Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Sally Brooker' 'Katie Heslop' _publ_contact_author_name 'Dr Sally Brooker' _publ_contact_author_address ; Department of Chemistry University of Otago PO Box 56 Dunedin NEW ZEALAND ; _publ_contact_author_email SBROOKER@ALKALI.OTAGO.AC.NZ _publ_section_title ; Monomeric, Trimeric and Polymeric Assemblies of Dicopper(II) Complexes of a Triazolate-Containing Schiff-base Macrocycle ; data_pbt _database_code_CSD 207829 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H27 Cl2 N11 O8 Pb2' _chemical_formula_weight 1034.81 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' O O 0.0106 0.0060 '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' Pb Pb -3.3944 10.1111 '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 12.025(5) _cell_length_b 11.018(5) _cell_length_c 21.943(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 94.246(5) _cell_angle_gamma 90.000(5) _cell_volume 2899.3(19) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 11.848 _exptl_absorpt_correction_type Semi-empirical(SADABS) _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35598 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.70 _reflns_number_total 5996 _reflns_number_gt 5022 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0603P)^2^+19.1966P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5996 _refine_ls_number_parameters 393 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 Pb1 Pb 0.43481(2) 0.04813(3) 0.380336(13) 0.01954(10) Uani 1 1 d . . . Pb2 Pb 0.72139(2) 0.32703(3) 0.391803(13) 0.02305(10) Uani 1 1 d . . . N1 N 0.5203(6) 0.1649(6) 0.3037(3) 0.0211(14) Uani 1 1 d . . . N2 N 0.6047(5) 0.2466(6) 0.3074(3) 0.0201(14) Uani 1 1 d . . . C3 C 0.5948(7) 0.3100(7) 0.2560(3) 0.0208(16) Uani 1 1 d . . . N3 N 0.5096(5) 0.2738(6) 0.2187(3) 0.0190(13) Uani 1 1 d . . . C5 C 0.4652(6) 0.1853(7) 0.2506(3) 0.0185(15) Uani 1 1 d . . . C6 C 0.3587(7) 0.1242(7) 0.2363(3) 0.0215(16) Uani 1 1 d . . . C7 C 0.3010(8) 0.1396(9) 0.1751(4) 0.033(2) Uani 1 1 d . . . H7A H 0.2760 0.0603 0.1592 0.039 Uiso 1 1 calc R . . H7B H 0.3523 0.1759 0.1476 0.039 Uiso 1 1 calc R . . H7C H 0.2363 0.1929 0.1779 0.039 Uiso 1 1 calc R . . N4 N 0.3221(6) 0.0636(6) 0.2805(3) 0.0218(14) Uani 1 1 d . . . C8 C 0.2130(7) 0.0073(8) 0.2737(4) 0.0264(18) Uani 1 1 d . . . H8A H 0.2174 -0.0687 0.2499 0.032 Uiso 1 1 calc R . . H8B H 0.1599 0.0625 0.2509 0.032 Uiso 1 1 calc R . . C9 C 0.1711(7) -0.0210(8) 0.3356(4) 0.0266(18) Uani 1 1 d . . . H9A H 0.1018 -0.0692 0.3293 0.032 Uiso 1 1 calc R . . H9B H 0.2272 -0.0724 0.3587 0.032 Uiso 1 1 calc R . . C10 C 0.1479(7) 0.0868(8) 0.3738(4) 0.0237(17) Uani 1 1 d . . . H10A H 0.0933 0.1404 0.3511 0.028 Uiso 1 1 calc R . . H10B H 0.1153 0.0600 0.4117 0.028 Uiso 1 1 calc R . . N5 N 0.2513(6) 0.1542(6) 0.3895(3) 0.0213(14) Uani 1 1 d . . . C11 C 0.1474(7) 0.3365(8) 0.4174(4) 0.032(2) Uani 1 1 d . . . H11A H 0.1095 0.3570 0.3777 0.038 Uiso 1 1 calc R . . H11B H 0.1696 0.4113 0.4393 0.038 Uiso 1 1 calc R . . H11C H 0.0968 0.2899 0.4415 0.038 Uiso 1 1 calc R . . C12 C 0.2474(7) 0.2633(8) 0.4081(3) 0.0236(17) Uani 1 1 d . . . C13 C 0.3564(7) 0.3246(7) 0.4180(3) 0.0213(16) Uani 1 1 d . . . N6 N 0.4493(5) 0.2571(6) 0.4153(3) 0.0213(14) Uani 1 1 d . . . N7 N 0.5333(6) 0.3382(7) 0.4185(3) 0.0259(15) Uani 1 1 d . . . C15 C 0.4852(7) 0.4466(7) 0.4236(3) 0.0211(16) Uani 1 1 d . . . N8 N 0.3744(6) 0.4410(6) 0.4242(3) 0.0256(15) Uani 1 1 d . . . C16 C 0.5525(7) 0.5565(8) 0.4207(3) 0.0251(18) Uani 1 1 d . . . C17 C 0.4994(8) 0.6763(8) 0.4279(4) 0.033(2) Uani 1 1 d . . . H17A H 0.5428 0.7231 0.4593 0.039 Uiso 1 1 calc R . . H17B H 0.4234 0.6648 0.4403 0.039 Uiso 1 1 calc R . . H17C H 0.4968 0.7202 0.3890 0.039 Uiso 1 1 calc R . . N9 N 0.6549(6) 0.5372(7) 0.4098(3) 0.0281(16) Uani 1 1 d . . . C18 C 0.7291(8) 0.6407(8) 0.4003(4) 0.033(2) Uani 1 1 d . . . H18A H 0.7590 0.6732 0.4402 0.039 Uiso 1 1 calc R . . H18B H 0.6867 0.7062 0.3781 0.039 Uiso 1 1 calc R . . C19 C 0.8244(8) 0.5993(10) 0.3636(4) 0.038(2) Uani 1 1 d . . . H19A H 0.8781 0.6670 0.3613 0.045 Uiso 1 1 calc R . . H19B H 0.8637 0.5315 0.3855 0.045 Uiso 1 1 calc R . . C20 C 0.7881(7) 0.5584(8) 0.2996(4) 0.0258(18) Uani 1 1 d . . . H20A H 0.7469 0.6252 0.2779 0.031 Uiso 1 1 calc R . . H20B H 0.8551 0.5408 0.2775 0.031 Uiso 1 1 calc R . . N10 N 0.7188(6) 0.4527(6) 0.2985(3) 0.0243(15) Uani 1 1 d . . . C21 C 0.6680(8) 0.4761(8) 0.1893(4) 0.0292(19) Uani 1 1 d . . . H21A H 0.6173 0.5459 0.1875 0.035 Uiso 1 1 calc R . . H21B H 0.6444 0.4185 0.1568 0.035 Uiso 1 1 calc R . . H21C H 0.7440 0.5039 0.1836 0.035 Uiso 1 1 calc R . . C22 C 0.6655(6) 0.4155(8) 0.2497(3) 0.0205(16) Uani 1 1 d . . . Cl1 Cl 0.70095(17) 0.02338(19) 0.47342(9) 0.0257(4) Uani 1 1 d . . . O11 O 0.6627(5) 0.0831(6) 0.4170(3) 0.0302(14) Uani 1 1 d . . . O12 O 0.6202(7) -0.0657(6) 0.4867(3) 0.0464(19) Uani 1 1 d . . . O13 O 0.7094(6) 0.1088(6) 0.5213(3) 0.0395(16) Uani 1 1 d . . . O14 O 0.8057(7) -0.0295(9) 0.4674(4) 0.059(2) Uani 1 1 d . . . Cl2 Cl 0.51355(18) -0.2144(2) 0.25428(10) 0.0324(5) Uani 1 1 d . . . O21 O 0.5606(7) -0.1287(7) 0.2988(3) 0.053(2) Uani 1 1 d . . . O22 O 0.5682(7) -0.2044(8) 0.1987(3) 0.052(2) Uani 1 1 d . . . O23 O 0.3968(6) -0.1943(7) 0.2425(4) 0.056(2) Uani 1 1 d . . . O24 O 0.5285(7) -0.3336(6) 0.2774(3) 0.0449(18) Uani 1 1 d . . . N50 N 0.9783(9) 0.1950(10) 0.5474(5) 0.060(3) Uani 1 1 d . . . C50 C 0.9281(8) 0.3062(10) 0.5237(4) 0.036(2) Uani 1 1 d . . . C51 C 0.8911(9) 0.3909(9) 0.5030(4) 0.037(2) Uani 1 1 d . . . H51A H 0.9286 0.4616 0.5222 0.045 Uiso 1 1 calc R . . H51B H 0.8114 0.3939 0.5096 0.045 Uiso 1 1 calc R . . H51C H 0.9007 0.3915 0.4590 0.045 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 Pb1 0.02112(16) 0.01655(16) 0.02069(16) 0.00254(10) -0.00023(11) -0.00131(11) Pb2 0.02108(17) 0.02700(18) 0.02037(16) 0.00439(11) -0.00306(11) -0.00477(12) N1 0.023(3) 0.022(4) 0.018(3) 0.002(3) 0.000(3) -0.003(3) N2 0.021(3) 0.020(3) 0.019(3) 0.008(3) -0.001(3) 0.000(3) C3 0.024(4) 0.022(4) 0.017(4) 0.001(3) 0.005(3) -0.002(3) N3 0.021(3) 0.019(3) 0.017(3) -0.002(2) 0.000(2) 0.004(3) C5 0.021(4) 0.017(4) 0.018(4) -0.006(3) 0.004(3) 0.004(3) C6 0.024(4) 0.019(4) 0.022(4) -0.008(3) 0.001(3) 0.001(3) C7 0.036(5) 0.041(5) 0.021(4) 0.003(4) -0.002(4) -0.004(4) N4 0.023(4) 0.018(3) 0.024(3) -0.002(3) -0.002(3) 0.000(3) C8 0.024(4) 0.021(4) 0.033(5) -0.004(3) -0.003(3) -0.002(3) C9 0.024(4) 0.025(5) 0.031(4) 0.000(3) 0.001(3) -0.010(3) C10 0.019(4) 0.027(4) 0.024(4) 0.003(3) -0.001(3) -0.006(3) N5 0.020(3) 0.022(4) 0.022(3) 0.001(3) 0.000(3) -0.003(3) C11 0.029(5) 0.025(5) 0.043(5) -0.010(4) 0.008(4) 0.000(4) C12 0.024(4) 0.032(5) 0.015(4) 0.004(3) 0.006(3) -0.002(3) C13 0.031(4) 0.018(4) 0.015(4) -0.001(3) 0.005(3) -0.004(3) N6 0.018(3) 0.020(3) 0.025(3) 0.006(3) 0.001(3) -0.002(3) N7 0.025(4) 0.027(4) 0.026(4) -0.002(3) 0.002(3) -0.008(3) C15 0.028(4) 0.021(4) 0.015(4) -0.003(3) 0.003(3) -0.005(3) N8 0.033(4) 0.022(4) 0.022(3) 0.000(3) 0.003(3) -0.002(3) C16 0.033(5) 0.025(5) 0.017(4) -0.001(3) 0.001(3) -0.007(3) C17 0.047(6) 0.024(5) 0.028(4) -0.003(3) 0.005(4) -0.006(4) N9 0.041(5) 0.026(4) 0.018(3) 0.002(3) 0.004(3) -0.016(3) C18 0.053(6) 0.011(4) 0.035(5) -0.003(3) 0.003(4) -0.017(4) C19 0.037(5) 0.049(6) 0.028(5) -0.001(4) 0.005(4) -0.030(5) C20 0.027(4) 0.024(4) 0.026(4) 0.001(3) 0.000(3) -0.006(3) N10 0.027(4) 0.026(4) 0.020(3) 0.004(3) 0.003(3) -0.007(3) C21 0.041(5) 0.025(5) 0.022(4) 0.007(3) 0.005(4) -0.002(4) C22 0.016(4) 0.026(4) 0.019(4) 0.003(3) 0.005(3) -0.001(3) Cl1 0.0277(10) 0.0267(11) 0.0221(9) 0.0019(7) -0.0015(8) 0.0016(8) O11 0.031(3) 0.028(3) 0.031(3) 0.012(3) -0.007(3) -0.005(3) O12 0.067(5) 0.038(4) 0.033(4) 0.014(3) -0.005(3) -0.019(4) O13 0.046(4) 0.038(4) 0.034(4) -0.008(3) -0.001(3) -0.006(3) O14 0.045(5) 0.088(7) 0.043(4) 0.002(4) 0.002(3) 0.033(4) Cl2 0.0321(11) 0.0306(12) 0.0343(11) -0.0044(9) 0.0018(9) -0.0016(9) O21 0.069(5) 0.045(5) 0.045(4) -0.013(3) 0.002(4) -0.009(4) O22 0.056(5) 0.065(5) 0.036(4) -0.003(4) 0.007(3) -0.021(4) O23 0.041(4) 0.045(5) 0.083(6) -0.002(4) 0.010(4) 0.004(3) O24 0.056(5) 0.030(4) 0.048(4) -0.004(3) -0.002(4) 0.003(3) N50 0.069(7) 0.053(7) 0.058(6) 0.007(5) -0.009(5) 0.004(5) C50 0.035(5) 0.049(6) 0.024(4) -0.011(4) 0.007(4) -0.006(4) C51 0.046(6) 0.035(6) 0.029(5) -0.005(4) -0.009(4) 0.002(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 Pb1 N1 2.407(6) . y Pb1 N6 2.430(7) . y Pb1 N4 2.496(7) . y Pb1 N5 2.519(7) . y Pb1 O11 2.825(6) . y Pb1 O12 3.045(7) 3_656 y Pb2 N7 2.381(7) . y Pb2 N2 2.408(6) . y Pb2 N10 2.471(7) . y Pb2 N9 2.491(8) . y Pb2 O11 2.843(7) . y N1 C5 1.317(10) . ? N1 N2 1.355(9) . ? N2 C3 1.324(10) . ? C3 N3 1.324(10) . ? C3 C22 1.453(11) . ? N3 C5 1.335(10) . ? C5 C6 1.460(11) . ? C6 N4 1.281(11) . ? C6 C7 1.475(11) . ? N4 C8 1.449(10) . ? C8 C9 1.516(12) . ? C9 C10 1.493(12) . ? C10 N5 1.467(10) . ? N5 C12 1.271(11) . ? C11 C12 1.475(12) . ? C12 C13 1.476(11) . ? C13 N8 1.305(10) . ? C13 N6 1.347(11) . ? N6 N7 1.346(9) . ? N7 C15 1.336(11) . ? C15 N8 1.335(11) . ? C15 C16 1.460(11) . ? C16 N9 1.289(11) . ? C16 C17 1.480(12) . ? N9 C18 1.473(10) . ? C18 C19 1.518(14) . ? C19 C20 1.508(12) . ? C20 N10 1.432(10) . ? N10 C22 1.273(10) . ? C21 C22 1.487(11) . ? Cl1 O14 1.403(8) . ? Cl1 O13 1.409(7) . ? Cl1 O12 1.426(7) . ? Cl1 O11 1.446(6) . ? Cl2 O24 1.415(7) . ? Cl2 O23 1.426(8) . ? Cl2 O22 1.432(7) . ? Cl2 O21 1.443(8) . ? N50 C50 1.446(15) . ? C50 C51 1.115(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pb1 N6 71.9(2) . . y N1 Pb1 N4 65.3(2) . . y N6 Pb1 N4 103.5(2) . . y N1 Pb1 N5 103.3(2) . . y N6 Pb1 N5 65.0(2) . . y N4 Pb1 N5 67.5(2) . . y N7 Pb2 N2 72.4(2) . . y N7 Pb2 N10 102.8(2) . . y N2 Pb2 N10 66.3(2) . . y N7 Pb2 N9 65.9(2) . . y N2 Pb2 N9 106.7(2) . . y N10 Pb2 N9 68.0(2) . . y C5 N1 N2 105.3(6) . . ? C5 N1 Pb1 119.8(5) . . ? N2 N1 Pb1 132.1(5) . . ? C3 N2 N1 106.3(6) . . ? C3 N2 Pb2 118.2(5) . . ? N1 N2 Pb2 132.9(5) . . ? N2 C3 N3 112.7(7) . . ? N2 C3 C22 119.1(7) . . ? N3 C3 C22 127.8(7) . . ? C3 N3 C5 102.5(6) . . ? N1 C5 N3 113.2(7) . . ? N1 C5 C6 119.2(7) . . ? N3 C5 C6 127.1(7) . . ? N4 C6 C5 115.0(7) . . ? N4 C6 C7 125.7(8) . . ? C5 C6 C7 119.2(7) . . ? C6 N4 C8 120.3(7) . . ? C6 N4 Pb1 120.3(5) . . ? C8 N4 Pb1 119.3(5) . . ? N4 C8 C9 110.8(7) . . ? C10 C9 C8 115.3(7) . . ? N5 C10 C9 110.2(7) . . ? C12 N5 C10 120.2(7) . . ? C12 N5 Pb1 121.2(5) . . ? C10 N5 Pb1 118.6(5) . . ? N5 C12 C11 127.7(8) . . ? N5 C12 C13 115.3(7) . . ? C11 C12 C13 117.0(8) . . ? N8 C13 N6 114.5(7) . . ? N8 C13 C12 127.1(8) . . ? N6 C13 C12 118.1(7) . . ? N7 N6 C13 104.7(7) . . ? N7 N6 Pb1 132.9(5) . . ? C13 N6 Pb1 119.8(5) . . ? C15 N7 N6 105.6(7) . . ? C15 N7 Pb2 119.5(5) . . ? N6 N7 Pb2 132.5(5) . . ? N8 C15 N7 113.5(7) . . ? N8 C15 C16 126.6(8) . . ? N7 C15 C16 119.6(7) . . ? C13 N8 C15 101.7(7) . . ? N9 C16 C15 114.3(8) . . ? N9 C16 C17 126.3(8) . . ? C15 C16 C17 119.3(8) . . ? C16 N9 C18 119.7(8) . . ? C16 N9 Pb2 120.3(5) . . ? C18 N9 Pb2 119.5(6) . . ? N9 C18 C19 109.3(7) . . ? C20 C19 C18 113.9(8) . . ? N10 C20 C19 112.8(7) . . ? C22 N10 C20 122.2(7) . . ? C22 N10 Pb2 119.4(5) . . ? C20 N10 Pb2 118.0(5) . . ? N10 C22 C3 116.1(7) . . ? N10 C22 C21 124.2(8) . . ? C3 C22 C21 119.7(7) . . ? O14 Cl1 O13 109.4(5) . . ? O14 Cl1 O12 111.3(5) . . ? O13 Cl1 O12 108.7(4) . . ? O14 Cl1 O11 109.8(4) . . ? O13 Cl1 O11 109.6(4) . . ? O12 Cl1 O11 108.0(4) . . ? O24 Cl2 O23 107.9(5) . . ? O24 Cl2 O22 108.8(5) . . ? O23 Cl2 O22 110.0(5) . . ? O24 Cl2 O21 109.4(5) . . ? O23 Cl2 O21 110.6(5) . . ? O22 Cl2 O21 110.2(5) . . ? C51 C50 N50 177.0(11) . . ? 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 N6 Pb1 N1 C5 -110.7(6) . . . . ? N4 Pb1 N1 C5 4.2(5) . . . . ? N5 Pb1 N1 C5 -53.0(6) . . . . ? N6 Pb1 N1 N2 47.5(7) . . . . ? N4 Pb1 N1 N2 162.4(7) . . . . ? N5 Pb1 N1 N2 105.3(7) . . . . ? C5 N1 N2 C3 -0.4(8) . . . . ? Pb1 N1 N2 C3 -160.9(6) . . . . ? C5 N1 N2 Pb2 160.2(5) . . . . ? Pb1 N1 N2 Pb2 -0.3(10) . . . . ? N7 Pb2 N2 C3 110.7(6) . . . . ? N10 Pb2 N2 C3 -2.4(6) . . . . ? N9 Pb2 N2 C3 53.6(6) . . . . ? N7 Pb2 N2 N1 -48.0(7) . . . . ? N10 Pb2 N2 N1 -161.1(7) . . . . ? N9 Pb2 N2 N1 -105.1(7) . . . . ? N1 N2 C3 N3 -0.6(9) . . . . ? Pb2 N2 C3 N3 -164.6(5) . . . . ? N1 N2 C3 C22 172.2(7) . . . . ? Pb2 N2 C3 C22 8.3(9) . . . . ? N2 C3 N3 C5 1.3(9) . . . . ? C22 C3 N3 C5 -170.8(8) . . . . ? N2 N1 C5 N3 1.2(9) . . . . ? Pb1 N1 C5 N3 164.7(5) . . . . ? N2 N1 C5 C6 -170.9(6) . . . . ? Pb1 N1 C5 C6 -7.5(9) . . . . ? C3 N3 C5 N1 -1.6(8) . . . . ? C3 N3 C5 C6 169.8(7) . . . . ? N1 C5 C6 N4 6.7(11) . . . . ? N3 C5 C6 N4 -164.2(7) . . . . ? N1 C5 C6 C7 -175.4(7) . . . . ? N3 C5 C6 C7 13.6(12) . . . . ? C5 C6 N4 C8 174.8(7) . . . . ? C7 C6 N4 C8 -2.9(13) . . . . ? C5 C6 N4 Pb1 -2.8(9) . . . . ? C7 C6 N4 Pb1 179.5(7) . . . . ? N1 Pb1 N4 C6 -0.5(6) . . . . ? N6 Pb1 N4 C6 62.0(6) . . . . ? N5 Pb1 N4 C6 117.2(6) . . . . ? N1 Pb1 N4 C8 -178.1(6) . . . . ? N6 Pb1 N4 C8 -115.7(6) . . . . ? N5 Pb1 N4 C8 -60.4(6) . . . . ? C6 N4 C8 C9 -160.6(7) . . . . ? Pb1 N4 C8 C9 17.0(9) . . . . ? N4 C8 C9 C10 65.9(9) . . . . ? C8 C9 C10 N5 -63.9(9) . . . . ? C9 C10 N5 C12 162.2(7) . . . . ? C9 C10 N5 Pb1 -18.7(8) . . . . ? N1 Pb1 N5 C12 -63.4(6) . . . . ? N6 Pb1 N5 C12 -0.9(6) . . . . ? N4 Pb1 N5 C12 -119.1(6) . . . . ? N1 Pb1 N5 C10 117.5(5) . . . . ? N6 Pb1 N5 C10 180.0(6) . . . . ? N4 Pb1 N5 C10 61.8(5) . . . . ? C10 N5 C12 C11 0.8(12) . . . . ? Pb1 N5 C12 C11 -178.3(7) . . . . ? C10 N5 C12 C13 -175.5(7) . . . . ? Pb1 N5 C12 C13 5.4(9) . . . . ? N5 C12 C13 N8 164.5(8) . . . . ? C11 C12 C13 N8 -12.3(12) . . . . ? N5 C12 C13 N6 -9.3(10) . . . . ? C11 C12 C13 N6 174.0(7) . . . . ? N8 C13 N6 N7 -1.7(9) . . . . ? C12 C13 N6 N7 172.8(6) . . . . ? N8 C13 N6 Pb1 -165.7(5) . . . . ? C12 C13 N6 Pb1 8.9(9) . . . . ? N1 Pb1 N6 N7 -48.1(7) . . . . ? N4 Pb1 N6 N7 -106.1(7) . . . . ? N5 Pb1 N6 N7 -162.9(7) . . . . ? N1 Pb1 N6 C13 110.4(6) . . . . ? N4 Pb1 N6 C13 52.5(6) . . . . ? N5 Pb1 N6 C13 -4.4(5) . . . . ? C13 N6 N7 C15 0.8(8) . . . . ? Pb1 N6 N7 C15 161.7(5) . . . . ? C13 N6 N7 Pb2 -161.0(6) . . . . ? Pb1 N6 N7 Pb2 -0.1(11) . . . . ? N2 Pb2 N7 C15 -112.0(6) . . . . ? N10 Pb2 N7 C15 -52.3(6) . . . . ? N9 Pb2 N7 C15 6.2(5) . . . . ? N2 Pb2 N7 N6 47.8(7) . . . . ? N10 Pb2 N7 N6 107.5(7) . . . . ? N9 Pb2 N7 N6 166.0(8) . . . . ? N6 N7 C15 N8 0.3(9) . . . . ? Pb2 N7 C15 N8 164.9(5) . . . . ? N6 N7 C15 C16 -172.7(7) . . . . ? Pb2 N7 C15 C16 -8.0(9) . . . . ? N6 C13 N8 C15 1.8(9) . . . . ? C12 C13 N8 C15 -172.1(7) . . . . ? N7 C15 N8 C13 -1.3(9) . . . . ? C16 C15 N8 C13 171.1(7) . . . . ? N8 C15 C16 N9 -168.3(7) . . . . ? N7 C15 C16 N9 3.6(11) . . . . ? N8 C15 C16 C17 9.6(12) . . . . ? N7 C15 C16 C17 -178.5(7) . . . . ? C15 C16 N9 C18 174.6(7) . . . . ? C17 C16 N9 C18 -3.1(12) . . . . ? C15 C16 N9 Pb2 2.3(9) . . . . ? C17 C16 N9 Pb2 -175.4(6) . . . . ? N7 Pb2 N9 C16 -4.5(6) . . . . ? N2 Pb2 N9 C16 56.8(6) . . . . ? N10 Pb2 N9 C16 111.8(6) . . . . ? N7 Pb2 N9 C18 -176.8(6) . . . . ? N2 Pb2 N9 C18 -115.5(6) . . . . ? N10 Pb2 N9 C18 -60.6(6) . . . . ? C16 N9 C18 C19 -156.7(8) . . . . ? Pb2 N9 C18 C19 15.7(9) . . . . ? N9 C18 C19 C20 64.6(10) . . . . ? C18 C19 C20 N10 -64.3(11) . . . . ? C19 C20 N10 C22 168.6(8) . . . . ? C19 C20 N10 Pb2 -18.6(10) . . . . ? N7 Pb2 N10 C22 -68.3(7) . . . . ? N2 Pb2 N10 C22 -4.3(6) . . . . ? N9 Pb2 N10 C22 -125.4(7) . . . . ? N7 Pb2 N10 C20 118.6(6) . . . . ? N2 Pb2 N10 C20 -177.3(7) . . . . ? N9 Pb2 N10 C20 61.6(6) . . . . ? C20 N10 C22 C3 -177.5(7) . . . . ? Pb2 N10 C22 C3 9.8(10) . . . . ? C20 N10 C22 C21 -0.3(13) . . . . ? Pb2 N10 C22 C21 -173.0(6) . . . . ? N2 C3 C22 N10 -12.1(11) . . . . ? N3 C3 C22 N10 159.6(8) . . . . ? N2 C3 C22 C21 170.6(8) . . . . ? N3 C3 C22 C21 -17.7(12) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.70 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 3.981 _refine_diff_density_min -1.940 _refine_diff_density_rms 0.238 data_cutz _database_code_CSD 207830 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H30 Cu2 N12, C2 H3 N, 2(Cl O4)' _chemical_formula_sum 'C24 H33 Cl2 Cu2 N13 O8' _chemical_formula_weight 829.61 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' Cl Cl 0.1484 0.1585 '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)/c 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 17.905(4) _cell_length_b 12.063(2) _cell_length_c 15.845(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.812(3) _cell_angle_gamma 90.00 _cell_volume 3418.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour dk_green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 1.466 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.881936 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26314 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.51 _reflns_number_total 7367 _reflns_number_gt 6231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0443P)^2^+5.8156P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7367 _refine_ls_number_parameters 449 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.266217(18) 0.71337(2) 0.17410(2) 0.01963(9) Uani 1 1 d . . . Cu2 Cu 0.265732(18) 0.42539(2) 0.040677(19) 0.01869(9) Uani 1 1 d . . . N1 N 0.31158(12) 0.56688(17) 0.19474(14) 0.0203(4) Uani 1 1 d . . . N2 N 0.31061(12) 0.47184(18) 0.15056(14) 0.0202(4) Uani 1 1 d . . . N3 N 0.31788(13) 0.42690(18) 0.28853(14) 0.0227(5) Uani 1 1 d . . . N4 N 0.27754(13) 0.71649(18) 0.30017(14) 0.0210(5) Uani 1 1 d . . . N5 N 0.17941(13) 0.82038(18) 0.16836(15) 0.0242(5) Uani 1 1 d . . . N6 N 0.21599(12) 0.66612(17) 0.06657(13) 0.0196(4) Uani 1 1 d . . . N7 N 0.21515(12) 0.56936(17) 0.02389(13) 0.0189(4) Uani 1 1 d . . . N8 N 0.10091(13) 0.64592(19) 0.00356(14) 0.0242(5) Uani 1 1 d . . . N9 N 0.17998(13) 0.37839(19) -0.03730(14) 0.0223(5) Uani 1 1 d . . . N10 N 0.27777(13) 0.27646(18) 0.09588(14) 0.0226(5) Uani 1 1 d . . . C3 C 0.31341(15) 0.3904(2) 0.20797(17) 0.0213(5) Uani 1 1 d . . . C5 C 0.31516(15) 0.5376(2) 0.27636(16) 0.0208(5) Uani 1 1 d . . . C6 C 0.30311(15) 0.6276(2) 0.33712(16) 0.0226(5) Uani 1 1 d . . . C7 C 0.31635(18) 0.6102(3) 0.43032(17) 0.0296(6) Uani 1 1 d . . . H7A H 0.2682 0.6064 0.4571 0.044 Uiso 1 1 calc R . . H7B H 0.3457 0.6722 0.4544 0.044 Uiso 1 1 calc R . . H7C H 0.3438 0.5408 0.4404 0.044 Uiso 1 1 calc R . . C8 C 0.25724(18) 0.8146(2) 0.35040(18) 0.0294(6) Uani 1 1 d . . . H8B H 0.2991 0.8333 0.3910 0.035 Uiso 1 1 calc R . . H8A H 0.2130 0.7970 0.3831 0.035 Uiso 1 1 calc R . . C9 C 0.23978(18) 0.9137(2) 0.29322(19) 0.0295(6) Uani 1 1 d . . . H9A H 0.2347 0.9800 0.3294 0.035 Uiso 1 1 calc R . . H9B H 0.2832 0.9264 0.2581 0.035 Uiso 1 1 calc R . . C10 C 0.16998(18) 0.9051(2) 0.2347(2) 0.0324(7) Uani 1 1 d . . . H10B H 0.1266 0.8852 0.2681 0.039 Uiso 1 1 calc R . . H10A H 0.1596 0.9779 0.2078 0.039 Uiso 1 1 calc R . . C11 C 0.05661(17) 0.8653(3) 0.0953(2) 0.0326(7) Uani 1 1 d . . . H11A H 0.0240 0.8473 0.1413 0.049 Uiso 1 1 calc R . . H11B H 0.0322 0.8434 0.0412 0.049 Uiso 1 1 calc R . . H11C H 0.0663 0.9453 0.0951 0.049 Uiso 1 1 calc R . . C12 C 0.12890(16) 0.8043(2) 0.10827(18) 0.0246(6) Uani 1 1 d . . . C13 C 0.14732(16) 0.7086(2) 0.05388(17) 0.0224(5) Uani 1 1 d . . . C15 C 0.14605(15) 0.5595(2) -0.01209(16) 0.0211(5) Uani 1 1 d . . . C16 C 0.12843(15) 0.4513(2) -0.05158(16) 0.0228(5) Uani 1 1 d . . . C17 C 0.05470(17) 0.4328(3) -0.0981(2) 0.0324(7) Uani 1 1 d . . . H17A H 0.0626 0.3939 -0.1513 0.049 Uiso 1 1 calc R . . H17B H 0.0307 0.5044 -0.1103 0.049 Uiso 1 1 calc R . . H17C H 0.0225 0.3879 -0.0633 0.049 Uiso 1 1 calc R . . C18 C 0.16968(18) 0.2618(2) -0.06374(19) 0.0292(6) Uani 1 1 d . . . H18B H 0.1581 0.2589 -0.1254 0.035 Uiso 1 1 calc R . . H18A H 0.1268 0.2297 -0.0351 0.035 Uiso 1 1 calc R . . C19 C 0.23963(18) 0.1929(2) -0.04223(19) 0.0315(7) Uani 1 1 d . . . H19B H 0.2338 0.1201 -0.0707 0.038 Uiso 1 1 calc R . . H19A H 0.2830 0.2305 -0.0661 0.038 Uiso 1 1 calc R . . C20 C 0.25734(18) 0.1729(2) 0.05129(19) 0.0297(6) Uani 1 1 d . . . H20B H 0.2132 0.1397 0.0769 0.036 Uiso 1 1 calc R . . H20A H 0.2992 0.1195 0.0581 0.036 Uiso 1 1 calc R . . C21 C 0.3103(2) 0.1792(2) 0.2307(2) 0.0339(7) Uani 1 1 d . . . H21A H 0.2614 0.1457 0.2395 0.051 Uiso 1 1 calc R . . H21B H 0.3332 0.2026 0.2853 0.051 Uiso 1 1 calc R . . H21C H 0.3426 0.1247 0.2047 0.051 Uiso 1 1 calc R . . C22 C 0.30048(16) 0.2778(2) 0.17390(18) 0.0232(6) Uani 1 1 d . . . N30 N 0.36322(15) 0.8125(2) 0.14230(16) 0.0300(5) Uani 1 1 d . . . C30 C 0.42038(17) 0.8489(2) 0.13188(18) 0.0284(6) Uani 1 1 d . . . C31 C 0.4944(2) 0.8951(3) 0.1176(2) 0.0453(9) Uani 1 1 d . . . H31C H 0.5116 0.8680 0.0636 0.068 Uiso 1 1 calc R . . H31B H 0.5298 0.8720 0.1634 0.068 Uiso 1 1 calc R . . H31A H 0.4914 0.9762 0.1162 0.068 Uiso 1 1 calc R . . N40 N 0.36239(15) 0.4316(2) -0.04235(16) 0.0306(5) Uani 1 1 d . . . C40 C 0.41822(17) 0.4293(2) -0.07335(18) 0.0279(6) Uani 1 1 d . . . C41 C 0.49047(19) 0.4260(3) -0.1133(2) 0.0425(8) Uani 1 1 d . . . H41C H 0.5069 0.5017 -0.1248 0.064 Uiso 1 1 calc R . . H41B H 0.4851 0.3846 -0.1665 0.064 Uiso 1 1 calc R . . H41A H 0.5276 0.3893 -0.0753 0.064 Uiso 1 1 calc R . . Cl1 Cl 0.50125(4) 0.73770(7) 0.37100(5) 0.03577(18) Uani 1 1 d . . . O11 O 0.45002(17) 0.7955(2) 0.4228(2) 0.0648(9) Uani 1 1 d . . . O12 O 0.55748(16) 0.6817(3) 0.42390(19) 0.0623(8) Uani 1 1 d . . . O13 O 0.46148(14) 0.6565(2) 0.32011(17) 0.0497(6) Uani 1 1 d . . . O14 O 0.53688(15) 0.8147(2) 0.31692(19) 0.0547(7) Uani 1 1 d . . . Cl2 Cl 0.07331(5) 0.25788(7) 0.16910(5) 0.0411(2) Uani 1 1 d . . . O21 O 0.1301(2) 0.2137(4) 0.2233(2) 0.1039(16) Uani 1 1 d . . . O22 O 0.0977(2) 0.3481(3) 0.1220(2) 0.0851(12) Uani 1 1 d . . . O23 O 0.01016(18) 0.2895(3) 0.2164(2) 0.0709(9) Uani 1 1 d . . . O24 O 0.0518(2) 0.1716(4) 0.1092(2) 0.0926(12) Uani 1 1 d . . . N50 N 0.1362(2) -0.0552(4) -0.0730(3) 0.0687(11) Uani 1 1 d . . . C50 C 0.1152(2) -0.0544(3) -0.1417(3) 0.0479(9) Uani 1 1 d . . . C51 C 0.0893(3) -0.0542(4) -0.2298(3) 0.0638(12) Uani 1 1 d . . . H51A H 0.1316 -0.0405 -0.2653 0.096 Uiso 1 1 calc R . . H51B H 0.0518 0.0043 -0.2393 0.096 Uiso 1 1 calc R . . H51C H 0.0669 -0.1263 -0.2443 0.096 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 0.02333(18) 0.01785(15) 0.01798(16) -0.00169(11) 0.00382(12) -0.00081(12) Cu2 0.02192(17) 0.01788(15) 0.01641(16) -0.00116(11) 0.00232(12) -0.00052(12) N1 0.0213(11) 0.0211(11) 0.0184(11) -0.0008(8) 0.0015(9) -0.0015(8) N2 0.0222(11) 0.0197(10) 0.0187(11) -0.0020(8) 0.0014(9) 0.0009(9) N3 0.0251(12) 0.0242(11) 0.0189(11) 0.0015(9) 0.0029(9) -0.0009(9) N4 0.0257(12) 0.0206(11) 0.0175(11) -0.0053(8) 0.0084(9) -0.0037(9) N5 0.0299(13) 0.0186(10) 0.0247(12) -0.0023(9) 0.0073(10) 0.0014(9) N6 0.0229(11) 0.0178(10) 0.0183(11) -0.0001(8) 0.0037(9) 0.0006(8) N7 0.0202(11) 0.0199(10) 0.0167(10) 0.0000(8) 0.0033(8) -0.0018(8) N8 0.0221(12) 0.0263(11) 0.0245(12) 0.0007(9) 0.0029(9) 0.0003(9) N9 0.0258(12) 0.0246(11) 0.0169(11) -0.0004(9) 0.0047(9) -0.0048(9) N10 0.0257(12) 0.0183(10) 0.0239(12) -0.0016(9) 0.0037(9) 0.0011(9) C3 0.0210(13) 0.0212(12) 0.0219(13) 0.0019(10) 0.0021(10) 0.0013(10) C5 0.0199(13) 0.0235(12) 0.0192(13) -0.0008(10) 0.0022(10) -0.0016(10) C6 0.0237(14) 0.0269(13) 0.0175(13) -0.0029(10) 0.0046(10) -0.0066(11) C7 0.0374(17) 0.0329(15) 0.0185(14) -0.0012(11) 0.0023(12) -0.0074(13) C8 0.0393(17) 0.0265(14) 0.0228(14) -0.0092(11) 0.0066(12) -0.0030(12) C9 0.0398(17) 0.0206(13) 0.0292(15) -0.0081(11) 0.0129(13) -0.0060(12) C10 0.0404(18) 0.0229(14) 0.0347(16) -0.0072(12) 0.0099(13) 0.0039(12) C11 0.0302(16) 0.0325(15) 0.0356(17) 0.0024(13) 0.0080(13) 0.0088(12) C12 0.0267(15) 0.0212(13) 0.0267(14) 0.0030(10) 0.0098(11) 0.0006(11) C13 0.0250(14) 0.0220(13) 0.0204(13) 0.0030(10) 0.0043(11) -0.0011(10) C15 0.0227(13) 0.0245(13) 0.0165(12) 0.0040(10) 0.0037(10) -0.0022(10) C16 0.0226(14) 0.0297(14) 0.0164(12) 0.0001(10) 0.0050(10) -0.0060(11) C17 0.0263(15) 0.0383(17) 0.0322(16) -0.0063(13) -0.0024(12) -0.0039(12) C18 0.0382(17) 0.0252(14) 0.0240(14) -0.0052(11) 0.0005(12) -0.0059(12) C19 0.0384(17) 0.0244(14) 0.0322(16) -0.0100(11) 0.0054(13) -0.0010(12) C20 0.0381(17) 0.0178(13) 0.0335(16) -0.0054(11) 0.0039(13) 0.0014(11) C21 0.0460(19) 0.0226(14) 0.0329(17) 0.0067(12) 0.0015(14) 0.0033(13) C22 0.0236(14) 0.0205(13) 0.0258(14) 0.0028(10) 0.0043(11) 0.0028(10) N30 0.0325(14) 0.0297(13) 0.0280(13) 0.0014(10) 0.0033(11) -0.0075(11) C30 0.0336(17) 0.0280(14) 0.0235(14) -0.0013(11) 0.0015(12) -0.0037(12) C31 0.0361(19) 0.053(2) 0.048(2) -0.0058(16) 0.0113(16) -0.0178(16) N40 0.0322(14) 0.0335(13) 0.0265(13) -0.0031(10) 0.0070(11) -0.0018(10) C40 0.0296(16) 0.0282(14) 0.0260(15) -0.0020(11) 0.0037(12) -0.0013(11) C41 0.0344(18) 0.0441(19) 0.051(2) -0.0032(15) 0.0195(16) -0.0011(14) Cl1 0.0295(4) 0.0403(4) 0.0380(4) -0.0018(3) 0.0069(3) -0.0090(3) O11 0.0593(18) 0.0544(17) 0.084(2) -0.0287(15) 0.0366(16) -0.0181(14) O12 0.0448(16) 0.086(2) 0.0551(17) 0.0245(16) -0.0076(13) -0.0108(15) O13 0.0389(14) 0.0522(15) 0.0579(16) -0.0188(13) 0.0014(12) -0.0077(12) O14 0.0439(15) 0.0551(16) 0.0663(18) 0.0207(14) 0.0159(13) -0.0054(12) Cl2 0.0421(5) 0.0512(5) 0.0312(4) 0.0039(3) 0.0122(3) 0.0092(4) O21 0.071(2) 0.190(5) 0.050(2) 0.044(2) -0.0005(17) 0.025(3) O22 0.115(3) 0.065(2) 0.081(2) 0.0236(18) 0.059(2) 0.018(2) O23 0.066(2) 0.073(2) 0.078(2) -0.0122(17) 0.0453(17) 0.0074(16) O24 0.088(3) 0.103(3) 0.088(3) -0.048(2) 0.021(2) -0.008(2) N50 0.041(2) 0.104(3) 0.061(2) 0.009(2) 0.0031(17) -0.015(2) C50 0.0312(19) 0.050(2) 0.063(3) 0.0023(18) 0.0068(18) -0.0011(15) C51 0.062(3) 0.070(3) 0.058(3) -0.001(2) -0.007(2) 0.008(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 N1 1.965(2) . ? Cu1 N6 1.971(2) . ? Cu1 N4 1.998(2) . ? Cu1 N5 2.019(2) . ? Cu1 N30 2.188(3) . ? Cu2 N2 1.963(2) . ? Cu2 N7 1.971(2) . ? Cu2 N9 2.005(2) . ? Cu2 N10 2.005(2) . ? Cu2 N40 2.226(3) . ? N1 C5 1.339(3) . ? N1 N2 1.343(3) . ? N2 C3 1.339(3) . ? N3 C3 1.349(3) . ? N3 C5 1.350(3) . ? N4 C6 1.295(4) . ? N4 C8 1.481(3) . ? N5 C12 1.295(4) . ? N5 C10 1.481(3) . ? N6 C13 1.338(4) . ? N6 N7 1.349(3) . ? N7 C15 1.342(4) . ? N8 C15 1.349(4) . ? N8 C13 1.354(4) . ? N9 C16 1.287(4) . ? N9 C18 1.476(3) . ? N10 C22 1.282(4) . ? N10 C20 1.473(3) . ? C3 C22 1.476(4) . ? C5 C6 1.474(4) . ? C6 C7 1.499(4) . ? C8 C9 1.523(4) . ? C9 C10 1.523(5) . ? C11 C12 1.494(4) . ? C12 C13 1.487(4) . ? C15 C16 1.475(4) . ? C16 C17 1.497(4) . ? C18 C19 1.528(4) . ? C19 C20 1.519(4) . ? C21 C22 1.497(4) . ? N30 C30 1.133(4) . ? C30 C31 1.466(4) . ? N40 C40 1.136(4) . ? C40 C41 1.468(4) . ? Cl1 O14 1.435(3) . ? Cl1 O13 1.435(3) . ? Cl1 O11 1.440(3) . ? Cl1 O12 1.446(3) . ? Cl2 O22 1.402(3) . ? Cl2 O21 1.403(3) . ? Cl2 O23 1.438(3) . ? Cl2 O24 1.448(4) . ? N50 C50 1.134(5) . ? C50 C51 1.449(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N6 92.93(9) . . ? N1 Cu1 N4 80.20(9) . . ? N6 Cu1 N4 152.76(9) . . ? N1 Cu1 N5 153.28(9) . . ? N6 Cu1 N5 80.11(9) . . ? N4 Cu1 N5 94.20(9) . . ? N1 Cu1 N30 101.74(10) . . ? N6 Cu1 N30 107.01(9) . . ? N4 Cu1 N30 100.21(9) . . ? N5 Cu1 N30 104.97(10) . . ? N2 Cu2 N7 91.93(9) . . ? N2 Cu2 N9 153.52(9) . . ? N7 Cu2 N9 80.39(9) . . ? N2 Cu2 N10 80.69(9) . . ? N7 Cu2 N10 152.54(9) . . ? N9 Cu2 N10 94.48(9) . . ? N2 Cu2 N40 102.60(9) . . ? N7 Cu2 N40 104.82(9) . . ? N9 Cu2 N40 103.85(9) . . ? N10 Cu2 N40 102.60(9) . . ? C5 N1 N2 106.1(2) . . ? C5 N1 Cu1 113.43(17) . . ? N2 N1 Cu1 133.32(17) . . ? C3 N2 N1 105.9(2) . . ? C3 N2 Cu2 113.16(18) . . ? N1 N2 Cu2 134.45(17) . . ? C3 N3 C5 100.8(2) . . ? C6 N4 C8 120.6(2) . . ? C6 N4 Cu1 116.91(17) . . ? C8 N4 Cu1 122.45(18) . . ? C12 N5 C10 121.7(2) . . ? C12 N5 Cu1 116.46(18) . . ? C10 N5 Cu1 121.55(19) . . ? C13 N6 N7 105.6(2) . . ? C13 N6 Cu1 113.33(17) . . ? N7 N6 Cu1 132.61(17) . . ? C15 N7 N6 106.1(2) . . ? C15 N7 Cu2 112.78(17) . . ? N6 N7 Cu2 134.53(17) . . ? C15 N8 C13 100.6(2) . . ? C16 N9 C18 121.5(2) . . ? C16 N9 Cu2 115.87(18) . . ? C18 N9 Cu2 121.70(18) . . ? C22 N10 C20 122.2(2) . . ? C22 N10 Cu2 115.59(18) . . ? C20 N10 Cu2 122.14(18) . . ? N2 C3 N3 113.7(2) . . ? N2 C3 C22 115.3(2) . . ? N3 C3 C22 130.4(2) . . ? N1 C5 N3 113.5(2) . . ? N1 C5 C6 115.8(2) . . ? N3 C5 C6 129.8(2) . . ? N4 C6 C5 112.0(2) . . ? N4 C6 C7 126.6(2) . . ? C5 C6 C7 121.3(2) . . ? N4 C8 C9 110.9(2) . . ? C10 C9 C8 116.5(2) . . ? N5 C10 C9 111.1(2) . . ? N5 C12 C13 112.1(2) . . ? N5 C12 C11 126.6(3) . . ? C13 C12 C11 121.2(3) . . ? N6 C13 N8 114.0(2) . . ? N6 C13 C12 116.0(2) . . ? N8 C13 C12 128.9(3) . . ? N7 C15 N8 113.7(2) . . ? N7 C15 C16 115.6(2) . . ? N8 C15 C16 130.1(2) . . ? N9 C16 C15 113.2(2) . . ? N9 C16 C17 126.3(3) . . ? C15 C16 C17 120.4(2) . . ? N9 C18 C19 111.4(2) . . ? C20 C19 C18 115.7(2) . . ? N10 C20 C19 111.6(2) . . ? N10 C22 C3 113.6(2) . . ? N10 C22 C21 126.4(3) . . ? C3 C22 C21 120.0(2) . . ? C30 N30 Cu1 168.0(3) . . ? N30 C30 C31 179.3(4) . . ? C40 N40 Cu2 168.9(3) . . ? N40 C40 C41 179.8(4) . . ? O14 Cl1 O13 109.22(18) . . ? O14 Cl1 O11 109.97(18) . . ? O13 Cl1 O11 109.75(16) . . ? O14 Cl1 O12 109.36(17) . . ? O13 Cl1 O12 108.62(18) . . ? O11 Cl1 O12 109.9(2) . . ? O22 Cl2 O21 112.6(3) . . ? O22 Cl2 O23 110.2(2) . . ? O21 Cl2 O23 110.3(2) . . ? O22 Cl2 O24 106.8(2) . . ? O21 Cl2 O24 106.8(3) . . ? O23 Cl2 O24 110.0(2) . . ? N50 C50 C51 179.2(5) . . ? 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 N6 Cu1 N1 C5 -143.46(19) . . . . ? N4 Cu1 N1 C5 9.99(18) . . . . ? N5 Cu1 N1 C5 -69.8(3) . . . . ? N30 Cu1 N1 C5 108.49(19) . . . . ? N6 Cu1 N1 N2 2.0(2) . . . . ? N4 Cu1 N1 N2 155.4(2) . . . . ? N5 Cu1 N1 N2 75.7(3) . . . . ? N30 Cu1 N1 N2 -106.1(2) . . . . ? C5 N1 N2 C3 0.2(3) . . . . ? Cu1 N1 N2 C3 -147.0(2) . . . . ? C5 N1 N2 Cu2 148.6(2) . . . . ? Cu1 N1 N2 Cu2 1.4(4) . . . . ? N7 Cu2 N2 C3 142.32(19) . . . . ? N9 Cu2 N2 C3 70.2(3) . . . . ? N10 Cu2 N2 C3 -11.09(18) . . . . ? N40 Cu2 N2 C3 -112.03(19) . . . . ? N7 Cu2 N2 N1 -4.4(2) . . . . ? N9 Cu2 N2 N1 -76.5(3) . . . . ? N10 Cu2 N2 N1 -157.8(3) . . . . ? N40 Cu2 N2 N1 101.2(2) . . . . ? N1 Cu1 N4 C6 -3.5(2) . . . . ? N6 Cu1 N4 C6 73.6(3) . . . . ? N5 Cu1 N4 C6 150.1(2) . . . . ? N30 Cu1 N4 C6 -103.8(2) . . . . ? N1 Cu1 N4 C8 177.1(2) . . . . ? N6 Cu1 N4 C8 -105.7(3) . . . . ? N5 Cu1 N4 C8 -29.2(2) . . . . ? N30 Cu1 N4 C8 76.8(2) . . . . ? N1 Cu1 N5 C12 -69.3(3) . . . . ? N6 Cu1 N5 C12 7.4(2) . . . . ? N4 Cu1 N5 C12 -145.7(2) . . . . ? N30 Cu1 N5 C12 112.5(2) . . . . ? N1 Cu1 N5 C10 104.4(3) . . . . ? N6 Cu1 N5 C10 -178.9(2) . . . . ? N4 Cu1 N5 C10 27.9(2) . . . . ? N30 Cu1 N5 C10 -73.8(2) . . . . ? N1 Cu1 N6 C13 141.56(18) . . . . ? N4 Cu1 N6 C13 67.4(3) . . . . ? N5 Cu1 N6 C13 -12.46(18) . . . . ? N30 Cu1 N6 C13 -115.22(18) . . . . ? N1 Cu1 N6 N7 -1.0(2) . . . . ? N4 Cu1 N6 N7 -75.2(3) . . . . ? N5 Cu1 N6 N7 -155.0(2) . . . . ? N30 Cu1 N6 N7 102.2(2) . . . . ? C13 N6 N7 C15 0.1(3) . . . . ? Cu1 N6 N7 C15 144.7(2) . . . . ? C13 N6 N7 Cu2 -148.0(2) . . . . ? Cu1 N6 N7 Cu2 -3.4(4) . . . . ? N2 Cu2 N7 C15 -141.18(18) . . . . ? N9 Cu2 N7 C15 13.33(17) . . . . ? N10 Cu2 N7 C15 -67.8(3) . . . . ? N40 Cu2 N7 C15 115.25(18) . . . . ? N2 Cu2 N7 N6 5.4(2) . . . . ? N9 Cu2 N7 N6 159.9(2) . . . . ? N10 Cu2 N7 N6 78.8(3) . . . . ? N40 Cu2 N7 N6 -98.2(2) . . . . ? N2 Cu2 N9 C16 64.8(3) . . . . ? N7 Cu2 N9 C16 -9.89(19) . . . . ? N10 Cu2 N9 C16 142.91(19) . . . . ? N40 Cu2 N9 C16 -112.92(19) . . . . ? N2 Cu2 N9 C18 -104.2(3) . . . . ? N7 Cu2 N9 C18 -178.9(2) . . . . ? N10 Cu2 N9 C18 -26.1(2) . . . . ? N40 Cu2 N9 C18 78.0(2) . . . . ? N2 Cu2 N10 C22 6.0(2) . . . . ? N7 Cu2 N10 C22 -70.0(3) . . . . ? N9 Cu2 N10 C22 -147.8(2) . . . . ? N40 Cu2 N10 C22 106.9(2) . . . . ? N2 Cu2 N10 C20 -177.7(2) . . . . ? N7 Cu2 N10 C20 106.2(3) . . . . ? N9 Cu2 N10 C20 28.5(2) . . . . ? N40 Cu2 N10 C20 -76.8(2) . . . . ? N1 N2 C3 N3 -1.4(3) . . . . ? Cu2 N2 C3 N3 -157.37(18) . . . . ? N1 N2 C3 C22 170.4(2) . . . . ? Cu2 N2 C3 C22 14.4(3) . . . . ? C5 N3 C3 N2 1.9(3) . . . . ? C5 N3 C3 C22 -168.3(3) . . . . ? N2 N1 C5 N3 1.0(3) . . . . ? Cu1 N1 C5 N3 155.62(19) . . . . ? N2 N1 C5 C6 -169.3(2) . . . . ? Cu1 N1 C5 C6 -14.7(3) . . . . ? C3 N3 C5 N1 -1.8(3) . . . . ? C3 N3 C5 C6 166.9(3) . . . . ? C8 N4 C6 C5 176.3(2) . . . . ? Cu1 N4 C6 C5 -3.1(3) . . . . ? C8 N4 C6 C7 -0.6(4) . . . . ? Cu1 N4 C6 C7 180.0(2) . . . . ? N1 C5 C6 N4 11.8(3) . . . . ? N3 C5 C6 N4 -156.7(3) . . . . ? N1 C5 C6 C7 -171.1(2) . . . . ? N3 C5 C6 C7 20.4(4) . . . . ? C6 N4 C8 C9 171.6(2) . . . . ? Cu1 N4 C8 C9 -9.1(3) . . . . ? N4 C8 C9 C10 67.1(3) . . . . ? C12 N5 C10 C9 -175.3(2) . . . . ? Cu1 N5 C10 C9 11.3(3) . . . . ? C8 C9 C10 N5 -68.4(3) . . . . ? C10 N5 C12 C13 -174.8(2) . . . . ? Cu1 N5 C12 C13 -1.1(3) . . . . ? C10 N5 C12 C11 0.6(4) . . . . ? Cu1 N5 C12 C11 174.2(2) . . . . ? N7 N6 C13 N8 -1.1(3) . . . . ? Cu1 N6 C13 N8 -153.41(18) . . . . ? N7 N6 C13 C12 168.1(2) . . . . ? Cu1 N6 C13 C12 15.8(3) . . . . ? C15 N8 C13 N6 1.5(3) . . . . ? C15 N8 C13 C12 -166.0(3) . . . . ? N5 C12 C13 N6 -9.7(3) . . . . ? C11 C12 C13 N6 174.7(2) . . . . ? N5 C12 C13 N8 157.6(3) . . . . ? C11 C12 C13 N8 -18.0(4) . . . . ? N6 N7 C15 N8 0.9(3) . . . . ? Cu2 N7 C15 N8 156.76(17) . . . . ? N6 N7 C15 C16 -171.0(2) . . . . ? Cu2 N7 C15 C16 -15.1(3) . . . . ? C13 N8 C15 N7 -1.4(3) . . . . ? C13 N8 C15 C16 168.9(3) . . . . ? C18 N9 C16 C15 173.6(2) . . . . ? Cu2 N9 C16 C15 4.5(3) . . . . ? C18 N9 C16 C17 -2.8(4) . . . . ? Cu2 N9 C16 C17 -171.8(2) . . . . ? N7 C15 C16 N9 7.1(3) . . . . ? N8 C15 C16 N9 -163.1(3) . . . . ? N7 C15 C16 C17 -176.3(2) . . . . ? N8 C15 C16 C17 13.4(4) . . . . ? C16 N9 C18 C19 178.1(2) . . . . ? Cu2 N9 C18 C19 -13.4(3) . . . . ? N9 C18 C19 C20 69.0(3) . . . . ? C22 N10 C20 C19 -174.5(3) . . . . ? Cu2 N10 C20 C19 9.5(3) . . . . ? C18 C19 C20 N10 -66.6(3) . . . . ? C20 N10 C22 C3 -176.3(2) . . . . ? Cu2 N10 C22 C3 0.0(3) . . . . ? C20 N10 C22 C21 0.4(4) . . . . ? Cu2 N10 C22 C21 176.7(2) . . . . ? N2 C3 C22 N10 -9.6(4) . . . . ? N3 C3 C22 N10 160.5(3) . . . . ? N2 C3 C22 C21 173.5(3) . . . . ? N3 C3 C22 C21 -16.4(4) . . . . ? N1 Cu1 N30 C30 -16.1(12) . . . . ? N6 Cu1 N30 C30 -112.8(12) . . . . ? N4 Cu1 N30 C30 65.9(12) . . . . ? N5 Cu1 N30 C30 163.1(12) . . . . ? Cu1 N30 C30 C31 75(36) . . . . ? N2 Cu2 N40 C40 34.9(13) . . . . ? N7 Cu2 N40 C40 130.3(12) . . . . ? N9 Cu2 N40 C40 -146.1(12) . . . . ? N10 Cu2 N40 C40 -48.2(13) . . . . ? Cu2 N40 C40 C41 48(100) . . . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.672 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.081 data_ube _database_code_CSD 207831 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H27 Cu2 N13 S2' _chemical_formula_weight 664.77 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.144(16) _cell_length_b 12.482(8) _cell_length_c 16.676(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.22(4) _cell_angle_gamma 90.00 _cell_volume 5532(6) _cell_formula_units_Z 8 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 1.728 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.649364 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 10769 _diffrn_reflns_av_R_equivalents 0.0984 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 23.46 _reflns_number_total 3047 _reflns_number_gt 2376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0787P)^2^+26.4853P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3047 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1411 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 0.10389(3) 0.26686(7) 0.04178(7) 0.0231(4) Uani 1 1 d . . . Cu2 Cu 0.22895(3) 0.22210(7) 0.24862(7) 0.0214(4) Uani 1 1 d . . . N1 N 0.1163(2) 0.2567(4) 0.1635(4) 0.0149(19) Uani 1 1 d . . . N2 N 0.1569(2) 0.2485(4) 0.2341(5) 0.0179(18) Uani 1 1 d . . . C3 C 0.1420(3) 0.1957(5) 0.2909(6) 0.017(2) Uani 1 1 d . . . N3 N 0.0931(2) 0.1694(5) 0.2634(5) 0.0195(19) Uani 1 1 d . . . C5 C 0.0793(2) 0.2064(5) 0.1848(6) 0.020(3) Uani 1 1 d . . . C6 C 0.0320(3) 0.1924(6) 0.1132(7) 0.019(3) Uani 1 1 d . . . C7 C -0.0125(3) 0.1493(6) 0.1331(6) 0.033(2) Uani 1 1 d . . . H7A H -0.0272 0.2062 0.1580 0.040 Uiso 1 1 calc R . . H7B H -0.0018 0.0900 0.1736 0.040 Uiso 1 1 calc R . . H7C H -0.0377 0.1234 0.0808 0.040 Uiso 1 1 calc R . . N4 N 0.0350(2) 0.2172(5) 0.0412(6) 0.022(2) Uani 1 1 d . . . C8 C -0.0059(3) 0.2108(7) -0.0392(6) 0.033(3) Uani 1 1 d . . . H8A H -0.0147 0.2839 -0.0624 0.039 Uiso 1 1 calc R . . H8B H -0.0359 0.1796 -0.0297 0.039 Uiso 1 1 calc R . . C9 C 0.0082(3) 0.1440(7) -0.1023(6) 0.040(3) Uani 1 1 d . . . H9A H -0.0227 0.1290 -0.1506 0.048 Uiso 1 1 calc R . . H9B H 0.0212 0.0745 -0.0753 0.048 Uiso 1 1 calc R . . C10 C 0.0475(3) 0.1920(7) -0.1377(6) 0.042(3) Uani 1 1 d . . . H10A H 0.0505 0.1460 -0.1841 0.050 Uiso 1 1 calc R . . H10B H 0.0363 0.2639 -0.1615 0.050 Uiso 1 1 calc R . . N5 N 0.0966(2) 0.2008(5) -0.0711(5) 0.0276(19) Uani 1 1 d . . . C11 C 0.1441(3) 0.1298(7) -0.1630(6) 0.036(3) Uani 1 1 d . . . H11A H 0.1219 0.0681 -0.1832 0.043 Uiso 1 1 calc R . . H11B H 0.1792 0.1078 -0.1515 0.043 Uiso 1 1 calc R . . H11C H 0.1355 0.1860 -0.2065 0.043 Uiso 1 1 calc R . . C12 C 0.1378(3) 0.1718(5) -0.0839(6) 0.023(2) Uani 1 1 d . . . C13 C 0.1818(3) 0.1831(6) -0.0069(6) 0.020(2) Uani 1 1 d . . . N6 N 0.1757(2) 0.2429(4) 0.0562(5) 0.0205(19) Uani 1 1 d . . . N7 N 0.2164(2) 0.2233(4) 0.1255(5) 0.022(2) Uani 1 1 d . . . C15 C 0.2439(3) 0.1517(5) 0.0994(7) 0.021(3) Uani 1 1 d . . . N8 N 0.2247(2) 0.1258(5) 0.0169(5) 0.020(2) Uani 1 1 d . . . C16 C 0.2848(2) 0.1001(6) 0.1677(7) 0.022(3) Uani 1 1 d . . . C17 C 0.3198(3) 0.0279(7) 0.1416(6) 0.034(3) Uani 1 1 d . . . H17A H 0.3547 0.0456 0.1747 0.041 Uiso 1 1 calc R . . H17B H 0.3146 0.0378 0.0810 0.041 Uiso 1 1 calc R . . H17C H 0.3129 -0.0469 0.1522 0.041 Uiso 1 1 calc R . . N9 N 0.2839(2) 0.1209(4) 0.2420(6) 0.019(2) Uani 1 1 d . . . C18 C 0.3194(3) 0.0726(7) 0.3179(6) 0.035(3) Uani 1 1 d . . . H18A H 0.3446 0.1268 0.3482 0.042 Uiso 1 1 calc R . . H18B H 0.3374 0.0131 0.3010 0.042 Uiso 1 1 calc R . . C19 C 0.2928(3) 0.0305(6) 0.3766(6) 0.035(3) Uani 1 1 d . . . H19A H 0.3171 -0.0127 0.4214 0.042 Uiso 1 1 calc R . . H19B H 0.2656 -0.0182 0.3437 0.042 Uiso 1 1 calc R . . C20 C 0.2700(3) 0.1148(6) 0.4195(6) 0.036(3) Uani 1 1 d . . . H20A H 0.2611 0.0817 0.4666 0.043 Uiso 1 1 calc R . . H20B H 0.2948 0.1725 0.4433 0.043 Uiso 1 1 calc R . . N10 N 0.2252(2) 0.1595(4) 0.3574(4) 0.0215(18) Uani 1 1 d . . . C21 C 0.1679(3) 0.1208(6) 0.4417(6) 0.031(3) Uani 1 1 d . . . H21A H 0.1933 0.0704 0.4754 0.037 Uiso 1 1 calc R . . H21B H 0.1350 0.0851 0.4217 0.037 Uiso 1 1 calc R . . H21C H 0.1661 0.1826 0.4769 0.037 Uiso 1 1 calc R . . C22 C 0.1817(3) 0.1577(5) 0.3673(6) 0.019(2) Uani 1 1 d . . . N50 N 0.0856(2) 0.4240(5) -0.0016(5) 0.035(2) Uani 1 1 d . . . C50 C 0.0879(3) 0.5074(6) -0.0294(6) 0.029(2) Uani 1 1 d . . . S50 S 0.09097(8) 0.62601(16) -0.06837(19) 0.0477(9) Uani 1 1 d . . . N60 N 0.2750(2) 0.3535(5) 0.3042(5) 0.030(2) Uani 1 1 d . . . C60 C 0.3097(3) 0.4084(5) 0.3325(6) 0.021(2) Uani 1 1 d . . . S60 S 0.35868(8) 0.48556(17) 0.37158(17) 0.0393(7) Uani 1 1 d . . . N70 N 0.0694(3) 0.3402(7) -0.2784(6) 0.067(3) Uani 1 1 d . . . C70 C 0.0564(3) 0.4248(7) -0.2969(7) 0.041(3) Uani 1 1 d . . . C71 C 0.0410(4) 0.5324(8) -0.3224(8) 0.064(4) Uani 1 1 d . . . H71A H 0.0543 0.5542 -0.3673 0.077 Uiso 1 1 calc R . . H71B H 0.0540 0.5805 -0.2735 0.077 Uiso 1 1 calc R . . H71C H 0.0042 0.5362 -0.3437 0.077 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 0.0260(5) 0.0220(5) 0.0225(11) 0.0041(4) 0.0095(5) 0.0022(4) Cu2 0.0244(5) 0.0197(5) 0.0208(11) -0.0004(4) 0.0083(5) 0.0013(3) N1 0.022(3) 0.017(3) 0.006(6) 0.003(3) 0.005(3) 0.006(2) N2 0.027(3) 0.020(3) 0.012(6) 0.008(3) 0.013(3) 0.006(2) C3 0.026(4) 0.021(4) 0.005(7) -0.004(4) 0.005(4) 0.011(3) N3 0.025(3) 0.027(3) 0.010(7) 0.003(3) 0.011(3) 0.006(3) C5 0.014(4) 0.022(4) 0.028(9) -0.003(4) 0.011(4) 0.007(3) C6 0.023(4) 0.022(4) 0.017(9) 0.000(4) 0.016(4) 0.004(3) C7 0.038(5) 0.042(5) 0.020(8) 0.013(4) 0.012(4) -0.003(4) N4 0.026(3) 0.029(3) 0.012(8) 0.003(4) 0.010(4) 0.002(3) C8 0.026(4) 0.046(5) 0.024(8) -0.001(4) 0.005(4) 0.000(4) C9 0.038(5) 0.050(5) 0.025(9) 0.005(5) 0.001(5) -0.005(4) C10 0.038(5) 0.051(5) 0.034(9) -0.002(5) 0.011(5) 0.008(4) N5 0.038(4) 0.030(4) 0.014(6) 0.001(3) 0.007(4) 0.003(3) C11 0.046(5) 0.037(5) 0.025(9) -0.001(5) 0.013(5) 0.011(4) C12 0.036(5) 0.020(4) 0.015(8) 0.004(4) 0.009(4) 0.006(3) C13 0.032(4) 0.022(4) 0.010(7) 0.001(4) 0.013(4) -0.002(3) N6 0.031(4) 0.017(3) 0.017(7) 0.000(3) 0.012(4) -0.005(2) N7 0.025(3) 0.022(3) 0.021(7) 0.003(3) 0.008(3) -0.004(3) C15 0.024(4) 0.022(4) 0.024(9) -0.003(4) 0.017(4) -0.003(3) N8 0.022(3) 0.025(3) 0.017(7) 0.000(3) 0.011(3) -0.003(3) C16 0.018(4) 0.026(4) 0.020(10) -0.006(4) 0.002(4) -0.008(3) C17 0.030(4) 0.054(5) 0.017(8) -0.014(4) 0.005(4) 0.008(4) N9 0.022(3) 0.020(3) 0.014(8) -0.003(3) 0.001(4) 0.003(2) C18 0.020(4) 0.041(5) 0.042(9) -0.013(5) 0.006(4) 0.006(3) C19 0.019(4) 0.033(4) 0.044(9) 0.001(4) -0.001(4) 0.005(3) C20 0.033(4) 0.038(5) 0.031(9) 0.001(4) 0.005(4) 0.002(4) N10 0.022(3) 0.024(3) 0.014(6) 0.004(3) -0.002(3) 0.004(2) C21 0.043(5) 0.029(4) 0.023(9) 0.007(4) 0.013(5) 0.005(3) C22 0.034(5) 0.012(3) 0.011(8) 0.002(3) 0.006(4) 0.005(3) N50 0.035(4) 0.031(4) 0.032(7) 0.009(4) 0.003(4) 0.003(3) C50 0.033(4) 0.023(4) 0.029(8) 0.004(4) 0.009(4) 0.000(3) S50 0.0431(13) 0.0261(11) 0.073(3) 0.0164(12) 0.0173(13) 0.0016(9) N60 0.034(4) 0.030(4) 0.020(6) -0.008(3) 0.003(3) -0.005(3) C60 0.030(4) 0.020(4) 0.018(8) -0.002(4) 0.015(4) 0.004(3) S60 0.0427(13) 0.0343(11) 0.045(2) -0.0099(11) 0.0197(12) -0.0167(9) N70 0.094(7) 0.039(5) 0.062(9) -0.002(5) 0.017(5) -0.013(4) C70 0.043(5) 0.042(6) 0.033(9) -0.004(5) 0.007(5) -0.025(4) C71 0.064(7) 0.050(6) 0.080(11) 0.019(6) 0.024(6) 0.003(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 N1 1.947(7) . ? Cu1 N6 1.977(6) . ? Cu1 N5 2.003(7) . ? Cu1 N4 2.034(7) . ? Cu1 N50 2.095(7) . ? Cu2 N7 1.964(8) . ? Cu2 N2 1.989(6) . ? Cu2 N10 2.010(7) . ? Cu2 N9 2.028(6) . ? Cu2 N60 2.107(6) . ? N1 N2 1.348(9) . ? N1 C5 1.358(9) . ? N2 C3 1.331(10) . ? C3 N3 1.340(9) . ? C3 C22 1.470(11) . ? N3 C5 1.322(10) . ? C5 C6 1.477(12) . ? C6 N4 1.268(10) . ? C6 C7 1.498(11) . ? N4 C8 1.454(11) . ? C8 C9 1.494(12) . ? C9 C10 1.536(12) . ? C10 N5 1.464(11) . ? N5 C12 1.297(10) . ? C11 C12 1.484(12) . ? C12 C13 1.469(11) . ? C13 N8 1.346(9) . ? C13 N6 1.346(10) . ? N6 N7 1.356(9) . ? N7 C15 1.345(10) . ? C15 N8 1.342(10) . ? C15 C16 1.474(12) . ? C16 N9 1.274(10) . ? C16 C17 1.502(11) . ? N9 C18 1.459(11) . ? C18 C19 1.508(12) . ? C19 C20 1.529(12) . ? C20 N10 1.454(10) . ? N10 C22 1.286(9) . ? C21 C22 1.491(12) . ? N50 C50 1.150(9) . ? C50 S50 1.631(8) . ? N60 C60 1.158(9) . ? C60 S60 1.631(8) . ? N70 C70 1.127(12) . ? C70 C71 1.433(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N6 92.2(3) . . ? N1 Cu1 N5 151.7(2) . . ? N6 Cu1 N5 80.6(3) . . ? N1 Cu1 N4 80.1(3) . . ? N6 Cu1 N4 152.8(2) . . ? N5 Cu1 N4 93.8(3) . . ? N1 Cu1 N50 111.1(3) . . ? N6 Cu1 N50 108.0(2) . . ? N5 Cu1 N50 97.1(3) . . ? N4 Cu1 N50 99.1(3) . . ? N7 Cu2 N2 92.6(3) . . ? N7 Cu2 N10 154.3(2) . . ? N2 Cu2 N10 79.6(3) . . ? N7 Cu2 N9 80.0(3) . . ? N2 Cu2 N9 149.5(2) . . ? N10 Cu2 N9 94.3(3) . . ? N7 Cu2 N60 109.1(3) . . ? N2 Cu2 N60 112.3(2) . . ? N10 Cu2 N60 96.5(3) . . ? N9 Cu2 N60 98.0(2) . . ? N2 N1 C5 103.8(7) . . ? N2 N1 Cu1 136.4(5) . . ? C5 N1 Cu1 114.4(6) . . ? C3 N2 N1 106.5(6) . . ? C3 N2 Cu2 112.3(5) . . ? N1 N2 Cu2 131.1(6) . . ? N2 C3 N3 114.0(7) . . ? N2 C3 C22 116.6(7) . . ? N3 C3 C22 128.4(8) . . ? C5 N3 C3 100.8(6) . . ? N3 C5 N1 114.9(6) . . ? N3 C5 C6 130.7(7) . . ? N1 C5 C6 114.0(9) . . ? N4 C6 C5 114.4(7) . . ? N4 C6 C7 128.1(8) . . ? C5 C6 C7 117.4(9) . . ? C6 N4 C8 125.6(7) . . ? C6 N4 Cu1 115.5(5) . . ? C8 N4 Cu1 118.9(7) . . ? N4 C8 C9 111.6(7) . . ? C8 C9 C10 116.3(7) . . ? N5 C10 C9 110.9(8) . . ? C12 N5 C10 121.7(8) . . ? C12 N5 Cu1 116.6(6) . . ? C10 N5 Cu1 121.6(6) . . ? N5 C12 C13 111.9(8) . . ? N5 C12 C11 128.3(8) . . ? C13 C12 C11 119.7(7) . . ? N8 C13 N6 113.4(7) . . ? N8 C13 C12 128.6(8) . . ? N6 C13 C12 116.6(7) . . ? C13 N6 N7 106.1(6) . . ? C13 N6 Cu1 112.2(5) . . ? N7 N6 Cu1 132.3(6) . . ? C15 N7 N6 104.9(7) . . ? C15 N7 Cu2 114.1(6) . . ? N6 N7 Cu2 134.8(5) . . ? N8 C15 N7 114.4(7) . . ? N8 C15 C16 129.4(7) . . ? N7 C15 C16 115.2(9) . . ? C15 N8 C13 101.1(7) . . ? N9 C16 C15 113.8(7) . . ? N9 C16 C17 128.9(8) . . ? C15 C16 C17 117.3(10) . . ? C16 N9 C18 122.2(7) . . ? C16 N9 Cu2 116.0(5) . . ? C18 N9 Cu2 121.8(7) . . ? N9 C18 C19 111.3(6) . . ? C18 C19 C20 116.0(7) . . ? N10 C20 C19 109.3(7) . . ? C22 N10 C20 122.7(7) . . ? C22 N10 Cu2 117.2(5) . . ? C20 N10 Cu2 120.0(5) . . ? N10 C22 C3 111.6(8) . . ? N10 C22 C21 129.2(7) . . ? C3 C22 C21 119.2(7) . . ? C50 N50 Cu1 161.3(7) . . ? N50 C50 S50 179.7(10) . . ? C60 N60 Cu2 162.6(6) . . ? N60 C60 S60 179.4(8) . . ? N70 C70 C71 177.9(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 N6 Cu1 N1 N2 6.5(6) . . . . ? N5 Cu1 N1 N2 80.7(8) . . . . ? N4 Cu1 N1 N2 160.2(6) . . . . ? N50 Cu1 N1 N2 -103.8(6) . . . . ? N6 Cu1 N1 C5 -142.5(5) . . . . ? N5 Cu1 N1 C5 -68.3(7) . . . . ? N4 Cu1 N1 C5 11.3(4) . . . . ? N50 Cu1 N1 C5 107.3(5) . . . . ? C5 N1 N2 C3 -0.1(7) . . . . ? Cu1 N1 N2 C3 -151.1(5) . . . . ? C5 N1 N2 Cu2 141.3(5) . . . . ? Cu1 N1 N2 Cu2 -9.7(9) . . . . ? N7 Cu2 N2 C3 143.2(5) . . . . ? N10 Cu2 N2 C3 -12.1(5) . . . . ? N9 Cu2 N2 C3 68.6(9) . . . . ? N60 Cu2 N2 C3 -105.0(5) . . . . ? N7 Cu2 N2 N1 3.4(6) . . . . ? N10 Cu2 N2 N1 -151.9(6) . . . . ? N9 Cu2 N2 N1 -71.2(9) . . . . ? N60 Cu2 N2 N1 115.3(6) . . . . ? N1 N2 C3 N3 -1.3(8) . . . . ? Cu2 N2 C3 N3 -150.7(5) . . . . ? N1 N2 C3 C22 168.1(6) . . . . ? Cu2 N2 C3 C22 18.6(8) . . . . ? N2 C3 N3 C5 2.0(8) . . . . ? C22 C3 N3 C5 -165.8(7) . . . . ? C3 N3 C5 N1 -2.1(8) . . . . ? C3 N3 C5 C6 170.6(7) . . . . ? N2 N1 C5 N3 1.5(8) . . . . ? Cu1 N1 C5 N3 160.0(5) . . . . ? N2 N1 C5 C6 -172.5(6) . . . . ? Cu1 N1 C5 C6 -14.0(7) . . . . ? N3 C5 C6 N4 -164.4(7) . . . . ? N1 C5 C6 N4 8.3(9) . . . . ? N3 C5 C6 C7 14.3(11) . . . . ? N1 C5 C6 C7 -173.0(6) . . . . ? C5 C6 N4 C8 180.0(6) . . . . ? C7 C6 N4 C8 1.5(12) . . . . ? C5 C6 N4 Cu1 1.1(8) . . . . ? C7 C6 N4 Cu1 -177.4(6) . . . . ? N1 Cu1 N4 C6 -6.8(5) . . . . ? N6 Cu1 N4 C6 68.5(9) . . . . ? N5 Cu1 N4 C6 145.4(5) . . . . ? N50 Cu1 N4 C6 -116.8(5) . . . . ? N1 Cu1 N4 C8 174.3(6) . . . . ? N6 Cu1 N4 C8 -110.4(8) . . . . ? N5 Cu1 N4 C8 -33.5(6) . . . . ? N50 Cu1 N4 C8 64.3(6) . . . . ? C6 N4 C8 C9 -124.7(8) . . . . ? Cu1 N4 C8 C9 54.0(8) . . . . ? N4 C8 C9 C10 -70.4(10) . . . . ? C8 C9 C10 N5 66.7(10) . . . . ? C9 C10 N5 C12 135.0(8) . . . . ? C9 C10 N5 Cu1 -49.0(9) . . . . ? N1 Cu1 N5 C12 -75.7(8) . . . . ? N6 Cu1 N5 C12 1.3(5) . . . . ? N4 Cu1 N5 C12 -151.9(6) . . . . ? N50 Cu1 N5 C12 108.4(6) . . . . ? N1 Cu1 N5 C10 108.1(7) . . . . ? N6 Cu1 N5 C10 -174.9(6) . . . . ? N4 Cu1 N5 C10 31.9(6) . . . . ? N50 Cu1 N5 C10 -67.8(6) . . . . ? C10 N5 C12 C13 -177.3(7) . . . . ? Cu1 N5 C12 C13 6.5(8) . . . . ? C10 N5 C12 C11 1.9(12) . . . . ? Cu1 N5 C12 C11 -174.3(6) . . . . ? N5 C12 C13 N8 150.4(8) . . . . ? C11 C12 C13 N8 -28.8(12) . . . . ? N5 C12 C13 N6 -15.1(10) . . . . ? C11 C12 C13 N6 165.6(7) . . . . ? N8 C13 N6 N7 -0.7(8) . . . . ? C12 C13 N6 N7 167.0(6) . . . . ? N8 C13 N6 Cu1 -151.7(5) . . . . ? C12 C13 N6 Cu1 16.1(8) . . . . ? N1 Cu1 N6 C13 143.0(5) . . . . ? N5 Cu1 N6 C13 -9.5(5) . . . . ? N4 Cu1 N6 C13 70.5(10) . . . . ? N50 Cu1 N6 C13 -104.0(5) . . . . ? N1 Cu1 N6 N7 2.1(6) . . . . ? N5 Cu1 N6 N7 -150.4(6) . . . . ? N4 Cu1 N6 N7 -70.4(10) . . . . ? N50 Cu1 N6 N7 115.1(6) . . . . ? C13 N6 N7 C15 -0.8(7) . . . . ? Cu1 N6 N7 C15 141.8(5) . . . . ? C13 N6 N7 Cu2 -150.1(6) . . . . ? Cu1 N6 N7 Cu2 -7.5(9) . . . . ? N2 Cu2 N7 C15 -142.6(5) . . . . ? N10 Cu2 N7 C15 -71.3(7) . . . . ? N9 Cu2 N7 C15 7.7(5) . . . . ? N60 Cu2 N7 C15 102.7(5) . . . . ? N2 Cu2 N7 N6 4.7(6) . . . . ? N10 Cu2 N7 N6 76.0(8) . . . . ? N9 Cu2 N7 N6 155.0(6) . . . . ? N60 Cu2 N7 N6 -110.0(6) . . . . ? N6 N7 C15 N8 2.1(8) . . . . ? Cu2 N7 C15 N8 158.7(5) . . . . ? N6 N7 C15 C16 -167.6(6) . . . . ? Cu2 N7 C15 C16 -11.0(7) . . . . ? N7 C15 N8 C13 -2.4(8) . . . . ? C16 C15 N8 C13 165.5(7) . . . . ? N6 C13 N8 C15 1.8(8) . . . . ? C12 C13 N8 C15 -164.1(8) . . . . ? N8 C15 C16 N9 -159.3(7) . . . . ? N7 C15 C16 N9 8.6(9) . . . . ? N8 C15 C16 C17 18.1(11) . . . . ? N7 C15 C16 C17 -174.0(6) . . . . ? C15 C16 N9 C18 176.4(6) . . . . ? C17 C16 N9 C18 -0.7(11) . . . . ? C15 C16 N9 Cu2 -2.0(7) . . . . ? C17 C16 N9 Cu2 -179.0(6) . . . . ? N7 Cu2 N9 C16 -3.0(5) . . . . ? N2 Cu2 N9 C16 75.0(8) . . . . ? N10 Cu2 N9 C16 151.7(5) . . . . ? N60 Cu2 N9 C16 -111.1(5) . . . . ? N7 Cu2 N9 C18 178.7(6) . . . . ? N2 Cu2 N9 C18 -103.4(8) . . . . ? N10 Cu2 N9 C18 -26.6(6) . . . . ? N60 Cu2 N9 C18 70.6(6) . . . . ? C16 N9 C18 C19 -133.1(7) . . . . ? Cu2 N9 C18 C19 45.1(8) . . . . ? N9 C18 C19 C20 -68.2(9) . . . . ? C18 C19 C20 N10 73.4(9) . . . . ? C19 C20 N10 C22 123.1(8) . . . . ? C19 C20 N10 Cu2 -54.4(8) . . . . ? N7 Cu2 N10 C22 -70.4(8) . . . . ? N2 Cu2 N10 C22 3.8(5) . . . . ? N9 Cu2 N10 C22 -146.1(5) . . . . ? N60 Cu2 N10 C22 115.3(5) . . . . ? N7 Cu2 N10 C20 107.3(7) . . . . ? N2 Cu2 N10 C20 -178.6(6) . . . . ? N9 Cu2 N10 C20 31.5(6) . . . . ? N60 Cu2 N10 C20 -67.0(6) . . . . ? C20 N10 C22 C3 -172.9(6) . . . . ? Cu2 N10 C22 C3 4.7(7) . . . . ? C20 N10 C22 C21 5.1(11) . . . . ? Cu2 N10 C22 C21 -177.3(6) . . . . ? N2 C3 C22 N10 -15.6(9) . . . . ? N3 C3 C22 N10 152.0(7) . . . . ? N2 C3 C22 C21 166.1(7) . . . . ? N3 C3 C22 C21 -26.3(11) . . . . ? N1 Cu1 N50 C50 114(2) . . . . ? N6 Cu1 N50 C50 15(2) . . . . ? N5 Cu1 N50 C50 -68(2) . . . . ? N4 Cu1 N50 C50 -163(2) . . . . ? Cu1 N50 C50 S50 -131(100) . . . . ? N7 Cu2 N60 C60 -79(2) . . . . ? N2 Cu2 N60 C60 180(2) . . . . ? N10 Cu2 N60 C60 98(2) . . . . ? N9 Cu2 N60 C60 3(2) . . . . ? Cu2 N60 C60 S60 45(100) . . . . ? _diffrn_measured_fraction_theta_max 0.749 _diffrn_reflns_theta_full 23.46 _diffrn_measured_fraction_theta_full 0.749 _refine_diff_density_max 1.096 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.118 data_cutx _database_code_CSD 207832 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H76.50 Cl4 Cu6 N33.50 O16 S2' _chemical_formula_weight 2098.20 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' Cl Cl 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.686(4) _cell_length_b 14.481(4) _cell_length_c 24.546(7) _cell_angle_alpha 87.383(4) _cell_angle_beta 84.732(4) _cell_angle_gamma 64.267(4) _cell_volume 4045(2) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description wedge _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2134 _exptl_absorpt_coefficient_mu 1.818 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.603877 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 51507 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.0769 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.61 _reflns_number_total 16862 _reflns_number_gt 11017 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0481P)^2^+23.2696P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16862 _refine_ls_number_parameters 1276 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1036 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.1731 _refine_ls_wR_factor_gt 0.1644 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.003 _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 0.75578(7) 0.44634(6) 0.28705(3) 0.0288(2) Uani 1 1 d . . . Cu2 Cu 0.66670(7) 0.43396(6) 0.13505(3) 0.02412(18) Uani 1 1 d . . . Cu3 Cu 0.57597(8) 0.14470(7) 0.33036(3) 0.0324(2) Uani 1 1 d . . . Cu4 Cu 0.48627(7) 0.15052(6) 0.17519(3) 0.0294(2) Uani 1 1 d . . . Cu5 Cu 0.35207(8) 0.57537(7) 0.35481(3) 0.0364(2) Uani 1 1 d . . . Cu6 Cu 0.25975(7) 0.57875(6) 0.20183(3) 0.02478(18) Uani 1 1 d . . . S1 S 0.57810(15) 0.48007(13) 0.35602(7) 0.0313(4) Uani 1 1 d . . . S2 S 0.43855(14) 0.49600(12) 0.13617(6) 0.0247(3) Uani 1 1 d . . . N1 N 0.5830(5) 0.2851(5) 0.3481(2) 0.0376(14) Uani 1 1 d . . . N2 N 0.4531(5) 0.2958(5) 0.1442(2) 0.0369(14) Uani 1 1 d . . . N11 N 0.7075(5) 0.5455(4) 0.2268(2) 0.0284(12) Uani 1 1 d . . . N12 N 0.6791(5) 0.5405(4) 0.1762(2) 0.0273(12) Uani 1 1 d . . . N13 N 0.7724(5) 0.6425(4) 0.1722(3) 0.0361(14) Uani 1 1 d . . . N14 N 0.8249(5) 0.5391(5) 0.3077(2) 0.0355(14) Uani 1 1 d . . . N15 N 0.8725(5) 0.3236(5) 0.3253(2) 0.0333(14) Uani 1 1 d . . . N16 N 0.7541(5) 0.3365(4) 0.2444(2) 0.0253(12) Uani 1 1 d . . . N17 N 0.7232(4) 0.3322(4) 0.1943(2) 0.0223(11) Uani 1 1 d . . . N18 N 0.8659(5) 0.1782(4) 0.2125(2) 0.0291(12) Uani 1 1 d . . . N19 N 0.7291(4) 0.3050(4) 0.0919(2) 0.0249(12) Uani 1 1 d . . . N20 N 0.6861(4) 0.5201(4) 0.0725(2) 0.0254(12) Uani 1 1 d . . . N31 N 0.6676(5) 0.0984(4) 0.2596(2) 0.0298(13) Uani 1 1 d . . . N32 N 0.6375(5) 0.1001(4) 0.2079(2) 0.0301(13) Uani 1 1 d . . . N33 N 0.8029(5) -0.0456(4) 0.2172(3) 0.0402(15) Uani 1 1 d . . . N34 N 0.7278(6) 0.0390(5) 0.3567(3) 0.0420(16) Uani 1 1 d . . . N35 N 0.4843(6) 0.1221(5) 0.3963(2) 0.0416(15) Uani 1 1 d . . . N36 N 0.4263(5) 0.1792(4) 0.2988(2) 0.0303(13) Uani 1 1 d . . . N37 N 0.3974(5) 0.1785(4) 0.2474(2) 0.0301(13) Uani 1 1 d . . . N38 N 0.2782(5) 0.1313(5) 0.3030(3) 0.0403(15) Uani 1 1 d . . . N39 N 0.3483(5) 0.1265(4) 0.1586(3) 0.0365(14) Uani 1 1 d . . . N40 N 0.5911(6) 0.0508(4) 0.1170(2) 0.0375(14) Uani 1 1 d . . . N51 N 0.3183(5) 0.4792(4) 0.3135(2) 0.0290(12) Uani 1 1 d . A . N52 N 0.2847(4) 0.4834(4) 0.2634(2) 0.0255(12) Uani 1 1 d . . . N53 N 0.1987(5) 0.4024(4) 0.3175(2) 0.0369(14) Uani 1 1 d . . . N54 N 0.3167(5) 0.4981(6) 0.4170(3) 0.0466(17) Uani 1 1 d . A . N56 N 0.3157(5) 0.6758(4) 0.2957(2) 0.0326(14) Uani 1 1 d . A . N57 N 0.2853(5) 0.6766(4) 0.2443(2) 0.0273(12) Uani 1 1 d . . . N58 N 0.1955(5) 0.8389(5) 0.2752(3) 0.0431(16) Uani 1 1 d . . . N59 N 0.1681(5) 0.7072(4) 0.1609(2) 0.0284(12) Uani 1 1 d . . . N60 N 0.1627(5) 0.5091(4) 0.1821(2) 0.0322(13) Uani 1 1 d . . . C1 C 0.5812(6) 0.3651(6) 0.3512(3) 0.0299(15) Uani 1 1 d . . . C2 C 0.4472(5) 0.3778(5) 0.1412(2) 0.0269(14) Uani 1 1 d . . . C13 C 0.7206(6) 0.5978(5) 0.1445(3) 0.0305(15) Uani 1 1 d . . . C15 C 0.7626(6) 0.6070(5) 0.2232(3) 0.0307(15) Uani 1 1 d . . . C16 C 0.8180(6) 0.6096(6) 0.2732(3) 0.0388(18) Uani 1 1 d . . . C17 C 0.8626(8) 0.6889(7) 0.2773(4) 0.054(2) Uani 1 1 d . . . H17A H 0.9346 0.6598 0.2965 0.081 Uiso 1 1 calc R . . H17B H 0.8030 0.7480 0.2977 0.081 Uiso 1 1 calc R . . H17C H 0.8793 0.7109 0.2405 0.081 Uiso 1 1 calc R . . C18 C 0.8816(7) 0.5258(6) 0.3586(3) 0.047(2) Uani 1 1 d . . . H18A H 0.8453 0.5914 0.3788 0.056 Uiso 1 1 calc R . . H18B H 0.9655 0.5091 0.3497 0.056 Uiso 1 1 calc R . . C19 C 0.8724(8) 0.4441(7) 0.3946(3) 0.052(2) Uani 1 1 d . . . H19A H 0.7880 0.4624 0.4036 0.062 Uiso 1 1 calc R . . H19B H 0.9064 0.4445 0.4293 0.062 Uiso 1 1 calc R . . C20 C 0.9307(7) 0.3348(6) 0.3729(3) 0.047(2) Uani 1 1 d . . . H20A H 1.0144 0.3161 0.3617 0.057 Uiso 1 1 calc R . . H20B H 0.9271 0.2871 0.4024 0.057 Uiso 1 1 calc R . . C21 C 0.9824(7) 0.1346(6) 0.3263(3) 0.0438(19) Uani 1 1 d . . . H21A H 0.9583 0.1269 0.3646 0.066 Uiso 1 1 calc R . . H21B H 1.0614 0.1315 0.3236 0.066 Uiso 1 1 calc R . . H21C H 0.9827 0.0791 0.3047 0.066 Uiso 1 1 calc R . . C22 C 0.8980(6) 0.2359(5) 0.3047(3) 0.0294(15) Uani 1 1 d . . . C23 C 0.8381(6) 0.2435(5) 0.2545(2) 0.0247(14) Uani 1 1 d . . . C25 C 0.7918(6) 0.2372(5) 0.1764(3) 0.0257(14) Uani 1 1 d . . . C26 C 0.7883(6) 0.2220(5) 0.1175(3) 0.0270(14) Uani 1 1 d . . . C27 C 0.8595(7) 0.1195(5) 0.0921(3) 0.0378(17) Uani 1 1 d . . . H27A H 0.8112 0.1034 0.0687 0.057 Uiso 1 1 calc R . . H27B H 0.8865 0.0672 0.1209 0.057 Uiso 1 1 calc R . . H27C H 0.9274 0.1204 0.0700 0.057 Uiso 1 1 calc R . . C28 C 0.7239(6) 0.3069(5) 0.0319(3) 0.0309(15) Uani 1 1 d . . . H28A H 0.6961 0.2563 0.0218 0.037 Uiso 1 1 calc R . . H28B H 0.8039 0.2865 0.0139 0.037 Uiso 1 1 calc R . . C29 C 0.6437(6) 0.4111(5) 0.0112(3) 0.0294(15) Uani 1 1 d . . . H29A H 0.5663 0.4337 0.0321 0.035 Uiso 1 1 calc R . . H29B H 0.6322 0.4048 -0.0276 0.035 Uiso 1 1 calc R . . C30 C 0.6864(6) 0.4946(6) 0.0150(3) 0.0337(16) Uani 1 1 d . . . H30A H 0.7669 0.4705 -0.0029 0.040 Uiso 1 1 calc R . . H30B H 0.6347 0.5569 -0.0046 0.040 Uiso 1 1 calc R . . C31 C 0.7556(7) 0.6508(6) 0.0450(3) 0.0434(19) Uani 1 1 d . . . H31A H 0.7017 0.6759 0.0159 0.065 Uiso 1 1 calc R . . H31B H 0.8351 0.6083 0.0291 0.065 Uiso 1 1 calc R . . H31C H 0.7551 0.7092 0.0639 0.065 Uiso 1 1 calc R . . C32 C 0.7173(6) 0.5886(5) 0.0848(3) 0.0309(15) Uani 1 1 d . . . C33 C 0.7181(6) 0.0133(5) 0.1845(3) 0.0358(16) Uani 1 1 d . . . C35 C 0.7654(6) 0.0106(5) 0.2642(3) 0.0359(17) Uani 1 1 d . . . C36 C 0.8020(7) -0.0175(6) 0.3188(3) 0.0425(19) Uani 1 1 d . . . C37 C 0.9165(7) -0.1080(7) 0.3285(4) 0.058(2) Uani 1 1 d . . . H37A H 0.9010 -0.1603 0.3498 0.086 Uiso 1 1 calc R . . H37B H 0.9646 -0.0859 0.3487 0.086 Uiso 1 1 calc R . . H37C H 0.9585 -0.1368 0.2933 0.086 Uiso 1 1 calc R . . C38 C 0.7478(8) 0.0180(7) 0.4144(3) 0.059(2) Uani 1 1 d . . . H38A H 0.8230 0.0191 0.4212 0.071 Uiso 1 1 calc R . . H38B H 0.7542 -0.0514 0.4237 0.071 Uiso 1 1 calc R . . C39 C 0.6508(8) 0.0949(8) 0.4502(3) 0.059(2) Uani 1 1 d . . . H39A H 0.6415 0.1642 0.4385 0.070 Uiso 1 1 calc R . . H39B H 0.6743 0.0842 0.4881 0.070 Uiso 1 1 calc R . . C40 C 0.5323(9) 0.0922(8) 0.4502(3) 0.063(3) Uani 1 1 d . . . H40A H 0.5411 0.0222 0.4596 0.075 Uiso 1 1 calc R . . H40B H 0.4768 0.1396 0.4784 0.075 Uiso 1 1 calc R . . C41 C 0.3071(8) 0.1001(8) 0.4292(4) 0.063(3) Uani 1 1 d . . . H41A H 0.3486 0.0290 0.4416 0.094 Uiso 1 1 calc R . . H41B H 0.2365 0.1086 0.4122 0.094 Uiso 1 1 calc R . . H41C H 0.2846 0.1461 0.4606 0.094 Uiso 1 1 calc R . . C42 C 0.3858(7) 0.1256(6) 0.3883(3) 0.0440(19) Uani 1 1 d . . . C43 C 0.3556(6) 0.1497(6) 0.3303(3) 0.0362(17) Uani 1 1 d . . . C45 C 0.3110(6) 0.1489(6) 0.2521(3) 0.0373(17) Uani 1 1 d . . . C46 C 0.2804(7) 0.1245(6) 0.1997(3) 0.0409(18) Uani 1 1 d . . . C47 C 0.1791(8) 0.0972(7) 0.1990(4) 0.059(2) Uani 1 1 d . . . H47A H 0.1648 0.0910 0.1611 0.088 Uiso 1 1 calc R . . H47B H 0.1088 0.1509 0.2174 0.088 Uiso 1 1 calc R . . H47C H 0.1976 0.0317 0.2181 0.088 Uiso 1 1 calc R . . C48 C 0.3353(7) 0.0996(6) 0.1029(3) 0.047(2) Uani 1 1 d . . . H48A H 0.2543 0.1427 0.0930 0.056 Uiso 1 1 calc R . . H48B H 0.3485 0.0271 0.1025 0.056 Uiso 1 1 calc R . . C49 C 0.4200(8) 0.1152(6) 0.0620(3) 0.052(2) Uani 1 1 d . . . H49A H 0.4135 0.1850 0.0665 0.063 Uiso 1 1 calc R . . H49B H 0.3968 0.1117 0.0250 0.063 Uiso 1 1 calc R . . C50 C 0.5480(8) 0.0388(6) 0.0650(3) 0.047(2) Uani 1 1 d . . . H50A H 0.5555 -0.0319 0.0626 0.057 Uiso 1 1 calc R . . H50B H 0.5962 0.0503 0.0338 0.057 Uiso 1 1 calc R . . C51 C 0.7810(8) -0.1024(6) 0.1002(4) 0.060(2) Uani 1 1 d . . . H51A H 0.7421 -0.1203 0.0725 0.089 Uiso 1 1 calc R . . H51B H 0.8147 -0.1603 0.1255 0.089 Uiso 1 1 calc R . . H51C H 0.8436 -0.0868 0.0822 0.089 Uiso 1 1 calc R . . C52 C 0.6926(7) -0.0099(6) 0.1316(3) 0.0426(19) Uani 1 1 d . . . C53 C 0.2120(6) 0.4368(5) 0.2671(3) 0.0309(15) Uani 1 1 d . A . C55 C 0.2653(6) 0.4317(5) 0.3448(3) 0.0353(17) Uani 1 1 d . A . C56 C 0.2764(7) 0.4347(7) 0.4045(3) 0.049(2) Uani 1 1 d . . . C57 C 0.2332(8) 0.3732(7) 0.4426(4) 0.068(3) Uani 1 1 d . . . H57A H 0.1704 0.4191 0.4683 0.101 Uiso 1 1 calc R . . H57B H 0.2979 0.3247 0.4630 0.101 Uiso 1 1 calc R . . H57C H 0.2028 0.3353 0.4216 0.101 Uiso 1 1 calc R . . C58 C 0.3304(10) 0.5176(9) 0.4739(3) 0.080(4) Uani 0.50 1 d P A 1 H58A H 0.2543 0.5354 0.4954 0.096 Uiso 0.50 1 calc PR A 1 H58B H 0.3880 0.4527 0.4892 0.096 Uiso 0.50 1 calc PR A 1 C59 C 0.364(2) 0.589(2) 0.4818(9) 0.068(8) Uani 0.50 1 d P A 1 H59A H 0.4438 0.5675 0.4638 0.082 Uiso 0.50 1 calc PR A 1 H59B H 0.3692 0.5926 0.5216 0.082 Uiso 0.50 1 calc PR A 1 C60 C 0.289(2) 0.692(2) 0.4623(8) 0.058(6) Uani 0.50 1 d P A 1 H60A H 0.2075 0.7123 0.4777 0.069 Uiso 0.50 1 calc PR A 1 H60B H 0.3163 0.7411 0.4751 0.069 Uiso 0.50 1 calc PR A 1 N55 N 0.293(2) 0.695(2) 0.4026(10) 0.035(5) Uani 0.50 1 d P A 1 C61 C 0.1817(17) 0.8849(14) 0.4008(8) 0.063(6) Uani 0.50 1 d P A 1 H61A H 0.2313 0.9216 0.3974 0.095 Uiso 0.50 1 calc PR A 1 H61B H 0.1576 0.8799 0.4395 0.095 Uiso 0.50 1 calc PR A 1 H61C H 0.1120 0.9223 0.3807 0.095 Uiso 0.50 1 calc PR A 1 C62 C 0.249(2) 0.779(2) 0.3776(11) 0.040(6) Uani 0.50 1 d P A 1 C58A C 0.3304(10) 0.5176(9) 0.4739(3) 0.080(4) Uani 0.50 1 d P A 2 H58C H 0.4133 0.4766 0.4817 0.096 Uiso 0.50 1 calc PR A 2 H58D H 0.2816 0.4938 0.4990 0.096 Uiso 0.50 1 calc PR A 2 C59A C 0.296(2) 0.630(2) 0.4859(8) 0.045(5) Uani 0.50 1 d P A 2 H59C H 0.3125 0.6320 0.5244 0.054 Uiso 0.50 1 calc PR A 2 H59D H 0.2100 0.6657 0.4849 0.054 Uiso 0.50 1 calc PR A 2 C60A C 0.3470(17) 0.7000(14) 0.4523(7) 0.039(4) Uani 0.50 1 d P A 2 H60C H 0.3100 0.7695 0.4684 0.047 Uiso 0.50 1 calc PR A 2 H60D H 0.4324 0.6715 0.4560 0.047 Uiso 0.50 1 calc PR A 2 N55A N 0.3269(17) 0.7086(17) 0.3934(9) 0.024(4) Uani 0.50 1 d P A 2 C61A C 0.2575(16) 0.8968(11) 0.3852(7) 0.040(4) Uani 0.50 1 d P A 2 H61D H 0.2610 0.8948 0.4250 0.059 Uiso 0.50 1 calc PR A 2 H61E H 0.1785 0.9445 0.3759 0.059 Uiso 0.50 1 calc PR A 2 H61F H 0.3147 0.9199 0.3677 0.059 Uiso 0.50 1 calc PR A 2 C62A C 0.285(2) 0.7941(19) 0.3656(10) 0.030(5) Uani 0.50 1 d P A 2 C63 C 0.2595(7) 0.7718(6) 0.3131(3) 0.046(2) Uani 1 1 d . A . C65 C 0.2134(6) 0.7738(5) 0.2336(3) 0.0304(15) Uani 1 1 d . A . C66 C 0.1552(6) 0.7915(5) 0.1829(3) 0.0320(16) Uani 1 1 d . A . C67 C 0.0875(7) 0.8988(5) 0.1619(3) 0.0425(19) Uani 1 1 d . . . H67A H 0.0061 0.9112 0.1585 0.064 Uiso 1 1 calc R A . H67B H 0.1235 0.9069 0.1261 0.064 Uiso 1 1 calc R . . H67C H 0.0890 0.9480 0.1876 0.064 Uiso 1 1 calc R . . C68 C 0.1195(6) 0.7023(5) 0.1096(3) 0.0330(16) Uani 1 1 d . A . H68A H 0.1845 0.6687 0.0812 0.040 Uiso 1 1 calc R . . H68B H 0.0704 0.7727 0.0969 0.040 Uiso 1 1 calc R . . C69 C 0.0461(6) 0.6432(6) 0.1174(3) 0.0385(17) Uani 1 1 d . . . H69A H 0.0046 0.6521 0.0839 0.046 Uiso 1 1 calc R A . H69B H -0.0144 0.6750 0.1479 0.046 Uiso 1 1 calc R . . C70 C 0.1088(7) 0.5295(6) 0.1292(3) 0.0389(18) Uani 1 1 d . A . H70A H 0.0522 0.4991 0.1300 0.047 Uiso 1 1 calc R . . H70B H 0.1707 0.4962 0.0995 0.047 Uiso 1 1 calc R . . C71 C 0.0815(7) 0.3850(6) 0.2143(3) 0.0430(19) Uani 1 1 d . . . H71A H 0.0015 0.4312 0.2056 0.065 Uiso 1 1 calc R A . H71B H 0.0789 0.3507 0.2494 0.065 Uiso 1 1 calc R . . H71C H 0.1187 0.3334 0.1855 0.065 Uiso 1 1 calc R . . C72 C 0.1509(6) 0.4453(5) 0.2177(3) 0.0340(16) Uani 1 1 d . A . Cl10 Cl 0.01644(18) 0.32292(17) 0.06996(10) 0.0537(5) Uani 1 1 d . . . O11 O 0.1278(5) 0.3193(5) 0.0769(3) 0.0562(15) Uani 1 1 d . B . O12 O 0.0245(15) 0.2184(14) 0.0882(11) 0.111(8) Uani 0.50 1 d P B 1 O13 O -0.027(3) 0.349(3) 0.0216(9) 0.144(16) Uani 0.50 1 d P B 1 O14 O -0.0748(14) 0.3864(14) 0.1150(9) 0.084(7) Uani 0.50 1 d P B 1 O12A O 0.030(2) 0.2402(18) 0.0403(14) 0.136(10) Uani 0.50 1 d PU B 2 O13A O -0.031(2) 0.4117(18) 0.0316(12) 0.102(9) Uani 0.50 1 d P B 2 O14A O -0.0547(18) 0.3387(16) 0.1138(8) 0.075(6) Uani 0.50 1 d PU B 2 Cl20 Cl 0.4120(2) 0.79832(17) 0.07592(10) 0.0574(6) Uani 1 1 d . . . O21 O 0.4966(7) 0.8240(6) 0.0956(3) 0.090(2) Uani 1 1 d . . . O22 O 0.3946(8) 0.7261(7) 0.1072(4) 0.112(3) Uani 1 1 d . . . O23 O 0.3121(8) 0.8798(7) 0.0579(4) 0.120(3) Uani 1 1 d . . . O24 O 0.4724(7) 0.7397(7) 0.0244(3) 0.100(3) Uani 1 1 d . . . Cl30 Cl 0.0211(6) 0.3297(5) 0.5445(3) 0.0383(13) Uani 0.50 1 d P C 1 O31 O -0.0071(14) 0.2856(11) 0.5002(6) 0.086(5) Uani 0.50 1 d P C 1 O32 O 0.0001(12) 0.4321(11) 0.5293(6) 0.066(4) Uani 0.50 1 d P C 1 O33 O 0.1407(10) 0.2733(11) 0.5541(6) 0.062(4) Uani 0.50 1 d P C 1 O34 O -0.052(2) 0.333(2) 0.5949(11) 0.074(11) Uani 0.50 1 d P C 1 N200 N -0.0817(14) 0.3375(12) 0.6392(7) 0.051(5) Uani 0.50 1 d P D 2 C200 C -0.031(4) 0.333(3) 0.596(3) 0.07(2) Uani 0.50 1 d P D 2 C201 C 0.039(5) 0.315(5) 0.543(2) 0.16(3) Uani 0.50 1 d P D 2 H20C H 0.1217 0.2943 0.5493 0.233 Uiso 0.50 1 calc PR D 2 H20D H 0.0107 0.3779 0.5209 0.233 Uiso 0.50 1 calc PR D 2 H20E H 0.0330 0.2603 0.5232 0.233 Uiso 0.50 1 calc PR D 2 Cl40 Cl 0.0218(3) 0.9113(3) 0.49821(16) 0.0442(9) Uani 0.50 1 d P . . O41 O -0.002(3) 1.0137(17) 0.4828(9) 0.104(8) Uani 0.50 1 d P . . O42 O 0.1144(11) 0.8722(11) 0.5333(5) 0.074(4) Uani 0.50 1 d P . . O43 O 0.0552(10) 0.8517(9) 0.4491(4) 0.053(3) Uani 0.50 1 d P . . O44 O -0.0775(12) 0.9056(13) 0.5256(6) 0.085(5) Uani 0.50 1 d P . . N100 N 0.5613(10) 0.9372(8) 0.2573(6) 0.119(4) Uani 1 1 d . . . C100 C 0.5259(8) 0.8824(8) 0.2489(4) 0.062(3) Uani 1 1 d . . . C101 C 0.4828(11) 0.8093(9) 0.2378(5) 0.089(4) Uani 1 1 d . . . H10A H 0.5192 0.7484 0.2609 0.134 Uiso 1 1 calc R . . H10B H 0.5024 0.7897 0.1992 0.134 Uiso 1 1 calc R . . H10C H 0.3974 0.8398 0.2457 0.134 Uiso 1 1 calc R . . Cl50 Cl 0.6142(5) 0.7818(4) 0.40269(19) 0.0411(11) Uani 0.50 1 d P E 1 O51 O 0.603(2) 0.719(2) 0.3585(12) 0.092(10) Uani 0.50 1 d P E 1 O52 O 0.5112(13) 0.8732(12) 0.4138(6) 0.071(4) Uani 0.50 1 d P E 1 O53 O 0.6377(19) 0.7148(16) 0.4494(8) 0.096(6) Uani 0.50 1 d P E 1 O54 O 0.7110(14) 0.7989(14) 0.3877(7) 0.096(5) Uani 0.50 1 d P E 1 Cl5A Cl 0.5594(5) 0.7609(4) 0.4036(2) 0.0553(13) Uani 0.50 1 d P F 2 O5A O 0.587(4) 0.718(3) 0.3583(10) 0.20(2) Uani 0.50 1 d P F 2 O5B O 0.4414(15) 0.8319(13) 0.4048(10) 0.125(7) Uani 0.50 1 d P F 2 O5C O 0.568(2) 0.6999(17) 0.4502(8) 0.111(8) Uani 0.50 1 d P F 2 O5D O 0.611(3) 0.829(3) 0.4066(13) 0.157(14) Uani 0.50 1 d PU F 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0274(4) 0.0358(5) 0.0249(4) -0.0045(3) -0.0111(3) -0.0133(4) Cu2 0.0261(4) 0.0279(4) 0.0208(4) -0.0001(3) -0.0097(3) -0.0125(3) Cu3 0.0354(5) 0.0414(5) 0.0261(5) -0.0006(4) -0.0098(4) -0.0204(4) Cu4 0.0392(5) 0.0265(4) 0.0268(4) -0.0029(3) -0.0104(4) -0.0164(4) Cu5 0.0326(5) 0.0431(5) 0.0255(5) -0.0080(4) -0.0110(4) -0.0064(4) Cu6 0.0253(4) 0.0269(4) 0.0227(4) -0.0020(3) -0.0078(3) -0.0105(3) S1 0.0272(9) 0.0345(9) 0.0285(9) -0.0080(7) -0.0051(7) -0.0085(7) S2 0.0238(8) 0.0241(8) 0.0266(8) -0.0013(6) -0.0053(6) -0.0102(7) N1 0.034(3) 0.045(4) 0.037(4) -0.002(3) -0.010(3) -0.019(3) N2 0.048(4) 0.030(3) 0.036(3) 0.001(3) -0.008(3) -0.018(3) N11 0.028(3) 0.033(3) 0.030(3) -0.003(2) -0.009(2) -0.016(2) N12 0.025(3) 0.029(3) 0.030(3) 0.000(2) -0.009(2) -0.013(2) N13 0.033(3) 0.035(3) 0.048(4) -0.001(3) -0.010(3) -0.021(3) N14 0.032(3) 0.046(4) 0.030(3) -0.013(3) -0.013(3) -0.016(3) N15 0.029(3) 0.046(4) 0.023(3) -0.002(3) -0.014(2) -0.012(3) N16 0.028(3) 0.028(3) 0.022(3) 0.000(2) -0.011(2) -0.012(2) N17 0.025(3) 0.026(3) 0.020(3) 0.000(2) -0.006(2) -0.013(2) N18 0.031(3) 0.030(3) 0.027(3) 0.000(2) -0.009(2) -0.012(2) N19 0.023(3) 0.030(3) 0.025(3) 0.000(2) -0.009(2) -0.013(2) N20 0.025(3) 0.029(3) 0.020(3) -0.003(2) -0.005(2) -0.009(2) N31 0.028(3) 0.034(3) 0.033(3) -0.002(2) -0.008(2) -0.018(3) N32 0.034(3) 0.028(3) 0.030(3) -0.004(2) -0.002(2) -0.015(3) N33 0.036(3) 0.031(3) 0.052(4) -0.009(3) -0.003(3) -0.012(3) N34 0.040(4) 0.054(4) 0.040(4) 0.005(3) -0.020(3) -0.026(3) N35 0.046(4) 0.055(4) 0.031(3) 0.003(3) -0.009(3) -0.029(3) N36 0.030(3) 0.035(3) 0.030(3) 0.000(2) -0.007(2) -0.017(3) N37 0.030(3) 0.034(3) 0.032(3) -0.003(2) -0.009(2) -0.018(3) N38 0.035(3) 0.049(4) 0.044(4) 0.000(3) -0.004(3) -0.024(3) N39 0.045(4) 0.027(3) 0.041(4) -0.005(3) -0.020(3) -0.015(3) N40 0.055(4) 0.033(3) 0.032(3) -0.008(3) -0.007(3) -0.025(3) N51 0.027(3) 0.033(3) 0.023(3) 0.000(2) -0.005(2) -0.008(2) N52 0.024(3) 0.026(3) 0.025(3) 0.001(2) -0.004(2) -0.009(2) N53 0.033(3) 0.034(3) 0.039(4) 0.005(3) -0.002(3) -0.011(3) N54 0.027(3) 0.064(5) 0.032(4) -0.002(3) -0.009(3) -0.003(3) N56 0.034(3) 0.034(3) 0.025(3) -0.009(2) -0.015(2) -0.007(3) N57 0.027(3) 0.031(3) 0.025(3) -0.004(2) -0.009(2) -0.012(2) N58 0.040(4) 0.037(4) 0.041(4) -0.016(3) -0.017(3) -0.003(3) N59 0.025(3) 0.036(3) 0.026(3) 0.000(2) -0.008(2) -0.013(2) N60 0.029(3) 0.029(3) 0.036(3) -0.004(3) -0.008(2) -0.009(3) C1 0.025(4) 0.041(4) 0.023(4) -0.003(3) -0.007(3) -0.011(3) C2 0.022(3) 0.039(4) 0.019(3) -0.003(3) -0.008(3) -0.011(3) C13 0.030(4) 0.029(4) 0.035(4) -0.002(3) -0.013(3) -0.012(3) C15 0.031(4) 0.034(4) 0.034(4) -0.004(3) -0.011(3) -0.019(3) C16 0.036(4) 0.045(5) 0.047(5) -0.010(4) -0.010(3) -0.025(4) C17 0.057(6) 0.063(6) 0.065(6) -0.003(4) -0.021(4) -0.044(5) C18 0.045(5) 0.053(5) 0.045(5) -0.015(4) -0.019(4) -0.020(4) C19 0.053(5) 0.067(6) 0.033(4) -0.014(4) -0.023(4) -0.019(4) C20 0.045(5) 0.060(5) 0.034(4) -0.005(4) -0.024(4) -0.017(4) C21 0.045(5) 0.049(5) 0.033(4) 0.009(4) -0.018(3) -0.014(4) C22 0.025(3) 0.038(4) 0.018(3) 0.002(3) -0.004(3) -0.008(3) C23 0.028(3) 0.027(3) 0.023(3) 0.000(3) -0.003(3) -0.015(3) C25 0.029(4) 0.030(4) 0.022(3) 0.003(3) -0.007(3) -0.017(3) C26 0.029(4) 0.028(4) 0.028(4) -0.001(3) -0.011(3) -0.015(3) C27 0.050(5) 0.033(4) 0.028(4) -0.009(3) -0.003(3) -0.015(3) C28 0.033(4) 0.038(4) 0.022(3) -0.006(3) -0.008(3) -0.013(3) C29 0.030(4) 0.041(4) 0.018(3) -0.001(3) -0.011(3) -0.014(3) C30 0.034(4) 0.044(4) 0.023(4) 0.000(3) -0.009(3) -0.016(3) C31 0.053(5) 0.048(5) 0.037(4) 0.010(4) -0.011(4) -0.028(4) C32 0.026(4) 0.034(4) 0.027(4) 0.004(3) -0.007(3) -0.008(3) C33 0.041(4) 0.031(4) 0.039(4) -0.002(3) -0.008(3) -0.018(3) C35 0.029(4) 0.035(4) 0.050(5) 0.006(3) -0.013(3) -0.019(3) C36 0.039(4) 0.044(5) 0.052(5) 0.006(4) -0.020(4) -0.023(4) C37 0.043(5) 0.056(6) 0.073(6) 0.007(5) -0.029(4) -0.017(4) C38 0.069(6) 0.064(6) 0.047(5) 0.010(4) -0.028(5) -0.028(5) C39 0.074(6) 0.079(7) 0.036(5) 0.009(4) -0.029(4) -0.042(5) C40 0.086(7) 0.089(7) 0.024(4) 0.009(4) -0.015(4) -0.047(6) C41 0.065(6) 0.084(7) 0.053(6) 0.016(5) -0.005(5) -0.047(6) C42 0.046(5) 0.056(5) 0.037(4) 0.003(4) -0.005(4) -0.028(4) C43 0.039(4) 0.042(4) 0.033(4) 0.006(3) -0.006(3) -0.023(3) C45 0.034(4) 0.039(4) 0.043(5) 0.002(3) -0.009(3) -0.018(3) C46 0.040(4) 0.036(4) 0.056(5) -0.004(4) -0.018(4) -0.022(4) C47 0.049(5) 0.066(6) 0.078(7) -0.011(5) -0.021(5) -0.037(5) C48 0.056(5) 0.043(5) 0.040(5) -0.010(4) -0.028(4) -0.014(4) C49 0.083(7) 0.045(5) 0.033(4) -0.002(4) -0.027(4) -0.027(5) C50 0.076(6) 0.053(5) 0.026(4) -0.012(3) -0.005(4) -0.038(5) C51 0.059(6) 0.049(5) 0.072(6) -0.031(5) 0.004(5) -0.023(4) C52 0.054(5) 0.031(4) 0.044(5) -0.011(3) -0.001(4) -0.018(4) C53 0.030(4) 0.026(4) 0.035(4) -0.001(3) -0.001(3) -0.011(3) C55 0.026(4) 0.037(4) 0.028(4) 0.007(3) -0.003(3) -0.001(3) C56 0.035(4) 0.055(5) 0.029(4) 0.017(4) 0.000(3) 0.005(4) C57 0.064(6) 0.069(6) 0.047(5) 0.022(5) 0.008(4) -0.011(5) C58 0.075(7) 0.088(8) 0.021(4) -0.002(5) -0.014(4) 0.020(6) C59 0.050(13) 0.10(2) 0.034(11) -0.042(12) -0.008(10) -0.004(13) C60 0.059(16) 0.097(19) 0.026(11) -0.021(11) 0.000(11) -0.041(15) N55 0.034(14) 0.049(11) 0.033(10) -0.014(8) 0.001(8) -0.027(9) C61 0.049(11) 0.056(12) 0.068(13) -0.030(10) -0.031(10) 0.000(9) C62 0.036(16) 0.038(13) 0.053(16) -0.014(11) -0.012(10) -0.020(10) C58A 0.075(7) 0.088(8) 0.021(4) -0.002(5) -0.014(4) 0.020(6) C59A 0.055(13) 0.065(15) 0.021(9) -0.011(9) -0.007(10) -0.029(12) C60A 0.037(10) 0.051(10) 0.033(10) -0.012(7) -0.015(8) -0.020(9) N55A 0.015(10) 0.035(10) 0.021(8) -0.012(7) 0.000(6) -0.010(7) C61A 0.046(10) 0.033(8) 0.043(10) -0.012(7) -0.012(8) -0.017(8) C62A 0.032(14) 0.030(10) 0.030(10) -0.005(7) 0.001(8) -0.017(8) C63 0.046(5) 0.035(4) 0.048(5) -0.012(4) -0.026(4) -0.002(4) C65 0.028(4) 0.029(4) 0.036(4) -0.004(3) -0.010(3) -0.012(3) C66 0.028(4) 0.031(4) 0.036(4) -0.002(3) -0.010(3) -0.011(3) C67 0.050(5) 0.029(4) 0.054(5) 0.001(3) -0.025(4) -0.018(3) C68 0.033(4) 0.040(4) 0.026(4) -0.002(3) -0.007(3) -0.015(3) C69 0.036(4) 0.053(5) 0.033(4) 0.001(3) -0.019(3) -0.023(4) C70 0.039(4) 0.052(5) 0.035(4) 0.002(3) -0.017(3) -0.025(4) C71 0.036(4) 0.043(5) 0.058(5) 0.004(4) -0.009(4) -0.024(4) C72 0.027(4) 0.030(4) 0.039(4) -0.005(3) -0.003(3) -0.006(3) Cl10 0.0421(12) 0.0600(14) 0.0657(15) -0.0001(11) -0.0244(10) -0.0243(10) O11 0.035(3) 0.064(4) 0.074(4) -0.004(3) -0.012(3) -0.024(3) O12 0.057(10) 0.070(11) 0.22(2) 0.052(14) -0.036(13) -0.042(9) O13 0.100(19) 0.32(5) 0.038(10) 0.04(2) -0.041(10) -0.11(3) O14 0.027(7) 0.084(13) 0.125(16) -0.071(12) -0.019(8) -0.003(8) O12A 0.130(17) 0.090(15) 0.23(3) -0.083(16) -0.030(19) -0.073(14) O13A 0.045(10) 0.103(15) 0.14(2) 0.051(15) -0.032(11) -0.014(10) O14A 0.070(9) 0.098(11) 0.063(9) 0.007(8) 0.001(6) -0.044(8) Cl20 0.0574(14) 0.0441(12) 0.0798(17) 0.0013(11) -0.0155(12) -0.0288(11) O21 0.099(6) 0.091(5) 0.111(6) -0.011(5) -0.024(5) -0.067(5) O22 0.132(8) 0.097(6) 0.140(8) 0.022(6) 0.004(6) -0.084(6) O23 0.093(7) 0.082(6) 0.171(9) -0.030(6) -0.019(6) -0.019(5) O24 0.079(5) 0.132(7) 0.100(6) -0.031(5) -0.006(5) -0.054(5) Cl30 0.031(2) 0.045(3) 0.039(4) 0.002(2) -0.013(2) -0.015(2) O31 0.092(11) 0.091(11) 0.092(11) -0.014(9) -0.043(9) -0.046(9) O32 0.060(8) 0.057(8) 0.081(10) -0.001(7) -0.009(7) -0.024(7) O33 0.029(6) 0.070(9) 0.086(10) 0.008(7) -0.026(6) -0.016(6) O34 0.055(15) 0.108(19) 0.050(16) 0.020(12) 0.014(11) -0.031(12) N200 0.037(9) 0.054(10) 0.057(11) -0.010(8) -0.014(7) -0.014(7) C200 0.05(2) 0.036(15) 0.14(5) 0.012(19) -0.07(3) -0.015(13) C201 0.18(6) 0.20(6) 0.13(5) -0.04(4) -0.07(4) -0.12(5) Cl40 0.037(2) 0.053(3) 0.042(2) -0.0157(18) -0.0050(16) -0.0169(18) O41 0.134(14) 0.044(12) 0.13(2) -0.015(13) 0.041(19) -0.039(11) O42 0.050(8) 0.111(11) 0.059(8) -0.020(8) -0.022(6) -0.028(8) O43 0.054(7) 0.068(8) 0.037(6) -0.028(6) -0.003(5) -0.022(6) O44 0.058(9) 0.137(13) 0.079(10) -0.056(9) 0.030(7) -0.059(9) N100 0.109(9) 0.067(7) 0.204(13) 0.037(7) -0.029(8) -0.059(7) C100 0.038(5) 0.055(6) 0.085(7) 0.020(5) -0.004(5) -0.016(4) C101 0.088(9) 0.089(8) 0.108(10) -0.003(7) -0.028(7) -0.050(7) Cl50 0.037(3) 0.045(3) 0.041(2) -0.002(2) -0.012(2) -0.015(2) O51 0.064(13) 0.093(17) 0.11(2) -0.053(15) -0.006(12) -0.023(12) O52 0.038(8) 0.082(11) 0.072(9) -0.031(8) 0.000(7) -0.005(8) O53 0.120(17) 0.109(15) 0.067(11) 0.028(9) -0.053(11) -0.052(12) O54 0.058(10) 0.117(14) 0.111(14) -0.002(10) 0.006(9) -0.039(10) Cl5A 0.046(3) 0.058(3) 0.049(3) -0.008(2) -0.011(2) -0.009(3) O5A 0.22(4) 0.26(4) 0.010(11) -0.001(16) -0.005(15) -0.01(3) O5B 0.061(11) 0.081(12) 0.22(2) 0.010(13) 0.015(12) -0.025(10) O5C 0.16(2) 0.118(15) 0.073(12) 0.025(10) -0.064(14) -0.073(16) O5D 0.19(3) 0.20(3) 0.19(2) -0.02(2) -0.03(2) -0.18(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 N16 1.953(5) . ? Cu1 N11 1.958(5) . ? Cu1 N14 1.998(6) . ? Cu1 N15 2.013(5) . ? Cu1 S1 2.570(2) . ? Cu2 N12 1.951(5) . ? Cu2 N17 1.969(5) . ? Cu2 N19 1.995(5) . ? Cu2 N20 1.999(5) . ? Cu2 S2 2.6296(19) . ? Cu3 N36 1.966(5) . ? Cu3 N31 1.970(6) . ? Cu3 N35 2.005(6) . ? Cu3 N34 2.012(6) . ? Cu3 N1 2.139(6) . ? Cu4 N32 1.968(6) . ? Cu4 N37 1.969(6) . ? Cu4 N39 2.006(6) . ? Cu4 N40 2.017(6) . ? Cu4 N2 2.080(6) . ? Cu5 N56 1.944(6) . ? Cu5 N55 1.96(2) . ? Cu5 N51 1.970(6) . ? Cu5 N54 1.985(7) . ? Cu5 N55A 2.07(2) . ? Cu5 S1 2.589(2) . ? Cu6 N57 1.949(5) . ? Cu6 N52 1.952(5) . ? Cu6 N59 1.997(5) . ? Cu6 N60 2.000(6) . ? Cu6 S2 2.5146(18) . ? S1 C1 1.658(8) . ? S2 C2 1.666(7) . ? N1 C1 1.155(9) . ? N2 C2 1.157(8) . ? N11 N12 1.339(7) . ? N11 C15 1.346(8) . ? N12 C13 1.346(9) . ? N13 C13 1.343(8) . ? N13 C15 1.348(9) . ? N14 C16 1.276(9) . ? N14 C18 1.463(9) . ? N15 C22 1.283(9) . ? N15 C20 1.488(8) . ? N16 C23 1.335(8) . ? N16 N17 1.337(7) . ? N17 C25 1.337(8) . ? N18 C25 1.337(8) . ? N18 C23 1.346(8) . ? N19 C26 1.280(8) . ? N19 C28 1.479(8) . ? N20 C32 1.273(8) . ? N20 C30 1.475(8) . ? N31 C35 1.346(9) . ? N31 N32 1.353(7) . ? N32 C33 1.340(9) . ? N33 C33 1.352(9) . ? N33 C35 1.367(9) . ? N34 C36 1.289(10) . ? N34 C38 1.456(10) . ? N35 C42 1.261(9) . ? N35 C40 1.475(9) . ? N36 C43 1.327(9) . ? N36 N37 1.348(7) . ? N37 C45 1.335(9) . ? N38 C45 1.329(9) . ? N38 C43 1.359(9) . ? N39 C46 1.273(10) . ? N39 C48 1.480(9) . ? N40 C52 1.278(10) . ? N40 C50 1.478(9) . ? N51 N52 1.327(7) . ? N51 C55 1.332(9) . ? N52 C53 1.354(8) . ? N53 C53 1.336(9) . ? N53 C55 1.337(9) . ? N54 C56 1.289(11) . ? N54 C58 1.477(11) . ? N56 C63 1.326(9) . ? N56 N57 1.351(7) . ? N57 C65 1.333(8) . ? N58 C63 1.356(9) . ? N58 C65 1.358(8) . ? N59 C66 1.296(8) . ? N59 C68 1.469(8) . ? N60 C72 1.290(9) . ? N60 C70 1.481(8) . ? C13 C32 1.485(9) . ? C15 C16 1.478(9) . ? C16 C17 1.494(10) . ? C18 C19 1.483(12) . ? C19 C20 1.524(11) . ? C21 C22 1.500(9) . ? C22 C23 1.482(9) . ? C25 C26 1.480(9) . ? C26 C27 1.492(9) . ? C28 C29 1.503(9) . ? C29 C30 1.534(9) . ? C31 C32 1.488(10) . ? C33 C52 1.456(10) . ? C35 C36 1.442(10) . ? C36 C37 1.505(11) . ? C38 C39 1.492(13) . ? C39 C40 1.520(13) . ? C41 C42 1.498(11) . ? C42 C43 1.495(10) . ? C45 C46 1.479(10) . ? C46 C47 1.502(10) . ? C48 C49 1.485(12) . ? C49 C50 1.523(12) . ? C51 C52 1.509(11) . ? C53 C72 1.470(10) . ? C55 C56 1.488(10) . ? C56 C57 1.493(12) . ? C58 C59 1.30(3) . ? C59 C60 1.46(3) . ? C60 N55 1.46(3) . ? N55 C62 1.26(4) . ? C61 C62 1.50(3) . ? C62 C63 1.58(3) . ? C59A C60A 1.59(3) . ? C60A N55A 1.48(3) . ? N55A C62A 1.30(4) . ? C61A C62A 1.47(3) . ? C62A C63 1.44(3) . ? C65 C66 1.460(9) . ? C66 C67 1.505(9) . ? C68 C69 1.510(10) . ? C69 C70 1.513(10) . ? C71 C72 1.495(10) . ? Cl10 O14A 1.30(2) . ? Cl10 O13 1.32(2) . ? Cl10 O12A 1.367(15) . ? Cl10 O11 1.417(6) . ? Cl10 O13A 1.49(2) . ? Cl10 O12 1.521(16) . ? Cl10 O14 1.530(18) . ? Cl20 O22 1.351(7) . ? Cl20 O23 1.396(9) . ? Cl20 O21 1.409(7) . ? Cl20 O24 1.504(8) . ? Cl30 O33 1.414(13) . ? Cl30 O32 1.426(17) . ? Cl30 O31 1.431(16) . ? Cl30 O34 1.46(3) . ? N200 C200 1.19(7) . ? C200 C201 1.47(8) . ? Cl40 O41 1.11(3) 2_576 ? Cl40 O44 1.406(13) . ? Cl40 O42 1.416(12) . ? Cl40 O41 1.42(2) . ? Cl40 O43 1.437(10) . ? Cl40 Cl40 2.384(9) 2_576 ? O41 O41 0.91(3) 2_576 ? O41 Cl40 1.11(3) 2_576 ? O41 O42 1.71(3) 2_576 ? O42 O41 1.71(3) 2_576 ? N100 C100 1.102(13) . ? C100 C101 1.431(14) . ? Cl50 O54 1.371(19) . ? Cl50 O52 1.414(14) . ? Cl50 O53 1.434(18) . ? Cl50 O51 1.50(2) . ? Cl5A O5A 1.25(3) . ? Cl5A O5C 1.40(2) . ? Cl5A O5B 1.400(17) . ? Cl5A O5D 1.407(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N16 Cu1 N11 93.2(2) . . ? N16 Cu1 N14 153.4(2) . . ? N11 Cu1 N14 80.8(2) . . ? N16 Cu1 N15 80.0(2) . . ? N11 Cu1 N15 153.4(2) . . ? N14 Cu1 N15 93.8(2) . . ? N16 Cu1 S1 100.14(17) . . ? N11 Cu1 S1 109.37(17) . . ? N14 Cu1 S1 106.31(18) . . ? N15 Cu1 S1 97.16(17) . . ? N12 Cu2 N17 92.9(2) . . ? N12 Cu2 N19 155.0(2) . . ? N17 Cu2 N19 80.1(2) . . ? N12 Cu2 N20 80.9(2) . . ? N17 Cu2 N20 154.2(2) . . ? N19 Cu2 N20 94.9(2) . . ? N12 Cu2 S2 102.86(16) . . ? N17 Cu2 S2 107.47(15) . . ? N19 Cu2 S2 102.16(15) . . ? N20 Cu2 S2 98.31(15) . . ? N36 Cu3 N31 92.8(2) . . ? N36 Cu3 N35 80.4(2) . . ? N31 Cu3 N35 150.6(2) . . ? N36 Cu3 N34 150.0(2) . . ? N31 Cu3 N34 80.3(3) . . ? N35 Cu3 N34 91.4(3) . . ? N36 Cu3 N1 107.9(2) . . ? N31 Cu3 N1 106.0(2) . . ? N35 Cu3 N1 103.4(2) . . ? N34 Cu3 N1 102.1(2) . . ? N32 Cu4 N37 92.3(2) . . ? N32 Cu4 N39 148.5(2) . . ? N37 Cu4 N39 79.9(2) . . ? N32 Cu4 N40 80.2(2) . . ? N37 Cu4 N40 150.5(2) . . ? N39 Cu4 N40 91.6(2) . . ? N32 Cu4 N2 106.1(2) . . ? N37 Cu4 N2 103.5(2) . . ? N39 Cu4 N2 105.4(2) . . ? N40 Cu4 N2 106.0(2) . . ? N56 Cu5 N55 84.6(8) . . ? N56 Cu5 N51 93.4(2) . . ? N55 Cu5 N51 148.3(6) . . ? N56 Cu5 N54 156.0(2) . . ? N55 Cu5 N54 88.2(7) . . ? N51 Cu5 N54 80.9(3) . . ? N56 Cu5 N55A 76.7(6) . . ? N55 Cu5 N55A 15.9(5) . . ? N51 Cu5 N55A 159.9(6) . . ? N54 Cu5 N55A 101.0(6) . . ? N56 Cu5 S1 108.25(18) . . ? N55 Cu5 S1 109.1(7) . . ? N51 Cu5 S1 101.55(16) . . ? N54 Cu5 S1 95.77(18) . . ? N55A Cu5 S1 98.2(5) . . ? N57 Cu6 N52 92.5(2) . . ? N57 Cu6 N59 80.5(2) . . ? N52 Cu6 N59 153.9(2) . . ? N57 Cu6 N60 152.1(2) . . ? N52 Cu6 N60 80.5(2) . . ? N59 Cu6 N60 93.9(2) . . ? N57 Cu6 S2 106.72(17) . . ? N52 Cu6 S2 105.38(16) . . ? N59 Cu6 S2 100.69(16) . . ? N60 Cu6 S2 101.18(17) . . ? C1 S1 Cu1 95.8(2) . . ? C1 S1 Cu5 93.8(2) . . ? Cu1 S1 Cu5 136.11(8) . . ? C2 S2 Cu6 96.7(2) . . ? C2 S2 Cu2 94.1(2) . . ? Cu6 S2 Cu2 138.20(7) . . ? C1 N1 Cu3 171.2(6) . . ? C2 N2 Cu4 160.0(5) . . ? N12 N11 C15 106.0(5) . . ? N12 N11 Cu1 133.1(4) . . ? C15 N11 Cu1 112.9(4) . . ? N11 N12 C13 105.7(5) . . ? N11 N12 Cu2 133.9(4) . . ? C13 N12 Cu2 112.6(4) . . ? C13 N13 C15 100.9(6) . . ? C16 N14 C18 122.1(6) . . ? C16 N14 Cu1 115.7(5) . . ? C18 N14 Cu1 122.2(5) . . ? C22 N15 C20 122.1(6) . . ? C22 N15 Cu1 116.2(4) . . ? C20 N15 Cu1 121.6(5) . . ? C23 N16 N17 106.0(5) . . ? C23 N16 Cu1 114.5(4) . . ? N17 N16 Cu1 133.5(4) . . ? N16 N17 C25 105.9(5) . . ? N16 N17 Cu2 133.2(4) . . ? C25 N17 Cu2 113.6(4) . . ? C25 N18 C23 101.2(5) . . ? C26 N19 C28 121.5(5) . . ? C26 N19 Cu2 116.2(4) . . ? C28 N19 Cu2 121.6(4) . . ? C32 N20 C30 121.1(6) . . ? C32 N20 Cu2 115.4(4) . . ? C30 N20 Cu2 122.5(4) . . ? C35 N31 N32 106.0(5) . . ? C35 N31 Cu3 112.3(5) . . ? N32 N31 Cu3 133.3(4) . . ? C33 N32 N31 106.0(5) . . ? C33 N32 Cu4 112.2(4) . . ? N31 N32 Cu4 133.6(4) . . ? C33 N33 C35 100.6(6) . . ? C36 N34 C38 121.5(7) . . ? C36 N34 Cu3 114.8(5) . . ? C38 N34 Cu3 123.2(6) . . ? C42 N35 C40 120.7(7) . . ? C42 N35 Cu3 116.1(5) . . ? C40 N35 Cu3 122.9(5) . . ? C43 N36 N37 105.2(5) . . ? C43 N36 Cu3 112.8(5) . . ? N37 N36 Cu3 133.2(4) . . ? C45 N37 N36 105.4(6) . . ? C45 N37 Cu4 113.9(5) . . ? N36 N37 Cu4 133.9(4) . . ? C45 N38 C43 99.5(6) . . ? C46 N39 C48 122.1(7) . . ? C46 N39 Cu4 115.8(5) . . ? C48 N39 Cu4 121.7(5) . . ? C52 N40 C50 122.6(7) . . ? C52 N40 Cu4 114.4(5) . . ? C50 N40 Cu4 122.5(5) . . ? N52 N51 C55 106.6(6) . . ? N52 N51 Cu5 132.1(4) . . ? C55 N51 Cu5 112.8(5) . . ? N51 N52 C53 105.5(5) . . ? N51 N52 Cu6 134.9(4) . . ? C53 N52 Cu6 113.6(4) . . ? C53 N53 C55 101.5(6) . . ? C56 N54 C58 123.3(9) . . ? C56 N54 Cu5 115.6(5) . . ? C58 N54 Cu5 121.1(7) . . ? C63 N56 N57 106.0(5) . . ? C63 N56 Cu5 113.2(5) . . ? N57 N56 Cu5 133.2(4) . . ? C65 N57 N56 106.0(5) . . ? C65 N57 Cu6 113.0(4) . . ? N56 N57 Cu6 133.6(4) . . ? C63 N58 C65 100.3(6) . . ? C66 N59 C68 124.2(6) . . ? C66 N59 Cu6 115.6(4) . . ? C68 N59 Cu6 120.2(4) . . ? C72 N60 C70 122.3(6) . . ? C72 N60 Cu6 116.3(5) . . ? C70 N60 Cu6 121.4(5) . . ? N1 C1 S1 179.6(8) . . ? N2 C2 S2 179.3(6) . . ? N13 C13 N12 113.8(6) . . ? N13 C13 C32 130.6(6) . . ? N12 C13 C32 114.9(6) . . ? N11 C15 N13 113.5(6) . . ? N11 C15 C16 114.5(6) . . ? N13 C15 C16 131.1(6) . . ? N14 C16 C15 113.8(6) . . ? N14 C16 C17 127.5(7) . . ? C15 C16 C17 118.7(7) . . ? N14 C18 C19 113.3(6) . . ? C18 C19 C20 117.6(7) . . ? N15 C20 C19 111.6(6) . . ? N15 C22 C23 112.9(6) . . ? N15 C22 C21 125.4(6) . . ? C23 C22 C21 121.7(6) . . ? N16 C23 N18 113.3(5) . . ? N16 C23 C22 114.8(5) . . ? N18 C23 C22 130.9(6) . . ? N18 C25 N17 113.6(5) . . ? N18 C25 C26 130.7(6) . . ? N17 C25 C26 114.6(5) . . ? N19 C26 C25 113.5(6) . . ? N19 C26 C27 125.8(6) . . ? C25 C26 C27 120.4(6) . . ? N19 C28 C29 112.2(5) . . ? C28 C29 C30 115.5(5) . . ? N20 C30 C29 111.0(5) . . ? N20 C32 C13 113.5(6) . . ? N20 C32 C31 125.6(6) . . ? C13 C32 C31 120.8(6) . . ? N32 C33 N33 114.1(6) . . ? N32 C33 C52 115.6(6) . . ? N33 C33 C52 129.6(7) . . ? N31 C35 N33 113.3(6) . . ? N31 C35 C36 116.0(7) . . ? N33 C35 C36 129.8(7) . . ? N34 C36 C35 114.3(7) . . ? N34 C36 C37 124.9(7) . . ? C35 C36 C37 120.8(8) . . ? N34 C38 C39 111.5(7) . . ? C38 C39 C40 115.6(8) . . ? N35 C40 C39 111.2(7) . . ? N35 C42 C43 113.2(7) . . ? N35 C42 C41 126.3(7) . . ? C43 C42 C41 120.3(7) . . ? N36 C43 N38 114.6(6) . . ? N36 C43 C42 115.1(6) . . ? N38 C43 C42 129.5(6) . . ? N38 C45 N37 115.2(6) . . ? N38 C45 C46 129.6(7) . . ? N37 C45 C46 114.4(7) . . ? N39 C46 C45 114.1(6) . . ? N39 C46 C47 126.2(7) . . ? C45 C46 C47 119.7(8) . . ? N39 C48 C49 111.2(6) . . ? C48 C49 C50 115.5(7) . . ? N40 C50 C49 110.3(6) . . ? N40 C52 C33 114.4(7) . . ? N40 C52 C51 125.7(7) . . ? C33 C52 C51 119.9(7) . . ? N53 C53 N52 113.0(6) . . ? N53 C53 C72 131.6(7) . . ? N52 C53 C72 114.8(6) . . ? N51 C55 N53 113.4(6) . . ? N51 C55 C56 114.5(7) . . ? N53 C55 C56 131.3(7) . . ? N54 C56 C55 113.5(7) . . ? N54 C56 C57 127.5(8) . . ? C55 C56 C57 118.8(9) . . ? C59 C58 N54 117.7(14) . . ? C58 C59 C60 116(2) . . ? N55 C60 C59 111.0(19) . . ? C62 N55 C60 121(2) . . ? C62 N55 Cu5 114.0(19) . . ? C60 N55 Cu5 125(2) . . ? N55 C62 C61 129(2) . . ? N55 C62 C63 115(2) . . ? C61 C62 C63 116(2) . . ? N55A C60A C59A 113.6(15) . . ? C62A N55A C60A 125.1(19) . . ? C62A N55A Cu5 117.9(17) . . ? C60A N55A Cu5 116.7(15) . . ? N55A C62A C63 107.7(18) . . ? N55A C62A C61A 127(2) . . ? C63 C62A C61A 125(2) . . ? N56 C63 N58 114.0(6) . . ? N56 C63 C62A 117.3(12) . . ? N58 C63 C62A 128.1(12) . . ? N56 C63 C62 112.4(11) . . ? N58 C63 C62 130.6(12) . . ? C62A C63 C62 23.2(8) . . ? N57 C65 N58 113.6(6) . . ? N57 C65 C66 115.9(6) . . ? N58 C65 C66 129.9(6) . . ? N59 C66 C65 112.6(6) . . ? N59 C66 C67 126.8(6) . . ? C65 C66 C67 120.6(6) . . ? N59 C68 C69 111.1(6) . . ? C68 C69 C70 117.6(6) . . ? N60 C70 C69 111.7(6) . . ? N60 C72 C53 113.1(6) . . ? N60 C72 C71 127.5(7) . . ? C53 C72 C71 119.4(6) . . ? O14A Cl10 O13 119.7(16) . . ? O14A Cl10 O12A 113.8(16) . . ? O13 Cl10 O12A 67.6(18) . . ? O14A Cl10 O11 116.4(10) . . ? O13 Cl10 O11 118.7(12) . . ? O12A Cl10 O11 109.7(10) . . ? O14A Cl10 O13A 110.1(15) . . ? O13 Cl10 O13A 37.6(17) . . ? O12A Cl10 O13A 104.6(17) . . ? O11 Cl10 O13A 100.9(10) . . ? O14A Cl10 O12 73.9(12) . . ? O13 Cl10 O12 111.5(18) . . ? O12A Cl10 O12 49.0(14) . . ? O11 Cl10 O12 105.7(7) . . ? O13A Cl10 O12 147.7(12) . . ? O14A Cl10 O14 23.8(12) . . ? O13 Cl10 O14 110.2(17) . . ? O12A Cl10 O14 133.3(13) . . ? O11 Cl10 O14 110.9(7) . . ? O13A Cl10 O14 89.6(14) . . ? O12 Cl10 O14 97.6(13) . . ? O22 Cl20 O23 116.7(6) . . ? O22 Cl20 O21 112.3(6) . . ? O23 Cl20 O21 116.3(5) . . ? O22 Cl20 O24 101.6(6) . . ? O23 Cl20 O24 103.5(6) . . ? O21 Cl20 O24 103.8(5) . . ? O33 Cl30 O32 109.0(9) . . ? O33 Cl30 O31 110.2(10) . . ? O32 Cl30 O31 107.9(9) . . ? O33 Cl30 O34 109.2(14) . . ? O32 Cl30 O34 108.6(14) . . ? O31 Cl30 O34 111.8(14) . . ? N200 C200 C201 173(5) . . ? O41 Cl40 O44 92.8(14) 2_576 . ? O41 Cl40 O42 84.1(17) 2_576 . ? O44 Cl40 O42 108.6(9) . . ? O41 Cl40 O41 40.0(18) 2_576 . ? O44 Cl40 O41 111.5(13) . . ? O42 Cl40 O41 109.8(15) . . ? O41 Cl40 O43 147.0(10) 2_576 . ? O44 Cl40 O43 109.4(8) . . ? O42 Cl40 O43 110.0(7) . . ? O41 Cl40 O43 107.5(11) . . ? O41 Cl40 Cl40 22.5(9) 2_576 2_576 ? O44 Cl40 Cl40 104.0(7) . 2_576 ? O42 Cl40 Cl40 98.8(7) . 2_576 ? O41 Cl40 Cl40 17.5(10) . 2_576 ? O43 Cl40 Cl40 124.9(6) . 2_576 ? O41 O41 Cl40 88(4) 2_576 2_576 ? O41 O41 Cl40 52(2) 2_576 . ? Cl40 O41 Cl40 140.0(18) 2_576 . ? O41 O41 O42 121(4) 2_576 2_576 ? Cl40 O41 O42 55.5(11) 2_576 2_576 ? Cl40 O41 O42 141(2) . 2_576 ? Cl40 O42 O41 40.4(11) . 2_576 ? N100 C100 C101 178.6(13) . . ? O54 Cl50 O52 113.0(12) . . ? O54 Cl50 O53 108.8(12) . . ? O52 Cl50 O53 110.5(12) . . ? O54 Cl50 O51 107.3(14) . . ? O52 Cl50 O51 113.2(14) . . ? O53 Cl50 O51 103.6(15) . . ? O5A Cl5A O5C 118(2) . . ? O5A Cl5A O5B 108(2) . . ? O5C Cl5A O5B 105.4(15) . . ? O5A Cl5A O5D 110(3) . . ? O5C Cl5A O5D 114.1(16) . . ? O5B Cl5A O5D 99.5(19) . . ? 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 N16 Cu1 S1 C1 23.7(3) . . . . ? N11 Cu1 S1 C1 120.7(3) . . . . ? N14 Cu1 S1 C1 -153.5(3) . . . . ? N15 Cu1 S1 C1 -57.4(3) . . . . ? N16 Cu1 S1 Cu5 -78.00(18) . . . . ? N11 Cu1 S1 Cu5 19.0(2) . . . . ? N14 Cu1 S1 Cu5 104.8(2) . . . . ? N15 Cu1 S1 Cu5 -159.10(19) . . . . ? N56 Cu5 S1 C1 -124.8(3) . . . . ? N55 Cu5 S1 C1 144.8(8) . . . . ? N51 Cu5 S1 C1 -27.3(3) . . . . ? N54 Cu5 S1 C1 54.6(3) . . . . ? N55A Cu5 S1 C1 156.6(6) . . . . ? N56 Cu5 S1 Cu1 -22.3(2) . . . . ? N55 Cu5 S1 Cu1 -112.7(7) . . . . ? N51 Cu5 S1 Cu1 75.2(2) . . . . ? N54 Cu5 S1 Cu1 157.1(2) . . . . ? N55A Cu5 S1 Cu1 -100.9(6) . . . . ? N57 Cu6 S2 C2 140.5(3) . . . . ? N52 Cu6 S2 C2 43.0(3) . . . . ? N59 Cu6 S2 C2 -136.3(3) . . . . ? N60 Cu6 S2 C2 -40.0(3) . . . . ? N57 Cu6 S2 Cu2 36.77(19) . . . . ? N52 Cu6 S2 Cu2 -60.74(19) . . . . ? N59 Cu6 S2 Cu2 119.97(18) . . . . ? N60 Cu6 S2 Cu2 -143.81(19) . . . . ? N12 Cu2 S2 C2 -143.7(3) . . . . ? N17 Cu2 S2 C2 -46.5(3) . . . . ? N19 Cu2 S2 C2 36.8(3) . . . . ? N20 Cu2 S2 C2 133.8(3) . . . . ? N12 Cu2 S2 Cu6 -38.99(19) . . . . ? N17 Cu2 S2 Cu6 58.22(19) . . . . ? N19 Cu2 S2 Cu6 141.57(18) . . . . ? N20 Cu2 S2 Cu6 -121.51(18) . . . . ? N36 Cu3 N1 C1 -43(4) . . . . ? N31 Cu3 N1 C1 55(4) . . . . ? N35 Cu3 N1 C1 -127(4) . . . . ? N34 Cu3 N1 C1 138(4) . . . . ? N32 Cu4 N2 C2 -41.4(18) . . . . ? N37 Cu4 N2 C2 55.0(17) . . . . ? N39 Cu4 N2 C2 138.1(17) . . . . ? N40 Cu4 N2 C2 -125.6(17) . . . . ? N16 Cu1 N11 N12 2.6(6) . . . . ? N14 Cu1 N11 N12 156.5(6) . . . . ? N15 Cu1 N11 N12 76.6(8) . . . . ? S1 Cu1 N11 N12 -99.3(6) . . . . ? N16 Cu1 N11 C15 -141.0(5) . . . . ? N14 Cu1 N11 C15 13.0(5) . . . . ? N15 Cu1 N11 C15 -67.0(7) . . . . ? S1 Cu1 N11 C15 117.1(4) . . . . ? C15 N11 N12 C13 1.2(7) . . . . ? Cu1 N11 N12 C13 -144.1(5) . . . . ? C15 N11 N12 Cu2 146.8(5) . . . . ? Cu1 N11 N12 Cu2 1.5(9) . . . . ? N17 Cu2 N12 N11 -3.9(6) . . . . ? N19 Cu2 N12 N11 -76.5(8) . . . . ? N20 Cu2 N12 N11 -158.7(6) . . . . ? S2 Cu2 N12 N11 104.8(6) . . . . ? N17 Cu2 N12 C13 140.1(4) . . . . ? N19 Cu2 N12 C13 67.4(7) . . . . ? N20 Cu2 N12 C13 -14.8(4) . . . . ? S2 Cu2 N12 C13 -111.3(4) . . . . ? N16 Cu1 N14 C16 72.5(8) . . . . ? N11 Cu1 N14 C16 -6.0(5) . . . . ? N15 Cu1 N14 C16 147.8(6) . . . . ? S1 Cu1 N14 C16 -113.6(5) . . . . ? N16 Cu1 N14 C18 -106.4(7) . . . . ? N11 Cu1 N14 C18 175.1(6) . . . . ? N15 Cu1 N14 C18 -31.1(6) . . . . ? S1 Cu1 N14 C18 67.4(6) . . . . ? N16 Cu1 N15 C22 4.1(5) . . . . ? N11 Cu1 N15 C22 -72.9(8) . . . . ? N14 Cu1 N15 C22 -149.9(5) . . . . ? S1 Cu1 N15 C22 103.2(5) . . . . ? N16 Cu1 N15 C20 -179.3(6) . . . . ? N11 Cu1 N15 C20 103.7(7) . . . . ? N14 Cu1 N15 C20 26.8(6) . . . . ? S1 Cu1 N15 C20 -80.2(6) . . . . ? N11 Cu1 N16 C23 144.0(5) . . . . ? N14 Cu1 N16 C23 68.3(7) . . . . ? N15 Cu1 N16 C23 -10.1(5) . . . . ? S1 Cu1 N16 C23 -105.7(4) . . . . ? N11 Cu1 N16 N17 -4.4(6) . . . . ? N14 Cu1 N16 N17 -80.1(8) . . . . ? N15 Cu1 N16 N17 -158.5(6) . . . . ? S1 Cu1 N16 N17 105.9(6) . . . . ? C23 N16 N17 C25 -1.0(6) . . . . ? Cu1 N16 N17 C25 149.2(5) . . . . ? C23 N16 N17 Cu2 -148.0(5) . . . . ? Cu1 N16 N17 Cu2 2.2(9) . . . . ? N12 Cu2 N17 N16 2.1(6) . . . . ? N19 Cu2 N17 N16 157.9(6) . . . . ? N20 Cu2 N17 N16 77.0(8) . . . . ? S2 Cu2 N17 N16 -102.4(5) . . . . ? N12 Cu2 N17 C25 -143.1(4) . . . . ? N19 Cu2 N17 C25 12.7(4) . . . . ? N20 Cu2 N17 C25 -68.1(7) . . . . ? S2 Cu2 N17 C25 112.5(4) . . . . ? N12 Cu2 N19 C26 66.0(7) . . . . ? N17 Cu2 N19 C26 -9.4(5) . . . . ? N20 Cu2 N19 C26 145.1(5) . . . . ? S2 Cu2 N19 C26 -115.3(5) . . . . ? N12 Cu2 N19 C28 -104.4(6) . . . . ? N17 Cu2 N19 C28 -179.7(5) . . . . ? N20 Cu2 N19 C28 -25.2(5) . . . . ? S2 Cu2 N19 C28 74.4(5) . . . . ? N12 Cu2 N20 C32 11.7(5) . . . . ? N17 Cu2 N20 C32 -65.9(7) . . . . ? N19 Cu2 N20 C32 -143.4(5) . . . . ? S2 Cu2 N20 C32 113.5(5) . . . . ? N12 Cu2 N20 C30 -179.3(5) . . . . ? N17 Cu2 N20 C30 103.1(6) . . . . ? N19 Cu2 N20 C30 25.6(5) . . . . ? S2 Cu2 N20 C30 -77.5(5) . . . . ? N36 Cu3 N31 C35 -136.5(5) . . . . ? N35 Cu3 N31 C35 -61.2(7) . . . . ? N34 Cu3 N31 C35 14.0(5) . . . . ? N1 Cu3 N31 C35 114.0(5) . . . . ? N36 Cu3 N31 N32 6.1(6) . . . . ? N35 Cu3 N31 N32 81.4(8) . . . . ? N34 Cu3 N31 N32 156.6(6) . . . . ? N1 Cu3 N31 N32 -103.4(6) . . . . ? C35 N31 N32 C33 0.3(7) . . . . ? Cu3 N31 N32 C33 -143.9(5) . . . . ? C35 N31 N32 Cu4 144.8(5) . . . . ? Cu3 N31 N32 Cu4 0.6(9) . . . . ? N37 Cu4 N32 C33 135.2(5) . . . . ? N39 Cu4 N32 C33 60.9(7) . . . . ? N40 Cu4 N32 C33 -16.1(5) . . . . ? N2 Cu4 N32 C33 -120.0(5) . . . . ? N37 Cu4 N32 N31 -7.8(6) . . . . ? N39 Cu4 N32 N31 -82.1(7) . . . . ? N40 Cu4 N32 N31 -159.0(6) . . . . ? N2 Cu4 N32 N31 97.0(6) . . . . ? N36 Cu3 N34 C36 68.5(8) . . . . ? N31 Cu3 N34 C36 -10.1(6) . . . . ? N35 Cu3 N34 C36 141.5(6) . . . . ? N1 Cu3 N34 C36 -114.5(6) . . . . ? N36 Cu3 N34 C38 -103.9(7) . . . . ? N31 Cu3 N34 C38 177.5(7) . . . . ? N35 Cu3 N34 C38 -30.9(6) . . . . ? N1 Cu3 N34 C38 73.1(7) . . . . ? N36 Cu3 N35 C42 8.6(6) . . . . ? N31 Cu3 N35 C42 -69.9(8) . . . . ? N34 Cu3 N35 C42 -142.4(6) . . . . ? N1 Cu3 N35 C42 114.8(6) . . . . ? N36 Cu3 N35 C40 -177.8(7) . . . . ? N31 Cu3 N35 C40 103.7(7) . . . . ? N34 Cu3 N35 C40 31.3(7) . . . . ? N1 Cu3 N35 C40 -71.5(7) . . . . ? N31 Cu3 N36 C43 137.3(5) . . . . ? N35 Cu3 N36 C43 -13.9(5) . . . . ? N34 Cu3 N36 C43 62.0(7) . . . . ? N1 Cu3 N36 C43 -115.0(5) . . . . ? N31 Cu3 N36 N37 -4.4(6) . . . . ? N35 Cu3 N36 N37 -155.5(6) . . . . ? N34 Cu3 N36 N37 -79.6(8) . . . . ? N1 Cu3 N36 N37 103.4(6) . . . . ? C43 N36 N37 C45 0.3(7) . . . . ? Cu3 N36 N37 C45 143.9(5) . . . . ? C43 N36 N37 Cu4 -147.8(5) . . . . ? Cu3 N36 N37 Cu4 -4.2(9) . . . . ? N32 Cu4 N37 C45 -136.6(5) . . . . ? N39 Cu4 N37 C45 12.7(5) . . . . ? N40 Cu4 N37 C45 -62.5(7) . . . . ? N2 Cu4 N37 C45 116.3(5) . . . . ? N32 Cu4 N37 N36 9.5(6) . . . . ? N39 Cu4 N37 N36 158.8(6) . . . . ? N40 Cu4 N37 N36 83.6(8) . . . . ? N2 Cu4 N37 N36 -97.6(6) . . . . ? N32 Cu4 N39 C46 68.2(7) . . . . ? N37 Cu4 N39 C46 -9.6(5) . . . . ? N40 Cu4 N39 C46 142.0(5) . . . . ? N2 Cu4 N39 C46 -110.9(5) . . . . ? N32 Cu4 N39 C48 -104.3(6) . . . . ? N37 Cu4 N39 C48 177.9(5) . . . . ? N40 Cu4 N39 C48 -30.5(5) . . . . ? N2 Cu4 N39 C48 76.6(5) . . . . ? N32 Cu4 N40 C52 13.2(5) . . . . ? N37 Cu4 N40 C52 -64.0(8) . . . . ? N39 Cu4 N40 C52 -136.2(6) . . . . ? N2 Cu4 N40 C52 117.2(6) . . . . ? N32 Cu4 N40 C50 -175.5(6) . . . . ? N37 Cu4 N40 C50 107.3(7) . . . . ? N39 Cu4 N40 C50 35.1(6) . . . . ? N2 Cu4 N40 C50 -71.5(6) . . . . ? N56 Cu5 N51 N52 0.8(6) . . . . ? N55 Cu5 N51 N52 85.9(16) . . . . ? N54 Cu5 N51 N52 157.3(6) . . . . ? N55A Cu5 N51 N52 60.1(18) . . . . ? S1 Cu5 N51 N52 -108.6(5) . . . . ? N56 Cu5 N51 C55 -142.1(5) . . . . ? N55 Cu5 N51 C55 -57.0(16) . . . . ? N54 Cu5 N51 C55 14.4(5) . . . . ? N55A Cu5 N51 C55 -82.8(17) . . . . ? S1 Cu5 N51 C55 108.5(4) . . . . ? C55 N51 N52 C53 -0.3(7) . . . . ? Cu5 N51 N52 C53 -144.8(5) . . . . ? C55 N51 N52 Cu6 149.2(5) . . . . ? Cu5 N51 N52 Cu6 4.7(9) . . . . ? N57 Cu6 N52 N51 -6.3(6) . . . . ? N59 Cu6 N52 N51 -79.7(8) . . . . ? N60 Cu6 N52 N51 -159.1(6) . . . . ? S2 Cu6 N52 N51 101.9(6) . . . . ? N57 Cu6 N52 C53 141.4(5) . . . . ? N59 Cu6 N52 C53 67.9(7) . . . . ? N60 Cu6 N52 C53 -11.4(4) . . . . ? S2 Cu6 N52 C53 -110.5(4) . . . . ? N56 Cu5 N54 C56 69.7(9) . . . . ? N55 Cu5 N54 C56 142.1(9) . . . . ? N51 Cu5 N54 C56 -8.0(5) . . . . ? N55A Cu5 N54 C56 151.7(8) . . . . ? S1 Cu5 N54 C56 -108.8(5) . . . . ? N56 Cu5 N54 C58 -107.1(8) . . . . ? N55 Cu5 N54 C58 -34.7(9) . . . . ? N51 Cu5 N54 C58 175.2(6) . . . . ? N55A Cu5 N54 C58 -25.1(8) . . . . ? S1 Cu5 N54 C58 74.4(6) . . . . ? N55 Cu5 N56 C63 -7.0(8) . . . . ? N51 Cu5 N56 C63 141.3(5) . . . . ? N54 Cu5 N56 C63 66.2(9) . . . . ? N55A Cu5 N56 C63 -21.0(7) . . . . ? S1 Cu5 N56 C63 -115.4(5) . . . . ? N55 Cu5 N56 N57 -151.7(8) . . . . ? N51 Cu5 N56 N57 -3.4(6) . . . . ? N54 Cu5 N56 N57 -78.5(9) . . . . ? N55A Cu5 N56 N57 -165.7(8) . . . . ? S1 Cu5 N56 N57 100.0(6) . . . . ? C63 N56 N57 C65 0.8(8) . . . . ? Cu5 N56 N57 C65 147.3(5) . . . . ? C63 N56 N57 Cu6 -145.7(6) . . . . ? Cu5 N56 N57 Cu6 0.8(9) . . . . ? N52 Cu6 N57 C65 -141.3(5) . . . . ? N59 Cu6 N57 C65 13.4(5) . . . . ? N60 Cu6 N57 C65 -66.9(7) . . . . ? S2 Cu6 N57 C65 111.9(5) . . . . ? N52 Cu6 N57 N56 3.5(6) . . . . ? N59 Cu6 N57 N56 158.2(6) . . . . ? N60 Cu6 N57 N56 77.8(8) . . . . ? S2 Cu6 N57 N56 -103.4(6) . . . . ? N57 Cu6 N59 C66 -7.8(5) . . . . ? N52 Cu6 N59 C66 68.3(7) . . . . ? N60 Cu6 N59 C66 144.6(5) . . . . ? S2 Cu6 N59 C66 -113.2(5) . . . . ? N57 Cu6 N59 C68 172.6(5) . . . . ? N52 Cu6 N59 C68 -111.2(6) . . . . ? N60 Cu6 N59 C68 -34.9(5) . . . . ? S2 Cu6 N59 C68 67.2(5) . . . . ? N57 Cu6 N60 C72 -71.3(7) . . . . ? N52 Cu6 N60 C72 6.0(5) . . . . ? N59 Cu6 N60 C72 -148.4(5) . . . . ? S2 Cu6 N60 C72 109.9(5) . . . . ? N57 Cu6 N60 C70 109.3(6) . . . . ? N52 Cu6 N60 C70 -173.5(5) . . . . ? N59 Cu6 N60 C70 32.2(5) . . . . ? S2 Cu6 N60 C70 -69.5(5) . . . . ? Cu3 N1 C1 S1 123(100) . . . . ? Cu1 S1 C1 N1 164(100) . . . . ? Cu5 S1 C1 N1 -59(100) . . . . ? Cu4 N2 C2 S2 160(53) . . . . ? Cu6 S2 C2 N2 124(54) . . . . ? Cu2 S2 C2 N2 -97(54) . . . . ? C15 N13 C13 N12 1.3(8) . . . . ? C15 N13 C13 C32 -168.4(7) . . . . ? N11 N12 C13 N13 -1.6(8) . . . . ? Cu2 N12 C13 N13 -155.5(5) . . . . ? N11 N12 C13 C32 169.8(5) . . . . ? Cu2 N12 C13 C32 15.9(7) . . . . ? N12 N11 C15 N13 -0.4(8) . . . . ? Cu1 N11 C15 N13 152.8(5) . . . . ? N12 N11 C15 C16 -170.8(6) . . . . ? Cu1 N11 C15 C16 -17.6(7) . . . . ? C13 N13 C15 N11 -0.5(8) . . . . ? C13 N13 C15 C16 167.8(7) . . . . ? C18 N14 C16 C15 177.2(6) . . . . ? Cu1 N14 C16 C15 -1.7(8) . . . . ? C18 N14 C16 C17 -0.5(12) . . . . ? Cu1 N14 C16 C17 -179.4(7) . . . . ? N11 C15 C16 N14 12.9(9) . . . . ? N13 C15 C16 N14 -155.4(7) . . . . ? N11 C15 C16 C17 -169.2(7) . . . . ? N13 C15 C16 C17 22.5(12) . . . . ? C16 N14 C18 C19 175.9(7) . . . . ? Cu1 N14 C18 C19 -5.2(9) . . . . ? N14 C18 C19 C20 62.8(9) . . . . ? C22 N15 C20 C19 -171.6(7) . . . . ? Cu1 N15 C20 C19 12.0(9) . . . . ? C18 C19 C20 N15 -66.3(9) . . . . ? C20 N15 C22 C23 -174.4(6) . . . . ? Cu1 N15 C22 C23 2.2(8) . . . . ? C20 N15 C22 C21 3.3(11) . . . . ? Cu1 N15 C22 C21 179.9(6) . . . . ? N17 N16 C23 N18 1.2(7) . . . . ? Cu1 N16 C23 N18 -155.4(4) . . . . ? N17 N16 C23 C22 171.0(5) . . . . ? Cu1 N16 C23 C22 14.3(7) . . . . ? C25 N18 C23 N16 -0.9(7) . . . . ? C25 N18 C23 C22 -168.5(7) . . . . ? N15 C22 C23 N16 -10.8(8) . . . . ? C21 C22 C23 N16 171.4(6) . . . . ? N15 C22 C23 N18 156.7(7) . . . . ? C21 C22 C23 N18 -21.2(11) . . . . ? C23 N18 C25 N17 0.2(7) . . . . ? C23 N18 C25 C26 167.1(7) . . . . ? N16 N17 C25 N18 0.5(7) . . . . ? Cu2 N17 C25 N18 154.9(4) . . . . ? N16 N17 C25 C26 -168.6(5) . . . . ? Cu2 N17 C25 C26 -14.2(7) . . . . ? C28 N19 C26 C25 174.6(5) . . . . ? Cu2 N19 C26 C25 4.3(7) . . . . ? C28 N19 C26 C27 1.0(10) . . . . ? Cu2 N19 C26 C27 -169.4(5) . . . . ? N18 C25 C26 N19 -160.2(7) . . . . ? N17 C25 C26 N19 6.6(8) . . . . ? N18 C25 C26 C27 13.9(11) . . . . ? N17 C25 C26 C27 -179.4(6) . . . . ? C26 N19 C28 C29 176.6(6) . . . . ? Cu2 N19 C28 C29 -13.5(7) . . . . ? N19 C28 C29 C30 68.7(8) . . . . ? C32 N20 C30 C29 -179.2(6) . . . . ? Cu2 N20 C30 C29 12.4(7) . . . . ? C28 C29 C30 N20 -67.8(7) . . . . ? C30 N20 C32 C13 -175.3(5) . . . . ? Cu2 N20 C32 C13 -6.2(7) . . . . ? C30 N20 C32 C31 0.6(10) . . . . ? Cu2 N20 C32 C31 169.8(6) . . . . ? N13 C13 C32 N20 163.1(7) . . . . ? N12 C13 C32 N20 -6.5(8) . . . . ? N13 C13 C32 C31 -13.0(11) . . . . ? N12 C13 C32 C31 177.4(6) . . . . ? N31 N32 C33 N33 -1.7(8) . . . . ? Cu4 N32 C33 N33 -154.7(5) . . . . ? N31 N32 C33 C52 170.1(6) . . . . ? Cu4 N32 C33 C52 17.1(8) . . . . ? C35 N33 C33 N32 2.2(8) . . . . ? C35 N33 C33 C52 -168.2(8) . . . . ? N32 N31 C35 N33 1.1(8) . . . . ? Cu3 N31 C35 N33 153.7(5) . . . . ? N32 N31 C35 C36 -168.9(6) . . . . ? Cu3 N31 C35 C36 -16.3(8) . . . . ? C33 N33 C35 N31 -2.0(8) . . . . ? C33 N33 C35 C36 166.3(7) . . . . ? C38 N34 C36 C35 176.7(7) . . . . ? Cu3 N34 C36 C35 4.2(9) . . . . ? C38 N34 C36 C37 -1.4(12) . . . . ? Cu3 N34 C36 C37 -173.9(6) . . . . ? N31 C35 C36 N34 8.1(10) . . . . ? N33 C35 C36 N34 -159.9(7) . . . . ? N31 C35 C36 C37 -173.7(7) . . . . ? N33 C35 C36 C37 18.2(12) . . . . ? C36 N34 C38 C39 179.0(8) . . . . ? Cu3 N34 C38 C39 -9.1(10) . . . . ? N34 C38 C39 C40 67.1(10) . . . . ? C42 N35 C40 C39 -179.3(8) . . . . ? Cu3 N35 C40 C39 7.3(11) . . . . ? C38 C39 C40 N35 -66.2(10) . . . . ? C40 N35 C42 C43 -175.6(7) . . . . ? Cu3 N35 C42 C43 -1.8(9) . . . . ? C40 N35 C42 C41 -1.0(13) . . . . ? Cu3 N35 C42 C41 172.9(7) . . . . ? N37 N36 C43 N38 -1.5(8) . . . . ? Cu3 N36 C43 N38 -153.6(5) . . . . ? N37 N36 C43 C42 169.1(6) . . . . ? Cu3 N36 C43 C42 17.1(8) . . . . ? C45 N38 C43 N36 2.0(8) . . . . ? C45 N38 C43 C42 -166.9(8) . . . . ? N35 C42 C43 N36 -10.2(10) . . . . ? C41 C42 C43 N36 174.7(7) . . . . ? N35 C42 C43 N38 158.7(8) . . . . ? C41 C42 C43 N38 -16.3(13) . . . . ? C43 N38 C45 N37 -1.8(8) . . . . ? C43 N38 C45 C46 166.8(8) . . . . ? N36 N37 C45 N38 1.1(8) . . . . ? Cu4 N37 C45 N38 156.5(5) . . . . ? N36 N37 C45 C46 -169.4(6) . . . . ? Cu4 N37 C45 C46 -14.0(8) . . . . ? C48 N39 C46 C45 177.2(6) . . . . ? Cu4 N39 C46 C45 4.7(8) . . . . ? C48 N39 C46 C47 -0.7(12) . . . . ? Cu4 N39 C46 C47 -173.2(6) . . . . ? N38 C45 C46 N39 -162.6(8) . . . . ? N37 C45 C46 N39 6.1(10) . . . . ? N38 C45 C46 C47 15.4(12) . . . . ? N37 C45 C46 C47 -175.8(7) . . . . ? C46 N39 C48 C49 176.0(7) . . . . ? Cu4 N39 C48 C49 -12.0(8) . . . . ? N39 C48 C49 C50 70.8(8) . . . . ? C52 N40 C50 C49 173.9(7) . . . . ? Cu4 N40 C50 C49 3.3(9) . . . . ? C48 C49 C50 N40 -65.6(9) . . . . ? C50 N40 C52 C33 -178.8(6) . . . . ? Cu4 N40 C52 C33 -7.5(9) . . . . ? C50 N40 C52 C51 -1.8(13) . . . . ? Cu4 N40 C52 C51 169.5(7) . . . . ? N32 C33 C52 N40 -6.4(10) . . . . ? N33 C33 C52 N40 163.9(8) . . . . ? N32 C33 C52 C51 176.4(7) . . . . ? N33 C33 C52 C51 -13.3(13) . . . . ? C55 N53 C53 N52 1.0(7) . . . . ? C55 N53 C53 C72 -169.7(7) . . . . ? N51 N52 C53 N53 -0.5(7) . . . . ? Cu6 N52 C53 N53 -157.3(5) . . . . ? N51 N52 C53 C72 171.9(5) . . . . ? Cu6 N52 C53 C72 15.0(7) . . . . ? N52 N51 C55 N53 1.0(8) . . . . ? Cu5 N51 C55 N53 153.1(5) . . . . ? N52 N51 C55 C56 -170.4(5) . . . . ? Cu5 N51 C55 C56 -18.2(7) . . . . ? C53 N53 C55 N51 -1.2(8) . . . . ? C53 N53 C55 C56 168.3(7) . . . . ? C58 N54 C56 C55 177.2(7) . . . . ? Cu5 N54 C56 C55 0.5(8) . . . . ? C58 N54 C56 C57 2.2(13) . . . . ? Cu5 N54 C56 C57 -174.5(6) . . . . ? N51 C55 C56 N54 11.9(9) . . . . ? N53 C55 C56 N54 -157.5(7) . . . . ? N51 C55 C56 C57 -172.6(7) . . . . ? N53 C55 C56 C57 18.0(12) . . . . ? C56 N54 C58 C59 -175.0(15) . . . . ? Cu5 N54 C58 C59 1.5(17) . . . . ? N54 C58 C59 C60 58(2) . . . . ? C58 C59 C60 N55 -67(3) . . . . ? C59 C60 N55 C62 -169(2) . . . . ? C59 C60 N55 Cu5 16(3) . . . . ? N56 Cu5 N55 C62 6.2(17) . . . . ? N51 Cu5 N55 C62 -81.3(18) . . . . ? N54 Cu5 N55 C62 -150.8(17) . . . . ? N55A Cu5 N55 C62 66(5) . . . . ? S1 Cu5 N55 C62 113.7(18) . . . . ? N56 Cu5 N55 C60 -178.3(19) . . . . ? N51 Cu5 N55 C60 94(3) . . . . ? N54 Cu5 N55 C60 24.6(18) . . . . ? N55A Cu5 N55 C60 -119(6) . . . . ? S1 Cu5 N55 C60 -70.9(18) . . . . ? C60 N55 C62 C61 -5(4) . . . . ? Cu5 N55 C62 C61 170.6(18) . . . . ? C60 N55 C62 C63 -179.9(17) . . . . ? Cu5 N55 C62 C63 -4(2) . . . . ? C59A C60A N55A C62A 132(2) . . . . ? C59A C60A N55A Cu5 -42(2) . . . . ? N56 Cu5 N55A C62A 9.3(14) . . . . ? N55 Cu5 N55A C62A -109(6) . . . . ? N51 Cu5 N55A C62A -53(2) . . . . ? N54 Cu5 N55A C62A -146.3(14) . . . . ? S1 Cu5 N55A C62A 116.2(15) . . . . ? N56 Cu5 N55A C60A -176.7(14) . . . . ? N55 Cu5 N55A C60A 65(5) . . . . ? N51 Cu5 N55A C60A 121.5(19) . . . . ? N54 Cu5 N55A C60A 27.8(14) . . . . ? S1 Cu5 N55A C60A -69.8(13) . . . . ? C60A N55A C62A C63 -169.9(16) . . . . ? Cu5 N55A C62A C63 4(2) . . . . ? C60A N55A C62A C61A 5(3) . . . . ? Cu5 N55A C62A C61A 178.2(16) . . . . ? N57 N56 C63 N58 -2.4(9) . . . . ? Cu5 N56 C63 N58 -156.4(6) . . . . ? N57 N56 C63 C62A -174.5(10) . . . . ? Cu5 N56 C63 C62A 31.4(12) . . . . ? N57 N56 C63 C62 160.4(10) . . . . ? Cu5 N56 C63 C62 6.4(12) . . . . ? C65 N58 C63 N56 2.8(9) . . . . ? C65 N58 C63 C62A 173.9(12) . . . . ? C65 N58 C63 C62 -156.1(13) . . . . ? N55A C62A C63 N56 -22.4(19) . . . . ? C61A C62A C63 N56 162.9(15) . . . . ? N55A C62A C63 N58 166.7(13) . . . . ? C61A C62A C63 N58 -8(3) . . . . ? N55A C62A C63 C62 61(4) . . . . ? C61A C62A C63 C62 -114(6) . . . . ? N55 C62 C63 N56 -1(2) . . . . ? C61 C62 C63 N56 -177.0(15) . . . . ? N55 C62 C63 N58 157.7(16) . . . . ? C61 C62 C63 N58 -18(2) . . . . ? N55 C62 C63 C62A -109(6) . . . . ? C61 C62 C63 C62A 76(5) . . . . ? N56 N57 C65 N58 1.0(8) . . . . ? Cu6 N57 C65 N58 155.2(5) . . . . ? N56 N57 C65 C66 -171.4(6) . . . . ? Cu6 N57 C65 C66 -17.2(8) . . . . ? C63 N58 C65 N57 -2.2(8) . . . . ? C63 N58 C65 C66 168.8(8) . . . . ? C68 N59 C66 C65 -179.5(6) . . . . ? Cu6 N59 C66 C65 0.9(8) . . . . ? C68 N59 C66 C67 1.5(11) . . . . ? Cu6 N59 C66 C67 -178.0(6) . . . . ? N57 C65 C66 N59 10.7(9) . . . . ? N58 C65 C66 N59 -160.2(7) . . . . ? N57 C65 C66 C67 -170.2(7) . . . . ? N58 C65 C66 C67 18.9(12) . . . . ? C66 N59 C68 C69 -126.0(7) . . . . ? Cu6 N59 C68 C69 53.5(7) . . . . ? N59 C68 C69 C70 -67.4(8) . . . . ? C72 N60 C70 C69 132.8(7) . . . . ? Cu6 N60 C70 C69 -47.9(8) . . . . ? C68 C69 C70 N60 64.1(8) . . . . ? C70 N60 C72 C53 179.8(6) . . . . ? Cu6 N60 C72 C53 0.4(7) . . . . ? C70 N60 C72 C71 -2.1(11) . . . . ? Cu6 N60 C72 C71 178.5(6) . . . . ? N53 C53 C72 N60 160.4(7) . . . . ? N52 C53 C72 N60 -10.2(9) . . . . ? N53 C53 C72 C71 -17.8(11) . . . . ? N52 C53 C72 C71 171.6(6) . . . . ? O44 Cl40 O41 O41 67(4) . . . 2_576 ? O42 Cl40 O41 O41 -53(4) . . . 2_576 ? O43 Cl40 O41 O41 -173(4) . . . 2_576 ? Cl40 Cl40 O41 O41 0.00(2) 2_576 . . 2_576 ? O41 Cl40 O41 Cl40 0.000(2) 2_576 . . 2_576 ? O44 Cl40 O41 Cl40 67(4) . . . 2_576 ? O42 Cl40 O41 Cl40 -53(4) . . . 2_576 ? O43 Cl40 O41 Cl40 -173(4) . . . 2_576 ? O41 Cl40 O41 O42 -94(4) 2_576 . . 2_576 ? O44 Cl40 O41 O42 -27(3) . . . 2_576 ? O42 Cl40 O41 O42 -148(2) . . . 2_576 ? O43 Cl40 O41 O42 93(3) . . . 2_576 ? Cl40 Cl40 O41 O42 -94(4) 2_576 . . 2_576 ? O44 Cl40 O42 O41 -91.0(12) . . . 2_576 ? O41 Cl40 O42 O41 31.2(19) . . . 2_576 ? O43 Cl40 O42 O41 149.3(12) . . . 2_576 ? Cl40 Cl40 O42 O41 17.1(10) 2_576 . . 2_576 ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.898 _refine_diff_density_max 1.159 _refine_diff_density_min -0.897 _refine_diff_density_rms 0.115 data_cutd _database_code_CSD 207833 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H50 Cl2 Cu4 N22 O9 S2' _chemical_formula_weight 1348.18 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' Cl Cl 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.203(3) _cell_length_b 15.172(4) _cell_length_c 15.802(4) _cell_angle_alpha 102.925(4) _cell_angle_beta 96.256(4) _cell_angle_gamma 112.461(4) _cell_volume 2572.9(12) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max .8 _exptl_crystal_size_mid .5 _exptl_crystal_size_min .4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 1.891 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28660 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.43 _reflns_number_total 10278 _reflns_number_gt 8911 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0605P)^2^+5.1108P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10278 _refine_ls_number_parameters 711 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 0.36024(3) 0.20395(3) 0.44498(2) 0.01715(10) Uani 1 1 d . . . Cu2 Cu 0.65051(3) 0.18543(3) 0.35364(2) 0.01771(10) Uani 1 1 d . . . N1 N 0.4572(2) 0.26594(19) 0.36578(17) 0.0178(5) Uani 1 1 d . . . N2 N 0.5568(2) 0.26224(19) 0.33986(16) 0.0175(5) Uani 1 1 d . . . N3 N 0.5694(2) 0.4160(2) 0.35093(18) 0.0207(5) Uani 1 1 d . . . N4 N 0.3264(2) 0.3255(2) 0.45876(18) 0.0208(6) Uani 1 1 d . . . N5 N 0.3314(2) 0.1882(2) 0.56387(18) 0.0215(6) Uani 1 1 d . . . N6 N 0.4598(2) 0.13230(19) 0.46460(17) 0.0177(5) Uani 1 1 d . . . N7 N 0.5524(2) 0.12234(19) 0.43212(17) 0.0175(5) Uani 1 1 d . . . N8 N 0.5767(2) 0.1132(2) 0.57139(17) 0.0205(5) Uani 1 1 d . . . N9 N 0.7699(2) 0.1493(2) 0.41642(18) 0.0207(5) Uani 1 1 d . . . N10 N 0.7768(2) 0.3010(2) 0.32781(17) 0.0189(5) Uani 1 1 d . . . C3 C 0.6218(3) 0.3519(2) 0.33262(19) 0.0185(6) Uani 1 1 d . . . C5 C 0.4675(3) 0.3580(2) 0.3727(2) 0.0191(6) Uani 1 1 d . . . C6 C 0.3793(3) 0.3854(2) 0.4157(2) 0.0205(6) Uani 1 1 d . . . C7 C 0.3619(3) 0.4750(3) 0.4065(2) 0.0278(7) Uani 1 1 d . . . H7A H 0.2882 0.4544 0.3614 0.033 Uiso 1 1 calc R . . H7B H 0.4322 0.5188 0.3885 0.033 Uiso 1 1 calc R . . H7C H 0.3539 0.5109 0.4637 0.033 Uiso 1 1 calc R . . C8 C 0.2358(3) 0.3362(3) 0.5097(2) 0.0268(7) Uani 1 1 d . . . H8A H 0.1537 0.2868 0.4762 0.032 Uiso 1 1 calc R . . H8B H 0.2381 0.4035 0.5173 0.032 Uiso 1 1 calc R . . C9 C 0.2599(4) 0.3211(3) 0.5999(3) 0.0327(8) Uani 1 1 d . . . H9A H 0.2059 0.3403 0.6349 0.039 Uiso 1 1 calc R . . H9B H 0.3444 0.3680 0.6303 0.039 Uiso 1 1 calc R . . C10 C 0.2435(3) 0.2178(3) 0.6037(3) 0.0301(8) Uani 1 1 d . . . H10A H 0.2532 0.2169 0.6665 0.036 Uiso 1 1 calc R . . H10B H 0.1603 0.1690 0.5719 0.036 Uiso 1 1 calc R . . C11 C 0.3946(3) 0.1332(3) 0.6900(2) 0.0311(8) Uani 1 1 d . . . H11A H 0.4092 0.1947 0.7351 0.037 Uiso 1 1 calc R . . H11B H 0.4585 0.1115 0.7045 0.037 Uiso 1 1 calc R . . H11C H 0.3155 0.0812 0.6886 0.037 Uiso 1 1 calc R . . C12 C 0.3953(3) 0.1515(2) 0.6016(2) 0.0207(6) Uani 1 1 d . . . C13 C 0.4770(3) 0.1277(2) 0.5477(2) 0.0188(6) Uani 1 1 d . . . C15 C 0.6206(3) 0.1123(2) 0.4974(2) 0.0182(6) Uani 1 1 d . . . C16 C 0.7412(3) 0.1200(2) 0.4838(2) 0.0211(6) Uani 1 1 d . . . C17 C 0.8200(3) 0.1002(3) 0.5479(2) 0.0303(8) Uani 1 1 d . . . H17A H 0.7701 0.0586 0.5808 0.036 Uiso 1 1 calc R . . H17B H 0.8792 0.1634 0.5896 0.036 Uiso 1 1 calc R . . H17C H 0.8629 0.0653 0.5157 0.036 Uiso 1 1 calc R . . C18 C 0.8919(3) 0.1718(3) 0.3985(2) 0.0279(7) Uani 1 1 d . . . H18A H 0.9057 0.1104 0.3879 0.033 Uiso 1 1 calc R . . H18B H 0.9531 0.2215 0.4516 0.033 Uiso 1 1 calc R . . C19 C 0.9096(3) 0.2112(3) 0.3196(2) 0.0276(7) Uani 1 1 d . . . H19A H 0.8482 0.1606 0.2671 0.033 Uiso 1 1 calc R . . H19B H 0.9905 0.2187 0.3083 0.033 Uiso 1 1 calc R . . C20 C 0.9011(3) 0.3100(3) 0.3264(2) 0.0247(7) Uani 1 1 d . . . H20A H 0.9572 0.3603 0.3814 0.030 Uiso 1 1 calc R . . H20B H 0.9268 0.3334 0.2752 0.030 Uiso 1 1 calc R . . C21 C 0.8231(3) 0.4658(3) 0.3031(2) 0.0283(7) Uani 1 1 d . . . H21A H 0.7714 0.4904 0.2729 0.034 Uiso 1 1 calc R . . H21B H 0.8783 0.4545 0.2658 0.034 Uiso 1 1 calc R . . H21C H 0.8704 0.5152 0.3601 0.034 Uiso 1 1 calc R . . C22 C 0.7460(3) 0.3709(2) 0.31901(19) 0.0197(6) Uani 1 1 d . . . Cu3 Cu -0.14715(3) 0.25763(3) 0.04791(2) 0.01892(10) Uani 1 1 d . . . Cu4 Cu 0.16052(3) 0.21541(3) 0.10383(2) 0.02089(10) Uani 1 1 d . . . N11 N -0.0922(2) 0.1554(2) -0.00471(17) 0.0184(5) Uani 1 1 d . . . N12 N 0.0046(2) 0.13664(19) 0.01565(17) 0.0183(5) Uani 1 1 d . . . N13 N -0.0588(2) 0.0805(2) -0.13150(18) 0.0229(6) Uani 1 1 d . . . N14 N -0.2464(2) 0.2080(2) -0.07633(18) 0.0250(6) Uani 1 1 d . . . N15 N -0.1459(3) 0.3941(2) 0.0641(2) 0.0265(6) Uani 1 1 d . . . N16 N 0.0147(2) 0.3419(2) 0.12770(17) 0.0197(5) Uani 1 1 d . . . N17 N 0.1163(2) 0.3284(2) 0.14210(17) 0.0210(6) Uani 1 1 d . . . N18 N 0.1721(3) 0.4896(2) 0.15137(19) 0.0276(6) Uani 1 1 d . . . N19 N 0.3263(2) 0.3303(2) 0.13629(18) 0.0269(6) Uani 1 1 d . . . N20 N 0.2116(3) 0.1286(2) 0.01599(19) 0.0246(6) Uani 1 1 d . . . C23 C 0.0222(3) 0.0932(2) -0.0611(2) 0.0200(6) Uani 1 1 d . . . C25 C -0.1271(3) 0.1217(2) -0.0925(2) 0.0207(6) Uani 1 1 d . . . C26 C -0.2220(3) 0.1469(3) -0.1320(2) 0.0251(7) Uani 1 1 d . . . C27 C -0.2753(4) 0.1042(4) -0.2291(2) 0.0398(10) Uani 1 1 d . . . H27A H -0.3594 0.0552 -0.2388 0.048 Uiso 1 1 calc R . . H27B H -0.2278 0.0716 -0.2577 0.048 Uiso 1 1 calc R . . H27C H -0.2740 0.1576 -0.2549 0.048 Uiso 1 1 calc R . . C28 C -0.3371(4) 0.2444(4) -0.1027(3) 0.0407(10) Uani 1 1 d . . . H28A H -0.4152 0.1868 -0.1332 0.049 Uiso 1 1 calc R . . H28B H -0.3097 0.2831 -0.1451 0.049 Uiso 1 1 calc R . . C29 C -0.3564(4) 0.3097(3) -0.0229(3) 0.0378(9) Uani 1 1 d . . . H29A H -0.4264 0.3233 -0.0432 0.045 Uiso 1 1 calc R . . H29B H -0.3793 0.2710 0.0201 0.045 Uiso 1 1 calc R . . C30 C -0.2512(4) 0.4080(3) 0.0258(3) 0.0367(9) Uani 1 1 d . . . H30A H -0.2279 0.4484 -0.0159 0.044 Uiso 1 1 calc R . . H30B H -0.2766 0.4448 0.0739 0.044 Uiso 1 1 calc R . . C31 C -0.0178(4) 0.5761(3) 0.1230(3) 0.0443(11) Uani 1 1 d . . . H31A H -0.0628 0.5860 0.0735 0.053 Uiso 1 1 calc R . . H31B H 0.0695 0.6145 0.1295 0.053 Uiso 1 1 calc R . . H31C H -0.0421 0.5986 0.1780 0.053 Uiso 1 1 calc R . . C32 C -0.0451(3) 0.4684(3) 0.1051(2) 0.0286(8) Uani 1 1 d . . . C33 C 0.0506(3) 0.4379(2) 0.1331(2) 0.0247(7) Uani 1 1 d . . . C35 C 0.2081(3) 0.4168(2) 0.1552(2) 0.0235(7) Uani 1 1 d . . . C36 C 0.3299(3) 0.4173(3) 0.1573(2) 0.0292(8) Uani 1 1 d . . . C37 C 0.4394(4) 0.5130(3) 0.1770(3) 0.0439(10) Uani 1 1 d . . . H37A H 0.4619 0.5237 0.1212 0.053 Uiso 1 1 calc R . . H37B H 0.5069 0.5105 0.2147 0.053 Uiso 1 1 calc R . . H37C H 0.4216 0.5679 0.2081 0.053 Uiso 1 1 calc R . . C38 C 0.4353(3) 0.3136(3) 0.1249(2) 0.0352(9) Uani 1 1 d . . . H38A H 0.5028 0.3585 0.1763 0.042 Uiso 1 1 calc R . . H38B H 0.4597 0.3299 0.0706 0.042 Uiso 1 1 calc R . . C39 C 0.4131(3) 0.2067(4) 0.1173(3) 0.0396(10) Uani 1 1 d . . . H39A H 0.3740 0.1873 0.1660 0.047 Uiso 1 1 calc R . . H39B H 0.4926 0.2029 0.1262 0.047 Uiso 1 1 calc R . . C40 C 0.3345(3) 0.1314(3) 0.0295(3) 0.0362(9) Uani 1 1 d . . . H40A H 0.3726 0.1496 -0.0200 0.043 Uiso 1 1 calc R . . H40B H 0.3289 0.0645 0.0292 0.043 Uiso 1 1 calc R . . C41 C 0.1562(4) 0.0210(3) -0.1384(3) 0.0329(8) Uani 1 1 d . . . H41A H 0.1481 -0.0431 -0.1300 0.039 Uiso 1 1 calc R . . H41B H 0.2378 0.0569 -0.1475 0.039 Uiso 1 1 calc R . . H41C H 0.0956 0.0094 -0.1906 0.039 Uiso 1 1 calc R . . C42 C 0.1367(3) 0.0811(2) -0.0585(2) 0.0236(7) Uani 1 1 d . . . S50 S 0.15155(7) 0.08315(6) 0.35760(5) 0.02266(17) Uani 1 1 d . . . C50 C 0.1568(3) 0.1319(2) 0.2746(2) 0.0195(6) Uani 1 1 d . . . N50 N 0.1584(3) 0.1655(2) 0.21618(19) 0.0275(6) Uani 1 1 d . . . S60 S 0.57661(8) 0.05521(6) 0.19826(6) 0.02651(18) Uani 1 1 d . . . C60 C 0.6622(3) 0.1303(2) 0.1480(2) 0.0216(7) Uani 1 1 d . . . N60 N 0.7243(3) 0.1846(2) 0.11486(19) 0.0254(6) Uani 1 1 d . . . Cl1 Cl -0.27949(8) 0.66554(7) 0.10348(6) 0.0329(2) Uani 1 1 d . . . O11 O -0.2549(3) 0.6332(3) 0.1782(2) 0.0475(7) Uani 1 1 d . . . O12 O -0.1763(3) 0.6973(3) 0.0646(2) 0.0507(8) Uani 1 1 d . . . O13 O -0.3723(3) 0.5797(3) 0.0373(2) 0.0693(11) Uani 1 1 d . . . O14 O -0.3251(5) 0.7383(3) 0.1240(3) 0.0811(13) Uani 1 1 d . . . Cl2 Cl 0.15661(9) 0.59320(7) 0.43194(6) 0.0372(2) Uani 1 1 d . . . O21 O 0.2809(3) 0.6646(2) 0.4594(2) 0.0442(7) Uani 1 1 d . . . O22 O 0.1314(3) 0.5354(2) 0.34128(18) 0.0432(7) Uani 1 1 d . . . O23 O 0.0789(3) 0.6433(3) 0.4449(3) 0.0584(9) Uani 1 1 d . . . O24 O 0.1378(3) 0.5263(2) 0.4855(2) 0.0505(8) Uani 1 1 d . . . O50 O -0.0270(5) 0.8199(5) 0.2812(3) 0.0493(17) Uani 0.50 1 d P . . H50A H -0.0888 0.7807 0.2411 0.059 Uiso 0.50 1 d P . . H50B H -0.0054 0.8558 0.2470 0.059 Uiso 0.50 1 d P . . O60 O 0.3446(5) 0.6821(3) 0.2837(3) 0.0360(13) Uani 0.50 1 d P . . H60A H 0.3299 0.6611 0.3285 0.043 Uiso 0.50 1 d P . . H60B H 0.2890 0.6958 0.2640 0.043 Uiso 0.50 1 d P . . 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 0.01592(18) 0.0207(2) 0.01672(18) 0.00622(14) 0.00438(14) 0.00895(15) Cu2 0.01511(18) 0.0209(2) 0.01983(19) 0.00799(15) 0.00485(14) 0.00894(15) N1 0.0159(12) 0.0209(13) 0.0178(12) 0.0056(10) 0.0032(10) 0.0090(11) N2 0.0157(12) 0.0216(13) 0.0156(12) 0.0045(10) 0.0039(10) 0.0085(11) N3 0.0205(13) 0.0221(14) 0.0220(13) 0.0090(11) 0.0064(11) 0.0095(11) N4 0.0175(13) 0.0224(14) 0.0229(13) 0.0048(11) 0.0042(11) 0.0098(11) N5 0.0190(13) 0.0255(14) 0.0197(13) 0.0060(11) 0.0061(11) 0.0089(11) N6 0.0172(13) 0.0198(13) 0.0163(12) 0.0051(10) 0.0038(10) 0.0078(11) N7 0.0145(12) 0.0178(13) 0.0202(13) 0.0064(10) 0.0029(10) 0.0064(10) N8 0.0199(13) 0.0206(13) 0.0210(13) 0.0082(11) 0.0021(11) 0.0078(11) N9 0.0168(13) 0.0243(14) 0.0232(13) 0.0066(11) 0.0042(11) 0.0109(11) N10 0.0180(13) 0.0226(13) 0.0163(12) 0.0040(10) 0.0058(10) 0.0090(11) C3 0.0208(15) 0.0214(16) 0.0145(14) 0.0055(12) 0.0035(12) 0.0099(13) C5 0.0192(15) 0.0225(16) 0.0166(14) 0.0055(12) 0.0019(12) 0.0102(13) C6 0.0187(15) 0.0223(16) 0.0208(15) 0.0047(12) 0.0018(12) 0.0105(13) C7 0.0312(19) 0.0300(18) 0.0329(19) 0.0153(15) 0.0131(15) 0.0189(15) C8 0.0222(17) 0.0284(18) 0.0352(19) 0.0095(15) 0.0129(14) 0.0145(14) C9 0.039(2) 0.0312(19) 0.0329(19) 0.0070(15) 0.0178(16) 0.0178(17) C10 0.0296(18) 0.040(2) 0.0327(19) 0.0163(16) 0.0176(15) 0.0213(17) C11 0.0327(19) 0.043(2) 0.0227(17) 0.0154(15) 0.0092(15) 0.0167(17) C12 0.0198(15) 0.0200(15) 0.0180(15) 0.0044(12) 0.0036(12) 0.0045(13) C13 0.0167(15) 0.0174(15) 0.0185(15) 0.0053(12) 0.0018(12) 0.0038(12) C15 0.0173(15) 0.0155(14) 0.0197(15) 0.0045(12) 0.0008(12) 0.0058(12) C16 0.0188(15) 0.0203(15) 0.0240(16) 0.0060(12) 0.0008(12) 0.0091(13) C17 0.0251(18) 0.042(2) 0.0332(19) 0.0197(16) 0.0059(15) 0.0190(16) C18 0.0187(16) 0.037(2) 0.0343(19) 0.0135(15) 0.0079(14) 0.0159(15) C19 0.0227(17) 0.0334(19) 0.0305(18) 0.0089(15) 0.0088(14) 0.0150(15) C20 0.0164(15) 0.0298(18) 0.0287(17) 0.0085(14) 0.0079(13) 0.0097(14) C21 0.0276(18) 0.0272(18) 0.0353(19) 0.0131(15) 0.0143(15) 0.0128(15) C22 0.0213(16) 0.0238(16) 0.0131(14) 0.0040(12) 0.0052(12) 0.0090(13) Cu3 0.01888(19) 0.0239(2) 0.01771(19) 0.00709(15) 0.00516(15) 0.01193(16) Cu4 0.01654(19) 0.0310(2) 0.01838(19) 0.00941(16) 0.00414(15) 0.01200(17) N11 0.0153(12) 0.0232(13) 0.0176(12) 0.0070(10) 0.0034(10) 0.0085(11) N12 0.0174(13) 0.0206(13) 0.0202(13) 0.0077(10) 0.0054(10) 0.0099(11) N13 0.0197(13) 0.0242(14) 0.0211(13) 0.0025(11) 0.0048(11) 0.0074(11) N14 0.0189(14) 0.0404(17) 0.0216(14) 0.0121(12) 0.0046(11) 0.0167(13) N15 0.0315(16) 0.0318(16) 0.0306(15) 0.0162(13) 0.0171(13) 0.0215(14) N16 0.0197(13) 0.0219(14) 0.0181(12) 0.0061(10) 0.0070(10) 0.0085(11) N17 0.0187(13) 0.0272(14) 0.0157(12) 0.0068(11) 0.0041(10) 0.0075(11) N18 0.0301(16) 0.0240(15) 0.0215(14) 0.0015(11) 0.0111(12) 0.0054(12) N19 0.0158(13) 0.0429(18) 0.0182(13) 0.0088(12) 0.0022(11) 0.0086(13) N20 0.0228(14) 0.0342(16) 0.0274(15) 0.0154(12) 0.0104(12) 0.0180(13) C23 0.0209(16) 0.0175(15) 0.0229(15) 0.0061(12) 0.0074(12) 0.0086(13) C25 0.0165(15) 0.0246(16) 0.0183(15) 0.0040(12) 0.0033(12) 0.0071(13) C26 0.0164(15) 0.039(2) 0.0201(16) 0.0092(14) 0.0033(12) 0.0112(14) C27 0.030(2) 0.066(3) 0.0203(18) 0.0051(17) 0.0002(15) 0.023(2) C28 0.036(2) 0.071(3) 0.032(2) 0.019(2) 0.0065(16) 0.038(2) C29 0.033(2) 0.061(3) 0.042(2) 0.028(2) 0.0166(17) 0.034(2) C30 0.039(2) 0.047(2) 0.047(2) 0.0262(19) 0.0204(18) 0.0326(19) C31 0.057(3) 0.027(2) 0.065(3) 0.0197(19) 0.036(2) 0.025(2) C32 0.037(2) 0.0271(18) 0.0327(18) 0.0130(15) 0.0229(16) 0.0188(16) C33 0.0305(18) 0.0234(17) 0.0217(16) 0.0063(13) 0.0142(14) 0.0108(14) C35 0.0228(16) 0.0248(17) 0.0147(14) 0.0041(12) 0.0036(12) 0.0025(13) C36 0.0189(16) 0.044(2) 0.0141(15) 0.0088(14) 0.0020(12) 0.0023(15) C37 0.026(2) 0.050(3) 0.034(2) 0.0077(18) 0.0033(16) -0.0036(18) C38 0.0142(16) 0.064(3) 0.0235(17) 0.0127(17) 0.0028(13) 0.0131(17) C39 0.0261(19) 0.077(3) 0.033(2) 0.027(2) 0.0094(16) 0.033(2) C40 0.0289(19) 0.057(3) 0.040(2) 0.0206(19) 0.0128(16) 0.0305(19) C41 0.033(2) 0.035(2) 0.035(2) 0.0072(16) 0.0135(16) 0.0201(17) C42 0.0252(17) 0.0237(17) 0.0298(17) 0.0124(14) 0.0119(14) 0.0142(14) S50 0.0212(4) 0.0248(4) 0.0198(4) 0.0098(3) 0.0010(3) 0.0063(3) C50 0.0172(15) 0.0233(16) 0.0188(15) 0.0052(12) 0.0034(12) 0.0099(13) N50 0.0263(15) 0.0375(17) 0.0248(15) 0.0136(13) 0.0045(12) 0.0176(13) S60 0.0311(4) 0.0216(4) 0.0237(4) 0.0066(3) 0.0097(3) 0.0067(3) C60 0.0209(16) 0.0267(17) 0.0193(15) 0.0052(13) 0.0036(13) 0.0133(14) N60 0.0229(14) 0.0347(16) 0.0223(14) 0.0115(12) 0.0082(12) 0.0134(13) Cl1 0.0309(5) 0.0358(5) 0.0368(5) 0.0162(4) 0.0103(4) 0.0151(4) O11 0.0498(18) 0.065(2) 0.0355(16) 0.0246(15) 0.0088(13) 0.0272(16) O12 0.0394(17) 0.066(2) 0.063(2) 0.0404(17) 0.0218(15) 0.0236(16) O13 0.056(2) 0.074(3) 0.0405(18) 0.0134(17) -0.0049(16) -0.0062(19) O14 0.115(4) 0.089(3) 0.092(3) 0.044(3) 0.051(3) 0.080(3) Cl2 0.0384(5) 0.0318(5) 0.0349(5) 0.0029(4) 0.0042(4) 0.0126(4) O21 0.0400(16) 0.0324(15) 0.0427(16) -0.0006(12) -0.0021(13) 0.0062(13) O22 0.0384(16) 0.0480(17) 0.0257(14) -0.0014(12) 0.0034(12) 0.0076(13) O23 0.053(2) 0.0496(19) 0.070(2) 0.0020(17) 0.0040(17) 0.0286(17) O24 0.061(2) 0.0469(18) 0.0452(18) 0.0199(14) 0.0164(15) 0.0195(16) O50 0.030(3) 0.064(4) 0.019(2) 0.016(3) -0.009(2) -0.015(3) O60 0.044(3) 0.015(2) 0.020(2) -0.0056(18) 0.020(2) -0.015(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 N6 1.957(3) . ? Cu1 N1 1.962(3) . ? Cu1 N5 1.998(3) . ? Cu1 N4 2.010(3) . ? Cu1 S50 2.5073(10) . ? Cu2 N2 1.947(3) . ? Cu2 N7 1.967(3) . ? Cu2 N9 1.986(3) . ? Cu2 N10 2.002(3) . ? Cu2 S60 2.5945(11) . ? N1 C5 1.332(4) . ? N1 N2 1.341(4) . ? N2 C3 1.326(4) . ? N3 C3 1.352(4) . ? N3 C5 1.354(4) . ? N4 C6 1.276(4) . ? N4 C8 1.473(4) . ? N5 C12 1.286(4) . ? N5 C10 1.462(4) . ? N6 C13 1.328(4) . ? N6 N7 1.336(4) . ? N7 C15 1.328(4) . ? N8 C15 1.338(4) . ? N8 C13 1.346(4) . ? N9 C16 1.275(4) . ? N9 C18 1.471(4) . ? N10 C22 1.283(4) . ? N10 C20 1.473(4) . ? C3 C22 1.480(4) . ? C5 C6 1.472(4) . ? C6 C7 1.489(4) . ? C8 C9 1.509(5) . ? C9 C10 1.518(5) . ? C11 C12 1.484(4) . ? C12 C13 1.473(4) . ? C15 C16 1.474(4) . ? C16 C17 1.479(4) . ? C18 C19 1.501(5) . ? C19 C20 1.522(5) . ? C21 C22 1.483(5) . ? Cu3 N11 1.971(3) . ? Cu3 N16 1.983(3) . ? Cu3 N14 2.003(3) . ? Cu3 N15 2.023(3) . ? Cu3 N60 2.089(3) 1_455 ? Cu4 N17 1.977(3) . ? Cu4 N12 1.982(3) . ? Cu4 N20 2.012(3) . ? Cu4 N19 2.018(3) . ? Cu4 N50 2.079(3) . ? N11 C25 1.325(4) . ? N11 N12 1.340(4) . ? N12 C23 1.326(4) . ? N13 C23 1.331(4) . ? N13 C25 1.342(4) . ? N14 C26 1.275(5) . ? N14 C28 1.474(4) . ? N15 C32 1.282(5) . ? N15 C30 1.469(4) . ? N16 C33 1.331(4) . ? N16 N17 1.335(4) . ? N17 C35 1.332(4) . ? N18 C35 1.346(5) . ? N18 C33 1.347(5) . ? N19 C36 1.269(5) . ? N19 C38 1.468(4) . ? N20 C42 1.274(5) . ? N20 C40 1.475(4) . ? C23 C42 1.473(4) . ? C25 C26 1.471(4) . ? C26 C27 1.488(5) . ? C28 C29 1.519(6) . ? C29 C30 1.507(6) . ? C31 C32 1.489(5) . ? C32 C33 1.471(5) . ? C35 C36 1.480(5) . ? C36 C37 1.489(5) . ? C38 C39 1.513(6) . ? C39 C40 1.521(6) . ? C41 C42 1.484(5) . ? S50 C50 1.639(3) . ? C50 N50 1.149(4) . ? S60 C60 1.641(4) . ? C60 N60 1.154(4) . ? N60 Cu3 2.089(3) 1_655 ? Cl1 O14 1.408(4) . ? Cl1 O11 1.420(3) . ? Cl1 O12 1.425(3) . ? Cl1 O13 1.441(3) . ? Cl2 O23 1.429(3) . ? Cl2 O24 1.431(3) . ? Cl2 O22 1.432(3) . ? Cl2 O21 1.433(3) . ? 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 N6 Cu1 N1 92.41(11) . . ? N6 Cu1 N5 80.93(11) . . ? N1 Cu1 N5 153.57(11) . . ? N6 Cu1 N4 154.66(11) . . ? N1 Cu1 N4 80.16(11) . . ? N5 Cu1 N4 94.96(11) . . ? N6 Cu1 S50 109.97(8) . . ? N1 Cu1 S50 109.69(8) . . ? N5 Cu1 S50 96.58(8) . . ? N4 Cu1 S50 95.32(8) . . ? N2 Cu2 N7 92.16(11) . . ? N2 Cu2 N9 156.10(11) . . ? N7 Cu2 N9 81.32(11) . . ? N2 Cu2 N10 80.75(11) . . ? N7 Cu2 N10 152.74(11) . . ? N9 Cu2 N10 94.54(11) . . ? N2 Cu2 S60 101.21(8) . . ? N7 Cu2 S60 106.90(8) . . ? N9 Cu2 S60 102.69(8) . . ? N10 Cu2 S60 100.31(8) . . ? C5 N1 N2 106.1(3) . . ? C5 N1 Cu1 112.9(2) . . ? N2 N1 Cu1 132.5(2) . . ? C3 N2 N1 106.1(2) . . ? C3 N2 Cu2 113.9(2) . . ? N1 N2 Cu2 135.1(2) . . ? C3 N3 C5 100.4(3) . . ? C6 N4 C8 123.8(3) . . ? C6 N4 Cu1 116.4(2) . . ? C8 N4 Cu1 119.5(2) . . ? C12 N5 C10 123.5(3) . . ? C12 N5 Cu1 115.5(2) . . ? C10 N5 Cu1 121.0(2) . . ? C13 N6 N7 106.3(2) . . ? C13 N6 Cu1 112.6(2) . . ? N7 N6 Cu1 134.5(2) . . ? C15 N7 N6 105.9(3) . . ? C15 N7 Cu2 111.3(2) . . ? N6 N7 Cu2 132.9(2) . . ? C15 N8 C13 101.1(3) . . ? C16 N9 C18 121.1(3) . . ? C16 N9 Cu2 114.8(2) . . ? C18 N9 Cu2 123.2(2) . . ? C22 N10 C20 121.5(3) . . ? C22 N10 Cu2 115.9(2) . . ? C20 N10 Cu2 122.4(2) . . ? N2 C3 N3 113.8(3) . . ? N2 C3 C22 115.8(3) . . ? N3 C3 C22 129.7(3) . . ? N1 C5 N3 113.4(3) . . ? N1 C5 C6 115.9(3) . . ? N3 C5 C6 129.9(3) . . ? N4 C6 C5 112.2(3) . . ? N4 C6 C7 127.9(3) . . ? C5 C6 C7 119.9(3) . . ? N4 C8 C9 111.2(3) . . ? C8 C9 C10 118.1(3) . . ? N5 C10 C9 111.8(3) . . ? N5 C12 C13 113.0(3) . . ? N5 C12 C11 127.2(3) . . ? C13 C12 C11 119.8(3) . . ? N6 C13 N8 113.1(3) . . ? N6 C13 C12 116.0(3) . . ? N8 C13 C12 130.4(3) . . ? N7 C15 N8 113.6(3) . . ? N7 C15 C16 115.8(3) . . ? N8 C15 C16 129.5(3) . . ? N9 C16 C15 113.8(3) . . ? N9 C16 C17 125.6(3) . . ? C15 C16 C17 120.5(3) . . ? N9 C18 C19 112.7(3) . . ? C18 C19 C20 116.7(3) . . ? N10 C20 C19 111.8(3) . . ? N10 C22 C3 112.7(3) . . ? N10 C22 C21 126.9(3) . . ? C3 C22 C21 120.2(3) . . ? N11 Cu3 N16 91.50(11) . . ? N11 Cu3 N14 80.13(11) . . ? N16 Cu3 N14 146.40(11) . . ? N11 Cu3 N15 150.78(11) . . ? N16 Cu3 N15 79.73(12) . . ? N14 Cu3 N15 91.83(12) . . ? N11 Cu3 N60 102.85(11) . 1_455 ? N16 Cu3 N60 112.43(11) . 1_455 ? N14 Cu3 N60 101.17(12) . 1_455 ? N15 Cu3 N60 106.27(12) . 1_455 ? N17 Cu4 N12 91.84(11) . . ? N17 Cu4 N20 152.40(11) . . ? N12 Cu4 N20 80.25(11) . . ? N17 Cu4 N19 79.84(12) . . ? N12 Cu4 N19 147.18(11) . . ? N20 Cu4 N19 92.54(12) . . ? N17 Cu4 N50 101.53(11) . . ? N12 Cu4 N50 111.04(11) . . ? N20 Cu4 N50 105.99(12) . . ? N19 Cu4 N50 101.74(12) . . ? C25 N11 N12 105.6(3) . . ? C25 N11 Cu3 113.1(2) . . ? N12 N11 Cu3 135.4(2) . . ? C23 N12 N11 106.0(2) . . ? C23 N12 Cu4 110.9(2) . . ? N11 N12 Cu4 132.1(2) . . ? C23 N13 C25 101.0(3) . . ? C26 N14 C28 122.2(3) . . ? C26 N14 Cu3 115.9(2) . . ? C28 N14 Cu3 121.9(2) . . ? C32 N15 C30 121.7(3) . . ? C32 N15 Cu3 116.0(2) . . ? C30 N15 Cu3 122.2(3) . . ? C33 N16 N17 105.8(3) . . ? C33 N16 Cu3 112.4(2) . . ? N17 N16 Cu3 132.7(2) . . ? C35 N17 N16 106.3(3) . . ? C35 N17 Cu4 113.3(2) . . ? N16 N17 Cu4 134.9(2) . . ? C35 N18 C33 100.6(3) . . ? C36 N19 C38 121.6(3) . . ? C36 N19 Cu4 116.8(2) . . ? C38 N19 Cu4 121.1(3) . . ? C42 N20 C40 120.9(3) . . ? C42 N20 Cu4 115.3(2) . . ? C40 N20 Cu4 123.0(2) . . ? N12 C23 N13 113.7(3) . . ? N12 C23 C42 116.6(3) . . ? N13 C23 C42 128.8(3) . . ? N11 C25 N13 113.6(3) . . ? N11 C25 C26 115.6(3) . . ? N13 C25 C26 130.2(3) . . ? N14 C26 C25 113.5(3) . . ? N14 C26 C27 127.1(3) . . ? C25 C26 C27 119.4(3) . . ? N14 C28 C29 111.7(3) . . ? C30 C29 C28 117.2(3) . . ? N15 C30 C29 111.6(3) . . ? N15 C32 C33 112.8(3) . . ? N15 C32 C31 127.2(4) . . ? C33 C32 C31 120.0(4) . . ? N16 C33 N18 113.8(3) . . ? N16 C33 C32 116.2(3) . . ? N18 C33 C32 129.2(3) . . ? N17 C35 N18 113.4(3) . . ? N17 C35 C36 116.2(3) . . ? N18 C35 C36 129.6(3) . . ? N19 C36 C35 112.8(3) . . ? N19 C36 C37 126.8(4) . . ? C35 C36 C37 120.3(4) . . ? N19 C38 C39 111.4(3) . . ? C38 C39 C40 115.1(3) . . ? N20 C40 C39 110.8(3) . . ? N20 C42 C23 112.9(3) . . ? N20 C42 C41 126.8(3) . . ? C23 C42 C41 120.2(3) . . ? C50 S50 Cu1 95.51(12) . . ? N50 C50 S50 178.9(3) . . ? C50 N50 Cu4 175.3(3) . . ? C60 S60 Cu2 95.58(12) . . ? N60 C60 S60 178.2(3) . . ? C60 N60 Cu3 166.5(3) . 1_655 ? O14 Cl1 O11 112.0(2) . . ? O14 Cl1 O12 112.3(2) . . ? O11 Cl1 O12 111.42(19) . . ? O14 Cl1 O13 107.7(3) . . ? O11 Cl1 O13 106.7(2) . . ? O12 Cl1 O13 106.3(2) . . ? O23 Cl2 O24 109.6(2) . . ? O23 Cl2 O22 111.6(2) . . ? O24 Cl2 O22 107.46(19) . . ? O23 Cl2 O21 109.6(2) . . ? O24 Cl2 O21 108.0(2) . . ? O22 Cl2 O21 110.51(18) . . ? 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 N6 Cu1 N1 C5 -145.4(2) . . . . ? N5 Cu1 N1 C5 -71.1(3) . . . . ? N4 Cu1 N1 C5 10.2(2) . . . . ? S50 Cu1 N1 C5 102.3(2) . . . . ? N6 Cu1 N1 N2 -2.6(3) . . . . ? N5 Cu1 N1 N2 71.7(4) . . . . ? N4 Cu1 N1 N2 153.0(3) . . . . ? S50 Cu1 N1 N2 -114.9(3) . . . . ? C5 N1 N2 C3 0.1(3) . . . . ? Cu1 N1 N2 C3 -144.5(2) . . . . ? C5 N1 N2 Cu2 152.6(2) . . . . ? Cu1 N1 N2 Cu2 8.0(4) . . . . ? N7 Cu2 N2 C3 145.6(2) . . . . ? N9 Cu2 N2 C3 72.3(4) . . . . ? N10 Cu2 N2 C3 -7.9(2) . . . . ? S60 Cu2 N2 C3 -106.7(2) . . . . ? N7 Cu2 N2 N1 -5.4(3) . . . . ? N9 Cu2 N2 N1 -78.7(4) . . . . ? N10 Cu2 N2 N1 -158.9(3) . . . . ? S60 Cu2 N2 N1 102.3(3) . . . . ? N6 Cu1 N4 C6 73.3(4) . . . . ? N1 Cu1 N4 C6 -1.2(2) . . . . ? N5 Cu1 N4 C6 152.6(2) . . . . ? S50 Cu1 N4 C6 -110.3(2) . . . . ? N6 Cu1 N4 C8 -112.2(3) . . . . ? N1 Cu1 N4 C8 173.2(2) . . . . ? N5 Cu1 N4 C8 -33.0(2) . . . . ? S50 Cu1 N4 C8 64.1(2) . . . . ? N6 Cu1 N5 C12 6.8(2) . . . . ? N1 Cu1 N5 C12 -70.1(4) . . . . ? N4 Cu1 N5 C12 -148.0(2) . . . . ? S50 Cu1 N5 C12 116.1(2) . . . . ? N6 Cu1 N5 C10 -173.6(3) . . . . ? N1 Cu1 N5 C10 109.5(3) . . . . ? N4 Cu1 N5 C10 31.6(3) . . . . ? S50 Cu1 N5 C10 -64.3(3) . . . . ? N1 Cu1 N6 C13 142.2(2) . . . . ? N5 Cu1 N6 C13 -12.1(2) . . . . ? N4 Cu1 N6 C13 70.3(3) . . . . ? S50 Cu1 N6 C13 -105.9(2) . . . . ? N1 Cu1 N6 N7 -4.5(3) . . . . ? N5 Cu1 N6 N7 -158.7(3) . . . . ? N4 Cu1 N6 N7 -76.4(4) . . . . ? S50 Cu1 N6 N7 107.5(3) . . . . ? C13 N6 N7 C15 0.0(3) . . . . ? Cu1 N6 N7 C15 148.1(2) . . . . ? C13 N6 N7 Cu2 -141.3(2) . . . . ? Cu1 N6 N7 Cu2 6.8(4) . . . . ? N2 Cu2 N7 C15 -141.6(2) . . . . ? N9 Cu2 N7 C15 15.3(2) . . . . ? N10 Cu2 N7 C15 -67.7(3) . . . . ? S60 Cu2 N7 C15 116.0(2) . . . . ? N2 Cu2 N7 N6 -1.8(3) . . . . ? N9 Cu2 N7 N6 155.1(3) . . . . ? N10 Cu2 N7 N6 72.0(4) . . . . ? S60 Cu2 N7 N6 -104.2(3) . . . . ? N2 Cu2 N9 C16 64.8(4) . . . . ? N7 Cu2 N9 C16 -10.7(2) . . . . ? N10 Cu2 N9 C16 142.2(2) . . . . ? S60 Cu2 N9 C16 -116.2(2) . . . . ? N2 Cu2 N9 C18 -104.1(3) . . . . ? N7 Cu2 N9 C18 -179.6(3) . . . . ? N10 Cu2 N9 C18 -26.8(3) . . . . ? S60 Cu2 N9 C18 74.9(3) . . . . ? N2 Cu2 N10 C22 3.3(2) . . . . ? N7 Cu2 N10 C22 -73.3(3) . . . . ? N9 Cu2 N10 C22 -153.1(2) . . . . ? S60 Cu2 N10 C22 103.1(2) . . . . ? N2 Cu2 N10 C20 178.2(2) . . . . ? N7 Cu2 N10 C20 101.7(3) . . . . ? N9 Cu2 N10 C20 21.8(2) . . . . ? S60 Cu2 N10 C20 -82.0(2) . . . . ? N1 N2 C3 N3 -1.2(3) . . . . ? Cu2 N2 C3 N3 -160.3(2) . . . . ? N1 N2 C3 C22 170.3(2) . . . . ? Cu2 N2 C3 C22 11.2(3) . . . . ? C5 N3 C3 N2 1.7(3) . . . . ? C5 N3 C3 C22 -168.3(3) . . . . ? N2 N1 C5 N3 1.1(3) . . . . ? Cu1 N1 C5 N3 153.4(2) . . . . ? N2 N1 C5 C6 -169.5(2) . . . . ? Cu1 N1 C5 C6 -17.2(3) . . . . ? C3 N3 C5 N1 -1.7(3) . . . . ? C3 N3 C5 C6 167.2(3) . . . . ? C8 N4 C6 C5 178.7(3) . . . . ? Cu1 N4 C6 C5 -7.2(3) . . . . ? C8 N4 C6 C7 -0.6(5) . . . . ? Cu1 N4 C6 C7 173.6(3) . . . . ? N1 C5 C6 N4 16.2(4) . . . . ? N3 C5 C6 N4 -152.5(3) . . . . ? N1 C5 C6 C7 -164.5(3) . . . . ? N3 C5 C6 C7 26.8(5) . . . . ? C6 N4 C8 C9 -134.7(3) . . . . ? Cu1 N4 C8 C9 51.3(3) . . . . ? N4 C8 C9 C10 -67.2(4) . . . . ? C12 N5 C10 C9 131.5(3) . . . . ? Cu1 N5 C10 C9 -48.0(4) . . . . ? C8 C9 C10 N5 65.3(4) . . . . ? C10 N5 C12 C13 179.9(3) . . . . ? Cu1 N5 C12 C13 -0.5(4) . . . . ? C10 N5 C12 C11 -0.7(5) . . . . ? Cu1 N5 C12 C11 178.9(3) . . . . ? N7 N6 C13 N8 -1.1(3) . . . . ? Cu1 N6 C13 N8 -157.0(2) . . . . ? N7 N6 C13 C12 171.5(3) . . . . ? Cu1 N6 C13 C12 15.6(3) . . . . ? C15 N8 C13 N6 1.8(3) . . . . ? C15 N8 C13 C12 -169.5(3) . . . . ? N5 C12 C13 N6 -10.1(4) . . . . ? C11 C12 C13 N6 170.5(3) . . . . ? N5 C12 C13 N8 160.9(3) . . . . ? C11 C12 C13 N8 -18.5(5) . . . . ? N6 N7 C15 N8 1.2(3) . . . . ? Cu2 N7 C15 N8 151.7(2) . . . . ? N6 N7 C15 C16 -168.3(3) . . . . ? Cu2 N7 C15 C16 -17.8(3) . . . . ? C13 N8 C15 N7 -1.8(3) . . . . ? C13 N8 C15 C16 165.9(3) . . . . ? C18 N9 C16 C15 173.2(3) . . . . ? Cu2 N9 C16 C15 4.1(4) . . . . ? C18 N9 C16 C17 -3.2(5) . . . . ? Cu2 N9 C16 C17 -172.4(3) . . . . ? N7 C15 C16 N9 9.4(4) . . . . ? N8 C15 C16 N9 -158.1(3) . . . . ? N7 C15 C16 C17 -173.9(3) . . . . ? N8 C15 C16 C17 18.6(5) . . . . ? C16 N9 C18 C19 -176.4(3) . . . . ? Cu2 N9 C18 C19 -8.1(4) . . . . ? N9 C18 C19 C20 63.0(4) . . . . ? C22 N10 C20 C19 -168.7(3) . . . . ? Cu2 N10 C20 C19 16.6(4) . . . . ? C18 C19 C20 N10 -67.8(4) . . . . ? C20 N10 C22 C3 -173.4(3) . . . . ? Cu2 N10 C22 C3 1.6(3) . . . . ? C20 N10 C22 C21 2.6(5) . . . . ? Cu2 N10 C22 C21 177.6(3) . . . . ? N2 C3 C22 N10 -8.5(4) . . . . ? N3 C3 C22 N10 161.4(3) . . . . ? N2 C3 C22 C21 175.3(3) . . . . ? N3 C3 C22 C21 -14.9(5) . . . . ? N16 Cu3 N11 C25 -135.6(2) . . . . ? N14 Cu3 N11 C25 11.7(2) . . . . ? N15 Cu3 N11 C25 -64.1(3) . . . . ? N60 Cu3 N11 C25 111.0(2) 1_455 . . . ? N16 Cu3 N11 N12 12.6(3) . . . . ? N14 Cu3 N11 N12 159.8(3) . . . . ? N15 Cu3 N11 N12 84.0(4) . . . . ? N60 Cu3 N11 N12 -100.8(3) 1_455 . . . ? C25 N11 N12 C23 0.2(3) . . . . ? Cu3 N11 N12 C23 -149.5(3) . . . . ? C25 N11 N12 Cu4 139.7(3) . . . . ? Cu3 N11 N12 Cu4 -10.0(5) . . . . ? N17 Cu4 N12 C23 135.8(2) . . . . ? N20 Cu4 N12 C23 -17.6(2) . . . . ? N19 Cu4 N12 C23 61.9(3) . . . . ? N50 Cu4 N12 C23 -121.1(2) . . . . ? N17 Cu4 N12 N11 -2.2(3) . . . . ? N20 Cu4 N12 N11 -155.6(3) . . . . ? N19 Cu4 N12 N11 -76.2(4) . . . . ? N50 Cu4 N12 N11 100.9(3) . . . . ? N11 Cu3 N14 C26 -7.6(3) . . . . ? N16 Cu3 N14 C26 70.1(4) . . . . ? N15 Cu3 N14 C26 144.1(3) . . . . ? N60 Cu3 N14 C26 -108.9(3) 1_455 . . . ? N11 Cu3 N14 C28 175.8(3) . . . . ? N16 Cu3 N14 C28 -106.5(3) . . . . ? N15 Cu3 N14 C28 -32.4(3) . . . . ? N60 Cu3 N14 C28 74.5(3) 1_455 . . . ? N11 Cu3 N15 C32 -66.3(4) . . . . ? N16 Cu3 N15 C32 8.1(3) . . . . ? N14 Cu3 N15 C32 -139.2(3) . . . . ? N60 Cu3 N15 C32 118.6(3) 1_455 . . . ? N11 Cu3 N15 C30 109.4(3) . . . . ? N16 Cu3 N15 C30 -176.2(3) . . . . ? N14 Cu3 N15 C30 36.5(3) . . . . ? N60 Cu3 N15 C30 -65.7(3) 1_455 . . . ? N11 Cu3 N16 C33 137.7(2) . . . . ? N14 Cu3 N16 C33 63.4(3) . . . . ? N15 Cu3 N16 C33 -14.3(2) . . . . ? N60 Cu3 N16 C33 -117.8(2) 1_455 . . . ? N11 Cu3 N16 N17 -3.9(3) . . . . ? N14 Cu3 N16 N17 -78.2(4) . . . . ? N15 Cu3 N16 N17 -155.8(3) . . . . ? N60 Cu3 N16 N17 100.7(3) 1_455 . . . ? C33 N16 N17 C35 -0.1(3) . . . . ? Cu3 N16 N17 C35 143.2(2) . . . . ? C33 N16 N17 Cu4 -150.9(3) . . . . ? Cu3 N16 N17 Cu4 -7.6(5) . . . . ? N12 Cu4 N17 C35 -138.6(2) . . . . ? N20 Cu4 N17 C35 -66.3(3) . . . . ? N19 Cu4 N17 C35 9.5(2) . . . . ? N50 Cu4 N17 C35 109.5(2) . . . . ? N12 Cu4 N17 N16 10.7(3) . . . . ? N20 Cu4 N17 N16 83.0(4) . . . . ? N19 Cu4 N17 N16 158.8(3) . . . . ? N50 Cu4 N17 N16 -101.2(3) . . . . ? N17 Cu4 N19 C36 -5.8(2) . . . . ? N12 Cu4 N19 C36 71.7(3) . . . . ? N20 Cu4 N19 C36 147.5(3) . . . . ? N50 Cu4 N19 C36 -105.6(3) . . . . ? N17 Cu4 N19 C38 -178.2(3) . . . . ? N12 Cu4 N19 C38 -100.7(3) . . . . ? N20 Cu4 N19 C38 -24.9(3) . . . . ? N50 Cu4 N19 C38 82.0(3) . . . . ? N17 Cu4 N20 C42 -62.3(4) . . . . ? N12 Cu4 N20 C42 12.8(2) . . . . ? N19 Cu4 N20 C42 -135.0(3) . . . . ? N50 Cu4 N20 C42 122.0(3) . . . . ? N17 Cu4 N20 C40 107.9(3) . . . . ? N12 Cu4 N20 C40 -177.1(3) . . . . ? N19 Cu4 N20 C40 35.1(3) . . . . ? N50 Cu4 N20 C40 -67.8(3) . . . . ? N11 N12 C23 N13 -1.0(4) . . . . ? Cu4 N12 C23 N13 -150.0(2) . . . . ? N11 N12 C23 C42 169.4(3) . . . . ? Cu4 N12 C23 C42 20.5(3) . . . . ? C25 N13 C23 N12 1.3(4) . . . . ? C25 N13 C23 C42 -167.7(3) . . . . ? N12 N11 C25 N13 0.7(4) . . . . ? Cu3 N11 C25 N13 158.0(2) . . . . ? N12 N11 C25 C26 -171.5(3) . . . . ? Cu3 N11 C25 C26 -14.1(4) . . . . ? C23 N13 C25 N11 -1.2(4) . . . . ? C23 N13 C25 C26 169.5(3) . . . . ? C28 N14 C26 C25 178.8(3) . . . . ? Cu3 N14 C26 C25 2.2(4) . . . . ? C28 N14 C26 C27 1.0(6) . . . . ? Cu3 N14 C26 C27 -175.5(3) . . . . ? N11 C25 C26 N14 8.0(5) . . . . ? N13 C25 C26 N14 -162.6(3) . . . . ? N11 C25 C26 C27 -174.1(3) . . . . ? N13 C25 C26 C27 15.4(6) . . . . ? C26 N14 C28 C29 175.5(4) . . . . ? Cu3 N14 C28 C29 -8.1(5) . . . . ? N14 C28 C29 C30 66.3(5) . . . . ? C32 N15 C30 C29 177.0(3) . . . . ? Cu3 N15 C30 C29 1.5(4) . . . . ? C28 C29 C30 N15 -62.1(4) . . . . ? C30 N15 C32 C33 -176.3(3) . . . . ? Cu3 N15 C32 C33 -0.6(4) . . . . ? C30 N15 C32 C31 1.9(6) . . . . ? Cu3 N15 C32 C31 177.6(3) . . . . ? N17 N16 C33 N18 -0.6(4) . . . . ? Cu3 N16 C33 N18 -152.2(2) . . . . ? N17 N16 C33 C32 170.2(3) . . . . ? Cu3 N16 C33 C32 18.6(4) . . . . ? C35 N18 C33 N16 1.0(4) . . . . ? C35 N18 C33 C32 -168.3(3) . . . . ? N15 C32 C33 N16 -12.1(4) . . . . ? C31 C32 C33 N16 169.6(3) . . . . ? N15 C32 C33 N18 157.0(3) . . . . ? C31 C32 C33 N18 -21.3(5) . . . . ? N16 N17 C35 N18 0.8(4) . . . . ? Cu4 N17 C35 N18 158.7(2) . . . . ? N16 N17 C35 C36 -169.8(3) . . . . ? Cu4 N17 C35 C36 -12.0(3) . . . . ? C33 N18 C35 N17 -1.1(4) . . . . ? C33 N18 C35 C36 168.0(3) . . . . ? C38 N19 C36 C35 173.4(3) . . . . ? Cu4 N19 C36 C35 1.1(4) . . . . ? C38 N19 C36 C37 -2.7(5) . . . . ? Cu4 N19 C36 C37 -175.0(3) . . . . ? N17 C35 C36 N19 7.3(4) . . . . ? N18 C35 C36 N19 -161.6(3) . . . . ? N17 C35 C36 C37 -176.3(3) . . . . ? N18 C35 C36 C37 14.8(5) . . . . ? C36 N19 C38 C39 169.2(3) . . . . ? Cu4 N19 C38 C39 -18.8(4) . . . . ? N19 C38 C39 C40 73.4(4) . . . . ? C42 N20 C40 C39 170.1(3) . . . . ? Cu4 N20 C40 C39 0.5(4) . . . . ? C38 C39 C40 N20 -62.4(4) . . . . ? C40 N20 C42 C23 -175.7(3) . . . . ? Cu4 N20 C42 C23 -5.3(4) . . . . ? C40 N20 C42 C41 2.5(5) . . . . ? Cu4 N20 C42 C41 172.8(3) . . . . ? N12 C23 C42 N20 -10.4(4) . . . . ? N13 C23 C42 N20 158.3(3) . . . . ? N12 C23 C42 C41 171.3(3) . . . . ? N13 C23 C42 C41 -19.9(5) . . . . ? N6 Cu1 S50 C50 -120.94(14) . . . . ? N1 Cu1 S50 C50 -20.72(14) . . . . ? N5 Cu1 S50 C50 156.35(14) . . . . ? N4 Cu1 S50 C50 60.72(14) . . . . ? Cu1 S50 C50 N50 -152(16) . . . . ? S50 C50 N50 Cu4 -92(16) . . . . ? N17 Cu4 N50 C50 162(3) . . . . ? N12 Cu4 N50 C50 65(3) . . . . ? N20 Cu4 N50 C50 -20(3) . . . . ? N19 Cu4 N50 C50 -116(3) . . . . ? N2 Cu2 S60 C60 79.17(14) . . . . ? N7 Cu2 S60 C60 174.94(13) . . . . ? N9 Cu2 S60 C60 -100.41(14) . . . . ? N10 Cu2 S60 C60 -3.33(14) . . . . ? Cu2 S60 C60 N60 19(10) . . . . ? S60 C60 N60 Cu3 102(10) . . . 1_655 ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 3.700 _refine_diff_density_min -1.231 _refine_diff_density_rms 0.097 data_cute _database_code_CSD 207834 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H24 Cu2 N11 S, C3 H7 N O, Cl O4' _chemical_formula_sum 'C22 H31 Cl Cu2 N12 O5 S' _chemical_formula_weight 738.18 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' Cu Cu 0.3201 1.2651 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 17.297(6) _cell_length_b 11.743(4) _cell_length_c 16.131(6) _cell_angle_alpha 90.00 _cell_angle_beta 112.506(5) _cell_angle_gamma 90.00 _cell_volume 3027.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 5216 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 26.22 _exptl_crystal_description Block _exptl_crystal_colour bluegreen _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 1.617 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.792776 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 38745 _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.43 _reflns_number_total 6163 _reflns_number_gt 4431 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0420P)^2^+2.3994P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6163 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.0944 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 0.34071(2) 0.41716(3) 0.21332(3) 0.02177(11) Uani 1 1 d . . . Cu2 Cu 0.32195(2) 0.72062(3) 0.32253(3) 0.02142(11) Uani 1 1 d . . . N1 N 0.27068(16) 0.5524(2) 0.16666(17) 0.0191(6) Uani 1 1 d . . . N2 N 0.26639(16) 0.6549(2) 0.20100(17) 0.0204(6) Uani 1 1 d . . . N3 N 0.13814(17) 0.6137(2) 0.09739(18) 0.0252(6) Uani 1 1 d . . . N4 N 0.24621(17) 0.3483(2) 0.10818(17) 0.0246(6) Uani 1 1 d . . . N5 N 0.37543(17) 0.2731(2) 0.28335(18) 0.0249(6) Uani 1 1 d . . . N6 N 0.39142(16) 0.4800(2) 0.33535(17) 0.0212(6) Uani 1 1 d . . . N7 N 0.38136(16) 0.5789(2) 0.37134(17) 0.0212(6) Uani 1 1 d . . . N8 N 0.40559(17) 0.4444(2) 0.47850(17) 0.0249(6) Uani 1 1 d . . . N9 N 0.33211(17) 0.7330(2) 0.45191(18) 0.0248(6) Uani 1 1 d . . . N10 N 0.21798(18) 0.8185(2) 0.27517(19) 0.0264(6) Uani 1 1 d . . . C3 C 0.1863(2) 0.6890(3) 0.1588(2) 0.0226(7) Uani 1 1 d . . . C5 C 0.1940(2) 0.5292(3) 0.1063(2) 0.0216(7) Uani 1 1 d . . . C6 C 0.1824(2) 0.4123(3) 0.0697(2) 0.0247(7) Uani 1 1 d . . . C7 C 0.1005(2) 0.3777(3) -0.0019(3) 0.0409(10) Uani 1 1 d . . . H7A H 0.1108 0.3404 -0.0510 0.061 Uiso 1 1 calc R . . H7B H 0.0657 0.4454 -0.0248 0.061 Uiso 1 1 calc R . . H7C H 0.0716 0.3248 0.0235 0.061 Uiso 1 1 calc R . . C8 C 0.2470(2) 0.2266(3) 0.0859(2) 0.0345(9) Uani 1 1 d . . . H8A H 0.2324 0.2185 0.0206 0.041 Uiso 1 1 calc R . . H8B H 0.2042 0.1858 0.1012 0.041 Uiso 1 1 calc R . . C9 C 0.3321(3) 0.1732(3) 0.1363(3) 0.0413(10) Uani 1 1 d . . . H9A H 0.3746 0.2189 0.1239 0.050 Uiso 1 1 calc R . . H9B H 0.3321 0.0962 0.1112 0.050 Uiso 1 1 calc R . . C10 C 0.3601(2) 0.1618(3) 0.2377(2) 0.0344(9) Uani 1 1 d . . . H10A H 0.3165 0.1206 0.2515 0.041 Uiso 1 1 calc R . . H10B H 0.4121 0.1160 0.2612 0.041 Uiso 1 1 calc R . . C11 C 0.4270(2) 0.1899(3) 0.4375(2) 0.0346(9) Uani 1 1 d . . . H11A H 0.3766 0.1558 0.4409 0.052 Uiso 1 1 calc R . . H11B H 0.4621 0.2211 0.4963 0.052 Uiso 1 1 calc R . . H11C H 0.4585 0.1316 0.4201 0.052 Uiso 1 1 calc R . . C12 C 0.4027(2) 0.2830(3) 0.3696(2) 0.0254(7) Uani 1 1 d . . . C13 C 0.40508(19) 0.4017(3) 0.3998(2) 0.0222(7) Uani 1 1 d . . . C15 C 0.3895(2) 0.5546(3) 0.4563(2) 0.0217(7) Uani 1 1 d . . . C16 C 0.3679(2) 0.6492(3) 0.5042(2) 0.0247(7) Uani 1 1 d . . . C17 C 0.3855(2) 0.6413(3) 0.6027(2) 0.0325(8) Uani 1 1 d . . . H17A H 0.4118 0.7120 0.6324 0.049 Uiso 1 1 calc R . . H17B H 0.4233 0.5771 0.6287 0.049 Uiso 1 1 calc R . . H17C H 0.3329 0.6295 0.6111 0.049 Uiso 1 1 calc R . . C18 C 0.2990(2) 0.8315(3) 0.4837(2) 0.0342(9) Uani 1 1 d . . . H18A H 0.3407 0.8568 0.5423 0.041 Uiso 1 1 calc R . . H18B H 0.2476 0.8088 0.4926 0.041 Uiso 1 1 calc R . . C19 C 0.2792(2) 0.9288(3) 0.4176(3) 0.0366(9) Uani 1 1 d . . . H19A H 0.3295 0.9438 0.4041 0.044 Uiso 1 1 calc R . . H19B H 0.2690 0.9976 0.4474 0.044 Uiso 1 1 calc R . . C20 C 0.2044(2) 0.9135(3) 0.3281(3) 0.0360(9) Uani 1 1 d . . . H20A H 0.1533 0.8985 0.3401 0.043 Uiso 1 1 calc R . . H20B H 0.1954 0.9848 0.2929 0.043 Uiso 1 1 calc R . . C21 C 0.0813(2) 0.8508(3) 0.1486(3) 0.0379(9) Uani 1 1 d . . . H21A H 0.0542 0.8675 0.1907 0.057 Uiso 1 1 calc R . . H21B H 0.0448 0.8017 0.1004 0.057 Uiso 1 1 calc R . . H21C H 0.0916 0.9221 0.1230 0.057 Uiso 1 1 calc R . . C22 C 0.1626(2) 0.7916(3) 0.1972(2) 0.0269(8) Uani 1 1 d . . . N50 N 0.41704(19) 0.8304(2) 0.32065(19) 0.0303(7) Uani 1 1 d . . . C50 C 0.4749(2) 0.8877(3) 0.3347(2) 0.0230(7) Uani 1 1 d . . . S50 S 0.55583(6) 0.97451(8) 0.35793(6) 0.0296(2) Uani 1 1 d . . . Cl1 Cl 0.16765(6) 0.26952(9) 0.29996(7) 0.0418(2) Uani 1 1 d . . . O11 O 0.2038(2) 0.3726(3) 0.2851(3) 0.0742(11) Uani 1 1 d . . . O12 O 0.2280(2) 0.2091(3) 0.3739(2) 0.0651(9) Uani 1 1 d . . . O13 O 0.09478(17) 0.2931(3) 0.3194(2) 0.0536(8) Uani 1 1 d . . . O14 O 0.1477(2) 0.1960(4) 0.2230(2) 0.0883(12) Uani 1 1 d . . . N60 N 0.0931(2) 0.6153(3) 0.3751(2) 0.0481(9) Uani 1 1 d . . . O60 O 0.1867(2) 0.5839(3) 0.5184(2) 0.0740(10) Uani 1 1 d . . . C60 C 0.1575(3) 0.5624(4) 0.4364(4) 0.0594(13) Uani 1 1 d . . . H60 H 0.1836 0.5033 0.4162 0.071 Uiso 1 1 calc R . . C61 C 0.0573(3) 0.5792(4) 0.2810(3) 0.0530(12) Uani 1 1 d . . . H61A H 0.0925 0.5195 0.2711 0.080 Uiso 1 1 calc R . . H61B H 0.0549 0.6445 0.2422 0.080 Uiso 1 1 calc R . . H61C H 0.0007 0.5495 0.2667 0.080 Uiso 1 1 calc R . . C62 C 0.0491(3) 0.7052(5) 0.4011(4) 0.0747(16) Uani 1 1 d . . . H62A H 0.0868 0.7398 0.4574 0.112 Uiso 1 1 calc R . . H62B H 0.0004 0.6731 0.4096 0.112 Uiso 1 1 calc R . . H62C H 0.0306 0.7634 0.3540 0.112 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 0.0267(2) 0.0203(2) 0.0185(2) -0.00037(17) 0.00902(17) 0.00232(17) Cu2 0.0242(2) 0.0203(2) 0.0210(2) -0.00215(17) 0.01003(17) -0.00161(17) N1 0.0206(14) 0.0193(14) 0.0176(14) 0.0001(11) 0.0076(12) -0.0003(11) N2 0.0238(15) 0.0185(14) 0.0210(14) -0.0014(11) 0.0110(12) -0.0015(11) N3 0.0247(15) 0.0280(15) 0.0220(15) -0.0012(12) 0.0081(12) -0.0007(12) N4 0.0350(17) 0.0230(15) 0.0189(14) -0.0051(12) 0.0137(13) -0.0041(13) N5 0.0292(16) 0.0208(14) 0.0267(16) -0.0027(12) 0.0128(13) 0.0023(12) N6 0.0218(14) 0.0225(14) 0.0201(14) -0.0006(12) 0.0088(12) 0.0009(11) N7 0.0214(14) 0.0236(14) 0.0187(14) -0.0027(12) 0.0077(12) -0.0011(11) N8 0.0274(16) 0.0296(16) 0.0174(14) -0.0004(12) 0.0083(12) -0.0015(12) N9 0.0295(16) 0.0219(15) 0.0252(15) -0.0073(12) 0.0128(13) -0.0047(12) N10 0.0308(16) 0.0199(14) 0.0303(17) -0.0018(12) 0.0137(14) 0.0006(12) C3 0.0219(18) 0.0256(18) 0.0198(17) 0.0039(14) 0.0075(14) 0.0015(14) C5 0.0268(18) 0.0255(17) 0.0148(16) 0.0011(13) 0.0107(14) -0.0005(14) C6 0.0294(19) 0.0283(18) 0.0184(17) -0.0039(14) 0.0114(15) -0.0050(15) C7 0.034(2) 0.045(2) 0.038(2) -0.0141(19) 0.0070(18) -0.0066(18) C8 0.050(2) 0.0213(18) 0.030(2) -0.0068(16) 0.0131(18) -0.0040(17) C9 0.063(3) 0.027(2) 0.039(2) -0.0095(17) 0.025(2) 0.0039(19) C10 0.044(2) 0.0222(18) 0.037(2) -0.0006(16) 0.0148(18) 0.0054(16) C11 0.044(2) 0.028(2) 0.033(2) 0.0058(16) 0.0158(18) 0.0048(16) C12 0.0234(18) 0.0267(18) 0.0281(19) 0.0054(15) 0.0122(15) 0.0058(15) C13 0.0198(17) 0.0273(18) 0.0194(17) 0.0026(14) 0.0074(14) 0.0022(14) C15 0.0205(17) 0.0281(18) 0.0159(16) 0.0003(14) 0.0065(13) -0.0036(14) C16 0.0230(18) 0.0309(19) 0.0212(17) -0.0068(15) 0.0095(14) -0.0093(15) C17 0.037(2) 0.038(2) 0.0228(19) -0.0063(16) 0.0124(16) -0.0045(17) C18 0.040(2) 0.031(2) 0.035(2) -0.0129(17) 0.0181(18) -0.0028(17) C19 0.047(2) 0.0248(19) 0.042(2) -0.0097(17) 0.0219(19) -0.0001(17) C20 0.039(2) 0.028(2) 0.043(2) -0.0077(17) 0.0178(19) 0.0038(17) C21 0.035(2) 0.036(2) 0.039(2) 0.0013(18) 0.0107(18) 0.0114(17) C22 0.0279(19) 0.0221(17) 0.034(2) 0.0039(15) 0.0155(16) 0.0027(14) N50 0.0333(17) 0.0326(17) 0.0255(16) -0.0016(13) 0.0118(14) -0.0111(14) C50 0.033(2) 0.0245(18) 0.0150(16) 0.0019(13) 0.0134(15) 0.0038(15) S50 0.0293(5) 0.0279(5) 0.0369(5) -0.0071(4) 0.0187(4) -0.0075(4) Cl1 0.0383(5) 0.0533(6) 0.0376(5) 0.0045(5) 0.0188(4) 0.0045(5) O11 0.077(2) 0.059(2) 0.120(3) 0.029(2) 0.074(2) 0.0164(18) O12 0.059(2) 0.074(2) 0.062(2) 0.0225(18) 0.0226(17) 0.0257(18) O13 0.0444(18) 0.059(2) 0.070(2) 0.0140(16) 0.0351(16) 0.0106(14) O14 0.073(3) 0.127(3) 0.062(2) -0.035(2) 0.023(2) -0.005(2) N60 0.044(2) 0.053(2) 0.046(2) -0.0047(18) 0.0160(18) -0.0018(17) O60 0.049(2) 0.099(3) 0.059(2) -0.007(2) 0.0053(17) -0.0025(19) C60 0.050(3) 0.059(3) 0.070(4) -0.001(3) 0.025(3) 0.002(2) C61 0.068(3) 0.044(3) 0.050(3) 0.003(2) 0.026(2) 0.003(2) C62 0.068(4) 0.088(4) 0.061(3) -0.020(3) 0.016(3) 0.014(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 N1 1.964(3) . ? Cu1 N6 1.967(3) . ? Cu1 N5 1.995(3) . ? Cu1 N4 2.020(3) . ? Cu1 S50 2.5595(11) 2_645 ? Cu2 N7 1.956(3) . ? Cu2 N2 1.980(3) . ? Cu2 N10 2.022(3) . ? Cu2 N9 2.032(3) . ? Cu2 N50 2.100(3) . ? N1 C5 1.339(4) . ? N1 N2 1.339(3) . ? N2 C3 1.349(4) . ? N3 C3 1.352(4) . ? N3 C5 1.353(4) . ? N4 C6 1.282(4) . ? N4 C8 1.475(4) . ? N5 C12 1.292(4) . ? N5 C10 1.474(4) . ? N6 C13 1.339(4) . ? N6 N7 1.339(3) . ? N7 C15 1.354(4) . ? N8 C15 1.343(4) . ? N8 C13 1.362(4) . ? N9 C16 1.290(4) . ? N9 C18 1.467(4) . ? N10 C22 1.295(4) . ? N10 C20 1.477(4) . ? C3 C22 1.483(5) . ? C5 C6 1.478(4) . ? C6 C7 1.501(5) . ? C8 C9 1.519(5) . ? C9 C10 1.523(5) . ? C11 C12 1.490(5) . ? C12 C13 1.472(5) . ? C15 C16 1.479(5) . ? C16 C17 1.502(4) . ? C18 C19 1.511(5) . ? C19 C20 1.537(5) . ? C21 C22 1.493(5) . ? N50 C50 1.154(4) . ? C50 S50 1.654(4) . ? S50 Cu1 2.5595(11) 2_655 ? Cl1 O11 1.424(3) . ? Cl1 O12 1.436(3) . ? Cl1 O13 1.437(3) . ? Cl1 O14 1.442(4) . ? N60 C60 1.328(6) . ? N60 C62 1.454(6) . ? N60 C61 1.466(5) . ? O60 C60 1.247(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N6 93.07(11) . . ? N1 Cu1 N5 155.57(11) . . ? N6 Cu1 N5 80.16(11) . . ? N1 Cu1 N4 79.62(11) . . ? N6 Cu1 N4 153.93(11) . . ? N5 Cu1 N4 96.17(11) . . ? N1 Cu1 S50 92.86(8) . 2_645 ? N6 Cu1 S50 103.30(8) . 2_645 ? N5 Cu1 S50 111.52(8) . 2_645 ? N4 Cu1 S50 102.03(8) . 2_645 ? N7 Cu2 N2 92.77(11) . . ? N7 Cu2 N10 152.89(11) . . ? N2 Cu2 N10 79.80(11) . . ? N7 Cu2 N9 79.73(11) . . ? N2 Cu2 N9 149.72(11) . . ? N10 Cu2 N9 93.56(11) . . ? N7 Cu2 N50 103.57(12) . . ? N2 Cu2 N50 108.12(11) . . ? N10 Cu2 N50 103.52(12) . . ? N9 Cu2 N50 102.16(11) . . ? C5 N1 N2 106.7(3) . . ? C5 N1 Cu1 114.1(2) . . ? N2 N1 Cu1 133.8(2) . . ? N1 N2 C3 105.5(2) . . ? N1 N2 Cu2 132.6(2) . . ? C3 N2 Cu2 113.6(2) . . ? C3 N3 C5 100.8(3) . . ? C6 N4 C8 122.5(3) . . ? C6 N4 Cu1 116.2(2) . . ? C8 N4 Cu1 120.8(2) . . ? C12 N5 C10 122.7(3) . . ? C12 N5 Cu1 116.1(2) . . ? C10 N5 Cu1 120.8(2) . . ? C13 N6 N7 105.8(3) . . ? C13 N6 Cu1 113.4(2) . . ? N7 N6 Cu1 132.6(2) . . ? N6 N7 C15 106.0(3) . . ? N6 N7 Cu2 134.3(2) . . ? C15 N7 Cu2 115.0(2) . . ? C15 N8 C13 100.3(3) . . ? C16 N9 C18 121.8(3) . . ? C16 N9 Cu2 116.6(2) . . ? C18 N9 Cu2 121.6(2) . . ? C22 N10 C20 121.5(3) . . ? C22 N10 Cu2 116.7(2) . . ? C20 N10 Cu2 121.8(2) . . ? N2 C3 N3 113.7(3) . . ? N2 C3 C22 115.2(3) . . ? N3 C3 C22 130.3(3) . . ? N1 C5 N3 113.4(3) . . ? N1 C5 C6 115.1(3) . . ? N3 C5 C6 131.1(3) . . ? N4 C6 C5 113.0(3) . . ? N4 C6 C7 126.7(3) . . ? C5 C6 C7 120.1(3) . . ? N4 C8 C9 111.6(3) . . ? C8 C9 C10 117.2(3) . . ? N5 C10 C9 112.4(3) . . ? N5 C12 C13 113.2(3) . . ? N5 C12 C11 127.6(3) . . ? C13 C12 C11 119.2(3) . . ? N6 C13 N8 114.0(3) . . ? N6 C13 C12 114.8(3) . . ? N8 C13 C12 130.2(3) . . ? N8 C15 N7 113.8(3) . . ? N8 C15 C16 130.7(3) . . ? N7 C15 C16 114.9(3) . . ? N9 C16 C15 112.7(3) . . ? N9 C16 C17 126.2(3) . . ? C15 C16 C17 121.1(3) . . ? N9 C18 C19 111.2(3) . . ? C18 C19 C20 117.2(3) . . ? N10 C20 C19 111.6(3) . . ? N10 C22 C3 112.6(3) . . ? N10 C22 C21 126.4(3) . . ? C3 C22 C21 121.0(3) . . ? C50 N50 Cu2 168.7(3) . . ? N50 C50 S50 176.9(3) . . ? C50 S50 Cu1 114.38(12) . 2_655 ? O11 Cl1 O12 109.5(2) . . ? O11 Cl1 O13 110.58(18) . . ? O12 Cl1 O13 109.49(19) . . ? O11 Cl1 O14 109.8(2) . . ? O12 Cl1 O14 106.1(2) . . ? O13 Cl1 O14 111.3(2) . . ? C60 N60 C62 120.5(4) . . ? C60 N60 C61 122.5(4) . . ? C62 N60 C61 116.7(4) . . ? O60 C60 N60 125.3(5) . . ? 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 N6 Cu1 N1 C5 -142.2(2) . . . . ? N5 Cu1 N1 C5 -69.4(4) . . . . ? N4 Cu1 N1 C5 12.6(2) . . . . ? S50 Cu1 N1 C5 114.3(2) 2_645 . . . ? N6 Cu1 N1 N2 7.6(3) . . . . ? N5 Cu1 N1 N2 80.4(4) . . . . ? N4 Cu1 N1 N2 162.4(3) . . . . ? S50 Cu1 N1 N2 -95.9(3) 2_645 . . . ? C5 N1 N2 C3 -0.3(3) . . . . ? Cu1 N1 N2 C3 -151.6(2) . . . . ? C5 N1 N2 Cu2 144.6(2) . . . . ? Cu1 N1 N2 Cu2 -6.7(4) . . . . ? N7 Cu2 N2 N1 -1.3(3) . . . . ? N10 Cu2 N2 N1 -155.1(3) . . . . ? N9 Cu2 N2 N1 -75.6(4) . . . . ? N50 Cu2 N2 N1 103.9(3) . . . . ? N7 Cu2 N2 C3 141.4(2) . . . . ? N10 Cu2 N2 C3 -12.3(2) . . . . ? N9 Cu2 N2 C3 67.2(3) . . . . ? N50 Cu2 N2 C3 -113.3(2) . . . . ? N1 Cu1 N4 C6 -9.5(2) . . . . ? N6 Cu1 N4 C6 66.0(4) . . . . ? N5 Cu1 N4 C6 146.2(2) . . . . ? S50 Cu1 N4 C6 -100.2(2) 2_645 . . . ? N1 Cu1 N4 C8 178.3(3) . . . . ? N6 Cu1 N4 C8 -106.2(3) . . . . ? N5 Cu1 N4 C8 -26.0(3) . . . . ? S50 Cu1 N4 C8 87.6(2) 2_645 . . . ? N1 Cu1 N5 C12 -67.2(4) . . . . ? N6 Cu1 N5 C12 8.3(2) . . . . ? N4 Cu1 N5 C12 -145.7(2) . . . . ? S50 Cu1 N5 C12 108.8(2) 2_645 . . . ? N1 Cu1 N5 C10 105.2(3) . . . . ? N6 Cu1 N5 C10 -179.3(3) . . . . ? N4 Cu1 N5 C10 26.8(3) . . . . ? S50 Cu1 N5 C10 -78.7(3) 2_645 . . . ? N1 Cu1 N6 C13 142.9(2) . . . . ? N5 Cu1 N6 C13 -13.4(2) . . . . ? N4 Cu1 N6 C13 70.5(3) . . . . ? S50 Cu1 N6 C13 -123.4(2) 2_645 . . . ? N1 Cu1 N6 N7 -0.5(3) . . . . ? N5 Cu1 N6 N7 -156.8(3) . . . . ? N4 Cu1 N6 N7 -72.9(4) . . . . ? S50 Cu1 N6 N7 93.2(3) 2_645 . . . ? C13 N6 N7 C15 -0.1(3) . . . . ? Cu1 N6 N7 C15 145.3(2) . . . . ? C13 N6 N7 Cu2 -153.4(2) . . . . ? Cu1 N6 N7 Cu2 -8.1(4) . . . . ? N2 Cu2 N7 N6 8.6(3) . . . . ? N10 Cu2 N7 N6 81.5(4) . . . . ? N9 Cu2 N7 N6 159.1(3) . . . . ? N50 Cu2 N7 N6 -100.8(3) . . . . ? N2 Cu2 N7 C15 -143.0(2) . . . . ? N10 Cu2 N7 C15 -70.1(3) . . . . ? N9 Cu2 N7 C15 7.5(2) . . . . ? N50 Cu2 N7 C15 107.6(2) . . . . ? N7 Cu2 N9 C16 -1.5(2) . . . . ? N2 Cu2 N9 C16 76.2(3) . . . . ? N10 Cu2 N9 C16 152.1(2) . . . . ? N50 Cu2 N9 C16 -103.3(2) . . . . ? N7 Cu2 N9 C18 179.6(3) . . . . ? N2 Cu2 N9 C18 -102.7(3) . . . . ? N10 Cu2 N9 C18 -26.9(3) . . . . ? N50 Cu2 N9 C18 77.8(3) . . . . ? N7 Cu2 N10 C22 -70.4(4) . . . . ? N2 Cu2 N10 C22 5.5(2) . . . . ? N9 Cu2 N10 C22 -144.7(3) . . . . ? N50 Cu2 N10 C22 111.9(3) . . . . ? N7 Cu2 N10 C20 107.5(3) . . . . ? N2 Cu2 N10 C20 -176.6(3) . . . . ? N9 Cu2 N10 C20 33.2(3) . . . . ? N50 Cu2 N10 C20 -70.3(3) . . . . ? N1 N2 C3 N3 -0.8(4) . . . . ? Cu2 N2 C3 N3 -153.3(2) . . . . ? N1 N2 C3 C22 169.5(3) . . . . ? Cu2 N2 C3 C22 17.1(3) . . . . ? C5 N3 C3 N2 1.4(3) . . . . ? C5 N3 C3 C22 -167.1(3) . . . . ? N2 N1 C5 N3 1.2(3) . . . . ? Cu1 N1 C5 N3 158.9(2) . . . . ? N2 N1 C5 C6 -171.8(2) . . . . ? Cu1 N1 C5 C6 -14.1(3) . . . . ? C3 N3 C5 N1 -1.6(3) . . . . ? C3 N3 C5 C6 170.0(3) . . . . ? C8 N4 C6 C5 176.6(3) . . . . ? Cu1 N4 C6 C5 4.6(4) . . . . ? C8 N4 C6 C7 -0.1(5) . . . . ? Cu1 N4 C6 C7 -172.1(3) . . . . ? N1 C5 C6 N4 6.2(4) . . . . ? N3 C5 C6 N4 -165.3(3) . . . . ? N1 C5 C6 C7 -176.9(3) . . . . ? N3 C5 C6 C7 11.6(5) . . . . ? C6 N4 C8 C9 175.9(3) . . . . ? Cu1 N4 C8 C9 -12.5(4) . . . . ? N4 C8 C9 C10 67.6(4) . . . . ? C12 N5 C10 C9 -177.3(3) . . . . ? Cu1 N5 C10 C9 10.7(4) . . . . ? C8 C9 C10 N5 -67.0(4) . . . . ? C10 N5 C12 C13 -174.1(3) . . . . ? Cu1 N5 C12 C13 -1.8(4) . . . . ? C10 N5 C12 C11 3.2(5) . . . . ? Cu1 N5 C12 C11 175.5(3) . . . . ? N7 N6 C13 N8 -0.7(4) . . . . ? Cu1 N6 C13 N8 -153.6(2) . . . . ? N7 N6 C13 C12 169.4(3) . . . . ? Cu1 N6 C13 C12 16.5(3) . . . . ? C15 N8 C13 N6 1.2(3) . . . . ? C15 N8 C13 C12 -167.0(3) . . . . ? N5 C12 C13 N6 -9.7(4) . . . . ? C11 C12 C13 N6 172.7(3) . . . . ? N5 C12 C13 N8 158.4(3) . . . . ? C11 C12 C13 N8 -19.1(5) . . . . ? C13 N8 C15 N7 -1.2(3) . . . . ? C13 N8 C15 C16 169.3(3) . . . . ? N6 N7 C15 N8 0.9(4) . . . . ? Cu2 N7 C15 N8 160.1(2) . . . . ? N6 N7 C15 C16 -171.2(3) . . . . ? Cu2 N7 C15 C16 -11.9(3) . . . . ? C18 N9 C16 C15 174.7(3) . . . . ? Cu2 N9 C16 C15 -4.3(4) . . . . ? C18 N9 C16 C17 -3.6(5) . . . . ? Cu2 N9 C16 C17 177.4(3) . . . . ? N8 C15 C16 N9 -159.9(3) . . . . ? N7 C15 C16 N9 10.5(4) . . . . ? N8 C15 C16 C17 18.6(5) . . . . ? N7 C15 C16 C17 -171.1(3) . . . . ? C16 N9 C18 C19 166.5(3) . . . . ? Cu2 N9 C18 C19 -14.6(4) . . . . ? N9 C18 C19 C20 69.9(4) . . . . ? C22 N10 C20 C19 -179.7(3) . . . . ? Cu2 N10 C20 C19 2.6(4) . . . . ? C18 C19 C20 N10 -63.1(4) . . . . ? C20 N10 C22 C3 -176.0(3) . . . . ? Cu2 N10 C22 C3 1.8(4) . . . . ? C20 N10 C22 C21 2.2(5) . . . . ? Cu2 N10 C22 C21 -180.0(3) . . . . ? N2 C3 C22 N10 -12.5(4) . . . . ? N3 C3 C22 N10 155.9(3) . . . . ? N2 C3 C22 C21 169.2(3) . . . . ? N3 C3 C22 C21 -22.4(5) . . . . ? N7 Cu2 N50 C50 -60.0(15) . . . . ? N2 Cu2 N50 C50 -157.5(14) . . . . ? N10 Cu2 N50 C50 119.0(14) . . . . ? N9 Cu2 N50 C50 22.3(15) . . . . ? Cu2 N50 C50 S50 -67(7) . . . . ? N50 C50 S50 Cu1 -177(100) . . . 2_655 ? C62 N60 C60 O60 -1.1(8) . . . . ? C61 N60 C60 O60 -174.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.540 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.083 data_uber#2 _database_code_CSD 207835 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H27 Cl Cu2 N12 O4 S' _chemical_formula_weight 706.14 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' Cu Cu 0.3201 1.2651 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 16.854(6) _cell_length_b 11.891(4) _cell_length_c 16.280(5) _cell_angle_alpha 90.00 _cell_angle_beta 118.727(3) _cell_angle_gamma 90.00 _cell_volume 2861.0(16) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 1.705 _exptl_absorpt_correction_type Semi-empirical(SADABS) _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35477 _diffrn_reflns_av_R_equivalents 0.1164 _diffrn_reflns_av_sigmaI/netI 0.0834 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 26.38 _reflns_number_total 5770 _reflns_number_gt 4064 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0000P)^2^+14.5929P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5770 _refine_ls_number_parameters 375 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1315 _refine_ls_R_factor_gt 0.0848 _refine_ls_wR_factor_ref 0.1267 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.260 _refine_ls_restrained_S_all 1.260 _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 0.19053(5) 1.22547(7) 0.19462(5) 0.0222(2) Uani 1 1 d . . . Cu2 Cu 0.17221(5) 0.92669(7) 0.30417(5) 0.0223(2) Uani 1 1 d . . . N1 N 0.1271(3) 1.0834(4) 0.1389(3) 0.0209(12) Uani 1 1 d . . . N2 N 0.1192(3) 0.9854(4) 0.1753(3) 0.0212(12) Uani 1 1 d . . . N3 N 0.1058(4) 0.9480(4) 0.0327(4) 0.0259(13) Uani 1 1 d . . . N4 N 0.1816(4) 1.2357(4) 0.0653(4) 0.0258(13) Uani 1 1 d . . . N5 N 0.3033(4) 1.3244(4) 0.2567(4) 0.0258(13) Uani 1 1 d . . . N6 N 0.2483(3) 1.1644(4) 0.3229(4) 0.0214(12) Uani 1 1 d . . . N7 N 0.2428(3) 1.0647(4) 0.3580(3) 0.0196(11) Uani 1 1 d . . . N8 N 0.3848(3) 1.1310(5) 0.4509(4) 0.0260(13) Uani 1 1 d . . . N9 N 0.2714(3) 0.8648(4) 0.4264(4) 0.0232(12) Uani 1 1 d . . . N10 N 0.1413(3) 0.7810(5) 0.2340(4) 0.0268(13) Uani 1 1 d . . . C3 C 0.1063(4) 0.9068(5) 0.1106(4) 0.0216(14) Uani 1 1 d . . . C5 C 0.1189(4) 1.0584(6) 0.0541(4) 0.0263(15) Uani 1 1 d . . . C6 C 0.1412(4) 1.1523(6) 0.0081(4) 0.0271(16) Uani 1 1 d . . . C7 C 0.1217(5) 1.1445(6) -0.0918(4) 0.0312(17) Uani 1 1 d . . . H7A H 0.0885 1.2116 -0.1260 0.037 Uiso 1 1 calc R . . H7B H 0.0850 1.0774 -0.1209 0.037 Uiso 1 1 calc R . . H7C H 0.1787 1.1393 -0.0938 0.037 Uiso 1 1 calc R . . C8 C 0.2177(5) 1.3332(6) 0.0380(5) 0.0328(17) Uani 1 1 d . . . H8A H 0.1731 1.3575 -0.0259 0.039 Uiso 1 1 calc R . . H8B H 0.2738 1.3111 0.0371 0.039 Uiso 1 1 calc R . . C9 C 0.2379(5) 1.4308(6) 0.1057(5) 0.0318(16) Uani 1 1 d . . . H9A H 0.1833 1.4448 0.1123 0.038 Uiso 1 1 calc R . . H9B H 0.2483 1.4988 0.0771 0.038 Uiso 1 1 calc R . . C10 C 0.3191(5) 1.4167(6) 0.2047(5) 0.0359(18) Uani 1 1 d . . . H10A H 0.3742 1.4001 0.1996 0.043 Uiso 1 1 calc R . . H10B H 0.3294 1.4880 0.2399 0.043 Uiso 1 1 calc R . . C11 C 0.4492(4) 1.3608(6) 0.4017(5) 0.0343(17) Uani 1 1 d . . . H11A H 0.4381 1.4418 0.4016 0.041 Uiso 1 1 calc R . . H11B H 0.4900 1.3474 0.3756 0.041 Uiso 1 1 calc R . . H11C H 0.4769 1.3324 0.4661 0.041 Uiso 1 1 calc R . . C12 C 0.3610(4) 1.3010(5) 0.3431(5) 0.0258(15) Uani 1 1 d . . . C13 C 0.3343(4) 1.2011(5) 0.3792(4) 0.0234(15) Uani 1 1 d . . . C15 C 0.3246(4) 1.0459(5) 0.4336(4) 0.0206(14) Uani 1 1 d . . . C16 C 0.3371(4) 0.9323(6) 0.4759(4) 0.0246(15) Uani 1 1 d . . . C17 C 0.4225(4) 0.9062(6) 0.5644(5) 0.0344(18) Uani 1 1 d . . . H17A H 0.4093 0.8526 0.6020 0.041 Uiso 1 1 calc R . . H17B H 0.4471 0.9756 0.6003 0.041 Uiso 1 1 calc R . . H17C H 0.4669 0.8734 0.5488 0.041 Uiso 1 1 calc R . . C18 C 0.2724(5) 0.7445(5) 0.4514(5) 0.0293(16) Uani 1 1 d . . . H18A H 0.2835 0.7388 0.5167 0.035 Uiso 1 1 calc R . . H18B H 0.3223 0.7055 0.4475 0.035 Uiso 1 1 calc R . . C19 C 0.1815(5) 0.6867(6) 0.3849(5) 0.0323(17) Uani 1 1 d . . . H19A H 0.1811 0.6112 0.4104 0.039 Uiso 1 1 calc R . . H19B H 0.1320 0.7306 0.3857 0.039 Uiso 1 1 calc R . . C20 C 0.1605(5) 0.6731(6) 0.2830(5) 0.0346(18) Uani 1 1 d . . . H20A H 0.2129 0.6374 0.2814 0.042 Uiso 1 1 calc R . . H20B H 0.1077 0.6227 0.2501 0.042 Uiso 1 1 calc R . . C21 C 0.0922(5) 0.6944(6) 0.0759(5) 0.0368(18) Uani 1 1 d . . . H21A H 0.0586 0.6356 0.0884 0.044 Uiso 1 1 calc R . . H21B H 0.1486 0.6629 0.0823 0.044 Uiso 1 1 calc R . . H21C H 0.0553 0.7230 0.0121 0.044 Uiso 1 1 calc R . . C22 C 0.1135(4) 0.7885(5) 0.1444(5) 0.0244(15) Uani 1 1 d . . . S50 S 0.05398(12) 0.98686(15) 0.35571(14) 0.0328(4) Uani 1 1 d . . . C50 C -0.0280(4) 0.8957(5) 0.3321(4) 0.0206(14) Uani 1 1 d . . . N50 N -0.0865(4) 0.8337(5) 0.3181(4) 0.0319(14) Uani 1 1 d . . . Cl1 Cl 0.38239(14) 0.78335(19) 0.26622(14) 0.0478(5) Uani 1 1 d . . . O11 O 0.3401(5) 0.8831(6) 0.2770(6) 0.095(3) Uani 1 1 d . . . O12 O 0.4560(4) 0.8133(5) 0.2488(5) 0.0666(19) Uani 1 1 d . . . O13 O 0.4132(5) 0.7130(8) 0.3468(5) 0.103(3) Uani 1 1 d . . . O14 O 0.3156(4) 0.7206(6) 0.1882(4) 0.0698(19) Uani 1 1 d . . . N60 N 0.3338(5) 1.4569(7) 0.5019(6) 0.065(2) Uani 1 1 d . . . C60 C 0.3656(6) 1.4392(7) 0.5806(7) 0.050(2) Uani 1 1 d . . . C61 C 0.4074(7) 1.4144(8) 0.6797(7) 0.072(3) Uani 1 1 d . . . H41A H 0.4344 1.3391 0.6913 0.086 Uiso 1 1 calc R . . H41B H 0.3615 1.4170 0.7003 0.086 Uiso 1 1 calc R . . H41C H 0.4546 1.4701 0.7147 0.086 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 0.0249(4) 0.0191(4) 0.0261(4) 0.0031(4) 0.0150(4) 0.0021(4) Cu2 0.0269(4) 0.0182(4) 0.0227(4) 0.0006(4) 0.0126(4) -0.0012(4) N1 0.023(3) 0.021(3) 0.022(3) 0.004(2) 0.015(2) -0.001(2) N2 0.022(3) 0.017(3) 0.025(3) -0.002(2) 0.011(2) 0.000(2) N3 0.027(3) 0.025(3) 0.026(3) 0.003(3) 0.014(3) 0.004(3) N4 0.030(3) 0.022(3) 0.033(3) 0.011(3) 0.022(3) 0.008(3) N5 0.028(3) 0.016(3) 0.038(4) 0.003(3) 0.019(3) -0.001(2) N6 0.024(3) 0.014(3) 0.031(3) -0.001(2) 0.017(3) -0.004(2) N7 0.020(3) 0.017(3) 0.021(3) -0.001(2) 0.010(2) 0.004(2) N8 0.026(3) 0.029(3) 0.027(3) -0.004(3) 0.016(3) -0.004(3) N9 0.028(3) 0.018(3) 0.031(3) 0.006(2) 0.021(3) 0.004(3) N10 0.027(3) 0.025(3) 0.028(3) 0.004(3) 0.014(3) 0.001(3) C3 0.015(3) 0.027(4) 0.019(3) 0.002(3) 0.005(3) 0.000(3) C5 0.024(4) 0.030(4) 0.026(4) 0.006(3) 0.014(3) 0.002(3) C6 0.021(4) 0.032(4) 0.024(4) 0.008(3) 0.007(3) 0.010(3) C7 0.036(4) 0.034(4) 0.025(4) 0.007(3) 0.016(3) 0.007(3) C8 0.036(4) 0.033(4) 0.032(4) 0.019(3) 0.019(4) 0.011(3) C9 0.040(4) 0.019(4) 0.049(5) 0.012(3) 0.032(4) 0.005(3) C10 0.036(4) 0.028(4) 0.051(5) 0.011(4) 0.027(4) 0.000(4) C11 0.028(4) 0.031(4) 0.039(4) -0.002(3) 0.012(3) -0.008(3) C12 0.025(4) 0.018(4) 0.040(4) -0.003(3) 0.020(3) -0.005(3) C13 0.024(4) 0.026(4) 0.023(4) 0.000(3) 0.013(3) 0.004(3) C15 0.021(3) 0.022(4) 0.023(3) -0.005(3) 0.014(3) -0.005(3) C16 0.025(4) 0.028(4) 0.027(4) 0.002(3) 0.016(3) 0.004(3) C17 0.031(4) 0.037(5) 0.033(4) 0.011(3) 0.013(3) 0.005(3) C18 0.042(4) 0.020(4) 0.028(4) 0.008(3) 0.019(3) 0.004(3) C19 0.035(4) 0.023(4) 0.044(4) 0.012(3) 0.023(4) -0.001(3) C20 0.042(5) 0.022(4) 0.038(5) 0.000(3) 0.018(4) -0.006(3) C21 0.045(5) 0.025(4) 0.041(5) -0.007(3) 0.022(4) 0.001(3) C22 0.023(4) 0.023(4) 0.028(4) -0.008(3) 0.014(3) -0.006(3) S50 0.0311(10) 0.0258(10) 0.0506(12) -0.0108(9) 0.0268(9) -0.0086(8) C50 0.018(3) 0.022(4) 0.025(4) -0.005(3) 0.013(3) -0.002(3) N50 0.034(4) 0.030(3) 0.035(4) -0.001(3) 0.020(3) -0.006(3) Cl1 0.0473(12) 0.0619(14) 0.0454(12) -0.0069(11) 0.0314(10) -0.0085(11) O11 0.119(6) 0.071(5) 0.158(7) -0.055(5) 0.118(6) -0.034(4) O12 0.071(4) 0.060(4) 0.105(5) 0.005(4) 0.071(4) -0.004(3) O13 0.083(5) 0.166(8) 0.059(4) 0.039(5) 0.034(4) -0.016(5) O14 0.062(4) 0.089(5) 0.061(4) -0.026(4) 0.031(3) -0.007(4) N60 0.054(5) 0.066(6) 0.073(6) -0.001(5) 0.028(5) 0.002(4) C60 0.038(5) 0.040(5) 0.065(6) -0.005(5) 0.021(5) -0.006(4) C61 0.083(8) 0.058(7) 0.071(7) 0.007(6) 0.033(6) -0.002(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 Cu1 N6 1.970(5) . y Cu1 N1 1.972(5) . y Cu1 N4 2.040(5) . y Cu1 N5 2.043(5) . y Cu1 N50 2.104(6) 2 y Cu2 N7 1.969(5) . y Cu2 N2 1.971(5) . y Cu2 N10 2.002(6) . y Cu2 N9 2.025(5) . y Cu2 S50 2.607(2) . y N1 N2 1.342(7) . ? N1 C5 1.353(8) . ? N2 C3 1.345(8) . ? N3 C5 1.348(8) . ? N3 C3 1.356(8) . ? N4 C6 1.306(8) . ? N4 C8 1.474(8) . ? N5 C12 1.298(8) . ? N5 C10 1.486(8) . ? N6 N7 1.338(7) . ? N6 C13 1.362(8) . ? N7 C15 1.355(8) . ? N8 C13 1.352(8) . ? N8 C15 1.362(7) . ? N9 C16 1.290(8) . ? N9 C18 1.484(8) . ? N10 C22 1.303(8) . ? N10 C20 1.463(8) . ? C3 C22 1.493(9) . ? C5 C6 1.489(9) . ? C6 C7 1.500(9) . ? C8 C9 1.522(9) . ? C9 C10 1.542(10) . ? C11 C12 1.504(9) . ? C12 C13 1.488(9) . ? C15 C16 1.485(9) . ? C16 C17 1.500(9) . ? C18 C19 1.549(9) . ? C19 C20 1.530(9) . ? C21 C22 1.498(9) . ? S50 C50 1.649(6) . ? C50 N50 1.162(8) . ? N50 Cu1 2.104(6) 2_545 ? Cl1 O13 1.427(7) . ? Cl1 O11 1.437(7) . ? Cl1 O14 1.437(6) . ? Cl1 O12 1.444(5) . ? N60 C60 1.146(10) . ? C60 C61 1.447(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Cu1 N1 93.1(2) . . y N6 Cu1 N4 150.4(2) . . y N1 Cu1 N4 79.7(2) . . y N6 Cu1 N5 79.6(2) . . y N1 Cu1 N5 153.0(2) . . y N4 Cu1 N5 93.8(2) . . y N6 Cu1 N50 107.1(2) . 2 y N1 Cu1 N50 103.7(2) . 2 y N4 Cu1 N50 102.6(2) . 2 y N5 Cu1 N50 103.3(2) . 2 y N7 Cu2 N2 92.6(2) . . y N7 Cu2 N10 155.8(2) . . y N2 Cu2 N10 80.7(2) . . y N7 Cu2 N9 80.2(2) . . y N2 Cu2 N9 155.9(2) . . y N10 Cu2 N9 96.4(2) . . y N7 Cu2 S50 91.13(15) . . y N2 Cu2 S50 102.70(15) . . y N10 Cu2 S50 113.04(15) . . y N9 Cu2 S50 100.43(15) . . y N2 N1 C5 106.1(5) . . ? N2 N1 Cu1 133.4(4) . . ? C5 N1 Cu1 115.1(4) . . ? N1 N2 C3 105.7(5) . . ? N1 N2 Cu2 133.4(4) . . ? C3 N2 Cu2 114.0(4) . . ? C5 N3 C3 100.6(5) . . ? C6 N4 C8 122.2(6) . . ? C6 N4 Cu1 116.4(4) . . ? C8 N4 Cu1 121.4(4) . . ? C12 N5 C10 121.9(6) . . ? C12 N5 Cu1 116.6(4) . . ? C10 N5 Cu1 121.5(4) . . ? N7 N6 C13 105.5(5) . . ? N7 N6 Cu1 132.7(4) . . ? C13 N6 Cu1 114.8(4) . . ? N6 N7 C15 106.5(5) . . ? N6 N7 Cu2 134.4(4) . . ? C15 N7 Cu2 113.6(4) . . ? C13 N8 C15 100.5(5) . . ? C16 N9 C18 122.4(6) . . ? C16 N9 Cu2 116.3(4) . . ? C18 N9 Cu2 121.0(4) . . ? C22 N10 C20 122.5(6) . . ? C22 N10 Cu2 115.7(5) . . ? C20 N10 Cu2 121.3(4) . . ? N2 C3 N3 114.0(6) . . ? N2 C3 C22 114.3(5) . . ? N3 C3 C22 130.4(6) . . ? N3 C5 N1 113.7(6) . . ? N3 C5 C6 130.5(6) . . ? N1 C5 C6 114.9(6) . . ? N4 C6 C5 112.5(6) . . ? N4 C6 C7 126.0(6) . . ? C5 C6 C7 121.5(6) . . ? N4 C8 C9 111.3(5) . . ? C8 C9 C10 116.8(6) . . ? N5 C10 C9 111.3(6) . . ? N5 C12 C13 112.8(6) . . ? N5 C12 C11 125.7(6) . . ? C13 C12 C11 121.4(6) . . ? N8 C13 N6 114.0(6) . . ? N8 C13 C12 130.5(6) . . ? N6 C13 C12 114.6(5) . . ? N7 C15 N8 113.4(5) . . ? N7 C15 C16 115.3(5) . . ? N8 C15 C16 130.9(6) . . ? N9 C16 C15 112.9(5) . . ? N9 C16 C17 127.6(6) . . ? C15 C16 C17 119.3(6) . . ? N9 C18 C19 111.1(5) . . ? C20 C19 C18 116.1(6) . . ? N10 C20 C19 111.9(5) . . ? N10 C22 C3 113.5(6) . . ? N10 C22 C21 127.7(6) . . ? C3 C22 C21 118.8(6) . . ? C50 S50 Cu2 115.4(2) . . ? N50 C50 S50 177.2(6) . . ? C50 N50 Cu1 174.6(5) . 2_545 ? O13 Cl1 O11 110.8(5) . . ? O13 Cl1 O14 107.0(5) . . ? O11 Cl1 O14 108.2(4) . . ? O13 Cl1 O12 111.0(4) . . ? O11 Cl1 O12 110.1(4) . . ? O14 Cl1 O12 109.6(4) . . ? N60 C60 C61 178.4(11) . . ? 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 N6 Cu1 N1 N2 5.5(5) . . . . ? N4 Cu1 N1 N2 156.6(6) . . . . ? N5 Cu1 N1 N2 78.6(7) . . . . ? N50 Cu1 N1 N2 -102.9(5) 2 . . . ? N6 Cu1 N1 C5 -144.2(4) . . . . ? N4 Cu1 N1 C5 6.8(4) . . . . ? N5 Cu1 N1 C5 -71.2(7) . . . . ? N50 Cu1 N1 C5 107.4(5) 2 . . . ? C5 N1 N2 C3 -0.3(6) . . . . ? Cu1 N1 N2 C3 -152.0(5) . . . . ? C5 N1 N2 Cu2 147.6(5) . . . . ? Cu1 N1 N2 Cu2 -4.0(8) . . . . ? N7 Cu2 N2 N1 -1.3(5) . . . . ? N10 Cu2 N2 N1 -157.8(6) . . . . ? N9 Cu2 N2 N1 -72.9(8) . . . . ? S50 Cu2 N2 N1 90.5(5) . . . . ? N7 Cu2 N2 C3 144.7(4) . . . . ? N10 Cu2 N2 C3 -11.8(4) . . . . ? N9 Cu2 N2 C3 73.1(7) . . . . ? S50 Cu2 N2 C3 -123.5(4) . . . . ? N6 Cu1 N4 C6 78.6(6) . . . . ? N1 Cu1 N4 C6 0.5(4) . . . . ? N5 Cu1 N4 C6 154.1(5) . . . . ? N50 Cu1 N4 C6 -101.4(5) 2 . . . ? N6 Cu1 N4 C8 -102.5(6) . . . . ? N1 Cu1 N4 C8 179.5(5) . . . . ? N5 Cu1 N4 C8 -27.0(5) . . . . ? N50 Cu1 N4 C8 77.6(5) 2 . . . ? N6 Cu1 N5 C12 4.2(5) . . . . ? N1 Cu1 N5 C12 -72.1(7) . . . . ? N4 Cu1 N5 C12 -146.7(5) . . . . ? N50 Cu1 N5 C12 109.4(5) 2 . . . ? N6 Cu1 N5 C10 -177.1(5) . . . . ? N1 Cu1 N5 C10 106.7(6) . . . . ? N4 Cu1 N5 C10 32.0(5) . . . . ? N50 Cu1 N5 C10 -71.8(5) 2 . . . ? N1 Cu1 N6 N7 -2.3(5) . . . . ? N4 Cu1 N6 N7 -76.9(7) . . . . ? N5 Cu1 N6 N7 -156.1(5) . . . . ? N50 Cu1 N6 N7 103.1(5) 2 . . . ? N1 Cu1 N6 C13 143.4(4) . . . . ? N4 Cu1 N6 C13 68.8(6) . . . . ? N5 Cu1 N6 C13 -10.4(4) . . . . ? N50 Cu1 N6 C13 -111.2(4) 2 . . . ? C13 N6 N7 C15 0.4(6) . . . . ? Cu1 N6 N7 C15 148.4(5) . . . . ? C13 N6 N7 Cu2 -150.7(5) . . . . ? Cu1 N6 N7 Cu2 -2.7(8) . . . . ? N2 Cu2 N7 N6 4.6(5) . . . . ? N10 Cu2 N7 N6 77.7(8) . . . . ? N9 Cu2 N7 N6 161.5(6) . . . . ? S50 Cu2 N7 N6 -98.1(5) . . . . ? N2 Cu2 N7 C15 -145.0(4) . . . . ? N10 Cu2 N7 C15 -71.9(7) . . . . ? N9 Cu2 N7 C15 11.8(4) . . . . ? S50 Cu2 N7 C15 112.2(4) . . . . ? N7 Cu2 N9 C16 -7.7(4) . . . . ? N2 Cu2 N9 C16 66.5(7) . . . . ? N10 Cu2 N9 C16 148.1(4) . . . . ? S50 Cu2 N9 C16 -97.0(4) . . . . ? N7 Cu2 N9 C18 178.9(5) . . . . ? N2 Cu2 N9 C18 -107.0(6) . . . . ? N10 Cu2 N9 C18 -25.4(5) . . . . ? S50 Cu2 N9 C18 89.5(4) . . . . ? N7 Cu2 N10 C22 -67.8(7) . . . . ? N2 Cu2 N10 C22 7.8(5) . . . . ? N9 Cu2 N10 C22 -148.0(5) . . . . ? S50 Cu2 N10 C22 107.7(4) . . . . ? N7 Cu2 N10 C20 104.3(6) . . . . ? N2 Cu2 N10 C20 179.9(5) . . . . ? N9 Cu2 N10 C20 24.1(5) . . . . ? S50 Cu2 N10 C20 -80.2(5) . . . . ? N1 N2 C3 N3 0.4(7) . . . . ? Cu2 N2 C3 N3 -154.6(4) . . . . ? N1 N2 C3 C22 168.9(5) . . . . ? Cu2 N2 C3 C22 13.8(6) . . . . ? C5 N3 C3 N2 -0.4(7) . . . . ? C5 N3 C3 C22 -166.5(6) . . . . ? C3 N3 C5 N1 0.1(7) . . . . ? C3 N3 C5 C6 168.4(6) . . . . ? N2 N1 C5 N3 0.1(7) . . . . ? Cu1 N1 C5 N3 157.7(4) . . . . ? N2 N1 C5 C6 -170.0(5) . . . . ? Cu1 N1 C5 C6 -12.4(7) . . . . ? C8 N4 C6 C5 174.2(5) . . . . ? Cu1 N4 C6 C5 -6.9(7) . . . . ? C8 N4 C6 C7 -2.9(10) . . . . ? Cu1 N4 C6 C7 176.1(5) . . . . ? N3 C5 C6 N4 -155.5(7) . . . . ? N1 C5 C6 N4 12.6(8) . . . . ? N3 C5 C6 C7 21.7(10) . . . . ? N1 C5 C6 C7 -170.2(6) . . . . ? C6 N4 C8 C9 164.6(6) . . . . ? Cu1 N4 C8 C9 -14.3(7) . . . . ? N4 C8 C9 C10 70.6(7) . . . . ? C12 N5 C10 C9 -176.7(6) . . . . ? Cu1 N5 C10 C9 4.6(7) . . . . ? C8 C9 C10 N5 -64.9(8) . . . . ? C10 N5 C12 C13 -176.3(5) . . . . ? Cu1 N5 C12 C13 2.4(7) . . . . ? C10 N5 C12 C11 -0.1(10) . . . . ? Cu1 N5 C12 C11 178.6(5) . . . . ? C15 N8 C13 N6 1.7(7) . . . . ? C15 N8 C13 C12 -167.2(6) . . . . ? N7 N6 C13 N8 -1.4(7) . . . . ? Cu1 N6 C13 N8 -156.0(4) . . . . ? N7 N6 C13 C12 169.3(5) . . . . ? Cu1 N6 C13 C12 14.8(7) . . . . ? N5 C12 C13 N8 157.7(6) . . . . ? C11 C12 C13 N8 -18.7(10) . . . . ? N5 C12 C13 N6 -11.2(8) . . . . ? C11 C12 C13 N6 172.4(6) . . . . ? N6 N7 C15 N8 0.6(7) . . . . ? Cu2 N7 C15 N8 158.5(4) . . . . ? N6 N7 C15 C16 -172.2(5) . . . . ? Cu2 N7 C15 C16 -14.4(6) . . . . ? C13 N8 C15 N7 -1.4(7) . . . . ? C13 N8 C15 C16 170.1(6) . . . . ? C18 N9 C16 C15 175.5(5) . . . . ? Cu2 N9 C16 C15 2.1(7) . . . . ? C18 N9 C16 C17 -1.0(10) . . . . ? Cu2 N9 C16 C17 -174.3(5) . . . . ? N7 C15 C16 N9 8.1(8) . . . . ? N8 C15 C16 N9 -163.3(6) . . . . ? N7 C15 C16 C17 -175.2(5) . . . . ? N8 C15 C16 C17 13.5(10) . . . . ? C16 N9 C18 C19 174.9(6) . . . . ? Cu2 N9 C18 C19 -12.0(7) . . . . ? N9 C18 C19 C20 67.6(7) . . . . ? C22 N10 C20 C19 -173.4(6) . . . . ? Cu2 N10 C20 C19 15.0(8) . . . . ? C18 C19 C20 N10 -69.8(8) . . . . ? C20 N10 C22 C3 -174.6(6) . . . . ? Cu2 N10 C22 C3 -2.6(7) . . . . ? C20 N10 C22 C21 3.2(10) . . . . ? Cu2 N10 C22 C21 175.2(5) . . . . ? N2 C3 C22 N10 -7.4(8) . . . . ? N3 C3 C22 N10 158.6(6) . . . . ? N2 C3 C22 C21 174.6(6) . . . . ? N3 C3 C22 C21 -19.3(10) . . . . ? N7 Cu2 S50 C50 -177.7(3) . . . . ? N2 Cu2 S50 C50 89.4(3) . . . . ? N10 Cu2 S50 C50 4.2(3) . . . . ? N9 Cu2 S50 C50 -97.5(3) . . . . ? Cu2 S50 C50 N50 163(13) . . . . ? S50 C50 N50 Cu1 -25(18) . . . 2_545 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.524 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.110