# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name S.Kar _publ_contact_author_name 'Prof. Susanta Kar' _publ_contact_author_email 'skkar cu@yahoo.co.in' data_lkj_gm _database_code_depnum_ccdc_archive 'CCDC 796246' #TrackingRef '- Rev. Complex 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H56 Cu4 N28 O4, 4(N O3)' _chemical_formula_sum 'C64 H56 Cu4 N32 O16' _chemical_formula_weight 1783.61 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/C' _symmetry_space_group_name_Hall '-C 2yC' 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' '-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 19.921(7) _cell_length_b 38.224(16) _cell_length_c 14.084(5) _cell_angle_alpha 90.00 _cell_angle_beta 134.890(5) _cell_angle_gamma 90.00 _cell_volume 7598(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 22805 _cell_measurement_theta_min 1.1 _cell_measurement_theta_max 20.4 _exptl_crystal_description Rectangular _exptl_crystal_colour Blue _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3632 _exptl_absorpt_coefficient_mu 1.192 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.840 _exptl_absorpt_correction_T_max 0.867 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22805 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 20.41 _reflns_number_total 3741 _reflns_number_gt 3032 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX V1.80.05' _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^)+(0.0000P)^2^+39.2710P] 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_extinction_coef ? _refine_ls_number_reflns 3741 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1178 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_restrained_S_all 1.190 _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 0.69986(6) 0.11679(3) 1.00819(9) 0.0770(3) Uani 1 1 d . . . Cu2 Cu 0.55841(6) 0.13327(3) 0.60857(9) 0.0766(3) Uani 1 1 d . . . N2 N 0.5412(5) 0.18501(19) 0.6022(9) 0.086(2) Uani 1 1 d . . . N3 N 0.5798(5) 0.2026(2) 0.7153(9) 0.101(2) Uani 1 1 d . . . N7 N 0.4848(6) 0.2382(3) 0.4684(10) 0.155(4) Uani 1 1 d . . . H7A H 0.5116 0.2517 0.5359 0.186 Uiso 1 1 calc R . . H7B H 0.4528 0.2469 0.3903 0.186 Uiso 1 1 calc R . . N2A N 0.3104(6) 0.06541(18) 0.5188(7) 0.0821(19) Uani 1 1 d . . . N3A N 0.3843(6) 0.0478(2) 0.5564(7) 0.093(2) Uani 1 1 d . . . N7A N 0.2331(7) 0.0114(3) 0.4976(9) 0.146(3) Uani 1 1 d . . . H14A H 0.2753 -0.0021 0.5153 0.176 Uiso 1 1 calc R . . H14B H 0.1861 0.0026 0.4814 0.176 Uiso 1 1 calc R . . O2 O 0.4282(3) 0.10537(15) 0.5560(5) 0.0763(15) Uani 1 1 d . . . O1 O 0.6235(3) 0.14442(16) 0.8017(5) 0.0770(15) Uani 1 1 d . . . N1 N 0.4749(4) 0.1439(3) 0.4079(7) 0.090(2) Uani 1 1 d . . . C1 C 0.4397(6) 0.1204(3) 0.3079(11) 0.114(3) Uani 1 1 d . . . H1 H 0.4484 0.0965 0.3255 0.137 Uiso 1 1 calc R . . C2 C 0.3906(8) 0.1327(4) 0.1790(12) 0.135(4) Uani 1 1 d . . . H2 H 0.3671 0.1171 0.1107 0.161 Uiso 1 1 calc R . . C3 C 0.3773(8) 0.1687(5) 0.1541(12) 0.137(5) Uani 1 1 d . . . H3 H 0.3439 0.1771 0.0686 0.164 Uiso 1 1 calc R . . C4 C 0.4134(6) 0.1917(3) 0.2559(11) 0.118(4) Uani 1 1 d . . . H4 H 0.4052 0.2157 0.2389 0.141 Uiso 1 1 calc R . . C5 C 0.4619(6) 0.1797(4) 0.3836(10) 0.088(3) Uani 1 1 d . . . C6 C 0.4941(7) 0.1984(3) 0.4875(13) 0.093(3) Uani 1 1 d . . . C7 C 0.6211(6) 0.1769(3) 0.8134(9) 0.081(2) Uani 1 1 d . . . N4 N 0.7050(5) 0.16547(19) 1.0383(8) 0.0793(19) Uani 1 1 d . . . C8 C 0.6639(6) 0.1913(3) 0.9419(9) 0.081(2) Uani 1 1 d . . . C9 C 0.6753(7) 0.2230(3) 0.9999(13) 0.110(3) Uani 1 1 d . . . H9 H 0.6541 0.2447 0.9573 0.132 Uiso 1 1 calc R . . C10 C 0.7246(8) 0.2167(4) 1.1347(14) 0.111(4) Uani 1 1 d . . . N5 N 0.7420(5) 0.1811(3) 1.1549(9) 0.094(2) Uani 1 1 d . . . C11 C 0.7445(7) 0.2444(3) 1.2136(11) 0.141(4) Uani 1 1 d . . . H11A H 0.7784 0.2361 1.3021 0.212 Uiso 1 1 calc R . . H11B H 0.6864 0.2552 1.1755 0.212 Uiso 1 1 calc R . . H11C H 0.7826 0.2612 1.2183 0.212 Uiso 1 1 calc R . . N6 N 0.7742(5) 0.1248(3) 1.2284(8) 0.095(2) Uani 1 1 d . . . C12 C 0.7854(6) 0.1588(4) 1.2636(10) 0.100(3) Uani 1 1 d . . . C13 C 0.8324(7) 0.1694(4) 1.3927(12) 0.124(4) Uani 1 1 d . . . H13 H 0.8390 0.1930 1.4141 0.148 Uiso 1 1 calc R . . C14 C 0.8688(10) 0.1439(5) 1.4879(15) 0.162(7) Uani 1 1 d . . . H14 H 0.9004 0.1505 1.5746 0.195 Uiso 1 1 calc R . . C15 C 0.8593(10) 0.1096(5) 1.4578(14) 0.159(6) Uani 1 1 d . . . H15 H 0.8837 0.0928 1.5231 0.191 Uiso 1 1 calc R . . C16 C 0.8125(6) 0.0995(3) 1.3272(12) 0.129(4) Uani 1 1 d . . . H16 H 0.8069 0.0759 1.3066 0.155 Uiso 1 1 calc R . . N1A N 0.1815(5) 0.1058(3) 0.4566(6) 0.088(2) Uani 1 1 d . . . C1A C 0.1171(8) 0.1294(3) 0.4280(9) 0.110(3) Uani 1 1 d . . . H1A H 0.1254 0.1533 0.4265 0.131 Uiso 1 1 calc R . . C2A C 0.0382(8) 0.1170(4) 0.4008(11) 0.142(4) Uani 1 1 d . . . H2A H -0.0058 0.1325 0.3823 0.170 Uiso 1 1 calc R . . C3A C 0.0275(9) 0.0810(5) 0.4022(11) 0.135(5) Uani 1 1 d . . . H3A H -0.0244 0.0725 0.3838 0.162 Uiso 1 1 calc R . . C4A C 0.0924(8) 0.0582(3) 0.4304(9) 0.117(4) Uani 1 1 d . . . H4A H 0.0841 0.0342 0.4309 0.141 Uiso 1 1 calc R . . C5A C 0.1702(7) 0.0702(3) 0.4583(8) 0.085(3) Uani 1 1 d . . . C6A C 0.2418(9) 0.0515(3) 0.4952(8) 0.088(3) Uani 1 1 d . . . C7A C 0.4433(7) 0.0731(3) 0.5742(8) 0.083(2) Uani 1 1 d . . . N4A N 0.5836(6) 0.0842(2) 0.6277(6) 0.083(2) Uani 1 1 d . . . C8A C 0.5281(7) 0.0590(3) 0.6136(8) 0.078(2) Uani 1 1 d . . . C9A C 0.5761(10) 0.0286(3) 0.6479(10) 0.120(4) Uani 1 1 d . . . H9A H 0.5550 0.0068 0.6470 0.144 Uiso 1 1 calc R . . C10A C 0.6611(9) 0.0342(4) 0.6847(9) 0.111(4) Uani 1 1 d . . . N5A N 0.6624(6) 0.0691(3) 0.6684(7) 0.095(2) Uani 1 1 d . . . C11A C 0.7229(8) 0.0060(3) 0.7253(10) 0.134(4) Uani 1 1 d . . . H11D H 0.7773 0.0146 0.7460 0.201 Uiso 1 1 calc R . . H11E H 0.6904 -0.0108 0.6540 0.201 Uiso 1 1 calc R . . H11F H 0.7430 -0.0050 0.8033 0.201 Uiso 1 1 calc R . . N6A N 0.7062(5) 0.1253(3) 0.6828(7) 0.101(3) Uani 1 1 d . . . C12A C 0.7289(7) 0.0911(4) 0.6947(8) 0.101(4) Uani 1 1 d . . . C13A C 0.8114(8) 0.0799(4) 0.7312(10) 0.128(4) Uani 1 1 d . . . H29 H 0.8249 0.0562 0.7399 0.153 Uiso 1 1 calc R . . C14A C 0.8726(13) 0.1044(5) 0.7542(15) 0.165(7) Uani 1 1 d . . . H30 H 0.9279 0.0975 0.7789 0.198 Uiso 1 1 calc R . . C15A C 0.8504(9) 0.1379(5) 0.7402(12) 0.147(6) Uani 1 1 d . . . H31 H 0.8909 0.1543 0.7533 0.176 Uiso 1 1 calc R . . C16A C 0.7682(8) 0.1506(3) 0.7063(9) 0.121(4) Uani 1 1 d . . . H32 H 0.7560 0.1744 0.7000 0.145 Uiso 1 1 calc R . . N100 N 0.4278(8) 0.3045(3) 0.4514(12) 0.132(3) Uani 1 1 d . . . O100 O 0.4112(5) 0.2922(2) 0.5230(8) 0.143(3) Uani 1 1 d . . . O101 O 0.4872(7) 0.3308(3) 0.4932(9) 0.161(3) Uani 1 1 d . . . O102 O 0.3816(6) 0.2897(2) 0.3279(9) 0.144(3) Uani 1 1 d . . . N200 N 0.3669(9) 0.2391(3) 0.0282(13) 0.136(3) Uani 1 1 d . . . O200 O 0.3433(7) 0.2104(3) -0.0433(10) 0.171(3) Uani 1 1 d . . . O201 O 0.4572(8) 0.2465(2) 0.1394(11) 0.178(3) Uani 1 1 d . . . O202 O 0.2981(8) 0.2610(3) -0.0083(10) 0.183(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0520(6) 0.1155(9) 0.0614(6) -0.0031(6) 0.0393(5) -0.0006(5) Cu2 0.0630(6) 0.1139(9) 0.0523(6) 0.0040(5) 0.0404(5) 0.0049(6) N2 0.066(4) 0.109(6) 0.081(5) 0.024(5) 0.051(4) 0.007(4) N3 0.099(6) 0.106(7) 0.089(6) -0.010(6) 0.063(5) -0.002(5) N7 0.103(7) 0.143(9) 0.160(9) 0.025(7) 0.071(6) 0.008(6) N2A 0.094(6) 0.083(5) 0.078(5) 0.000(4) 0.064(5) -0.015(5) N3A 0.098(6) 0.091(6) 0.091(5) 0.002(4) 0.067(5) 0.003(5) N7A 0.175(9) 0.136(9) 0.152(8) -0.017(6) 0.124(8) -0.030(7) O2 0.086(4) 0.063(4) 0.083(4) -0.007(3) 0.061(3) 0.001(3) O1 0.079(4) 0.067(4) 0.082(4) -0.008(3) 0.056(3) -0.007(3) N1 0.067(5) 0.138(8) 0.074(5) 0.002(5) 0.053(4) 0.011(5) C1 0.086(7) 0.175(11) 0.085(7) -0.023(8) 0.061(6) -0.013(7) C2 0.129(10) 0.198(14) 0.091(9) -0.019(9) 0.082(8) -0.029(10) C3 0.080(8) 0.215(16) 0.080(9) 0.023(10) 0.044(7) 0.013(9) C4 0.070(6) 0.187(12) 0.072(7) 0.049(8) 0.042(6) 0.019(7) C5 0.054(5) 0.136(11) 0.080(8) 0.022(7) 0.049(6) 0.008(6) C6 0.067(6) 0.099(9) 0.106(9) 0.017(8) 0.059(7) 0.005(6) C7 0.072(6) 0.075(7) 0.090(7) 0.004(6) 0.055(6) -0.006(5) N4 0.064(4) 0.098(6) 0.087(5) -0.023(5) 0.057(4) -0.023(4) C8 0.066(5) 0.101(8) 0.078(6) -0.028(7) 0.052(5) -0.019(5) C9 0.101(8) 0.102(9) 0.132(10) -0.039(8) 0.084(8) -0.031(6) C10 0.088(8) 0.125(11) 0.159(12) -0.071(10) 0.101(9) -0.043(7) N5 0.058(5) 0.132(9) 0.082(7) -0.050(6) 0.045(5) -0.031(5) C11 0.095(8) 0.138(10) 0.159(10) -0.068(9) 0.079(8) -0.040(7) N6 0.056(5) 0.159(8) 0.078(6) -0.008(6) 0.050(4) -0.006(5) C12 0.052(6) 0.180(13) 0.063(7) -0.028(8) 0.038(6) -0.014(7) C13 0.095(8) 0.182(13) 0.099(9) -0.044(9) 0.070(7) -0.034(8) C14 0.091(9) 0.27(2) 0.082(10) -0.001(13) 0.046(8) -0.022(13) C15 0.113(10) 0.25(2) 0.074(10) 0.043(11) 0.053(8) 0.027(12) C16 0.069(7) 0.199(13) 0.080(8) 0.028(8) 0.038(6) 0.030(7) N1A 0.077(5) 0.126(7) 0.053(4) 0.007(4) 0.043(4) 0.005(5) C1A 0.088(7) 0.157(10) 0.080(6) 0.017(6) 0.058(6) 0.020(8) C2A 0.079(8) 0.201(15) 0.111(9) -0.007(10) 0.055(7) 0.012(9) C3A 0.120(10) 0.204(16) 0.108(9) 0.010(10) 0.090(9) -0.011(11) C4A 0.110(9) 0.167(12) 0.093(7) -0.008(7) 0.078(7) -0.035(9) C5A 0.080(7) 0.121(10) 0.053(5) -0.003(6) 0.046(5) -0.022(7) C6A 0.103(8) 0.103(9) 0.055(5) -0.011(5) 0.055(6) -0.019(7) C7A 0.099(7) 0.065(7) 0.078(6) -0.004(5) 0.060(6) 0.007(6) N4A 0.083(5) 0.099(6) 0.048(4) -0.007(4) 0.039(4) 0.015(5) C8A 0.087(7) 0.079(7) 0.068(5) 0.000(5) 0.055(5) 0.018(7) C9A 0.128(10) 0.075(8) 0.096(8) -0.017(6) 0.057(8) 0.003(7) C10A 0.109(10) 0.140(12) 0.059(6) -0.010(7) 0.050(7) 0.029(9) N5A 0.098(7) 0.123(8) 0.071(5) 0.006(5) 0.063(5) 0.037(7) C11A 0.158(10) 0.151(10) 0.111(8) 0.009(7) 0.101(8) 0.061(9) N6A 0.078(5) 0.154(9) 0.061(5) 0.006(5) 0.045(4) 0.017(6) C12A 0.073(7) 0.188(14) 0.057(6) -0.004(7) 0.051(6) 0.019(9) C13A 0.098(9) 0.176(13) 0.108(8) -0.005(8) 0.073(7) 0.030(8) C14A 0.140(14) 0.26(2) 0.131(11) -0.006(13) 0.109(11) 0.019(15) C15A 0.083(9) 0.263(19) 0.114(9) 0.011(12) 0.076(8) -0.019(11) C16A 0.118(9) 0.183(12) 0.082(7) 0.018(7) 0.078(7) -0.005(9) N100 0.140(9) 0.129(9) 0.140(10) -0.007(8) 0.103(8) -0.004(7) O100 0.142(7) 0.133(7) 0.151(7) 0.001(5) 0.102(6) 0.002(5) O101 0.165(8) 0.157(8) 0.166(8) 0.004(6) 0.118(7) 0.008(6) O102 0.139(6) 0.143(7) 0.151(7) 0.008(6) 0.103(6) 0.009(5) N200 0.144(11) 0.140(11) 0.143(10) 0.003(9) 0.109(9) 0.005(9) O200 0.174(8) 0.166(9) 0.182(9) 0.001(7) 0.128(8) 0.004(7) O201 0.195(10) 0.162(8) 0.185(9) 0.001(7) 0.137(9) -0.002(8) O202 0.179(9) 0.197(10) 0.170(8) -0.007(7) 0.123(8) -0.012(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 1.895(7) . ? Cu1 N2A 1.983(7) 2_656 ? Cu1 O2 2.064(5) 2_656 ? Cu1 N1A 2.086(7) 2_656 ? Cu1 N6 2.329(8) . ? Cu1 O1 2.376(5) . ? Cu2 N4A 1.913(7) . ? Cu2 N2 1.998(8) . ? Cu2 O1 2.070(5) . ? Cu2 N1 2.070(7) . ? Cu2 N6A 2.348(8) . ? Cu2 O2 2.388(5) . ? N2 C6 1.270(11) . ? N2 N3 1.362(9) . ? N3 C7 1.396(10) . ? N7 C6 1.532(12) . ? N7 H7A 0.8600 . ? N7 H7B 0.8600 . ? N2A C6A 1.273(11) . ? N2A N3A 1.342(9) . ? N2A Cu1 1.983(7) 2_656 ? N3A C7A 1.400(11) . ? N7A C6A 1.547(12) . ? N7A H14A 0.8600 . ? N7A H14B 0.8600 . ? O2 C7A 1.254(9) . ? O2 Cu1 2.064(5) 2_656 ? O1 C7 1.256(9) . ? N1 C1 1.376(11) . ? N1 C5 1.388(11) . ? C1 C2 1.402(14) . ? C1 H1 0.9300 . ? C2 C3 1.398(15) . ? C2 H2 0.9300 . ? C3 C4 1.376(15) . ? C3 H3 0.9300 . ? C4 C5 1.388(12) . ? C4 H4 0.9300 . ? C5 C6 1.318(12) . ? C7 C8 1.460(11) . ? N4 N5 1.376(9) . ? N4 C8 1.385(10) . ? C8 C9 1.388(12) . ? C9 C10 1.413(14) . ? C9 H9 0.9300 . ? C10 C11 1.375(13) . ? C10 N5 1.382(13) . ? N5 C12 1.396(12) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? N6 C12 1.355(12) . ? N6 C16 1.399(12) . ? C12 C13 1.394(13) . ? C13 C14 1.379(17) . ? C13 H13 0.9300 . ? C14 C15 1.348(18) . ? C14 H14 0.9300 . ? C15 C16 1.408(16) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? N1A C1A 1.378(11) . ? N1A C5A 1.382(11) . ? N1A Cu1 2.086(7) 2_656 ? C1A C2A 1.41(3) . ? C1A H1A 0.9300 . ? C2A C3A 1.392(15) . ? C2A H2A 0.9300 . ? C3A C4A 1.368(15) . ? C3A H3A 0.9300 . ? C4A C5A 1.381(12) . ? C4A H4A 0.9300 . ? C5A C6A 1.330(12) . ? C7A C8A 1.460(11) . ? N4A N5A 1.361(9) . ? N4A C8A 1.370(10) . ? C8A C9A 1.359(12) . ? C9A C10A 1.39(3) . ? C9A H9A 0.9300 . ? C10A N5A 1.357(13) . ? C10A C11A 1.419(13) . ? N5A C12A 1.381(13) . ? C11A H11D 0.9600 . ? C11A H11E 0.9600 . ? C11A H11F 0.9600 . ? N6A C12A 1.352(12) . ? N6A C16A 1.411(12) . ? C12A C13A 1.399(13) . ? C13A C14A 1.380(17) . ? C13A H29 0.9300 . ? C14A C15A 1.326(18) . ? C14A H30 0.9300 . ? C15A C16A 1.429(15) . ? C15A H31 0.9300 . ? C16A H32 0.9300 . ? N100 O101 1.332(11) . ? N100 O100 1.349(11) . ? N100 O102 1.390(11) . ? N200 O200 1.329(12) . ? N200 O201 1.338(13) . ? N200 O202 1.359(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N2A 175.7(3) . 2_656 ? N4 Cu1 O2 99.2(2) . 2_656 ? N2A Cu1 O2 77.2(3) 2_656 2_656 ? N4 Cu1 N1A 105.7(3) . 2_656 ? N2A Cu1 N1A 78.0(4) 2_656 2_656 ? O2 Cu1 N1A 154.7(3) 2_656 2_656 ? N4 Cu1 N6 72.0(4) . . ? N2A Cu1 N6 105.5(3) 2_656 . ? O2 Cu1 N6 92.2(2) 2_656 . ? N1A Cu1 N6 99.2(2) 2_656 . ? N4 Cu1 O1 74.0(3) . . ? N2A Cu1 O1 108.4(2) 2_656 . ? O2 Cu1 O1 91.83(18) 2_656 . ? N1A Cu1 O1 91.2(2) 2_656 . ? N6 Cu1 O1 145.9(3) . . ? N4A Cu2 N2 175.9(3) . . ? N4A Cu2 O1 99.1(2) . . ? N2 Cu2 O1 77.5(3) . . ? N4A Cu2 N1 105.3(3) . . ? N2 Cu2 N1 78.3(4) . . ? O1 Cu2 N1 155.3(3) . . ? N4A Cu2 N6A 71.8(4) . . ? N2 Cu2 N6A 105.7(3) . . ? O1 Cu2 N6A 90.9(2) . . ? N1 Cu2 N6A 100.4(2) . . ? N4A Cu2 O2 74.0(3) . . ? N2 Cu2 O2 108.3(2) . . ? O1 Cu2 O2 92.01(18) . . ? N1 Cu2 O2 90.8(2) . . ? N6A Cu2 O2 145.7(3) . . ? C6 N2 N3 126.1(9) . . ? C6 N2 Cu2 113.9(7) . . ? N3 N2 Cu2 120.0(6) . . ? N2 N3 C7 105.1(7) . . ? C6 N7 H7A 120.0 . . ? C6 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? C6A N2A N3A 124.8(9) . . ? C6A N2A Cu1 114.6(7) . 2_656 ? N3A N2A Cu1 120.5(6) . 2_656 ? N2A N3A C7A 105.9(7) . . ? C6A N7A H14A 120.0 . . ? C6A N7A H14B 120.0 . . ? H14A N7A H14B 120.0 . . ? C7A O2 Cu1 110.0(5) . 2_656 ? C7A O2 Cu2 109.0(6) . . ? Cu1 O2 Cu2 141.0(3) 2_656 . ? C7 O1 Cu2 109.2(5) . . ? C7 O1 Cu1 109.2(5) . . ? Cu2 O1 Cu1 141.6(3) . . ? C1 N1 C5 121.4(9) . . ? C1 N1 Cu2 127.4(8) . . ? C5 N1 Cu2 111.2(6) . . ? N1 C1 C2 119.4(11) . . ? N1 C1 H1 120.3 . . ? C2 C1 H1 120.3 . . ? C3 C2 C1 119.4(12) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C4 C3 C2 120.1(12) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.7(12) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 N1 113.6(9) . . ? C6 C5 C4 127.4(14) . . ? N1 C5 C4 118.9(12) . . ? N2 C6 C5 122.5(10) . . ? N2 C6 N7 120.8(11) . . ? C5 C6 N7 116.1(11) . . ? O1 C7 N3 128.1(9) . . ? O1 C7 C8 119.5(9) . . ? N3 C7 C8 112.4(10) . . ? N5 N4 C8 107.9(8) . . ? N5 N4 Cu1 126.4(8) . . ? C8 N4 Cu1 125.4(6) . . ? N4 C8 C9 108.0(8) . . ? N4 C8 C7 111.7(9) . . ? C9 C8 C7 140.3(12) . . ? C8 C9 C10 108.1(10) . . ? C8 C9 H9 125.9 . . ? C10 C9 H9 125.9 . . ? C11 C10 N5 134.7(14) . . ? C11 C10 C9 119.0(14) . . ? N5 C10 C9 106.3(10) . . ? N4 N5 C10 109.7(9) . . ? N4 N5 C12 116.0(10) . . ? C10 N5 C12 134.3(10) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 N6 C16 117.8(10) . . ? C12 N6 Cu1 113.5(7) . . ? C16 N6 Cu1 128.5(9) . . ? N6 C12 C13 122.8(13) . . ? N6 C12 N5 111.8(9) . . ? C13 C12 N5 125.4(14) . . ? C14 C13 C12 118.1(14) . . ? C14 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? C15 C14 C13 121.4(16) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 119.7(16) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? N6 C16 C15 120.2(13) . . ? N6 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C1A N1A C5A 121.3(9) . . ? C1A N1A Cu1 127.1(8) . 2_656 ? C5A N1A Cu1 111.5(6) . 2_656 ? N1A C1A C2A 119.2(11) . . ? N1A C1A H1A 120.4 . . ? C2A C1A H1A 120.4 . . ? C3A C2A C1A 118.8(12) . . ? C3A C2A H2A 120.6 . . ? C1A C2A H2A 120.6 . . ? C4A C3A C2A 120.8(13) . . ? C4A C3A H3A 119.6 . . ? C2A C3A H3A 119.6 . . ? C3A C4A C5A 120.7(12) . . ? C3A C4A H4A 119.6 . . ? C5A C4A H4A 119.6 . . ? C6A C5A C4A 127.6(13) . . ? C6A C5A N1A 113.1(9) . . ? C4A C5A N1A 119.2(11) . . ? N2A C6A C5A 122.4(10) . . ? N2A C6A N7A 121.6(10) . . ? C5A C6A N7A 115.9(11) . . ? O2 C7A N3A 126.4(8) . . ? O2 C7A C8A 119.1(9) . . ? N3A C7A C8A 114.5(9) . . ? N5A N4A C8A 109.7(8) . . ? N5A N4A Cu2 125.7(8) . . ? C8A N4A Cu2 124.4(7) . . ? C9A C8A N4A 104.8(9) . . ? C9A C8A C7A 141.8(12) . . ? N4A C8A C7A 113.3(9) . . ? C8A C9A C10A 111.5(11) . . ? C8A C9A H9A 124.3 . . ? C10A C9A H9A 124.3 . . ? N5A C10A C9A 104.5(10) . . ? N5A C10A C11A 134.5(13) . . ? C9A C10A C11A 120.9(15) . . ? C10A N5A N4A 109.5(10) . . ? C10A N5A C12A 133.0(11) . . ? N4A N5A C12A 117.3(10) . . ? C10A C11A H11D 109.5 . . ? C10A C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? C10A C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? C12A N6A C16A 118.2(10) . . ? C12A N6A Cu2 112.6(7) . . ? C16A N6A Cu2 129.0(9) . . ? N6A C12A N5A 112.5(9) . . ? N6A C12A C13A 122.9(13) . . ? N5A C12A C13A 124.7(14) . . ? C14A C13A C12A 119.6(14) . . ? C14A C13A H29 120.2 . . ? C12A C13A H29 120.2 . . ? C15A C14A C13A 118.3(17) . . ? C15A C14A H30 120.9 . . ? C13A C14A H30 120.9 . . ? C14A C15A C16A 124.0(16) . . ? C14A C15A H31 118.0 . . ? C16A C15A H31 118.0 . . ? N6A C16A C15A 117.0(12) . . ? N6A C16A H32 121.5 . . ? C15A C16A H32 121.5 . . ? O101 N100 O100 122.8(11) . . ? O101 N100 O102 117.3(11) . . ? O100 N100 O102 119.8(11) . . ? O200 N200 O201 121.7(12) . . ? O200 N200 O202 119.8(12) . . ? O201 N200 O202 118.4(12) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 20.41 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.255 _refine_diff_density_min -0.213 _refine_diff_density_rms 0.046 # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.012 214 94 ' ' 2 0.500 0.500 0.074 214 94 ' ' 3 0.500 0.046 0.250 85 80 ' ' 4 1.000 0.546 0.250 85 80 ' ' 5 0.906 0.203 0.222 9 50 ' ' 6 0.406 0.703 0.222 9 50 ' ' 7 0.094 0.203 0.278 9 50 ' ' 8 0.594 0.703 0.278 9 50 ' ' 9 1.000 0.454 0.750 85 80 ' ' 10 0.500 0.954 0.750 85 80 ' ' 11 0.406 0.297 0.722 9 50 ' ' 12 0.906 0.797 0.722 9 50 ' ' 13 0.594 0.297 0.778 9 50 ' ' 14 0.094 0.797 0.778 9 50 ' ' _platon_squeeze_details ; ; data_sksr25 _database_code_depnum_ccdc_archive 'CCDC 796247' #TrackingRef 'Rev CIF 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H88 Cl4 Cu8 N48 O24, 4(Cl O4)' _chemical_formula_sum 'C88 H88 Cl8 Cu8 N48 O40' _chemical_formula_weight 3250.07 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.745(1) _cell_length_b 21.597(1) _cell_length_c 26.180(2) _cell_angle_alpha 90.00 _cell_angle_beta 121.57(1) _cell_angle_gamma 90.00 _cell_volume 7103.1(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 58450 _cell_measurement_theta_min 4.7 _cell_measurement_theta_max 32.5 _exptl_crystal_description Rectangular _exptl_crystal_colour Green _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3280 _exptl_absorpt_coefficient_mu 1.413 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8195 _exptl_absorpt_correction_T_max 0.8401 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58450 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.1535 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 4.69 _diffrn_reflns_theta_max 32.48 _reflns_number_total 25170 _reflns_number_gt 15143 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX V1.80.05' _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^ > 2\s(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^)+(0.1886P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 25170 _refine_ls_number_parameters 869 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1792 _refine_ls_R_factor_gt 0.0992 _refine_ls_wR_factor_ref 0.3486 _refine_ls_wR_factor_gt 0.2698 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.004 _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 0.53547(6) 0.00067(3) 0.33340(3) 0.0453(2) Uani 1 1 d . . . Cu3 Cu 0.33335(7) -0.00228(3) 0.08849(3) 0.0520(2) Uani 1 1 d . . . Cu4 Cu 0.30068(7) -0.10226(3) 0.20686(3) 0.0537(2) Uani 1 1 d . . . Cu2 Cu 0.64366(7) 0.02019(3) 0.22195(3) 0.0499(2) Uani 1 1 d . . . Cl2 Cl 0.2261(2) -0.09088(9) 0.53420(9) 0.0789(6) Uani 1 1 d . . . Cl1 Cl 0.7505(2) -0.17199(9) 0.53803(10) 0.0826(6) Uani 1 1 d . . . O4 O 0.4453(3) -0.08458(17) 0.27328(18) 0.0498(9) Uani 1 1 d . . . O1 O 0.5627(4) 0.04153(16) 0.27594(17) 0.0476(10) Uani 1 1 d . . . O2 O 0.5198(4) -0.02125(16) 0.15474(17) 0.0492(10) Uani 1 1 d . . . C30 C 0.2222(5) 0.02213(19) 0.2012(2) 0.0422(13) Uani 1 1 d . . . O3 O 0.2941(4) -0.02026(16) 0.14883(16) 0.0466(9) Uani 1 1 d . . . N24 N 0.7468(4) -0.0684(2) 0.4005(2) 0.0494(11) Uani 1 1 d . . . H24 H 0.7820 -0.0391 0.4254 0.059 Uiso 1 1 calc R . . N3 N 0.4603(4) 0.0762(2) 0.3212(2) 0.0490(11) Uani 1 1 d . . . N5 N 0.5947(4) 0.1055(2) 0.2002(2) 0.0507(12) Uani 1 1 d . . . N1 N 0.4722(5) -0.0153(2) 0.3857(2) 0.0553(13) Uani 1 1 d . . . N23 N 0.6399(4) -0.0662(2) 0.35682(19) 0.0447(10) Uani 1 1 d . . . N2 N 0.3824(6) 0.1429(2) 0.3554(3) 0.0751(18) Uani 1 1 d . . . H2A H 0.3826 0.1736 0.3346 0.068 Uiso 1 1 calc R . . H2B H 0.3569 0.1474 0.3782 0.068 Uiso 1 1 calc R . . N17 N 0.2283(4) -0.0339(2) 0.2223(2) 0.0522(12) Uani 1 1 d . . . N6 N 0.5961(5) 0.1454(2) 0.1625(2) 0.0600(14) Uani 1 1 d . . . H6N H 0.6266 0.1391 0.1425 0.072 Uiso 1 1 calc R . . C41 C 0.6212(6) -0.1198(3) 0.3266(3) 0.0526(15) Uani 1 1 d . . . C40 C 0.5098(5) -0.1259(2) 0.2776(2) 0.0440(12) Uani 1 1 d . . . N21 N 0.3772(5) -0.1716(2) 0.2013(2) 0.0572(14) Uani 1 1 d . . . N4 N 0.4693(4) 0.1207(2) 0.2853(2) 0.0527(12) Uani 1 1 d . . . N22 N 0.4842(4) -0.1740(2) 0.2423(2) 0.0483(11) Uani 1 1 d . . . C7 C 0.5217(5) 0.0968(2) 0.2625(2) 0.0398(12) Uani 1 1 d . . . C18 C 0.5418(5) -0.0771(3) 0.1524(3) 0.0487(13) Uani 1 1 d . . . N16 N 0.2624(5) 0.0854(2) 0.1405(2) 0.0528(12) Uani 1 1 d . . . N9 N 0.6986(5) -0.0620(3) 0.2307(2) 0.0589(14) Uani 1 1 d . . . C29 C 0.2635(4) 0.0294(3) 0.1618(3) 0.0434(12) Uani 1 1 d . . . N15 N 0.2985(5) 0.0780(2) 0.1012(2) 0.0577(14) Uani 1 1 d . . . N10 N 0.6313(5) -0.1056(2) 0.1883(2) 0.0554(13) Uani 1 1 d . . . N11 N 0.3595(5) -0.0875(2) 0.0726(3) 0.0598(14) Uani 1 1 d . . . C8 C 0.5369(5) 0.1333(2) 0.2207(2) 0.0429(12) Uani 1 1 d . . . C19 C 0.4530(6) -0.1156(2) 0.1028(3) 0.0514(14) Uani 1 1 d . . . N18 N 0.1847(6) -0.0324(3) 0.2567(2) 0.0694(16) Uani 1 1 d . . . H18N H 0.1794 -0.0632 0.2758 0.083 Uiso 1 1 calc R . . N12 N 0.2947(6) -0.1285(3) 0.0293(3) 0.0748(19) Uani 1 1 d . . . H12N H 0.2282 -0.1221 0.0039 0.090 Uiso 1 1 calc R . . N19 N 0.1772(6) -0.1486(3) 0.1391(3) 0.0787(19) Uani 1 1 d . . . C15 C 0.9547(7) -0.0165(4) 0.3568(3) 0.0693(19) Uani 1 1 d . . . H15 H 0.9960 -0.0522 0.3687 0.083 Uiso 1 1 calc R . . C16 C 0.8549(6) -0.0185(3) 0.3084(3) 0.0523(14) Uani 1 1 d . . . N13 N 0.3503(5) 0.0455(3) 0.0272(3) 0.0664(15) Uani 1 1 d . . . N14 N 0.2570(5) 0.1811(2) 0.0684(2) 0.0684(16) Uani 1 1 d . . . H14A H 0.2368 0.1897 0.0931 0.062 Uiso 1 1 calc R . . H14B H 0.2549 0.2091 0.0445 0.062 Uiso 1 1 calc R . . C43 C 0.7868(6) -0.1228(3) 0.3981(3) 0.0565(15) Uani 1 1 d . . . N20 N 0.3633(5) -0.2662(2) 0.1562(2) 0.0665(16) Uani 1 1 d . . . H20A H 0.4304 -0.2727 0.1795 0.060 Uiso 1 1 calc R . . H20B H 0.3241 -0.2932 0.1296 0.060 Uiso 1 1 calc R . . C28 C 0.2918(6) 0.1238(3) 0.0674(3) 0.0586(16) Uani 1 1 d . . . C27 C 0.3230(7) 0.1044(3) 0.0230(3) 0.0669(19) Uani 1 1 d . . . C39 C 0.3196(7) -0.2134(3) 0.1613(3) 0.064(2) Uani 1 1 d . . . C42 C 0.7100(6) -0.1552(3) 0.3522(3) 0.0568(16) Uani 1 1 d . . . H42 H 0.7165 -0.1946 0.3402 0.068 Uiso 1 1 calc R . . N7 N 0.7926(5) 0.0323(3) 0.2902(2) 0.0613(14) Uani 1 1 d . . . C6 C 0.4209(5) 0.0890(3) 0.3525(3) 0.0581(16) Uani 1 1 d . . . C5 C 0.4176(6) 0.0355(3) 0.3862(3) 0.0601(18) Uani 1 1 d . . . C10 C 0.5416(6) 0.1989(3) 0.1595(3) 0.0612(17) Uani 1 1 d . . . C17 C 0.7977(6) -0.0707(3) 0.2677(3) 0.0605(17) Uani 1 1 d . . . C32 C 0.1504(7) 0.0269(4) 0.2557(4) 0.080(2) Uani 1 1 d . . . C9 C 0.5052(6) 0.1926(3) 0.1964(3) 0.0633(18) Uani 1 1 d . . . H9 H 0.4671 0.2214 0.2042 0.076 Uiso 1 1 calc R . . C38 C 0.2050(7) -0.2010(3) 0.1246(3) 0.074(2) Uani 1 1 d . . . N8 N 0.8467(6) -0.1266(4) 0.2731(3) 0.093(2) Uani 1 1 d . . . H8A H 0.8103 -0.1574 0.2510 0.084 Uiso 1 1 calc R . . H8B H 0.9137 -0.1308 0.2986 0.084 Uiso 1 1 calc R . . C1 C 0.4779(8) -0.0670(3) 0.4145(4) 0.082(2) Uani 1 1 d . . . H1 H 0.5225 -0.0991 0.4176 0.098 Uiso 1 1 calc R . . C21 C 0.3452(8) -0.1788(4) 0.0308(3) 0.076(2) Uani 1 1 d . . . C12 C 0.8331(8) 0.0841(5) 0.3208(4) 0.084(2) Uani 1 1 d . . . H12 H 0.7926 0.1201 0.3098 0.101 Uiso 1 1 calc R . . C13 C 0.9429(6) 0.0839(5) 0.3721(4) 0.086(3) Uani 1 1 d . . . H13 H 0.9724 0.1208 0.3925 0.104 Uiso 1 1 calc R . . C23 C 0.3691(9) 0.0208(4) -0.0127(4) 0.086(3) Uani 1 1 d . . . H23 H 0.3857 -0.0210 -0.0100 0.104 Uiso 1 1 calc R . . C20 C 0.4453(7) -0.1738(3) 0.0795(3) 0.067(2) Uani 1 1 d . . . H20 H 0.4982 -0.2038 0.0943 0.081 Uiso 1 1 calc R . . C31 C 0.1783(5) 0.0633(4) 0.2225(3) 0.0624(17) Uani 1 1 d . . . H31 H 0.1694 0.1058 0.2160 0.075 Uiso 1 1 calc R . . C3 C 0.3656(9) -0.0232(4) 0.4433(5) 0.089(3) Uani 1 1 d . . . H3 H 0.3289 -0.0260 0.4632 0.107 Uiso 1 1 calc R . . C4 C 0.3670(7) 0.0322(4) 0.4173(3) 0.075(2) Uani 1 1 d . . . H4 H 0.3337 0.0670 0.4210 0.090 Uiso 1 1 calc R . . C26 C 0.3189(8) 0.1434(4) -0.0191(4) 0.090(3) Uani 1 1 d . . . H26 H 0.3039 0.1853 -0.0199 0.108 Uiso 1 1 calc R . . C2 C 0.4162(9) -0.0723(4) 0.4400(4) 0.091(3) Uani 1 1 d . . . H2 H 0.4103 -0.1102 0.4548 0.109 Uiso 1 1 calc R . . C11 C 0.5302(8) 0.2515(4) 0.1192(5) 0.099(3) Uani 1 1 d . . . H11A H 0.5118 0.2355 0.0807 0.149 Uiso 1 1 calc R . . H11B H 0.5964 0.2736 0.1365 0.149 Uiso 1 1 calc R . . H11C H 0.4753 0.2790 0.1146 0.149 Uiso 1 1 calc R . . C14 C 0.9965(7) 0.0374(6) 0.3889(4) 0.094(3) Uani 1 1 d . . . H14 H 1.0646 0.0379 0.4228 0.112 Uiso 1 1 calc R . . C22 C 0.2904(10) -0.2333(5) -0.0092(5) 0.125(4) Uani 1 1 d . . . H22A H 0.2222 -0.2208 -0.0422 0.188 Uiso 1 1 calc R . . H22B H 0.2810 -0.2652 0.0132 0.188 Uiso 1 1 calc R . . H22C H 0.3330 -0.2489 -0.0242 0.188 Uiso 1 1 calc R . . C25 C 0.3393(11) 0.1157(6) -0.0620(5) 0.121(4) Uani 1 1 d . . . H25 H 0.3346 0.1402 -0.0926 0.145 Uiso 1 1 calc R . . O5 O 0.7640(16) -0.2109(5) 0.5072(8) 0.284(10) Uani 1 1 d . . . C33 C 0.0898(9) 0.0400(7) 0.2867(4) 0.115(4) Uani 1 1 d . . . H33A H 0.0182 0.0249 0.2624 0.172 Uiso 1 1 calc R . . H33B H 0.0885 0.0838 0.2924 0.172 Uiso 1 1 calc R . . H33C H 0.1243 0.0195 0.3249 0.172 Uiso 1 1 calc R . . C37 C 0.1384(10) -0.2374(4) 0.0776(5) 0.123(4) Uani 1 1 d . . . H37 H 0.1609 -0.2745 0.0698 0.147 Uiso 1 1 calc R . . C36 C 0.0390(13) -0.2171(5) 0.0431(10) 0.240(13) Uani 1 1 d . . . H36 H -0.0063 -0.2378 0.0075 0.288 Uiso 1 1 calc R . . C34 C 0.0773(8) -0.1301(5) 0.1081(7) 0.176(8) Uani 1 1 d . . . H34 H 0.0582 -0.0936 0.1190 0.211 Uiso 1 1 calc R . . O11 O 0.2427(13) -0.1224(6) 0.5841(6) 0.216(6) Uani 1 1 d . . . C35 C -0.0015(11) -0.1645(6) 0.0586(8) 0.192(9) Uani 1 1 d . . . H35 H -0.0732 -0.1540 0.0379 0.230 Uiso 1 1 calc R . . O9 O 0.3165(9) -0.0624(11) 0.5553(6) 0.303(12) Uani 1 1 d . . . Cl4 Cl 0.8026(5) 0.0848(4) 0.1446(3) 0.194(2) Uani 1 1 d . . . C24 C 0.3643(12) 0.0568(6) -0.0595(5) 0.125(5) Uani 1 1 d . . . H24N H 0.3784 0.0395 -0.0871 0.150 Uiso 1 1 calc R . . O17 O 0.6949(12) 0.1015(9) 0.1033(7) 0.242(8) Uani 1 1 d . . . O8 O 0.7643(11) -0.1090(3) 0.5272(5) 0.169(5) Uani 1 1 d . . . O7 O 0.809(4) -0.1729(11) 0.6010(11) 0.46(3) Uani 1 1 d . . . O19 O 0.843(2) 0.1332(14) 0.1936(13) 0.352(14) Uani 1 1 d . . . O18 O 0.798(3) 0.0253(13) 0.1725(8) 0.400(19) Uani 1 1 d . . . O20 O 0.8453(16) 0.078(2) 0.1131(8) 0.50(3) Uani 1 1 d . . . C44 C 0.9038(7) -0.1364(4) 0.4437(4) 0.085(2) Uani 1 1 d . . . H44A H 0.9191 -0.1788 0.4400 0.128 Uiso 1 1 calc R . . H44B H 0.9181 -0.1292 0.4834 0.128 Uiso 1 1 calc R . . H44C H 0.9478 -0.1097 0.4363 0.128 Uiso 1 1 calc R . . Cl5 Cl 0.1819(8) -0.1997(7) 0.2797(6) 0.435(12) Uani 1 1 d . . . O13 O 0.245(2) -0.1588(11) 0.2852(11) 0.349(14) Uani 1 1 d . . . O15 O 0.085(2) -0.210(2) 0.244(2) 0.66(5) Uani 1 1 d . . . O16 O 0.196(3) -0.2230(15) 0.3362(12) 0.418(18) Uani 1 1 d . . . O14 O 0.1225(16) -0.1629(12) 0.2903(16) 0.345(17) Uani 1 1 d . . . O12 O 0.1597(13) -0.0402(4) 0.5247(5) 0.253(9) Uani 1 1 d . . . O6 O 0.6694(15) -0.1891(5) 0.5466(9) 0.224(7) Uani 1 1 d . . . O10 O 0.1741(9) -0.1184(8) 0.4850(7) 0.311(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0556(5) 0.0324(3) 0.0511(4) -0.0010(2) 0.0301(4) 0.0043(3) Cu3 0.0622(5) 0.0431(4) 0.0504(4) 0.0033(3) 0.0293(4) 0.0051(3) Cu4 0.0564(5) 0.0343(3) 0.0572(4) -0.0001(3) 0.0205(4) -0.0012(3) Cu2 0.0563(5) 0.0411(4) 0.0524(4) -0.0004(3) 0.0287(4) 0.0040(3) Cl2 0.0894(15) 0.0613(10) 0.0635(10) -0.0015(8) 0.0244(10) -0.0219(10) Cl1 0.1002(17) 0.0654(11) 0.0917(13) -0.0234(9) 0.0567(13) -0.0095(11) O4 0.046(2) 0.0411(19) 0.054(2) -0.0021(16) 0.020(2) 0.0062(18) O1 0.062(3) 0.0329(17) 0.058(2) 0.0148(16) 0.039(2) 0.0101(18) O2 0.058(3) 0.0332(17) 0.051(2) -0.0022(15) 0.025(2) 0.0083(18) C30 0.056(3) 0.0191(19) 0.055(3) 0.0070(18) 0.031(3) 0.023(2) O3 0.064(3) 0.0312(17) 0.049(2) 0.0064(14) 0.032(2) 0.0148(18) N24 0.050(3) 0.043(2) 0.046(2) -0.0060(19) 0.019(2) 0.005(2) N3 0.051(3) 0.045(2) 0.055(3) -0.006(2) 0.030(2) 0.005(2) N5 0.055(3) 0.028(2) 0.053(3) 0.0022(18) 0.017(3) 0.000(2) N1 0.068(4) 0.044(2) 0.065(3) -0.002(2) 0.042(3) -0.009(3) N23 0.051(3) 0.047(2) 0.041(2) -0.0018(18) 0.027(2) 0.009(2) N2 0.115(6) 0.042(3) 0.099(4) -0.002(3) 0.077(4) 0.016(3) N17 0.047(3) 0.040(2) 0.073(3) -0.005(2) 0.034(3) -0.004(2) N6 0.080(4) 0.050(3) 0.060(3) 0.006(2) 0.043(3) -0.003(3) C41 0.071(4) 0.038(3) 0.047(3) 0.007(2) 0.030(3) 0.019(3) C40 0.040(3) 0.035(2) 0.043(3) 0.006(2) 0.012(2) 0.016(2) N21 0.068(4) 0.035(2) 0.051(3) 0.0003(19) 0.019(3) 0.008(2) N4 0.057(3) 0.043(2) 0.053(3) 0.004(2) 0.025(3) 0.005(2) N22 0.045(3) 0.034(2) 0.058(3) -0.0014(19) 0.022(3) 0.004(2) C7 0.056(3) 0.0230(19) 0.043(3) -0.0016(17) 0.028(3) 0.004(2) C18 0.051(4) 0.041(3) 0.047(3) 0.005(2) 0.022(3) 0.002(3) N16 0.067(4) 0.041(2) 0.059(3) -0.001(2) 0.038(3) -0.001(2) N9 0.068(4) 0.054(3) 0.057(3) 0.005(2) 0.034(3) 0.017(3) C29 0.033(3) 0.045(3) 0.054(3) 0.007(2) 0.024(3) -0.006(2) N15 0.091(4) 0.046(2) 0.046(2) 0.007(2) 0.043(3) 0.019(3) N10 0.071(4) 0.039(2) 0.062(3) -0.008(2) 0.039(3) -0.006(3) N11 0.069(4) 0.044(3) 0.071(3) 0.002(2) 0.040(3) 0.003(3) C8 0.045(3) 0.027(2) 0.047(3) 0.0060(18) 0.018(3) 0.009(2) C19 0.063(4) 0.031(2) 0.055(3) -0.003(2) 0.027(3) 0.001(3) N18 0.089(5) 0.067(3) 0.058(3) 0.017(3) 0.042(3) 0.015(3) N12 0.094(5) 0.053(3) 0.065(3) -0.022(3) 0.033(4) -0.022(3) N19 0.065(4) 0.053(3) 0.090(4) -0.011(3) 0.021(4) -0.015(3) C15 0.068(5) 0.087(5) 0.069(4) 0.003(4) 0.048(4) -0.008(4) C16 0.056(4) 0.063(4) 0.048(3) 0.008(3) 0.034(3) 0.006(3) N13 0.065(4) 0.078(4) 0.070(3) 0.011(3) 0.045(3) 0.008(3) N14 0.090(5) 0.050(3) 0.063(3) 0.016(2) 0.039(3) 0.013(3) C43 0.057(4) 0.063(4) 0.046(3) 0.001(3) 0.024(3) 0.007(3) N20 0.075(4) 0.043(3) 0.063(3) -0.016(2) 0.024(3) -0.007(3) C28 0.064(4) 0.052(3) 0.059(4) 0.012(3) 0.032(4) 0.009(3) C27 0.080(5) 0.051(3) 0.078(5) 0.018(3) 0.046(4) 0.013(4) C39 0.102(6) 0.035(3) 0.048(3) -0.003(2) 0.036(4) 0.008(3) C42 0.062(4) 0.034(3) 0.077(4) 0.012(3) 0.039(4) 0.021(3) N7 0.063(4) 0.061(3) 0.055(3) -0.001(2) 0.028(3) -0.004(3) C6 0.042(3) 0.054(3) 0.056(4) 0.009(3) 0.010(3) 0.005(3) C5 0.084(5) 0.051(3) 0.058(4) -0.003(3) 0.046(4) 0.019(3) C10 0.047(4) 0.052(3) 0.072(4) 0.009(3) 0.022(3) 0.002(3) C17 0.063(4) 0.059(4) 0.066(4) 0.019(3) 0.038(4) 0.019(3) C32 0.076(6) 0.093(6) 0.092(5) 0.005(4) 0.059(5) 0.019(5) C9 0.079(5) 0.045(3) 0.072(4) 0.005(3) 0.044(4) -0.001(3) C38 0.085(6) 0.026(2) 0.071(4) 0.017(3) 0.013(4) 0.015(3) N8 0.080(5) 0.089(5) 0.090(5) 0.015(4) 0.031(4) 0.035(4) C1 0.111(7) 0.050(4) 0.098(5) 0.010(4) 0.065(6) -0.013(4) C21 0.087(6) 0.068(5) 0.065(4) -0.010(3) 0.033(4) -0.026(4) C12 0.082(6) 0.091(6) 0.078(5) 0.010(4) 0.040(5) 0.023(5) C13 0.034(4) 0.105(7) 0.098(6) -0.053(5) 0.020(4) -0.003(4) C23 0.122(8) 0.069(5) 0.104(6) -0.003(4) 0.084(6) -0.001(5) C20 0.084(6) 0.032(3) 0.078(4) -0.012(3) 0.037(4) 0.007(3) C31 0.039(3) 0.077(4) 0.065(4) 0.009(3) 0.023(3) 0.003(3) C3 0.128(8) 0.058(4) 0.122(7) 0.014(4) 0.093(7) 0.000(5) C4 0.066(5) 0.083(5) 0.073(4) -0.006(4) 0.034(4) 0.003(4) C26 0.119(8) 0.084(5) 0.075(5) 0.051(4) 0.056(5) 0.011(5) C2 0.130(8) 0.057(4) 0.109(6) 0.017(4) 0.078(7) -0.012(5) C11 0.092(7) 0.080(5) 0.124(7) 0.048(5) 0.056(6) 0.000(5) C14 0.052(5) 0.164(10) 0.066(5) -0.030(6) 0.031(4) 0.005(6) C22 0.117(9) 0.072(5) 0.121(8) -0.045(5) 0.016(7) -0.027(6) C25 0.172(12) 0.122(9) 0.098(7) 0.059(6) 0.091(8) 0.030(8) O5 0.52(3) 0.118(7) 0.51(2) -0.134(11) 0.47(2) -0.105(11) C33 0.091(7) 0.196(13) 0.086(6) 0.008(7) 0.067(6) 0.024(8) C37 0.110(9) 0.059(5) 0.138(9) -0.050(5) 0.023(7) -0.023(6) C36 0.113(11) 0.063(6) 0.33(2) -0.077(10) -0.036(13) -0.016(7) C34 0.040(5) 0.102(8) 0.226(14) -0.077(9) -0.041(7) 0.019(5) O11 0.290(17) 0.181(11) 0.256(14) 0.117(10) 0.197(14) 0.083(11) C35 0.093(9) 0.098(8) 0.245(17) -0.067(10) -0.008(10) 0.026(7) O9 0.110(9) 0.58(3) 0.161(10) 0.082(14) 0.028(7) -0.148(15) Cl4 0.182(5) 0.267(7) 0.147(3) 0.009(4) 0.097(4) 0.059(5) C24 0.194(14) 0.107(8) 0.119(8) 0.036(7) 0.112(10) 0.049(9) O17 0.163(12) 0.37(2) 0.188(12) -0.034(12) 0.084(11) 0.089(13) O8 0.288(14) 0.066(4) 0.209(9) 0.002(5) 0.167(10) -0.023(6) O7 0.84(8) 0.29(3) 0.28(2) -0.108(19) 0.31(4) -0.19(4) O19 0.31(3) 0.45(4) 0.41(3) -0.12(3) 0.27(3) -0.01(2) O18 0.64(5) 0.39(3) 0.181(14) 0.019(16) 0.22(2) -0.18(3) O20 0.25(2) 1.14(8) 0.188(14) 0.03(3) 0.162(15) 0.23(3) C44 0.074(6) 0.064(4) 0.099(6) 0.017(4) 0.033(5) 0.000(4) Cl5 0.149(6) 0.60(2) 0.453(15) 0.423(17) 0.085(9) 0.030(11) O13 0.31(3) 0.31(2) 0.41(3) 0.12(2) 0.17(2) -0.11(2) O15 0.21(3) 0.67(7) 0.65(6) 0.06(5) -0.09(3) -0.28(4) O16 0.52(4) 0.48(4) 0.37(3) 0.22(3) 0.31(3) 0.02(3) O14 0.090(10) 0.28(2) 0.54(4) 0.03(3) 0.080(18) -0.058(13) O12 0.322(18) 0.062(4) 0.161(8) 0.008(5) -0.022(9) 0.055(7) O6 0.302(18) 0.127(8) 0.40(2) -0.070(11) 0.297(19) -0.063(10) O10 0.110(9) 0.288(17) 0.307(17) -0.207(15) -0.050(10) 0.049(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N3 1.902(5) . ? Cu1 O1 1.959(4) . ? Cu1 N23 1.962(5) . ? Cu1 N1 2.051(5) . ? Cu1 O4 2.333(4) . ? Cu3 N15 1.888(5) . ? Cu3 N11 1.969(5) . ? Cu3 O3 1.985(4) . ? Cu3 N13 2.031(6) . ? Cu3 O2 2.396(4) . ? Cu4 N21 1.926(5) . ? Cu4 O4 1.958(4) . ? Cu4 N17 1.983(5) . ? Cu4 N19 2.021(6) . ? Cu4 O3 2.302(4) . ? Cu2 N9 1.915(5) . ? Cu2 N5 1.952(4) . ? Cu2 O2 1.967(4) . ? Cu2 N7 1.994(6) . ? Cu2 O1 2.324(4) . ? Cl2 O10 1.252(11) . ? Cl2 O9 1.299(11) . ? Cl2 O11 1.376(10) . ? Cl2 O12 1.401(12) . ? Cl1 O5 1.251(18) . ? Cl1 O6 1.378(11) . ? Cl1 O7 1.41(2) . ? Cl1 O8 1.427(7) . ? O4 C40 1.266(6) . ? O1 C7 1.300(6) . ? O2 C18 1.258(7) . ? C30 N17 1.315(7) . ? C30 C31 1.378(9) . ? C30 C29 1.455(8) . ? O3 C29 1.276(7) . ? N24 C43 1.332(8) . ? N24 N23 1.380(7) . ? N24 H24 0.8600 . ? N3 C6 1.258(9) . ? N3 N4 1.399(7) . ? N5 N6 1.320(7) . ? N5 C8 1.360(8) . ? N1 C1 1.325(8) . ? N1 C5 1.363(8) . ? N23 C41 1.346(7) . ? N2 C6 1.314(8) . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? N17 N18 1.353(8) . ? N6 C10 1.386(9) . ? N6 H6N 0.8600 . ? C41 C42 1.352(9) . ? C41 C40 1.468(9) . ? C40 N22 1.308(7) . ? N21 C39 1.304(8) . ? N21 N22 1.368(8) . ? N4 C7 1.304(8) . ? C7 C8 1.460(7) . ? C18 N10 1.306(8) . ? C18 C19 1.521(9) . ? N16 C29 1.328(7) . ? N16 N15 1.393(7) . ? N9 C17 1.275(9) . ? N9 N10 1.396(8) . ? N15 C28 1.297(8) . ? N11 C19 1.323(9) . ? N11 N12 1.360(8) . ? C8 C9 1.397(8) . ? C19 C20 1.374(7) . ? N18 C32 1.371(10) . ? N18 H18N 0.8600 . ? N12 C21 1.305(11) . ? N12 H12N 0.8600 . ? N19 C34 1.318(11) . ? N19 C38 1.324(9) . ? C15 C16 1.349(10) . ? C15 C14 1.378(13) . ? C15 H15 0.9300 . ? C16 N7 1.348(9) . ? C16 C17 1.476(10) . ? N13 C27 1.321(9) . ? N13 C23 1.323(10) . ? N14 C28 1.345(8) . ? N14 H14A 0.8600 . ? N14 H14B 0.8600 . ? C43 C42 1.337(9) . ? C43 C44 1.527(11) . ? N20 C39 1.350(8) . ? N20 H20A 0.8600 . ? N20 H20B 0.8600 . ? C28 C27 1.516(10) . ? C27 C26 1.362(9) . ? C39 C38 1.466(11) . ? C42 H42 0.9300 . ? N7 C12 1.321(11) . ? C6 C5 1.472(9) . ? C5 C4 1.364(11) . ? C10 C9 1.334(10) . ? C10 C11 1.499(10) . ? C17 N8 1.376(9) . ? C32 C31 1.385(11) . ? C32 C33 1.516(11) . ? C9 H9 0.9300 . ? C38 C37 1.353(11) . ? N8 H8A 0.8600 . ? N8 H8B 0.8600 . ? C1 C2 1.386(13) . ? C1 H1 0.9300 . ? C21 C20 1.358(11) . ? C21 C22 1.501(11) . ? C12 C13 1.467(12) . ? C12 H12 0.9300 . ? C13 C14 1.210(13) . ? C13 H13 0.9300 . ? C23 C24 1.422(12) . ? C23 H23 0.9300 . ? C20 H20 0.9300 . ? C31 H31 0.9300 . ? C3 C2 1.324(13) . ? C3 C4 1.381(11) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C26 C25 1.437(14) . ? C26 H26 0.9300 . ? C2 H2 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C14 H14 0.9300 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C25 C24 1.317(15) . ? C25 H25 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C37 C36 1.331(18) . ? C37 H37 0.9300 . ? C36 C35 1.43(2) . ? C36 H36 0.9300 . ? C34 C35 1.417(16) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? Cl4 O20 1.28(3) . ? Cl4 O17 1.422(14) . ? Cl4 O18 1.50(2) . ? Cl4 O19 1.51(2) . ? C24 H24N 0.9300 . ? O7 O6 1.82(4) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? Cl5 O13 1.233(19) . ? Cl5 O15 1.25(2) . ? Cl5 O14 1.32(3) . ? Cl5 O16 1.474(18) . ? O15 O14 1.46(6) . ? O16 O14 1.71(3) . ? 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 N3 Cu1 O1 79.67(19) . . ? N3 Cu1 N23 167.7(2) . . ? O1 Cu1 N23 97.40(18) . . ? N3 Cu1 N1 80.0(2) . . ? O1 Cu1 N1 159.5(2) . . ? N23 Cu1 N1 103.0(2) . . ? N3 Cu1 O4 119.15(19) . . ? O1 Cu1 O4 96.38(16) . . ? N23 Cu1 O4 72.94(17) . . ? N1 Cu1 O4 91.15(18) . . ? N15 Cu3 N11 176.2(3) . . ? N15 Cu3 O3 79.61(18) . . ? N11 Cu3 O3 98.98(19) . . ? N15 Cu3 N13 80.2(2) . . ? N11 Cu3 N13 100.9(2) . . ? O3 Cu3 N13 159.5(2) . . ? N15 Cu3 O2 110.2(2) . . ? N11 Cu3 O2 73.5(2) . . ? O3 Cu3 O2 95.32(16) . . ? N13 Cu3 O2 95.1(2) . . ? N21 Cu4 O4 79.1(2) . . ? N21 Cu4 N17 173.3(2) . . ? O4 Cu4 N17 97.2(2) . . ? N21 Cu4 N19 80.9(3) . . ? O4 Cu4 N19 159.7(2) . . ? N17 Cu4 N19 102.4(3) . . ? N21 Cu4 O3 111.87(19) . . ? O4 Cu4 O3 94.95(16) . . ? N17 Cu4 O3 73.80(18) . . ? N19 Cu4 O3 95.4(2) . . ? N9 Cu2 N5 168.2(2) . . ? N9 Cu2 O2 79.7(2) . . ? N5 Cu2 O2 98.06(18) . . ? N9 Cu2 N7 79.4(3) . . ? N5 Cu2 N7 101.7(2) . . ? O2 Cu2 N7 158.9(2) . . ? N9 Cu2 O1 115.56(19) . . ? N5 Cu2 O1 76.12(19) . . ? O2 Cu2 O1 95.88(17) . . ? N7 Cu2 O1 95.9(2) . . ? O10 Cl2 O9 127.0(13) . . ? O10 Cl2 O11 116.8(13) . . ? O9 Cl2 O11 101.4(9) . . ? O10 Cl2 O12 101.2(7) . . ? O9 Cl2 O12 99.8(13) . . ? O11 Cl2 O12 108.4(9) . . ? O5 Cl1 O6 111.7(8) . . ? O5 Cl1 O7 123(2) . . ? O6 Cl1 O7 81.5(18) . . ? O5 Cl1 O8 115.2(7) . . ? O6 Cl1 O8 120.9(8) . . ? O7 Cl1 O8 100.6(11) . . ? C40 O4 Cu4 111.1(3) . . ? C40 O4 Cu1 111.1(4) . . ? Cu4 O4 Cu1 136.40(19) . . ? C7 O1 Cu1 111.6(3) . . ? C7 O1 Cu2 109.4(3) . . ? Cu1 O1 Cu2 139.02(18) . . ? C18 O2 Cu2 109.7(4) . . ? C18 O2 Cu3 110.8(4) . . ? Cu2 O2 Cu3 138.24(18) . . ? N17 C30 C31 111.5(5) . . ? N17 C30 C29 115.9(4) . . ? C31 C30 C29 132.6(5) . . ? C29 O3 Cu3 109.7(3) . . ? C29 O3 Cu4 111.7(3) . . ? Cu3 O3 Cu4 138.30(18) . . ? C43 N24 N23 109.4(5) . . ? C43 N24 H24 125.3 . . ? N23 N24 H24 125.3 . . ? C6 N3 N4 121.6(5) . . ? C6 N3 Cu1 120.5(4) . . ? N4 N3 Cu1 116.7(4) . . ? N6 N5 C8 105.3(4) . . ? N6 N5 Cu2 133.3(4) . . ? C8 N5 Cu2 121.0(4) . . ? C1 N1 C5 122.3(6) . . ? C1 N1 Cu1 127.3(6) . . ? C5 N1 Cu1 110.4(4) . . ? C41 N23 N24 104.6(5) . . ? C41 N23 Cu1 124.3(4) . . ? N24 N23 Cu1 130.7(3) . . ? C6 N2 H2A 120.0 . . ? C6 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C30 N17 N18 107.8(5) . . ? C30 N17 Cu4 121.7(4) . . ? N18 N17 Cu4 130.4(4) . . ? N5 N6 C10 110.6(5) . . ? N5 N6 H6N 124.7 . . ? C10 N6 H6N 124.7 . . ? N23 C41 C42 110.3(6) . . ? N23 C41 C40 112.5(5) . . ? C42 C41 C40 137.1(6) . . ? O4 C40 N22 124.9(5) . . ? O4 C40 C41 117.4(5) . . ? N22 C40 C41 117.8(5) . . ? C39 N21 N22 127.1(6) . . ? C39 N21 Cu4 116.0(5) . . ? N22 N21 Cu4 116.8(3) . . ? C7 N4 N3 108.8(4) . . ? C40 N22 N21 108.2(5) . . ? O1 C7 N4 122.9(5) . . ? O1 C7 C8 117.8(5) . . ? N4 C7 C8 119.3(4) . . ? O2 C18 N10 127.3(6) . . ? O2 C18 C19 116.0(5) . . ? N10 C18 C19 116.8(5) . . ? C29 N16 N15 106.3(5) . . ? C17 N9 N10 124.0(6) . . ? C17 N9 Cu2 118.2(5) . . ? N10 N9 Cu2 116.7(4) . . ? O3 C29 N16 125.6(5) . . ? O3 C29 C30 115.8(4) . . ? N16 C29 C30 118.5(5) . . ? C28 N15 N16 119.8(5) . . ? C28 N15 Cu3 120.7(4) . . ? N16 N15 Cu3 118.6(4) . . ? C18 N10 N9 106.5(5) . . ? C19 N11 N12 104.9(5) . . ? C19 N11 Cu3 124.1(5) . . ? N12 N11 Cu3 130.9(5) . . ? N5 C8 C9 110.8(5) . . ? N5 C8 C7 115.4(4) . . ? C9 C8 C7 133.7(6) . . ? N11 C19 C20 109.6(6) . . ? N11 C19 C18 114.9(5) . . ? C20 C19 C18 135.5(7) . . ? N17 N18 C32 108.0(6) . . ? N17 N18 H18N 126.0 . . ? C32 N18 H18N 126.0 . . ? C21 N12 N11 112.0(7) . . ? C21 N12 H12N 124.0 . . ? N11 N12 H12N 124.0 . . ? C34 N19 C38 119.8(7) . . ? C34 N19 Cu4 126.3(6) . . ? C38 N19 Cu4 113.8(6) . . ? C16 C15 C14 121.3(9) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? N7 C16 C15 120.8(7) . . ? N7 C16 C17 110.0(6) . . ? C15 C16 C17 129.2(7) . . ? C27 N13 C23 120.1(7) . . ? C27 N13 Cu3 113.4(5) . . ? C23 N13 Cu3 125.6(6) . . ? C28 N14 H14A 120.0 . . ? C28 N14 H14B 120.0 . . ? H14A N14 H14B 120.0 . . ? N24 C43 C42 108.5(6) . . ? N24 C43 C44 118.7(6) . . ? C42 C43 C44 132.9(7) . . ? C39 N20 H20A 120.0 . . ? C39 N20 H20B 120.0 . . ? H20A N20 H20B 120.0 . . ? N15 C28 N14 125.5(6) . . ? N15 C28 C27 111.5(6) . . ? N14 C28 C27 122.9(6) . . ? N13 C27 C26 123.1(8) . . ? N13 C27 C28 113.9(6) . . ? C26 C27 C28 123.0(7) . . ? N21 C39 N20 121.3(7) . . ? N21 C39 C38 116.2(6) . . ? N20 C39 C38 122.4(6) . . ? C43 C42 C41 107.1(6) . . ? C43 C42 H42 126.4 . . ? C41 C42 H42 126.4 . . ? C12 N7 C16 117.8(7) . . ? C12 N7 Cu2 126.2(6) . . ? C16 N7 Cu2 115.9(5) . . ? N3 C6 N2 126.5(6) . . ? N3 C6 C5 112.8(6) . . ? N2 C6 C5 120.6(7) . . ? N1 C5 C4 118.3(7) . . ? N1 C5 C6 114.9(6) . . ? C4 C5 C6 126.8(7) . . ? C9 C10 N6 108.3(6) . . ? C9 C10 C11 130.4(7) . . ? N6 C10 C11 121.3(7) . . ? N9 C17 N8 122.6(7) . . ? N9 C17 C16 115.5(6) . . ? N8 C17 C16 121.7(7) . . ? N18 C32 C31 108.4(7) . . ? N18 C32 C33 118.6(9) . . ? C31 C32 C33 133.0(9) . . ? C10 C9 C8 104.9(6) . . ? C10 C9 H9 127.5 . . ? C8 C9 H9 127.5 . . ? N19 C38 C37 124.8(9) . . ? N19 C38 C39 113.0(6) . . ? C37 C38 C39 121.9(8) . . ? C17 N8 H8A 120.0 . . ? C17 N8 H8B 120.0 . . ? H8A N8 H8B 120.0 . . ? N1 C1 C2 118.8(8) . . ? N1 C1 H1 120.6 . . ? C2 C1 H1 120.6 . . ? N12 C21 C20 106.5(6) . . ? N12 C21 C22 122.8(9) . . ? C20 C21 C22 129.9(9) . . ? N7 C12 C13 119.0(8) . . ? N7 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C14 C13 C12 122.2(8) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? N13 C23 C24 121.5(8) . . ? N13 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C21 C20 C19 106.6(7) . . ? C21 C20 H20 126.7 . . ? C19 C20 H20 126.7 . . ? C30 C31 C32 104.1(7) . . ? C30 C31 H31 127.9 . . ? C32 C31 H31 127.9 . . ? C2 C3 C4 120.5(8) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.5(8) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C27 C26 C25 115.9(8) . . ? C27 C26 H26 122.1 . . ? C25 C26 H26 122.1 . . ? C3 C2 C1 119.9(7) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C14 C15 118.8(9) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C25 C26 122.0(8) . . ? C24 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C36 C37 C38 116.3(11) . . ? C36 C37 H37 121.9 . . ? C38 C37 H37 121.9 . . ? C37 C36 C35 122.8(13) . . ? C37 C36 H36 118.6 . . ? C35 C36 H36 118.6 . . ? N19 C34 C35 121.4(10) . . ? N19 C34 H34 119.3 . . ? C35 C34 H34 119.3 . . ? C34 C35 C36 114.2(12) . . ? C34 C35 H35 122.9 . . ? C36 C35 H35 122.9 . . ? O20 Cl4 O17 105.6(11) . . ? O20 Cl4 O18 112(2) . . ? O17 Cl4 O18 105.8(16) . . ? O20 Cl4 O19 121(2) . . ? O17 Cl4 O19 104.8(12) . . ? O18 Cl4 O19 106.2(14) . . ? C25 C24 C23 117.3(9) . . ? C25 C24 H24N 121.4 . . ? C23 C24 H24N 121.4 . . ? Cl1 O7 O6 48.6(13) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O13 Cl5 O15 136(3) . . ? O13 Cl5 O14 95(2) . . ? O15 Cl5 O14 69(3) . . ? O13 Cl5 O16 115(2) . . ? O15 Cl5 O16 101(3) . . ? O14 Cl5 O16 75.5(18) . . ? Cl5 O15 O14 57.5(19) . . ? Cl5 O16 O14 48.1(13) . . ? Cl5 O14 O15 53(2) . . ? Cl5 O14 O16 56.4(13) . . ? O15 O14 O16 83(2) . . ? Cl1 O6 O7 49.9(10) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 32.48 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.289 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.135 # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.004 0.001 1233 139 ' ' 2 0.449 0.681 0.010 15 1 ' ' 3 0.449 0.819 0.510 15 1 ' ' 4 0.551 0.319 -0.010 15 1 ' ' 5 0.551 0.181 0.490 15 1 ' ' _platon_squeeze_details ; ; # Attachment '- Rev. Complex 3.cif' data_pom_gm _database_code_depnum_ccdc_archive 'CCDC 796248' #TrackingRef '- Rev. Complex 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H56 N28 Ni4 O4, 4(N O3), 4(H2 O), 2(C2 N), 4(O)' _chemical_formula_sum 'C68 H75 N34 Ni4 O24' _chemical_formula_weight 1987.29 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 14.105(9) _cell_length_b 14.105(9) _cell_length_c 38.379(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7636(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3019 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 24.07 _exptl_crystal_description Cubic _exptl_crystal_colour Green _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4056 _exptl_absorpt_coefficient_mu 1.076 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.860 _exptl_absorpt_correction_T_max 0.898 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41211 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 24.07 _reflns_number_total 3019 _reflns_number_gt 2836 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX V1.80.05' _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^)+(0.0479P)^2^+42.3926P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3019 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1284 _refine_ls_wR_factor_gt 0.1256 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 Ni1 Ni 0.80406(3) 0.30358(3) 0.120487(13) 0.0313(2) Uani 1 1 d . . . O1 O 0.87468(18) 0.19267(19) 0.14493(7) 0.0323(6) Uani 1 1 d . . . N1 N 0.7306(2) 0.4342(2) 0.11877(9) 0.0374(8) Uani 1 1 d . . . N2 N 0.7918(2) 0.3363(2) 0.16986(9) 0.0356(8) Uani 1 1 d . . . N3 N 0.8349(2) 0.2789(2) 0.19436(9) 0.0356(8) Uani 1 1 d . . . N4 N 0.9663(2) 0.0722(2) 0.17898(9) 0.0358(8) Uani 1 1 d . . . N5 N 1.0124(2) 0.0086(2) 0.19913(9) 0.0377(8) Uani 1 1 d . . . N6 N 1.0343(2) -0.0646(2) 0.14600(10) 0.0378(8) Uani 1 1 d . . . N7 N 0.7428(3) 0.4423(3) 0.21264(11) 0.0514(10) Uani 1 1 d . . . H7A H 0.7672 0.4089 0.2291 0.062 Uiso 1 1 calc R . . H7B H 0.7139 0.4944 0.2174 0.062 Uiso 1 1 calc R . . C1 C 0.7004(3) 0.4823(3) 0.09056(12) 0.0445(11) Uani 1 1 d . . . H1 H 0.7139 0.4579 0.0686 0.053 Uiso 1 1 calc R . . C2 C 0.6501(3) 0.5666(3) 0.09283(15) 0.0524(12) Uani 1 1 d . . . H2 H 0.6299 0.5980 0.0729 0.063 Uiso 1 1 calc R . . C3 C 0.6311(3) 0.6018(3) 0.12469(15) 0.0524(13) Uani 1 1 d . . . H3 H 0.5975 0.6582 0.1268 0.063 Uiso 1 1 calc R . . C4 C 0.6616(3) 0.5542(3) 0.15448(14) 0.0484(12) Uani 1 1 d . . . H4 H 0.6489 0.5783 0.1766 0.058 Uiso 1 1 calc R . . C5 C 0.7113(3) 0.4698(3) 0.15035(12) 0.0372(10) Uani 1 1 d . . . C6 C 0.7498(3) 0.4133(3) 0.17962(11) 0.0353(9) Uani 1 1 d . . . C7 C 0.8762(3) 0.2077(3) 0.17833(10) 0.0335(9) Uani 1 1 d . . . C8 C 0.9290(3) 0.1372(3) 0.19859(10) 0.0343(9) Uani 1 1 d . . . C9 C 0.9522(3) 0.1176(4) 0.23336(12) 0.0481(11) Uani 1 1 d . . . H9 H 0.9350 0.1535 0.2527 0.058 Uiso 1 1 calc R . . C10 C 1.0048(3) 0.0364(3) 0.23370(12) 0.0456(11) Uani 1 1 d . . . C11 C 1.0487(4) -0.0148(4) 0.26342(14) 0.0675(15) Uani 1 1 d . . . H11A H 1.0813 -0.0699 0.2549 0.101 Uiso 1 1 calc R . . H11B H 1.0003 -0.0338 0.2795 0.101 Uiso 1 1 calc R . . H11C H 1.0930 0.0262 0.2750 0.101 Uiso 1 1 calc R . . C12 C 1.0507(3) -0.0681(3) 0.18059(12) 0.0407(10) Uani 1 1 d . . . C13 C 1.1023(3) -0.1414(3) 0.19593(14) 0.0498(12) Uani 1 1 d . . . H13 H 1.1122 -0.1433 0.2199 0.060 Uiso 1 1 calc R . . C14 C 1.1378(4) -0.2105(4) 0.17459(16) 0.0603(14) Uani 1 1 d . . . H14 H 1.1718 -0.2606 0.1842 0.072 Uiso 1 1 calc R . . C15 C 1.1244(4) -0.2074(4) 0.13970(15) 0.0568(13) Uani 1 1 d . . . H15 H 1.1498 -0.2537 0.1252 0.068 Uiso 1 1 calc R . . C16 C 1.0709(3) -0.1319(3) 0.12593(14) 0.0483(12) Uani 1 1 d . . . H16 H 1.0610 -0.1291 0.1020 0.058 Uiso 1 1 calc R . . O1W O 0.8258(6) 0.3165(5) 0.2690(2) 0.174(3) Uiso 1 1 d . . . H1W1 H 0.8660 0.3266 0.2850 0.208 Uiso 1 1 d R . . H2W1 H 0.7739 0.3007 0.2786 0.208 Uiso 1 1 d R . . N20 N 0.5000 0.7500 0.0658(4) 0.189(11) Uani 1 2 d S . . C20 C 0.5000 0.7500 0.0059(12) 0.30(3) Uani 1 2 d S . . C21 C 0.5000 0.7500 0.0443(13) 0.22(2) Uani 1 2 d S . . N100 N 0.6871(8) 0.6593(14) 0.2472(3) 0.171(6) Uani 1 1 d . . . O100 O 0.7463(8) 0.6507(9) 0.2675(2) 0.201(5) Uani 1 1 d . . . O101 O 0.6385(9) 0.6064(5) 0.2384(3) 0.188(5) Uani 1 1 d . . . O102 O 0.6827(8) 0.7335(13) 0.2297(4) 0.245(7) Uani 1 1 d . . . O2W O 0.9676(8) 0.1809(7) 0.3074(3) 0.222(4) 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 Ni1 0.0288(3) 0.0294(3) 0.0358(3) 0.0004(2) -0.0022(2) 0.0006(2) O1 0.0331(15) 0.0352(15) 0.0284(15) -0.0014(11) 0.0006(11) 0.0008(12) N1 0.0299(18) 0.0375(19) 0.045(2) 0.0039(16) 0.0002(15) 0.0009(15) N2 0.0319(18) 0.0335(18) 0.041(2) 0.0043(15) -0.0008(15) 0.0006(15) N3 0.0358(19) 0.0392(19) 0.0316(18) -0.0005(15) 0.0028(15) 0.0022(15) N4 0.0386(19) 0.0323(18) 0.0365(19) 0.0070(15) -0.0018(15) 0.0015(15) N5 0.0350(19) 0.0352(19) 0.043(2) 0.0089(16) 0.0009(15) 0.0056(15) N6 0.0339(18) 0.0315(18) 0.048(2) 0.0016(16) 0.0027(16) -0.0031(15) N7 0.058(3) 0.043(2) 0.053(2) -0.0031(18) 0.0019(19) 0.0062(19) C1 0.040(2) 0.046(3) 0.048(3) 0.012(2) -0.005(2) -0.004(2) C2 0.045(3) 0.041(3) 0.071(4) 0.014(2) -0.008(2) 0.002(2) C3 0.039(3) 0.035(2) 0.083(4) 0.008(2) -0.009(2) 0.009(2) C4 0.040(2) 0.038(2) 0.066(3) -0.004(2) 0.004(2) 0.006(2) C5 0.028(2) 0.032(2) 0.051(3) -0.0033(19) 0.0009(18) -0.0071(17) C6 0.030(2) 0.032(2) 0.044(2) -0.0059(18) 0.0051(18) -0.0019(17) C7 0.031(2) 0.035(2) 0.034(2) 0.0031(17) 0.0033(17) -0.0019(17) C8 0.030(2) 0.043(2) 0.030(2) 0.0017(18) 0.0047(17) 0.0003(18) C9 0.052(3) 0.057(3) 0.035(2) 0.002(2) 0.005(2) 0.011(2) C10 0.039(2) 0.055(3) 0.043(3) 0.006(2) 0.000(2) 0.006(2) C11 0.075(4) 0.077(4) 0.051(3) 0.011(3) -0.002(3) 0.016(3) C12 0.034(2) 0.037(2) 0.051(3) 0.008(2) -0.0022(19) -0.0028(18) C13 0.042(3) 0.041(3) 0.066(3) 0.007(2) -0.010(2) 0.008(2) C14 0.052(3) 0.042(3) 0.087(4) 0.003(3) -0.014(3) 0.013(2) C15 0.049(3) 0.041(3) 0.080(4) -0.014(3) -0.004(3) 0.008(2) C16 0.045(3) 0.033(2) 0.066(3) -0.008(2) 0.000(2) 0.003(2) N20 0.28(2) 0.186(15) 0.100(8) 0.000 0.000 0.184(16) C20 0.18(3) 0.20(3) 0.51(7) 0.000 0.000 0.03(2) C21 0.036(6) 0.071(9) 0.56(7) 0.000 0.000 -0.013(6) N100 0.095(7) 0.31(2) 0.102(7) -0.007(10) -0.028(6) 0.058(10) O100 0.157(8) 0.302(13) 0.144(7) -0.023(7) -0.035(6) 0.076(9) O101 0.264(12) 0.069(4) 0.231(11) -0.034(5) 0.130(9) -0.030(5) O102 0.163(9) 0.350(19) 0.223(13) 0.039(12) -0.074(9) -0.051(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N4 1.936(3) 15_665 ? Ni1 N2 1.958(4) . ? Ni1 O1 2.079(3) . ? Ni1 N1 2.115(3) . ? Ni1 N6 2.177(3) 15_665 ? Ni1 O1 2.280(3) 15_665 ? O1 C7 1.299(5) . ? O1 Ni1 2.280(3) 12_756 ? N1 C5 1.339(6) . ? N1 C1 1.346(5) . ? N2 C6 1.293(5) . ? N2 N3 1.382(5) . ? N3 C7 1.315(5) . ? N4 C8 1.298(5) . ? N4 N5 1.352(5) . ? N4 Ni1 1.936(3) 12_756 ? N5 C10 1.388(6) . ? N5 C12 1.403(6) . ? N6 C16 1.327(6) . ? N6 C12 1.349(6) . ? N6 Ni1 2.177(3) 12_756 ? N7 C6 1.335(6) . ? N7 H7A 0.8600 . ? N7 H7B 0.8600 . ? C1 C2 1.389(7) . ? C1 H1 0.9300 . ? C2 C3 1.346(7) . ? C2 H2 0.9300 . ? C3 C4 1.393(7) . ? C3 H3 0.9300 . ? C4 C5 1.391(6) . ? C4 H4 0.9300 . ? C5 C6 1.480(6) . ? C7 C8 1.465(6) . ? C8 C9 1.402(6) . ? C9 C10 1.364(6) . ? C9 H9 0.9300 . ? C10 C11 1.486(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.395(6) . ? C13 C14 1.368(7) . ? C13 H13 0.9300 . ? C14 C15 1.353(8) . ? C14 H14 0.9300 . ? C15 C16 1.407(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? O1W H1W1 0.8500 . ? O1W H2W1 0.8500 . ? N20 C21 0.82(5) . ? C20 C21 1.47(5) . ? N100 O101 1.068(15) . ? N100 O100 1.149(12) . ? N100 O102 1.243(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ni1 N2 174.16(14) 15_665 . ? N4 Ni1 O1 105.69(12) 15_665 . ? N2 Ni1 O1 77.47(12) . . ? N4 Ni1 N1 99.22(14) 15_665 . ? N2 Ni1 N1 77.37(14) . . ? O1 Ni1 N1 154.77(12) . . ? N4 Ni1 N6 74.57(14) 15_665 15_665 ? N2 Ni1 N6 110.35(14) . 15_665 ? O1 Ni1 N6 94.09(11) . 15_665 ? N1 Ni1 N6 96.34(13) . 15_665 ? N4 Ni1 O1 72.33(12) 15_665 15_665 ? N2 Ni1 O1 102.84(12) . 15_665 ? O1 Ni1 O1 92.30(14) . 15_665 ? N1 Ni1 O1 91.44(11) . 15_665 ? N6 Ni1 O1 146.80(12) 15_665 15_665 ? C7 O1 Ni1 109.3(2) . . ? C7 O1 Ni1 112.9(2) . 12_756 ? Ni1 O1 Ni1 137.82(12) . 12_756 ? C5 N1 C1 118.3(4) . . ? C5 N1 Ni1 113.4(3) . . ? C1 N1 Ni1 128.2(3) . . ? C6 N2 N3 119.8(4) . . ? C6 N2 Ni1 121.3(3) . . ? N3 N2 Ni1 118.8(3) . . ? C7 N3 N2 108.9(3) . . ? C8 N4 N5 109.4(3) . . ? C8 N4 Ni1 127.1(3) . 12_756 ? N5 N4 Ni1 122.9(3) . 12_756 ? N4 N5 C10 108.8(3) . . ? N4 N5 C12 114.0(3) . . ? C10 N5 C12 137.2(4) . . ? C16 N6 C12 118.6(4) . . ? C16 N6 Ni1 127.1(3) . 12_756 ? C12 N6 Ni1 114.3(3) . 12_756 ? C6 N7 H7A 120.0 . . ? C6 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? N1 C1 C2 122.9(5) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 118.3(5) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C2 C3 C4 120.4(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 118.3(5) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? N1 C5 C4 121.7(4) . . ? N1 C5 C6 114.2(4) . . ? C4 C5 C6 124.0(4) . . ? N2 C6 N7 124.5(4) . . ? N2 C6 C5 113.6(4) . . ? N7 C6 C5 121.9(4) . . ? O1 C7 N3 125.4(4) . . ? O1 C7 C8 115.0(3) . . ? N3 C7 C8 119.7(4) . . ? N4 C8 C9 108.5(4) . . ? N4 C8 C7 112.2(3) . . ? C9 C8 C7 139.3(4) . . ? C10 C9 C8 107.6(4) . . ? C10 C9 H9 126.2 . . ? C8 C9 H9 126.2 . . ? C9 C10 N5 105.7(4) . . ? C9 C10 C11 130.0(5) . . ? N5 C10 C11 124.3(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N6 C12 C13 122.2(4) . . ? N6 C12 N5 113.9(4) . . ? C13 C12 N5 124.0(4) . . ? C14 C13 C12 117.8(5) . . ? C14 C13 H13 121.1 . . ? C12 C13 H13 121.1 . . ? C15 C14 C13 121.2(5) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 118.2(5) . . ? C14 C15 H15 120.9 . . ? C16 C15 H15 120.9 . . ? N6 C16 C15 122.1(5) . . ? N6 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? H1W1 O1W H2W1 107.7 . . ? N20 C21 C20 180.000(6) . . ? O101 N100 O100 127(2) . . ? O101 N100 O102 112.7(15) . . ? O100 N100 O102 119.4(19) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.07 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.351 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.070 # Attachment 'Rev. CIF 4.CIF' data_sksr32 _database_code_depnum_ccdc_archive 'CCDC 796249' #TrackingRef 'Rev. CIF 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H24 Cu2 N10 O12' _chemical_formula_weight 711.56 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8162(4) _cell_length_b 10.2990(5) _cell_length_c 16.3062(5) _cell_angle_alpha 74.779(3) _cell_angle_beta 88.629(3) _cell_angle_gamma 65.135(4) _cell_volume 1289.87(9) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 10440 _cell_measurement_theta_min 4.5424 _cell_measurement_theta_max 34.6732 _exptl_crystal_description 'triangular chunk' _exptl_crystal_colour 'deep green' _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.832 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 1.733 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.73843 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 22018 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 4.55 _diffrn_reflns_theta_max 34.78 _reflns_number_total 10328 _reflns_number_gt 6972 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10328 _refine_ls_number_parameters 454 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.002 _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 0.56129(2) 0.31680(2) 0.771445(12) 0.02043(5) Uani 1 1 d . . . Cu2 Cu 0.93425(2) 0.16561(2) 0.704380(12) 0.02163(5) Uani 1 1 d . . . O O 0.79908(14) 0.19763(14) 0.79718(7) 0.0254(3) Uani 1 1 d D A . H1O H 0.820(3) 0.1258(19) 0.8337(12) 0.030 Uiso 1 1 d D . . O1A O 0.18357(15) 0.45368(17) 0.53444(8) 0.0376(3) Uani 1 1 d . . . O1B O 0.82308(15) 0.21742(16) 0.41683(8) 0.0353(3) Uani 1 1 d . . . O1W O 1.01050(16) -0.10358(15) 0.72973(9) 0.0319(3) Uani 1 1 d D . . H1W1 H 1.003(3) -0.129(3) 0.7791(10) 0.048 Uiso 1 1 d D . . H1W2 H 1.099(2) -0.151(2) 0.7178(14) 0.048 Uiso 1 1 d D . . O2W O 1.21179(18) 0.12623(19) 0.37602(9) 0.0394(3) Uani 1 1 d D . . H2W1 H 1.232(3) 0.193(2) 0.3570(16) 0.059 Uiso 1 1 d D . . H2W2 H 1.143(3) 0.130(3) 0.3414(14) 0.059 Uiso 1 1 d D . . O3W O -0.10924(19) 0.4696(2) 0.64409(11) 0.0579(5) Uani 1 1 d D . . H3W1 H -0.200(3) 0.493(3) 0.6707(17) 0.087 Uiso 1 1 d D . . H3W2 H -0.139(4) 0.573(2) 0.623(2) 0.087 Uiso 1 1 d D . . O11A O 0.6021(6) 0.5261(5) 0.7262(5) 0.0525(10) Uani 0.80 1 d PU A 1 O12A O 0.3777(12) 0.6841(13) 0.7647(5) 0.0395(12) Uani 0.80 1 d PU A 1 O13A O 0.5347(3) 0.7604(2) 0.68067(19) 0.0669(7) Uani 0.80 1 d PU A 1 O11B O 0.570(3) 0.551(3) 0.714(2) 0.0525(10) Uani 0.20 1 d PU A 2 O12B O 0.396(5) 0.687(5) 0.779(2) 0.030(3) Uani 0.20 1 d PU A 2 O13B O 0.6169(14) 0.7149(10) 0.7409(8) 0.0669(7) Uani 0.20 1 d PU A 2 O21A O -0.0192(18) 0.728(2) 1.0186(10) 0.050(3) Uani 0.550(5) 1 d PU B 1 O22A O -0.1626(5) 0.9430(6) 0.9340(3) 0.0487(12) Uani 0.550(5) 1 d PU B 1 O23A O 0.0692(4) 0.7970(4) 0.89792(18) 0.0709(15) Uani 0.550(5) 1 d PU B 1 O21B O 0.014(2) 0.723(2) 1.0214(11) 0.0375(19) Uani 0.450(5) 1 d PU B 2 O22B O -0.1036(11) 0.9554(7) 0.9500(4) 0.069(2) Uani 0.450(5) 1 d PU B 2 O23B O -0.0806(6) 0.7872(5) 0.8893(2) 0.0565(14) Uani 0.450(5) 1 d PU B 2 N1A N 0.50156(17) 0.33163(16) 0.88621(9) 0.0239(3) Uani 1 1 d . A . N2A N 0.30823(16) 0.40628(15) 0.74778(8) 0.0215(3) Uani 1 1 d . A . N3A N 0.21769(16) 0.43758(16) 0.67157(9) 0.0248(3) Uani 1 1 d . . . H3AB H 0.1076 0.4750 0.6709 0.030 Uiso 1 1 calc R A . N4A N 0.58251(15) 0.29673(15) 0.65689(8) 0.0209(3) Uani 1 1 d . A . N1B N 1.15295(16) 0.11122(15) 0.76322(8) 0.0214(3) Uani 1 1 d . A . N2B N 1.07227(16) 0.14176(15) 0.60442(8) 0.0202(3) Uani 1 1 d . A . N3B N 1.01731(16) 0.15950(16) 0.52238(8) 0.0240(3) Uani 1 1 d . . . H3BB H 1.0940 0.1371 0.4865 0.029 Uiso 1 1 calc R A . N4B N 0.73370(15) 0.24073(16) 0.62909(8) 0.0212(3) Uani 1 1 d . A . N1 N 0.5081(2) 0.65750(18) 0.72891(10) 0.0329(3) Uani 1 1 d . . . N2 N -0.0460(2) 0.8227(2) 0.95182(10) 0.0364(4) Uani 1 1 d . . . C1A C 0.6079(2) 0.2908(2) 0.95525(11) 0.0302(4) Uani 1 1 d . . . H1AA H 0.7253 0.2479 0.9505 0.036 Uiso 1 1 calc R A . C2A C 0.5523(3) 0.3091(2) 1.03312(11) 0.0346(4) Uani 1 1 d . A . H2AA H 0.6303 0.2776 1.0814 0.042 Uiso 1 1 calc R . . C3A C 0.3824(3) 0.3735(2) 1.03963(12) 0.0397(5) Uani 1 1 d . . . H3AA H 0.3414 0.3870 1.0926 0.048 Uiso 1 1 calc R A . C4A C 0.2714(2) 0.4187(2) 0.96805(12) 0.0345(4) Uani 1 1 d . A . H4AA H 0.1536 0.4646 0.9713 0.041 Uiso 1 1 calc R . . C5A C 0.3342(2) 0.39617(19) 0.89217(11) 0.0248(3) Uani 1 1 d . . . C6A C 0.22587(19) 0.43899(18) 0.81223(11) 0.0239(3) Uani 1 1 d . A . C7A C 0.0403(2) 0.5116(2) 0.80977(13) 0.0360(4) Uani 1 1 d . . . H7AA H -0.0069 0.5876 0.7550 0.054 Uiso 1 1 calc R A . H7AB H 0.0085 0.5586 0.8564 0.054 Uiso 1 1 calc R . . H7AC H -0.0034 0.4367 0.8163 0.054 Uiso 1 1 calc R . . C8A C 0.28358(19) 0.4158(2) 0.59724(10) 0.0249(3) Uani 1 1 d . A . C9A C 0.46528(18) 0.34639(19) 0.59031(10) 0.0215(3) Uani 1 1 d . . . C10 C 0.54413(19) 0.3204(2) 0.51766(10) 0.0242(3) Uani 1 1 d . A . H10A H 0.4932 0.3430 0.4619 0.029 Uiso 1 1 calc R . . C1B C 1.1848(2) 0.0990(2) 0.84560(10) 0.0270(3) Uani 1 1 d . . . H1BA H 1.0943 0.1211 0.8804 0.032 Uiso 1 1 calc R A . C2B C 1.3453(2) 0.0551(2) 0.88149(11) 0.0295(4) Uani 1 1 d . A . H2BA H 1.3647 0.0479 0.9399 0.035 Uiso 1 1 calc R . . C3B C 1.4764(2) 0.0221(2) 0.83118(12) 0.0294(4) Uani 1 1 d . . . H3BA H 1.5877 -0.0088 0.8547 0.035 Uiso 1 1 calc R A . C4B C 1.4449(2) 0.03423(19) 0.74566(11) 0.0258(3) Uani 1 1 d . A . H4BA H 1.5339 0.0123 0.7100 0.031 Uiso 1 1 calc R . . C5B C 1.28081(18) 0.07905(18) 0.71338(10) 0.0210(3) Uani 1 1 d . . . C6B C 1.23181(19) 0.09621(19) 0.62347(10) 0.0218(3) Uani 1 1 d . A . C7B C 1.3566(2) 0.0639(2) 0.56053(12) 0.0338(4) Uani 1 1 d . . . H7BA H 1.3309 0.1548 0.5140 0.051 Uiso 1 1 calc R A . H7BB H 1.3521 -0.0133 0.5374 0.051 Uiso 1 1 calc R . . H7BC H 1.4693 0.0289 0.5885 0.051 Uiso 1 1 calc R . . C8B C 0.8529(2) 0.20921(19) 0.49128(10) 0.0236(3) Uani 1 1 d . A . C9B C 0.71355(19) 0.25430(18) 0.54488(10) 0.0209(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01400(9) 0.02611(11) 0.01852(9) -0.00678(8) 0.00418(6) -0.00591(7) Cu2 0.01271(9) 0.03197(12) 0.01803(9) -0.00924(8) 0.00324(6) -0.00632(7) O 0.0160(5) 0.0334(7) 0.0189(5) -0.0066(5) 0.0035(4) -0.0039(5) O1A 0.0190(6) 0.0610(9) 0.0265(6) -0.0086(6) -0.0011(5) -0.0133(6) O1B 0.0259(6) 0.0578(9) 0.0216(6) -0.0177(6) 0.0045(5) -0.0138(6) O1W 0.0287(6) 0.0344(7) 0.0319(7) -0.0116(6) 0.0083(5) -0.0118(5) O2W 0.0317(7) 0.0601(10) 0.0289(7) -0.0123(7) 0.0035(5) -0.0221(7) O3W 0.0276(8) 0.1080(15) 0.0436(9) -0.0283(10) 0.0104(6) -0.0303(9) O11A 0.038(2) 0.021(2) 0.094(3) -0.0159(19) 0.037(2) -0.0102(14) O12A 0.036(2) 0.051(2) 0.030(3) -0.022(2) 0.0070(19) -0.0102(14) O13A 0.0782(18) 0.0334(12) 0.0925(19) -0.0145(12) 0.0367(14) -0.0304(12) O11B 0.038(2) 0.021(2) 0.094(3) -0.0159(19) 0.037(2) -0.0102(14) O12B 0.030(7) 0.050(6) 0.018(7) -0.029(6) 0.011(6) -0.015(6) O13B 0.0782(18) 0.0334(12) 0.0925(19) -0.0145(12) 0.0367(14) -0.0304(12) O21A 0.059(7) 0.035(3) 0.043(4) -0.002(3) 0.012(4) -0.013(4) O22A 0.0294(16) 0.051(2) 0.046(2) -0.0032(18) 0.0036(14) -0.0043(14) O23A 0.0445(19) 0.095(3) 0.0261(15) -0.0001(15) 0.0095(12) 0.0039(17) O21B 0.034(4) 0.045(3) 0.024(3) -0.008(2) -0.003(2) -0.010(3) O22B 0.132(6) 0.029(2) 0.030(2) -0.0018(17) 0.006(3) -0.024(4) O23B 0.089(3) 0.071(3) 0.0257(17) -0.0155(17) 0.0032(17) -0.048(2) N1A 0.0218(6) 0.0259(7) 0.0231(7) -0.0094(6) 0.0060(5) -0.0080(5) N2A 0.0165(6) 0.0240(7) 0.0210(6) -0.0043(5) 0.0037(5) -0.0069(5) N3A 0.0119(6) 0.0334(8) 0.0229(7) -0.0048(6) 0.0017(5) -0.0057(5) N4A 0.0125(5) 0.0284(7) 0.0195(6) -0.0065(5) 0.0034(4) -0.0067(5) N1B 0.0174(6) 0.0252(7) 0.0204(6) -0.0079(5) 0.0021(5) -0.0070(5) N2B 0.0160(6) 0.0260(7) 0.0193(6) -0.0098(5) 0.0043(4) -0.0079(5) N3B 0.0170(6) 0.0365(8) 0.0185(6) -0.0117(6) 0.0062(5) -0.0094(5) N4B 0.0151(6) 0.0287(7) 0.0193(6) -0.0083(5) 0.0054(4) -0.0083(5) N1 0.0388(9) 0.0301(8) 0.0333(8) -0.0146(7) 0.0105(6) -0.0151(7) N2 0.0369(9) 0.0447(10) 0.0250(8) -0.0114(7) 0.0011(6) -0.0141(8) C1A 0.0284(9) 0.0355(10) 0.0269(9) -0.0126(8) 0.0037(6) -0.0118(7) C2A 0.0411(10) 0.0422(11) 0.0231(8) -0.0140(8) 0.0052(7) -0.0174(9) C3A 0.0461(11) 0.0508(13) 0.0255(9) -0.0188(9) 0.0149(8) -0.0197(10) C4A 0.0306(9) 0.0431(11) 0.0307(9) -0.0163(8) 0.0149(7) -0.0136(8) C5A 0.0223(7) 0.0245(8) 0.0266(8) -0.0086(7) 0.0078(6) -0.0085(6) C6A 0.0181(7) 0.0236(8) 0.0263(8) -0.0043(7) 0.0044(6) -0.0072(6) C7A 0.0189(8) 0.0402(11) 0.0368(10) -0.0100(8) 0.0085(7) -0.0022(7) C8A 0.0160(7) 0.0313(9) 0.0234(8) -0.0027(7) 0.0023(5) -0.0092(6) C9A 0.0144(6) 0.0289(8) 0.0204(7) -0.0051(6) 0.0020(5) -0.0097(6) C10 0.0186(7) 0.0345(9) 0.0200(7) -0.0071(7) 0.0018(5) -0.0122(6) C1B 0.0250(8) 0.0331(9) 0.0215(8) -0.0082(7) 0.0030(6) -0.0107(7) C2B 0.0289(9) 0.0351(10) 0.0231(8) -0.0056(7) -0.0024(6) -0.0136(7) C3B 0.0215(8) 0.0314(9) 0.0316(9) -0.0044(7) -0.0055(6) -0.0101(7) C4B 0.0176(7) 0.0273(8) 0.0321(9) -0.0100(7) 0.0026(6) -0.0081(6) C5B 0.0169(6) 0.0216(8) 0.0242(8) -0.0079(6) 0.0041(5) -0.0071(6) C6B 0.0183(7) 0.0272(8) 0.0230(7) -0.0108(6) 0.0064(5) -0.0107(6) C7B 0.0191(7) 0.0545(12) 0.0320(9) -0.0217(9) 0.0106(6) -0.0145(8) C8B 0.0210(7) 0.0297(9) 0.0215(7) -0.0102(7) 0.0051(6) -0.0105(6) C9B 0.0187(7) 0.0267(8) 0.0193(7) -0.0076(6) 0.0044(5) -0.0110(6) _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 O 1.9197(11) . ? Cu1 N4A 1.9289(13) . ? Cu1 N1A 1.9590(14) . ? Cu1 N2A 2.0251(13) . ? Cu1 O11A 2.264(7) . ? Cu1 O11B 2.38(3) . ? Cu2 O 1.9142(11) . ? Cu2 N4B 1.9201(13) . ? Cu2 N1B 1.9622(13) . ? Cu2 N2B 2.0154(13) . ? O H1O 0.772(14) . ? O1A C8A 1.234(2) . ? O1B C8B 1.2216(19) . ? O1W H1W1 0.789(15) . ? O1W H1W2 0.778(15) . ? O2W H2W1 0.774(15) . ? O2W H2W2 0.821(15) . ? O3W H3W1 0.875(17) . ? O3W H3W2 0.946(17) . ? O11A N1 1.267(5) . ? O12A N1 1.234(10) . ? O13A N1 1.249(3) . ? O11B N1 1.09(3) . ? O12B N1 1.26(3) . ? O13B N1 1.362(11) . ? O21A N2 1.208(16) . ? O22A N2 1.196(5) . ? O23A N2 1.314(3) . ? O21B N2 1.257(19) . ? O22B N2 1.234(6) . ? O23B N2 1.252(4) . ? N1A C1A 1.339(2) . ? N1A C5A 1.353(2) . ? N2A C6A 1.300(2) . ? N2A N3A 1.3807(18) . ? N3A C8A 1.363(2) . ? N3A H3AB 0.8800 . ? N4A N4B 1.3329(17) . ? N4A C9A 1.3513(19) . ? N1B C1B 1.341(2) . ? N1B C5B 1.351(2) . ? N2B C6B 1.2978(19) . ? N2B N3B 1.3733(18) . ? N3B C8B 1.377(2) . ? N3B H3BB 0.8800 . ? N4B C9B 1.352(2) . ? C1A C2A 1.380(3) . ? C1A H1AA 0.9500 . ? C2A C3A 1.375(3) . ? C2A H2AA 0.9500 . ? C3A C4A 1.387(3) . ? C3A H3AA 0.9500 . ? C4A C5A 1.379(2) . ? C4A H4AA 0.9500 . ? C5A C6A 1.486(2) . ? C6A C7A 1.482(2) . ? C7A H7AA 0.9800 . ? C7A H7AB 0.9800 . ? C7A H7AC 0.9800 . ? C8A C9A 1.470(2) . ? C9A C10 1.389(2) . ? C10 C9B 1.382(2) . ? C10 H10A 0.9500 . ? C1B C2B 1.383(2) . ? C1B H1BA 0.9500 . ? C2B C3B 1.377(3) . ? C2B H2BA 0.9500 . ? C3B C4B 1.391(2) . ? C3B H3BA 0.9500 . ? C4B C5B 1.389(2) . ? C4B H4BA 0.9500 . ? C5B C6B 1.482(2) . ? C6B C7B 1.480(2) . ? C7B H7BA 0.9800 . ? C7B H7BB 0.9800 . ? C7B H7BC 0.9800 . ? C8B C9B 1.473(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O Cu1 N4A 88.91(5) . . ? O Cu1 N1A 99.14(5) . . ? N4A Cu1 N1A 169.25(6) . . ? O Cu1 N2A 169.48(6) . . ? N4A Cu1 N2A 89.32(5) . . ? N1A Cu1 N2A 81.47(6) . . ? O Cu1 O11A 90.59(12) . . ? N4A Cu1 O11A 88.7(2) . . ? N1A Cu1 O11A 98.3(2) . . ? N2A Cu1 O11A 99.73(12) . . ? O Cu1 O11B 97.3(6) . . ? N4A Cu1 O11B 86.0(10) . . ? N1A Cu1 O11B 99.9(10) . . ? N2A Cu1 O11B 92.9(6) . . ? O11A Cu1 O11B 7.3(9) . . ? O Cu2 N4B 89.32(5) . . ? O Cu2 N1B 98.88(5) . . ? N4B Cu2 N1B 169.02(6) . . ? O Cu2 N2B 177.46(5) . . ? N4B Cu2 N2B 89.71(5) . . ? N1B Cu2 N2B 81.79(5) . . ? Cu2 O Cu1 118.43(6) . . ? Cu2 O H1O 113.3(16) . . ? Cu1 O H1O 111.7(16) . . ? H1W1 O1W H1W2 111(2) . . ? H2W1 O2W H2W2 107(2) . . ? H3W1 O3W H3W2 87.8(18) . . ? N1 O11A Cu1 129.3(4) . . ? N1 O11B Cu1 132(2) . . ? C1A N1A C5A 119.12(15) . . ? C1A N1A Cu1 126.73(12) . . ? C5A N1A Cu1 114.08(11) . . ? C6A N2A N3A 118.23(13) . . ? C6A N2A Cu1 114.67(11) . . ? N3A N2A Cu1 127.09(10) . . ? C8A N3A N2A 125.82(13) . . ? C8A N3A H3AB 117.1 . . ? N2A N3A H3AB 117.1 . . ? N4B N4A C9A 108.22(13) . . ? N4B N4A Cu1 120.37(10) . . ? C9A N4A Cu1 130.96(11) . . ? C1B N1B C5B 119.49(14) . . ? C1B N1B Cu2 126.67(11) . . ? C5B N1B Cu2 113.80(10) . . ? C6B N2B N3B 118.42(13) . . ? C6B N2B Cu2 114.14(10) . . ? N3B N2B Cu2 127.31(10) . . ? N2B N3B C8B 125.83(13) . . ? N2B N3B H3BB 117.1 . . ? C8B N3B H3BB 117.1 . . ? N4A N4B C9B 108.64(12) . . ? N4A N4B Cu2 120.80(10) . . ? C9B N4B Cu2 130.51(10) . . ? O11B N1 O12A 119.0(18) . . ? O11B N1 O13A 114.0(18) . . ? O12A N1 O13A 121.0(6) . . ? O11B N1 O12B 125(3) . . ? O12A N1 O12B 13.9(13) . . ? O13A N1 O12B 120(2) . . ? O11B N1 O11A 13(2) . . ? O12A N1 O11A 120.6(7) . . ? O13A N1 O11A 116.9(4) . . ? O12B N1 O11A 123(2) . . ? O11B N1 O13B 112.7(18) . . ? O12A N1 O13B 121.9(6) . . ? O13A N1 O13B 49.8(4) . . ? O12B N1 O13B 109.7(15) . . ? O11A N1 O13B 104.3(6) . . ? O22A N2 O21A 124.9(8) . . ? O22A N2 O22B 31.4(3) . . ? O21A N2 O22B 120.7(9) . . ? O22A N2 O23B 94.6(3) . . ? O21A N2 O23B 113.0(8) . . ? O22B N2 O23B 119.5(4) . . ? O22A N2 O21B 132.2(9) . . ? O21A N2 O21B 12.7(15) . . ? O22B N2 O21B 120.3(10) . . ? O23B N2 O21B 118.3(9) . . ? O22A N2 O23A 117.4(3) . . ? O21A N2 O23A 117.4(8) . . ? O22B N2 O23A 108.5(4) . . ? O23B N2 O23A 64.9(3) . . ? O21B N2 O23A 108.0(9) . . ? N1A C1A C2A 122.14(17) . . ? N1A C1A H1AA 118.9 . . ? C2A C1A H1AA 118.9 . . ? C3A C2A C1A 118.92(18) . . ? C3A C2A H2AA 120.5 . . ? C1A C2A H2AA 120.5 . . ? C2A C3A C4A 119.33(17) . . ? C2A C3A H3AA 120.3 . . ? C4A C3A H3AA 120.3 . . ? C5A C4A C3A 119.17(17) . . ? C5A C4A H4AA 120.4 . . ? C3A C4A H4AA 120.4 . . ? N1A C5A C4A 121.31(16) . . ? N1A C5A C6A 115.39(14) . . ? C4A C5A C6A 123.30(15) . . ? N2A C6A C7A 124.84(16) . . ? N2A C6A C5A 114.24(14) . . ? C7A C6A C5A 120.92(15) . . ? C6A C7A H7AA 109.5 . . ? C6A C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? C6A C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? O1A C8A N3A 117.16(14) . . ? O1A C8A C9A 119.91(15) . . ? N3A C8A C9A 122.91(14) . . ? N4A C9A C10 109.45(13) . . ? N4A C9A C8A 123.41(14) . . ? C10 C9A C8A 127.13(14) . . ? C9B C10 C9A 104.28(14) . . ? C9B C10 H10A 127.9 . . ? C9A C10 H10A 127.9 . . ? N1B C1B C2B 122.00(16) . . ? N1B C1B H1BA 119.0 . . ? C2B C1B H1BA 119.0 . . ? C3B C2B C1B 118.93(16) . . ? C3B C2B H2BA 120.5 . . ? C1B C2B H2BA 120.5 . . ? C2B C3B C4B 119.55(15) . . ? C2B C3B H3BA 120.2 . . ? C4B C3B H3BA 120.2 . . ? C5B C4B C3B 118.75(16) . . ? C5B C4B H4BA 120.6 . . ? C3B C4B H4BA 120.6 . . ? N1B C5B C4B 121.28(15) . . ? N1B C5B C6B 115.08(13) . . ? C4B C5B C6B 123.64(14) . . ? N2B C6B C7B 122.89(15) . . ? N2B C6B C5B 115.03(14) . . ? C7B C6B C5B 122.08(14) . . ? C6B C7B H7BA 109.5 . . ? C6B C7B H7BB 109.5 . . ? H7BA C7B H7BB 109.5 . . ? C6B C7B H7BC 109.5 . . ? H7BA C7B H7BC 109.5 . . ? H7BB C7B H7BC 109.5 . . ? O1B C8B N3B 118.49(14) . . ? O1B C8B C9B 119.74(14) . . ? N3B C8B C9B 121.76(14) . . ? N4B C9B C10 109.40(14) . . ? N4B C9B C8B 124.33(13) . . ? C10 C9B C8B 126.24(14) . . ? 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 N4B Cu2 O Cu1 -13.26(8) . . . . ? N1B Cu2 O Cu1 159.39(8) . . . . ? N2B Cu2 O Cu1 54.4(12) . . . . ? N4A Cu1 O Cu2 14.79(8) . . . . ? N1A Cu1 O Cu2 -172.36(7) . . . . ? N2A Cu1 O Cu2 95.2(3) . . . . ? O11A Cu1 O Cu2 -73.9(2) . . . . ? O11B Cu1 O Cu2 -71.0(10) . . . . ? O Cu1 O11A N1 -149.0(6) . . . . ? N4A Cu1 O11A N1 122.1(6) . . . . ? N1A Cu1 O11A N1 -49.7(7) . . . . ? N2A Cu1 O11A N1 33.0(7) . . . . ? O11B Cu1 O11A N1 54(8) . . . . ? O Cu1 O11B N1 -126(3) . . . . ? N4A Cu1 O11B N1 145(3) . . . . ? N1A Cu1 O11B N1 -26(3) . . . . ? N2A Cu1 O11B N1 56(3) . . . . ? O11A Cu1 O11B N1 -103(11) . . . . ? O Cu1 N1A C1A 10.55(16) . . . . ? N4A Cu1 N1A C1A 148.6(3) . . . . ? N2A Cu1 N1A C1A 179.92(16) . . . . ? O11A Cu1 N1A C1A -81.40(19) . . . . ? O11B Cu1 N1A C1A -88.6(7) . . . . ? O Cu1 N1A C5A -172.38(12) . . . . ? N4A Cu1 N1A C5A -34.3(4) . . . . ? N2A Cu1 N1A C5A -3.01(12) . . . . ? O11A Cu1 N1A C5A 95.67(17) . . . . ? O11B Cu1 N1A C5A 88.5(7) . . . . ? O Cu1 N2A C6A 97.7(3) . . . . ? N4A Cu1 N2A C6A 178.02(12) . . . . ? N1A Cu1 N2A C6A 3.57(12) . . . . ? O11A Cu1 N2A C6A -93.5(2) . . . . ? O11B Cu1 N2A C6A -96.0(10) . . . . ? O Cu1 N2A N3A -83.7(3) . . . . ? N4A Cu1 N2A N3A -3.34(13) . . . . ? N1A Cu1 N2A N3A -177.78(14) . . . . ? O11A Cu1 N2A N3A 85.2(3) . . . . ? O11B Cu1 N2A N3A 82.6(10) . . . . ? C6A N2A N3A C8A 177.41(16) . . . . ? Cu1 N2A N3A C8A -1.2(2) . . . . ? O Cu1 N4A N4B -11.33(12) . . . . ? N1A Cu1 N4A N4B -150.1(3) . . . . ? N2A Cu1 N4A N4B 179.04(13) . . . . ? O11A Cu1 N4A N4B 79.29(16) . . . . ? O11B Cu1 N4A N4B 86.1(6) . . . . ? O Cu1 N4A C9A 177.42(15) . . . . ? N1A Cu1 N4A C9A 38.7(4) . . . . ? N2A Cu1 N4A C9A 7.79(15) . . . . ? O11A Cu1 N4A C9A -91.96(18) . . . . ? O11B Cu1 N4A C9A -85.2(6) . . . . ? O Cu2 N1B C1B 1.80(15) . . . . ? N4B Cu2 N1B C1B 139.7(3) . . . . ? N2B Cu2 N1B C1B 179.32(15) . . . . ? O Cu2 N1B C5B 179.35(12) . . . . ? N4B Cu2 N1B C5B -42.8(4) . . . . ? N2B Cu2 N1B C5B -3.12(12) . . . . ? O Cu2 N2B C6B 109.1(11) . . . . ? N4B Cu2 N2B C6B 176.70(12) . . . . ? N1B Cu2 N2B C6B 3.68(12) . . . . ? O Cu2 N2B N3B -75.1(12) . . . . ? N4B Cu2 N2B N3B -7.53(14) . . . . ? N1B Cu2 N2B N3B 179.45(14) . . . . ? C6B N2B N3B C8B -178.76(16) . . . . ? Cu2 N2B N3B C8B 5.6(2) . . . . ? C9A N4A N4B C9B -0.05(18) . . . . ? Cu1 N4A N4B C9B -173.11(11) . . . . ? C9A N4A N4B Cu2 177.52(11) . . . . ? Cu1 N4A N4B Cu2 4.47(17) . . . . ? O Cu2 N4B N4A 5.23(13) . . . . ? N1B Cu2 N4B N4A -133.3(3) . . . . ? N2B Cu2 N4B N4A -172.42(13) . . . . ? O Cu2 N4B C9B -177.79(15) . . . . ? N1B Cu2 N4B C9B 43.7(4) . . . . ? N2B Cu2 N4B C9B 4.56(15) . . . . ? Cu1 O11B N1 O12A -23(4) . . . . ? Cu1 O11B N1 O13A -175.5(19) . . . . ? Cu1 O11B N1 O12B -8(4) . . . . ? Cu1 O11B N1 O11A 78(9) . . . . ? Cu1 O11B N1 O13B 130(2) . . . . ? Cu1 O11A N1 O11B -82(9) . . . . ? Cu1 O11A N1 O12A 4.9(9) . . . . ? Cu1 O11A N1 O13A -161.5(4) . . . . ? Cu1 O11A N1 O12B 21.0(16) . . . . ? Cu1 O11A N1 O13B 146.7(7) . . . . ? C5A N1A C1A C2A 1.6(3) . . . . ? Cu1 N1A C1A C2A 178.56(14) . . . . ? N1A C1A C2A C3A -1.1(3) . . . . ? C1A C2A C3A C4A -0.1(3) . . . . ? C2A C3A C4A C5A 0.8(3) . . . . ? C1A N1A C5A C4A -0.9(3) . . . . ? Cu1 N1A C5A C4A -178.20(14) . . . . ? C1A N1A C5A C6A 179.47(15) . . . . ? Cu1 N1A C5A C6A 2.16(19) . . . . ? C3A C4A C5A N1A -0.3(3) . . . . ? C3A C4A C5A C6A 179.30(18) . . . . ? N3A N2A C6A C7A -1.7(3) . . . . ? Cu1 N2A C6A C7A 177.09(15) . . . . ? N3A N2A C6A C5A 177.90(14) . . . . ? Cu1 N2A C6A C5A -3.33(18) . . . . ? N1A C5A C6A N2A 0.8(2) . . . . ? C4A C5A C6A N2A -178.80(17) . . . . ? N1A C5A C6A C7A -179.56(16) . . . . ? C4A C5A C6A C7A 0.8(3) . . . . ? N2A N3A C8A O1A -178.18(16) . . . . ? N2A N3A C8A C9A 3.6(3) . . . . ? N4B N4A C9A C10 0.38(19) . . . . ? Cu1 N4A C9A C10 172.43(12) . . . . ? N4B N4A C9A C8A -179.91(15) . . . . ? Cu1 N4A C9A C8A -7.9(3) . . . . ? O1A C8A C9A N4A -177.39(16) . . . . ? N3A C8A C9A N4A 0.8(3) . . . . ? O1A C8A C9A C10 2.3(3) . . . . ? N3A C8A C9A C10 -179.52(17) . . . . ? N4A C9A C10 C9B -0.53(19) . . . . ? C8A C9A C10 C9B 179.77(17) . . . . ? C5B N1B C1B C2B 0.5(3) . . . . ? Cu2 N1B C1B C2B 177.90(13) . . . . ? N1B C1B C2B C3B -0.5(3) . . . . ? C1B C2B C3B C4B 0.4(3) . . . . ? C2B C3B C4B C5B -0.3(3) . . . . ? C1B N1B C5B C4B -0.4(2) . . . . ? Cu2 N1B C5B C4B -178.13(12) . . . . ? C1B N1B C5B C6B 179.98(15) . . . . ? Cu2 N1B C5B C6B 2.23(18) . . . . ? C3B C4B C5B N1B 0.3(3) . . . . ? C3B C4B C5B C6B 179.90(16) . . . . ? N3B N2B C6B C7B 0.6(2) . . . . ? Cu2 N2B C6B C7B 176.73(14) . . . . ? N3B N2B C6B C5B -179.62(13) . . . . ? Cu2 N2B C6B C5B -3.45(18) . . . . ? N1B C5B C6B N2B 0.9(2) . . . . ? C4B C5B C6B N2B -178.77(16) . . . . ? N1B C5B C6B C7B -179.31(16) . . . . ? C4B C5B C6B C7B 1.1(3) . . . . ? N2B N3B C8B O1B -179.01(16) . . . . ? N2B N3B C8B C9B 1.9(3) . . . . ? N4A N4B C9B C10 -0.29(19) . . . . ? Cu2 N4B C9B C10 -177.55(12) . . . . ? N4A N4B C9B C8B 177.84(15) . . . . ? Cu2 N4B C9B C8B 0.6(3) . . . . ? C9A C10 C9B N4B 0.50(19) . . . . ? C9A C10 C9B C8B -177.59(16) . . . . ? O1B C8B C9B N4B 175.65(16) . . . . ? N3B C8B C9B N4B -5.3(3) . . . . ? O1B C8B C9B C10 -6.5(3) . . . . ? N3B C8B C9B C10 172.51(17) . . . . ? 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 O H1O O22A 0.772(14) 2.095(16) 2.861(5) 172(2) 1_645 O H1O O22B 0.772(14) 2.110(16) 2.865(6) 166(2) 1_645 O1W H1W1 O23A 0.789(15) 1.892(17) 2.643(3) 159(2) 1_645 O1W H1W1 O23B 0.789(15) 2.043(17) 2.794(4) 159(2) 1_645 O1W H1W2 O12A 0.778(15) 2.33(2) 3.011(10) 148(2) 1_645 O1W H1W2 O1B 0.778(15) 2.47(2) 3.0159(19) 129(2) 2_756 O1W H1W2 O12B 0.778(15) 2.49(4) 3.15(4) 142(2) 1_645 O2W H2W1 O13B 0.774(15) 2.32(2) 2.982(9) 145(3) 2_766 O2W H2W1 O13A 0.774(15) 2.33(2) 2.957(3) 139(3) 2_766 O2W H2W2 O1W 0.821(15) 1.948(16) 2.762(2) 170(2) 2_756 O3W H3W1 O11A 0.875(17) 1.886(18) 2.758(7) 174(3) 1_455 O3W H3W1 O11B 0.875(17) 2.02(3) 2.88(3) 171(3) 1_455 N3A H3AB O3W 0.88 2.00 2.793(2) 149.7 . N3B H3BB O2W 0.88 2.06 2.914(2) 162.7 . _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.103 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.075