data_12acsf01 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H46 Cl6 Cu6 N14 O42, 2(Cl O4), 10(H2 O)' _chemical_formula_sum 'C28 H66 Cl8 Cu6 N14 O60' _chemical_formula_weight 2223.79 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' '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' '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7330(3) _cell_length_b 13.2580(3) _cell_length_c 15.4740(5) _cell_angle_alpha 67.589(2) _cell_angle_beta 76.747(2) _cell_angle_gamma 71.487(2) _cell_volume 1915.52(9) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.928 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1122 _exptl_absorpt_coefficient_mu 2.041 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7494 _exptl_absorpt_correction_T_max 0.8703 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1000' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13807 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 27.52 _reflns_number_total 8744 _reflns_number_gt 5543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software (Bruker, 2010)' _computing_cell_refinement 'APEX2 Software (Bruker, 2010)' _computing_data_reduction 'APEX2 Software (Bruker, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.2156P)^2^+0.2020P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0040(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8744 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1333 _refine_ls_R_factor_gt 0.0940 _refine_ls_wR_factor_ref 0.3329 _refine_ls_wR_factor_gt 0.2984 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.002 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 0.92017(9) 0.14786(7) 0.00820(7) 0.0400(3) Uani 1 1 d . . . Cu2 Cu 0.55822(9) 0.30508(7) -0.23185(7) 0.0405(3) Uani 1 1 d . . . Cu3 Cu 1.13345(9) 0.11599(7) 0.30121(6) 0.0409(3) Uani 1 1 d . . . Cl1 Cl 1.1251(3) 0.2138(2) -0.23735(19) 0.0662(7) Uani 1 1 d . . . Cl2 Cl 0.3442(2) 0.2556(2) -0.01169(17) 0.0656(6) Uani 1 1 d . . . Cl3 Cl 0.7831(2) 0.1552(2) 0.38780(17) 0.0714(8) Uani 1 1 d . . . O1 O 0.7353(8) 0.1118(7) 0.1294(6) 0.080(2) Uani 1 1 d . . . O2 O 0.5536(5) 0.1607(5) -0.2403(4) 0.0522(14) Uani 1 1 d . . . O3 O 0.4132(7) 0.3855(5) -0.3136(5) 0.0637(17) Uani 1 1 d . . . O4 O 0.7154(10) 0.3270(9) -0.3650(6) 0.096(3) Uani 1 1 d . . . O5 O 1.1867(6) 0.1246(5) 0.4126(4) 0.0560(15) Uani 1 1 d . . . O6 O 1.3484(7) 0.1010(7) 0.2376(5) 0.075(2) Uani 1 1 d . . . O7 O 1.1713(6) -0.0505(5) 0.3647(4) 0.0466(13) Uani 1 1 d . . . O11 O 1.1305(10) 0.1746(10) -0.1379(6) 0.107(3) Uani 1 1 d . . . O12 O 0.9934(9) 0.2709(9) -0.2611(8) 0.103(3) Uani 1 1 d . . . O13 O 1.2038(10) 0.2939(11) -0.2853(8) 0.120(4) Uani 1 1 d . . . O14 O 1.1652(17) 0.1213(9) -0.2680(8) 0.148(5) Uani 1 1 d . . . O17 O 0.8049(6) 0.2864(4) -0.0602(4) 0.0481(14) Uani 1 1 d . . . O21 O 0.3589(8) 0.2807(8) -0.1104(5) 0.078(2) Uani 1 1 d . . . O22 O 0.2875(15) 0.1594(12) 0.0332(8) 0.156(6) Uani 1 1 d . . . O23 O 0.2646(11) 0.3489(11) 0.0156(9) 0.130(4) Uani 1 1 d . . . O24 O 0.4728(8) 0.2228(8) 0.0190(6) 0.083(2) Uani 1 1 d . . . O27 O 0.9507(6) 0.2441(4) 0.0662(4) 0.0505(14) Uani 1 1 d . . . O31 O 0.9139(7) 0.1109(7) 0.4115(5) 0.079(2) Uani 1 1 d . . . O32 O 0.7676(12) 0.2703(9) 0.3399(10) 0.149(6) Uani 1 1 d . . . O33 O 0.7595(16) 0.1056(17) 0.3276(11) 0.184(7) Uani 1 1 d . . . O34 O 0.6937(8) 0.1395(11) 0.4725(7) 0.133(5) Uani 1 1 d . . . N1 N 0.8806(6) 0.0779(5) -0.0701(4) 0.0355(13) Uani 1 1 d . . . N2 N 1.0525(6) 0.0255(5) 0.0823(4) 0.0356(13) Uani 1 1 d . . . N3 N 0.8067(6) 0.0657(5) -0.1853(4) 0.0339(12) Uani 1 1 d . . . H3 H 0.7487 0.0883 -0.2269 0.041 Uiso 1 1 d R . . N11 N 0.5404(7) 0.4376(5) -0.1952(5) 0.0445(15) Uani 1 1 d . . . N18 N 0.7096(5) 0.2373(5) -0.1522(4) 0.0318(12) Uani 1 1 d . . . N21 N 1.0651(7) 0.2812(5) 0.2451(5) 0.0455(15) Uani 1 1 d . . . N28 N 1.0718(5) 0.1159(5) 0.1863(4) 0.0350(12) Uani 1 1 d . . . C12 C 0.4515(10) 0.5340(8) -0.2168(8) 0.068(3) Uani 1 1 d . . . H12 H 0.3937 0.5475 -0.2587 0.081 Uiso 1 1 d R . . C13 C 0.4407(13) 0.6162(8) -0.1810(10) 0.088(4) Uani 1 1 d . . . H13 H 0.3698 0.6800 -0.1915 0.106 Uiso 1 1 d R . . C14 C 0.5372(13) 0.6024(8) -0.1285(9) 0.082(4) Uani 1 1 d . . . H14 H 0.5385 0.6608 -0.1097 0.099 Uiso 1 1 d R . . C15 C 0.6314(10) 0.5010(7) -0.1044(7) 0.058(2) Uani 1 1 d . . . H15 H 0.6944 0.4875 -0.0662 0.070 Uiso 1 1 d R . . C16 C 0.6284(8) 0.4203(6) -0.1389(6) 0.0426(17) Uani 1 1 d . . . C17 C 0.7246(7) 0.3055(6) -0.1140(5) 0.0362(15) Uani 1 1 d . . . C19 C 0.7960(7) 0.1323(5) -0.1342(5) 0.0322(14) Uani 1 1 d . . . C22 C 1.0696(11) 0.3598(8) 0.2757(7) 0.068(3) Uani 1 1 d . . . H22 H 1.1103 0.3386 0.3292 0.082 Uiso 1 1 d R . . C23 C 1.0163(13) 0.4737(8) 0.2296(9) 0.081(3) Uani 1 1 d . . . H23 H 1.0266 0.5275 0.2502 0.097 Uiso 1 1 d R . . C24 C 0.9496(11) 0.5061(8) 0.1570(8) 0.066(3) Uani 1 1 d . . . H24 H 0.9106 0.5820 0.1278 0.079 Uiso 1 1 d R . . C25 C 0.9399(9) 0.4216(7) 0.1244(6) 0.052(2) Uani 1 1 d . . . H25 H 0.8935 0.4409 0.0741 0.062 Uiso 1 1 d R . . C26 C 1.0001(8) 0.3118(6) 0.1698(5) 0.0406(16) Uani 1 1 d . . . C27 C 1.0052(7) 0.2191(6) 0.1354(5) 0.0358(15) Uani 1 1 d . . . C29 C 1.1011(4) 0.0309(3) 0.1520(3) 0.0294(13) Uani 1 1 d . . . Cl4 Cl 0.2843(4) 0.3735(3) 0.4437(3) 0.154(2) Uani 1 1 d R . . O41 O 0.2240(4) 0.4728(3) 0.3696(3) 0.184 Uiso 1 1 d R . . O42 O 0.3026(4) 0.4308(3) 0.4978(3) 0.184 Uiso 1 1 d R . . O43 O 0.2145(4) 0.2903(3) 0.4865(3) 0.184 Uiso 1 1 d R . . O44 O 0.4229(4) 0.3134(3) 0.4204(3) 0.184 Uiso 1 1 d R . . O51 O 0.0268(9) 0.1549(8) 0.5718(6) 0.090(2) Uiso 1 1 d . . . O52 O 0.4158(10) 0.0296(9) 0.8987(8) 0.108 Uiso 1 1 d . . . O53 O 0.4580(11) 0.1441(9) 0.6215(8) 0.108 Uiso 1 1 d . . . O54 O 0.6044(11) 0.4122(9) 0.4558(8) 0.108 Uiso 1 1 d . . . O55 O 0.4540(10) 0.0880(9) 0.3940(8) 0.108 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 0.0452(5) 0.0324(5) 0.0476(6) -0.0165(4) -0.0277(4) 0.0026(4) Cu2 0.0396(5) 0.0370(5) 0.0463(6) -0.0123(4) -0.0211(4) -0.0027(4) Cu3 0.0482(6) 0.0404(5) 0.0363(5) -0.0159(4) -0.0170(4) -0.0022(4) Cl1 0.0650(14) 0.0761(16) 0.0713(16) -0.0337(13) -0.0027(12) -0.0291(12) Cl2 0.0603(13) 0.0867(17) 0.0519(13) -0.0244(12) -0.0046(10) -0.0215(12) Cl3 0.0508(13) 0.0907(18) 0.0503(13) -0.0059(12) -0.0171(10) -0.0026(12) O1 0.067(4) 0.091(5) 0.076(5) -0.036(4) -0.005(4) -0.006(4) O2 0.041(3) 0.057(3) 0.066(4) -0.027(3) -0.022(3) -0.002(3) O3 0.069(4) 0.061(4) 0.067(4) -0.013(3) -0.038(3) -0.014(3) O4 0.112(7) 0.107(6) 0.064(5) -0.021(4) -0.002(5) -0.038(5) O5 0.061(4) 0.065(4) 0.048(3) -0.026(3) -0.019(3) -0.007(3) O6 0.054(4) 0.100(6) 0.067(4) -0.032(4) -0.004(3) -0.014(4) O7 0.057(3) 0.043(3) 0.036(3) -0.014(2) -0.010(2) -0.003(2) O11 0.101(6) 0.184(11) 0.074(6) -0.054(6) -0.013(5) -0.071(7) O12 0.073(5) 0.109(7) 0.112(7) -0.021(6) -0.019(5) -0.015(5) O13 0.105(7) 0.145(9) 0.135(9) -0.038(7) -0.007(6) -0.080(7) O14 0.252(15) 0.086(7) 0.103(8) -0.053(6) -0.064(9) 0.016(8) O17 0.058(3) 0.034(3) 0.061(4) -0.019(2) -0.037(3) 0.001(2) O21 0.086(5) 0.105(6) 0.052(4) -0.023(4) -0.004(4) -0.045(5) O22 0.214(14) 0.186(12) 0.093(8) -0.023(8) 0.038(9) -0.152(12) O23 0.097(7) 0.150(10) 0.149(10) -0.099(9) -0.038(7) 0.038(7) O24 0.070(5) 0.093(6) 0.084(5) -0.028(4) -0.023(4) -0.008(4) O27 0.065(4) 0.035(3) 0.056(3) -0.018(2) -0.037(3) 0.004(2) O31 0.048(4) 0.100(6) 0.068(5) -0.019(4) -0.012(3) 0.003(4) O32 0.105(8) 0.093(7) 0.158(11) 0.034(7) -0.013(7) 0.000(6) O33 0.159(12) 0.30(2) 0.155(13) -0.136(14) -0.055(10) -0.037(13) O34 0.053(5) 0.175(11) 0.086(6) 0.003(6) 0.006(4) 0.015(5) N1 0.041(3) 0.031(3) 0.038(3) -0.016(2) -0.019(3) 0.001(2) N2 0.037(3) 0.033(3) 0.040(3) -0.015(2) -0.017(2) -0.001(2) N3 0.035(3) 0.036(3) 0.035(3) -0.015(2) -0.017(2) -0.001(2) N11 0.046(4) 0.032(3) 0.052(4) -0.011(3) -0.019(3) 0.000(3) N18 0.030(3) 0.031(3) 0.034(3) -0.009(2) -0.013(2) -0.002(2) N21 0.054(4) 0.034(3) 0.054(4) -0.019(3) -0.025(3) 0.000(3) N28 0.030(3) 0.037(3) 0.036(3) -0.014(2) -0.010(2) -0.001(2) C12 0.065(6) 0.048(5) 0.088(7) -0.016(5) -0.049(5) 0.007(4) C13 0.107(9) 0.044(5) 0.124(10) -0.032(6) -0.077(8) 0.015(5) C14 0.121(10) 0.035(4) 0.095(8) -0.024(5) -0.067(7) 0.016(5) C15 0.068(6) 0.040(4) 0.069(6) -0.022(4) -0.036(5) 0.008(4) C16 0.046(4) 0.035(4) 0.047(4) -0.013(3) -0.023(3) 0.001(3) C17 0.037(4) 0.033(3) 0.037(4) -0.008(3) -0.014(3) -0.004(3) C19 0.032(3) 0.034(3) 0.031(3) -0.008(3) -0.011(3) -0.007(3) C22 0.093(7) 0.054(5) 0.072(6) -0.031(5) -0.050(6) 0.004(5) C23 0.116(9) 0.045(5) 0.106(9) -0.038(5) -0.054(7) -0.009(5) C24 0.090(7) 0.041(4) 0.073(6) -0.019(4) -0.036(6) -0.006(5) C25 0.061(5) 0.042(4) 0.057(5) -0.020(4) -0.025(4) -0.001(4) C26 0.046(4) 0.041(4) 0.039(4) -0.015(3) -0.009(3) -0.012(3) C27 0.038(4) 0.034(3) 0.038(4) -0.017(3) -0.012(3) -0.002(3) C29 0.027(3) 0.033(3) 0.028(3) -0.012(3) -0.010(2) -0.002(3) Cl4 0.166(5) 0.142(4) 0.172(5) -0.032(4) -0.053(4) -0.067(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 O17 1.923(5) . y Cu1 O27 1.954(5) . y Cu1 N2 1.957(6) . y Cu1 N1 1.963(6) . y Cu1 O1 2.428(8) . y Cu1 O11 2.809(9) . y Cu2 N11 1.985(7) . y Cu2 O2 1.984(6) . y Cu2 O3 1.995(6) . y Cu2 N18 2.028(5) . y Cu2 O4 2.332(8) . y Cu2 O21 2.519(7) . y Cu3 N21 1.978(6) . y Cu3 O5 1.989(6) . y Cu3 O7 1.991(5) . y Cu3 N28 2.035(6) . y Cu3 O6 2.269(7) . y Cu3 O31 2.577(7) . y Cl1 O14 1.389(10) . ? Cl1 O11 1.433(9) . ? Cl1 O13 1.441(9) . ? Cl1 O12 1.434(10) . ? Cl2 O23 1.415(10) . ? Cl2 O21 1.416(8) . ? Cl2 O24 1.443(8) . ? Cl2 O22 1.450(10) . ? Cl3 O32 1.393(11) . ? Cl3 O31 1.413(7) . ? Cl3 O34 1.423(9) . ? Cl3 O33 1.430(13) . ? O17 C17 1.236(9) . ? O27 C27 1.221(9) . ? N1 C19 1.333(9) . ? N1 N2 1.393(8) 2_755 ? N2 C29 1.335(7) . ? N2 N1 1.393(8) 2_755 ? N3 C29 1.346(7) 2_755 ? N3 C19 1.358(9) . ? N3 H3 0.8995 . ? N11 C12 1.305(11) . ? N11 C16 1.338(10) . ? N18 C17 1.318(9) . ? N18 C19 1.370(8) . ? N21 C22 1.315(11) . ? N21 C26 1.357(10) . ? N28 C29 1.343(7) . ? N28 C27 1.349(9) . ? C12 C13 1.362(15) . ? C12 H12 0.9300 . ? C13 C14 1.386(15) . ? C13 H13 0.9300 . ? C14 C15 1.377(12) . ? C14 H14 0.9300 . ? C15 C16 1.378(12) . ? C15 H15 0.9300 . ? C16 C17 1.506(10) . ? C22 C23 1.390(14) . ? C22 H22 0.9300 . ? C23 C24 1.328(15) . ? C23 H23 0.9300 . ? C24 C25 1.430(12) . ? C24 H24 0.9300 . ? C25 C26 1.364(11) . ? C25 H25 0.9300 . ? C26 C27 1.496(10) . ? C29 N3 1.346(7) 2_755 ? Cl4 O43 1.3991 . ? Cl4 O42 1.4046 . ? Cl4 O41 1.4538 . ? Cl4 O44 1.4826 . ? 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 O17 Cu1 O27 83.0(2) . . y O17 Cu1 N2 169.3(2) . . y O27 Cu1 N2 86.8(2) . . y O17 Cu1 N1 87.0(2) . . y O27 Cu1 N1 169.1(2) . . y N2 Cu1 N1 102.8(2) . . y O17 Cu1 O1 89.0(3) . . y O27 Cu1 O1 89.4(3) . . y N2 Cu1 O1 94.4(3) . . y N1 Cu1 O1 94.9(3) . . y O17 Cu1 O11 92.2(3) . . y O27 Cu1 O11 96.0(3) . . y N2 Cu1 O11 85.3(3) . . y N1 Cu1 O11 79.9(3) . . y O1 Cu1 O11 174.6(3) . . y N11 Cu2 O2 167.2(3) . . y N11 Cu2 O3 93.5(3) . . y O2 Cu2 O3 89.1(2) . . y N11 Cu2 N18 82.0(2) . . y O2 Cu2 N18 95.9(2) . . y O3 Cu2 N18 174.7(2) . . y N11 Cu2 O4 103.3(3) . . y O2 Cu2 O4 89.2(3) . . y O3 Cu2 O4 90.2(3) . . y N18 Cu2 O4 88.1(3) . . y N11 Cu2 O21 83.6(3) . . y O2 Cu2 O21 84.6(3) . . y O3 Cu2 O21 79.5(3) . . y N18 Cu2 O21 102.7(2) . . y O4 Cu2 O21 168.0(3) . . y N21 Cu3 O5 94.3(3) . . y N21 Cu3 O7 170.6(3) . . y O5 Cu3 O7 87.6(2) . . y N21 Cu3 N28 82.7(3) . . y O5 Cu3 N28 176.8(2) . . y O7 Cu3 N28 95.2(2) . . y N21 Cu3 O6 98.6(3) . . y O5 Cu3 O6 86.8(3) . . y O7 Cu3 O6 90.7(3) . . y N28 Cu3 O6 94.8(3) . . y N21 Cu3 O31 88.8(3) . . y O5 Cu3 O31 80.9(3) . . y O7 Cu3 O31 82.4(3) . . y N28 Cu3 O31 97.8(3) . . y O6 Cu3 O31 166.1(3) . . y O14 Cl1 O11 108.8(7) . . ? O14 Cl1 O13 113.0(9) . . ? O11 Cl1 O13 110.0(6) . . ? O14 Cl1 O12 106.2(8) . . ? O11 Cl1 O12 112.3(6) . . ? O13 Cl1 O12 106.4(7) . . ? O23 Cl2 O21 111.9(7) . . ? O23 Cl2 O24 108.9(6) . . ? O21 Cl2 O24 109.5(5) . . ? O23 Cl2 O22 110.8(9) . . ? O21 Cl2 O22 108.2(6) . . ? O24 Cl2 O22 107.4(8) . . ? O32 Cl3 O31 106.6(7) . . ? O32 Cl3 O34 109.1(8) . . ? O31 Cl3 O34 108.5(5) . . ? O32 Cl3 O33 108.6(10) . . ? O31 Cl3 O33 112.1(8) . . ? O34 Cl3 O33 111.7(10) . . ? Cl1 O11 Cu1 128.0(5) . . ? C17 O17 Cu1 131.4(5) . . ? Cl2 O21 Cu2 130.4(5) . . ? C27 O27 Cu1 130.2(5) . . ? Cl3 O31 Cu3 128.7(5) . . ? C19 N1 N2 107.3(5) . 2_755 ? C19 N1 Cu1 123.8(5) . . ? N2 N1 Cu1 128.1(4) 2_755 . ? C29 N2 N1 107.2(5) . 2_755 ? C29 N2 Cu1 124.4(4) . . ? N1 N2 Cu1 128.2(4) 2_755 . ? C29 N3 C19 107.8(5) 2_755 . ? C29 N3 H3 133.3 2_755 . ? C19 N3 H3 118.4 . . ? C12 N11 C16 118.8(8) . . ? C12 N11 Cu2 127.4(7) . . ? C16 N11 Cu2 113.8(5) . . ? C17 N18 C19 117.4(6) . . ? C17 N18 Cu2 114.0(4) . . ? C19 N18 Cu2 128.6(5) . . ? C22 N21 C26 119.0(7) . . ? C22 N21 Cu3 127.6(6) . . ? C26 N21 Cu3 113.2(5) . . ? C29 N28 C27 118.5(6) . . ? C29 N28 Cu3 128.2(4) . . ? C27 N28 Cu3 112.9(5) . . ? N11 C12 C13 122.7(9) . . ? N11 C12 H12 118.6 . . ? C13 C12 H12 118.7 . . ? C12 C13 C14 118.6(9) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.8 . . ? C15 C14 C13 119.1(9) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.5 . . ? C14 C15 C16 117.4(9) . . ? C14 C15 H15 121.3 . . ? C16 C15 H15 121.3 . . ? N11 C16 C15 122.8(7) . . ? N11 C16 C17 115.9(7) . . ? C15 C16 C17 121.3(7) . . ? O17 C17 N18 128.4(6) . . ? O17 C17 C16 117.2(6) . . ? N18 C17 C16 114.4(6) . . ? N1 C19 N3 108.6(6) . . ? N1 C19 N18 130.0(6) . . ? N3 C19 N18 121.4(6) . . ? N21 C22 C23 121.7(9) . . ? N21 C22 H22 119.1 . . ? C23 C22 H22 119.2 . . ? C24 C23 C22 120.6(9) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 118.5(9) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.8 . . ? C26 C25 C24 118.0(8) . . ? C26 C25 H25 121.0 . . ? C24 C25 H25 121.0 . . ? N21 C26 C25 122.1(7) . . ? N21 C26 C27 116.2(6) . . ? C25 C26 C27 121.6(7) . . ? O27 C27 N28 127.7(7) . . ? O27 C27 C26 118.0(6) . . ? N28 C27 C26 114.3(6) . . ? N2 C29 N28 129.2(5) . . ? N2 C29 N3 109.0(4) . 2_755 ? N28 C29 N3 121.9(5) . 2_755 ? O43 Cl4 O42 119.0 . . ? O43 Cl4 O41 116.3 . . ? O42 Cl4 O41 97.0 . . ? O43 Cl4 O44 105.9 . . ? O42 Cl4 O44 100.9 . . ? O41 Cl4 O44 117.2 . . ? 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 O14 Cl1 O11 Cu1 -100.4(10) . . . . ? O13 Cl1 O11 Cu1 135.2(8) . . . . ? O12 Cl1 O11 Cu1 16.9(10) . . . . ? O17 Cu1 O11 Cl1 -40.8(8) . . . . ? O27 Cu1 O11 Cl1 -124.0(8) . . . . ? N2 Cu1 O11 Cl1 149.7(8) . . . . ? N1 Cu1 O11 Cl1 45.8(8) . . . . ? O1 Cu1 O11 Cl1 62(4) . . . . ? O27 Cu1 O17 C17 -171.6(8) . . . . ? N2 Cu1 O17 C17 168.9(12) . . . . ? N1 Cu1 O17 C17 12.9(7) . . . . ? O1 Cu1 O17 C17 -82.1(8) . . . . ? O11 Cu1 O17 C17 92.6(7) . . . . ? O23 Cl2 O21 Cu2 110.1(8) . . . . ? O24 Cl2 O21 Cu2 -10.8(8) . . . . ? O22 Cl2 O21 Cu2 -127.5(9) . . . . ? N11 Cu2 O21 Cl2 -64.9(7) . . . . ? O2 Cu2 O21 Cl2 110.2(7) . . . . ? O3 Cu2 O21 Cl2 -159.7(7) . . . . ? N18 Cu2 O21 Cl2 15.4(7) . . . . ? O4 Cu2 O21 Cl2 169.4(13) . . . . ? O17 Cu1 O27 C27 168.0(8) . . . . ? N2 Cu1 O27 C27 -15.6(7) . . . . ? N1 Cu1 O27 C27 -167.6(11) . . . . ? O1 Cu1 O27 C27 78.9(8) . . . . ? O11 Cu1 O27 C27 -100.5(8) . . . . ? O32 Cl3 O31 Cu3 -58.4(10) . . . . ? O34 Cl3 O31 Cu3 -175.8(8) . . . . ? O33 Cl3 O31 Cu3 60.4(11) . . . . ? N21 Cu3 O31 Cl3 52.6(7) . . . . ? O5 Cu3 O31 Cl3 147.2(7) . . . . ? O7 Cu3 O31 Cl3 -124.1(7) . . . . ? N28 Cu3 O31 Cl3 -29.8(7) . . . . ? O6 Cu3 O31 Cl3 175.2(9) . . . . ? O17 Cu1 N1 C19 -2.9(6) . . . . ? O27 Cu1 N1 C19 -27.2(17) . . . . ? N2 Cu1 N1 C19 -178.5(6) . . . . ? O1 Cu1 N1 C19 85.9(6) . . . . ? O11 Cu1 N1 C19 -95.6(6) . . . . ? O17 Cu1 N1 N2 165.0(6) . . . 2_755 ? O27 Cu1 N1 N2 140.7(12) . . . 2_755 ? N2 Cu1 N1 N2 -10.5(7) . . . 2_755 ? O1 Cu1 N1 N2 -106.2(6) . . . 2_755 ? O11 Cu1 N1 N2 72.3(6) . . . 2_755 ? O17 Cu1 N2 C29 30.6(17) . . . . ? O27 Cu1 N2 C29 11.3(5) . . . . ? N1 Cu1 N2 C29 -174.0(5) . . . . ? O1 Cu1 N2 C29 -77.9(5) . . . . ? O11 Cu1 N2 C29 107.5(5) . . . . ? O17 Cu1 N2 N1 -144.9(12) . . . 2_755 ? O27 Cu1 N2 N1 -164.2(6) . . . 2_755 ? N1 Cu1 N2 N1 10.5(7) . . . 2_755 ? O1 Cu1 N2 N1 106.6(6) . . . 2_755 ? O11 Cu1 N2 N1 -68.0(6) . . . 2_755 ? O2 Cu2 N11 C12 -96.5(13) . . . . ? O3 Cu2 N11 C12 5.1(9) . . . . ? N18 Cu2 N11 C12 -177.8(9) . . . . ? O4 Cu2 N11 C12 96.1(9) . . . . ? O21 Cu2 N11 C12 -74.0(9) . . . . ? O2 Cu2 N11 C16 80.5(13) . . . . ? O3 Cu2 N11 C16 -177.9(6) . . . . ? N18 Cu2 N11 C16 -0.8(6) . . . . ? O4 Cu2 N11 C16 -86.9(6) . . . . ? O21 Cu2 N11 C16 103.1(6) . . . . ? N11 Cu2 N18 C17 1.2(5) . . . . ? O2 Cu2 N18 C17 -166.1(5) . . . . ? O3 Cu2 N18 C17 34(3) . . . . ? O4 Cu2 N18 C17 104.9(5) . . . . ? O21 Cu2 N18 C17 -80.4(5) . . . . ? N11 Cu2 N18 C19 -178.6(6) . . . . ? O2 Cu2 N18 C19 14.2(6) . . . . ? O3 Cu2 N18 C19 -145(3) . . . . ? O4 Cu2 N18 C19 -74.8(6) . . . . ? O21 Cu2 N18 C19 99.9(6) . . . . ? O5 Cu3 N21 C22 4.3(9) . . . . ? O7 Cu3 N21 C22 105.7(17) . . . . ? N28 Cu3 N21 C22 -176.9(9) . . . . ? O6 Cu3 N21 C22 -83.1(9) . . . . ? O31 Cu3 N21 C22 85.1(9) . . . . ? O5 Cu3 N21 C26 -171.4(6) . . . . ? O7 Cu3 N21 C26 -70.0(18) . . . . ? N28 Cu3 N21 C26 7.4(6) . . . . ? O6 Cu3 N21 C26 101.2(6) . . . . ? O31 Cu3 N21 C26 -90.7(6) . . . . ? N21 Cu3 N28 C29 166.0(5) . . . . ? O5 Cu3 N28 C29 -172(4) . . . . ? O7 Cu3 N28 C29 -23.1(5) . . . . ? O6 Cu3 N28 C29 68.0(5) . . . . ? O31 Cu3 N28 C29 -106.2(5) . . . . ? N21 Cu3 N28 C27 -6.5(5) . . . . ? O5 Cu3 N28 C27 15(5) . . . . ? O7 Cu3 N28 C27 164.3(5) . . . . ? O6 Cu3 N28 C27 -104.6(5) . . . . ? O31 Cu3 N28 C27 81.3(5) . . . . ? C16 N11 C12 C13 -3.0(16) . . . . ? Cu2 N11 C12 C13 173.9(10) . . . . ? N11 C12 C13 C14 8(2) . . . . ? C12 C13 C14 C15 -8(2) . . . . ? C13 C14 C15 C16 3.5(19) . . . . ? C12 N11 C16 C15 -1.7(14) . . . . ? Cu2 N11 C16 C15 -179.0(7) . . . . ? C12 N11 C16 C17 177.7(8) . . . . ? Cu2 N11 C16 C17 0.4(9) . . . . ? C14 C15 C16 N11 1.3(15) . . . . ? C14 C15 C16 C17 -178.0(10) . . . . ? Cu1 O17 C17 N18 -12.1(13) . . . . ? Cu1 O17 C17 C16 166.7(5) . . . . ? C19 N18 C17 O17 -2.7(11) . . . . ? Cu2 N18 C17 O17 177.5(7) . . . . ? C19 N18 C17 C16 178.5(6) . . . . ? Cu2 N18 C17 C16 -1.3(8) . . . . ? N11 C16 C17 O17 -178.3(7) . . . . ? C15 C16 C17 O17 1.0(12) . . . . ? N11 C16 C17 N18 0.6(10) . . . . ? C15 C16 C17 N18 180.0(8) . . . . ? N2 N1 C19 N3 0.7(7) 2_755 . . . ? Cu1 N1 C19 N3 170.8(4) . . . . ? N2 N1 C19 N18 -178.8(7) 2_755 . . . ? Cu1 N1 C19 N18 -8.7(10) . . . . ? C29 N3 C19 N1 0.1(7) 2_755 . . . ? C29 N3 C19 N18 179.7(5) 2_755 . . . ? C17 N18 C19 N1 13.5(11) . . . . ? Cu2 N18 C19 N1 -166.8(6) . . . . ? C17 N18 C19 N3 -165.9(6) . . . . ? Cu2 N18 C19 N3 13.8(9) . . . . ? C26 N21 C22 C23 -3.9(17) . . . . ? Cu3 N21 C22 C23 -179.4(9) . . . . ? N21 C22 C23 C24 5(2) . . . . ? C22 C23 C24 C25 -3.2(19) . . . . ? C23 C24 C25 C26 0.0(16) . . . . ? C22 N21 C26 C25 0.4(13) . . . . ? Cu3 N21 C26 C25 176.6(7) . . . . ? C22 N21 C26 C27 176.8(8) . . . . ? Cu3 N21 C26 C27 -7.1(9) . . . . ? C24 C25 C26 N21 1.5(13) . . . . ? C24 C25 C26 C27 -174.6(8) . . . . ? Cu1 O27 C27 N28 7.1(13) . . . . ? Cu1 O27 C27 C26 -173.1(5) . . . . ? C29 N28 C27 O27 10.9(11) . . . . ? Cu3 N28 C27 O27 -175.8(7) . . . . ? C29 N28 C27 C26 -168.9(5) . . . . ? Cu3 N28 C27 C26 4.4(8) . . . . ? N21 C26 C27 O27 -178.1(7) . . . . ? C25 C26 C27 O27 -1.8(12) . . . . ? N21 C26 C27 N28 1.7(10) . . . . ? C25 C26 C27 N28 178.0(7) . . . . ? N1 N2 C29 N28 176.8(5) 2_755 . . . ? Cu1 N2 C29 N28 0.5(8) . . . . ? N1 N2 C29 N3 -1.4(6) 2_755 . . 2_755 ? Cu1 N2 C29 N3 -177.6(4) . . . 2_755 ? C27 N28 C29 N2 -14.7(9) . . . . ? Cu3 N28 C29 N2 173.2(4) . . . . ? C27 N28 C29 N3 163.3(6) . . . 2_755 ? Cu3 N28 C29 N3 -8.9(8) . . . 2_755 ? 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 N3 H3 O2 0.90 2.03 2.785(8) 140.8 . N3 H3 O7 0.90 2.29 2.810(8) 116.7 2_755 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.026 _refine_diff_density_min -1.887 _refine_diff_density_rms 0.238