Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email wxtang@netra.nju.edu.cn _publ_contact_author_name 'Prof. Wen-Xia Tang' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name W.Tang J.Huang S.-A.Li D.-F.Li Y.-Z.Li D.-X.Yang K.-B.Yu data_[(CuimCu)L](ClO4)3.1/2H2O _database_code_CSD 200693 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H46 Cu2 N6 O2, C3 H3 N2, 3(Cl O4), 0.5(H2 O)' _chemical_formula_sum 'C31 H50 Cl3 Cu2 N8 O14.5' _chemical_formula_weight 1000.22 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.709(4) _cell_length_b 19.238(4) _cell_length_c 23.100(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8314(3) _cell_formula_units_Z 8 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 10.55 _exptl_crystal_description dark-blue _exptl_crystal_colour block _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4108 _exptl_absorpt_coefficient_mu 1.290 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6845 _exptl_absorpt_correction_T_max 0.7236 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 297(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.72 _diffrn_reflns_number 8474 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.1932 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7303 _reflns_number_gt 2476 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0996P)^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 constra _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00024(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7303 _refine_ls_number_parameters 534 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.2001 _refine_ls_R_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.2115 _refine_ls_wR_factor_gt 0.1679 _refine_ls_goodness_of_fit_ref 0.797 _refine_ls_restrained_S_all 0.800 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.93862(6) 0.53063(6) 0.21086(5) 0.0474(3) Uani 1 1 d . . . Cu2 Cu 0.79195(7) 0.68714(6) 0.02025(5) 0.0553(4) Uani 1 1 d . . . O1 O 1.0385(4) 0.4980(5) 0.1687(4) 0.107(3) Uani 1 1 d . . . H1 H 1.0463 0.4977 0.1290 0.129 Uiso 1 1 calc R . . O2 O 0.7639(5) 0.7692(5) 0.0814(3) 0.110(3) Uani 1 1 d . . . H2 H 0.7671 0.7652 0.1214 0.132 Uiso 1 1 calc R . . N1 N 0.9924(4) 0.4927(4) 0.2817(4) 0.057(2) Uani 1 1 d . . . N2 N 0.8612(4) 0.4554(4) 0.2331(3) 0.053(2) Uani 1 1 d . . . H2N H 0.8527 0.4294 0.2010 0.064 Uiso 1 1 calc R . . N3 N 0.9604(6) 0.6282(4) 0.2484(4) 0.094(4) Uani 1 1 d . . . H3N H 0.9224 0.6571 0.2432 0.112 Uiso 1 1 calc R . . N4 N 0.8977(4) 0.5591(4) 0.1362(3) 0.045(2) Uani 1 1 d . . . N5 N 0.8444(4) 0.6171(4) 0.0654(3) 0.051(2) Uani 1 1 d . . . N6 N 0.7410(5) 0.7544(5) -0.0348(4) 0.066(2) Uani 1 1 d . . . N7 N 0.6941(5) 0.6340(5) 0.0142(4) 0.076(3) Uani 1 1 d . . . H7N H 0.7051 0.5896 0.0039 0.091 Uiso 1 1 calc R . . N8 N 0.8826(5) 0.7203(5) -0.0239(4) 0.073(3) Uani 1 1 d . . . H8N H 0.9109 0.6826 -0.0301 0.087 Uiso 1 1 calc R . . C1 C 1.0540(7) 0.4503(8) 0.2640(6) 0.114(5) Uani 1 1 d . . . H1A H 1.0382 0.4029 0.2572 0.136 Uiso 1 1 calc R . . H1B H 1.0887 0.4494 0.2951 0.136 Uiso 1 1 calc R . . C2 C 1.0887(5) 0.4776(6) 0.2104(6) 0.080(3) Uani 1 1 d . . . H2A H 1.1184 0.5171 0.2204 0.096 Uiso 1 1 calc R . . H2B H 1.1193 0.4419 0.1942 0.096 Uiso 1 1 calc R . . C3 C 0.9432(6) 0.4486(7) 0.3146(5) 0.097(4) Uani 1 1 d . . . H3A H 0.9161 0.4775 0.3412 0.116 Uiso 1 1 calc R . . H3B H 0.9707 0.4158 0.3375 0.116 Uiso 1 1 calc R . . C4 C 0.8924(5) 0.4093(5) 0.2767(4) 0.060(3) Uani 1 1 d . . . H4A H 0.9176 0.3717 0.2576 0.072 Uiso 1 1 calc R . . H4B H 0.8546 0.3893 0.3002 0.072 Uiso 1 1 calc R . . C5 C 1.0185(8) 0.5513(6) 0.3175(5) 0.101(5) Uani 1 1 d . . . H5A H 1.0666 0.5636 0.3058 0.121 Uiso 1 1 calc R . . H5B H 1.0200 0.5372 0.3579 0.121 Uiso 1 1 calc R . . C6 C 0.9701(7) 0.6136(6) 0.3110(5) 0.085(4) Uani 1 1 d . . . H6A H 0.9242 0.6042 0.3289 0.102 Uiso 1 1 calc R . . H6B H 0.9912 0.6536 0.3300 0.102 Uiso 1 1 calc R . . C7 C 0.9033(6) 0.5221(5) 0.0852(4) 0.064(3) Uani 1 1 d . . . H7 H 0.9260 0.4794 0.0810 0.077 Uiso 1 1 calc R . . C8 C 0.8714(6) 0.5571(5) 0.0434(4) 0.060(3) Uani 1 1 d . . . H8 H 0.8679 0.5429 0.0050 0.072 Uiso 1 1 calc R . . C9 C 0.8628(5) 0.6151(5) 0.1211(4) 0.047(2) Uani 1 1 d . . . H9 H 0.8517 0.6505 0.1470 0.056 Uiso 1 1 calc R . . C10 C 0.7002(8) 0.8048(7) -0.0010(5) 0.100(4) Uani 1 1 d . . . H10A H 0.6554 0.7838 0.0110 0.120 Uiso 1 1 calc R . . H10B H 0.6892 0.8446 -0.0251 0.120 Uiso 1 1 calc R . . C11 C 0.7405(8) 0.8289(7) 0.0519(6) 0.105(5) Uani 1 1 d . . . H11A H 0.7811 0.8572 0.0406 0.126 Uiso 1 1 calc R . . H11B H 0.7096 0.8564 0.0767 0.126 Uiso 1 1 calc R . . C12 C 0.6928(7) 0.7092(7) -0.0714(6) 0.101(4) Uani 1 1 d . . . H12A H 0.6609 0.7383 -0.0940 0.121 Uiso 1 1 calc R . . H12B H 0.7214 0.6818 -0.0979 0.121 Uiso 1 1 calc R . . C13 C 0.6506(7) 0.6627(7) -0.0340(5) 0.093(4) Uani 1 1 d . . . H13A H 0.6318 0.6247 -0.0571 0.111 Uiso 1 1 calc R . . H13B H 0.6104 0.6882 -0.0182 0.111 Uiso 1 1 calc R . . C14 C 0.7937(7) 0.7878(6) -0.0730(5) 0.089(4) Uani 1 1 d . . . H14A H 0.7718 0.7973 -0.1102 0.107 Uiso 1 1 calc R . . H14B H 0.8082 0.8319 -0.0563 0.107 Uiso 1 1 calc R . . C15 C 0.8557(6) 0.7448(7) -0.0813(4) 0.080(4) Uani 1 1 d . . . H15A H 0.8927 0.7710 -0.1010 0.096 Uiso 1 1 calc R . . H15B H 0.8434 0.7051 -0.1053 0.096 Uiso 1 1 calc R . . C16 C 0.7920(5) 0.4824(5) 0.2532(4) 0.060(3) Uani 1 1 d . . . H16A H 0.8000 0.5137 0.2855 0.072 Uiso 1 1 calc R . . H16B H 0.7631 0.4440 0.2671 0.072 Uiso 1 1 calc R . . C17 C 0.7517(5) 0.5203(5) 0.2066(5) 0.053(2) Uani 1 1 d . . . C18 C 0.7311(5) 0.5892(6) 0.2141(5) 0.068(3) Uani 1 1 d . . . H18 H 0.7397 0.6117 0.2490 0.082 Uiso 1 1 calc R . . C19 C 0.6970(5) 0.6246(6) 0.1684(6) 0.070(3) Uani 1 1 d . . . H19 H 0.6839 0.6710 0.1723 0.084 Uiso 1 1 calc R . . C20 C 0.6835(6) 0.5883(8) 0.1171(5) 0.072(3) Uani 1 1 d . . . C21 C 0.7016(6) 0.5200(7) 0.1128(5) 0.076(3) Uani 1 1 d . . . H21 H 0.6902 0.4955 0.0793 0.091 Uiso 1 1 calc R . . C22 C 0.7346(5) 0.4883(6) 0.1551(5) 0.064(3) Uani 1 1 d . . . H22 H 0.7473 0.4419 0.1502 0.077 Uiso 1 1 calc R . . C23 C 0.6484(6) 0.6284(7) 0.0685(5) 0.096(4) Uani 1 1 d . . . H23A H 0.6373 0.6749 0.0821 0.115 Uiso 1 1 calc R . . H23B H 0.6036 0.6059 0.0585 0.115 Uiso 1 1 calc R . . C24 C 1.0343(7) 0.6641(7) 0.2200(6) 0.099(4) Uani 1 1 d . . . H24A H 1.0541 0.6979 0.2466 0.119 Uiso 1 1 calc R . . H24B H 1.0700 0.6285 0.2130 0.119 Uiso 1 1 calc R . . C25 C 1.0138(6) 0.6990(7) 0.1637(6) 0.066(3) Uani 1 1 d . . . C26 C 0.9742(7) 0.7558(8) 0.1611(6) 0.090(4) Uani 1 1 d . . . H26 H 0.9629 0.7797 0.1949 0.108 Uiso 1 1 calc R . . C27 C 0.9498(8) 0.7796(8) 0.1090(7) 0.107(5) Uani 1 1 d . . . H27 H 0.9233 0.8205 0.1082 0.129 Uiso 1 1 calc R . . C28 C 0.9621(7) 0.7471(9) 0.0595(6) 0.082(4) Uani 1 1 d . . . C29 C 1.0047(7) 0.6930(8) 0.0579(6) 0.086(4) Uani 1 1 d . . . H29 H 1.0178 0.6732 0.0228 0.103 Uiso 1 1 calc R . . C30 C 1.0314(6) 0.6642(6) 0.1125(7) 0.087(4) Uani 1 1 d . . . H30 H 1.0591 0.6241 0.1130 0.105 Uiso 1 1 calc R . . C31 C 0.9275(7) 0.7758(7) 0.0054(5) 0.094(4) Uani 1 1 d . . . H31A H 0.9642 0.7919 -0.0211 0.112 Uiso 1 1 calc R . . H31B H 0.8975 0.8151 0.0154 0.112 Uiso 1 1 calc R . . Cl1 Cl 0.5330(2) 0.82231(19) 0.12829(15) 0.0848(10) Uani 1 1 d . . . Cl2 Cl 0.7889(2) 0.78177(17) 0.25247(15) 0.0906(10) Uani 1 1 d . . . O3 O 0.5016(7) 0.7981(5) 0.1794(4) 0.146(4) Uani 1 1 d . . . O4 O 0.4837(6) 0.8708(5) 0.0998(5) 0.133(4) Uani 1 1 d . . . O5 O 0.5415(5) 0.7659(5) 0.0911(5) 0.142(4) Uani 1 1 d . . . O6 O 0.5977(6) 0.8537(6) 0.1412(4) 0.142(4) Uani 1 1 d . . . O7 O 0.8120(8) 0.8334(5) 0.2866(5) 0.199(7) Uani 1 1 d . . . O8 O 0.8315(5) 0.7235(5) 0.2588(6) 0.165(5) Uani 1 1 d . . . O9 O 0.7787(8) 0.8040(7) 0.1977(4) 0.199(4) Uani 1 1 d . . . O10 O 0.7208(7) 0.7613(7) 0.2760(7) 0.207(6) Uani 1 1 d . . . Cl3 Cl 0.7357(8) 0.4802(11) -0.0859(9) 0.171(4) Uani 0.50 1 d PD A 1 O11 O 0.7385(14) 0.5526(11) -0.096(2) 0.210(6) Uani 0.50 1 d PD A 1 O12 O 0.7418(16) 0.467(2) -0.0254(9) 0.189(10) Uani 0.50 1 d PD A 1 O13 O 0.6693(9) 0.4529(14) -0.1064(12) 0.225(10) Uiso 0.50 1 d PD A 1 O14 O 0.7925(11) 0.4461(15) -0.1158(12) 0.254 Uiso 0.50 1 d PD A 1 Cl3' Cl 0.7647(8) 0.4900(11) -0.0837(10) 0.171(4) Uani 0.50 1 d PD B 2 O11' O 0.7761(14) 0.5587(11) -0.1037(19) 0.210(6) Uani 0.50 1 d PD B 2 O12' O 0.7229(13) 0.491(2) -0.0322(11) 0.189(10) Uani 0.50 1 d PD B 2 O13' O 0.7285(13) 0.4506(15) -0.1271(11) 0.225(10) Uiso 0.50 1 d PD B 2 O14' O 0.8320(10) 0.4580(14) -0.0719(12) 0.254 Uiso 0.50 1 d PD B 2 O15 O 0.5597(13) 0.4738(8) -0.0127(8) 0.149(9) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0433(6) 0.0533(7) 0.0455(6) 0.0056(6) -0.0066(6) -0.0039(6) Cu2 0.0533(7) 0.0675(8) 0.0449(7) 0.0094(7) 0.0023(7) 0.0110(7) O1 0.054(5) 0.187(9) 0.080(6) 0.049(6) 0.004(4) 0.025(5) O2 0.151(9) 0.117(8) 0.061(5) -0.003(5) -0.006(5) 0.038(7) N1 0.061(6) 0.058(5) 0.053(5) 0.001(4) -0.002(5) -0.004(5) N2 0.051(5) 0.052(5) 0.057(5) 0.001(4) -0.004(4) -0.010(4) N3 0.147(10) 0.053(5) 0.081(7) -0.015(6) -0.055(7) 0.031(6) N4 0.044(5) 0.053(5) 0.037(4) 0.007(4) 0.007(4) 0.002(4) N5 0.061(5) 0.056(5) 0.036(5) 0.003(4) -0.004(4) 0.010(5) N6 0.074(6) 0.076(6) 0.047(5) -0.004(5) -0.002(5) 0.019(6) N7 0.070(6) 0.081(6) 0.075(7) 0.011(5) -0.019(6) 0.011(5) N8 0.057(6) 0.103(7) 0.058(6) 0.020(6) 0.014(5) 0.012(6) C1 0.078(9) 0.160(14) 0.102(11) 0.046(10) -0.008(8) 0.050(10) C2 0.047(6) 0.090(9) 0.103(9) 0.017(9) 0.003(8) 0.009(6) C3 0.083(9) 0.112(10) 0.095(9) 0.044(8) -0.036(8) -0.027(8) C4 0.049(6) 0.061(7) 0.070(7) 0.000(6) -0.012(6) -0.002(6) C5 0.143(12) 0.076(9) 0.085(9) 0.002(7) -0.060(9) -0.009(9) C6 0.144(12) 0.047(7) 0.063(8) -0.012(6) -0.009(8) -0.014(8) C7 0.080(8) 0.060(7) 0.052(7) -0.001(6) 0.002(6) 0.021(6) C8 0.078(8) 0.062(7) 0.041(6) -0.004(6) -0.004(6) 0.018(6) C9 0.046(6) 0.045(6) 0.049(6) 0.004(5) 0.008(5) -0.002(5) C10 0.114(11) 0.113(11) 0.072(8) 0.015(8) 0.007(8) 0.044(10) C11 0.143(13) 0.084(10) 0.087(10) -0.015(9) 0.014(10) 0.019(10) C12 0.103(11) 0.120(12) 0.078(9) 0.014(9) -0.029(9) 0.022(9) C13 0.082(9) 0.106(10) 0.091(10) 0.017(8) -0.032(8) 0.001(8) C14 0.080(9) 0.095(10) 0.093(9) 0.051(8) 0.014(8) 0.011(8) C15 0.089(9) 0.111(10) 0.040(6) 0.016(7) 0.020(6) 0.008(8) C16 0.051(6) 0.069(7) 0.061(6) 0.007(6) 0.012(6) 0.001(6) C17 0.037(5) 0.062(8) 0.061(7) 0.002(7) 0.005(6) -0.007(5) C18 0.058(7) 0.085(9) 0.063(7) -0.004(7) 0.021(6) -0.020(6) C19 0.038(7) 0.069(8) 0.104(10) 0.023(8) 0.025(7) 0.011(6) C20 0.048(7) 0.114(11) 0.054(7) 0.024(8) 0.007(6) -0.002(8) C21 0.068(8) 0.088(10) 0.071(8) 0.009(8) 0.014(7) 0.003(8) C22 0.052(7) 0.068(8) 0.071(8) 0.007(7) 0.001(6) 0.001(6) C23 0.066(8) 0.130(12) 0.090(9) 0.013(9) 0.006(8) 0.024(8) C24 0.088(9) 0.096(10) 0.112(11) 0.016(9) -0.026(9) -0.038(8) C25 0.056(8) 0.065(8) 0.079(9) 0.021(8) -0.007(7) -0.024(7) C26 0.095(11) 0.085(10) 0.090(11) -0.012(9) 0.005(9) -0.039(9) C27 0.118(12) 0.098(11) 0.105(11) 0.036(10) -0.035(11) -0.063(10) C28 0.067(9) 0.113(12) 0.067(9) 0.015(9) -0.001(7) -0.052(9) C29 0.058(8) 0.116(12) 0.084(10) 0.036(9) -0.002(7) -0.007(8) C30 0.038(7) 0.062(8) 0.161(14) -0.001(9) 0.019(9) -0.018(6) C31 0.083(9) 0.127(11) 0.071(8) 0.046(8) 0.006(7) -0.013(9) Cl1 0.102(3) 0.072(2) 0.081(2) -0.011(2) -0.001(2) -0.013(2) Cl2 0.124(3) 0.072(2) 0.076(2) -0.0157(19) -0.014(2) 0.023(2) O3 0.211(12) 0.149(9) 0.079(6) 0.021(6) 0.011(8) -0.057(8) O4 0.140(8) 0.086(7) 0.172(10) 0.010(7) -0.022(8) 0.001(7) O5 0.131(9) 0.123(8) 0.172(10) -0.083(8) 0.008(7) 0.004(7) O6 0.138(9) 0.179(10) 0.110(8) -0.025(7) -0.020(7) -0.054(8) O7 0.350(19) 0.087(7) 0.160(10) -0.051(7) -0.117(12) 0.031(10) O8 0.114(8) 0.083(7) 0.298(15) -0.012(9) 0.007(10) 0.030(6) O9 0.319 0.215(13) 0.064(6) 0.026(8) -0.018(9) 0.023(12) O10 0.138(10) 0.225(14) 0.258(16) -0.014(12) 0.075(11) 0.027(10) Cl3 0.277(12) 0.140(7) 0.095(4) -0.024(4) -0.048(9) -0.016(9) O11 0.318 0.069(8) 0.244(18) 0.044(10) 0.13(3) 0.004(15) O12 0.325 0.18(3) 0.059(7) 0.010(12) 0.006(11) 0.023(19) Cl3' 0.277(12) 0.140(7) 0.095(4) -0.024(4) -0.048(9) -0.016(9) O11' 0.318 0.069(8) 0.244(18) 0.044(10) 0.13(3) 0.004(15) O12' 0.325 0.18(3) 0.059(7) 0.010(12) 0.006(11) 0.023(19) O15 0.26(3) 0.051(10) 0.138(16) 0.021(11) -0.064(18) -0.036(13) _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 N4 1.966(7) . yes Cu1 N1 2.055(8) . yes Cu1 N3 2.107(8) . yes Cu1 N2 2.111(7) . yes Cu1 O1 2.199(8) . yes Cu2 N5 1.967(7) . yes Cu2 N6 2.049(8) . yes Cu2 N8 2.079(8) . yes Cu2 N7 2.101(9) . yes Cu2 O2 2.182(8) . yes O1 C2 1.401(12) . ? O2 C11 1.404(13) . ? N1 C3 1.464(12) . ? N1 C1 1.470(13) . ? N1 C5 1.481(12) . ? N2 C4 1.462(11) . ? N2 C16 1.470(11) . ? N3 C6 1.485(13) . ? N3 C24 1.679(14) . ? N4 C9 1.307(10) . ? N4 C7 1.379(11) . ? N5 C9 1.331(11) . ? N5 C8 1.358(11) . ? N6 C10 1.460(13) . ? N6 C14 1.472(12) . ? N6 C12 1.511(14) . ? N7 C13 1.486(12) . ? N7 C23 1.521(13) . ? N8 C15 1.494(12) . ? N8 C31 1.518(14) . ? C1 C2 1.492(15) . ? C3 C4 1.498(13) . ? C5 C6 1.509(15) . ? C7 C8 1.319(12) . ? C10 C11 1.509(16) . ? C12 C13 1.472(15) . ? C14 C15 1.438(14) . ? C16 C17 1.504(13) . ? C17 C22 1.376(13) . ? C17 C18 1.391(13) . ? C18 C19 1.408(14) . ? C19 C20 1.400(15) . ? C20 C21 1.360(15) . ? C20 C23 1.513(15) . ? C21 C22 1.308(13) . ? C24 C25 1.513(15) . ? C25 C26 1.322(16) . ? C25 C30 1.399(16) . ? C26 C27 1.367(16) . ? C27 C28 1.323(17) . ? C28 C29 1.311(17) . ? C28 C31 1.512(16) . ? C29 C30 1.464(17) . ? Cl1 O6 1.386(10) . ? Cl1 O5 1.394(8) . ? Cl1 O3 1.398(9) . ? Cl1 O4 1.467(10) . ? Cl2 O7 1.340(10) . ? Cl2 O9 1.350(9) . ? Cl2 O8 1.383(9) . ? Cl2 O10 1.441(12) . ? Cl3 O11 1.414(5) . ? Cl3 O12 1.426(5) . ? Cl3 O14 1.426(5) . ? Cl3 O13 1.429(5) . ? Cl3' O11' 1.415(5) . ? Cl3' O12' 1.424(5) . ? Cl3' O13' 1.427(5) . ? Cl3' O14' 1.429(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N1 171.4(3) . . yes N4 Cu1 N3 100.9(3) . . yes N1 Cu1 N3 83.9(3) . . yes N4 Cu1 N2 97.9(3) . . yes N1 Cu1 N2 84.2(3) . . yes N3 Cu1 N2 130.0(4) . . yes N4 Cu1 O1 91.3(3) . . yes N1 Cu1 O1 80.5(3) . . yes N3 Cu1 O1 105.8(4) . . yes N2 Cu1 O1 119.7(3) . . yes N5 Cu2 N6 173.7(3) . . yes N5 Cu2 N8 93.7(3) . . yes N6 Cu2 N8 83.2(4) . . yes N5 Cu2 N7 97.9(3) . . yes N6 Cu2 N7 82.0(3) . . yes N8 Cu2 N7 145.8(4) . . yes N5 Cu2 O2 105.8(3) . . yes N6 Cu2 O2 80.4(3) . . yes N8 Cu2 O2 106.9(4) . . yes N7 Cu2 O2 100.7(4) . . yes C2 O1 Cu1 110.2(6) . . ? C11 O2 Cu2 110.7(7) . . ? C3 N1 C1 108.4(9) . . ? C3 N1 C5 110.9(10) . . ? C1 N1 C5 108.7(10) . . ? C3 N1 Cu1 108.2(6) . . ? C1 N1 Cu1 111.0(7) . . ? C5 N1 Cu1 109.6(6) . . ? C4 N2 C16 110.4(7) . . ? C4 N2 Cu1 108.0(5) . . ? C16 N2 Cu1 116.0(6) . . ? C6 N3 C24 111.0(9) . . ? C6 N3 Cu1 104.9(6) . . ? C24 N3 Cu1 111.4(7) . . ? C9 N4 C7 103.6(8) . . ? C9 N4 Cu1 131.2(7) . . ? C7 N4 Cu1 125.1(7) . . ? C9 N5 C8 104.0(8) . . ? C9 N5 Cu2 131.3(7) . . ? C8 N5 Cu2 124.7(6) . . ? C10 N6 C14 112.4(10) . . ? C10 N6 C12 111.7(10) . . ? C14 N6 C12 108.5(9) . . ? C10 N6 Cu2 109.2(7) . . ? C14 N6 Cu2 109.7(7) . . ? C12 N6 Cu2 105.2(7) . . ? C13 N7 C23 109.6(9) . . ? C13 N7 Cu2 110.3(7) . . ? C23 N7 Cu2 118.0(7) . . ? C15 N8 C31 111.2(9) . . ? C15 N8 Cu2 104.9(6) . . ? C31 N8 Cu2 116.6(7) . . ? N1 C1 C2 112.1(10) . . ? O1 C2 C1 112.2(9) . . ? N1 C3 C4 112.8(9) . . ? N2 C4 C3 110.5(8) . . ? N1 C5 C6 110.6(9) . . ? N3 C6 C5 108.7(10) . . ? C8 C7 N4 109.1(9) . . ? C7 C8 N5 109.1(9) . . ? N4 C9 N5 114.2(9) . . ? N6 C10 C11 112.1(11) . . ? O2 C11 C10 107.3(10) . . ? C13 C12 N6 110.0(10) . . ? C12 C13 N7 111.8(10) . . ? C15 C14 N6 111.6(9) . . ? C14 C15 N8 109.5(9) . . ? N2 C16 C17 112.8(8) . . ? C22 C17 C18 118.0(10) . . ? C22 C17 C16 121.1(10) . . ? C18 C17 C16 120.8(10) . . ? C17 C18 C19 119.6(11) . . ? C20 C19 C18 118.3(11) . . ? C21 C20 C19 119.9(11) . . ? C21 C20 C23 123.2(13) . . ? C19 C20 C23 117.0(13) . . ? C22 C21 C20 121.0(12) . . ? C21 C22 C17 123.0(11) . . ? C20 C23 N7 113.8(9) . . ? C25 C24 N3 108.1(9) . . ? C26 C25 C30 119.3(13) . . ? C26 C25 C24 123.2(15) . . ? C30 C25 C24 117.1(13) . . ? C25 C26 C27 120.2(15) . . ? C28 C27 C26 123.1(16) . . ? C29 C28 C27 120.3(15) . . ? C29 C28 C31 121.9(14) . . ? C27 C28 C31 117.9(16) . . ? C28 C29 C30 119.0(14) . . ? C25 C30 C29 117.9(12) . . ? C28 C31 N8 110.5(10) . . ? O6 Cl1 O5 111.8(7) . . ? O6 Cl1 O3 109.3(7) . . ? O5 Cl1 O3 108.0(7) . . ? O6 Cl1 O4 111.6(6) . . ? O5 Cl1 O4 106.9(6) . . ? O3 Cl1 O4 109.0(7) . . ? O7 Cl2 O9 111.3(8) . . ? O7 Cl2 O8 110.7(8) . . ? O9 Cl2 O8 116.0(9) . . ? O7 Cl2 O10 105.4(9) . . ? O9 Cl2 O10 108.4(10) . . ? O8 Cl2 O10 104.3(8) . . ? O11 Cl3 O12 110.0(4) . . ? O11 Cl3 O14 110.1(4) . . ? O12 Cl3 O14 109.3(4) . . ? O11 Cl3 O13 109.7(4) . . ? O12 Cl3 O13 109.0(4) . . ? O14 Cl3 O13 108.6(4) . . ? O11' Cl3' O12' 110.2(4) . . ? O11' Cl3' O13' 109.9(4) . . ? O12' Cl3' O13' 109.4(4) . . ? O11' Cl3' O14' 109.4(4) . . ? O12' Cl3' O14' 109.1(4) . . ? O13' Cl3' O14' 108.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cu1 O1 C2 175.1(8) . . . . ? N1 Cu1 O1 C2 -7.4(7) . . . . ? N3 Cu1 O1 C2 73.5(8) . . . . ? N2 Cu1 O1 C2 -85.0(8) . . . . ? N5 Cu2 O2 C11 166.8(9) . . . . ? N6 Cu2 O2 C11 -11.9(9) . . . . ? N8 Cu2 O2 C11 67.9(9) . . . . ? N7 Cu2 O2 C11 -91.8(9) . . . . ? N4 Cu1 N1 C3 -117(2) . . . . ? N3 Cu1 N1 C3 118.9(8) . . . . ? N2 Cu1 N1 C3 -12.5(7) . . . . ? O1 Cu1 N1 C3 -133.9(8) . . . . ? N4 Cu1 N1 C1 2(3) . . . . ? N3 Cu1 N1 C1 -122.3(9) . . . . ? N2 Cu1 N1 C1 106.4(8) . . . . ? O1 Cu1 N1 C1 -15.1(8) . . . . ? N4 Cu1 N1 C5 122(2) . . . . ? N3 Cu1 N1 C5 -2.2(8) . . . . ? N2 Cu1 N1 C5 -133.5(8) . . . . ? O1 Cu1 N1 C5 105.0(8) . . . . ? N4 Cu1 N2 C4 160.1(6) . . . . ? N1 Cu1 N2 C4 -11.5(6) . . . . ? N3 Cu1 N2 C4 -88.5(7) . . . . ? O1 Cu1 N2 C4 64.1(6) . . . . ? N4 Cu1 N2 C16 -75.4(7) . . . . ? N1 Cu1 N2 C16 113.1(7) . . . . ? N3 Cu1 N2 C16 36.0(8) . . . . ? O1 Cu1 N2 C16 -171.4(6) . . . . ? N4 Cu1 N3 C6 162.9(8) . . . . ? N1 Cu1 N3 C6 -24.3(8) . . . . ? N2 Cu1 N3 C6 52.8(9) . . . . ? O1 Cu1 N3 C6 -102.6(8) . . . . ? N4 Cu1 N3 C24 -77.0(7) . . . . ? N1 Cu1 N3 C24 95.8(7) . . . . ? N2 Cu1 N3 C24 172.9(6) . . . . ? O1 Cu1 N3 C24 17.5(7) . . . . ? N1 Cu1 N4 C9 -151.2(19) . . . . ? N3 Cu1 N4 C9 -28.2(9) . . . . ? N2 Cu1 N4 C9 105.3(8) . . . . ? O1 Cu1 N4 C9 -134.5(8) . . . . ? N1 Cu1 N4 C7 26(3) . . . . ? N3 Cu1 N4 C7 148.9(8) . . . . ? N2 Cu1 N4 C7 -77.7(8) . . . . ? O1 Cu1 N4 C7 42.5(8) . . . . ? N6 Cu2 N5 C9 168(3) . . . . ? N8 Cu2 N5 C9 107.9(9) . . . . ? N7 Cu2 N5 C9 -104.4(9) . . . . ? O2 Cu2 N5 C9 -0.9(9) . . . . ? N6 Cu2 N5 C8 -12(4) . . . . ? N8 Cu2 N5 C8 -71.4(8) . . . . ? N7 Cu2 N5 C8 76.3(8) . . . . ? O2 Cu2 N5 C8 179.9(8) . . . . ? N5 Cu2 N6 C10 176(3) . . . . ? N8 Cu2 N6 C10 -124.0(9) . . . . ? N7 Cu2 N6 C10 86.9(8) . . . . ? O2 Cu2 N6 C10 -15.5(8) . . . . ? N5 Cu2 N6 C14 -61(4) . . . . ? N8 Cu2 N6 C14 -0.4(8) . . . . ? N7 Cu2 N6 C14 -149.6(8) . . . . ? O2 Cu2 N6 C14 108.1(8) . . . . ? N5 Cu2 N6 C12 56(3) . . . . ? N8 Cu2 N6 C12 116.0(8) . . . . ? N7 Cu2 N6 C12 -33.1(7) . . . . ? O2 Cu2 N6 C12 -135.5(8) . . . . ? N5 Cu2 N7 C13 -160.9(8) . . . . ? N6 Cu2 N7 C13 12.7(8) . . . . ? N8 Cu2 N7 C13 -52.4(10) . . . . ? O2 Cu2 N7 C13 91.3(8) . . . . ? N5 Cu2 N7 C23 72.1(8) . . . . ? N6 Cu2 N7 C23 -114.3(8) . . . . ? N8 Cu2 N7 C23 -179.4(7) . . . . ? O2 Cu2 N7 C23 -35.7(8) . . . . ? N5 Cu2 N8 C15 150.3(7) . . . . ? N6 Cu2 N8 C15 -24.2(7) . . . . ? N7 Cu2 N8 C15 40.6(10) . . . . ? O2 Cu2 N8 C15 -101.9(7) . . . . ? N5 Cu2 N8 C31 -86.1(7) . . . . ? N6 Cu2 N8 C31 99.4(8) . . . . ? N7 Cu2 N8 C31 164.1(7) . . . . ? O2 Cu2 N8 C31 21.6(8) . . . . ? C3 N1 C1 C2 153.8(10) . . . . ? C5 N1 C1 C2 -85.5(12) . . . . ? Cu1 N1 C1 C2 35.1(13) . . . . ? Cu1 O1 C2 C1 28.2(13) . . . . ? N1 C1 C2 O1 -42.7(16) . . . . ? C1 N1 C3 C4 -85.5(11) . . . . ? C5 N1 C3 C4 155.2(10) . . . . ? Cu1 N1 C3 C4 35.0(11) . . . . ? C16 N2 C4 C3 -94.8(10) . . . . ? Cu1 N2 C4 C3 33.0(10) . . . . ? N1 C3 C4 N2 -46.7(13) . . . . ? C3 N1 C5 C6 -90.6(12) . . . . ? C1 N1 C5 C6 150.3(11) . . . . ? Cu1 N1 C5 C6 28.8(12) . . . . ? C24 N3 C6 C5 -74.1(11) . . . . ? Cu1 N3 C6 C5 46.3(11) . . . . ? N1 C5 C6 N3 -51.3(14) . . . . ? C9 N4 C7 C8 -0.7(11) . . . . ? Cu1 N4 C7 C8 -178.4(7) . . . . ? N4 C7 C8 N5 0.1(12) . . . . ? C9 N5 C8 C7 0.5(12) . . . . ? Cu2 N5 C8 C7 179.9(7) . . . . ? C7 N4 C9 N5 1.0(11) . . . . ? Cu1 N4 C9 N5 178.5(6) . . . . ? C8 N5 C9 N4 -1.0(11) . . . . ? Cu2 N5 C9 N4 179.6(6) . . . . ? C14 N6 C10 C11 -81.5(12) . . . . ? C12 N6 C10 C11 156.4(11) . . . . ? Cu2 N6 C10 C11 40.5(13) . . . . ? Cu2 O2 C11 C10 35.1(13) . . . . ? N6 C10 C11 O2 -50.9(14) . . . . ? C10 N6 C12 C13 -68.7(12) . . . . ? C14 N6 C12 C13 166.9(10) . . . . ? Cu2 N6 C12 C13 49.7(11) . . . . ? N6 C12 C13 N7 -40.9(14) . . . . ? C23 N7 C13 C12 143.5(11) . . . . ? Cu2 N7 C13 C12 11.9(13) . . . . ? C10 N6 C14 C15 148.7(11) . . . . ? C12 N6 C14 C15 -87.3(12) . . . . ? Cu2 N6 C14 C15 27.0(12) . . . . ? N6 C14 C15 N8 -49.7(14) . . . . ? C31 N8 C15 C14 -80.9(12) . . . . ? Cu2 N8 C15 C14 46.0(11) . . . . ? C4 N2 C16 C17 -170.4(8) . . . . ? Cu1 N2 C16 C17 66.3(9) . . . . ? N2 C16 C17 C22 57.2(12) . . . . ? N2 C16 C17 C18 -122.2(9) . . . . ? C22 C17 C18 C19 -3.1(14) . . . . ? C16 C17 C18 C19 176.3(8) . . . . ? C17 C18 C19 C20 1.6(14) . . . . ? C18 C19 C20 C21 1.6(15) . . . . ? C18 C19 C20 C23 -178.6(9) . . . . ? C19 C20 C21 C22 -3.2(17) . . . . ? C23 C20 C21 C22 177.0(10) . . . . ? C20 C21 C22 C17 1.7(17) . . . . ? C18 C17 C22 C21 1.6(15) . . . . ? C16 C17 C22 C21 -177.9(9) . . . . ? C21 C20 C23 N7 -62.6(15) . . . . ? C19 C20 C23 N7 117.6(11) . . . . ? C13 N7 C23 C20 169.8(11) . . . . ? Cu2 N7 C23 C20 -62.8(13) . . . . ? C6 N3 C24 C25 -161.4(10) . . . . ? Cu1 N3 C24 C25 82.2(10) . . . . ? N3 C24 C25 C26 69.8(14) . . . . ? N3 C24 C25 C30 -102.7(11) . . . . ? C30 C25 C26 C27 1.0(17) . . . . ? C24 C25 C26 C27 -171.3(11) . . . . ? C25 C26 C27 C28 2(2) . . . . ? C26 C27 C28 C29 -6(2) . . . . ? C26 C27 C28 C31 175.5(11) . . . . ? C27 C28 C29 C30 7.3(18) . . . . ? C31 C28 C29 C30 -174.7(10) . . . . ? C26 C25 C30 C29 0.1(15) . . . . ? C24 C25 C30 C29 172.9(10) . . . . ? C28 C29 C30 C25 -4.3(16) . . . . ? C29 C28 C31 N8 58.3(14) . . . . ? C27 C28 C31 N8 -123.5(12) . . . . ? C15 N8 C31 C28 -172.6(10) . . . . ? Cu2 N8 C31 C28 67.1(11) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.775 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.098 # END OF CIF OF COMPLEX 1 ########################################################################## data_[(CuimZn)L-2H][(CuimZn)L-H](ClO4)3 _database_code_CSD 200694 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H47 Cu N8 O2 Zn, C31 H48 Cu N8 O2 Zn, 3(Cl O4)' _chemical_formula_sum 'C62 H95 Cl3 Cu2 N16 O16 Zn2' _chemical_formula_weight 1684.71 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' Zn Zn 0.2839 1.4301 '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 14.172(2) _cell_length_b 16.673(2) _cell_length_c 21.284(3) _cell_angle_alpha 74.110(10) _cell_angle_beta 75.200(10) _cell_angle_gamma 82.220(10) _cell_volume 4665.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2188 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 17.14 _exptl_crystal_description platelet _exptl_crystal_colour green _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 1.103 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 0.802 _exptl_absorpt_process_details SADABS _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 'phi and omega scans' _diffrn_detector_area_resol_mean 9.98 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 23946 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16118 _reflns_number_gt 9292 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0597P)^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 16118 _refine_ls_number_parameters 914 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1282 _refine_ls_wR_factor_gt 0.1220 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.73496(3) 0.18639(3) 0.35488(2) 0.05144(14) Uani 1 1 d . . . Zn1 Zn 1.15301(4) 0.15127(3) 0.21364(3) 0.07252(17) Uani 1 1 d . . . N1 N 0.6700(3) 0.1948(2) 0.27316(19) 0.0781(11) Uani 1 1 d . . . H1C H 0.6974 0.2377 0.2395 0.094 Uiso 1 1 calc R . . N2 N 0.5866(2) 0.1693(2) 0.40983(19) 0.0679(10) Uani 1 1 d . . . N3 N 0.7583(2) 0.06148(18) 0.41207(18) 0.0620(9) Uani 1 1 d . . . H3C H 0.7974 0.0315 0.3842 0.074 Uiso 1 1 calc R . . N4 N 1.2206(3) 0.1724(2) 0.28341(19) 0.0770(11) Uani 1 1 d . . . H4C H 1.1887 0.2200 0.2936 0.092 Uiso 1 1 calc R . . N5 N 1.2978(3) 0.1245(3) 0.1658(2) 0.0909(13) Uani 1 1 d . . . N6 N 1.1326(3) 0.0196(3) 0.2230(2) 0.0878(12) Uani 1 1 d . . . H6C H 1.0980 -0.0037 0.2651 0.105 Uiso 1 1 calc R . . N7 N 0.8666(2) 0.21611(19) 0.30112(16) 0.0548(8) Uani 1 1 d . . . N8 N 1.0255(2) 0.1985(2) 0.24734(17) 0.0630(9) Uani 1 1 d . . . O1 O 0.72063(19) 0.27114(16) 0.40935(14) 0.0654(8) Uani 1 1 d . . . O2 O 1.1529(3) 0.2147(2) 0.11370(16) 0.1018(11) Uani 1 1 d . . . C1 C 0.5618(3) 0.2225(3) 0.2940(3) 0.0785(14) Uani 1 1 d . . . H1A H 0.5540 0.2809 0.2951 0.094 Uiso 1 1 calc R . . H1B H 0.5263 0.2154 0.2628 0.094 Uiso 1 1 calc R . . C2 C 0.5256(3) 0.1696(3) 0.3608(3) 0.0826(15) Uani 1 1 d . . . H2A H 0.5249 0.1129 0.3574 0.099 Uiso 1 1 calc R . . H2B H 0.4587 0.1890 0.3781 0.099 Uiso 1 1 calc R . . C3 C 0.6574(3) 0.0291(2) 0.4340(2) 0.0698(12) Uani 1 1 d . . . H3A H 0.6390 0.0189 0.3961 0.084 Uiso 1 1 calc R . . H3B H 0.6570 -0.0231 0.4682 0.084 Uiso 1 1 calc R . . C4 C 0.5863(3) 0.0934(3) 0.4613(3) 0.0772(14) Uani 1 1 d . . . H4A H 0.5212 0.0733 0.4766 0.093 Uiso 1 1 calc R . . H4B H 0.6048 0.1034 0.4992 0.093 Uiso 1 1 calc R . . C5 C 0.6389(3) 0.2667(3) 0.4607(2) 0.0648(12) Uani 1 1 d . . . H5A H 0.6242 0.3200 0.4724 0.078 Uiso 1 1 calc R . . H5B H 0.6516 0.2246 0.4998 0.078 Uiso 1 1 calc R . . C6 C 0.5505(3) 0.2446(3) 0.4411(2) 0.0711(12) Uani 1 1 d . . . H6A H 0.5275 0.2916 0.4089 0.085 Uiso 1 1 calc R . . H6B H 0.4974 0.2298 0.4804 0.085 Uiso 1 1 calc R . . C7 C 1.3212(3) 0.1968(3) 0.2470(3) 0.0894(15) Uani 1 1 d . . . H7A H 1.3196 0.2493 0.2133 0.107 Uiso 1 1 calc R . . H7B H 1.3591 0.2016 0.2777 0.107 Uiso 1 1 calc R . . C8 C 1.3614(4) 0.1264(3) 0.2158(3) 0.0957(17) Uani 1 1 d . . . H8A H 1.3591 0.0741 0.2501 0.115 Uiso 1 1 calc R . . H8B H 1.4290 0.1341 0.1920 0.115 Uiso 1 1 calc R . . C9 C 1.2351(4) -0.0221(3) 0.2117(3) 0.0925(16) Uani 1 1 d . . . H9A H 1.2599 -0.0324 0.2518 0.111 Uiso 1 1 calc R . . H9B H 1.2343 -0.0753 0.2016 0.111 Uiso 1 1 calc R . . C10 C 1.2990(4) 0.0336(3) 0.1547(3) 0.0963(17) Uani 1 1 d . . . H10A H 1.2776 0.0385 0.1139 0.116 Uiso 1 1 calc R . . H10B H 1.3655 0.0085 0.1489 0.116 Uiso 1 1 calc R . . C11 C 1.2482(4) 0.2014(4) 0.0662(3) 0.1078(19) Uani 1 1 d . . . H11A H 1.2464 0.1552 0.0471 0.129 Uiso 1 1 calc R . . H11B H 1.2623 0.2513 0.0300 0.129 Uiso 1 1 calc R . . C12 C 1.3216(4) 0.1829(4) 0.1058(3) 0.1008(17) Uani 1 1 d . . . H12A H 1.3822 0.1632 0.0794 0.121 Uiso 1 1 calc R . . H12B H 1.3333 0.2343 0.1146 0.121 Uiso 1 1 calc R . . C13 C 0.6847(4) 0.1175(3) 0.2423(3) 0.0882(15) Uani 1 1 d . . . H13A H 0.6481 0.0732 0.2753 0.106 Uiso 1 1 calc R . . H13B H 0.6552 0.1332 0.2039 0.106 Uiso 1 1 calc R . . C14 C 0.7802(4) 0.0843(4) 0.2216(3) 0.0886(15) Uani 1 1 d . . . C15 C 0.8194(4) 0.0074(3) 0.2565(3) 0.0862(15) Uani 1 1 d . . . H15 H 0.7763 -0.0259 0.2913 0.103 Uiso 1 1 calc R . . C16 C 0.9174(4) -0.0228(4) 0.2429(3) 0.0917(16) Uani 1 1 d . . . H16 H 0.9411 -0.0722 0.2687 0.110 Uiso 1 1 calc R . . C17 C 0.9767(4) 0.0274(4) 0.1876(3) 0.0943(16) Uani 1 1 d . . . C18 C 0.9361(4) 0.1040(4) 0.1511(3) 0.0969(16) Uani 1 1 d . . . H18 H 0.9768 0.1354 0.1134 0.116 Uiso 1 1 calc R . . C19 C 0.8419(4) 0.1332(4) 0.1685(3) 0.0896(15) Uani 1 1 d . . . H19 H 0.8194 0.1849 0.1451 0.107 Uiso 1 1 calc R . . C20 C 1.0843(4) 0.0059(3) 0.1710(3) 0.0981(17) Uani 1 1 d . . . H20A H 1.1131 0.0402 0.1272 0.118 Uiso 1 1 calc R . . H20B H 1.0964 -0.0522 0.1691 0.118 Uiso 1 1 calc R . . C21 C 1.2113(3) 0.1101(3) 0.3494(2) 0.0712(12) Uani 1 1 d . . . H21A H 1.2431 0.1296 0.3772 0.085 Uiso 1 1 calc R . . H21B H 1.2455 0.0577 0.3423 0.085 Uiso 1 1 calc R . . C22 C 1.1081(3) 0.0946(3) 0.3859(2) 0.0592(11) Uani 1 1 d . . . C23 C 1.0721(3) 0.0201(3) 0.3908(2) 0.0599(11) Uani 1 1 d . . . H23 H 1.1144 -0.0214 0.3751 0.072 Uiso 1 1 calc R . . C24 C 0.9799(3) 0.0060(2) 0.4171(2) 0.0624(11) Uani 1 1 d . . . H24 H 0.9594 -0.0458 0.4199 0.075 Uiso 1 1 calc R . . C25 C 0.9096(3) 0.0665(2) 0.4417(2) 0.0592(11) Uani 1 1 d . . . C26 C 0.9504(3) 0.1391(2) 0.4394(2) 0.0579(10) Uani 1 1 d . . . H26 H 0.9108 0.1793 0.4587 0.070 Uiso 1 1 calc R . . C27 C 1.0437(3) 0.1530(2) 0.4106(2) 0.0576(10) Uani 1 1 d . . . H27 H 1.0657 0.2045 0.4072 0.069 Uiso 1 1 calc R . . C28 C 0.8042(3) 0.0541(2) 0.4695(2) 0.0612(11) Uani 1 1 d . . . H28A H 0.7739 0.0961 0.4936 0.073 Uiso 1 1 calc R . . H28B H 0.7955 -0.0006 0.5003 0.073 Uiso 1 1 calc R . . C29 C 0.9426(3) 0.1646(3) 0.2816(2) 0.0598(11) Uani 1 1 d . . . H29 H 0.9374 0.1073 0.2916 0.072 Uiso 1 1 calc R . . C30 C 0.9089(3) 0.2921(3) 0.2790(2) 0.0714(13) Uani 1 1 d . . . H30 H 0.8752 0.3428 0.2836 0.086 Uiso 1 1 calc R . . C31 C 1.0047(3) 0.2837(3) 0.2502(2) 0.0708(12) Uani 1 1 d . . . H31 H 1.0488 0.3252 0.2352 0.085 Uiso 1 1 calc R . . Cu2 Cu 0.48379(4) 0.63327(3) 0.20502(3) 0.06777(17) Uani 1 1 d . . . Zn2 Zn 0.81220(3) 0.51403(3) 0.34139(2) 0.05008(13) Uani 1 1 d . . . N9 N 0.3671(2) 0.5720(2) 0.27835(18) 0.0663(9) Uani 1 1 d . . . H9C H 0.3881 0.5169 0.2875 0.080 Uiso 1 1 calc R . . N10 N 0.5095(3) 0.7557(2) 0.20295(19) 0.0759(10) Uani 1 1 d . . . H10C H 0.5204 0.7524 0.2439 0.091 Uiso 1 1 calc R . . N11 N 0.3687(3) 0.6929(3) 0.1582(2) 0.0791(11) Uani 1 1 d . . . N12 N 0.9338(2) 0.5472(2) 0.25763(18) 0.0735(10) Uani 1 1 d . . . H12C H 0.9265 0.5228 0.2260 0.088 Uiso 1 1 calc R . . N13 N 0.7564(2) 0.60878(18) 0.39517(17) 0.0558(8) Uani 1 1 d . . . H13C H 0.7389 0.6555 0.3653 0.067 Uiso 1 1 calc R . . N14 N 0.9236(2) 0.49751(19) 0.39688(18) 0.0598(9) Uani 1 1 d . . . N15 N 0.5883(2) 0.5648(2) 0.23881(18) 0.0645(9) Uani 1 1 d . . . N16 N 0.7152(2) 0.5132(2) 0.29220(17) 0.0590(9) Uani 1 1 d . . . O3 O 0.78752(19) 0.39961(16) 0.40101(14) 0.0598(7) Uani 1 1 d . . . H1 H 0.751(3) 0.356(3) 0.393(2) 0.097(15) Uiso 1 1 d . . . O4 O 0.5460(2) 0.6209(2) 0.10605(16) 0.1003(11) Uani 1 1 d . . . C32 C 0.2852(3) 0.5778(3) 0.2453(2) 0.0764(13) Uani 1 1 d . . . H32A H 0.2248 0.5647 0.2787 0.092 Uiso 1 1 calc R . . H32B H 0.2984 0.5388 0.2172 0.092 Uiso 1 1 calc R . . C33 C 0.2766(3) 0.6674(3) 0.2029(2) 0.0813(14) Uani 1 1 d . . . H33A H 0.2284 0.6719 0.1768 0.098 Uiso 1 1 calc R . . H33B H 0.2540 0.7049 0.2323 0.098 Uiso 1 1 calc R . . C34 C 0.4123(3) 0.8035(3) 0.2019(3) 0.0841(14) Uani 1 1 d . . . H34A H 0.4190 0.8628 0.1942 0.101 Uiso 1 1 calc R . . H34B H 0.3664 0.7849 0.2445 0.101 Uiso 1 1 calc R . . C35 C 0.3765(4) 0.7874(3) 0.1460(3) 0.0876(15) Uani 1 1 d . . . H35A H 0.4215 0.8080 0.1034 0.105 Uiso 1 1 calc R . . H35B H 0.3129 0.8168 0.1442 0.105 Uiso 1 1 calc R . . C36 C 0.4896(4) 0.6655(4) 0.0612(3) 0.0983(17) Uani 1 1 d . . . H36A H 0.4989 0.6391 0.0245 0.118 Uiso 1 1 calc R . . H36B H 0.5100 0.7221 0.0427 0.118 Uiso 1 1 calc R . . C37 C 0.3847(4) 0.6674(4) 0.0967(3) 0.0934(16) Uani 1 1 d . . . H37A H 0.3471 0.7058 0.0675 0.112 Uiso 1 1 calc R . . H37B H 0.3614 0.6122 0.1066 0.112 Uiso 1 1 calc R . . C38 C 1.0191(3) 0.5067(3) 0.2788(2) 0.0721(13) Uani 1 1 d . . . H38A H 1.0766 0.5276 0.2451 0.087 Uiso 1 1 calc R . . H38B H 1.0201 0.4471 0.2831 0.087 Uiso 1 1 calc R . . C39 C 1.0234(3) 0.5208(3) 0.3456(2) 0.0710(13) Uani 1 1 d . . . H39A H 1.0339 0.5789 0.3401 0.085 Uiso 1 1 calc R . . H39B H 1.0770 0.4862 0.3620 0.085 Uiso 1 1 calc R . . C40 C 0.8408(3) 0.6292(2) 0.4189(2) 0.0584(11) Uani 1 1 d . . . H40A H 0.8157 0.6581 0.4543 0.070 Uiso 1 1 calc R . . H40B H 0.8832 0.6655 0.3820 0.070 Uiso 1 1 calc R . . C41 C 0.8986(3) 0.5478(2) 0.4451(2) 0.0608(11) Uani 1 1 d . . . H41A H 0.9579 0.5607 0.4539 0.073 Uiso 1 1 calc R . . H41B H 0.8598 0.5165 0.4869 0.073 Uiso 1 1 calc R . . C42 C 0.8357(3) 0.3730(2) 0.4571(2) 0.0620(11) Uani 1 1 d . . . H42A H 0.7983 0.3946 0.4947 0.074 Uiso 1 1 calc R . . H42B H 0.8423 0.3125 0.4717 0.074 Uiso 1 1 calc R . . C43 C 0.9314(3) 0.4066(2) 0.4324(2) 0.0613(11) Uani 1 1 d . . . H43A H 0.9728 0.3757 0.4018 0.074 Uiso 1 1 calc R . . H43B H 0.9617 0.3999 0.4698 0.074 Uiso 1 1 calc R . . C44 C 0.5922(4) 0.8029(3) 0.1525(3) 0.0894(15) Uani 1 1 d . . . H44A H 0.5930 0.7979 0.1080 0.107 Uiso 1 1 calc R . . H44B H 0.5814 0.8616 0.1522 0.107 Uiso 1 1 calc R . . C45 C 0.6846(4) 0.7709(3) 0.1684(3) 0.0883(15) Uani 1 1 d . . . C46 C 0.7476(4) 0.7138(3) 0.1318(3) 0.0891(15) Uani 1 1 d . . . H46 H 0.7312 0.7057 0.0945 0.107 Uiso 1 1 calc R . . C47 C 0.8300(4) 0.6719(3) 0.1504(3) 0.0870(15) Uani 1 1 d . . . H47 H 0.8648 0.6312 0.1295 0.104 Uiso 1 1 calc R . . C48 C 0.8620(4) 0.6922(3) 0.2037(3) 0.0882(15) Uani 1 1 d . . . C49 C 0.8049(4) 0.7489(3) 0.2358(3) 0.0900(15) Uani 1 1 d . . . H49 H 0.8248 0.7632 0.2695 0.108 Uiso 1 1 calc R . . C50 C 0.7158(4) 0.7858(3) 0.2184(3) 0.0905(16) Uani 1 1 d . . . H50 H 0.6774 0.8220 0.2427 0.109 Uiso 1 1 calc R . . C51 C 0.9493(3) 0.6409(3) 0.2214(3) 0.0873(15) Uani 1 1 d . . . H51A H 0.9731 0.6657 0.2501 0.105 Uiso 1 1 calc R . . H51B H 1.0000 0.6434 0.1807 0.105 Uiso 1 1 calc R . . C52 C 0.6753(3) 0.5896(2) 0.4482(2) 0.0581(10) Uani 1 1 d . . . H52A H 0.6646 0.6308 0.4744 0.070 Uiso 1 1 calc R . . H52B H 0.6887 0.5355 0.4773 0.070 Uiso 1 1 calc R . . C53 C 0.5844(3) 0.5878(3) 0.4254(2) 0.0559(10) Uani 1 1 d . . . C54 C 0.5528(3) 0.5176(3) 0.42121(19) 0.0555(10) Uani 1 1 d . . . H54 H 0.5862 0.4663 0.4351 0.067 Uiso 1 1 calc R . . C55 C 0.4726(3) 0.5211(3) 0.3968(2) 0.0597(11) Uani 1 1 d . . . H55 H 0.4499 0.4709 0.3978 0.072 Uiso 1 1 calc R . . C56 C 0.4236(3) 0.5925(3) 0.3713(2) 0.0600(11) Uani 1 1 d . . . C57 C 0.4507(3) 0.6634(3) 0.3764(2) 0.0648(11) Uani 1 1 d . . . H57 H 0.4178 0.7141 0.3606 0.078 Uiso 1 1 calc R . . C58 C 0.5291(3) 0.6611(3) 0.4058(2) 0.0597(11) Uani 1 1 d . . . H58 H 0.5444 0.7102 0.4124 0.072 Uiso 1 1 calc R . . C59 C 0.3371(3) 0.5920(3) 0.3427(2) 0.0663(12) Uani 1 1 d . . . H59A H 0.2933 0.5513 0.3736 0.080 Uiso 1 1 calc R . . H59B H 0.3017 0.6466 0.3377 0.080 Uiso 1 1 calc R . . C60 C 0.6475(3) 0.5792(3) 0.2675(2) 0.0593(11) Uani 1 1 d . . . H60 H 0.6481 0.6325 0.2731 0.071 Uiso 1 1 calc R . . C61 C 0.6082(3) 0.4726(3) 0.2452(2) 0.0719(13) Uani 1 1 d . . . H61 H 0.5754 0.4403 0.2294 0.086 Uiso 1 1 calc R . . C62 C 0.6798(3) 0.4445(3) 0.2766(2) 0.0695(12) Uani 1 1 d . . . H62 H 0.7041 0.3890 0.2873 0.083 Uiso 1 1 calc R . . Cl1 Cl 0.26435(11) 0.34559(10) 0.37501(9) 0.0987(4) Uani 1 1 d . . . O5 O 0.2241(3) 0.4057(3) 0.4108(2) 0.1246(14) Uani 1 1 d . . . O6 O 0.3550(3) 0.3685(3) 0.3335(2) 0.1341(15) Uani 1 1 d . . . O7 O 0.2768(3) 0.2674(3) 0.4174(2) 0.1419(16) Uani 1 1 d . . . O8 O 0.2024(3) 0.3407(3) 0.3348(2) 0.1280(14) Uani 1 1 d . . . Cl2 Cl 0.08147(15) 0.77482(12) 0.35564(14) 0.1347(7) Uani 1 1 d D . . O9 O 0.0441(4) 0.7275(4) 0.4204(2) 0.211(3) Uani 1 1 d D . . O10 O 0.0275(4) 0.8515(2) 0.3437(3) 0.211(3) Uani 1 1 d D . . O11 O 0.1779(2) 0.7916(4) 0.3477(4) 0.199(3) Uani 1 1 d D . . O12 O 0.0712(4) 0.7360(4) 0.3078(2) 0.198(3) Uani 1 1 d D . . Cl3 Cl 0.47325(17) 0.92860(11) 0.33397(13) 0.1217(6) Uani 1 1 d D . . O13 O 0.5304(4) 0.8962(3) 0.3803(3) 0.188(2) Uani 1 1 d D . . O14 O 0.3961(4) 0.8786(4) 0.3488(3) 0.212(3) Uani 1 1 d D . . O15 O 0.5224(4) 0.9385(4) 0.26713(19) 0.200(3) Uani 1 1 d D . . O16 O 0.4347(4) 1.0057(2) 0.3448(3) 0.191(2) Uani 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 0.0395(3) 0.0410(3) 0.0761(3) -0.0199(2) -0.0109(2) -0.0040(2) Zn1 0.0578(3) 0.0789(4) 0.0712(4) -0.0198(3) -0.0047(3) 0.0109(3) N1 0.056(3) 0.090(3) 0.093(3) -0.022(2) -0.024(2) -0.0050(19) N2 0.044(2) 0.058(2) 0.102(3) -0.027(2) -0.009(2) -0.0059(16) N3 0.046(2) 0.0437(19) 0.092(3) -0.0207(18) -0.0018(19) -0.0069(15) N4 0.053(2) 0.078(3) 0.091(3) -0.018(2) -0.007(2) -0.0026(19) N5 0.066(3) 0.093(3) 0.093(3) -0.017(3) 0.007(2) 0.006(2) N6 0.066(3) 0.099(3) 0.093(3) -0.039(2) 0.002(2) 0.006(2) N7 0.041(2) 0.050(2) 0.069(2) -0.0140(17) -0.0097(16) 0.0041(15) N8 0.050(2) 0.054(2) 0.074(2) -0.0093(18) -0.0032(18) -0.0035(17) O1 0.0488(17) 0.0530(17) 0.095(2) -0.0355(15) 0.0061(15) -0.0130(13) O2 0.080(3) 0.120(3) 0.077(2) -0.011(2) 0.0036(19) 0.020(2) C1 0.050(3) 0.088(4) 0.107(4) -0.035(3) -0.022(3) -0.006(2) C2 0.049(3) 0.079(3) 0.132(5) -0.044(3) -0.023(3) -0.008(2) C3 0.043(3) 0.052(3) 0.108(4) -0.021(2) -0.001(2) -0.011(2) C4 0.049(3) 0.061(3) 0.117(4) -0.024(3) -0.002(3) -0.019(2) C5 0.051(3) 0.050(3) 0.087(3) -0.027(2) 0.007(2) -0.008(2) C6 0.048(3) 0.059(3) 0.105(4) -0.032(3) -0.005(2) -0.003(2) C7 0.046(3) 0.096(4) 0.108(4) -0.018(3) 0.006(3) -0.005(3) C8 0.057(3) 0.108(4) 0.098(4) -0.009(3) 0.002(3) 0.003(3) C9 0.070(4) 0.091(4) 0.105(4) -0.032(3) -0.003(3) 0.017(3) C10 0.066(4) 0.107(4) 0.097(4) -0.023(3) 0.006(3) 0.010(3) C11 0.082(4) 0.121(5) 0.087(4) -0.010(3) 0.014(3) 0.006(3) C12 0.075(4) 0.105(4) 0.096(4) -0.011(4) 0.006(3) 0.003(3) C13 0.067(4) 0.102(4) 0.115(4) -0.047(3) -0.033(3) -0.007(3) C14 0.073(4) 0.102(4) 0.108(4) -0.049(4) -0.027(3) -0.003(3) C15 0.076(4) 0.087(4) 0.110(4) -0.048(3) -0.020(3) -0.010(3) C16 0.075(4) 0.099(4) 0.106(4) -0.041(3) -0.012(3) -0.008(3) C17 0.076(4) 0.097(4) 0.122(5) -0.056(4) -0.019(4) 0.008(3) C18 0.092(5) 0.104(5) 0.101(4) -0.045(4) -0.015(3) -0.002(3) C19 0.069(4) 0.101(4) 0.109(4) -0.045(4) -0.019(3) -0.004(3) C20 0.075(4) 0.101(4) 0.129(5) -0.062(4) -0.015(3) 0.011(3) C21 0.046(3) 0.076(3) 0.087(3) -0.011(3) -0.016(2) -0.003(2) C22 0.035(2) 0.065(3) 0.077(3) -0.015(2) -0.016(2) -0.001(2) C23 0.038(3) 0.057(3) 0.081(3) -0.016(2) -0.014(2) 0.0098(19) C24 0.044(3) 0.047(2) 0.083(3) -0.007(2) -0.005(2) 0.0048(19) C25 0.041(2) 0.050(3) 0.076(3) -0.006(2) -0.006(2) 0.0016(19) C26 0.047(3) 0.048(3) 0.074(3) -0.015(2) -0.010(2) 0.0019(19) C27 0.036(2) 0.057(3) 0.081(3) -0.019(2) -0.017(2) 0.0025(19) C28 0.048(3) 0.044(2) 0.083(3) -0.009(2) -0.008(2) -0.0040(18) C29 0.047(3) 0.053(3) 0.070(3) -0.010(2) -0.004(2) 0.000(2) C30 0.065(3) 0.042(2) 0.088(3) -0.003(2) 0.003(3) -0.007(2) C31 0.059(3) 0.051(3) 0.082(3) -0.008(2) 0.011(2) -0.008(2) Cu2 0.0544(3) 0.0781(4) 0.0604(3) -0.0036(3) -0.0145(3) 0.0052(3) Zn2 0.0436(3) 0.0435(3) 0.0637(3) -0.0135(2) -0.0138(2) -0.00193(19) N9 0.052(2) 0.069(2) 0.076(3) -0.0147(19) -0.0190(19) 0.0018(17) N10 0.068(3) 0.078(3) 0.076(3) -0.002(2) -0.026(2) -0.002(2) N11 0.068(3) 0.095(3) 0.072(3) -0.013(2) -0.027(2) 0.003(2) N12 0.051(2) 0.086(3) 0.082(3) -0.024(2) -0.009(2) -0.0067(19) N13 0.058(2) 0.0371(18) 0.077(2) -0.0119(16) -0.0249(19) -0.0039(15) N14 0.047(2) 0.050(2) 0.091(3) -0.0224(19) -0.0247(18) -0.0040(15) N15 0.054(2) 0.068(2) 0.077(2) -0.0231(19) -0.0240(19) 0.0044(17) N16 0.049(2) 0.058(2) 0.079(2) -0.0275(18) -0.0245(18) 0.0089(16) O3 0.0632(18) 0.0410(16) 0.087(2) -0.0186(14) -0.0310(16) -0.0114(13) O4 0.084(3) 0.138(3) 0.070(2) -0.021(2) -0.020(2) 0.015(2) C32 0.052(3) 0.093(4) 0.086(3) -0.019(3) -0.026(3) 0.002(2) C33 0.065(3) 0.100(4) 0.081(3) -0.019(3) -0.031(3) 0.005(3) C34 0.070(3) 0.081(3) 0.093(4) -0.004(3) -0.029(3) 0.010(3) C35 0.072(4) 0.090(4) 0.086(4) -0.001(3) -0.024(3) 0.012(3) C36 0.094(4) 0.130(5) 0.069(3) -0.021(3) -0.024(3) 0.001(3) C37 0.078(4) 0.123(5) 0.081(4) -0.020(3) -0.035(3) 0.008(3) C38 0.040(3) 0.077(3) 0.096(4) -0.022(3) -0.008(2) -0.005(2) C39 0.051(3) 0.059(3) 0.101(4) -0.015(3) -0.019(3) -0.001(2) C40 0.051(3) 0.044(2) 0.087(3) -0.017(2) -0.030(2) -0.0003(18) C41 0.057(3) 0.047(2) 0.086(3) -0.014(2) -0.032(2) -0.0042(19) C42 0.061(3) 0.044(2) 0.085(3) -0.008(2) -0.032(2) -0.0031(19) C43 0.055(3) 0.048(3) 0.090(3) -0.015(2) -0.037(2) 0.0012(19) C44 0.074(4) 0.077(3) 0.100(4) 0.006(3) -0.021(3) -0.006(3) C45 0.070(4) 0.087(4) 0.096(4) 0.000(3) -0.020(3) -0.013(3) C46 0.071(4) 0.102(4) 0.077(4) 0.008(3) -0.017(3) -0.011(3) C47 0.064(3) 0.096(4) 0.083(4) 0.006(3) -0.011(3) -0.015(3) C48 0.060(4) 0.088(4) 0.096(4) 0.010(3) -0.013(3) -0.012(3) C49 0.067(4) 0.085(4) 0.107(4) 0.000(3) -0.021(3) -0.016(3) C50 0.075(4) 0.082(4) 0.101(4) 0.002(3) -0.017(3) -0.018(3) C51 0.055(3) 0.103(4) 0.087(4) 0.003(3) -0.008(3) -0.021(3) C52 0.054(3) 0.051(2) 0.069(3) -0.021(2) -0.008(2) -0.0044(19) C53 0.046(3) 0.058(3) 0.061(3) -0.016(2) -0.008(2) 0.000(2) C54 0.046(3) 0.054(3) 0.060(3) -0.012(2) -0.004(2) -0.0025(19) C55 0.040(3) 0.064(3) 0.068(3) -0.013(2) -0.005(2) -0.002(2) C56 0.047(3) 0.068(3) 0.062(3) -0.018(2) -0.007(2) -0.002(2) C57 0.048(3) 0.069(3) 0.068(3) -0.012(2) -0.008(2) 0.008(2) C58 0.049(3) 0.058(3) 0.066(3) -0.019(2) -0.001(2) 0.001(2) C59 0.052(3) 0.080(3) 0.062(3) -0.014(2) -0.009(2) -0.002(2) C60 0.055(3) 0.055(3) 0.071(3) -0.017(2) -0.021(2) 0.004(2) C61 0.066(3) 0.066(3) 0.097(4) -0.029(3) -0.039(3) 0.004(2) C62 0.061(3) 0.066(3) 0.095(3) -0.033(3) -0.037(3) 0.014(2) Cl1 0.0811(11) 0.0883(11) 0.1336(13) -0.0359(10) -0.0317(10) 0.0015(8) O5 0.132(4) 0.110(3) 0.146(4) -0.053(3) -0.048(3) 0.018(3) O6 0.093(3) 0.122(3) 0.181(4) -0.032(3) -0.028(3) -0.003(3) O7 0.121(4) 0.100(3) 0.175(4) -0.002(3) -0.025(3) 0.008(3) O8 0.095(3) 0.135(4) 0.174(4) -0.064(3) -0.043(3) 0.001(2) Cl2 0.1026(14) 0.0852(12) 0.207(2) -0.0547(13) -0.0007(14) -0.0046(10) O9 0.168(6) 0.191(6) 0.247(7) -0.012(5) -0.034(5) -0.038(5) O10 0.175(6) 0.142(5) 0.283(7) -0.060(5) -0.002(5) 0.019(4) O11 0.123(5) 0.158(5) 0.307(8) -0.089(5) 0.007(5) -0.027(4) O12 0.175(5) 0.166(5) 0.263(7) -0.107(5) 0.013(5) -0.054(4) Cl3 0.1418(17) 0.0807(11) 0.1669(18) -0.0415(12) -0.0721(14) 0.0020(10) O13 0.170(5) 0.160(5) 0.258(7) -0.071(5) -0.100(5) 0.040(4) O14 0.230(7) 0.166(6) 0.266(7) -0.050(5) -0.090(6) -0.046(5) O15 0.206(7) 0.200(6) 0.188(6) -0.060(5) -0.035(5) 0.011(5) O16 0.199(6) 0.114(4) 0.259(7) -0.045(4) -0.066(5) 0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N7 1.971(3) . ? Cu1 O1 2.020(3) . ? Cu1 N1 2.131(4) . ? Cu1 N3 2.135(3) . ? Cu1 N2 2.144(3) . ? Zn1 N8 1.914(3) . ? Zn1 N4 2.086(4) . ? Zn1 N5 2.093(4) . ? Zn1 O2 2.101(3) . ? Zn1 N6 2.201(4) . ? N1 C1 1.529(5) . ? N1 C13 1.566(6) . ? N1 H1C 0.9100 . ? N2 C4 1.429(5) . ? N2 C2 1.514(5) . ? N2 C6 1.546(5) . ? N3 C28 1.494(5) . ? N3 C3 1.512(5) . ? N3 H3C 0.9100 . ? N4 C21 1.487(5) . ? N4 C7 1.489(5) . ? N4 H4C 0.9100 . ? N5 C12 1.371(6) . ? N5 C8 1.571(6) . ? N5 C10 1.594(6) . ? N6 C9 1.514(5) . ? N6 C20 1.521(6) . ? N6 H6C 0.9100 . ? N7 C29 1.337(5) . ? N7 C30 1.386(5) . ? N8 C29 1.321(5) . ? N8 C31 1.427(5) . ? O1 C5 1.368(4) . ? O1 H1 1.45(5) . ? O2 C11 1.497(5) . ? C1 C2 1.457(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.501(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.534(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.481(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.483(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.451(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.399(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.375(7) . ? C14 C15 1.415(7) . ? C15 C16 1.397(6) . ? C15 H15 0.9300 . ? C16 C17 1.393(7) . ? C16 H16 0.9300 . ? C17 C18 1.432(7) . ? C17 C20 1.491(7) . ? C18 C19 1.352(7) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.491(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.361(5) . ? C22 C23 1.374(5) . ? C23 C24 1.308(5) . ? C23 H23 0.9300 . ? C24 C25 1.427(5) . ? C24 H24 0.9300 . ? C25 C26 1.394(5) . ? C25 C28 1.480(5) . ? C26 C27 1.330(5) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29 0.9300 . ? C30 C31 1.345(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? Cu2 N15 1.910(3) . ? Cu2 N10 2.109(4) . ? Cu2 N9 2.117(3) . ? Cu2 N11 2.119(4) . ? Cu2 O4 2.120(3) . ? Zn2 N16 1.933(3) . ? Zn2 O3 2.000(3) . ? Zn2 N12 2.146(4) . ? Zn2 N14 2.149(3) . ? Zn2 N13 2.150(3) . ? N9 C59 1.443(5) . ? N9 C32 1.483(5) . ? N9 H9C 0.9100 . ? N10 C34 1.497(5) . ? N10 C44 1.513(6) . ? N10 H10C 0.9100 . ? N11 C37 1.439(6) . ? N11 C33 1.442(6) . ? N11 C35 1.541(6) . ? N12 C38 1.419(5) . ? N12 C51 1.558(6) . ? N12 H12C 0.9100 . ? N13 C52 1.391(5) . ? N13 C40 1.521(4) . ? N13 H13C 0.9100 . ? N14 C41 1.445(5) . ? N14 C43 1.500(5) . ? N14 C39 1.572(5) . ? N15 C60 1.237(5) . ? N15 C61 1.500(5) . ? N16 C60 1.436(5) . ? N16 C62 1.456(5) . ? O3 C42 1.462(4) . ? O3 H1 1.02(5) . ? O4 C36 1.393(5) . ? C32 C33 1.527(6) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.506(6) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.486(6) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.519(6) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.530(5) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.452(5) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.433(7) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C50 1.344(7) . ? C45 C46 1.459(7) . ? C46 C47 1.369(6) . ? C46 H46 0.9300 . ? C47 C48 1.455(7) . ? C47 H47 0.9300 . ? C48 C49 1.372(7) . ? C48 C51 1.477(7) . ? C49 C50 1.419(7) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.495(5) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.342(5) . ? C53 C58 1.381(5) . ? C54 C55 1.354(5) . ? C54 H54 0.9300 . ? C55 C56 1.346(5) . ? C55 H55 0.9300 . ? C56 C57 1.332(5) . ? C56 C59 1.502(5) . ? C57 C58 1.399(6) . ? C57 H57 0.9300 . ? C58 H58 0.9300 . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60 0.9300 . ? C61 C62 1.320(5) . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? Cl1 O7 1.385(4) . ? Cl1 O6 1.395(4) . ? Cl1 O5 1.396(4) . ? Cl1 O8 1.398(4) . ? Cl2 O11 1.391(2) . ? Cl2 O10 1.392(2) . ? Cl2 O12 1.393(2) . ? Cl2 O9 1.395(2) . ? Cl3 O16 1.3822(19) . ? Cl3 O13 1.385(2) . ? Cl3 O14 1.385(2) . ? Cl3 O15 1.390(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 N7 Cu1 O1 94.83(12) . . ? N7 Cu1 N1 97.16(14) . . ? O1 Cu1 N1 127.53(13) . . ? N7 Cu1 N3 103.88(12) . . ? O1 Cu1 N3 112.25(13) . . ? N1 Cu1 N3 113.89(14) . . ? N7 Cu1 N2 173.28(13) . . ? O1 Cu1 N2 81.17(12) . . ? N1 Cu1 N2 81.23(14) . . ? N3 Cu1 N2 82.68(13) . . ? N8 Zn1 N4 97.11(14) . . ? N8 Zn1 N5 168.41(16) . . ? N4 Zn1 N5 82.30(17) . . ? N8 Zn1 O2 93.11(13) . . ? N4 Zn1 O2 132.28(15) . . ? N5 Zn1 O2 79.04(16) . . ? N8 Zn1 N6 104.96(14) . . ? N4 Zn1 N6 115.64(16) . . ? N5 Zn1 N6 85.56(16) . . ? O2 Zn1 N6 106.24(15) . . ? C1 N1 C13 111.7(3) . . ? C1 N1 Cu1 107.7(3) . . ? C13 N1 Cu1 118.3(3) . . ? C1 N1 H1C 106.1 . . ? C13 N1 H1C 106.1 . . ? Cu1 N1 H1C 106.1 . . ? C4 N2 C2 113.9(4) . . ? C4 N2 C6 110.4(4) . . ? C2 N2 C6 109.0(3) . . ? C4 N2 Cu1 107.7(3) . . ? C2 N2 Cu1 108.2(3) . . ? C6 N2 Cu1 107.5(2) . . ? C28 N3 C3 113.0(3) . . ? C28 N3 Cu1 114.8(2) . . ? C3 N3 Cu1 103.4(2) . . ? C28 N3 H3C 108.5 . . ? C3 N3 H3C 108.5 . . ? Cu1 N3 H3C 108.5 . . ? C21 N4 C7 116.6(4) . . ? C21 N4 Zn1 118.1(3) . . ? C7 N4 Zn1 107.3(3) . . ? C21 N4 H4C 104.4 . . ? C7 N4 H4C 104.4 . . ? Zn1 N4 H4C 104.4 . . ? C12 N5 C8 112.8(5) . . ? C12 N5 C10 111.3(5) . . ? C8 N5 C10 112.6(4) . . ? C12 N5 Zn1 109.0(3) . . ? C8 N5 Zn1 105.7(3) . . ? C10 N5 Zn1 104.8(3) . . ? C9 N6 C20 107.4(4) . . ? C9 N6 Zn1 104.8(3) . . ? C20 N6 Zn1 114.6(3) . . ? C9 N6 H6C 110.0 . . ? C20 N6 H6C 110.0 . . ? Zn1 N6 H6C 110.0 . . ? C29 N7 C30 101.1(3) . . ? C29 N7 Cu1 127.8(3) . . ? C30 N7 Cu1 130.8(3) . . ? C29 N8 C31 102.7(3) . . ? C29 N8 Zn1 132.5(3) . . ? C31 N8 Zn1 124.0(3) . . ? C5 O1 Cu1 115.2(2) . . ? C5 O1 H1 106.1(17) . . ? Cu1 O1 H1 133.3(17) . . ? C11 O2 Zn1 112.7(3) . . ? C2 C1 N1 106.2(4) . . ? C2 C1 H1A 110.5 . . ? N1 C1 H1A 110.5 . . ? C2 C1 H1B 110.5 . . ? N1 C1 H1B 110.5 . . ? H1A C1 H1B 108.7 . . ? C1 C2 N2 113.1(4) . . ? C1 C2 H2A 109.0 . . ? N2 C2 H2A 109.0 . . ? C1 C2 H2B 109.0 . . ? N2 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C4 C3 N3 108.5(3) . . ? C4 C3 H3A 110.0 . . ? N3 C3 H3A 110.0 . . ? C4 C3 H3B 110.0 . . ? N3 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? N2 C4 C3 109.2(4) . . ? N2 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? N2 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? O1 C5 C6 111.4(4) . . ? O1 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? O1 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C5 C6 N2 106.0(3) . . ? C5 C6 H6A 110.5 . . ? N2 C6 H6A 110.5 . . ? C5 C6 H6B 110.5 . . ? N2 C6 H6B 110.5 . . ? H6A C6 H6B 108.7 . . ? C8 C7 N4 102.5(4) . . ? C8 C7 H7A 111.3 . . ? N4 C7 H7A 111.3 . . ? C8 C7 H7B 111.3 . . ? N4 C7 H7B 111.3 . . ? H7A C7 H7B 109.2 . . ? C7 C8 N5 108.0(4) . . ? C7 C8 H8A 110.1 . . ? N5 C8 H8A 110.1 . . ? C7 C8 H8B 110.1 . . ? N5 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? C10 C9 N6 108.8(4) . . ? C10 C9 H9A 109.9 . . ? N6 C9 H9A 109.9 . . ? C10 C9 H9B 109.9 . . ? N6 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C9 C10 N5 112.5(4) . . ? C9 C10 H10A 109.1 . . ? N5 C10 H10A 109.1 . . ? C9 C10 H10B 109.1 . . ? N5 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C12 C11 O2 105.8(4) . . ? C12 C11 H11A 110.6 . . ? O2 C11 H11A 110.6 . . ? C12 C11 H11B 110.6 . . ? O2 C11 H11B 110.6 . . ? H11A C11 H11B 108.7 . . ? N5 C12 C11 114.9(5) . . ? N5 C12 H12A 108.5 . . ? C11 C12 H12A 108.5 . . ? N5 C12 H12B 108.5 . . ? C11 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C14 C13 N1 118.2(4) . . ? C14 C13 H13A 107.8 . . ? N1 C13 H13A 107.8 . . ? C14 C13 H13B 107.8 . . ? N1 C13 H13B 107.8 . . ? H13A C13 H13B 107.1 . . ? C19 C14 C13 117.9(6) . . ? C19 C14 C15 118.2(5) . . ? C13 C14 C15 123.6(6) . . ? C16 C15 C14 125.4(5) . . ? C16 C15 H15 117.3 . . ? C14 C15 H15 117.3 . . ? C17 C16 C15 114.4(6) . . ? C17 C16 H16 122.8 . . ? C15 C16 H16 122.8 . . ? C16 C17 C18 119.9(5) . . ? C16 C17 C20 119.7(6) . . ? C18 C17 C20 120.0(6) . . ? C19 C18 C17 123.6(6) . . ? C19 C18 H18 118.2 . . ? C17 C18 H18 118.2 . . ? C18 C19 C14 118.3(6) . . ? C18 C19 H19 120.9 . . ? C14 C19 H19 120.9 . . ? C17 C20 N6 111.3(4) . . ? C17 C20 H20A 109.4 . . ? N6 C20 H20A 109.4 . . ? C17 C20 H20B 109.4 . . ? N6 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N4 C21 C22 113.7(3) . . ? N4 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? N4 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C27 C22 C23 116.9(4) . . ? C27 C22 C21 123.7(4) . . ? C23 C22 C21 119.3(4) . . ? C24 C23 C22 121.9(4) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C23 C24 C25 122.9(4) . . ? C23 C24 H24 118.5 . . ? C25 C24 H24 118.5 . . ? C26 C25 C24 113.2(4) . . ? C26 C25 C28 122.2(3) . . ? C24 C25 C28 124.6(4) . . ? C27 C26 C25 122.6(4) . . ? C27 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? C26 C27 C22 122.3(4) . . ? C26 C27 H27 118.9 . . ? C22 C27 H27 118.9 . . ? C25 C28 N3 107.7(3) . . ? C25 C28 H28A 110.2 . . ? N3 C28 H28A 110.2 . . ? C25 C28 H28B 110.2 . . ? N3 C28 H28B 110.2 . . ? H28A C28 H28B 108.5 . . ? N8 C29 N7 117.4(4) . . ? N8 C29 H29 121.3 . . ? N7 C29 H29 121.3 . . ? C31 C30 N7 111.9(4) . . ? C31 C30 H30 124.1 . . ? N7 C30 H30 124.1 . . ? C30 C31 N8 106.4(4) . . ? C30 C31 H31 126.8 . . ? N8 C31 H31 126.8 . . ? N15 Cu2 N10 104.42(15) . . ? N15 Cu2 N9 97.26(14) . . ? N10 Cu2 N9 119.77(14) . . ? N15 Cu2 N11 169.82(16) . . ? N10 Cu2 N11 84.44(15) . . ? N9 Cu2 N11 82.24(15) . . ? N15 Cu2 O4 92.40(14) . . ? N10 Cu2 O4 104.95(15) . . ? N9 Cu2 O4 129.72(14) . . ? N11 Cu2 O4 80.31(15) . . ? N16 Zn2 O3 94.07(13) . . ? N16 Zn2 N12 98.39(14) . . ? O3 Zn2 N12 126.48(13) . . ? N16 Zn2 N14 172.38(12) . . ? O3 Zn2 N14 79.66(11) . . ? N12 Zn2 N14 82.13(13) . . ? N16 Zn2 N13 104.97(12) . . ? O3 Zn2 N13 111.31(12) . . ? N12 Zn2 N13 115.07(13) . . ? N14 Zn2 N13 81.51(12) . . ? C59 N9 C32 113.5(3) . . ? C59 N9 Cu2 119.3(3) . . ? C32 N9 Cu2 107.3(3) . . ? C59 N9 H9C 105.2 . . ? C32 N9 H9C 105.2 . . ? Cu2 N9 H9C 105.2 . . ? C34 N10 C44 112.1(3) . . ? C34 N10 Cu2 104.2(3) . . ? C44 N10 Cu2 122.6(3) . . ? C34 N10 H10C 105.5 . . ? C44 N10 H10C 105.5 . . ? Cu2 N10 H10C 105.5 . . ? C37 N11 C33 111.7(4) . . ? C37 N11 C35 112.5(4) . . ? C33 N11 C35 110.8(4) . . ? C37 N11 Cu2 106.8(3) . . ? C33 N11 Cu2 108.9(3) . . ? C35 N11 Cu2 105.9(3) . . ? C38 N12 C51 110.7(3) . . ? C38 N12 Zn2 106.9(3) . . ? C51 N12 Zn2 120.1(3) . . ? C38 N12 H12C 106.1 . . ? C51 N12 H12C 106.1 . . ? Zn2 N12 H12C 106.1 . . ? C52 N13 C40 111.0(3) . . ? C52 N13 Zn2 116.0(2) . . ? C40 N13 Zn2 107.1(2) . . ? C52 N13 H13C 107.5 . . ? C40 N13 H13C 107.5 . . ? Zn2 N13 H13C 107.5 . . ? C41 N14 C43 110.0(3) . . ? C41 N14 C39 111.3(3) . . ? C43 N14 C39 109.0(3) . . ? C41 N14 Zn2 111.0(2) . . ? C43 N14 Zn2 107.2(2) . . ? C39 N14 Zn2 108.3(2) . . ? C60 N15 C61 102.1(3) . . ? C60 N15 Cu2 131.6(3) . . ? C61 N15 Cu2 125.8(3) . . ? C60 N16 C62 98.7(3) . . ? C60 N16 Zn2 129.8(3) . . ? C62 N16 Zn2 131.0(3) . . ? C42 O3 Zn2 116.5(2) . . ? C42 O3 H1 116(3) . . ? Zn2 O3 H1 127(3) . . ? C36 O4 Cu2 111.9(3) . . ? N9 C32 C33 107.0(4) . . ? N9 C32 H32A 110.3 . . ? C33 C32 H32A 110.3 . . ? N9 C32 H32B 110.3 . . ? C33 C32 H32B 110.3 . . ? H32A C32 H32B 108.6 . . ? N11 C33 C32 112.0(4) . . ? N11 C33 H33A 109.2 . . ? C32 C33 H33A 109.2 . . ? N11 C33 H33B 109.2 . . ? C32 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? N10 C34 C35 107.3(4) . . ? N10 C34 H34A 110.3 . . ? C35 C34 H34A 110.3 . . ? N10 C34 H34B 110.3 . . ? C35 C34 H34B 110.3 . . ? H34A C34 H34B 108.5 . . ? C34 C35 N11 109.5(4) . . ? C34 C35 H35A 109.8 . . ? N11 C35 H35A 109.8 . . ? C34 C35 H35B 109.8 . . ? N11 C35 H35B 109.8 . . ? H35A C35 H35B 108.2 . . ? O4 C36 C37 109.5(4) . . ? O4 C36 H36A 109.8 . . ? C37 C36 H36A 109.8 . . ? O4 C36 H36B 109.8 . . ? C37 C36 H36B 109.8 . . ? H36A C36 H36B 108.2 . . ? N11 C37 C36 112.4(4) . . ? N11 C37 H37A 109.1 . . ? C36 C37 H37A 109.1 . . ? N11 C37 H37B 109.1 . . ? C36 C37 H37B 109.1 . . ? H37A C37 H37B 107.9 . . ? N12 C38 C39 111.7(4) . . ? N12 C38 H38A 109.3 . . ? C39 C38 H38A 109.3 . . ? N12 C38 H38B 109.3 . . ? C39 C38 H38B 109.3 . . ? H38A C38 H38B 107.9 . . ? C38 C39 N14 108.3(3) . . ? C38 C39 H39A 110.0 . . ? N14 C39 H39A 110.0 . . ? C38 C39 H39B 110.0 . . ? N14 C39 H39B 110.0 . . ? H39A C39 H39B 108.4 . . ? N13 C40 C41 109.0(3) . . ? N13 C40 H40A 109.9 . . ? C41 C40 H40A 109.9 . . ? N13 C40 H40B 109.9 . . ? C41 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? N14 C41 C40 110.9(3) . . ? N14 C41 H41A 109.5 . . ? C40 C41 H41A 109.5 . . ? N14 C41 H41B 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? C43 C42 O3 106.1(3) . . ? C43 C42 H42A 110.5 . . ? O3 C42 H42A 110.5 . . ? C43 C42 H42B 110.5 . . ? O3 C42 H42B 110.5 . . ? H42A C42 H42B 108.7 . . ? C42 C43 N14 111.1(3) . . ? C42 C43 H43A 109.4 . . ? N14 C43 H43A 109.4 . . ? C42 C43 H43B 109.4 . . ? N14 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? C45 C44 N10 111.0(4) . . ? C45 C44 H44A 109.4 . . ? N10 C44 H44A 109.4 . . ? C45 C44 H44B 109.4 . . ? N10 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? C50 C45 C44 124.2(6) . . ? C50 C45 C46 116.4(5) . . ? C44 C45 C46 119.2(6) . . ? C47 C46 C45 122.3(5) . . ? C47 C46 H46 118.8 . . ? C45 C46 H46 118.8 . . ? C46 C47 C48 118.7(5) . . ? C46 C47 H47 120.7 . . ? C48 C47 H47 120.7 . . ? C49 C48 C47 118.5(5) . . ? C49 C48 C51 127.1(6) . . ? C47 C48 C51 114.1(5) . . ? C48 C49 C50 120.8(6) . . ? C48 C49 H49 119.6 . . ? C50 C49 H49 119.6 . . ? C45 C50 C49 122.9(6) . . ? C45 C50 H50 118.6 . . ? C49 C50 H50 118.6 . . ? C48 C51 N12 115.8(4) . . ? C48 C51 H51A 108.3 . . ? N12 C51 H51A 108.3 . . ? C48 C51 H51B 108.3 . . ? N12 C51 H51B 108.3 . . ? H51A C51 H51B 107.4 . . ? N13 C52 C53 112.7(3) . . ? N13 C52 H52A 109.0 . . ? C53 C52 H52A 109.0 . . ? N13 C52 H52B 109.0 . . ? C53 C52 H52B 109.0 . . ? H52A C52 H52B 107.8 . . ? C54 C53 C58 116.4(4) . . ? C54 C53 C52 123.3(4) . . ? C58 C53 C52 120.3(4) . . ? C53 C54 C55 120.2(4) . . ? C53 C54 H54 119.9 . . ? C55 C54 H54 119.9 . . ? C56 C55 C54 124.3(4) . . ? C56 C55 H55 117.9 . . ? C54 C55 H55 117.9 . . ? C57 C56 C55 117.2(4) . . ? C57 C56 C59 121.1(4) . . ? C55 C56 C59 121.6(4) . . ? C56 C57 C58 119.6(4) . . ? C56 C57 H57 120.2 . . ? C58 C57 H57 120.2 . . ? C53 C58 C57 121.9(4) . . ? C53 C58 H58 119.1 . . ? C57 C58 H58 119.1 . . ? N9 C59 C56 111.4(3) . . ? N9 C59 H59A 109.4 . . ? C56 C59 H59A 109.4 . . ? N9 C59 H59B 109.4 . . ? C56 C59 H59B 109.4 . . ? H59A C59 H59B 108.0 . . ? N15 C60 N16 119.7(4) . . ? N15 C60 H60 120.1 . . ? N16 C60 H60 120.1 . . ? C62 C61 N15 109.2(4) . . ? C62 C61 H61 125.4 . . ? N15 C61 H61 125.4 . . ? C61 C62 N16 110.1(4) . . ? C61 C62 H62 125.0 . . ? N16 C62 H62 125.0 . . ? O7 Cl1 O6 108.7(3) . . ? O7 Cl1 O5 111.7(3) . . ? O6 Cl1 O5 109.9(3) . . ? O7 Cl1 O8 108.8(3) . . ? O6 Cl1 O8 108.4(3) . . ? O5 Cl1 O8 109.3(3) . . ? O11 Cl2 O10 107.1(4) . . ? O11 Cl2 O12 112.2(4) . . ? O10 Cl2 O12 105.5(4) . . ? O11 Cl2 O9 111.1(5) . . ? O10 Cl2 O9 109.9(4) . . ? O12 Cl2 O9 110.8(4) . . ? O16 Cl3 O13 105.3(4) . . ? O16 Cl3 O14 107.6(4) . . ? O13 Cl3 O14 108.8(4) . . ? O16 Cl3 O15 109.4(4) . . ? O13 Cl3 O15 115.4(4) . . ? O14 Cl3 O15 110.0(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H1 O1 1.02(5) 1.45(5) 2.403(3) 152(4) . _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.916 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.073 # END OF CIF OF COMPLEX 2 ##########################################################################