# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 182/1863 data_co132 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H31 Cl4 Cu N5 O8' _chemical_formula_weight 806.95 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 16.5741(9) _cell_length_b 13.5311(7) _cell_length_c 16.0711(8) _cell_angle_alpha 90.00 _cell_angle_beta 110.4390(10) _cell_angle_gamma 90.00 _cell_volume 3377.3(3) _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 tetrahedron _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652 _exptl_absorpt_coefficient_mu 1.022 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.690 _exptl_absorpt_correction_T_max 0.763 _exptl_absorpt_process_details SADABS _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 omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22994 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.32 _reflns_number_total 8154 _reflns_number_gt 6096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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 ; Disordered solvent molecule (acetonitrile). One of the ester groups ist disordered. ; _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^)+(0.0574P)^2^+2.7495P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8154 _refine_ls_number_parameters 597 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.022 _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 0.23192(2) 0.09296(2) 0.36736(2) 0.02252(9) Uani 1 1 d . . . Cl1 Cl 0.07035(5) -0.20419(6) 0.30079(5) 0.03890(18) Uani 1 1 d . . . Cl2 Cl 0.09957(5) -0.35754(5) 0.45698(5) 0.03983(18) Uani 1 1 d . . . Cl3 Cl 0.22516(7) -0.30140(7) 0.64813(6) 0.0577(3) Uani 1 1 d . . . Cl4 Cl 0.32091(5) -0.09864(5) 0.67895(5) 0.03676(17) Uani 1 1 d . . . O1 O 0.25487(16) 0.30363(18) 0.09866(14) 0.0374(5) Uani 1 1 d . . . O2 O 0.33717(15) 0.37290(16) 0.23399(15) 0.0368(5) Uani 1 1 d . . . O3 O 0.09488(16) 0.39884(16) 0.11541(14) 0.0442(6) Uani 1 1 d . . . O4 O 0.17390(15) 0.47329(15) 0.24083(16) 0.0440(5) Uani 1 1 d . . . O5 O 0.45270(16) 0.2472(2) 0.19621(18) 0.0563(7) Uani 1 1 d . . . O6 O 0.40064(16) 0.0982(2) 0.14773(16) 0.0538(7) Uani 1 1 d . . . O7 O 0.26758(13) 0.03240(14) 0.52009(13) 0.0306(4) Uani 1 1 d . . . O8 O 0.15898(13) -0.01931(14) 0.35527(12) 0.0311(4) Uani 1 1 d . . . N1 N 0.29975(13) 0.21840(16) 0.36543(13) 0.0221(4) Uani 1 1 d . . . N2 N 0.18255(14) 0.12004(16) 0.20775(14) 0.0248(5) Uani 1 1 d . . . N3 N 0.14908(14) 0.19431(16) 0.38148(14) 0.0240(4) Uani 1 1 d . . . N4 N 0.34208(14) 0.02737(17) 0.36726(14) 0.0262(5) Uani 1 1 d . . . C1 C 0.23688(17) 0.29954(19) 0.32596(16) 0.0224(5) Uani 1 1 d . . . C2 C 0.20170(17) 0.30119(19) 0.22283(16) 0.0244(5) Uani 1 1 d . . . C3 C 0.14051(18) 0.2160(2) 0.18080(17) 0.0263(6) Uani 1 1 d . . . C4 C 0.25593(19) 0.1124(2) 0.17717(18) 0.0276(6) Uani 1 1 d . . . C5 C 0.32206(18) 0.1940(2) 0.21758(17) 0.0263(6) Uani 1 1 d . . . C6 C 0.36235(17) 0.1925(2) 0.32062(17) 0.0245(5) Uani 1 1 d . . . C7 C 0.28025(18) 0.2976(2) 0.19029(18) 0.0279(6) Uani 1 1 d . . . C8 C 0.3505(2) 0.2460(2) 0.45846(18) 0.0284(6) Uani 1 1 d . . . C9 C 0.16519(17) 0.28791(19) 0.36402(16) 0.0231(5) Uani 1 1 d . . . C10 C 0.08701(18) 0.1761(2) 0.41456(18) 0.0293(6) Uani 1 1 d . . . C11 C 0.03706(19) 0.2493(2) 0.43026(18) 0.0311(6) Uani 1 1 d . . . C12 C 0.05322(19) 0.3457(2) 0.41314(18) 0.0322(6) Uani 1 1 d . . . C13 C 0.11930(19) 0.3656(2) 0.38080(18) 0.0295(6) Uani 1 1 d . . . C14 C 0.1534(2) 0.3983(2) 0.1903(2) 0.0342(7) Uani 1 1 d . . . C15A C 0.0494(5) 0.4903(5) 0.0903(5) 0.048(2) Uani 0.484(7) 1 d P . . H15A H 0.0266 0.5105 0.1364 0.094(14) Uiso 0.484(7) 1 calc PR . . H15B H 0.0017 0.4817 0.0339 0.094(14) Uiso 0.484(7) 1 calc PR . . H15C H 0.0887 0.5412 0.0836 0.094(14) Uiso 0.484(7) 1 calc PR . . C15B C 0.1166(5) 0.5587(5) 0.2103(5) 0.056(2) Uani 0.516(7) 1 d P . . H15D H 0.1132 0.5766 0.1500 0.094(14) Uiso 0.516(7) 1 calc PR . . H15E H 0.1394 0.6147 0.2503 0.094(14) Uiso 0.516(7) 1 calc PR . . H15F H 0.0590 0.5418 0.2100 0.094(14) Uiso 0.516(7) 1 calc PR . . C16 C 0.1201(2) 0.0408(2) 0.1674(2) 0.0330(6) Uani 1 1 d . . . C17 C 0.3990(2) 0.1849(2) 0.18551(19) 0.0364(7) Uani 1 1 d . . . C18 C 0.4768(3) 0.0762(4) 0.1273(3) 0.0798(16) Uani 1 1 d . . . H18A H 0.5265 0.0708 0.1825 0.149(15) Uiso 1 1 calc R . . H18B H 0.4870 0.1293 0.0906 0.149(15) Uiso 1 1 calc R . . H18C H 0.4688 0.0135 0.0948 0.149(15) Uiso 1 1 calc R . . C19 C 0.39794(17) 0.0911(2) 0.35347(17) 0.0255(5) Uani 1 1 d . . . C20 C 0.3673(2) -0.0662(2) 0.3897(2) 0.0334(6) Uani 1 1 d . . . C21 C 0.4496(2) -0.0981(2) 0.3992(2) 0.0401(8) Uani 1 1 d . . . C22 C 0.5083(2) -0.0322(2) 0.3881(2) 0.0377(7) Uani 1 1 d . . . C23 C 0.48225(19) 0.0649(2) 0.36499(19) 0.0315(6) Uani 1 1 d . . . C24 C 0.23122(17) -0.05416(19) 0.50868(18) 0.0257(5) Uani 1 1 d . . . C25 C 0.17363(17) -0.08150(19) 0.42162(18) 0.0265(5) Uani 1 1 d . . . C26 C 0.13539(17) -0.1743(2) 0.40855(18) 0.0276(6) Uani 1 1 d . . . C27 C 0.15003(18) -0.2428(2) 0.47762(19) 0.0295(6) Uani 1 1 d . . . C28 C 0.20573(19) -0.2186(2) 0.56114(19) 0.0309(6) Uani 1 1 d . . . C29 C 0.24634(18) -0.1259(2) 0.57519(18) 0.0281(6) Uani 1 1 d . . . N5 N 0.4326(3) -0.2999(4) 0.5314(4) 0.0837(17) Uani 0.851(6) 1 d P . . C30A C 0.3749(4) -0.3388(5) 0.4776(5) 0.0591(19) Uani 0.644(8) 1 d P A 1 C31A C 0.3009(6) -0.3796(10) 0.4060(8) 0.125(6) Uani 0.644(8) 1 d P A 1 H31A H 0.2747 -0.3279 0.3622 0.036(9) Uiso 0.644(8) 1 calc PR A 1 H31B H 0.2584 -0.4043 0.4306 0.036(9) Uiso 0.644(8) 1 calc PR A 1 H31C H 0.3201 -0.4340 0.3771 0.036(9) Uiso 0.644(8) 1 calc PR A 1 C30B C 0.4248(8) -0.3160(9) 0.5925(9) 0.023(3) Uani 0.209(6) 1 d P A 2 C31B C 0.4257(11) -0.3675(12) 0.6674(10) 0.042(4) Uani 0.209(6) 1 d P A 2 H31D H 0.4051 -0.4350 0.6506 0.036(9) Uiso 0.209(6) 1 calc PR A 2 H31E H 0.3881 -0.3343 0.6941 0.036(9) Uiso 0.209(6) 1 calc PR A 2 H31F H 0.4846 -0.3695 0.7104 0.036(9) Uiso 0.209(6) 1 calc PR A 2 C30C C 0.3170(14) -0.4355(16) 0.4060(15) 0.028(5) Uani 0.149(6) 1 d PU B 3 C31C C 0.2677(15) -0.3492(15) 0.3653(15) 0.026(5) Uani 0.149(6) 1 d P B 3 H31G H 0.2066 -0.3669 0.3391 0.036(9) Uiso 0.149(6) 1 calc PR B 3 H31H H 0.2879 -0.3242 0.3188 0.036(9) Uiso 0.149(6) 1 calc PR B 3 H31I H 0.2750 -0.2979 0.4104 0.036(9) Uiso 0.149(6) 1 calc PR B 3 N5C N 0.3451(14) -0.4992(12) 0.4337(13) 0.057(8) Uani 0.149(6) 1 d P B 3 H1O H 0.257(3) 0.352(3) 0.090(3) 0.072(17) Uiso 1 1 d . . . H2O H 0.382(4) 0.365(5) 0.222(4) 0.14(2) Uiso 1 1 d . . . H1 H 0.2641(19) 0.358(2) 0.3466(18) 0.023(7) Uiso 1 1 d . . . H3A H 0.0881(18) 0.215(2) 0.1996(18) 0.020(7) Uiso 1 1 d . . . H3B H 0.127(2) 0.220(2) 0.121(2) 0.037(9) Uiso 1 1 d . . . H4A H 0.235(2) 0.116(2) 0.113(2) 0.029(8) Uiso 1 1 d . . . H4B H 0.2815(18) 0.052(2) 0.1898(18) 0.022(7) Uiso 1 1 d . . . H6 H 0.4091(18) 0.244(2) 0.3368(17) 0.016(6) Uiso 1 1 d . . . H8A H 0.385(2) 0.192(2) 0.487(2) 0.029(8) Uiso 1 1 d . . . H8B H 0.316(2) 0.261(2) 0.484(2) 0.031(8) Uiso 1 1 d . . . H8C H 0.382(2) 0.304(2) 0.457(2) 0.031(8) Uiso 1 1 d . . . H10 H 0.0840(19) 0.114(2) 0.428(2) 0.025(8) Uiso 1 1 d . . . H11 H -0.002(2) 0.233(2) 0.449(2) 0.035(9) Uiso 1 1 d . . . H12 H 0.022(2) 0.403(2) 0.422(2) 0.038(9) Uiso 1 1 d . . . H13 H 0.134(2) 0.429(2) 0.369(2) 0.031(8) Uiso 1 1 d . . . H16A H 0.148(2) -0.022(3) 0.185(2) 0.038(9) Uiso 1 1 d . . . H16B H 0.069(2) 0.047(2) 0.186(2) 0.038(9) Uiso 1 1 d . . . H16C H 0.098(2) 0.047(2) 0.100(2) 0.038(9) Uiso 1 1 d . . . H20 H 0.3280(19) -0.107(2) 0.3983(19) 0.019(7) Uiso 1 1 d . . . H21 H 0.465(2) -0.161(3) 0.414(2) 0.051(10) Uiso 1 1 d . . . H22 H 0.566(2) -0.050(2) 0.3989(19) 0.029(8) Uiso 1 1 d . . . H23 H 0.522(2) 0.113(2) 0.3539(19) 0.027(8) Uiso 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 0.02387(16) 0.02276(16) 0.02366(16) 0.00436(12) 0.01173(12) 0.00385(12) Cl1 0.0365(4) 0.0467(4) 0.0320(4) -0.0019(3) 0.0101(3) -0.0108(3) Cl2 0.0473(4) 0.0303(4) 0.0471(4) -0.0037(3) 0.0232(4) -0.0132(3) Cl3 0.0835(7) 0.0417(5) 0.0405(4) 0.0149(4) 0.0122(4) -0.0203(4) Cl4 0.0424(4) 0.0371(4) 0.0291(3) -0.0005(3) 0.0104(3) -0.0070(3) O1 0.0552(15) 0.0364(13) 0.0306(11) 0.0187(10) 0.0276(10) 0.0215(11) O2 0.0356(12) 0.0351(11) 0.0450(12) 0.0152(9) 0.0207(10) 0.0030(9) O3 0.0565(15) 0.0435(13) 0.0305(11) 0.0128(9) 0.0124(10) 0.0259(11) O4 0.0487(14) 0.0263(11) 0.0531(13) 0.0094(10) 0.0129(11) 0.0137(10) O5 0.0446(14) 0.0748(18) 0.0650(16) 0.0225(14) 0.0388(13) 0.0102(13) O6 0.0509(15) 0.0721(18) 0.0463(14) -0.0007(12) 0.0270(12) 0.0282(13) O7 0.0365(11) 0.0229(9) 0.0353(10) 0.0008(8) 0.0162(9) -0.0026(8) O8 0.0322(11) 0.0309(10) 0.0298(10) 0.0091(8) 0.0103(8) 0.0000(8) N1 0.0221(11) 0.0265(11) 0.0195(10) 0.0069(8) 0.0096(8) 0.0060(9) N2 0.0290(12) 0.0228(11) 0.0232(10) 0.0021(8) 0.0096(9) 0.0072(9) N3 0.0235(11) 0.0295(12) 0.0202(10) 0.0015(8) 0.0092(9) 0.0029(9) N4 0.0274(12) 0.0296(12) 0.0245(11) 0.0100(9) 0.0127(9) 0.0092(9) C1 0.0254(13) 0.0231(13) 0.0213(12) 0.0018(10) 0.0113(10) 0.0038(10) C2 0.0297(14) 0.0263(13) 0.0211(12) 0.0069(10) 0.0137(10) 0.0098(11) C3 0.0321(15) 0.0305(14) 0.0162(12) 0.0059(10) 0.0084(10) 0.0114(11) C4 0.0344(15) 0.0268(14) 0.0221(13) 0.0048(10) 0.0105(11) 0.0131(11) C5 0.0306(14) 0.0303(14) 0.0237(12) 0.0099(10) 0.0167(11) 0.0125(11) C6 0.0255(13) 0.0280(13) 0.0237(12) 0.0085(10) 0.0133(10) 0.0077(11) C7 0.0326(15) 0.0290(14) 0.0278(13) 0.0106(11) 0.0176(11) 0.0107(11) C8 0.0278(14) 0.0360(16) 0.0215(12) 0.0018(11) 0.0088(11) 0.0026(13) C9 0.0265(13) 0.0262(13) 0.0166(11) 0.0017(9) 0.0077(10) 0.0031(10) C10 0.0271(14) 0.0350(16) 0.0278(13) 0.0025(12) 0.0119(11) -0.0012(12) C11 0.0233(13) 0.0491(18) 0.0237(13) -0.0006(12) 0.0118(11) 0.0021(12) C12 0.0303(15) 0.0408(17) 0.0261(13) -0.0016(12) 0.0107(11) 0.0113(13) C13 0.0314(15) 0.0312(15) 0.0271(13) 0.0009(11) 0.0118(11) 0.0061(12) C14 0.0440(17) 0.0302(15) 0.0397(16) 0.0154(13) 0.0289(14) 0.0160(13) C15A 0.050(4) 0.047(4) 0.047(4) 0.019(3) 0.017(3) 0.034(3) C15B 0.075(5) 0.031(3) 0.061(5) 0.011(3) 0.021(4) 0.029(3) C16 0.0391(17) 0.0277(15) 0.0288(14) -0.0022(11) 0.0073(13) 0.0034(13) C17 0.0372(17) 0.0511(19) 0.0278(14) 0.0210(13) 0.0202(13) 0.0212(15) C18 0.052(2) 0.138(5) 0.053(2) -0.011(3) 0.0221(19) 0.050(3) C19 0.0265(13) 0.0308(14) 0.0219(12) 0.0087(10) 0.0117(10) 0.0084(11) C20 0.0357(16) 0.0334(15) 0.0358(15) 0.0146(12) 0.0186(13) 0.0090(13) C21 0.0435(18) 0.0375(17) 0.0445(17) 0.0205(14) 0.0219(15) 0.0203(14) C22 0.0323(16) 0.0467(18) 0.0392(16) 0.0156(14) 0.0190(13) 0.0200(14) C23 0.0285(14) 0.0394(16) 0.0300(14) 0.0118(12) 0.0146(12) 0.0107(12) C24 0.0255(13) 0.0221(12) 0.0336(14) 0.0022(11) 0.0157(11) 0.0019(10) C25 0.0247(13) 0.0258(13) 0.0331(14) 0.0055(11) 0.0152(11) 0.0030(10) C26 0.0245(13) 0.0305(14) 0.0301(13) 0.0007(11) 0.0125(11) -0.0011(11) C27 0.0324(15) 0.0242(13) 0.0376(15) -0.0003(11) 0.0194(12) -0.0067(11) C28 0.0332(15) 0.0286(14) 0.0338(14) 0.0074(11) 0.0154(12) -0.0012(12) C29 0.0289(14) 0.0301(14) 0.0276(13) -0.0018(11) 0.0128(11) -0.0017(11) N5 0.057(3) 0.123(5) 0.073(3) 0.011(3) 0.025(3) -0.019(3) C30A 0.046(4) 0.057(4) 0.087(5) -0.009(3) 0.038(4) -0.002(3) C31A 0.045(6) 0.206(16) 0.128(10) -0.094(10) 0.037(6) -0.014(7) C30B 0.021(6) 0.016(6) 0.033(7) -0.007(5) 0.011(5) -0.005(4) C31B 0.058(10) 0.037(8) 0.040(8) 0.000(6) 0.027(8) 0.013(7) C30C 0.029(5) 0.028(5) 0.028(5) -0.0005(10) 0.010(2) 0.0000(10) C31C 0.031(12) 0.014(8) 0.034(11) -0.008(7) 0.015(9) 0.011(8) N5C 0.064(14) 0.016(8) 0.048(11) 0.013(8) -0.034(10) -0.002(8) _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 O8 1.909(2) . ? Cu1 N3 2.009(2) . ? Cu1 N4 2.031(2) . ? Cu1 N1 2.042(2) . ? Cu1 N2 2.433(2) . ? Cl1 C26 1.738(3) . ? Cl2 C27 1.739(3) . ? Cl3 C28 1.732(3) . ? Cl4 C29 1.733(3) . ? O1 C7 1.385(3) . ? O1 H1O 0.67(4) . ? O2 C7 1.400(4) . ? O2 H2O 0.84(6) . ? O3 C14 1.255(4) . ? O3 C15A 1.432(6) . ? O4 C14 1.269(4) . ? O4 C15B 1.467(6) . ? O5 C17 1.194(4) . ? O6 C17 1.326(4) . ? O6 C18 1.443(4) . ? O7 C24 1.301(3) . ? O8 C25 1.313(3) . ? N1 C8 1.485(3) . ? N1 C1 1.494(3) . ? N1 C6 1.497(3) . ? N2 C3 1.465(3) . ? N2 C4 1.466(3) . ? N2 C16 1.474(4) . ? N3 C10 1.336(3) . ? N3 C9 1.344(3) . ? N4 C19 1.339(3) . ? N4 C20 1.342(4) . ? C1 C9 1.523(3) . ? C1 C2 1.553(3) . ? C1 H1 0.92(3) . ? C2 C3 1.528(4) . ? C2 C14 1.532(4) . ? C2 C7 1.564(4) . ? C3 H3A 1.01(3) . ? C3 H3B 0.90(3) . ? C4 C5 1.532(4) . ? C4 H4A 0.97(3) . ? C4 H4B 0.91(3) . ? C5 C17 1.537(4) . ? C5 C6 1.554(4) . ? C5 C7 1.557(4) . ? C6 C19 1.515(3) . ? C6 H6 1.00(3) . ? C8 H8A 0.94(3) . ? C8 H8B 0.85(3) . ? C8 H8C 0.95(3) . ? C9 C13 1.378(4) . ? C10 C11 1.370(4) . ? C10 H10 0.87(3) . ? C11 C12 1.379(4) . ? C11 H11 0.84(3) . ? C12 C13 1.393(4) . ? C12 H12 0.97(3) . ? C13 H13 0.93(3) . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? C16 H16A 0.97(3) . ? C16 H16B 0.99(3) . ? C16 H16C 1.02(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C23 1.390(4) . ? C20 C21 1.388(4) . ? C20 H20 0.90(3) . ? C21 C22 1.376(5) . ? C21 H21 0.90(4) . ? C22 C23 1.392(4) . ? C22 H22 0.95(3) . ? C23 H23 0.99(3) . ? C24 C29 1.400(4) . ? C24 C25 1.440(4) . ? C25 C26 1.389(4) . ? C26 C27 1.401(4) . ? C27 C28 1.377(4) . ? C28 C29 1.405(4) . ? N5 C30B 1.057(14) . ? N5 C30A 1.167(8) . ? C30A C31A 1.466(11) . ? C31A H31A 0.9800 . ? C31A H31B 0.9800 . ? C31A H31C 0.9800 . ? C30B C31B 1.39(2) . ? C31B H31D 0.9800 . ? C31B H31E 0.9800 . ? C31B H31F 0.9800 . ? C30C N5C 1.01(3) . ? C30C C31C 1.44(3) . ? C31C H31G 0.9800 . ? C31C H31H 0.9800 . ? C31C H31I 0.9800 . ? 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 O8 Cu1 N3 96.97(9) . . ? O8 Cu1 N4 100.93(9) . . ? N3 Cu1 N4 161.58(9) . . ? O8 Cu1 N1 172.97(8) . . ? N3 Cu1 N1 80.56(9) . . ? N4 Cu1 N1 82.15(9) . . ? O8 Cu1 N2 92.56(8) . . ? N3 Cu1 N2 91.42(8) . . ? N4 Cu1 N2 92.09(8) . . ? N1 Cu1 N2 80.97(8) . . ? C7 O1 H1O 105(4) . . ? C7 O2 H2O 107(5) . . ? C14 O3 C15A 115.4(4) . . ? C14 O4 C15B 114.7(4) . . ? C17 O6 C18 116.6(3) . . ? C25 O8 Cu1 119.78(17) . . ? C8 N1 C1 107.9(2) . . ? C8 N1 C6 107.4(2) . . ? C1 N1 C6 117.75(19) . . ? C8 N1 Cu1 108.37(16) . . ? C1 N1 Cu1 108.13(16) . . ? C6 N1 Cu1 106.90(16) . . ? C3 N2 C4 109.2(2) . . ? C3 N2 C16 109.0(2) . . ? C4 N2 C16 109.8(2) . . ? C3 N2 Cu1 113.28(15) . . ? C4 N2 Cu1 109.26(15) . . ? C16 N2 Cu1 106.26(17) . . ? C10 N3 C9 119.6(2) . . ? C10 N3 Cu1 124.79(19) . . ? C9 N3 Cu1 115.23(17) . . ? C19 N4 C20 118.9(2) . . ? C19 N4 Cu1 113.13(17) . . ? C20 N4 Cu1 127.4(2) . . ? N1 C1 C9 106.25(19) . . ? N1 C1 C2 114.2(2) . . ? C9 C1 C2 112.0(2) . . ? N1 C1 H1 107.6(18) . . ? C9 C1 H1 107.3(18) . . ? C2 C1 H1 109.1(18) . . ? C3 C2 C14 108.0(2) . . ? C3 C2 C1 113.9(2) . . ? C14 C2 C1 109.4(2) . . ? C3 C2 C7 109.3(2) . . ? C14 C2 C7 108.0(2) . . ? C1 C2 C7 108.1(2) . . ? N2 C3 C2 111.3(2) . . ? N2 C3 H3A 105.8(15) . . ? C2 C3 H3A 112.3(15) . . ? N2 C3 H3B 107(2) . . ? C2 C3 H3B 107(2) . . ? H3A C3 H3B 113(3) . . ? N2 C4 C5 111.2(2) . . ? N2 C4 H4A 108.6(18) . . ? C5 C4 H4A 110.7(18) . . ? N2 C4 H4B 111.4(18) . . ? C5 C4 H4B 110.1(18) . . ? H4A C4 H4B 105(2) . . ? C4 C5 C17 110.8(2) . . ? C4 C5 C6 114.8(2) . . ? C17 C5 C6 105.0(2) . . ? C4 C5 C7 110.3(2) . . ? C17 C5 C7 108.5(2) . . ? C6 C5 C7 107.2(2) . . ? N1 C6 C19 107.2(2) . . ? N1 C6 C5 113.4(2) . . ? C19 C6 C5 110.7(2) . . ? N1 C6 H6 108.5(15) . . ? C19 C6 H6 111.3(15) . . ? C5 C6 H6 105.8(15) . . ? O1 C7 O2 113.1(2) . . ? O1 C7 C5 107.0(2) . . ? O2 C7 C5 111.0(2) . . ? O1 C7 C2 112.0(2) . . ? O2 C7 C2 107.7(2) . . ? C5 C7 C2 105.9(2) . . ? N1 C8 H8A 109.2(18) . . ? N1 C8 H8B 108(2) . . ? H8A C8 H8B 110(3) . . ? N1 C8 H8C 107.9(19) . . ? H8A C8 H8C 115(3) . . ? H8B C8 H8C 107(3) . . ? N3 C9 C13 121.0(2) . . ? N3 C9 C1 114.9(2) . . ? C13 C9 C1 124.1(2) . . ? N3 C10 C11 122.6(3) . . ? N3 C10 H10 114(2) . . ? C11 C10 H10 124(2) . . ? C10 C11 C12 118.4(3) . . ? C10 C11 H11 118(2) . . ? C12 C11 H11 124(2) . . ? C11 C12 C13 119.4(3) . . ? C11 C12 H12 125(2) . . ? C13 C12 H12 115(2) . . ? C9 C13 C12 119.0(3) . . ? C9 C13 H13 118(2) . . ? C12 C13 H13 123(2) . . ? O3 C14 O4 123.6(3) . . ? O3 C14 C2 118.0(3) . . ? O4 C14 C2 118.4(3) . . ? O3 C15A H15A 109.5 . . ? O3 C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? O3 C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? O4 C15B H15D 109.5 . . ? O4 C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? O4 C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? N2 C16 H16A 108.8(19) . . ? N2 C16 H16B 110.6(19) . . ? H16A C16 H16B 111(3) . . ? N2 C16 H16C 110.1(19) . . ? H16A C16 H16C 110(3) . . ? H16B C16 H16C 107(3) . . ? O5 C17 O6 123.8(3) . . ? O5 C17 C5 124.0(3) . . ? O6 C17 C5 112.1(3) . . ? O6 C18 H18A 109.5 . . ? O6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 C23 122.4(2) . . ? N4 C19 C6 115.7(2) . . ? C23 C19 C6 121.9(2) . . ? N4 C20 C21 121.7(3) . . ? N4 C20 H20 116.2(18) . . ? C21 C20 H20 122.1(18) . . ? C22 C21 C20 119.8(3) . . ? C22 C21 H21 120(2) . . ? C20 C21 H21 120(2) . . ? C21 C22 C23 118.6(3) . . ? C21 C22 H22 122.0(19) . . ? C23 C22 H22 119.3(19) . . ? C19 C23 C22 118.7(3) . . ? C19 C23 H23 121.3(17) . . ? C22 C23 H23 119.9(17) . . ? O7 C24 C29 124.5(3) . . ? O7 C24 C25 119.1(2) . . ? C29 C24 C25 116.4(2) . . ? O8 C25 C26 120.8(2) . . ? O8 C25 C24 119.8(2) . . ? C26 C25 C24 119.5(2) . . ? C25 C26 C27 122.3(3) . . ? C25 C26 Cl1 116.9(2) . . ? C27 C26 Cl1 120.7(2) . . ? C28 C27 C26 119.1(2) . . ? C28 C27 Cl2 120.8(2) . . ? C26 C27 Cl2 120.1(2) . . ? C27 C28 C29 119.3(2) . . ? C27 C28 Cl3 120.4(2) . . ? C29 C28 Cl3 120.3(2) . . ? C24 C29 C28 123.3(3) . . ? C24 C29 Cl4 117.7(2) . . ? C28 C29 Cl4 119.0(2) . . ? C30B N5 C30A 105.2(8) . . ? N5 C30A C31A 175.1(9) . . ? N5 C30B C31B 160.4(13) . . ? C30B C31B H31D 109.5 . . ? C30B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? C30B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? N5C C30C C31C 174(3) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.420 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.077 #============================================================================== data_co81 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H61 Cl6 Cu2 N9 O23' _chemical_formula_weight 1555.91 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)/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 12.1045(2) _cell_length_b 33.7116(5) _cell_length_c 15.8529(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.7980(10) _cell_angle_gamma 90.00 _cell_volume 6282.29(16) _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 column _exptl_crystal_colour blue _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3192 _exptl_absorpt_coefficient_mu 1.020 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.804 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details SADABS _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 omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51932 _diffrn_reflns_av_R_equivalents 0.103 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 21.97 _reflns_number_total 7686 _reflns_number_gt 4913 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0918P)^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 7686 _refine_ls_number_parameters 901 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1539 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.001 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 0.59846(7) 0.15718(2) 0.69603(5) 0.0283(3) Uani 1 1 d . . . Cu2 Cu 0.59515(7) 0.33362(2) 0.69718(5) 0.0269(2) Uani 1 1 d . . . Cl1 Cl 0.58610(17) 0.33743(5) 0.89885(12) 0.0445(5) Uani 1 1 d . . . Cl2 Cl 0.66823(16) 0.29030(6) 1.07298(11) 0.0455(5) Uani 1 1 d . . . Cl3 Cl 0.70386(16) 0.19843(6) 1.06677(11) 0.0436(5) Uani 1 1 d . . . Cl4 Cl 0.67875(15) 0.15638(5) 0.88730(11) 0.0386(5) Uani 1 1 d . . . O1 O 0.5634(4) 0.04916(15) 0.4786(3) 0.0476(14) Uani 1 1 d . . . O2 O 0.4767(4) 0.09817(16) 0.3829(3) 0.0485(14) Uani 1 1 d . . . O3 O 0.7377(5) 0.13417(17) 0.3976(4) 0.0624(17) Uani 1 1 d . . . O4 O 0.7767(5) 0.07580(17) 0.4626(3) 0.0600(17) Uani 1 1 d . . . O5 O 0.2432(5) 0.09354(16) 0.4586(4) 0.0693(19) Uani 1 1 d . . . O6 O 0.3410(4) 0.03894(15) 0.4983(4) 0.0558(16) Uani 1 1 d . . . O7 O 0.6735(4) 0.43432(13) 0.4925(3) 0.0348(12) Uani 1 1 d . . . O8 O 0.6193(4) 0.38473(14) 0.3889(3) 0.0361(12) Uani 1 1 d . . . O9 O 0.3711(4) 0.40538(14) 0.3859(3) 0.0511(15) Uani 1 1 d . . . O10 O 0.4345(4) 0.45572(14) 0.4755(3) 0.0380(12) Uani 1 1 d . . . O11 O 0.8618(4) 0.33307(15) 0.4703(3) 0.0377(12) Uani 1 1 d . . . O13 O 0.5902(4) 0.20998(13) 0.7357(3) 0.0332(12) Uani 1 1 d . . . O12 O 0.8821(4) 0.39722(15) 0.5073(3) 0.0386(12) Uani 1 1 d . . . O14 O 0.5421(4) 0.28690(13) 0.7407(3) 0.0299(11) Uani 1 1 d . . . O23 O 0.7961(5) 0.4754(2) 0.3955(5) 0.090(2) Uani 1 1 d D . . N1 N 0.6118(4) 0.10047(16) 0.6572(3) 0.0292(14) Uani 1 1 d . . . N2 N 0.5188(4) 0.16869(15) 0.5471(3) 0.0281(14) Uani 1 1 d . . . N3 N 0.7607(5) 0.15874(17) 0.6870(4) 0.0340(15) Uani 1 1 d . . . N4 N 0.4506(5) 0.13766(17) 0.7131(3) 0.0299(14) Uani 1 1 d . . . N5 N 0.6490(4) 0.38690(15) 0.6628(3) 0.0259(14) Uani 1 1 d . . . N6 N 0.5589(4) 0.32026(15) 0.5460(3) 0.0265(14) Uani 1 1 d . . . N7 N 0.4492(5) 0.36466(17) 0.6841(3) 0.0303(14) Uani 1 1 d . . . N8 N 0.7636(4) 0.32221(16) 0.7213(3) 0.0284(14) Uani 1 1 d . . . N9 N 0.6879(6) 0.2568(2) 0.3322(6) 0.070(2) Uani 1 1 d . . . C1 C 0.6922(5) 0.1010(2) 0.5988(4) 0.0308(18) Uani 1 1 d . . . H1 H 0.7231 0.0736 0.5961 0.008(7) Uiso 1 1 calc R . . C2 C 0.6371(6) 0.1150(2) 0.5054(4) 0.0322(18) Uani 1 1 d . . . C3 C 0.6020(6) 0.15911(19) 0.4968(4) 0.0313(17) Uani 1 1 d . . . H3A H 0.6704 0.1758 0.5171 0.012(5) Uiso 1 1 calc R . . H3B H 0.5692 0.1653 0.4349 0.012(5) Uiso 1 1 calc R . . C4 C 0.4170(6) 0.14357(19) 0.5161(4) 0.0313(18) Uani 1 1 d . . . H4A H 0.3828 0.1497 0.4544 0.012(5) Uiso 1 1 calc R . . H4B H 0.3601 0.1500 0.5497 0.012(5) Uiso 1 1 calc R . . C5 C 0.4441(6) 0.0997(2) 0.5251(4) 0.0320(18) Uani 1 1 d . . . C6 C 0.4946(5) 0.0858(2) 0.6207(4) 0.0284(17) Uani 1 1 d . . . H6 H 0.4944 0.0562 0.6230 0.008(7) Uiso 1 1 calc R . . C7 C 0.5294(6) 0.0890(2) 0.4704(4) 0.0365(19) Uani 1 1 d . . . C8 C 0.6629(6) 0.0751(2) 0.7337(4) 0.0358(19) Uani 1 1 d . . . H8A H 0.6122 0.0746 0.7736 0.029(7) Uiso 1 1 calc R . . H8B H 0.7368 0.0861 0.7638 0.029(7) Uiso 1 1 calc R . . H8C H 0.6731 0.0481 0.7141 0.029(7) Uiso 1 1 calc R . . C9 C 0.7900(6) 0.1285(2) 0.6411(4) 0.0326(18) Uani 1 1 d . . . C10 C 0.8415(6) 0.1851(2) 0.7241(5) 0.041(2) Uani 1 1 d . . . H10 H 0.8216 0.2062 0.7574 0.027(4) Uiso 1 1 calc R . . C11 C 0.9502(6) 0.1827(3) 0.7155(5) 0.050(2) Uani 1 1 d . . . H11 H 1.0048 0.2020 0.7415 0.027(4) Uiso 1 1 calc R . . C12 C 0.9803(7) 0.1519(3) 0.6690(5) 0.050(2) Uani 1 1 d . . . H12 H 1.0561 0.1496 0.6625 0.027(4) Uiso 1 1 calc R . . C13 C 0.8993(6) 0.1244(2) 0.6319(4) 0.0374(19) Uani 1 1 d . . . H13 H 0.9189 0.1027 0.6001 0.027(4) Uiso 1 1 calc R . . C14 C 0.7215(7) 0.1097(3) 0.4482(5) 0.043(2) Uani 1 1 d . . . C15 C 0.8600(8) 0.0679(3) 0.4130(6) 0.078(3) Uani 1 1 d . . . H15A H 0.8328 0.0464 0.3716 0.107(10) Uiso 1 1 calc R . . H15B H 0.9321 0.0601 0.4523 0.107(10) Uiso 1 1 calc R . . H15C H 0.8716 0.0919 0.3812 0.107(10) Uiso 1 1 calc R . . C16 C 0.3311(7) 0.0769(3) 0.4890(5) 0.044(2) Uani 1 1 d . . . C17 C 0.2350(8) 0.0185(3) 0.4659(7) 0.097(4) Uani 1 1 d . . . H17A H 0.1735 0.0331 0.4826 0.107(10) Uiso 1 1 calc R . . H17B H 0.2400 -0.0082 0.4906 0.107(10) Uiso 1 1 calc R . . H17C H 0.2194 0.0168 0.4024 0.107(10) Uiso 1 1 calc R . . C18 C 0.4198(6) 0.1021(2) 0.6780(4) 0.0312(18) Uani 1 1 d . . . C19 C 0.3837(6) 0.1553(2) 0.7574(4) 0.0375(19) Uani 1 1 d . . . H19 H 0.4058 0.1805 0.7826 0.027(4) Uiso 1 1 calc R . . C20 C 0.2856(6) 0.1390(2) 0.7682(4) 0.0362(19) Uani 1 1 d . . . H20 H 0.2384 0.1530 0.7980 0.027(4) Uiso 1 1 calc R . . C21 C 0.2562(6) 0.1017(2) 0.7349(5) 0.040(2) Uani 1 1 d . . . H21 H 0.1897 0.0891 0.7439 0.027(4) Uiso 1 1 calc R . . C22 C 0.3221(6) 0.0830(2) 0.6893(5) 0.0383(19) Uani 1 1 d . . . H22 H 0.3021 0.0574 0.6653 0.027(4) Uiso 1 1 calc R . . C23 C 0.4782(5) 0.21050(19) 0.5344(4) 0.0317(18) Uani 1 1 d . . . H23A H 0.4251 0.2150 0.5723 0.021(7) Uiso 1 1 calc R . . H23B H 0.4334 0.2131 0.4736 0.021(7) Uiso 1 1 calc R . . C24 C 0.5660(5) 0.24400(18) 0.5515(4) 0.0276(17) Uani 1 1 d . . . H24A H 0.6046 0.2452 0.6140 0.021(7) Uiso 1 1 calc R . . H24B H 0.6240 0.2398 0.5178 0.021(7) Uiso 1 1 calc R . . C25 C 0.5000(5) 0.28210(18) 0.5231(4) 0.0275(17) Uani 1 1 d . . . H25A H 0.4722 0.2812 0.4591 0.021(7) Uiso 1 1 calc R . . H25B H 0.4322 0.2820 0.5477 0.021(7) Uiso 1 1 calc R . . C26 C 0.6051(5) 0.2268(2) 0.8123(4) 0.0278(17) Uani 1 1 d . . . C27 C 0.5827(5) 0.2680(2) 0.8145(4) 0.0283(17) Uani 1 1 d . . . C28 C 0.6055(5) 0.2871(2) 0.8955(4) 0.0301(17) Uani 1 1 d . . . C29 C 0.6456(5) 0.2656(2) 0.9735(4) 0.0314(18) Uani 1 1 d . . . C30 C 0.6626(5) 0.2257(2) 0.9718(4) 0.0294(17) Uani 1 1 d . . . C31 C 0.6452(5) 0.2063(2) 0.8913(4) 0.0302(17) Uani 1 1 d . . . C32 C 0.5487(5) 0.4072(2) 0.6046(4) 0.0282(17) Uani 1 1 d . . . H32 H 0.5638 0.4364 0.6056 0.008(7) Uiso 1 1 calc R . . C33 C 0.5249(5) 0.39256(19) 0.5097(4) 0.0259(16) Uani 1 1 d . . . C34 C 0.4792(5) 0.35004(19) 0.4973(4) 0.0275(17) Uani 1 1 d . . . H34A H 0.4070 0.3486 0.5162 0.012(5) Uiso 1 1 calc R . . H34B H 0.4622 0.3434 0.4347 0.012(5) Uiso 1 1 calc R . . C35 C 0.6650(5) 0.32261(19) 0.5172(4) 0.0262(17) Uani 1 1 d . . . H35A H 0.6494 0.3156 0.4548 0.012(5) Uiso 1 1 calc R . . H35B H 0.7195 0.3029 0.5497 0.012(5) Uiso 1 1 calc R . . C36 C 0.7197(5) 0.36414(19) 0.5305(4) 0.0268(17) Uani 1 1 d . . . C37 C 0.7499(5) 0.37908(19) 0.6269(4) 0.0259(16) Uani 1 1 d . . . H37 H 0.7953 0.4041 0.6302 0.008(7) Uiso 1 1 calc R . . C38 C 0.6351(6) 0.3956(2) 0.4776(4) 0.0287(17) Uani 1 1 d . . . C39 C 0.6883(6) 0.41141(19) 0.7427(4) 0.0308(17) Uani 1 1 d . . . H39A H 0.7498 0.3975 0.7835 0.029(7) Uiso 1 1 calc R . . H39B H 0.6247 0.4157 0.7700 0.029(7) Uiso 1 1 calc R . . H39C H 0.7162 0.4370 0.7272 0.029(7) Uiso 1 1 calc R . . C40 C 0.4490(6) 0.3998(2) 0.6426(4) 0.0284(17) Uani 1 1 d . . . C41 C 0.3609(6) 0.3553(2) 0.7167(4) 0.0298(17) Uani 1 1 d . . . H41 H 0.3620 0.3307 0.7459 0.027(4) Uiso 1 1 calc R . . C42 C 0.2682(6) 0.3796(2) 0.7098(4) 0.0357(19) Uani 1 1 d . . . H42 H 0.2057 0.3716 0.7325 0.027(4) Uiso 1 1 calc R . . C43 C 0.2675(6) 0.4157(2) 0.6695(4) 0.0351(18) Uani 1 1 d . . . H43 H 0.2048 0.4332 0.6644 0.027(4) Uiso 1 1 calc R . . C44 C 0.3586(6) 0.4263(2) 0.6364(4) 0.0332(18) Uani 1 1 d . . . H44 H 0.3601 0.4514 0.6095 0.027(4) Uiso 1 1 calc R . . C45 C 0.4345(6) 0.4185(2) 0.4503(5) 0.0351(19) Uani 1 1 d . . . C46 C 0.3461(6) 0.4809(2) 0.4207(5) 0.044(2) Uani 1 1 d . . . H46A H 0.3595 0.4827 0.3622 0.107(10) Uiso 1 1 calc R . . H46B H 0.3490 0.5074 0.4461 0.107(10) Uiso 1 1 calc R . . H46C H 0.2711 0.4691 0.4173 0.107(10) Uiso 1 1 calc R . . C47 C 0.8283(6) 0.3625(2) 0.4980(4) 0.0336(18) Uani 1 1 d . . . C48 C 0.9856(6) 0.3991(2) 0.4788(5) 0.050(2) Uani 1 1 d . . . H48A H 1.0388 0.3790 0.5095 0.107(10) Uiso 1 1 calc R . . H48B H 1.0196 0.4255 0.4912 0.107(10) Uiso 1 1 calc R . . H48C H 0.9694 0.3941 0.4161 0.107(10) Uiso 1 1 calc R . . C49 C 0.8221(6) 0.3478(2) 0.6839(4) 0.0264(17) Uani 1 1 d . . . C50 C 0.8221(6) 0.2925(2) 0.7693(4) 0.0321(18) Uani 1 1 d . . . H50 H 0.7820 0.2740 0.7961 0.027(4) Uiso 1 1 calc R . . C51 C 0.9376(6) 0.2881(2) 0.7807(4) 0.0343(18) Uani 1 1 d . . . H51 H 0.9762 0.2667 0.8144 0.027(4) Uiso 1 1 calc R . . C52 C 0.9962(6) 0.3145(2) 0.7433(4) 0.0354(19) Uani 1 1 d . . . H52 H 1.0760 0.3117 0.7504 0.027(4) Uiso 1 1 calc R . . C53 C 0.9385(5) 0.3454(2) 0.6950(4) 0.0302(17) Uani 1 1 d . . . H53 H 0.9783 0.3647 0.6699 0.027(4) Uiso 1 1 calc R . . C54 C 0.7628(7) 0.2467(2) 0.3843(7) 0.053(2) Uani 1 1 d . . . C55 C 0.8576(7) 0.2346(3) 0.4539(7) 0.075(3) Uani 1 1 d . . . H55A H 0.9215 0.2529 0.4569 0.13(2) Uiso 1 1 calc R . . H55B H 0.8808 0.2077 0.4427 0.13(2) Uiso 1 1 calc R . . H55C H 0.8346 0.2352 0.5091 0.13(2) Uiso 1 1 calc R . . Cl5 Cl 0.4892(2) 0.02407(7) 0.2283(2) 0.0809(9) Uani 1 1 d . . . Cl6 Cl 0.51584(18) 0.47880(6) 0.21390(13) 0.0461(5) Uani 1 1 d . . . O15 O 0.5392(7) 0.0624(2) 0.2511(6) 0.039(3) Uani 0.592(11) 1 d P A 1 O16 O 0.3809(10) 0.0256(3) 0.1683(8) 0.071(4) Uani 0.592(11) 1 d P A 1 O17 O 0.5447(10) -0.0083(4) 0.2286(8) 0.080(4) Uiso 0.592(11) 1 d P A 1 O18 O 0.4338(9) 0.0169(3) 0.3116(7) 0.078(4) Uani 0.592(11) 1 d P A 1 O19 O 0.4588(8) 0.5109(2) 0.2379(5) 0.071(3) Uani 0.771(11) 1 d P B 1 O20 O 0.6395(7) 0.4887(2) 0.2331(5) 0.072(3) Uani 0.771(11) 1 d P B 1 O21 O 0.5064(7) 0.4445(2) 0.2665(5) 0.057(2) Uani 0.771(11) 1 d P B 1 O22 O 0.4831(10) 0.4692(2) 0.1249(5) 0.066(3) Uani 0.771(11) 1 d P B 1 O21A O 0.560(2) 0.4613(9) 0.2907(19) 0.055(9) Uiso 0.229(11) 1 d P B 2 O20A O 0.525(2) 0.5199(8) 0.2169(18) 0.054(9) Uiso 0.229(11) 1 d P B 2 O22A O 0.549(2) 0.4649(9) 0.139(2) 0.049(9) Uiso 0.229(11) 1 d P B 2 O19A O 0.3835(19) 0.4729(7) 0.1927(15) 0.052(8) Uiso 0.229(11) 1 d P B 2 O18A O 0.5175(19) 0.0576(8) 0.1806(19) 0.134(9) Uiso 0.408(11) 1 d P A 2 O15A O 0.585(2) 0.0102(8) 0.2800(17) 0.139(9) Uiso 0.408(11) 1 d P A 2 O16A O 0.509(3) 0.0102(11) 0.122(2) 0.245(17) Uiso 0.408(11) 1 d P A 2 O17A O 0.393(3) 0.0260(10) 0.218(2) 0.143(13) Uiso 0.408(11) 1 d P A 2 H2O H 0.5614 0.1022 0.3560 0.12(2) Uiso 1 1 d . . . H7O H 0.7360 0.4400 0.4702 0.12(2) Uiso 1 1 d . . . H8O H 0.5931 0.4064 0.3660 0.12(2) Uiso 1 1 d . . . H1O H 0.5172 0.0379 0.4760 0.12(2) Uiso 1 1 d . . . H23O H 0.8529 0.4789 0.3843 0.12(2) Uiso 1 1 d 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 0.0313(5) 0.0271(5) 0.0211(5) -0.0011(4) -0.0042(4) -0.0011(4) Cu2 0.0286(5) 0.0260(5) 0.0221(5) 0.0009(4) -0.0023(4) 0.0005(4) Cl1 0.0608(13) 0.0333(11) 0.0328(11) -0.0084(9) -0.0019(9) -0.0009(9) Cl2 0.0507(12) 0.0582(14) 0.0216(10) -0.0123(9) -0.0033(9) 0.0034(10) Cl3 0.0471(11) 0.0577(13) 0.0198(10) 0.0095(9) -0.0043(8) 0.0058(10) Cl4 0.0462(11) 0.0352(11) 0.0278(10) 0.0055(9) -0.0043(8) 0.0059(9) O1 0.060(3) 0.042(4) 0.029(3) -0.007(3) -0.013(2) 0.012(3) O2 0.055(3) 0.062(4) 0.019(3) 0.003(3) -0.012(2) 0.005(3) O3 0.093(5) 0.052(4) 0.051(4) 0.013(3) 0.035(3) 0.017(3) O4 0.079(4) 0.063(4) 0.042(4) 0.014(3) 0.021(3) 0.045(3) O5 0.040(4) 0.042(4) 0.104(5) -0.009(3) -0.026(3) -0.004(3) O6 0.055(4) 0.029(4) 0.062(4) -0.003(3) -0.028(3) -0.008(3) O7 0.042(3) 0.028(3) 0.031(3) 0.003(2) 0.001(2) -0.004(2) O8 0.046(3) 0.033(3) 0.025(3) 0.002(2) 0.000(2) 0.004(2) O9 0.050(3) 0.028(3) 0.054(4) 0.000(3) -0.028(3) 0.000(2) O10 0.047(3) 0.028(3) 0.033(3) 0.005(2) -0.004(2) 0.009(2) O11 0.035(3) 0.043(3) 0.033(3) -0.006(3) 0.003(2) 0.007(2) O13 0.050(3) 0.027(3) 0.018(3) 0.000(2) -0.001(2) 0.001(2) O12 0.033(3) 0.043(3) 0.039(3) 0.000(3) 0.008(2) -0.007(2) O14 0.036(3) 0.030(3) 0.018(3) 0.001(2) -0.005(2) -0.001(2) O23 0.086(5) 0.085(5) 0.104(6) 0.018(4) 0.032(4) -0.005(4) N1 0.029(3) 0.030(4) 0.022(3) 0.004(3) -0.007(3) 0.000(3) N2 0.033(3) 0.026(3) 0.021(3) 0.006(3) -0.003(3) -0.003(3) N3 0.037(4) 0.030(4) 0.029(3) 0.000(3) -0.004(3) 0.002(3) N4 0.039(4) 0.028(4) 0.018(3) -0.003(3) -0.001(3) 0.005(3) N5 0.029(3) 0.026(3) 0.019(3) -0.003(3) -0.004(3) 0.004(3) N6 0.034(3) 0.023(3) 0.018(3) 0.001(3) -0.001(3) -0.001(3) N7 0.029(4) 0.033(4) 0.024(3) -0.007(3) -0.003(3) -0.005(3) N8 0.028(3) 0.033(4) 0.020(3) 0.000(3) -0.003(3) 0.000(3) N9 0.048(5) 0.073(6) 0.079(6) -0.020(5) -0.003(5) -0.004(4) C1 0.037(4) 0.023(4) 0.026(4) 0.003(3) -0.007(3) 0.006(3) C2 0.043(5) 0.032(5) 0.016(4) 0.004(3) -0.003(3) 0.010(3) C3 0.035(4) 0.032(4) 0.022(4) 0.009(3) -0.001(3) 0.006(3) C4 0.040(4) 0.033(4) 0.014(4) -0.001(3) -0.006(3) -0.001(3) C5 0.037(4) 0.029(4) 0.021(4) -0.002(3) -0.011(3) 0.003(3) C6 0.038(4) 0.026(4) 0.015(4) 0.003(3) -0.007(3) -0.005(3) C7 0.040(5) 0.036(5) 0.026(4) -0.001(4) -0.009(4) 0.008(4) C8 0.045(5) 0.029(4) 0.025(4) 0.006(3) -0.009(4) 0.001(3) C9 0.047(5) 0.029(5) 0.017(4) 0.005(4) -0.001(3) 0.002(4) C10 0.039(5) 0.032(5) 0.045(5) 0.004(4) -0.003(4) -0.008(4) C11 0.030(5) 0.058(6) 0.054(6) 0.001(5) -0.004(4) -0.009(4) C12 0.030(5) 0.057(6) 0.059(6) 0.010(5) 0.003(4) 0.007(4) C13 0.036(5) 0.046(5) 0.029(4) 0.008(4) 0.006(4) 0.012(4) C14 0.053(5) 0.045(6) 0.025(5) 0.000(4) -0.002(4) 0.010(4) C15 0.101(8) 0.082(8) 0.062(7) 0.026(6) 0.037(6) 0.048(6) C16 0.046(6) 0.044(6) 0.034(5) -0.008(4) -0.004(4) -0.015(4) C17 0.092(8) 0.051(7) 0.116(9) -0.001(6) -0.039(7) -0.012(6) C18 0.034(4) 0.030(5) 0.025(4) 0.006(4) -0.003(3) 0.007(4) C19 0.045(5) 0.034(5) 0.025(4) -0.001(4) -0.010(4) 0.000(4) C20 0.030(5) 0.048(5) 0.028(4) 0.000(4) 0.001(3) -0.001(4) C21 0.034(5) 0.053(6) 0.033(5) 0.008(4) 0.007(4) -0.005(4) C22 0.040(5) 0.033(5) 0.036(5) -0.001(4) -0.002(4) -0.009(4) C23 0.038(4) 0.030(5) 0.022(4) 0.002(3) -0.003(3) 0.004(3) C24 0.037(4) 0.025(4) 0.016(4) 0.005(3) -0.004(3) 0.003(3) C25 0.031(4) 0.026(4) 0.021(4) 0.002(3) -0.004(3) -0.002(3) C26 0.025(4) 0.034(5) 0.021(4) -0.002(4) -0.003(3) -0.006(3) C27 0.025(4) 0.032(5) 0.023(4) 0.000(4) -0.004(3) -0.003(3) C28 0.033(4) 0.035(5) 0.019(4) -0.001(4) 0.000(3) 0.001(3) C29 0.030(4) 0.047(5) 0.016(4) -0.008(4) 0.001(3) -0.006(3) C30 0.024(4) 0.037(5) 0.025(4) 0.012(4) 0.001(3) 0.004(3) C31 0.031(4) 0.031(4) 0.025(4) 0.004(4) -0.002(3) 0.000(3) C32 0.030(4) 0.022(4) 0.028(4) 0.000(3) -0.004(3) 0.002(3) C33 0.031(4) 0.021(4) 0.020(4) 0.004(3) -0.006(3) 0.002(3) C34 0.026(4) 0.033(4) 0.021(4) 0.001(3) 0.000(3) 0.004(3) C35 0.028(4) 0.030(4) 0.014(4) 0.004(3) -0.007(3) 0.004(3) C36 0.032(4) 0.030(4) 0.015(4) 0.000(3) -0.003(3) 0.005(3) C37 0.030(4) 0.020(4) 0.022(4) -0.003(3) -0.004(3) 0.000(3) C38 0.040(4) 0.023(4) 0.019(4) -0.001(3) -0.001(3) 0.003(3) C39 0.036(4) 0.027(4) 0.024(4) -0.001(3) -0.003(3) 0.000(3) C40 0.033(4) 0.022(4) 0.025(4) -0.004(3) -0.005(3) -0.001(3) C41 0.034(5) 0.028(4) 0.023(4) -0.006(3) -0.002(3) -0.009(4) C42 0.028(4) 0.051(5) 0.024(4) -0.010(4) -0.001(3) -0.005(4) C43 0.033(5) 0.036(5) 0.030(4) -0.002(4) -0.005(4) 0.006(4) C44 0.035(5) 0.034(5) 0.023(4) 0.001(3) -0.008(3) 0.002(4) C45 0.033(5) 0.033(5) 0.035(5) 0.005(4) -0.001(4) -0.001(4) C46 0.047(5) 0.039(5) 0.037(5) 0.007(4) -0.007(4) 0.014(4) C47 0.037(5) 0.039(5) 0.019(4) 0.006(4) -0.007(3) 0.003(4) C48 0.037(5) 0.066(6) 0.048(5) 0.002(5) 0.012(4) -0.005(4) C49 0.031(4) 0.029(4) 0.014(4) -0.005(3) -0.004(3) -0.005(3) C50 0.033(5) 0.033(5) 0.025(4) 0.003(4) -0.002(3) -0.002(3) C51 0.035(5) 0.038(5) 0.024(4) 0.007(4) -0.004(3) -0.001(4) C52 0.024(4) 0.049(5) 0.027(4) -0.004(4) -0.007(3) 0.004(4) C53 0.027(4) 0.036(5) 0.025(4) 0.001(4) 0.001(3) -0.003(3) C54 0.036(5) 0.044(6) 0.079(7) -0.016(5) 0.014(5) -0.004(4) C55 0.045(6) 0.069(7) 0.107(9) 0.000(6) 0.011(6) 0.007(5) Cl5 0.0614(17) 0.0291(13) 0.129(3) -0.0052(15) -0.0227(17) 0.0058(12) Cl6 0.0630(15) 0.0312(12) 0.0393(13) 0.0012(10) 0.0028(10) 0.0044(10) O15 0.057(6) 0.019(5) 0.042(6) -0.017(4) 0.017(4) -0.021(4) O16 0.072(8) 0.072(8) 0.043(8) -0.007(6) -0.034(6) 0.008(6) O18 0.107(9) 0.061(7) 0.080(9) -0.038(6) 0.053(7) -0.046(6) O19 0.089(7) 0.048(5) 0.064(6) -0.008(4) -0.003(5) 0.032(5) O20 0.071(6) 0.051(5) 0.087(6) 0.021(5) 0.006(5) 0.001(4) O21 0.074(6) 0.046(5) 0.042(5) 0.020(4) -0.004(4) 0.005(5) O22 0.106(9) 0.047(5) 0.033(5) -0.006(4) -0.008(5) 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 O13 1.898(4) . ? Cu1 N4 1.985(6) . ? Cu1 N3 2.004(6) . ? Cu1 N1 2.027(5) . ? Cu1 N2 2.359(5) . ? Cu2 O14 1.892(4) . ? Cu2 N8 2.020(5) . ? Cu2 N7 2.021(6) . ? Cu2 N5 2.029(5) . ? Cu2 N6 2.374(5) . ? Cl1 C28 1.716(7) . ? Cl2 C29 1.747(7) . ? Cl3 C30 1.732(7) . ? Cl4 C31 1.736(7) . ? O1 C7 1.401(8) . ? O1 H1O 0.670(6) . ? O2 C7 1.415(8) . ? O2 H2O 1.209(5) . ? O3 C14 1.198(9) . ? O4 C14 1.317(9) . ? O4 C15 1.444(9) . ? O5 C16 1.197(9) . ? O6 C16 1.292(9) . ? O6 C17 1.438(9) . ? O7 C38 1.386(8) . ? O7 H7O 0.928(5) . ? O8 C38 1.422(8) . ? O8 H8O 0.843(4) . ? O9 C45 1.205(8) . ? O10 C45 1.318(8) . ? O10 C46 1.475(7) . ? O11 C47 1.194(8) . ? O13 C26 1.312(7) . ? O12 C47 1.331(8) . ? O12 C48 1.431(8) . ? O14 C27 1.319(7) . ? O23 H23O 0.759(6) . ? N1 C6 1.483(8) . ? N1 C8 1.492(8) . ? N1 C1 1.494(8) . ? N2 C3 1.462(8) . ? N2 C4 1.479(8) . ? N2 C23 1.491(8) . ? N3 C9 1.348(8) . ? N3 C10 1.348(9) . ? N4 C19 1.331(9) . ? N4 C18 1.337(8) . ? N5 C37 1.489(8) . ? N5 C39 1.492(8) . ? N5 C32 1.503(8) . ? N6 C35 1.465(8) . ? N6 C25 1.474(8) . ? N6 C34 1.476(8) . ? N7 C41 1.331(8) . ? N7 C40 1.355(8) . ? N8 C49 1.341(8) . ? N8 C50 1.352(8) . ? N9 C54 1.123(10) . ? C1 C9 1.527(9) . ? C1 C2 1.547(9) . ? C1 H1 1.0000 . ? C2 C14 1.530(10) . ? C2 C3 1.543(9) . ? C2 C7 1.560(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.514(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C7 1.541(10) . ? C5 C16 1.554(10) . ? C5 C6 1.565(9) . ? C6 C18 1.528(10) . ? C6 H6 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C13 1.372(9) . ? C10 C11 1.357(10) . ? C10 H10 0.9500 . ? C11 C12 1.372(11) . ? C11 H11 0.9500 . ? C12 C13 1.375(10) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C22 1.395(10) . ? C19 C20 1.356(10) . ? C19 H19 0.9500 . ? C20 C21 1.376(10) . ? C20 H20 0.9500 . ? C21 C22 1.354(10) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.530(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.523(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C31 1.411(9) . ? C26 C27 1.419(9) . ? C27 C28 1.403(9) . ? C28 C29 1.415(9) . ? C29 C30 1.362(10) . ? C30 C31 1.405(9) . ? C32 C40 1.493(9) . ? C32 C33 1.543(9) . ? C32 H32 1.0000 . ? C33 C34 1.532(9) . ? C33 C45 1.535(9) . ? C33 C38 1.541(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.541(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C47 1.523(10) . ? C36 C37 1.566(9) . ? C36 C38 1.572(9) . ? C37 C49 1.522(9) . ? C37 H37 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C44 1.397(9) . ? C41 C42 1.373(9) . ? C41 H41 0.9500 . ? C42 C43 1.373(10) . ? C42 H42 0.9500 . ? C43 C44 1.376(10) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C53 1.381(9) . ? C50 C51 1.374(9) . ? C50 H50 0.9500 . ? C51 C52 1.358(9) . ? C51 H51 0.9500 . ? C52 C53 1.381(9) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 C55 1.447(13) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? Cl5 O17A 1.14(4) . ? Cl5 O17 1.280(12) . ? Cl5 O15A 1.33(3) . ? Cl5 O16 1.426(10) . ? Cl5 O15 1.435(8) . ? Cl5 O18A 1.45(3) . ? Cl5 O18 1.635(10) . ? Cl5 O16A 1.82(4) . ? Cl6 O21A 1.34(3) . ? Cl6 O19 1.386(8) . ? Cl6 O20A 1.39(3) . ? Cl6 O22 1.409(8) . ? Cl6 O22A 1.42(3) . ? Cl6 O21 1.446(7) . ? Cl6 O20 1.492(8) . ? Cl6 O19A 1.57(2) . ? 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 O13 Cu1 N4 98.3(2) . . ? O13 Cu1 N3 97.4(2) . . ? N4 Cu1 N3 161.7(2) . . ? O13 Cu1 N1 178.1(2) . . ? N4 Cu1 N1 82.4(2) . . ? N3 Cu1 N1 81.5(2) . . ? O13 Cu1 N2 97.82(18) . . ? N4 Cu1 N2 91.4(2) . . ? N3 Cu1 N2 95.6(2) . . ? N1 Cu1 N2 83.93(19) . . ? O14 Cu2 N8 100.8(2) . . ? O14 Cu2 N7 96.0(2) . . ? N8 Cu2 N7 159.4(2) . . ? O14 Cu2 N5 173.4(2) . . ? N8 Cu2 N5 81.1(2) . . ? N7 Cu2 N5 81.0(2) . . ? O14 Cu2 N6 102.31(18) . . ? N8 Cu2 N6 95.19(19) . . ? N7 Cu2 N6 92.77(19) . . ? N5 Cu2 N6 83.74(19) . . ? C7 O1 H1O 108.5(6) . . ? C7 O2 H2O 98.5(4) . . ? C14 O4 C15 117.1(7) . . ? C16 O6 C17 112.5(6) . . ? C38 O7 H7O 113.5(5) . . ? C38 O8 H8O 98.6(5) . . ? C45 O10 C46 114.9(5) . . ? C26 O13 Cu1 134.8(4) . . ? C47 O12 C48 116.5(6) . . ? C27 O14 Cu2 129.6(4) . . ? C6 N1 C8 107.4(5) . . ? C6 N1 C1 117.8(5) . . ? C8 N1 C1 107.8(5) . . ? C6 N1 Cu1 107.1(4) . . ? C8 N1 Cu1 109.9(4) . . ? C1 N1 Cu1 106.8(4) . . ? C3 N2 C4 108.7(5) . . ? C3 N2 C23 112.5(5) . . ? C4 N2 C23 105.9(5) . . ? C3 N2 Cu1 109.8(4) . . ? C4 N2 Cu1 110.3(4) . . ? C23 N2 Cu1 109.5(4) . . ? C9 N3 C10 118.5(6) . . ? C9 N3 Cu1 114.0(5) . . ? C10 N3 Cu1 127.4(5) . . ? C19 N4 C18 118.4(6) . . ? C19 N4 Cu1 127.2(5) . . ? C18 N4 Cu1 114.3(5) . . ? C37 N5 C39 107.4(5) . . ? C37 N5 C32 117.5(5) . . ? C39 N5 C32 108.4(5) . . ? C37 N5 Cu2 106.9(4) . . ? C39 N5 Cu2 108.7(4) . . ? C32 N5 Cu2 107.7(4) . . ? C35 N6 C25 112.3(5) . . ? C35 N6 C34 108.2(5) . . ? C25 N6 C34 104.3(5) . . ? C35 N6 Cu2 109.9(3) . . ? C25 N6 Cu2 112.2(4) . . ? C34 N6 Cu2 109.8(4) . . ? C41 N7 C40 119.2(6) . . ? C41 N7 Cu2 126.9(5) . . ? C40 N7 Cu2 113.7(5) . . ? C49 N8 C50 117.8(6) . . ? C49 N8 Cu2 114.1(4) . . ? C50 N8 Cu2 128.1(5) . . ? N1 C1 C9 106.6(5) . . ? N1 C1 C2 113.6(5) . . ? C9 C1 C2 110.2(5) . . ? N1 C1 H1 108.8 . . ? C9 C1 H1 108.8 . . ? C2 C1 H1 108.8 . . ? C14 C2 C3 105.6(6) . . ? C14 C2 C1 109.6(6) . . ? C3 C2 C1 115.2(6) . . ? C14 C2 C7 110.1(6) . . ? C3 C2 C7 108.7(5) . . ? C1 C2 C7 107.5(6) . . ? N2 C3 C2 112.1(5) . . ? N2 C3 H3A 109.2 . . ? C2 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N2 C4 C5 112.5(5) . . ? N2 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? N2 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C4 C5 C7 109.6(6) . . ? C4 C5 C16 107.2(6) . . ? C7 C5 C16 109.0(6) . . ? C4 C5 C6 114.1(5) . . ? C7 C5 C6 108.4(5) . . ? C16 C5 C6 108.4(6) . . ? N1 C6 C18 107.2(5) . . ? N1 C6 C5 113.2(5) . . ? C18 C6 C5 108.6(5) . . ? N1 C6 H6 109.2 . . ? C18 C6 H6 109.2 . . ? C5 C6 H6 109.2 . . ? O1 C7 O2 110.8(6) . . ? O1 C7 C5 113.2(6) . . ? O2 C7 C5 107.1(5) . . ? O1 C7 C2 107.7(5) . . ? O2 C7 C2 111.6(6) . . ? C5 C7 C2 106.5(6) . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C13 121.2(7) . . ? N3 C9 C1 114.9(6) . . ? C13 C9 C1 123.9(7) . . ? N3 C10 C11 122.4(8) . . ? N3 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C10 C11 C12 119.2(8) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C11 C12 C13 119.1(7) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C9 C13 C12 119.6(7) . . ? C9 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? O3 C14 O4 123.8(8) . . ? O3 C14 C2 123.8(7) . . ? O4 C14 C2 112.3(7) . . ? O4 C15 H15A 109.5 . . ? O4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O5 C16 O6 124.0(7) . . ? O5 C16 C5 122.5(7) . . ? O6 C16 C5 113.5(7) . . ? O6 C17 H17A 109.5 . . ? O6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C18 C22 121.3(7) . . ? N4 C18 C6 115.0(6) . . ? C22 C18 C6 123.5(6) . . ? N4 C19 C20 123.1(7) . . ? N4 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? C19 C20 C21 118.4(7) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 120.8 . . ? C22 C21 C20 119.9(7) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C18 118.7(7) . . ? C21 C22 H22 120.6 . . ? C18 C22 H22 120.6 . . ? N2 C23 C24 118.8(5) . . ? N2 C23 H23A 107.6 . . ? C24 C23 H23A 107.6 . . ? N2 C23 H23B 107.6 . . ? C24 C23 H23B 107.6 . . ? H23A C23 H23B 107.1 . . ? C25 C24 C23 106.1(5) . . ? C25 C24 H24A 110.5 . . ? C23 C24 H24A 110.5 . . ? C25 C24 H24B 110.5 . . ? C23 C24 H24B 110.5 . . ? H24A C24 H24B 108.7 . . ? N6 C25 C24 118.3(5) . . ? N6 C25 H25A 107.7 . . ? C24 C25 H25A 107.7 . . ? N6 C25 H25B 107.7 . . ? C24 C25 H25B 107.7 . . ? H25A C25 H25B 107.1 . . ? O13 C26 C31 123.5(6) . . ? O13 C26 C27 117.5(6) . . ? C31 C26 C27 119.0(6) . . ? O14 C27 C28 122.8(6) . . ? O14 C27 C26 118.9(6) . . ? C28 C27 C26 118.3(6) . . ? C27 C28 C29 121.1(6) . . ? C27 C28 Cl1 118.8(5) . . ? C29 C28 Cl1 120.0(5) . . ? C30 C29 C28 120.7(6) . . ? C30 C29 Cl2 119.8(5) . . ? C28 C29 Cl2 119.5(5) . . ? C29 C30 C31 119.1(6) . . ? C29 C30 Cl3 121.4(5) . . ? C31 C30 Cl3 119.5(5) . . ? C30 C31 C26 121.7(6) . . ? C30 C31 Cl4 119.9(5) . . ? C26 C31 Cl4 118.4(5) . . ? C40 C32 N5 106.8(5) . . ? C40 C32 C33 111.0(5) . . ? N5 C32 C33 112.9(5) . . ? C40 C32 H32 108.7 . . ? N5 C32 H32 108.7 . . ? C33 C32 H32 108.7 . . ? C34 C33 C45 105.7(5) . . ? C34 C33 C38 109.6(5) . . ? C45 C33 C38 107.8(5) . . ? C34 C33 C32 113.7(5) . . ? C45 C33 C32 110.9(6) . . ? C38 C33 C32 109.0(5) . . ? N6 C34 C33 113.5(5) . . ? N6 C34 H34A 108.9 . . ? C33 C34 H34A 108.9 . . ? N6 C34 H34B 108.9 . . ? C33 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? N6 C35 C36 112.7(5) . . ? N6 C35 H35A 109.0 . . ? C36 C35 H35A 109.0 . . ? N6 C35 H35B 109.0 . . ? C36 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C47 C36 C35 107.3(5) . . ? C47 C36 C37 108.8(5) . . ? C35 C36 C37 114.7(5) . . ? C47 C36 C38 110.4(5) . . ? C35 C36 C38 109.6(5) . . ? C37 C36 C38 105.9(5) . . ? N5 C37 C49 107.6(5) . . ? N5 C37 C36 114.1(5) . . ? C49 C37 C36 108.9(5) . . ? N5 C37 H37 108.7 . . ? C49 C37 H37 108.7 . . ? C36 C37 H37 108.7 . . ? O7 C38 O8 111.8(5) . . ? O7 C38 C33 106.8(5) . . ? O8 C38 C33 112.8(5) . . ? O7 C38 C36 113.3(5) . . ? O8 C38 C36 105.7(5) . . ? C33 C38 C36 106.5(5) . . ? N5 C39 H39A 109.5 . . ? N5 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N5 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N7 C40 C44 120.2(6) . . ? N7 C40 C32 115.7(6) . . ? C44 C40 C32 124.0(6) . . ? N7 C41 C42 123.0(7) . . ? N7 C41 H41 118.5 . . ? C42 C41 H41 118.5 . . ? C41 C42 C43 118.7(7) . . ? C41 C42 H42 120.7 . . ? C43 C42 H42 120.7 . . ? C42 C43 C44 119.3(7) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? C43 C44 C40 119.6(7) . . ? C43 C44 H44 120.2 . . ? C40 C44 H44 120.2 . . ? O9 C45 O10 124.0(6) . . ? O9 C45 C33 121.9(7) . . ? O10 C45 C33 114.1(6) . . ? O10 C46 H46A 109.5 . . ? O10 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O10 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O11 C47 O12 124.8(7) . . ? O11 C47 C36 123.5(7) . . ? O12 C47 C36 111.7(6) . . ? O12 C48 H48A 109.5 . . ? O12 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O12 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N8 C49 C53 122.4(6) . . ? N8 C49 C37 114.8(6) . . ? C53 C49 C37 122.7(6) . . ? N8 C50 C51 122.2(6) . . ? N8 C50 H50 118.9 . . ? C51 C50 H50 118.9 . . ? C52 C51 C50 119.6(7) . . ? C52 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? C51 C52 C53 119.3(6) . . ? C51 C52 H52 120.4 . . ? C53 C52 H52 120.4 . . ? C49 C53 C52 118.7(6) . . ? C49 C53 H53 120.6 . . ? C52 C53 H53 120.6 . . ? N9 C54 C55 177.8(10) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O17A Cl5 O17 124.5(18) . . ? O17A Cl5 O15A 145(2) . . ? O17 Cl5 O15A 47.3(10) . . ? O17A Cl5 O16 32.5(16) . . ? O17 Cl5 O16 115.6(8) . . ? O15A Cl5 O16 161.5(13) . . ? O17A Cl5 O15 109.9(17) . . ? O17 Cl5 O15 125.2(7) . . ? O15A Cl5 O15 84.8(12) . . ? O16 Cl5 O15 113.6(6) . . ? O17A Cl5 O18A 104.0(19) . . ? O17 Cl5 O18A 118.6(12) . . ? O15A Cl5 O18A 108.6(14) . . ? O16 Cl5 O18A 85.2(11) . . ? O15 Cl5 O18A 44.7(10) . . ? O17A Cl5 O18 61.4(16) . . ? O17 Cl5 O18 100.8(7) . . ? O15A Cl5 O18 85.1(11) . . ? O16 Cl5 O18 93.1(8) . . ? O15 Cl5 O18 99.3(5) . . ? O18A Cl5 O18 137.1(12) . . ? O17A Cl5 O16A 103.8(19) . . ? O17 Cl5 O16A 66.4(12) . . ? O15A Cl5 O16A 101.2(16) . . ? O16 Cl5 O16A 72.2(12) . . ? O15 Cl5 O16A 108.8(12) . . ? O18A Cl5 O16A 67.4(15) . . ? O18 Cl5 O16A 151.6(12) . . ? O21A Cl6 O19 102.3(12) . . ? O21A Cl6 O20A 113.3(17) . . ? O19 Cl6 O20A 41.4(10) . . ? O21A Cl6 O22 139.7(13) . . ? O19 Cl6 O22 114.5(5) . . ? O20A Cl6 O22 105.3(12) . . ? O21A Cl6 O22A 118.9(17) . . ? O19 Cl6 O22A 138.1(13) . . ? O20A Cl6 O22A 108.8(17) . . ? O22 Cl6 O22A 32.1(10) . . ? O21A Cl6 O21 36.6(11) . . ? O19 Cl6 O21 110.8(6) . . ? O20A Cl6 O21 142.6(12) . . ? O22 Cl6 O21 110.6(5) . . ? O22A Cl6 O21 107.2(13) . . ? O21A Cl6 O20 75.3(12) . . ? O19 Cl6 O20 108.1(5) . . ? O20A Cl6 O20 72.9(12) . . ? O22 Cl6 O20 106.5(6) . . ? O22A Cl6 O20 77.1(12) . . ? O21 Cl6 O20 105.9(5) . . ? O21A Cl6 O19A 107.8(15) . . ? O19 Cl6 O19A 66.9(9) . . ? O20A Cl6 O19A 101.5(14) . . ? O22 Cl6 O19A 74.2(10) . . ? O22A Cl6 O19A 104.7(14) . . ? O21 Cl6 O19A 78.7(9) . . ? O20 Cl6 O19A 174.4(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.190 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.091 #============================================================================== data_co86 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H75 Cl8 Cu2 N15.50 O14' _chemical_formula_weight 1828.18 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' '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 19.3832(5) _cell_length_b 19.5174(5) _cell_length_c 24.2065(7) _cell_angle_alpha 71.184(2) _cell_angle_beta 80.390(2) _cell_angle_gamma 76.041(2) _cell_volume 8372.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour violet _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3758 _exptl_absorpt_coefficient_mu 0.834 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.647 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 89652 _diffrn_reflns_av_R_equivalents 0.074 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 24.71 _reflns_number_total 28535 _reflns_number_gt 18891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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 ; Some of the solvent molecules (acetonitrile) are heavily disordered. ; _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^)+(0.0914P)^2^+33.1541P] 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 28535 _refine_ls_number_parameters 2017 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1115 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.1994 _refine_ls_wR_factor_gt 0.1737 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.006 _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 0.06088(4) 0.49296(4) 0.34145(3) 0.02091(18) Uani 1 1 d . . . Cu2 Cu 0.32527(4) 0.61452(4) 0.09280(3) 0.01849(17) Uani 1 1 d . . . Cl1 Cl 0.20991(9) 0.34335(10) 0.49568(7) 0.0368(4) Uani 1 1 d . . . Cl2 Cl 0.15469(10) 0.19605(10) 0.56805(7) 0.0420(4) Uani 1 1 d . . . Cl3 Cl 0.01891(11) 0.16675(11) 0.53408(9) 0.0511(5) Uani 1 1 d . . . Cl4 Cl -0.06025(9) 0.28071(10) 0.42841(9) 0.0443(5) Uani 1 1 d . . . Cl5 Cl 0.11509(8) 0.81123(9) 0.06514(7) 0.0316(4) Uani 1 1 d . . . Cl6 Cl 0.15575(9) 0.96637(9) 0.04349(8) 0.0365(4) Uani 1 1 d . . . Cl7 Cl 0.31600(10) 0.97332(9) 0.04231(9) 0.0437(5) Uani 1 1 d . . . Cl8 Cl 0.43314(8) 0.82668(9) 0.06606(7) 0.0320(4) Uani 1 1 d . . . O1 O 0.1154(2) 0.7462(2) 0.34864(18) 0.0274(10) Uani 1 1 d . . . O2 O -0.0236(2) 0.8022(2) 0.2755(2) 0.0316(11) Uani 1 1 d . . . O3 O 0.0824(2) 0.7868(2) 0.22275(18) 0.0326(11) Uani 1 1 d . . . O4 O 0.1775(3) 0.6489(3) 0.4539(2) 0.0380(12) Uani 1 1 d . . . O5 O 0.2513(2) 0.5584(2) 0.42350(17) 0.0266(10) Uani 1 1 d . . . O6 O 0.0081(2) 0.4131(2) 0.36968(17) 0.0256(10) Uani 1 1 d . . . O7 O 0.1257(2) 0.4344(2) 0.39756(17) 0.0260(10) Uani 1 1 d . . . O8 O 0.2846(2) 0.4787(3) -0.05385(18) 0.0307(11) Uani 1 1 d . . . O9 O 0.1710(3) 0.6057(3) -0.0868(2) 0.0428(13) Uani 1 1 d . . . O10 O 0.1059(2) 0.6048(3) -0.0020(2) 0.0441(13) Uani 1 1 d . . . O11 O 0.4591(2) 0.4144(2) -0.01818(19) 0.0327(11) Uani 1 1 d . . . O12 O 0.3757(2) 0.3535(2) 0.03667(18) 0.0306(10) Uani 1 1 d . . . O13 O 0.2381(2) 0.6867(2) 0.08777(17) 0.0238(9) Uani 1 1 d . . . O14 O 0.3731(2) 0.6918(2) 0.08998(17) 0.0224(9) Uani 1 1 d . . . N1 N 0.1339(2) 0.5606(3) 0.29673(18) 0.0170(10) Uani 1 1 d . . . N2 N 0.0197(2) 0.5844(3) 0.3861(2) 0.0207(11) Uani 1 1 d . . . N3 N 0.2285(3) 0.6703(3) 0.2712(2) 0.0221(11) Uani 1 1 d . . . N4 N 0.0094(3) 0.5528(3) 0.2711(2) 0.0232(11) Uani 1 1 d . . . N5 N 0.2742(2) 0.5289(3) 0.10268(19) 0.0170(10) Uani 1 1 d . . . N6 N 0.3417(3) 0.6184(3) -0.00360(19) 0.0200(11) Uani 1 1 d . . . N7 N 0.2008(3) 0.4293(3) 0.0675(2) 0.0294(13) Uani 1 1 d . . . N8 N 0.4062(2) 0.5307(3) 0.11754(19) 0.0187(11) Uani 1 1 d . . . C1 C 0.0913(3) 0.6324(3) 0.2642(2) 0.0194(13) Uani 1 1 d . . . H1 H 0.1226 0.6571 0.2315 0.012(7) Uiso 1 1 calc R . . C2 C 0.0588(3) 0.6855(3) 0.3025(2) 0.0209(13) Uani 1 1 d . . . C3 C -0.0042(3) 0.6590(3) 0.3481(2) 0.0218(13) Uani 1 1 d . . . H3A H -0.0214 0.6926 0.3717 0.011(5) Uiso 1 1 calc R . . H3B H -0.0433 0.6596 0.3275 0.011(5) Uiso 1 1 calc R . . C4 C 0.0784(3) 0.5818(4) 0.4190(2) 0.0222(13) Uani 1 1 d . . . H4A H 0.0948 0.5311 0.4420 0.011(5) Uiso 1 1 calc R . . H4B H 0.0603 0.6109 0.4460 0.011(5) Uiso 1 1 calc R . . C5 C 0.1436(3) 0.6116(3) 0.3782(2) 0.0201(13) Uani 1 1 d . . . C6 C 0.1834(3) 0.5654(3) 0.3365(2) 0.0194(13) Uani 1 1 d . . . H6 H 0.2022 0.5153 0.3605 0.012(7) Uiso 1 1 calc R . . C7 C 0.1119(3) 0.6891(4) 0.3422(2) 0.0209(13) Uani 1 1 d . . . C8 C 0.1750(3) 0.5168(3) 0.2556(2) 0.0188(13) Uani 1 1 d . . . H8A H 0.1438 0.4877 0.2505 0.025(7) Uiso 1 1 calc R . . H8B H 0.2147 0.4823 0.2755 0.025(7) Uiso 1 1 calc R . . C9 C 0.0333(3) 0.6150(3) 0.2390(2) 0.0204(13) Uani 1 1 d . . . C10 C -0.0423(3) 0.5345(4) 0.2521(3) 0.0317(16) Uani 1 1 d . . . H10 H -0.0587 0.4917 0.2742 0.027(4) Uiso 1 1 calc R . . C11 C -0.0728(4) 0.5768(4) 0.2006(3) 0.0377(17) Uani 1 1 d . . . H11 H -0.1092 0.5630 0.1885 0.027(4) Uiso 1 1 calc R . . C12 C -0.0477(3) 0.6400(4) 0.1676(3) 0.0321(16) Uani 1 1 d . . . H12 H -0.0669 0.6691 0.1328 0.027(4) Uiso 1 1 calc R . . C13 C 0.0056(3) 0.6594(3) 0.1866(3) 0.0246(14) Uani 1 1 d . . . H13 H 0.0230 0.7016 0.1648 0.027(4) Uiso 1 1 calc R . . C14 C 0.0328(3) 0.7637(3) 0.2658(2) 0.0225(13) Uani 1 1 d . . . C15 C 0.0670(4) 0.8648(4) 0.1916(3) 0.0434(19) Uani 1 1 d . . . H15A H 0.0281 0.8751 0.1683 0.054(6) Uiso 1 1 calc R . . H15B H 0.1085 0.8783 0.1665 0.054(6) Uiso 1 1 calc R . . H15C H 0.0541 0.8927 0.2192 0.054(6) Uiso 1 1 calc R . . C16 C -0.0408(3) 0.5600(4) 0.4285(3) 0.0263(14) Uani 1 1 d . . . H16A H -0.0527 0.5882 0.4560 0.054(6) Uiso 1 1 calc R . . H16B H -0.0272 0.5085 0.4491 0.054(6) Uiso 1 1 calc R . . H16C H -0.0814 0.5677 0.4077 0.054(6) Uiso 1 1 calc R . . C17 C 0.1928(3) 0.6109(4) 0.4217(2) 0.0240(14) Uani 1 1 d . . . C18 C 0.2977(4) 0.5495(4) 0.4674(3) 0.0369(17) Uani 1 1 d . . . H18A H 0.3159 0.5938 0.4590 0.054(6) Uiso 1 1 calc R . . H18B H 0.3367 0.5086 0.4670 0.054(6) Uiso 1 1 calc R . . H18C H 0.2712 0.5403 0.5054 0.054(6) Uiso 1 1 calc R . . C19 C 0.2463(3) 0.5987(3) 0.3004(2) 0.0165(12) Uani 1 1 d . . . C20 C 0.2803(3) 0.7028(4) 0.2347(3) 0.0267(14) Uani 1 1 d . . . H20 H 0.2689 0.7525 0.2136 0.027(4) Uiso 1 1 calc R . . C21 C 0.3493(3) 0.6647(4) 0.2276(3) 0.0282(15) Uani 1 1 d . . . H21 H 0.3835 0.6882 0.2018 0.027(4) Uiso 1 1 calc R . . C22 C 0.3671(3) 0.5917(4) 0.2589(3) 0.0252(14) Uani 1 1 d . . . H22 H 0.4137 0.5657 0.2550 0.027(4) Uiso 1 1 calc R . . C23 C 0.3151(3) 0.5568(3) 0.2965(2) 0.0203(13) Uani 1 1 d . . . H23 H 0.3259 0.5073 0.3181 0.027(4) Uiso 1 1 calc R . . C24 C 0.0392(3) 0.3618(3) 0.4151(3) 0.0247(14) Uani 1 1 d . . . C25 C 0.1019(3) 0.3736(3) 0.4303(2) 0.0214(13) Uani 1 1 d . . . C26 C 0.1359(3) 0.3230(3) 0.4779(3) 0.0251(14) Uani 1 1 d . . . C27 C 0.1101(3) 0.2594(4) 0.5096(3) 0.0282(15) Uani 1 1 d . . . C28 C 0.0502(4) 0.2457(4) 0.4950(3) 0.0318(16) Uani 1 1 d . . . C29 C 0.0148(3) 0.2975(4) 0.4473(3) 0.0278(14) Uani 1 1 d . . . C30 C 0.2049(3) 0.5578(3) 0.1948(2) 0.0194(13) Uani 1 1 d . . . H30A H 0.1663 0.5863 0.1708 0.025(7) Uiso 1 1 calc R . . H30B H 0.2329 0.5913 0.1977 0.025(7) Uiso 1 1 calc R . . C31 C 0.2104(3) 0.5493(4) 0.0681(2) 0.0224(13) Uani 1 1 d . . . H31 H 0.1784 0.5929 0.0762 0.012(7) Uiso 1 1 calc R . . C32 C 0.2322(3) 0.5676(4) 0.0006(2) 0.0236(14) Uani 1 1 d . . . C33 C 0.2719(3) 0.6332(4) -0.0250(2) 0.0242(14) Uani 1 1 d . . . H33A H 0.2782 0.6449 -0.0674 0.011(5) Uiso 1 1 calc R . . H33B H 0.2424 0.6763 -0.0152 0.011(5) Uiso 1 1 calc R . . C34 C 0.3874(3) 0.5491(3) -0.0114(2) 0.0214(13) Uani 1 1 d . . . H34A H 0.4326 0.5408 0.0044 0.011(5) Uiso 1 1 calc R . . H34B H 0.3973 0.5536 -0.0529 0.011(5) Uiso 1 1 calc R . . C35 C 0.3509(3) 0.4825(3) 0.0199(2) 0.0187(13) Uani 1 1 d . . . C36 C 0.3321(3) 0.4687(3) 0.0881(2) 0.0162(12) Uani 1 1 d . . . H36 H 0.3165 0.4215 0.1050 0.012(7) Uiso 1 1 calc R . . C37 C 0.2847(3) 0.5018(4) -0.0134(2) 0.0244(14) Uani 1 1 d . . . C38 C 0.2516(3) 0.5000(3) 0.1676(2) 0.0198(13) Uani 1 1 d . . . H38A H 0.2941 0.4784 0.1882 0.025(7) Uiso 1 1 calc R . . H38B H 0.2258 0.4610 0.1735 0.025(7) Uiso 1 1 calc R . . C39 C 0.1695(3) 0.4871(4) 0.0853(3) 0.0237(14) Uani 1 1 d . . . C40 C 0.1691(4) 0.3713(4) 0.0820(3) 0.0410(18) Uani 1 1 d . . . H40 H 0.1922 0.3302 0.0698 0.027(4) Uiso 1 1 calc R . . C41 C 0.1035(4) 0.3704(5) 0.1143(4) 0.050(2) Uani 1 1 d . . . H41 H 0.0825 0.3295 0.1233 0.027(4) Uiso 1 1 calc R . . C42 C 0.0697(4) 0.4300(5) 0.1329(3) 0.046(2) Uani 1 1 d . . . H42 H 0.0254 0.4303 0.1546 0.027(4) Uiso 1 1 calc R . . C43 C 0.1025(4) 0.4900(4) 0.1188(3) 0.0351(17) Uani 1 1 d . . . H43 H 0.0807 0.5312 0.1312 0.027(4) Uiso 1 1 calc R . . C44 C 0.1669(3) 0.5927(4) -0.0344(3) 0.0288(15) Uani 1 1 d . . . C45 C 0.0427(4) 0.6291(6) -0.0331(4) 0.072(3) Uani 1 1 d . . . H45A H 0.0395 0.6799 -0.0561 0.054(6) Uiso 1 1 calc R . . H45B H 0.0012 0.6243 -0.0055 0.054(6) Uiso 1 1 calc R . . H45C H 0.0456 0.5993 -0.0585 0.054(6) Uiso 1 1 calc R . . C46 C 0.3781(3) 0.6805(3) -0.0351(3) 0.0251(14) Uani 1 1 d . . . H46A H 0.3880 0.6831 -0.0758 0.054(6) Uiso 1 1 calc R . . H46B H 0.4221 0.6729 -0.0186 0.054(6) Uiso 1 1 calc R . . H46C H 0.3479 0.7259 -0.0312 0.054(6) Uiso 1 1 calc R . . C47 C 0.4015(3) 0.4137(3) 0.0096(2) 0.0227(13) Uani 1 1 d . . . C48 C 0.4234(4) 0.2848(4) 0.0352(3) 0.0391(18) Uani 1 1 d . . . H48A H 0.4503 0.2909 -0.0026 0.054(6) Uiso 1 1 calc R . . H48B H 0.3962 0.2472 0.0422 0.054(6) Uiso 1 1 calc R . . H48C H 0.4555 0.2704 0.0650 0.054(6) Uiso 1 1 calc R . . C49 C 0.3977(3) 0.4654(3) 0.1158(2) 0.0160(12) Uani 1 1 d U . . C50 C 0.4639(3) 0.5339(4) 0.1402(2) 0.0227(14) Uani 1 1 d . . . H50 H 0.4703 0.5794 0.1408 0.027(4) Uiso 1 1 calc R . . C51 C 0.5139(3) 0.4705(3) 0.1625(2) 0.0213(13) Uani 1 1 d . . . H51 H 0.5533 0.4734 0.1784 0.027(4) Uiso 1 1 calc R . . C52 C 0.5047(3) 0.4030(4) 0.1611(2) 0.0228(14) Uani 1 1 d . . . H52 H 0.5378 0.3601 0.1759 0.027(4) Uiso 1 1 calc R . . C53 C 0.4457(3) 0.4001(3) 0.1372(2) 0.0215(13) Uani 1 1 d . . . H53 H 0.4384 0.3554 0.1357 0.027(4) Uiso 1 1 calc R . . C54 C 0.2531(3) 0.7517(3) 0.0797(2) 0.0198(13) Uani 1 1 d . . . C55 C 0.3258(3) 0.7549(3) 0.0805(2) 0.0216(13) Uani 1 1 d . . . C56 C 0.3431(3) 0.8237(3) 0.0692(2) 0.0228(13) Uani 1 1 d . . . C57 C 0.2910(3) 0.8890(3) 0.0592(3) 0.0264(14) Uani 1 1 d . . . C58 C 0.2208(3) 0.8854(3) 0.0597(3) 0.0257(14) Uani 1 1 d . . . C59 C 0.2023(3) 0.8173(3) 0.0690(2) 0.0209(13) Uani 1 1 d . . . Cu3 Cu 0.72692(4) 0.96105(4) 0.18659(3) 0.02292(18) Uani 1 1 d . . . Cu4 Cu 0.51034(4) 0.70358(4) 0.39450(3) 0.01830(17) Uani 1 1 d . . . Cl9 Cl 0.93587(8) 0.84964(10) 0.07718(7) 0.0352(4) Uani 1 1 d . . . Cl10 Cl 0.88808(10) 0.77872(12) -0.00632(8) 0.0473(5) Uani 1 1 d . . . Cl11 Cl 0.72440(10) 0.79423(11) -0.01414(8) 0.0417(4) Uani 1 1 d . . . Cl12 Cl 0.61042(8) 0.87225(10) 0.06864(7) 0.0320(4) Uani 1 1 d . . . Cl13 Cl 0.30328(9) 0.68267(10) 0.53974(7) 0.0364(4) Uani 1 1 d . . . Cl14 Cl 0.35170(10) 0.61613(10) 0.66749(7) 0.0391(4) Uani 1 1 d . . . Cl15 Cl 0.51307(10) 0.59018(10) 0.68559(6) 0.0387(4) Uani 1 1 d . . . Cl16 Cl 0.62644(9) 0.62309(10) 0.57528(7) 0.0340(4) Uani 1 1 d . . . O15 O 0.5383(3) 1.2111(3) 0.1838(2) 0.0442(13) Uani 1 1 d . . . O16 O 0.6812(4) 1.2282(4) 0.2326(3) 0.084(2) Uani 1 1 d . . . O17 O 0.6058(3) 1.1702(3) 0.3023(2) 0.0438(13) Uani 1 1 d . . . O18 O 0.4406(3) 1.1483(3) 0.1488(2) 0.0534(15) Uani 1 1 d . . . O19 O 0.4990(3) 1.0591(3) 0.1091(2) 0.0468(13) Uani 1 1 d . . . O20 O 0.6762(2) 0.9252(2) 0.14416(17) 0.0230(9) Uani 1 1 d . . . O21 O 0.8137(2) 0.9220(2) 0.14449(17) 0.0266(10) Uani 1 1 d . . . O22 O 0.6966(2) 0.5580(2) 0.25940(17) 0.0242(9) Uani 1 1 d . . . O23 O 0.7840(3) 0.5669(3) 0.3917(2) 0.0386(12) Uani 1 1 d . . . O24 O 0.7561(2) 0.4804(2) 0.3636(2) 0.0304(10) Uani 1 1 d . . . O25 O 0.5380(2) 0.6032(3) 0.20572(18) 0.0349(11) Uani 1 1 d . . . O26 O 0.6115(2) 0.6835(2) 0.17053(17) 0.0272(10) Uani 1 1 d . . . O27 O 0.5620(2) 0.6763(2) 0.46191(16) 0.0230(9) Uani 1 1 d . . . O28 O 0.4243(2) 0.7018(2) 0.44721(17) 0.0247(10) Uani 1 1 d . . . N9 N 0.6372(3) 0.9892(3) 0.2416(2) 0.0215(11) Uani 1 1 d . . . N10 N 0.6962(3) 1.0837(3) 0.1334(2) 0.0290(13) Uani 1 1 d . . . N11 N 0.7756(3) 0.9808(3) 0.2432(2) 0.0264(12) Uani 1 1 d . . . N12 N 0.4970(3) 1.0652(3) 0.2860(3) 0.0386(15) Uani 1 1 d . . . N13 N 0.5982(2) 0.7234(3) 0.33297(19) 0.0163(10) Uani 1 1 d . . . N14 N 0.5410(2) 0.5908(3) 0.37896(19) 0.0182(10) Uani 1 1 d . . . N15 N 0.7379(3) 0.7014(3) 0.2579(2) 0.0205(11) Uani 1 1 d . . . N16 N 0.4579(3) 0.7553(3) 0.3234(2) 0.0200(11) Uani 1 1 d . . . C61 C 0.6553(3) 1.0449(3) 0.2649(3) 0.0270(14) Uani 1 1 d . . . H61 H 0.6250 1.0458 0.3015 0.020(8) Uiso 1 1 calc R . . C62 C 0.6433(4) 1.1252(4) 0.2207(3) 0.0318(16) Uani 1 1 d . . . C63 C 0.6995(4) 1.1342(4) 0.1661(3) 0.0340(16) Uani 1 1 d . . . H63A H 0.6901 1.1848 0.1409 0.020(6) Uiso 1 1 calc R . . H63B H 0.7469 1.1236 0.1786 0.020(6) Uiso 1 1 calc R . . C64 C 0.6254(4) 1.0953(4) 0.1138(3) 0.0303(15) Uani 1 1 d . . . H64A H 0.6256 1.0578 0.0954 0.020(6) Uiso 1 1 calc R . . H64B H 0.6158 1.1431 0.0845 0.020(6) Uiso 1 1 calc R . . C65 C 0.5650(3) 1.0918(4) 0.1650(3) 0.0306(15) Uani 1 1 d . . . C66 C 0.5698(3) 1.0143(3) 0.2117(3) 0.0236(14) Uani 1 1 d . . . H66 H 0.5685 0.9783 0.1917 0.020(8) Uiso 1 1 calc R . . C67 C 0.5728(4) 1.1483(4) 0.1931(3) 0.0331(16) Uani 1 1 d . . . C68 C 0.6309(3) 0.9216(3) 0.2933(2) 0.0204(13) Uani 1 1 d . . . H68A H 0.6726 0.9084 0.3147 0.013(6) Uiso 1 1 calc R . . H68B H 0.5893 0.9337 0.3194 0.013(6) Uiso 1 1 calc R . . C69 C 0.7323(4) 1.0199(3) 0.2783(3) 0.0282(15) Uani 1 1 d . . . C70 C 0.8451(4) 0.9561(4) 0.2520(3) 0.0330(16) Uani 1 1 d . . . H70 H 0.8746 0.9297 0.2281 0.041(5) Uiso 1 1 calc R . . C71 C 0.8743(4) 0.9684(4) 0.2953(3) 0.0442(19) Uani 1 1 d . . . H71 H 0.9225 0.9510 0.3005 0.041(5) Uiso 1 1 calc R . . C72 C 0.8300(4) 1.0073(5) 0.3308(4) 0.049(2) Uani 1 1 d . . . H72 H 0.8484 1.0159 0.3605 0.041(5) Uiso 1 1 calc R . . C73 C 0.7588(4) 1.0332(4) 0.3224(3) 0.0385(17) Uani 1 1 d . . . H73 H 0.7289 1.0594 0.3462 0.041(5) Uiso 1 1 calc R . . C74 C 0.6469(4) 1.1798(4) 0.2518(4) 0.0430(19) Uani 1 1 d . . . C75 C 0.6034(5) 1.2209(5) 0.3352(4) 0.061(3) Uani 1 1 d . . . H75A H 0.6499 1.2148 0.3471 0.053(5) Uiso 1 1 calc R . . H75B H 0.5697 1.2110 0.3693 0.053(5) Uiso 1 1 calc R . . H75C H 0.5889 1.2708 0.3111 0.053(5) Uiso 1 1 calc R . . C76 C 0.7507(4) 1.0919(4) 0.0820(3) 0.0389(18) Uani 1 1 d . . . H76A H 0.7499 1.0571 0.0618 0.053(5) Uiso 1 1 calc R . . H76B H 0.7971 1.0827 0.0950 0.053(5) Uiso 1 1 calc R . . H76C H 0.7402 1.1412 0.0559 0.053(5) Uiso 1 1 calc R . . C77 C 0.4942(4) 1.1055(4) 0.1407(3) 0.0373(17) Uani 1 1 d . . . C78 C 0.4355(5) 1.0592(6) 0.0866(4) 0.064(3) Uani 1 1 d . . . H78A H 0.3987 1.0494 0.1183 0.053(5) Uiso 1 1 calc R . . H78B H 0.4449 1.0217 0.0671 0.053(5) Uiso 1 1 calc R . . H78C H 0.4200 1.1066 0.0592 0.053(5) Uiso 1 1 calc R . . C79 C 0.5024(3) 1.0190(3) 0.2546(3) 0.0266(14) Uani 1 1 d . . . C80 C 0.4367(4) 1.0736(5) 0.3223(4) 0.051(2) Uani 1 1 d . . . H80 H 0.4320 1.1052 0.3450 0.041(5) Uiso 1 1 calc R . . C81 C 0.3825(4) 1.0383(5) 0.3273(4) 0.056(2) Uani 1 1 d . . . H81 H 0.3416 1.0466 0.3525 0.041(5) Uiso 1 1 calc R . . C82 C 0.3879(4) 0.9910(4) 0.2954(4) 0.047(2) Uani 1 1 d . . . H82 H 0.3510 0.9668 0.2982 0.041(5) Uiso 1 1 calc R . . C83 C 0.4503(4) 0.9794(4) 0.2582(3) 0.0336(16) Uani 1 1 d . . . H83 H 0.4567 0.9462 0.2366 0.041(5) Uiso 1 1 calc R . . C84 C 0.7221(3) 0.8932(3) 0.1084(2) 0.0214(13) Uani 1 1 d . . . C85 C 0.7960(3) 0.8910(3) 0.1097(2) 0.0219(13) Uani 1 1 d . . . C86 C 0.8460(3) 0.8547(3) 0.0739(3) 0.0235(14) Uani 1 1 d . . . C87 C 0.8248(4) 0.8239(4) 0.0368(3) 0.0288(15) Uani 1 1 d . . . C88 C 0.7522(3) 0.8291(4) 0.0339(3) 0.0272(14) Uani 1 1 d . . . C89 C 0.7015(3) 0.8633(3) 0.0704(3) 0.0228(13) Uani 1 1 d . . . C90 C 0.6244(3) 0.8556(3) 0.2765(2) 0.0196(13) Uani 1 1 d . . . H90A H 0.6704 0.8332 0.2605 0.013(6) Uiso 1 1 calc R . . H90B H 0.5909 0.8704 0.2471 0.013(6) Uiso 1 1 calc R . . C91 C 0.6678(3) 0.6732(3) 0.3516(2) 0.0183(12) Uani 1 1 d . . . H91 H 0.6712 0.6709 0.3921 0.020(8) Uiso 1 1 calc R . . C92 C 0.6722(3) 0.5933(3) 0.3501(2) 0.0194(13) Uani 1 1 d . . . C93 C 0.6140(3) 0.5551(3) 0.3939(2) 0.0197(13) Uani 1 1 d . . . H93A H 0.6227 0.5039 0.3944 0.020(6) Uiso 1 1 calc R . . H93B H 0.6184 0.5558 0.4330 0.020(6) Uiso 1 1 calc R . . C94 C 0.5330(3) 0.5957(3) 0.3180(2) 0.0180(12) Uani 1 1 d . . . H94A H 0.4843 0.6193 0.3091 0.020(6) Uiso 1 1 calc R . . H94B H 0.5423 0.5464 0.3139 0.020(6) Uiso 1 1 calc R . . C95 C 0.5856(3) 0.6409(3) 0.2740(2) 0.0171(12) Uani 1 1 d . . . C96 C 0.5774(3) 0.7216(3) 0.2765(2) 0.0186(12) Uani 1 1 d . . . H96 H 0.6074 0.7479 0.2436 0.020(8) Uiso 1 1 calc R . . C97 C 0.6600(3) 0.5950(3) 0.2886(2) 0.0176(12) Uani 1 1 d . . . C98 C 0.5977(3) 0.8008(3) 0.3326(2) 0.0171(12) Uani 1 1 d . . . H98A H 0.6259 0.7970 0.3633 0.013(6) Uiso 1 1 calc R . . H98B H 0.5489 0.8227 0.3436 0.013(6) Uiso 1 1 calc R . . C99 C 0.7305(3) 0.7041(3) 0.3138(2) 0.0178(12) Uani 1 1 d . . . C100 C 0.7898(3) 0.7330(3) 0.2211(3) 0.0248(14) Uani 1 1 d . . . H100 H 0.7958 0.7322 0.1823 0.041(5) Uiso 1 1 calc R . . C101 C 0.8340(3) 0.7663(3) 0.2382(3) 0.0275(15) Uani 1 1 d . . . H101 H 0.8688 0.7876 0.2115 0.041(5) Uiso 1 1 calc R . . C102 C 0.8259(3) 0.7675(3) 0.2958(3) 0.0258(14) Uani 1 1 d . . . H102 H 0.8555 0.7895 0.3083 0.041(5) Uiso 1 1 calc R . . C103 C 0.7728(3) 0.7354(3) 0.3347(3) 0.0218(13) Uani 1 1 d . . . H103 H 0.7663 0.7353 0.3736 0.041(5) Uiso 1 1 calc R . . C104 C 0.7446(3) 0.5464(3) 0.3700(2) 0.0203(13) Uani 1 1 d . . . C105 C 0.8218(3) 0.4303(4) 0.3820(3) 0.0312(15) Uani 1 1 d . . . H10A H 0.8612 0.4547 0.3654 0.053(5) Uiso 1 1 calc R . . H10B H 0.8280 0.3876 0.3689 0.053(5) Uiso 1 1 calc R . . H10C H 0.8200 0.4154 0.4240 0.053(5) Uiso 1 1 calc R . . C106 C 0.4902(3) 0.5483(3) 0.4194(3) 0.0249(14) Uani 1 1 d . . . H10D H 0.5021 0.4984 0.4176 0.053(5) Uiso 1 1 calc R . . H10E H 0.4427 0.5704 0.4085 0.053(5) Uiso 1 1 calc R . . H10F H 0.4926 0.5484 0.4587 0.053(5) Uiso 1 1 calc R . . C107 C 0.5751(3) 0.6401(3) 0.2131(2) 0.0217(13) Uani 1 1 d . . . C108 C 0.6045(5) 0.6808(4) 0.1117(3) 0.045(2) Uani 1 1 d . . . H10G H 0.6191 0.6306 0.1104 0.053(5) Uiso 1 1 calc R . . H10H H 0.6342 0.7108 0.0831 0.053(5) Uiso 1 1 calc R . . H10I H 0.5556 0.6991 0.1033 0.053(5) Uiso 1 1 calc R . . C109 C 0.5006(3) 0.7611(3) 0.2716(2) 0.0179(12) Uani 1 1 d . . . C110 C 0.3887(3) 0.7858(3) 0.3234(3) 0.0256(14) Uani 1 1 d . . . H110 H 0.3607 0.7807 0.3591 0.041(5) Uiso 1 1 calc R . . C111 C 0.3570(4) 0.8249(4) 0.2724(3) 0.0317(16) Uani 1 1 d . . . H111 H 0.3085 0.8460 0.2734 0.041(5) Uiso 1 1 calc R . . C112 C 0.3999(3) 0.8322(4) 0.2187(3) 0.0293(15) Uani 1 1 d . . . H112 H 0.3802 0.8584 0.1835 0.041(5) Uiso 1 1 calc R . . C113 C 0.4719(3) 0.8000(3) 0.2188(3) 0.0237(14) Uani 1 1 d . . . H113 H 0.5009 0.8043 0.1836 0.041(5) Uiso 1 1 calc R . . C114 C 0.5159(3) 0.6646(3) 0.5100(2) 0.0207(13) Uani 1 1 d . . . C115 C 0.4423(3) 0.6778(3) 0.5019(2) 0.0205(13) Uani 1 1 d . . . C116 C 0.3924(3) 0.6649(3) 0.5509(3) 0.0258(14) Uani 1 1 d . . . C117 C 0.4146(4) 0.6374(3) 0.6078(3) 0.0286(15) Uani 1 1 d . . . C118 C 0.4848(4) 0.6253(4) 0.6157(2) 0.0287(15) Uani 1 1 d . . . C119 C 0.5360(3) 0.6392(3) 0.5668(2) 0.0226(13) Uani 1 1 d . . . N17 N 0.8627(8) 0.4051(7) 0.2318(5) 0.118(4) Uani 1 1 d . . . C121 C 0.8082(9) 0.4133(6) 0.2171(4) 0.083(4) Uani 1 1 d . . . C122 C 0.7401(6) 0.4232(6) 0.1975(4) 0.077(3) Uani 1 1 d . . . H12A H 0.7431 0.4429 0.1555 0.179(13) Uiso 1 1 calc R . . H12B H 0.7057 0.4570 0.2146 0.179(13) Uiso 1 1 calc R . . H12C H 0.7255 0.3765 0.2091 0.179(13) Uiso 1 1 calc R . . N18 N 0.9071(6) 0.5486(7) 0.0646(5) 0.102(3) Uani 1 1 d . . . C123 C 0.8526(7) 0.5826(7) 0.0790(5) 0.072(3) Uani 1 1 d . . . C124 C 0.7893(7) 0.6197(7) 0.0984(6) 0.099(4) Uani 1 1 d . . . H12D H 0.7537 0.6257 0.0731 0.179(13) Uiso 1 1 calc R . . H12E H 0.7947 0.6674 0.0982 0.179(13) Uiso 1 1 calc R . . H12F H 0.7748 0.5922 0.1376 0.179(13) Uiso 1 1 calc R . . N19 N 0.3258(6) 1.3817(6) 0.2840(4) 0.090(3) Uani 1 1 d . . . C125 C 0.3657(6) 1.3333(6) 0.2836(4) 0.064(3) Uani 1 1 d . . . C126 C 0.4200(7) 1.2641(6) 0.2861(5) 0.097(4) Uani 1 1 d . . . H12G H 0.4114 1.2272 0.3225 0.179(13) Uiso 1 1 calc R . . H12H H 0.4669 1.2739 0.2833 0.179(13) Uiso 1 1 calc R . . H12I H 0.4167 1.2466 0.2540 0.179(13) Uiso 1 1 calc R . . N20 N 0.9944(5) 0.0479(5) 0.1687(4) 0.086(3) Uani 1 1 d . . . C127 C 0.9779(5) 0.0456(5) 0.1262(4) 0.054(2) Uani 1 1 d . . . C128 C 0.9559(5) 0.0400(6) 0.0740(4) 0.072(3) Uani 1 1 d . . . H12J H 0.9966 0.0189 0.0520 0.179(13) Uiso 1 1 calc R . . H12K H 0.9353 0.0883 0.0505 0.179(13) Uiso 1 1 calc R . . H12L H 0.9212 0.0091 0.0849 0.179(13) Uiso 1 1 calc R . . N21 N 0.7908(10) 0.1273(10) 0.4259(9) 0.190(7) Uiso 1 1 d . . . C129 C 0.8050(7) 0.1741(8) 0.3848(7) 0.101(4) Uiso 1 1 d . . . C130 C 0.8183(9) 0.2322(9) 0.3385(7) 0.132(5) Uiso 1 1 d . . . N22 N 0.2295(10) -0.0576(11) 0.1979(8) 0.193(7) Uiso 1 1 d . . . C131 C 0.2148(9) 0.0096(10) 0.1712(7) 0.127(5) Uiso 1 1 d . . . C132 C 0.1737(6) 0.0748(6) 0.1349(5) 0.085(3) Uiso 1 1 d . . . H13D H 0.1358 0.0620 0.1218 0.14(3) Uiso 1 1 calc R . . H13E H 0.2040 0.0970 0.1016 0.14(3) Uiso 1 1 calc R . . H13F H 0.1539 0.1092 0.1570 0.14(3) Uiso 1 1 calc R . . N23 N 0.3025(6) 0.3000(6) 0.1806(4) 0.098(3) Uani 1 1 d . . . C133 C 0.2896(6) 0.2427(6) 0.1917(4) 0.066(3) Uani 1 1 d . . . C134 C 0.2678(8) 0.1757(8) 0.2039(8) 0.132(6) Uani 1 1 d . . . H13G H 0.2306 0.1717 0.2358 0.179(13) Uiso 1 1 calc R . . H13H H 0.3076 0.1355 0.2146 0.179(13) Uiso 1 1 calc R . . H13I H 0.2501 0.1738 0.1698 0.179(13) Uiso 1 1 calc R . . N24 N 0.2121(10) 0.0619(10) 0.4774(8) 0.188(7) Uiso 1 1 d . . . C135 C 0.1656(15) 0.0932(15) 0.4238(13) 0.222(11) Uiso 1 1 d . . . C136 C 0.1160(16) 0.1299(16) 0.3789(14) 0.252(13) Uiso 1 1 d . . . N25 N 0.2837(13) 1.1902(13) 0.3783(10) 0.238(9) Uiso 1 1 d . . . C137 C 0.2348(16) 1.2472(17) 0.3518(13) 0.227(11) Uiso 1 1 d . . . C138 C 0.1801(14) 1.3046(15) 0.3119(12) 0.216(10) Uiso 1 1 d . . . N26 N 0.2446(7) 0.9249(9) 0.3828(6) 0.159(6) Uani 1 1 d . . . C139 C 0.2164(6) 0.8769(7) 0.4033(5) 0.073(3) Uani 1 1 d . . . C140 C 0.1795(7) 0.8187(6) 0.4306(7) 0.113(5) Uani 1 1 d . . . H14A H 0.2132 0.7725 0.4395 0.179(13) Uiso 1 1 calc R . . H14B H 0.1473 0.8181 0.4048 0.179(13) Uiso 1 1 calc R . . H14C H 0.1530 0.8258 0.4663 0.179(13) Uiso 1 1 calc R . . N27 N 0.4836(5) 0.8828(5) 0.4206(4) 0.084(3) Uani 1 1 d . . . C141 C 0.4324(6) 0.8751(5) 0.4496(4) 0.062(3) Uani 1 1 d . . . C142 C 0.3677(6) 0.8670(6) 0.4856(6) 0.097(4) Uani 1 1 d . . . H14D H 0.3666 0.8842 0.5188 0.179(13) Uiso 1 1 calc R . . H14E H 0.3643 0.8158 0.4990 0.179(13) Uiso 1 1 calc R . . H14F H 0.3281 0.8955 0.4636 0.179(13) Uiso 1 1 calc R . . N28 N 0.5377(12) 0.8357(13) 0.5734(7) 0.229(11) Uani 1 1 d . . . C143 C 0.5859(11) 0.8208(8) 0.5371(6) 0.125(6) Uani 1 1 d . . . C144 C 0.6382(5) 0.8109(6) 0.4861(5) 0.079(3) Uani 1 1 d . . . H14G H 0.6226 0.7815 0.4674 0.179(13) Uiso 1 1 calc R . . H14H H 0.6843 0.7865 0.4995 0.179(13) Uiso 1 1 calc R . . H14I H 0.6414 0.8583 0.4585 0.179(13) Uiso 1 1 calc R . . N29 N 0.1469(5) 0.7902(5) -0.0933(5) 0.086(3) Uani 1 1 d . . . C145 C 0.1346(5) 0.7862(5) -0.1348(5) 0.062(2) Uani 1 1 d . . . C146 C 0.1202(9) 0.7794(8) -0.1866(6) 0.128(6) Uani 1 1 d . . . H14J H 0.1620 0.7524 -0.2034 0.179(13) Uiso 1 1 calc R . . H14K H 0.1068 0.8277 -0.2136 0.179(13) Uiso 1 1 calc R . . H14L H 0.0817 0.7535 -0.1789 0.179(13) Uiso 1 1 calc R . . N30 N 0.5000 1.0000 0.5000 0.231(12) Uiso 1 2 d S . . C147 C 0.6017(13) 1.0129(13) 0.4270(11) 0.087(7) Uiso 0.50 1 d P . . C148 C 0.663(2) 0.980(2) 0.4447(17) 0.160(14) Uiso 0.50 1 d P . . C149 C 0.0503(16) -0.0427(17) 0.5172(14) 0.117(9) Uiso 0.50 1 d P . . C150 C -0.0233(18) 0.0013(18) 0.5343(14) 0.126(10) Uiso 0.50 1 d P . . N32 N -0.0408(17) 0.1108(17) 0.3261(13) 0.151(10) Uiso 0.50 1 d P . . N33 N -0.0117(15) 0.0118(15) 0.3831(12) 0.133(9) Uiso 0.50 1 d P . . C151 C 0.0167(19) 0.0741(19) 0.3115(15) 0.129(11) Uiso 0.50 1 d P . . C152 C 0.0869(13) 0.0129(13) 0.2968(11) 0.195(9) Uiso 1 1 d . . . C153 C 0.0369(16) -0.0098(16) 0.3470(13) 0.107(8) Uiso 0.50 1 d P . . N34 N 1.0806(13) 0.2003(13) 0.2115(11) 0.116(7) Uiso 0.50 1 d P . . C154 C 1.0577(17) 0.2236(17) 0.2521(15) 0.119(10) Uiso 0.50 1 d P . . C155 C 1.023(2) 0.267(2) 0.2887(17) 0.153(13) Uiso 0.50 1 d P . . C156 C 0.9984(12) 0.3473(13) 0.2791(10) 0.181(8) Uiso 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 0.0194(4) 0.0310(4) 0.0102(3) -0.0021(3) 0.0023(3) -0.0092(3) Cu2 0.0159(4) 0.0254(4) 0.0123(3) -0.0050(3) 0.0030(3) -0.0043(3) Cl1 0.0355(10) 0.0436(10) 0.0297(9) -0.0002(8) -0.0121(7) -0.0136(8) Cl2 0.0520(11) 0.0383(10) 0.0293(9) 0.0038(8) -0.0124(8) -0.0102(9) Cl3 0.0473(12) 0.0373(11) 0.0570(12) 0.0120(9) -0.0083(9) -0.0204(9) Cl4 0.0315(10) 0.0381(10) 0.0584(12) 0.0030(9) -0.0126(9) -0.0158(8) Cl5 0.0190(8) 0.0373(9) 0.0323(9) -0.0056(7) 0.0004(6) -0.0027(7) Cl6 0.0319(9) 0.0263(9) 0.0380(9) -0.0014(7) 0.0040(7) 0.0024(7) Cl7 0.0415(10) 0.0254(9) 0.0580(12) -0.0035(8) -0.0006(9) -0.0102(8) Cl8 0.0243(8) 0.0354(9) 0.0360(9) -0.0073(7) -0.0001(7) -0.0115(7) O1 0.032(3) 0.031(3) 0.022(2) -0.013(2) -0.0004(19) -0.005(2) O2 0.021(2) 0.030(3) 0.039(3) -0.008(2) 0.001(2) -0.002(2) O3 0.033(3) 0.034(3) 0.021(2) -0.001(2) 0.0094(19) -0.006(2) O4 0.039(3) 0.051(3) 0.030(3) -0.024(2) -0.009(2) 0.001(2) O5 0.025(2) 0.039(3) 0.015(2) -0.0119(19) -0.0046(18) 0.002(2) O6 0.026(2) 0.028(2) 0.020(2) 0.0005(19) -0.0028(18) -0.0089(19) O7 0.024(2) 0.035(3) 0.016(2) -0.0014(19) 0.0025(17) -0.011(2) O8 0.030(3) 0.048(3) 0.018(2) -0.018(2) 0.0020(19) -0.007(2) O9 0.035(3) 0.067(4) 0.026(3) -0.018(2) -0.010(2) 0.001(3) O10 0.023(3) 0.072(4) 0.026(3) -0.007(2) -0.005(2) 0.005(2) O11 0.026(3) 0.037(3) 0.027(2) -0.010(2) 0.011(2) -0.001(2) O12 0.038(3) 0.030(3) 0.025(2) -0.012(2) 0.005(2) -0.011(2) O13 0.019(2) 0.028(2) 0.020(2) -0.0046(18) 0.0057(17) -0.0065(18) O14 0.018(2) 0.026(2) 0.021(2) -0.0056(18) 0.0002(17) -0.0043(18) N1 0.017(3) 0.028(3) 0.004(2) -0.004(2) 0.0034(18) -0.006(2) N2 0.016(3) 0.032(3) 0.011(2) -0.006(2) 0.0077(19) -0.006(2) N3 0.026(3) 0.026(3) 0.012(2) -0.003(2) 0.002(2) -0.008(2) N4 0.021(3) 0.032(3) 0.016(3) -0.005(2) 0.003(2) -0.010(2) N5 0.016(2) 0.027(3) 0.006(2) -0.004(2) 0.0054(18) -0.005(2) N6 0.021(3) 0.024(3) 0.011(2) -0.001(2) 0.003(2) -0.007(2) N7 0.024(3) 0.040(3) 0.030(3) -0.016(3) -0.001(2) -0.011(3) N8 0.020(3) 0.030(3) 0.006(2) -0.005(2) 0.0040(19) -0.007(2) C1 0.012(3) 0.031(3) 0.012(3) -0.006(3) 0.006(2) -0.005(3) C2 0.019(3) 0.029(3) 0.012(3) -0.004(3) 0.003(2) -0.007(3) C3 0.018(3) 0.032(4) 0.011(3) -0.005(3) 0.005(2) -0.002(3) C4 0.022(3) 0.034(4) 0.008(3) -0.006(3) 0.002(2) -0.003(3) C5 0.015(3) 0.032(3) 0.012(3) -0.007(3) 0.002(2) -0.002(3) C6 0.016(3) 0.030(3) 0.013(3) -0.006(3) 0.002(2) -0.010(3) C7 0.018(3) 0.033(4) 0.010(3) -0.009(3) 0.009(2) -0.005(3) C8 0.019(3) 0.026(3) 0.012(3) -0.005(2) 0.002(2) -0.009(3) C9 0.015(3) 0.035(4) 0.011(3) -0.011(3) 0.005(2) -0.004(3) C10 0.025(4) 0.049(4) 0.026(4) -0.013(3) 0.002(3) -0.016(3) C11 0.033(4) 0.052(5) 0.033(4) -0.008(3) -0.012(3) -0.015(4) C12 0.029(4) 0.047(4) 0.018(3) -0.005(3) -0.008(3) -0.007(3) C13 0.027(3) 0.027(3) 0.018(3) -0.007(3) 0.001(3) -0.004(3) C14 0.023(3) 0.031(4) 0.015(3) -0.007(3) -0.002(3) -0.006(3) C15 0.056(5) 0.031(4) 0.026(4) 0.005(3) 0.011(3) -0.005(4) C16 0.019(3) 0.039(4) 0.015(3) -0.006(3) 0.011(2) -0.008(3) C17 0.023(3) 0.036(4) 0.012(3) -0.006(3) 0.000(2) -0.005(3) C18 0.025(4) 0.059(5) 0.028(4) -0.019(3) -0.009(3) 0.001(3) C19 0.017(3) 0.027(3) 0.009(3) -0.010(2) 0.004(2) -0.008(3) C20 0.035(4) 0.027(3) 0.019(3) -0.002(3) 0.000(3) -0.015(3) C21 0.024(4) 0.047(4) 0.018(3) -0.009(3) 0.007(3) -0.023(3) C22 0.015(3) 0.044(4) 0.019(3) -0.013(3) 0.002(2) -0.008(3) C23 0.023(3) 0.025(3) 0.011(3) -0.004(2) -0.001(2) -0.003(3) C24 0.020(3) 0.029(4) 0.022(3) -0.007(3) 0.004(3) -0.005(3) C25 0.020(3) 0.031(3) 0.011(3) -0.005(3) 0.009(2) -0.009(3) C26 0.023(3) 0.029(4) 0.022(3) -0.007(3) -0.001(3) -0.003(3) C27 0.027(4) 0.037(4) 0.016(3) -0.004(3) 0.002(3) -0.004(3) C28 0.032(4) 0.028(4) 0.027(4) 0.001(3) 0.003(3) -0.007(3) C29 0.023(3) 0.029(4) 0.029(4) -0.006(3) 0.000(3) -0.008(3) C30 0.016(3) 0.032(3) 0.009(3) -0.002(2) 0.004(2) -0.010(3) C31 0.012(3) 0.037(4) 0.015(3) -0.008(3) 0.002(2) -0.001(3) C32 0.020(3) 0.041(4) 0.010(3) -0.006(3) 0.001(2) -0.008(3) C33 0.022(3) 0.034(4) 0.012(3) -0.006(3) 0.005(2) -0.004(3) C34 0.017(3) 0.032(4) 0.014(3) -0.008(3) 0.005(2) -0.005(3) C35 0.018(3) 0.025(3) 0.010(3) -0.005(2) 0.005(2) -0.003(3) C36 0.014(3) 0.024(3) 0.008(3) -0.004(2) 0.006(2) -0.006(2) C37 0.022(3) 0.039(4) 0.013(3) -0.005(3) 0.006(2) -0.016(3) C38 0.023(3) 0.032(3) 0.004(3) -0.003(2) 0.005(2) -0.011(3) C39 0.014(3) 0.032(4) 0.025(3) -0.010(3) -0.007(3) -0.001(3) C40 0.041(4) 0.040(4) 0.048(5) -0.018(4) -0.007(4) -0.009(4) C41 0.044(5) 0.050(5) 0.055(5) 0.001(4) -0.007(4) -0.030(4) C42 0.031(4) 0.061(5) 0.049(5) -0.014(4) 0.015(4) -0.029(4) C43 0.026(4) 0.050(5) 0.029(4) -0.015(3) 0.010(3) -0.012(3) C44 0.029(4) 0.038(4) 0.022(4) -0.013(3) -0.001(3) -0.006(3) C45 0.028(5) 0.115(9) 0.052(5) -0.009(6) -0.005(4) 0.000(5) C46 0.026(3) 0.030(4) 0.016(3) -0.002(3) 0.001(3) -0.010(3) C47 0.026(3) 0.030(4) 0.014(3) -0.008(3) -0.001(3) -0.006(3) C48 0.056(5) 0.026(4) 0.037(4) -0.011(3) -0.006(4) -0.007(3) C49 0.0159(15) 0.0167(15) 0.0143(14) -0.0046(10) 0.0006(9) -0.0028(9) C50 0.017(3) 0.036(4) 0.012(3) -0.003(3) 0.005(2) -0.008(3) C51 0.015(3) 0.040(4) 0.009(3) -0.008(3) 0.004(2) -0.008(3) C52 0.016(3) 0.037(4) 0.010(3) -0.006(3) 0.004(2) 0.000(3) C53 0.021(3) 0.031(4) 0.011(3) -0.008(3) 0.005(2) -0.006(3) C54 0.022(3) 0.027(3) 0.007(3) -0.005(2) 0.006(2) -0.006(3) C55 0.020(3) 0.030(4) 0.011(3) -0.006(3) 0.002(2) -0.002(3) C56 0.019(3) 0.030(4) 0.016(3) -0.005(3) 0.007(2) -0.007(3) C57 0.028(4) 0.025(3) 0.023(3) -0.002(3) 0.000(3) -0.008(3) C58 0.027(4) 0.023(3) 0.018(3) -0.001(3) 0.003(3) 0.001(3) C59 0.017(3) 0.032(4) 0.012(3) -0.004(3) 0.003(2) -0.008(3) Cu3 0.0229(4) 0.0261(4) 0.0179(4) -0.0068(3) 0.0059(3) -0.0064(3) Cu4 0.0177(4) 0.0250(4) 0.0094(3) -0.0023(3) 0.0033(3) -0.0060(3) Cl9 0.0214(8) 0.0490(11) 0.0341(9) -0.0166(8) 0.0059(7) -0.0050(7) Cl10 0.0333(10) 0.0708(14) 0.0421(11) -0.0366(10) 0.0075(8) 0.0016(9) Cl11 0.0392(10) 0.0611(12) 0.0343(9) -0.0295(9) 0.0023(8) -0.0108(9) Cl12 0.0245(8) 0.0433(10) 0.0292(8) -0.0133(7) 0.0017(7) -0.0080(7) Cl13 0.0263(9) 0.0568(11) 0.0319(9) -0.0215(8) 0.0144(7) -0.0195(8) Cl14 0.0541(11) 0.0445(10) 0.0202(8) -0.0136(7) 0.0226(8) -0.0246(9) Cl15 0.0591(12) 0.0406(10) 0.0105(7) -0.0043(7) 0.0008(7) -0.0061(9) Cl16 0.0334(9) 0.0468(10) 0.0195(8) -0.0071(7) -0.0058(7) -0.0051(8) O15 0.048(3) 0.022(3) 0.048(3) -0.004(2) 0.015(2) 0.000(2) O16 0.103(6) 0.060(4) 0.102(5) -0.048(4) 0.054(4) -0.054(4) O17 0.058(3) 0.038(3) 0.041(3) -0.024(2) 0.009(3) -0.013(3) O18 0.041(3) 0.039(3) 0.059(4) 0.001(3) -0.003(3) 0.009(3) O19 0.037(3) 0.053(3) 0.048(3) -0.014(3) -0.014(2) 0.002(3) O20 0.022(2) 0.029(2) 0.017(2) -0.0084(18) 0.0060(17) -0.0051(18) O21 0.025(2) 0.033(3) 0.020(2) -0.0080(19) 0.0036(18) -0.008(2) O22 0.024(2) 0.029(2) 0.019(2) -0.0099(19) 0.0052(18) -0.0056(19) O23 0.038(3) 0.031(3) 0.046(3) -0.005(2) -0.020(2) -0.002(2) O24 0.024(2) 0.027(3) 0.038(3) -0.009(2) -0.010(2) 0.003(2) O25 0.039(3) 0.055(3) 0.021(2) -0.016(2) 0.000(2) -0.023(3) O26 0.041(3) 0.031(2) 0.012(2) -0.0078(18) 0.0042(18) -0.013(2) O27 0.021(2) 0.038(3) 0.010(2) -0.0080(18) 0.0037(16) -0.0094(19) O28 0.021(2) 0.036(3) 0.016(2) -0.0076(19) 0.0048(17) -0.0077(19) N9 0.023(3) 0.015(3) 0.022(3) -0.003(2) 0.003(2) -0.002(2) N10 0.031(3) 0.026(3) 0.022(3) -0.004(2) 0.011(2) -0.005(2) N11 0.028(3) 0.026(3) 0.026(3) -0.008(2) 0.007(2) -0.012(2) N12 0.033(3) 0.044(4) 0.039(3) -0.021(3) 0.013(3) -0.006(3) N13 0.016(2) 0.019(3) 0.011(2) -0.001(2) 0.0006(19) -0.003(2) N14 0.020(3) 0.021(3) 0.011(2) -0.002(2) 0.0027(19) -0.007(2) N15 0.018(3) 0.024(3) 0.015(2) -0.003(2) 0.002(2) -0.005(2) N16 0.019(3) 0.022(3) 0.015(2) -0.002(2) 0.002(2) -0.005(2) C61 0.028(4) 0.030(4) 0.024(3) -0.011(3) 0.010(3) -0.010(3) C62 0.035(4) 0.028(4) 0.029(4) -0.011(3) 0.017(3) -0.011(3) C63 0.037(4) 0.025(4) 0.032(4) -0.002(3) 0.013(3) -0.011(3) C64 0.040(4) 0.023(3) 0.019(3) 0.001(3) 0.004(3) -0.004(3) C65 0.027(4) 0.031(4) 0.026(3) -0.004(3) 0.005(3) -0.003(3) C66 0.027(3) 0.019(3) 0.021(3) -0.002(3) 0.005(3) -0.007(3) C67 0.036(4) 0.025(4) 0.027(4) -0.001(3) 0.017(3) -0.006(3) C68 0.022(3) 0.018(3) 0.017(3) -0.001(2) 0.001(2) -0.003(3) C69 0.033(4) 0.025(3) 0.027(3) -0.010(3) 0.005(3) -0.010(3) C70 0.026(4) 0.044(4) 0.032(4) -0.015(3) 0.004(3) -0.012(3) C71 0.037(4) 0.052(5) 0.051(5) -0.021(4) -0.004(4) -0.015(4) C72 0.048(5) 0.067(6) 0.048(5) -0.035(4) -0.006(4) -0.016(4) C73 0.042(5) 0.041(4) 0.039(4) -0.021(3) 0.006(3) -0.014(4) C74 0.040(4) 0.037(4) 0.055(5) -0.023(4) 0.016(4) -0.016(4) C75 0.075(7) 0.049(5) 0.070(6) -0.042(5) 0.003(5) -0.004(5) C76 0.048(5) 0.034(4) 0.023(4) -0.003(3) 0.020(3) -0.010(3) C77 0.042(5) 0.029(4) 0.026(4) 0.010(3) -0.002(3) -0.005(3) C78 0.053(6) 0.085(7) 0.049(5) -0.018(5) -0.028(4) 0.010(5) C79 0.026(4) 0.027(4) 0.022(3) -0.004(3) 0.003(3) -0.003(3) C80 0.044(5) 0.061(5) 0.049(5) -0.032(4) 0.021(4) -0.010(4) C81 0.035(5) 0.057(5) 0.062(6) -0.019(5) 0.027(4) -0.005(4) C82 0.030(4) 0.045(5) 0.057(5) -0.009(4) 0.013(4) -0.008(4) C83 0.030(4) 0.033(4) 0.037(4) -0.010(3) 0.003(3) -0.009(3) C84 0.028(3) 0.020(3) 0.012(3) 0.000(2) 0.001(2) -0.004(3) C85 0.027(3) 0.018(3) 0.015(3) 0.000(2) 0.006(2) -0.006(3) C86 0.019(3) 0.024(3) 0.021(3) -0.005(3) 0.006(2) -0.002(3) C87 0.033(4) 0.032(4) 0.019(3) -0.011(3) 0.007(3) -0.002(3) C88 0.030(4) 0.031(4) 0.019(3) -0.010(3) 0.002(3) -0.004(3) C89 0.020(3) 0.026(3) 0.019(3) -0.003(3) 0.000(2) -0.002(3) C90 0.018(3) 0.023(3) 0.011(3) 0.000(2) 0.003(2) -0.002(3) C91 0.016(3) 0.025(3) 0.012(3) -0.002(2) 0.000(2) -0.007(3) C92 0.018(3) 0.022(3) 0.012(3) -0.001(2) 0.004(2) -0.003(3) C93 0.022(3) 0.024(3) 0.008(3) 0.001(2) 0.002(2) -0.007(3) C94 0.016(3) 0.022(3) 0.014(3) -0.002(2) 0.002(2) -0.007(2) C95 0.021(3) 0.023(3) 0.010(3) -0.006(2) 0.001(2) -0.010(3) C96 0.019(3) 0.022(3) 0.012(3) -0.002(2) 0.003(2) -0.007(3) C97 0.017(3) 0.020(3) 0.014(3) -0.001(2) 0.004(2) -0.011(3) C98 0.014(3) 0.020(3) 0.015(3) -0.005(2) 0.002(2) -0.002(2) C99 0.016(3) 0.015(3) 0.016(3) 0.001(2) 0.002(2) 0.000(2) C100 0.027(3) 0.029(3) 0.014(3) -0.001(3) 0.006(3) -0.009(3) C101 0.021(3) 0.024(3) 0.027(3) 0.003(3) 0.002(3) -0.003(3) C102 0.019(3) 0.030(4) 0.026(3) -0.003(3) -0.003(3) -0.008(3) C103 0.019(3) 0.030(3) 0.015(3) -0.002(3) -0.002(2) -0.005(3) C104 0.021(3) 0.026(3) 0.011(3) 0.001(2) 0.002(2) -0.011(3) C105 0.021(3) 0.030(4) 0.035(4) -0.005(3) -0.003(3) 0.003(3) C106 0.026(3) 0.029(4) 0.016(3) 0.000(3) 0.004(3) -0.009(3) C107 0.025(3) 0.029(3) 0.008(3) -0.003(3) 0.002(2) -0.005(3) C108 0.080(6) 0.045(5) 0.010(3) -0.008(3) 0.003(3) -0.016(4) C109 0.018(3) 0.020(3) 0.016(3) -0.006(2) 0.001(2) -0.005(2) C110 0.017(3) 0.031(4) 0.022(3) -0.003(3) 0.002(3) -0.001(3) C111 0.021(3) 0.045(4) 0.028(4) -0.011(3) -0.004(3) -0.002(3) C112 0.030(4) 0.036(4) 0.018(3) -0.008(3) -0.004(3) 0.000(3) C113 0.022(3) 0.028(3) 0.018(3) -0.008(3) -0.001(3) 0.000(3) C114 0.027(3) 0.020(3) 0.013(3) -0.006(2) 0.004(2) -0.004(3) C115 0.023(3) 0.022(3) 0.015(3) -0.004(2) 0.005(2) -0.009(3) C116 0.026(3) 0.029(4) 0.024(3) -0.010(3) 0.009(3) -0.011(3) C117 0.047(4) 0.029(4) 0.012(3) -0.012(3) 0.017(3) -0.018(3) C118 0.046(4) 0.030(4) 0.008(3) -0.006(3) 0.004(3) -0.008(3) C119 0.024(3) 0.025(3) 0.016(3) -0.008(3) 0.005(2) -0.002(3) N17 0.170(13) 0.122(9) 0.082(8) -0.037(7) -0.061(8) -0.027(9) C121 0.165(14) 0.060(7) 0.029(5) -0.015(5) -0.021(7) -0.025(8) C122 0.103(9) 0.093(8) 0.044(6) -0.038(5) 0.023(6) -0.035(7) N18 0.093(8) 0.121(9) 0.092(8) -0.024(7) -0.008(7) -0.030(7) C123 0.078(8) 0.088(8) 0.057(6) -0.008(6) -0.033(6) -0.032(7) C124 0.106(10) 0.088(9) 0.106(10) -0.034(8) -0.053(8) 0.010(8) N19 0.093(7) 0.086(7) 0.092(7) -0.038(6) -0.044(6) 0.020(6) C125 0.064(7) 0.063(6) 0.060(6) -0.022(5) -0.003(5) -0.002(5) C126 0.108(10) 0.077(8) 0.084(8) -0.021(7) -0.010(7) 0.016(7) N20 0.100(7) 0.075(6) 0.077(6) -0.023(5) -0.024(6) 0.006(5) C127 0.054(6) 0.048(5) 0.049(5) -0.009(4) -0.009(4) 0.004(4) C128 0.049(6) 0.104(8) 0.061(6) -0.031(6) -0.010(5) -0.002(5) N23 0.100(8) 0.099(8) 0.073(7) 0.000(6) 0.006(5) -0.022(7) C133 0.072(7) 0.061(7) 0.058(6) -0.012(5) -0.003(5) -0.010(6) C134 0.124(13) 0.112(12) 0.185(17) -0.062(11) -0.017(11) -0.046(10) N26 0.121(11) 0.186(15) 0.143(12) -0.004(10) 0.041(9) -0.078(11) C139 0.051(6) 0.093(8) 0.073(7) -0.028(6) -0.007(5) -0.004(6) C140 0.109(10) 0.069(8) 0.176(14) -0.027(9) -0.049(10) -0.034(8) N27 0.078(6) 0.095(7) 0.072(6) -0.044(5) 0.016(5) 0.001(5) C141 0.082(7) 0.050(5) 0.048(5) -0.024(4) 0.006(5) -0.001(5) C142 0.092(9) 0.063(7) 0.126(11) -0.027(7) 0.030(8) -0.026(6) N28 0.31(3) 0.32(3) 0.106(12) -0.105(15) 0.085(14) -0.17(2) C143 0.212(19) 0.102(10) 0.064(8) -0.016(8) -0.014(10) -0.048(11) C144 0.061(7) 0.081(8) 0.090(8) -0.030(6) -0.006(6) 0.003(6) N29 0.089(7) 0.068(6) 0.104(8) -0.019(6) -0.027(6) -0.016(5) C145 0.066(7) 0.058(6) 0.062(6) -0.019(5) -0.011(5) -0.007(5) C146 0.194(17) 0.110(11) 0.076(9) -0.027(8) -0.009(10) -0.030(11) _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 O7 1.898(4) . ? Cu1 O6 1.947(4) . ? Cu1 N4 1.995(5) . ? Cu1 N1 2.094(5) . ? Cu1 N2 2.293(5) . ? Cu2 O13 1.914(4) . ? Cu2 O14 1.930(4) . ? Cu2 N8 1.986(5) . ? Cu2 N5 2.071(5) . ? Cu2 N6 2.281(5) . ? Cl1 C26 1.730(6) . ? Cl2 C27 1.743(6) . ? Cl3 C28 1.719(7) . ? Cl4 C29 1.726(6) . ? Cl5 C59 1.742(6) . ? Cl6 C58 1.744(6) . ? Cl7 C57 1.731(6) . ? Cl8 C56 1.748(6) . ? O1 C7 1.193(7) . ? O2 C14 1.201(7) . ? O3 C14 1.336(7) . ? O3 C15 1.447(8) . ? O4 C17 1.198(7) . ? O5 C17 1.328(7) . ? O5 C18 1.447(7) . ? O6 C24 1.340(7) . ? O7 C25 1.334(7) . ? O8 C37 1.204(7) . ? O9 C44 1.203(7) . ? O10 C44 1.321(8) . ? O10 C45 1.445(9) . ? O11 C47 1.204(7) . ? O12 C47 1.318(7) . ? O12 C48 1.441(8) . ? O13 C54 1.315(7) . ? O14 C55 1.324(7) . ? N1 C1 1.487(7) . ? N1 C6 1.506(7) . ? N1 C8 1.520(7) . ? N2 C3 1.460(8) . ? N2 C4 1.477(7) . ? N2 C16 1.485(7) . ? N3 C19 1.335(7) . ? N3 C20 1.358(8) . ? N4 C10 1.332(8) . ? N4 C9 1.355(8) . ? N5 C36 1.505(7) . ? N5 C31 1.510(7) . ? N5 C38 1.516(6) . ? N6 C33 1.459(8) . ? N6 C34 1.478(8) . ? N6 C46 1.479(7) . ? N7 C39 1.312(8) . ? N7 C40 1.338(9) . ? N8 C49 1.339(7) . ? N8 C50 1.346(7) . ? C1 C9 1.516(8) . ? C1 C2 1.562(8) . ? C2 C14 1.510(9) . ? C2 C7 1.548(8) . ? C2 C3 1.570(8) . ? C4 C5 1.576(8) . ? C5 C7 1.518(8) . ? C5 C17 1.528(8) . ? C5 C6 1.555(8) . ? C6 C19 1.526(7) . ? C8 C30 1.525(7) . ? C9 C13 1.394(8) . ? C10 C11 1.392(9) . ? C11 C12 1.385(10) . ? C12 C13 1.373(9) . ? C19 C23 1.393(8) . ? C20 C21 1.377(9) . ? C21 C22 1.369(9) . ? C22 C23 1.390(8) . ? C24 C29 1.392(9) . ? C24 C25 1.415(8) . ? C25 C26 1.395(8) . ? C26 C27 1.392(9) . ? C27 C28 1.376(9) . ? C28 C29 1.416(9) . ? C30 C38 1.519(8) . ? C31 C39 1.517(9) . ? C31 C32 1.562(8) . ? C32 C37 1.527(9) . ? C32 C44 1.534(8) . ? C32 C33 1.557(9) . ? C34 C35 1.548(8) . ? C35 C47 1.524(8) . ? C35 C37 1.535(8) . ? C35 C36 1.577(7) . ? C36 C49 1.512(8) . ? C39 C43 1.411(9) . ? C40 C41 1.378(11) . ? C41 C42 1.362(11) . ? C42 C43 1.386(10) . ? C49 C53 1.386(8) . ? C50 C51 1.390(8) . ? C51 C52 1.384(9) . ? C52 C53 1.385(8) . ? C54 C59 1.393(8) . ? C54 C55 1.428(8) . ? C55 C56 1.392(9) . ? C56 C57 1.402(9) . ? C57 C58 1.377(9) . ? C58 C59 1.400(9) . ? Cu3 O20 1.910(4) . ? Cu3 O21 1.938(4) . ? Cu3 N11 1.966(5) . ? Cu3 N9 2.082(5) . ? Cu3 N10 2.306(5) . ? Cu4 O27 1.918(4) . ? Cu4 O28 1.923(4) . ? Cu4 N16 1.996(5) . ? Cu4 N13 2.090(4) . ? Cu4 N14 2.273(5) . ? Cl9 C86 1.735(6) . ? Cl10 C87 1.736(6) . ? Cl11 C88 1.734(6) . ? Cl12 C89 1.738(6) . ? Cl13 C116 1.728(7) . ? Cl14 C117 1.736(6) . ? Cl15 C118 1.735(6) . ? Cl16 C119 1.741(6) . ? O15 C67 1.215(8) . ? O16 C74 1.211(9) . ? O17 C74 1.327(9) . ? O17 C75 1.448(9) . ? O18 C77 1.197(9) . ? O19 C77 1.340(9) . ? O19 C78 1.428(9) . ? O20 C84 1.323(7) . ? O21 C85 1.310(7) . ? O22 C97 1.199(7) . ? O23 C104 1.199(7) . ? O24 C104 1.308(7) . ? O24 C105 1.444(7) . ? O25 C107 1.201(7) . ? O26 C107 1.327(7) . ? O26 C108 1.471(7) . ? O27 C114 1.337(7) . ? O28 C115 1.331(7) . ? N9 C66 1.500(8) . ? N9 C61 1.506(8) . ? N9 C68 1.512(7) . ? N10 C64 1.469(9) . ? N10 C63 1.468(9) . ? N10 C76 1.484(8) . ? N11 C70 1.346(8) . ? N11 C69 1.371(8) . ? N12 C79 1.331(8) . ? N12 C80 1.349(9) . ? N13 C96 1.503(7) . ? N13 C98 1.505(7) . ? N13 C91 1.505(7) . ? N14 C93 1.467(7) . ? N14 C106 1.471(7) . ? N14 C94 1.480(7) . ? N15 C99 1.354(7) . ? N15 C100 1.354(7) . ? N16 C110 1.330(8) . ? N16 C109 1.370(7) . ? C61 C69 1.510(9) . ? C61 C62 1.575(9) . ? C62 C74 1.511(10) . ? C62 C67 1.527(10) . ? C62 C63 1.556(8) . ? C64 C65 1.554(9) . ? C65 C77 1.513(10) . ? C65 C67 1.519(10) . ? C65 C66 1.562(8) . ? C66 C79 1.532(8) . ? C68 C90 1.507(8) . ? C69 C73 1.376(9) . ? C70 C71 1.379(10) . ? C71 C72 1.382(11) . ? C72 C73 1.376(11) . ? C79 C83 1.388(9) . ? C80 C81 1.359(12) . ? C81 C82 1.359(12) . ? C82 C83 1.401(10) . ? C84 C89 1.389(8) . ? C84 C85 1.429(9) . ? C85 C86 1.405(8) . ? C86 C87 1.389(9) . ? C87 C88 1.397(9) . ? C88 C89 1.402(8) . ? C90 C98 1.534(7) . ? C91 C99 1.516(8) . ? C91 C92 1.553(8) . ? C92 C97 1.535(8) . ? C92 C104 1.537(8) . ? C92 C93 1.564(7) . ? C94 C95 1.555(7) . ? C95 C107 1.528(8) . ? C95 C97 1.533(8) . ? C95 C96 1.562(8) . ? C96 C109 1.506(8) . ? C99 C103 1.373(8) . ? C100 C101 1.373(9) . ? C101 C102 1.384(9) . ? C102 C103 1.395(8) . ? C109 C113 1.389(8) . ? C110 C111 1.381(9) . ? C111 C112 1.406(9) . ? C112 C113 1.386(9) . ? C114 C119 1.390(8) . ? C114 C115 1.421(8) . ? C115 C116 1.395(8) . ? C116 C117 1.407(9) . ? C117 C118 1.359(10) . ? C118 C119 1.412(8) . ? N17 C121 1.132(17) . ? C121 C122 1.425(17) . ? N18 C123 1.167(15) . ? C123 C124 1.360(17) . ? N19 C125 1.070(11) . ? C125 C126 1.490(14) . ? N20 C127 1.146(11) . ? C127 C128 1.441(13) . ? N21 C129 1.16(2) . ? C129 C130 1.354(19) . ? N22 C131 1.25(2) . ? C131 C132 1.432(19) . ? N23 C133 1.140(13) . ? C133 C134 1.399(16) . ? N24 C135 1.57(3) . ? C135 C136 1.46(3) . ? N25 C137 1.33(3) . ? C137 C138 1.54(3) . ? N26 C139 1.131(15) . ? C139 C140 1.411(16) . ? N27 C141 1.126(12) . ? C141 C142 1.416(14) . ? N28 C143 1.22(2) . ? C143 C144 1.495(19) . ? N29 C145 1.102(12) . ? C145 C146 1.381(15) . ? C147 C148 1.27(4) . ? C149 C150 1.36(4) 2_556 ? C149 C150 1.54(4) . ? C150 C149 1.36(4) 2_556 ? C150 C150 1.76(6) 2_556 ? N32 C151 1.24(4) . ? N33 C153 1.27(3) . ? N33 C151 1.85(4) . ? C151 C153 1.57(4) . ? C151 C152 1.65(4) . ? C152 C153 1.44(3) . ? N34 C154 1.19(3) . ? C154 C155 1.41(4) . ? C155 C156 1.47(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 O7 Cu1 O6 86.71(17) . . ? O7 Cu1 N4 168.79(19) . . ? O6 Cu1 N4 98.66(18) . . ? O7 Cu1 N1 91.77(17) . . ? O6 Cu1 N1 164.11(18) . . ? N4 Cu1 N1 80.36(18) . . ? O7 Cu1 N2 95.10(18) . . ? O6 Cu1 N2 113.65(17) . . ? N4 Cu1 N2 91.76(19) . . ? N1 Cu1 N2 82.24(17) . . ? O13 Cu2 O14 87.22(17) . . ? O13 Cu2 N8 166.42(17) . . ? O14 Cu2 N8 96.70(18) . . ? O13 Cu2 N5 93.48(18) . . ? O14 Cu2 N5 175.64(17) . . ? N8 Cu2 N5 81.66(19) . . ? O13 Cu2 N6 96.32(17) . . ? O14 Cu2 N6 100.47(17) . . ? N8 Cu2 N6 95.74(18) . . ? N5 Cu2 N6 83.74(17) . . ? C14 O3 C15 114.9(5) . . ? C17 O5 C18 115.6(5) . . ? C24 O6 Cu1 108.4(4) . . ? C25 O7 Cu1 110.1(4) . . ? C44 O10 C45 115.3(6) . . ? C47 O12 C48 115.7(5) . . ? C54 O13 Cu2 108.8(3) . . ? C55 O14 Cu2 108.3(4) . . ? C1 N1 C6 115.4(5) . . ? C1 N1 C8 111.6(4) . . ? C6 N1 C8 109.9(4) . . ? C1 N1 Cu1 106.6(3) . . ? C6 N1 Cu1 112.6(3) . . ? C8 N1 Cu1 99.7(3) . . ? C3 N2 C4 111.1(5) . . ? C3 N2 C16 109.6(5) . . ? C4 N2 C16 108.8(4) . . ? C3 N2 Cu1 116.9(3) . . ? C4 N2 Cu1 105.4(3) . . ? C16 N2 Cu1 104.6(4) . . ? C19 N3 C20 117.6(5) . . ? C10 N4 C9 118.8(5) . . ? C10 N4 Cu1 125.7(4) . . ? C9 N4 Cu1 115.3(4) . . ? C36 N5 C31 113.7(4) . . ? C36 N5 C38 105.9(4) . . ? C31 N5 C38 109.9(4) . . ? C36 N5 Cu2 104.8(3) . . ? C31 N5 Cu2 115.3(4) . . ? C38 N5 Cu2 106.6(3) . . ? C33 N6 C34 112.2(5) . . ? C33 N6 C46 109.5(5) . . ? C34 N6 C46 109.2(4) . . ? C33 N6 Cu2 108.7(3) . . ? C34 N6 Cu2 110.7(3) . . ? C46 N6 Cu2 106.4(3) . . ? C39 N7 C40 119.6(6) . . ? C49 N8 C50 119.4(5) . . ? C49 N8 Cu2 115.2(4) . . ? C50 N8 Cu2 125.1(4) . . ? N1 C1 C9 107.1(5) . . ? N1 C1 C2 113.7(4) . . ? C9 C1 C2 111.1(5) . . ? C14 C2 C7 106.8(5) . . ? C14 C2 C1 112.3(5) . . ? C7 C2 C1 113.5(5) . . ? C14 C2 C3 108.7(5) . . ? C7 C2 C3 102.3(4) . . ? C1 C2 C3 112.6(5) . . ? N2 C3 C2 110.4(5) . . ? N2 C4 C5 113.1(4) . . ? C7 C5 C17 112.9(5) . . ? C7 C5 C6 109.6(5) . . ? C17 C5 C6 111.0(5) . . ? C7 C5 C4 104.8(5) . . ? C17 C5 C4 103.3(4) . . ? C6 C5 C4 115.1(5) . . ? N1 C6 C19 110.4(4) . . ? N1 C6 C5 111.4(5) . . ? C19 C6 C5 110.1(5) . . ? O1 C7 C5 127.6(5) . . ? O1 C7 C2 121.4(6) . . ? C5 C7 C2 109.9(5) . . ? N1 C8 C30 119.4(5) . . ? N4 C9 C13 121.5(5) . . ? N4 C9 C1 115.4(5) . . ? C13 C9 C1 123.1(5) . . ? N4 C10 C11 122.5(6) . . ? C12 C11 C10 118.4(6) . . ? C13 C12 C11 119.7(6) . . ? C12 C13 C9 119.0(6) . . ? O2 C14 O3 123.8(6) . . ? O2 C14 C2 124.9(5) . . ? O3 C14 C2 111.2(5) . . ? O4 C17 O5 123.8(5) . . ? O4 C17 C5 123.9(6) . . ? O5 C17 C5 112.0(5) . . ? N3 C19 C23 123.5(5) . . ? N3 C19 C6 113.9(5) . . ? C23 C19 C6 122.6(5) . . ? N3 C20 C21 122.2(6) . . ? C22 C21 C20 119.4(6) . . ? C21 C22 C23 119.6(6) . . ? C22 C23 C19 117.6(6) . . ? O6 C24 C29 124.5(6) . . ? O6 C24 C25 117.2(5) . . ? C29 C24 C25 118.3(6) . . ? O7 C25 C26 122.7(5) . . ? O7 C25 C24 117.3(5) . . ? C26 C25 C24 119.9(5) . . ? C27 C26 C25 120.6(6) . . ? C27 C26 Cl1 122.2(5) . . ? C25 C26 Cl1 117.3(5) . . ? C28 C27 C26 120.6(6) . . ? C28 C27 Cl2 119.7(5) . . ? C26 C27 Cl2 119.6(5) . . ? C27 C28 C29 119.0(6) . . ? C27 C28 Cl3 120.4(5) . . ? C29 C28 Cl3 120.5(5) . . ? C24 C29 C28 121.4(6) . . ? C24 C29 Cl4 119.2(5) . . ? C28 C29 Cl4 119.4(5) . . ? C38 C30 C8 107.3(5) . . ? N5 C31 C39 111.6(5) . . ? N5 C31 C32 112.3(4) . . ? C39 C31 C32 107.3(5) . . ? C37 C32 C44 112.4(5) . . ? C37 C32 C33 104.8(5) . . ? C44 C32 C33 103.2(5) . . ? C37 C32 C31 110.0(5) . . ? C44 C32 C31 112.0(5) . . ? C33 C32 C31 114.1(5) . . ? N6 C33 C32 113.7(5) . . ? N6 C34 C35 111.1(4) . . ? C47 C35 C37 110.5(5) . . ? C47 C35 C34 107.6(5) . . ? C37 C35 C34 102.4(5) . . ? C47 C35 C36 108.4(5) . . ? C37 C35 C36 113.0(4) . . ? C34 C35 C36 114.7(5) . . ? N5 C36 C49 107.7(4) . . ? N5 C36 C35 112.6(4) . . ? C49 C36 C35 109.7(4) . . ? O8 C37 C32 126.3(6) . . ? O8 C37 C35 121.6(6) . . ? C32 C37 C35 109.9(5) . . ? N5 C38 C30 114.8(5) . . ? N7 C39 C43 121.4(6) . . ? N7 C39 C31 115.7(5) . . ? C43 C39 C31 122.9(6) . . ? N7 C40 C41 122.2(7) . . ? C42 C41 C40 119.4(7) . . ? C41 C42 C43 118.9(7) . . ? C42 C43 C39 118.5(7) . . ? O9 C44 O10 123.1(6) . . ? O9 C44 C32 123.5(6) . . ? O10 C44 C32 113.2(5) . . ? O11 C47 O12 124.4(6) . . ? O11 C47 C35 123.7(6) . . ? O12 C47 C35 111.9(5) . . ? N8 C49 C53 122.4(5) . . ? N8 C49 C36 114.7(5) . . ? C53 C49 C36 122.9(5) . . ? N8 C50 C51 121.0(6) . . ? C52 C51 C50 119.5(5) . . ? C51 C52 C53 119.2(6) . . ? C49 C53 C52 118.5(6) . . ? O13 C54 C59 123.4(5) . . ? O13 C54 C55 117.9(5) . . ? C59 C54 C55 118.7(5) . . ? O14 C55 C56 124.0(5) . . ? O14 C55 C54 117.3(5) . . ? C56 C55 C54 118.6(5) . . ? C55 C56 C57 121.8(5) . . ? C55 C56 Cl8 117.8(5) . . ? C57 C56 Cl8 120.4(5) . . ? C58 C57 C56 119.3(6) . . ? C58 C57 Cl7 120.7(5) . . ? C56 C57 Cl7 119.9(5) . . ? C57 C58 C59 120.0(6) . . ? C57 C58 Cl6 120.1(5) . . ? C59 C58 Cl6 119.7(5) . . ? C54 C59 C58 121.5(5) . . ? C54 C59 Cl5 117.1(5) . . ? C58 C59 Cl5 121.4(5) . . ? O20 Cu3 O21 87.16(17) . . ? O20 Cu3 N11 168.65(19) . . ? O21 Cu3 N11 95.4(2) . . ? O20 Cu3 N9 94.06(18) . . ? O21 Cu3 N9 171.81(18) . . ? N11 Cu3 N9 81.8(2) . . ? O20 Cu3 N10 95.53(19) . . ? O21 Cu3 N10 105.08(18) . . ? N11 Cu3 N10 94.5(2) . . ? N9 Cu3 N10 82.88(18) . . ? O27 Cu4 O28 87.56(17) . . ? O27 Cu4 N16 166.91(19) . . ? O28 Cu4 N16 93.53(18) . . ? O27 Cu4 N13 95.46(17) . . ? O28 Cu4 N13 171.04(18) . . ? N16 Cu4 N13 81.64(18) . . ? O27 Cu4 N14 95.91(17) . . ? O28 Cu4 N14 105.70(17) . . ? N16 Cu4 N14 96.34(18) . . ? N13 Cu4 N14 82.42(17) . . ? C74 O17 C75 116.7(6) . . ? C77 O19 C78 117.3(6) . . ? C84 O20 Cu3 109.3(4) . . ? C85 O21 Cu3 108.1(4) . . ? C104 O24 C105 117.4(5) . . ? C107 O26 C108 113.4(5) . . ? C114 O27 Cu4 108.5(4) . . ? C115 O28 Cu4 108.4(3) . . ? C66 N9 C61 115.3(5) . . ? C66 N9 C68 109.1(4) . . ? C61 N9 C68 106.7(4) . . ? C66 N9 Cu3 112.6(4) . . ? C61 N9 Cu3 105.0(3) . . ? C68 N9 Cu3 107.7(3) . . ? C64 N10 C63 113.1(5) . . ? C64 N10 C76 109.5(5) . . ? C63 N10 C76 109.7(5) . . ? C64 N10 Cu3 107.6(4) . . ? C63 N10 Cu3 112.7(4) . . ? C76 N10 Cu3 103.7(4) . . ? C70 N11 C69 118.8(6) . . ? C70 N11 Cu3 125.8(4) . . ? C69 N11 Cu3 115.2(4) . . ? C79 N12 C80 116.8(6) . . ? C96 N13 C98 112.0(4) . . ? C96 N13 C91 114.9(4) . . ? C98 N13 C91 110.3(4) . . ? C96 N13 Cu4 105.6(3) . . ? C98 N13 Cu4 98.7(3) . . ? C91 N13 Cu4 114.2(3) . . ? C93 N14 C106 109.6(4) . . ? C93 N14 C94 111.0(4) . . ? C106 N14 C94 109.4(4) . . ? C93 N14 Cu4 110.4(3) . . ? C106 N14 Cu4 104.5(4) . . ? C94 N14 Cu4 111.8(3) . . ? C99 N15 C100 116.8(5) . . ? C110 N16 C109 120.4(5) . . ? C110 N16 Cu4 125.7(4) . . ? C109 N16 Cu4 113.9(4) . . ? N9 C61 C69 108.2(5) . . ? N9 C61 C62 112.7(5) . . ? C69 C61 C62 110.0(5) . . ? C74 C62 C67 109.2(6) . . ? C74 C62 C63 108.3(5) . . ? C67 C62 C63 102.6(5) . . ? C74 C62 C61 109.3(6) . . ? C67 C62 C61 113.9(5) . . ? C63 C62 C61 113.3(5) . . ? N10 C63 C62 110.1(5) . . ? N10 C64 C65 112.4(5) . . ? C77 C65 C67 115.5(6) . . ? C77 C65 C64 108.8(5) . . ? C67 C65 C64 104.8(5) . . ? C77 C65 C66 104.1(5) . . ? C67 C65 C66 109.8(5) . . ? C64 C65 C66 114.1(5) . . ? N9 C66 C79 112.9(5) . . ? N9 C66 C65 113.1(5) . . ? C79 C66 C65 106.7(5) . . ? O15 C67 C65 125.5(7) . . ? O15 C67 C62 121.6(7) . . ? C65 C67 C62 110.7(5) . . ? C90 C68 N9 113.8(5) . . ? N11 C69 C73 121.1(6) . . ? N11 C69 C61 114.6(5) . . ? C73 C69 C61 124.3(6) . . ? N11 C70 C71 122.3(7) . . ? C70 C71 C72 118.4(7) . . ? C73 C72 C71 120.2(7) . . ? C69 C73 C72 119.2(7) . . ? O16 C74 O17 123.5(7) . . ? O16 C74 C62 124.7(7) . . ? O17 C74 C62 111.8(6) . . ? O18 C77 O19 123.5(7) . . ? O18 C77 C65 127.6(7) . . ? O19 C77 C65 108.9(6) . . ? N12 C79 C83 123.5(6) . . ? N12 C79 C66 115.0(6) . . ? C83 C79 C66 121.4(6) . . ? N12 C80 C81 123.4(8) . . ? C82 C81 C80 119.9(7) . . ? C81 C82 C83 118.6(7) . . ? C79 C83 C82 117.8(7) . . ? O20 C84 C89 123.3(6) . . ? O20 C84 C85 116.9(5) . . ? C89 C84 C85 119.9(5) . . ? O21 C85 C86 123.6(6) . . ? O21 C85 C84 118.5(5) . . ? C86 C85 C84 117.9(6) . . ? C87 C86 C85 121.7(6) . . ? C87 C86 Cl9 120.5(5) . . ? C85 C86 Cl9 117.8(5) . . ? C86 C87 C88 120.0(6) . . ? C86 C87 Cl10 120.3(5) . . ? C88 C87 Cl10 119.6(5) . . ? C87 C88 C89 119.3(6) . . ? C87 C88 Cl11 120.9(5) . . ? C89 C88 Cl11 119.9(5) . . ? C84 C89 C88 121.2(6) . . ? C84 C89 Cl12 117.2(5) . . ? C88 C89 Cl12 121.6(5) . . ? C68 C90 C98 106.8(5) . . ? N13 C91 C99 110.7(4) . . ? N13 C91 C92 112.2(4) . . ? C99 C91 C92 110.3(5) . . ? C97 C92 C104 113.5(5) . . ? C97 C92 C91 109.5(4) . . ? C104 C92 C91 108.3(5) . . ? C97 C92 C93 106.8(5) . . ? C104 C92 C93 106.1(4) . . ? C91 C92 C93 112.6(5) . . ? N14 C93 C92 113.2(4) . . ? N14 C94 C95 110.6(4) . . ? C107 C95 C97 107.5(5) . . ? C107 C95 C94 106.3(4) . . ? C97 C95 C94 104.7(4) . . ? C107 C95 C96 111.3(5) . . ? C97 C95 C96 111.3(4) . . ? C94 C95 C96 115.2(5) . . ? N13 C96 C109 107.5(4) . . ? N13 C96 C95 112.2(4) . . ? C109 C96 C95 109.7(5) . . ? O22 C97 C95 123.4(5) . . ? O22 C97 C92 126.6(5) . . ? C95 C97 C92 109.1(5) . . ? N13 C98 C90 119.8(5) . . ? N15 C99 C103 123.8(5) . . ? N15 C99 C91 114.2(5) . . ? C103 C99 C91 121.9(5) . . ? N15 C100 C101 123.1(6) . . ? C100 C101 C102 119.1(6) . . ? C101 C102 C103 119.0(6) . . ? C99 C103 C102 118.2(5) . . ? O23 C104 O24 124.3(6) . . ? O23 C104 C92 123.5(6) . . ? O24 C104 C92 112.2(5) . . ? O25 C107 O26 124.8(5) . . ? O25 C107 C95 122.5(5) . . ? O26 C107 C95 112.7(5) . . ? N16 C109 C113 120.0(5) . . ? N16 C109 C96 116.0(5) . . ? C113 C109 C96 124.0(5) . . ? N16 C110 C111 122.4(6) . . ? C110 C111 C112 118.3(6) . . ? C113 C112 C111 119.1(6) . . ? C109 C113 C112 119.8(6) . . ? O27 C114 C119 123.8(5) . . ? O27 C114 C115 117.4(5) . . ? C119 C114 C115 118.8(5) . . ? O28 C115 C116 122.9(5) . . ? O28 C115 C114 117.8(5) . . ? C116 C115 C114 119.4(5) . . ? C115 C116 C117 120.6(6) . . ? C115 C116 Cl13 118.3(5) . . ? C117 C116 Cl13 121.1(5) . . ? C118 C117 C116 120.2(5) . . ? C118 C117 Cl14 120.5(5) . . ? C116 C117 Cl14 119.2(5) . . ? C117 C118 C119 120.0(6) . . ? C117 C118 Cl15 120.8(5) . . ? C119 C118 Cl15 119.2(5) . . ? C114 C119 C118 121.0(6) . . ? C114 C119 Cl16 117.7(4) . . ? C118 C119 Cl16 121.2(5) . . ? N17 C121 C122 178.9(13) . . ? N18 C123 C124 177.2(13) . . ? N19 C125 C126 177.3(13) . . ? N20 C127 C128 177.6(11) . . ? N21 C129 C130 175.9(19) . . ? N22 C131 C132 154.9(18) . . ? N23 C133 C134 174.9(13) . . ? C136 C135 N24 171(3) . . ? N25 C137 C138 168(3) . . ? N26 C139 C140 177.4(15) . . ? N27 C141 C142 178.8(12) . . ? N28 C143 C144 171.5(19) . . ? N29 C145 C146 178.7(14) . . ? C150 C149 C150 74(3) 2_556 . ? C149 C150 C149 106(3) 2_556 . ? C149 C150 C150 58(2) 2_556 2_556 ? C149 C150 C150 48.0(18) . 2_556 ? C153 N33 C151 57(2) . . ? N32 C151 C153 118(3) . . ? N32 C151 C152 170(3) . . ? C153 C151 C152 53.0(17) . . ? N32 C151 N33 78(3) . . ? C153 C151 N33 42.4(15) . . ? C152 C151 N33 95(2) . . ? C153 C152 C151 60.6(18) . . ? N33 C153 C152 145(3) . . ? N33 C153 C151 81(2) . . ? C152 C153 C151 66(2) . . ? N34 C154 C155 165(4) . . ? C154 C155 C156 134(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.183 _refine_diff_density_min -0.989 _refine_diff_density_rms 0.120 #====END