Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Chebrolu Pulla Rao' 'Muktha Bharathy' 'Philippe Guionneau' 'T. N. GuruRow' 'Gudneppanavar Rajsekhar' 'Ajay K. Sah' _publ_contact_author_name 'Dr Chebrolu Pulla Rao' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Bombay Mumbai 400 076 INDIA ; _publ_contact_author_email CPRAO@CHEM.IITB.AC.IN _publ_section_title ; Bis-(u-saccharide-C-2-oxo) Dinuclear Cu(II) Complexes of 4,6-O-butylidene/ethylidene-N-(alpha-hydroxynapthylidene/o-hydroxybenzyl idene/5-bormo-o- hydroxybenzylidene)-beta-D-glucopyranosylamine: Structural Aspects and Data Correlations ; data_3 _database_code_CSD 193689 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H38 Cu2 N2 O13 S0.50' _chemical_formula_weight 789.74 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.184(1) _cell_length_b 13.683(1) _cell_length_c 35.411(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6388.0(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 36000 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 1.436 _exptl_absorpt_correction_type 'Empirical from multiple refl.' _exptl_absorpt_correction_T_min 0.6498 _exptl_absorpt_correction_T_max 0.7054 _exptl_absorpt_process_details 'MULABS (Platon2000; cf. Blessing 1995)' _exptl_special_details ; dx = 35 mm; 120 sec./deg., 1 deg.; mos. = 0.764(1) deg. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31835 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10241 _reflns_number_gt 8800 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (A.L.Spek, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+6.9922P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(9) _refine_ls_number_reflns 10241 _refine_ls_number_parameters 886 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 0.21005(4) 0.15097(4) 0.540604(19) 0.02244(15) Uani 1 1 d . . . Cu2 Cu 0.39556(4) 0.27238(4) 0.535554(19) 0.02089(15) Uani 1 1 d . . . Cu3 Cu 0.78494(4) 0.19392(4) 0.663728(19) 0.02361(16) Uani 1 1 d . . . Cu4 Cu 0.66853(4) 0.37267(4) 0.656519(19) 0.02378(15) Uani 1 1 d . . . C2A C 0.0076(3) 0.0931(3) 0.55897(16) 0.0235(12) Uani 1 1 d . . . C2B C 0.6044(3) 0.3247(3) 0.54392(15) 0.0220(11) Uani 1 1 d . . . C2C C 0.8326(4) -0.0087(4) 0.67793(15) 0.0253(12) Uani 1 1 d . . . C2D C 0.6110(3) 0.5768(3) 0.65282(14) 0.0221(12) Uani 1 1 d . . . C3A C -0.0917(3) 0.1184(4) 0.57000(17) 0.0355(15) Uani 1 1 d . . . H3A H -0.1081 0.1852 0.5739 0.043 Uiso 1 1 calc R . . C3B C 0.7067(3) 0.2990(3) 0.54690(15) 0.0270(12) Uani 1 1 d . . . H3B H 0.7262 0.2345 0.5401 0.032 Uiso 1 1 calc R . . C3C C 0.8009(4) -0.1070(3) 0.68104(16) 0.0320(14) Uani 1 1 d . . . H3C H 0.7315 -0.1229 0.6772 0.038 Uiso 1 1 calc R . . C3D C 0.6368(3) 0.6768(4) 0.65278(16) 0.0307(13) Uani 1 1 d . . . H3D H 0.7062 0.6946 0.6550 0.037 Uiso 1 1 calc R . . C4A C -0.1651(4) 0.0488(3) 0.57523(17) 0.0346(14) Uani 1 1 d . . . H4A H -0.2320 0.0678 0.5818 0.041 Uiso 1 1 calc R . . C4B C 0.7805(3) 0.3624(3) 0.55916(14) 0.0255(12) Uani 1 1 d . . . H4B H 0.8487 0.3409 0.5615 0.031 Uiso 1 1 calc R . . C4C C 0.8689(4) -0.1804(4) 0.68956(16) 0.0327(13) Uani 1 1 d . . . H4C H 0.8456 -0.2460 0.6909 0.039 Uiso 1 1 calc R . . C4D C 0.5647(4) 0.7502(4) 0.64959(16) 0.0315(14) Uani 1 1 d . . . H4D H 0.5851 0.8167 0.6503 0.038 Uiso 1 1 calc R . . C5A C -0.1415(4) -0.0497(4) 0.57084(19) 0.0417(17) Uani 1 1 d . . . H5A H -0.1918 -0.0980 0.5753 0.050 Uiso 1 1 calc R . . C5B C 0.7547(4) 0.4585(4) 0.56817(15) 0.0278(13) Uani 1 1 d . . . H5B H 0.8049 0.5030 0.5768 0.033 Uiso 1 1 calc R . . C5C C 0.9710(3) -0.1606(4) 0.69630(16) 0.0315(13) Uani 1 1 d . . . H5C H 1.0172 -0.2116 0.7022 0.038 Uiso 1 1 calc R . . C5D C 0.4632(4) 0.7271(4) 0.64544(17) 0.0348(14) Uani 1 1 d . . . H5D H 0.4138 0.7774 0.6433 0.042 Uiso 1 1 calc R . . C6A C -0.0465(4) -0.0768(4) 0.56012(18) 0.0364(15) Uani 1 1 d . . . H6A H -0.0318 -0.1441 0.5566 0.044 Uiso 1 1 calc R . . C6B C 0.6569(4) 0.4872(4) 0.56442(14) 0.0247(12) Uani 1 1 d . . . H6B H 0.6397 0.5528 0.5704 0.030 Uiso 1 1 calc R . . C6C C 1.0032(4) -0.0651(3) 0.69411(16) 0.0286(13) Uani 1 1 d . . . H6C H 1.0724 -0.0505 0.6989 0.034 Uiso 1 1 calc R . . C6D C 0.4346(3) 0.6301(4) 0.64447(15) 0.0299(13) Uani 1 1 d . . . H6D H 0.3650 0.6143 0.6412 0.036 Uiso 1 1 calc R . . C7A C 0.0308(3) -0.0071(4) 0.55410(15) 0.0251(12) Uani 1 1 d . . . C7B C 0.5800(3) 0.4240(3) 0.55208(15) 0.0229(12) Uani 1 1 d . . . C7C C 0.9360(3) 0.0119(3) 0.68492(14) 0.0229(12) Uani 1 1 d . . . C7D C 0.5062(3) 0.5533(3) 0.64820(14) 0.0205(11) Uani 1 1 d . . . C8A C 0.1294(3) -0.0427(3) 0.54402(15) 0.0203(11) Uani 1 1 d . . . H8A H 0.1378 -0.1115 0.5420 0.024 Uiso 1 1 calc R . . C8B C 0.4778(3) 0.4638(4) 0.55009(15) 0.0240(12) Uani 1 1 d . . . H8B H 0.4689 0.5317 0.5545 0.029 Uiso 1 1 calc R . . C8C C 0.9787(3) 0.1100(4) 0.68237(15) 0.0237(12) Uani 1 1 d . . . H8C H 1.0496 0.1174 0.6862 0.028 Uiso 1 1 calc R . . C8D C 0.4683(3) 0.4553(4) 0.64430(14) 0.0241(12) Uani 1 1 d . . . H8D H 0.3976 0.4467 0.6403 0.029 Uiso 1 1 calc R . . C10A C 0.3066(3) -0.0273(3) 0.52726(15) 0.0213(12) Uani 1 1 d . . . H10A H 0.3123 -0.0272 0.4991 0.026 Uiso 1 1 calc R . . C10B C 0.2970(3) 0.4523(3) 0.54265(16) 0.0222(11) Uani 1 1 d . . . H10B H 0.2739 0.4623 0.5160 0.027 Uiso 1 1 calc R . . C10C C 0.9738(3) 0.2825(3) 0.67152(15) 0.0223(12) Uani 1 1 d . . . H10C H 0.9940 0.2925 0.6446 0.027 Uiso 1 1 calc R . . C10D C 0.4854(3) 0.2826(3) 0.63746(15) 0.0201(11) Uani 1 1 d . . . H10D H 0.4946 0.2706 0.6098 0.024 Uiso 1 1 calc R . . C12A C 0.4185(3) -0.1567(3) 0.52603(15) 0.0206(11) Uani 1 1 d . . . H12A H 0.4188 -0.1520 0.4979 0.025 Uiso 1 1 calc R . . C12B C 0.1899(3) 0.5778(3) 0.56136(15) 0.0219(12) Uani 1 1 d . . . H12B H 0.1680 0.5863 0.5345 0.026 Uiso 1 1 calc R . . C12C C 1.1064(3) 0.3847(3) 0.68727(15) 0.0237(12) Uani 1 1 d . . . H12C H 1.1207 0.3904 0.6596 0.028 Uiso 1 1 calc R . . C12D C 0.3470(3) 0.1792(3) 0.63360(14) 0.0181(11) Uani 1 1 d . . . H12D H 0.3606 0.1719 0.6060 0.022 Uiso 1 1 calc R . . C13A C 0.5036(3) -0.0930(3) 0.54226(15) 0.0176(11) Uani 1 1 d . . . H13A H 0.5020 -0.0965 0.5705 0.021 Uiso 1 1 calc R . . C13B C 0.1191(3) 0.5070(3) 0.58135(15) 0.0193(11) Uani 1 1 d . . . H13B H 0.1423 0.4996 0.6081 0.023 Uiso 1 1 calc R . . C13C C 1.0323(3) 0.4656(3) 0.69913(15) 0.0226(12) Uani 1 1 d . . . H13C H 1.0147 0.4567 0.7264 0.027 Uiso 1 1 calc R . . C13D C 0.4027(3) 0.0985(3) 0.65531(15) 0.0226(12) Uani 1 1 d . . . H13D H 0.3884 0.1062 0.6829 0.027 Uiso 1 1 calc R . . C14A C 0.4909(3) 0.0121(3) 0.52991(15) 0.0194(11) Uani 1 1 d . . . H14A H 0.4955 0.0167 0.5018 0.023 Uiso 1 1 calc R . . C14B C 0.1208(3) 0.4073(3) 0.56271(15) 0.0198(12) Uani 1 1 d . . . H14B H 0.0935 0.4122 0.5364 0.024 Uiso 1 1 calc R . . C14C C 0.9362(3) 0.4607(3) 0.67607(15) 0.0212(12) Uani 1 1 d . . . H14C H 0.9521 0.4718 0.6488 0.025 Uiso 1 1 calc R . . C14D C 0.5157(3) 0.1048(3) 0.64908(16) 0.0227(12) Uani 1 1 d . . . H14D H 0.5316 0.0906 0.6220 0.027 Uiso 1 1 calc R . . C16A C 0.3857(3) 0.0435(3) 0.54315(15) 0.0170(11) Uani 1 1 d . . . H16A H 0.3834 0.0410 0.5714 0.020 Uiso 1 1 calc R . . C16B C 0.2310(3) 0.3737(3) 0.56157(14) 0.0181(11) Uani 1 1 d . . . H16B H 0.2553 0.3642 0.5881 0.022 Uiso 1 1 calc R . . C16C C 0.8922(3) 0.3567(3) 0.68167(14) 0.0211(11) Uani 1 1 d . . . H16C H 0.8718 0.3478 0.7087 0.025 Uiso 1 1 calc R . . C16D C 0.5510(3) 0.2074(3) 0.65907(15) 0.0206(11) Uani 1 1 d . . . H16D H 0.5424 0.2179 0.6868 0.025 Uiso 1 1 calc R . . C19A C 0.6115(3) -0.2286(3) 0.54127(17) 0.0250(11) Uani 1 1 d . . . H19A H 0.6110 -0.2317 0.5695 0.030 Uiso 1 1 calc R . . C19B C 0.0208(3) 0.6395(3) 0.60151(15) 0.0229(12) Uani 1 1 d . . . H19B H 0.0458 0.6291 0.6279 0.027 Uiso 1 1 calc R . . C19C C 1.1721(3) 0.5615(3) 0.71675(16) 0.0285(13) Uani 1 1 d . . . H19C H 1.1550 0.5482 0.7438 0.034 Uiso 1 1 calc R . . C19D C 0.2576(3) 0.0011(3) 0.64986(15) 0.0231(12) Uani 1 1 d . . . H19D H 0.2432 0.0088 0.6774 0.028 Uiso 1 1 calc R . . C20A C 0.7119(3) -0.2631(3) 0.52614(17) 0.0337(14) Uani 1 1 d . . . H20A H 0.7238 -0.3306 0.5342 0.051 Uiso 1 1 calc R . . H20B H 0.7662 -0.2211 0.5359 0.051 Uiso 1 1 calc R . . H20C H 0.7112 -0.2601 0.4985 0.051 Uiso 1 1 calc R . . C20B C -0.0854(3) 0.6786(4) 0.60230(16) 0.0325(14) Uani 1 1 d . . . H20D H -0.1298 0.6319 0.6152 0.049 Uiso 1 1 calc R . . H20E H -0.1095 0.6883 0.5764 0.049 Uiso 1 1 calc R . . H20F H -0.0864 0.7411 0.6158 0.049 Uiso 1 1 calc R . . C20C C 1.2189(4) 0.6612(4) 0.71318(18) 0.0465(17) Uani 1 1 d . . . H20G H 1.2808 0.6641 0.7285 0.070 Uiso 1 1 calc R . . H20H H 1.1708 0.7106 0.7221 0.070 Uiso 1 1 calc R . . H20I H 1.2358 0.6738 0.6867 0.070 Uiso 1 1 calc R . . C20D C 0.2232(3) -0.0985(3) 0.63632(16) 0.0303(13) Uani 1 1 d . . . H20J H 0.2588 -0.1494 0.6506 0.045 Uiso 1 1 calc R . . H20K H 0.2386 -0.1055 0.6094 0.045 Uiso 1 1 calc R . . H20L H 0.1499 -0.1051 0.6402 0.045 Uiso 1 1 calc R . . C22A C 0.4360(3) -0.2620(3) 0.53775(17) 0.0268(12) Uani 1 1 d . . . H22E H 0.4295 -0.2683 0.5655 0.032 Uiso 1 1 calc R . . H22F H 0.3846 -0.3048 0.5258 0.032 Uiso 1 1 calc R . . C22B C 0.1865(3) 0.6762(3) 0.58180(16) 0.0275(13) Uani 1 1 d . . . H22A H 0.2128 0.6691 0.6078 0.033 Uiso 1 1 calc R . . H22B H 0.2289 0.7246 0.5683 0.033 Uiso 1 1 calc R . . C22C C 1.2042(3) 0.3939(3) 0.70890(16) 0.0286(13) Uani 1 1 d . . . H22G H 1.1921 0.3814 0.7361 0.034 Uiso 1 1 calc R . . H22H H 1.2540 0.3454 0.6996 0.034 Uiso 1 1 calc R . . C22D C 0.2338(3) 0.1686(3) 0.64093(16) 0.0280(13) Uani 1 1 d . . . H22C H 0.2191 0.1772 0.6681 0.034 Uiso 1 1 calc R . . H22D H 0.1955 0.2186 0.6266 0.034 Uiso 1 1 calc R . . N9A N 0.2067(3) 0.0107(2) 0.53752(12) 0.0190(9) Uani 1 1 d . . . N9B N 0.3989(3) 0.4122(2) 0.54264(12) 0.0199(9) Uani 1 1 d . . . N9C N 0.9273(3) 0.1859(3) 0.67535(12) 0.0224(10) Uani 1 1 d . . . N9D N 0.5243(3) 0.3785(3) 0.64583(12) 0.0217(10) Uani 1 1 d . . . O1A O 0.0734(2) 0.1649(2) 0.55385(11) 0.0293(9) Uani 1 1 d . . . O1B O 0.5371(2) 0.2578(2) 0.53395(10) 0.0245(8) Uani 1 1 d . . . O1C O 0.7638(2) 0.0581(2) 0.67002(11) 0.0309(9) Uani 1 1 d . . . O1D O 0.6830(2) 0.5116(2) 0.65741(11) 0.0249(8) Uani 1 1 d . . . O11A O 0.32210(19) -0.1242(2) 0.54033(10) 0.0200(7) Uani 1 1 d . . . O11B O 0.2926(2) 0.5423(2) 0.56251(10) 0.0226(8) Uani 1 1 d . . . O11C O 1.0620(2) 0.2913(2) 0.69489(10) 0.0236(8) Uani 1 1 d . . . O11D O 0.3801(2) 0.2735(2) 0.64589(10) 0.0231(8) Uani 1 1 d . . . O15A O 0.5699(2) 0.0670(2) 0.54681(12) 0.0321(10) Uani 1 1 d D . . H15A H 0.563(4) 0.1276(10) 0.5442(18) 0.048 Uiso 1 1 d D . . O15B O 0.0587(2) 0.3429(2) 0.58465(11) 0.0261(8) Uani 1 1 d D . . H15B H 0.056(4) 0.291(2) 0.5722(13) 0.039 Uiso 1 1 d D . . O15C O 0.8680(2) 0.5347(2) 0.68937(11) 0.0299(9) Uani 1 1 d D . . H15C H 0.815(2) 0.520(4) 0.6777(14) 0.045 Uiso 1 1 d D . . O15D O 0.5625(2) 0.0317(2) 0.67301(11) 0.0317(9) Uani 1 1 d D . . H15D H 0.6258(10) 0.037(4) 0.6704(17) 0.048 Uiso 1 1 d D . . O17A O 0.3553(2) 0.1375(2) 0.53114(10) 0.0222(8) Uani 1 1 d . . . O17B O 0.2492(2) 0.2873(2) 0.54116(11) 0.0227(8) Uani 1 1 d . . . O17C O 0.81020(19) 0.3343(2) 0.65814(10) 0.0217(8) Uani 1 1 d . . . O17D O 0.6508(2) 0.2308(2) 0.64890(10) 0.0234(8) Uani 1 1 d . . . O18A O 0.5977(2) -0.1310(2) 0.52890(10) 0.0239(8) Uani 1 1 d . . . O18B O 0.0194(2) 0.5485(2) 0.58158(10) 0.0236(8) Uani 1 1 d . . . O18C O 1.0825(2) 0.5582(2) 0.69453(10) 0.0290(9) Uani 1 1 d . . . O18D O 0.3643(2) 0.0064(2) 0.64304(10) 0.0231(8) Uani 1 1 d . . . O21A O 0.5356(2) -0.2909(2) 0.52608(11) 0.0304(9) Uani 1 1 d . . . O21B O 0.0835(2) 0.7081(2) 0.58268(11) 0.0271(8) Uani 1 1 d . . . O21C O 1.2434(2) 0.4916(2) 0.70371(11) 0.0332(9) Uani 1 1 d . . . O21D O 0.2050(2) 0.0725(2) 0.62886(10) 0.0265(8) Uani 1 1 d . . . O40 O 0.8237(3) 0.6227(3) 0.75841(12) 0.0581(12) Uani 1 1 d . . . O30 O 0.6599(3) 0.3441(3) 0.72282(11) 0.0449(10) Uani 1 1 d . . . S31 S 0.60977(12) 0.38747(13) 0.75723(5) 0.0505(4) Uani 1 1 d . . . C32 C 0.5754(5) 0.5097(4) 0.74599(18) 0.0554(19) Uani 1 1 d . . . H32A H 0.6367 0.5499 0.7440 0.083 Uiso 1 1 calc R . . H32B H 0.5316 0.5360 0.7659 0.083 Uiso 1 1 calc R . . H32C H 0.5389 0.5107 0.7219 0.083 Uiso 1 1 calc R . . C33 C 0.4828(5) 0.3422(5) 0.7583(2) 0.073(2) Uani 1 1 d . . . H33A H 0.4835 0.2723 0.7643 0.110 Uiso 1 1 calc R . . H33B H 0.4510 0.3522 0.7336 0.110 Uiso 1 1 calc R . . H33C H 0.4441 0.3774 0.7777 0.110 Uiso 1 1 calc R . . 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 0.0166(3) 0.0145(3) 0.0362(4) -0.0009(3) -0.0015(3) 0.0001(2) Cu2 0.0174(3) 0.0134(3) 0.0318(4) -0.0005(3) 0.0023(3) -0.0007(2) Cu3 0.0152(3) 0.0209(3) 0.0348(4) -0.0009(3) -0.0008(3) -0.0009(2) Cu4 0.0159(3) 0.0208(3) 0.0346(4) 0.0000(3) -0.0023(3) -0.0009(2) C2A 0.016(3) 0.015(3) 0.039(4) -0.004(2) 0.000(2) 0.001(2) C2B 0.018(2) 0.018(3) 0.030(3) 0.006(2) 0.004(2) 0.002(2) C2C 0.025(3) 0.025(3) 0.026(3) -0.002(2) 0.001(2) 0.003(2) C2D 0.023(3) 0.023(3) 0.020(3) -0.003(2) -0.003(2) 0.004(2) C3A 0.019(3) 0.025(3) 0.063(5) -0.005(3) -0.003(3) 0.003(2) C3B 0.023(3) 0.020(3) 0.038(4) -0.002(2) 0.004(2) -0.002(2) C3C 0.024(3) 0.021(3) 0.051(4) 0.001(3) -0.003(2) -0.002(2) C3D 0.027(3) 0.028(3) 0.038(4) -0.006(3) 0.000(2) -0.001(2) C4A 0.019(3) 0.025(3) 0.061(4) -0.008(3) 0.004(3) 0.002(2) C4B 0.017(2) 0.027(3) 0.032(3) 0.003(3) 0.003(2) -0.001(2) C4C 0.039(3) 0.026(3) 0.033(4) -0.003(3) 0.000(2) -0.004(2) C4D 0.033(3) 0.024(3) 0.038(4) -0.002(3) -0.005(3) 0.000(2) C5A 0.022(3) 0.025(3) 0.078(5) -0.004(3) 0.013(3) -0.003(2) C5B 0.024(3) 0.025(3) 0.035(4) -0.005(3) 0.002(2) -0.006(2) C5C 0.028(3) 0.026(3) 0.041(4) 0.006(3) 0.001(2) 0.004(2) C5D 0.031(3) 0.023(3) 0.050(4) -0.006(3) -0.012(3) 0.006(2) C6A 0.022(3) 0.023(3) 0.065(5) -0.005(3) 0.002(3) -0.005(2) C6B 0.028(3) 0.022(3) 0.024(3) 0.001(2) 0.004(2) -0.006(2) C6C 0.022(3) 0.024(3) 0.040(4) 0.003(3) 0.000(2) 0.004(2) C6D 0.019(3) 0.036(3) 0.034(4) 0.001(3) -0.005(2) 0.002(2) C7A 0.016(3) 0.025(3) 0.034(3) -0.004(2) 0.002(2) -0.001(2) C7B 0.021(3) 0.021(3) 0.026(3) 0.006(2) 0.005(2) 0.001(2) C7C 0.021(3) 0.025(3) 0.023(3) -0.002(2) 0.006(2) 0.000(2) C7D 0.019(2) 0.019(3) 0.023(3) -0.002(2) 0.002(2) -0.001(2) C8A 0.021(3) 0.009(2) 0.031(3) -0.002(2) -0.002(2) 0.0013(19) C8B 0.023(3) 0.020(3) 0.029(4) 0.001(2) 0.007(2) 0.004(2) C8C 0.019(3) 0.026(3) 0.027(3) -0.003(2) 0.003(2) -0.006(2) C8D 0.017(2) 0.030(3) 0.025(3) 0.000(2) 0.000(2) 0.000(2) C10A 0.016(2) 0.016(3) 0.031(3) -0.002(2) 0.005(2) 0.0011(19) C10B 0.021(2) 0.014(2) 0.031(3) 0.002(2) 0.005(2) 0.001(2) C10C 0.017(2) 0.020(3) 0.030(3) 0.000(2) 0.003(2) -0.006(2) C10D 0.016(2) 0.020(3) 0.025(3) 0.001(2) 0.000(2) -0.0055(19) C12A 0.020(2) 0.015(3) 0.027(3) -0.003(2) 0.004(2) 0.001(2) C12B 0.018(3) 0.015(3) 0.033(3) -0.001(2) -0.004(2) 0.0012(19) C12C 0.015(2) 0.024(3) 0.033(3) 0.002(2) 0.003(2) -0.004(2) C12D 0.020(2) 0.014(3) 0.020(3) -0.003(2) 0.000(2) -0.007(2) C13A 0.009(2) 0.018(3) 0.025(3) -0.003(2) 0.006(2) -0.0007(17) C13B 0.016(2) 0.014(3) 0.028(3) 0.001(2) 0.000(2) 0.0018(19) C13C 0.021(3) 0.018(3) 0.029(3) 0.001(2) 0.000(2) -0.004(2) C13D 0.020(2) 0.022(3) 0.026(3) 0.002(2) -0.005(2) -0.002(2) C14A 0.019(2) 0.012(3) 0.028(3) -0.002(2) 0.000(2) -0.0017(19) C14B 0.021(3) 0.018(3) 0.021(3) 0.001(2) -0.001(2) -0.003(2) C14C 0.019(3) 0.014(3) 0.031(3) 0.001(2) 0.001(2) 0.0026(19) C14D 0.019(2) 0.022(3) 0.028(3) 0.005(2) 0.002(2) 0.003(2) C16A 0.015(2) 0.011(2) 0.025(3) -0.001(2) -0.002(2) 0.0001(18) C16B 0.020(2) 0.013(2) 0.022(3) 0.006(2) 0.002(2) 0.0024(19) C16C 0.018(2) 0.022(3) 0.023(3) 0.001(2) -0.001(2) -0.003(2) C16D 0.012(2) 0.023(3) 0.028(3) 0.007(2) 0.002(2) -0.0046(19) C19A 0.024(2) 0.014(3) 0.036(3) -0.001(3) 0.002(2) 0.002(2) C19B 0.023(3) 0.014(3) 0.031(3) -0.005(2) 0.000(2) -0.001(2) C19C 0.022(3) 0.024(3) 0.039(4) -0.005(2) -0.005(2) -0.002(2) C19D 0.018(2) 0.025(3) 0.026(3) 0.002(2) 0.001(2) -0.006(2) C20A 0.020(2) 0.023(3) 0.058(4) -0.007(3) 0.002(3) 0.001(2) C20B 0.026(3) 0.025(3) 0.047(4) -0.005(3) 0.009(2) -0.001(2) C20C 0.038(3) 0.035(3) 0.067(5) -0.012(3) -0.007(3) -0.006(3) C20D 0.019(3) 0.029(3) 0.044(4) -0.001(3) 0.000(2) -0.004(2) C22A 0.017(2) 0.019(3) 0.045(4) 0.003(3) 0.004(2) 0.0021(19) C22B 0.023(3) 0.019(3) 0.041(4) 0.000(2) 0.003(2) 0.000(2) C22C 0.019(2) 0.022(3) 0.044(4) -0.004(2) 0.000(2) -0.001(2) C22D 0.017(3) 0.023(3) 0.044(4) -0.006(3) -0.003(2) -0.001(2) N9A 0.0154(19) 0.016(2) 0.025(3) -0.0042(19) -0.0028(19) 0.0023(16) N9B 0.018(2) 0.013(2) 0.028(3) -0.0002(19) 0.0055(19) -0.0015(16) N9C 0.015(2) 0.020(2) 0.032(3) -0.001(2) 0.0008(17) 0.0037(18) N9D 0.020(2) 0.020(2) 0.024(3) 0.000(2) 0.0001(17) -0.0015(18) O1A 0.0161(17) 0.0165(19) 0.055(3) 0.0022(17) -0.0005(16) -0.0006(14) O1B 0.0160(16) 0.0138(17) 0.044(2) 0.0008(17) 0.0026(16) -0.0003(13) O1C 0.0197(18) 0.0220(19) 0.051(3) 0.0011(18) -0.0060(16) -0.0024(15) O1D 0.0147(17) 0.0199(18) 0.040(2) -0.0022(17) -0.0050(16) 0.0005(13) O11A 0.0141(15) 0.0103(16) 0.036(2) 0.0033(16) 0.0024(15) 0.0031(12) O11B 0.0155(16) 0.0127(17) 0.040(2) -0.0043(16) 0.0033(15) 0.0003(14) O11C 0.0138(16) 0.0207(19) 0.036(2) 0.0022(17) -0.0036(14) -0.0020(13) O11D 0.0152(16) 0.0207(18) 0.033(2) -0.0019(16) -0.0006(14) -0.0022(13) O15A 0.0199(18) 0.0143(18) 0.062(3) -0.003(2) -0.0031(17) -0.0009(15) O15B 0.0224(17) 0.0133(19) 0.043(3) -0.0031(17) 0.0064(16) -0.0033(14) O15C 0.0201(19) 0.026(2) 0.044(3) -0.0100(18) -0.0043(16) 0.0035(15) O15D 0.0184(18) 0.026(2) 0.051(3) 0.0154(19) -0.0033(17) 0.0023(15) O17A 0.0203(16) 0.0111(17) 0.035(2) 0.0006(16) 0.0000(14) -0.0003(13) O17B 0.0189(16) 0.0171(19) 0.032(2) -0.0051(17) 0.0022(15) -0.0006(12) O17C 0.0169(17) 0.0196(17) 0.029(2) -0.0041(16) -0.0031(14) 0.0017(13) O17D 0.0149(16) 0.0225(18) 0.033(2) -0.0005(16) 0.0008(15) 0.0015(14) O18A 0.0180(16) 0.0144(17) 0.039(2) -0.0009(16) 0.0023(15) 0.0037(14) O18B 0.0185(17) 0.0181(19) 0.034(2) -0.0054(16) 0.0022(15) 0.0029(13) O18C 0.0226(18) 0.027(2) 0.038(2) 0.0003(17) -0.0043(16) -0.0060(15) O18D 0.0122(16) 0.0174(19) 0.039(2) 0.0006(16) -0.0021(14) -0.0048(13) O21A 0.0197(17) 0.020(2) 0.051(3) -0.0048(17) 0.0016(16) 0.0044(14) O21B 0.0200(17) 0.0165(18) 0.045(3) 0.0009(16) 0.0012(16) 0.0033(14) O21C 0.0222(18) 0.024(2) 0.054(3) -0.0036(19) 0.0001(17) -0.0081(14) O21D 0.0195(17) 0.0192(19) 0.041(2) -0.0030(17) -0.0066(16) -0.0006(14) O40 0.062(3) 0.067(3) 0.045(3) 0.001(2) -0.003(2) -0.002(2) O30 0.040(2) 0.060(3) 0.035(3) -0.003(2) -0.0018(19) 0.001(2) S31 0.0567(10) 0.0699(12) 0.0249(10) -0.0006(8) -0.0027(8) -0.0008(9) C32 0.077(5) 0.060(4) 0.030(4) -0.016(4) 0.015(3) -0.004(4) C33 0.073(5) 0.072(5) 0.075(6) -0.011(4) 0.042(4) -0.019(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1A 1.872(3) . ? Cu1 N9A 1.923(3) . ? Cu1 O17B 1.935(3) . ? Cu1 O17A 1.953(3) . ? Cu1 Cu2 2.9620(7) . ? Cu2 O1B 1.878(3) . ? Cu2 O17A 1.927(3) . ? Cu2 N9B 1.930(3) . ? Cu2 O17B 1.951(3) . ? Cu3 O1C 1.893(3) . ? Cu3 O17D 1.913(3) . ? Cu3 N9C 1.924(4) . ? Cu3 O17C 1.960(3) . ? Cu3 Cu4 2.8988(8) . ? Cu4 O1D 1.910(3) . ? Cu4 N9D 1.941(4) . ? Cu4 O17C 1.941(3) . ? Cu4 O17D 1.973(3) . ? Cu4 O30 2.383(4) . ? C2A O1A 1.323(5) . ? C2A C3A 1.409(7) . ? C2A C7A 1.414(6) . ? C2B O1B 1.322(5) . ? C2B C3B 1.398(6) . ? C2B C7B 1.426(6) . ? C2C O1C 1.318(5) . ? C2C C7C 1.413(6) . ? C2C C3C 1.414(7) . ? C2D O1D 1.313(5) . ? C2D C3D 1.410(6) . ? C2D C7D 1.428(6) . ? C3A C4A 1.369(7) . ? C3A H3A 0.9500 . ? C3B C4B 1.374(6) . ? C3B H3B 0.9500 . ? C3C C4C 1.379(7) . ? C3C H3C 0.9500 . ? C3D C4D 1.387(6) . ? C3D H3D 0.9500 . ? C4A C5A 1.392(7) . ? C4A H4A 0.9500 . ? C4B C5B 1.394(7) . ? C4B H4B 0.9500 . ? C4C C5C 1.394(7) . ? C4C H4C 0.9500 . ? C4D C5D 1.383(7) . ? C4D H4D 0.9500 . ? C5A C6A 1.360(7) . ? C5A H5A 0.9500 . ? C5B C6B 1.354(6) . ? C5B H5B 0.9500 . ? C5C C6C 1.375(7) . ? C5C H5C 0.9500 . ? C5D C6D 1.381(7) . ? C5D H5D 0.9500 . ? C6A C7A 1.412(7) . ? C6A H6A 0.9500 . ? C6B C7B 1.402(7) . ? C6B H6B 0.9500 . ? C6C C7C 1.415(6) . ? C6C H6C 0.9500 . ? C6D C7D 1.418(6) . ? C6D H6D 0.9500 . ? C7A C8A 1.433(6) . ? C7B C8B 1.456(6) . ? C7C C8C 1.458(7) . ? C7D C8D 1.438(6) . ? C8A N9A 1.276(5) . ? C8A H8A 0.9500 . ? C8B N9B 1.285(6) . ? C8B H8B 0.9500 . ? C8C N9C 1.264(6) . ? C8C H8C 0.9500 . ? C8D N9D 1.284(6) . ? C8D H8D 0.9500 . ? C10A O11A 1.420(5) . ? C10A N9A 1.462(5) . ? C10A C16A 1.531(6) . ? C10A H10A 1.0000 . ? C10B O11B 1.419(5) . ? C10B N9B 1.450(5) . ? C10B C16B 1.537(6) . ? C10B H10B 1.0000 . ? C10C O11C 1.432(5) . ? C10C N9C 1.464(6) . ? C10C C16C 1.521(6) . ? C10C H10C 1.0000 . ? C10D O11D 1.425(5) . ? C10D N9D 1.440(6) . ? C10D C16D 1.547(6) . ? C10D H10D 1.0000 . ? C12A O11A 1.439(5) . ? C12A C22A 1.516(6) . ? C12A C13A 1.532(6) . ? C12A H12A 1.0000 . ? C12B O11B 1.438(5) . ? C12B C13B 1.521(6) . ? C12B C22B 1.529(6) . ? C12B H12B 1.0000 . ? C12C O11C 1.431(5) . ? C12C C22C 1.505(6) . ? C12C C13C 1.535(6) . ? C12C H12C 1.0000 . ? C12D O11D 1.430(5) . ? C12D C22D 1.522(6) . ? C12D C13D 1.533(6) . ? C12D H12D 1.0000 . ? C13A O18A 1.426(5) . ? C13A C14A 1.512(6) . ? C13A H13A 1.0000 . ? C13B O18B 1.432(5) . ? C13B C14B 1.516(6) . ? C13B H13B 1.0000 . ? C13C O18C 1.440(5) . ? C13C C14C 1.508(6) . ? C13C H13C 1.0000 . ? C13D O18D 1.426(5) . ? C13D C14D 1.508(6) . ? C13D H13D 1.0000 . ? C14A O15A 1.417(5) . ? C14A C16A 1.527(6) . ? C14A H14A 1.0000 . ? C14B O15B 1.432(5) . ? C14B C16B 1.524(6) . ? C14B H14B 1.0000 . ? C14C O15C 1.434(5) . ? C14C C16C 1.550(6) . ? C14C H14C 1.0000 . ? C14D O15D 1.449(6) . ? C14D C16D 1.521(6) . ? C14D H14D 1.0000 . ? C16A O17A 1.412(5) . ? C16A H16A 1.0000 . ? C16B O17B 1.406(5) . ? C16B H16B 1.0000 . ? C16C O17C 1.399(5) . ? C16C H16C 1.0000 . ? C16D O17D 1.401(5) . ? C16D H16D 1.0000 . ? C19A O18A 1.417(5) . ? C19A O21A 1.420(5) . ? C19A C20A 1.504(6) . ? C19A H19A 1.0000 . ? C19B O21B 1.418(5) . ? C19B O18B 1.430(5) . ? C19B C20B 1.500(6) . ? C19B H19B 1.0000 . ? C19C O21C 1.418(6) . ? C19C O18C 1.420(6) . ? C19C C20C 1.503(7) . ? C19C H19C 1.0000 . ? C19D O21D 1.410(6) . ? C19D O18D 1.429(5) . ? C19D C20D 1.514(6) . ? C19D H19D 1.0000 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C20C H20G 0.9800 . ? C20C H20H 0.9800 . ? C20C H20I 0.9800 . ? C20D H20J 0.9800 . ? C20D H20K 0.9800 . ? C20D H20L 0.9800 . ? C22A O21A 1.433(5) . ? C22A H22E 0.9900 . ? C22A H22F 0.9900 . ? C22B O21B 1.426(5) . ? C22B H22A 0.9900 . ? C22B H22B 0.9900 . ? C22C O21C 1.444(5) . ? C22C H22G 0.9900 . ? C22C H22H 0.9900 . ? C22D O21D 1.434(5) . ? C22D H22C 0.9900 . ? C22D H22D 0.9900 . ? O15A H15A 0.838(10) . ? O15B H15B 0.840(10) . ? O15C H15C 0.842(10) . ? O15D H15D 0.843(10) . ? O30 S31 1.508(4) . ? S31 C32 1.778(6) . ? S31 C33 1.786(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Cu1 N9A 95.40(14) . . ? O1A Cu1 O17B 98.97(13) . . ? N9A Cu1 O17B 165.60(13) . . ? O1A Cu1 O17A 175.34(16) . . ? N9A Cu1 O17A 85.31(13) . . ? O17B Cu1 O17A 80.29(12) . . ? O1A Cu1 Cu2 138.84(10) . . ? N9A Cu1 Cu2 125.11(10) . . ? O17B Cu1 Cu2 40.53(8) . . ? O17A Cu1 Cu2 39.90(9) . . ? O1B Cu2 O17A 99.78(12) . . ? O1B Cu2 N9B 94.97(14) . . ? O17A Cu2 N9B 165.08(14) . . ? O1B Cu2 O17B 175.89(16) . . ? O17A Cu2 O17B 80.55(12) . . ? N9B Cu2 O17B 84.58(13) . . ? O1B Cu2 Cu1 139.73(9) . . ? O17A Cu2 Cu1 40.55(8) . . ? N9B Cu2 Cu1 124.53(11) . . ? O17B Cu2 Cu1 40.15(9) . . ? O1C Cu3 O17D 98.94(13) . . ? O1C Cu3 N9C 93.57(15) . . ? O17D Cu3 N9C 167.29(15) . . ? O1C Cu3 O17C 178.38(14) . . ? O17D Cu3 O17C 82.56(12) . . ? N9C Cu3 O17C 84.95(14) . . ? O1C Cu3 Cu4 139.56(10) . . ? O17D Cu3 Cu4 42.56(9) . . ? N9C Cu3 Cu4 125.69(12) . . ? O17C Cu3 Cu4 41.75(8) . . ? O1D Cu4 N9D 93.43(14) . . ? O1D Cu4 O17C 99.93(12) . . ? N9D Cu4 O17C 163.73(15) . . ? O1D Cu4 O17D 172.99(16) . . ? N9D Cu4 O17D 84.12(14) . . ? O17C Cu4 O17D 81.52(12) . . ? O1D Cu4 O30 98.73(15) . . ? N9D Cu4 O30 98.75(15) . . ? O17C Cu4 O30 88.42(14) . . ? O17D Cu4 O30 88.14(14) . . ? O1D Cu4 Cu3 141.74(9) . . ? N9D Cu4 Cu3 124.81(12) . . ? O17C Cu4 Cu3 42.25(9) . . ? O17D Cu4 Cu3 40.98(8) . . ? O30 Cu4 Cu3 78.47(9) . . ? O1A C2A C3A 117.6(4) . . ? O1A C2A C7A 124.1(4) . . ? C3A C2A C7A 118.2(4) . . ? O1B C2B C3B 119.6(4) . . ? O1B C2B C7B 124.2(4) . . ? C3B C2B C7B 116.2(4) . . ? O1C C2C C7C 124.3(4) . . ? O1C C2C C3C 118.2(4) . . ? C7C C2C C3C 117.5(4) . . ? O1D C2D C3D 119.0(4) . . ? O1D C2D C7D 124.1(4) . . ? C3D C2D C7D 116.8(4) . . ? C4A C3A C2A 121.5(5) . . ? C4A C3A H3A 119.2 . . ? C2A C3A H3A 119.2 . . ? C4B C3B C2B 123.3(5) . . ? C4B C3B H3B 118.4 . . ? C2B C3B H3B 118.4 . . ? C4C C3C C2C 121.2(5) . . ? C4C C3C H3C 119.4 . . ? C2C C3C H3C 119.4 . . ? C4D C3D C2D 122.5(4) . . ? C4D C3D H3D 118.8 . . ? C2D C3D H3D 118.8 . . ? C3A C4A C5A 120.0(5) . . ? C3A C4A H4A 120.0 . . ? C5A C4A H4A 120.0 . . ? C3B C4B C5B 119.7(4) . . ? C3B C4B H4B 120.2 . . ? C5B C4B H4B 120.2 . . ? C3C C4C C5C 121.6(5) . . ? C3C C4C H4C 119.2 . . ? C5C C4C H4C 119.2 . . ? C5D C4D C3D 120.5(5) . . ? C5D C4D H4D 119.8 . . ? C3D C4D H4D 119.8 . . ? C6A C5A C4A 120.0(5) . . ? C6A C5A H5A 120.0 . . ? C4A C5A H5A 120.0 . . ? C6B C5B C4B 118.9(5) . . ? C6B C5B H5B 120.6 . . ? C4B C5B H5B 120.6 . . ? C6C C5C C4C 118.2(5) . . ? C6C C5C H5C 120.9 . . ? C4C C5C H5C 120.9 . . ? C6D C5D C4D 119.1(5) . . ? C6D C5D H5D 120.5 . . ? C4D C5D H5D 120.5 . . ? C5A C6A C7A 121.5(5) . . ? C5A C6A H6A 119.2 . . ? C7A C6A H6A 119.2 . . ? C5B C6B C7B 122.7(5) . . ? C5B C6B H6B 118.7 . . ? C7B C6B H6B 118.7 . . ? C5C C6C C7C 121.8(5) . . ? C5C C6C H6C 119.1 . . ? C7C C6C H6C 119.1 . . ? C5D C6D C7D 121.9(4) . . ? C5D C6D H6D 119.1 . . ? C7D C6D H6D 119.1 . . ? C6A C7A C2A 118.7(4) . . ? C6A C7A C8A 117.5(4) . . ? C2A C7A C8A 123.8(4) . . ? C6B C7B C2B 119.2(4) . . ? C6B C7B C8B 117.0(4) . . ? C2B C7B C8B 123.7(4) . . ? C2C C7C C6C 119.7(4) . . ? C2C C7C C8C 123.0(4) . . ? C6C C7C C8C 117.3(4) . . ? C6D C7D C2D 119.2(4) . . ? C6D C7D C8D 116.8(4) . . ? C2D C7D C8D 123.8(4) . . ? N9A C8A C7A 125.1(4) . . ? N9A C8A H8A 117.5 . . ? C7A C8A H8A 117.5 . . ? N9B C8B C7B 123.7(4) . . ? N9B C8B H8B 118.2 . . ? C7B C8B H8B 118.2 . . ? N9C C8C C7C 124.1(4) . . ? N9C C8C H8C 117.9 . . ? C7C C8C H8C 117.9 . . ? N9D C8D C7D 124.0(4) . . ? N9D C8D H8D 118.0 . . ? C7D C8D H8D 118.0 . . ? O11A C10A N9A 112.4(3) . . ? O11A C10A C16A 112.0(4) . . ? N9A C10A C16A 107.3(4) . . ? O11A C10A H10A 108.4 . . ? N9A C10A H10A 108.4 . . ? C16A C10A H10A 108.4 . . ? O11B C10B N9B 111.5(4) . . ? O11B C10B C16B 111.5(4) . . ? N9B C10B C16B 105.1(3) . . ? O11B C10B H10B 109.5 . . ? N9B C10B H10B 109.5 . . ? C16B C10B H10B 109.5 . . ? O11C C10C N9C 111.3(4) . . ? O11C C10C C16C 112.4(4) . . ? N9C C10C C16C 106.5(3) . . ? O11C C10C H10C 108.9 . . ? N9C C10C H10C 108.9 . . ? C16C C10C H10C 108.9 . . ? O11D C10D N9D 112.5(4) . . ? O11D C10D C16D 112.5(4) . . ? N9D C10D C16D 107.8(4) . . ? O11D C10D H10D 107.9 . . ? N9D C10D H10D 107.9 . . ? C16D C10D H10D 107.9 . . ? O11A C12A C22A 109.3(4) . . ? O11A C12A C13A 109.8(4) . . ? C22A C12A C13A 109.1(4) . . ? O11A C12A H12A 109.5 . . ? C22A C12A H12A 109.5 . . ? C13A C12A H12A 109.5 . . ? O11B C12B C13B 110.5(4) . . ? O11B C12B C22B 108.2(3) . . ? C13B C12B C22B 108.8(4) . . ? O11B C12B H12B 109.8 . . ? C13B C12B H12B 109.8 . . ? C22B C12B H12B 109.8 . . ? O11C C12C C22C 109.2(4) . . ? O11C C12C C13C 109.3(3) . . ? C22C C12C C13C 110.2(4) . . ? O11C C12C H12C 109.3 . . ? C22C C12C H12C 109.3 . . ? C13C C12C H12C 109.3 . . ? O11D C12D C22D 109.5(4) . . ? O11D C12D C13D 110.6(4) . . ? C22D C12D C13D 108.4(4) . . ? O11D C12D H12D 109.5 . . ? C22D C12D H12D 109.5 . . ? C13D C12D H12D 109.5 . . ? O18A C13A C14A 110.3(3) . . ? O18A C13A C12A 107.7(4) . . ? C14A C13A C12A 110.6(4) . . ? O18A C13A H13A 109.4 . . ? C14A C13A H13A 109.4 . . ? C12A C13A H13A 109.4 . . ? O18B C13B C14B 112.0(4) . . ? O18B C13B C12B 108.3(3) . . ? C14B C13B C12B 111.2(4) . . ? O18B C13B H13B 108.4 . . ? C14B C13B H13B 108.4 . . ? C12B C13B H13B 108.4 . . ? O18C C13C C14C 111.4(4) . . ? O18C C13C C12C 108.1(4) . . ? C14C C13C C12C 110.8(4) . . ? O18C C13C H13C 108.9 . . ? C14C C13C H13C 108.9 . . ? C12C C13C H13C 108.9 . . ? O18D C13D C14D 110.9(4) . . ? O18D C13D C12D 108.3(4) . . ? C14D C13D C12D 111.0(4) . . ? O18D C13D H13D 108.9 . . ? C14D C13D H13D 108.9 . . ? C12D C13D H13D 108.9 . . ? O15A C14A C13A 107.6(4) . . ? O15A C14A C16A 112.8(4) . . ? C13A C14A C16A 106.2(4) . . ? O15A C14A H14A 110.0 . . ? C13A C14A H14A 110.0 . . ? C16A C14A H14A 110.0 . . ? O15B C14B C13B 108.0(4) . . ? O15B C14B C16B 111.9(4) . . ? C13B C14B C16B 107.3(3) . . ? O15B C14B H14B 109.8 . . ? C13B C14B H14B 109.8 . . ? C16B C14B H14B 109.8 . . ? O15C C14C C13C 108.5(4) . . ? O15C C14C C16C 111.8(4) . . ? C13C C14C C16C 106.6(4) . . ? O15C C14C H14C 109.9 . . ? C13C C14C H14C 109.9 . . ? C16C C14C H14C 109.9 . . ? O15D C14D C13D 107.2(4) . . ? O15D C14D C16D 111.7(4) . . ? C13D C14D C16D 108.7(4) . . ? O15D C14D H14D 109.7 . . ? C13D C14D H14D 109.7 . . ? C16D C14D H14D 109.7 . . ? O17A C16A C14A 115.0(4) . . ? O17A C16A C10A 105.8(3) . . ? C14A C16A C10A 109.1(4) . . ? O17A C16A H16A 108.9 . . ? C14A C16A H16A 108.9 . . ? C10A C16A H16A 108.9 . . ? O17B C16B C14B 115.5(4) . . ? O17B C16B C10B 105.5(4) . . ? C14B C16B C10B 109.9(4) . . ? O17B C16B H16B 108.6 . . ? C14B C16B H16B 108.6 . . ? C10B C16B H16B 108.6 . . ? O17C C16C C10C 105.1(4) . . ? O17C C16C C14C 114.4(4) . . ? C10C C16C C14C 108.5(3) . . ? O17C C16C H16C 109.6 . . ? C10C C16C H16C 109.6 . . ? C14C C16C H16C 109.6 . . ? O17D C16D C14D 116.1(4) . . ? O17D C16D C10D 104.2(3) . . ? C14D C16D C10D 109.1(4) . . ? O17D C16D H16D 109.1 . . ? C14D C16D H16D 109.1 . . ? C10D C16D H16D 109.1 . . ? O18A C19A O21A 111.0(4) . . ? O18A C19A C20A 107.4(4) . . ? O21A C19A C20A 107.2(4) . . ? O18A C19A H19A 110.4 . . ? O21A C19A H19A 110.4 . . ? C20A C19A H19A 110.4 . . ? O21B C19B O18B 110.6(4) . . ? O21B C19B C20B 108.5(4) . . ? O18B C19B C20B 107.9(4) . . ? O21B C19B H19B 109.9 . . ? O18B C19B H19B 109.9 . . ? C20B C19B H19B 109.9 . . ? O21C C19C O18C 110.5(4) . . ? O21C C19C C20C 108.2(4) . . ? O18C C19C C20C 108.9(4) . . ? O21C C19C H19C 109.8 . . ? O18C C19C H19C 109.8 . . ? C20C C19C H19C 109.8 . . ? O21D C19D O18D 111.1(4) . . ? O21D C19D C20D 108.0(4) . . ? O18D C19D C20D 106.7(4) . . ? O21D C19D H19D 110.3 . . ? O18D C19D H19D 110.3 . . ? C20D C19D H19D 110.3 . . ? C19A C20A H20A 109.5 . . ? C19A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? C19A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C19B C20B H20D 109.5 . . ? C19B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C19B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C19C C20C H20G 109.5 . . ? C19C C20C H20H 109.5 . . ? H20G C20C H20H 109.5 . . ? C19C C20C H20I 109.5 . . ? H20G C20C H20I 109.5 . . ? H20H C20C H20I 109.5 . . ? C19D C20D H20J 109.5 . . ? C19D C20D H20K 109.5 . . ? H20J C20D H20K 109.5 . . ? C19D C20D H20L 109.5 . . ? H20J C20D H20L 109.5 . . ? H20K C20D H20L 109.5 . . ? O21A C22A C12A 108.8(4) . . ? O21A C22A H22E 109.9 . . ? C12A C22A H22E 109.9 . . ? O21A C22A H22F 109.9 . . ? C12A C22A H22F 109.9 . . ? H22E C22A H22F 108.3 . . ? O21B C22B C12B 107.9(4) . . ? O21B C22B H22A 110.1 . . ? C12B C22B H22A 110.1 . . ? O21B C22B H22B 110.1 . . ? C12B C22B H22B 110.1 . . ? H22A C22B H22B 108.4 . . ? O21C C22C C12C 108.6(4) . . ? O21C C22C H22G 110.0 . . ? C12C C22C H22G 110.0 . . ? O21C C22C H22H 110.0 . . ? C12C C22C H22H 110.0 . . ? H22G C22C H22H 108.3 . . ? O21D C22D C12D 107.2(4) . . ? O21D C22D H22C 110.3 . . ? C12D C22D H22C 110.3 . . ? O21D C22D H22D 110.3 . . ? C12D C22D H22D 110.3 . . ? H22C C22D H22D 108.5 . . ? C8A N9A C10A 124.1(4) . . ? C8A N9A Cu1 125.4(3) . . ? C10A N9A Cu1 110.4(3) . . ? C8B N9B C10B 122.8(4) . . ? C8B N9B Cu2 126.2(3) . . ? C10B N9B Cu2 110.7(3) . . ? C8C N9C C10C 122.4(4) . . ? C8C N9C Cu3 127.7(3) . . ? C10C N9C Cu3 109.7(3) . . ? C8D N9D C10D 122.1(4) . . ? C8D N9D Cu4 127.2(3) . . ? C10D N9D Cu4 110.6(3) . . ? C2A O1A Cu1 126.1(3) . . ? C2B O1B Cu2 125.8(3) . . ? C2C O1C Cu3 127.2(3) . . ? C2D O1D Cu4 127.0(3) . . ? C10A O11A C12A 107.5(3) . . ? C10B O11B C12B 108.6(3) . . ? C12C O11C C10C 107.4(3) . . ? C10D O11D C12D 108.2(3) . . ? C14A O15A H15A 114(4) . . ? C14B O15B H15B 105(4) . . ? C14C O15C H15C 101(4) . . ? C14D O15D H15D 107(4) . . ? C16A O17A Cu2 140.3(3) . . ? C16A O17A Cu1 108.2(2) . . ? Cu2 O17A Cu1 99.55(13) . . ? C16B O17B Cu1 140.4(3) . . ? C16B O17B Cu2 108.0(2) . . ? Cu1 O17B Cu2 99.32(13) . . ? C16C O17C Cu4 134.6(3) . . ? C16C O17C Cu3 106.6(3) . . ? Cu4 O17C Cu3 96.00(12) . . ? C16D O17D Cu3 137.5(3) . . ? C16D O17D Cu4 107.6(3) . . ? Cu3 O17D Cu4 96.45(13) . . ? C19A O18A C13A 110.6(3) . . ? C19B O18B C13B 109.6(3) . . ? C19C O18C C13C 110.3(4) . . ? C13D O18D C19D 110.1(3) . . ? C19A O21A C22A 111.8(4) . . ? C19B O21B C22B 111.3(3) . . ? C19C O21C C22C 110.2(4) . . ? C19D O21D C22D 110.4(4) . . ? S31 O30 Cu4 138.8(2) . . ? O30 S31 C32 107.5(3) . . ? O30 S31 C33 107.0(3) . . ? C32 S31 C33 95.3(3) . . ? S31 C32 H32A 109.5 . . ? S31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? S31 C33 H33A 109.5 . . ? S31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? S31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? 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 O1A Cu1 Cu2 O1B 160.4(3) . . . . ? N9A Cu1 Cu2 O1B -7.8(2) . . . . ? O17B Cu1 Cu2 O1B 173.6(3) . . . . ? O17A Cu1 Cu2 O1B -12.7(2) . . . . ? O1A Cu1 Cu2 O17A 173.1(2) . . . . ? N9A Cu1 Cu2 O17A 4.9(2) . . . . ? O17B Cu1 Cu2 O17A -173.7(2) . . . . ? O1A Cu1 Cu2 N9B -6.7(2) . . . . ? N9A Cu1 Cu2 N9B -174.9(2) . . . . ? O17B Cu1 Cu2 N9B 6.6(2) . . . . ? O17A Cu1 Cu2 N9B -179.8(2) . . . . ? O1A Cu1 Cu2 O17B -13.2(3) . . . . ? N9A Cu1 Cu2 O17B 178.5(2) . . . . ? O17A Cu1 Cu2 O17B 173.7(2) . . . . ? O1C Cu3 Cu4 O1D 167.5(3) . . . . ? O17D Cu3 Cu4 O1D -169.9(2) . . . . ? N9C Cu3 Cu4 O1D 3.6(2) . . . . ? O17C Cu3 Cu4 O1D -11.0(2) . . . . ? O1C Cu3 Cu4 N9D -14.7(2) . . . . ? O17D Cu3 Cu4 N9D 7.9(2) . . . . ? N9C Cu3 Cu4 N9D -178.6(2) . . . . ? O17C Cu3 Cu4 N9D 166.8(2) . . . . ? O1C Cu3 Cu4 O17C 178.6(2) . . . . ? O17D Cu3 Cu4 O17C -158.8(2) . . . . ? N9C Cu3 Cu4 O17C 14.6(2) . . . . ? O1C Cu3 Cu4 O17D -22.6(2) . . . . ? N9C Cu3 Cu4 O17D 173.5(2) . . . . ? O17C Cu3 Cu4 O17D 158.8(2) . . . . ? O1C Cu3 Cu4 O30 78.0(2) . . . . ? O17D Cu3 Cu4 O30 100.63(18) . . . . ? N9C Cu3 Cu4 O30 -85.89(18) . . . . ? O17C Cu3 Cu4 O30 -100.53(18) . . . . ? O1A C2A C3A C4A 178.8(5) . . . . ? C7A C2A C3A C4A -1.3(8) . . . . ? O1B C2B C3B C4B -176.1(5) . . . . ? C7B C2B C3B C4B 3.9(8) . . . . ? O1C C2C C3C C4C -179.5(5) . . . . ? C7C C2C C3C C4C -1.8(8) . . . . ? O1D C2D C3D C4D -177.4(5) . . . . ? C7D C2D C3D C4D 1.9(8) . . . . ? C2A C3A C4A C5A 2.1(9) . . . . ? C2B C3B C4B C5B -2.1(8) . . . . ? C2C C3C C4C C5C 1.5(9) . . . . ? C2D C3D C4D C5D -1.4(9) . . . . ? C3A C4A C5A C6A -2.2(10) . . . . ? C3B C4B C5B C6B -0.3(8) . . . . ? C3C C4C C5C C6C -0.3(9) . . . . ? C3D C4D C5D C6D -0.1(9) . . . . ? C4A C5A C6A C7A 1.6(10) . . . . ? C4B C5B C6B C7B 0.5(8) . . . . ? C4C C5C C6C C7C -0.7(8) . . . . ? C4D C5D C6D C7D 1.0(9) . . . . ? C5A C6A C7A C2A -0.8(9) . . . . ? C5A C6A C7A C8A 178.1(6) . . . . ? O1A C2A C7A C6A -179.4(5) . . . . ? C3A C2A C7A C6A 0.6(8) . . . . ? O1A C2A C7A C8A 1.8(9) . . . . ? C3A C2A C7A C8A -178.2(5) . . . . ? C5B C6B C7B C2B 1.5(8) . . . . ? C5B C6B C7B C8B 178.7(5) . . . . ? O1B C2B C7B C6B 176.5(5) . . . . ? C3B C2B C7B C6B -3.6(7) . . . . ? O1B C2B C7B C8B -0.5(8) . . . . ? C3B C2B C7B C8B 179.4(5) . . . . ? O1C C2C C7C C6C 178.4(5) . . . . ? C3C C2C C7C C6C 0.8(8) . . . . ? O1C C2C C7C C8C -2.9(8) . . . . ? C3C C2C C7C C8C 179.5(5) . . . . ? C5C C6C C7C C2C 0.3(8) . . . . ? C5C C6C C7C C8C -178.4(5) . . . . ? C5D C6D C7D C2D -0.5(8) . . . . ? C5D C6D C7D C8D -176.1(5) . . . . ? O1D C2D C7D C6D 178.3(5) . . . . ? C3D C2D C7D C6D -0.9(7) . . . . ? O1D C2D C7D C8D -6.4(8) . . . . ? C3D C2D C7D C8D 174.3(5) . . . . ? C6A C7A C8A N9A 179.7(5) . . . . ? C2A C7A C8A N9A -1.5(9) . . . . ? C6B C7B C8B N9B -173.4(5) . . . . ? C2B C7B C8B N9B 3.6(8) . . . . ? C2C C7C C8C N9C 3.2(8) . . . . ? C6C C7C C8C N9C -178.1(5) . . . . ? C6D C7D C8D N9D 177.9(5) . . . . ? C2D C7D C8D N9D 2.5(8) . . . . ? O11A C12A C13A O18A 177.0(4) . . . . ? C22A C12A C13A O18A 57.2(5) . . . . ? O11A C12A C13A C14A -62.4(5) . . . . ? C22A C12A C13A C14A 177.8(4) . . . . ? O11B C12B C13B O18B 176.3(4) . . . . ? C22B C12B C13B O18B 57.7(5) . . . . ? O11B C12B C13B C14B -60.3(5) . . . . ? C22B C12B C13B C14B -178.9(4) . . . . ? O11C C12C C13C O18C 174.6(4) . . . . ? C22C C12C C13C O18C 54.5(5) . . . . ? O11C C12C C13C C14C -63.1(5) . . . . ? C22C C12C C13C C14C 176.7(4) . . . . ? O11D C12D C13D O18D 177.8(3) . . . . ? C22D C12D C13D O18D 57.8(5) . . . . ? O11D C12D C13D C14D -60.2(5) . . . . ? C22D C12D C13D C14D 179.8(4) . . . . ? O18A C13A C14A O15A -62.7(5) . . . . ? C12A C13A C14A O15A 178.2(4) . . . . ? O18A C13A C14A C16A 176.2(4) . . . . ? C12A C13A C14A C16A 57.1(5) . . . . ? O18B C13B C14B O15B -63.1(5) . . . . ? C12B C13B C14B O15B 175.6(4) . . . . ? O18B C13B C14B C16B 176.1(4) . . . . ? C12B C13B C14B C16B 54.8(5) . . . . ? O18C C13C C14C O15C -62.2(5) . . . . ? C12C C13C C14C O15C 177.4(4) . . . . ? O18C C13C C14C C16C 177.2(4) . . . . ? C12C C13C C14C C16C 56.9(5) . . . . ? O18D C13D C14D O15D -64.4(5) . . . . ? C12D C13D C14D O15D 175.2(4) . . . . ? O18D C13D C14D C16D 174.6(4) . . . . ? C12D C13D C14D C16D 54.2(6) . . . . ? O15A C14A C16A O17A 68.1(5) . . . . ? C13A C14A C16A O17A -174.3(4) . . . . ? O15A C14A C16A C10A -173.3(4) . . . . ? C13A C14A C16A C10A -55.6(5) . . . . ? O11A C10A C16A O17A -174.1(4) . . . . ? N9A C10A C16A O17A -50.4(5) . . . . ? O11A C10A C16A C14A 61.6(5) . . . . ? N9A C10A C16A C14A -174.7(4) . . . . ? O15B C14B C16B O17B 68.9(5) . . . . ? C13B C14B C16B O17B -172.8(4) . . . . ? O15B C14B C16B C10B -172.0(4) . . . . ? C13B C14B C16B C10B -53.6(5) . . . . ? O11B C10B C16B O17B -175.1(3) . . . . ? N9B C10B C16B O17B -54.1(5) . . . . ? O11B C10B C16B C14B 59.8(5) . . . . ? N9B C10B C16B C14B -179.2(4) . . . . ? O11C C10C C16C O17C -176.4(3) . . . . ? N9C C10C C16C O17C -54.3(5) . . . . ? O11C C10C C16C C14C 60.8(5) . . . . ? N9C C10C C16C C14C -177.1(4) . . . . ? O15C C14C C16C O17C 70.0(5) . . . . ? C13C C14C C16C O17C -171.5(4) . . . . ? O15C C14C C16C C10C -173.0(4) . . . . ? C13C C14C C16C C10C -54.6(5) . . . . ? O15D C14D C16D O17D 72.2(6) . . . . ? C13D C14D C16D O17D -169.6(4) . . . . ? O15D C14D C16D C10D -170.5(4) . . . . ? C13D C14D C16D C10D -52.3(5) . . . . ? O11D C10D C16D O17D -176.9(4) . . . . ? N9D C10D C16D O17D -52.3(5) . . . . ? O11D C10D C16D C14D 58.5(5) . . . . ? N9D C10D C16D C14D -176.8(4) . . . . ? O11A C12A C22A O21A -175.2(4) . . . . ? C13A C12A C22A O21A -55.1(6) . . . . ? O11B C12B C22B O21B -176.4(4) . . . . ? C13B C12B C22B O21B -56.3(5) . . . . ? O11C C12C C22C O21C -174.8(4) . . . . ? C13C C12C C22C O21C -54.6(5) . . . . ? O11D C12D C22D O21D -178.8(4) . . . . ? C13D C12D C22D O21D -58.2(5) . . . . ? C7A C8A N9A C10A -180.0(5) . . . . ? C7A C8A N9A Cu1 1.2(8) . . . . ? O11A C10A N9A C8A -25.1(7) . . . . ? C16A C10A N9A C8A -148.6(5) . . . . ? O11A C10A N9A Cu1 153.9(3) . . . . ? C16A C10A N9A Cu1 30.4(4) . . . . ? O1A Cu1 N9A C8A -0.9(5) . . . . ? O17B Cu1 N9A C8A 175.2(6) . . . . ? O17A Cu1 N9A C8A 174.5(4) . . . . ? Cu2 Cu1 N9A C8A 171.3(4) . . . . ? O1A Cu1 N9A C10A -179.9(3) . . . . ? O17B Cu1 N9A C10A -3.7(9) . . . . ? O17A Cu1 N9A C10A -4.5(3) . . . . ? Cu2 Cu1 N9A C10A -7.6(4) . . . . ? C7B C8B N9B C10B 176.8(5) . . . . ? C7B C8B N9B Cu2 3.9(7) . . . . ? O11B C10B N9B C8B -18.1(7) . . . . ? C16B C10B N9B C8B -139.0(5) . . . . ? O11B C10B N9B Cu2 155.8(3) . . . . ? C16B C10B N9B Cu2 34.8(5) . . . . ? O1B Cu2 N9B C8B -10.3(5) . . . . ? O17A Cu2 N9B C8B 160.7(5) . . . . ? O17B Cu2 N9B C8B 165.6(5) . . . . ? Cu1 Cu2 N9B C8B 161.3(4) . . . . ? O1B Cu2 N9B C10B 176.1(3) . . . . ? O17A Cu2 N9B C10B -12.9(9) . . . . ? O17B Cu2 N9B C10B -8.0(3) . . . . ? Cu1 Cu2 N9B C10B -12.3(4) . . . . ? C7C C8C N9C C10C -177.5(5) . . . . ? C7C C8C N9C Cu3 -3.5(8) . . . . ? O11C C10C N9C C8C -31.2(6) . . . . ? C16C C10C N9C C8C -154.0(5) . . . . ? O11C C10C N9C Cu3 154.0(3) . . . . ? C16C C10C N9C Cu3 31.1(5) . . . . ? O1C Cu3 N9C C8C 2.9(5) . . . . ? O17D Cu3 N9C C8C -167.1(6) . . . . ? O17C Cu3 N9C C8C -177.8(5) . . . . ? Cu4 Cu3 N9C C8C 172.5(4) . . . . ? O1C Cu3 N9C C10C 177.4(3) . . . . ? O17D Cu3 N9C C10C 7.5(9) . . . . ? O17C Cu3 N9C C10C -3.3(3) . . . . ? Cu4 Cu3 N9C C10C -13.0(4) . . . . ? C7D C8D N9D C10D -172.6(5) . . . . ? C7D C8D N9D Cu4 4.0(7) . . . . ? O11D C10D N9D C8D -29.2(7) . . . . ? C16D C10D N9D C8D -153.8(4) . . . . ? O11D C10D N9D Cu4 153.7(3) . . . . ? C16D C10D N9D Cu4 29.1(4) . . . . ? O1D Cu4 N9D C8D -5.3(4) . . . . ? O17C Cu4 N9D C8D -150.6(5) . . . . ? O17D Cu4 N9D C8D -178.7(4) . . . . ? O30 Cu4 N9D C8D 94.1(4) . . . . ? Cu3 Cu4 N9D C8D 176.1(4) . . . . ? O1D Cu4 N9D C10D 171.7(3) . . . . ? O17C Cu4 N9D C10D 26.4(8) . . . . ? O17D Cu4 N9D C10D -1.7(3) . . . . ? O30 Cu4 N9D C10D -88.9(3) . . . . ? Cu3 Cu4 N9D C10D -7.0(4) . . . . ? C3A C2A O1A Cu1 178.2(4) . . . . ? C7A C2A O1A Cu1 -1.8(7) . . . . ? N9A Cu1 O1A C2A 1.2(4) . . . . ? O17B Cu1 O1A C2A -177.8(4) . . . . ? O17A Cu1 O1A C2A -97.4(16) . . . . ? Cu2 Cu1 O1A C2A -169.2(3) . . . . ? C3B C2B O1B Cu2 170.0(4) . . . . ? C7B C2B O1B Cu2 -10.0(7) . . . . ? O17A Cu2 O1B C2B -164.5(4) . . . . ? N9B Cu2 O1B C2B 13.2(4) . . . . ? O17B Cu2 O1B C2B -70.2(19) . . . . ? Cu1 Cu2 O1B C2B -156.1(3) . . . . ? C7C C2C O1C Cu3 3.1(7) . . . . ? C3C C2C O1C Cu3 -179.3(4) . . . . ? O17D Cu3 O1C C2C 175.2(4) . . . . ? N9C Cu3 O1C C2C -2.6(4) . . . . ? O17C Cu3 O1C C2C -26(6) . . . . ? Cu4 Cu3 O1C C2C -169.6(3) . . . . ? C3D C2D O1D Cu4 -177.3(4) . . . . ? C7D C2D O1D Cu4 3.4(7) . . . . ? N9D Cu4 O1D C2D 1.6(4) . . . . ? O17C Cu4 O1D C2D 172.2(4) . . . . ? O17D Cu4 O1D C2D 70.9(11) . . . . ? O30 Cu4 O1D C2D -97.8(4) . . . . ? Cu3 Cu4 O1D C2D 179.7(3) . . . . ? N9A C10A O11A C12A 175.3(4) . . . . ? C16A C10A O11A C12A -63.9(5) . . . . ? C22A C12A O11A C10A -177.3(4) . . . . ? C13A C12A O11A C10A 63.1(5) . . . . ? N9B C10B O11B C12B 179.9(4) . . . . ? C16B C10B O11B C12B -63.0(5) . . . . ? C13B C12B O11B C10B 62.7(5) . . . . ? C22B C12B O11B C10B -178.3(4) . . . . ? C22C C12C O11C C10C -175.5(4) . . . . ? C13C C12C O11C C10C 63.8(5) . . . . ? N9C C10C O11C C12C 175.8(4) . . . . ? C16C C10C O11C C12C -64.9(5) . . . . ? N9D C10D O11D C12D 175.0(4) . . . . ? C16D C10D O11D C12D -63.0(5) . . . . ? C22D C12D O11D C10D -178.0(4) . . . . ? C13D C12D O11D C10D 62.7(5) . . . . ? C14A C16A O17A Cu2 -61.1(6) . . . . ? C10A C16A O17A Cu2 178.5(3) . . . . ? C14A C16A O17A Cu1 166.9(3) . . . . ? C10A C16A O17A Cu1 46.4(4) . . . . ? O1B Cu2 O17A C16A 37.4(5) . . . . ? N9B Cu2 O17A C16A -133.6(6) . . . . ? O17B Cu2 O17A C16A -138.5(5) . . . . ? Cu1 Cu2 O17A C16A -134.3(5) . . . . ? O1B Cu2 O17A Cu1 171.71(16) . . . . ? N9B Cu2 O17A Cu1 0.8(7) . . . . ? O17B Cu2 O17A Cu1 -4.14(16) . . . . ? O1A Cu1 O17A C16A 74.2(17) . . . . ? N9A Cu1 O17A C16A -24.8(3) . . . . ? O17B Cu1 O17A C16A 155.4(3) . . . . ? Cu2 Cu1 O17A C16A 151.2(4) . . . . ? O1A Cu1 O17A Cu2 -77.0(16) . . . . ? N9A Cu1 O17A Cu2 -176.02(18) . . . . ? O17B Cu1 O17A Cu2 4.17(16) . . . . ? C14B C16B O17B Cu1 -59.3(6) . . . . ? C10B C16B O17B Cu1 179.1(3) . . . . ? C14B C16B O17B Cu2 169.5(3) . . . . ? C10B C16B O17B Cu2 47.9(4) . . . . ? O1A Cu1 O17B C16B 37.7(5) . . . . ? N9A Cu1 O17B C16B -138.4(6) . . . . ? O17A Cu1 O17B C16B -137.6(5) . . . . ? Cu2 Cu1 O17B C16B -133.5(5) . . . . ? O1A Cu1 O17B Cu2 171.22(17) . . . . ? N9A Cu1 O17B Cu2 -4.9(8) . . . . ? O17A Cu1 O17B Cu2 -4.12(16) . . . . ? O1B Cu2 O17B C16B 60.1(18) . . . . ? O17A Cu2 O17B C16B 155.1(3) . . . . ? N9B Cu2 O17B C16B -23.7(3) . . . . ? Cu1 Cu2 O17B C16B 150.9(4) . . . . ? O1B Cu2 O17B Cu1 -90.8(18) . . . . ? O17A Cu2 O17B Cu1 4.17(16) . . . . ? N9B Cu2 O17B Cu1 -174.56(19) . . . . ? C10C C16C O17C Cu4 167.4(3) . . . . ? C14C C16C O17C Cu4 -73.6(5) . . . . ? C10C C16C O17C Cu3 50.9(4) . . . . ? C14C C16C O17C Cu3 169.8(3) . . . . ? O1D Cu4 O17C C16C 52.6(4) . . . . ? N9D Cu4 O17C C16C -162.6(5) . . . . ? O17D Cu4 O17C C16C -134.3(4) . . . . ? O30 Cu4 O17C C16C -45.9(4) . . . . ? Cu3 Cu4 O17C C16C -120.5(5) . . . . ? O1D Cu4 O17C Cu3 173.10(15) . . . . ? N9D Cu4 O17C Cu3 -42.1(6) . . . . ? O17D Cu4 O17C Cu3 -13.85(14) . . . . ? O30 Cu4 O17C Cu3 74.51(15) . . . . ? O1C Cu3 O17C C16C -4(6) . . . . ? O17D Cu3 O17C C16C 154.5(3) . . . . ? N9C Cu3 O17C C16C -27.9(3) . . . . ? Cu4 Cu3 O17C C16C 140.2(3) . . . . ? O1C Cu3 O17C Cu4 -144(6) . . . . ? O17D Cu3 O17C Cu4 14.25(15) . . . . ? N9C Cu3 O17C Cu4 -168.11(18) . . . . ? C14D C16D O17D Cu3 -68.7(6) . . . . ? C10D C16D O17D Cu3 171.3(3) . . . . ? C14D C16D O17D Cu4 170.0(3) . . . . ? C10D C16D O17D Cu4 50.0(4) . . . . ? O1C Cu3 O17D C16D 40.4(5) . . . . ? N9C Cu3 O17D C16D -149.7(7) . . . . ? O17C Cu3 O17D C16D -139.0(5) . . . . ? Cu4 Cu3 O17D C16D -124.9(5) . . . . ? O1C Cu3 O17D Cu4 165.38(15) . . . . ? N9C Cu3 O17D Cu4 -24.8(8) . . . . ? O17C Cu3 O17D Cu4 -14.03(14) . . . . ? O1D Cu4 O17D C16D -98.8(10) . . . . ? N9D Cu4 O17D C16D -29.0(3) . . . . ? O17C Cu4 O17D C16D 158.7(3) . . . . ? O30 Cu4 O17D C16D 70.0(3) . . . . ? Cu3 Cu4 O17D C16D 144.5(4) . . . . ? O1D Cu4 O17D Cu3 116.7(10) . . . . ? N9D Cu4 O17D Cu3 -173.47(17) . . . . ? O17C Cu4 O17D Cu3 14.20(15) . . . . ? O30 Cu4 O17D Cu3 -74.47(14) . . . . ? O21A C19A O18A C13A 63.1(5) . . . . ? C20A C19A O18A C13A -179.9(4) . . . . ? C14A C13A O18A C19A 178.3(4) . . . . ? C12A C13A O18A C19A -60.9(5) . . . . ? O21B C19B O18B C13B 63.5(5) . . . . ? C20B C19B O18B C13B -178.0(4) . . . . ? C14B C13B O18B C19B 176.4(4) . . . . ? C12B C13B O18B C19B -60.7(5) . . . . ? O21C C19C O18C C13C 64.8(5) . . . . ? C20C C19C O18C C13C -176.5(4) . . . . ? C14C C13C O18C C19C 179.4(4) . . . . ? C12C C13C O18C C19C -58.6(5) . . . . ? C14D C13D O18D C19D 178.8(4) . . . . ? C12D C13D O18D C19D -59.1(5) . . . . ? O21D C19D O18D C13D 62.8(5) . . . . ? C20D C19D O18D C13D -179.7(4) . . . . ? O18A C19A O21A C22A -60.9(5) . . . . ? C20A C19A O21A C22A -177.9(4) . . . . ? C12A C22A O21A C19A 56.9(6) . . . . ? O18B C19B O21B C22B -63.3(5) . . . . ? C20B C19B O21B C22B 178.5(4) . . . . ? C12B C22B O21B C19B 59.1(5) . . . . ? O18C C19C O21C C22C -64.6(5) . . . . ? C20C C19C O21C C22C 176.3(4) . . . . ? C12C C22C O21C C19C 59.2(5) . . . . ? O18D C19D O21D C22D -64.1(5) . . . . ? C20D C19D O21D C22D 179.2(4) . . . . ? C12D C22D O21D C19D 61.3(5) . . . . ? O1D Cu4 O30 S31 43.1(3) . . . . ? N9D Cu4 O30 S31 -51.8(4) . . . . ? O17C Cu4 O30 S31 142.9(3) . . . . ? O17D Cu4 O30 S31 -135.5(3) . . . . ? Cu3 Cu4 O30 S31 -175.7(3) . . . . ? Cu4 O30 S31 C32 -20.2(4) . . . . ? Cu4 O30 S31 C33 81.2(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O15A H15A O1B 0.838(10) 1.851(13) 2.685(4) 173(6) . O15B H15B O1A 0.840(10) 1.853(17) 2.675(4) 166(5) . O15C H15C O1D 0.842(10) 1.881(16) 2.708(4) 167(5) . O15C H15C O17C 0.842(10) 2.63(5) 3.053(4) 112(4) . O15D H15D O1C 0.843(10) 1.842(13) 2.680(4) 173(6) . _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.382 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.072 data_4 _database_code_CSD 193690 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H40 Br2 Cu2 N2 O14' _chemical_formula_weight 963.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 _symmetry_Int_Tables_number 1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.488(1) _cell_length_b 12.677(1) _cell_length_c 14.761(1) _cell_angle_alpha 110.07(1) _cell_angle_beta 102.19(1) _cell_angle_gamma 91.21(1) _cell_volume 1792.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18400 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description cubic _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 3.487 _exptl_absorpt_correction_type 'Empirical from multiple refl.' _exptl_absorpt_correction_T_min 0.6458 _exptl_absorpt_correction_T_max 0.6771 _exptl_absorpt_process_details 'MULABS (Platon2000; cf. Blessing 1995)' _exptl_special_details ; dx = 35 mm; 200 sec./deg., 1 deg.; mos. = 0.536(2) deg. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15930 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9701 _reflns_number_gt 9165 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (A.L.Spek, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+0.9402P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(6) _refine_ls_number_reflns 9701 _refine_ls_number_parameters 957 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0711 _refine_ls_wR_factor_gt 0.0697 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.030 _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 0.62749(5) 0.90592(5) 0.40813(3) 0.02560(14) Uani 1 1 d . . . Cu2 Cu 0.60919(6) 0.81230(5) 0.55931(4) 0.03175(16) Uani 1 1 d . . . Cu3 Cu 0.80551(6) 0.54391(5) 0.46162(4) 0.02891(15) Uani 1 1 d . . . Cu4 Cu 0.76956(6) 0.46082(5) 0.61701(4) 0.02880(15) Uani 1 1 d . . . C2A C 0.7052(5) 1.0503(4) 0.3119(3) 0.0256(11) Uani 1 1 d . . . C2B C 0.5225(5) 0.6785(4) 0.6640(3) 0.0319(12) Uani 1 1 d . . . C2C C 0.8578(5) 0.7070(4) 0.3729(3) 0.0277(11) Uani 1 1 d . . . C2D C 0.6402(5) 0.3590(4) 0.7248(3) 0.0263(11) Uani 1 1 d . . . C3A C 0.7964(5) 1.1338(4) 0.3128(3) 0.0297(11) Uani 1 1 d . . . H3A H 0.8537 1.1787 0.3739 0.036 Uiso 1 1 calc R . . C3B C 0.4447(6) 0.5857(4) 0.6630(3) 0.0366(13) Uani 1 1 d . . . H3B H 0.4028 0.5297 0.6012 0.044 Uiso 1 1 calc R . . C3C C 0.9313(6) 0.8032(4) 0.3761(3) 0.0361(13) Uani 1 1 d . . . H3C H 0.9882 0.8488 0.4371 0.043 Uiso 1 1 calc R . . C3D C 0.5445(5) 0.2798(4) 0.7235(3) 0.0346(13) Uani 1 1 d . . . H3D H 0.4948 0.2288 0.6617 0.041 Uiso 1 1 calc R . . C4A C 0.8049(5) 1.1522(4) 0.2272(3) 0.0302(12) Uani 1 1 d . . . H4A H 0.8679 1.2085 0.2293 0.036 Uiso 1 1 calc R . . C4B C 0.4281(5) 0.5744(4) 0.7498(3) 0.0318(12) Uani 1 1 d . . . H4B H 0.3733 0.5125 0.7476 0.038 Uiso 1 1 calc R . . C4C C 0.9235(6) 0.8331(4) 0.2949(3) 0.0355(13) Uani 1 1 d . . . H4C H 0.9760 0.8975 0.2993 0.043 Uiso 1 1 calc R . . C4D C 0.5207(5) 0.2742(4) 0.8100(3) 0.0336(12) Uani 1 1 d . . . H4D H 0.4553 0.2198 0.8079 0.040 Uiso 1 1 calc R . . C5A C 0.7196(5) 1.0871(4) 0.1374(3) 0.0271(11) Uani 1 1 d . . . C5B C 0.4925(5) 0.6546(4) 0.8404(3) 0.0267(11) Uani 1 1 d . . . C5C C 0.8385(5) 0.7689(4) 0.2057(3) 0.0295(11) Uani 1 1 d . . . C5D C 0.5935(5) 0.3491(4) 0.9007(3) 0.0281(11) Uani 1 1 d . . . C7A C 0.6244(5) 1.0102(4) 0.1335(3) 0.0247(11) Uani 1 1 d . . . H7A H 0.5644 0.9702 0.0723 0.030 Uiso 1 1 calc R . . C7B C 0.5703(5) 0.7443(4) 0.8441(3) 0.0262(11) Uani 1 1 d . . . H7B H 0.6128 0.7984 0.9068 0.031 Uiso 1 1 calc R . . C7C C 0.7597(5) 0.6787(4) 0.1987(3) 0.0272(11) Uani 1 1 d . . . H7C H 0.6995 0.6373 0.1380 0.033 Uiso 1 1 calc R . . C7D C 0.6917(5) 0.4248(4) 0.9061(3) 0.0283(11) Uani 1 1 d . . . H7D H 0.7424 0.4728 0.9688 0.034 Uiso 1 1 calc R . . C8A C 0.6139(5) 0.9890(4) 0.2214(3) 0.0244(11) Uani 1 1 d . . . C8B C 0.5889(5) 0.7583(4) 0.7579(3) 0.0254(11) Uani 1 1 d . . . C8C C 0.7677(5) 0.6463(4) 0.2833(3) 0.0249(10) Uani 1 1 d . . . C8D C 0.7181(5) 0.4317(4) 0.8173(3) 0.0258(11) Uani 1 1 d . . . C9A C 0.5227(5) 0.8969(4) 0.2078(3) 0.0246(11) Uani 1 1 d . . . H9A H 0.4611 0.8654 0.1458 0.030 Uiso 1 1 calc R . . C9B C 0.6803(5) 0.8514(4) 0.7692(3) 0.0262(11) Uani 1 1 d . . . H9B H 0.7257 0.8971 0.8345 0.031 Uiso 1 1 calc R . . C9C C 0.6843(5) 0.5466(4) 0.2679(3) 0.0248(11) Uani 1 1 d . . . H9C H 0.6214 0.5150 0.2065 0.030 Uiso 1 1 calc R . . C9D C 0.8257(5) 0.5103(4) 0.8282(3) 0.0266(11) Uani 1 1 d . . . H9D H 0.8732 0.5542 0.8934 0.032 Uiso 1 1 calc R . . C11A C 0.4377(5) 0.7492(4) 0.2539(3) 0.0211(10) Uani 1 1 d . . . H11A H 0.4869 0.6843 0.2244 0.025 Uiso 1 1 calc R . . C11B C 0.8069(5) 0.9590(4) 0.7075(3) 0.0247(11) Uani 1 1 d . . . H11B H 0.8842 0.9185 0.6903 0.030 Uiso 1 1 calc R . . C11C C 0.6086(4) 0.3950(4) 0.3109(3) 0.0241(10) Uani 1 1 d . . . H11C H 0.6602 0.3297 0.2874 0.029 Uiso 1 1 calc R . . C11D C 0.9758(5) 0.5987(4) 0.7654(3) 0.0274(11) Uani 1 1 d . . . H11D H 1.0479 0.5510 0.7475 0.033 Uiso 1 1 calc R . . C13A C 0.2500(5) 0.6298(4) 0.1651(3) 0.0243(10) Uani 1 1 d . . . H13A H 0.3039 0.5687 0.1357 0.029 Uiso 1 1 calc R . . C13B C 0.9603(5) 1.1065(4) 0.8134(3) 0.0260(11) Uani 1 1 d . . . H13B H 1.0310 1.0578 0.7941 0.031 Uiso 1 1 calc R . . C13C C 0.4192(5) 0.2777(4) 0.2164(3) 0.0253(10) Uani 1 1 d . . . H13C H 0.4720 0.2134 0.1926 0.030 Uiso 1 1 calc R . . C13D C 1.1364(5) 0.7415(4) 0.8684(3) 0.0274(11) Uani 1 1 d . . . H13D H 1.2049 0.6906 0.8480 0.033 Uiso 1 1 calc R . . C14A C 0.2232(5) 0.6214(4) 0.2609(3) 0.0229(10) Uani 1 1 d . . . H14A H 0.1681 0.6824 0.2886 0.028 Uiso 1 1 calc R . . C14B C 0.9259(5) 1.1731(4) 0.7444(3) 0.0243(11) Uani 1 1 d . . . H14B H 0.8547 1.2209 0.7641 0.029 Uiso 1 1 calc R . . C14C C 0.3795(5) 0.2768(4) 0.3104(3) 0.0279(11) Uani 1 1 d . . . H14C H 0.3256 0.3406 0.3329 0.034 Uiso 1 1 calc R . . C14D C 1.1036(5) 0.8098(4) 0.8000(3) 0.0275(11) Uani 1 1 d . . . H14D H 1.0323 0.8579 0.8191 0.033 Uiso 1 1 calc R . . C15A C 0.3482(5) 0.6338(4) 0.3382(3) 0.0255(11) Uani 1 1 d . . . H15A H 0.4025 0.5710 0.3133 0.031 Uiso 1 1 calc R . . C15B C 0.8786(5) 1.0951(4) 0.6375(3) 0.0280(11) Uani 1 1 d . . . H15B H 0.9502 1.0490 0.6159 0.034 Uiso 1 1 calc R . . C15C C 0.5002(5) 0.2891(4) 0.3937(3) 0.0292(11) Uani 1 1 d . . . H15C H 0.5536 0.2245 0.3723 0.035 Uiso 1 1 calc R . . C15D C 1.0579(5) 0.7306(4) 0.6927(3) 0.0306(11) Uani 1 1 d . . . H15D H 1.1285 0.6825 0.6722 0.037 Uiso 1 1 calc R . . C17A C 0.4209(5) 0.7470(4) 0.3547(3) 0.0238(10) Uani 1 1 d . . . H17A H 0.3679 0.8092 0.3836 0.029 Uiso 1 1 calc R . . C17B C 0.7622(5) 1.0177(4) 0.6332(3) 0.0272(11) Uani 1 1 d . . . H17B H 0.6881 1.0629 0.6506 0.033 Uiso 1 1 calc R . . C17C C 0.5792(4) 0.3989(4) 0.4109(3) 0.0246(10) Uani 1 1 d . . . H17C H 0.5270 0.4635 0.4351 0.029 Uiso 1 1 calc R . . C17D C 0.9377(5) 0.6571(4) 0.6900(3) 0.0254(10) Uani 1 1 d . . . H17D H 0.8667 0.7062 0.7078 0.030 Uiso 1 1 calc R . . C20A C 0.0290(5) 0.5105(4) 0.1702(3) 0.0267(11) Uani 1 1 d . . . H20A H -0.0188 0.5753 0.2022 0.032 Uiso 1 1 calc R . . C20B C 1.0832(5) 1.3188(4) 0.8575(3) 0.0296(11) Uani 1 1 d . . . H20B H 1.0120 1.3664 0.8776 0.035 Uiso 1 1 calc R . . C20C C 0.1872(5) 0.1641(5) 0.2116(3) 0.0318(12) Uani 1 1 d . . . H20C H 0.1347 0.2282 0.2369 0.038 Uiso 1 1 calc R . . C20D C 1.2592(5) 0.9561(4) 0.9117(3) 0.0324(12) Uani 1 1 d . . . H20D H 1.1870 1.0028 0.9311 0.039 Uiso 1 1 calc R . . C21A C -0.0505(5) 0.3993(4) 0.1503(3) 0.0347(12) Uani 1 1 d . . . H21A H -0.1356 0.3945 0.1053 0.052 Uiso 1 1 calc R . . H21B H -0.0641 0.3959 0.2129 0.052 Uiso 1 1 calc R . . H21C H -0.0028 0.3361 0.1197 0.052 Uiso 1 1 calc R . . C21B C 1.2012(6) 1.3929(5) 0.8658(4) 0.0424(14) Uani 1 1 d . . . H21D H 1.1782 1.4362 0.8219 0.064 Uiso 1 1 calc R . . H21E H 1.2711 1.3462 0.8464 0.064 Uiso 1 1 calc R . . H21F H 1.2316 1.4451 0.9344 0.064 Uiso 1 1 calc R . . C21C C 0.1081(6) 0.0543(5) 0.1879(4) 0.0408(14) Uani 1 1 d . . . H21G H 0.0282 0.0475 0.1369 0.061 Uiso 1 1 calc R . . H21H H 0.0843 0.0518 0.2479 0.061 Uiso 1 1 calc R . . H21I H 0.1600 -0.0082 0.1633 0.061 Uiso 1 1 calc R . . C21D C 1.3763(6) 1.0307(5) 0.9181(4) 0.0436(15) Uani 1 1 d . . . H21J H 1.4072 1.0838 0.9863 0.065 Uiso 1 1 calc R . . H21K H 1.3517 1.0729 0.8735 0.065 Uiso 1 1 calc R . . H21L H 1.4463 0.9843 0.8986 0.065 Uiso 1 1 calc R . . C23A C 0.1194(5) 0.6183(4) 0.0928(3) 0.0308(12) Uani 1 1 d . . . H23A H 0.0698 0.6829 0.1195 0.037 Uiso 1 1 calc R . . H23B H 0.1343 0.6183 0.0287 0.037 Uiso 1 1 calc R . . C23B C 1.0079(5) 1.1881(5) 0.9193(3) 0.0326(12) Uani 1 1 d . . . H23C H 0.9376 1.2350 0.9403 0.039 Uiso 1 1 calc R . . H23D H 1.0338 1.1463 0.9649 0.039 Uiso 1 1 calc R . . C23C C 0.2948(5) 0.2657(4) 0.1379(3) 0.0303(12) Uani 1 1 d . . . H23E H 0.2448 0.3314 0.1599 0.036 Uiso 1 1 calc R . . H23F H 0.3171 0.2627 0.0752 0.036 Uiso 1 1 calc R . . C23D C 1.1875(5) 0.8243(4) 0.9752(3) 0.0330(12) Uani 1 1 d . . . H23G H 1.1176 0.8708 0.9975 0.040 Uiso 1 1 calc R . . H23H H 1.2150 0.7823 1.0204 0.040 Uiso 1 1 calc R . . N10A N 0.5188(4) 0.8536(3) 0.2750(2) 0.0220(8) Uani 1 1 d . . . N10B N 0.7040(4) 0.8761(3) 0.6971(3) 0.0276(10) Uani 1 1 d . . . N10C N 0.6896(4) 0.4982(3) 0.3313(2) 0.0245(9) Uani 1 1 d . . . N10D N 0.8613(4) 0.5245(3) 0.7558(3) 0.0260(9) Uani 1 1 d . . . O1A O 0.7073(3) 1.0337(3) 0.3962(2) 0.0309(8) Uani 1 1 d . . . O1B O 0.5310(4) 0.6857(3) 0.5774(2) 0.0356(9) Uani 1 1 d . . . O1C O 0.8776(3) 0.6784(3) 0.4526(2) 0.0337(9) Uani 1 1 d . . . O1D O 0.6514(4) 0.3633(3) 0.6381(2) 0.0338(9) Uani 1 1 d . . . O12A O 0.3172(3) 0.7389(3) 0.1861(2) 0.0251(7) Uani 1 1 d . . . O12B O 0.8469(3) 1.0374(3) 0.8071(2) 0.0307(8) Uani 1 1 d . . . O12C O 0.4935(3) 0.3818(3) 0.2362(2) 0.0263(8) Uani 1 1 d . . . O12D O 1.0204(3) 0.6756(3) 0.8645(2) 0.0292(8) Uani 1 1 d . . . O16A O 0.3144(4) 0.6307(4) 0.4243(2) 0.0457(11) Uani 1 1 d D . . H16A H 0.381(4) 0.637(6) 0.470(3) 0.069 Uiso 1 1 d D . . O16B O 0.8445(4) 1.1637(3) 0.5783(2) 0.0400(10) Uani 1 1 d D . . H16B H 0.820(6) 1.119(4) 0.5195(17) 0.060 Uiso 1 1 d D . . O16C O 0.4552(4) 0.2873(4) 0.4773(2) 0.0414(10) Uani 1 1 d D . . H16C H 0.521(4) 0.292(5) 0.522(3) 0.062 Uiso 1 1 d D . . O16D O 1.0271(4) 0.7979(3) 0.6335(2) 0.0343(9) Uani 1 1 d D . . H16D H 0.968(4) 0.763(5) 0.583(3) 0.051 Uiso 1 1 d D . . O18A O 0.5482(3) 0.7684(3) 0.4161(2) 0.0296(8) Uani 1 1 d . . . O18B O 0.7178(4) 0.9276(3) 0.5413(2) 0.0324(9) Uani 1 1 d . . . O18C O 0.7038(3) 0.4194(3) 0.4764(2) 0.0286(8) Uani 1 1 d . . . O18D O 0.8872(3) 0.5682(3) 0.5988(2) 0.0323(8) Uani 1 1 d . . . O19A O 0.1507(3) 0.5143(3) 0.2347(2) 0.0257(7) Uani 1 1 d . . . O19B O 1.0398(3) 1.2450(3) 0.7566(2) 0.0291(8) Uani 1 1 d . . . O19C O 0.3017(3) 0.1723(3) 0.2849(2) 0.0307(8) Uani 1 1 d . . . O19D O 1.2174(3) 0.8800(3) 0.8116(2) 0.0322(8) Uani 1 1 d . . . O22A O 0.0457(3) 0.5141(3) 0.0780(2) 0.0328(8) Uani 1 1 d . . . O22B O 1.1186(3) 1.2579(3) 0.9211(2) 0.0322(8) Uani 1 1 d . . . O22C O 0.2183(3) 0.1649(3) 0.1226(2) 0.0327(8) Uani 1 1 d . . . O22D O 1.2962(4) 0.8946(3) 0.9766(2) 0.0350(9) Uani 1 1 d . . . Br6A Br 0.74649(5) 1.09896(4) 0.01770(3) 0.03662(14) Uani 1 1 d . . . Br6B Br 0.46666(5) 0.63809(4) 0.95913(3) 0.03200(12) Uani 1 1 d . . . Br6C Br 0.83855(5) 0.80276(4) 0.08911(3) 0.03459(13) Uani 1 1 d . . . Br6D Br 0.54896(5) 0.34843(4) 1.01945(3) 0.03665(14) Uani 1 1 d . . . C40 C 0.2553(11) 1.0279(8) 0.4198(7) 0.116(4) Uani 1 1 d . . . H40A H 0.2134 0.9869 0.4530 0.174 Uiso 1 1 calc R . . H40B H 0.2544 0.9775 0.3523 0.174 Uiso 1 1 calc R . . H40C H 0.2074 1.0927 0.4172 0.174 Uiso 1 1 calc R . . O41 O 0.3893(7) 1.0672(5) 0.4744(5) 0.106(2) Uani 1 1 d . . . H41 H 0.4301 1.0117 0.4774 0.160 Uiso 1 1 calc R . . C50 C 0.3313(8) 0.9162(7) 0.6315(6) 0.086(3) Uani 1 1 d . . . H50A H 0.3618 0.9036 0.6942 0.129 Uiso 1 1 calc R . . H50B H 0.2786 0.8482 0.5820 0.129 Uiso 1 1 calc R . . H50C H 0.2778 0.9798 0.6421 0.129 Uiso 1 1 calc R . . O51 O 0.4438(5) 0.9414(4) 0.5964(4) 0.0642(12) Uani 1 1 d . . . H51 H 0.4269 0.9900 0.5698 0.096 Uiso 1 1 calc R . . C60 C 1.0899(5) 0.4768(5) 0.4360(4) 0.0426(14) Uani 1 1 d . . . H60A H 1.0882 0.5237 0.3950 0.064 Uiso 1 1 calc R . . H60B H 1.1534 0.4214 0.4210 0.064 Uiso 1 1 calc R . . H60C H 1.1155 0.5248 0.5062 0.064 Uiso 1 1 calc R . . O61 O 0.9619(3) 0.4190(3) 0.4150(2) 0.0353(8) Uani 1 1 d . . . H61 H 0.9600 0.3874 0.4563 0.053 Uiso 1 1 calc R . . C70 C 1.1409(8) 0.3023(8) 0.5797(6) 0.091(3) Uani 1 1 d . . . H70A H 1.1913 0.3763 0.6157 0.137 Uiso 1 1 calc R . . H70B H 1.1696 0.2652 0.5183 0.137 Uiso 1 1 calc R . . H70C H 1.1553 0.2556 0.6211 0.137 Uiso 1 1 calc R . . O71 O 1.0060(6) 0.3164(5) 0.5563(4) 0.093(2) Uani 1 1 d . . . H71 H 0.9621 0.2650 0.5636 0.139 Uiso 1 1 calc R . . 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 0.0285(3) 0.0316(3) 0.0144(2) 0.0099(2) -0.0010(2) -0.0123(3) Cu2 0.0402(4) 0.0337(4) 0.0170(3) 0.0123(2) -0.0061(2) -0.0174(3) Cu3 0.0289(4) 0.0388(4) 0.0159(3) 0.0116(2) -0.0031(2) -0.0120(3) Cu4 0.0345(4) 0.0331(3) 0.0158(3) 0.0104(2) -0.0021(2) -0.0090(3) C2A 0.029(3) 0.029(3) 0.019(2) 0.0105(19) 0.0035(19) 0.000(2) C2B 0.040(3) 0.030(3) 0.022(2) 0.011(2) 0.000(2) -0.006(2) C2C 0.033(3) 0.029(3) 0.020(2) 0.0087(19) 0.006(2) -0.007(2) C2D 0.032(3) 0.027(3) 0.019(2) 0.0077(19) 0.004(2) -0.004(2) C3A 0.039(3) 0.028(3) 0.021(2) 0.0086(19) 0.006(2) -0.006(2) C3B 0.049(4) 0.031(3) 0.023(2) 0.011(2) -0.006(2) -0.015(3) C3C 0.043(3) 0.031(3) 0.024(2) 0.006(2) -0.004(2) -0.009(2) C3D 0.044(3) 0.031(3) 0.019(2) 0.001(2) 0.000(2) -0.007(2) C4A 0.037(3) 0.024(3) 0.032(2) 0.012(2) 0.010(2) -0.006(2) C4B 0.035(3) 0.026(3) 0.033(3) 0.016(2) -0.002(2) -0.009(2) C4C 0.045(3) 0.030(3) 0.031(3) 0.014(2) 0.004(2) -0.006(2) C4D 0.038(3) 0.035(3) 0.026(2) 0.012(2) 0.004(2) -0.009(2) C5A 0.033(3) 0.028(3) 0.027(2) 0.015(2) 0.012(2) 0.000(2) C5B 0.032(3) 0.031(3) 0.021(2) 0.017(2) 0.004(2) 0.002(2) C5C 0.031(3) 0.038(3) 0.027(2) 0.020(2) 0.010(2) 0.004(2) C5D 0.037(3) 0.030(3) 0.021(2) 0.013(2) 0.010(2) 0.005(2) C7A 0.030(3) 0.027(3) 0.016(2) 0.0091(19) 0.0028(19) -0.003(2) C7B 0.033(3) 0.028(3) 0.017(2) 0.0092(19) 0.0008(19) -0.004(2) C7C 0.022(3) 0.036(3) 0.024(2) 0.013(2) 0.0042(19) 0.000(2) C7D 0.035(3) 0.031(3) 0.018(2) 0.010(2) 0.002(2) 0.000(2) C8A 0.028(3) 0.026(3) 0.020(2) 0.0092(18) 0.0053(19) -0.005(2) C8B 0.026(3) 0.028(3) 0.024(2) 0.0136(19) 0.0007(19) 0.000(2) C8C 0.022(3) 0.033(3) 0.023(2) 0.015(2) 0.0040(19) -0.001(2) C8D 0.032(3) 0.028(3) 0.019(2) 0.0118(19) 0.0026(19) 0.002(2) C9A 0.027(3) 0.031(3) 0.015(2) 0.0074(19) 0.0039(18) -0.002(2) C9B 0.031(3) 0.028(3) 0.015(2) 0.0080(19) -0.0029(18) -0.009(2) C9C 0.024(3) 0.032(3) 0.016(2) 0.0053(19) 0.0037(18) -0.001(2) C9D 0.028(3) 0.031(3) 0.017(2) 0.0074(19) -0.0018(19) 0.004(2) C11A 0.022(2) 0.023(2) 0.017(2) 0.0072(18) 0.0012(17) -0.0046(19) C11B 0.028(3) 0.026(3) 0.014(2) 0.0062(18) -0.0037(18) -0.012(2) C11C 0.020(3) 0.035(3) 0.016(2) 0.0075(19) 0.0027(18) -0.002(2) C11D 0.029(3) 0.036(3) 0.013(2) 0.0066(19) -0.0001(19) -0.006(2) C13A 0.028(3) 0.025(3) 0.018(2) 0.0078(18) 0.0010(19) -0.008(2) C13B 0.023(3) 0.029(3) 0.021(2) 0.0093(19) -0.0059(18) -0.006(2) C13C 0.023(3) 0.032(3) 0.016(2) 0.0060(18) 0.0011(18) -0.006(2) C13D 0.026(3) 0.030(3) 0.021(2) 0.0075(19) -0.0016(19) -0.004(2) C14A 0.026(3) 0.024(2) 0.019(2) 0.0088(18) 0.0045(18) -0.003(2) C14B 0.020(3) 0.029(3) 0.022(2) 0.0102(19) -0.0003(19) -0.010(2) C14C 0.031(3) 0.028(3) 0.020(2) 0.0070(19) 0.001(2) -0.008(2) C14D 0.023(3) 0.030(3) 0.025(2) 0.011(2) -0.0038(19) -0.011(2) C15A 0.029(3) 0.028(3) 0.019(2) 0.0117(19) 0.0018(19) -0.009(2) C15B 0.031(3) 0.033(3) 0.016(2) 0.0090(19) -0.0021(19) -0.010(2) C15C 0.034(3) 0.034(3) 0.022(2) 0.015(2) 0.004(2) -0.004(2) C15D 0.036(3) 0.038(3) 0.013(2) 0.0083(19) -0.0043(19) -0.003(2) C17A 0.026(3) 0.030(3) 0.0136(19) 0.0074(18) 0.0026(18) -0.007(2) C17B 0.026(3) 0.032(3) 0.018(2) 0.0083(19) -0.0039(18) -0.007(2) C17C 0.021(3) 0.033(3) 0.017(2) 0.0100(18) -0.0007(18) -0.007(2) C17D 0.026(3) 0.028(3) 0.020(2) 0.0104(19) -0.0010(18) -0.003(2) C20A 0.021(3) 0.030(3) 0.028(2) 0.011(2) 0.0026(19) -0.004(2) C20B 0.029(3) 0.027(3) 0.025(2) 0.0070(19) -0.004(2) -0.011(2) C20C 0.022(3) 0.046(3) 0.023(2) 0.008(2) 0.002(2) -0.009(2) C20D 0.041(3) 0.027(3) 0.021(2) 0.0066(19) -0.005(2) -0.005(2) C21A 0.029(3) 0.036(3) 0.030(2) 0.008(2) -0.003(2) -0.014(2) C21B 0.047(4) 0.036(3) 0.033(3) 0.013(2) -0.013(2) -0.018(3) C21C 0.035(3) 0.049(4) 0.032(3) 0.012(2) 0.002(2) -0.015(3) C21D 0.052(4) 0.034(3) 0.035(3) 0.013(2) -0.010(3) -0.015(3) C23A 0.030(3) 0.037(3) 0.028(2) 0.019(2) 0.001(2) -0.009(2) C23B 0.035(3) 0.037(3) 0.021(2) 0.010(2) -0.002(2) -0.012(2) C23C 0.027(3) 0.039(3) 0.021(2) 0.010(2) 0.000(2) -0.004(2) C23D 0.038(3) 0.037(3) 0.016(2) 0.006(2) -0.005(2) -0.009(2) N10A 0.022(2) 0.024(2) 0.0181(18) 0.0072(15) 0.0024(15) -0.0086(16) N10B 0.033(3) 0.028(2) 0.0180(19) 0.0093(16) -0.0025(16) -0.0079(19) N10C 0.024(2) 0.032(2) 0.0152(17) 0.0068(16) 0.0031(15) -0.0042(17) N10D 0.029(2) 0.029(2) 0.0192(18) 0.0106(16) 0.0013(16) -0.0028(18) O1A 0.035(2) 0.038(2) 0.0178(15) 0.0122(14) -0.0008(14) -0.0150(16) O1B 0.053(2) 0.034(2) 0.0184(16) 0.0135(14) -0.0004(15) -0.0166(17) O1C 0.043(2) 0.037(2) 0.0193(16) 0.0143(14) -0.0025(14) -0.0123(17) O1D 0.040(2) 0.042(2) 0.0171(15) 0.0127(14) -0.0001(14) -0.0123(17) O12A 0.0262(19) 0.0288(18) 0.0199(15) 0.0127(13) -0.0013(13) -0.0063(14) O12B 0.035(2) 0.036(2) 0.0159(15) 0.0087(14) -0.0022(13) -0.0150(16) O12C 0.0230(18) 0.036(2) 0.0162(14) 0.0096(13) -0.0021(12) -0.0053(15) O12D 0.032(2) 0.0368(19) 0.0120(13) 0.0063(13) -0.0042(12) -0.0107(16) O16A 0.047(3) 0.065(3) 0.0211(17) 0.0203(17) -0.0061(15) -0.035(2) O16B 0.053(3) 0.041(2) 0.0212(16) 0.0168(16) -0.0105(16) -0.0200(19) O16C 0.034(2) 0.068(3) 0.0232(17) 0.0226(17) -0.0003(15) -0.021(2) O16D 0.048(2) 0.033(2) 0.0186(16) 0.0123(14) -0.0020(15) -0.0089(17) O18A 0.032(2) 0.0353(19) 0.0182(15) 0.0120(14) -0.0026(13) -0.0142(15) O18B 0.044(2) 0.033(2) 0.0151(15) 0.0108(14) -0.0054(14) -0.0171(16) O18C 0.0246(19) 0.039(2) 0.0188(15) 0.0115(14) -0.0022(13) -0.0077(15) O18D 0.041(2) 0.036(2) 0.0129(14) 0.0074(13) -0.0047(14) -0.0167(16) O19A 0.0263(19) 0.0254(18) 0.0220(15) 0.0081(13) 0.0003(13) -0.0077(14) O19B 0.0289(19) 0.0321(19) 0.0207(15) 0.0082(14) -0.0025(13) -0.0127(15) O19C 0.028(2) 0.035(2) 0.0262(16) 0.0122(14) 0.0002(14) -0.0127(16) O19D 0.035(2) 0.035(2) 0.0192(15) 0.0076(14) -0.0044(14) -0.0132(16) O22A 0.032(2) 0.038(2) 0.0241(16) 0.0129(14) -0.0055(14) -0.0142(16) O22B 0.033(2) 0.0331(19) 0.0235(16) 0.0114(14) -0.0085(14) -0.0137(15) O22C 0.033(2) 0.037(2) 0.0202(15) 0.0064(14) -0.0003(14) -0.0143(16) O22D 0.042(2) 0.032(2) 0.0236(16) 0.0106(14) -0.0079(14) -0.0082(16) Br6A 0.0465(3) 0.0419(3) 0.0265(2) 0.0180(2) 0.0106(2) -0.0099(3) Br6B 0.0364(3) 0.0373(3) 0.0261(2) 0.0172(2) 0.0059(2) -0.0049(2) Br6C 0.0344(3) 0.0457(3) 0.0333(3) 0.0257(2) 0.0088(2) 0.0034(2) Br6D 0.0438(3) 0.0436(3) 0.0227(2) 0.0127(2) 0.0078(2) -0.0096(2) C40 0.152(10) 0.069(6) 0.107(7) 0.049(5) -0.039(6) -0.011(6) O41 0.119(5) 0.098(4) 0.092(4) 0.063(4) -0.039(4) -0.063(4) C50 0.075(6) 0.095(6) 0.151(8) 0.081(6) 0.091(6) 0.038(5) O51 0.059(3) 0.069(3) 0.073(3) 0.037(2) 0.014(2) 0.004(2) C60 0.034(3) 0.061(4) 0.033(3) 0.018(3) 0.007(2) -0.010(3) O61 0.033(2) 0.039(2) 0.0345(18) 0.0162(16) 0.0053(15) -0.0104(16) C70 0.073(6) 0.136(8) 0.083(5) 0.068(6) 0.009(5) -0.012(6) O71 0.098(5) 0.100(4) 0.094(4) 0.079(4) -0.018(3) -0.045(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1A 1.885(3) . ? Cu1 O18B 1.915(3) . ? Cu1 N10A 1.931(3) . ? Cu1 O18A 1.965(3) . ? Cu1 Cu2 2.9007(7) . ? Cu2 O1B 1.911(3) . ? Cu2 N10B 1.940(3) . ? Cu2 O18A 1.948(3) . ? Cu2 O18B 1.957(3) . ? Cu3 O1C 1.908(3) . ? Cu3 N10C 1.932(3) . ? Cu3 O18D 1.938(3) . ? Cu3 O18C 1.986(3) . ? Cu3 Cu4 2.9189(7) . ? Cu4 O1D 1.877(3) . ? Cu4 O18C 1.921(3) . ? Cu4 O18D 1.941(3) . ? Cu4 N10D 1.942(3) . ? C2A O1A 1.328(5) . ? C2A C3A 1.407(7) . ? C2A C8A 1.421(6) . ? C2B O1B 1.333(6) . ? C2B C3B 1.411(7) . ? C2B C8B 1.425(6) . ? C2C O1C 1.323(5) . ? C2C C8C 1.406(6) . ? C2C C3C 1.409(7) . ? C2D O1D 1.328(5) . ? C2D C3D 1.397(7) . ? C2D C8D 1.419(6) . ? C3A C4A 1.382(6) . ? C3A H3A 0.9500 . ? C3B C4B 1.384(7) . ? C3B H3B 0.9500 . ? C3C C4C 1.364(7) . ? C3C H3C 0.9500 . ? C3D C4D 1.375(7) . ? C3D H3D 0.9500 . ? C4A C5A 1.398(7) . ? C4A H4A 0.9500 . ? C4B C5B 1.391(6) . ? C4B H4B 0.9500 . ? C4C C5C 1.389(7) . ? C4C H4C 0.9500 . ? C4D C5D 1.394(7) . ? C4D H4D 0.9500 . ? C5A C7A 1.359(7) . ? C5A Br6A 1.901(4) . ? C5B C7B 1.364(7) . ? C5B Br6B 1.908(4) . ? C5C C7C 1.359(7) . ? C5C Br6C 1.911(4) . ? C5D C7D 1.364(7) . ? C5D Br6D 1.909(4) . ? C7A C8A 1.437(6) . ? C7A H7A 0.9500 . ? C7B C8B 1.396(6) . ? C7B H7B 0.9500 . ? C7C C8C 1.430(6) . ? C7C H7C 0.9500 . ? C7D C8D 1.426(6) . ? C7D H7D 0.9500 . ? C8A C9A 1.425(6) . ? C8B C9B 1.446(6) . ? C8C C9C 1.444(6) . ? C8D C9D 1.435(7) . ? C9A N10A 1.295(6) . ? C9A H9A 0.9500 . ? C9B N10B 1.277(6) . ? C9B H9B 0.9500 . ? C9C N10C 1.277(6) . ? C9C H9C 0.9500 . ? C9D N10D 1.270(6) . ? C9D H9D 0.9500 . ? C11A O12A 1.409(5) . ? C11A N10A 1.458(6) . ? C11A C17A 1.545(6) . ? C11A H11A 1.0000 . ? C11B O12B 1.430(5) . ? C11B N10B 1.437(6) . ? C11B C17B 1.528(6) . ? C11B H11B 1.0000 . ? C11C O12C 1.416(5) . ? C11C N10C 1.448(6) . ? C11C C17C 1.555(6) . ? C11C H11C 1.0000 . ? C11D O12D 1.422(5) . ? C11D N10D 1.462(6) . ? C11D C17D 1.529(6) . ? C11D H11D 1.0000 . ? C13A O12A 1.442(5) . ? C13A C23A 1.518(6) . ? C13A C14A 1.536(6) . ? C13A H13A 1.0000 . ? C13B O12B 1.429(5) . ? C13B C23B 1.517(6) . ? C13B C14B 1.527(6) . ? C13B H13B 1.0000 . ? C13C O12C 1.424(5) . ? C13C C23C 1.516(6) . ? C13C C14C 1.535(6) . ? C13C H13C 1.0000 . ? C13D O12D 1.440(6) . ? C13D C14D 1.535(6) . ? C13D C23D 1.535(6) . ? C13D H13D 1.0000 . ? C14A O19A 1.430(5) . ? C14A C15A 1.511(6) . ? C14A H14A 1.0000 . ? C14B O19B 1.429(5) . ? C14B C15B 1.514(6) . ? C14B H14B 1.0000 . ? C14C O19C 1.430(6) . ? C14C C15C 1.530(6) . ? C14C H14C 1.0000 . ? C14D O19D 1.418(6) . ? C14D C15D 1.521(6) . ? C14D H14D 1.0000 . ? C15A O16A 1.402(5) . ? C15A C17A 1.529(6) . ? C15A H15A 1.0000 . ? C15B O16B 1.433(6) . ? C15B C17B 1.527(6) . ? C15B H15B 1.0000 . ? C15C O16C 1.418(6) . ? C15C C17C 1.520(6) . ? C15C H15C 1.0000 . ? C15D O16D 1.415(6) . ? C15D C17D 1.537(7) . ? C15D H15D 1.0000 . ? C17A O18A 1.408(5) . ? C17A H17A 1.0000 . ? C17B O18B 1.417(5) . ? C17B H17B 1.0000 . ? C17C O18C 1.411(5) . ? C17C H17C 1.0000 . ? C17D O18D 1.412(5) . ? C17D H17D 1.0000 . ? C20A O19A 1.410(6) . ? C20A O22A 1.424(5) . ? C20A C21A 1.527(6) . ? C20A H20A 1.0000 . ? C20B O22B 1.406(6) . ? C20B O19B 1.428(5) . ? C20B C21B 1.496(7) . ? C20B H20B 1.0000 . ? C20C O19C 1.411(6) . ? C20C O22C 1.422(5) . ? C20C C21C 1.498(7) . ? C20C H20C 1.0000 . ? C20D O19D 1.426(5) . ? C20D O22D 1.430(6) . ? C20D C21D 1.501(7) . ? C20D H20D 1.0000 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C21C H21G 0.9800 . ? C21C H21H 0.9800 . ? C21C H21I 0.9800 . ? C21D H21J 0.9800 . ? C21D H21K 0.9800 . ? C21D H21L 0.9800 . ? C23A O22A 1.442(6) . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? C23B O22B 1.436(6) . ? C23B H23C 0.9900 . ? C23B H23D 0.9900 . ? C23C O22C 1.418(6) . ? C23C H23E 0.9900 . ? C23C H23F 0.9900 . ? C23D O22D 1.424(6) . ? C23D H23G 0.9900 . ? C23D H23H 0.9900 . ? O16A H16A 0.839(10) . ? O16B H16B 0.839(10) . ? O16C H16C 0.836(10) . ? O16D H16D 0.834(10) . ? C40 O41 1.445(11) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? O41 H41 0.8400 . ? C50 O51 1.456(7) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? O51 H51 0.8400 . ? C60 O61 1.436(6) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? O61 H61 0.8400 . ? C70 O71 1.414(10) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? O71 H71 0.8400 . ? 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 O1A Cu1 O18B 98.50(13) . . ? O1A Cu1 N10A 94.35(14) . . ? O18B Cu1 N10A 167.14(15) . . ? O1A Cu1 O18A 177.44(15) . . ? O18B Cu1 O18A 82.51(13) . . ? N10A Cu1 O18A 84.63(14) . . ? O1A Cu1 Cu2 139.54(9) . . ? O18B Cu1 Cu2 42.03(10) . . ? N10A Cu1 Cu2 125.39(11) . . ? O18A Cu1 Cu2 41.93(8) . . ? O1B Cu2 N10B 92.78(15) . . ? O1B Cu2 O18A 99.64(13) . . ? N10B Cu2 O18A 166.20(15) . . ? O1B Cu2 O18B 169.63(17) . . ? N10B Cu2 O18B 84.81(14) . . ? O18A Cu2 O18B 81.90(12) . . ? O1B Cu2 Cu1 141.99(9) . . ? N10B Cu2 Cu1 125.14(12) . . ? O18A Cu2 Cu1 42.40(9) . . ? O18B Cu2 Cu1 40.94(9) . . ? O1C Cu3 N10C 93.52(14) . . ? O1C Cu3 O18D 99.38(13) . . ? N10C Cu3 O18D 165.36(15) . . ? O1C Cu3 O18C 169.82(16) . . ? N10C Cu3 O18C 84.58(14) . . ? O18D Cu3 O18C 81.51(12) . . ? O1C Cu3 Cu4 137.77(9) . . ? N10C Cu3 Cu4 124.31(11) . . ? O18D Cu3 Cu4 41.24(9) . . ? O18C Cu3 Cu4 40.81(8) . . ? O1D Cu4 O18C 97.91(13) . . ? O1D Cu4 O18D 177.00(16) . . ? O18C Cu4 O18D 83.12(13) . . ? O1D Cu4 N10D 93.93(15) . . ? O18C Cu4 N10D 168.17(15) . . ? O18D Cu4 N10D 85.05(14) . . ? O1D Cu4 Cu3 139.36(9) . . ? O18C Cu4 Cu3 42.51(10) . . ? O18D Cu4 Cu3 41.17(8) . . ? N10D Cu4 Cu3 125.79(12) . . ? O1A C2A C3A 118.2(4) . . ? O1A C2A C8A 123.1(4) . . ? C3A C2A C8A 118.6(4) . . ? O1B C2B C3B 118.3(4) . . ? O1B C2B C8B 123.9(4) . . ? C3B C2B C8B 117.8(4) . . ? O1C C2C C8C 123.9(4) . . ? O1C C2C C3C 119.0(4) . . ? C8C C2C C3C 117.1(4) . . ? O1D C2D C3D 117.5(4) . . ? O1D C2D C8D 123.4(4) . . ? C3D C2D C8D 119.1(4) . . ? C4A C3A C2A 121.7(4) . . ? C4A C3A H3A 119.2 . . ? C2A C3A H3A 119.2 . . ? C4B C3B C2B 121.6(4) . . ? C4B C3B H3B 119.2 . . ? C2B C3B H3B 119.2 . . ? C4C C3C C2C 122.4(4) . . ? C4C C3C H3C 118.8 . . ? C2C C3C H3C 118.8 . . ? C4D C3D C2D 121.4(4) . . ? C4D C3D H3D 119.3 . . ? C2D C3D H3D 119.3 . . ? C3A C4A C5A 119.2(5) . . ? C3A C4A H4A 120.4 . . ? C5A C4A H4A 120.4 . . ? C3B C4B C5B 119.3(4) . . ? C3B C4B H4B 120.4 . . ? C5B C4B H4B 120.4 . . ? C3C C4C C5C 119.6(5) . . ? C3C C4C H4C 120.2 . . ? C5C C4C H4C 120.2 . . ? C3D C4D C5D 119.3(5) . . ? C3D C4D H4D 120.4 . . ? C5D C4D H4D 120.4 . . ? C7A C5A C4A 121.3(4) . . ? C7A C5A Br6A 119.6(3) . . ? C4A C5A Br6A 119.0(4) . . ? C7B C5B C4B 120.7(4) . . ? C7B C5B Br6B 120.8(3) . . ? C4B C5B Br6B 118.5(4) . . ? C7C C5C C4C 121.0(4) . . ? C7C C5C Br6C 119.2(4) . . ? C4C C5C Br6C 119.7(4) . . ? C7D C5D C4D 121.6(4) . . ? C7D C5D Br6D 119.7(3) . . ? C4D C5D Br6D 118.6(4) . . ? C5A C7A C8A 120.5(4) . . ? C5A C7A H7A 119.7 . . ? C8A C7A H7A 119.7 . . ? C5B C7B C8B 121.4(4) . . ? C5B C7B H7B 119.3 . . ? C8B C7B H7B 119.3 . . ? C5C C7C C8C 119.7(4) . . ? C5C C7C H7C 120.1 . . ? C8C C7C H7C 120.1 . . ? C5D C7D C8D 119.8(4) . . ? C5D C7D H7D 120.1 . . ? C8D C7D H7D 120.1 . . ? C2A C8A C9A 124.7(4) . . ? C2A C8A C7A 118.4(4) . . ? C9A C8A C7A 116.4(4) . . ? C7B C8B C2B 119.2(4) . . ? C7B C8B C9B 117.5(4) . . ? C2B C8B C9B 123.3(4) . . ? C2C C8C C7C 120.0(4) . . ? C2C C8C C9C 124.1(4) . . ? C7C C8C C9C 115.8(4) . . ? C2D C8D C7D 118.6(4) . . ? C2D C8D C9D 124.4(4) . . ? C7D C8D C9D 116.9(4) . . ? N10A C9A C8A 123.9(4) . . ? N10A C9A H9A 118.1 . . ? C8A C9A H9A 118.1 . . ? N10B C9B C8B 124.2(4) . . ? N10B C9B H9B 117.9 . . ? C8B C9B H9B 117.9 . . ? N10C C9C C8C 124.2(4) . . ? N10C C9C H9C 117.9 . . ? C8C C9C H9C 117.9 . . ? N10D C9D C8D 123.8(4) . . ? N10D C9D H9D 118.1 . . ? C8D C9D H9D 118.1 . . ? O12A C11A N10A 112.6(4) . . ? O12A C11A C17A 112.9(4) . . ? N10A C11A C17A 106.6(3) . . ? O12A C11A H11A 108.2 . . ? N10A C11A H11A 108.2 . . ? C17A C11A H11A 108.2 . . ? O12B C11B N10B 111.7(3) . . ? O12B C11B C17B 112.2(4) . . ? N10B C11B C17B 109.2(4) . . ? O12B C11B H11B 107.9 . . ? N10B C11B H11B 107.9 . . ? C17B C11B H11B 107.9 . . ? O12C C11C N10C 111.6(4) . . ? O12C C11C C17C 112.9(4) . . ? N10C C11C C17C 107.0(3) . . ? O12C C11C H11C 108.4 . . ? N10C C11C H11C 108.4 . . ? C17C C11C H11C 108.4 . . ? O12D C11D N10D 111.1(3) . . ? O12D C11D C17D 113.2(4) . . ? N10D C11D C17D 107.3(4) . . ? O12D C11D H11D 108.4 . . ? N10D C11D H11D 108.4 . . ? C17D C11D H11D 108.4 . . ? O12A C13A C23A 108.2(4) . . ? O12A C13A C14A 109.8(3) . . ? C23A C13A C14A 108.4(4) . . ? O12A C13A H13A 110.1 . . ? C23A C13A H13A 110.1 . . ? C14A C13A H13A 110.1 . . ? O12B C13B C23B 109.0(4) . . ? O12B C13B C14B 109.9(4) . . ? C23B C13B C14B 109.3(4) . . ? O12B C13B H13B 109.6 . . ? C23B C13B H13B 109.6 . . ? C14B C13B H13B 109.6 . . ? O12C C13C C23C 109.1(4) . . ? O12C C13C C14C 110.1(3) . . ? C23C C13C C14C 108.0(4) . . ? O12C C13C H13C 109.9 . . ? C23C C13C H13C 109.9 . . ? C14C C13C H13C 109.9 . . ? O12D C13D C14D 110.3(4) . . ? O12D C13D C23D 108.4(4) . . ? C14D C13D C23D 108.4(4) . . ? O12D C13D H13D 109.9 . . ? C14D C13D H13D 109.9 . . ? C23D C13D H13D 109.9 . . ? O19A C14A C15A 110.9(4) . . ? O19A C14A C13A 107.2(3) . . ? C15A C14A C13A 112.1(4) . . ? O19A C14A H14A 108.9 . . ? C15A C14A H14A 108.9 . . ? C13A C14A H14A 108.9 . . ? O19B C14B C15B 110.9(4) . . ? O19B C14B C13B 108.1(4) . . ? C15B C14B C13B 111.3(4) . . ? O19B C14B H14B 108.8 . . ? C15B C14B H14B 108.8 . . ? C13B C14B H14B 108.8 . . ? O19C C14C C15C 110.7(4) . . ? O19C C14C C13C 107.4(3) . . ? C15C C14C C13C 111.2(4) . . ? O19C C14C H14C 109.2 . . ? C15C C14C H14C 109.2 . . ? C13C C14C H14C 109.2 . . ? O19D C14D C15D 110.2(4) . . ? O19D C14D C13D 108.6(4) . . ? C15D C14D C13D 110.1(4) . . ? O19D C14D H14D 109.3 . . ? C15D C14D H14D 109.3 . . ? C13D C14D H14D 109.3 . . ? O16A C15A C14A 108.2(4) . . ? O16A C15A C17A 112.3(3) . . ? C14A C15A C17A 106.0(4) . . ? O16A C15A H15A 110.1 . . ? C14A C15A H15A 110.1 . . ? C17A C15A H15A 110.1 . . ? O16B C15B C14B 107.8(4) . . ? O16B C15B C17B 112.9(4) . . ? C14B C15B C17B 106.9(3) . . ? O16B C15B H15B 109.7 . . ? C14B C15B H15B 109.7 . . ? C17B C15B H15B 109.7 . . ? O16C C15C C17C 113.9(4) . . ? O16C C15C C14C 107.6(4) . . ? C17C C15C C14C 106.3(4) . . ? O16C C15C H15C 109.6 . . ? C17C C15C H15C 109.6 . . ? C14C C15C H15C 109.6 . . ? O16D C15D C14D 107.6(4) . . ? O16D C15D C17D 112.7(4) . . ? C14D C15D C17D 105.4(4) . . ? O16D C15D H15D 110.3 . . ? C14D C15D H15D 110.3 . . ? C17D C15D H15D 110.3 . . ? O18A C17A C15A 114.7(4) . . ? O18A C17A C11A 105.8(4) . . ? C15A C17A C11A 109.0(3) . . ? O18A C17A H17A 109.1 . . ? C15A C17A H17A 109.1 . . ? C11A C17A H17A 109.1 . . ? O18B C17B C15B 114.5(4) . . ? O18B C17B C11B 104.1(4) . . ? C15B C17B C11B 108.0(4) . . ? O18B C17B H17B 110.0 . . ? C15B C17B H17B 110.0 . . ? C11B C17B H17B 110.0 . . ? O18C C17C C15C 115.5(4) . . ? O18C C17C C11C 104.4(3) . . ? C15C C17C C11C 108.6(3) . . ? O18C C17C H17C 109.4 . . ? C15C C17C H17C 109.4 . . ? C11C C17C H17C 109.4 . . ? O18D C17D C11D 104.7(4) . . ? O18D C17D C15D 115.1(4) . . ? C11D C17D C15D 109.2(4) . . ? O18D C17D H17D 109.2 . . ? C11D C17D H17D 109.2 . . ? C15D C17D H17D 109.2 . . ? O19A C20A O22A 111.4(4) . . ? O19A C20A C21A 107.9(4) . . ? O22A C20A C21A 108.4(4) . . ? O19A C20A H20A 109.7 . . ? O22A C20A H20A 109.7 . . ? C21A C20A H20A 109.7 . . ? O22B C20B O19B 111.3(4) . . ? O22B C20B C21B 108.4(4) . . ? O19B C20B C21B 108.3(4) . . ? O22B C20B H20B 109.6 . . ? O19B C20B H20B 109.6 . . ? C21B C20B H20B 109.6 . . ? O19C C20C O22C 111.3(4) . . ? O19C C20C C21C 108.6(4) . . ? O22C C20C C21C 107.6(4) . . ? O19C C20C H20C 109.8 . . ? O22C C20C H20C 109.8 . . ? C21C C20C H20C 109.8 . . ? O19D C20D O22D 110.1(4) . . ? O19D C20D C21D 107.8(4) . . ? O22D C20D C21D 109.0(4) . . ? O19D C20D H20D 110.0 . . ? O22D C20D H20D 110.0 . . ? C21D C20D H20D 110.0 . . ? C20A C21A H21A 109.5 . . ? C20A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C20A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C20B C21B H21D 109.5 . . ? C20B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C20B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C20C C21C H21G 109.5 . . ? C20C C21C H21H 109.5 . . ? H21G C21C H21H 109.5 . . ? C20C C21C H21I 109.5 . . ? H21G C21C H21I 109.5 . . ? H21H C21C H21I 109.5 . . ? C20D C21D H21J 109.5 . . ? C20D C21D H21K 109.5 . . ? H21J C21D H21K 109.5 . . ? C20D C21D H21L 109.5 . . ? H21J C21D H21L 109.5 . . ? H21K C21D H21L 109.5 . . ? O22A C23A C13A 108.9(4) . . ? O22A C23A H23A 109.9 . . ? C13A C23A H23A 109.9 . . ? O22A C23A H23B 109.9 . . ? C13A C23A H23B 109.9 . . ? H23A C23A H23B 108.3 . . ? O22B C23B C13B 106.8(4) . . ? O22B C23B H23C 110.4 . . ? C13B C23B H23C 110.4 . . ? O22B C23B H23D 110.4 . . ? C13B C23B H23D 110.4 . . ? H23C C23B H23D 108.6 . . ? O22C C23C C13C 108.7(4) . . ? O22C C23C H23E 110.0 . . ? C13C C23C H23E 110.0 . . ? O22C C23C H23F 110.0 . . ? C13C C23C H23F 110.0 . . ? H23E C23C H23F 108.3 . . ? O22D C23D C13D 107.9(4) . . ? O22D C23D H23G 110.1 . . ? C13D C23D H23G 110.1 . . ? O22D C23D H23H 110.1 . . ? C13D C23D H23H 110.1 . . ? H23G C23D H23H 108.4 . . ? C9A N10A C11A 122.3(4) . . ? C9A N10A Cu1 126.1(3) . . ? C11A N10A Cu1 111.4(3) . . ? C9B N10B C11B 123.9(4) . . ? C9B N10B Cu2 126.8(3) . . ? C11B N10B Cu2 109.3(3) . . ? C9C N10C C11C 122.5(4) . . ? C9C N10C Cu3 127.0(3) . . ? C11C N10C Cu3 110.5(3) . . ? C9D N10D C11D 124.4(4) . . ? C9D N10D Cu4 126.6(3) . . ? C11D N10D Cu4 108.9(3) . . ? C2A O1A Cu1 125.7(3) . . ? C2B O1B Cu2 126.0(3) . . ? C2C O1C Cu3 126.6(3) . . ? C2D O1D Cu4 127.0(3) . . ? C11A O12A C13A 107.8(3) . . ? C13B O12B C11B 107.8(3) . . ? C11C O12C C13C 109.6(3) . . ? C11D O12D C13D 107.4(3) . . ? C15A O16A H16A 112(5) . . ? C15B O16B H16B 106(5) . . ? C15C O16C H16C 108(5) . . ? C15D O16D H16D 110(4) . . ? C17A O18A Cu2 131.4(3) . . ? C17A O18A Cu1 106.1(3) . . ? Cu2 O18A Cu1 95.67(13) . . ? C17B O18B Cu1 138.5(3) . . ? C17B O18B Cu2 109.4(3) . . ? Cu1 O18B Cu2 97.04(14) . . ? C17C O18C Cu4 136.2(3) . . ? C17C O18C Cu3 108.3(3) . . ? Cu4 O18C Cu3 96.68(14) . . ? C17D O18D Cu3 140.4(3) . . ? C17D O18D Cu4 110.0(3) . . ? Cu3 O18D Cu4 97.59(13) . . ? C20A O19A C14A 109.1(3) . . ? C20B O19B C14B 110.6(3) . . ? C20C O19C C14C 110.4(4) . . ? C14D O19D C20D 110.4(4) . . ? C20A O22A C23A 110.6(3) . . ? C20B O22B C23B 111.1(4) . . ? C23C O22C C20C 111.8(3) . . ? C23D O22D C20D 111.3(4) . . ? O41 C40 H40A 109.5 . . ? O41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C40 O41 H41 109.5 . . ? O51 C50 H50A 109.5 . . ? O51 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O51 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C50 O51 H51 109.5 . . ? O61 C60 H60A 109.5 . . ? O61 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O61 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C60 O61 H61 109.5 . . ? O71 C70 H70A 109.5 . . ? O71 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? O71 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C70 O71 H71 109.5 . . ? 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 O1A Cu1 Cu2 O1B 179.6(3) . . . . ? O18B Cu1 Cu2 O1B -164.3(3) . . . . ? N10A Cu1 Cu2 O1B 12.1(3) . . . . ? O18A Cu1 Cu2 O1B -3.6(2) . . . . ? O1A Cu1 Cu2 N10B -4.8(2) . . . . ? O18B Cu1 Cu2 N10B 11.3(2) . . . . ? N10A Cu1 Cu2 N10B -172.3(2) . . . . ? O18A Cu1 Cu2 N10B 172.0(2) . . . . ? O1A Cu1 Cu2 O18A -176.8(2) . . . . ? O18B Cu1 Cu2 O18A -160.7(2) . . . . ? N10A Cu1 Cu2 O18A 15.7(2) . . . . ? O1A Cu1 Cu2 O18B -16.1(2) . . . . ? N10A Cu1 Cu2 O18B 176.4(2) . . . . ? O18A Cu1 Cu2 O18B 160.7(2) . . . . ? O1C Cu3 Cu4 O1D 148.2(3) . . . . ? N10C Cu3 Cu4 O1D -1.4(2) . . . . ? O18D Cu3 Cu4 O1D 175.5(3) . . . . ? O18C Cu3 Cu4 O1D -16.6(2) . . . . ? O1C Cu3 Cu4 O18C 164.8(2) . . . . ? N10C Cu3 Cu4 O18C 15.2(2) . . . . ? O18D Cu3 Cu4 O18C -168.0(2) . . . . ? O1C Cu3 Cu4 O18D -27.3(2) . . . . ? N10C Cu3 Cu4 O18D -176.8(2) . . . . ? O18C Cu3 Cu4 O18D 168.0(2) . . . . ? O1C Cu3 Cu4 N10D -17.6(2) . . . . ? N10C Cu3 Cu4 N10D -167.2(2) . . . . ? O18D Cu3 Cu4 N10D 9.7(2) . . . . ? O18C Cu3 Cu4 N10D 177.6(2) . . . . ? O1A C2A C3A C4A 176.7(5) . . . . ? C8A C2A C3A C4A -4.4(8) . . . . ? O1B C2B C3B C4B -178.1(5) . . . . ? C8B C2B C3B C4B 2.9(8) . . . . ? O1C C2C C3C C4C 175.0(5) . . . . ? C8C C2C C3C C4C -4.4(8) . . . . ? O1D C2D C3D C4D -176.0(5) . . . . ? C8D C2D C3D C4D 2.7(8) . . . . ? C2A C3A C4A C5A 0.8(8) . . . . ? C2B C3B C4B C5B -1.9(9) . . . . ? C2C C3C C4C C5C 1.5(9) . . . . ? C2D C3D C4D C5D 0.1(9) . . . . ? C3A C4A C5A C7A 3.4(8) . . . . ? C3A C4A C5A Br6A -171.9(4) . . . . ? C3B C4B C5B C7B 0.7(8) . . . . ? C3B C4B C5B Br6B 179.3(4) . . . . ? C3C C4C C5C C7C 2.1(9) . . . . ? C3C C4C C5C Br6C -174.6(4) . . . . ? C3D C4D C5D C7D -2.9(8) . . . . ? C3D C4D C5D Br6D 174.8(4) . . . . ? C4A C5A C7A C8A -3.7(8) . . . . ? Br6A C5A C7A C8A 171.6(4) . . . . ? C4B C5B C7B C8B -0.5(8) . . . . ? Br6B C5B C7B C8B -179.2(4) . . . . ? C4C C5C C7C C8C -2.5(8) . . . . ? Br6C C5C C7C C8C 174.2(4) . . . . ? C4D C5D C7D C8D 2.7(8) . . . . ? Br6D C5D C7D C8D -174.9(4) . . . . ? O1A C2A C8A C9A -5.9(8) . . . . ? C3A C2A C8A C9A 175.2(5) . . . . ? O1A C2A C8A C7A -177.2(5) . . . . ? C3A C2A C8A C7A 4.0(7) . . . . ? C5A C7A C8A C2A 0.0(7) . . . . ? C5A C7A C8A C9A -172.0(5) . . . . ? C5B C7B C8B C2B 1.6(8) . . . . ? C5B C7B C8B C9B -175.7(5) . . . . ? O1B C2B C8B C7B 178.3(5) . . . . ? C3B C2B C8B C7B -2.7(8) . . . . ? O1B C2B C8B C9B -4.6(9) . . . . ? C3B C2B C8B C9B 174.4(5) . . . . ? O1C C2C C8C C7C -175.4(5) . . . . ? C3C C2C C8C C7C 3.9(7) . . . . ? O1C C2C C8C C9C 1.1(8) . . . . ? C3C C2C C8C C9C -179.5(5) . . . . ? C5C C7C C8C C2C -0.6(7) . . . . ? C5C C7C C8C C9C -177.5(5) . . . . ? O1D C2D C8D C7D 175.8(5) . . . . ? C3D C2D C8D C7D -2.8(8) . . . . ? O1D C2D C8D C9D -6.3(8) . . . . ? C3D C2D C8D C9D 175.0(5) . . . . ? C5D C7D C8D C2D 0.2(8) . . . . ? C5D C7D C8D C9D -177.9(5) . . . . ? C2A C8A C9A N10A -4.8(8) . . . . ? C7A C8A C9A N10A 166.5(5) . . . . ? C7B C8B C9B N10B -177.9(5) . . . . ? C2B C8B C9B N10B 5.0(8) . . . . ? C2C C8C C9C N10C -5.2(8) . . . . ? C7C C8C C9C N10C 171.6(5) . . . . ? C2D C8D C9D N10D 1.3(8) . . . . ? C7D C8D C9D N10D 179.2(5) . . . . ? O12A C13A C14A O19A 177.0(4) . . . . ? C23A C13A C14A O19A 59.0(5) . . . . ? O12A C13A C14A C15A -61.1(5) . . . . ? C23A C13A C14A C15A -179.1(4) . . . . ? O12B C13B C14B O19B 177.2(4) . . . . ? C23B C13B C14B O19B 57.6(5) . . . . ? O12B C13B C14B C15B -60.8(5) . . . . ? C23B C13B C14B C15B 179.6(4) . . . . ? O12C C13C C14C O19C 178.0(4) . . . . ? C23C C13C C14C O19C 59.0(5) . . . . ? O12C C13C C14C C15C -60.8(5) . . . . ? C23C C13C C14C C15C -179.8(4) . . . . ? O12D C13D C14D O19D 175.5(4) . . . . ? C23D C13D C14D O19D 56.9(5) . . . . ? O12D C13D C14D C15D -63.8(5) . . . . ? C23D C13D C14D C15D 177.6(4) . . . . ? O19A C14A C15A O16A -63.1(5) . . . . ? C13A C14A C15A O16A 177.1(4) . . . . ? O19A C14A C15A C17A 176.2(4) . . . . ? C13A C14A C15A C17A 56.5(5) . . . . ? O19B C14B C15B O16B -61.5(5) . . . . ? C13B C14B C15B O16B 178.2(4) . . . . ? O19B C14B C15B C17B 176.8(4) . . . . ? C13B C14B C15B C17B 56.5(5) . . . . ? O19C C14C C15C O16C -60.6(5) . . . . ? C13C C14C C15C O16C -179.9(4) . . . . ? O19C C14C C15C C17C 176.9(4) . . . . ? C13C C14C C15C C17C 57.6(5) . . . . ? O19D C14D C15D O16D -61.1(5) . . . . ? C13D C14D C15D O16D 179.1(4) . . . . ? O19D C14D C15D C17D 178.3(4) . . . . ? C13D C14D C15D C17D 58.5(5) . . . . ? O16A C15A C17A O18A 69.3(5) . . . . ? C14A C15A C17A O18A -172.8(4) . . . . ? O16A C15A C17A C11A -172.3(4) . . . . ? C14A C15A C17A C11A -54.4(5) . . . . ? O12A C11A C17A O18A -174.7(3) . . . . ? N10A C11A C17A O18A -50.5(5) . . . . ? O12A C11A C17A C15A 61.4(5) . . . . ? N10A C11A C17A C15A -174.4(4) . . . . ? O16B C15B C17B O18B 70.8(6) . . . . ? C14B C15B C17B O18B -170.9(4) . . . . ? O16B C15B C17B C11B -173.8(4) . . . . ? C14B C15B C17B C11B -55.4(5) . . . . ? O12B C11B C17B O18B -175.8(4) . . . . ? N10B C11B C17B O18B -51.4(5) . . . . ? O12B C11B C17B C15B 62.1(5) . . . . ? N10B C11B C17B C15B -173.5(4) . . . . ? O16C C15C C17C O18C 69.5(6) . . . . ? C14C C15C C17C O18C -172.2(4) . . . . ? O16C C15C C17C C11C -173.6(4) . . . . ? C14C C15C C17C C11C -55.3(5) . . . . ? O12C C11C C17C O18C -176.4(4) . . . . ? N10C C11C C17C O18C -53.3(5) . . . . ? O12C C11C C17C C15C 59.8(5) . . . . ? N10C C11C C17C C15C -177.0(4) . . . . ? O12D C11D C17D O18D -175.6(4) . . . . ? N10D C11D C17D O18D -52.6(5) . . . . ? O12D C11D C17D C15D 60.6(5) . . . . ? N10D C11D C17D C15D -176.4(4) . . . . ? O16D C15D C17D O18D 69.5(6) . . . . ? C14D C15D C17D O18D -173.4(4) . . . . ? O16D C15D C17D C11D -173.0(4) . . . . ? C14D C15D C17D C11D -55.9(5) . . . . ? O12A C13A C23A O22A -174.8(3) . . . . ? C14A C13A C23A O22A -55.8(5) . . . . ? O12B C13B C23B O22B -178.0(4) . . . . ? C14B C13B C23B O22B -57.9(5) . . . . ? O12C C13C C23C O22C -176.9(4) . . . . ? C14C C13C C23C O22C -57.2(5) . . . . ? O12D C13D C23D O22D -175.7(4) . . . . ? C14D C13D C23D O22D -56.0(6) . . . . ? C8A C9A N10A C11A -170.7(4) . . . . ? C8A C9A N10A Cu1 2.8(7) . . . . ? O12A C11A N10A C9A -36.4(6) . . . . ? C17A C11A N10A C9A -160.8(4) . . . . ? O12A C11A N10A Cu1 149.3(3) . . . . ? C17A C11A N10A Cu1 24.9(4) . . . . ? O1A Cu1 N10A C9A 5.6(4) . . . . ? O18B Cu1 N10A C9A -171.7(6) . . . . ? O18A Cu1 N10A C9A -172.1(4) . . . . ? Cu2 Cu1 N10A C9A 177.4(3) . . . . ? O1A Cu1 N10A C11A 179.6(3) . . . . ? O18B Cu1 N10A C11A 2.3(9) . . . . ? O18A Cu1 N10A C11A 2.0(3) . . . . ? Cu2 Cu1 N10A C11A -8.5(4) . . . . ? C8B C9B N10B C11B -171.4(5) . . . . ? C8B C9B N10B Cu2 9.4(8) . . . . ? O12B C11B N10B C9B -21.3(7) . . . . ? C17B C11B N10B C9B -146.0(5) . . . . ? O12B C11B N10B Cu2 157.9(3) . . . . ? C17B C11B N10B Cu2 33.3(5) . . . . ? O1B Cu2 N10B C9B -17.5(5) . . . . ? O18A Cu2 N10B C9B -171.7(6) . . . . ? O18B Cu2 N10B C9B 172.6(5) . . . . ? Cu1 Cu2 N10B C9B 165.2(4) . . . . ? O1B Cu2 N10B C11B 163.2(3) . . . . ? O18A Cu2 N10B C11B 9.0(9) . . . . ? O18B Cu2 N10B C11B -6.7(3) . . . . ? Cu1 Cu2 N10B C11B -14.1(4) . . . . ? C8C C9C N10C C11C -176.8(4) . . . . ? C8C C9C N10C Cu3 0.6(7) . . . . ? O12C C11C N10C C9C -24.0(6) . . . . ? C17C C11C N10C C9C -147.9(4) . . . . ? O12C C11C N10C Cu3 158.2(3) . . . . ? C17C C11C N10C Cu3 34.2(4) . . . . ? O1C Cu3 N10C C9C 4.9(4) . . . . ? O18D Cu3 N10C C9C 156.7(6) . . . . ? O18C Cu3 N10C C9C 174.9(4) . . . . ? Cu4 Cu3 N10C C9C 165.0(4) . . . . ? O1C Cu3 N10C C11C -177.4(3) . . . . ? O18D Cu3 N10C C11C -25.6(8) . . . . ? O18C Cu3 N10C C11C -7.4(3) . . . . ? Cu4 Cu3 N10C C11C -17.3(4) . . . . ? C8D C9D N10D C11D -175.8(5) . . . . ? C8D C9D N10D Cu4 8.3(7) . . . . ? O12D C11D N10D C9D -16.4(7) . . . . ? C17D C11D N10D C9D -140.6(5) . . . . ? O12D C11D N10D Cu4 160.2(3) . . . . ? C17D C11D N10D Cu4 35.9(4) . . . . ? O1D Cu4 N10D C9D -10.3(4) . . . . ? O18C Cu4 N10D C9D 168.3(7) . . . . ? O18D Cu4 N10D C9D 166.8(4) . . . . ? Cu3 Cu4 N10D C9D 160.5(4) . . . . ? O1D Cu4 N10D C11D 173.3(3) . . . . ? O18C Cu4 N10D C11D -8.1(10) . . . . ? O18D Cu4 N10D C11D -9.6(3) . . . . ? Cu3 Cu4 N10D C11D -15.9(4) . . . . ? C3A C2A O1A Cu1 -163.5(4) . . . . ? C8A C2A O1A Cu1 17.7(7) . . . . ? O18B Cu1 O1A C2A 163.8(4) . . . . ? N10A Cu1 O1A C2A -15.6(4) . . . . ? O18A Cu1 O1A C2A 51(3) . . . . ? Cu2 Cu1 O1A C2A 174.7(3) . . . . ? C3B C2B O1B Cu2 170.8(4) . . . . ? C8B C2B O1B Cu2 -10.2(8) . . . . ? N10B Cu2 O1B C2B 17.6(5) . . . . ? O18A Cu2 O1B C2B -168.4(4) . . . . ? O18B Cu2 O1B C2B 93.9(8) . . . . ? Cu1 Cu2 O1B C2B -165.9(3) . . . . ? C8C C2C O1C Cu3 6.9(7) . . . . ? C3C C2C O1C Cu3 -172.4(4) . . . . ? N10C Cu3 O1C C2C -8.6(4) . . . . ? O18D Cu3 O1C C2C 178.3(4) . . . . ? O18C Cu3 O1C C2C -87.5(8) . . . . ? Cu4 Cu3 O1C C2C -163.8(3) . . . . ? C3D C2D O1D Cu4 179.6(4) . . . . ? C8D C2D O1D Cu4 1.0(7) . . . . ? O18C Cu4 O1D C2D -174.1(4) . . . . ? O18D Cu4 O1D C2D -64(3) . . . . ? N10D Cu4 O1D C2D 5.6(4) . . . . ? Cu3 Cu4 O1D C2D -162.9(3) . . . . ? N10A C11A O12A C13A 175.8(3) . . . . ? C17A C11A O12A C13A -63.3(4) . . . . ? C23A C13A O12A C11A 179.5(4) . . . . ? C14A C13A O12A C11A 61.4(5) . . . . ? C23B C13B O12B C11B -178.1(4) . . . . ? C14B C13B O12B C11B 62.2(5) . . . . ? N10B C11B O12B C13B 172.3(4) . . . . ? C17B C11B O12B C13B -64.7(5) . . . . ? N10C C11C O12C C13C 178.1(3) . . . . ? C17C C11C O12C C13C -61.4(5) . . . . ? C23C C13C O12C C11C 178.8(4) . . . . ? C14C C13C O12C C11C 60.5(5) . . . . ? N10D C11D O12D C13D 177.3(4) . . . . ? C17D C11D O12D C13D -61.9(5) . . . . ? C14D C13D O12D C11D 62.2(5) . . . . ? C23D C13D O12D C11D -179.3(4) . . . . ? C15A C17A O18A Cu2 -75.4(5) . . . . ? C11A C17A O18A Cu2 164.5(3) . . . . ? C15A C17A O18A Cu1 171.6(3) . . . . ? C11A C17A O18A Cu1 51.5(4) . . . . ? O1B Cu2 O18A C17A 60.5(4) . . . . ? N10B Cu2 O18A C17A -145.7(7) . . . . ? O18B Cu2 O18A C17A -129.9(4) . . . . ? Cu1 Cu2 O18A C17A -117.3(4) . . . . ? O1B Cu2 O18A Cu1 177.75(15) . . . . ? N10B Cu2 O18A Cu1 -28.4(8) . . . . ? O18B Cu2 O18A Cu1 -12.63(16) . . . . ? O1A Cu1 O18A C17A -98(3) . . . . ? O18B Cu1 O18A C17A 148.9(3) . . . . ? N10A Cu1 O18A C17A -31.1(3) . . . . ? Cu2 Cu1 O18A C17A 136.0(3) . . . . ? O1A Cu1 O18A Cu2 126(3) . . . . ? O18B Cu1 O18A Cu2 12.89(16) . . . . ? N10A Cu1 O18A Cu2 -167.20(17) . . . . ? C15B C17B O18B Cu1 -71.1(6) . . . . ? C11B C17B O18B Cu1 171.3(3) . . . . ? C15B C17B O18B Cu2 162.6(3) . . . . ? C11B C17B O18B Cu2 44.9(4) . . . . ? O1A Cu1 O18B C17B 39.4(5) . . . . ? N10A Cu1 O18B C17B -143.3(7) . . . . ? O18A Cu1 O18B C17B -142.9(5) . . . . ? Cu2 Cu1 O18B C17B -130.1(5) . . . . ? O1A Cu1 O18B Cu2 169.51(16) . . . . ? N10A Cu1 O18B Cu2 -13.3(8) . . . . ? O18A Cu1 O18B Cu2 -12.87(16) . . . . ? O1B Cu2 O18B C17B -100.2(7) . . . . ? N10B Cu2 O18B C17B -23.3(3) . . . . ? O18A Cu2 O18B C17B 160.5(3) . . . . ? Cu1 Cu2 O18B C17B 147.5(4) . . . . ? O1B Cu2 O18B Cu1 112.3(7) . . . . ? N10B Cu2 O18B Cu1 -170.73(18) . . . . ? O18A Cu2 O18B Cu1 13.00(16) . . . . ? C15C C17C O18C Cu4 -72.7(6) . . . . ? C11C C17C O18C Cu4 168.1(3) . . . . ? C15C C17C O18C Cu3 165.9(3) . . . . ? C11C C17C O18C Cu3 46.7(4) . . . . ? O1D Cu4 O18C C17C 43.9(5) . . . . ? O18D Cu4 O18C C17C -133.3(4) . . . . ? N10D Cu4 O18C C17C -134.8(8) . . . . ? Cu3 Cu4 O18C C17C -125.3(5) . . . . ? O1D Cu4 O18C Cu3 169.20(15) . . . . ? O18D Cu4 O18C Cu3 -7.95(16) . . . . ? N10D Cu4 O18C Cu3 -9.5(9) . . . . ? O1C Cu3 O18C C17C 55.7(8) . . . . ? N10C Cu3 O18C C17C -24.0(3) . . . . ? O18D Cu3 O18C C17C 151.5(3) . . . . ? Cu4 Cu3 O18C C17C 143.5(4) . . . . ? O1C Cu3 O18C Cu4 -87.8(7) . . . . ? N10C Cu3 O18C Cu4 -167.44(17) . . . . ? O18D Cu3 O18C Cu4 7.99(16) . . . . ? C11D C17D O18D Cu3 175.8(4) . . . . ? C15D C17D O18D Cu3 -64.2(6) . . . . ? C11D C17D O18D Cu4 44.7(4) . . . . ? C15D C17D O18D Cu4 164.6(3) . . . . ? O1C Cu3 O18D C17D 27.4(5) . . . . ? N10C Cu3 O18D C17D -124.1(7) . . . . ? O18C Cu3 O18D C17D -142.4(5) . . . . ? Cu4 Cu3 O18D C17D -134.4(6) . . . . ? O1C Cu3 O18D Cu4 161.81(16) . . . . ? N10C Cu3 O18D Cu4 10.4(7) . . . . ? O18C Cu3 O18D Cu4 -7.93(16) . . . . ? O1D Cu4 O18D C17D 49(3) . . . . ? O18C Cu4 O18D C17D 159.2(3) . . . . ? N10D Cu4 O18D C17D -21.1(3) . . . . ? Cu3 Cu4 O18D C17D 151.0(4) . . . . ? O1D Cu4 O18D Cu3 -102(3) . . . . ? O18C Cu4 O18D Cu3 8.16(16) . . . . ? N10D Cu4 O18D Cu3 -172.15(18) . . . . ? O22A C20A O19A C14A 65.7(5) . . . . ? C21A C20A O19A C14A -175.5(4) . . . . ? C15A C14A O19A C20A 174.1(4) . . . . ? C13A C14A O19A C20A -63.2(5) . . . . ? O22B C20B O19B C14B 61.7(5) . . . . ? C21B C20B O19B C14B -179.2(4) . . . . ? C15B C14B O19B C20B 179.6(4) . . . . ? C13B C14B O19B C20B -58.2(5) . . . . ? O22C C20C O19C C14C 62.2(5) . . . . ? C21C C20C O19C C14C -179.5(4) . . . . ? C15C C14C O19C C20C 177.0(4) . . . . ? C13C C14C O19C C20C -61.4(5) . . . . ? C15D C14D O19D C20D 178.8(4) . . . . ? C13D C14D O19D C20D -60.5(5) . . . . ? O22D C20D O19D C14D 63.4(5) . . . . ? C21D C20D O19D C14D -177.8(4) . . . . ? O19A C20A O22A C23A -62.0(5) . . . . ? C21A C20A O22A C23A 179.5(4) . . . . ? C13A C23A O22A C20A 56.7(5) . . . . ? O19B C20B O22B C23B -63.2(5) . . . . ? C21B C20B O22B C23B 177.8(4) . . . . ? C13B C23B O22B C20B 60.6(5) . . . . ? C13C C23C O22C C20C 57.9(5) . . . . ? O19C C20C O22C C23C -60.5(5) . . . . ? C21C C20C O22C C23C -179.3(4) . . . . ? C13D C23D O22D C20D 59.6(5) . . . . ? O19D C20D O22D C23D -63.4(5) . . . . ? C21D C20D O22D C23D 178.5(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O16A H16A O1B 0.839(10) 1.903(19) 2.728(5) 167(7) . O16B H16B O1A 0.839(10) 1.89(3) 2.690(4) 160(6) . O16C H16C O1D 0.836(10) 1.87(3) 2.661(4) 156(6) . O16D H16D O1C 0.834(10) 1.88(2) 2.691(4) 163(6) . O16D H16D O18D 0.834(10) 2.69(6) 3.061(5) 108(5) . O41 H41 O51 0.84 2.21 2.772(7) 124.6 . O51 H51 O41 0.84 1.96 2.772(7) 163.9 . O61 H61 O71 0.84 1.96 2.782(5) 164.8 . O71 H71 O16B 0.84 1.86 2.692(6) 171.7 1_545 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.754 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.070 data_5 _database_code_CSD 193691 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H54 Cu2 N6 O12' _chemical_formula_weight 1058.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.304(1) _cell_length_b 13.548(1) _cell_length_c 26.292(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4738.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 27000 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type 'Empirical from multiple refl.' _exptl_absorpt_correction_T_min 0.8044 _exptl_absorpt_correction_T_max 0.9153 _exptl_absorpt_process_details 'MULABS (Platon2000; cf. Blessing 1995)' _exptl_special_details ; dx = 35 mm; 120 sec./deg., 1 deg.; mos. = 0.526(2) deg. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23119 _diffrn_reflns_av_R_equivalents 0.0793 _diffrn_reflns_av_sigmaI/netI 0.0915 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8318 _reflns_number_gt 6730 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (A.L.Spek, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+5.4545P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.002(13) _refine_ls_number_reflns 8318 _refine_ls_number_parameters 619 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1049 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.26014(4) 0.29874(4) 0.63273(2) 0.01976(14) Uani 1 1 d . . . Cu2 Cu 0.44623(4) 0.42063(4) 0.62983(2) 0.01895(14) Uani 1 1 d . . . C2A C 0.0559(4) 0.2537(4) 0.66495(17) 0.0216(11) Uani 1 1 d . . . C2B C 0.6466(4) 0.4807(4) 0.66277(17) 0.0196(11) Uani 1 1 d . . . C3A C -0.0477(4) 0.2793(4) 0.66682(19) 0.0301(13) Uani 1 1 d . . . H3A H -0.0687 0.3418 0.6543 0.036 Uiso 1 1 calc R . . C3B C 0.7465(4) 0.4569(4) 0.67407(19) 0.0280(12) Uani 1 1 d . . . H3B H 0.7670 0.3898 0.6725 0.034 Uiso 1 1 calc R . . C4A C -0.1189(4) 0.2147(4) 0.6867(2) 0.0330(14) Uani 1 1 d . . . H4A H -0.1878 0.2334 0.6869 0.040 Uiso 1 1 calc R . . C4B C 0.8159(4) 0.5274(4) 0.6874(2) 0.0296(13) Uani 1 1 d . . . H4B H 0.8836 0.5087 0.6937 0.036 Uiso 1 1 calc R . . C5A C -0.0910(4) 0.1232(4) 0.7061(2) 0.0332(14) Uani 1 1 d . . . H5A H -0.1398 0.0797 0.7200 0.040 Uiso 1 1 calc R . . C5B C 0.7882(4) 0.6257(4) 0.69167(19) 0.0260(13) Uani 1 1 d . . . H5B H 0.8357 0.6742 0.7019 0.031 Uiso 1 1 calc R . . C6A C 0.0077(4) 0.0977(4) 0.70468(19) 0.0271(13) Uani 1 1 d . . . H6A H 0.0269 0.0357 0.7185 0.033 Uiso 1 1 calc R . . C6B C 0.6899(4) 0.6518(4) 0.68075(19) 0.0244(12) Uani 1 1 d . . . H6B H 0.6707 0.7192 0.6830 0.029 Uiso 1 1 calc R . . C7A C 0.0827(3) 0.1583(4) 0.68381(18) 0.0193(11) Uani 1 1 d . . . C7B C 0.6187(4) 0.5819(4) 0.66665(17) 0.0206(11) Uani 1 1 d . . . C8A C 0.1834(4) 0.1201(4) 0.68058(18) 0.0209(11) Uani 1 1 d . . . H8A H 0.1960 0.0574 0.6954 0.025 Uiso 1 1 calc R . . C8B C 0.5191(4) 0.6176(4) 0.65518(17) 0.0192(11) Uani 1 1 d . . . H8B H 0.5063 0.6858 0.6607 0.023 Uiso 1 1 calc R . . C10A C 0.3568(3) 0.1218(3) 0.65680(18) 0.0167(11) Uani 1 1 d . . . H10A H 0.3696 0.1003 0.6210 0.020 Uiso 1 1 calc R . . C10B C 0.3484(3) 0.6053(3) 0.62655(18) 0.0170(10) Uani 1 1 d . . . H10B H 0.3414 0.6094 0.5887 0.020 Uiso 1 1 calc R . . C12A C 0.4615(4) -0.0048(4) 0.68355(17) 0.0196(11) Uani 1 1 d . . . H12A H 0.4731 -0.0213 0.6469 0.023 Uiso 1 1 calc R . . C12B C 0.2381(3) 0.7367(3) 0.6312(2) 0.0198(10) Uani 1 1 d . . . H12B H 0.2347 0.7362 0.5932 0.024 Uiso 1 1 calc R . . C13A C 0.5397(4) 0.0690(4) 0.70077(17) 0.0190(11) Uani 1 1 d . . . H13A H 0.5248 0.0881 0.7367 0.023 Uiso 1 1 calc R . . C13B C 0.1557(4) 0.6721(3) 0.65207(18) 0.0203(11) Uani 1 1 d . . . H13B H 0.1586 0.6738 0.6901 0.024 Uiso 1 1 calc R . . C14A C 0.5389(4) 0.1621(4) 0.66813(17) 0.0209(11) Uani 1 1 d . . . H14A H 0.5562 0.1445 0.6322 0.025 Uiso 1 1 calc R . . C14B C 0.1643(3) 0.5651(3) 0.6345(2) 0.0210(11) Uani 1 1 d . . . H14B H 0.1526 0.5613 0.5970 0.025 Uiso 1 1 calc R . . C16A C 0.4321(3) 0.2024(3) 0.67013(17) 0.0174(10) Uani 1 1 d . . . H16A H 0.4180 0.2262 0.7054 0.021 Uiso 1 1 calc R . . C16B C 0.2710(3) 0.5309(3) 0.64665(17) 0.0202(11) Uani 1 1 d . . . H16B H 0.2783 0.5263 0.6844 0.024 Uiso 1 1 calc R . . C19A C 0.6360(4) -0.0637(3) 0.73105(17) 0.0186(11) Uani 1 1 d . . . H19A H 0.6162 -0.0440 0.7663 0.022 Uiso 1 1 calc R . . C19B C 0.0489(4) 0.8101(4) 0.6541(2) 0.0290(12) Uani 1 1 d . . . H19B H 0.0493 0.8112 0.6921 0.035 Uiso 1 1 calc R . . C20A C 0.7395(4) -0.1077(4) 0.73205(18) 0.0234(12) Uani 1 1 d . . . H20A H 0.7875 -0.0585 0.7447 0.035 Uiso 1 1 calc R . . H20B H 0.7587 -0.1279 0.6976 0.035 Uiso 1 1 calc R . . H20C H 0.7400 -0.1654 0.7545 0.035 Uiso 1 1 calc R . . C20B C -0.0507(4) 0.8466(4) 0.6340(3) 0.0395(14) Uani 1 1 d . . . H20D H -0.1048 0.8042 0.6468 0.059 Uiso 1 1 calc R . . H20E H -0.0500 0.8447 0.5968 0.059 Uiso 1 1 calc R . . H20F H -0.0619 0.9145 0.6455 0.059 Uiso 1 1 calc R . . C22A C 0.4660(3) -0.0986(4) 0.71484(18) 0.0214(11) Uani 1 1 d . . . H22A H 0.4468 -0.0846 0.7505 0.026 Uiso 1 1 calc R . . H22B H 0.4189 -0.1483 0.7009 0.026 Uiso 1 1 calc R . . C22B C 0.2237(4) 0.8419(4) 0.6501(2) 0.0302(13) Uani 1 1 d . . . H22C H 0.2299 0.8443 0.6876 0.036 Uiso 1 1 calc R . . H22D H 0.2753 0.8858 0.6352 0.036 Uiso 1 1 calc R . . C31 C 0.2439(4) 0.1891(4) 0.52482(19) 0.0298(12) Uani 1 1 d . . . H31 H 0.2557 0.1334 0.5459 0.036 Uiso 1 1 calc R . . C32 C 0.2325(4) 0.1734(5) 0.4729(2) 0.0363(15) Uani 1 1 d . . . H32 H 0.2374 0.1088 0.4590 0.044 Uiso 1 1 calc R . . C33 C 0.2140(5) 0.2533(5) 0.4422(2) 0.0401(16) Uani 1 1 d . . . H33 H 0.2056 0.2454 0.4066 0.048 Uiso 1 1 calc R . . C34 C 0.2080(4) 0.3453(5) 0.4644(2) 0.0385(15) Uani 1 1 d . . . H34 H 0.1950 0.4019 0.4442 0.046 Uiso 1 1 calc R . . C35 C 0.2210(4) 0.3544(4) 0.5160(2) 0.0297(13) Uani 1 1 d . . . H35 H 0.2168 0.4183 0.5306 0.036 Uiso 1 1 calc R . . C41 C 0.4694(4) 0.3322(4) 0.5182(2) 0.0334(14) Uani 1 1 d . . . H41 H 0.4461 0.2741 0.5347 0.040 Uiso 1 1 calc R . . C42 C 0.4861(5) 0.3302(6) 0.4661(2) 0.052(2) Uani 1 1 d . . . H42 H 0.4742 0.2718 0.4471 0.062 Uiso 1 1 calc R . . C43 C 0.5206(5) 0.4152(6) 0.4422(2) 0.0534(19) Uani 1 1 d . . . H43 H 0.5306 0.4160 0.4064 0.064 Uiso 1 1 calc R . . C44 C 0.5399(5) 0.4969(5) 0.4704(2) 0.0487(18) Uani 1 1 d . . . H44 H 0.5666 0.5548 0.4552 0.058 Uiso 1 1 calc R . . C45 C 0.5193(4) 0.4933(4) 0.5227(2) 0.0321(14) Uani 1 1 d . . . H45 H 0.5305 0.5512 0.5423 0.039 Uiso 1 1 calc R . . C51 C 0.3267(5) -0.0875(5) 0.5122(3) 0.0530(18) Uani 1 1 d . . . H51 H 0.2749 -0.1242 0.5284 0.064 Uiso 1 1 calc R . . C52 C 0.3435(7) -0.1046(5) 0.4612(2) 0.0684(17) Uani 1 1 d . . . H52 H 0.3037 -0.1506 0.4428 0.082 Uiso 1 1 calc R . . C53 C 0.4189(6) -0.0537(5) 0.4380(2) 0.0621(16) Uani 1 1 d . . . H53 H 0.4340 -0.0650 0.4031 0.074 Uiso 1 1 calc R . . C54 C 0.4723(5) 0.0139(5) 0.4654(3) 0.0580(13) Uani 1 1 d . . . H54 H 0.5243 0.0515 0.4499 0.070 Uiso 1 1 calc R . . C55 C 0.4490(5) 0.0260(5) 0.5160(2) 0.0436(16) Uani 1 1 d . . . H55 H 0.4866 0.0732 0.5348 0.052 Uiso 1 1 calc R . . C61 C 0.2390(7) 0.6180(6) 0.4640(3) 0.070(2) Uani 1 1 d . . . H61 H 0.3020 0.5850 0.4651 0.084 Uiso 1 1 calc R . . C62 C 0.1821(7) 0.6167(6) 0.4185(3) 0.0684(17) Uani 1 1 d . . . H62 H 0.2054 0.5818 0.3895 0.082 Uiso 1 1 calc R . . C63 C 0.0981(6) 0.6639(5) 0.4172(3) 0.0621(16) Uani 1 1 d . . . H63 H 0.0611 0.6651 0.3863 0.074 Uiso 1 1 calc R . . C64 C 0.0594(6) 0.7133(5) 0.4594(3) 0.0580(13) Uani 1 1 d . . . H64 H -0.0033 0.7468 0.4583 0.070 Uiso 1 1 calc R . . C65 C 0.1177(6) 0.7104(5) 0.5026(2) 0.057(2) Uani 1 1 d . . . H65 H 0.0934 0.7432 0.5321 0.068 Uiso 1 1 calc R . . N9A N 0.2573(3) 0.1641(3) 0.65933(13) 0.0188(9) Uani 1 1 d . . . N9B N 0.4468(3) 0.5653(3) 0.63824(14) 0.0201(9) Uani 1 1 d . . . N30 N 0.2392(3) 0.2774(3) 0.54669(15) 0.0271(10) Uani 1 1 d . . . N40 N 0.4851(3) 0.4142(3) 0.54608(15) 0.0263(10) Uani 1 1 d . . . N50 N 0.3778(4) -0.0235(4) 0.54035(18) 0.0430(13) Uani 1 1 d . . . N60 N 0.2061(5) 0.6646(4) 0.50558(19) 0.0540(16) Uani 1 1 d . . . O1A O 0.1188(2) 0.3166(2) 0.64465(13) 0.0266(9) Uani 1 1 d . . . O1B O 0.5834(2) 0.4094(3) 0.65081(12) 0.0248(8) Uani 1 1 d . . . O11A O 0.3639(2) 0.0370(2) 0.68912(11) 0.0190(7) Uani 1 1 d . . . O11B O 0.3353(2) 0.7008(2) 0.64702(12) 0.0239(8) Uani 1 1 d . . . O15A O 0.6115(3) 0.2275(3) 0.68740(14) 0.0276(9) Uani 1 1 d D . . H15A H 0.603(4) 0.2845(18) 0.676(2) 0.041 Uiso 1 1 d D . . O15B O 0.0902(3) 0.5099(3) 0.66018(15) 0.0303(9) Uani 1 1 d D . . H15B H 0.107(4) 0.4508(14) 0.660(2) 0.045 Uiso 1 1 d D . . O17A O 0.4100(2) 0.2800(2) 0.63518(13) 0.0204(7) Uani 1 1 d . . . O17B O 0.2989(2) 0.4387(2) 0.62502(13) 0.0205(8) Uani 1 1 d . . . O18A O 0.6373(2) 0.0214(2) 0.69924(12) 0.0213(8) Uani 1 1 d . . . O18B O 0.0615(2) 0.7122(2) 0.63588(12) 0.0239(7) Uani 1 1 d . . . O21A O 0.5682(2) -0.1356(2) 0.71275(12) 0.0213(8) Uani 1 1 d . . . O21B O 0.1246(2) 0.8729(2) 0.63461(15) 0.0297(8) 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 0.0198(3) 0.0150(3) 0.0245(3) 0.0017(3) 0.0005(3) 0.0002(2) Cu2 0.0212(3) 0.0131(3) 0.0225(3) 0.0004(3) 0.0006(3) 0.0005(3) C2A 0.026(3) 0.021(3) 0.018(2) -0.006(2) -0.001(2) 0.005(2) C2B 0.024(3) 0.017(3) 0.017(2) 0.000(2) 0.003(2) -0.003(2) C3A 0.031(3) 0.017(3) 0.042(3) 0.002(2) 0.004(3) 0.003(3) C3B 0.025(3) 0.016(3) 0.042(3) 0.001(2) 0.005(3) 0.007(2) C4A 0.024(3) 0.028(3) 0.047(3) 0.007(3) 0.005(3) 0.002(3) C4B 0.019(3) 0.035(4) 0.035(3) -0.005(3) -0.004(2) 0.001(3) C5A 0.022(3) 0.035(4) 0.043(3) 0.009(3) 0.005(3) -0.003(3) C5B 0.026(3) 0.026(3) 0.026(3) -0.004(2) -0.006(2) -0.006(2) C6A 0.033(3) 0.022(3) 0.027(3) 0.006(2) 0.001(2) 0.005(3) C6B 0.030(3) 0.015(3) 0.028(3) -0.001(2) -0.006(2) 0.004(2) C7A 0.021(3) 0.020(3) 0.017(2) -0.003(2) 0.002(2) -0.002(2) C7B 0.023(3) 0.017(3) 0.022(3) 0.001(2) 0.002(2) 0.001(2) C8A 0.022(3) 0.019(3) 0.022(3) -0.002(2) -0.003(2) 0.002(2) C8B 0.026(3) 0.011(3) 0.020(3) 0.000(2) 0.003(2) -0.001(2) C10A 0.021(3) 0.012(3) 0.017(2) 0.003(2) -0.002(2) 0.002(2) C10B 0.023(2) 0.012(3) 0.016(2) 0.000(2) -0.005(2) 0.0017(19) C12A 0.023(3) 0.019(3) 0.017(2) 0.000(2) 0.005(2) 0.005(2) C12B 0.022(2) 0.017(2) 0.020(2) 0.000(2) -0.003(3) 0.006(2) C13A 0.022(3) 0.018(3) 0.017(2) -0.003(2) 0.002(2) 0.001(2) C13B 0.025(3) 0.015(3) 0.020(2) -0.003(2) 0.001(2) 0.005(2) C14A 0.021(3) 0.024(3) 0.017(2) 0.001(2) 0.000(2) 0.000(2) C14B 0.026(3) 0.015(3) 0.022(2) 0.002(2) 0.003(3) 0.002(2) C16A 0.021(3) 0.012(2) 0.019(2) 0.000(2) -0.005(2) 0.003(2) C16B 0.023(3) 0.014(3) 0.023(3) 0.000(2) 0.001(2) 0.002(2) C19A 0.022(3) 0.011(3) 0.022(2) -0.001(2) 0.002(2) 0.000(2) C19B 0.028(3) 0.023(3) 0.037(3) 0.001(2) 0.002(3) 0.007(3) C20A 0.025(3) 0.017(3) 0.028(3) -0.002(2) -0.002(2) 0.006(2) C20B 0.026(3) 0.028(3) 0.065(4) 0.015(3) 0.011(4) 0.007(3) C22A 0.018(3) 0.016(3) 0.030(3) 0.001(2) 0.000(2) 0.004(2) C22B 0.031(3) 0.023(3) 0.037(3) -0.003(2) -0.006(3) 0.005(2) C31 0.027(3) 0.027(3) 0.035(3) -0.001(2) 0.001(3) -0.001(3) C32 0.029(3) 0.043(4) 0.036(3) -0.017(3) -0.001(3) 0.002(3) C33 0.049(4) 0.049(4) 0.023(3) -0.001(3) -0.007(3) 0.008(3) C34 0.047(4) 0.037(4) 0.032(3) 0.005(3) -0.006(3) 0.000(3) C35 0.035(3) 0.019(3) 0.034(3) -0.002(2) -0.004(3) 0.007(2) C41 0.024(3) 0.037(4) 0.040(3) -0.008(3) 0.001(3) 0.001(3) C42 0.045(4) 0.074(6) 0.035(4) -0.021(4) -0.004(3) 0.011(4) C43 0.055(5) 0.081(6) 0.025(3) 0.005(4) 0.005(3) 0.015(4) C44 0.063(5) 0.050(4) 0.032(3) 0.019(3) 0.011(3) 0.011(4) C45 0.041(3) 0.026(3) 0.029(3) -0.001(3) 0.007(3) 0.005(3) C51 0.053(4) 0.042(4) 0.064(5) 0.006(4) 0.010(4) -0.003(4) C52 0.121(5) 0.046(3) 0.038(3) -0.002(2) 0.007(3) -0.026(3) C53 0.099(5) 0.054(3) 0.034(3) 0.006(2) -0.018(3) -0.012(3) C54 0.063(3) 0.049(3) 0.063(3) 0.014(3) -0.005(3) 0.002(3) C55 0.040(4) 0.041(4) 0.050(4) -0.016(3) -0.007(3) 0.007(3) C61 0.099(7) 0.059(5) 0.052(4) 0.004(4) 0.021(5) -0.030(5) C62 0.121(5) 0.046(3) 0.038(3) -0.002(2) 0.007(3) -0.026(3) C63 0.099(5) 0.054(3) 0.034(3) 0.006(2) -0.018(3) -0.012(3) C64 0.063(3) 0.049(3) 0.063(3) 0.014(3) -0.005(3) 0.002(3) C65 0.081(6) 0.057(5) 0.032(3) 0.001(4) -0.010(4) -0.013(4) N9A 0.019(2) 0.019(2) 0.018(2) -0.0030(17) -0.0034(19) 0.0006(19) N9B 0.023(2) 0.015(2) 0.022(2) -0.0005(18) 0.000(2) -0.0006(19) N30 0.028(2) 0.026(3) 0.028(2) -0.002(2) -0.004(2) 0.001(2) N40 0.027(2) 0.030(3) 0.022(2) 0.000(2) 0.0035(18) -0.001(2) N50 0.052(3) 0.038(3) 0.039(3) -0.004(3) 0.006(3) 0.003(3) N60 0.071(4) 0.060(4) 0.032(3) -0.009(3) 0.003(3) -0.019(3) O1A 0.0231(19) 0.0137(19) 0.043(2) 0.0072(16) 0.0035(17) -0.0022(15) O1B 0.0227(19) 0.0158(18) 0.036(2) -0.0014(16) 0.0012(15) -0.0011(15) O11A 0.0188(18) 0.0139(18) 0.0241(17) 0.0037(15) 0.0024(15) 0.0016(15) O11B 0.0266(19) 0.0161(19) 0.0289(19) -0.0023(16) -0.0081(15) 0.0054(16) O15A 0.0243(19) 0.017(2) 0.041(2) 0.0021(17) -0.0058(18) -0.0044(17) O15B 0.025(2) 0.015(2) 0.051(2) 0.0004(19) 0.0068(17) 0.0015(16) O17A 0.0232(17) 0.0146(17) 0.0235(17) 0.0035(16) -0.0020(16) -0.0019(14) O17B 0.0228(17) 0.0083(17) 0.0304(19) -0.0004(16) -0.0005(16) 0.0004(13) O18A 0.0204(18) 0.0158(19) 0.0275(18) 0.0035(15) -0.0001(15) 0.0026(15) O18B 0.0235(17) 0.0165(17) 0.0317(18) 0.0021(17) 0.0015(18) 0.0036(15) O21A 0.021(2) 0.0175(19) 0.0250(18) -0.0018(15) -0.0004(16) -0.0006(15) O21B 0.0258(19) 0.0180(18) 0.045(2) 0.0025(19) -0.002(2) 0.0034(15) _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 O1A 1.921(3) . ? Cu1 N9A 1.955(4) . ? Cu1 O17B 1.976(3) . ? Cu1 O17A 2.011(3) . ? Cu1 N30 2.297(4) . ? Cu1 Cu2 2.9770(8) . ? Cu2 O1B 1.913(3) . ? Cu2 O17A 1.970(3) . ? Cu2 N9B 1.972(4) . ? Cu2 O17B 1.979(3) . ? Cu2 N40 2.264(4) . ? C2A O1A 1.308(6) . ? C2A C3A 1.422(8) . ? C2A C7A 1.430(7) . ? C2B O1B 1.320(6) . ? C2B C3B 1.400(7) . ? C2B C7B 1.424(7) . ? C3A C4A 1.392(7) . ? C3A H3A 0.9500 . ? C3B C4B 1.374(7) . ? C3B H3B 0.9500 . ? C4A C5A 1.391(8) . ? C4A H4A 0.9500 . ? C4B C5B 1.386(7) . ? C4B H4B 0.9500 . ? C5A C6A 1.359(7) . ? C5A H5A 0.9500 . ? C5B C6B 1.385(7) . ? C5B H5B 0.9500 . ? C6A C7A 1.403(7) . ? C6A H6A 0.9500 . ? C6B C7B 1.390(7) . ? C6B H6B 0.9500 . ? C7A C8A 1.439(7) . ? C7B C8B 1.442(7) . ? C8A N9A 1.278(6) . ? C8A H8A 0.9500 . ? C8B N9B 1.276(6) . ? C8B H8B 0.9500 . ? C10A O11A 1.432(5) . ? C10A N9A 1.444(6) . ? C10A C16A 1.522(7) . ? C10A H10A 1.0000 . ? C10B O11B 1.412(5) . ? C10B N9B 1.450(6) . ? C10B C16B 1.535(6) . ? C10B H10B 1.0000 . ? C12A O11A 1.423(6) . ? C12A C13A 1.513(7) . ? C12A C22A 1.514(6) . ? C12A H12A 1.0000 . ? C12B O11B 1.443(5) . ? C12B C13B 1.507(7) . ? C12B C22B 1.521(7) . ? C12B H12B 1.0000 . ? C13A O18A 1.451(6) . ? C13A C14A 1.525(7) . ? C13A H13A 1.0000 . ? C13B O18B 1.430(6) . ? C13B C14B 1.525(6) . ? C13B H13B 1.0000 . ? C14A O15A 1.404(6) . ? C14A C16A 1.524(7) . ? C14A H14A 1.0000 . ? C14B O15B 1.411(6) . ? C14B C16B 1.527(7) . ? C14B H14B 1.0000 . ? C16A O17A 1.427(5) . ? C16A H16A 1.0000 . ? C16B O17B 1.422(5) . ? C16B H16B 1.0000 . ? C19A O21A 1.412(6) . ? C19A O18A 1.424(5) . ? C19A C20A 1.501(7) . ? C19A H19A 1.0000 . ? C19B O21B 1.415(6) . ? C19B O18B 1.421(6) . ? C19B C20B 1.509(7) . ? C19B H19B 1.0000 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C22A O21A 1.450(6) . ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? C22B O21B 1.444(6) . ? C22B H22C 0.9900 . ? C22B H22D 0.9900 . ? C31 N30 1.328(6) . ? C31 C32 1.390(7) . ? C31 H31 0.9500 . ? C32 C33 1.372(8) . ? C32 H32 0.9500 . ? C33 C34 1.379(8) . ? C33 H33 0.9500 . ? C34 C35 1.372(7) . ? C34 H34 0.9500 . ? C35 N30 1.341(6) . ? C35 H35 0.9500 . ? C41 N40 1.347(7) . ? C41 C42 1.389(8) . ? C41 H41 0.9500 . ? C42 C43 1.389(10) . ? C42 H42 0.9500 . ? C43 C44 1.357(9) . ? C43 H43 0.9500 . ? C44 C45 1.403(7) . ? C44 H44 0.9500 . ? C45 N40 1.316(7) . ? C45 H45 0.9500 . ? C51 N50 1.327(8) . ? C51 C52 1.379(9) . ? C51 H51 0.9500 . ? C52 C53 1.362(10) . ? C52 H52 0.9500 . ? C53 C54 1.365(9) . ? C53 H53 0.9500 . ? C54 C55 1.376(9) . ? C54 H54 0.9500 . ? C55 N50 1.326(8) . ? C55 H55 0.9500 . ? C61 N60 1.335(8) . ? C61 C62 1.418(10) . ? C61 H61 0.9500 . ? C62 C63 1.287(11) . ? C62 H62 0.9500 . ? C63 C64 1.393(9) . ? C63 H63 0.9500 . ? C64 C65 1.377(9) . ? C64 H64 0.9500 . ? C65 N60 1.332(9) . ? C65 H65 0.9500 . ? O15A H15A 0.838(10) . ? O15B H15B 0.833(10) . ? 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 O1A Cu1 N9A 92.32(15) . . ? O1A Cu1 O17B 98.69(13) . . ? N9A Cu1 O17B 159.69(15) . . ? O1A Cu1 O17A 168.77(14) . . ? N9A Cu1 O17A 83.68(15) . . ? O17B Cu1 O17A 82.27(12) . . ? O1A Cu1 N30 93.31(15) . . ? N9A Cu1 N30 103.44(15) . . ? O17B Cu1 N30 92.96(15) . . ? O17A Cu1 N30 97.82(15) . . ? O1A Cu1 Cu2 138.42(10) . . ? N9A Cu1 Cu2 122.89(12) . . ? O17B Cu1 Cu2 41.22(9) . . ? O17A Cu1 Cu2 41.07(9) . . ? N30 Cu1 Cu2 98.37(11) . . ? O1B Cu2 O17A 97.80(14) . . ? O1B Cu2 N9B 92.49(16) . . ? O17A Cu2 N9B 162.51(14) . . ? O1B Cu2 O17B 166.69(14) . . ? O17A Cu2 O17B 83.23(12) . . ? N9B Cu2 O17B 83.55(14) . . ? O1B Cu2 N40 93.40(14) . . ? O17A Cu2 N40 95.08(15) . . ? N9B Cu2 N40 98.41(16) . . ? O17B Cu2 N40 99.74(15) . . ? O1B Cu2 Cu1 137.89(10) . . ? O17A Cu2 Cu1 42.12(9) . . ? N9B Cu2 Cu1 123.46(12) . . ? O17B Cu2 Cu1 41.14(9) . . ? N40 Cu2 Cu1 101.18(11) . . ? O1A C2A C3A 118.4(4) . . ? O1A C2A C7A 124.8(5) . . ? C3A C2A C7A 116.7(5) . . ? O1B C2B C3B 119.1(4) . . ? O1B C2B C7B 123.8(4) . . ? C3B C2B C7B 117.1(4) . . ? C4A C3A C2A 121.3(5) . . ? C4A C3A H3A 119.3 . . ? C2A C3A H3A 119.3 . . ? C4B C3B C2B 122.1(5) . . ? C4B C3B H3B 119.0 . . ? C2B C3B H3B 119.0 . . ? C5A C4A C3A 121.1(5) . . ? C5A C4A H4A 119.5 . . ? C3A C4A H4A 119.5 . . ? C3B C4B C5B 120.7(5) . . ? C3B C4B H4B 119.7 . . ? C5B C4B H4B 119.7 . . ? C6A C5A C4A 118.3(5) . . ? C6A C5A H5A 120.8 . . ? C4A C5A H5A 120.8 . . ? C6B C5B C4B 118.7(5) . . ? C6B C5B H5B 120.7 . . ? C4B C5B H5B 120.7 . . ? C5A C6A C7A 123.3(5) . . ? C5A C6A H6A 118.4 . . ? C7A C6A H6A 118.4 . . ? C5B C6B C7B 121.7(5) . . ? C5B C6B H6B 119.2 . . ? C7B C6B H6B 119.2 . . ? C6A C7A C2A 119.2(5) . . ? C6A C7A C8A 118.4(5) . . ? C2A C7A C8A 122.4(5) . . ? C6B C7B C2B 119.8(4) . . ? C6B C7B C8B 117.0(5) . . ? C2B C7B C8B 123.2(5) . . ? N9A C8A C7A 125.1(5) . . ? N9A C8A H8A 117.4 . . ? C7A C8A H8A 117.4 . . ? N9B C8B C7B 125.4(5) . . ? N9B C8B H8B 117.3 . . ? C7B C8B H8B 117.3 . . ? O11A C10A N9A 110.6(4) . . ? O11A C10A C16A 113.3(4) . . ? N9A C10A C16A 107.9(4) . . ? O11A C10A H10A 108.3 . . ? N9A C10A H10A 108.3 . . ? C16A C10A H10A 108.3 . . ? O11B C10B N9B 111.9(4) . . ? O11B C10B C16B 112.8(4) . . ? N9B C10B C16B 106.7(4) . . ? O11B C10B H10B 108.4 . . ? N9B C10B H10B 108.4 . . ? C16B C10B H10B 108.4 . . ? O11A C12A C13A 109.4(4) . . ? O11A C12A C22A 108.3(4) . . ? C13A C12A C22A 111.4(4) . . ? O11A C12A H12A 109.2 . . ? C13A C12A H12A 109.2 . . ? C22A C12A H12A 109.2 . . ? O11B C12B C13B 110.6(4) . . ? O11B C12B C22B 109.5(4) . . ? C13B C12B C22B 109.5(4) . . ? O11B C12B H12B 109.1 . . ? C13B C12B H12B 109.1 . . ? C22B C12B H12B 109.1 . . ? O18A C13A C12A 108.2(4) . . ? O18A C13A C14A 111.0(4) . . ? C12A C13A C14A 112.0(4) . . ? O18A C13A H13A 108.5 . . ? C12A C13A H13A 108.5 . . ? C14A C13A H13A 108.5 . . ? O18B C13B C12B 108.0(4) . . ? O18B C13B C14B 109.7(4) . . ? C12B C13B C14B 112.7(4) . . ? O18B C13B H13B 108.8 . . ? C12B C13B H13B 108.8 . . ? C14B C13B H13B 108.8 . . ? O15A C14A C16A 113.8(4) . . ? O15A C14A C13A 108.3(4) . . ? C16A C14A C13A 106.4(4) . . ? O15A C14A H14A 109.4 . . ? C16A C14A H14A 109.4 . . ? C13A C14A H14A 109.4 . . ? O15B C14B C13B 107.8(4) . . ? O15B C14B C16B 112.9(4) . . ? C13B C14B C16B 107.2(4) . . ? O15B C14B H14B 109.6 . . ? C13B C14B H14B 109.6 . . ? C16B C14B H14B 109.6 . . ? O17A C16A C10A 104.2(3) . . ? O17A C16A C14A 115.7(4) . . ? C10A C16A C14A 110.4(4) . . ? O17A C16A H16A 108.8 . . ? C10A C16A H16A 108.8 . . ? C14A C16A H16A 108.8 . . ? O17B C16B C14B 115.2(4) . . ? O17B C16B C10B 105.3(3) . . ? C14B C16B C10B 110.6(4) . . ? O17B C16B H16B 108.5 . . ? C14B C16B H16B 108.5 . . ? C10B C16B H16B 108.5 . . ? O21A C19A O18A 111.5(4) . . ? O21A C19A C20A 108.6(4) . . ? O18A C19A C20A 108.7(4) . . ? O21A C19A H19A 109.4 . . ? O18A C19A H19A 109.4 . . ? C20A C19A H19A 109.4 . . ? O21B C19B O18B 110.8(4) . . ? O21B C19B C20B 107.5(4) . . ? O18B C19B C20B 107.0(4) . . ? O21B C19B H19B 110.5 . . ? O18B C19B H19B 110.5 . . ? C20B C19B H19B 110.5 . . ? C19A C20A H20A 109.5 . . ? C19A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? C19A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C19B C20B H20D 109.5 . . ? C19B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C19B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? O21A C22A C12A 107.9(4) . . ? O21A C22A H22A 110.1 . . ? C12A C22A H22A 110.1 . . ? O21A C22A H22B 110.1 . . ? C12A C22A H22B 110.1 . . ? H22A C22A H22B 108.4 . . ? O21B C22B C12B 107.2(4) . . ? O21B C22B H22C 110.3 . . ? C12B C22B H22C 110.3 . . ? O21B C22B H22D 110.3 . . ? C12B C22B H22D 110.3 . . ? H22C C22B H22D 108.5 . . ? N30 C31 C32 123.9(5) . . ? N30 C31 H31 118.0 . . ? C32 C31 H31 118.0 . . ? C33 C32 C31 118.4(5) . . ? C33 C32 H32 120.8 . . ? C31 C32 H32 120.8 . . ? C32 C33 C34 118.3(5) . . ? C32 C33 H33 120.8 . . ? C34 C33 H33 120.8 . . ? C35 C34 C33 119.5(5) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? N30 C35 C34 123.2(5) . . ? N30 C35 H35 118.4 . . ? C34 C35 H35 118.4 . . ? N40 C41 C42 121.9(6) . . ? N40 C41 H41 119.1 . . ? C42 C41 H41 119.1 . . ? C41 C42 C43 118.9(6) . . ? C41 C42 H42 120.6 . . ? C43 C42 H42 120.6 . . ? C44 C43 C42 119.4(6) . . ? C44 C43 H43 120.3 . . ? C42 C43 H43 120.3 . . ? C43 C44 C45 118.0(6) . . ? C43 C44 H44 121.0 . . ? C45 C44 H44 121.0 . . ? N40 C45 C44 123.6(6) . . ? N40 C45 H45 118.2 . . ? C44 C45 H45 118.2 . . ? N50 C51 C52 124.6(7) . . ? N50 C51 H51 117.7 . . ? C52 C51 H51 117.7 . . ? C53 C52 C51 118.1(7) . . ? C53 C52 H52 120.9 . . ? C51 C52 H52 120.9 . . ? C52 C53 C54 119.1(7) . . ? C52 C53 H53 120.5 . . ? C54 C53 H53 120.5 . . ? C53 C54 C55 118.2(7) . . ? C53 C54 H54 120.9 . . ? C55 C54 H54 120.9 . . ? N50 C55 C54 124.6(6) . . ? N50 C55 H55 117.7 . . ? C54 C55 H55 117.7 . . ? N60 C61 C62 121.4(9) . . ? N60 C61 H61 119.3 . . ? C62 C61 H61 119.3 . . ? C63 C62 C61 118.6(8) . . ? C63 C62 H62 120.7 . . ? C61 C62 H62 120.7 . . ? C62 C63 C64 122.7(7) . . ? C62 C63 H63 118.7 . . ? C64 C63 H63 118.7 . . ? C65 C64 C63 115.7(7) . . ? C65 C64 H64 122.1 . . ? C63 C64 H64 122.1 . . ? N60 C65 C64 124.0(7) . . ? N60 C65 H65 118.0 . . ? C64 C65 H65 118.0 . . ? C8A N9A C10A 122.7(4) . . ? C8A N9A Cu1 127.3(4) . . ? C10A N9A Cu1 109.6(3) . . ? C8B N9B C10B 123.2(4) . . ? C8B N9B Cu2 126.5(3) . . ? C10B N9B Cu2 110.2(3) . . ? C31 N30 C35 116.6(4) . . ? C31 N30 Cu1 122.3(3) . . ? C35 N30 Cu1 121.1(3) . . ? C45 N40 C41 118.1(5) . . ? C45 N40 Cu2 120.2(4) . . ? C41 N40 Cu2 121.7(4) . . ? C55 N50 C51 115.3(5) . . ? C65 N60 C61 117.5(7) . . ? C2A O1A Cu1 127.6(3) . . ? C2B O1B Cu2 128.2(3) . . ? C12A O11A C10A 108.5(3) . . ? C10B O11B C12B 108.0(3) . . ? C14A O15A H15A 111(4) . . ? C14B O15B H15B 109(4) . . ? C16A O17A Cu2 135.1(3) . . ? C16A O17A Cu1 108.5(3) . . ? Cu2 O17A Cu1 96.80(13) . . ? C16B O17B Cu1 137.2(3) . . ? C16B O17B Cu2 110.0(3) . . ? Cu1 O17B Cu2 97.64(13) . . ? C19A O18A C13A 109.5(3) . . ? C19B O18B C13B 111.0(4) . . ? C19A O21A C22A 110.3(4) . . ? C19B O21B C22B 111.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1A Cu1 Cu2 O1B 140.2(2) . . . . ? N9A Cu1 Cu2 O1B -3.1(2) . . . . ? O17B Cu1 Cu2 O1B 160.0(2) . . . . ? O17A Cu1 Cu2 O1B -22.8(2) . . . . ? N30 Cu1 Cu2 O1B -115.14(18) . . . . ? O1A Cu1 Cu2 O17A 163.0(2) . . . . ? N9A Cu1 Cu2 O17A 19.70(19) . . . . ? O17B Cu1 Cu2 O17A -177.2(2) . . . . ? N30 Cu1 Cu2 O17A -92.32(18) . . . . ? O1A Cu1 Cu2 N9B -3.8(2) . . . . ? N9A Cu1 Cu2 N9B -147.10(18) . . . . ? O17B Cu1 Cu2 N9B 15.97(19) . . . . ? O17A Cu1 Cu2 N9B -166.80(19) . . . . ? N30 Cu1 Cu2 N9B 100.88(17) . . . . ? O1A Cu1 Cu2 O17B -19.8(2) . . . . ? N9A Cu1 Cu2 O17B -163.1(2) . . . . ? O17A Cu1 Cu2 O17B 177.2(2) . . . . ? N30 Cu1 Cu2 O17B 84.91(19) . . . . ? O1A Cu1 Cu2 N40 -111.8(2) . . . . ? N9A Cu1 Cu2 N40 104.87(17) . . . . ? O17B Cu1 Cu2 N40 -92.06(19) . . . . ? O17A Cu1 Cu2 N40 85.18(19) . . . . ? N30 Cu1 Cu2 N40 -7.14(16) . . . . ? O1A C2A C3A C4A 178.2(5) . . . . ? C7A C2A C3A C4A 0.7(7) . . . . ? O1B C2B C3B C4B -179.2(4) . . . . ? C7B C2B C3B C4B -1.3(7) . . . . ? C2A C3A C4A C5A 1.0(8) . . . . ? C2B C3B C4B C5B 2.0(8) . . . . ? C3A C4A C5A C6A -0.9(9) . . . . ? C3B C4B C5B C6B -1.9(8) . . . . ? C4A C5A C6A C7A -1.1(9) . . . . ? C4B C5B C6B C7B 1.2(8) . . . . ? C5A C6A C7A C2A 2.9(8) . . . . ? C5A C6A C7A C8A -174.9(5) . . . . ? O1A C2A C7A C6A -179.9(5) . . . . ? C3A C2A C7A C6A -2.6(7) . . . . ? O1A C2A C7A C8A -2.2(7) . . . . ? C3A C2A C7A C8A 175.1(5) . . . . ? C5B C6B C7B C2B -0.5(7) . . . . ? C5B C6B C7B C8B -178.8(4) . . . . ? O1B C2B C7B C6B 178.4(4) . . . . ? C3B C2B C7B C6B 0.5(7) . . . . ? O1B C2B C7B C8B -3.5(7) . . . . ? C3B C2B C7B C8B 178.7(4) . . . . ? C6A C7A C8A N9A 174.8(5) . . . . ? C2A C7A C8A N9A -2.9(8) . . . . ? C6B C7B C8B N9B 174.7(5) . . . . ? C2B C7B C8B N9B -3.5(8) . . . . ? O11A C12A C13A O18A 174.7(3) . . . . ? C22A C12A C13A O18A 55.0(5) . . . . ? O11A C12A C13A C14A -62.7(5) . . . . ? C22A C12A C13A C14A 177.6(4) . . . . ? O11B C12B C13B O18B 179.1(4) . . . . ? C22B C12B C13B O18B 58.3(5) . . . . ? O11B C12B C13B C14B -59.6(5) . . . . ? C22B C12B C13B C14B 179.6(4) . . . . ? O18A C13A C14A O15A -60.5(5) . . . . ? C12A C13A C14A O15A 178.5(4) . . . . ? O18A C13A C14A C16A 176.8(4) . . . . ? C12A C13A C14A C16A 55.8(5) . . . . ? O18B C13B C14B O15B -65.5(5) . . . . ? C12B C13B C14B O15B 174.2(4) . . . . ? O18B C13B C14B C16B 172.7(4) . . . . ? C12B C13B C14B C16B 52.4(5) . . . . ? O11A C10A C16A O17A -178.0(3) . . . . ? N9A C10A C16A O17A -55.2(4) . . . . ? O11A C10A C16A C14A 57.2(5) . . . . ? N9A C10A C16A C14A 180.0(4) . . . . ? O15A C14A C16A O17A 71.2(5) . . . . ? C13A C14A C16A O17A -169.6(4) . . . . ? O15A C14A C16A C10A -170.8(4) . . . . ? C13A C14A C16A C10A -51.6(5) . . . . ? O15B C14B C16B O17B 72.0(5) . . . . ? C13B C14B C16B O17B -169.4(4) . . . . ? O15B C14B C16B C10B -168.7(4) . . . . ? C13B C14B C16B C10B -50.2(5) . . . . ? O11B C10B C16B O17B -176.3(3) . . . . ? N9B C10B C16B O17B -53.0(4) . . . . ? O11B C10B C16B C14B 58.6(5) . . . . ? N9B C10B C16B C14B -178.1(4) . . . . ? O11A C12A C22A O21A -174.8(4) . . . . ? C13A C12A C22A O21A -54.4(5) . . . . ? O11B C12B C22B O21B -178.3(4) . . . . ? C13B C12B C22B O21B -56.9(5) . . . . ? N30 C31 C32 C33 -0.9(9) . . . . ? C31 C32 C33 C34 0.2(9) . . . . ? C32 C33 C34 C35 0.3(9) . . . . ? C33 C34 C35 N30 -0.2(9) . . . . ? N40 C41 C42 C43 0.4(9) . . . . ? C41 C42 C43 C44 1.9(10) . . . . ? C42 C43 C44 C45 -3.1(10) . . . . ? C43 C44 C45 N40 2.1(9) . . . . ? N50 C51 C52 C53 1.2(12) . . . . ? C51 C52 C53 C54 -2.0(12) . . . . ? C52 C53 C54 C55 1.5(11) . . . . ? C53 C54 C55 N50 0.0(10) . . . . ? N60 C61 C62 C63 1.8(11) . . . . ? C61 C62 C63 C64 -2.3(12) . . . . ? C62 C63 C64 C65 1.3(11) . . . . ? C63 C64 C65 N60 0.2(11) . . . . ? C7A C8A N9A C10A -179.4(4) . . . . ? C7A C8A N9A Cu1 7.7(7) . . . . ? O11A C10A N9A C8A -11.3(6) . . . . ? C16A C10A N9A C8A -135.7(4) . . . . ? O11A C10A N9A Cu1 162.7(3) . . . . ? C16A C10A N9A Cu1 38.3(4) . . . . ? O1A Cu1 N9A C8A -6.3(4) . . . . ? O17B Cu1 N9A C8A 116.8(5) . . . . ? O17A Cu1 N9A C8A 163.2(4) . . . . ? N30 Cu1 N9A C8A -100.2(4) . . . . ? Cu2 Cu1 N9A C8A 150.3(4) . . . . ? O1A Cu1 N9A C10A -179.9(3) . . . . ? O17B Cu1 N9A C10A -56.9(5) . . . . ? O17A Cu1 N9A C10A -10.5(3) . . . . ? N30 Cu1 N9A C10A 86.1(3) . . . . ? Cu2 Cu1 N9A C10A -23.3(3) . . . . ? C7B C8B N9B C10B -179.0(4) . . . . ? C7B C8B N9B Cu2 6.8(7) . . . . ? O11B C10B N9B C8B -13.9(6) . . . . ? C16B C10B N9B C8B -137.8(4) . . . . ? O11B C10B N9B Cu2 161.1(3) . . . . ? C16B C10B N9B Cu2 37.3(4) . . . . ? O1B Cu2 N9B C8B -3.5(4) . . . . ? O17A Cu2 N9B C8B 122.6(5) . . . . ? O17B Cu2 N9B C8B 163.7(4) . . . . ? N40 Cu2 N9B C8B -97.3(4) . . . . ? Cu1 Cu2 N9B C8B 153.2(3) . . . . ? O1B Cu2 N9B C10B -178.4(3) . . . . ? O17A Cu2 N9B C10B -52.3(6) . . . . ? O17B Cu2 N9B C10B -11.1(3) . . . . ? N40 Cu2 N9B C10B 87.8(3) . . . . ? Cu1 Cu2 N9B C10B -21.6(3) . . . . ? C32 C31 N30 C35 0.9(8) . . . . ? C32 C31 N30 Cu1 -179.4(4) . . . . ? C34 C35 N30 C31 -0.4(8) . . . . ? C34 C35 N30 Cu1 179.9(4) . . . . ? O1A Cu1 N30 C31 -103.7(4) . . . . ? N9A Cu1 N30 C31 -10.5(5) . . . . ? O17B Cu1 N30 C31 157.4(4) . . . . ? O17A Cu1 N30 C31 74.9(4) . . . . ? Cu2 Cu1 N30 C31 116.4(4) . . . . ? O1A Cu1 N30 C35 76.0(4) . . . . ? N9A Cu1 N30 C35 169.2(4) . . . . ? O17B Cu1 N30 C35 -22.9(4) . . . . ? O17A Cu1 N30 C35 -105.5(4) . . . . ? Cu2 Cu1 N30 C35 -64.0(4) . . . . ? C44 C45 N40 C41 0.1(8) . . . . ? C44 C45 N40 Cu2 -176.4(4) . . . . ? C42 C41 N40 C45 -1.3(8) . . . . ? C42 C41 N40 Cu2 175.1(4) . . . . ? O1B Cu2 N40 C45 -79.4(4) . . . . ? O17A Cu2 N40 C45 -177.5(4) . . . . ? N9B Cu2 N40 C45 13.6(4) . . . . ? O17B Cu2 N40 C45 98.5(4) . . . . ? Cu1 Cu2 N40 C45 140.3(4) . . . . ? O1B Cu2 N40 C41 104.2(4) . . . . ? O17A Cu2 N40 C41 6.1(4) . . . . ? N9B Cu2 N40 C41 -162.8(4) . . . . ? O17B Cu2 N40 C41 -77.9(4) . . . . ? Cu1 Cu2 N40 C41 -36.1(4) . . . . ? C54 C55 N50 C51 -0.9(9) . . . . ? C52 C51 N50 C55 0.3(10) . . . . ? C64 C65 N60 C61 -0.6(10) . . . . ? C62 C61 N60 C65 -0.3(10) . . . . ? C3A C2A O1A Cu1 -175.4(3) . . . . ? C7A C2A O1A Cu1 1.9(7) . . . . ? N9A Cu1 O1A C2A 1.6(4) . . . . ? O17B Cu1 O1A C2A -161.3(4) . . . . ? O17A Cu1 O1A C2A -67.2(8) . . . . ? N30 Cu1 O1A C2A 105.2(4) . . . . ? Cu2 Cu1 O1A C2A -148.3(3) . . . . ? C3B C2B O1B Cu2 -175.9(3) . . . . ? C7B C2B O1B Cu2 6.3(6) . . . . ? O17A Cu2 O1B C2B -168.7(4) . . . . ? N9B Cu2 O1B C2B -2.9(4) . . . . ? O17B Cu2 O1B C2B -75.2(7) . . . . ? N40 Cu2 O1B C2B 95.7(4) . . . . ? Cu1 Cu2 O1B C2B -153.5(3) . . . . ? C13A C12A O11A C10A 62.4(4) . . . . ? C22A C12A O11A C10A -176.0(4) . . . . ? N9A C10A O11A C12A 177.3(4) . . . . ? C16A C10A O11A C12A -61.5(5) . . . . ? N9B C10B O11B C12B 176.9(4) . . . . ? C16B C10B O11B C12B -62.8(5) . . . . ? C13B C12B O11B C10B 62.4(5) . . . . ? C22B C12B O11B C10B -176.9(4) . . . . ? C10A C16A O17A Cu2 166.2(3) . . . . ? C14A C16A O17A Cu2 -72.5(5) . . . . ? C10A C16A O17A Cu1 45.3(4) . . . . ? C14A C16A O17A Cu1 166.7(3) . . . . ? O1B Cu2 O17A C16A 39.9(4) . . . . ? N9B Cu2 O17A C16A -85.6(6) . . . . ? O17B Cu2 O17A C16A -126.8(4) . . . . ? N40 Cu2 O17A C16A 134.0(4) . . . . ? Cu1 Cu2 O17A C16A -124.9(4) . . . . ? O1B Cu2 O17A Cu1 164.79(14) . . . . ? N9B Cu2 O17A Cu1 39.3(5) . . . . ? O17B Cu2 O17A Cu1 -1.83(15) . . . . ? N40 Cu2 O17A Cu1 -101.07(15) . . . . ? O1A Cu1 O17A C16A 48.5(8) . . . . ? N9A Cu1 O17A C16A -21.1(3) . . . . ? O17B Cu1 O17A C16A 144.2(3) . . . . ? N30 Cu1 O17A C16A -123.8(3) . . . . ? Cu2 Cu1 O17A C16A 142.4(3) . . . . ? O1A Cu1 O17A Cu2 -93.9(7) . . . . ? N9A Cu1 O17A Cu2 -163.46(16) . . . . ? O17B Cu1 O17A Cu2 1.84(15) . . . . ? N30 Cu1 O17A Cu2 93.79(15) . . . . ? C14B C16B O17B Cu1 -66.8(6) . . . . ? C10B C16B O17B Cu1 171.0(3) . . . . ? C14B C16B O17B Cu2 166.2(3) . . . . ? C10B C16B O17B Cu2 44.1(4) . . . . ? O1A Cu1 O17B C16B 36.1(4) . . . . ? N9A Cu1 O17B C16B -86.0(6) . . . . ? O17A Cu1 O17B C16B -132.6(4) . . . . ? N30 Cu1 O17B C16B 129.9(4) . . . . ? Cu2 Cu1 O17B C16B -130.8(5) . . . . ? O1A Cu1 O17B Cu2 166.86(14) . . . . ? N9A Cu1 O17B Cu2 44.8(5) . . . . ? O17A Cu1 O17B Cu2 -1.83(15) . . . . ? N30 Cu1 O17B Cu2 -99.33(16) . . . . ? O1B Cu2 O17B C16B 53.4(7) . . . . ? O17A Cu2 O17B C16B 148.7(3) . . . . ? N9B Cu2 O17B C16B -19.8(3) . . . . ? N40 Cu2 O17B C16B -117.3(3) . . . . ? Cu1 Cu2 O17B C16B 146.8(3) . . . . ? O1B Cu2 O17B Cu1 -93.4(6) . . . . ? O17A Cu2 O17B Cu1 1.87(15) . . . . ? N9B Cu2 O17B Cu1 -166.65(16) . . . . ? N40 Cu2 O17B Cu1 95.89(17) . . . . ? O21A C19A O18A C13A 64.6(4) . . . . ? C20A C19A O18A C13A -175.8(4) . . . . ? C12A C13A O18A C19A -58.2(4) . . . . ? C14A C13A O18A C19A 178.6(4) . . . . ? O21B C19B O18B C13B 61.6(5) . . . . ? C20B C19B O18B C13B 178.6(4) . . . . ? C12B C13B O18B C19B -60.0(5) . . . . ? C14B C13B O18B C19B 176.8(4) . . . . ? O18A C19A O21A C22A -64.7(5) . . . . ? C20A C19A O21A C22A 175.7(4) . . . . ? C12A C22A O21A C19A 57.9(5) . . . . ? O18B C19B O21B C22B -61.2(5) . . . . ? C20B C19B O21B C22B -177.8(4) . . . . ? C12B C22B O21B C19B 58.3(5) . . . . ? 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 O15A H15A O1B 0.838(10) 1.834(11) 2.672(5) 179(7) . O15B H15B O1A 0.833(10) 1.87(2) 2.678(5) 163(6) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.568 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.077 data_6 _database_code_CSD 193692 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H42 Br2 Cu2 N4 O12' _chemical_formula_weight 1057.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 _symmetry_Int_Tables_number 1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 13.230(1) _cell_length_b 13.242(1) _cell_length_c 13.426(1) _cell_angle_alpha 104.83(1) _cell_angle_beta 105.40(1) _cell_angle_gamma 104.06(1) _cell_volume 2066.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19400 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 3.031 _exptl_absorpt_correction_type 'Empirical from multiple refl.' _exptl_absorpt_correction_T_min 0.5356 _exptl_absorpt_correction_T_max 0.6555 _exptl_absorpt_process_details 'MULABS (Platon2000; cf. Blessing 1995)' _exptl_special_details ; dx = 35 mm; 160 sec./deg., 1 deg.; mos. = 1.428(3) deg. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16737 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0838 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11552 _reflns_number_gt 10246 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (A.L.Spek, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+9.5313P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.052(13) _refine_ls_number_reflns 11552 _refine_ls_number_parameters 1081 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1545 _refine_ls_wR_factor_gt 0.1488 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2A C 0.4724(9) 0.7461(9) 1.0539(8) 0.032(2) Uani 1 1 d . . . C2B C 0.0863(9) 0.0552(8) 0.7206(8) 0.032(3) Uani 1 1 d . . . C2C C 0.6929(9) 1.2362(9) 0.8262(9) 0.031(2) Uani 1 1 d . . . C2D C 0.3507(10) 0.5464(8) 0.4416(9) 0.032(3) Uani 1 1 d . . . C3A C 0.5574(9) 0.8344(10) 1.0549(9) 0.038(3) Uani 1 1 d . . . H3A H 0.5963 0.8198 1.0056 0.046 Uiso 1 1 calc R . . C3B C 0.0104(10) -0.0352(9) 0.7290(9) 0.035(3) Uani 1 1 d . . . H3B H -0.0260 -0.0218 0.7808 0.042 Uiso 1 1 calc R . . C3C C 0.6883(10) 1.3257(9) 0.9084(9) 0.033(3) Uani 1 1 d . . . H3C H 0.6401 1.3130 0.9485 0.040 Uiso 1 1 calc R . . C3D C 0.3521(9) 0.4558(10) 0.3576(9) 0.037(3) Uani 1 1 d . . . H3D H 0.4031 0.4693 0.3205 0.044 Uiso 1 1 calc R . . C4B C -0.0116(9) -0.1421(9) 0.6635(9) 0.0346(16) Uani 1 1 d . . . H4B H -0.0631 -0.2019 0.6700 0.041 Uiso 1 1 calc R . . C4A C 0.5863(9) 0.9414(9) 1.1251(9) 0.0346(16) Uani 1 1 d . . . H4A H 0.6424 0.9999 1.1223 0.041 Uiso 1 1 calc R . . C4C C 0.7549(10) 1.4301(9) 0.9279(8) 0.0352(17) Uani 1 1 d . . . H4C H 0.7502 1.4910 0.9799 0.042 Uiso 1 1 calc R . . C4D C 0.2809(9) 0.3484(9) 0.3287(8) 0.0352(17) Uani 1 1 d . . . H4D H 0.2822 0.2896 0.2715 0.042 Uiso 1 1 calc R . . C5A C 0.5321(9) 0.9624(9) 1.2003(9) 0.036(3) Uani 1 1 d . . . C5B C 0.0412(8) -0.1628(9) 0.5882(9) 0.030(2) Uani 1 1 d . . . C5C C 0.8293(10) 1.4498(8) 0.8738(8) 0.030(2) Uani 1 1 d . . . C5D C 0.2091(9) 0.3288(9) 0.3839(8) 0.030(2) Uani 1 1 d . . . C7A C 0.4501(9) 0.8780(9) 1.2031(9) 0.034(2) Uani 1 1 d . . . H7A H 0.4150 0.8923 1.2559 0.041 Uiso 1 1 calc R . . C7B C 0.1126(10) -0.0819(9) 0.5764(9) 0.034(3) Uani 1 1 d . . . H7B H 0.1450 -0.0990 0.5217 0.041 Uiso 1 1 calc R . . C7C C 0.8386(10) 1.3692(9) 0.8000(10) 0.037(3) Uani 1 1 d . . . H7C H 0.8901 1.3850 0.7638 0.044 Uiso 1 1 calc R . . C7D C 0.2033(9) 0.4145(9) 0.4673(9) 0.032(2) Uani 1 1 d . . . H7D H 0.1499 0.3992 0.5015 0.039 Uiso 1 1 calc R . . C8A C 0.4181(8) 0.7706(8) 1.1280(8) 0.026(2) Uani 1 1 d . . . C8B C 0.1429(8) 0.0326(8) 0.6451(8) 0.029(2) Uani 1 1 d . . . C8C C 0.7710(9) 1.2583(9) 0.7745(8) 0.033(3) Uani 1 1 d . . . C8D C 0.2790(9) 0.5259(8) 0.5004(9) 0.028(2) Uani 1 1 d . . . C9A C 0.3217(9) 0.6920(8) 1.1291(9) 0.031(2) Uani 1 1 d . . . H9A H 0.2864 0.7186 1.1783 0.037 Uiso 1 1 calc R . . C9B C 0.2258(9) 0.1177(9) 0.6306(8) 0.031(2) Uani 1 1 d . . . H9B H 0.2584 0.0943 0.5776 0.037 Uiso 1 1 calc R . . C9C C 0.7846(8) 1.1683(8) 0.6913(8) 0.027(2) Uani 1 1 d . . . H9C H 0.8400 1.1898 0.6609 0.033 Uiso 1 1 calc R . . C9D C 0.2779(9) 0.6000(9) 0.5954(9) 0.030(2) Uani 1 1 d . . . H9D H 0.2290 0.5737 0.6308 0.036 Uiso 1 1 calc R . . C11A C 0.1761(9) 0.5146(8) 1.0614(8) 0.033(2) Uani 1 1 d . . . H11A H 0.1152 0.5207 1.0029 0.040 Uiso 1 1 calc R . . C11B C 0.3364(9) 0.3009(9) 0.6632(8) 0.033(2) Uani 1 1 d . . . H11B H 0.2940 0.3333 0.6142 0.039 Uiso 1 1 calc R . . C11C C 0.7513(9) 0.9846(9) 0.5813(8) 0.034(2) Uani 1 1 d . . . H11C H 0.7997 0.9511 0.6233 0.041 Uiso 1 1 calc R . . C11D C 0.3514(9) 0.7784(8) 0.7410(9) 0.034(2) Uani 1 1 d . . . H11D H 0.4133 0.7741 0.7999 0.040 Uiso 1 1 calc R . . C13A C 0.0454(9) 0.4676(9) 1.1418(9) 0.034(2) Uani 1 1 d . . . H13A H -0.0101 0.4771 1.0810 0.040 Uiso 1 1 calc R . . C13B C 0.4695(9) 0.3437(9) 0.5859(9) 0.035(2) Uani 1 1 d . . . H13B H 0.4186 0.3727 0.5404 0.042 Uiso 1 1 calc R . . C13C C 0.8266(9) 0.9400(8) 0.4466(9) 0.035(2) Uani 1 1 d . . . H13C H 0.8722 0.9087 0.4944 0.042 Uiso 1 1 calc R . . C13D C 0.2751(9) 0.8271(8) 0.8756(8) 0.031(2) Uani 1 1 d . . . H13D H 0.3398 0.8210 0.9297 0.037 Uiso 1 1 calc R . . C14A C 0.0393(9) 0.3486(8) 1.1082(8) 0.029(2) Uani 1 1 d . . . H14A H 0.0944 0.3385 1.1689 0.035 Uiso 1 1 calc R . . C14B C 0.5465(9) 0.4387(9) 0.6923(9) 0.033(2) Uani 1 1 d . . . H14B H 0.5998 0.4112 0.7369 0.039 Uiso 1 1 calc R . . C14C C 0.7175(9) 0.8477(9) 0.3680(9) 0.031(2) Uani 1 1 d . . . H14C H 0.6732 0.8777 0.3177 0.037 Uiso 1 1 calc R . . C14D C 0.3016(9) 0.9460(9) 0.8746(8) 0.032(2) Uani 1 1 d . . . H14D H 0.2373 0.9511 0.8192 0.039 Uiso 1 1 calc R . . C15A C 0.0663(10) 0.3144(8) 1.0039(9) 0.033(2) Uani 1 1 d . . . H15A H 0.0079 0.3165 0.9402 0.040 Uiso 1 1 calc R . . C15B C 0.4846(9) 0.4866(9) 0.7606(8) 0.033(3) Uani 1 1 d . . . H15B H 0.4413 0.5254 0.7207 0.040 Uiso 1 1 calc R . . C15C C 0.6501(9) 0.8031(10) 0.4314(8) 0.034(3) Uani 1 1 d . . . H15C H 0.6922 0.7655 0.4742 0.041 Uiso 1 1 calc R . . C15D C 0.4055(9) 0.9830(8) 0.8475(9) 0.029(2) Uani 1 1 d . . . H15D H 0.4716 0.9835 0.9053 0.035 Uiso 1 1 calc R . . C17A C 0.1767(10) 0.3963(8) 1.0245(9) 0.039(3) Uani 1 1 d . . . H17A H 0.2352 0.3876 1.0832 0.047 Uiso 1 1 calc R . . C17B C 0.4041(9) 0.3939(9) 0.7761(8) 0.029(2) Uani 1 1 d . . . H17B H 0.4478 0.3627 0.8256 0.035 Uiso 1 1 calc R . . C17C C 0.6354(8) 0.8929(9) 0.5091(7) 0.025(2) Uani 1 1 d . . . H17C H 0.5874 0.9265 0.4668 0.029 Uiso 1 1 calc R . . C17D C 0.3842(9) 0.8954(9) 0.7364(9) 0.035(3) Uani 1 1 d . . . H17D H 0.3213 0.9004 0.6793 0.042 Uiso 1 1 calc R . . C20A C -0.0914(10) 0.3096(9) 1.1922(10) 0.041(3) Uani 1 1 d . . . H20A H -0.0353 0.2997 1.2522 0.049 Uiso 1 1 calc R . . C20B C 0.6675(10) 0.4820(11) 0.5954(10) 0.042(3) Uani 1 1 d . . . H20B H 0.7239 0.4587 0.6415 0.051 Uiso 1 1 calc R . . C20C C 0.8086(11) 0.8046(11) 0.2435(10) 0.048(3) Uani 1 1 d . . . H20C H 0.7619 0.8333 0.1937 0.058 Uiso 1 1 calc R . . C20D C 0.2183(11) 0.9847(9) 1.0065(10) 0.041(3) Uani 1 1 d . . . H20D H 0.1551 0.9893 0.9492 0.049 Uiso 1 1 calc R . . C21A C -0.2075(13) 0.2320(10) 1.1690(14) 0.067(4) Uani 1 1 d . . . H21A H -0.2086 0.1551 1.1473 0.100 Uiso 1 1 calc R . . H21B H -0.2615 0.2417 1.1094 0.100 Uiso 1 1 calc R . . H21C H -0.2269 0.2493 1.2354 0.100 Uiso 1 1 calc R . . C21B C 0.7264(12) 0.5717(12) 0.5659(11) 0.058(4) Uani 1 1 d . . . H21D H 0.7733 0.6350 0.6329 0.087 Uiso 1 1 calc R . . H21E H 0.6724 0.5942 0.5188 0.087 Uiso 1 1 calc R . . H21F H 0.7730 0.5462 0.5264 0.087 Uiso 1 1 calc R . . C21C C 0.8334(14) 0.7117(13) 0.1756(12) 0.065(4) Uani 1 1 d . . . H21G H 0.7637 0.6517 0.1283 0.097 Uiso 1 1 calc R . . H21H H 0.8804 0.6841 0.2241 0.097 Uiso 1 1 calc R . . H21I H 0.8725 0.7385 0.1299 0.097 Uiso 1 1 calc R . . C21D C 0.2366(13) 1.0661(12) 1.1175(11) 0.057(4) Uani 1 1 d . . . H21J H 0.1696 1.0466 1.1364 0.086 Uiso 1 1 calc R . . H21K H 0.2526 1.1412 1.1142 0.086 Uiso 1 1 calc R . . H21L H 0.2996 1.0631 1.1735 0.086 Uiso 1 1 calc R . . C23A C 0.0162(10) 0.5000(9) 1.2452(10) 0.037(3) Uani 1 1 d . . . H23A H 0.0732 0.4975 1.3087 0.044 Uiso 1 1 calc R . . H23B H 0.0127 0.5761 1.2622 0.044 Uiso 1 1 calc R . . C23B C 0.5376(11) 0.3042(10) 0.5239(10) 0.043(3) Uani 1 1 d . . . H23C H 0.5881 0.2748 0.5678 0.051 Uiso 1 1 calc R . . H23D H 0.4884 0.2433 0.4545 0.051 Uiso 1 1 calc R . . C23C C 0.8888(11) 0.9795(10) 0.3764(10) 0.045(3) Uani 1 1 d . . . H23E H 0.8443 1.0106 0.3286 0.054 Uiso 1 1 calc R . . H23F H 0.9603 1.0387 0.4243 0.054 Uiso 1 1 calc R . . C23D C 0.1726(12) 0.7946(9) 0.9060(10) 0.043(3) Uani 1 1 d . . . H23G H 0.1067 0.7937 0.8491 0.052 Uiso 1 1 calc R . . H23H H 0.1589 0.7196 0.9115 0.052 Uiso 1 1 calc R . . C31 C 0.5408(10) 0.5178(9) 1.1585(9) 0.045(3) Uani 1 1 d D . . H31 H 0.5539 0.5948 1.1729 0.054 Uiso 1 1 calc R . . C32 C 0.6076(14) 0.4865(11) 1.2321(11) 0.064(4) Uani 1 1 d . . . H32 H 0.6675 0.5393 1.2950 0.077 Uiso 1 1 calc R . . C33 C 0.5834(13) 0.3722(13) 1.2102(12) 0.066(4) Uani 1 1 d . . . H33 H 0.6272 0.3471 1.2604 0.080 Uiso 1 1 calc R . . C34 C 0.5004(11) 0.2971(10) 1.1206(11) 0.052(3) Uani 1 1 d . . . H34 H 0.4853 0.2197 1.1055 0.062 Uiso 1 1 calc R . . C35 C 0.4375(10) 0.3384(8) 1.0506(10) 0.044(3) Uani 1 1 d D . . H35 H 0.3768 0.2867 0.9877 0.053 Uiso 1 1 calc R . . C41 C 0.0822(10) 0.4518(8) 0.7067(10) 0.039(3) Uani 1 1 d D . . H41 H 0.1377 0.5048 0.7727 0.047 Uiso 1 1 calc R . . C42 C 0.0124(12) 0.4878(11) 0.6404(10) 0.050(3) Uani 1 1 d . . . H42 H 0.0177 0.5636 0.6607 0.060 Uiso 1 1 calc R . . C43 C -0.0673(12) 0.4097(13) 0.5417(12) 0.059(4) Uani 1 1 d . . . H43 H -0.1173 0.4321 0.4940 0.071 Uiso 1 1 calc R . . C44 C -0.0728(12) 0.2981(12) 0.5137(11) 0.055(3) Uani 1 1 d . . . H44 H -0.1249 0.2440 0.4464 0.066 Uiso 1 1 calc R . . C45 C -0.0009(9) 0.2706(10) 0.5865(9) 0.040(3) Uani 1 1 d D . . H45 H -0.0051 0.1952 0.5686 0.048 Uiso 1 1 calc R . . C51 C 0.3631(11) 0.9499(8) 0.4696(10) 0.041(3) Uani 1 1 d D . . H51 H 0.4270 1.0018 0.5290 0.049 Uiso 1 1 calc R . . C52 C 0.2989(13) 0.9863(11) 0.3985(11) 0.054(4) Uani 1 1 d . . . H52 H 0.3232 1.0622 0.4052 0.065 Uiso 1 1 calc R . . C53 C 0.1983(12) 0.9147(11) 0.3160(11) 0.050(3) Uani 1 1 d . . . H53 H 0.1507 0.9402 0.2695 0.060 Uiso 1 1 calc R . . C54 C 0.1736(11) 0.8055(11) 0.3071(10) 0.044(3) Uani 1 1 d . . . H54 H 0.1070 0.7525 0.2520 0.052 Uiso 1 1 calc R . . C55 C 0.2439(9) 0.7707(8) 0.3771(9) 0.038(3) Uani 1 1 d D . . H55 H 0.2249 0.6941 0.3677 0.046 Uiso 1 1 calc R . . C61 C 0.8149(9) 1.0166(10) 0.9149(9) 0.043(3) Uani 1 1 d D . . H61 H 0.8291 1.0926 0.9227 0.052 Uiso 1 1 calc R . . C62 C 0.8898(13) 0.9908(12) 0.9878(11) 0.062(4) Uani 1 1 d . . . H62 H 0.9532 1.0471 1.0441 0.075 Uiso 1 1 calc R . . C63 C 0.8707(12) 0.8813(14) 0.9771(13) 0.074(5) Uani 1 1 d . . . H63 H 0.9203 0.8594 1.0257 0.089 Uiso 1 1 calc R . . C64 C 0.7745(12) 0.8021(12) 0.8912(14) 0.064(4) Uani 1 1 d . . . H64 H 0.7579 0.7255 0.8814 0.077 Uiso 1 1 calc R . . C65 C 0.7052(11) 0.8369(9) 0.8219(11) 0.049(3) Uani 1 1 d D . . H65 H 0.6417 0.7832 0.7632 0.059 Uiso 1 1 calc R . . N10A N 0.2799(7) 0.5893(7) 1.0690(7) 0.032(2) Uani 1 1 d . . . N10B N 0.2570(7) 0.2196(7) 0.6832(6) 0.0281(19) Uani 1 1 d . . . N10C N 0.7303(7) 1.0680(7) 0.6581(7) 0.035(2) Uani 1 1 d . . . N10D N 0.3413(8) 0.7037(7) 0.6372(7) 0.033(2) Uani 1 1 d . . . N30 N 0.4573(8) 0.4463(7) 1.0665(7) 0.041(2) Uani 1 1 d D . . N40 N 0.0762(8) 0.3439(7) 0.6828(7) 0.039(2) Uani 1 1 d D . . N50 N 0.3365(7) 0.8410(7) 0.4564(7) 0.037(2) Uani 1 1 d D . . N60 N 0.7245(7) 0.9439(6) 0.8346(7) 0.035(2) Uani 1 1 d D . . O1A O 0.4480(7) 0.6436(6) 0.9820(7) 0.043(2) Uani 1 1 d . . . O1B O 0.1026(6) 0.1547(6) 0.7852(6) 0.0337(17) Uani 1 1 d . . . O1C O 0.6247(6) 1.1373(6) 0.8102(6) 0.0355(18) Uani 1 1 d . . . O1D O 0.4214(7) 0.6459(6) 0.4640(7) 0.0405(19) Uani 1 1 d . . . O12A O 0.1528(6) 0.5421(6) 1.1616(6) 0.0359(18) Uani 1 1 d . . . O12B O 0.4036(6) 0.2581(6) 0.6121(6) 0.0352(18) Uani 1 1 d . . . O12C O 0.8045(6) 1.0275(6) 0.5141(6) 0.0358(18) Uani 1 1 d . . . O12D O 0.2521(7) 0.7510(6) 0.7667(6) 0.0354(18) Uani 1 1 d . . . O16A O 0.0707(7) 0.2053(6) 0.9846(6) 0.0409(18) Uani 1 1 d D . . H16A H 0.093(11) 0.184(11) 0.933(7) 0.061 Uiso 1 1 d D . . O16B O 0.5657(7) 0.5665(6) 0.8620(6) 0.045(2) Uani 1 1 d D . . H16B H 0.541(11) 0.596(11) 0.909(9) 0.068 Uiso 1 1 d D . . O16C O 0.5472(7) 0.7205(7) 0.3527(6) 0.047(2) Uani 1 1 d D . . H16C H 0.495(8) 0.695(12) 0.373(11) 0.071 Uiso 1 1 d D . . O16D O 0.4217(7) 1.0883(6) 0.8395(6) 0.0413(18) Uani 1 1 d D . . H16D H 0.475(7) 1.108(11) 0.818(11) 0.062 Uiso 1 1 d D . . O18A O 0.2084(7) 0.3870(6) 0.9308(6) 0.043(2) Uani 1 1 d . . . O18B O 0.3278(6) 0.4230(6) 0.8184(6) 0.0363(18) Uani 1 1 d . . . O18C O 0.5913(6) 0.8664(6) 0.5853(6) 0.0314(16) Uani 1 1 d . . . O18D O 0.4762(7) 0.9086(6) 0.7014(6) 0.043(2) Uani 1 1 d . . . O19A O -0.0687(6) 0.2804(6) 1.0920(6) 0.0351(17) Uani 1 1 d . . . O19B O 0.6091(7) 0.5252(6) 0.6604(6) 0.0381(19) Uani 1 1 d . . . O19C O 0.7487(7) 0.7622(6) 0.3042(6) 0.0390(19) Uani 1 1 d . . . O19D O 0.3166(6) 1.0160(6) 0.9819(6) 0.0374(19) Uani 1 1 d . . . O22A O -0.0918(6) 0.4207(7) 1.2237(6) 0.0400(19) Uani 1 1 d . . . O22B O 0.6006(7) 0.3907(7) 0.4999(6) 0.045(2) Uani 1 1 d . . . O22C O 0.9093(7) 0.8898(7) 0.3107(7) 0.044(2) Uani 1 1 d . . . O22D O 0.1916(7) 0.8747(7) 1.0103(6) 0.0384(18) Uani 1 1 d . . . Cu1 Cu 0.34110(11) 0.51282(10) 0.96537(10) 0.0357(3) Uani 1 1 d . . . Cu2 Cu 0.20446(10) 0.29171(10) 0.79401(10) 0.0314(3) Uani 1 1 d . . . Cu3 Cu 0.61810(10) 0.99763(10) 0.71152(10) 0.0318(3) Uani 1 1 d . . . Cu4 Cu 0.44285(11) 0.77772(10) 0.57446(10) 0.0337(3) Uani 1 1 d . . . Br6A Br 0.57528(11) 1.10912(9) 1.30047(11) 0.0524(4) Uani 1 1 d . . . Br6B Br 0.00400(10) -0.31155(9) 0.49237(10) 0.0460(3) Uani 1 1 d . . . Br6C Br 0.92498(10) 1.59930(9) 0.90976(10) 0.0455(3) Uani 1 1 d . . . Br6D Br 0.11362(10) 0.18008(8) 0.34824(10) 0.0448(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 C2A 0.041(6) 0.027(6) 0.029(6) 0.010(4) 0.013(5) 0.012(5) C2B 0.029(6) 0.013(5) 0.027(5) -0.008(4) -0.011(4) -0.002(4) C2C 0.029(5) 0.021(6) 0.041(6) 0.010(5) 0.014(5) 0.003(5) C2D 0.040(6) 0.011(5) 0.039(6) 0.002(4) 0.007(5) 0.010(5) C3A 0.038(6) 0.032(6) 0.048(7) 0.012(5) 0.026(6) 0.003(5) C3B 0.044(7) 0.021(6) 0.029(6) 0.005(4) 0.003(5) 0.007(5) C3C 0.042(6) 0.027(6) 0.036(6) 0.019(5) 0.013(5) 0.015(5) C3D 0.030(6) 0.038(7) 0.033(6) 0.002(5) 0.015(5) 0.003(5) C4B 0.027(4) 0.026(4) 0.041(4) 0.007(3) 0.007(3) 0.000(3) C4A 0.027(4) 0.026(4) 0.041(4) 0.007(3) 0.007(3) 0.000(3) C4C 0.043(4) 0.021(3) 0.026(4) -0.001(3) 0.001(3) 0.008(3) C4D 0.043(4) 0.021(3) 0.026(4) -0.001(3) 0.001(3) 0.008(3) C5A 0.034(6) 0.021(6) 0.042(6) 0.004(5) 0.005(5) 0.008(5) C5B 0.024(5) 0.022(5) 0.034(6) 0.009(4) -0.001(4) 0.004(5) C5C 0.047(7) 0.010(5) 0.035(6) 0.009(4) 0.010(5) 0.015(5) C5D 0.031(6) 0.020(5) 0.024(5) 0.005(4) 0.001(4) -0.003(4) C7A 0.033(6) 0.024(6) 0.038(6) 0.006(5) 0.008(5) 0.008(5) C7B 0.044(7) 0.025(6) 0.038(6) 0.011(5) 0.018(5) 0.016(5) C7C 0.032(6) 0.032(6) 0.044(6) 0.012(5) 0.013(5) 0.010(5) C7D 0.032(6) 0.031(6) 0.039(6) 0.019(5) 0.012(5) 0.012(5) C8A 0.027(5) 0.019(5) 0.032(5) 0.010(4) 0.008(4) 0.010(4) C8B 0.020(5) 0.028(6) 0.026(5) 0.006(4) -0.002(4) 0.001(4) C8C 0.040(6) 0.022(6) 0.033(6) 0.006(4) 0.010(5) 0.008(5) C8D 0.029(6) 0.018(5) 0.042(6) 0.017(5) 0.012(5) 0.010(4) C9A 0.035(6) 0.017(5) 0.039(6) 0.011(4) 0.005(5) 0.016(5) C9B 0.031(6) 0.033(6) 0.022(5) 0.004(4) 0.006(4) 0.006(5) C9C 0.024(5) 0.017(5) 0.031(5) 0.001(4) 0.004(4) 0.004(4) C9D 0.036(6) 0.026(6) 0.036(6) 0.019(5) 0.015(5) 0.013(5) C11A 0.034(6) 0.023(5) 0.031(6) 0.002(4) 0.013(5) -0.004(5) C11B 0.031(6) 0.038(6) 0.029(5) 0.012(5) 0.009(5) 0.012(5) C11C 0.031(6) 0.028(6) 0.035(6) 0.002(5) 0.011(5) 0.006(5) C11D 0.032(6) 0.020(5) 0.039(6) -0.001(4) 0.012(5) 0.004(5) C13A 0.027(6) 0.023(5) 0.040(6) 0.012(4) 0.002(5) 0.002(5) C13B 0.029(6) 0.026(6) 0.042(6) 0.007(5) 0.012(5) 0.002(5) C13C 0.032(6) 0.022(5) 0.038(6) 0.005(4) 0.004(5) 0.003(5) C13D 0.037(6) 0.022(5) 0.030(5) 0.005(4) 0.009(5) 0.012(5) C14A 0.028(5) 0.019(5) 0.032(5) 0.006(4) 0.004(4) 0.004(4) C14B 0.033(6) 0.028(6) 0.030(5) 0.013(5) 0.005(5) 0.003(5) C14C 0.037(6) 0.027(6) 0.033(5) 0.008(4) 0.015(5) 0.019(5) C14D 0.040(6) 0.030(6) 0.024(5) 0.006(4) 0.007(5) 0.013(5) C15A 0.045(7) 0.020(5) 0.037(6) 0.011(5) 0.020(5) 0.008(5) C15B 0.026(6) 0.028(6) 0.024(5) -0.003(4) -0.004(4) -0.001(5) C15C 0.028(6) 0.036(6) 0.020(5) 0.003(4) -0.002(4) -0.003(5) C15D 0.037(6) 0.012(5) 0.037(6) 0.005(4) 0.014(5) 0.010(5) C17A 0.050(7) 0.018(5) 0.033(6) -0.005(4) 0.018(5) -0.006(5) C17B 0.029(5) 0.030(6) 0.032(5) 0.018(5) 0.002(4) 0.018(5) C17C 0.018(5) 0.035(6) 0.013(4) 0.012(4) -0.007(4) 0.006(4) C17D 0.036(6) 0.033(6) 0.038(6) 0.010(5) 0.017(5) 0.013(5) C20A 0.045(7) 0.026(6) 0.053(7) 0.010(5) 0.027(6) 0.005(5) C20B 0.030(6) 0.052(8) 0.046(7) 0.024(6) 0.015(5) 0.006(6) C20C 0.052(8) 0.047(8) 0.047(7) 0.009(6) 0.032(6) 0.011(6) C20D 0.050(7) 0.020(6) 0.053(7) 0.004(5) 0.024(6) 0.017(5) C21A 0.074(10) 0.018(6) 0.098(11) 0.014(7) 0.045(9) -0.011(6) C21B 0.062(9) 0.053(8) 0.060(8) 0.014(7) 0.036(7) 0.010(7) C21C 0.073(10) 0.056(9) 0.071(9) 0.011(7) 0.047(8) 0.016(8) C21D 0.079(10) 0.044(8) 0.060(8) 0.009(6) 0.043(8) 0.028(8) C23A 0.036(6) 0.023(6) 0.049(7) 0.010(5) 0.016(5) 0.009(5) C23B 0.049(7) 0.035(7) 0.045(7) 0.016(5) 0.027(6) 0.000(6) C23C 0.040(7) 0.032(7) 0.050(7) -0.008(5) 0.025(6) 0.001(6) C23D 0.074(9) 0.020(6) 0.047(7) 0.014(5) 0.028(6) 0.025(6) C31 0.066(8) 0.029(6) 0.045(7) 0.011(5) 0.022(6) 0.021(6) C32 0.080(10) 0.031(7) 0.052(8) 0.003(6) 0.002(7) 0.005(7) C33 0.078(10) 0.063(10) 0.069(9) 0.036(8) 0.012(8) 0.042(9) C34 0.058(8) 0.024(6) 0.064(8) 0.012(6) 0.006(7) 0.018(6) C35 0.043(7) 0.029(6) 0.048(7) 0.010(5) 0.006(6) 0.006(5) C41 0.045(7) 0.020(6) 0.053(7) 0.011(5) 0.020(6) 0.008(5) C42 0.068(9) 0.046(8) 0.050(7) 0.022(6) 0.028(7) 0.029(7) C43 0.064(9) 0.069(10) 0.069(9) 0.046(8) 0.024(7) 0.040(8) C44 0.053(8) 0.054(8) 0.051(8) 0.015(6) 0.022(6) 0.007(7) C45 0.035(6) 0.044(7) 0.043(7) 0.016(6) 0.013(5) 0.013(6) C51 0.052(7) 0.025(6) 0.055(7) 0.014(5) 0.034(6) 0.011(5) C52 0.096(12) 0.043(8) 0.068(9) 0.038(7) 0.056(9) 0.049(8) C53 0.056(8) 0.040(7) 0.060(8) 0.024(6) 0.018(7) 0.022(6) C54 0.056(8) 0.045(7) 0.044(7) 0.024(6) 0.021(6) 0.027(6) C55 0.043(7) 0.016(5) 0.051(7) 0.008(5) 0.012(6) 0.010(5) C61 0.045(7) 0.032(6) 0.038(6) 0.007(5) 0.001(6) 0.007(6) C62 0.065(9) 0.043(8) 0.057(8) 0.022(7) -0.003(7) 0.003(7) C63 0.046(8) 0.079(11) 0.078(10) 0.030(9) -0.005(7) 0.016(8) C64 0.060(9) 0.039(8) 0.125(13) 0.053(9) 0.044(9) 0.030(7) C65 0.044(7) 0.033(7) 0.058(8) 0.004(6) 0.007(6) 0.013(6) N10A 0.029(5) 0.026(5) 0.042(5) 0.014(4) 0.014(4) 0.008(4) N10B 0.033(5) 0.024(5) 0.021(4) 0.004(3) 0.009(4) 0.004(4) N10C 0.028(5) 0.021(5) 0.044(5) 0.006(4) 0.012(4) -0.004(4) N10D 0.039(5) 0.019(4) 0.042(5) 0.015(4) 0.016(4) 0.007(4) N30 0.045(6) 0.032(5) 0.046(6) 0.016(4) 0.018(5) 0.007(4) N40 0.048(6) 0.036(5) 0.044(5) 0.018(4) 0.030(5) 0.014(5) N50 0.047(6) 0.031(5) 0.047(5) 0.017(4) 0.026(5) 0.023(5) N60 0.035(5) 0.023(5) 0.044(5) 0.016(4) 0.006(4) 0.007(4) O1A 0.051(5) 0.019(4) 0.059(5) 0.009(3) 0.032(4) 0.003(4) O1B 0.038(4) 0.016(3) 0.034(4) -0.004(3) 0.009(3) 0.003(3) O1C 0.030(4) 0.021(4) 0.033(4) -0.005(3) 0.009(3) -0.012(3) O1D 0.047(5) 0.019(4) 0.066(5) 0.011(4) 0.032(4) 0.019(4) O12A 0.038(4) 0.027(4) 0.039(4) 0.008(3) 0.019(3) 0.002(3) O12B 0.038(4) 0.028(4) 0.039(4) 0.007(3) 0.018(3) 0.011(4) O12C 0.040(4) 0.031(4) 0.037(4) 0.008(3) 0.021(3) 0.008(4) O12D 0.045(5) 0.026(4) 0.035(4) 0.009(3) 0.018(4) 0.009(4) O16A 0.051(5) 0.023(4) 0.042(4) 0.005(3) 0.025(4) -0.001(4) O16B 0.037(4) 0.032(4) 0.044(5) -0.005(3) 0.014(4) -0.009(3) O16C 0.043(5) 0.040(5) 0.033(4) -0.004(3) 0.008(3) -0.008(4) O16D 0.050(5) 0.024(4) 0.053(5) 0.009(3) 0.025(4) 0.014(4) O18A 0.050(5) 0.023(4) 0.042(4) -0.001(3) 0.026(4) -0.007(4) O18B 0.046(4) 0.015(3) 0.032(4) -0.008(3) 0.016(3) -0.004(3) O18C 0.027(4) 0.020(4) 0.035(4) 0.001(3) 0.008(3) -0.003(3) O18D 0.041(5) 0.029(4) 0.045(5) -0.005(3) 0.023(4) -0.004(4) O19A 0.035(4) 0.025(4) 0.037(4) 0.004(3) 0.014(3) 0.000(3) O19B 0.039(4) 0.029(4) 0.041(4) 0.011(3) 0.014(4) 0.004(4) O19C 0.041(4) 0.029(4) 0.043(4) 0.007(4) 0.017(4) 0.009(4) O19D 0.044(5) 0.028(4) 0.034(4) 0.003(3) 0.013(4) 0.009(4) O22A 0.035(4) 0.038(5) 0.048(5) 0.015(4) 0.018(4) 0.011(4) O22B 0.047(5) 0.044(5) 0.042(4) 0.008(4) 0.028(4) 0.006(4) O22C 0.039(4) 0.037(5) 0.053(5) 0.004(4) 0.022(4) 0.013(4) O22D 0.044(4) 0.039(5) 0.039(4) 0.019(4) 0.016(4) 0.016(4) Cu1 0.0386(7) 0.0221(7) 0.0380(7) 0.0029(6) 0.0158(6) 0.0010(6) Cu2 0.0339(7) 0.0203(6) 0.0334(7) 0.0030(5) 0.0125(6) 0.0035(5) Cu3 0.0324(7) 0.0208(6) 0.0343(7) 0.0030(5) 0.0122(6) 0.0018(5) Cu4 0.0358(7) 0.0200(6) 0.0376(7) 0.0016(5) 0.0157(6) 0.0015(6) Br6A 0.0621(8) 0.0204(6) 0.0659(8) 0.0028(5) 0.0287(7) 0.0044(6) Br6B 0.0608(8) 0.0200(5) 0.0546(7) 0.0089(5) 0.0245(6) 0.0085(5) Br6C 0.0482(7) 0.0190(5) 0.0648(8) 0.0105(5) 0.0198(6) 0.0079(5) Br6D 0.0548(7) 0.0181(5) 0.0577(7) 0.0079(5) 0.0244(6) 0.0059(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2A O1A 1.353(13) . ? C2A C8A 1.392(15) . ? C2A C3A 1.406(16) . ? C2B O1B 1.308(12) . ? C2B C3B 1.415(17) . ? C2B C8B 1.426(16) . ? C2C O1C 1.325(13) . ? C2C C8C 1.404(16) . ? C2C C3C 1.425(16) . ? C2D O1D 1.322(13) . ? C2D C8D 1.407(16) . ? C2D C3D 1.428(15) . ? C3A C4A 1.380(16) . ? C3A H3A 0.9500 . ? C3B C4B 1.374(15) . ? C3B H3B 0.9500 . ? C3C C4C 1.362(16) . ? C3C H3C 0.9500 . ? C3D C4D 1.390(16) . ? C3D H3D 0.9500 . ? C4B C5B 1.383(16) . ? C4B H4B 0.9500 . ? C4A C5A 1.396(17) . ? C4A H4A 0.9500 . ? C4C C5C 1.384(17) . ? C4C H4C 0.9500 . ? C4D C5D 1.368(16) . ? C4D H4D 0.9500 . ? C5A C7A 1.373(17) . ? C5A Br6A 1.904(11) . ? C5B C7B 1.319(16) . ? C5B Br6B 1.916(11) . ? C5C C7C 1.312(16) . ? C5C Br6C 1.930(11) . ? C5D C7D 1.410(15) . ? C5D Br6D 1.921(10) . ? C7A C8A 1.402(14) . ? C7A H7A 0.9500 . ? C7B C8B 1.450(15) . ? C7B H7B 0.9500 . ? C7C C8C 1.420(16) . ? C7C H7C 0.9500 . ? C7D C8D 1.444(15) . ? C7D H7D 0.9500 . ? C8A C9A 1.444(16) . ? C8B C9B 1.462(15) . ? C8C C9C 1.493(14) . ? C8D C9D 1.403(15) . ? C9A N10A 1.282(13) . ? C9A H9A 0.9500 . ? C9B N10B 1.255(13) . ? C9B H9B 0.9500 . ? C9C N10C 1.242(13) . ? C9C H9C 0.9500 . ? C9D N10D 1.304(14) . ? C9D H9D 0.9500 . ? C11A O12A 1.436(12) . ? C11A N10A 1.445(14) . ? C11A C17A 1.520(15) . ? C11A H11A 1.0000 . ? C11B O12B 1.397(13) . ? C11B N10B 1.443(14) . ? C11B C17B 1.549(14) . ? C11B H11B 1.0000 . ? C11C O12C 1.426(13) . ? C11C N10C 1.442(14) . ? C11C C17C 1.571(13) . ? C11C H11C 1.0000 . ? C11D O12D 1.431(13) . ? C11D N10D 1.440(13) . ? C11D C17D 1.526(15) . ? C11D H11D 1.0000 . ? C13A O12A 1.430(13) . ? C13A C14A 1.499(14) . ? C13A C23A 1.524(16) . ? C13A H13A 1.0000 . ? C13B O12B 1.434(13) . ? C13B C23B 1.477(17) . ? C13B C14B 1.532(13) . ? C13B H13B 1.0000 . ? C13C O12C 1.421(13) . ? C13C C23C 1.515(17) . ? C13C C14C 1.538(14) . ? C13C H13C 1.0000 . ? C13D O12D 1.452(12) . ? C13D C23D 1.514(17) . ? C13D C14D 1.531(15) . ? C13D H13D 1.0000 . ? C14A O19A 1.418(13) . ? C14A C15A 1.522(15) . ? C14A H14A 1.0000 . ? C14B O19B 1.469(13) . ? C14B C15B 1.506(16) . ? C14B H14B 1.0000 . ? C14C O19C 1.451(13) . ? C14C C15C 1.506(15) . ? C14C H14C 1.0000 . ? C14D O19D 1.432(12) . ? C14D C15D 1.514(16) . ? C14D H14D 1.0000 . ? C15A O16A 1.419(13) . ? C15A C17A 1.500(16) . ? C15A H15A 1.0000 . ? C15B O16B 1.436(12) . ? C15B C17B 1.515(16) . ? C15B H15B 1.0000 . ? C15C O16C 1.445(12) . ? C15C C17C 1.458(15) . ? C15C H15C 1.0000 . ? C15D O16D 1.395(13) . ? C15D C17D 1.543(14) . ? C15D H15D 1.0000 . ? C17A O18A 1.414(13) . ? C17A H17A 1.0000 . ? C17B O18B 1.368(13) . ? C17B H17B 1.0000 . ? C17C O18C 1.383(12) . ? C17C H17C 1.0000 . ? C17D O18D 1.406(13) . ? C17D H17D 1.0000 . ? C20A O22A 1.424(14) . ? C20A O19A 1.433(14) . ? C20A C21A 1.526(18) . ? C20A H20A 1.0000 . ? C20B O22B 1.404(15) . ? C20B O19B 1.416(15) . ? C20B C21B 1.459(18) . ? C20B H20B 1.0000 . ? C20C O19C 1.402(15) . ? C20C O22C 1.404(15) . ? C20C C21C 1.494(19) . ? C20C H20C 1.0000 . ? C20D O19D 1.417(15) . ? C20D O22D 1.431(14) . ? C20D C21D 1.516(17) . ? C20D H20D 1.0000 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C21C H21G 0.9800 . ? C21C H21H 0.9800 . ? C21C H21I 0.9800 . ? C21D H21J 0.9800 . ? C21D H21K 0.9800 . ? C21D H21L 0.9800 . ? C23A O22A 1.457(14) . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? C23B O22B 1.406(14) . ? C23B H23C 0.9900 . ? C23B H23D 0.9900 . ? C23C O22C 1.418(14) . ? C23C H23E 0.9900 . ? C23C H23F 0.9900 . ? C23D O22D 1.440(14) . ? C23D H23G 0.9900 . ? C23D H23H 0.9900 . ? C31 N30 1.346(11) . ? C31 C32 1.362(18) . ? C31 H31 0.9500 . ? C32 C33 1.40(2) . ? C32 H32 0.9500 . ? C33 C34 1.340(19) . ? C33 H33 0.9500 . ? C34 C35 1.394(17) . ? C34 H34 0.9500 . ? C35 N30 1.337(11) . ? C35 H35 0.9500 . ? C41 N40 1.360(10) . ? C41 C42 1.367(17) . ? C41 H41 0.9500 . ? C42 C43 1.40(2) . ? C42 H42 0.9500 . ? C43 C44 1.41(2) . ? C43 H43 0.9500 . ? C44 C45 1.360(18) . ? C44 H44 0.9500 . ? C45 N40 1.353(11) . ? C45 H45 0.9500 . ? C51 N50 1.351(10) . ? C51 C52 1.367(18) . ? C51 H51 0.9500 . ? C52 C53 1.40(2) . ? C52 H52 0.9500 . ? C53 C54 1.369(17) . ? C53 H53 0.9500 . ? C54 C55 1.388(16) . ? C54 H54 0.9500 . ? C55 N50 1.322(10) . ? C55 H55 0.9500 . ? C61 N60 1.321(11) . ? C61 C62 1.370(17) . ? C61 H61 0.9500 . ? C62 C63 1.37(2) . ? C62 H62 0.9500 . ? C63 C64 1.41(2) . ? C63 H63 0.9500 . ? C64 C65 1.376(18) . ? C64 H64 0.9500 . ? C65 N60 1.333(11) . ? C65 H65 0.9500 . ? N10A Cu1 1.973(9) . ? N10B Cu2 1.937(8) . ? N10C Cu3 1.955(9) . ? N10D Cu4 1.964(9) . ? N30 Cu1 2.268(9) . ? N40 Cu2 2.310(9) . ? N50 Cu4 2.294(9) . ? N60 Cu3 2.252(8) . ? O1A Cu1 1.869(8) . ? O1B Cu2 1.934(7) . ? O1C Cu3 1.946(7) . ? O1D Cu4 1.881(7) . ? O16A H16A 0.839(10) . ? O16B H16B 0.841(10) . ? O16C H16C 0.841(11) . ? O16D H16D 0.841(11) . ? O18A Cu2 1.923(7) . ? O18A Cu1 1.955(7) . ? O18B Cu2 1.960(7) . ? O18B Cu1 1.963(7) . ? O18C Cu3 1.972(7) . ? O18C Cu4 1.974(7) . ? O18D Cu3 1.908(8) . ? O18D Cu4 1.955(7) . ? Cu1 Cu2 2.9842(17) . ? Cu3 Cu4 2.9920(17) . ? 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 O1A C2A C8A 124.0(10) . . ? O1A C2A C3A 118.8(10) . . ? C8A C2A C3A 117.2(10) . . ? O1B C2B C3B 117.6(11) . . ? O1B C2B C8B 124.0(10) . . ? C3B C2B C8B 118.4(9) . . ? O1C C2C C8C 126.2(10) . . ? O1C C2C C3C 115.0(10) . . ? C8C C2C C3C 118.7(10) . . ? O1D C2D C8D 122.8(9) . . ? O1D C2D C3D 118.0(11) . . ? C8D C2D C3D 119.2(10) . . ? C4A C3A C2A 122.2(11) . . ? C4A C3A H3A 118.9 . . ? C2A C3A H3A 118.9 . . ? C4B C3B C2B 121.1(11) . . ? C4B C3B H3B 119.5 . . ? C2B C3B H3B 119.5 . . ? C4C C3C C2C 118.2(11) . . ? C4C C3C H3C 120.9 . . ? C2C C3C H3C 120.9 . . ? C4D C3D C2D 122.0(11) . . ? C4D C3D H3D 119.0 . . ? C2D C3D H3D 119.0 . . ? C3B C4B C5B 120.0(11) . . ? C3B C4B H4B 120.0 . . ? C5B C4B H4B 120.0 . . ? C3A C4A C5A 119.1(10) . . ? C3A C4A H4A 120.4 . . ? C5A C4A H4A 120.4 . . ? C3C C4C C5C 121.8(11) . . ? C3C C4C H4C 119.1 . . ? C5C C4C H4C 119.1 . . ? C5D C4D C3D 118.9(10) . . ? C5D C4D H4D 120.5 . . ? C3D C4D H4D 120.5 . . ? C7A C5A C4A 120.4(10) . . ? C7A C5A Br6A 120.4(9) . . ? C4A C5A Br6A 119.2(9) . . ? C7B C5B C4B 121.6(10) . . ? C7B C5B Br6B 118.8(9) . . ? C4B C5B Br6B 119.5(8) . . ? C7C C5C C4C 121.9(11) . . ? C7C C5C Br6C 118.7(9) . . ? C4C C5C Br6C 119.4(8) . . ? C4D C5D C7D 122.0(10) . . ? C4D C5D Br6D 119.5(8) . . ? C7D C5D Br6D 118.5(8) . . ? C5A C7A C8A 119.9(11) . . ? C5A C7A H7A 120.1 . . ? C8A C7A H7A 120.1 . . ? C5B C7B C8B 121.5(11) . . ? C5B C7B H7B 119.3 . . ? C8B C7B H7B 119.3 . . ? C5C C7C C8C 119.5(11) . . ? C5C C7C H7C 120.2 . . ? C8C C7C H7C 120.2 . . ? C5D C7D C8D 119.6(10) . . ? C5D C7D H7D 120.2 . . ? C8D C7D H7D 120.2 . . ? C2A C8A C7A 121.2(10) . . ? C2A C8A C9A 123.8(10) . . ? C7A C8A C9A 114.9(10) . . ? C2B C8B C7B 117.3(10) . . ? C2B C8B C9B 124.0(9) . . ? C7B C8B C9B 118.7(10) . . ? C2C C8C C7C 119.8(10) . . ? C2C C8C C9C 122.0(10) . . ? C7C C8C C9C 118.2(10) . . ? C9D C8D C2D 127.2(10) . . ? C9D C8D C7D 114.4(10) . . ? C2D C8D C7D 118.2(10) . . ? N10A C9A C8A 125.2(10) . . ? N10A C9A H9A 117.4 . . ? C8A C9A H9A 117.4 . . ? N10B C9B C8B 124.6(10) . . ? N10B C9B H9B 117.7 . . ? C8B C9B H9B 117.7 . . ? N10C C9C C8C 126.1(10) . . ? N10C C9C H9C 116.9 . . ? C8C C9C H9C 116.9 . . ? N10D C9D C8D 122.5(10) . . ? N10D C9D H9D 118.7 . . ? C8D C9D H9D 118.7 . . ? O12A C11A N10A 112.8(8) . . ? O12A C11A C17A 111.9(9) . . ? N10A C11A C17A 109.1(9) . . ? O12A C11A H11A 107.6 . . ? N10A C11A H11A 107.6 . . ? C17A C11A H11A 107.6 . . ? O12B C11B N10B 114.2(9) . . ? O12B C11B C17B 112.9(8) . . ? N10B C11B C17B 106.1(8) . . ? O12B C11B H11B 107.8 . . ? N10B C11B H11B 107.8 . . ? C17B C11B H11B 107.8 . . ? O12C C11C N10C 113.0(9) . . ? O12C C11C C17C 110.9(8) . . ? N10C C11C C17C 106.5(8) . . ? O12C C11C H11C 108.8 . . ? N10C C11C H11C 108.8 . . ? C17C C11C H11C 108.8 . . ? O12D C11D N10D 112.5(8) . . ? O12D C11D C17D 112.2(9) . . ? N10D C11D C17D 107.3(9) . . ? O12D C11D H11D 108.2 . . ? N10D C11D H11D 108.2 . . ? C17D C11D H11D 108.2 . . ? O12A C13A C14A 112.8(9) . . ? O12A C13A C23A 108.4(8) . . ? C14A C13A C23A 110.9(10) . . ? O12A C13A H13A 108.2 . . ? C14A C13A H13A 108.2 . . ? C23A C13A H13A 108.2 . . ? O12B C13B C23B 112.8(9) . . ? O12B C13B C14B 109.4(9) . . ? C23B C13B C14B 108.9(10) . . ? O12B C13B H13B 108.6 . . ? C23B C13B H13B 108.6 . . ? C14B C13B H13B 108.6 . . ? O12C C13C C23C 111.7(9) . . ? O12C C13C C14C 110.6(9) . . ? C23C C13C C14C 107.2(9) . . ? O12C C13C H13C 109.1 . . ? C23C C13C H13C 109.1 . . ? C14C C13C H13C 109.1 . . ? O12D C13D C23D 107.6(9) . . ? O12D C13D C14D 109.7(8) . . ? C23D C13D C14D 110.5(9) . . ? O12D C13D H13D 109.6 . . ? C23D C13D H13D 109.6 . . ? C14D C13D H13D 109.6 . . ? O19A C14A C13A 109.4(9) . . ? O19A C14A C15A 109.9(8) . . ? C13A C14A C15A 111.6(9) . . ? O19A C14A H14A 108.6 . . ? C13A C14A H14A 108.6 . . ? C15A C14A H14A 108.6 . . ? O19B C14B C15B 109.5(9) . . ? O19B C14B C13B 107.0(8) . . ? C15B C14B C13B 113.0(9) . . ? O19B C14B H14B 109.1 . . ? C15B C14B H14B 109.1 . . ? C13B C14B H14B 109.1 . . ? O19C C14C C15C 111.3(9) . . ? O19C C14C C13C 106.4(9) . . ? C15C C14C C13C 110.8(9) . . ? O19C C14C H14C 109.4 . . ? C15C C14C H14C 109.4 . . ? C13C C14C H14C 109.4 . . ? O19D C14D C15D 109.7(9) . . ? O19D C14D C13D 107.1(8) . . ? C15D C14D C13D 112.3(9) . . ? O19D C14D H14D 109.2 . . ? C15D C14D H14D 109.2 . . ? C13D C14D H14D 109.2 . . ? O16A C15A C17A 111.8(9) . . ? O16A C15A C14A 108.0(8) . . ? C17A C15A C14A 106.5(9) . . ? O16A C15A H15A 110.2 . . ? C17A C15A H15A 110.2 . . ? C14A C15A H15A 110.2 . . ? O16B C15B C14B 107.5(9) . . ? O16B C15B C17B 113.5(9) . . ? C14B C15B C17B 109.6(9) . . ? O16B C15B H15B 108.7 . . ? C14B C15B H15B 108.7 . . ? C17B C15B H15B 108.7 . . ? O16C C15C C17C 114.1(9) . . ? O16C C15C C14C 107.8(8) . . ? C17C C15C C14C 110.8(9) . . ? O16C C15C H15C 108.0 . . ? C17C C15C H15C 108.0 . . ? C14C C15C H15C 108.0 . . ? O16D C15D C14D 110.2(9) . . ? O16D C15D C17D 111.4(9) . . ? C14D C15D C17D 105.0(8) . . ? O16D C15D H15D 110.1 . . ? C14D C15D H15D 110.1 . . ? C17D C15D H15D 110.1 . . ? O18A C17A C15A 114.5(8) . . ? O18A C17A C11A 103.9(9) . . ? C15A C17A C11A 111.4(10) . . ? O18A C17A H17A 109.0 . . ? C15A C17A H17A 109.0 . . ? C11A C17A H17A 109.0 . . ? O18B C17B C15B 115.5(9) . . ? O18B C17B C11B 106.2(8) . . ? C15B C17B C11B 109.3(8) . . ? O18B C17B H17B 108.5 . . ? C15B C17B H17B 108.5 . . ? C11B C17B H17B 108.5 . . ? O18C C17C C15C 117.0(9) . . ? O18C C17C C11C 103.9(7) . . ? C15C C17C C11C 109.8(8) . . ? O18C C17C H17C 108.6 . . ? C15C C17C H17C 108.6 . . ? C11C C17C H17C 108.6 . . ? O18D C17D C11D 106.7(9) . . ? O18D C17D C15D 114.0(9) . . ? C11D C17D C15D 111.4(9) . . ? O18D C17D H17D 108.2 . . ? C11D C17D H17D 108.2 . . ? C15D C17D H17D 108.2 . . ? O22A C20A O19A 111.1(9) . . ? O22A C20A C21A 108.4(10) . . ? O19A C20A C21A 106.5(10) . . ? O22A C20A H20A 110.2 . . ? O19A C20A H20A 110.2 . . ? C21A C20A H20A 110.2 . . ? O22B C20B O19B 114.6(9) . . ? O22B C20B C21B 109.8(10) . . ? O19B C20B C21B 107.5(11) . . ? O22B C20B H20B 108.2 . . ? O19B C20B H20B 108.2 . . ? C21B C20B H20B 108.2 . . ? O19C C20C O22C 112.7(10) . . ? O19C C20C C21C 107.8(11) . . ? O22C C20C C21C 108.8(11) . . ? O19C C20C H20C 109.2 . . ? O22C C20C H20C 109.2 . . ? C21C C20C H20C 109.2 . . ? O19D C20D O22D 112.0(9) . . ? O19D C20D C21D 107.7(10) . . ? O22D C20D C21D 109.4(10) . . ? O19D C20D H20D 109.2 . . ? O22D C20D H20D 109.2 . . ? C21D C20D H20D 109.2 . . ? C20A C21A H21A 109.5 . . ? C20A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C20A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C20B C21B H21D 109.5 . . ? C20B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C20B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C20C C21C H21G 109.5 . . ? C20C C21C H21H 109.5 . . ? H21G C21C H21H 109.5 . . ? C20C C21C H21I 109.5 . . ? H21G C21C H21I 109.5 . . ? H21H C21C H21I 109.5 . . ? C20D C21D H21J 109.5 . . ? C20D C21D H21K 109.5 . . ? H21J C21D H21K 109.5 . . ? C20D C21D H21L 109.5 . . ? H21J C21D H21L 109.5 . . ? H21K C21D H21L 109.5 . . ? O22A C23A C13A 107.1(9) . . ? O22A C23A H23A 110.3 . . ? C13A C23A H23A 110.3 . . ? O22A C23A H23B 110.3 . . ? C13A C23A H23B 110.3 . . ? H23A C23A H23B 108.6 . . ? O22B C23B C13B 110.8(10) . . ? O22B C23B H23C 109.5 . . ? C13B C23B H23C 109.5 . . ? O22B C23B H23D 109.5 . . ? C13B C23B H23D 109.5 . . ? H23C C23B H23D 108.1 . . ? O22C C23C C13C 109.8(10) . . ? O22C C23C H23E 109.7 . . ? C13C C23C H23E 109.7 . . ? O22C C23C H23F 109.7 . . ? C13C C23C H23F 109.7 . . ? H23E C23C H23F 108.2 . . ? O22D C23D C13D 107.9(10) . . ? O22D C23D H23G 110.1 . . ? C13D C23D H23G 110.1 . . ? O22D C23D H23H 110.1 . . ? C13D C23D H23H 110.1 . . ? H23G C23D H23H 108.4 . . ? N30 C31 C32 124.0(11) . . ? N30 C31 H31 118.0 . . ? C32 C31 H31 118.0 . . ? C31 C32 C33 116.4(12) . . ? C31 C32 H32 121.8 . . ? C33 C32 H32 121.8 . . ? C34 C33 C32 122.2(12) . . ? C34 C33 H33 118.9 . . ? C32 C33 H33 118.9 . . ? C33 C34 C35 116.5(11) . . ? C33 C34 H34 121.7 . . ? C35 C34 H34 121.7 . . ? N30 C35 C34 124.0(11) . . ? N30 C35 H35 118.0 . . ? C34 C35 H35 118.0 . . ? N40 C41 C42 123.3(11) . . ? N40 C41 H41 118.4 . . ? C42 C41 H41 118.4 . . ? C41 C42 C43 118.1(12) . . ? C41 C42 H42 121.0 . . ? C43 C42 H42 121.0 . . ? C42 C43 C44 119.7(12) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C45 C44 C43 117.5(12) . . ? C45 C44 H44 121.2 . . ? C43 C44 H44 121.2 . . ? N40 C45 C44 124.2(12) . . ? N40 C45 H45 117.9 . . ? C44 C45 H45 117.9 . . ? N50 C51 C52 120.7(12) . . ? N50 C51 H51 119.6 . . ? C52 C51 H51 119.6 . . ? C51 C52 C53 121.8(12) . . ? C51 C52 H52 119.1 . . ? C53 C52 H52 119.1 . . ? C54 C53 C52 115.3(11) . . ? C54 C53 H53 122.4 . . ? C52 C53 H53 122.4 . . ? C53 C54 C55 121.2(12) . . ? C53 C54 H54 119.4 . . ? C55 C54 H54 119.4 . . ? N50 C55 C54 122.0(10) . . ? N50 C55 H55 119.0 . . ? C54 C55 H55 119.0 . . ? N60 C61 C62 125.0(12) . . ? N60 C61 H61 117.5 . . ? C62 C61 H61 117.5 . . ? C61 C62 C63 118.1(12) . . ? C61 C62 H62 120.9 . . ? C63 C62 H62 120.9 . . ? C62 C63 C64 117.7(13) . . ? C62 C63 H63 121.2 . . ? C64 C63 H63 121.2 . . ? C65 C64 C63 119.5(13) . . ? C65 C64 H64 120.3 . . ? C63 C64 H64 120.3 . . ? N60 C65 C64 121.9(12) . . ? N60 C65 H65 119.1 . . ? C64 C65 H65 119.1 . . ? C9A N10A C11A 124.6(10) . . ? C9A N10A Cu1 125.3(8) . . ? C11A N10A Cu1 110.0(6) . . ? C9B N10B C11B 122.5(9) . . ? C9B N10B Cu2 127.1(8) . . ? C11B N10B Cu2 110.3(6) . . ? C9C N10C C11C 123.3(10) . . ? C9C N10C Cu3 126.4(8) . . ? C11C N10C Cu3 109.9(7) . . ? C9D N10D C11D 123.8(9) . . ? C9D N10D Cu4 125.8(8) . . ? C11D N10D Cu4 110.3(7) . . ? C35 N30 C31 116.8(10) . . ? C35 N30 Cu1 123.5(7) . . ? C31 N30 Cu1 118.8(7) . . ? C45 N40 C41 117.2(10) . . ? C45 N40 Cu2 121.5(7) . . ? C41 N40 Cu2 120.9(7) . . ? C55 N50 C51 118.8(10) . . ? C55 N50 Cu4 119.6(7) . . ? C51 N50 Cu4 121.4(8) . . ? C61 N60 C65 117.8(10) . . ? C61 N60 Cu3 120.7(7) . . ? C65 N60 Cu3 121.1(7) . . ? C2A O1A Cu1 127.3(7) . . ? C2B O1B Cu2 126.3(8) . . ? C2C O1C Cu3 125.1(7) . . ? C2D O1D Cu4 127.0(7) . . ? C13A O12A C11A 107.7(8) . . ? C11B O12B C13B 108.7(8) . . ? C13C O12C C11C 108.0(8) . . ? C11D O12D C13D 107.3(8) . . ? C15A O16A H16A 113(10) . . ? C15B O16B H16B 116(10) . . ? C15C O16C H16C 121(10) . . ? C15D O16D H16D 112(10) . . ? C17A O18A Cu2 147.5(6) . . ? C17A O18A Cu1 109.3(6) . . ? Cu2 O18A Cu1 100.6(3) . . ? C17B O18B Cu2 111.0(6) . . ? C17B O18B Cu1 132.5(7) . . ? Cu2 O18B Cu1 99.1(3) . . ? C17C O18C Cu3 112.8(6) . . ? C17C O18C Cu4 133.5(6) . . ? Cu3 O18C Cu4 98.6(3) . . ? C17D O18D Cu3 150.2(7) . . ? C17D O18D Cu4 108.1(6) . . ? Cu3 O18D Cu4 101.5(4) . . ? C14A O19A C20A 109.5(8) . . ? C20B O19B C14B 110.6(8) . . ? C20C O19C C14C 110.4(9) . . ? C20D O19D C14D 110.2(8) . . ? C20A O22A C23A 111.7(8) . . ? C20B O22B C23B 111.8(9) . . ? C20C O22C C23C 110.3(9) . . ? C20D O22D C23D 111.2(8) . . ? O1A Cu1 O18A 168.5(4) . . ? O1A Cu1 O18B 98.9(3) . . ? O18A Cu1 O18B 79.4(3) . . ? O1A Cu1 N10A 93.7(4) . . ? O18A Cu1 N10A 83.2(3) . . ? O18B Cu1 N10A 152.1(4) . . ? O1A Cu1 N30 97.4(4) . . ? O18A Cu1 N30 94.1(3) . . ? O18B Cu1 N30 98.5(3) . . ? N10A Cu1 N30 104.4(3) . . ? O1A Cu1 Cu2 139.1(3) . . ? O18A Cu1 Cu2 39.3(2) . . ? O18B Cu1 Cu2 40.4(2) . . ? N10A Cu1 Cu2 120.9(3) . . ? N30 Cu1 Cu2 94.5(2) . . ? O18A Cu2 O1B 99.2(3) . . ? O18A Cu2 N10B 159.6(3) . . ? O1B Cu2 N10B 94.0(3) . . ? O18A Cu2 O18B 80.3(3) . . ? O1B Cu2 O18B 169.9(3) . . ? N10B Cu2 O18B 84.0(3) . . ? O18A Cu2 N40 95.7(3) . . ? O1B Cu2 N40 97.4(3) . . ? N10B Cu2 N40 98.0(3) . . ? O18B Cu2 N40 92.7(3) . . ? O18A Cu2 Cu1 40.1(2) . . ? O1B Cu2 Cu1 137.1(2) . . ? N10B Cu2 Cu1 122.1(3) . . ? O18B Cu2 Cu1 40.5(2) . . ? N40 Cu2 Cu1 99.3(2) . . ? O18D Cu3 O1C 98.2(3) . . ? O18D Cu3 N10C 156.7(3) . . ? O1C Cu3 N10C 94.0(3) . . ? O18D Cu3 O18C 80.5(3) . . ? O1C Cu3 O18C 166.8(3) . . ? N10C Cu3 O18C 83.1(3) . . ? O18D Cu3 N60 98.0(4) . . ? O1C Cu3 N60 99.1(3) . . ? N10C Cu3 N60 99.6(4) . . ? O18C Cu3 N60 94.1(3) . . ? O18D Cu3 Cu4 39.8(2) . . ? O1C Cu3 Cu4 136.2(2) . . ? N10C Cu3 Cu4 121.7(3) . . ? O18C Cu3 Cu4 40.7(2) . . ? N60 Cu3 Cu4 98.8(2) . . ? O1D Cu4 O18D 173.2(4) . . ? O1D Cu4 N10D 93.9(4) . . ? O18D Cu4 N10D 84.4(4) . . ? O1D Cu4 O18C 99.5(3) . . ? O18D Cu4 O18C 79.3(3) . . ? N10D Cu4 O18C 151.9(3) . . ? O1D Cu4 N50 94.2(3) . . ? O18D Cu4 N50 92.7(3) . . ? N10D Cu4 N50 104.9(3) . . ? O18C Cu4 N50 98.7(3) . . ? O1D Cu4 Cu3 139.9(2) . . ? O18D Cu4 Cu3 38.7(2) . . ? N10D Cu4 Cu3 120.1(3) . . ? O18C Cu4 Cu3 40.7(2) . . ? N50 Cu4 Cu3 96.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1A C2A C3A C4A 179.4(10) . . . . ? C8A C2A C3A C4A -0.5(17) . . . . ? O1B C2B C3B C4B 179.6(10) . . . . ? C8B C2B C3B C4B -2.3(16) . . . . ? O1C C2C C3C C4C -178.9(9) . . . . ? C8C C2C C3C C4C 4.4(16) . . . . ? O1D C2D C3D C4D 179.9(10) . . . . ? C8D C2D C3D C4D 3.1(17) . . . . ? C2B C3B C4B C5B 0.3(17) . . . . ? C2A C3A C4A C5A 2.2(18) . . . . ? C2C C3C C4C C5C -3.0(16) . . . . ? C2D C3D C4D C5D -1.4(17) . . . . ? C3A C4A C5A C7A -0.9(17) . . . . ? C3A C4A C5A Br6A 177.9(9) . . . . ? C3B C4B C5B C7B -0.5(16) . . . . ? C3B C4B C5B Br6B -176.9(8) . . . . ? C3C C4C C5C C7C 0.9(17) . . . . ? C3C C4C C5C Br6C -177.7(8) . . . . ? C3D C4D C5D C7D 1.6(17) . . . . ? C3D C4D C5D Br6D -178.0(8) . . . . ? C4A C5A C7A C8A -1.9(17) . . . . ? Br6A C5A C7A C8A 179.2(8) . . . . ? C4B C5B C7B C8B 2.6(16) . . . . ? Br6B C5B C7B C8B 179.0(8) . . . . ? C4C C5C C7C C8C -0.3(17) . . . . ? Br6C C5C C7C C8C 178.3(8) . . . . ? C4D C5D C7D C8D -3.4(16) . . . . ? Br6D C5D C7D C8D 176.1(7) . . . . ? O1A C2A C8A C7A 177.7(9) . . . . ? C3A C2A C8A C7A -2.4(16) . . . . ? O1A C2A C8A C9A -6.8(17) . . . . ? C3A C2A C8A C9A 173.1(9) . . . . ? C5A C7A C8A C2A 3.6(16) . . . . ? C5A C7A C8A C9A -172.3(10) . . . . ? O1B C2B C8B C7B -177.9(9) . . . . ? C3B C2B C8B C7B 4.2(15) . . . . ? O1B C2B C8B C9B -0.1(16) . . . . ? C3B C2B C8B C9B -178.0(9) . . . . ? C5B C7B C8B C2B -4.4(16) . . . . ? C5B C7B C8B C9B 177.6(10) . . . . ? O1C C2C C8C C7C 179.9(10) . . . . ? C3C C2C C8C C7C -3.8(17) . . . . ? O1C C2C C8C C9C 0.9(18) . . . . ? C3C C2C C8C C9C 177.2(9) . . . . ? C5C C7C C8C C2C 1.8(17) . . . . ? C5C C7C C8C C9C -179.2(10) . . . . ? O1D C2D C8D C9D -7.1(17) . . . . ? C3D C2D C8D C9D 169.5(10) . . . . ? O1D C2D C8D C7D 178.6(9) . . . . ? C3D C2D C8D C7D -4.8(15) . . . . ? C5D C7D C8D C9D -170.0(9) . . . . ? C5D C7D C8D C2D 5.0(15) . . . . ? C2A C8A C9A N10A 5.8(16) . . . . ? C7A C8A C9A N10A -178.5(10) . . . . ? C2B C8B C9B N10B 0.6(16) . . . . ? C7B C8B C9B N10B 178.4(10) . . . . ? C2C C8C C9C N10C 0.9(17) . . . . ? C7C C8C C9C N10C -178.1(11) . . . . ? C2D C8D C9D N10D 5.2(17) . . . . ? C7D C8D C9D N10D 179.7(10) . . . . ? O12A C13A C14A O19A 179.0(8) . . . . ? C23A C13A C14A O19A 57.2(11) . . . . ? O12A C13A C14A C15A -59.1(11) . . . . ? C23A C13A C14A C15A 179.0(9) . . . . ? O12B C13B C14B O19B -178.2(8) . . . . ? C23B C13B C14B O19B 58.2(12) . . . . ? O12B C13B C14B C15B -57.5(12) . . . . ? C23B C13B C14B C15B 178.8(10) . . . . ? O12C C13C C14C O19C -179.2(8) . . . . ? C23C C13C C14C O19C 58.7(11) . . . . ? O12C C13C C14C C15C -58.0(12) . . . . ? C23C C13C C14C C15C 179.9(10) . . . . ? O12D C13D C14D O19D 176.5(8) . . . . ? C23D C13D C14D O19D 58.0(11) . . . . ? O12D C13D C14D C15D -63.0(11) . . . . ? C23D C13D C14D C15D 178.5(9) . . . . ? O19A C14A C15A O16A -64.7(11) . . . . ? C13A C14A C15A O16A 173.7(8) . . . . ? O19A C14A C15A C17A 175.1(9) . . . . ? C13A C14A C15A C17A 53.5(12) . . . . ? O19B C14B C15B O16B -66.4(11) . . . . ? C13B C14B C15B O16B 174.4(9) . . . . ? O19B C14B C15B C17B 169.8(8) . . . . ? C13B C14B C15B C17B 50.6(11) . . . . ? O19C C14C C15C O16C -64.2(12) . . . . ? C13C C14C C15C O16C 177.6(9) . . . . ? O19C C14C C15C C17C 170.3(8) . . . . ? C13C C14C C15C C17C 52.1(11) . . . . ? O19D C14D C15D O16D -65.4(11) . . . . ? C13D C14D C15D O16D 175.6(8) . . . . ? O19D C14D C15D C17D 174.5(8) . . . . ? C13D C14D C15D C17D 55.6(11) . . . . ? O16A C15A C17A O18A 70.8(13) . . . . ? C14A C15A C17A O18A -171.5(9) . . . . ? O16A C15A C17A C11A -171.7(9) . . . . ? C14A C15A C17A C11A -54.0(12) . . . . ? O12A C11A C17A O18A -176.0(9) . . . . ? N10A C11A C17A O18A -50.4(11) . . . . ? O12A C11A C17A C15A 60.3(12) . . . . ? N10A C11A C17A C15A -174.1(9) . . . . ? O16B C15B C17B O18B 71.7(12) . . . . ? C14B C15B C17B O18B -168.1(8) . . . . ? O16B C15B C17B C11B -168.6(9) . . . . ? C14B C15B C17B C11B -48.4(11) . . . . ? O12B C11B C17B O18B -176.8(8) . . . . ? N10B C11B C17B O18B -51.0(10) . . . . ? O12B C11B C17B C15B 57.9(11) . . . . ? N10B C11B C17B C15B -176.3(8) . . . . ? O16C C15C C17C O18C 68.5(11) . . . . ? C14C C15C C17C O18C -169.6(8) . . . . ? O16C C15C C17C C11C -173.4(8) . . . . ? C14C C15C C17C C11C -51.5(11) . . . . ? O12C C11C C17C O18C -175.5(8) . . . . ? N10C C11C C17C O18C -52.2(10) . . . . ? O12C C11C C17C C15C 58.7(11) . . . . ? N10C C11C C17C C15C -178.1(9) . . . . ? O12D C11D C17D O18D -175.0(8) . . . . ? N10D C11D C17D O18D -50.9(11) . . . . ? O12D C11D C17D C15D 60.0(11) . . . . ? N10D C11D C17D C15D -175.8(9) . . . . ? O16D C15D C17D O18D 66.7(12) . . . . ? C14D C15D C17D O18D -174.1(9) . . . . ? O16D C15D C17D C11D -172.5(9) . . . . ? C14D C15D C17D C11D -53.3(11) . . . . ? O12A C13A C23A O22A -178.3(8) . . . . ? C14A C13A C23A O22A -53.9(11) . . . . ? O12B C13B C23B O22B 179.9(9) . . . . ? C14B C13B C23B O22B -58.5(13) . . . . ? O12C C13C C23C O22C 179.9(9) . . . . ? C14C C13C C23C O22C -58.7(12) . . . . ? O12D C13D C23D O22D -175.7(8) . . . . ? C14D C13D C23D O22D -55.9(11) . . . . ? N30 C31 C32 C33 -2(2) . . . . ? C31 C32 C33 C34 1(3) . . . . ? C32 C33 C34 C35 -1(2) . . . . ? C33 C34 C35 N30 2(2) . . . . ? N40 C41 C42 C43 -1.7(19) . . . . ? C41 C42 C43 C44 0(2) . . . . ? C42 C43 C44 C45 2(2) . . . . ? C43 C44 C45 N40 -1(2) . . . . ? N50 C51 C52 C53 6.1(19) . . . . ? C51 C52 C53 C54 -4.5(19) . . . . ? C52 C53 C54 C55 0.9(19) . . . . ? C53 C54 C55 N50 1.2(19) . . . . ? N60 C61 C62 C63 0(2) . . . . ? C61 C62 C63 C64 0(2) . . . . ? C62 C63 C64 C65 1(2) . . . . ? C63 C64 C65 N60 -2(2) . . . . ? C8A C9A N10A C11A -172.3(9) . . . . ? C8A C9A N10A Cu1 2.7(14) . . . . ? O12A C11A N10A C9A -31.4(15) . . . . ? C17A C11A N10A C9A -156.4(10) . . . . ? O12A C11A N10A Cu1 153.0(7) . . . . ? C17A C11A N10A Cu1 28.0(10) . . . . ? C8B C9B N10B C11B -177.8(9) . . . . ? C8B C9B N10B Cu2 -1.0(15) . . . . ? O12B C11B N10B C9B -21.5(14) . . . . ? C17B C11B N10B C9B -146.5(9) . . . . ? O12B C11B N10B Cu2 161.2(6) . . . . ? C17B C11B N10B Cu2 36.2(9) . . . . ? C8C C9C N10C C11C -176.9(10) . . . . ? C8C C9C N10C Cu3 -4.2(16) . . . . ? O12C C11C N10C C9C -24.4(15) . . . . ? C17C C11C N10C C9C -146.4(10) . . . . ? O12C C11C N10C Cu3 161.9(7) . . . . ? C17C C11C N10C Cu3 39.8(9) . . . . ? C8D C9D N10D C11D -172.6(9) . . . . ? C8D C9D N10D Cu4 3.2(15) . . . . ? O12D C11D N10D C9D -29.8(15) . . . . ? C17D C11D N10D C9D -153.6(10) . . . . ? O12D C11D N10D Cu4 153.9(7) . . . . ? C17D C11D N10D Cu4 30.0(10) . . . . ? C34 C35 N30 C31 -2.7(19) . . . . ? C34 C35 N30 Cu1 -171.4(10) . . . . ? C32 C31 N30 C35 2.9(19) . . . . ? C32 C31 N30 Cu1 172.1(11) . . . . ? C44 C45 N40 C41 -0.8(18) . . . . ? C44 C45 N40 Cu2 -174.7(10) . . . . ? C42 C41 N40 C45 2.3(17) . . . . ? C42 C41 N40 Cu2 176.2(9) . . . . ? C54 C55 N50 C51 0.2(17) . . . . ? C54 C55 N50 Cu4 176.5(9) . . . . ? C52 C51 N50 C55 -3.7(17) . . . . ? C52 C51 N50 Cu4 180.0(8) . . . . ? C62 C61 N60 C65 -1(2) . . . . ? C62 C61 N60 Cu3 -174.1(12) . . . . ? C64 C65 N60 C61 2(2) . . . . ? C64 C65 N60 Cu3 174.7(11) . . . . ? C8A C2A O1A Cu1 -1.0(16) . . . . ? C3A C2A O1A Cu1 179.1(8) . . . . ? C3B C2B O1B Cu2 178.0(7) . . . . ? C8B C2B O1B Cu2 0.1(14) . . . . ? C8C C2C O1C Cu3 0.8(16) . . . . ? C3C C2C O1C Cu3 -175.6(7) . . . . ? C8D C2D O1D Cu4 0.1(15) . . . . ? C3D C2D O1D Cu4 -176.6(8) . . . . ? C14A C13A O12A C11A 60.2(11) . . . . ? C23A C13A O12A C11A -176.6(9) . . . . ? N10A C11A O12A C13A 176.2(9) . . . . ? C17A C11A O12A C13A -60.3(11) . . . . ? N10B C11B O12B C13B 173.6(8) . . . . ? C17B C11B O12B C13B -65.1(11) . . . . ? C23B C13B O12B C11B -175.7(9) . . . . ? C14B C13B O12B C11B 63.0(11) . . . . ? C23C C13C O12C C11C -177.0(9) . . . . ? C14C C13C O12C C11C 63.6(11) . . . . ? N10C C11C O12C C13C 176.8(8) . . . . ? C17C C11C O12C C13C -63.8(11) . . . . ? N10D C11D O12D C13D 176.3(8) . . . . ? C17D C11D O12D C13D -62.6(10) . . . . ? C23D C13D O12D C11D -176.9(9) . . . . ? C14D C13D O12D C11D 62.8(11) . . . . ? C15A C17A O18A Cu2 -33(2) . . . . ? C11A C17A O18A Cu2 -154.5(11) . . . . ? C15A C17A O18A Cu1 171.2(8) . . . . ? C11A C17A O18A Cu1 49.5(10) . . . . ? C15B C17B O18B Cu2 163.3(6) . . . . ? C11B C17B O18B Cu2 42.0(9) . . . . ? C15B C17B O18B Cu1 -71.3(11) . . . . ? C11B C17B O18B Cu1 167.4(7) . . . . ? C15C C17C O18C Cu3 162.2(7) . . . . ? C11C C17C O18C Cu3 40.9(9) . . . . ? C15C C17C O18C Cu4 -69.3(11) . . . . ? C11C C17C O18C Cu4 169.5(7) . . . . ? C11D C17D O18D Cu3 -139.5(13) . . . . ? C15D C17D O18D Cu3 -16(2) . . . . ? C11D C17D O18D Cu4 47.0(9) . . . . ? C15D C17D O18D Cu4 170.4(7) . . . . ? C13A C14A O19A C20A -59.9(11) . . . . ? C15A C14A O19A C20A 177.2(9) . . . . ? O22A C20A O19A C14A 63.0(12) . . . . ? C21A C20A O19A C14A -179.1(10) . . . . ? O22B C20B O19B C14B 57.0(12) . . . . ? C21B C20B O19B C14B 179.4(9) . . . . ? C15B C14B O19B C20B -179.6(8) . . . . ? C13B C14B O19B C20B -56.8(11) . . . . ? O22C C20C O19C C14C 62.7(13) . . . . ? C21C C20C O19C C14C -177.3(10) . . . . ? C15C C14C O19C C20C 178.3(9) . . . . ? C13C C14C O19C C20C -60.8(12) . . . . ? O22D C20D O19D C14D 63.2(12) . . . . ? C21D C20D O19D C14D -176.4(9) . . . . ? C15D C14D O19D C20D 177.8(9) . . . . ? C13D C14D O19D C20D -60.1(11) . . . . ? O19A C20A O22A C23A -62.1(12) . . . . ? C21A C20A O22A C23A -178.9(10) . . . . ? C13A C23A O22A C20A 56.3(12) . . . . ? O19B C20B O22B C23B -55.7(14) . . . . ? C21B C20B O22B C23B -176.8(11) . . . . ? C13B C23B O22B C20B 56.0(14) . . . . ? O19C C20C O22C C23C -60.5(14) . . . . ? C21C C20C O22C C23C 180.0(12) . . . . ? C13C C23C O22C C20C 58.6(13) . . . . ? O19D C20D O22D C23D -61.1(12) . . . . ? C21D C20D O22D C23D 179.5(11) . . . . ? C13D C23D O22D C20D 56.3(12) . . . . ? C2A O1A Cu1 O18A 81(2) . . . . ? C2A O1A Cu1 O18B 161.7(9) . . . . ? C2A O1A Cu1 N10A 6.6(9) . . . . ? C2A O1A Cu1 N30 -98.4(9) . . . . ? C2A O1A Cu1 Cu2 156.0(7) . . . . ? C17A O18A Cu1 O1A -104.0(18) . . . . ? Cu2 O18A Cu1 O1A 88.8(18) . . . . ? C17A O18A Cu1 O18B 173.0(8) . . . . ? Cu2 O18A Cu1 O18B 5.9(4) . . . . ? C17A O18A Cu1 N10A -28.9(8) . . . . ? Cu2 O18A Cu1 N10A 163.9(4) . . . . ? C17A O18A Cu1 N30 75.2(8) . . . . ? Cu2 O18A Cu1 N30 -92.0(4) . . . . ? C17A O18A Cu1 Cu2 167.2(10) . . . . ? C17B O18B Cu1 O1A 56.2(9) . . . . ? Cu2 O18B Cu1 O1A -174.2(4) . . . . ? C17B O18B Cu1 O18A -135.4(9) . . . . ? Cu2 O18B Cu1 O18A -5.7(4) . . . . ? C17B O18B Cu1 N10A 172.2(8) . . . . ? Cu2 O18B Cu1 N10A -58.2(9) . . . . ? C17B O18B Cu1 N30 -42.7(9) . . . . ? Cu2 O18B Cu1 N30 86.9(4) . . . . ? C17B O18B Cu1 Cu2 -129.6(10) . . . . ? C9A N10A Cu1 O1A -7.5(9) . . . . ? C11A N10A Cu1 O1A 168.2(7) . . . . ? C9A N10A Cu1 O18A -176.3(9) . . . . ? C11A N10A Cu1 O18A -0.7(7) . . . . ? C9A N10A Cu1 O18B -124.6(9) . . . . ? C11A N10A Cu1 O18B 51.0(11) . . . . ? C9A N10A Cu1 N30 91.1(9) . . . . ? C11A N10A Cu1 N30 -93.2(7) . . . . ? C9A N10A Cu1 Cu2 -164.6(7) . . . . ? C11A N10A Cu1 Cu2 11.1(8) . . . . ? C35 N30 Cu1 O1A -153.0(10) . . . . ? C31 N30 Cu1 O1A 38.4(9) . . . . ? C35 N30 Cu1 O18A 27.1(10) . . . . ? C31 N30 Cu1 O18A -141.4(9) . . . . ? C35 N30 Cu1 O18B -52.8(10) . . . . ? C31 N30 Cu1 O18B 138.7(9) . . . . ? C35 N30 Cu1 N10A 111.2(10) . . . . ? C31 N30 Cu1 N10A -57.3(9) . . . . ? C35 N30 Cu1 Cu2 -12.3(10) . . . . ? C31 N30 Cu1 Cu2 179.2(9) . . . . ? C17A O18A Cu2 O1B 6.9(15) . . . . ? Cu1 O18A Cu2 O1B 163.9(4) . . . . ? C17A O18A Cu2 N10B -122.6(15) . . . . ? Cu1 O18A Cu2 N10B 34.4(12) . . . . ? C17A O18A Cu2 O18B -162.9(15) . . . . ? Cu1 O18A Cu2 O18B -5.9(4) . . . . ? C17A O18A Cu2 N40 105.3(15) . . . . ? Cu1 O18A Cu2 N40 -97.6(4) . . . . ? C17A O18A Cu2 Cu1 -157.0(17) . . . . ? C2B O1B Cu2 O18A -164.6(8) . . . . ? C2B O1B Cu2 N10B -0.3(8) . . . . ? C2B O1B Cu2 O18B -78.6(19) . . . . ? C2B O1B Cu2 N40 98.4(8) . . . . ? C2B O1B Cu2 Cu1 -149.4(7) . . . . ? C9B N10B Cu2 O18A 131.0(11) . . . . ? C11B N10B Cu2 O18A -51.9(13) . . . . ? C9B N10B Cu2 O1B 0.7(9) . . . . ? C11B N10B Cu2 O1B 177.9(6) . . . . ? C9B N10B Cu2 O18B 170.8(9) . . . . ? C11B N10B Cu2 O18B -12.0(6) . . . . ? C9B N10B Cu2 N40 -97.3(9) . . . . ? C11B N10B Cu2 N40 79.9(7) . . . . ? C9B N10B Cu2 Cu1 156.4(8) . . . . ? C11B N10B Cu2 Cu1 -26.4(7) . . . . ? C17B O18B Cu2 O18A 148.3(7) . . . . ? Cu1 O18B Cu2 O18A 5.8(4) . . . . ? C17B O18B Cu2 O1B 60.6(19) . . . . ? Cu1 O18B Cu2 O1B -81.9(18) . . . . ? C17B O18B Cu2 N10B -18.5(6) . . . . ? Cu1 O18B Cu2 N10B -161.1(4) . . . . ? C17B O18B Cu2 N40 -116.4(6) . . . . ? Cu1 O18B Cu2 N40 101.1(4) . . . . ? C17B O18B Cu2 Cu1 142.5(8) . . . . ? C45 N40 Cu2 O18A -144.8(9) . . . . ? C41 N40 Cu2 O18A 41.6(9) . . . . ? C45 N40 Cu2 O1B -44.7(9) . . . . ? C41 N40 Cu2 O1B 141.6(8) . . . . ? C45 N40 Cu2 N10B 50.4(9) . . . . ? C41 N40 Cu2 N10B -123.2(9) . . . . ? C45 N40 Cu2 O18B 134.7(9) . . . . ? C41 N40 Cu2 O18B -38.9(9) . . . . ? C45 N40 Cu2 Cu1 174.9(8) . . . . ? C41 N40 Cu2 Cu1 1.3(9) . . . . ? O1A Cu1 Cu2 O18A -162.3(6) . . . . ? O18B Cu1 Cu2 O18A -171.1(6) . . . . ? N10A Cu1 Cu2 O18A -18.7(5) . . . . ? N30 Cu1 Cu2 O18A 91.1(5) . . . . ? O1A Cu1 Cu2 O1B 174.1(6) . . . . ? O18A Cu1 Cu2 O1B -23.7(5) . . . . ? O18B Cu1 Cu2 O1B 165.3(5) . . . . ? N10A Cu1 Cu2 O1B -42.3(5) . . . . ? N30 Cu1 Cu2 O1B 67.4(4) . . . . ? O1A Cu1 Cu2 N10B 31.2(5) . . . . ? O18A Cu1 Cu2 N10B -166.5(5) . . . . ? O18B Cu1 Cu2 N10B 22.4(5) . . . . ? N10A Cu1 Cu2 N10B 174.8(4) . . . . ? N30 Cu1 Cu2 N10B -75.5(4) . . . . ? O1A Cu1 Cu2 O18B 8.8(5) . . . . ? O18A Cu1 Cu2 O18B 171.1(6) . . . . ? N10A Cu1 Cu2 O18B 152.4(5) . . . . ? N30 Cu1 Cu2 O18B -97.9(4) . . . . ? O1A Cu1 Cu2 N40 -74.4(5) . . . . ? O18A Cu1 Cu2 N40 87.8(5) . . . . ? O18B Cu1 Cu2 N40 -83.2(4) . . . . ? N10A Cu1 Cu2 N40 69.2(4) . . . . ? N30 Cu1 Cu2 N40 178.9(4) . . . . ? C17D O18D Cu3 O1C -8.3(16) . . . . ? Cu4 O18D Cu3 O1C 165.3(4) . . . . ? C17D O18D Cu3 N10C -129.0(14) . . . . ? Cu4 O18D Cu3 N10C 44.6(11) . . . . ? C17D O18D Cu3 O18C -175.0(16) . . . . ? Cu4 O18D Cu3 O18C -1.4(4) . . . . ? C17D O18D Cu3 N60 92.2(16) . . . . ? Cu4 O18D Cu3 N60 -94.2(4) . . . . ? C17D O18D Cu3 Cu4 -173.6(18) . . . . ? C2C O1C Cu3 O18D -162.8(8) . . . . ? C2C O1C Cu3 N10C -2.7(9) . . . . ? C2C O1C Cu3 O18C -79.6(16) . . . . ? C2C O1C Cu3 N60 97.6(8) . . . . ? C2C O1C Cu3 Cu4 -149.3(7) . . . . ? C9C N10C Cu3 O18D 125.9(10) . . . . ? C11C N10C Cu3 O18D -60.5(13) . . . . ? C9C N10C Cu3 O1C 4.4(10) . . . . ? C11C N10C Cu3 O1C 178.0(7) . . . . ? C9C N10C Cu3 O18C 171.5(10) . . . . ? C11C N10C Cu3 O18C -15.0(7) . . . . ? C9C N10C Cu3 N60 -95.5(9) . . . . ? C11C N10C Cu3 N60 78.0(7) . . . . ? C9C N10C Cu3 Cu4 157.8(8) . . . . ? C11C N10C Cu3 Cu4 -28.7(8) . . . . ? C17C O18C Cu3 O18D 146.4(6) . . . . ? Cu4 O18C Cu3 O18D 1.3(4) . . . . ? C17C O18C Cu3 O1C 61.1(15) . . . . ? Cu4 O18C Cu3 O1C -83.9(14) . . . . ? C17C O18C Cu3 N10C -17.0(6) . . . . ? Cu4 O18C Cu3 N10C -162.0(4) . . . . ? C17C O18C Cu3 N60 -116.1(6) . . . . ? Cu4 O18C Cu3 N60 98.8(3) . . . . ? C17C O18C Cu3 Cu4 145.0(8) . . . . ? C61 N60 Cu3 O18D -139.3(10) . . . . ? C65 N60 Cu3 O18D 48.1(10) . . . . ? C61 N60 Cu3 O1C -39.7(10) . . . . ? C65 N60 Cu3 O1C 147.8(10) . . . . ? C61 N60 Cu3 N10C 56.0(10) . . . . ? C65 N60 Cu3 N10C -116.6(10) . . . . ? C61 N60 Cu3 O18C 139.7(10) . . . . ? C65 N60 Cu3 O18C -32.9(10) . . . . ? C61 N60 Cu3 Cu4 -179.6(9) . . . . ? C65 N60 Cu3 Cu4 7.9(10) . . . . ? C2D O1D Cu4 O18D 81(3) . . . . ? C2D O1D Cu4 N10D 5.4(9) . . . . ? C2D O1D Cu4 O18C 160.6(9) . . . . ? C2D O1D Cu4 N50 -99.9(9) . . . . ? C2D O1D Cu4 Cu3 155.0(7) . . . . ? C17D O18D Cu4 O1D -101(3) . . . . ? Cu3 O18D Cu4 O1D 82(3) . . . . ? C17D O18D Cu4 N10D -25.0(7) . . . . ? Cu3 O18D Cu4 N10D 158.3(4) . . . . ? C17D O18D Cu4 O18C 178.0(7) . . . . ? Cu3 O18D Cu4 O18C 1.4(4) . . . . ? C17D O18D Cu4 N50 79.7(7) . . . . ? Cu3 O18D Cu4 N50 -96.9(4) . . . . ? C17D O18D Cu4 Cu3 176.7(9) . . . . ? C9D N10D Cu4 O1D -7.1(9) . . . . ? C11D N10D Cu4 O1D 169.2(7) . . . . ? C9D N10D Cu4 O18D 179.5(9) . . . . ? C11D N10D Cu4 O18D -4.2(7) . . . . ? C9D N10D Cu4 O18C -125.9(9) . . . . ? C11D N10D Cu4 O18C 50.4(11) . . . . ? C9D N10D Cu4 N50 88.3(9) . . . . ? C11D N10D Cu4 N50 -95.4(7) . . . . ? C9D N10D Cu4 Cu3 -165.0(8) . . . . ? C11D N10D Cu4 Cu3 11.3(8) . . . . ? C17C O18C Cu4 O1D 52.3(9) . . . . ? Cu3 O18C Cu4 O1D -174.5(3) . . . . ? C17C O18C Cu4 O18D -134.6(9) . . . . ? Cu3 O18C Cu4 O18D -1.3(4) . . . . ? C17C O18C Cu4 N10D 169.8(9) . . . . ? Cu3 O18C Cu4 N10D -57.0(8) . . . . ? C17C O18C Cu4 N50 -43.5(9) . . . . ? Cu3 O18C Cu4 N50 89.8(3) . . . . ? C17C O18C Cu4 Cu3 -133.2(10) . . . . ? C55 N50 Cu4 O1D 39.4(9) . . . . ? C51 N50 Cu4 O1D -144.4(8) . . . . ? C55 N50 Cu4 O18D -140.7(8) . . . . ? C51 N50 Cu4 O18D 35.6(9) . . . . ? C55 N50 Cu4 N10D -55.8(9) . . . . ? C51 N50 Cu4 N10D 120.4(8) . . . . ? C55 N50 Cu4 O18C 139.7(8) . . . . ? C51 N50 Cu4 O18C -44.0(9) . . . . ? C55 N50 Cu4 Cu3 -179.3(8) . . . . ? C51 N50 Cu4 Cu3 -3.1(8) . . . . ? O18D Cu3 Cu4 O1D -169.4(6) . . . . ? O1C Cu3 Cu4 O1D 169.3(6) . . . . ? N10C Cu3 Cu4 O1D 29.6(5) . . . . ? O18C Cu3 Cu4 O1D 8.5(5) . . . . ? N60 Cu3 Cu4 O1D -77.5(5) . . . . ? O1C Cu3 Cu4 O18D -21.2(5) . . . . ? N10C Cu3 Cu4 O18D -161.0(5) . . . . ? O18C Cu3 Cu4 O18D 177.9(6) . . . . ? N60 Cu3 Cu4 O18D 92.0(5) . . . . ? O18D Cu3 Cu4 N10D -25.1(5) . . . . ? O1C Cu3 Cu4 N10D -46.3(5) . . . . ? N10C Cu3 Cu4 N10D 173.9(4) . . . . ? O18C Cu3 Cu4 N10D 152.8(5) . . . . ? N60 Cu3 Cu4 N10D 66.9(4) . . . . ? O18D Cu3 Cu4 O18C -177.9(6) . . . . ? O1C Cu3 Cu4 O18C 160.8(5) . . . . ? N10C Cu3 Cu4 O18C 21.1(5) . . . . ? N60 Cu3 Cu4 O18C -86.0(4) . . . . ? O18D Cu3 Cu4 N50 86.2(5) . . . . ? O1C Cu3 Cu4 N50 65.0(4) . . . . ? N10C Cu3 Cu4 N50 -74.7(4) . . . . ? O18C Cu3 Cu4 N50 -95.8(4) . . . . ? N60 Cu3 Cu4 N50 178.2(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O16A H16A O1B 0.839(10) 1.96(5) 2.760(10) 159(13) . O16B H16B O1A 0.841(10) 1.89(4) 2.705(12) 164(14) . O16C H16C O1D 0.841(11) 1.89(5) 2.694(11) 159(14) . O16D H16D O1C 0.841(11) 1.96(5) 2.762(11) 159(13) . _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.886 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.109 #Compound 1a data_gr3_m _database_code_CSD 210436 _audit_creation_date 'May 25 07:56:53 2003' _audit_creation_method 'PLATON option' _audit_update_record ; ? ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Cu2 N4 O12' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C52 H44 Cu2 N4 O12' # Pyridine was treated as solvent. _chemical_formula_weight 1044.01 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' Cu Cu 0.3201 1.2651 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 11.143(9) _cell_length_b 17.542(2) _cell_length_c 13.495(6) _cell_angle_alpha 90 _cell_angle_beta 100.318(15) _cell_angle_gamma 90 _cell_volume 2595(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5570 _cell_measurement_theta_min 1.53 _cell_measurement_theta_max 21.96 _cell_special_details ; ? ; _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.167 _exptl_crystal_size_mid 0.313 _exptl_crystal_size_min 0.121 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 0.883 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # cylinder 'cylindrical' # empirical 'empirical from intensities' # gaussian 'Gaussian from crystal shape' # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # refdelf 'refined from delta-F' # sphere 'spherical' _exptl_absorpt_correction_type empirical # Example: '(North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.7139 _exptl_absorpt_correction_T_max 0.7154 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 7885 _diffrn_reflns_av_R_equivalents 0.176 _diffrn_reflns_av_sigmaI/netI 0.075 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 14 _diffrn_reflns_limit_l_max -14 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 22 _diffrn_reflns_theta_full 22 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 7885 # number of observed reflections (> n sig(I)) _reflns_number_gt 5570 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997) and CAMERON (Watkin et al., 1996)' _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _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^)+(0.1534P)^2^+0.0248P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # (mixed) SHELXL _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.048(4) # Permitted for _chemical_absolute_configuration: # Absolute configuration details # rm = Det. by chiral ref. mol. with known abs.conf # ad = Det. by anomalous dispersion # rmad = Det. by 'rm' and 'ad' # syn = Det. with reference to synthesis # unk = Unknown/Arbitrary _chemical_absolute_configuration ? _refine_ls_number_reflns 5570 _refine_ls_number_parameters 575 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.176 _refine_ls_R_factor_gt 0.075 _refine_ls_wR_factor_ref 0.2 _refine_ls_wR_factor_gt 0.156 _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_restrained_S_all 0.884 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.003 _refine_diff_density_max 0.605 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.084 #=============================================================================== #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 0 '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 0.006 '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' 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 1.0775(2) 0.64929(13) 0.74532(19) 0.0552(9) Uani 1 1 d . . . Cu2 Cu 0.9101(2) 0.78246(13) 0.76190(18) 0.0522(8) Uani 1 1 d . . . O5 O 0.9596(12) 0.4983(8) 0.9388(9) 0.049(4) Uani 1 1 d . . . O8 O 0.8029(12) 0.4578(8) 1.1531(8) 0.062(4) Uani 1 1 d . . . O7 O 0.7690(13) 0.5870(8) 1.1071(9) 0.055(4) Uani 1 1 d . . . O1 O 0.9780(13) 0.6932(8) 0.8444(9) 0.050(4) Uani 1 1 d . . . O26 O 1.2525(13) 0.9754(8) 0.4023(9) 0.072(4) Uani 1 1 d . . . O3 O 1.1489(13) 0.5979(9) 0.6432(10) 0.049(4) Uani 1 1 d . . . O11 O 1.2548(13) 0.8416(9) 0.4266(10) 0.064(5) Uani 1 1 d . . . O2 O 1.0066(11) 0.7355(8) 0.6687(8) 0.039(4) Uani 1 1 d . . . O9 O 1.1294(14) 0.7072(7) 0.4883(9) 0.071(4) Uani 1 1 d . . . H9 H 1.1362 0.6721 0.5291 0.106 Uiso 1 1 calc R . . N3 N 1.0697(13) 0.5539(11) 0.8168(11) 0.040(5) Uani 1 1 d . . . O10 O 1.0348(12) 0.9299(9) 0.5689(10) 0.057(5) Uani 1 1 d . . . O6 O 0.7761(12) 0.7069(7) 0.9637(10) 0.070(4) Uani 1 1 d . . . H6 H 0.7980 0.7394 0.9271 0.105 Uiso 1 1 calc R . . N4 N 0.9398(14) 0.8793(12) 0.7034(12) 0.049(5) Uani 1 1 d . . . C11 C 1.0085(17) 0.5666(13) 0.9095(14) 0.053(6) Uani 1 1 d . . . H11 H 1.0722 0.5830 0.9652 0.064 Uiso 1 1 calc R . . C29 C 1.1312(18) 0.7771(15) 0.5395(16) 0.052(6) Uani 1 1 d . . . H29 H 1.2046 0.7773 0.5919 0.062 Uiso 1 1 calc R . . C41 C 0.686(2) 1.0005(17) 0.9475(17) 0.073(8) Uani 1 1 d . . . H41 H 0.6399 1.0117 0.9966 0.088 Uiso 1 1 calc R . . C2 C 0.8627(16) 0.6481(14) 0.9796(13) 0.043(6) Uani 1 1 d . . . H2 H 0.9283 0.6668 1.0322 0.052 Uiso 1 1 calc R . . C9 C 0.9143(17) 0.5145(11) 1.0333(13) 0.049(5) Uani 1 1 d . . . C1 C 0.9260(14) 0.6303(11) 0.8836(13) 0.037(5) Uani 1 1 d . . . H1 H 0.8608 0.6122 0.8302 0.044 Uiso 1 1 calc R . . C36 C 1.1407(17) 0.9223(11) 0.5211(14) 0.053(5) Uani 1 1 d . . . H36 H 1.2136 0.9250 0.5737 0.063 Uiso 1 1 calc R . . O4 O 0.8397(13) 0.8338(10) 0.8668(11) 0.056(4) Uani 1 1 d . . . C47 C 0.7674(17) 1.0398(14) 0.7968(15) 0.051(7) Uani 1 1 d . . . C28 C 1.0237(14) 0.7910(13) 0.5914(12) 0.044(5) Uani 1 1 d . . . H28 H 0.9497 0.7909 0.5398 0.053 Uiso 1 1 calc R . . C3 C 0.8188(16) 0.5795(14) 1.0193(14) 0.043(6) Uani 1 1 d . . . H3 H 0.7518 0.5616 0.9674 0.052 Uiso 1 1 calc R . . C35 C 1.147(2) 0.9864(14) 0.4483(16) 0.072(8) Uani 1 1 d . . . H35A H 1.0734 0.9868 0.3970 0.086 Uiso 1 1 calc R . . H35B H 1.1522 1.0348 0.4835 0.086 Uiso 1 1 calc R . . C40 C 0.7352(17) 0.9267(16) 0.9465(15) 0.061(7) Uani 1 1 d . . . H40 H 0.7264 0.8921 0.9969 0.073 Uiso 1 1 calc R . . C30 C 1.1406(17) 0.8468(13) 0.4703(16) 0.048(6) Uani 1 1 d . . . H30 H 1.0708 0.8453 0.4147 0.057 Uiso 1 1 calc R . . C13 C 1.1655(17) 0.4674(13) 0.7091(15) 0.037(5) Uani 1 1 d . . . C8 C 0.8582(17) 0.4411(12) 1.0631(13) 0.042(6) Uani 1 1 d . . . H8A H 0.7962 0.4231 1.0082 0.051 Uiso 1 1 calc R . . H8B H 0.9203 0.4020 1.0787 0.051 Uiso 1 1 calc R . . C31 C 1.2565(18) 0.9043(15) 0.3587(15) 0.053(6) Uani 1 1 d . . . H31 H 1.1841 0.8998 0.3058 0.063 Uiso 1 1 calc R . . C19 C 1.2669(19) 0.3736(14) 0.6169(17) 0.052(6) Uani 1 1 d . . . C5 C 0.667(2) 0.5321(14) 1.2348(16) 0.071(7) Uani 1 1 d . . . H5A H 0.7342 0.5384 1.2908 0.085 Uiso 1 1 calc R . . H5B H 0.6196 0.5788 1.2288 0.085 Uiso 1 1 calc R . . C12 C 1.1021(17) 0.4874(16) 0.7948(14) 0.051(7) Uani 1 1 d . . . H12 H 1.0849 0.4476 0.8355 0.061 Uiso 1 1 calc R . . C4 C 0.7198(17) 0.5217(14) 1.1385(16) 0.053(7) Uani 1 1 d . . . H4 H 0.6518 0.5072 1.0852 0.064 Uiso 1 1 calc R . . C18 C 1.310(2) 0.2996(18) 0.6030(18) 0.081(8) Uani 1 1 d . . . H18 H 1.3474 0.2891 0.5480 0.097 Uiso 1 1 calc R . . C46 C 0.782(2) 1.0997(15) 0.7275(17) 0.061(7) Uani 1 1 d . . . H46 H 0.8260 1.0904 0.6764 0.073 Uiso 1 1 calc R . . C32 C 1.3669(18) 0.8986(14) 0.3085(14) 0.064(6) Uani 1 1 d . . . H32A H 1.4389 0.9060 0.3598 0.076 Uiso 1 1 calc R . . H32B H 1.3704 0.8471 0.2832 0.076 Uiso 1 1 calc R . . C17 C 1.298(3) 0.2449(17) 0.668(2) 0.111(11) Uani 1 1 d . . . H17 H 1.3300 0.1968 0.6597 0.134 Uiso 1 1 calc R . . C49 C 0.897(2) 0.9461(13) 0.7215(15) 0.053(6) Uani 1 1 d . . . H49 H 0.9195 0.9875 0.6857 0.064 Uiso 1 1 calc R . . C21 C 1.246(2) 0.5024(13) 0.5587(14) 0.063(8) Uani 1 1 d . . . H21 H 1.2591 0.5383 0.5112 0.076 Uiso 1 1 calc R . . C14 C 1.206(2) 0.3926(14) 0.6979(14) 0.053(6) Uani 1 1 d . . . C7 C 0.527(2) 0.4898(16) 1.3523(15) 0.076(8) Uani 1 1 d . . . H7A H 0.5889 0.4996 1.4098 0.113 Uiso 1 1 calc R . . H7B H 0.4763 0.4484 1.3671 0.113 Uiso 1 1 calc R . . H7C H 0.4774 0.5346 1.3366 0.113 Uiso 1 1 calc R . . C37 C 1.0351(17) 0.8693(10) 0.6409(11) 0.040(5) Uani 1 1 d . . . C42 C 0.702(2) 1.0595(14) 0.8778(16) 0.057(7) Uani 1 1 d . . . C6 C 0.588(2) 0.4681(14) 1.2594(16) 0.063(7) Uani 1 1 d . . . H6A H 0.6365 0.4224 1.2749 0.075 Uiso 1 1 calc R . . H6B H 0.5247 0.4574 1.2015 0.075 Uiso 1 1 calc R . . C20 C 1.2845(19) 0.4321(13) 0.5473(15) 0.049(6) Uani 1 1 d . . . H20 H 1.3233 0.4208 0.4936 0.059 Uiso 1 1 calc R . . C15 C 1.194(3) 0.3313(16) 0.7668(19) 0.080(8) Uani 1 1 d . . . H15 H 1.1568 0.3403 0.8222 0.097 Uiso 1 1 calc R . . C33 C 1.375(2) 0.9524(17) 0.2235(17) 0.090(10) Uani 1 1 d . . . H33A H 1.3004 0.9479 0.1743 0.108 Uiso 1 1 calc R . . H33B H 1.3782 1.0040 0.2498 0.108 Uiso 1 1 calc R . . C45 C 0.732(2) 1.1707(14) 0.7354(18) 0.081(8) Uani 1 1 d . . . H45 H 0.7398 1.2084 0.6886 0.097 Uiso 1 1 calc R . . C22 C 1.184(2) 0.5287(16) 0.6394(15) 0.054(7) Uani 1 1 d . . . C43 C 0.650(2) 1.1310(13) 0.8829(18) 0.079(8) Uani 1 1 d . . . H43 H 0.6033 1.1408 0.9320 0.095 Uiso 1 1 calc R . . C16 C 1.238(3) 0.258(2) 0.751(2) 0.125(14) Uani 1 1 d . . . H16 H 1.2284 0.2178 0.7948 0.150 Uiso 1 1 calc R . . C44 C 0.667(3) 1.1866(18) 0.817(2) 0.105(10) Uani 1 1 d . . . H44 H 0.6366 1.2352 0.8241 0.125 Uiso 1 1 calc R . . C34 C 1.478(2) 0.942(2) 0.171(2) 0.119(12) Uani 1 1 d . . . H34A H 1.5520 0.9386 0.2196 0.178 Uiso 1 1 calc R . . H34B H 1.4825 0.9851 0.1278 0.178 Uiso 1 1 calc R . . H34C H 1.4664 0.8964 0.1318 0.178 Uiso 1 1 calc R . . N2 N 0.7185(14) 0.7383(11) 0.6820(12) 0.057(5) Uiso 1 1 d . . . N1 N 1.2640(15) 0.6959(11) 0.8229(13) 0.064(5) Uiso 1 1 d . . . C23 C 0.7035(16) 0.6711(10) 0.6346(12) 0.045(5) Uiso 1 1 d . . . C25 C 0.492(2) 0.6953(15) 0.5727(18) 0.089(8) Uiso 1 1 d . . . C50 C 1.367(2) 0.6534(18) 0.8193(18) 0.087(8) Uiso 1 1 d . . . C51 C 1.483(2) 0.6846(13) 0.8648(16) 0.075(7) Uiso 1 1 d . . . C52 C 1.493(2) 0.7494(14) 0.9258(17) 0.084(8) Uiso 1 1 d . . . C24 C 0.591(2) 0.6458(15) 0.5833(15) 0.072(6) Uiso 1 1 d . . . C27 C 0.6229(18) 0.7847(15) 0.6755(14) 0.057(6) Uiso 1 1 d . . . C53 C 1.383(2) 0.7891(18) 0.9296(18) 0.099(8) Uiso 1 1 d . . . C54 C 1.260(2) 0.7616(15) 0.8758(18) 0.095(8) Uiso 1 1 d . . . C48 C 0.8192(19) 0.9598(15) 0.7922(15) 0.051(6) Uani 1 1 d . . . C39 C 0.8027(18) 0.9037(15) 0.8628(15) 0.046(6) Uani 1 1 d . . . C26 C 0.5081(18) 0.7682(13) 0.6177(14) 0.068(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0570(17) 0.058(2) 0.0558(16) 0.0072(15) 0.0236(14) 0.0030(16) Cu2 0.0552(17) 0.054(2) 0.0517(15) 0.0056(15) 0.0213(13) 0.0070(15) O5 0.062(10) 0.053(11) 0.043(8) 0.020(8) 0.043(8) 0.005(8) O8 0.080(10) 0.065(9) 0.051(8) 0.018(7) 0.039(7) 0.013(8) O7 0.084(10) 0.044(9) 0.047(8) 0.008(7) 0.036(7) -0.003(8) O1 0.077(10) 0.049(10) 0.034(7) 0.007(6) 0.038(7) -0.002(8) O26 0.101(12) 0.063(10) 0.065(9) 0.001(8) 0.054(9) -0.012(9) O3 0.072(11) 0.031(10) 0.049(9) 0.001(7) 0.023(8) 0.002(8) O11 0.069(10) 0.077(11) 0.057(9) 0.015(8) 0.045(8) 0.010(8) O2 0.037(7) 0.060(10) 0.023(6) 0.007(6) 0.010(6) 0.013(7) O9 0.105(11) 0.056(9) 0.066(8) -0.002(7) 0.054(8) 0.018(9) N3 0.033(10) 0.061(13) 0.031(9) -0.022(9) 0.020(7) 0.003(9) O10 0.043(9) 0.070(13) 0.059(10) -0.013(9) 0.013(8) 0.007(8) O6 0.068(9) 0.062(10) 0.091(10) 0.031(8) 0.045(7) 0.015(8) N4 0.027(9) 0.076(16) 0.047(10) 0.004(10) 0.013(7) 0.021(9) C11 0.048(13) 0.076(17) 0.040(12) 0.002(12) 0.022(10) -0.006(12) C29 0.037(11) 0.064(16) 0.061(12) 0.022(14) 0.026(10) 0.001(13) C41 0.073(17) 0.10(2) 0.056(15) -0.004(15) 0.034(13) 0.010(15) C2 0.036(11) 0.058(16) 0.037(10) 0.005(11) 0.012(9) 0.033(12) C9 0.055(13) 0.052(13) 0.047(11) 0.015(10) 0.025(10) 0.003(11) C1 0.016(9) 0.056(15) 0.037(10) 0.016(10) 0.004(8) -0.011(9) C36 0.052(13) 0.046(13) 0.065(13) 0.006(11) 0.026(11) -0.001(10) O4 0.058(10) 0.055(12) 0.060(10) 0.024(8) 0.028(8) 0.015(8) C47 0.034(12) 0.063(17) 0.049(13) -0.021(12) -0.011(10) 0.036(11) C28 0.023(10) 0.068(14) 0.041(10) 0.004(11) 0.006(8) -0.004(11) C3 0.023(11) 0.076(17) 0.032(11) 0.029(11) 0.008(8) -0.004(10) C35 0.10(2) 0.07(2) 0.062(15) 0.014(13) 0.047(15) 0.010(15) C40 0.030(12) 0.11(2) 0.044(13) 0.003(13) 0.004(10) 0.020(13) C30 0.038(12) 0.054(16) 0.060(13) 0.021(11) 0.032(10) 0.015(10) C13 0.020(11) 0.037(15) 0.051(13) -0.010(11) -0.006(9) -0.011(10) C8 0.045(13) 0.052(17) 0.034(11) -0.009(10) 0.019(10) 0.000(11) C31 0.045(13) 0.079(19) 0.040(13) 0.004(13) 0.023(10) 0.002(13) C19 0.057(14) 0.043(16) 0.058(15) 0.010(12) 0.017(11) 0.018(11) C5 0.078(16) 0.077(17) 0.061(15) -0.014(13) 0.020(13) 0.013(14) C12 0.036(13) 0.10(2) 0.023(10) 0.009(13) 0.020(9) -0.013(13) C4 0.024(11) 0.08(2) 0.059(14) 0.025(13) 0.015(10) 0.014(12) C18 0.107(19) 0.09(2) 0.053(14) 0.011(14) 0.032(13) 0.008(17) C46 0.072(16) 0.056(19) 0.062(15) 0.023(13) 0.030(12) 0.018(13) C32 0.060(14) 0.089(17) 0.048(12) -0.005(12) 0.027(11) 0.000(13) C17 0.18(3) 0.06(2) 0.11(2) -0.012(18) 0.08(2) 0.028(19) C49 0.075(16) 0.034(15) 0.054(14) 0.001(11) 0.017(12) 0.014(12) C21 0.115(19) 0.056(18) 0.033(12) -0.013(11) 0.050(13) -0.041(15) C14 0.079(15) 0.056(17) 0.030(11) 0.001(11) 0.021(11) -0.021(13) C7 0.059(15) 0.12(2) 0.051(13) -0.005(13) 0.026(11) 0.000(14) C37 0.071(14) 0.034(12) 0.018(9) 0.008(9) 0.022(9) 0.001(10) C42 0.080(16) 0.036(15) 0.054(14) -0.022(11) 0.010(12) -0.016(12) C6 0.081(16) 0.062(15) 0.051(12) -0.007(11) 0.026(11) -0.011(13) C20 0.064(14) 0.034(15) 0.049(13) -0.016(11) 0.008(10) 0.012(11) C15 0.12(2) 0.06(2) 0.073(17) 0.002(15) 0.041(16) 0.003(17) C33 0.065(15) 0.14(3) 0.073(16) 0.058(17) 0.031(13) -0.012(16) C45 0.14(2) 0.036(17) 0.078(16) 0.008(12) 0.041(16) 0.018(15) C22 0.066(15) 0.06(2) 0.030(12) 0.003(13) 0.002(11) -0.032(15) C43 0.15(2) 0.029(16) 0.072(16) 0.005(12) 0.043(15) 0.030(14) C16 0.18(3) 0.12(3) 0.09(2) 0.051(19) 0.08(2) 0.08(2) C44 0.15(2) 0.08(2) 0.095(19) 0.031(17) 0.046(18) 0.060(18) C34 0.11(2) 0.17(3) 0.087(19) 0.05(2) 0.038(18) -0.02(2) C48 0.050(14) 0.068(19) 0.039(13) -0.010(13) 0.018(11) 0.001(13) C39 0.036(12) 0.057(18) 0.044(13) 0.011(13) 0.005(10) 0.011(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.920(13) . ? Cu1 O3 1.933(14) . ? Cu1 N3 1.941(19) . ? Cu1 O1 2.035(12) . ? Cu1 N1 2.303(18) . ? Cu1 Cu2 3.022(3) . ? Cu2 N4 1.93(2) . ? Cu2 O4 1.956(14) . ? Cu2 O2 1.975(12) . ? Cu2 O1 1.991(14) . ? Cu2 N2 2.344(17) . ? O5 C11 1.40(2) . ? O5 C9 1.481(19) . ? O8 C4 1.45(2) . ? O8 C8 1.486(19) . ? O7 C4 1.37(2) . ? O7 C3 1.40(2) . ? O1 C1 1.39(2) . ? O26 C31 1.38(3) . ? O26 C35 1.44(2) . ? O3 C22 1.28(3) . ? O11 C31 1.43(2) . ? O11 C30 1.50(2) . ? O2 C28 1.46(2) . ? O9 C29 1.41(3) . ? N3 C12 1.27(3) . ? N3 C11 1.54(2) . ? O10 C37 1.44(2) . ? O10 C36 1.45(2) . ? O6 C2 1.40(2) . ? N4 C49 1.30(3) . ? N4 C37 1.48(2) . ? C11 C1 1.45(2) . ? C29 C28 1.51(2) . ? C29 C30 1.55(3) . ? C41 C40 1.41(3) . ? C41 C42 1.43(3) . ? C2 C3 1.44(3) . ? C2 C1 1.61(2) . ? C9 C8 1.52(3) . ? C9 C3 1.55(3) . ? C36 C30 1.49(3) . ? C36 C35 1.50(3) . ? O4 C39 1.29(2) . ? C47 C46 1.44(3) . ? C47 C42 1.46(3) . ? C47 C48 1.52(3) . ? C28 C37 1.52(3) . ? C40 C39 1.52(3) . ? C13 C14 1.40(3) . ? C13 C22 1.47(3) . ? C13 C12 1.50(3) . ? C31 C32 1.51(2) . ? C19 C18 1.41(3) . ? C19 C20 1.43(3) . ? C19 C14 1.43(3) . ? C5 C6 1.50(3) . ? C5 C4 1.53(3) . ? C18 C17 1.33(3) . ? C46 C45 1.38(3) . ? C32 C33 1.50(3) . ? C17 C16 1.42(3) . ? C49 C48 1.42(3) . ? C21 C20 1.32(3) . ? C21 C22 1.46(3) . ? C14 C15 1.44(3) . ? C7 C6 1.58(3) . ? C42 C43 1.39(3) . ? C15 C16 1.41(4) . ? C33 C34 1.46(3) . ? C45 C44 1.45(3) . ? C43 C44 1.36(3) . ? N2 C27 1.33(3) . ? N2 C23 1.34(2) . ? N1 C54 1.36(3) . ? N1 C50 1.38(3) . ? C23 C24 1.39(3) . ? C25 C24 1.39(3) . ? C25 C26 1.41(3) . ? C50 C51 1.44(3) . ? C51 C52 1.40(3) . ? C52 C53 1.42(3) . ? C27 C26 1.40(3) . ? C53 C54 1.50(3) . ? C48 C39 1.40(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 O2 Cu1 O3 99.5(6) . . ? O2 Cu1 N3 153.6(6) . . ? O3 Cu1 N3 90.7(6) . . ? O2 Cu1 O1 80.6(5) . . ? O3 Cu1 O1 170.8(7) . . ? N3 Cu1 O1 85.5(6) . . ? O2 Cu1 N1 102.5(6) . . ? O3 Cu1 N1 92.1(6) . . ? N3 Cu1 N1 101.4(7) . . ? O1 Cu1 N1 96.9(6) . . ? O2 Cu1 Cu2 39.8(3) . . ? O3 Cu1 Cu2 138.7(5) . . ? N3 Cu1 Cu2 123.1(4) . . ? O1 Cu1 Cu2 40.8(4) . . ? N1 Cu1 Cu2 102.2(5) . . ? N4 Cu2 O4 90.6(7) . . ? N4 Cu2 O2 87.4(6) . . ? O4 Cu2 O2 170.8(6) . . ? N4 Cu2 O1 147.9(6) . . ? O4 Cu2 O1 96.8(6) . . ? O2 Cu2 O1 80.4(5) . . ? N4 Cu2 N2 108.2(7) . . ? O4 Cu2 N2 92.0(6) . . ? O2 Cu2 N2 97.2(5) . . ? O1 Cu2 N2 102.8(6) . . ? N4 Cu2 Cu1 119.9(4) . . ? O4 Cu2 Cu1 137.9(5) . . ? O2 Cu2 Cu1 38.5(4) . . ? O1 Cu2 Cu1 41.9(3) . . ? N2 Cu2 Cu1 103.5(5) . . ? C11 O5 C9 106.8(14) . . ? C4 O8 C8 113.0(14) . . ? C4 O7 C3 115.1(17) . . ? C1 O1 Cu2 133.8(12) . . ? C1 O1 Cu1 105.2(11) . . ? Cu2 O1 Cu1 97.3(5) . . ? C31 O26 C35 113.3(16) . . ? C22 O3 Cu1 129.7(14) . . ? C31 O11 C30 108.3(14) . . ? C28 O2 Cu1 144.5(10) . . ? C28 O2 Cu2 109.4(11) . . ? Cu1 O2 Cu2 101.8(5) . . ? C12 N3 C11 120.4(18) . . ? C12 N3 Cu1 129.4(13) . . ? C11 N3 Cu1 110.1(13) . . ? C37 O10 C36 109.2(14) . . ? C49 N4 C37 122.3(18) . . ? C49 N4 Cu2 128.4(14) . . ? C37 N4 Cu2 108.8(13) . . ? O5 C11 C1 117.7(15) . . ? O5 C11 N3 110.8(16) . . ? C1 C11 N3 105.6(15) . . ? O9 C29 C28 115.1(18) . . ? O9 C29 C30 112.8(16) . . ? C28 C29 C30 107.3(19) . . ? C40 C41 C42 124(2) . . ? O6 C2 C3 113.7(14) . . ? O6 C2 C1 114.0(15) . . ? C3 C2 C1 111.4(18) . . ? O5 C9 C8 106.6(15) . . ? O5 C9 C3 111.7(14) . . ? C8 C9 C3 110.5(15) . . ? O1 C1 C11 114.4(14) . . ? O1 C1 C2 115.1(16) . . ? C11 C1 C2 107.8(14) . . ? O10 C36 C30 110.7(15) . . ? O10 C36 C35 110.9(16) . . ? C30 C36 C35 111.2(17) . . ? C39 O4 Cu2 124.9(13) . . ? C46 C47 C42 116(2) . . ? C46 C47 C48 124.0(18) . . ? C42 C47 C48 119(2) . . ? O2 C28 C29 116.0(17) . . ? O2 C28 C37 107.4(13) . . ? C29 C28 C37 109.7(18) . . ? O7 C3 C2 116.7(19) . . ? O7 C3 C9 109.5(14) . . ? C2 C3 C9 112.9(14) . . ? O26 C35 C36 108.4(18) . . ? C41 C40 C39 120(2) . . ? C36 C30 O11 107.7(16) . . ? C36 C30 C29 114.6(17) . . ? O11 C30 C29 110.0(15) . . ? C14 C13 C22 122.2(19) . . ? C14 C13 C12 120(2) . . ? C22 C13 C12 117(2) . . ? O8 C8 C9 107.5(15) . . ? O26 C31 O11 114.5(16) . . ? O26 C31 C32 110.0(19) . . ? O11 C31 C32 109.9(18) . . ? C18 C19 C20 119(2) . . ? C18 C19 C14 123(2) . . ? C20 C19 C14 118(2) . . ? C6 C5 C4 115.5(19) . . ? N3 C12 C13 126(2) . . ? O7 C4 O8 114.1(15) . . ? O7 C4 C5 114(2) . . ? O8 C4 C5 108.1(17) . . ? C17 C18 C19 120(2) . . ? C45 C46 C47 121(2) . . ? C33 C32 C31 118(2) . . ? C18 C17 C16 122(3) . . ? N4 C49 C48 124(2) . . ? C20 C21 C22 126(2) . . ? C13 C14 C19 120(2) . . ? C13 C14 C15 124.1(19) . . ? C19 C14 C15 115(2) . . ? O10 C37 N4 112.5(15) . . ? O10 C37 C28 112.3(13) . . ? N4 C37 C28 110.2(15) . . ? C43 C42 C41 121(2) . . ? C43 C42 C47 121(2) . . ? C41 C42 C47 117(2) . . ? C5 C6 C7 110.5(19) . . ? C21 C20 C19 120.4(19) . . ? C16 C15 C14 121(2) . . ? C34 C33 C32 117(2) . . ? C46 C45 C44 120(2) . . ? O3 C22 C21 121(2) . . ? O3 C22 C13 126(2) . . ? C21 C22 C13 113(2) . . ? C44 C43 C42 121(2) . . ? C15 C16 C17 119(3) . . ? C43 C44 C45 121(2) . . ? C27 N2 C23 118.5(18) . . ? C27 N2 Cu2 118.8(15) . . ? C23 N2 Cu2 122.4(13) . . ? C54 N1 C50 125(2) . . ? C54 N1 Cu1 115.4(15) . . ? C50 N1 Cu1 118.9(17) . . ? N2 C23 C24 122.9(19) . . ? C24 C25 C26 119(2) . . ? N1 C50 C51 118(2) . . ? C52 C51 C50 122(2) . . ? C51 C52 C53 116(2) . . ? C23 C24 C25 119(2) . . ? N2 C27 C26 123(2) . . ? C52 C53 C54 123(3) . . ? N1 C54 C53 115(2) . . ? C39 C48 C49 120(2) . . ? C39 C48 C47 121.4(18) . . ? C49 C48 C47 118(2) . . ? O4 C39 C48 127.9(19) . . ? O4 C39 C40 115(2) . . ? C48 C39 C40 117(2) . . ? C27 C26 C25 117(2) . . ? #Compound 3a data_rajxrd8 _database_code_CSD 210437 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H44 Cu2 N2 O16' _chemical_formula_weight 911.83 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' 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' N N 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 4.989(5) _cell_length_b 22.735(5) _cell_length_c 16.938(5) _cell_angle_alpha 90.000 _cell_angle_beta 96.590(5) _cell_angle_gamma 90.000 _cell_volume 1908(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 1.193 _exptl_absorpt_correction_type no _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'K-CCD Nonius' _diffrn_measurement_method 'P and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% no _diffrn_reflns_number 11907 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0859 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7071 _reflns_number_gt 4568 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Attempts to refine in P21/c failed. Water hydrogen atoms were not seen on difference fourier maps are included in the structure only to fit the chemical formula ; _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^)+(0.0646P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 7071 _refine_ls_number_parameters 525 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0995 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1386 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0459(16) 0.7814(4) 1.0573(6) 0.049(2) Uani 1 1 d . . . H1 H 0.0219 0.7462 1.0401 0.059 Uiso 1 1 calc R . . C2 C -0.2166(15) 0.7806(5) 1.1143(5) 0.056(2) Uani 1 1 d . . . H2 H -0.2664 0.7447 1.1346 0.068 Uiso 1 1 calc R . . C3 C -0.3186(13) 0.8328(6) 1.1430(4) 0.057(2) Uani 1 1 d . . . H3 H -0.4310 0.8316 1.1831 0.068 Uiso 1 1 calc R . . C4 C -0.2525(14) 0.8846(4) 1.1120(5) 0.046(2) Uani 1 1 d . . . H4 H -0.3237 0.9193 1.1298 0.055 Uiso 1 1 calc R . . C5 C -0.0722(16) 0.8866(4) 1.0513(5) 0.039(2) Uani 1 1 d . . . C6 C 0.0300(11) 0.8344(4) 1.0238(4) 0.0347(16) Uani 1 1 d . . . C7 C -0.0021(15) 0.9407(4) 1.0200(5) 0.047(2) Uani 1 1 d . . . H7 H -0.0773 0.9748 1.0381 0.056 Uiso 1 1 calc R . . C8 C 0.1706(14) 0.9452(4) 0.9644(5) 0.043(2) Uani 1 1 d . . . H8 H 0.2219 0.9822 0.9482 0.052 Uiso 1 1 calc R . . C9 C 0.2764(15) 0.8935(4) 0.9299(5) 0.035(2) Uani 1 1 d . . . C10 C 0.2073(11) 0.8369(4) 0.9595(4) 0.0314(16) Uani 1 1 d . . . C11 C 0.2991(15) 0.7834(4) 0.9283(5) 0.039(2) Uani 1 1 d . . . H11 H 0.2516 0.7483 0.9512 0.047 Uiso 1 1 calc R . . C12 C 0.4843(13) 0.7252(3) 0.8313(4) 0.0331(17) Uani 1 1 d . . . H12 H 0.3316 0.7192 0.7902 0.040 Uiso 1 1 calc R . . C13 C 0.7419(12) 0.7296(3) 0.7897(4) 0.0348(16) Uani 1 1 d . . . H13 H 0.8994 0.7289 0.8300 0.042 Uiso 1 1 calc R . . C14 C 0.7501(11) 0.6754(4) 0.7358(4) 0.0317(19) Uani 1 1 d . . . H14 H 0.5902 0.6751 0.6964 0.038 Uiso 1 1 calc R . . C15 C 0.7437(11) 0.6232(3) 0.7890(4) 0.0316(15) Uani 1 1 d . . . H15 H 0.9081 0.6235 0.8267 0.038 Uiso 1 1 calc R . . C16 C 0.4991(13) 0.6229(3) 0.8367(4) 0.0352(17) Uani 1 1 d . . . H16 H 0.3334 0.6209 0.7996 0.042 Uiso 1 1 calc R . . C17 C 0.5124(14) 0.5700(4) 0.8908(5) 0.042(2) Uani 1 1 d . . . H17A H 0.6732 0.5717 0.9288 0.051 Uiso 1 1 calc R . . H17B H 0.3557 0.5688 0.9197 0.051 Uiso 1 1 calc R . . C18 C 0.7455(13) 0.5201(4) 0.7971(5) 0.0431(18) Uani 1 1 d . . . H18 H 0.9127 0.5213 0.8337 0.052 Uiso 1 1 calc R . . C19 C 0.7373(15) 0.4651(5) 0.7487(5) 0.062(3) Uani 1 1 d . . . H19A H 0.7381 0.4315 0.7831 0.093 Uiso 1 1 calc R . . H19B H 0.8924 0.4636 0.7200 0.093 Uiso 1 1 calc R . . H19C H 0.5762 0.4647 0.7118 0.093 Uiso 1 1 calc R . . C20 C 1.6147(15) 0.8993(4) 0.4593(5) 0.0368(19) Uani 1 1 d . . . H20 H 1.5446 0.9344 0.4761 0.044 Uiso 1 1 calc R . . C21 C 1.7945(15) 0.9002(4) 0.4030(5) 0.049(2) Uani 1 1 d . . . H21 H 1.8444 0.9362 0.3830 0.059 Uiso 1 1 calc R . . C22 C 1.9011(13) 0.8495(5) 0.3758(4) 0.052(2) Uani 1 1 d . . . H22 H 2.0218 0.8510 0.3379 0.062 Uiso 1 1 calc R . . C23 C 1.8284(15) 0.7973(4) 0.4049(5) 0.050(2) Uani 1 1 d . . . H23 H 1.9016 0.7629 0.3866 0.059 Uiso 1 1 calc R . . C24 C 1.6455(14) 0.7933(4) 0.4619(5) 0.040(2) Uani 1 1 d . . . C25 C 1.5365(11) 0.8459(5) 0.4915(4) 0.0365(18) Uani 1 1 d . . . C26 C 1.3454(11) 0.8411(4) 0.5511(4) 0.0322(15) Uani 1 1 d . . . C27 C 1.2780(16) 0.7860(4) 0.5764(5) 0.040(2) Uani 1 1 d . . . C28 C 1.3904(14) 0.7348(4) 0.5472(5) 0.044(2) Uani 1 1 d . . . H28 H 1.3448 0.6983 0.5666 0.053 Uiso 1 1 calc R . . C29 C 1.5643(14) 0.7377(4) 0.4912(5) 0.048(2) Uani 1 1 d . . . H29 H 1.6316 0.7032 0.4716 0.057 Uiso 1 1 calc R . . C30 C 1.2267(13) 0.8942(4) 0.5770(5) 0.030(2) Uani 1 1 d . . . H30 H 1.2726 0.9292 0.5537 0.036 Uiso 1 1 calc R . . C31 C 0.9241(13) 0.9508(3) 0.6482(5) 0.0371(17) Uani 1 1 d . . . H31 H 0.7498 0.9518 0.6150 0.045 Uiso 1 1 calc R . . C32 C 0.8689(13) 0.9476(3) 0.7350(4) 0.0343(15) Uani 1 1 d . . . H32 H 1.0413 0.9480 0.7692 0.041 Uiso 1 1 calc R . . C33 C 0.7080(14) 0.9995(4) 0.7540(4) 0.036(2) Uani 1 1 d . . . H33 H 0.5302 0.9978 0.7227 0.043 Uiso 1 1 calc R . . C34 C 0.8580(13) 1.0544(3) 0.7307(4) 0.0386(17) Uani 1 1 d . . . H34 H 1.0316 1.0562 0.7642 0.046 Uiso 1 1 calc R . . C35 C 0.9135(13) 1.0530(3) 0.6442(4) 0.0382(17) Uani 1 1 d . . . H35 H 0.7413 1.0507 0.6101 0.046 Uiso 1 1 calc R . . C36 C 1.0555(17) 1.1072(4) 0.6247(5) 0.050(2) Uani 1 1 d . . . H36A H 1.2336 1.1083 0.6545 0.060 Uiso 1 1 calc R . . H36B H 1.0766 1.1078 0.5685 0.060 Uiso 1 1 calc R . . C37 C 0.8535(14) 1.1575(4) 0.7255(5) 0.0467(19) Uani 1 1 d . . . H37 H 1.0265 1.1587 0.7594 0.056 Uiso 1 1 calc R . . C38 C 0.6908(17) 1.2114(5) 0.7407(6) 0.060(3) Uani 1 1 d . . . H38A H 0.7920 1.2461 0.7308 0.090 Uiso 1 1 calc R . . H38B H 0.6525 1.2115 0.7950 0.090 Uiso 1 1 calc R . . H38C H 0.5246 1.2111 0.7060 0.090 Uiso 1 1 calc R . . O1 O 0.7095(10) 1.1067(3) 0.7440(3) 0.0469(17) Uani 1 1 d . . . O2 O 0.9013(10) 1.1573(2) 0.6447(3) 0.0522(14) Uani 1 1 d . . . O3 O 1.0710(8) 1.0022(2) 0.6308(3) 0.0385(12) Uani 1 1 d . . . O4 O 0.6749(9) 1.0029(2) 0.8366(3) 0.0503(12) Uani 1 1 d . . . H4O H 0.5855 1.0321 0.8447 0.075 Uiso 1 1 calc R . . O5 O 0.7453(9) 0.8927(3) 0.7418(3) 0.043(2) Uani 1 1 d . . . O6 O 0.7350(8) 0.5692(3) 0.7458(3) 0.0377(15) Uani 1 1 d . . . O7 O 0.5189(9) 0.5193(2) 0.8415(3) 0.0438(13) Uani 1 1 d . . . O8 O 0.4959(8) 0.6766(2) 0.8834(3) 0.0392(12) Uani 1 1 d . . . O9 O 0.9857(8) 0.6727(2) 0.6966(3) 0.0390(11) Uani 1 1 d . . . H9O H 0.9797 0.6984 0.6625 0.059 Uiso 1 1 calc R . . O10 O 0.7323(9) 0.7839(3) 0.7502(3) 0.045(2) Uani 1 1 d . . . O11 O 0.4353(11) 0.9016(3) 0.8758(4) 0.0369(14) Uani 1 1 d . . . O12 O 1.1120(11) 0.7767(3) 0.6329(4) 0.0424(16) Uani 1 1 d . . . O15 O 0.0995(11) 0.5884(3) 0.0487(4) 0.0815(18) Uani 1 1 d . . . O14 O 0.6159(15) 0.6348(6) 0.0854(7) 0.202(6) Uani 1 1 d . . . O13 O 0.136(3) 0.5736(5) 0.6025(8) 0.241(7) Uani 1 1 d . . . O16 O 0.411(3) 0.0487(6) 0.4602(9) 0.266(7) Uani 1 1 d . . . Cu1 Cu 0.92441(14) 0.83327(3) 0.68446(5) 0.0381(3) Uani 1 1 d . . . Cu2 Cu 0.58818(13) 0.84427(3) 0.81541(5) 0.0369(3) Uani 1 1 d . . . N1 N 0.4441(13) 0.7808(3) 0.8701(5) 0.0366(19) Uani 1 1 d . . . N2 N 1.0612(13) 0.8970(3) 0.6300(4) 0.0318(18) Uani 1 1 d . . . H150 H 0.2840 0.6001 0.0684 0.050 Uiso 1 1 d . . . H151 H -0.063(13) 0.6079 0.0585 0.050 Uiso 1 1 d . . . H130 H 0.0195 0.5382 0.5994 0.050 Uiso 1 1 d . . . H131 H 0.2595 0.6001 0.6322 0.050 Uiso 1 1 d . . . H140 H 0.5963 0.6276 0.1391 0.050 Uiso 1 1 d . . . H141 H 0.4771 0.6427 0.0412 0.050 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 C1 0.051(5) 0.054(6) 0.047(6) -0.006(4) 0.023(4) 0.000(4) C2 0.064(5) 0.058(6) 0.052(6) 0.013(5) 0.030(4) 0.001(4) C3 0.058(4) 0.073(6) 0.045(4) -0.007(5) 0.027(3) -0.001(5) C4 0.051(4) 0.049(5) 0.041(5) -0.013(4) 0.021(4) 0.003(4) C5 0.044(4) 0.041(5) 0.035(5) -0.009(4) 0.015(3) 0.005(3) C6 0.034(3) 0.036(4) 0.035(4) 0.000(4) 0.009(2) 0.002(3) C7 0.069(5) 0.030(5) 0.046(6) -0.005(4) 0.023(4) 0.013(4) C8 0.052(4) 0.032(5) 0.047(5) -0.001(4) 0.014(3) 0.007(3) C9 0.038(4) 0.033(5) 0.036(5) -0.003(4) 0.015(3) -0.003(3) C10 0.035(3) 0.031(4) 0.030(3) 0.003(4) 0.011(2) 0.007(3) C11 0.036(4) 0.037(6) 0.044(6) -0.001(4) 0.006(4) 0.002(4) C12 0.032(3) 0.029(4) 0.041(4) 0.003(3) 0.017(3) -0.004(3) C13 0.029(3) 0.034(4) 0.043(5) -0.005(3) 0.013(3) -0.003(3) C14 0.029(3) 0.034(5) 0.034(4) -0.003(4) 0.012(3) -0.002(3) C15 0.027(3) 0.030(4) 0.040(4) -0.002(3) 0.015(3) -0.001(3) C16 0.034(3) 0.026(4) 0.047(5) -0.002(3) 0.015(3) 0.000(3) C17 0.049(4) 0.038(5) 0.043(5) 0.008(4) 0.017(3) 0.001(3) C18 0.049(4) 0.035(4) 0.049(5) 0.008(4) 0.021(3) 0.003(3) C19 0.085(6) 0.040(6) 0.070(7) -0.003(4) 0.042(5) 0.002(4) C20 0.044(4) 0.029(4) 0.039(5) 0.001(3) 0.012(3) -0.002(3) C21 0.050(4) 0.055(6) 0.045(5) 0.009(4) 0.017(4) -0.003(4) C22 0.051(4) 0.061(6) 0.050(5) 0.005(5) 0.029(3) -0.002(4) C23 0.049(4) 0.053(6) 0.049(5) -0.006(4) 0.018(4) 0.006(4) C24 0.036(4) 0.048(5) 0.040(5) -0.005(4) 0.014(3) 0.000(3) C25 0.031(3) 0.050(5) 0.029(4) 0.000(4) 0.006(2) 0.001(4) C26 0.041(3) 0.024(4) 0.032(4) 0.001(4) 0.006(2) -0.009(4) C27 0.044(4) 0.044(6) 0.034(5) -0.001(4) 0.016(3) 0.002(4) C28 0.059(4) 0.029(5) 0.049(5) 0.000(4) 0.019(3) -0.007(3) C29 0.054(4) 0.042(6) 0.049(5) -0.005(4) 0.014(4) 0.003(3) C30 0.025(3) 0.031(5) 0.036(5) 0.000(4) 0.012(3) -0.003(3) C31 0.037(4) 0.029(4) 0.048(5) -0.002(4) 0.014(3) 0.002(3) C32 0.041(4) 0.027(4) 0.037(4) 0.000(3) 0.016(3) -0.004(3) C33 0.042(4) 0.031(5) 0.037(5) -0.003(4) 0.013(3) -0.008(3) C34 0.038(3) 0.029(4) 0.050(5) -0.004(3) 0.013(3) 0.000(3) C35 0.044(3) 0.032(4) 0.040(4) 0.005(3) 0.008(3) 0.003(3) C36 0.079(5) 0.019(4) 0.058(5) -0.001(4) 0.033(4) -0.001(4) C37 0.057(4) 0.026(4) 0.059(5) 0.004(4) 0.016(4) -0.004(3) C38 0.073(5) 0.035(6) 0.075(8) 0.000(4) 0.028(5) 0.003(4) O1 0.055(3) 0.026(4) 0.062(5) 0.002(3) 0.019(3) -0.001(2) O2 0.074(3) 0.035(3) 0.052(3) 0.011(3) 0.026(3) 0.001(2) O3 0.041(2) 0.025(3) 0.054(3) 0.006(3) 0.024(2) -0.005(2) O4 0.075(3) 0.035(3) 0.045(3) -0.001(2) 0.027(2) 0.001(3) O5 0.065(4) 0.024(4) 0.046(5) -0.001(2) 0.029(4) -0.009(2) O6 0.046(3) 0.031(4) 0.040(4) -0.002(2) 0.021(3) 0.0026(19) O7 0.048(2) 0.033(3) 0.054(3) -0.004(3) 0.021(2) -0.004(2) O8 0.049(2) 0.031(3) 0.043(3) 0.002(2) 0.025(2) 0.000(2) O9 0.046(2) 0.033(3) 0.044(3) 0.007(2) 0.027(2) 0.010(2) O10 0.052(4) 0.028(5) 0.062(5) 0.003(3) 0.032(4) 0.000(2) O11 0.050(3) 0.024(3) 0.041(3) -0.006(3) 0.024(3) 0.000(2) O12 0.051(3) 0.030(4) 0.050(4) 0.008(3) 0.023(3) -0.004(2) O15 0.080(3) 0.083(5) 0.085(5) 0.004(4) 0.024(3) -0.003(3) O14 0.091(5) 0.243(13) 0.265(13) -0.165(11) -0.004(6) 0.003(7) O13 0.343(16) 0.146(10) 0.269(14) -0.135(10) 0.189(12) -0.079(10) O16 0.293(15) 0.181(13) 0.326(19) -0.079(12) 0.045(13) 0.053(11) Cu1 0.0459(5) 0.0318(8) 0.0403(5) 0.0004(5) 0.0205(4) -0.0053(5) Cu2 0.0418(4) 0.0302(8) 0.0427(5) -0.0006(5) 0.0217(4) -0.0026(4) N1 0.038(3) 0.029(5) 0.047(5) -0.009(4) 0.020(3) -0.004(3) N2 0.035(3) 0.029(5) 0.033(4) 0.002(3) 0.015(3) 0.000(3) _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 C1 C2 1.359(12) . ? C1 C6 1.402(13) . ? C2 C3 1.400(13) . ? C3 C4 1.347(13) . ? C4 C5 1.442(12) . ? C5 C6 1.393(12) . ? C5 C7 1.399(12) . ? C6 C10 1.480(9) . ? C7 C8 1.352(11) . ? C8 C9 1.438(11) . ? C9 O11 1.292(11) . ? C9 C10 1.438(13) . ? C10 C11 1.423(12) . ? C11 N1 1.289(12) . ? C12 O8 1.411(8) . ? C12 N1 1.448(10) . ? C12 C13 1.537(9) . ? C13 O10 1.404(10) . ? C13 C14 1.537(11) . ? C14 O9 1.417(7) . ? C14 C15 1.492(11) . ? C15 O6 1.427(9) . ? C15 C16 1.538(9) . ? C16 O8 1.456(8) . ? C16 C17 1.509(10) . ? C17 O7 1.427(9) . ? C18 O6 1.411(9) . ? C18 O7 1.428(8) . ? C18 C19 1.496(12) . ? C20 C21 1.382(12) . ? C20 C25 1.404(12) . ? C21 C22 1.372(12) . ? C22 C23 1.351(12) . ? C23 C24 1.406(12) . ? C24 C25 1.428(12) . ? C24 C29 1.433(12) . ? C25 C26 1.470(9) . ? C26 C27 1.378(13) . ? C26 C30 1.434(12) . ? C27 O12 1.352(11) . ? C27 C28 1.408(11) . ? C28 C29 1.359(11) . ? C30 N2 1.289(12) . ? C31 O3 1.427(8) . ? C31 N2 1.452(10) . ? C31 C32 1.530(10) . ? C32 O5 1.403(9) . ? C32 C33 1.483(11) . ? C33 O4 1.430(8) . ? C33 C34 1.530(11) . ? C34 O1 1.433(9) . ? C34 C35 1.523(10) . ? C35 O3 1.429(8) . ? C35 C36 1.477(10) . ? C36 O2 1.436(9) . ? C37 O1 1.413(9) . ? C37 O2 1.417(9) . ? C37 C38 1.510(12) . ? O5 Cu2 1.898(6) . ? O5 Cu1 1.941(6) . ? O10 Cu1 1.914(6) . ? O10 Cu2 1.950(6) . ? O11 Cu2 1.872(6) . ? O12 Cu1 1.866(7) . ? Cu1 N2 1.887(8) . ? Cu1 Cu2 2.9411(15) . ? Cu2 N1 1.901(8) . ? 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 C2 C1 C6 121.4(9) . . ? C1 C2 C3 121.1(9) . . ? C4 C3 C2 119.5(7) . . ? C3 C4 C5 120.4(8) . . ? C6 C5 C7 120.3(8) . . ? C6 C5 C4 119.6(8) . . ? C7 C5 C4 120.1(8) . . ? C5 C6 C1 118.0(6) . . ? C5 C6 C10 119.1(8) . . ? C1 C6 C10 122.9(8) . . ? C8 C7 C5 122.6(8) . . ? C7 C8 C9 120.9(8) . . ? O11 C9 C10 124.5(8) . . ? O11 C9 C8 117.1(8) . . ? C10 C9 C8 118.4(8) . . ? C11 C10 C9 122.3(6) . . ? C11 C10 C6 119.1(9) . . ? C9 C10 C6 118.6(8) . . ? N1 C11 C10 123.9(9) . . ? O8 C12 N1 113.3(6) . . ? O8 C12 C13 111.1(5) . . ? N1 C12 C13 108.6(6) . . ? O10 C13 C14 115.1(6) . . ? O10 C13 C12 106.9(5) . . ? C14 C13 C12 107.5(6) . . ? O9 C14 C15 109.0(6) . . ? O9 C14 C13 113.2(6) . . ? C15 C14 C13 105.9(6) . . ? O6 C15 C14 112.1(6) . . ? O6 C15 C16 106.6(5) . . ? C14 C15 C16 113.2(6) . . ? O8 C16 C17 109.9(6) . . ? O8 C16 C15 109.9(5) . . ? C17 C16 C15 109.9(6) . . ? O7 C17 C16 107.0(6) . . ? O6 C18 O7 111.1(6) . . ? O6 C18 C19 109.1(7) . . ? O7 C18 C19 107.7(6) . . ? C21 C20 C25 120.9(8) . . ? C22 C21 C20 121.7(8) . . ? C23 C22 C21 119.1(7) . . ? C22 C23 C24 122.0(9) . . ? C23 C24 C25 119.4(8) . . ? C23 C24 C29 121.7(8) . . ? C25 C24 C29 118.8(7) . . ? C20 C25 C24 116.9(6) . . ? C20 C25 C26 124.1(8) . . ? C24 C25 C26 118.9(8) . . ? C27 C26 C30 123.0(6) . . ? C27 C26 C25 118.8(9) . . ? C30 C26 C25 118.1(8) . . ? O12 C27 C26 123.7(9) . . ? O12 C27 C28 114.8(8) . . ? C26 C27 C28 121.4(8) . . ? C29 C28 C27 121.1(8) . . ? C28 C29 C24 120.9(8) . . ? N2 C30 C26 125.1(8) . . ? O3 C31 N2 112.4(6) . . ? O3 C31 C32 113.0(6) . . ? N2 C31 C32 107.7(6) . . ? O5 C32 C33 115.8(6) . . ? O5 C32 C31 104.5(5) . . ? C33 C32 C31 109.4(6) . . ? O4 C33 C32 112.4(6) . . ? O4 C33 C34 108.9(6) . . ? C32 C33 C34 107.5(6) . . ? O1 C34 C35 108.8(6) . . ? O1 C34 C33 111.1(6) . . ? C35 C34 C33 112.3(6) . . ? O3 C35 C36 110.6(6) . . ? O3 C35 C34 109.5(6) . . ? C36 C35 C34 110.0(6) . . ? O2 C36 C35 109.0(6) . . ? O1 C37 O2 111.0(6) . . ? O1 C37 C38 109.2(7) . . ? O2 C37 C38 108.7(7) . . ? C37 O1 C34 111.0(6) . . ? C37 O2 C36 112.6(6) . . ? C31 O3 C35 108.9(5) . . ? C32 O5 Cu2 142.1(5) . . ? C32 O5 Cu1 110.3(4) . . ? Cu2 O5 Cu1 100.0(3) . . ? C18 O6 C15 111.5(5) . . ? C17 O7 C18 111.7(5) . . ? C12 O8 C16 108.6(5) . . ? C13 O10 Cu1 143.3(4) . . ? C13 O10 Cu2 110.1(4) . . ? Cu1 O10 Cu2 99.1(3) . . ? C9 O11 Cu2 127.6(6) . . ? C27 O12 Cu1 127.1(6) . . ? O12 Cu1 N2 94.1(2) . . ? O12 Cu1 O10 100.3(3) . . ? N2 Cu1 O10 165.5(3) . . ? O12 Cu1 O5 177.1(2) . . ? N2 Cu1 O5 85.6(3) . . ? O10 Cu1 O5 80.0(2) . . ? O12 Cu1 Cu2 140.50(19) . . ? N2 Cu1 Cu2 124.9(2) . . ? O10 Cu1 Cu2 40.9(2) . . ? O5 Cu1 Cu2 39.47(19) . . ? O11 Cu2 O5 100.3(3) . . ? O11 Cu2 N1 93.6(2) . . ? O5 Cu2 N1 165.5(3) . . ? O11 Cu2 O10 177.6(2) . . ? O5 Cu2 O10 80.2(2) . . ? N1 Cu2 O10 85.8(3) . . ? O11 Cu2 Cu1 140.73(19) . . ? O5 Cu2 Cu1 40.6(2) . . ? N1 Cu2 Cu1 125.7(2) . . ? O10 Cu2 Cu1 39.98(19) . . ? C11 N1 C12 120.5(8) . . ? C11 N1 Cu2 127.9(7) . . ? C12 N1 Cu2 111.2(5) . . ? C30 N2 C31 123.0(8) . . ? C30 N2 Cu1 126.7(6) . . ? C31 N2 Cu1 109.8(5) . . ? 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 C6 C1 C2 C3 -1.4(12) . . . . ? C1 C2 C3 C4 1.9(12) . . . . ? C2 C3 C4 C5 -1.8(11) . . . . ? C3 C4 C5 C6 1.1(11) . . . . ? C3 C4 C5 C7 -179.3(8) . . . . ? C7 C5 C6 C1 179.8(8) . . . . ? C4 C5 C6 C1 -0.6(9) . . . . ? C7 C5 C6 C10 -1.7(10) . . . . ? C4 C5 C6 C10 177.9(7) . . . . ? C2 C1 C6 C5 0.7(10) . . . . ? C2 C1 C6 C10 -177.7(7) . . . . ? C6 C5 C7 C8 -2.0(12) . . . . ? C4 C5 C7 C8 178.5(7) . . . . ? C5 C7 C8 C9 4.8(11) . . . . ? C7 C8 C9 O11 178.4(7) . . . . ? C7 C8 C9 C10 -3.8(11) . . . . ? O11 C9 C10 C11 -3.4(10) . . . . ? C8 C9 C10 C11 179.0(7) . . . . ? O11 C9 C10 C6 177.8(7) . . . . ? C8 C9 C10 C6 0.3(9) . . . . ? C5 C6 C10 C11 -176.4(6) . . . . ? C1 C6 C10 C11 2.0(9) . . . . ? C5 C6 C10 C9 2.4(8) . . . . ? C1 C6 C10 C9 -179.2(6) . . . . ? C9 C10 C11 N1 -1.9(9) . . . . ? C6 C10 C11 N1 176.9(7) . . . . ? O8 C12 C13 O10 -170.2(6) . . . . ? N1 C12 C13 O10 -44.9(8) . . . . ? O8 C12 C13 C14 65.7(7) . . . . ? N1 C12 C13 C14 -169.0(6) . . . . ? O10 C13 C14 O9 63.7(7) . . . . ? C12 C13 C14 O9 -177.3(6) . . . . ? O10 C13 C14 C15 -176.9(5) . . . . ? C12 C13 C14 C15 -57.9(6) . . . . ? O9 C14 C15 O6 -61.2(7) . . . . ? C13 C14 C15 O6 176.7(4) . . . . ? O9 C14 C15 C16 178.2(5) . . . . ? C13 C14 C15 C16 56.1(7) . . . . ? O6 C15 C16 O8 179.3(5) . . . . ? C14 C15 C16 O8 -57.1(8) . . . . ? O6 C15 C16 C17 58.2(7) . . . . ? C14 C15 C16 C17 -178.1(6) . . . . ? O8 C16 C17 O7 -179.2(5) . . . . ? C15 C16 C17 O7 -58.1(7) . . . . ? C25 C20 C21 C22 0.7(12) . . . . ? C20 C21 C22 C23 0.0(11) . . . . ? C21 C22 C23 C24 0.3(12) . . . . ? C22 C23 C24 C25 -1.3(12) . . . . ? C22 C23 C24 C29 178.6(7) . . . . ? C21 C20 C25 C24 -1.6(9) . . . . ? C21 C20 C25 C26 -179.6(7) . . . . ? C23 C24 C25 C20 1.9(9) . . . . ? C29 C24 C25 C20 -178.0(7) . . . . ? C23 C24 C25 C26 -180.0(6) . . . . ? C29 C24 C25 C26 0.1(10) . . . . ? C20 C25 C26 C27 178.0(6) . . . . ? C24 C25 C26 C27 0.0(9) . . . . ? C20 C25 C26 C30 1.3(9) . . . . ? C24 C25 C26 C30 -176.7(6) . . . . ? C30 C26 C27 O12 -5.9(10) . . . . ? C25 C26 C27 O12 177.6(7) . . . . ? C30 C26 C27 C28 177.3(7) . . . . ? C25 C26 C27 C28 0.8(10) . . . . ? O12 C27 C28 C29 -178.9(7) . . . . ? C26 C27 C28 C29 -1.8(12) . . . . ? C27 C28 C29 C24 2.0(12) . . . . ? C23 C24 C29 C28 179.0(7) . . . . ? C25 C24 C29 C28 -1.1(11) . . . . ? C27 C26 C30 N2 5.1(10) . . . . ? C25 C26 C30 N2 -178.3(7) . . . . ? O3 C31 C32 O5 -175.2(5) . . . . ? N2 C31 C32 O5 -50.5(7) . . . . ? O3 C31 C32 C33 60.1(7) . . . . ? N2 C31 C32 C33 -175.1(6) . . . . ? O5 C32 C33 O4 68.9(8) . . . . ? C31 C32 C33 O4 -173.3(5) . . . . ? O5 C32 C33 C34 -171.4(6) . . . . ? C31 C32 C33 C34 -53.6(7) . . . . ? O4 C33 C34 O1 -60.5(7) . . . . ? C32 C33 C34 O1 177.5(6) . . . . ? O4 C33 C34 C35 177.3(5) . . . . ? C32 C33 C34 C35 55.4(7) . . . . ? O1 C34 C35 O3 177.7(5) . . . . ? C33 C34 C35 O3 -58.9(7) . . . . ? O1 C34 C35 C36 56.0(7) . . . . ? C33 C34 C35 C36 179.3(6) . . . . ? O3 C35 C36 O2 -175.6(6) . . . . ? C34 C35 C36 O2 -54.5(8) . . . . ? O2 C37 O1 C34 60.5(7) . . . . ? C38 C37 O1 C34 -179.7(7) . . . . ? C35 C34 O1 C37 -58.3(7) . . . . ? C33 C34 O1 C37 177.6(6) . . . . ? O1 C37 O2 C36 -59.9(8) . . . . ? C38 C37 O2 C36 -180.0(6) . . . . ? C35 C36 O2 C37 57.0(8) . . . . ? N2 C31 O3 C35 175.4(6) . . . . ? C32 C31 O3 C35 -62.4(7) . . . . ? C36 C35 O3 C31 -178.4(6) . . . . ? C34 C35 O3 C31 60.2(7) . . . . ? C33 C32 O5 Cu2 -57.3(10) . . . . ? C31 C32 O5 Cu2 -177.7(5) . . . . ? C33 C32 O5 Cu1 162.0(5) . . . . ? C31 C32 O5 Cu1 41.6(6) . . . . ? O7 C18 O6 C15 61.8(7) . . . . ? C19 C18 O6 C15 -179.7(5) . . . . ? C14 C15 O6 C18 176.4(5) . . . . ? C16 C15 O6 C18 -59.2(6) . . . . ? C16 C17 O7 C18 59.2(7) . . . . ? O6 C18 O7 C17 -61.6(8) . . . . ? C19 C18 O7 C17 179.1(6) . . . . ? N1 C12 O8 C16 172.3(5) . . . . ? C13 C12 O8 C16 -65.2(6) . . . . ? C17 C16 O8 C12 179.8(5) . . . . ? C15 C16 O8 C12 58.8(6) . . . . ? C14 C13 O10 Cu1 -60.7(9) . . . . ? C12 C13 O10 Cu1 -180.0(6) . . . . ? C14 C13 O10 Cu2 158.6(4) . . . . ? C12 C13 O10 Cu2 39.3(6) . . . . ? C10 C9 O11 Cu2 6.5(11) . . . . ? C8 C9 O11 Cu2 -175.9(5) . . . . ? C26 C27 O12 Cu1 3.7(11) . . . . ? C28 C27 O12 Cu1 -179.3(5) . . . . ? C27 O12 Cu1 N2 -0.7(6) . . . . ? C27 O12 Cu1 O10 177.9(6) . . . . ? C27 O12 Cu1 O5 -85(6) . . . . ? C27 O12 Cu1 Cu2 -172.8(5) . . . . ? C13 O10 Cu1 O12 28.0(8) . . . . ? Cu2 O10 Cu1 O12 171.0(2) . . . . ? C13 O10 Cu1 N2 -157.6(9) . . . . ? Cu2 O10 Cu1 N2 -14.6(10) . . . . ? C13 O10 Cu1 O5 -149.1(8) . . . . ? Cu2 O10 Cu1 O5 -6.1(2) . . . . ? C13 O10 Cu1 Cu2 -143.0(9) . . . . ? C32 O5 Cu1 O12 65(6) . . . . ? Cu2 O5 Cu1 O12 -91(6) . . . . ? C32 O5 Cu1 N2 -19.1(5) . . . . ? Cu2 O5 Cu1 N2 -175.8(3) . . . . ? C32 O5 Cu1 O10 163.0(5) . . . . ? Cu2 O5 Cu1 O10 6.3(2) . . . . ? C32 O5 Cu1 Cu2 156.7(6) . . . . ? C9 O11 Cu2 O5 172.0(7) . . . . ? C9 O11 Cu2 N1 -4.0(6) . . . . ? C9 O11 Cu2 O10 70(7) . . . . ? C9 O11 Cu2 Cu1 175.9(5) . . . . ? C32 O5 Cu2 O11 33.3(8) . . . . ? Cu1 O5 Cu2 O11 176.2(2) . . . . ? C32 O5 Cu2 N1 -163.0(9) . . . . ? Cu1 O5 Cu2 N1 -20.1(10) . . . . ? C32 O5 Cu2 O10 -149.1(8) . . . . ? Cu1 O5 Cu2 O10 -6.2(2) . . . . ? C32 O5 Cu2 Cu1 -142.9(8) . . . . ? C13 O10 Cu2 O11 -94(7) . . . . ? Cu1 O10 Cu2 O11 108(7) . . . . ? C13 O10 Cu2 O5 163.8(4) . . . . ? Cu1 O10 Cu2 O5 6.3(2) . . . . ? C13 O10 Cu2 N1 -19.7(4) . . . . ? Cu1 O10 Cu2 N1 -177.2(3) . . . . ? C13 O10 Cu2 Cu1 157.5(5) . . . . ? O12 Cu1 Cu2 O11 169.6(4) . . . . ? N2 Cu1 Cu2 O11 -0.8(4) . . . . ? O10 Cu1 Cu2 O11 -176.4(3) . . . . ? O5 Cu1 Cu2 O11 -5.9(3) . . . . ? O12 Cu1 Cu2 O5 175.5(4) . . . . ? N2 Cu1 Cu2 O5 5.1(3) . . . . ? O10 Cu1 Cu2 O5 -170.4(3) . . . . ? O12 Cu1 Cu2 N1 -10.6(4) . . . . ? N2 Cu1 Cu2 N1 179.1(4) . . . . ? O10 Cu1 Cu2 N1 3.5(3) . . . . ? O5 Cu1 Cu2 N1 173.9(3) . . . . ? O12 Cu1 Cu2 O10 -14.1(4) . . . . ? N2 Cu1 Cu2 O10 175.6(3) . . . . ? O5 Cu1 Cu2 O10 170.4(3) . . . . ? C10 C11 N1 C12 -167.5(6) . . . . ? C10 C11 N1 Cu2 3.7(12) . . . . ? O8 C12 N1 C11 -34.0(9) . . . . ? C13 C12 N1 C11 -157.9(7) . . . . ? O8 C12 N1 Cu2 153.4(4) . . . . ? C13 C12 N1 Cu2 29.5(7) . . . . ? O11 Cu2 N1 C11 -1.0(7) . . . . ? O5 Cu2 N1 C11 -165.0(8) . . . . ? O10 Cu2 N1 C11 -178.7(7) . . . . ? Cu1 Cu2 N1 C11 179.1(6) . . . . ? O11 Cu2 N1 C12 170.9(5) . . . . ? O5 Cu2 N1 C12 6.9(13) . . . . ? O10 Cu2 N1 C12 -6.8(5) . . . . ? Cu1 Cu2 N1 C12 -9.1(6) . . . . ? C26 C30 N2 C31 -173.2(6) . . . . ? C26 C30 N2 Cu1 -2.1(11) . . . . ? O3 C31 N2 C30 -26.5(10) . . . . ? C32 C31 N2 C30 -151.5(7) . . . . ? O3 C31 N2 Cu1 161.1(5) . . . . ? C32 C31 N2 Cu1 36.0(6) . . . . ? O12 Cu1 N2 C30 0.0(7) . . . . ? O10 Cu1 N2 C30 -174.5(8) . . . . ? O5 Cu1 N2 C30 177.2(7) . . . . ? Cu2 Cu1 N2 C30 173.9(6) . . . . ? O12 Cu1 N2 C31 172.1(5) . . . . ? O10 Cu1 N2 C31 -2.4(12) . . . . ? O5 Cu1 N2 C31 -10.8(5) . . . . ? Cu2 Cu1 N2 C31 -14.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.338 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.093 #Compound 2a data_gr1_m _database_code_CSD 210438 _audit_creation_date 'Jul 24 21:00:49 2002' _audit_creation_method 'PLATON
option' _audit_update_record ; ? ; # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H52 Cu2 N4 O12, 2(O)' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C44 H52 Cu2 N4 O14' _chemical_formula_weight 988.00 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' Cu Cu 0.3201 1.2651 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall 'P 1' _symmetry_space_group_name_H-M 'P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z _cell_length_a 9.740(3) _cell_length_b 11.316(3) _cell_length_c 12.034(4) _cell_angle_alpha 96.248(5) _cell_angle_beta 107.684(5) _cell_angle_gamma 113.876(4) _cell_volume 1114.0(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9107 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.8 _cell_special_details ; ? ; _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.117 _exptl_crystal_size_mid 0.072 _exptl_crystal_size_min 0.040 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 514 _exptl_absorpt_coefficient_mu 1.026 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # cylinder 'cylindrical # empirical 'empirical from intensities' # gaussian 'Gaussian from crystal shape' # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # refdelf 'refined from delta-F' # sphere 'spherical' _exptl_absorpt_correction_type ' ? ' # Example: '(North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 9107 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_av_sigmaI/netI 0.038 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.77 _diffrn_reflns_theta_full 27.77 _diffrn_measured_fraction_theta_max 0.910 _diffrn_measured_fraction_theta_full 0.910 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 12295 # number of observed reflections (> n sig(I)) _reflns_number_gt 9107 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997) and CAMERON (Watkin et al., 1996)' _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _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^)+(0.1534P)^2^+0.0248P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # (mixed) SHELXL _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0077(9) _refine_ls_number_reflns 9107 _refine_ls_number_parameters 731 _refine_ls_number_restraints 3 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.046 _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_ref 0.09 _refine_ls_wR_factor_gt 0.086 _refine_ls_goodness_of_fit_ref 0.96 _refine_ls_restrained_S_all 0.96 _refine_ls_shift/su_max 0.07 _refine_ls_shift/su_mean 0.005 _refine_diff_density_max 0.52 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.056 #=============================================================================== 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 0.68717(4) 1.02149(3) 0.41045(3) 0.04054(13) Uani 1 1 d . . . Cu2 Cu 0.87046(4) 0.91491(3) 0.30462(3) 0.04433(14) Uani 1 1 d . . . O2 O 0.6425(4) 0.8707(3) 0.2819(3) 0.0405(8) Uani 1 1 d . . . O1 O 0.9098(4) 1.0596(3) 0.4320(3) 0.0468(9) Uani 1 1 d . . . O12 O 0.8278(5) 0.7859(4) 0.1664(3) 0.0532(10) Uani 1 1 d . . . O11 O 0.7354(4) 1.1487(4) 0.5544(3) 0.0501(9) Uani 1 1 d . . . O6 O 0.2517(4) 0.6836(3) 0.2990(3) 0.0467(8) Uani 1 1 d . . . O10 O 0.2041(4) 0.4269(3) 0.0572(3) 0.0453(8) Uani 1 1 d . . . N1 N 1.0721(4) 1.0448(4) 0.2949(3) 0.0399(8) Uani 1 1 d . . . N2 N 0.4697(5) 0.9057(4) 0.3990(3) 0.0434(9) Uani 1 1 d . . . O7 O 1.3171(4) 1.5223(3) 0.6321(3) 0.0498(8) Uani 1 1 d . . . C23 C 0.6336(6) 1.1441(5) 0.6080(4) 0.0412(12) Uani 1 1 d . . . C11 C 0.9196(6) 0.7913(5) 0.1059(5) 0.0445(12) Uani 1 1 d . . . C38 C 0.4419(6) 0.6421(5) 0.1652(4) 0.0372(10) Uani 1 1 d . . . N4 N 0.6468(5) 1.1531(4) 0.2852(4) 0.0510(10) Uani 1 1 d . . . C2 C 1.1006(6) 1.2945(5) 0.5435(5) 0.0443(12) Uani 1 1 d . . . C16 C 1.0743(6) 0.9027(5) 0.1334(4) 0.0412(11) Uani 1 1 d . . . N3 N 0.9128(5) 0.7866(4) 0.4295(4) 0.0471(10) Uani 1 1 d . . . C28 C 0.4772(6) 1.0391(5) 0.5743(4) 0.0440(12) Uani 1 1 d . . . C4 C 1.4862(8) 1.6076(6) 0.6712(6) 0.0680(16) Uani 1 1 d . . . C29 C 0.4044(6) 0.9241(5) 0.4723(5) 0.0471(12) Uani 1 1 d . . . C17 C 1.1394(6) 1.0258(5) 0.2232(4) 0.0413(10) Uani 1 1 d . . . C8 C 1.5067(7) 1.4834(6) 0.5120(6) 0.0676(16) Uani 1 1 d . . . C14 C 1.1088(7) 0.7903(6) -0.0324(5) 0.0558(14) Uani 1 1 d . . . C26 C 0.4408(8) 1.1524(7) 0.7379(5) 0.0660(17) Uani 1 1 d . . . C44 C 0.6137(10) 1.2522(7) 0.3112(7) 0.079(2) Uani 1 1 d . . . C3 C 1.2799(5) 1.3892(4) 0.5780(4) 0.0419(10) Uani 1 1 d . . . C43 C 0.5779(11) 1.3222(8) 0.2349(7) 0.094(2) Uani 1 1 d . . . H43 H 0.5564 1.3914 0.2595 0.113 Uiso 1 1 calc R . . C25 C 0.5931(8) 1.2558(7) 0.7680(5) 0.0540(15) Uani 1 1 d . . . C13 C 0.9570(8) 0.6802(7) -0.0609(5) 0.0578(15) Uani 1 1 d . . . C12 C 0.8649(7) 0.6802(5) 0.0067(5) 0.0486(13) Uani 1 1 d . . . C24 C 0.6863(7) 1.2515(6) 0.7052(5) 0.0542(14) Uani 1 1 d . . . H24 H 0.7894 1.3231 0.7282 0.065 Uiso 1 1 calc R . . O8 O 1.5366(4) 1.6133(3) 0.5731(3) 0.0723(9) Uani 1 1 d . . . C27 C 0.3830(7) 1.0451(6) 0.6418(5) 0.0545(14) Uani 1 1 d . . . C37 C 0.2909(5) 0.5316(4) 0.1679(4) 0.0402(10) Uani 1 1 d . . . C30 C 0.3872(4) 0.7927(3) 0.2932(3) 0.0410(8) Uani 1 1 d . . . C31 C 0.1737(4) 0.5817(4) 0.1860(4) 0.0469(8) Uani 1 1 d . . . C15 C 1.1629(7) 0.8964(6) 0.0605(5) 0.0501(13) Uani 1 1 d . . . C22 C 0.8965(7) 0.7995(6) 0.5349(5) 0.0592(14) Uani 1 1 d . . . C1 C 1.0700(4) 1.1600(4) 0.4760(3) 0.0366(8) Uani 1 1 d . . . C21 C 0.9299(9) 0.7318(7) 0.6171(6) 0.0700(17) Uani 1 1 d . . . C41 C 0.6129(9) 1.1977(8) 0.0954(6) 0.0739(19) Uani 1 1 d . . . C20 C 0.9837(11) 0.6419(9) 0.5870(8) 0.091(3) Uani 1 1 d . . . C42 C 0.5733(8) 1.2925(7) 0.1239(7) 0.077(2) Uani 1 1 d . . . O3 O 1.2905(4) 1.2614(3) 0.4059(3) 0.0508(9) Uani 1 1 d . . . C9 C 1.3284(5) 1.3927(4) 0.4697(4) 0.0490(9) Uani 1 1 d . . . C10 C 1.1229(4) 1.1778(3) 0.3693(3) 0.0404(8) Uani 1 1 d . . . C39 C 0.5155(4) 0.7534(4) 0.2808(3) 0.0359(8) Uani 1 1 d . . . C40 C 0.6467(9) 1.1298(8) 0.1764(6) 0.0647(18) Uani 1 1 d . . . C18 C 0.9665(7) 0.7003(6) 0.4029(5) 0.0590(13) Uani 1 1 d . . . C19 C 1.0044(10) 0.6264(7) 0.4792(7) 0.086(2) Uani 1 1 d . . . O9 O -0.0435(3) 0.3641(3) 0.0771(3) 0.0741(9) Uani 1 1 d . . . C35 C 0.0965(7) 0.1531(6) -0.0739(5) 0.0753(15) Uani 1 1 d . . . H35A H 0.1884 0.2242 -0.0816 0.090 Uiso 1 1 calc R . . H35B H 0.1384 0.1223 -0.0054 0.090 Uiso 1 1 calc R . . C32 C 0.0219(7) 0.4661(7) 0.1827(7) 0.0677(18) Uani 1 1 d . . . C34 C -0.0121(7) 0.2098(6) -0.0487(6) 0.0708(16) Uani 1 1 d . . . C33 C 0.0700(6) 0.3203(5) 0.0627(5) 0.0557(13) Uani 1 1 d . . . C5 C 1.5184(9) 1.7472(6) 0.7273(7) 0.106(3) Uani 1 1 d . . . H5A H 1.4491 1.7732 0.6699 0.127 Uiso 1 1 calc R . . H5B H 1.6304 1.8099 0.7445 0.127 Uiso 1 1 calc R . . C6 C 1.4871(10) 1.7558(7) 0.8432(7) 0.122(3) Uani 1 1 d . . . H6A H 1.3705 1.7107 0.8219 0.147 Uiso 1 1 calc R . . H6B H 1.5321 1.7062 0.8900 0.147 Uiso 1 1 calc R . . C36 C 0.0100(9) 0.0380(6) -0.1874(5) 0.0853(18) Uani 1 1 d . . . H36A H -0.0849 -0.0306 -0.1827 0.128 Uiso 1 1 calc R . . H36B H 0.0817 0.0019 -0.1945 0.128 Uiso 1 1 calc R . . H36C H -0.0214 0.0699 -0.2568 0.128 Uiso 1 1 calc R . . C7 C 1.5461(16) 1.8772(11) 0.9136(10) 0.201(6) Uani 1 1 d . . . H7A H 1.6610 1.9125 0.9567 0.302 Uiso 1 1 calc R . . H7B H 1.4941 1.8726 0.9703 0.302 Uiso 1 1 calc R . . H7C H 1.5261 1.9347 0.8649 0.302 Uiso 1 1 calc R . . O4 O 1.0650(4) 1.2903(3) 0.6492(2) 0.0572(7) Uani 1 1 d . . . O5 O 0.5439(4) 0.5875(3) 0.1517(3) 0.0550(7) Uani 1 1 d . . . O13 O 1.1112(6) 1.5055(5) 0.8222(4) 0.0951(14) Uani 1 1 d . . . O14 O 0.4254(9) 0.4295(7) -0.1074(6) 0.142(2) Uani 1 1 d . . . H26 H 0.383(6) 1.152(5) 0.778(4) 0.057(15) Uiso 1 1 d . . . H17 H 1.237(5) 1.104(4) 0.234(3) 0.041(11) Uiso 1 1 d . . . H12 H 0.775(5) 0.617(4) -0.015(4) 0.053(12) Uiso 1 1 d . . . H18' H 1.346(4) 1.360(3) 0.636(3) 0.033(8) Uiso 1 1 d . . . H15 H 1.237(5) 0.964(4) 0.072(3) 0.027(10) Uiso 1 1 d . . . H27 H 0.266(5) 0.974(4) 0.609(3) 0.037(10) Uiso 1 1 d . . . H25 H 0.635(7) 1.318(6) 0.832(5) 0.070(19) Uiso 1 1 d . . . H13 H 0.929(5) 0.612(5) -0.121(4) 0.038(13) Uiso 1 1 d . . . H29 H 0.314(5) 0.864(4) 0.469(3) 0.033(11) Uiso 1 1 d . . . H22 H 0.885(5) 0.885(4) 0.561(3) 0.048(12) Uiso 1 1 d . . . H32A H 0.062(6) 0.455(5) 0.245(4) 0.046(15) Uiso 1 1 d . . . H38 H 0.419(4) 0.663(4) 0.095(3) 0.044(10) Uiso 1 1 d . . . H44 H 0.617(6) 1.263(5) 0.374(4) 0.052(15) Uiso 1 1 d . . . H8A H 1.527(5) 1.506(4) 0.434(4) 0.050(11) Uiso 1 1 d . . . H20 H 0.993(6) 0.605(5) 0.618(4) 0.037(14) Uiso 1 1 d . . . H31 H 0.141(4) 0.611(3) 0.125(3) 0.044(10) Uiso 1 1 d . . . H4 H 1.550(4) 1.574(3) 0.731(3) 0.043(10) Uiso 1 1 d . . . H37 H 0.329(4) 0.487(3) 0.246(3) 0.041(9) Uiso 1 1 d . . . H18 H 0.978(6) 0.693(5) 0.319(4) 0.077(16) Uiso 1 1 d . . . H21 H 0.910(6) 0.741(5) 0.696(5) 0.085(17) Uiso 1 1 d . . . H34A H -0.103(6) 0.157(5) -0.064(4) 0.062(13) Uiso 1 1 d . . . H19 H 1.057(6) 0.579(5) 0.462(5) 0.097(16) Uiso 1 1 d . . . H32B H -0.046(5) 0.502(4) 0.197(4) 0.067(13) Uiso 1 1 d . . . H2 H 1.035(4) 1.331(3) 0.490(3) 0.030(8) Uiso 1 1 d . . . H9 H 1.275(4) 1.432(3) 0.410(3) 0.047(10) Uiso 1 1 d . . . H5C H 0.611(4) 0.640(4) 0.149(3) 0.033(11) Uiso 1 1 d . . . H1 H 1.132(4) 1.136(3) 0.531(3) 0.023(7) Uiso 1 1 d . . . H39 H 0.553(3) 0.718(3) 0.346(3) 0.025(7) Uiso 1 1 d . . . H10 H 1.069(4) 1.221(3) 0.313(3) 0.042(9) Uiso 1 1 d . . . H33 H 0.108(5) 0.297(4) 0.138(4) 0.053(11) Uiso 1 1 d . . . H14 H 1.168(7) 0.792(6) -0.078(5) 0.067(17) Uiso 1 1 d . . . H30 H 0.344(4) 0.822(3) 0.221(3) 0.031(8) Uiso 1 1 d . . . H34B H -0.059(6) 0.227(4) -0.120(4) 0.065(14) Uiso 1 1 d . . . H4A H 0.974(6) 1.245(5) 0.633(4) 0.072(15) Uiso 1 1 d . . . H41 H 0.597(6) 1.156(5) 0.028(4) 0.057(14) Uiso 1 1 d . . . H40 H 0.675(5) 1.094(4) 0.172(4) 0.015(11) Uiso 1 1 d . . . H4' H 0.552(7) 1.332(6) 0.070(5) 0.09(2) Uiso 1 1 d . . . H8B H 1.589(6) 1.467(5) 0.573(5) 0.078(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0405(3) 0.0371(3) 0.0456(3) 0.0050(2) 0.0225(2) 0.0166(2) Cu2 0.0421(3) 0.0381(3) 0.0498(3) 0.0001(2) 0.0264(2) 0.0123(3) O2 0.0354(17) 0.0340(18) 0.0509(19) 0.0027(15) 0.0222(15) 0.0131(15) O1 0.0390(18) 0.0342(18) 0.058(2) -0.0017(16) 0.0256(16) 0.0066(15) O12 0.048(2) 0.048(2) 0.056(2) -0.0048(18) 0.0292(18) 0.0128(19) O11 0.045(2) 0.050(2) 0.049(2) -0.0005(17) 0.0259(17) 0.0133(19) O6 0.0324(16) 0.0493(19) 0.0480(18) -0.0002(15) 0.0192(14) 0.0098(15) O10 0.0449(16) 0.0393(15) 0.0425(15) 0.0027(12) 0.0157(12) 0.0139(13) N1 0.0386(18) 0.0374(18) 0.0418(19) 0.0053(15) 0.0209(15) 0.0131(15) N2 0.0420(19) 0.045(2) 0.046(2) 0.0062(16) 0.0216(16) 0.0207(17) O7 0.0413(16) 0.0366(15) 0.0549(18) -0.0034(13) 0.0208(14) 0.0049(13) C23 0.053(3) 0.052(3) 0.028(2) 0.008(2) 0.016(2) 0.034(3) C11 0.045(3) 0.047(3) 0.049(3) 0.012(2) 0.026(2) 0.023(3) C38 0.038(2) 0.035(2) 0.043(3) 0.010(2) 0.022(2) 0.018(2) N4 0.063(3) 0.045(2) 0.056(3) 0.017(2) 0.029(2) 0.028(2) C2 0.044(3) 0.043(3) 0.038(2) 0.004(2) 0.018(2) 0.013(2) C16 0.048(3) 0.050(3) 0.037(2) 0.010(2) 0.021(2) 0.030(2) N3 0.045(2) 0.049(3) 0.049(2) 0.0084(19) 0.0191(19) 0.023(2) C28 0.040(3) 0.054(3) 0.044(3) 0.011(2) 0.020(2) 0.025(2) C4 0.059(3) 0.054(3) 0.066(3) -0.006(3) 0.027(3) 0.006(3) C29 0.041(3) 0.051(3) 0.051(3) 0.010(2) 0.022(2) 0.021(2) C17 0.038(2) 0.046(2) 0.041(2) 0.0119(19) 0.0207(18) 0.016(2) C8 0.055(3) 0.064(3) 0.061(3) -0.006(3) 0.033(3) 0.004(3) C14 0.065(3) 0.073(4) 0.047(3) 0.014(3) 0.034(3) 0.040(3) C26 0.074(4) 0.090(5) 0.061(3) 0.013(3) 0.042(3) 0.052(4) C44 0.121(6) 0.068(4) 0.077(4) 0.025(3) 0.052(4) 0.060(4) C3 0.040(2) 0.038(2) 0.039(2) 0.0043(17) 0.0131(17) 0.0130(17) C43 0.149(7) 0.090(5) 0.099(5) 0.050(4) 0.064(5) 0.088(5) C25 0.062(4) 0.066(4) 0.039(3) -0.001(3) 0.022(3) 0.037(3) C13 0.071(4) 0.064(4) 0.040(3) 0.005(3) 0.021(3) 0.035(3) C12 0.051(3) 0.043(3) 0.047(3) -0.004(2) 0.018(2) 0.022(3) C24 0.052(3) 0.061(3) 0.051(3) 0.014(3) 0.022(3) 0.026(3) O8 0.0660(19) 0.0487(17) 0.082(2) -0.0009(15) 0.0443(18) 0.0014(15) C27 0.050(3) 0.067(4) 0.052(3) 0.008(3) 0.025(2) 0.031(3) C37 0.0364(19) 0.037(2) 0.040(2) 0.0060(17) 0.0120(16) 0.0136(16) C30 0.0387(19) 0.0402(19) 0.043(2) 0.0046(16) 0.0175(16) 0.0176(16) C31 0.0388(19) 0.046(2) 0.049(2) 0.0080(18) 0.0159(16) 0.0144(17) C15 0.047(3) 0.059(3) 0.054(3) 0.017(3) 0.030(2) 0.025(3) C22 0.069(3) 0.063(4) 0.058(3) 0.010(3) 0.030(3) 0.041(3) C1 0.0369(18) 0.0376(19) 0.037(2) 0.0095(16) 0.0176(16) 0.0161(16) C21 0.081(4) 0.073(4) 0.056(4) 0.023(3) 0.027(3) 0.034(4) C41 0.081(5) 0.088(5) 0.062(4) 0.030(4) 0.037(4) 0.039(4) C20 0.113(6) 0.087(6) 0.093(6) 0.056(5) 0.042(5) 0.056(5) C42 0.073(4) 0.073(4) 0.092(5) 0.048(4) 0.027(4) 0.039(4) O3 0.0454(19) 0.0416(18) 0.059(2) 0.0008(16) 0.0291(16) 0.0108(16) C9 0.047(2) 0.0402(19) 0.049(2) 0.0051(17) 0.0222(18) 0.0092(17) C10 0.0380(18) 0.0372(18) 0.041(2) 0.0042(15) 0.0179(15) 0.0118(16) C39 0.0347(18) 0.0341(18) 0.039(2) 0.0115(16) 0.0138(15) 0.0155(15) C40 0.072(4) 0.070(4) 0.066(4) 0.024(3) 0.033(3) 0.040(4) C18 0.072(3) 0.063(3) 0.064(3) 0.022(3) 0.038(3) 0.042(3) C19 0.115(5) 0.082(5) 0.100(5) 0.033(4) 0.050(4) 0.072(4) O9 0.0405(15) 0.0560(17) 0.094(2) -0.0165(16) 0.0240(16) 0.0038(13) C35 0.080(3) 0.055(3) 0.072(3) 0.007(2) 0.016(3) 0.024(3) C32 0.038(3) 0.058(3) 0.082(4) -0.005(3) 0.025(3) 0.004(3) C34 0.047(3) 0.056(3) 0.077(4) -0.009(3) 0.016(3) 0.005(3) C33 0.043(3) 0.040(3) 0.063(3) 0.007(2) 0.021(2) 0.002(2) C5 0.085(4) 0.057(3) 0.132(6) -0.027(4) 0.066(4) -0.011(3) C6 0.115(5) 0.079(4) 0.141(6) -0.029(5) 0.070(5) 0.015(4) C36 0.113(5) 0.042(3) 0.088(4) -0.005(3) 0.033(4) 0.033(3) C7 0.197(12) 0.146(9) 0.160(9) -0.032(8) 0.098(9) -0.017(8) O4 0.0558(17) 0.0533(16) 0.0507(16) -0.0007(12) 0.0329(14) 0.0089(14) O5 0.0470(15) 0.0343(14) 0.084(2) 0.0029(13) 0.0356(15) 0.0150(13) O13 0.115(4) 0.085(3) 0.086(3) 0.003(3) 0.044(3) 0.047(3) O14 0.174(6) 0.151(6) 0.132(5) 0.059(5) 0.071(4) 0.089(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O11 1.925(4) . ? Cu1 N2 1.939(4) . ? Cu1 O1 1.957(4) . ? Cu1 O2 1.977(3) . ? Cu1 N4 2.291(4) . ? Cu1 Cu2 3.0090(7) . ? Cu2 O12 1.906(4) . ? Cu2 O1 1.941(3) . ? Cu2 N1 1.968(4) . ? Cu2 O2 1.989(4) . ? Cu2 N3 2.263(4) . ? O2 C39 1.397(5) . ? O1 C1 1.392(5) . ? O12 C11 1.301(6) . ? O11 C23 1.326(6) . ? O6 C30 1.423(5) . ? O6 C31 1.441(5) . ? O10 C33 1.400(6) . ? O10 C37 1.434(5) . ? N1 C17 1.280(5) . ? N1 C10 1.465(5) . ? N2 C29 1.279(6) . ? N2 C30 1.447(5) . ? O7 C4 1.418(7) . ? O7 C3 1.423(5) . ? C23 C24 1.389(7) . ? C23 C28 1.397(7) . ? C11 C12 1.427(7) . ? C11 C16 1.427(7) . ? C38 O5 1.404(5) . ? C38 C37 1.509(6) . ? C38 C39 1.522(6) . ? C38 H38 0.89(4) . ? N4 C40 1.306(8) . ? N4 C44 1.318(7) . ? C2 O4 1.417(6) . ? C2 C1 1.511(6) . ? C2 C3 1.523(7) . ? C2 H2 1.00(3) . ? C16 C15 1.420(7) . ? C16 C17 1.432(7) . ? N3 C22 1.326(7) . ? N3 C18 1.333(6) . ? C28 C27 1.413(7) . ? C28 C29 1.442(7) . ? C4 O8 1.407(7) . ? C4 C5 1.513(8) . ? C4 H4 1.02(4) . ? C29 H29 0.85(4) . ? C17 H17 0.96(4) . ? C8 O8 1.441(7) . ? C8 C9 1.495(7) . ? C8 H8A 1.05(4) . ? C8 H8B 1.00(5) . ? C14 C15 1.345(8) . ? C14 C13 1.402(9) . ? C14 H14 0.91(6) . ? C26 C27 1.369(8) . ? C26 C25 1.370(9) . ? C26 H26 0.84(5) . ? C44 C43 1.334(9) . ? C44 H44 0.74(4) . ? C3 C9 1.514(6) . ? C3 H18 0.98(3) . ? C43 C42 1.323(10) . ? C43 H43 0.9300 . ? C25 C24 1.357(7) . ? C25 H25 0.84(6) . ? C13 C12 1.382(7) . ? C13 H13 0.88(5) . ? C12 H12 0.81(4) . ? C24 H24 0.9300 . ? C27 H27 1.01(4) . ? C37 C31 1.523(6) . ? C37 H37 1.15(3) . ? C30 C39 1.527(5) . ? C30 H30 1.00(3) . ? C31 C32 1.513(7) . ? C31 H31 0.86(4) . ? C15 H15 0.78(4) . ? C22 C21 1.357(8) . ? C22 H22 1.04(4) . ? C1 C10 1.526(5) . ? C1 H1 0.89(3) . ? C21 C20 1.381(10) . ? C21 H21 1.03(5) . ? C41 C42 1.324(9) . ? C41 C40 1.349(9) . ? C41 H41 0.83(5) . ? C20 C19 1.376(11) . ? C20 H20 0.60(4) . ? C42 H4 0.85(5) . ? O3 C10 1.406(5) . ? O3 C9 1.439(5) . ? C9 H9 1.01(4) . ? C10 H10 1.02(3) . ? C39 H39 0.96(3) . ? C40 H40 0.58(4) . ? C18 C19 1.374(9) . ? C18 H18 1.04(5) . ? C19 H19 0.93(5) . ? O9 C32 1.395(7) . ? O9 C33 1.428(6) . ? C35 C36 1.515(7) . ? C35 C34 1.525(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C32 H32A 0.79(4) . ? C32 H32B 0.96(5) . ? C34 C33 1.475(8) . ? C34 H34A 0.79(5) . ? C34 H34B 0.92(5) . ? C33 H33 0.98(4) . ? C5 C6 1.517(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.322(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? O4 H4A 0.77(5) . ? O5 H5C 0.70(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Cu1 N2 93.61(16) . . ? O11 Cu1 O1 98.49(15) . . ? N2 Cu1 O1 152.71(14) . . ? O11 Cu1 O2 169.91(16) . . ? N2 Cu1 O2 83.74(15) . . ? O1 Cu1 O2 80.08(13) . . ? O11 Cu1 N4 94.26(16) . . ? N2 Cu1 N4 103.31(16) . . ? O1 Cu1 N4 100.09(15) . . ? O2 Cu1 N4 95.83(15) . . ? O11 Cu1 Cu2 137.10(11) . . ? N2 Cu1 Cu2 121.59(11) . . ? O1 Cu1 Cu2 39.27(10) . . ? O2 Cu1 Cu2 40.81(10) . . ? N4 Cu1 Cu2 99.80(11) . . ? O12 Cu2 O1 172.96(19) . . ? O12 Cu2 N1 92.06(15) . . ? O1 Cu2 N1 85.11(16) . . ? O12 Cu2 O2 98.77(15) . . ? O1 Cu2 O2 80.18(14) . . ? N1 Cu2 O2 145.44(14) . . ? O12 Cu2 N3 92.35(16) . . ? O1 Cu2 N3 94.69(15) . . ? N1 Cu2 N3 112.88(15) . . ? O2 Cu2 N3 99.43(14) . . ? O12 Cu2 Cu1 138.73(11) . . ? O1 Cu2 Cu1 39.67(11) . . ? N1 Cu2 Cu1 118.12(11) . . ? O2 Cu2 Cu1 40.51(10) . . ? N3 Cu2 Cu1 99.86(10) . . ? C39 O2 Cu1 109.6(3) . . ? C39 O2 Cu2 130.9(3) . . ? Cu1 O2 Cu2 98.67(15) . . ? C1 O1 Cu2 111.4(3) . . ? C1 O1 Cu1 144.3(3) . . ? Cu2 O1 Cu1 101.05(15) . . ? C11 O12 Cu2 128.5(3) . . ? C23 O11 Cu1 126.1(3) . . ? C30 O6 C31 108.0(3) . . ? C33 O10 C37 111.2(4) . . ? C17 N1 C10 122.8(4) . . ? C17 N1 Cu2 127.3(3) . . ? C10 N1 Cu2 109.2(2) . . ? C29 N2 C30 123.4(4) . . ? C29 N2 Cu1 126.2(4) . . ? C30 N2 Cu1 110.4(3) . . ? C4 O7 C3 109.9(4) . . ? O11 C23 C24 117.6(5) . . ? O11 C23 C28 124.9(4) . . ? C24 C23 C28 117.5(5) . . ? O12 C11 C12 118.9(5) . . ? O12 C11 C16 123.7(5) . . ? C12 C11 C16 117.3(5) . . ? O5 C38 C37 108.2(4) . . ? O5 C38 C39 114.5(3) . . ? C37 C38 C39 107.0(4) . . ? O5 C38 H38 98(2) . . ? C37 C38 H38 110(2) . . ? C39 C38 H38 118(2) . . ? C40 N4 C44 113.9(5) . . ? C40 N4 Cu1 121.2(4) . . ? C44 N4 Cu1 124.8(4) . . ? O4 C2 C1 113.1(4) . . ? O4 C2 C3 109.6(4) . . ? C1 C2 C3 106.4(4) . . ? O4 C2 H2 108.5(19) . . ? C1 C2 H2 110.9(18) . . ? C3 C2 H2 108.1(18) . . ? C15 C16 C11 118.3(5) . . ? C15 C16 C17 117.6(5) . . ? C11 C16 C17 123.9(5) . . ? C22 N3 C18 117.0(5) . . ? C22 N3 Cu2 122.2(3) . . ? C18 N3 Cu2 120.6(3) . . ? C23 C28 C27 119.1(5) . . ? C23 C28 C29 123.4(5) . . ? C27 C28 C29 117.5(5) . . ? O8 C4 O7 111.2(5) . . ? O8 C4 C5 107.9(5) . . ? O7 C4 C5 107.6(5) . . ? O8 C4 H4 109(2) . . ? O7 C4 H4 110(2) . . ? C5 C4 H4 111(2) . . ? N2 C29 C28 125.6(5) . . ? N2 C29 H29 122(3) . . ? C28 C29 H29 112(3) . . ? N1 C17 C16 124.0(5) . . ? N1 C17 H17 113(2) . . ? C16 C17 H17 123(2) . . ? O8 C8 C9 107.2(4) . . ? O8 C8 H8A 99(2) . . ? C9 C8 H8A 105(2) . . ? O8 C8 H8B 102(3) . . ? C9 C8 H8B 122(3) . . ? H8A C8 H8B 119(4) . . ? C15 C14 C13 119.2(6) . . ? C15 C14 H14 120(4) . . ? C13 C14 H14 121(4) . . ? C27 C26 C25 118.7(6) . . ? C27 C26 H26 119(4) . . ? C25 C26 H26 122(4) . . ? N4 C44 C43 124.8(6) . . ? N4 C44 H44 110(4) . . ? C43 C44 H44 125(4) . . ? O7 C3 C9 107.6(3) . . ? O7 C3 C2 110.5(4) . . ? C9 C3 C2 112.3(4) . . ? O7 C3 H18 108.9(18) . . ? C9 C3 H18 108.3(18) . . ? C2 C3 H18 109.1(19) . . ? C42 C43 C44 119.5(7) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? C24 C25 C26 120.9(6) . . ? C24 C25 H25 118(4) . . ? C26 C25 H25 120(4) . . ? C12 C13 C14 120.3(6) . . ? C12 C13 H13 124(3) . . ? C14 C13 H13 115(3) . . ? C13 C12 C11 121.6(5) . . ? C13 C12 H12 118(3) . . ? C11 C12 H12 121(3) . . ? C25 C24 C23 122.4(6) . . ? C25 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? C4 O8 C8 111.7(4) . . ? C26 C27 C28 121.4(6) . . ? C26 C27 H27 121(2) . . ? C28 C27 H27 117(2) . . ? O10 C37 C38 111.3(4) . . ? O10 C37 C31 107.2(3) . . ? C38 C37 C31 112.3(4) . . ? O10 C37 H37 108.5(16) . . ? C38 C37 H37 108.4(16) . . ? C31 C37 H37 109.1(16) . . ? O6 C30 N2 113.2(3) . . ? O6 C30 C39 112.3(3) . . ? N2 C30 C39 106.3(3) . . ? O6 C30 H30 106.9(17) . . ? N2 C30 H30 108.5(17) . . ? C39 C30 H30 109.5(17) . . ? O6 C31 C32 110.8(4) . . ? O6 C31 C37 110.0(3) . . ? C32 C31 C37 110.1(4) . . ? O6 C31 H31 112(2) . . ? C32 C31 H31 105(2) . . ? C37 C31 H31 108(2) . . ? C14 C15 C16 123.2(6) . . ? C14 C15 H15 123(3) . . ? C16 C15 H15 113(3) . . ? N3 C22 C21 125.1(5) . . ? N3 C22 H22 113(2) . . ? C21 C22 H22 120(2) . . ? O1 C1 C2 115.5(4) . . ? O1 C1 C10 108.1(3) . . ? C2 C1 C10 108.7(3) . . ? O1 C1 H1 108.8(19) . . ? C2 C1 H1 103.9(18) . . ? C10 C1 H1 112.0(18) . . ? C22 C21 C20 116.9(6) . . ? C22 C21 H21 122(3) . . ? C20 C21 H21 121(3) . . ? C42 C41 C40 119.7(7) . . ? C42 C41 H41 130(3) . . ? C40 C41 H41 108(3) . . ? C19 C20 C21 120.1(7) . . ? C19 C20 H20 118(5) . . ? C21 C20 H20 122(5) . . ? C43 C42 C41 117.9(6) . . ? C43 C42 H4 126(4) . . ? C41 C42 H4 116(4) . . ? C10 O3 C9 108.5(3) . . ? O3 C9 C8 109.8(4) . . ? O3 C9 C3 112.0(3) . . ? C8 C9 C3 108.9(4) . . ? O3 C9 H9 108(2) . . ? C8 C9 H9 105(2) . . ? C3 C9 H9 113(2) . . ? O3 C10 N1 111.8(3) . . ? O3 C10 C1 112.6(3) . . ? N1 C10 C1 108.3(3) . . ? O3 C10 H10 104.4(19) . . ? N1 C10 H10 105.7(18) . . ? C1 C10 H10 113.8(19) . . ? O2 C39 C38 113.0(3) . . ? O2 C39 C30 105.7(3) . . ? C38 C39 C30 109.8(3) . . ? O2 C39 H39 110.7(17) . . ? C38 C39 H39 106.4(17) . . ? C30 C39 H39 111.3(18) . . ? N4 C40 C41 124.1(7) . . ? N4 C40 H40 110(4) . . ? C41 C40 H40 125(4) . . ? N3 C18 C19 123.0(6) . . ? N3 C18 H18 115(3) . . ? C19 C18 H18 122(3) . . ? C18 C19 C20 118.0(6) . . ? C18 C19 H19 119(3) . . ? C20 C19 H19 122(3) . . ? C32 O9 C33 113.0(4) . . ? C36 C35 C34 113.5(5) . . ? C36 C35 H35A 108.9 . . ? C34 C35 H35A 108.9 . . ? C36 C35 H35B 108.9 . . ? C34 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? O9 C32 C31 109.6(5) . . ? O9 C32 H32A 119(4) . . ? C31 C32 H32A 97(4) . . ? O9 C32 H32B 118(3) . . ? C31 C32 H32B 107(3) . . ? H32A C32 H32B 104(4) . . ? C33 C34 C35 114.0(5) . . ? C33 C34 H34A 118(3) . . ? C35 C34 H34A 115(3) . . ? C33 C34 H34B 117(3) . . ? C35 C34 H34B 105(3) . . ? H34A C34 H34B 82(4) . . ? O10 C33 O9 110.2(4) . . ? O10 C33 C34 110.7(5) . . ? O9 C33 C34 108.8(4) . . ? O10 C33 H33 107(2) . . ? O9 C33 H33 104(2) . . ? C34 C33 H33 116(2) . . ? C4 C5 C6 112.1(6) . . ? C4 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? C4 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C7 C6 C5 116.8(8) . . ? C7 C6 H6A 108.1 . . ? C5 C6 H6A 108.1 . . ? C7 C6 H6B 108.1 . . ? C5 C6 H6B 108.1 . . ? H6A C6 H6B 107.3 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 O4 H4A 111(4) . . ? C38 O5 H5C 106(3) . . ?