# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Xian-Ming Zhang' _publ_contact_author_email ZHANGXM@DNS.SXNU.EDU.CN _publ_section_title ; Red Phosphorescent Cuprous Halide/Pseudohalide Coordination Polymers with Pyrimidine-2-thionates as Co-ligands ; loop_ _publ_author_name 'Xian-Ming Zhang.' 'Zheng-Ming Hao.' 'Jun Wang.' # Attachment 'zhang.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 737922' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H3 Cl Cu2 N2 S' _chemical_formula_weight 273.67 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' Cu Cu 0.3201 1.2651 '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' Cl Cl 0.1484 0.1585 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 3.8822(8) _cell_length_b 8.0900(17) _cell_length_c 10.318(2) _cell_angle_alpha 96.751(4) _cell_angle_beta 91.577(4) _cell_angle_gamma 93.729(4) _cell_volume 320.93(11) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.832 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 264 _exptl_absorpt_coefficient_mu 7.264 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1914 _exptl_absorpt_correction_T_max 0.8683 _exptl_absorpt_process_details 'SADABS, Sheldrick 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1777 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0795 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 26.99 _reflns_number_total 1331 _reflns_number_gt 1049 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0735P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1331 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1475 _refine_ls_wR_factor_gt 0.1390 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 Cu1 Cu 0.1436(2) 0.60477(13) 0.89183(9) 0.0321(3) Uani 1 1 d . . . Cu2 Cu -0.5961(3) 1.06910(15) 1.12623(11) 0.0492(4) Uani 1 1 d . . . S1 S -0.3153(4) 0.7218(2) 0.98338(15) 0.0190(4) Uani 1 1 d . . . Cl1 Cl 0.0249(5) 0.7781(3) 0.70882(16) 0.0286(5) Uani 1 1 d . . . N1 N -0.5304(14) 0.8681(8) 1.2098(5) 0.0204(12) Uani 1 1 d . . . N2 N -0.2802(14) 0.6070(7) 1.2110(5) 0.0191(12) Uani 1 1 d . . . C1 C -0.3810(16) 0.7339(8) 1.1514(6) 0.0173(14) Uani 1 1 d . . . C2 C -0.3461(19) 0.6132(9) 1.3402(6) 0.0228(15) Uani 1 1 d . . . H2A H -0.2861 0.5257 1.3854 0.027 Uiso 1 1 calc R . . C3 C -0.498(2) 0.7448(10) 1.4054(7) 0.0271(17) Uani 1 1 d . . . H3A H -0.5400 0.7486 1.4940 0.033 Uiso 1 1 calc R . . C4 C -0.5871(19) 0.8697(10) 1.3367(7) 0.0258(16) Uani 1 1 d . . . H4A H -0.6913 0.9598 1.3798 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0292(5) 0.0386(6) 0.0282(5) -0.0055(4) 0.0017(4) 0.0175(4) Cu2 0.0684(9) 0.0388(7) 0.0485(7) 0.0249(6) 0.0152(6) 0.0240(6) S1 0.0193(8) 0.0248(10) 0.0140(8) 0.0033(7) 0.0026(6) 0.0086(7) Cl1 0.0323(10) 0.0360(11) 0.0202(9) 0.0072(8) 0.0055(7) 0.0144(8) N1 0.017(3) 0.023(3) 0.021(3) 0.001(2) 0.002(2) 0.008(2) N2 0.021(3) 0.022(3) 0.016(3) 0.004(2) 0.005(2) 0.004(2) C1 0.016(3) 0.020(4) 0.015(3) -0.003(3) -0.003(2) 0.003(3) C2 0.038(4) 0.021(4) 0.012(3) 0.014(3) 0.005(3) 0.001(3) C3 0.037(4) 0.034(4) 0.011(3) 0.004(3) 0.008(3) 0.006(4) C4 0.028(4) 0.025(4) 0.023(4) -0.006(3) 0.005(3) 0.009(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 Cu1 N2 2.016(6) 2_567 ? Cu1 S1 2.2506(18) . ? Cu1 S1 2.371(2) 1_655 ? Cu1 Cl1 2.530(2) . ? Cu2 N1 1.955(6) . ? Cu2 S1 2.182(2) 2_477 ? Cu2 Cl1 2.669(2) 2_477 ? Cu2 Cu2 2.850(2) 2_477 ? S1 C1 1.752(7) . ? S1 Cu2 2.182(2) 2_477 ? S1 Cu1 2.371(2) 1_455 ? Cl1 Cu2 2.669(2) 2_477 ? N1 C4 1.333(9) . ? N1 C1 1.351(8) . ? N2 C1 1.331(9) . ? N2 C2 1.361(8) . ? N2 Cu1 2.016(6) 2_567 ? C2 C3 1.368(10) . ? C2 H2A 0.9300 . ? C3 C4 1.357(11) . ? C3 H3A 0.9300 . ? C4 H4A 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 N2 Cu1 S1 141.65(18) 2_567 . ? N2 Cu1 S1 101.50(17) 2_567 1_655 ? S1 Cu1 S1 114.25(8) . 1_655 ? N2 Cu1 Cl1 100.56(16) 2_567 . ? S1 Cu1 Cl1 84.66(7) . . ? S1 Cu1 Cl1 103.61(8) 1_655 . ? N1 Cu2 S1 174.69(18) . 2_477 ? N1 Cu2 Cl1 100.34(17) . 2_477 ? S1 Cu2 Cl1 82.71(7) 2_477 2_477 ? N1 Cu2 Cu2 95.39(17) . 2_477 ? S1 Cu2 Cu2 80.20(6) 2_477 2_477 ? Cl1 Cu2 Cu2 153.21(8) 2_477 2_477 ? C1 S1 Cu2 121.6(2) . 2_477 ? C1 S1 Cu1 122.2(2) . . ? Cu2 S1 Cu1 104.80(8) 2_477 . ? C1 S1 Cu1 102.5(2) . 1_455 ? Cu2 S1 Cu1 85.72(7) 2_477 1_455 ? Cu1 S1 Cu1 114.25(8) . 1_455 ? Cu1 Cl1 Cu2 84.94(6) . 2_477 ? C4 N1 C1 116.5(6) . . ? C4 N1 Cu2 119.3(5) . . ? C1 N1 Cu2 123.5(5) . . ? C1 N2 C2 116.1(6) . . ? C1 N2 Cu1 121.2(4) . 2_567 ? C2 N2 Cu1 121.1(5) . 2_567 ? N2 C1 N1 125.3(6) . . ? N2 C1 S1 116.3(5) . . ? N1 C1 S1 118.3(5) . . ? N2 C2 C3 121.6(6) . . ? N2 C2 H2A 119.2 . . ? C3 C2 H2A 119.2 . . ? C4 C3 C2 117.9(6) . . ? C4 C3 H3A 121.1 . . ? C2 C3 H3A 121.1 . . ? N1 C4 C3 122.5(7) . . ? N1 C4 H4A 118.7 . . ? C3 C4 H4A 118.7 . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.875 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.212 #====================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 737923' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H6 Cu3 N5 S3' _chemical_formula_weight 470.99 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.764(3) _cell_length_b 7.732(2) _cell_length_c 16.538(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.929(5) _cell_angle_gamma 90.00 _cell_volume 1346.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description column _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 5.151 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2102 _exptl_absorpt_correction_T_max 0.8608 _exptl_absorpt_process_details 'SADABS, Sheldrick 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6344 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.00 _reflns_number_total 2901 _reflns_number_gt 2329 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0497P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2901 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 Cu1 Cu 0.58014(6) 0.22894(8) 0.22278(4) 0.02826(19) Uani 1 1 d . . . Cu2 Cu 0.43811(6) 0.51600(8) 0.23027(4) 0.0317(2) Uani 1 1 d . . . Cu3 Cu 0.64809(6) 0.51885(8) 0.14893(4) 0.0324(2) Uani 1 1 d . . . S1 S 0.44169(12) 0.48889(16) 0.09391(8) 0.0271(3) Uani 1 1 d . . . S2 S 0.71378(11) 0.75740(16) 0.22722(7) 0.0224(3) Uani 1 1 d . . . S3 S 0.47309(13) 0.26583(19) 0.32767(8) 0.0334(3) Uani 1 1 d . . . N1 N 0.3235(5) 0.2417(6) -0.0020(3) 0.0455(13) Uani 1 1 d . . . N2 N 0.4661(4) 0.1480(5) 0.1202(3) 0.0281(10) Uani 1 1 d . . . N3 N 0.5340(4) 0.6932(5) 0.3140(3) 0.0277(10) Uani 1 1 d . . . N4 N 0.7006(3) 0.8853(5) 0.3730(2) 0.0196(8) Uani 1 1 d . . . N5 N 0.2435(5) 0.0897(7) 0.2708(3) 0.0503(14) Uani 1 1 d . . . C1 C 0.2943(6) 0.0764(9) -0.0193(4) 0.060(2) Uani 1 1 d . . . H1A H 0.2361 0.0509 -0.0677 0.072 Uiso 1 1 calc R . . C2 C 0.3455(7) -0.0575(8) 0.0306(4) 0.060(2) Uani 1 1 d . . . H2A H 0.3223 -0.1717 0.0180 0.071 Uiso 1 1 calc R . . C3 C 0.4328(6) -0.0140(7) 0.1002(4) 0.0469(16) Uani 1 1 d . . . H3A H 0.4704 -0.1022 0.1350 0.056 Uiso 1 1 calc R . . C4 C 0.4079(5) 0.2737(6) 0.0683(3) 0.0287(12) Uani 1 1 d . . . C5 C 0.4839(5) 0.7159(7) 0.3815(3) 0.0378(14) Uani 1 1 d . . . H5A H 0.4084 0.6597 0.3841 0.045 Uiso 1 1 calc R . . C6 C 0.5389(5) 0.8172(7) 0.4458(3) 0.0340(13) Uani 1 1 d . . . H6A H 0.5046 0.8279 0.4928 0.041 Uiso 1 1 calc R . . C7 C 0.6485(5) 0.9039(7) 0.4385(3) 0.0283(11) Uani 1 1 d . . . H7A H 0.6868 0.9776 0.4808 0.034 Uiso 1 1 calc R . . C8 C 0.6427(4) 0.7774(6) 0.3129(3) 0.0198(10) Uani 1 1 d . . . C9 C 0.3373(5) 0.1613(7) 0.2929(3) 0.0346(13) 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 Cu1 0.0195(3) 0.0346(4) 0.0288(4) 0.0041(3) 0.0007(3) -0.0027(3) Cu2 0.0239(4) 0.0341(4) 0.0374(4) -0.0115(3) 0.0072(3) -0.0003(3) Cu3 0.0246(4) 0.0262(4) 0.0458(4) -0.0059(3) 0.0057(3) 0.0017(3) S1 0.0279(7) 0.0214(6) 0.0291(7) -0.0018(5) -0.0011(5) 0.0037(5) S2 0.0166(6) 0.0289(7) 0.0217(6) -0.0025(5) 0.0042(5) -0.0030(5) S3 0.0278(7) 0.0420(8) 0.0316(7) 0.0031(6) 0.0088(6) -0.0066(6) N1 0.051(3) 0.033(3) 0.040(3) -0.007(2) -0.021(2) 0.003(2) N2 0.026(2) 0.023(2) 0.032(2) 0.0001(18) -0.0035(18) 0.0015(17) N3 0.027(2) 0.028(2) 0.031(2) -0.0109(19) 0.0142(19) -0.0117(18) N4 0.020(2) 0.019(2) 0.019(2) 0.0002(16) 0.0030(16) -0.0018(16) N5 0.030(3) 0.055(4) 0.069(4) 0.008(3) 0.018(3) -0.011(3) C1 0.060(5) 0.040(4) 0.063(5) -0.014(3) -0.027(4) -0.007(3) C2 0.064(5) 0.026(3) 0.071(5) -0.010(3) -0.026(4) -0.006(3) C3 0.051(4) 0.029(3) 0.052(4) 0.005(3) -0.012(3) 0.003(3) C4 0.026(3) 0.024(3) 0.033(3) -0.003(2) 0.000(2) 0.004(2) C5 0.032(3) 0.038(3) 0.048(4) -0.009(3) 0.020(3) -0.015(2) C6 0.039(3) 0.037(3) 0.030(3) -0.010(2) 0.017(3) -0.006(2) C7 0.035(3) 0.025(3) 0.023(3) -0.003(2) 0.002(2) 0.001(2) C8 0.018(2) 0.019(2) 0.022(2) 0.0015(19) 0.0041(19) 0.0010(18) C9 0.027(3) 0.038(3) 0.045(3) 0.013(3) 0.022(3) -0.002(2) _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 Cu1 N2 1.979(4) . ? Cu1 S2 2.2122(14) 2_645 ? Cu1 S3 2.2901(15) . ? Cu1 Cu2 2.7124(10) . ? Cu1 Cu3 2.7240(11) . ? Cu2 N5 2.032(5) 2 ? Cu2 N3 2.067(4) . ? Cu2 S1 2.2731(16) . ? Cu2 S3 2.4955(17) . ? Cu2 Cu3 2.8591(11) . ? Cu3 N4 2.024(4) 2_645 ? Cu3 S1 2.2320(15) . ? Cu3 S2 2.2803(14) . ? S1 C4 1.737(5) . ? S2 C8 1.750(5) . ? S2 Cu1 2.2122(14) 2_655 ? S3 C9 1.665(6) . ? N1 C1 1.333(8) . ? N1 C4 1.342(6) . ? N2 C3 1.326(7) . ? N2 C4 1.361(6) . ? N3 C8 1.342(6) . ? N3 C5 1.348(6) . ? N4 C7 1.327(6) . ? N4 C8 1.348(6) . ? N4 Cu3 2.024(4) 2_655 ? N5 C9 1.144(7) . ? N5 Cu2 2.032(5) 2_545 ? C1 C2 1.367(9) . ? C1 H1A 0.9300 . ? C2 C3 1.368(8) . ? C2 H2A 0.9300 . ? C3 H3A 0.9300 . ? C5 C6 1.354(7) . ? C5 H5A 0.9300 . ? C6 C7 1.384(7) . ? C6 H6A 0.9300 . ? C7 H7A 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 N2 Cu1 S2 138.41(13) . 2_645 ? N2 Cu1 S3 111.66(13) . . ? S2 Cu1 S3 109.09(5) 2_645 . ? N2 Cu1 Cu2 92.44(12) . . ? S2 Cu1 Cu2 115.63(4) 2_645 . ? S3 Cu1 Cu2 59.13(4) . . ? N2 Cu1 Cu3 92.98(13) . . ? S2 Cu1 Cu3 75.19(4) 2_645 . ? S3 Cu1 Cu3 117.44(5) . . ? Cu2 Cu1 Cu3 63.46(3) . . ? N5 Cu2 N3 99.6(2) 2 . ? N5 Cu2 S1 103.35(16) 2 . ? N3 Cu2 S1 128.14(12) . . ? N5 Cu2 S3 103.83(17) 2 . ? N3 Cu2 S3 95.36(13) . . ? S1 Cu2 S3 122.53(5) . . ? N5 Cu2 Cu1 141.17(16) 2 . ? N3 Cu2 Cu1 111.40(13) . . ? S1 Cu2 Cu1 75.76(4) . . ? S3 Cu2 Cu1 51.97(4) . . ? N5 Cu2 Cu3 147.80(16) 2 . ? N3 Cu2 Cu3 88.64(11) . . ? S1 Cu2 Cu3 49.97(4) . . ? S3 Cu2 Cu3 106.33(4) . . ? Cu1 Cu2 Cu3 58.47(2) . . ? N4 Cu3 S1 130.12(11) 2_645 . ? N4 Cu3 S2 110.35(11) 2_645 . ? S1 Cu3 S2 118.76(5) . . ? N4 Cu3 Cu1 87.77(11) 2_645 . ? S1 Cu3 Cu1 76.14(4) . . ? S2 Cu3 Cu1 119.44(5) . . ? N4 Cu3 Cu2 145.50(11) 2_645 . ? S1 Cu3 Cu2 51.25(4) . . ? S2 Cu3 Cu2 85.50(4) . . ? Cu1 Cu3 Cu2 58.07(2) . . ? C4 S1 Cu3 109.85(17) . . ? C4 S1 Cu2 106.57(18) . . ? Cu3 S1 Cu2 78.78(5) . . ? C8 S2 Cu1 106.18(16) . 2_655 ? C8 S2 Cu3 113.25(16) . . ? Cu1 S2 Cu3 107.52(5) 2_655 . ? C9 S3 Cu1 102.75(19) . . ? C9 S3 Cu2 98.5(2) . . ? Cu1 S3 Cu2 68.90(4) . . ? C1 N1 C4 116.7(5) . . ? C3 N2 C4 116.9(5) . . ? C3 N2 Cu1 126.9(4) . . ? C4 N2 Cu1 116.0(3) . . ? C8 N3 C5 116.6(4) . . ? C8 N3 Cu2 128.9(3) . . ? C5 N3 Cu2 114.3(3) . . ? C7 N4 C8 117.4(4) . . ? C7 N4 Cu3 125.6(3) . 2_655 ? C8 N4 Cu3 116.8(3) . 2_655 ? C9 N5 Cu2 157.3(5) . 2_545 ? N1 C1 C2 123.3(6) . . ? N1 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C3 C2 C1 116.3(6) . . ? C3 C2 H2A 121.9 . . ? C1 C2 H2A 121.9 . . ? N2 C3 C2 123.0(5) . . ? N2 C3 H3A 118.5 . . ? C2 C3 H3A 118.5 . . ? N1 C4 N2 123.8(5) . . ? N1 C4 S1 117.3(4) . . ? N2 C4 S1 119.0(4) . . ? N3 C5 C6 122.7(5) . . ? N3 C5 H5A 118.6 . . ? C6 C5 H5A 118.6 . . ? C5 C6 C7 117.0(5) . . ? C5 C6 H6A 121.5 . . ? C7 C6 H6A 121.5 . . ? N4 C7 C6 122.0(5) . . ? N4 C7 H7A 119.0 . . ? C6 C7 H7A 119.0 . . ? N3 C8 N4 124.1(4) . . ? N3 C8 S2 119.8(3) . . ? N4 C8 S2 116.0(3) . . ? N5 C9 S3 178.4(5) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.741 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.131 #====================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 737924' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H6 Cu3 I N4 S2' _chemical_formula_weight 539.81 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.4687(16) _cell_length_b 7.7318(12) _cell_length_c 15.289(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.702(3) _cell_angle_gamma 90.00 _cell_volume 1231.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.912 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 7.961 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.3283 _exptl_absorpt_correction_T_max 0.8570 _exptl_absorpt_process_details 'SADABS, Sheldrick 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6039 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 28.48 _reflns_number_total 2835 _reflns_number_gt 2125 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0402P)^2^+0.6850P] 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 2835 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.1010 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _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 I1 I 0.46578(5) 0.23069(7) 0.40480(4) 0.03390(18) Uani 1 1 d . . . Cu1 Cu 0.70043(10) 0.25959(13) 0.36198(6) 0.0295(3) Uani 1 1 d . . . Cu2 Cu 0.86175(10) -0.04336(13) 0.35605(7) 0.0331(3) Uani 1 1 d . . . Cu3 Cu 0.63207(9) -0.03640(13) 0.43226(7) 0.0338(3) Uani 1 1 d . . . S1 S 0.83087(17) 0.0003(2) 0.49777(12) 0.0191(4) Uani 1 1 d . . . S2 S 0.73388(17) 0.2314(2) 0.22271(12) 0.0220(4) Uani 1 1 d . . . N1 N 0.8021(5) 0.3407(8) 0.4709(4) 0.0200(13) Uani 1 1 d . . . N2 N 0.9368(6) 0.2527(8) 0.5977(4) 0.0257(15) Uani 1 1 d . . . N3 N 0.9616(5) 0.1017(7) 0.2760(4) 0.0189(13) Uani 1 1 d . . . N4 N 0.9556(6) 0.2927(8) 0.1534(4) 0.0237(14) Uani 1 1 d . . . C1 C 0.8986(6) 0.2101(8) 0.2169(4) 0.0154(15) Uani 1 1 d . . . C2 C 1.0807(7) 0.2698(10) 0.1531(6) 0.032(2) Uani 1 1 d . . . H2A H 1.1222 0.3242 0.1096 0.038 Uiso 1 1 calc R . . C3 C 1.1523(7) 0.1699(11) 0.2137(5) 0.0290(19) Uani 1 1 d . . . H3A H 1.2409 0.1614 0.2140 0.035 Uiso 1 1 calc R . . C4 C 1.0882(7) 0.0840(9) 0.2732(5) 0.0246(17) Uani 1 1 d . . . H4A H 1.1336 0.0107 0.3133 0.030 Uiso 1 1 calc R . . C5 C 0.8601(7) 0.2156(9) 0.5233(5) 0.0185(15) Uani 1 1 d . . . C6 C 0.8143(7) 0.5070(10) 0.4973(6) 0.0304(19) Uani 1 1 d . . . H6A H 0.7748 0.5945 0.4627 0.036 Uiso 1 1 calc R . . C7 C 0.8862(7) 0.5482(10) 0.5765(5) 0.0298(19) Uani 1 1 d . . . H7A H 0.8912 0.6614 0.5971 0.036 Uiso 1 1 calc R . . C8 C 0.9486(7) 0.4173(9) 0.6225(5) 0.0276(18) Uani 1 1 d . . . H8A H 1.0014 0.4440 0.6732 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0242(3) 0.0382(3) 0.0399(3) 0.0069(3) 0.0061(2) 0.0070(2) Cu1 0.0302(6) 0.0375(6) 0.0202(5) 0.0005(4) -0.0006(4) 0.0045(4) Cu2 0.0456(7) 0.0307(6) 0.0249(6) -0.0038(4) 0.0126(5) -0.0132(5) Cu3 0.0280(6) 0.0346(6) 0.0371(6) -0.0140(5) -0.0058(5) -0.0028(4) S1 0.0209(9) 0.0187(9) 0.0170(9) -0.0007(7) -0.0015(7) -0.0024(7) S2 0.0164(9) 0.0295(10) 0.0198(9) 0.0055(8) 0.0008(7) 0.0011(8) N1 0.018(3) 0.026(3) 0.016(3) 0.006(3) 0.005(3) 0.005(3) N2 0.029(4) 0.027(4) 0.019(3) 0.001(3) -0.009(3) -0.005(3) N3 0.017(3) 0.021(3) 0.018(3) 0.001(3) -0.003(3) -0.002(2) N4 0.024(3) 0.025(3) 0.024(3) 0.008(3) 0.011(3) 0.008(3) C1 0.013(3) 0.015(3) 0.016(3) 0.001(3) -0.010(3) 0.002(3) C2 0.027(4) 0.034(5) 0.037(5) 0.016(4) 0.018(4) 0.007(4) C3 0.020(4) 0.048(5) 0.021(4) 0.012(4) 0.011(3) 0.005(4) C4 0.024(4) 0.022(4) 0.026(4) 0.001(3) -0.005(3) 0.004(3) C5 0.017(4) 0.025(4) 0.015(4) -0.002(3) 0.005(3) 0.003(3) C6 0.035(5) 0.019(4) 0.039(5) 0.003(4) 0.011(4) 0.003(3) C7 0.035(5) 0.017(4) 0.037(5) -0.010(4) 0.002(4) -0.003(3) C8 0.029(4) 0.022(4) 0.031(5) -0.011(4) -0.002(4) -0.002(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 I1 Cu1 2.6139(12) . ? I1 Cu3 2.7066(12) . ? Cu1 N1 1.987(6) . ? Cu1 S2 2.203(2) . ? Cu1 Cu3 2.6565(15) . ? Cu1 Cu2 2.8943(15) . ? Cu2 N3 2.025(6) . ? Cu2 S1 2.248(2) . ? Cu2 S2 2.290(2) 2_645 ? Cu2 Cu3 2.7747(15) . ? Cu3 N4 2.016(6) 2_645 ? Cu3 S1 2.2363(19) . ? S1 C5 1.730(7) . ? S2 C1 1.743(7) . ? S2 Cu2 2.290(2) 2_655 ? N1 C6 1.350(9) . ? N1 C5 1.360(9) . ? N2 C8 1.330(9) . ? N2 C5 1.357(8) . ? N3 C4 1.337(9) . ? N3 C1 1.355(8) . ? N4 C2 1.322(9) . ? N4 C1 1.350(9) . ? N4 Cu3 2.016(6) 2_655 ? C2 C3 1.371(10) . ? C3 C4 1.358(10) . ? C6 C7 1.397(11) . ? C7 C8 1.362(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 I1 Cu3 59.88(3) . . ? N1 Cu1 S2 135.92(18) . . ? N1 Cu1 I1 104.79(17) . . ? S2 Cu1 I1 118.50(6) . . ? N1 Cu1 Cu3 94.37(18) . . ? S2 Cu1 Cu3 112.38(7) . . ? I1 Cu1 Cu3 61.80(3) . . ? N1 Cu1 Cu2 90.93(17) . . ? S2 Cu1 Cu2 74.95(6) . . ? I1 Cu1 Cu2 120.29(4) . . ? Cu3 Cu1 Cu2 59.80(4) . . ? N3 Cu2 S1 129.16(17) . . ? N3 Cu2 S2 109.17(17) . 2_645 ? S1 Cu2 S2 121.58(8) . 2_645 ? N3 Cu2 Cu3 139.79(17) . . ? S1 Cu2 Cu3 51.59(5) . . ? S2 Cu2 Cu3 83.33(6) 2_645 . ? N3 Cu2 Cu1 84.75(17) . . ? S1 Cu2 Cu1 73.03(6) . . ? S2 Cu2 Cu1 113.95(6) 2_645 . ? Cu3 Cu2 Cu1 55.84(4) . . ? N4 Cu3 S1 135.85(19) 2_645 . ? N4 Cu3 Cu1 115.18(19) 2_645 . ? S1 Cu3 Cu1 78.21(6) . . ? N4 Cu3 I1 98.91(18) 2_645 . ? S1 Cu3 I1 121.89(6) . . ? Cu1 Cu3 I1 58.33(3) . . ? N4 Cu3 Cu2 94.14(18) 2_645 . ? S1 Cu3 Cu2 51.96(6) . . ? Cu1 Cu3 Cu2 64.36(4) . . ? I1 Cu3 Cu2 121.37(5) . . ? C5 S1 Cu3 111.0(2) . . ? C5 S1 Cu2 108.8(2) . . ? Cu3 S1 Cu2 76.45(7) . . ? C1 S2 Cu1 108.2(2) . . ? C1 S2 Cu2 115.3(2) . 2_655 ? Cu1 S2 Cu2 109.25(9) . 2_655 ? C6 N1 C5 118.5(6) . . ? C6 N1 Cu1 125.3(5) . . ? C5 N1 Cu1 116.1(5) . . ? C8 N2 C5 118.1(6) . . ? C4 N3 C1 117.4(6) . . ? C4 N3 Cu2 122.3(5) . . ? C1 N3 Cu2 119.9(5) . . ? C2 N4 C1 116.7(6) . . ? C2 N4 Cu3 118.2(5) . 2_655 ? C1 N4 Cu3 124.9(5) . 2_655 ? N4 C1 N3 123.5(6) . . ? N4 C1 S2 120.2(5) . . ? N3 C1 S2 116.3(5) . . ? N4 C2 C3 123.2(7) . . ? C4 C3 C2 117.1(7) . . ? N3 C4 C3 121.9(7) . . ? N2 C5 N1 122.4(6) . . ? N2 C5 S1 118.0(5) . . ? N1 C5 S1 119.5(5) . . ? N1 C6 C7 120.2(7) . . ? C8 C7 C6 117.9(7) . . ? N2 C8 C7 122.5(7) . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.472 _refine_diff_density_min -0.917 _refine_diff_density_rms 0.214 #====================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 737925' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H12 Cu11 I7 N8 S4' _chemical_formula_weight 2031.82 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Othorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 17.3499(12) _cell_length_b 15.4640(10) _cell_length_c 13.2336(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3550.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.801 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3672 _exptl_absorpt_coefficient_mu 12.794 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.0823 _exptl_absorpt_correction_T_max 0.7839 _exptl_absorpt_process_details 'SADABS, Sheldrick 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16998 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4002 _reflns_number_gt 3448 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0899P)^2^+82.5477P] 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 4002 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1816 _refine_ls_wR_factor_gt 0.1599 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _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 Cu1 Cu 0.17955(15) -0.2500 -0.2188(2) 0.0365(6) Uani 1 2 d S . . Cu2 Cu 0.21676(16) -0.2500 -0.6726(2) 0.0364(6) Uani 1 2 d S . . Cu3 Cu 0.31042(10) -0.07747(14) -0.65855(15) 0.0402(5) Uani 1 1 d . . . Cu4 Cu 0.06191(15) -0.2500 -0.5711(2) 0.0372(6) Uani 1 2 d S . . Cu5 Cu 0.03457(14) -0.2500 -0.1119(2) 0.0343(6) Uani 1 2 d S . . Cu6 Cu 0.19601(17) -0.2500 -0.4498(2) 0.0522(8) Uani 1 2 d S . . Cu7 Cu 0.2262(2) 0.0522(2) -0.6569(4) 0.0526(6) Uani 0.592(3) 1 d P A 1 Cu7' Cu 0.2218(3) 0.0635(3) -0.5835(6) 0.0526(6) Uani 0.408(3) 1 d P A 2 Cu8 Cu 0.2700(2) 0.1618(2) -0.4398(3) 0.0526(6) Uani 0.592(3) 1 d P . 1 Cu8' Cu 0.2255(3) 0.1903(4) -0.3483(5) 0.0526(6) Uani 0.408(3) 1 d P . 2 I1 I 0.06599(7) -0.2500 -0.34763(8) 0.0249(3) Uani 1 2 d S . . I2 I 0.30985(7) -0.2500 -0.31833(10) 0.0325(3) Uani 1 2 d S A . I3 I 0.15073(6) 0.2500 -0.50669(9) 0.0243(3) Uani 1 2 d S . . I4 I 0.26901(5) -0.02206(5) -0.84055(6) 0.0252(2) Uani 1 1 d . . . I5 I 0.12683(7) -0.2500 -0.82916(9) 0.0263(3) Uani 1 2 d S . . I6 I 0.37247(7) -0.2500 -0.69273(10) 0.0278(3) Uani 1 2 d S . . S1 S 0.32246(18) 0.13369(19) -0.6049(2) 0.0236(6) Uani 1 1 d . . . S2 S 0.20897(17) -0.1292(2) -0.5644(2) 0.0225(6) Uani 1 1 d . A . N1 N 0.4085(5) -0.0111(6) -0.6245(7) 0.0139(18) Uani 1 1 d . A . N2 N 0.4738(6) 0.1255(6) -0.6082(8) 0.023(2) Uani 1 1 d . . . N3 N 0.0562(5) -0.1257(6) -0.5960(8) 0.019(2) Uani 1 1 d . . . N4 N 0.1250(6) 0.0055(7) -0.6164(10) 0.032(3) Uani 1 1 d . . . C1 C 0.4083(6) 0.0769(8) -0.6139(8) 0.015(2) Uani 1 1 d . A . C2 C 0.4780(8) -0.0491(8) -0.6260(9) 0.023(3) Uani 1 1 d . . . H2A H 0.4800 -0.1089 -0.6329 0.028 Uiso 1 1 calc R A . C3 C 0.5465(6) -0.0046(9) -0.6180(10) 0.025(3) Uani 1 1 d . A . H3A H 0.5937 -0.0331 -0.6187 0.030 Uiso 1 1 calc R . . C4 C 0.5420(6) 0.0831(8) -0.6089(9) 0.022(2) Uani 1 1 d . A . H4A H 0.5873 0.1148 -0.6030 0.026 Uiso 1 1 calc R . . C5 C 0.1219(7) -0.0790(7) -0.5965(9) 0.023(3) Uani 1 1 d . A . C6 C -0.0088(7) -0.0845(8) -0.6150(9) 0.023(3) Uani 1 1 d . A . H6A H -0.0546 -0.1156 -0.6176 0.027 Uiso 1 1 calc R . . C7 C -0.0104(7) 0.0037(8) -0.6311(9) 0.020(2) Uani 1 1 d . . . H7A H -0.0569 0.0324 -0.6412 0.024 Uiso 1 1 calc R A . C8 C 0.0572(8) 0.0473(8) -0.6318(11) 0.028(3) Uani 1 1 d . A . H8A H 0.0572 0.1066 -0.6430 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0285(13) 0.0421(15) 0.0390(14) 0.000 0.0013(11) 0.000 Cu2 0.0338(14) 0.0351(14) 0.0404(15) 0.000 -0.0024(11) 0.000 Cu3 0.0242(9) 0.0457(11) 0.0507(11) 0.0154(9) -0.0058(8) -0.0114(8) Cu4 0.0287(13) 0.0164(11) 0.0666(18) 0.000 0.0046(12) 0.000 Cu5 0.0250(12) 0.0155(11) 0.0625(17) 0.000 0.0047(11) 0.000 Cu6 0.0345(15) 0.075(2) 0.0474(17) 0.000 0.0017(13) 0.000 Cu7 0.0346(10) 0.0328(10) 0.0905(19) 0.0055(12) -0.0104(11) -0.0034(8) Cu7' 0.0346(10) 0.0328(10) 0.0905(19) 0.0055(12) -0.0104(11) -0.0034(8) Cu8 0.0346(10) 0.0328(10) 0.0905(19) 0.0055(12) -0.0104(11) -0.0034(8) Cu8' 0.0346(10) 0.0328(10) 0.0905(19) 0.0055(12) -0.0104(11) -0.0034(8) I1 0.0220(6) 0.0318(6) 0.0210(6) 0.000 -0.0006(4) 0.000 I2 0.0188(6) 0.0426(8) 0.0361(7) 0.000 0.0049(5) 0.000 I3 0.0197(6) 0.0250(6) 0.0282(6) 0.000 -0.0016(4) 0.000 I4 0.0244(4) 0.0248(4) 0.0264(4) 0.0019(3) -0.0025(3) -0.0017(3) I5 0.0228(6) 0.0270(6) 0.0290(6) 0.000 0.0013(4) 0.000 I6 0.0218(6) 0.0184(6) 0.0432(7) 0.000 0.0009(5) 0.000 S1 0.0203(14) 0.0181(14) 0.0324(16) -0.0001(12) 0.0052(12) 0.0049(12) S2 0.0149(13) 0.0218(15) 0.0308(16) 0.0006(12) 0.0001(11) 0.0003(11) N1 0.013(4) 0.011(4) 0.018(5) 0.002(3) -0.001(3) 0.000(3) N2 0.026(5) 0.013(5) 0.029(5) 0.001(4) -0.008(4) -0.001(4) N3 0.012(4) 0.014(5) 0.030(5) 0.000(4) 0.006(4) -0.001(4) N4 0.025(6) 0.019(5) 0.054(8) -0.001(5) 0.000(5) 0.003(5) C1 0.013(5) 0.025(6) 0.008(5) 0.000(4) 0.000(4) -0.002(4) C2 0.033(7) 0.016(6) 0.021(6) 0.006(5) 0.007(5) 0.003(5) C3 0.003(5) 0.038(7) 0.033(7) 0.005(6) -0.002(4) 0.001(5) C4 0.009(5) 0.024(6) 0.033(7) 0.007(5) -0.005(5) -0.007(5) C5 0.035(7) 0.012(5) 0.022(6) -0.009(4) 0.004(5) 0.002(5) C6 0.015(6) 0.029(7) 0.023(6) 0.003(5) -0.003(4) -0.004(5) C7 0.017(6) 0.018(6) 0.026(6) 0.001(5) 0.002(5) 0.000(5) C8 0.026(7) 0.013(6) 0.044(8) -0.004(5) 0.001(6) 0.002(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 Cu1 S1 2.347(4) 2 ? Cu1 S1 2.347(4) 8_656 ? Cu1 I1 2.606(3) . ? Cu1 I2 2.617(3) . ? Cu1 Cu5 2.886(4) . ? Cu2 S2 2.358(3) . ? Cu2 S2 2.358(3) 7 ? Cu2 I5 2.593(3) . ? Cu2 Cu8' 2.694(7) 8_655 ? Cu2 Cu8' 2.694(7) 2_554 ? Cu2 I6 2.715(3) . ? Cu2 Cu6 2.971(4) . ? Cu2 Cu4 3.004(4) . ? Cu3 N1 2.038(9) . ? Cu3 S2 2.300(4) . ? Cu3 Cu7 2.481(4) . ? Cu3 I4 2.655(2) . ? Cu3 Cu7' 2.847(6) . ? Cu3 I6 2.912(2) . ? Cu4 N3 1.953(10) 7 ? Cu4 N3 1.953(10) . ? Cu4 Cu6 2.827(4) . ? Cu4 I1 2.958(3) . ? Cu5 N2 1.931(10) 8_656 ? Cu5 N2 1.931(10) 2 ? Cu6 S2 2.417(4) 7 ? Cu6 S2 2.417(4) . ? Cu6 I1 2.630(3) . ? Cu6 I2 2.632(3) . ? Cu7 N4 1.973(12) . ? Cu7 S1 2.203(5) . ? Cu7 I4 2.789(5) . ? Cu7' N4 1.953(13) . ? Cu7' S1 2.075(6) . ? Cu8 S1 2.406(6) . ? Cu8 I4 2.617(4) 2 ? Cu8 I3 2.632(4) . ? Cu8 I5 2.685(4) 2 ? Cu8 Cu8 2.729(7) 7_565 ? Cu8' Cu8' 1.845(11) 7_565 ? Cu8' I4 2.606(5) 2 ? Cu8' I3 2.632(6) . ? Cu8' Cu2 2.694(7) 2 ? Cu8' I5 2.735(5) 2 ? Cu8' I6 2.824(6) 2 ? I3 Cu8' 2.632(6) 7_565 ? I3 Cu8 2.632(4) 7_565 ? I4 Cu8' 2.606(6) 2_554 ? I4 Cu8 2.617(4) 2_554 ? I5 Cu8 2.685(4) 2_554 ? I5 Cu8 2.685(4) 8_655 ? I5 Cu8' 2.735(5) 2_554 ? I5 Cu8' 2.735(5) 8_655 ? I6 Cu8' 2.824(6) 8_655 ? I6 Cu8' 2.824(6) 2_554 ? I6 Cu3 2.912(2) 7 ? S1 C1 1.732(11) . ? S1 Cu1 2.347(4) 2_554 ? S2 C5 1.751(13) . ? N1 C2 1.341(16) . ? N1 C1 1.368(15) . ? N2 C4 1.353(16) . ? N2 C1 1.364(15) . ? N2 Cu5 1.931(10) 2_554 ? N3 C6 1.319(15) . ? N3 C5 1.350(16) . ? N4 C5 1.334(17) . ? N4 C8 1.357(17) . ? C2 C3 1.378(17) . ? C2 H2A 0.9300 . ? C3 C4 1.364(18) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C6 C7 1.380(17) . ? C6 H6A 0.9300 . ? C7 C8 1.353(18) . ? C7 H7A 0.9300 . ? C8 H8A 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 S1 Cu1 S1 100.07(18) 2 8_656 ? S1 Cu1 I1 114.14(10) 2 . ? S1 Cu1 I1 114.14(10) 8_656 . ? S1 Cu1 I2 109.64(11) 2 . ? S1 Cu1 I2 109.64(11) 8_656 . ? I1 Cu1 I2 108.90(10) . . ? S1 Cu1 Cu5 70.88(10) 2 . ? S1 Cu1 Cu5 70.88(10) 8_656 . ? I1 Cu1 Cu5 70.22(9) . . ? I2 Cu1 Cu5 179.11(13) . . ? S2 Cu2 S2 104.79(18) . 7 ? S2 Cu2 I5 116.79(10) . . ? S2 Cu2 I5 116.79(10) 7 . ? S2 Cu2 Cu8' 144.76(16) . 8_655 ? S2 Cu2 Cu8' 105.91(14) 7 8_655 ? I5 Cu2 Cu8' 62.28(14) . 8_655 ? S2 Cu2 Cu8' 105.91(14) . 2_554 ? S2 Cu2 Cu8' 144.76(16) 7 2_554 ? I5 Cu2 Cu8' 62.28(14) . 2_554 ? Cu8' Cu2 Cu8' 40.0(2) 8_655 2_554 ? S2 Cu2 I6 96.70(10) . . ? S2 Cu2 I6 96.70(10) 7 . ? I5 Cu2 I6 121.37(11) . . ? Cu8' Cu2 I6 62.95(14) 8_655 . ? Cu8' Cu2 I6 62.95(14) 2_554 . ? S2 Cu2 Cu6 52.41(9) . . ? S2 Cu2 Cu6 52.41(9) 7 . ? I5 Cu2 Cu6 136.05(12) . . ? Cu8' Cu2 Cu6 154.35(14) 8_655 . ? Cu8' Cu2 Cu6 154.35(14) 2_554 . ? I6 Cu2 Cu6 102.58(11) . . ? S2 Cu2 Cu4 71.15(10) . . ? S2 Cu2 Cu4 71.15(10) 7 . ? I5 Cu2 Cu4 79.58(10) . . ? Cu8' Cu2 Cu4 135.94(16) 8_655 . ? Cu8' Cu2 Cu4 135.94(16) 2_554 . ? I6 Cu2 Cu4 159.05(12) . . ? Cu6 Cu2 Cu4 56.47(10) . . ? N1 Cu3 S2 134.0(3) . . ? N1 Cu3 Cu7 94.7(3) . . ? S2 Cu3 Cu7 79.96(14) . . ? N1 Cu3 I4 105.3(3) . . ? S2 Cu3 I4 113.36(11) . . ? Cu7 Cu3 I4 65.66(13) . . ? N1 Cu3 Cu7' 89.3(3) . . ? S2 Cu3 Cu7' 70.38(15) . . ? Cu7 Cu3 Cu7' 19.93(14) . . ? I4 Cu3 Cu7' 85.58(16) . . ? N1 Cu3 I6 100.8(3) . . ? S2 Cu3 I6 92.77(10) . . ? Cu7 Cu3 I6 163.61(12) . . ? I4 Cu3 I6 104.76(8) . . ? Cu7' Cu3 I6 162.85(15) . . ? N3 Cu4 N3 159.7(6) 7 . ? N3 Cu4 Cu6 97.9(3) 7 . ? N3 Cu4 Cu6 97.9(3) . . ? N3 Cu4 I1 99.8(3) 7 . ? N3 Cu4 I1 99.8(3) . . ? Cu6 Cu4 I1 54.02(9) . . ? N3 Cu4 Cu2 88.3(3) 7 . ? N3 Cu4 Cu2 88.3(3) . . ? Cu6 Cu4 Cu2 61.18(10) . . ? I1 Cu4 Cu2 115.20(11) . . ? N2 Cu5 N2 170.9(6) 8_656 2 ? N2 Cu5 Cu1 94.5(3) 8_656 . ? N2 Cu5 Cu1 94.5(3) 2 . ? S2 Cu6 S2 101.23(19) 7 . ? S2 Cu6 I1 113.73(11) 7 . ? S2 Cu6 I1 113.73(11) . . ? S2 Cu6 I2 110.19(11) 7 . ? S2 Cu6 I2 110.19(11) . . ? I1 Cu6 I2 107.70(12) . . ? S2 Cu6 Cu4 73.74(11) 7 . ? S2 Cu6 Cu4 73.74(11) . . ? I1 Cu6 Cu4 65.54(9) . . ? I2 Cu6 Cu4 173.24(14) . . ? S2 Cu6 Cu2 50.63(9) 7 . ? S2 Cu6 Cu2 50.63(9) . . ? I1 Cu6 Cu2 127.89(13) . . ? I2 Cu6 Cu2 124.41(13) . . ? Cu4 Cu6 Cu2 62.35(10) . . ? N4 Cu7 S1 143.1(5) . . ? N4 Cu7 Cu3 103.3(4) . . ? S1 Cu7 Cu3 91.05(15) . . ? N4 Cu7 I4 108.9(4) . . ? S1 Cu7 I4 107.81(18) . . ? Cu3 Cu7 I4 60.18(11) . . ? N4 Cu7' S1 159.0(6) . . ? N4 Cu7' Cu3 92.0(4) . . ? S1 Cu7' Cu3 84.2(2) . . ? S1 Cu8 I4 113.86(16) . 2 ? S1 Cu8 I3 94.91(16) . . ? I4 Cu8 I3 113.17(13) 2 . ? S1 Cu8 I5 109.55(16) . 2 ? I4 Cu8 I5 108.55(15) 2 2 ? I3 Cu8 I5 116.37(13) . 2 ? S1 Cu8 Cu8 100.40(11) . 7_565 ? I4 Cu8 Cu8 145.63(10) 2 7_565 ? I3 Cu8 Cu8 58.77(8) . 7_565 ? I5 Cu8 Cu8 59.46(8) 2 7_565 ? Cu8' Cu8' I4 176.92(13) 7_565 2 ? Cu8' Cu8' I3 69.48(12) 7_565 . ? I4 Cu8' I3 113.5(2) 2 . ? Cu8' Cu8' Cu2 69.98(12) 7_565 2 ? I4 Cu8' Cu2 107.1(2) 2 2 ? I3 Cu8' Cu2 138.6(2) . 2 ? Cu8' Cu8' I5 70.29(11) 7_565 2 ? I4 Cu8' I5 107.37(18) 2 2 ? I3 Cu8' I5 114.6(2) . 2 ? Cu2 Cu8' I5 57.06(12) 2 2 ? Cu8' Cu8' I6 70.93(11) 7_565 2 ? I4 Cu8' I6 108.7(2) 2 2 ? I3 Cu8' I6 99.77(17) . 2 ? Cu2 Cu8' I6 58.88(15) 2 2 ? I5 Cu8' I6 112.7(2) 2 2 ? Cu1 I1 Cu6 71.81(10) . . ? Cu1 I1 Cu4 132.24(9) . . ? Cu6 I1 Cu4 60.44(9) . . ? Cu1 I2 Cu6 71.60(10) . . ? Cu8' I3 Cu8' 41.0(2) . 7_565 ? Cu8' I3 Cu8 33.19(16) . . ? Cu8' I3 Cu8 61.74(15) 7_565 . ? Cu8' I3 Cu8 61.74(15) . 7_565 ? Cu8' I3 Cu8 33.19(16) 7_565 7_565 ? Cu8 I3 Cu8 62.45(15) . 7_565 ? Cu8' I4 Cu8 33.45(16) 2_554 2_554 ? Cu8' I4 Cu3 72.74(15) 2_554 . ? Cu8 I4 Cu3 105.00(11) 2_554 . ? Cu8' I4 Cu7 117.08(16) 2_554 . ? Cu8 I4 Cu7 135.11(12) 2_554 . ? Cu3 I4 Cu7 54.17(10) . . ? Cu2 I5 Cu8 91.97(11) . 2_554 ? Cu2 I5 Cu8 91.97(11) . 8_655 ? Cu8 I5 Cu8 61.07(15) 2_554 8_655 ? Cu2 I5 Cu8' 60.67(15) . 2_554 ? Cu8 I5 Cu8' 32.18(16) 2_554 2_554 ? Cu8 I5 Cu8' 59.76(14) 8_655 2_554 ? Cu2 I5 Cu8' 60.67(15) . 8_655 ? Cu8 I5 Cu8' 59.76(14) 2_554 8_655 ? Cu8 I5 Cu8' 32.18(16) 8_655 8_655 ? Cu8' I5 Cu8' 39.4(2) 2_554 8_655 ? Cu2 I6 Cu8' 58.17(12) . 8_655 ? Cu2 I6 Cu8' 58.17(12) . 2_554 ? Cu8' I6 Cu8' 38.1(2) 8_655 2_554 ? Cu2 I6 Cu3 67.47(4) . 7 ? Cu8' I6 Cu3 65.89(12) 8_655 7 ? Cu8' I6 Cu3 100.95(12) 2_554 7 ? Cu2 I6 Cu3 67.47(4) . . ? Cu8' I6 Cu3 100.95(12) 8_655 . ? Cu8' I6 Cu3 65.89(12) 2_554 . ? Cu3 I6 Cu3 132.72(8) 7 . ? C1 S1 Cu7' 117.9(4) . . ? C1 S1 Cu7 109.9(4) . . ? Cu7' S1 Cu7 26.5(2) . . ? C1 S1 Cu1 110.9(4) . 2_554 ? Cu7' S1 Cu1 118.4(2) . 2_554 ? Cu7 S1 Cu1 103.09(18) . 2_554 ? C1 S1 Cu8 118.6(4) . . ? Cu7' S1 Cu8 69.7(2) . . ? Cu7 S1 Cu8 95.74(19) . . ? Cu1 S1 Cu8 116.05(16) 2_554 . ? C5 S2 Cu3 112.0(4) . . ? C5 S2 Cu2 104.7(4) . . ? Cu3 S2 Cu2 84.41(13) . . ? C5 S2 Cu6 114.5(4) . . ? Cu3 S2 Cu6 132.84(16) . . ? Cu2 S2 Cu6 76.96(12) . . ? C2 N1 C1 116.1(10) . . ? C2 N1 Cu3 121.7(8) . . ? C1 N1 Cu3 121.4(7) . . ? C4 N2 C1 117.5(10) . . ? C4 N2 Cu5 123.3(8) . 2_554 ? C1 N2 Cu5 119.0(8) . 2_554 ? C6 N3 C5 117.5(10) . . ? C6 N3 Cu4 123.4(8) . . ? C5 N3 Cu4 119.0(8) . . ? C5 N4 C8 117.5(12) . . ? C5 N4 Cu7' 116.1(9) . . ? C8 N4 Cu7' 124.1(9) . . ? C5 N4 Cu7 116.6(9) . . ? C8 N4 Cu7 123.8(9) . . ? Cu7' N4 Cu7 29.2(3) . . ? N2 C1 N1 123.4(10) . . ? N2 C1 S1 115.7(9) . . ? N1 C1 S1 120.9(8) . . ? N1 C2 C3 123.7(11) . . ? N1 C2 H2A 118.1 . . ? C3 C2 H2A 118.1 . . ? C4 C3 C2 116.9(11) . . ? C4 C3 H3A 121.5 . . ? C2 C3 H3A 121.5 . . ? N2 C4 C3 122.2(11) . . ? N2 C4 H4A 118.9 . . ? C3 C4 H4A 118.9 . . ? N4 C5 N3 124.0(12) . . ? N4 C5 S2 116.6(10) . . ? N3 C5 S2 119.3(9) . . ? N3 C6 C7 121.6(11) . . ? N3 C6 H6A 119.2 . . ? C7 C6 H6A 119.2 . . ? C8 C7 C6 118.4(12) . . ? C8 C7 H7A 120.8 . . ? C6 C7 H7A 120.8 . . ? C7 C8 N4 120.9(11) . . ? C7 C8 H8A 119.6 . . ? N4 C8 H8A 119.6 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 5.093 _refine_diff_density_min -3.715 _refine_diff_density_rms 0.636