data_global _journal_coden_Cambridge 188 _publ_requested_journal 'Perkin Transactions 2' loop_ _publ_author_name 'Ito, Tasuku' 'Oshio, Hiroki' 'Yoshida, Noboru' _publ_contact_author_name 'Prof Noboru Yoshida' _publ_contact_author_address ; Prof Noboru Yoshida Laboratory of Molecular Functional Chemistry Hokkaido University Divison of Material Science Graduate School of Environmental Ea Sapporo 060-0810 JAPAN ; _publ_contact_author_email 'NYOSHIDA@EES.HOKUDAI.AC.JP' data_2_E2CHCl3_EEt2O _database_code_CSD 163701 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common L56-Cu(II) complex _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C145 H65 Cl3 Cu4 N4 O18S4' _chemical_formula_weight 1637.284 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 12.6528(10) _cell_length_b 20.1218(15) _cell_length_c 30.263(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.8150(10) _cell_angle_gamma 90.00 _cell_volume 7567.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour Dark brown _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7608 _exptl_absorpt_coefficient_mu 0.837 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 52032 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 26.85 _reflns_number_total 14946 _reflns_number_gt 10867 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.1031P)^2^+0.1563P] 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 14946 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1560 _refine_ls_wR_factor_gt 0.1410 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.467 _refine_ls_shift/su_mean 0.018 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 1.37675(3) 0.329122(19) 0.817065(11) 0.03259(11) Uani 1 1 d . . . Cu2 Cu 0.44526(3) 0.362469(18) 0.363590(11) 0.03044(11) Uani 1 1 d . . . O1 O 1.52496(16) 0.33263(11) 0.84404(7) 0.0385(5) Uani 1 1 d . . . O2 O 1.0890(2) 0.13682(12) 0.64932(9) 0.0661(8) Uani 1 1 d . . . O3 O 0.70933(18) 0.21938(15) 0.54316(8) 0.0588(7) Uani 1 1 d . . . O4 O 0.44431(16) 0.38334(12) 0.30249(7) 0.0397(5) Uani 1 1 d . . . O8 O 0.29370(16) 0.34828(12) 0.34968(7) 0.0390(5) Uani 1 1 d . . . O5 O 1.34822(16) 0.33418(11) 0.87654(7) 0.0387(5) Uani 1 1 d . . . O6 O 1.16950(17) 0.42655(12) 0.60706(7) 0.0436(5) Uani 1 1 d . . . O7 O 0.78610(16) 0.53333(10) 0.51706(7) 0.0405(5) Uani 1 1 d . . . N1 N 1.40595(18) 0.27981(12) 0.76475(8) 0.0315(5) Uani 1 1 d . . . N2 N 0.59616(19) 0.33449(12) 0.37368(8) 0.0292(5) Uani 1 1 d . . . N3 N 1.24500(19) 0.37763(12) 0.79202(8) 0.0326(5) Uani 1 1 d . . . N4 N 0.43772(18) 0.38631(11) 0.42570(7) 0.0286(5) Uani 1 1 d . . . C1 C 1.6083(2) 0.31987(14) 0.82626(11) 0.0344(7) Uani 1 1 d . . . C2 C 1.7124(2) 0.33097(15) 0.85358(11) 0.0397(7) Uani 1 1 d . . . H2 H 1.7173 0.3458 0.8830 0.048 Uiso 1 1 calc R . . C3 C 1.8035(2) 0.32028(15) 0.83730(13) 0.0439(8) Uani 1 1 d . . . H3 H 1.8696 0.3285 0.8559 0.053 Uiso 1 1 calc R . . C4 C 1.8020(3) 0.29703(15) 0.79302(12) 0.0415(8) Uani 1 1 d . . . C5 C 1.8983(3) 0.28774(17) 0.77630(15) 0.0534(10) Uani 1 1 d . . . H5 H 1.9641 0.2974 0.7946 0.064 Uiso 1 1 calc R . . C6 C 1.8953(3) 0.2647(2) 0.73348(16) 0.0614(11) Uani 1 1 d . . . H6 H 1.9590 0.2582 0.7229 0.074 Uiso 1 1 calc R . . C7 C 1.7967(3) 0.2508(2) 0.70575(14) 0.0587(10) Uani 1 1 d . . . H7 H 1.7951 0.2349 0.6768 0.070 Uiso 1 1 calc R . . C8 C 1.7023(3) 0.26042(18) 0.72071(13) 0.0493(9) Uani 1 1 d . . . H8 H 1.6374 0.2518 0.7014 0.059 Uiso 1 1 calc R . . C9 C 1.7010(2) 0.28314(15) 0.76491(11) 0.0385(7) Uani 1 1 d . . . C10 C 1.6027(2) 0.29358(14) 0.78255(10) 0.0327(6) Uani 1 1 d . . . C11 C 1.5031(2) 0.27104(14) 0.75676(10) 0.0333(6) Uani 1 1 d . . . H11 H 1.5078 0.2470 0.7309 0.040 Uiso 1 1 calc R . . C12 C 1.3203(2) 0.24811(15) 0.73391(10) 0.0332(6) Uani 1 1 d . . . C13 C 1.3163(3) 0.24926(19) 0.68754(11) 0.0466(8) Uani 1 1 d . . . H13 H 1.3665 0.2738 0.6756 0.056 Uiso 1 1 calc R . . C14 C 1.2370(3) 0.2135(2) 0.65924(11) 0.0552(10) Uani 1 1 d . . . H14 H 1.2351 0.2133 0.6284 0.066 Uiso 1 1 calc R . . C15 C 1.1608(3) 0.17830(17) 0.67696(12) 0.0460(8) Uani 1 1 d . . . C16 C 1.1627(3) 0.17863(18) 0.72224(12) 0.0486(9) Uani 1 1 d . . . H16 H 1.1107 0.1553 0.7339 0.058 Uiso 1 1 calc R . . C17 C 1.2421(2) 0.21367(17) 0.75101(10) 0.0396(7) Uani 1 1 d . . . H17 H 1.2426 0.2140 0.7818 0.047 Uiso 1 1 calc R . . C18 C 1.0001(3) 0.16353(17) 0.62138(11) 0.0457(8) Uani 1 1 d . . . C19 C 0.9366(3) 0.1180(2) 0.59428(14) 0.0662(12) Uani 1 1 d . . . H19 H 0.9573 0.0737 0.5946 0.079 Uiso 1 1 calc R . . C20 C 0.8427(3) 0.1382(2) 0.56670(13) 0.0619(11) Uani 1 1 d . . . H20 H 0.8003 0.1076 0.5483 0.074 Uiso 1 1 calc R . . C21 C 0.8122(3) 0.20359(19) 0.56660(10) 0.0437(8) Uani 1 1 d . . . C22 C 0.8759(3) 0.24909(17) 0.59289(11) 0.0443(8) Uani 1 1 d . . . H22 H 0.8554 0.2935 0.5923 0.053 Uiso 1 1 calc R . . C23 C 0.9708(3) 0.22902(16) 0.62036(10) 0.0411(7) Uani 1 1 d . . . H23 H 1.0144 0.2599 0.6380 0.049 Uiso 1 1 calc R . . C24 C 0.6938(2) 0.24409(17) 0.50005(10) 0.0375(7) Uani 1 1 d . . . C25 C 0.5952(2) 0.22907(15) 0.47331(10) 0.0353(7) Uani 1 1 d . . . H25 H 0.5485 0.1999 0.4838 0.042 Uiso 1 1 calc R . . C26 C 0.5658(2) 0.25711(14) 0.43121(10) 0.0320(6) Uani 1 1 d . . . H26 H 0.4996 0.2469 0.4135 0.038 Uiso 1 1 calc R . . C27 C 0.6357(2) 0.30090(14) 0.41528(9) 0.0287(6) Uani 1 1 d . . . C28 C 0.7360(2) 0.31427(15) 0.44165(10) 0.0327(6) Uani 1 1 d . . . H28 H 0.7834 0.3425 0.4308 0.039 Uiso 1 1 calc R . . C29 C 0.7658(2) 0.28584(16) 0.48388(10) 0.0371(7) Uani 1 1 d . . . H29 H 0.8331 0.2946 0.5013 0.044 Uiso 1 1 calc R . . C30 C 0.6609(2) 0.34625(14) 0.34584(9) 0.0305(6) Uani 1 1 d . . . H30 H 0.7314 0.3315 0.3546 0.037 Uiso 1 1 calc R . . C31 C 0.6356(2) 0.37925(14) 0.30344(9) 0.0309(6) Uani 1 1 d . . . C32 C 0.7216(2) 0.39408(14) 0.27894(10) 0.0331(6) Uani 1 1 d . . . C33 C 0.8317(3) 0.38722(16) 0.29722(11) 0.0414(7) Uani 1 1 d . . . H33 H 0.8520 0.3718 0.3266 0.050 Uiso 1 1 calc R . . C34 C 0.9103(3) 0.40256(19) 0.27316(13) 0.0523(9) Uani 1 1 d . . . H34 H 0.9823 0.3975 0.2865 0.063 Uiso 1 1 calc R . . C35 C 0.8834(3) 0.42565(19) 0.22900(13) 0.0535(9) Uani 1 1 d . . . H35 H 0.9368 0.4356 0.2127 0.064 Uiso 1 1 calc R . . C36 C 0.7767(3) 0.43341(17) 0.20997(12) 0.0478(8) Uani 1 1 d . . . H36 H 0.7581 0.4486 0.1805 0.057 Uiso 1 1 calc R . . C37 C 0.6946(3) 0.41865(15) 0.23437(10) 0.0394(7) Uani 1 1 d . . . C38 C 0.5849(3) 0.42797(18) 0.21464(11) 0.0470(8) Uani 1 1 d . . . H38 H 0.5673 0.4425 0.1850 0.056 Uiso 1 1 calc R . . C39 C 0.5051(3) 0.41630(19) 0.23777(11) 0.0482(8) Uani 1 1 d . . . H39 H 0.4342 0.4239 0.2239 0.058 Uiso 1 1 calc R . . C40 C 0.5275(2) 0.39251(15) 0.28319(9) 0.0343(6) Uani 1 1 d . . . C41 C 1.2664(2) 0.35958(15) 0.89065(10) 0.0340(6) Uani 1 1 d . . . C42 C 1.2691(3) 0.35830(17) 0.93819(11) 0.0412(7) Uani 1 1 d . . . H42 H 1.3279 0.3392 0.9569 0.049 Uiso 1 1 calc R . . C43 C 1.1894(3) 0.38377(17) 0.95651(11) 0.0456(8) Uani 1 1 d . . . H43 H 1.1951 0.3827 0.9876 0.055 Uiso 1 1 calc R . . C44 C 1.0955(3) 0.41264(16) 0.92930(12) 0.0418(7) Uani 1 1 d . . . C45 C 1.0095(3) 0.43597(18) 0.94910(13) 0.0529(9) Uani 1 1 d . . . H45 H 1.0148 0.4330 0.9801 0.064 Uiso 1 1 calc R . . C46 C 0.9189(3) 0.46276(18) 0.92351(15) 0.0558(10) Uani 1 1 d . . . H46 H 0.8625 0.4772 0.9368 0.067 Uiso 1 1 calc R . . C47 C 0.9124(3) 0.46801(17) 0.87738(14) 0.0510(9) Uani 1 1 d . . . H47 H 0.8517 0.4870 0.8599 0.061 Uiso 1 1 calc R . . C48 C 0.9946(2) 0.44552(16) 0.85691(12) 0.0424(8) Uani 1 1 d . . . H48 H 0.9878 0.4494 0.8259 0.051 Uiso 1 1 calc R . . C49 C 1.0891(2) 0.41657(14) 0.88236(10) 0.0340(6) Uani 1 1 d . . . C50 C 1.1770(2) 0.39042(15) 0.86234(10) 0.0328(6) Uani 1 1 d . . . C51 C 1.1746(2) 0.39832(14) 0.81554(10) 0.0328(6) Uani 1 1 d . . . H51 H 1.1155 0.4210 0.7996 0.039 Uiso 1 1 calc R . . C52 C 1.2226(2) 0.39240(14) 0.74484(10) 0.0315(6) Uani 1 1 d . . . C53 C 1.1210(2) 0.38133(15) 0.71890(10) 0.0363(7) Uani 1 1 d . . . H53 H 1.0661 0.3654 0.7326 0.044 Uiso 1 1 calc R . . C54 C 1.1006(2) 0.39360(16) 0.67347(10) 0.0369(7) Uani 1 1 d . . . H54 H 1.0325 0.3862 0.6564 0.044 Uiso 1 1 calc R . . C55 C 1.1832(2) 0.41728(15) 0.65330(10) 0.0347(7) Uani 1 1 d . . . C56 C 1.2847(2) 0.42974(15) 0.67843(10) 0.0364(7) Uani 1 1 d . . . H56 H 1.3391 0.4466 0.6648 0.044 Uiso 1 1 calc R . . C57 C 1.3038(2) 0.41670(15) 0.72419(10) 0.0346(6) Uani 1 1 d . . . H57 H 1.3718 0.4243 0.7413 0.042 Uiso 1 1 calc R . . C58 C 1.0698(2) 0.45213(15) 0.58531(10) 0.0344(6) Uani 1 1 d . . . C59 C 1.0173(3) 0.42053(16) 0.54751(10) 0.0395(7) Uani 1 1 d . . . H59 H 1.0459 0.3821 0.5374 0.047 Uiso 1 1 calc R . . C60 C 0.9209(3) 0.44636(15) 0.52423(11) 0.0397(7) Uani 1 1 d . . . H60 H 0.8852 0.4257 0.4982 0.048 Uiso 1 1 calc R . . C61 C 0.8785(2) 0.50280(14) 0.54002(10) 0.0316(6) Uani 1 1 d . . . C62 C 0.9317(3) 0.53437(16) 0.57811(11) 0.0412(7) Uani 1 1 d . . . H62 H 0.9029 0.5726 0.5885 0.049 Uiso 1 1 calc R . . C63 C 1.0282(3) 0.50891(16) 0.60090(11) 0.0436(8) Uani 1 1 d . . . H63 H 1.0648 0.5300 0.6266 0.052 Uiso 1 1 calc R . . C64 C 0.7016(2) 0.49371(14) 0.49557(10) 0.0326(6) Uani 1 1 d . . . C65 C 0.6566(2) 0.44552(15) 0.51819(9) 0.0337(6) Uani 1 1 d . . . H65 H 0.6847 0.4370 0.5483 0.040 Uiso 1 1 calc R . . C66 C 0.5689(2) 0.40947(15) 0.49594(9) 0.0321(6) Uani 1 1 d . . . H66 H 0.5391 0.3761 0.5110 0.039 Uiso 1 1 calc R . . C67 C 0.5252(2) 0.42329(14) 0.45095(9) 0.0286(6) Uani 1 1 d . . . C68 C 0.5723(2) 0.47257(15) 0.42899(10) 0.0342(6) Uani 1 1 d . . . H68 H 0.5440 0.4821 0.3990 0.041 Uiso 1 1 calc R . . C69 C 0.6608(2) 0.50783(15) 0.45095(10) 0.0367(7) Uani 1 1 d . . . H69 H 0.6922 0.5405 0.4359 0.044 Uiso 1 1 calc R . . C70 C 0.3605(2) 0.36632(13) 0.44576(9) 0.0283(6) Uani 1 1 d . . . H70 H 0.3678 0.3762 0.4762 0.034 Uiso 1 1 calc R . . C71 C 0.2661(2) 0.33088(14) 0.42554(10) 0.0300(6) Uani 1 1 d . . . C72 C 0.1967(2) 0.30359(14) 0.45380(10) 0.0332(6) Uani 1 1 d . . . C73 C 0.2269(3) 0.29766(16) 0.50090(11) 0.0396(7) Uani 1 1 d . . . H73 H 0.2941 0.3131 0.5151 0.048 Uiso 1 1 calc R . . C74 C 0.1595(3) 0.26960(17) 0.52638(12) 0.0477(8) Uani 1 1 d . . . H74 H 0.1811 0.2669 0.5574 0.057 Uiso 1 1 calc R . . C75 C 0.0582(3) 0.24495(17) 0.50598(13) 0.0512(9) Uani 1 1 d . . . H75 H 0.0136 0.2254 0.5234 0.061 Uiso 1 1 calc R . . C76 C 0.0259(3) 0.24971(17) 0.46101(13) 0.0478(8) Uani 1 1 d . . . H76 H -0.0415 0.2337 0.4478 0.057 Uiso 1 1 calc R . . C77 C 0.0932(2) 0.27882(15) 0.43338(11) 0.0374(7) Uani 1 1 d . . . C78 C 0.0616(3) 0.28239(17) 0.38591(12) 0.0430(8) Uani 1 1 d . . . H78 H -0.0071 0.2685 0.3726 0.052 Uiso 1 1 calc R . . C79 C 0.1281(2) 0.30515(16) 0.35983(11) 0.0392(7) Uani 1 1 d . . . H79 H 0.1045 0.3059 0.3288 0.047 Uiso 1 1 calc R . . C80 C 0.2346(2) 0.32846(15) 0.37806(10) 0.0331(6) Uani 1 1 d . . . Cl1S Cl 0.58382(9) 0.49980(5) 0.09171(4) 0.0679(3) Uani 1 1 d . . . Cl2S Cl 0.38369(9) 0.50473(7) 0.12392(4) 0.0808(4) Uani 1 1 d . . . Cl3S Cl 0.39035(14) 0.54777(7) 0.03388(4) 0.1007(5) Uani 1 1 d . . . Cl4S Cl 0.3525(9) 0.5549(3) 0.2748(4) 0.100(2) Uani 0.33 1 d P . . Cl5S Cl 0.1284(7) 0.4986(5) 0.2878(5) 0.131(4) Uani 0.33 1 d P . . Cl6S Cl 0.2613(15) 0.5191(4) 0.3506(3) 0.151(6) Uani 0.33 1 d P . . Cl7S Cl 0.3834(6) 0.5477(4) 0.3049(5) 0.123(3) Uani 0.33 1 d P . . Cl8S Cl 0.1817(8) 0.5093(4) 0.3282(5) 0.133(3) Uani 0.33 1 d P . . Cl9S Cl 0.2096(10) 0.5138(8) 0.2405(3) 0.161(5) Uani 0.33 1 d P . . Cl10 Cl 0.2877(16) 0.5353(5) 0.2432(5) 0.175(5) Uani 0.33 1 d P . . Cl11 Cl 0.1535(13) 0.4996(6) 0.2561(9) 0.245(13) Uani 0.33 1 d P . . Cl12 Cl 0.3356(18) 0.5320(8) 0.3397(7) 0.278(11) Uani 0.33 1 d P . . O1S O 0.4772(4) 0.23811(18) 0.61845(13) 0.1031(12) Uani 1 1 d . . . C1S C 0.4624(3) 0.5448(2) 0.08925(13) 0.0609(10) Uani 1 1 d . . . C2S C 0.2688(4) 0.4974(2) 0.29386(17) 0.0737(13) Uani 1 1 d . . . C3S C 0.5089(9) 0.1736(3) 0.6105(5) 0.241(7) Uani 1 1 d . . . C4S C 0.4056(3) 0.1643(3) 0.55838(14) 0.0709(13) Uani 1 1 d . . . C5S C 0.5109(5) 0.2930(2) 0.59665(14) 0.0864(17) Uani 1 1 d . . . C6S C 0.4865(7) 0.3522(3) 0.6123(2) 0.120(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02668(19) 0.0422(2) 0.02803(19) 0.00234(15) 0.00295(14) 0.00574(15) Cu2 0.02825(19) 0.0375(2) 0.02383(18) -0.00017(14) 0.00037(13) -0.00010(14) O1 0.0267(10) 0.0539(14) 0.0337(11) -0.0024(10) 0.0025(8) 0.0047(9) O2 0.0652(17) 0.0425(14) 0.0703(17) -0.0098(13) -0.0391(14) 0.0140(12) O3 0.0343(12) 0.101(2) 0.0404(13) 0.0349(14) 0.0066(10) 0.0130(13) O4 0.0351(11) 0.0540(14) 0.0280(11) 0.0064(9) 0.0007(9) -0.0016(10) O8 0.0300(11) 0.0557(14) 0.0294(11) -0.0022(9) 0.0003(8) -0.0050(10) O5 0.0340(11) 0.0531(13) 0.0294(11) 0.0057(10) 0.0075(9) 0.0084(10) O6 0.0377(12) 0.0614(15) 0.0308(11) 0.0099(10) 0.0039(9) 0.0152(11) O7 0.0322(11) 0.0272(11) 0.0544(14) -0.0046(10) -0.0120(10) 0.0019(9) N1 0.0290(12) 0.0369(14) 0.0289(12) 0.0062(10) 0.0059(10) 0.0028(10) N2 0.0327(13) 0.0282(12) 0.0249(12) 0.0005(9) 0.0006(9) 0.0027(10) N3 0.0289(12) 0.0369(14) 0.0314(13) 0.0057(10) 0.0040(10) 0.0038(10) N4 0.0287(12) 0.0286(12) 0.0270(12) -0.0010(10) 0.0015(9) 0.0007(10) C1 0.0269(14) 0.0293(15) 0.0466(18) 0.0068(13) 0.0060(13) 0.0043(11) C2 0.0333(16) 0.0351(17) 0.0484(19) -0.0008(14) 0.0020(14) 0.0013(13) C3 0.0283(16) 0.0287(16) 0.072(2) 0.0059(15) 0.0030(15) 0.0002(12) C4 0.0361(17) 0.0242(15) 0.067(2) 0.0116(15) 0.0182(15) 0.0035(12) C5 0.0357(18) 0.0386(19) 0.090(3) 0.0156(19) 0.0232(18) 0.0064(15) C6 0.050(2) 0.053(2) 0.092(3) 0.010(2) 0.041(2) 0.0091(18) C7 0.056(2) 0.058(2) 0.071(3) 0.006(2) 0.035(2) 0.0042(19) C8 0.0447(19) 0.050(2) 0.059(2) 0.0075(17) 0.0247(17) 0.0044(16) C9 0.0359(16) 0.0267(15) 0.055(2) 0.0119(14) 0.0149(14) 0.0050(12) C10 0.0291(14) 0.0281(15) 0.0413(17) 0.0070(12) 0.0076(12) 0.0026(11) C11 0.0379(16) 0.0297(15) 0.0338(16) 0.0073(12) 0.0109(12) 0.0041(12) C12 0.0316(15) 0.0366(16) 0.0292(15) 0.0033(12) 0.0003(12) 0.0080(12) C13 0.0481(19) 0.060(2) 0.0321(17) 0.0058(15) 0.0083(14) 0.0016(16) C14 0.064(2) 0.069(3) 0.0280(17) 0.0001(16) -0.0039(16) 0.014(2) C15 0.0426(18) 0.0443(19) 0.0433(19) -0.0024(15) -0.0125(15) 0.0093(15) C16 0.0368(18) 0.051(2) 0.052(2) 0.0097(16) -0.0059(15) -0.0035(15) C17 0.0375(17) 0.052(2) 0.0268(15) 0.0086(14) 0.0002(12) 0.0006(14) C18 0.0483(19) 0.0428(19) 0.0387(18) -0.0015(14) -0.0104(14) 0.0120(15) C19 0.066(3) 0.042(2) 0.075(3) -0.0093(19) -0.029(2) 0.0103(18) C20 0.058(2) 0.061(3) 0.055(2) -0.0025(19) -0.0214(18) 0.0001(19) C21 0.0364(17) 0.064(2) 0.0295(16) 0.0179(15) 0.0032(13) 0.0126(16) C22 0.0464(19) 0.0438(19) 0.0430(19) 0.0093(15) 0.0092(15) 0.0163(15) C23 0.0479(19) 0.0378(17) 0.0341(16) -0.0038(13) -0.0013(14) 0.0066(14) C24 0.0346(16) 0.0488(19) 0.0288(15) 0.0086(13) 0.0052(12) 0.0121(14) C25 0.0367(16) 0.0344(16) 0.0356(16) 0.0045(13) 0.0085(13) 0.0000(13) C26 0.0331(15) 0.0311(15) 0.0315(15) -0.0016(12) 0.0054(12) 0.0029(12) C27 0.0325(15) 0.0283(14) 0.0249(14) -0.0008(11) 0.0044(11) 0.0043(11) C28 0.0322(15) 0.0349(16) 0.0313(15) 0.0017(12) 0.0065(12) 0.0028(12) C29 0.0251(14) 0.0503(19) 0.0339(16) 0.0032(14) 0.0007(12) 0.0042(13) C30 0.0325(15) 0.0290(15) 0.0292(15) -0.0050(11) 0.0040(12) 0.0024(11) C31 0.0411(16) 0.0246(14) 0.0273(14) -0.0027(11) 0.0067(12) -0.0004(12) C32 0.0466(17) 0.0212(14) 0.0334(15) -0.0027(12) 0.0120(13) 0.0021(12) C33 0.0454(18) 0.0395(18) 0.0404(18) 0.0061(14) 0.0108(14) 0.0055(14) C34 0.049(2) 0.053(2) 0.059(2) 0.0109(18) 0.0208(17) 0.0088(17) C35 0.059(2) 0.050(2) 0.058(2) 0.0145(17) 0.0309(19) 0.0049(18) C36 0.064(2) 0.0405(19) 0.0433(19) 0.0096(15) 0.0208(17) 0.0036(16) C37 0.056(2) 0.0288(16) 0.0358(16) 0.0014(13) 0.0148(14) 0.0031(14) C38 0.058(2) 0.054(2) 0.0274(16) 0.0102(14) 0.0060(15) -0.0003(17) C39 0.0468(19) 0.060(2) 0.0351(17) 0.0086(16) 0.0002(14) -0.0005(16) C40 0.0404(17) 0.0347(16) 0.0269(14) -0.0011(12) 0.0039(12) -0.0034(13) C41 0.0332(15) 0.0364(16) 0.0336(16) 0.0017(13) 0.0094(12) -0.0022(12) C42 0.0424(18) 0.0449(19) 0.0369(17) 0.0059(14) 0.0092(14) 0.0000(14) C43 0.057(2) 0.0454(19) 0.0383(18) 0.0027(15) 0.0199(15) -0.0011(16) C44 0.0455(18) 0.0328(16) 0.052(2) -0.0022(14) 0.0219(15) -0.0040(14) C45 0.061(2) 0.048(2) 0.058(2) -0.0027(17) 0.0311(19) -0.0043(18) C46 0.047(2) 0.044(2) 0.085(3) -0.0111(19) 0.035(2) -0.0009(16) C47 0.0354(18) 0.0399(19) 0.080(3) -0.0131(18) 0.0157(17) -0.0005(14) C48 0.0341(17) 0.0366(17) 0.058(2) -0.0089(15) 0.0115(15) -0.0028(13) C49 0.0313(15) 0.0261(15) 0.0461(17) -0.0033(13) 0.0112(13) -0.0061(12) C50 0.0313(15) 0.0317(15) 0.0359(16) 0.0008(12) 0.0079(12) -0.0026(12) C51 0.0283(14) 0.0315(15) 0.0377(16) 0.0032(12) 0.0035(12) 0.0029(12) C52 0.0305(15) 0.0313(15) 0.0320(15) 0.0050(12) 0.0040(12) 0.0055(12) C53 0.0312(15) 0.0378(17) 0.0401(17) 0.0079(13) 0.0076(13) 0.0025(13) C54 0.0287(15) 0.0399(17) 0.0393(17) 0.0032(13) -0.0007(12) 0.0052(13) C55 0.0359(16) 0.0334(16) 0.0332(15) 0.0064(12) 0.0028(12) 0.0088(12) C56 0.0341(16) 0.0352(16) 0.0406(17) 0.0069(13) 0.0085(13) 0.0055(13) C57 0.0274(15) 0.0362(16) 0.0390(16) 0.0016(13) 0.0028(12) 0.0018(12) C58 0.0319(15) 0.0399(17) 0.0309(15) 0.0070(13) 0.0045(12) 0.0064(13) C59 0.0424(17) 0.0349(17) 0.0406(17) -0.0055(14) 0.0062(14) 0.0086(14) C60 0.0402(17) 0.0344(17) 0.0412(17) -0.0090(13) -0.0011(13) 0.0029(13) C61 0.0304(15) 0.0264(14) 0.0355(15) 0.0026(12) -0.0001(12) -0.0009(11) C62 0.0446(18) 0.0330(16) 0.0421(18) -0.0067(14) -0.0019(14) 0.0076(14) C63 0.0486(19) 0.0413(18) 0.0342(16) -0.0057(14) -0.0094(14) 0.0026(15) C64 0.0280(14) 0.0277(15) 0.0391(16) -0.0073(12) -0.0014(12) 0.0032(11) C65 0.0341(15) 0.0379(17) 0.0256(14) -0.0025(12) -0.0031(12) 0.0041(13) C66 0.0324(15) 0.0334(16) 0.0297(15) -0.0003(12) 0.0036(11) 0.0007(12) C67 0.0275(14) 0.0310(15) 0.0258(13) -0.0038(11) 0.0014(11) 0.0029(11) C68 0.0348(15) 0.0379(17) 0.0277(15) 0.0021(12) 0.0001(12) -0.0004(13) C69 0.0322(16) 0.0359(17) 0.0412(17) 0.0013(13) 0.0049(13) -0.0021(13) C70 0.0299(14) 0.0288(14) 0.0256(14) -0.0010(11) 0.0036(11) 0.0056(11) C71 0.0280(14) 0.0257(14) 0.0350(15) -0.0011(12) 0.0027(11) 0.0035(11) C72 0.0344(16) 0.0239(14) 0.0426(17) -0.0016(12) 0.0108(13) 0.0043(12) C73 0.0385(17) 0.0362(17) 0.0450(18) 0.0046(14) 0.0097(14) 0.0029(13) C74 0.053(2) 0.0437(19) 0.050(2) 0.0103(16) 0.0199(17) 0.0079(16) C75 0.050(2) 0.043(2) 0.070(3) 0.0089(18) 0.0339(19) 0.0071(16) C76 0.0389(18) 0.0395(19) 0.070(2) -0.0053(17) 0.0232(17) -0.0028(14) C77 0.0322(16) 0.0304(16) 0.0509(19) -0.0030(13) 0.0112(14) 0.0022(12) C78 0.0302(16) 0.0458(19) 0.052(2) -0.0156(15) 0.0054(14) -0.0039(14) C79 0.0311(16) 0.0475(19) 0.0371(17) -0.0113(14) 0.0011(13) -0.0010(13) C80 0.0293(15) 0.0339(16) 0.0346(16) -0.0034(12) 0.0018(12) 0.0004(12) Cl1S 0.0630(6) 0.0648(6) 0.0799(7) 0.0073(5) 0.0236(5) -0.0055(5) Cl2S 0.0644(7) 0.0869(8) 0.0964(9) 0.0205(7) 0.0284(6) 0.0235(6) Cl3S 0.1416(13) 0.0755(8) 0.0667(7) 0.0113(6) -0.0276(8) 0.0039(8) Cl4S 0.141(6) 0.057(3) 0.112(5) 0.007(4) 0.050(4) -0.019(4) Cl5S 0.067(4) 0.113(5) 0.212(12) 0.010(7) 0.024(7) 0.006(3) Cl6S 0.301(17) 0.083(4) 0.093(5) -0.006(4) 0.096(9) -0.012(7) Cl7S 0.093(4) 0.093(4) 0.170(9) 0.018(6) -0.013(6) -0.002(3) Cl8S 0.114(5) 0.125(5) 0.173(9) -0.025(5) 0.059(5) 0.020(4) Cl9S 0.127(9) 0.206(13) 0.126(5) 0.086(7) -0.037(6) 0.010(7) Cl10 0.253(14) 0.097(6) 0.206(12) 0.082(7) 0.118(12) 0.062(7) Cl11 0.136(13) 0.128(7) 0.39(3) 0.109(14) -0.168(15) -0.041(9) Cl12 0.292(17) 0.179(13) 0.256(16) -0.128(12) -0.224(14) 0.130(12) O1S 0.141(3) 0.074(2) 0.107(3) 0.011(2) 0.055(3) 0.005(2) C1S 0.068(3) 0.057(2) 0.055(2) 0.0106(19) 0.0045(19) 0.011(2) C2S 0.062(3) 0.067(3) 0.085(3) 0.020(2) -0.003(2) 0.005(2) C3S 0.307(13) 0.028(3) 0.482(18) 0.051(6) 0.314(14) 0.058(5) C4S 0.052(2) 0.113(4) 0.043(2) -0.023(2) -0.0032(18) -0.011(2) C5S 0.181(6) 0.044(2) 0.045(2) 0.0084(18) 0.047(3) -0.032(3) C6S 0.179(7) 0.085(4) 0.101(5) 0.014(4) 0.041(5) 0.003(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 Cu1 O1 1.901(2) . ? Cu1 O5 1.904(2) . ? Cu1 N3 1.957(2) . ? Cu1 N1 1.961(2) . ? Cu2 O4 1.894(2) . ? Cu2 O8 1.906(2) . ? Cu2 N2 1.959(2) . ? Cu2 N4 1.960(2) . ? O1 C1 1.296(4) . ? O2 C18 1.383(4) . ? O2 C15 1.392(4) . ? O3 C24 1.376(4) . ? O3 C21 1.397(4) . ? O4 C40 1.309(4) . ? O8 C80 1.303(4) . ? O5 C41 1.297(4) . ? O6 C55 1.390(3) . ? O6 C58 1.407(3) . ? O7 C61 1.387(3) . ? O7 C64 1.393(3) . ? N1 C11 1.308(4) . ? N1 C12 1.440(4) . ? N2 C30 1.302(4) . ? N2 C27 1.434(3) . ? N3 C51 1.309(4) . ? N3 C52 1.434(4) . ? N4 C70 1.307(4) . ? N4 C67 1.430(3) . ? C1 C10 1.414(4) . ? C1 C2 1.435(4) . ? C2 C3 1.354(5) . ? C3 C4 1.416(5) . ? C4 C5 1.416(5) . ? C4 C9 1.424(5) . ? C5 C6 1.370(6) . ? C6 C7 1.395(6) . ? C7 C8 1.369(5) . ? C8 C9 1.417(5) . ? C9 C10 1.458(4) . ? C10 C11 1.426(4) . ? C12 C17 1.386(4) . ? C12 C13 1.395(4) . ? C13 C14 1.391(5) . ? C14 C15 1.383(5) . ? C15 C16 1.366(5) . ? C16 C17 1.391(5) . ? C18 C23 1.367(5) . ? C18 C19 1.382(5) . ? C19 C20 1.379(5) . ? C20 C21 1.371(5) . ? C21 C22 1.371(5) . ? C22 C23 1.386(4) . ? C24 C25 1.388(4) . ? C24 C29 1.393(4) . ? C25 C26 1.379(4) . ? C26 C27 1.396(4) . ? C27 C28 1.393(4) . ? C28 C29 1.386(4) . ? C30 C31 1.427(4) . ? C31 C40 1.415(4) . ? C31 C32 1.458(4) . ? C32 C33 1.406(4) . ? C32 C37 1.417(4) . ? C33 C34 1.373(5) . ? C34 C35 1.395(5) . ? C35 C36 1.374(5) . ? C36 C37 1.414(5) . ? C37 C38 1.417(5) . ? C38 C39 1.352(5) . ? C39 C40 1.433(4) . ? C41 C50 1.426(4) . ? C41 C42 1.433(4) . ? C42 C43 1.340(5) . ? C43 C44 1.435(5) . ? C44 C49 1.410(5) . ? C44 C45 1.417(5) . ? C45 C46 1.368(5) . ? C46 C47 1.387(6) . ? C47 C48 1.382(5) . ? C48 C49 1.421(4) . ? C49 C50 1.460(4) . ? C50 C51 1.420(4) . ? C52 C57 1.387(4) . ? C52 C53 1.393(4) . ? C53 C54 1.373(4) . ? C54 C55 1.389(4) . ? C55 C56 1.388(4) . ? C56 C57 1.386(4) . ? C58 C59 1.367(4) . ? C58 C63 1.378(4) . ? C59 C60 1.390(4) . ? C60 C61 1.379(4) . ? C61 C62 1.376(4) . ? C62 C63 1.383(4) . ? C64 C65 1.371(4) . ? C64 C69 1.382(4) . ? C65 C66 1.390(4) . ? C66 C67 1.398(4) . ? C67 C68 1.389(4) . ? C68 C69 1.385(4) . ? C70 C71 1.426(4) . ? C71 C80 1.418(4) . ? C71 C72 1.444(4) . ? C72 C73 1.410(4) . ? C72 C77 1.429(4) . ? C73 C74 1.375(5) . ? C74 C75 1.404(5) . ? C75 C76 1.349(5) . ? C76 C77 1.426(5) . ? C77 C78 1.419(5) . ? C78 C79 1.337(5) . ? C79 C80 1.436(4) . ? Cl1S C1S 1.773(4) . ? Cl2S C1S 1.771(4) . ? Cl3S C1S 1.752(4) . ? Cl4S Cl7S 0.933(8) . ? Cl4S Cl10 1.204(16) . ? Cl4S C2S 1.738(7) . ? Cl4S Cl12 2.07(3) . ? Cl4S Cl9S 2.080(12) . ? Cl5S Cl11 1.07(3) . ? Cl5S Cl8S 1.300(13) . ? Cl5S C2S 1.752(9) . ? Cl5S Cl9S 1.938(16) . ? Cl5S Cl6S 2.325(16) . ? Cl6S Cl12 1.08(3) . ? Cl6S Cl8S 1.120(11) . ? Cl6S C2S 1.790(9) . ? Cl6S Cl7S 2.330(12) . ? Cl7S Cl12 1.35(3) . ? Cl7S C2S 1.748(9) . ? Cl7S Cl10 2.042(16) . ? Cl8S C2S 1.669(9) . ? Cl8S Cl12 1.97(2) . ? Cl8S Cl11 2.15(2) . ? Cl9S Cl11 0.97(2) . ? Cl9S Cl10 1.067(13) . ? Cl9S C2S 1.681(9) . ? Cl10 C2S 1.768(10) . ? Cl10 Cl11 1.948(18) . ? Cl11 C2S 1.676(10) . ? Cl12 C2S 1.638(9) . ? O1S C3S 1.393(6) . ? O1S C5S 1.394(5) . ? C3S C4S 1.859(16) . ? C5S C6S 1.338(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O5 86.49(9) . . ? O1 Cu1 N3 147.95(10) . . ? O5 Cu1 N3 92.33(9) . . ? O1 Cu1 N1 92.59(9) . . ? O5 Cu1 N1 152.63(10) . . ? N3 Cu1 N1 102.44(10) . . ? O4 Cu2 O8 89.76(9) . . ? O4 Cu2 N2 92.49(9) . . ? O8 Cu2 N2 154.45(10) . . ? O4 Cu2 N4 152.83(10) . . ? O8 Cu2 N4 91.17(9) . . ? N2 Cu2 N4 98.18(9) . . ? C1 O1 Cu1 128.9(2) . . ? C18 O2 C15 119.9(3) . . ? C24 O3 C21 121.1(2) . . ? C40 O4 Cu2 127.48(18) . . ? C80 O8 Cu2 125.36(18) . . ? C41 O5 Cu1 129.58(19) . . ? C55 O6 C58 116.8(2) . . ? C61 O7 C64 118.8(2) . . ? C11 N1 C12 116.1(3) . . ? C11 N1 Cu1 122.9(2) . . ? C12 N1 Cu1 120.96(18) . . ? C30 N2 C27 119.7(2) . . ? C30 N2 Cu2 124.05(19) . . ? C27 N2 Cu2 116.20(18) . . ? C51 N3 C52 116.6(2) . . ? C51 N3 Cu1 124.4(2) . . ? C52 N3 Cu1 118.92(18) . . ? C70 N4 C67 118.9(2) . . ? C70 N4 Cu2 123.05(19) . . ? C67 N4 Cu2 117.88(18) . . ? O1 C1 C10 124.1(3) . . ? O1 C1 C2 117.4(3) . . ? C10 C1 C2 118.5(3) . . ? C3 C2 C1 121.2(3) . . ? C2 C3 C4 122.4(3) . . ? C3 C4 C5 121.5(3) . . ? C3 C4 C9 118.8(3) . . ? C5 C4 C9 119.8(3) . . ? C6 C5 C4 120.7(4) . . ? C5 C6 C7 119.9(3) . . ? C8 C7 C6 120.7(4) . . ? C7 C8 C9 121.6(4) . . ? C8 C9 C4 117.3(3) . . ? C8 C9 C10 123.7(3) . . ? C4 C9 C10 119.0(3) . . ? C1 C10 C11 121.0(3) . . ? C1 C10 C9 120.0(3) . . ? C11 C10 C9 118.7(3) . . ? N1 C11 C10 128.3(3) . . ? C17 C12 C13 119.4(3) . . ? C17 C12 N1 118.9(3) . . ? C13 C12 N1 121.7(3) . . ? C14 C13 C12 119.8(3) . . ? C15 C14 C13 120.1(3) . . ? C16 C15 C14 120.2(3) . . ? C16 C15 O2 119.5(4) . . ? C14 C15 O2 119.9(3) . . ? C15 C16 C17 120.4(3) . . ? C12 C17 C16 120.1(3) . . ? C23 C18 O2 125.0(3) . . ? C23 C18 C19 120.0(3) . . ? O2 C18 C19 114.9(3) . . ? C20 C19 C18 120.2(4) . . ? C21 C20 C19 119.6(4) . . ? C20 C21 C22 120.3(3) . . ? C20 C21 O3 117.0(3) . . ? C22 C21 O3 122.2(3) . . ? C21 C22 C23 120.2(3) . . ? C18 C23 C22 119.6(3) . . ? O3 C24 C25 115.3(3) . . ? O3 C24 C29 124.4(3) . . ? C25 C24 C29 120.1(3) . . ? C26 C25 C24 120.4(3) . . ? C25 C26 C27 119.9(3) . . ? C28 C27 C26 119.4(3) . . ? C28 C27 N2 122.8(3) . . ? C26 C27 N2 117.5(2) . . ? C29 C28 C27 120.6(3) . . ? C28 C29 C24 119.3(3) . . ? N2 C30 C31 127.2(3) . . ? C40 C31 C30 120.9(3) . . ? C40 C31 C32 119.6(3) . . ? C30 C31 C32 119.3(3) . . ? C33 C32 C37 116.9(3) . . ? C33 C32 C31 124.0(3) . . ? C37 C32 C31 119.1(3) . . ? C34 C33 C32 122.1(3) . . ? C33 C34 C35 120.8(3) . . ? C36 C35 C34 118.9(3) . . ? C35 C36 C37 121.2(3) . . ? C36 C37 C32 120.1(3) . . ? C36 C37 C38 120.6(3) . . ? C32 C37 C38 119.3(3) . . ? C39 C38 C37 121.8(3) . . ? C38 C39 C40 121.5(3) . . ? O4 C40 C31 124.9(3) . . ? O4 C40 C39 116.4(3) . . ? C31 C40 C39 118.6(3) . . ? O5 C41 C50 124.4(3) . . ? O5 C41 C42 117.0(3) . . ? C50 C41 C42 118.5(3) . . ? C43 C42 C41 122.0(3) . . ? C42 C43 C44 121.6(3) . . ? C49 C44 C45 120.3(3) . . ? C49 C44 C43 119.1(3) . . ? C45 C44 C43 120.7(3) . . ? C46 C45 C44 121.3(4) . . ? C45 C46 C47 119.0(3) . . ? C48 C47 C46 121.3(4) . . ? C47 C48 C49 121.3(3) . . ? C44 C49 C48 116.9(3) . . ? C44 C49 C50 119.6(3) . . ? C48 C49 C50 123.5(3) . . ? C51 C50 C41 121.0(3) . . ? C51 C50 C49 119.9(3) . . ? C41 C50 C49 119.1(3) . . ? N3 C51 C50 128.1(3) . . ? C57 C52 C53 119.0(3) . . ? C57 C52 N3 119.8(3) . . ? C53 C52 N3 121.1(3) . . ? C54 C53 C52 121.1(3) . . ? C53 C54 C55 119.1(3) . . ? C56 C55 O6 117.1(3) . . ? C56 C55 C54 121.1(3) . . ? O6 C55 C54 121.8(3) . . ? C57 C56 C55 118.9(3) . . ? C56 C57 C52 120.8(3) . . ? C59 C58 C63 121.1(3) . . ? C59 C58 O6 118.3(3) . . ? C63 C58 O6 120.6(3) . . ? C58 C59 C60 119.5(3) . . ? C61 C60 C59 119.6(3) . . ? C62 C61 C60 120.6(3) . . ? C62 C61 O7 116.7(3) . . ? C60 C61 O7 122.5(3) . . ? C61 C62 C63 119.6(3) . . ? C58 C63 C62 119.6(3) . . ? C65 C64 C69 121.3(3) . . ? C65 C64 O7 121.7(3) . . ? C69 C64 O7 116.9(3) . . ? C64 C65 C66 119.7(3) . . ? C65 C66 C67 120.1(3) . . ? C68 C67 C66 118.8(3) . . ? C68 C67 N4 118.3(2) . . ? C66 C67 N4 122.8(3) . . ? C69 C68 C67 121.1(3) . . ? C64 C69 C68 118.9(3) . . ? N4 C70 C71 126.4(3) . . ? C80 C71 C70 120.4(3) . . ? C80 C71 C72 120.0(3) . . ? C70 C71 C72 119.3(3) . . ? C73 C72 C77 117.4(3) . . ? C73 C72 C71 123.5(3) . . ? C77 C72 C71 119.1(3) . . ? C74 C73 C72 121.5(3) . . ? C73 C74 C75 120.7(3) . . ? C76 C75 C74 119.8(3) . . ? C75 C76 C77 121.3(3) . . ? C78 C77 C76 121.9(3) . . ? C78 C77 C72 118.7(3) . . ? C76 C77 C72 119.3(3) . . ? C79 C78 C77 121.7(3) . . ? C78 C79 C80 122.3(3) . . ? O8 C80 C71 124.8(3) . . ? O8 C80 C79 117.4(3) . . ? C71 C80 C79 117.8(3) . . ? Cl7S Cl4S Cl10 145.5(9) . . ? Cl7S Cl4S C2S 75.1(6) . . ? Cl10 Cl4S C2S 71.3(5) . . ? Cl7S Cl4S Cl12 30.3(7) . . ? Cl10 Cl4S Cl12 120.4(8) . . ? C2S Cl4S Cl12 50.1(5) . . ? Cl7S Cl4S Cl9S 126.3(7) . . ? Cl10 Cl4S Cl9S 22.2(5) . . ? C2S Cl4S Cl9S 51.3(3) . . ? Cl12 Cl4S Cl9S 98.7(6) . . ? Cl11 Cl5S Cl8S 130.8(12) . . ? Cl11 Cl5S C2S 68.1(8) . . ? Cl8S Cl5S C2S 64.3(5) . . ? Cl11 Cl5S Cl9S 16.8(8) . . ? Cl8S Cl5S Cl9S 114.6(7) . . ? C2S Cl5S Cl9S 53.9(4) . . ? Cl11 Cl5S Cl6S 116.1(10) . . ? Cl8S Cl5S Cl6S 14.9(4) . . ? C2S Cl5S Cl6S 49.7(4) . . ? Cl9S Cl5S Cl6S 100.0(5) . . ? Cl12 Cl6S Cl8S 126.3(12) . . ? Cl12 Cl6S C2S 64.1(7) . . ? Cl8S Cl6S C2S 65.3(5) . . ? Cl12 Cl6S Cl7S 18.5(8) . . ? Cl8S Cl6S Cl7S 107.9(7) . . ? C2S Cl6S Cl7S 48.1(3) . . ? Cl12 Cl6S Cl5S 109.3(10) . . ? Cl8S Cl6S Cl5S 17.3(5) . . ? C2S Cl6S Cl5S 48.3(4) . . ? Cl7S Cl6S Cl5S 91.0(5) . . ? Cl4S Cl7S Cl12 129.2(10) . . ? Cl4S Cl7S C2S 73.8(6) . . ? Cl12 Cl7S C2S 62.4(6) . . ? Cl4S Cl7S Cl10 19.5(6) . . ? Cl12 Cl7S Cl10 114.2(7) . . ? C2S Cl7S Cl10 54.9(4) . . ? Cl4S Cl7S Cl6S 114.5(8) . . ? Cl12 Cl7S Cl6S 14.8(5) . . ? C2S Cl7S Cl6S 49.6(4) . . ? Cl10 Cl7S Cl6S 99.6(5) . . ? Cl6S Cl8S Cl5S 147.8(9) . . ? Cl6S Cl8S C2S 77.1(6) . . ? Cl5S Cl8S C2S 71.1(6) . . ? Cl6S Cl8S Cl12 26.4(8) . . ? Cl5S Cl8S Cl12 121.8(10) . . ? C2S Cl8S Cl12 52.8(6) . . ? Cl6S Cl8S Cl11 125.9(8) . . ? Cl5S Cl8S Cl11 22.0(6) . . ? C2S Cl8S Cl11 50.1(5) . . ? Cl12 Cl8S Cl11 99.8(7) . . ? Cl11 Cl9S Cl10 146.7(18) . . ? Cl11 Cl9S C2S 73.0(10) . . ? Cl10 Cl9S C2S 76.5(8) . . ? Cl11 Cl9S Cl5S 18.5(14) . . ? Cl10 Cl9S Cl5S 128.2(11) . . ? C2S Cl9S Cl5S 57.4(5) . . ? Cl11 Cl9S Cl4S 121.5(16) . . ? Cl10 Cl9S Cl4S 25.2(8) . . ? C2S Cl9S Cl4S 53.8(3) . . ? Cl5S Cl9S Cl4S 103.0(6) . . ? Cl9S Cl10 Cl4S 132.6(12) . . ? Cl9S Cl10 C2S 67.6(6) . . ? Cl4S Cl10 C2S 68.6(6) . . ? Cl9S Cl10 Cl11 15.8(10) . . ? Cl4S Cl10 Cl11 116.8(11) . . ? C2S Cl10 Cl11 53.4(5) . . ? Cl9S Cl10 Cl7S 120.1(9) . . ? Cl4S Cl10 Cl7S 15.0(4) . . ? C2S Cl10 Cl7S 54.0(5) . . ? Cl11 Cl10 Cl7S 104.6(9) . . ? Cl9S Cl11 Cl5S 145(2) . . ? Cl9S Cl11 C2S 73.5(7) . . ? Cl5S Cl11 C2S 75.8(10) . . ? Cl9S Cl11 Cl10 17.5(9) . . ? Cl5S Cl11 Cl10 127.3(14) . . ? C2S Cl11 Cl10 57.8(5) . . ? Cl9S Cl11 Cl8S 118.1(12) . . ? Cl5S Cl11 Cl8S 27.2(8) . . ? C2S Cl11 Cl8S 49.8(6) . . ? Cl10 Cl11 Cl8S 100.7(8) . . ? Cl6S Cl12 Cl7S 146.7(10) . . ? Cl6S Cl12 C2S 79.4(8) . . ? Cl7S Cl12 C2S 70.9(7) . . ? Cl6S Cl12 Cl8S 27.3(6) . . ? Cl7S Cl12 Cl8S 119.4(7) . . ? C2S Cl12 Cl8S 54.2(5) . . ? Cl6S Cl12 Cl4S 126.3(9) . . ? Cl7S Cl12 Cl4S 20.5(4) . . ? C2S Cl12 Cl4S 54.4(6) . . ? Cl8S Cl12 Cl4S 99.2(5) . . ? C3S O1S C5S 122.2(5) . . ? Cl3S C1S Cl2S 109.4(2) . . ? Cl3S C1S Cl1S 110.4(2) . . ? Cl2S C1S Cl1S 108.8(2) . . ? Cl12 C2S Cl8S 73.0(9) . . ? Cl12 C2S Cl11 144.2(9) . . ? Cl8S C2S Cl11 80.2(10) . . ? Cl12 C2S Cl9S 142.8(8) . . ? Cl8S C2S Cl9S 110.1(6) . . ? Cl11 C2S Cl9S 33.5(8) . . ? Cl12 C2S Cl4S 75.4(10) . . ? Cl8S C2S Cl4S 128.8(5) . . ? Cl11 C2S Cl4S 105.2(7) . . ? Cl9S C2S Cl4S 74.9(5) . . ? Cl12 C2S Cl7S 46.7(9) . . ? Cl8S C2S Cl7S 114.8(5) . . ? Cl11 C2S Cl7S 134.4(6) . . ? Cl9S C2S Cl7S 106.0(6) . . ? Cl4S C2S Cl7S 31.1(3) . . ? Cl12 C2S Cl5S 115.8(9) . . ? Cl8S C2S Cl5S 44.6(4) . . ? Cl11 C2S Cl5S 36.2(9) . . ? Cl9S C2S Cl5S 68.7(6) . . ? Cl4S C2S Cl5S 128.8(5) . . ? Cl7S C2S Cl5S 143.2(5) . . ? Cl12 C2S Cl10 114.8(10) . . ? Cl8S C2S Cl10 133.7(5) . . ? Cl11 C2S Cl10 68.8(8) . . ? Cl9S C2S Cl10 35.9(5) . . ? Cl4S C2S Cl10 40.2(5) . . ? Cl7S C2S Cl10 71.0(6) . . ? Cl5S C2S Cl10 101.7(6) . . ? Cl12 C2S Cl6S 36.5(9) . . ? Cl8S C2S Cl6S 37.6(4) . . ? Cl11 C2S Cl6S 116.8(11) . . ? Cl9S C2S Cl6S 141.2(8) . . ? Cl4S C2S Cl6S 107.5(5) . . ? Cl7S C2S Cl6S 82.4(5) . . ? Cl5S C2S Cl6S 82.1(6) . . ? Cl10 C2S Cl6S 140.0(6) . . ? O1S C3S C4S 93.5(7) . . ? C6S C5S O1S 115.2(5) . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 26.85 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 1.416 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.089 data_ 1·CHCl3·2Et2O _database_code_CSD 163702 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common L55-Cu(II) complex _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C145 H65 Cl3 Cu4 N8 O18 S4' _chemical_formula_weight 2695.960 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' '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' _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 16.3594(8) _cell_length_b 18.2027(9) _cell_length_c 24.3250(13) _cell_angle_alpha 84.8100(10) _cell_angle_beta 86.7900(10) _cell_angle_gamma 65.3210(10) _cell_volume 6553.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour Dark brown _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 28611 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0961 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.76 _reflns_number_total 28611 _reflns_number_gt 15755 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.1292P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28611 _refine_ls_number_parameters 1711 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1218 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1936 _refine_ls_wR_factor_gt 0.1577 _refine_ls_goodness_of_fit_ref 0.843 _refine_ls_restrained_S_all 0.843 _refine_ls_shift/su_max 1.623 _refine_ls_shift/su_mean 0.042 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 1.06356(4) 0.27941(4) 0.42760(3) 0.04071(16) Uani 1 1 d . . . Cu2 Cu 0.82159(3) 0.34915(3) 0.32785(2) 0.03040(14) Uani 1 1 d . . . Cu3 Cu 0.79100(3) 0.39283(3) 0.16450(2) 0.02277(12) Uani 1 1 d . . . Cu4 Cu 0.57731(4) 0.39298(3) 0.06096(2) 0.02941(14) Uani 1 1 d . . . S1 S 0.80883(8) 0.11957(7) 0.47266(6) 0.0405(3) Uani 1 1 d . . . S2 S 1.07861(8) 0.45209(7) 0.19674(5) 0.0313(3) Uani 1 1 d . . . S3 S 0.46182(7) 0.49168(7) 0.30820(4) 0.0261(2) Uani 1 1 d . . . S4 S 0.96528(7) 0.21270(6) -0.00618(5) 0.0281(2) Uani 1 1 d . . . O1 O 0.7707(2) 0.0797(2) 0.51438(17) 0.0542(10) Uani 1 1 d . . . O2 O 0.8237(2) 0.0944(2) 0.41689(16) 0.0499(9) Uani 1 1 d . . . O3 O 1.1777(3) 0.2621(2) 0.3965(2) 0.0760(14) Uani 1 1 d . . . O4 O 0.8437(2) 0.44175(19) 0.30556(14) 0.0367(8) Uani 1 1 d . . . O5 O 0.9886(2) 0.51459(19) 0.19142(14) 0.0385(8) Uani 1 1 d . . . O6 O 1.1513(2) 0.4607(2) 0.16360(13) 0.0430(9) Uani 1 1 d . . . O7 O 0.9579(2) 0.2995(2) 0.47136(15) 0.0459(9) Uani 1 1 d . . . O8 O 0.71100(19) 0.34238(17) 0.18230(13) 0.0299(7) Uani 1 1 d . . . O9 O 0.5143(2) 0.53679(18) 0.31555(13) 0.0309(7) Uani 1 1 d . . . O10 O 0.3831(2) 0.50544(19) 0.34381(13) 0.0357(7) Uani 1 1 d . . . O11 O 0.9430(2) 0.2826(2) 0.30913(15) 0.0426(8) Uani 1 1 d . . . O12 O 0.6632(2) 0.42241(18) 0.01979(13) 0.0352(7) Uani 1 1 d . . . O13 O 1.0311(2) 0.1836(2) -0.05041(14) 0.0401(8) Uani 1 1 d . . . O14 O 0.9750(2) 0.16249(18) 0.04428(14) 0.0355(8) Uani 1 1 d . . . O15 O 0.4888(2) 0.36729(19) 0.10018(15) 0.0399(8) Uani 1 1 d . . . O16 O 0.70244(19) 0.48637(16) 0.19600(13) 0.0278(7) Uani 1 1 d . . . N1 N 1.1022(3) 0.1616(2) 0.43995(18) 0.0407(10) Uani 1 1 d . . . N2 N 0.7328(2) 0.4049(2) 0.38560(15) 0.0287(8) Uani 1 1 d . . . N3 N 1.0229(3) 0.3946(2) 0.40512(15) 0.0299(8) Uani 1 1 d . . . N4 N 0.8975(2) 0.28886(19) 0.16809(14) 0.0217(7) Uani 1 1 d . . . N5 N 0.7802(2) 0.2667(2) 0.31211(15) 0.0292(8) Uani 1 1 d . . . N6 N 0.5305(2) 0.4948(2) 0.09742(15) 0.0256(8) Uani 1 1 d . . . N7 N 0.8378(2) 0.4570(2) 0.11267(14) 0.0225(7) Uani 1 1 d . . . N8 N 0.6260(2) 0.2878(2) 0.02820(16) 0.0309(8) Uani 1 1 d . . . C1 C 0.9119(3) 0.1133(3) 0.4959(2) 0.0385(11) Uani 1 1 d . . . C2 C 0.9301(3) 0.0929(3) 0.5512(2) 0.0435(13) Uani 1 1 d . . . H2B H 0.8902 0.0819 0.5757 0.052 Uiso 1 1 calc R . . C3 C 1.0103(4) 0.0898(4) 0.5686(2) 0.0540(15) Uani 1 1 d . . . H3A H 1.0268 0.0733 0.6051 0.065 Uiso 1 1 calc R . . C4 C 1.0675(4) 0.1110(3) 0.5320(2) 0.0515(14) Uani 1 1 d . . . H4A H 1.1202 0.1105 0.5449 0.062 Uiso 1 1 calc R . . C5 C 1.0463(3) 0.1328(3) 0.4771(2) 0.0378(11) Uani 1 1 d . . . C6 C 0.9700(3) 0.1312(3) 0.4577(2) 0.0349(11) Uani 1 1 d . . . H6B H 0.9570 0.1417 0.4204 0.042 Uiso 1 1 calc R . . C7 C 1.1744(3) 0.1064(3) 0.4183(2) 0.0398(12) Uani 1 1 d . . . H7A H 1.1839 0.0526 0.4266 0.048 Uiso 1 1 calc R . . C8 C 1.2403(3) 0.1207(3) 0.3829(2) 0.0432(12) Uani 1 1 d . . . C9 C 1.2387(4) 0.1986(4) 0.3752(3) 0.0605(17) Uani 1 1 d . . . C10 C 1.3104(5) 0.2100(4) 0.3423(3) 0.084(2) Uani 1 1 d . . . H10B H 1.3118 0.2608 0.3389 0.101 Uiso 1 1 calc R . . C11 C 1.3748(4) 0.1483(5) 0.3168(3) 0.083(2) Uani 1 1 d . . . H11A H 1.4202 0.1573 0.2966 0.100 Uiso 1 1 calc R . . C12 C 1.3749(4) 0.0698(4) 0.3200(3) 0.0612(17) Uani 1 1 d . . . C13 C 1.4391(4) 0.0079(5) 0.2895(3) 0.074(2) Uani 1 1 d . . . H13B H 1.4824 0.0184 0.2680 0.089 Uiso 1 1 calc R . . C14 C 1.4385(5) -0.0666(5) 0.2910(3) 0.088(2) Uani 1 1 d . . . H14B H 1.4806 -0.1067 0.2704 0.105 Uiso 1 1 calc R . . C15 C 1.3731(5) -0.0824(4) 0.3242(3) 0.082(2) Uani 1 1 d . . . H15A H 1.3722 -0.1332 0.3254 0.098 Uiso 1 1 calc R . . C16 C 1.3105(4) -0.0232(4) 0.3550(3) 0.0630(17) Uani 1 1 d . . . H16A H 1.2687 -0.0353 0.3769 0.076 Uiso 1 1 calc R . . C17 C 1.3084(3) 0.0548(3) 0.3540(2) 0.0473(14) Uani 1 1 d . . . C18 C 0.7364(3) 0.2248(3) 0.4687(2) 0.0364(11) Uani 1 1 d . . . C19 C 0.6499(3) 0.2499(3) 0.4919(2) 0.0466(13) Uani 1 1 d . . . H19A H 0.6333 0.2139 0.5142 0.056 Uiso 1 1 calc R . . C20 C 0.5893(3) 0.3298(3) 0.4809(2) 0.0486(14) Uani 1 1 d . . . H20A H 0.5317 0.3482 0.4966 0.058 Uiso 1 1 calc R . . C21 C 0.6145(3) 0.3824(3) 0.44642(19) 0.0357(11) Uani 1 1 d . . . H21A H 0.5726 0.4353 0.4382 0.043 Uiso 1 1 calc R . . C22 C 0.7023(3) 0.3570(3) 0.42383(18) 0.0299(10) Uani 1 1 d . . . C23 C 0.7631(3) 0.2782(3) 0.43656(18) 0.0308(10) Uani 1 1 d . . . H23A H 0.8223 0.2608 0.4235 0.037 Uiso 1 1 calc R . . C24 C 0.6970(3) 0.4839(3) 0.38862(19) 0.0308(10) Uani 1 1 d . . . H24A H 0.6516 0.5047 0.4150 0.037 Uiso 1 1 calc R . . C25 C 0.7211(3) 0.5412(3) 0.35522(19) 0.0307(10) Uani 1 1 d . . . C26 C 0.7977(3) 0.5164(3) 0.31825(19) 0.0315(10) Uani 1 1 d . . . C27 C 0.8291(3) 0.5753(3) 0.2953(2) 0.0390(12) Uani 1 1 d . . . H27A H 0.8791 0.5593 0.2716 0.047 Uiso 1 1 calc R . . C28 C 0.7883(3) 0.6527(3) 0.3072(2) 0.0428(12) Uani 1 1 d . . . H28A H 0.8124 0.6888 0.2931 0.051 Uiso 1 1 calc R . . C29 C 0.7077(4) 0.6818(3) 0.3414(2) 0.0420(12) Uani 1 1 d . . . C30 C 0.6628(4) 0.7653(3) 0.3512(2) 0.0539(15) Uani 1 1 d . . . H30A H 0.6870 0.8014 0.3371 0.065 Uiso 1 1 calc R . . C31 C 0.5830(5) 0.7930(4) 0.3818(3) 0.071(2) Uani 1 1 d . . . H31A H 0.5555 0.8470 0.3901 0.085 Uiso 1 1 calc R . . C32 C 0.5440(5) 0.7402(4) 0.4000(3) 0.0659(18) Uani 1 1 d . . . H32A H 0.4885 0.7600 0.4183 0.079 Uiso 1 1 calc R . . C33 C 0.5864(4) 0.6594(3) 0.3915(2) 0.0501(14) Uani 1 1 d . . . H33A H 0.5590 0.6252 0.4042 0.060 Uiso 1 1 calc R . . C34 C 0.6708(3) 0.6268(3) 0.3636(2) 0.0369(11) Uani 1 1 d . . . C35 C 1.1070(3) 0.4403(3) 0.26643(19) 0.0312(10) Uani 1 1 d . . . C36 C 1.0542(3) 0.4208(3) 0.30727(18) 0.0284(9) Uani 1 1 d . . . H36A H 1.0062 0.4100 0.2977 0.034 Uiso 1 1 calc R . . C37 C 1.0744(3) 0.4178(3) 0.36208(18) 0.0294(10) Uani 1 1 d . . . C38 C 1.1458(4) 0.4341(3) 0.3754(2) 0.0455(13) Uani 1 1 d . . . H38A H 1.1589 0.4329 0.4122 0.055 Uiso 1 1 calc R . . C39 C 1.1980(4) 0.4524(4) 0.3341(2) 0.0490(14) Uani 1 1 d . . . H39A H 1.2459 0.4633 0.3437 0.059 Uiso 1 1 calc R . . C40 C 1.1800(3) 0.4547(3) 0.2795(2) 0.0411(12) Uani 1 1 d . . . H40A H 1.2159 0.4656 0.2519 0.049 Uiso 1 1 calc R . . C41 C 0.9523(3) 0.4527(3) 0.42476(18) 0.0321(10) Uani 1 1 d . . . H41A H 0.9408 0.5049 0.4100 0.038 Uiso 1 1 calc R . . C42 C 0.8897(3) 0.4454(3) 0.46684(18) 0.0313(10) Uani 1 1 d . . . C43 C 0.8955(3) 0.3685(3) 0.4865(2) 0.0367(11) Uani 1 1 d . . . C44 C 0.8286(3) 0.3640(3) 0.5264(2) 0.0409(12) Uani 1 1 d . . . H44A H 0.8340 0.3133 0.5411 0.049 Uiso 1 1 calc R . . C45 C 0.7583(3) 0.4307(3) 0.5431(2) 0.0391(12) Uani 1 1 d . . . H45A H 0.7155 0.4248 0.5676 0.047 Uiso 1 1 calc R . . C46 C 0.7491(3) 0.5104(3) 0.5234(2) 0.0374(11) Uani 1 1 d . . . C47 C 0.6762(3) 0.5792(3) 0.5419(2) 0.0435(12) Uani 1 1 d . . . H47A H 0.6319 0.5730 0.5651 0.052 Uiso 1 1 calc R . . C48 C 0.6708(4) 0.6543(4) 0.5259(3) 0.0608(17) Uani 1 1 d . . . H48A H 0.6227 0.6997 0.5381 0.073 Uiso 1 1 calc R . . C49 C 0.7384(4) 0.6636(4) 0.4906(2) 0.0572(16) Uani 1 1 d . . . H49A H 0.7351 0.7152 0.4803 0.069 Uiso 1 1 calc R . . C50 C 0.8086(4) 0.5971(3) 0.4715(2) 0.0435(12) Uani 1 1 d . . . H50A H 0.8519 0.6046 0.4482 0.052 Uiso 1 1 calc R . . C51 C 0.8168(3) 0.5177(3) 0.48646(18) 0.0337(10) Uani 1 1 d . . . C52 C 1.0754(3) 0.3602(3) 0.18187(17) 0.0266(9) Uani 1 1 d . . . C53 C 1.1508(3) 0.3006(3) 0.15858(19) 0.0338(11) Uani 1 1 d . . . H53A H 1.2053 0.3056 0.1557 0.041 Uiso 1 1 calc R . . C54 C 1.1441(3) 0.2342(3) 0.1397(2) 0.0376(11) Uani 1 1 d . . . H54A H 1.1945 0.1930 0.1253 0.045 Uiso 1 1 calc R . . C55 C 1.0609(3) 0.2294(3) 0.14245(19) 0.0308(10) Uani 1 1 d . . . H55A H 1.0554 0.1864 0.1275 0.037 Uiso 1 1 calc R . . C56 C 0.9857(3) 0.2881(2) 0.16728(17) 0.0230(9) Uani 1 1 d . . . C57 C 0.9929(3) 0.3540(2) 0.18818(17) 0.0239(9) Uani 1 1 d . . . H57A H 0.9441 0.3928 0.2058 0.029 Uiso 1 1 calc R . . C58 C 0.8922(3) 0.2188(2) 0.16678(17) 0.0242(9) Uani 1 1 d . . . H58A H 0.9464 0.1731 0.1662 0.029 Uiso 1 1 calc R . . C59 C 0.8124(3) 0.2054(2) 0.16616(17) 0.0237(9) Uani 1 1 d . . . C60 C 0.8208(3) 0.1248(3) 0.15726(19) 0.0309(10) Uani 1 1 d . . . C61 C 0.9010(3) 0.0624(3) 0.1390(2) 0.0417(12) Uani 1 1 d . . . H61A H 0.9517 0.0730 0.1322 0.050 Uiso 1 1 calc R . . C62 C 0.9069(4) -0.0133(3) 0.1309(3) 0.0590(16) Uani 1 1 d . . . H62A H 0.9610 -0.0533 0.1193 0.071 Uiso 1 1 calc R . . C63 C 0.8309(5) -0.0298(4) 0.1402(3) 0.072(2) Uani 1 1 d . . . H63A H 0.8345 -0.0811 0.1352 0.087 Uiso 1 1 calc R . . C64 C 0.7514(4) 0.0293(3) 0.1568(3) 0.0656(19) Uani 1 1 d . . . H64A H 0.7010 0.0180 0.1617 0.079 Uiso 1 1 calc R . . C65 C 0.7437(3) 0.1076(3) 0.1666(2) 0.0396(12) Uani 1 1 d . . . C66 C 0.6609(3) 0.1695(3) 0.1837(2) 0.0385(11) Uani 1 1 d . . . H66A H 0.6115 0.1572 0.1912 0.046 Uiso 1 1 calc R . . C67 C 0.6520(3) 0.2458(3) 0.18928(19) 0.0313(10) Uani 1 1 d . . . H67A H 0.5968 0.2850 0.2003 0.038 Uiso 1 1 calc R . . C68 C 0.7271(3) 0.2670(2) 0.17839(17) 0.0253(9) Uani 1 1 d . . . C69 C 0.5347(3) 0.3875(2) 0.31561(17) 0.0254(9) Uani 1 1 d . . . C70 C 0.6265(3) 0.3651(3) 0.30535(17) 0.0259(9) Uani 1 1 d . . . H70A H 0.6474 0.4031 0.2905 0.031 Uiso 1 1 calc R . . C71 C 0.6856(3) 0.2856(3) 0.31761(19) 0.0300(10) Uani 1 1 d . . . C72 C 0.6515(3) 0.2294(3) 0.3384(2) 0.0384(11) Uani 1 1 d . . . H72A H 0.6912 0.1761 0.3477 0.046 Uiso 1 1 calc R . . C73 C 0.5606(3) 0.2515(3) 0.3452(2) 0.0428(12) Uani 1 1 d . . . H73A H 0.5393 0.2126 0.3572 0.051 Uiso 1 1 calc R . . C74 C 0.4999(3) 0.3318(3) 0.3341(2) 0.0371(11) Uani 1 1 d . . . H74A H 0.4383 0.3475 0.3390 0.045 Uiso 1 1 calc R . . C75 C 0.8341(3) 0.1928(3) 0.29989(18) 0.0344(11) Uani 1 1 d . . . H75A H 0.8068 0.1588 0.2935 0.041 Uiso 1 1 calc R . . C76 C 0.9306(3) 0.1589(3) 0.29532(19) 0.0357(11) Uani 1 1 d . . . C77 C 0.9773(4) 0.0731(3) 0.2838(2) 0.0462(14) Uani 1 1 d . . . C78 C 0.9355(4) 0.0193(3) 0.2832(3) 0.0599(17) Uani 1 1 d . . . H78A H 0.8740 0.0387 0.2907 0.072 Uiso 1 1 calc R . . C79 C 0.9817(5) -0.0604(4) 0.2722(3) 0.073(2) Uani 1 1 d . . . H79A H 0.9515 -0.0936 0.2716 0.088 Uiso 1 1 calc R . . C80 C 1.0763(6) -0.0921(5) 0.2615(3) 0.090(3) Uani 1 1 d . . . H80A H 1.1081 -0.1464 0.2547 0.108 Uiso 1 1 calc R . . C81 C 1.1197(5) -0.0426(4) 0.2613(3) 0.081(2) Uani 1 1 d . . . H81A H 1.1813 -0.0632 0.2539 0.097 Uiso 1 1 calc R . . C82 C 1.0715(4) 0.0415(4) 0.2726(2) 0.0571(16) Uani 1 1 d . . . C83 C 1.1169(4) 0.0919(4) 0.2740(3) 0.0644(19) Uani 1 1 d . . . H83A H 1.1786 0.0702 0.2666 0.077 Uiso 1 1 calc R . . C84 C 1.0742(3) 0.1723(4) 0.2859(2) 0.0522(15) Uani 1 1 d . . . H84A H 1.1064 0.2039 0.2862 0.063 Uiso 1 1 calc R . . C85 C 0.9786(3) 0.2062(3) 0.29782(19) 0.0389(12) Uani 1 1 d . . . C86 C 0.4287(3) 0.5078(2) 0.23937(17) 0.0243(9) Uani 1 1 d . . . C87 C 0.4928(3) 0.4952(2) 0.19650(17) 0.0256(9) Uani 1 1 d . . . H87A H 0.5532 0.4786 0.2043 0.031 Uiso 1 1 calc R . . C88 C 0.4658(3) 0.5076(2) 0.14331(18) 0.0258(9) Uani 1 1 d . . . C89 C 0.3753(3) 0.5315(3) 0.1320(2) 0.0355(11) Uani 1 1 d . . . H89A H 0.3571 0.5386 0.0956 0.043 Uiso 1 1 calc R . . C90 C 0.3120(3) 0.5449(3) 0.1754(2) 0.0374(11) Uani 1 1 d . . . H90A H 0.2516 0.5620 0.1674 0.045 Uiso 1 1 calc R . . C91 C 0.3373(3) 0.5334(3) 0.22922(19) 0.0294(10) Uani 1 1 d . . . H91A H 0.2952 0.5423 0.2580 0.035 Uiso 1 1 calc R . . C92 C 0.5562(3) 0.5540(3) 0.08681(18) 0.0254(9) Uani 1 1 d . . . H92A H 0.5315 0.5972 0.1092 0.030 Uiso 1 1 calc R . . C93 C 0.6187(3) 0.5591(3) 0.04416(17) 0.0243(9) Uani 1 1 d . . . C94 C 0.6298(3) 0.6343(3) 0.03355(18) 0.0277(9) Uani 1 1 d . . . C95 C 0.5785(3) 0.7058(3) 0.0611(2) 0.0361(11) Uani 1 1 d . . . H95A H 0.5362 0.7053 0.0881 0.043 Uiso 1 1 calc R . . C96 C 0.5909(4) 0.7758(3) 0.0480(2) 0.0469(13) Uani 1 1 d . . . H96A H 0.5572 0.8217 0.0667 0.056 Uiso 1 1 calc R . . C97 C 0.6538(4) 0.7791(3) 0.0069(2) 0.0460(13) Uani 1 1 d . . . H97A H 0.6613 0.8268 -0.0016 0.055 Uiso 1 1 calc R . . C98 C 0.7034(3) 0.7115(3) -0.0205(2) 0.0383(11) Uani 1 1 d . . . H98A H 0.7449 0.7136 -0.0476 0.046 Uiso 1 1 calc R . . C99 C 0.6930(3) 0.6386(3) -0.00841(18) 0.0305(10) Uani 1 1 d . . . C100 C 0.7459(3) 0.5681(3) -0.03765(18) 0.0309(10) Uani 1 1 d . . . H10C H 0.7878 0.5704 -0.0644 0.037 Uiso 1 1 calc R . . C101 C 0.7351(3) 0.4976(3) -0.02635(18) 0.0296(10) Uani 1 1 d . . . H10D H 0.7708 0.4524 -0.0453 0.035 Uiso 1 1 calc R . . C102 C 0.6706(3) 0.4914(3) 0.01359(18) 0.0271(9) Uani 1 1 d . . . C103 C 0.9638(3) 0.3052(2) 0.01251(17) 0.0239(9) Uani 1 1 d . . . C104 C 0.8956(3) 0.3528(2) 0.04796(17) 0.0224(8) Uani 1 1 d . . . H10E H 0.8453 0.3420 0.0558 0.027 Uiso 1 1 calc R . . C105 C 0.9035(3) 0.4168(2) 0.07147(17) 0.0220(8) Uani 1 1 d . . . C106 C 0.9784(3) 0.4334(2) 0.05674(17) 0.0238(9) Uani 1 1 d . . . H10F H 0.9846 0.4757 0.0720 0.029 Uiso 1 1 calc R . . C107 C 1.0433(3) 0.3878(3) 0.01986(18) 0.0293(10) Uani 1 1 d . . . H10G H 1.0910 0.4017 0.0096 0.035 Uiso 1 1 calc R . . C108 C 1.0389(3) 0.3213(3) -0.00232(18) 0.0286(9) Uani 1 1 d . . . H10H H 1.0839 0.2893 -0.0259 0.034 Uiso 1 1 calc R . . C109 C 0.8159(3) 0.5343(2) 0.11719(17) 0.0242(9) Uani 1 1 d . . . H10I H 0.8438 0.5587 0.0921 0.029 Uiso 1 1 calc R . . C110 C 0.7542(3) 0.5857(2) 0.15608(17) 0.0231(9) Uani 1 1 d . . . C111 C 0.7435(3) 0.6693(3) 0.15567(19) 0.0289(10) Uani 1 1 d . . . C112 C 0.8016(4) 0.6991(3) 0.1256(2) 0.0426(13) Uani 1 1 d . . . H11B H 0.8509 0.6637 0.1064 0.051 Uiso 1 1 calc R . . C113 C 0.7863(4) 0.7787(3) 0.1245(3) 0.0615(18) Uani 1 1 d . . . H11C H 0.8245 0.7970 0.1038 0.074 Uiso 1 1 calc R . . C114 C 0.7147(4) 0.8332(3) 0.1539(3) 0.0605(17) Uani 1 1 d . . . H11D H 0.7043 0.8876 0.1522 0.073 Uiso 1 1 calc R . . C115 C 0.6589(4) 0.8057(3) 0.1857(2) 0.0486(14) Uani 1 1 d . . . H11E H 0.6117 0.8417 0.2060 0.058 Uiso 1 1 calc R . . C116 C 0.6726(3) 0.7245(3) 0.1875(2) 0.0323(10) Uani 1 1 d . . . C117 C 0.6158(3) 0.6958(3) 0.2207(2) 0.0338(11) Uani 1 1 d . . . H11F H 0.5693 0.7321 0.2414 0.041 Uiso 1 1 calc R . . C118 C 0.6274(3) 0.6174(3) 0.22322(19) 0.0300(10) Uani 1 1 d . . . H11G H 0.5895 0.6008 0.2458 0.036 Uiso 1 1 calc R . . C119 C 0.6971(3) 0.5599(2) 0.19146(18) 0.0250(9) Uani 1 1 d . . . C120 C 0.8570(3) 0.2369(2) -0.03007(19) 0.0273(9) Uani 1 1 d . . . C121 C 0.8464(3) 0.2436(3) -0.0867(2) 0.0383(11) Uani 1 1 d . . . H12A H 0.8945 0.2362 -0.1112 0.046 Uiso 1 1 calc R . . C122 C 0.7616(4) 0.2617(4) -0.1049(2) 0.0481(14) Uani 1 1 d . . . H12B H 0.7522 0.2649 -0.1426 0.058 Uiso 1 1 calc R . . C123 C 0.6888(3) 0.2754(3) -0.0676(2) 0.0423(12) Uani 1 1 d . . . H12C H 0.6318 0.2887 -0.0809 0.051 Uiso 1 1 calc R . . C124 C 0.7010(3) 0.2694(3) -0.01109(19) 0.0296(10) Uani 1 1 d . . . C125 C 0.7865(3) 0.2476(3) 0.00769(18) 0.0270(9) Uani 1 1 d . . . H12D H 0.7970 0.2400 0.0454 0.032 Uiso 1 1 calc R . . C126 C 0.5978(3) 0.2304(3) 0.03817(19) 0.0296(10) Uani 1 1 d . . . H12E H 0.6257 0.1847 0.0183 0.036 Uiso 1 1 calc R . . C127 C 0.5280(3) 0.2309(3) 0.0767(2) 0.0328(10) Uani 1 1 d . . . C128 C 0.5102(3) 0.1590(3) 0.0879(2) 0.0403(12) Uani 1 1 d . . . C129 C 0.5550(4) 0.0878(3) 0.0588(3) 0.0507(14) Uani 1 1 d . . . H12F H 0.5974 0.0864 0.0314 0.061 Uiso 1 1 calc R . . C130 C 0.5360(4) 0.0205(4) 0.0710(3) 0.0654(18) Uani 1 1 d . . . H13C H 0.5654 -0.0251 0.0513 0.078 Uiso 1 1 calc R . . C131 C 0.4730(5) 0.0203(4) 0.1127(3) 0.0686(19) Uani 1 1 d . . . H13D H 0.4618 -0.0256 0.1210 0.082 Uiso 1 1 calc R . . C132 C 0.4288(4) 0.0872(4) 0.1407(3) 0.0569(16) Uani 1 1 d . . . H13E H 0.3864 0.0869 0.1678 0.068 Uiso 1 1 calc R . . C133 C 0.4454(3) 0.1585(3) 0.1299(2) 0.0449(13) Uani 1 1 d . . . C134 C 0.3992(3) 0.2281(3) 0.1597(2) 0.0444(13) Uani 1 1 d . . . H13F H 0.3586 0.2266 0.1877 0.053 Uiso 1 1 calc R . . C135 C 0.4122(3) 0.2970(3) 0.1488(2) 0.0417(12) Uani 1 1 d . . . H13G H 0.3793 0.3423 0.1682 0.050 Uiso 1 1 calc R . . C136 C 0.4782(3) 0.2995(3) 0.1066(2) 0.0345(11) Uani 1 1 d . . . C1S C 1.1700(4) 0.0226(4) 0.0520(3) 0.0646(18) Uani 1 1 d . . . Cl1 Cl 1.1902(6) -0.0603(4) 0.0153(4) 0.087(2) Uani 0.50 1 d P . . Cl2 Cl 1.1523(5) -0.0094(9) 0.1220(6) 0.129(4) Uani 0.50 1 d P . . Cl3 Cl 1.1646(8) 0.0013(8) 0.1215(5) 0.168(6) Uani 0.50 1 d P . . Cl1' Cl 1.2413(5) 0.0676(4) 0.0267(4) 0.127(3) Uani 0.50 1 d P . . Cl2' Cl 1.2751(4) 0.0322(4) 0.0550(3) 0.0994(18) Uani 0.50 1 d P . . Cl3' Cl 1.1805(9) -0.0480(8) 0.0063(6) 0.179(5) Uani 0.50 1 d P . . O1S O 0.3068(5) 0.7714(5) 0.2659(3) 0.122(2) Uani 1 1 d . . . C2S C 0.3714(6) 0.7475(8) 0.2318(6) 0.140(5) Uani 1 1 d . . . C3S C 0.3692(6) 0.8165(7) 0.1866(4) 0.116(3) Uani 1 1 d . . . C4S C 0.3059(8) 0.7212(5) 0.3154(6) 0.148(5) Uani 1 1 d . . . C5S C 0.2691(10) 0.7625(8) 0.3702(5) 0.169(6) Uani 1 1 d . . . O2S O 0.9764(6) 0.7219(5) 0.2989(3) 0.053(2) Uani 0.50 1 d P . . C6S C 0.9990(11) 0.6771(12) 0.3540(9) 0.116(7) Uani 0.50 1 d P . . C7S C 0.9482(14) 0.7109(15) 0.3942(6) 0.110(8) Uani 0.50 1 d P . . C8S C 1.0197(10) 0.6812(8) 0.2542(8) 0.082(5) Uani 0.50 1 d P . . C9S C 0.9987(15) 0.7211(13) 0.2040(6) 0.112(7) Uani 0.50 1 d P . . O3S O 0.6240(9) 0.0355(7) 0.3895(6) 0.112(4) Uani 0.50 1 d P . . C10S C 0.7004(13) -0.0074(13) 0.3074(9) 0.120(7) Uani 0.50 1 d P . . C11S C 0.7297(14) -0.0120(10) 0.3637(6) 0.157(12) Uani 0.50 1 d P . . C12S C 0.601(2) 0.031(2) 0.4503(10) 0.163(14) Uani 0.50 1 d P . . C13S C 0.516(2) 0.1007(14) 0.4651(12) 0.169(14) Uani 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 0.0343(3) 0.0389(3) 0.0472(4) -0.0018(3) 0.0111(3) -0.0151(3) Cu2 0.0204(3) 0.0341(3) 0.0336(3) -0.0005(2) 0.0041(2) -0.0092(2) Cu3 0.0172(3) 0.0215(2) 0.0302(3) -0.0035(2) 0.0040(2) -0.0089(2) Cu4 0.0247(3) 0.0313(3) 0.0345(3) -0.0080(2) 0.0064(2) -0.0135(2) S1 0.0323(7) 0.0383(7) 0.0458(8) 0.0101(6) 0.0015(5) -0.0125(5) S2 0.0333(6) 0.0461(7) 0.0256(6) -0.0047(5) 0.0022(5) -0.0275(6) S3 0.0202(5) 0.0331(6) 0.0243(6) -0.0034(4) 0.0039(4) -0.0108(4) S4 0.0233(5) 0.0258(5) 0.0350(6) -0.0107(5) 0.0061(4) -0.0092(4) O1 0.040(2) 0.049(2) 0.070(3) 0.0239(19) 0.0005(18) -0.0206(18) O2 0.046(2) 0.046(2) 0.051(2) 0.0005(17) -0.0021(17) -0.0128(18) O3 0.045(3) 0.048(2) 0.135(4) -0.014(3) 0.035(3) -0.023(2) O4 0.0245(17) 0.0390(18) 0.045(2) -0.0020(15) 0.0077(14) -0.0130(15) O5 0.041(2) 0.0373(18) 0.040(2) -0.0008(15) -0.0066(15) -0.0190(16) O6 0.046(2) 0.073(2) 0.0312(19) -0.0097(17) 0.0105(15) -0.045(2) O7 0.048(2) 0.0369(19) 0.049(2) -0.0035(16) 0.0156(17) -0.0164(17) O8 0.0242(16) 0.0235(15) 0.046(2) -0.0055(13) 0.0049(13) -0.0138(13) O9 0.0280(17) 0.0346(17) 0.0326(18) -0.0077(13) -0.0013(13) -0.0144(14) O10 0.0274(17) 0.0457(19) 0.0304(18) -0.0048(14) 0.0099(13) -0.0125(15) O11 0.0234(17) 0.043(2) 0.053(2) 0.0008(17) 0.0061(15) -0.0073(15) O12 0.0319(18) 0.0356(17) 0.041(2) -0.0116(15) 0.0127(14) -0.0164(15) O13 0.0269(17) 0.0433(19) 0.052(2) -0.0286(16) 0.0146(15) -0.0131(15) O14 0.0319(18) 0.0286(16) 0.044(2) 0.0017(14) -0.0036(14) -0.0110(14) O15 0.0298(18) 0.0389(18) 0.055(2) -0.0108(16) 0.0134(15) -0.0187(15) O16 0.0224(15) 0.0218(14) 0.0403(19) -0.0057(13) 0.0089(13) -0.0106(12) N1 0.031(2) 0.042(2) 0.044(3) 0.0027(19) 0.0059(18) -0.0117(19) N2 0.0234(19) 0.035(2) 0.028(2) -0.0014(16) 0.0003(15) -0.0122(16) N3 0.033(2) 0.037(2) 0.024(2) -0.0072(16) 0.0065(16) -0.0189(18) N4 0.0171(17) 0.0239(17) 0.0263(19) -0.0019(14) -0.0001(14) -0.0107(14) N5 0.0234(19) 0.031(2) 0.028(2) -0.0003(16) -0.0009(15) -0.0071(16) N6 0.0184(18) 0.0293(18) 0.027(2) -0.0040(15) 0.0015(14) -0.0081(15) N7 0.0201(17) 0.0244(17) 0.0241(19) -0.0074(14) 0.0032(14) -0.0097(14) N8 0.0229(19) 0.036(2) 0.037(2) -0.0074(17) 0.0027(16) -0.0155(17) C1 0.031(3) 0.033(2) 0.043(3) 0.005(2) 0.001(2) -0.007(2) C2 0.035(3) 0.048(3) 0.039(3) 0.011(2) 0.005(2) -0.012(2) C3 0.051(4) 0.068(4) 0.033(3) 0.012(3) -0.004(2) -0.017(3) C4 0.038(3) 0.065(4) 0.047(3) 0.013(3) -0.005(2) -0.020(3) C5 0.031(3) 0.032(2) 0.040(3) 0.007(2) 0.009(2) -0.005(2) C6 0.029(2) 0.033(2) 0.035(3) 0.005(2) 0.001(2) -0.008(2) C7 0.029(3) 0.035(3) 0.045(3) 0.005(2) 0.002(2) -0.005(2) C8 0.028(3) 0.049(3) 0.044(3) 0.008(2) 0.003(2) -0.010(2) C9 0.033(3) 0.057(4) 0.083(5) -0.002(3) 0.019(3) -0.013(3) C10 0.056(4) 0.069(5) 0.125(7) 0.002(4) 0.034(4) -0.030(4) C11 0.044(4) 0.081(5) 0.107(6) 0.011(4) 0.035(4) -0.016(4) C12 0.041(3) 0.067(4) 0.058(4) 0.010(3) 0.015(3) -0.009(3) C13 0.046(4) 0.079(5) 0.073(5) 0.005(4) 0.025(3) -0.006(4) C14 0.071(5) 0.086(6) 0.085(6) -0.021(4) 0.037(4) -0.014(4) C15 0.069(5) 0.066(4) 0.091(6) -0.020(4) 0.030(4) -0.010(4) C16 0.047(4) 0.056(4) 0.067(4) -0.001(3) 0.018(3) -0.007(3) C17 0.031(3) 0.049(3) 0.046(3) 0.009(3) 0.004(2) -0.003(2) C18 0.030(3) 0.038(3) 0.035(3) 0.005(2) 0.000(2) -0.010(2) C19 0.037(3) 0.053(3) 0.046(3) 0.013(3) 0.011(2) -0.019(3) C20 0.029(3) 0.052(3) 0.053(3) 0.006(3) 0.018(2) -0.010(2) C21 0.026(2) 0.041(3) 0.032(3) 0.000(2) 0.0043(19) -0.007(2) C22 0.028(2) 0.039(3) 0.023(2) -0.0026(19) 0.0012(18) -0.014(2) C23 0.023(2) 0.038(2) 0.029(2) 0.0022(19) 0.0014(18) -0.011(2) C24 0.024(2) 0.039(3) 0.028(2) -0.0019(19) -0.0006(18) -0.012(2) C25 0.031(2) 0.033(2) 0.030(2) 0.0009(19) -0.0036(19) -0.015(2) C26 0.027(2) 0.037(3) 0.030(3) 0.000(2) -0.0017(19) -0.013(2) C27 0.029(3) 0.041(3) 0.049(3) 0.002(2) 0.000(2) -0.018(2) C28 0.040(3) 0.045(3) 0.051(3) 0.004(2) -0.005(2) -0.026(3) C29 0.048(3) 0.040(3) 0.040(3) -0.007(2) -0.003(2) -0.019(2) C30 0.077(4) 0.038(3) 0.049(4) -0.002(3) 0.000(3) -0.027(3) C31 0.099(6) 0.040(3) 0.061(4) -0.014(3) 0.015(4) -0.016(4) C32 0.072(5) 0.046(3) 0.067(4) -0.008(3) 0.030(3) -0.015(3) C33 0.052(4) 0.038(3) 0.053(4) -0.005(2) 0.014(3) -0.013(3) C34 0.040(3) 0.042(3) 0.029(3) -0.003(2) -0.002(2) -0.016(2) C35 0.028(2) 0.044(3) 0.029(2) -0.009(2) 0.0019(18) -0.020(2) C36 0.023(2) 0.035(2) 0.032(2) -0.0043(19) -0.0002(18) -0.0169(19) C37 0.032(2) 0.036(2) 0.023(2) -0.0045(18) 0.0040(18) -0.018(2) C38 0.056(3) 0.071(4) 0.029(3) -0.005(2) -0.008(2) -0.045(3) C39 0.054(3) 0.085(4) 0.037(3) -0.006(3) -0.005(2) -0.056(3) C40 0.041(3) 0.067(3) 0.035(3) -0.003(2) 0.002(2) -0.042(3) C41 0.038(3) 0.039(3) 0.023(2) -0.0022(19) -0.0028(19) -0.020(2) C42 0.030(2) 0.043(3) 0.023(2) -0.0026(19) -0.0005(18) -0.017(2) C43 0.038(3) 0.045(3) 0.029(3) -0.006(2) 0.002(2) -0.019(2) C44 0.049(3) 0.048(3) 0.035(3) -0.008(2) 0.009(2) -0.030(3) C45 0.035(3) 0.061(3) 0.026(3) -0.010(2) 0.008(2) -0.024(3) C46 0.032(3) 0.053(3) 0.026(3) -0.006(2) -0.002(2) -0.017(2) C47 0.031(3) 0.058(3) 0.035(3) -0.005(2) 0.003(2) -0.012(2) C48 0.048(4) 0.058(4) 0.052(4) -0.004(3) 0.003(3) 0.001(3) C49 0.064(4) 0.047(3) 0.044(3) 0.007(3) 0.009(3) -0.009(3) C50 0.046(3) 0.047(3) 0.034(3) -0.002(2) 0.005(2) -0.016(3) C51 0.033(3) 0.045(3) 0.023(2) -0.003(2) -0.0048(19) -0.015(2) C52 0.024(2) 0.041(2) 0.023(2) -0.0055(18) -0.0001(17) -0.020(2) C53 0.020(2) 0.049(3) 0.034(3) -0.005(2) 0.0005(19) -0.016(2) C54 0.019(2) 0.041(3) 0.046(3) -0.010(2) 0.002(2) -0.004(2) C55 0.026(2) 0.032(2) 0.035(3) -0.006(2) 0.0002(19) -0.012(2) C56 0.019(2) 0.028(2) 0.024(2) 0.0007(17) -0.0031(16) -0.0116(18) C57 0.019(2) 0.031(2) 0.023(2) -0.0061(17) 0.0029(16) -0.0114(18) C58 0.023(2) 0.023(2) 0.024(2) -0.0049(17) 0.0000(17) -0.0065(17) C59 0.026(2) 0.023(2) 0.025(2) -0.0021(17) 0.0005(17) -0.0131(18) C60 0.032(3) 0.030(2) 0.034(3) -0.0047(19) 0.0012(19) -0.017(2) C61 0.039(3) 0.032(3) 0.057(3) -0.010(2) 0.011(2) -0.017(2) C62 0.054(4) 0.037(3) 0.088(5) -0.021(3) 0.018(3) -0.020(3) C63 0.075(5) 0.040(3) 0.122(6) -0.035(4) 0.027(4) -0.041(3) C64 0.060(4) 0.044(3) 0.110(6) -0.031(3) 0.015(4) -0.035(3) C65 0.040(3) 0.034(3) 0.055(3) -0.006(2) 0.003(2) -0.025(2) C66 0.036(3) 0.041(3) 0.049(3) -0.008(2) 0.004(2) -0.026(2) C67 0.025(2) 0.031(2) 0.042(3) -0.011(2) 0.0050(19) -0.0153(19) C68 0.028(2) 0.027(2) 0.025(2) -0.0029(17) -0.0021(17) -0.0155(19) C69 0.023(2) 0.028(2) 0.025(2) 0.0006(17) 0.0006(17) -0.0098(18) C70 0.026(2) 0.032(2) 0.023(2) -0.0013(18) 0.0015(17) -0.0150(19) C71 0.026(2) 0.034(2) 0.029(2) -0.0046(19) -0.0021(18) -0.010(2) C72 0.035(3) 0.030(2) 0.047(3) 0.001(2) -0.006(2) -0.011(2) C73 0.039(3) 0.041(3) 0.055(3) 0.004(2) -0.002(2) -0.023(2) C74 0.030(3) 0.043(3) 0.041(3) 0.003(2) 0.000(2) -0.019(2) C75 0.038(3) 0.035(3) 0.025(2) 0.0018(19) -0.001(2) -0.011(2) C76 0.031(3) 0.034(2) 0.028(3) 0.001(2) 0.000(2) 0.000(2) C77 0.042(3) 0.046(3) 0.029(3) 0.004(2) -0.008(2) 0.002(3) C78 0.062(4) 0.041(3) 0.054(4) -0.006(3) -0.008(3) 0.002(3) C79 0.088(5) 0.045(3) 0.063(4) -0.007(3) -0.002(4) -0.004(4) C80 0.099(7) 0.048(4) 0.084(6) -0.018(4) -0.005(5) 0.012(4) C81 0.060(4) 0.056(4) 0.075(5) -0.014(4) 0.006(4) 0.027(4) C82 0.042(3) 0.058(4) 0.046(4) -0.003(3) 0.002(3) 0.003(3) C83 0.026(3) 0.076(4) 0.053(4) 0.004(3) 0.003(3) 0.014(3) C84 0.023(3) 0.065(4) 0.049(3) 0.001(3) 0.002(2) 0.000(3) C85 0.025(2) 0.047(3) 0.027(3) 0.005(2) -0.0001(19) 0.000(2) C86 0.020(2) 0.028(2) 0.026(2) -0.0049(17) 0.0005(17) -0.0108(18) C87 0.015(2) 0.030(2) 0.028(2) -0.0025(18) 0.0000(17) -0.0059(17) C88 0.019(2) 0.027(2) 0.030(2) -0.0051(18) 0.0045(17) -0.0080(18) C89 0.025(2) 0.053(3) 0.031(3) -0.005(2) -0.0048(19) -0.018(2) C90 0.015(2) 0.059(3) 0.038(3) -0.009(2) 0.0007(19) -0.014(2) C91 0.018(2) 0.041(3) 0.031(3) -0.005(2) 0.0084(17) -0.0144(19) C92 0.023(2) 0.028(2) 0.025(2) -0.0044(17) 0.0017(17) -0.0099(18) C93 0.024(2) 0.032(2) 0.019(2) -0.0010(17) -0.0032(16) -0.0133(18) C94 0.023(2) 0.032(2) 0.027(2) -0.0029(18) -0.0024(18) -0.0100(19) C95 0.033(3) 0.040(3) 0.039(3) -0.003(2) 0.004(2) -0.019(2) C96 0.053(3) 0.034(3) 0.054(4) -0.010(2) 0.006(3) -0.017(3) C97 0.049(3) 0.038(3) 0.058(4) 0.001(2) 0.003(3) -0.027(3) C98 0.032(3) 0.045(3) 0.041(3) 0.006(2) 0.001(2) -0.020(2) C99 0.026(2) 0.042(3) 0.026(2) -0.0004(19) -0.0040(18) -0.017(2) C100 0.024(2) 0.043(3) 0.026(2) -0.001(2) 0.0006(18) -0.015(2) C101 0.021(2) 0.042(3) 0.024(2) -0.0066(19) 0.0040(17) -0.012(2) C102 0.023(2) 0.034(2) 0.025(2) -0.0020(18) -0.0031(17) -0.0136(19) C103 0.024(2) 0.024(2) 0.024(2) -0.0037(17) 0.0013(17) -0.0100(18) C104 0.018(2) 0.026(2) 0.024(2) -0.0033(17) 0.0023(16) -0.0096(17) C105 0.018(2) 0.023(2) 0.022(2) -0.0006(16) 0.0017(16) -0.0068(17) C106 0.023(2) 0.022(2) 0.028(2) -0.0025(17) -0.0009(17) -0.0106(17) C107 0.026(2) 0.034(2) 0.033(3) -0.0027(19) 0.0056(18) -0.018(2) C108 0.023(2) 0.031(2) 0.029(2) -0.0045(18) 0.0107(18) -0.0097(19) C109 0.024(2) 0.027(2) 0.027(2) -0.0009(17) 0.0001(17) -0.0164(18) C110 0.021(2) 0.023(2) 0.026(2) -0.0049(17) 0.0018(17) -0.0095(17) C111 0.031(2) 0.025(2) 0.034(3) -0.0066(18) 0.0034(19) -0.0145(19) C112 0.046(3) 0.035(3) 0.054(3) -0.018(2) 0.025(2) -0.024(2) C113 0.066(4) 0.045(3) 0.087(5) -0.024(3) 0.040(3) -0.039(3) C114 0.067(4) 0.031(3) 0.090(5) -0.023(3) 0.035(3) -0.027(3) C115 0.045(3) 0.030(3) 0.071(4) -0.024(3) 0.024(3) -0.015(2) C116 0.030(2) 0.026(2) 0.044(3) -0.009(2) 0.008(2) -0.013(2) C117 0.025(2) 0.031(2) 0.044(3) -0.017(2) 0.014(2) -0.010(2) C118 0.027(2) 0.034(2) 0.032(3) -0.0062(19) 0.0083(18) -0.016(2) C119 0.020(2) 0.025(2) 0.030(2) -0.0073(18) -0.0001(17) -0.0090(18) C120 0.023(2) 0.027(2) 0.033(3) -0.0116(18) 0.0023(18) -0.0091(18) C121 0.034(3) 0.049(3) 0.034(3) -0.009(2) 0.009(2) -0.019(2) C122 0.045(3) 0.075(4) 0.026(3) -0.005(3) -0.003(2) -0.025(3) C123 0.031(3) 0.052(3) 0.041(3) -0.005(2) -0.005(2) -0.013(2) C124 0.029(2) 0.025(2) 0.039(3) -0.0103(19) 0.0067(19) -0.0143(19) C125 0.030(2) 0.030(2) 0.025(2) -0.0104(18) 0.0021(18) -0.0151(19) C126 0.025(2) 0.030(2) 0.035(3) -0.0102(19) 0.0019(19) -0.0110(19) C127 0.027(2) 0.036(2) 0.042(3) -0.005(2) -0.001(2) -0.018(2) C128 0.031(3) 0.042(3) 0.052(3) 0.003(2) -0.010(2) -0.020(2) C129 0.047(3) 0.044(3) 0.070(4) -0.009(3) 0.005(3) -0.028(3) C130 0.067(4) 0.042(3) 0.095(5) -0.009(3) -0.001(4) -0.031(3) C131 0.070(5) 0.048(4) 0.100(6) 0.007(4) 0.004(4) -0.040(3) C132 0.052(4) 0.059(4) 0.070(4) 0.014(3) -0.002(3) -0.037(3) C133 0.032(3) 0.055(3) 0.055(3) 0.007(3) -0.006(2) -0.027(3) C134 0.026(3) 0.055(3) 0.056(4) 0.004(3) 0.002(2) -0.022(2) C135 0.024(2) 0.047(3) 0.054(3) -0.008(2) 0.006(2) -0.014(2) C136 0.025(2) 0.043(3) 0.038(3) -0.003(2) 0.001(2) -0.017(2) C1S 0.058(4) 0.046(3) 0.089(5) -0.015(3) 0.007(3) -0.020(3) Cl1 0.091(4) 0.054(2) 0.132(5) -0.044(3) 0.035(4) -0.045(3) Cl2 0.048(3) 0.169(10) 0.137(8) 0.045(6) -0.002(4) -0.024(5) Cl3 0.220(11) 0.107(6) 0.085(6) -0.008(4) -0.006(6) 0.025(7) Cl1' 0.093(5) 0.101(5) 0.209(9) -0.033(4) 0.021(4) -0.061(4) Cl2' 0.065(3) 0.104(5) 0.141(6) -0.035(4) 0.014(3) -0.043(3) Cl3' 0.154(8) 0.155(9) 0.208(11) -0.054(7) -0.075(7) -0.027(6) O1S 0.090(5) 0.152(6) 0.115(5) -0.012(5) 0.031(4) -0.045(5) C2S 0.039(5) 0.189(12) 0.160(11) -0.043(10) -0.015(6) -0.007(6) C3S 0.076(6) 0.159(10) 0.095(7) -0.048(7) 0.004(5) -0.023(6) C4S 0.141(10) 0.056(5) 0.216(15) 0.027(7) 0.026(9) -0.023(6) C5S 0.220(14) 0.137(10) 0.145(11) -0.011(8) 0.107(10) -0.081(10) O2S 0.071(6) 0.052(5) 0.042(5) -0.012(4) 0.006(4) -0.029(4) C6S 0.058(10) 0.131(17) 0.130(16) 0.012(13) -0.049(10) -0.008(10) C7S 0.168(17) 0.20(2) 0.034(8) 0.020(11) -0.026(9) -0.155(18) C8S 0.080(11) 0.054(8) 0.108(14) -0.028(9) -0.003(9) -0.019(8) C9S 0.174(19) 0.167(18) 0.043(9) -0.034(10) 0.047(10) -0.120(16) O3S 0.138(11) 0.119(9) 0.123(11) 0.038(8) -0.052(8) -0.099(9) C10S 0.122(16) 0.174(19) 0.124(18) -0.037(14) -0.005(12) -0.116(15) C11S 0.163(18) 0.094(12) 0.060(10) -0.029(9) -0.049(11) 0.110(12) C12S 0.24(3) 0.24(4) 0.089(17) 0.04(2) -0.053(19) -0.19(3) C13S 0.20(3) 0.100(16) 0.17(3) -0.017(16) 0.12(2) -0.041(17) _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 O3 1.884(4) . ? Cu1 O7 1.895(4) . ? Cu1 N3 1.951(4) . ? Cu1 N1 1.965(4) . ? Cu2 O4 1.894(3) . ? Cu2 O11 1.900(3) . ? Cu2 N5 1.959(4) . ? Cu2 N2 1.978(4) . ? Cu3 O8 1.900(3) . ? Cu3 O16 1.907(3) . ? Cu3 N4 1.964(3) . ? Cu3 N7 1.977(3) . ? Cu4 O15 1.886(3) . ? Cu4 O12 1.908(3) . ? Cu4 N6 1.960(4) . ? Cu4 N8 1.966(4) . ? S1 O2 1.446(4) . ? S1 O1 1.455(4) . ? S1 C1 1.764(5) . ? S1 C18 1.779(5) . ? S2 O5 1.441(3) . ? S2 O6 1.454(3) . ? S2 C35 1.753(5) . ? S2 C52 1.766(4) . ? S3 O9 1.441(3) . ? S3 O10 1.454(3) . ? S3 C86 1.750(4) . ? S3 C69 1.767(4) . ? S4 O14 1.437(3) . ? S4 O13 1.447(3) . ? S4 C120 1.757(4) . ? S4 C103 1.773(4) . ? O3 C9 1.300(7) . ? O4 C26 1.306(5) . ? O7 C43 1.313(6) . ? O8 C68 1.297(5) . ? O11 C85 1.312(6) . ? O12 C102 1.305(5) . ? O15 C136 1.311(5) . ? O16 C119 1.299(5) . ? N1 C7 1.311(6) . ? N1 C5 1.466(6) . ? N2 C24 1.315(5) . ? N2 C22 1.427(5) . ? N3 C41 1.300(6) . ? N3 C37 1.450(5) . ? N4 C58 1.317(5) . ? N4 C56 1.435(5) . ? N5 C75 1.315(6) . ? N5 C71 1.440(5) . ? N6 C92 1.312(5) . ? N6 C88 1.459(5) . ? N7 C109 1.314(5) . ? N7 C105 1.432(5) . ? N8 C126 1.307(5) . ? N8 C124 1.454(6) . ? C1 C2 1.378(7) . ? C1 C6 1.406(7) . ? C2 C3 1.377(7) . ? C3 C4 1.401(7) . ? C4 C5 1.379(7) . ? C5 C6 1.370(7) . ? C7 C8 1.435(7) . ? C8 C9 1.403(8) . ? C8 C17 1.456(7) . ? C9 C10 1.459(8) . ? C10 C11 1.350(9) . ? C11 C12 1.423(9) . ? C12 C13 1.414(9) . ? C12 C17 1.432(8) . ? C13 C14 1.357(10) . ? C14 C15 1.413(10) . ? C15 C16 1.381(8) . ? C16 C17 1.404(8) . ? C18 C23 1.388(6) . ? C18 C19 1.395(7) . ? C19 C20 1.388(7) . ? C20 C21 1.392(7) . ? C21 C22 1.409(6) . ? C22 C23 1.380(6) . ? C24 C25 1.434(6) . ? C25 C26 1.435(6) . ? C25 C34 1.454(6) . ? C26 C27 1.428(6) . ? C27 C28 1.335(7) . ? C28 C29 1.444(7) . ? C29 C30 1.422(7) . ? C29 C34 1.425(7) . ? C30 C31 1.386(9) . ? C31 C32 1.389(9) . ? C32 C33 1.370(7) . ? C33 C34 1.414(7) . ? C35 C40 1.384(6) . ? C35 C36 1.398(6) . ? C36 C37 1.383(6) . ? C37 C38 1.380(6) . ? C38 C39 1.390(7) . ? C39 C40 1.370(7) . ? C41 C42 1.444(6) . ? C42 C43 1.404(7) . ? C42 C51 1.457(7) . ? C43 C44 1.446(7) . ? C44 C45 1.353(7) . ? C45 C46 1.434(7) . ? C46 C47 1.410(7) . ? C46 C51 1.428(7) . ? C47 C48 1.354(8) . ? C48 C49 1.420(8) . ? C49 C50 1.371(7) . ? C50 C51 1.410(7) . ? C52 C53 1.391(6) . ? C52 C57 1.399(5) . ? C53 C54 1.379(7) . ? C54 C55 1.398(6) . ? C55 C56 1.398(6) . ? C56 C57 1.396(6) . ? C58 C59 1.426(6) . ? C59 C68 1.414(6) . ? C59 C60 1.450(6) . ? C60 C61 1.410(6) . ? C60 C65 1.424(6) . ? C61 C62 1.372(7) . ? C62 C63 1.399(8) . ? C63 C64 1.364(8) . ? C64 C65 1.417(7) . ? C65 C66 1.423(7) . ? C66 C67 1.354(6) . ? C67 C68 1.438(6) . ? C69 C74 1.388(6) . ? C69 C70 1.395(6) . ? C70 C71 1.380(6) . ? C71 C72 1.402(6) . ? C72 C73 1.373(7) . ? C73 C74 1.393(7) . ? C75 C76 1.436(6) . ? C76 C85 1.394(7) . ? C76 C77 1.471(7) . ? C77 C78 1.410(8) . ? C77 C82 1.422(8) . ? C78 C79 1.372(8) . ? C79 C80 1.424(11) . ? C80 C81 1.362(11) . ? C81 C82 1.443(9) . ? C82 C83 1.404(9) . ? C83 C84 1.384(8) . ? C84 C85 1.444(7) . ? C86 C91 1.397(5) . ? C86 C87 1.401(6) . ? C87 C88 1.360(6) . ? C88 C89 1.393(6) . ? C89 C90 1.400(6) . ? C90 C91 1.368(6) . ? C92 C93 1.440(6) . ? C93 C102 1.420(6) . ? C93 C94 1.452(6) . ? C94 C95 1.425(6) . ? C94 C99 1.433(6) . ? C95 C96 1.377(7) . ? C96 C97 1.411(7) . ? C97 C98 1.367(7) . ? C98 C99 1.410(6) . ? C99 C100 1.440(6) . ? C100 C101 1.369(6) . ? C101 C102 1.426(6) . ? C103 C104 1.400(6) . ? C103 C108 1.399(6) . ? C104 C105 1.398(5) . ? C105 C106 1.400(5) . ? C106 C107 1.383(6) . ? C107 C108 1.399(6) . ? C109 C110 1.433(6) . ? C110 C119 1.428(6) . ? C110 C111 1.455(6) . ? C111 C112 1.419(6) . ? C111 C116 1.423(6) . ? C112 C113 1.362(7) . ? C113 C114 1.389(8) . ? C114 C115 1.383(7) . ? C115 C116 1.395(6) . ? C116 C117 1.426(6) . ? C117 C118 1.356(6) . ? C118 C119 1.429(6) . ? C120 C121 1.385(6) . ? C120 C125 1.393(6) . ? C121 C122 1.376(7) . ? C122 C123 1.405(7) . ? C123 C124 1.387(7) . ? C124 C125 1.377(6) . ? C126 C127 1.434(6) . ? C127 C136 1.413(7) . ? C127 C128 1.455(6) . ? C128 C129 1.425(7) . ? C128 C133 1.432(7) . ? C129 C130 1.388(7) . ? C130 C131 1.405(9) . ? C131 C132 1.353(9) . ? C132 C133 1.431(7) . ? C133 C134 1.417(8) . ? C134 C135 1.358(7) . ? C135 C136 1.460(7) . ? C1S Cl3' 1.723(14) . ? C1S Cl3 1.706(14) . ? C1S Cl1 1.725(9) . ? C1S Cl1' 1.744(9) . ? C1S Cl2 1.795(15) . ? C1S Cl2' 1.806(9) . ? Cl1' Cl2' 0.926(8) . ? O1S C2S 1.256(12) . ? O1S C4S 1.447(13) . ? C2S C3S 1.582(16) . ? C4S C5S 1.555(17) . ? O2S C8S 1.361(17) . ? O2S C6S 1.48(2) . ? C6S C7S 1.27(3) . ? C8S C9S 1.35(2) . ? O3S C12S 1.51(3) . ? O3S C11S 1.69(2) . ? C10S C11S 1.46(2) . ? C12S C13S 1.50(4) . ? 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 O3 Cu1 O7 169.0(2) . . ? O3 Cu1 N3 88.80(17) . . ? O7 Cu1 N3 91.28(15) . . ? O3 Cu1 N1 89.77(17) . . ? O7 Cu1 N1 91.55(16) . . ? N3 Cu1 N1 172.35(17) . . ? O4 Cu2 O11 89.05(14) . . ? O4 Cu2 N5 150.88(15) . . ? O11 Cu2 N5 92.74(15) . . ? O4 Cu2 N2 93.20(15) . . ? O11 Cu2 N2 147.82(15) . . ? N5 Cu2 N2 100.42(15) . . ? O8 Cu3 O16 86.82(12) . . ? O8 Cu3 N4 92.82(13) . . ? O16 Cu3 N4 153.29(14) . . ? O8 Cu3 N7 151.10(14) . . ? O16 Cu3 N7 93.47(13) . . ? N4 Cu3 N7 99.41(14) . . ? O15 Cu4 O12 177.76(15) . . ? O15 Cu4 N6 88.01(14) . . ? O12 Cu4 N6 91.06(14) . . ? O15 Cu4 N8 90.63(15) . . ? O12 Cu4 N8 90.40(14) . . ? N6 Cu4 N8 177.01(15) . . ? O2 S1 O1 119.7(2) . . ? O2 S1 C1 107.5(2) . . ? O1 S1 C1 109.2(2) . . ? O2 S1 C18 107.1(2) . . ? O1 S1 C18 107.3(2) . . ? C1 S1 C18 105.1(2) . . ? O5 S2 O6 119.4(2) . . ? O5 S2 C35 107.5(2) . . ? O6 S2 C35 108.1(2) . . ? O5 S2 C52 107.43(19) . . ? O6 S2 C52 107.5(2) . . ? C35 S2 C52 106.2(2) . . ? O9 S3 O10 118.48(19) . . ? O9 S3 C86 108.73(19) . . ? O10 S3 C86 108.64(19) . . ? O9 S3 C69 107.55(19) . . ? O10 S3 C69 108.4(2) . . ? C86 S3 C69 104.1(2) . . ? O14 S4 O13 119.3(2) . . ? O14 S4 C120 106.6(2) . . ? O13 S4 C120 110.0(2) . . ? O14 S4 C103 106.22(19) . . ? O13 S4 C103 108.2(2) . . ? C120 S4 C103 105.74(19) . . ? C9 O3 Cu1 130.3(4) . . ? C26 O4 Cu2 128.4(3) . . ? C43 O7 Cu1 129.7(3) . . ? C68 O8 Cu3 127.2(3) . . ? C85 O11 Cu2 128.7(3) . . ? C102 O12 Cu4 130.5(3) . . ? C136 O15 Cu4 131.0(3) . . ? C119 O16 Cu3 128.2(3) . . ? C7 N1 C5 117.0(4) . . ? C7 N1 Cu1 125.5(3) . . ? C5 N1 Cu1 117.4(3) . . ? C24 N2 C22 118.6(4) . . ? C24 N2 Cu2 123.3(3) . . ? C22 N2 Cu2 117.9(3) . . ? C41 N3 C37 116.8(4) . . ? C41 N3 Cu1 125.6(3) . . ? C37 N3 Cu1 117.6(3) . . ? C58 N4 C56 117.5(3) . . ? C58 N4 Cu3 122.5(3) . . ? C56 N4 Cu3 119.7(3) . . ? C75 N5 C71 117.2(4) . . ? C75 N5 Cu2 124.0(3) . . ? C71 N5 Cu2 118.7(3) . . ? C92 N6 C88 113.8(4) . . ? C92 N6 Cu4 125.7(3) . . ? C88 N6 Cu4 120.4(3) . . ? C109 N7 C105 118.3(3) . . ? C109 N7 Cu3 122.3(3) . . ? C105 N7 Cu3 119.3(2) . . ? C126 N8 C124 114.7(4) . . ? C126 N8 Cu4 126.4(3) . . ? C124 N8 Cu4 118.9(3) . . ? C2 C1 C6 123.4(5) . . ? C2 C1 S1 117.8(4) . . ? C6 C1 S1 118.8(4) . . ? C3 C2 C1 116.7(5) . . ? C2 C3 C4 121.1(5) . . ? C5 C4 C3 120.6(5) . . ? C6 C5 C4 119.7(5) . . ? C6 C5 N1 119.7(4) . . ? C4 C5 N1 120.5(5) . . ? C5 C6 C1 118.2(5) . . ? N1 C7 C8 126.5(5) . . ? C9 C8 C7 120.2(5) . . ? C9 C8 C17 119.5(5) . . ? C7 C8 C17 120.3(5) . . ? O3 C9 C8 124.1(5) . . ? O3 C9 C10 117.0(6) . . ? C8 C9 C10 118.9(6) . . ? C11 C10 C9 121.3(7) . . ? C10 C11 C12 121.6(6) . . ? C13 C12 C11 120.5(6) . . ? C13 C12 C17 120.5(6) . . ? C11 C12 C17 119.0(6) . . ? C14 C13 C12 121.1(7) . . ? C13 C14 C15 119.1(7) . . ? C16 C15 C14 120.9(7) . . ? C15 C16 C17 121.7(6) . . ? C16 C17 C12 116.7(5) . . ? C16 C17 C8 123.7(5) . . ? C12 C17 C8 119.5(5) . . ? C23 C18 C19 121.6(4) . . ? C23 C18 S1 118.9(4) . . ? C19 C18 S1 119.0(4) . . ? C20 C19 C18 118.4(5) . . ? C19 C20 C21 120.1(5) . . ? C20 C21 C22 121.1(4) . . ? C23 C22 C21 118.4(4) . . ? C23 C22 N2 116.5(4) . . ? C21 C22 N2 125.1(4) . . ? C22 C23 C18 120.3(4) . . ? N2 C24 C25 126.5(4) . . ? C24 C25 C26 122.2(4) . . ? C24 C25 C34 118.0(4) . . ? C26 C25 C34 119.5(4) . . ? O4 C26 C27 117.0(4) . . ? O4 C26 C25 123.9(4) . . ? C27 C26 C25 119.1(4) . . ? C28 C27 C26 121.5(5) . . ? C27 C28 C29 121.6(5) . . ? C30 C29 C34 119.7(5) . . ? C30 C29 C28 120.6(5) . . ? C34 C29 C28 119.6(5) . . ? C31 C30 C29 120.0(6) . . ? C30 C31 C32 120.1(6) . . ? C33 C32 C31 120.9(6) . . ? C32 C33 C34 121.4(5) . . ? C33 C34 C29 117.7(5) . . ? C33 C34 C25 124.2(5) . . ? C29 C34 C25 118.1(4) . . ? C40 C35 C36 121.7(4) . . ? C40 C35 S2 117.9(4) . . ? C36 C35 S2 120.4(3) . . ? C37 C36 C35 118.9(4) . . ? C36 C37 C38 119.6(4) . . ? C36 C37 N3 120.0(4) . . ? C38 C37 N3 120.4(4) . . ? C37 C38 C39 120.5(4) . . ? C40 C39 C38 120.9(4) . . ? C39 C40 C35 118.4(4) . . ? N3 C41 C42 127.5(4) . . ? C43 C42 C41 120.0(4) . . ? C43 C42 C51 119.6(4) . . ? C41 C42 C51 120.2(4) . . ? O7 C43 C42 124.8(4) . . ? O7 C43 C44 117.0(4) . . ? C42 C43 C44 118.2(5) . . ? C45 C44 C43 122.6(5) . . ? C44 C45 C46 120.9(5) . . ? C47 C46 C45 120.0(5) . . ? C47 C46 C51 121.6(5) . . ? C45 C46 C51 118.3(4) . . ? C48 C47 C46 119.8(5) . . ? C47 C48 C49 120.0(5) . . ? C50 C49 C48 120.6(5) . . ? C49 C50 C51 121.7(5) . . ? C50 C51 C46 116.3(5) . . ? C50 C51 C42 123.6(5) . . ? C46 C51 C42 120.2(4) . . ? C53 C52 C57 122.1(4) . . ? C53 C52 S2 119.6(3) . . ? C57 C52 S2 117.9(3) . . ? C54 C53 C52 119.3(4) . . ? C53 C54 C55 119.5(4) . . ? C54 C55 C56 121.1(4) . . ? C57 C56 C55 119.6(4) . . ? C57 C56 N4 116.8(4) . . ? C55 C56 N4 123.4(4) . . ? C56 C57 C52 118.2(4) . . ? N4 C58 C59 127.2(4) . . ? C68 C59 C58 121.2(4) . . ? C68 C59 C60 120.0(4) . . ? C58 C59 C60 118.6(4) . . ? C61 C60 C65 117.8(4) . . ? C61 C60 C59 123.7(4) . . ? C65 C60 C59 118.5(4) . . ? C62 C61 C60 122.4(5) . . ? C61 C62 C63 119.5(5) . . ? C64 C63 C62 120.0(5) . . ? C63 C64 C65 121.8(5) . . ? C64 C65 C60 118.5(5) . . ? C64 C65 C66 122.0(5) . . ? C60 C65 C66 119.5(4) . . ? C67 C66 C65 121.9(4) . . ? C66 C67 C68 120.6(4) . . ? O8 C68 C59 124.8(4) . . ? O8 C68 C67 116.1(4) . . ? C59 C68 C67 119.0(4) . . ? C74 C69 C70 122.5(4) . . ? C74 C69 S3 119.3(3) . . ? C70 C69 S3 118.1(3) . . ? C71 C70 C69 118.9(4) . . ? C70 C71 C72 119.1(4) . . ? C70 C71 N5 117.1(4) . . ? C72 C71 N5 123.6(4) . . ? C73 C72 C71 121.3(4) . . ? C72 C73 C74 120.5(5) . . ? C69 C74 C73 117.7(4) . . ? N5 C75 C76 127.2(5) . . ? C85 C76 C75 121.8(4) . . ? C85 C76 C77 120.5(5) . . ? C75 C76 C77 117.6(5) . . ? C78 C77 C82 117.3(5) . . ? C78 C77 C76 124.7(5) . . ? C82 C77 C76 118.0(6) . . ? C79 C78 C77 122.8(7) . . ? C78 C79 C80 119.8(8) . . ? C81 C80 C79 119.7(7) . . ? C80 C81 C82 120.9(7) . . ? C83 C82 C77 119.6(5) . . ? C83 C82 C81 120.8(6) . . ? C77 C82 C81 119.6(7) . . ? C84 C83 C82 123.0(5) . . ? C83 C84 C85 118.8(6) . . ? O11 C85 C76 124.7(4) . . ? O11 C85 C84 115.3(5) . . ? C76 C85 C84 119.9(5) . . ? C91 C86 C87 122.0(4) . . ? C91 C86 S3 117.9(3) . . ? C87 C86 S3 120.1(3) . . ? C88 C87 C86 119.2(4) . . ? C87 C88 C89 120.0(4) . . ? C87 C88 N6 121.0(4) . . ? C89 C88 N6 119.0(4) . . ? C88 C89 C90 120.0(4) . . ? C91 C90 C89 121.2(4) . . ? C90 C91 C86 117.6(4) . . ? N6 C92 C93 126.8(4) . . ? C102 C93 C92 120.9(4) . . ? C102 C93 C94 120.1(4) . . ? C92 C93 C94 119.1(4) . . ? C95 C94 C99 117.4(4) . . ? C95 C94 C93 123.7(4) . . ? C99 C94 C93 118.8(4) . . ? C96 C95 C94 120.7(5) . . ? C95 C96 C97 121.3(5) . . ? C98 C97 C96 119.3(5) . . ? C97 C98 C99 121.4(5) . . ? C98 C99 C94 119.9(4) . . ? C98 C99 C100 120.5(4) . . ? C94 C99 C100 119.5(4) . . ? C101 C100 C99 120.5(4) . . ? C100 C101 C102 121.9(4) . . ? O12 C102 C93 123.8(4) . . ? O12 C102 C101 117.0(4) . . ? C93 C102 C101 119.2(4) . . ? C104 C103 C108 122.1(4) . . ? C104 C103 S4 119.5(3) . . ? C108 C103 S4 117.6(3) . . ? C103 C104 C105 119.7(4) . . ? C106 C105 C104 118.4(4) . . ? C106 C105 N7 124.1(4) . . ? C104 C105 N7 117.3(3) . . ? C107 C106 C105 121.2(4) . . ? C106 C107 C108 121.4(4) . . ? C107 C108 C103 117.1(4) . . ? N7 C109 C110 127.8(4) . . ? C119 C110 C109 122.0(4) . . ? C119 C110 C111 119.0(4) . . ? C109 C110 C111 118.7(4) . . ? C112 C111 C116 117.3(4) . . ? C112 C111 C110 123.4(4) . . ? C116 C111 C110 119.3(4) . . ? C113 C112 C111 121.1(5) . . ? C112 C113 C114 121.2(5) . . ? C115 C114 C113 119.3(5) . . ? C114 C115 C116 120.8(5) . . ? C115 C116 C111 120.0(4) . . ? C115 C116 C117 121.0(4) . . ? C111 C116 C117 119.0(4) . . ? C118 C117 C116 122.2(4) . . ? C117 C118 C119 120.7(4) . . ? O16 C119 C110 124.0(4) . . ? O16 C119 C118 116.4(4) . . ? C110 C119 C118 119.6(4) . . ? C121 C120 C125 122.9(4) . . ? C121 C120 S4 117.4(3) . . ? C125 C120 S4 119.7(3) . . ? C122 C121 C120 116.9(4) . . ? C121 C122 C123 121.1(5) . . ? C124 C123 C122 120.8(5) . . ? C125 C124 C123 118.5(4) . . ? C125 C124 N8 119.6(4) . . ? C123 C124 N8 121.9(4) . . ? C124 C125 C120 119.7(4) . . ? N8 C126 C127 126.4(4) . . ? C136 C127 C126 120.9(4) . . ? C136 C127 C128 118.6(4) . . ? C126 C127 C128 120.4(4) . . ? C129 C128 C133 117.8(5) . . ? C129 C128 C127 122.7(5) . . ? C133 C128 C127 119.5(5) . . ? C130 C129 C128 120.7(6) . . ? C129 C130 C131 121.0(6) . . ? C132 C131 C130 119.7(5) . . ? C131 C132 C133 121.8(6) . . ? C134 C133 C128 119.6(5) . . ? C134 C133 C132 121.5(5) . . ? C128 C133 C132 119.0(5) . . ? C135 C134 C133 122.1(5) . . ? C134 C135 C136 119.8(5) . . ? O15 C136 C127 124.0(4) . . ? O15 C136 C135 115.6(4) . . ? C127 C136 C135 120.4(4) . . ? Cl3' C1S Cl3 121.1(8) . . ? Cl3' C1S Cl1 9.9(8) . . ? Cl3 C1S Cl1 112.4(7) . . ? Cl3' C1S Cl1' 105.9(7) . . ? Cl3 C1S Cl1' 118.5(7) . . ? Cl1 C1S Cl1' 108.9(5) . . ? Cl3' C1S Cl2 112.5(8) . . ? Cl3 C1S Cl2 10.5(8) . . ? Cl1 C1S Cl2 104.5(6) . . ? Cl1' C1S Cl2 128.9(6) . . ? Cl3' C1S Cl2' 109.7(6) . . ? Cl3 C1S Cl2' 93.6(6) . . ? Cl1 C1S Cl2' 107.3(5) . . ? Cl1' C1S Cl2' 30.2(3) . . ? Cl2 C1S Cl2' 103.0(5) . . ? Cl2' Cl1' C1S 78.6(8) . . ? Cl1' Cl2' C1S 71.2(7) . . ? C2S O1S C4S 120.5(10) . . ? O1S C2S C3S 112.9(10) . . ? O1S C4S C5S 118.8(8) . . ? C8S O2S C6S 117.3(12) . . ? C7S C6S O2S 116.5(16) . . ? C9S C8S O2S 117.6(14) . . ? C12S O3S C11S 122.7(16) . . ? C10S C11S O3S 94.2(14) . . ? C13S C12S O3S 112(2) . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 27.76 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 1.370 _refine_diff_density_min -0.875 _refine_diff_density_rms 0.103