Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0222 _publ_contact_author_name 'Konstantin V. Domasevitch' _publ_contact_author_address ; Konstantin V. Domasevitch Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; _publ_contact_author_phone ? _publ_contact_author_fax +380(44)296-2467 _publ_contact_author_email dk@univ.kiev.ua _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Metal-Organic Frameworks Incorporating Cu3(mu3-OH) Clusters ; loop_ _publ_author_name _publ_author_address A.B.Lysenko ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; E.V.Govor ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; H.Krautscheid ; Institute of Inorganic Chemistry Leipzig University Linnestrasse 3 D-04103 Leipzig Germany ; K.V.Domasevitch ; Inorganic Chemistry Department Kiev Shevchenko University Volodimirska Str. 64 01033 Kiev Ukraine ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; KVD and HK acknowledge support from Deutsche Forschungsgemeinschaft. ; #============================================================================== data_xtal21d _database_code_depnum_ccdc_archive 'CCDC 600030' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Hexachloro Dihydroxo Tetraaqua mu-3-Hydroxotricopper(II) mu-3-Oxotricopper(II) Complex with 4,4'-(1,2,4-bitriazole), Chloride Semihydrate ; _chemical_name_common ; Hexachloro Dihydroxo Tetraaqua mu-3-Hydroxotricopper(ii) mu-3- Oxotricopper(ii) Complex with 4,4'-(1,2,4-bitriazole), Chloride Semihydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H24 Cl7 Cu6 N18 O8.50' _chemical_formula_weight 1185.88 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 Cubic _symmetry_space_group_name_H-M Fd-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+3/4, z+1/2' '-x+3/4, y+1/2, -z+1/4' 'x+1/2, -y+1/4, -z+3/4' 'z, x, y' 'z+1/2, -x+1/4, -y+3/4' '-z+1/4, -x+3/4, y+1/2' '-z+3/4, x+1/2, -y+1/4' 'y, z, x' '-y+3/4, z+1/2, -x+1/4' 'y+1/2, -z+1/4, -x+3/4' '-y+1/4, -z+3/4, x+1/2' 'y+3/4, x+1/4, -z' '-y+1/2, -x+1/2, -z+1/2' 'y+1/4, -x, z+3/4' '-y, x+3/4, z+1/4' 'x+3/4, z+1/4, -y' '-x, z+3/4, y+1/4' '-x+1/2, -z+1/2, -y+1/2' 'x+1/4, -z, y+3/4' 'z+3/4, y+1/4, -x' 'z+1/4, -y, x+3/4' '-z, y+3/4, x+1/4' '-z+1/2, -y+1/2, -x+1/2' 'x, y+1/2, z+1/2' '-x+1/4, -y+5/4, z+1' '-x+3/4, y+1, -z+3/4' 'x+1/2, -y+3/4, -z+5/4' 'z, x+1/2, y+1/2' 'z+1/2, -x+3/4, -y+5/4' '-z+1/4, -x+5/4, y+1' '-z+3/4, x+1, -y+3/4' 'y, z+1/2, x+1/2' '-y+3/4, z+1, -x+3/4' 'y+1/2, -z+3/4, -x+5/4' '-y+1/4, -z+5/4, x+1' 'y+3/4, x+3/4, -z+1/2' '-y+1/2, -x+1, -z+1' 'y+1/4, -x+1/2, z+5/4' '-y, x+5/4, z+3/4' 'x+3/4, z+3/4, -y+1/2' '-x, z+5/4, y+3/4' '-x+1/2, -z+1, -y+1' 'x+1/4, -z+1/2, y+5/4' 'z+3/4, y+3/4, -x+1/2' 'z+1/4, -y+1/2, x+5/4' '-z, y+5/4, x+3/4' '-z+1/2, -y+1, -x+1' 'x+1/2, y, z+1/2' '-x+3/4, -y+3/4, z+1' '-x+5/4, y+1/2, -z+3/4' 'x+1, -y+1/4, -z+5/4' 'z+1/2, x, y+1/2' 'z+1, -x+1/4, -y+5/4' '-z+3/4, -x+3/4, y+1' '-z+5/4, x+1/2, -y+3/4' 'y+1/2, z, x+1/2' '-y+5/4, z+1/2, -x+3/4' 'y+1, -z+1/4, -x+5/4' '-y+3/4, -z+3/4, x+1' 'y+5/4, x+1/4, -z+1/2' '-y+1, -x+1/2, -z+1' 'y+3/4, -x, z+5/4' '-y+1/2, x+3/4, z+3/4' 'x+5/4, z+1/4, -y+1/2' '-x+1/2, z+3/4, y+3/4' '-x+1, -z+1/2, -y+1' 'x+3/4, -z, y+5/4' 'z+5/4, y+1/4, -x+1/2' 'z+3/4, -y, x+5/4' '-z+1/2, y+3/4, x+3/4' '-z+1, -y+1/2, -x+1' 'x+1/2, y+1/2, z' '-x+3/4, -y+5/4, z+1/2' '-x+5/4, y+1, -z+1/4' 'x+1, -y+3/4, -z+3/4' 'z+1/2, x+1/2, y' 'z+1, -x+3/4, -y+3/4' '-z+3/4, -x+5/4, y+1/2' '-z+5/4, x+1, -y+1/4' 'y+1/2, z+1/2, x' '-y+5/4, z+1, -x+1/4' 'y+1, -z+3/4, -x+3/4' '-y+3/4, -z+5/4, x+1/2' 'y+5/4, x+3/4, -z' '-y+1, -x+1, -z+1/2' 'y+3/4, -x+1/2, z+3/4' '-y+1/2, x+5/4, z+1/4' 'x+5/4, z+3/4, -y' '-x+1/2, z+5/4, y+1/4' '-x+1, -z+1, -y+1/2' 'x+3/4, -z+1/2, y+3/4' 'z+5/4, y+3/4, -x' 'z+3/4, -y+1/2, x+3/4' '-z+1/2, y+5/4, x+1/4' '-z+1, -y+1, -x+1/2' '-x, -y, -z' 'x-1/4, y-3/4, -z-1/2' 'x-3/4, -y-1/2, z-1/4' '-x-1/2, y-1/4, z-3/4' '-z, -x, -y' '-z-1/2, x-1/4, y-3/4' 'z-1/4, x-3/4, -y-1/2' 'z-3/4, -x-1/2, y-1/4' '-y, -z, -x' 'y-3/4, -z-1/2, x-1/4' '-y-1/2, z-1/4, x-3/4' 'y-1/4, z-3/4, -x-1/2' '-y-3/4, -x-1/4, z' 'y-1/2, x-1/2, z-1/2' '-y-1/4, x, -z-3/4' 'y, -x-3/4, -z-1/4' '-x-3/4, -z-1/4, y' 'x, -z-3/4, -y-1/4' 'x-1/2, z-1/2, y-1/2' '-x-1/4, z, -y-3/4' '-z-3/4, -y-1/4, x' '-z-1/4, y, -x-3/4' 'z, -y-3/4, -x-1/4' 'z-1/2, y-1/2, x-1/2' '-x, -y+1/2, -z+1/2' 'x-1/4, y-1/4, -z' 'x-3/4, -y, z+1/4' '-x-1/2, y+1/4, z-1/4' '-z, -x+1/2, -y+1/2' '-z-1/2, x+1/4, y-1/4' 'z-1/4, x-1/4, -y' 'z-3/4, -x, y+1/4' '-y, -z+1/2, -x+1/2' 'y-3/4, -z, x+1/4' '-y-1/2, z+1/4, x-1/4' 'y-1/4, z-1/4, -x' '-y-3/4, -x+1/4, z+1/2' 'y-1/2, x, z' '-y-1/4, x+1/2, -z-1/4' 'y, -x-1/4, -z+1/4' '-x-3/4, -z+1/4, y+1/2' 'x, -z-1/4, -y+1/4' 'x-1/2, z, y' '-x-1/4, z+1/2, -y-1/4' '-z-3/4, -y+1/4, x+1/2' '-z-1/4, y+1/2, -x-1/4' 'z, -y-1/4, -x+1/4' 'z-1/2, y, x' '-x+1/2, -y, -z+1/2' 'x+1/4, y-3/4, -z' 'x-1/4, -y-1/2, z+1/4' '-x, y-1/4, z-1/4' '-z+1/2, -x, -y+1/2' '-z, x-1/4, y-1/4' 'z+1/4, x-3/4, -y' 'z-1/4, -x-1/2, y+1/4' '-y+1/2, -z, -x+1/2' 'y-1/4, -z-1/2, x+1/4' '-y, z-1/4, x-1/4' 'y+1/4, z-3/4, -x' '-y-1/4, -x-1/4, z+1/2' 'y, x-1/2, z' '-y+1/4, x, -z-1/4' 'y+1/2, -x-3/4, -z+1/4' '-x-1/4, -z-1/4, y+1/2' 'x+1/2, -z-3/4, -y+1/4' 'x, z-1/2, y' '-x+1/4, z, -y-1/4' '-z-1/4, -y-1/4, x+1/2' '-z+1/4, y, -x-1/4' 'z+1/2, -y-3/4, -x+1/4' 'z, y-1/2, x' '-x+1/2, -y+1/2, -z' 'x+1/4, y-1/4, -z-1/2' 'x-1/4, -y, z-1/4' '-x, y+1/4, z-3/4' '-z+1/2, -x+1/2, -y' '-z, x+1/4, y-3/4' 'z+1/4, x-1/4, -y-1/2' 'z-1/4, -x, y-1/4' '-y+1/2, -z+1/2, -x' 'y-1/4, -z, x-1/4' '-y, z+1/4, x-3/4' 'y+1/4, z-1/4, -x-1/2' '-y-1/4, -x+1/4, z' 'y, x, z-1/2' '-y+1/4, x+1/2, -z-3/4' 'y+1/2, -x-1/4, -z-1/4' '-x-1/4, -z+1/4, y' 'x+1/2, -z-1/4, -y-1/4' 'x, z, y-1/2' '-x+1/4, z+1/2, -y-3/4' '-z-1/4, -y+1/4, x' '-z+1/4, y+1/2, -x-3/4' 'z+1/2, -y-1/4, -x-1/4' 'z, y, x-1/2' _cell_length_a 30.0968(12) _cell_length_b 30.0968(12) _cell_length_c 30.0968(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 27262.2(19) _cell_formula_units_Z 32 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8263 _cell_measurement_theta_min 4.31 _cell_measurement_theta_max 25.89 _exptl_crystal_description octahedron _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 18656 _exptl_absorpt_coefficient_mu 4.297 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6110 _exptl_absorpt_correction_T_max 0.8840 _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Stoe IPDS' _diffrn_measurement_method 'phi oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8263 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 4.31 _diffrn_reflns_theta_max 25.89 _reflns_number_total 1078 _reflns_number_gt 932 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie GmbH, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie GmbH, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie GmbH, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1006P)^2^+365.3029P] 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 none _refine_ls_number_reflns 1078 _refine_ls_number_parameters 81 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1472 _refine_ls_wR_factor_gt 0.1440 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.04574(2) 0.57552(2) 0.48487(2) 0.0219(3) Uani 1 1 d . . . Cl1 Cl 0.05580(4) 0.62062(5) 0.42425(4) 0.0235(4) Uani 1 1 d . . . O1 O 0.02604(15) 0.52604(15) 0.52604(15) 0.0255(14) Uani 1 3 d S . . H1 H 0.0097 0.5097 0.5097 0.038 Uiso 0.50 3 d SPR . . O2 O 0.08033(18) 0.61644(19) 0.53458(19) 0.0435(12) Uani 1 1 d . . . H2 H 0.0741 0.6437 0.5304 0.065 Uiso 1 1 d R . . H3 H 0.1082 0.6133 0.5315 0.065 Uiso 0.50 1 d PR . . N1 N -0.01167(14) 0.60654(15) 0.49803(15) 0.0184(10) Uani 1 1 d . . . N2 N -0.03384(14) 0.59649(14) 0.53712(14) 0.0149(9) Uani 1 1 d . . . N3 N -0.06653(13) 0.65205(13) 0.50507(13) 0.0117(8) Uani 1 1 d . . . C1 C -0.03123(18) 0.64021(18) 0.47940(17) 0.0192(11) Uani 1 1 d . . . H1A H -0.0224 0.6543 0.4522 0.023 Uiso 1 1 d R . . C2 C -0.06732(17) 0.62410(17) 0.54077(17) 0.0155(10) Uani 1 1 d . . . H2A H -0.0887 0.6245 0.5644 0.019 Uiso 1 1 d R . . Cl2 Cl 0.03794(12) 0.71206(12) 0.53794(12) 0.0385(12) Uani 0.50 3 d SP . . O3 O 0.0000 0.7500 0.5000 0.062(10) Uani 0.50 6 d SP . . 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 0.0218(4) 0.0221(4) 0.0217(4) 0.0075(3) 0.0076(3) 0.0087(3) Cl1 0.0247(7) 0.0253(7) 0.0205(7) 0.0058(5) 0.0052(5) 0.0086(5) O1 0.0255(14) 0.0255(14) 0.0255(14) 0.0037(17) 0.0037(17) 0.0037(17) O2 0.039(3) 0.047(3) 0.045(3) -0.008(2) -0.001(2) -0.002(2) N1 0.016(2) 0.023(2) 0.017(2) 0.0099(18) 0.0070(17) 0.0090(17) N2 0.015(2) 0.017(2) 0.0122(19) 0.0075(16) 0.0055(16) 0.0071(17) N3 0.0113(19) 0.011(2) 0.0132(19) 0.0035(15) -0.0006(15) 0.0039(15) C1 0.020(3) 0.021(2) 0.017(2) 0.0071(19) 0.006(2) 0.009(2) C2 0.015(2) 0.018(2) 0.013(2) 0.0066(19) 0.0030(19) 0.0053(19) Cl2 0.0385(12) 0.0385(12) 0.0385(12) -0.0018(14) 0.0018(14) -0.0018(14) O3 0.062(10) 0.062(10) 0.062(10) -0.052(12) 0.052(12) -0.052(12) _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 N2 1.996(4) 57_455 ? Cu1 N1 2.004(4) . ? Cu1 O1 2.0261(19) . ? Cu1 O2 2.200(5) . ? Cu1 Cl1 2.2941(14) . ? O1 Cu1 2.0261(19) 57_455 ? O1 Cu1 2.0261(19) 77_455 ? O1 H1 0.8500 . ? O2 H2 0.8500 . ? O2 H3 0.8500 . ? N1 C1 1.299(7) . ? N1 N2 1.386(6) . ? N2 C2 1.311(6) . ? N2 Cu1 1.996(4) 77_455 ? N3 C1 1.361(7) . ? N3 C2 1.365(6) . ? N3 N3 1.372(8) 85_356 ? C1 H1A 0.9600 . ? C2 H2A 0.9600 . ? 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 N2 Cu1 N1 170.2(2) 57_455 . ? N2 Cu1 O1 88.33(12) 57_455 . ? N1 Cu1 O1 88.23(13) . . ? N2 Cu1 O2 98.9(2) 57_455 . ? N1 Cu1 O2 90.7(2) . . ? O1 Cu1 O2 97.7(3) . . ? N2 Cu1 Cl1 90.99(12) 57_455 . ? N1 Cu1 Cl1 89.73(13) . . ? O1 Cu1 Cl1 163.7(2) . . ? O2 Cu1 Cl1 98.47(17) . . ? Cu1 O1 Cu1 114.42(16) 57_455 . ? Cu1 O1 Cu1 114.42(16) 57_455 77_455 ? Cu1 O1 Cu1 114.42(16) . 77_455 ? Cu1 O1 H1 103.9 57_455 . ? Cu1 O1 H1 103.9 . . ? Cu1 O1 H1 103.9 77_455 . ? Cu1 O2 H2 109.5 . . ? Cu1 O2 H3 109.4 . . ? H2 O2 H3 108.1 . . ? C1 N1 N2 108.6(4) . . ? C1 N1 Cu1 132.0(4) . . ? N2 N1 Cu1 118.8(3) . . ? C2 N2 N1 107.6(4) . . ? C2 N2 Cu1 130.8(3) . 77_455 ? N1 N2 Cu1 121.5(3) . 77_455 ? C1 N3 C2 107.4(4) . . ? C1 N3 N3 126.3(5) . 85_356 ? C2 N3 N3 126.0(4) . 85_356 ? N1 C1 N3 108.2(4) . . ? N1 C1 H1A 126.0 . . ? N3 C1 H1A 125.8 . . ? N2 C2 N3 108.1(4) . . ? N2 C2 H2A 125.9 . . ? N3 C2 H2A 125.9 . . ? 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 N2 Cu1 O1 Cu1 25.5(3) 57_455 . . 57_455 ? N1 Cu1 O1 Cu1 -163.8(3) . . . 57_455 ? O2 Cu1 O1 Cu1 -73.3(3) . . . 57_455 ? Cl1 Cu1 O1 Cu1 113.3(3) . . . 57_455 ? N2 Cu1 O1 Cu1 160.3(3) 57_455 . . 77_455 ? N1 Cu1 O1 Cu1 -28.9(3) . . . 77_455 ? O2 Cu1 O1 Cu1 61.6(3) . . . 77_455 ? Cl1 Cu1 O1 Cu1 -111.9(4) . . . 77_455 ? N2 Cu1 N1 C1 -97.9(11) 57_455 . . . ? O1 Cu1 N1 C1 -167.5(6) . . . . ? O2 Cu1 N1 C1 94.9(6) . . . . ? Cl1 Cu1 N1 C1 -3.6(5) . . . . ? N2 Cu1 N1 N2 92.7(11) 57_455 . . . ? O1 Cu1 N1 N2 23.1(4) . . . . ? O2 Cu1 N1 N2 -74.6(4) . . . . ? Cl1 Cu1 N1 N2 -173.0(4) . . . . ? C1 N1 N2 C2 1.3(6) . . . . ? Cu1 N1 N2 C2 173.0(4) . . . . ? C1 N1 N2 Cu1 178.7(4) . . . 77_455 ? Cu1 N1 N2 Cu1 -9.6(6) . . . 77_455 ? N2 N1 C1 N3 -1.2(6) . . . . ? Cu1 N1 C1 N3 -171.4(4) . . . . ? C2 N3 C1 N1 0.6(6) . . . . ? N3 N3 C1 N1 -173.8(4) 85_356 . . . ? N1 N2 C2 N3 -0.9(6) . . . . ? Cu1 N2 C2 N3 -177.9(4) 77_455 . . . ? C1 N3 C2 N2 0.2(6) . . . . ? N3 N3 C2 N2 174.7(4) 85_356 . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.89 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.366 _refine_diff_density_min -0.893 _refine_diff_density_rms 0.154 #============================================================================== data_xtal28s _database_code_depnum_ccdc_archive 'CCDC 600031' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[mu-3-hydroxotricopper(II)] heptakis[4,4'-bi(1,2,4-triazole)] Decabromide Hexahydrate ; _chemical_name_common ; Bis(mu-3-hydroxotricopper(ii)) heptakis(4,4'-bi(1,2,4- triazole)) Decabromide Hexahydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H42 Br10 Cu6 N42 O8' _chemical_formula_weight 2275.38 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 11.9996(11) _cell_length_b 21.0665(17) _cell_length_c 15.6477(17) _cell_angle_alpha 90.00 _cell_angle_beta 109.555(11) _cell_angle_gamma 90.00 _cell_volume 3727.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 7.110 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.4010 _exptl_absorpt_correction_T_max 0.4804 _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Stoe IPDS' _diffrn_measurement_method 'phi oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11860 _diffrn_reflns_av_R_equivalents 0.0697 _diffrn_reflns_av_sigmaI/netI 0.1117 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.24 _diffrn_reflns_theta_max 26.73 _reflns_number_total 3893 _reflns_number_gt 2208 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie GmbH, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie GmbH, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie GmbH, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Solvate water molecules (three equivalents per one mu-3-hydroxotricopper fragment) and part of non-coordinated bromide ions (0.5 equivalent per mu-3-hydroxotricopper fragment) are disordered and this electron density was modelled using SQUEEZE. ; _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^)+(0.0583P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00046(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3893 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1125 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 0.817 _refine_ls_restrained_S_all 0.817 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.24235(7) 0.08181(3) 0.16413(6) 0.0289(2) Uani 1 1 d . . . Cu2 Cu 0.00936(8) 0.0000 0.17987(6) 0.0163(2) Uani 1 2 d S . . Br1 Br -0.33108(13) 0.10828(5) -0.01287(6) 0.0860(6) Uani 0.877(3) 1 d P . . Br1A Br -0.2722(9) 0.1780(4) -0.0751(6) 0.082(4) Uani 0.123(3) 1 d P . . Br2 Br 0.0000 0.0000 0.0000 0.0431(4) Uani 1 4 d S . . Br3 Br -0.60026(7) 0.16880(3) 0.29950(6) 0.0539(3) Uani 1 1 d . . . O1 O -0.1704(5) 0.0000 0.1361(3) 0.0188(11) Uani 1 2 d S . . H1B H -0.1898 0.0000 0.0786 0.023 Uiso 1 2 d SR . . N1 N -0.3714(4) 0.03314(19) 0.1889(3) 0.0208(10) Uani 1 1 d . . . N2 N -0.5238(6) 0.0000 0.2188(4) 0.0214(14) Uani 1 2 d S . . N3 N -0.0895(4) 0.1283(2) 0.1830(4) 0.0310(12) Uani 1 1 d . . . N4 N 0.0105(4) 0.0954(2) 0.1859(3) 0.0238(10) Uani 1 1 d . . . N5 N 0.0518(5) 0.1948(2) 0.2067(4) 0.0381(14) Uani 1 1 d . . . N6 N -0.3055(5) 0.1611(2) 0.2045(4) 0.0382(14) Uani 1 1 d . . . N7 N -0.2731(5) 0.1720(2) 0.2970(5) 0.0452(16) Uani 1 1 d . . . N8 N -0.3837(5) 0.2489(2) 0.2247(5) 0.0395(15) Uani 1 1 d . . . N9 N 0.1884(6) 0.0000 0.2224(4) 0.0219(15) Uani 1 2 d S . . N10 N 0.2493(6) 0.0000 0.3151(5) 0.0301(17) Uani 1 2 d S . . N11 N 0.3724(6) 0.0000 0.2397(5) 0.0217(14) Uani 1 2 d S . . N12 N -0.0218(7) 0.0000 0.3161(5) 0.0377(19) Uani 1 2 d S . . N13 N -0.1189(8) 0.0447(4) 0.3135(6) 0.022(2) Uani 0.50 1 d P . . N14 N -0.0168(8) 0.0255(4) 0.4535(6) 0.0213(19) Uani 0.50 1 d P . . C1 C -0.4642(5) 0.0521(3) 0.2070(4) 0.0257(13) Uani 1 1 d . . . H1A H -0.4858 0.0941 0.2112 0.031 Uiso 1 1 d R . . C2 C -0.0630(6) 0.1879(3) 0.1962(6) 0.0433(18) Uani 1 1 d . . . H2A H -0.1147 0.2203 0.1982 0.052 Uiso 1 1 d R . . C3 C 0.0965(6) 0.1363(3) 0.2001(5) 0.0334(15) Uani 1 1 d . . . H3A H 0.1742 0.1272 0.2048 0.040 Uiso 1 1 d R . . C4 C -0.3207(7) 0.2250(3) 0.3069(6) 0.0471(19) Uani 1 1 d . . . H4A H -0.3133 0.2440 0.3622 0.056 Uiso 1 1 d R . . C5 C -0.3715(6) 0.2076(3) 0.1628(5) 0.0380(16) Uani 1 1 d . . . H5A H -0.4051 0.2119 0.1002 0.046 Uiso 1 1 d R . . C6 C 0.3610(8) 0.0000 0.3231(6) 0.033(2) Uani 1 2 d S . . H6A H 0.4235 0.0000 0.3778 0.040 Uiso 1 2 d SR . . C7 C 0.2617(7) 0.0000 0.1766(5) 0.0203(16) Uani 1 2 d S . . H7A H 0.2425 0.0000 0.1139 0.024 Uiso 1 2 d SR . . C8 C -0.1153(11) 0.0557(5) 0.3964(7) 0.022(2) Uani 0.50 1 d P . . C9 C 0.0409(8) 0.0000 0.4026(5) 0.030(2) Uani 1 2 d S . . 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 0.0219(4) 0.0177(3) 0.0501(5) -0.0078(3) 0.0160(4) -0.0027(3) Cu2 0.0141(5) 0.0163(4) 0.0171(5) 0.000 0.0035(4) 0.000 Br1 0.1350(12) 0.0661(7) 0.0284(6) 0.0013(5) -0.0103(6) 0.0408(7) Br1A 0.092(7) 0.081(6) 0.069(6) 0.020(4) 0.023(5) -0.021(5) Br2 0.0318(8) 0.0844(11) 0.0145(7) 0.000 0.0095(6) 0.000 Br3 0.0464(5) 0.0411(4) 0.0827(6) -0.0129(4) 0.0329(4) -0.0040(3) O1 0.020(3) 0.025(3) 0.009(3) 0.000 0.002(2) 0.000 N1 0.022(3) 0.016(2) 0.024(3) -0.0053(18) 0.008(2) -0.0005(18) N2 0.016(3) 0.025(3) 0.026(4) 0.000 0.012(3) 0.000 N3 0.022(3) 0.022(2) 0.050(3) -0.004(2) 0.012(3) 0.0013(19) N4 0.021(3) 0.023(2) 0.029(3) 0.000(2) 0.010(2) -0.0002(18) N5 0.027(3) 0.017(2) 0.072(4) -0.008(2) 0.019(3) -0.003(2) N6 0.021(3) 0.024(2) 0.069(4) -0.003(3) 0.014(3) -0.002(2) N7 0.043(4) 0.025(3) 0.074(5) 0.002(3) 0.028(3) 0.004(2) N8 0.030(3) 0.014(2) 0.077(5) 0.002(3) 0.023(3) 0.005(2) N9 0.024(4) 0.022(3) 0.017(3) 0.000 0.003(3) 0.000 N10 0.022(4) 0.052(4) 0.013(4) 0.000 0.001(3) 0.000 N11 0.015(3) 0.024(3) 0.027(4) 0.000 0.008(3) 0.000 N12 0.028(4) 0.071(5) 0.015(4) 0.000 0.007(3) 0.000 N13 0.019(5) 0.028(5) 0.017(5) 0.005(4) 0.003(4) 0.010(4) N14 0.018(5) 0.037(5) 0.013 0.003(3) 0.010(3) 0.012(4) C1 0.020(3) 0.025(3) 0.035(3) 0.004(3) 0.013(3) -0.002(2) C2 0.026(4) 0.024(3) 0.081(6) -0.005(3) 0.020(4) 0.000(3) C3 0.028(3) 0.022(3) 0.052(4) -0.007(3) 0.014(3) -0.002(2) C4 0.046(5) 0.026(3) 0.071(6) 0.005(3) 0.022(4) 0.007(3) C5 0.026(3) 0.022(3) 0.067(5) 0.007(3) 0.017(3) 0.004(2) C6 0.026(5) 0.053(5) 0.016(4) 0.000 0.001(4) 0.000 C7 0.022(4) 0.031(4) 0.010(4) 0.000 0.008(3) 0.000 C8 0.031(7) 0.028(6) 0.009(5) -0.001(4) 0.011(5) -0.003(5) C9 0.032(5) 0.044(5) 0.009(4) 0.000 0.002(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.000(5) . ? Cu1 N3 2.012(5) . ? Cu1 N6 2.021(5) . ? Cu1 O1 2.040(3) . ? Cu1 N13 2.440(9) . ? Cu1 Br1 2.6724(13) . ? Cu2 N4 2.012(4) . ? Cu2 N4 2.012(4) 6 ? Cu2 N9 2.025(7) . ? Cu2 O1 2.033(5) . ? Cu2 N12 2.284(7) . ? Cu2 Br2 2.7790(10) . ? Br2 Cu2 2.7790(10) 5 ? O1 Cu1 2.040(3) 6 ? N1 C1 1.301(7) . ? N1 N1 1.396(8) 6 ? N2 C1 1.355(6) 6 ? N2 C1 1.355(6) . ? N2 N11 1.390(9) 1_455 ? N3 C2 1.294(7) . ? N3 N4 1.374(7) . ? N4 C3 1.305(7) . ? N5 C2 1.339(8) . ? N5 C3 1.361(7) . ? N5 N8 1.394(7) 8 ? N6 C5 1.292(8) . ? N6 N7 1.386(8) . ? N7 C4 1.287(8) . ? N8 C5 1.345(9) . ? N8 C4 1.352(10) . ? N8 N5 1.394(6) 8_455 ? N9 C7 1.308(10) . ? N9 N10 1.388(9) . ? N10 C6 1.303(12) . ? N11 C6 1.357(11) . ? N11 C7 1.364(10) . ? N11 N2 1.390(9) 1_655 ? N12 C9 1.310(10) . ? N12 N13 1.488(10) 6 ? N12 N13 1.488(10) . ? N13 C8 1.304(13) . ? N13 N13 1.882(18) 6 ? N14 N14 1.074(17) 6 ? N14 C9 1.331(12) . ? N14 N14 1.374(17) 2_556 ? N14 C8 1.376(14) . ? N14 N14 1.744(17) 5_556 ? C9 N14 1.331(12) 6 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N3 161.4(2) . . ? N1 Cu1 N6 88.12(19) . . ? N3 Cu1 N6 88.3(2) . . ? N1 Cu1 O1 91.12(18) . . ? N3 Cu1 O1 90.70(18) . . ? N6 Cu1 O1 174.5(2) . . ? N1 Cu1 N13 84.9(3) . . ? N3 Cu1 N13 77.5(3) . . ? N6 Cu1 N13 97.8(3) . . ? O1 Cu1 N13 76.7(3) . . ? N1 Cu1 Br1 104.02(14) . . ? N3 Cu1 Br1 94.46(16) . . ? N6 Cu1 Br1 95.20(18) . . ? O1 Cu1 Br1 90.23(14) . . ? N13 Cu1 Br1 164.4(2) . . ? N4 Cu2 N4 174.8(3) . 6 ? N4 Cu2 N9 89.68(14) . . ? N4 Cu2 N9 89.68(14) 6 . ? N4 Cu2 O1 90.34(14) . . ? N4 Cu2 O1 90.34(14) 6 . ? N9 Cu2 O1 179.5(2) . . ? N4 Cu2 N12 87.52(14) . . ? N4 Cu2 N12 87.52(14) 6 . ? N9 Cu2 N12 100.4(3) . . ? O1 Cu2 N12 80.1(2) . . ? N4 Cu2 Br2 92.58(14) . . ? N4 Cu2 Br2 92.58(14) 6 . ? N9 Cu2 Br2 90.68(19) . . ? O1 Cu2 Br2 88.86(15) . . ? N12 Cu2 Br2 169.0(2) . . ? Cu2 Br2 Cu2 180.00(4) . 5 ? Cu2 O1 Cu1 113.91(15) . 6 ? Cu2 O1 Cu1 113.91(15) . . ? Cu1 O1 Cu1 115.3(3) 6 . ? C1 N1 N1 107.8(3) . 6 ? C1 N1 Cu1 131.3(4) . . ? N1 N1 Cu1 120.83(12) 6 . ? C1 N2 C1 108.1(7) 6 . ? C1 N2 N11 126.0(3) 6 1_455 ? C1 N2 N11 126.0(3) . 1_455 ? C2 N3 N4 108.6(5) . . ? C2 N3 Cu1 131.2(4) . . ? N4 N3 Cu1 120.2(3) . . ? C3 N4 N3 107.7(4) . . ? C3 N4 Cu2 131.4(4) . . ? N3 N4 Cu2 120.7(3) . . ? C2 N5 C3 107.9(5) . . ? C2 N5 N8 126.6(5) . 8 ? C3 N5 N8 125.4(5) . 8 ? C5 N6 N7 108.2(6) . . ? C5 N6 Cu1 134.4(6) . . ? N7 N6 Cu1 117.4(4) . . ? C4 N7 N6 106.8(6) . . ? C5 N8 C4 106.6(5) . . ? C5 N8 N5 126.2(6) . 8_455 ? C4 N8 N5 127.2(6) . 8_455 ? C7 N9 N10 110.9(7) . . ? C7 N9 Cu2 130.8(5) . . ? N10 N9 Cu2 118.3(5) . . ? C6 N10 N9 105.4(7) . . ? C6 N11 C7 108.0(7) . . ? C6 N11 N2 127.8(7) . 1_655 ? C7 N11 N2 124.2(7) . 1_655 ? C9 N12 N13 101.6(6) . 6 ? C9 N12 N13 101.6(6) . . ? N13 N12 N13 78.5(8) 6 . ? C9 N12 Cu2 138.4(7) . . ? N13 N12 Cu2 110.3(5) 6 . ? N13 N12 Cu2 110.3(5) . . ? C8 N13 N12 108.7(8) . . ? C8 N13 N13 100.2(6) . 6 ? N12 N13 N13 50.8(4) . 6 ? C8 N13 Cu1 134.6(7) . . ? N12 N13 Cu1 116.6(6) . . ? N13 N13 Cu1 108.7(2) 6 . ? N14 N14 C9 66.2(4) 6 . ? N14 N14 N14 90.000(2) 6 2_556 ? C9 N14 N14 127.3(10) . 2_556 ? N14 N14 C8 117.5(6) 6 . ? C9 N14 C8 107.7(8) . . ? N14 N14 C8 124.9(10) 2_556 . ? N14 N14 N14 52.0(6) 6 5_556 ? C9 N14 N14 103.3(8) . 5_556 ? N14 N14 N14 38.0(6) 2_556 5_556 ? C8 N14 N14 137.3(11) . 5_556 ? N1 C1 N2 108.1(5) . . ? N3 C2 N5 108.2(5) . . ? N4 C3 N5 107.5(6) . . ? N7 C4 N8 109.7(7) . . ? N6 C5 N8 108.8(7) . . ? N10 C6 N11 109.8(7) . . ? N9 C7 N11 105.9(7) . . ? N13 C8 N14 107.4(10) . . ? N12 C9 N14 112.6(8) . . ? N12 C9 N14 112.6(8) . 6 ? N14 C9 N14 47.6(8) . 6 ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.005 _refine_diff_density_min -1.280 _refine_diff_density_rms 0.132 #============================================================================== data_xtal33d _database_code_depnum_ccdc_archive 'CCDC 600032' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[mu-3-hydroxotricopper(II)] heptakis[4,4'-bi(1,2,4-triazole)] Decahloride Octahydrate ; _chemical_name_common ; Bis(mu-3-hydroxotricopper(ii)) heptakis(4,4'-bi(1,2,4- triazole)) Decahloride Octahydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H46 Cl10 Cu6 N42 O10' _chemical_formula_weight 1866.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 21.3590(19) _cell_length_b 12.0195(8) _cell_length_c 28.954(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.896(10) _cell_angle_gamma 90.00 _cell_volume 7362.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 12531 _cell_measurement_theta_min 5.24 _cell_measurement_theta_max 26.73 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3728 _exptl_absorpt_coefficient_mu 2.138 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_absorpt_correction_T_min 0.6812 _exptl_absorpt_correction_T_max 0.8106 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Stoe IPDS' _diffrn_measurement_method 'phi oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17532 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 5.24 _diffrn_reflns_theta_max 26.73 _reflns_number_total 12531 _reflns_number_gt 9855 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie GmbH, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie GmbH, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie GmbH, 2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0870P)^2^+144.3722P] 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 0.0043(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(2) _refine_ls_number_reflns 12531 _refine_ls_number_parameters 846 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0845 _refine_ls_R_factor_gt 0.0757 _refine_ls_wR_factor_ref 0.2019 _refine_ls_wR_factor_gt 0.1985 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.48910(7) -0.50958(9) -0.04398(5) 0.0163(3) Uani 1 1 d . . . Cu2 Cu -0.40429(6) -0.26484(10) -0.03215(5) 0.0186(3) Uani 1 1 d . . . Cu3 Cu -0.57379(6) -0.26591(10) -0.04738(5) 0.0153(3) Uani 1 1 d . . . Cu4 Cu -0.63888(6) -0.43489(10) -0.36781(5) 0.0148(3) Uani 1 1 d . . . Cu5 Cu -0.55772(7) -0.18877(10) -0.37636(5) 0.0174(3) Uani 1 1 d . . . Cu6 Cu -0.47465(6) -0.43236(10) -0.37968(5) 0.0176(3) Uani 1 1 d . . . Cl1 Cl -0.45263(18) -0.5794(3) 0.04044(10) 0.0334(7) Uani 1 1 d . . . Cl2 Cl -0.3781(2) -0.2253(3) 0.04799(12) 0.0407(8) Uani 1 1 d . . . Cl3 Cl -0.5851(2) -0.2218(3) 0.02790(12) 0.0416(9) Uani 1 1 d . . . Cl4 Cl -0.68521(18) -0.4865(3) -0.44026(11) 0.0362(8) Uani 1 1 d . . . Cl5 Cl -0.5693(3) -0.1301(3) -0.46135(12) 0.0515(11) Uani 1 1 d . . . Cl6 Cl -0.3803(2) 0.1537(3) -0.31700(16) 0.0459(9) Uani 1 1 d . . . Cl7A Cl -0.3252(2) -0.8482(4) -0.0644(3) 0.0408(15) Uani 0.65 1 d P . . Cl7B Cl -0.3345(9) -0.8521(14) -0.0995(7) 0.033(3) Uiso 0.20 1 d P . . Cl7C Cl -0.2758(12) -0.7650(18) -0.0335(8) 0.035(5) Uiso 0.15 1 d P . . Cl8A Cl -0.7222(4) 0.1522(7) -0.3545(5) 0.0378(19) Uani 0.45 1 d P . . Cl8B Cl -0.7164(8) 0.1466(12) -0.3324(9) 0.039(4) Uiso 0.30 1 d P . . Cl8C Cl -0.7122(8) 0.1466(11) -0.3079(7) 0.036(3) Uiso 0.25 1 d P . . Cl9A Cl -0.4917(7) -0.0385(8) -0.1796(3) 0.084(3) Uani 0.65 1 d P . . Cl9B Cl -0.542(2) -0.022(3) -0.1863(12) 0.122(9) Uiso 0.35 1 d P . . Cl10 Cl -0.6671(2) 0.1594(4) -0.1015(2) 0.0598(12) Uani 1 1 d . . . O1 O -0.4794(5) -0.3528(6) -0.0225(3) 0.0235(19) Uani 1 1 d . . . H1 H -0.4779 -0.3566 0.0069 0.035 Uiso 1 1 d R . . O2 O -0.5535(4) -0.3457(6) -0.3944(3) 0.0189(16) Uani 1 1 d . . . H2 H -0.5618 -0.3463 -0.4240 0.028 Uiso 1 1 d R . . N1 N -0.5840(5) -0.5113(8) -0.0398(4) 0.021(2) Uani 1 1 d . . . N2 N -0.6186(5) -0.4123(7) -0.0430(3) 0.0151(18) Uani 1 1 d . . . N3 N -0.6847(5) -0.5432(8) -0.0496(4) 0.0242(18) Uani 1 1 d . . . N4 N -0.8259(6) -0.6689(9) -0.0986(4) 0.029(2) Uani 1 1 d . . . N5 N -0.8310(5) -0.6799(9) -0.0502(4) 0.025(2) Uani 1 1 d . . . N6 N -0.7429(5) -0.6026(8) -0.0577(4) 0.025(2) Uani 1 1 d . . . N7 N -0.3995(5) -0.5049(7) -0.0584(3) 0.0151(19) Uani 1 1 d . . . N8 N -0.3679(5) -0.4031(8) -0.0598(4) 0.024(2) Uani 1 1 d . . . N9 N -0.3078(5) -0.5379(8) -0.0759(4) 0.0258(19) Uani 1 1 d . . . N10 N -0.1655(6) -0.6823(9) -0.0796(5) 0.034(3) Uani 1 1 d . . . N11 N -0.1878(7) -0.6691(13) -0.1256(5) 0.047(3) Uani 1 1 d . . . N12 N -0.2529(5) -0.5918(8) -0.0878(4) 0.029(2) Uani 1 1 d . . . N13 N -0.4619(5) -0.1251(7) -0.0553(4) 0.0182(17) Uani 1 1 d . . . N14 N -0.5268(5) -0.1243(8) -0.0538(3) 0.019(2) Uani 1 1 d . . . N15 N -0.4957(5) 0.0430(8) -0.0676(3) 0.022(2) Uani 1 1 d . . . N16 N -0.4959(5) 0.3341(7) -0.0667(4) 0.019(2) Uani 1 1 d . . . N17 N -0.5042(6) 0.3103(8) -0.1150(4) 0.029(3) Uani 1 1 d . . . N18 N -0.4967(5) 0.1547(7) -0.0764(3) 0.0165(19) Uani 1 1 d . . . N19 N -0.6881(5) -0.2917(8) -0.3705(4) 0.022(2) Uani 1 1 d . . . N20 N -0.6559(5) -0.1918(8) -0.3742(3) 0.0177(19) Uani 1 1 d . . . N21 N -0.7515(6) -0.1552(8) -0.3624(4) 0.027(2) Uani 1 1 d . . . N22 N -0.8737(6) -0.0304(10) -0.3131(4) 0.032(3) Uani 1 1 d . . . N23 N -0.8935(5) -0.0173(7) -0.3601(4) 0.021(2) Uani 1 1 d . . . N24 N -0.8042(5) -0.1009(8) -0.3535(4) 0.0225(18) Uani 1 1 d . . . N25 N -0.5859(5) -0.5764(8) -0.3621(4) 0.022(2) Uani 1 1 d . . . N26 N -0.5226(5) -0.5757(8) -0.3681(4) 0.024(2) Uani 1 1 d . . . N27 N -0.5506(5) -0.7421(7) -0.3546(4) 0.021(2) Uani 1 1 d . . . N28 N -0.5462(7) -1.0123(9) -0.3070(4) 0.035(3) Uani 1 1 d . . . N29 N -0.5559(5) -1.0299(8) -0.3543(4) 0.020(2) Uani 1 1 d . . . N30 N -0.5507(5) -0.8541(7) -0.3443(4) 0.021(2) Uani 1 1 d . . . N31 N -0.4288(5) -0.2899(8) -0.3567(4) 0.021(2) Uani 1 1 d . . . N32 N -0.4620(5) -0.1913(7) -0.3589(3) 0.0166(19) Uani 1 1 d . . . N33 N -0.3618(5) -0.1611(8) -0.3383(4) 0.023(2) Uani 1 1 d . . . N34 N -0.2207(7) -0.0379(14) -0.2855(5) 0.049(4) Uani 1 1 d . . . N35 N -0.2174(6) -0.0249(8) -0.3332(4) 0.028(2) Uani 1 1 d . . . N36 N -0.3063(6) -0.1064(8) -0.3250(4) 0.026(2) Uani 1 1 d . . . N37 N -0.5199(6) -0.4180(9) -0.1147(4) 0.027(2) Uani 1 1 d . . . N38 N -0.5538(5) -0.3211(7) -0.1129(3) 0.019(2) Uani 1 1 d . . . N39 N -0.5508(6) -0.3558(8) -0.1844(3) 0.024(2) Uani 1 1 d . . . N40 N -0.5930(5) -0.3783(7) -0.3052(3) 0.019(2) Uani 1 1 d . . . N41 N -0.5580(6) -0.2808(9) -0.3022(4) 0.032(3) Uani 1 1 d . . . N42 N -0.5599(6) -0.3458(9) -0.2327(3) 0.027(2) Uani 1 1 d . . . C1 C -0.6266(7) -0.5930(11) -0.0443(5) 0.033(3) Uani 1 1 d . . . H1A H -0.6183 -0.6698 -0.0439 0.039 Uiso 1 1 calc R . . C2 C -0.6770(6) -0.4344(10) -0.0490(5) 0.025(3) Uani 1 1 d . . . H2A H -0.7097 -0.3816 -0.0526 0.030 Uiso 1 1 calc R . . C3 C -0.7732(7) -0.6208(11) -0.1010(5) 0.031(3) Uani 1 1 d . . . H3A H -0.7578 -0.6010 -0.1287 0.037 Uiso 1 1 calc R . . C4 C -0.7805(6) -0.6384(10) -0.0272(4) 0.022(3) Uani 1 1 d . . . H4A H -0.7715 -0.6338 0.0054 0.027 Uiso 1 1 calc R . . C5 C -0.3615(7) -0.5839(11) -0.0676(5) 0.031(3) Uani 1 1 d . . . H5A H -0.3706 -0.6604 -0.0683 0.037 Uiso 1 1 calc R . . C6 C -0.3116(7) -0.4236(10) -0.0707(5) 0.029(3) Uani 1 1 d . . . H6A H -0.2800 -0.3712 -0.0743 0.035 Uiso 1 1 calc R . . C7 C -0.2390(13) -0.614(3) -0.1295(9) 0.081(8) Uani 1 1 d . . . H7A H -0.2632 -0.5932 -0.1577 0.097 Uiso 1 1 calc R . . C8 C -0.2071(7) -0.6320(11) -0.0569(6) 0.033(3) Uani 1 1 d . . . H8A H -0.2046 -0.6258 -0.0243 0.039 Uiso 1 1 calc R . . C9 C -0.4444(7) -0.0240(10) -0.0634(5) 0.028(3) Uani 1 1 d . . . H9A H -0.4029 -0.0014 -0.0659 0.034 Uiso 1 1 calc R . . C10 C -0.5453(6) -0.0231(8) -0.0626(4) 0.019(2) Uani 1 1 d . . . H10A H -0.5875 0.0010 -0.0652 0.023 Uiso 1 1 calc R . . C11 C -0.5056(8) 0.2040(11) -0.1200(5) 0.034(3) Uani 1 1 d . . . H11A H -0.5117 0.1659 -0.1486 0.041 Uiso 1 1 calc R . . C12 C -0.4897(6) 0.2406(8) -0.0444(5) 0.020(2) Uani 1 1 d . . . H12A H -0.4817 0.2325 -0.0118 0.024 Uiso 1 1 calc R . . C13 C -0.7450(6) -0.2701(9) -0.3657(4) 0.022(3) Uani 1 1 d . . . H13A H -0.7773 -0.3227 -0.3645 0.026 Uiso 1 1 calc R . . C14 C -0.6945(6) -0.1098(10) -0.3677(5) 0.023(3) Uani 1 1 d . . . H14A H -0.6845 -0.0336 -0.3668 0.028 Uiso 1 1 calc R . . C15 C -0.8193(8) -0.0828(11) -0.3087(5) 0.036(3) Uani 1 1 d . . . H15A H -0.7950 -0.1042 -0.2805 0.043 Uiso 1 1 calc R . . C16 C -0.8515(6) -0.0562(9) -0.3834(5) 0.026(3) Uani 1 1 d . . . H16A H -0.8534 -0.0539 -0.4160 0.032 Uiso 1 1 calc R . . C17 C -0.6012(7) -0.6745(10) -0.3541(6) 0.030(3) Uani 1 1 d . . . H17A H -0.6416 -0.6976 -0.3485 0.036 Uiso 1 1 calc R . . C18 C -0.5020(7) -0.6752(10) -0.3626(6) 0.032(3) Uani 1 1 d . . . H18A H -0.4602 -0.6983 -0.3638 0.038 Uiso 1 1 calc R . . C19 C -0.5417(9) -0.9012(11) -0.3025(5) 0.038(4) Uani 1 1 d . . . H19A H -0.5333 -0.8628 -0.2740 0.045 Uiso 1 1 calc R . . C20 C -0.5630(10) -0.9354(9) -0.3772(6) 0.040(4) Uani 1 1 d . . . H20A H -0.5743 -0.9258 -0.4095 0.048 Uiso 1 1 calc R . . C21 C -0.3699(8) -0.2699(11) -0.3427(5) 0.035(3) Uani 1 1 d . . . H21A H -0.3379 -0.3238 -0.3367 0.042 Uiso 1 1 calc R . . C22 C -0.4200(6) -0.1127(9) -0.3488(5) 0.023(3) Uani 1 1 d . . . H22A H -0.4285 -0.0360 -0.3487 0.028 Uiso 1 1 calc R . . C23 C -0.2760(9) -0.0856(16) -0.2819(7) 0.050(4) Uani 1 1 d . . . H23A H -0.2914 -0.1022 -0.2538 0.060 Uiso 1 1 calc R . . C24 C -0.2673(7) -0.0680(10) -0.3553(5) 0.030(3) Uani 1 1 d . . . H24A H -0.2761 -0.0727 -0.3879 0.036 Uiso 1 1 calc R . . C25 C -0.5185(7) -0.4362(11) -0.1599(4) 0.029(3) Uani 1 1 d . . . H25A H -0.4981 -0.4960 -0.1725 0.034 Uiso 1 1 calc R . . C26 C -0.5725(6) -0.2842(10) -0.1545(4) 0.025(3) Uani 1 1 d . . . H26A H -0.5966 -0.2198 -0.1624 0.029 Uiso 1 1 calc R . . C27 C -0.5948(7) -0.4121(10) -0.2620(4) 0.027(3) Uani 1 1 d . . . H27A H -0.6175 -0.4740 -0.2534 0.033 Uiso 1 1 calc R . . C28 C -0.5394(8) -0.2615(12) -0.2583(5) 0.038(3) Uani 1 1 d . . . H28A H -0.5157 -0.1996 -0.2462 0.045 Uiso 1 1 calc R . . O3 O -0.6783(10) -0.488(2) -0.1630(7) 0.104(7) Uani 1 1 d . . . O4 O -0.4387(11) -0.0210(19) -0.4550(8) 0.103(6) Uiso 1 1 d . . . O5 O -0.5365(11) 0.3333(17) -0.2444(8) 0.094(5) Uiso 1 1 d . . . O6 O -0.1918(15) -0.681(2) -0.2529(11) 0.131(8) Uiso 1 1 d . . . O7 O -0.4169(16) 0.287(3) -0.2286(12) 0.138(9) Uiso 1 1 d . . . O8 O -0.3531(18) -0.183(3) -0.4458(13) 0.152(10) Uiso 1 1 d . . . O9 O -0.7687(17) -0.342(3) -0.2163(12) 0.146(10) Uiso 1 1 d . . . O10 O -0.6429(14) -0.699(2) -0.1943(10) 0.124(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 0.0125(7) 0.0134(5) 0.0232(6) -0.0015(5) 0.0034(5) -0.0007(5) Cu2 0.0122(7) 0.0155(6) 0.0283(7) -0.0023(5) 0.0031(6) -0.0031(5) Cu3 0.0148(7) 0.0119(6) 0.0195(6) -0.0025(5) 0.0034(6) -0.0021(5) Cu4 0.0113(7) 0.0139(6) 0.0180(6) -0.0018(5) -0.0021(5) 0.0031(5) Cu5 0.0116(7) 0.0134(5) 0.0270(7) -0.0017(5) 0.0023(6) 0.0008(5) Cu6 0.0095(7) 0.0148(6) 0.0280(7) 0.0002(5) 0.0001(6) 0.0033(5) Cl1 0.036(2) 0.0433(17) 0.0196(13) 0.0033(11) 0.0007(14) -0.0081(14) Cl2 0.051(2) 0.0394(17) 0.0286(16) 0.0003(13) -0.0057(16) -0.0079(16) Cl3 0.058(3) 0.0366(17) 0.0336(16) -0.0133(13) 0.0170(17) -0.0106(16) Cl4 0.035(2) 0.0476(18) 0.0229(14) -0.0107(13) -0.0078(14) 0.0052(15) Cl5 0.089(4) 0.0401(19) 0.0284(16) 0.0076(14) 0.018(2) 0.015(2) Cl6 0.040(2) 0.0324(17) 0.065(2) -0.0034(16) 0.009(2) 0.0011(15) Cl7A 0.010(2) 0.0130(19) 0.097(5) 0.002(2) 0.000(3) -0.0008(16) Cl8A 0.026(5) 0.037(4) 0.050(6) -0.009(4) 0.007(4) -0.005(3) Cl9A 0.132(11) 0.066(5) 0.055(4) -0.029(4) 0.014(5) -0.010(5) Cl10 0.034(2) 0.050(2) 0.094(4) 0.007(2) 0.005(2) 0.0024(18) O1 0.046(6) 0.016(3) 0.012(3) -0.004(3) 0.014(4) -0.003(3) O2 0.022(5) 0.022(4) 0.014(3) 0.006(3) 0.008(3) 0.003(3) N1 0.015(5) 0.016(4) 0.034(5) -0.005(4) 0.011(5) -0.002(4) N2 0.015(5) 0.007(4) 0.023(4) -0.008(3) 0.001(4) -0.002(3) N3 0.023 0.024(4) 0.028(5) 0.004(4) 0.011(4) -0.007(4) N4 0.026(6) 0.023(5) 0.038(6) -0.002(4) 0.005(5) -0.004(4) N5 0.009(5) 0.027(5) 0.038(6) -0.006(4) -0.001(5) -0.003(4) N6 0.011(5) 0.025(5) 0.040(6) -0.006(4) 0.010(5) -0.011(4) N7 0.011(5) 0.015(4) 0.021(4) 0.002(3) 0.006(4) 0.004(3) N8 0.016(5) 0.023(5) 0.036(6) 0.009(4) 0.015(5) 0.011(4) N9 0.021 0.020(4) 0.036(5) 0.003(4) 0.006(5) 0.011(4) N10 0.018(6) 0.025(5) 0.062(8) -0.020(5) 0.012(6) 0.009(4) N11 0.034(8) 0.065(8) 0.043(7) 0.004(6) 0.009(6) 0.032(7) N12 0.016(6) 0.022(5) 0.051(7) 0.007(4) 0.015(6) 0.007(4) N13 0.014 0.012(4) 0.032(5) 0.000(4) 0.014(4) 0.009(3) N14 0.010(5) 0.026(5) 0.022(5) -0.001(4) 0.005(4) -0.004(4) N15 0.019(6) 0.026(5) 0.020(5) 0.002(4) -0.004(4) -0.001(4) N16 0.014(5) 0.016(4) 0.027(5) 0.005(4) 0.002(4) -0.008(4) N17 0.041(7) 0.016(4) 0.032(5) -0.008(4) 0.003(5) -0.006(4) N18 0.012(5) 0.013(4) 0.026(5) 0.001(3) 0.010(4) -0.002(3) N19 0.019(6) 0.020(5) 0.028(5) -0.002(4) 0.002(5) 0.001(4) N20 0.002(4) 0.026(5) 0.025(5) 0.003(4) 0.000(4) 0.001(3) N21 0.025(6) 0.015(4) 0.041(6) 0.000(4) 0.004(5) -0.010(4) N22 0.017(6) 0.038(6) 0.041(6) 0.007(5) 0.001(5) 0.014(5) N23 0.018(5) 0.011(4) 0.033(5) -0.004(4) 0.004(4) -0.007(4) N24 0.019 0.018(4) 0.035(5) -0.004(4) 0.021(4) -0.004(4) N25 0.017(5) 0.015(4) 0.032(5) -0.001(4) 0.003(5) -0.003(4) N26 0.019(6) 0.015(4) 0.040(6) 0.006(4) 0.012(5) 0.000(4) N27 0.023(6) 0.007(4) 0.033(5) 0.005(3) 0.002(5) 0.002(4) N28 0.051(8) 0.019(5) 0.037(6) 0.004(4) 0.014(6) 0.006(5) N29 0.013(5) 0.017(4) 0.031(5) 0.005(4) 0.007(4) 0.002(4) N30 0.018(5) 0.013(4) 0.033(5) -0.002(4) 0.004(5) 0.003(4) N31 0.008(5) 0.021(4) 0.036(5) -0.014(4) 0.008(5) 0.001(4) N32 0.014(5) 0.012(4) 0.025(5) 0.002(3) 0.007(4) 0.002(3) N33 0.010(5) 0.022(5) 0.039(6) -0.002(4) 0.011(5) -0.009(4) N34 0.029(7) 0.082(10) 0.033(6) -0.003(6) -0.006(6) -0.025(7) N35 0.021(6) 0.019(5) 0.046(6) -0.004(4) 0.010(5) -0.003(4) N36 0.025(6) 0.019(4) 0.033(5) 0.001(4) 0.005(5) -0.002(4) N37 0.025(6) 0.036(6) 0.017(4) -0.001(4) -0.002(5) 0.014(5) N38 0.020(5) 0.015(4) 0.025(5) -0.010(3) 0.014(4) -0.004(4) N39 0.031(6) 0.030(5) 0.009(4) 0.004(4) -0.002(4) 0.008(4) N40 0.013(5) 0.020(4) 0.024(5) -0.002(4) -0.001(4) 0.003(4) N41 0.042(8) 0.030(5) 0.021(5) 0.006(4) -0.005(5) -0.007(5) N42 0.027(6) 0.040(6) 0.013(4) 0.009(4) -0.007(4) -0.016(5) C1 0.031(8) 0.030(6) 0.041(7) -0.010(5) 0.019(7) 0.003(6) C2 0.014(6) 0.027(6) 0.034(6) -0.010(5) 0.004(5) 0.005(5) C3 0.029(8) 0.037(7) 0.025(6) 0.004(5) 0.001(6) -0.010(6) C4 0.016(6) 0.030(6) 0.022(5) -0.015(5) 0.007(5) -0.015(5) C5 0.035(8) 0.025(6) 0.033(7) -0.013(5) 0.008(6) -0.004(5) C6 0.018(7) 0.025(6) 0.046(7) 0.000(5) 0.010(6) -0.001(5) C7 0.060(14) 0.12(2) 0.063(13) 0.004(13) 0.019(12) 0.045(14) C8 0.018(7) 0.031(7) 0.053(8) -0.005(6) 0.019(7) 0.002(5) C9 0.019(7) 0.019(5) 0.049(8) 0.009(5) 0.013(6) 0.007(5) C10 0.022(7) 0.013(5) 0.022(5) -0.003(4) -0.002(5) 0.001(4) C11 0.045(9) 0.034(7) 0.020(6) -0.005(5) -0.009(6) 0.001(6) C12 0.015(5) 0.017 0.028(5) 0.017(5) 0.003(5) 0.008(5) C13 0.021(6) 0.013(5) 0.036(6) 0.009(4) 0.019(6) 0.004(4) C14 0.012(6) 0.023(6) 0.035(6) 0.001(5) 0.001(6) 0.001(4) C15 0.034(8) 0.032(7) 0.042(8) -0.003(5) 0.008(7) 0.006(6) C16 0.007(6) 0.017(5) 0.058(8) 0.019(5) 0.013(6) 0.008(4) C17 0.016(7) 0.016(5) 0.058(8) -0.010(5) 0.002(6) 0.005(5) C18 0.019(7) 0.020(6) 0.059(9) 0.004(6) 0.015(7) 0.006(5) C19 0.061(11) 0.023(6) 0.031(7) 0.004(5) 0.009(7) -0.006(6) C20 0.081(12) 0.008(4) 0.035(6) -0.008(5) 0.022(7) 0.003(6) C21 0.031(8) 0.023(6) 0.048(8) 0.005(5) -0.001(7) 0.005(5) C22 0.017(6) 0.014(5) 0.038(6) -0.004(4) 0.000(6) -0.009(4) C23 0.033(9) 0.063(10) 0.054(10) 0.005(8) 0.010(8) -0.008(8) C24 0.027(8) 0.024(6) 0.042(7) -0.009(5) 0.015(7) -0.001(5) C25 0.038(8) 0.037(6) 0.010(5) -0.010(4) 0.000(5) 0.014(6) C26 0.025(7) 0.025(5) 0.022(5) 0.001(4) 0.001(5) 0.009(5) C27 0.036(8) 0.027(6) 0.019(5) -0.003(4) 0.006(6) 0.004(5) C28 0.042(9) 0.039(7) 0.028(7) -0.002(5) -0.008(7) -0.013(6) O3 0.077(13) 0.149(18) 0.090(12) 0.023(12) 0.029(11) -0.042(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.986(7) . ? Cu1 N16 1.990(9) 1_545 ? Cu1 N7 2.014(10) . ? Cu1 N1 2.047(10) . ? Cu1 N37 2.339(10) . ? Cu1 Cl1 2.601(3) . ? Cu2 O1 1.973(9) . ? Cu2 N5 1.998(11) 3 ? Cu2 N8 2.044(10) . ? Cu2 N13 2.135(9) . ? Cu2 Cl2 2.359(4) . ? Cu3 N14 1.997(10) . ? Cu3 N2 2.015(9) . ? Cu3 N38 2.109(9) . ? Cu3 N10 2.283(13) 3_455 ? Cu3 Cl3 2.288(3) . ? Cu3 O1 2.296(10) . ? Cu4 N19 2.012(10) . ? Cu4 N25 2.037(10) . ? Cu4 N40 2.055(10) . ? Cu4 Cl4 2.279(3) . ? Cu4 O2 2.334(8) . ? Cu4 N35 2.335(11) 3_445 ? Cu5 O2 1.963(8) . ? Cu5 N29 2.012(10) 1_565 ? Cu5 N32 2.038(11) . ? Cu5 N20 2.108(10) . ? Cu5 N41 2.416(10) . ? Cu5 Cl5 2.539(4) . ? Cu6 O2 1.977(8) . ? Cu6 N23 2.025(11) 3_545 ? Cu6 N31 2.039(10) . ? Cu6 N26 2.056(10) . ? Cu6 Cl1 2.427(3) 2_544 ? Cl1 Cu6 2.427(3) 2_545 ? O1 H1 0.8500 . ? O2 H2 0.8500 . ? N1 C1 1.333(18) . ? N1 N2 1.397(13) . ? N2 C2 1.264(17) . ? N3 C2 1.318(16) . ? N3 C1 1.367(19) . ? N3 N6 1.425(15) . ? N4 C3 1.276(19) . ? N4 N5 1.425(17) . ? N5 C4 1.289(16) . ? N5 Cu2 1.998(11) 3_445 ? N6 C4 1.343(16) . ? N6 C3 1.346(18) . ? N7 C5 1.300(17) . ? N7 N8 1.400(14) . ? N8 C6 1.309(17) . ? N9 C5 1.324(19) . ? N9 C6 1.385(16) . ? N9 N12 1.423(15) . ? N10 C8 1.323(17) . ? N10 N11 1.36(2) . ? N10 Cu3 2.283(13) 3_545 ? N11 C7 1.27(3) . ? N12 C7 1.31(3) . ? N12 C8 1.32(2) . ? N13 C9 1.301(15) . ? N13 N14 1.393(14) . ? N14 C10 1.293(15) . ? N15 C10 1.348(17) . ? N15 C9 1.352(17) . ? N15 N18 1.366(13) . ? N16 C12 1.294(13) . ? N16 N17 1.414(15) . ? N16 Cu1 1.990(9) 1_565 ? N17 C11 1.286(17) . ? N18 C12 1.382(16) . ? N18 C11 1.382(17) . ? N19 C13 1.270(17) . ? N19 N20 1.395(14) . ? N20 C14 1.314(16) . ? N21 N24 1.357(16) . ? N21 C14 1.363(17) . ? N21 C13 1.392(15) . ? N22 C15 1.312(19) . ? N22 N23 1.378(17) . ? N23 C16 1.281(16) . ? N23 Cu6 2.025(11) 3_455 ? N24 C16 1.348(18) . ? N24 C15 1.396(18) . ? N25 C17 1.254(16) . ? N25 N26 1.386(14) . ? N26 C18 1.277(16) . ? N27 C17 1.353(17) . ? N27 C18 1.358(18) . ? N27 N30 1.379(13) . ? N28 C19 1.343(17) . ? N28 N29 1.373(16) . ? N29 C20 1.313(16) . ? N29 Cu5 2.012(10) 1_545 ? N30 C19 1.327(18) . ? N30 C20 1.365(17) . ? N31 C21 1.290(19) . ? N31 N32 1.378(13) . ? N32 C22 1.307(15) . ? N33 C21 1.323(17) . ? N33 N36 1.364(15) . ? N33 C22 1.369(17) . ? N34 C23 1.33(2) . ? N34 N35 1.401(18) . ? N35 C24 1.28(2) . ? N35 Cu4 2.335(11) 3 ? N36 C23 1.35(2) . ? N36 C24 1.370(18) . ? N37 C25 1.332(15) . ? N37 N38 1.376(14) . ? N38 C26 1.295(16) . ? N39 C25 1.334(17) . ? N39 C26 1.347(16) . ? N39 N42 1.390(13) . ? N40 C27 1.319(16) . ? N40 N41 1.388(15) . ? N41 C28 1.300(18) . ? N42 C27 1.317(18) . ? N42 C28 1.363(18) . ? C1 H1A 0.9400 . ? C2 H2A 0.9400 . ? C3 H3A 0.9400 . ? C4 H4A 0.9400 . ? C5 H5A 0.9400 . ? C6 H6A 0.9400 . ? C7 H7A 0.9400 . ? C8 H8A 0.9400 . ? C9 H9A 0.9400 . ? C10 H10A 0.9400 . ? C11 H11A 0.9400 . ? C12 H12A 0.9400 . ? C13 H13A 0.9400 . ? C14 H14A 0.9400 . ? C15 H15A 0.9400 . ? C16 H16A 0.9400 . ? C17 H17A 0.9400 . ? C18 H18A 0.9400 . ? C19 H19A 0.9400 . ? C20 H20A 0.9400 . ? C21 H21A 0.9400 . ? C22 H22A 0.9400 . ? C23 H23A 0.9400 . ? C24 H24A 0.9400 . ? C25 H25A 0.9400 . ? C26 H26A 0.9400 . ? C27 H27A 0.9400 . ? C28 H28A 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N16 177.8(4) . 1_545 ? O1 Cu1 N7 88.7(4) . . ? N16 Cu1 N7 89.2(4) 1_545 . ? O1 Cu1 N1 93.0(4) . . ? N16 Cu1 N1 88.9(4) 1_545 . ? N7 Cu1 N1 171.4(4) . . ? O1 Cu1 N37 80.3(4) . . ? N16 Cu1 N37 99.0(4) 1_545 . ? N7 Cu1 N37 88.1(4) . . ? N1 Cu1 N37 83.9(4) . . ? O1 Cu1 Cl1 90.4(2) . . ? N16 Cu1 Cl1 90.3(3) 1_545 . ? N7 Cu1 Cl1 91.9(3) . . ? N1 Cu1 Cl1 96.5(3) . . ? N37 Cu1 Cl1 170.7(3) . . ? O1 Cu2 N5 172.9(4) . 3 ? O1 Cu2 N8 88.8(4) . . ? N5 Cu2 N8 87.7(4) 3 . ? O1 Cu2 N13 91.2(4) . . ? N5 Cu2 N13 87.4(4) 3 . ? N8 Cu2 N13 138.7(4) . . ? O1 Cu2 Cl2 93.2(2) . . ? N5 Cu2 Cl2 93.8(3) 3 . ? N8 Cu2 Cl2 119.8(3) . . ? N13 Cu2 Cl2 101.5(3) . . ? N14 Cu3 N2 177.2(4) . . ? N14 Cu3 N38 91.0(4) . . ? N2 Cu3 N38 86.5(3) . . ? N14 Cu3 N10 90.0(4) . 3_455 ? N2 Cu3 N10 91.3(4) . 3_455 ? N38 Cu3 N10 92.2(4) . 3_455 ? N14 Cu3 Cl3 90.7(3) . . ? N2 Cu3 Cl3 91.6(3) . . ? N38 Cu3 Cl3 172.4(3) . . ? N10 Cu3 Cl3 95.2(3) 3_455 . ? N14 Cu3 O1 89.2(4) . . ? N2 Cu3 O1 89.3(3) . . ? N38 Cu3 O1 82.0(3) . . ? N10 Cu3 O1 174.2(4) 3_455 . ? Cl3 Cu3 O1 90.6(2) . . ? N19 Cu4 N25 176.9(4) . . ? N19 Cu4 N40 86.2(4) . . ? N25 Cu4 N40 90.7(4) . . ? N19 Cu4 Cl4 92.2(3) . . ? N25 Cu4 Cl4 90.8(3) . . ? N40 Cu4 Cl4 175.2(3) . . ? N19 Cu4 O2 91.3(4) . . ? N25 Cu4 O2 87.7(3) . . ? N40 Cu4 O2 80.8(3) . . ? Cl4 Cu4 O2 94.7(2) . . ? N19 Cu4 N35 90.6(4) . 3_445 ? N25 Cu4 N35 90.1(4) . 3_445 ? N40 Cu4 N35 93.3(4) . 3_445 ? Cl4 Cu4 N35 91.3(3) . 3_445 ? O2 Cu4 N35 173.7(4) . 3_445 ? O2 Cu5 N29 175.6(4) . 1_565 ? O2 Cu5 N32 88.4(4) . . ? N29 Cu5 N32 87.7(4) 1_565 . ? O2 Cu5 N20 94.2(4) . . ? N29 Cu5 N20 89.0(4) 1_565 . ? N32 Cu5 N20 164.0(4) . . ? O2 Cu5 N41 78.6(3) . . ? N29 Cu5 N41 98.9(4) 1_565 . ? N32 Cu5 N41 84.1(4) . . ? N20 Cu5 N41 80.9(4) . . ? O2 Cu5 Cl5 90.6(2) . . ? N29 Cu5 Cl5 92.2(3) 1_565 . ? N32 Cu5 Cl5 101.9(3) . . ? N20 Cu5 Cl5 93.9(3) . . ? N41 Cu5 Cl5 167.6(3) . . ? O2 Cu6 N23 176.2(4) . 3_545 ? O2 Cu6 N31 89.1(4) . . ? N23 Cu6 N31 88.7(4) 3_545 . ? O2 Cu6 N26 92.7(4) . . ? N23 Cu6 N26 87.6(4) 3_545 . ? N31 Cu6 N26 151.5(4) . . ? O2 Cu6 Cl1 92.0(2) . 2_544 ? N23 Cu6 Cl1 91.4(3) 3_545 2_544 ? N31 Cu6 Cl1 96.6(3) . 2_544 ? N26 Cu6 Cl1 111.7(3) . 2_544 ? Cu6 Cl1 Cu1 143.60(17) 2_545 . ? Cu2 O1 Cu1 121.1(4) . . ? Cu2 O1 Cu3 114.1(4) . . ? Cu1 O1 Cu3 106.5(4) . . ? Cu2 O1 H1 104.5 . . ? Cu1 O1 H1 104.5 . . ? Cu3 O1 H1 104.5 . . ? Cu5 O2 Cu6 121.2(5) . . ? Cu5 O2 Cu4 106.7(3) . . ? Cu6 O2 Cu4 111.6(3) . . ? Cu5 O2 H2 105.4 . . ? Cu6 O2 H2 105.4 . . ? Cu4 O2 H2 105.4 . . ? C1 N1 N2 105.9(10) . . ? C1 N1 Cu1 132.1(8) . . ? N2 N1 Cu1 120.4(7) . . ? C2 N2 N1 109.4(9) . . ? C2 N2 Cu3 130.0(8) . . ? N1 N2 Cu3 119.8(7) . . ? C2 N3 C1 108.8(11) . . ? C2 N3 N6 127.2(11) . . ? C1 N3 N6 123.8(10) . . ? C3 N4 N5 106.4(11) . . ? C4 N5 N4 107.5(10) . . ? C4 N5 Cu2 133.8(9) . 3_445 ? N4 N5 Cu2 118.3(8) . 3_445 ? C4 N6 C3 107.8(10) . . ? C4 N6 N3 129.7(11) . . ? C3 N6 N3 122.1(10) . . ? C5 N7 N8 108.3(10) . . ? C5 N7 Cu1 131.3(8) . . ? N8 N7 Cu1 120.4(6) . . ? C6 N8 N7 107.8(9) . . ? C6 N8 Cu2 131.2(9) . . ? N7 N8 Cu2 119.3(7) . . ? C5 N9 C6 109.2(11) . . ? C5 N9 N12 128.1(10) . . ? C6 N9 N12 122.7(11) . . ? C8 N10 N11 105.3(12) . . ? C8 N10 Cu3 126.6(11) . 3_545 ? N11 N10 Cu3 128.1(8) . 3_545 ? C7 N11 N10 109.1(15) . . ? C7 N12 C8 108.0(14) . . ? C7 N12 N9 127.9(14) . . ? C8 N12 N9 124.1(11) . . ? C9 N13 N14 108.1(9) . . ? C9 N13 Cu2 128.6(9) . . ? N14 N13 Cu2 121.9(7) . . ? C10 N14 N13 106.2(9) . . ? C10 N14 Cu3 132.5(9) . . ? N13 N14 Cu3 120.8(7) . . ? C10 N15 C9 106.1(10) . . ? C10 N15 N18 127.4(10) . . ? C9 N15 N18 126.5(10) . . ? C12 N16 N17 108.0(10) . . ? C12 N16 Cu1 131.1(9) . 1_565 ? N17 N16 Cu1 120.8(7) . 1_565 ? C11 N17 N16 108.0(10) . . ? N15 N18 C12 127.7(9) . . ? N15 N18 C11 126.0(10) . . ? C12 N18 C11 106.3(9) . . ? C13 N19 N20 108.7(9) . . ? C13 N19 Cu4 132.4(8) . . ? N20 N19 Cu4 118.6(8) . . ? C14 N20 N19 108.1(10) . . ? C14 N20 Cu5 129.6(8) . . ? N19 N20 Cu5 121.3(7) . . ? N24 N21 C14 127.3(10) . . ? N24 N21 C13 125.7(10) . . ? C14 N21 C13 106.9(11) . . ? C15 N22 N23 107.4(11) . . ? C16 N23 N22 109.7(11) . . ? C16 N23 Cu6 132.2(9) . 3_455 ? N22 N23 Cu6 117.9(8) . 3_455 ? C16 N24 N21 129.6(11) . . ? C16 N24 C15 106.6(11) . . ? N21 N24 C15 123.8(12) . . ? C17 N25 N26 108.2(10) . . ? C17 N25 Cu4 130.1(9) . . ? N26 N25 Cu4 121.7(7) . . ? C18 N26 N25 107.7(10) . . ? C18 N26 Cu6 129.4(10) . . ? N25 N26 Cu6 122.8(7) . . ? C17 N27 C18 106.1(9) . . ? C17 N27 N30 124.0(11) . . ? C18 N27 N30 129.7(10) . . ? C19 N28 N29 104.5(10) . . ? C20 N29 N28 111.2(10) . . ? C20 N29 Cu5 131.7(9) . 1_545 ? N28 N29 Cu5 117.2(7) . 1_545 ? C19 N30 C20 108.7(10) . . ? C19 N30 N27 127.5(10) . . ? C20 N30 N27 123.7(11) . . ? C21 N31 N32 109.2(10) . . ? C21 N31 Cu6 131.5(8) . . ? N32 N31 Cu6 119.1(8) . . ? C22 N32 N31 106.1(10) . . ? C22 N32 Cu5 132.8(8) . . ? N31 N32 Cu5 121.1(7) . . ? C21 N33 N36 126.9(12) . . ? C21 N33 C22 107.2(11) . . ? N36 N33 C22 125.9(10) . . ? C23 N34 N35 106.8(13) . . ? C24 N35 N34 107.4(11) . . ? C24 N35 Cu4 124.9(10) . 3 ? N34 N35 Cu4 127.7(9) . 3 ? C23 N36 N33 129.8(11) . . ? C23 N36 C24 105.8(12) . . ? N33 N36 C24 124.2(11) . . ? C25 N37 N38 105.0(10) . . ? C25 N37 Cu1 137.9(9) . . ? N38 N37 Cu1 116.8(7) . . ? C26 N38 N37 110.6(9) . . ? C26 N38 Cu3 130.9(8) . . ? N37 N38 Cu3 118.2(7) . . ? C25 N39 C26 108.7(9) . . ? C25 N39 N42 126.0(10) . . ? C26 N39 N42 125.3(10) . . ? C27 N40 N41 106.6(10) . . ? C27 N40 Cu4 131.5(9) . . ? N41 N40 Cu4 121.5(7) . . ? C28 N41 N40 107.5(10) . . ? C28 N41 Cu5 138.6(9) . . ? N40 N41 Cu5 113.5(7) . . ? C27 N42 C28 107.2(10) . . ? C27 N42 N39 125.7(10) . . ? C28 N42 N39 126.9(11) . . ? N1 C1 N3 106.6(11) . . ? N1 C1 H1A 126.7 . . ? N3 C1 H1A 126.7 . . ? N2 C2 N3 109.3(11) . . ? N2 C2 H2A 125.4 . . ? N3 C2 H2A 125.4 . . ? N4 C3 N6 109.8(11) . . ? N4 C3 H3A 125.1 . . ? N6 C3 H3A 125.1 . . ? N5 C4 N6 108.5(11) . . ? N5 C4 H4A 125.7 . . ? N6 C4 H4A 125.7 . . ? N7 C5 N9 108.3(11) . . ? N7 C5 H5A 125.9 . . ? N9 C5 H5A 125.9 . . ? N8 C6 N9 106.4(11) . . ? N8 C6 H6A 126.8 . . ? N9 C6 H6A 126.8 . . ? N11 C7 N12 109(2) . . ? N11 C7 H7A 125.4 . . ? N12 C7 H7A 125.4 . . ? N10 C8 N12 108.4(14) . . ? N10 C8 H8A 125.8 . . ? N12 C8 H8A 125.8 . . ? N13 C9 N15 108.9(11) . . ? N13 C9 H9A 125.5 . . ? N15 C9 H9A 125.5 . . ? N14 C10 N15 110.7(11) . . ? N14 C10 H10A 124.7 . . ? N15 C10 H10A 124.7 . . ? N17 C11 N18 109.0(11) . . ? N17 C11 H11A 125.5 . . ? N18 C11 H11A 125.5 . . ? N16 C12 N18 108.6(11) . . ? N16 C12 H12A 125.7 . . ? N18 C12 H12A 125.7 . . ? N19 C13 N21 108.4(10) . . ? N19 C13 H13A 125.8 . . ? N21 C13 H13A 125.8 . . ? N20 C14 N21 107.6(10) . . ? N20 C14 H14A 126.2 . . ? N21 C14 H14A 126.2 . . ? N22 C15 N24 107.3(13) . . ? N22 C15 H15A 126.3 . . ? N24 C15 H15A 126.3 . . ? N23 C16 N24 108.9(12) . . ? N23 C16 H16A 125.5 . . ? N24 C16 H16A 125.5 . . ? N25 C17 N27 109.5(12) . . ? N25 C17 H17A 125.3 . . ? N27 C17 H17A 125.3 . . ? N26 C18 N27 108.5(12) . . ? N26 C18 H18A 125.8 . . ? N27 C18 H18A 125.8 . . ? N30 C19 N28 109.6(12) . . ? N30 C19 H19A 125.2 . . ? N28 C19 H19A 125.2 . . ? N29 C20 N30 105.6(13) . . ? N29 C20 H20A 127.2 . . ? N30 C20 H20A 127.2 . . ? N31 C21 N33 108.8(12) . . ? N31 C21 H21A 125.6 . . ? N33 C21 H21A 125.6 . . ? N32 C22 N33 108.5(10) . . ? N32 C22 H22A 125.7 . . ? N33 C22 H22A 125.7 . . ? N34 C23 N36 109.1(15) . . ? N34 C23 H23A 125.4 . . ? N36 C23 H23A 125.4 . . ? N35 C24 N36 110.8(13) . . ? N35 C24 H24A 124.6 . . ? N36 C24 H24A 124.6 . . ? N37 C25 N39 108.8(10) . . ? N37 C25 H25A 125.6 . . ? N39 C25 H25A 125.6 . . ? N38 C26 N39 106.8(10) . . ? N38 C26 H26A 126.6 . . ? N39 C26 H26A 126.6 . . ? N42 C27 N40 109.7(11) . . ? N42 C27 H27A 125.1 . . ? N40 C27 H27A 125.1 . . ? N41 C28 N42 108.7(12) . . ? N41 C28 H28A 125.6 . . ? N42 C28 H28A 125.6 . . ? 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 O1 Cu1 Cl1 Cu6 55.8(4) . . . 2_545 ? N16 Cu1 Cl1 Cu6 -126.2(4) 1_545 . . 2_545 ? N7 Cu1 Cl1 Cu6 144.5(3) . . . 2_545 ? N1 Cu1 Cl1 Cu6 -37.3(4) . . . 2_545 ? N37 Cu1 Cl1 Cu6 55(2) . . . 2_545 ? N5 Cu2 O1 Cu1 57(3) 3 . . . ? N8 Cu2 O1 Cu1 -3.5(5) . . . . ? N13 Cu2 O1 Cu1 135.1(5) . . . . ? Cl2 Cu2 O1 Cu1 -123.3(4) . . . . ? N5 Cu2 O1 Cu3 -72(3) 3 . . . ? N8 Cu2 O1 Cu3 -132.8(4) . . . . ? N13 Cu2 O1 Cu3 5.9(4) . . . . ? Cl2 Cu2 O1 Cu3 107.4(3) . . . . ? N16 Cu1 O1 Cu2 -8(12) 1_545 . . . ? N7 Cu1 O1 Cu2 8.7(5) . . . . ? N1 Cu1 O1 Cu2 -162.9(5) . . . . ? N37 Cu1 O1 Cu2 -79.6(5) . . . . ? Cl1 Cu1 O1 Cu2 100.6(5) . . . . ? N16 Cu1 O1 Cu3 124(11) 1_545 . . . ? N7 Cu1 O1 Cu3 141.2(4) . . . . ? N1 Cu1 O1 Cu3 -30.4(4) . . . . ? N37 Cu1 O1 Cu3 52.9(4) . . . . ? Cl1 Cu1 O1 Cu3 -126.9(3) . . . . ? N14 Cu3 O1 Cu2 -12.0(4) . . . . ? N2 Cu3 O1 Cu2 165.7(4) . . . . ? N38 Cu3 O1 Cu2 79.1(4) . . . . ? N10 Cu3 O1 Cu2 70(4) 3_455 . . . ? Cl3 Cu3 O1 Cu2 -102.7(3) . . . . ? N14 Cu3 O1 Cu1 -148.3(4) . . . . ? N2 Cu3 O1 Cu1 29.4(4) . . . . ? N38 Cu3 O1 Cu1 -57.2(4) . . . . ? N10 Cu3 O1 Cu1 -66(4) 3_455 . . . ? Cl3 Cu3 O1 Cu1 121.1(3) . . . . ? N29 Cu5 O2 Cu6 -18(5) 1_565 . . . ? N32 Cu5 O2 Cu6 9.8(4) . . . . ? N20 Cu5 O2 Cu6 -154.3(4) . . . . ? N41 Cu5 O2 Cu6 -74.5(5) . . . . ? Cl5 Cu5 O2 Cu6 111.7(4) . . . . ? N29 Cu5 O2 Cu4 111(5) 1_565 . . . ? N32 Cu5 O2 Cu4 138.9(4) . . . . ? N20 Cu5 O2 Cu4 -25.2(4) . . . . ? N41 Cu5 O2 Cu4 54.6(4) . . . . ? Cl5 Cu5 O2 Cu4 -119.2(3) . . . . ? N23 Cu6 O2 Cu5 49(5) 3_545 . . . ? N31 Cu6 O2 Cu5 -7.0(5) . . . . ? N26 Cu6 O2 Cu5 144.5(5) . . . . ? Cl1 Cu6 O2 Cu5 -103.6(4) 2_544 . . . ? N23 Cu6 O2 Cu4 -78(5) 3_545 . . . ? N31 Cu6 O2 Cu4 -133.9(4) . . . . ? N26 Cu6 O2 Cu4 17.6(4) . . . . ? Cl1 Cu6 O2 Cu4 129.5(3) 2_544 . . . ? N19 Cu4 O2 Cu5 26.0(4) . . . . ? N25 Cu4 O2 Cu5 -151.1(4) . . . . ? N40 Cu4 O2 Cu5 -60.0(4) . . . . ? Cl4 Cu4 O2 Cu5 118.4(3) . . . . ? N35 Cu4 O2 Cu5 -81(3) 3_445 . . . ? N19 Cu4 O2 Cu6 160.4(4) . . . . ? N25 Cu4 O2 Cu6 -16.7(4) . . . . ? N40 Cu4 O2 Cu6 74.5(4) . . . . ? Cl4 Cu4 O2 Cu6 -107.2(3) . . . . ? N35 Cu4 O2 Cu6 53(3) 3_445 . . . ? O1 Cu1 N1 C1 -172.2(13) . . . . ? N16 Cu1 N1 C1 8.7(13) 1_545 . . . ? N7 Cu1 N1 C1 86(3) . . . . ? N37 Cu1 N1 C1 107.9(13) . . . . ? Cl1 Cu1 N1 C1 -81.4(13) . . . . ? O1 Cu1 N1 N2 24.5(8) . . . . ? N16 Cu1 N1 N2 -154.5(9) 1_545 . . . ? N7 Cu1 N1 N2 -77(3) . . . . ? N37 Cu1 N1 N2 -55.4(8) . . . . ? Cl1 Cu1 N1 N2 115.3(8) . . . . ? C1 N1 N2 C2 -0.3(13) . . . . ? Cu1 N1 N2 C2 166.9(8) . . . . ? C1 N1 N2 Cu3 -171.2(8) . . . . ? Cu1 N1 N2 Cu3 -4.0(11) . . . . ? N14 Cu3 N2 C2 -128(9) . . . . ? N38 Cu3 N2 C2 -102.6(11) . . . . ? N10 Cu3 N2 C2 -10.4(11) 3_455 . . . ? Cl3 Cu3 N2 C2 84.8(11) . . . . ? O1 Cu3 N2 C2 175.4(11) . . . . ? N14 Cu3 N2 N1 41(10) . . . . ? N38 Cu3 N2 N1 66.2(8) . . . . ? N10 Cu3 N2 N1 158.3(8) 3_455 . . . ? Cl3 Cu3 N2 N1 -106.4(8) . . . . ? O1 Cu3 N2 N1 -15.9(8) . . . . ? C3 N4 N5 C4 -0.6(14) . . . . ? C3 N4 N5 Cu2 -174.4(9) . . . 3_445 ? C2 N3 N6 C4 -90.8(17) . . . . ? C1 N3 N6 C4 94.2(16) . . . . ? C2 N3 N6 C3 80.9(16) . . . . ? C1 N3 N6 C3 -94.1(16) . . . . ? O1 Cu1 N7 C5 166.6(12) . . . . ? N16 Cu1 N7 C5 -14.0(12) 1_545 . . . ? N1 Cu1 N7 C5 -92(3) . . . . ? N37 Cu1 N7 C5 -113.0(12) . . . . ? Cl1 Cu1 N7 C5 76.2(12) . . . . ? O1 Cu1 N7 N8 -13.6(8) . . . . ? N16 Cu1 N7 N8 165.7(9) 1_545 . . . ? N1 Cu1 N7 N8 88(3) . . . . ? N37 Cu1 N7 N8 66.8(9) . . . . ? Cl1 Cu1 N7 N8 -104.0(8) . . . . ? C5 N7 N8 C6 1.1(14) . . . . ? Cu1 N7 N8 C6 -178.7(9) . . . . ? C5 N7 N8 Cu2 -165.6(9) . . . . ? Cu1 N7 N8 Cu2 14.6(12) . . . . ? O1 Cu2 N8 C6 -169.5(13) . . . . ? N5 Cu2 N8 C6 16.6(13) 3 . . . ? N13 Cu2 N8 C6 100.0(13) . . . . ? Cl2 Cu2 N8 C6 -76.4(12) . . . . ? O1 Cu2 N8 N7 -6.5(9) . . . . ? N5 Cu2 N8 N7 179.7(9) 3 . . . ? N13 Cu2 N8 N7 -97.0(9) . . . . ? Cl2 Cu2 N8 N7 86.6(9) . . . . ? C8 N10 N11 C7 0(2) . . . . ? Cu3 N10 N11 C7 -177.3(17) 3_545 . . . ? C5 N9 N12 C7 91(2) . . . . ? C6 N9 N12 C7 -90(2) . . . . ? C5 N9 N12 C8 -86.2(18) . . . . ? C6 N9 N12 C8 92.8(16) . . . . ? O1 Cu2 N13 C9 170.7(11) . . . . ? N5 Cu2 N13 C9 -16.2(11) 3 . . . ? N8 Cu2 N13 C9 -99.7(12) . . . . ? Cl2 Cu2 N13 C9 77.2(11) . . . . ? O1 Cu2 N13 N14 5.9(9) . . . . ? N5 Cu2 N13 N14 179.0(9) 3 . . . ? N8 Cu2 N13 N14 95.5(10) . . . . ? Cl2 Cu2 N13 N14 -87.7(9) . . . . ? C9 N13 N14 C10 2.0(13) . . . . ? Cu2 N13 N14 C10 169.6(7) . . . . ? C9 N13 N14 Cu3 174.9(9) . . . . ? Cu2 N13 N14 Cu3 -17.5(12) . . . . ? N2 Cu3 N14 C10 131(9) . . . . ? N38 Cu3 N14 C10 105.8(11) . . . . ? N10 Cu3 N14 C10 13.6(11) 3_455 . . . ? Cl3 Cu3 N14 C10 -81.6(11) . . . . ? O1 Cu3 N14 C10 -172.1(11) . . . . ? N2 Cu3 N14 N13 -39(10) . . . . ? N38 Cu3 N14 N13 -64.9(9) . . . . ? N10 Cu3 N14 N13 -157.2(9) 3_455 . . . ? Cl3 Cu3 N14 N13 107.6(8) . . . . ? O1 Cu3 N14 N13 17.1(9) . . . . ? C12 N16 N17 C11 2.9(15) . . . . ? Cu1 N16 N17 C11 178.4(10) 1_565 . . . ? C10 N15 N18 C12 91.0(16) . . . . ? C9 N15 N18 C12 -90.9(16) . . . . ? C10 N15 N18 C11 -88.3(16) . . . . ? C9 N15 N18 C11 89.7(17) . . . . ? N25 Cu4 N19 C13 -118(8) . . . . ? N40 Cu4 N19 C13 -107.9(12) . . . . ? Cl4 Cu4 N19 C13 76.6(12) . . . . ? O2 Cu4 N19 C13 171.4(12) . . . . ? N35 Cu4 N19 C13 -14.7(12) 3_445 . . . ? N25 Cu4 N19 N20 55(8) . . . . ? N40 Cu4 N19 N20 65.4(8) . . . . ? Cl4 Cu4 N19 N20 -110.0(8) . . . . ? O2 Cu4 N19 N20 -15.3(8) . . . . ? N35 Cu4 N19 N20 158.7(8) 3_445 . . . ? C13 N19 N20 C14 5.0(14) . . . . ? Cu4 N19 N20 C14 -169.8(8) . . . . ? C13 N19 N20 Cu5 174.2(9) . . . . ? Cu4 N19 N20 Cu5 -0.7(11) . . . . ? O2 Cu5 N20 C14 -174.0(11) . . . . ? N29 Cu5 N20 C14 9.1(11) 1_565 . . . ? N32 Cu5 N20 C14 87.3(17) . . . . ? N41 Cu5 N20 C14 108.2(11) . . . . ? Cl5 Cu5 N20 C14 -83.1(11) . . . . ? O2 Cu5 N20 N19 19.4(9) . . . . ? N29 Cu5 N20 N19 -157.6(9) 1_565 . . . ? N32 Cu5 N20 N19 -79.3(16) . . . . ? N41 Cu5 N20 N19 -58.4(8) . . . . ? Cl5 Cu5 N20 N19 110.3(8) . . . . ? C15 N22 N23 C16 -2.5(14) . . . . ? C15 N22 N23 Cu6 -177.2(9) . . . 3_455 ? C14 N21 N24 C16 88.5(17) . . . . ? C13 N21 N24 C16 -94.9(16) . . . . ? C14 N21 N24 C15 -92.5(16) . . . . ? C13 N21 N24 C15 84.1(16) . . . . ? N19 Cu4 N25 C17 119(8) . . . . ? N40 Cu4 N25 C17 108.6(13) . . . . ? Cl4 Cu4 N25 C17 -76.0(13) . . . . ? O2 Cu4 N25 C17 -170.6(13) . . . . ? N35 Cu4 N25 C17 15.3(13) 3_445 . . . ? N19 Cu4 N25 N26 -63(8) . . . . ? N40 Cu4 N25 N26 -72.7(10) . . . . ? Cl4 Cu4 N25 N26 102.7(9) . . . . ? O2 Cu4 N25 N26 8.1(9) . . . . ? N35 Cu4 N25 N26 -166.0(10) 3_445 . . . ? C17 N25 N26 C18 -1.0(16) . . . . ? Cu4 N25 N26 C18 -179.9(10) . . . . ? C17 N25 N26 Cu6 -177.7(10) . . . . ? Cu4 N25 N26 Cu6 3.4(14) . . . . ? O2 Cu6 N26 C18 169.5(13) . . . . ? N23 Cu6 N26 C18 -14.3(13) 3_545 . . . ? N31 Cu6 N26 C18 -97.3(14) . . . . ? Cl1 Cu6 N26 C18 76.3(13) 2_544 . . . ? O2 Cu6 N26 N25 -14.5(10) . . . . ? N23 Cu6 N26 N25 161.6(10) 3_545 . . . ? N31 Cu6 N26 N25 78.7(14) . . . . ? Cl1 Cu6 N26 N25 -107.8(9) 2_544 . . . ? C19 N28 N29 C20 -5.9(18) . . . . ? C19 N28 N29 Cu5 174.7(10) . . . 1_545 ? C17 N27 N30 C19 -83.1(19) . . . . ? C18 N27 N30 C19 90.0(19) . . . . ? C17 N27 N30 C20 94.1(17) . . . . ? C18 N27 N30 C20 -92.7(19) . . . . ? O2 Cu6 N31 C21 -174.4(13) . . . . ? N23 Cu6 N31 C21 8.8(13) 3_545 . . . ? N26 Cu6 N31 C21 91.5(14) . . . . ? Cl1 Cu6 N31 C21 -82.5(13) 2_544 . . . ? O2 Cu6 N31 N32 -0.9(8) . . . . ? N23 Cu6 N31 N32 -177.7(8) 3_545 . . . ? N26 Cu6 N31 N32 -95.0(12) . . . . ? Cl1 Cu6 N31 N32 91.0(8) 2_544 . . . ? C21 N31 N32 C22 4.1(14) . . . . ? Cu6 N31 N32 C22 -170.7(8) . . . . ? C21 N31 N32 Cu5 -176.9(9) . . . . ? Cu6 N31 N32 Cu5 8.3(11) . . . . ? O2 Cu5 N32 C22 168.1(11) . . . . ? N29 Cu5 N32 C22 -14.0(11) 1_565 . . . ? N20 Cu5 N32 C22 -92.4(16) . . . . ? N41 Cu5 N32 C22 -113.2(11) . . . . ? Cl5 Cu5 N32 C22 77.8(11) . . . . ? O2 Cu5 N32 N31 -10.6(8) . . . . ? N29 Cu5 N32 N31 167.3(8) 1_565 . . . ? N20 Cu5 N32 N31 88.9(15) . . . . ? N41 Cu5 N32 N31 68.1(8) . . . . ? Cl5 Cu5 N32 N31 -100.9(8) . . . . ? C23 N34 N35 C24 -2.7(18) . . . . ? C23 N34 N35 Cu4 174.6(11) . . . 3 ? C21 N33 N36 C23 -83.2(19) . . . . ? C22 N33 N36 C23 95.3(18) . . . . ? C21 N33 N36 C24 91.5(17) . . . . ? C22 N33 N36 C24 -90.0(16) . . . . ? O1 Cu1 N37 C25 150.0(16) . . . . ? N16 Cu1 N37 C25 -27.9(16) 1_545 . . . ? N7 Cu1 N37 C25 61.0(16) . . . . ? N1 Cu1 N37 C25 -115.9(16) . . . . ? Cl1 Cu1 N37 C25 151.2(15) . . . . ? O1 Cu1 N37 N38 -36.5(9) . . . . ? N16 Cu1 N37 N38 145.6(9) 1_545 . . . ? N7 Cu1 N37 N38 -125.5(9) . . . . ? N1 Cu1 N37 N38 57.6(9) . . . . ? Cl1 Cu1 N37 N38 -35(3) . . . . ? C25 N37 N38 C26 1.0(15) . . . . ? Cu1 N37 N38 C26 -174.5(9) . . . . ? C25 N37 N38 Cu3 175.6(9) . . . . ? Cu1 N37 N38 Cu3 0.1(11) . . . . ? N14 Cu3 N38 C26 -67.0(12) . . . . ? N2 Cu3 N38 C26 114.2(12) . . . . ? N10 Cu3 N38 C26 23.1(12) 3_455 . . . ? Cl3 Cu3 N38 C26 -169.7(16) . . . . ? O1 Cu3 N38 C26 -156.1(12) . . . . ? N14 Cu3 N38 N37 119.7(9) . . . . ? N2 Cu3 N38 N37 -59.1(9) . . . . ? N10 Cu3 N38 N37 -150.2(9) 3_455 . . . ? Cl3 Cu3 N38 N37 17(3) . . . . ? O1 Cu3 N38 N37 30.7(8) . . . . ? N19 Cu4 N40 C27 110.4(12) . . . . ? N25 Cu4 N40 C27 -70.1(12) . . . . ? Cl4 Cu4 N40 C27 -178(90) . . . . ? O2 Cu4 N40 C27 -157.7(12) . . . . ? N35 Cu4 N40 C27 20.0(12) 3_445 . . . ? N19 Cu4 N40 N41 -61.1(9) . . . . ? N25 Cu4 N40 N41 118.3(9) . . . . ? Cl4 Cu4 N40 N41 10(4) . . . . ? O2 Cu4 N40 N41 30.8(9) . . . . ? N35 Cu4 N40 N41 -151.5(9) 3_445 . . . ? C27 N40 N41 C28 1.2(16) . . . . ? Cu4 N40 N41 C28 174.6(10) . . . . ? C27 N40 N41 Cu5 -173.1(9) . . . . ? Cu4 N40 N41 Cu5 0.3(12) . . . . ? O2 Cu5 N41 C28 149.9(18) . . . . ? N29 Cu5 N41 C28 -26.3(18) 1_565 . . . ? N32 Cu5 N41 C28 60.4(17) . . . . ? N20 Cu5 N41 C28 -113.9(18) . . . . ? Cl5 Cu5 N41 C28 179.9(14) . . . . ? O2 Cu5 N41 N40 -38.3(8) . . . . ? N29 Cu5 N41 N40 145.5(9) 1_565 . . . ? N32 Cu5 N41 N40 -127.8(9) . . . . ? N20 Cu5 N41 N40 57.9(9) . . . . ? Cl5 Cu5 N41 N40 -8(2) . . . . ? C25 N39 N42 C27 69(2) . . . . ? C26 N39 N42 C27 -112.0(16) . . . . ? C25 N39 N42 C28 -117.0(17) . . . . ? C26 N39 N42 C28 62(2) . . . . ? N2 N1 C1 N3 -0.4(13) . . . . ? Cu1 N1 C1 N3 -165.4(9) . . . . ? C2 N3 C1 N1 1.0(15) . . . . ? N6 N3 C1 N1 176.8(10) . . . . ? N1 N2 C2 N3 0.9(14) . . . . ? Cu3 N2 C2 N3 170.6(8) . . . . ? C1 N3 C2 N2 -1.2(15) . . . . ? N6 N3 C2 N2 -176.8(11) . . . . ? N5 N4 C3 N6 1.8(15) . . . . ? C4 N6 C3 N4 -2.3(16) . . . . ? N3 N6 C3 N4 -175.6(11) . . . . ? N4 N5 C4 N6 -0.7(14) . . . . ? Cu2 N5 C4 N6 171.6(9) 3_445 . . . ? C3 N6 C4 N5 1.8(15) . . . . ? N3 N6 C4 N5 174.5(11) . . . . ? N8 N7 C5 N9 -1.5(15) . . . . ? Cu1 N7 C5 N9 178.3(9) . . . . ? C6 N9 C5 N7 1.3(16) . . . . ? N12 N9 C5 N7 -179.6(12) . . . . ? N7 N8 C6 N9 -0.3(15) . . . . ? Cu2 N8 C6 N9 164.2(9) . . . . ? C5 N9 C6 N8 -0.6(16) . . . . ? N12 N9 C6 N8 -179.8(12) . . . . ? N10 N11 C7 N12 -1(3) . . . . ? C8 N12 C7 N11 2(3) . . . . ? N9 N12 C7 N11 -175.9(16) . . . . ? N11 N10 C8 N12 0.9(15) . . . . ? Cu3 N10 C8 N12 178.4(9) 3_545 . . . ? C7 N12 C8 N10 -2(2) . . . . ? N9 N12 C8 N10 176.2(11) . . . . ? N14 N13 C9 N15 -0.4(15) . . . . ? Cu2 N13 C9 N15 -166.9(8) . . . . ? C10 N15 C9 N13 -1.2(15) . . . . ? N18 N15 C9 N13 -179.7(11) . . . . ? N13 N14 C10 N15 -2.8(13) . . . . ? Cu3 N14 C10 N15 -174.6(8) . . . . ? C9 N15 C10 N14 2.6(14) . . . . ? N18 N15 C10 N14 -179.0(10) . . . . ? N16 N17 C11 N18 -1.6(16) . . . . ? N15 N18 C11 N17 179.4(12) . . . . ? C12 N18 C11 N17 -0.1(16) . . . . ? N17 N16 C12 N18 -2.9(14) . . . . ? Cu1 N16 C12 N18 -177.8(8) 1_565 . . . ? N15 N18 C12 N16 -177.6(11) . . . . ? C11 N18 C12 N16 1.9(15) . . . . ? N20 N19 C13 N21 -4.5(14) . . . . ? Cu4 N19 C13 N21 169.3(9) . . . . ? N24 N21 C13 N19 -174.6(12) . . . . ? C14 N21 C13 N19 2.5(14) . . . . ? N19 N20 C14 N21 -3.3(14) . . . . ? Cu5 N20 C14 N21 -171.3(8) . . . . ? N24 N21 C14 N20 177.7(12) . . . . ? C13 N21 C14 N20 0.6(14) . . . . ? N23 N22 C15 N24 1.1(15) . . . . ? C16 N24 C15 N22 0.6(15) . . . . ? N21 N24 C15 N22 -178.6(11) . . . . ? N22 N23 C16 N24 2.9(13) . . . . ? Cu6 N23 C16 N24 176.5(8) 3_455 . . . ? N21 N24 C16 N23 177.0(10) . . . . ? C15 N24 C16 N23 -2.2(13) . . . . ? N26 N25 C17 N27 -0.4(16) . . . . ? Cu4 N25 C17 N27 178.4(9) . . . . ? C18 N27 C17 N25 1.6(16) . . . . ? N30 N27 C17 N25 176.1(11) . . . . ? N25 N26 C18 N27 1.9(16) . . . . ? Cu6 N26 C18 N27 178.3(9) . . . . ? C17 N27 C18 N26 -2.2(16) . . . . ? N30 N27 C18 N26 -176.3(12) . . . . ? C20 N30 C19 N28 1(2) . . . . ? N27 N30 C19 N28 179.1(12) . . . . ? N29 N28 C19 N30 2.5(18) . . . . ? N28 N29 C20 N30 6.8(18) . . . . ? Cu5 N29 C20 N30 -174.0(9) 1_545 . . . ? C19 N30 C20 N29 -5.0(19) . . . . ? N27 N30 C20 N29 177.3(12) . . . . ? N32 N31 C21 N33 -3.9(15) . . . . ? Cu6 N31 C21 N33 170.1(9) . . . . ? N36 N33 C21 N31 -179.1(12) . . . . ? C22 N33 C21 N31 2.2(16) . . . . ? N31 N32 C22 N33 -2.7(13) . . . . ? Cu5 N32 C22 N33 178.5(8) . . . . ? C21 N33 C22 N32 0.4(14) . . . . ? N36 N33 C22 N32 -178.3(11) . . . . ? N35 N34 C23 N36 2(2) . . . . ? N33 N36 C23 N34 174.8(13) . . . . ? C24 N36 C23 N34 -0.7(18) . . . . ? N34 N35 C24 N36 2.4(15) . . . . ? Cu4 N35 C24 N36 -175.0(8) 3 . . . ? C23 N36 C24 N35 -1.1(15) . . . . ? N33 N36 C24 N35 -176.9(11) . . . . ? N38 N37 C25 N39 -1.1(16) . . . . ? Cu1 N37 C25 N39 172.9(10) . . . . ? C26 N39 C25 N37 0.9(17) . . . . ? N42 N39 C25 N37 179.8(12) . . . . ? N37 N38 C26 N39 -0.5(15) . . . . ? Cu3 N38 C26 N39 -174.2(8) . . . . ? C25 N39 C26 N38 -0.2(16) . . . . ? N42 N39 C26 N38 -179.1(12) . . . . ? C28 N42 C27 N40 5.0(16) . . . . ? N39 N42 C27 N40 179.8(12) . . . . ? N41 N40 C27 N42 -3.9(15) . . . . ? Cu4 N40 C27 N42 -176.4(9) . . . . ? N40 N41 C28 N42 1.8(17) . . . . ? Cu5 N41 C28 N42 173.9(11) . . . . ? C27 N42 C28 N41 -4.2(18) . . . . ? N39 N42 C28 N41 -178.9(14) . . . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.417 _refine_diff_density_min -0.839 _refine_diff_density_rms 0.167 #==============================================================================