0.3726(4) 0.3566(2) 0.2950(3) 0.0655(10) Uani 1 1 d . . . H9 H 0.3743 0.3924 0.2387 0.079 Uiso 1 1 calc R . . C10 C 0.3210(4) 0.2790(2) 0.2746(3) 0.0634(10) Uani 1 1 d . . . H10 H 0.2805 0.2518 0.2030 0.076 Uiso 1 1 calc R . . C12 C 0.7610(6) 0.3258(2) 0.2674(4) 0.1077(16) Uani 1 1 d . . . H12A H 0.8691 0.3463 0.2881 0.161 Uiso 1 1 d R . . H12B H 0.7677 0.2698 0.2919 0.161 Uiso 1 1 d R . . H12C H 0.7100 0.3577 0.3058 0.161 Uiso 1 1 d R . . C11 C 0.9118(5) -0.0127(3) 0.1205(4) 0.1069(15) Uani 1 1 d . . . H11A H 0.8894 -0.0700 0.1066 0.160 Uiso 1 1 d R . . H11B H 0.9379 -0.0004 0.2008 0.160 Uiso 1 1 d R . . H11C H 1.0029 0.0016 0.1050 0.160 Uiso 1 1 d R . . N1 N 0.5187(3) 0.05641(14) 0.1740(2) 0.0433(6) Uani 1 1 d . . . N2 N 0.4432(3) 0.08948(13) 0.3118(2) 0.0398(6) Uani 1 1 d . . . N3 N 0.3397(3) 0.24765(15) 0.3800(2) 0.0436(6) Uani 1 1 d . . . N4 N 0.4226(3) 0.37572(15) 0.4114(2) 0.0502(7) Uani 1 1 d . . . N5 N 0.9305(5) 0.2231(3) 0.0660(3) 0.0850(11) Uani 1 1 d . . . O1 O 0.7729(3) 0.03240(13) 0.04642(19) 0.0673(7) Uani 1 1 d . . . H1A H 0.7887 0.0823 0.0666 0.101 Uiso 1 1 d R . . O2 O 0.6711(4) 0.33016(17) 0.1508(3) 0.1236(12) Uani 1 1 d . . . H2A H 0.7288 0.3191 0.1180 0.185 Uiso 1 1 d R . . O3 O 0.8120(4) 0.19522(18) 0.0796(3) 0.1291(13) Uani 1 1 d . . . O4 O 1.0349(4) 0.17710(19) 0.0613(3) 0.0979(10) Uani 1 1 d . . . O5 O 0.9392(3) 0.2977(2) 0.0582(3) 0.0985(10) Uani 1 1 d . . . S1 S 0.16484(12) 0.05691(6) 0.47116(8) 0.0708(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0483(2) 0.03758(18) 0.04008(18) -0.00315(17) 0.02626(15) -0.00077(17) C1 0.052(2) 0.0420(19) 0.0444(19) -0.0098(16) 0.0258(17) -0.0076(15) C3 0.052(2) 0.055(2) 0.054(2) -0.0077(17) 0.0340(18) -0.0084(17) C2 0.053(2) 0.056(2) 0.048(2) -0.0184(17) 0.0237(18) -0.0172(17) C5 0.052(2) 0.0420(19) 0.0382(18) -0.0081(15) 0.0277(16) -0.0076(15) C4 0.069(2) 0.048(2) 0.058(2) -0.0080(16) 0.0399(19) -0.0109(16) C7 0.068(2) 0.059(2) 0.062(2) -0.0109(18) 0.045(2) -0.0054(18) C6 0.053(2) 0.046(2) 0.0371(18) -0.0078(15) 0.0263(16) -0.0046(16) C8 0.067(2) 0.045(2) 0.0387(19) -0.0059(17) 0.0272(17) 0.0003(17) C9 0.101(3) 0.051(2) 0.041(2) 0.0046(18) 0.028(2) -0.005(2) C10 0.095(3) 0.058(2) 0.0350(19) -0.0066(18) 0.026(2) -0.008(2) C12 0.148(5) 0.085(3) 0.096(4) -0.007(3) 0.058(3) -0.007(3) C11 0.055(3) 0.150(4) 0.107(3) 0.003(3) 0.028(3) -0.001(3) N1 0.0504(17) 0.0416(16) 0.0455(16) -0.0050(13) 0.0279(14) -0.0028(13) N2 0.0513(17) 0.0360(15) 0.0390(15) -0.0084(12) 0.0261(13) -0.0074(12) N3 0.0552(17) 0.0398(16) 0.0396(15) -0.0051(13) 0.0244(14) -0.0012(13) N4 0.0689(19) 0.0418(17) 0.0432(17) -0.0005(14) 0.0275(15) -0.0006(14) N5 0.075(3) 0.112(4) 0.083(2) -0.034(3) 0.049(2) -0.041(3) O1 0.0508(15) 0.0751(17) 0.0754(17) -0.0152(13) 0.0272(13) -0.0126(12) O2 0.152(3) 0.113(3) 0.091(2) 0.011(2) 0.039(2) 0.050(2) O3 0.135(3) 0.116(3) 0.200(3) -0.066(2) 0.133(3) -0.067(2) O4 0.085(2) 0.110(2) 0.115(2) -0.0318(19) 0.058(2) -0.0219(18) O5 0.083(2) 0.102(2) 0.123(2) 0.007(2) 0.0556(18) -0.0168(19) S1 0.0871(7) 0.0761(7) 0.0747(6) -0.0104(6) 0.0590(6) -0.0242(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N4 2.282(2) 4_565 ? Cd1 N4 2.282(2) 2_645 ? Cd1 N1 2.329(2) . ? Cd1 N1 2.329(2) 3_655 ? Cd1 O1 2.345(2) . ? Cd1 O1 2.345(2) 3_655 ? C1 N1 1.315(3) . ? C1 N2 1.347(3) . ? C1 H1 0.9300 . ? C3 C2 1.347(4) . ? C3 N1 1.365(3) . ? C3 H3 0.9300 . ? C2 N2 1.369(3) . ? C2 H2 0.9300 . ? C5 C4 1.353(4) . ? C5 C6 1.419(4) . ? C5 N2 1.419(3) . ? C4 S1 1.696(3) . ? C4 H4 0.9300 . ? C7 C6 1.343(4) . ? C7 S1 1.694(3) . ? C7 H7 0.9300 . ? C6 N3 1.424(3) . ? C8 N4 1.311(3) . ? C8 N3 1.348(3) . ? C8 H8 0.9300 . ? C9 C10 1.340(4) . ? C9 N4 1.375(4) . ? C9 H9 0.9300 . ? C10 N3 1.371(4) . ? C10 H10 0.9300 . ? C12 O2 1.342(4) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C11 O1 1.408(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? N4 Cd1 2.282(2) 2_655 ? N5 O5 1.231(4) . ? N5 O4 1.234(4) . ? N5 O3 1.249(4) . ? O1 H1A 0.8500 . ? O2 H2A 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cd1 N4 180.00(5) 4_565 2_645 ? N4 Cd1 N1 89.51(8) 4_565 . ? N4 Cd1 N1 90.49(8) 2_645 . ? N4 Cd1 N1 90.49(8) 4_565 3_655 ? N4 Cd1 N1 89.51(8) 2_645 3_655 ? N1 Cd1 N1 180.00(15) . 3_655 ? N4 Cd1 O1 89.17(8) 4_565 . ? N4 Cd1 O1 90.83(8) 2_645 . ? N1 Cd1 O1 92.46(8) . . ? N1 Cd1 O1 87.54(8) 3_655 . ? N4 Cd1 O1 90.83(8) 4_565 3_655 ? N4 Cd1 O1 89.17(8) 2_645 3_655 ? N1 Cd1 O1 87.54(8) . 3_655 ? N1 Cd1 O1 92.46(8) 3_655 3_655 ? O1 Cd1 O1 180.00(15) . 3_655 ? N1 C1 N2 111.9(3) . . ? N1 C1 H1 124.1 . . ? N2 C1 H1 124.1 . . ? C2 C3 N1 110.3(3) . . ? C2 C3 H3 124.8 . . ? N1 C3 H3 124.8 . . ? C3 C2 N2 106.3(3) . . ? C3 C2 H2 126.9 . . ? N2 C2 H2 126.9 . . ? C4 C5 C6 111.8(3) . . ? C4 C5 N2 123.7(3) . . ? C6 C5 N2 124.5(3) . . ? C5 C4 S1 111.8(2) . . ? C5 C4 H4 124.1 . . ? S1 C4 H4 124.1 . . ? C6 C7 S1 111.7(2) . . ? C6 C7 H7 124.2 . . ? S1 C7 H7 124.2 . . ? C7 C6 C5 112.7(3) . . ? C7 C6 N3 123.8(3) . . ? C5 C6 N3 123.5(3) . . ? N4 C8 N3 112.0(3) . . ? N4 C8 H8 124.0 . . ? N3 C8 H8 124.0 . . ? C10 C9 N4 110.3(3) . . ? C10 C9 H9 124.9 . . ? N4 C9 H9 124.9 . . ? C9 C10 N3 106.4(3) . . ? C9 C10 H10 126.8 . . ? N3 C10 H10 126.8 . . ? O2 C12 H12A 109.7 . . ? O2 C12 H12B 109.2 . . ? H12A C12 H12B 109.5 . . ? O2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 C11 H11A 109.5 . . ? O1 C11 H11B 109.3 . . ? H11A C11 H11B 109.5 . . ? O1 C11 H11C 109.7 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 N1 C3 105.0(2) . . ? C1 N1 Cd1 123.8(2) . . ? C3 N1 Cd1 131.2(2) . . ? C1 N2 C2 106.4(3) . . ? C1 N2 C5 125.6(3) . . ? C2 N2 C5 127.9(2) . . ? C8 N3 C10 106.4(3) . . ? C8 N3 C6 125.5(3) . . ? C10 N3 C6 127.9(3) . . ? C8 N4 C9 104.9(3) . . ? C8 N4 Cd1 126.7(2) . 2_655 ? C9 N4 Cd1 128.1(2) . 2_655 ? O5 N5 O4 121.6(4) . . ? O5 N5 O3 117.6(4) . . ? O4 N5 O3 120.7(4) . . ? C11 O1 Cd1 126.1(2) . . ? C11 O1 H1A 108.7 . . ? Cd1 O1 H1A 108.3 . . ? C12 O2 H2A 109.4 . . ? C7 S1 C4 92.04(16) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.374 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.053 #===END