# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Yue-Qing Zheng' _publ_contact_author_email ZHENGYUEQING@NBU.EDU.CN _publ_section_title ; New Cu(II) complexes based on the hydroxo-bridged dinuclear [Cu(OH)2Cu] units: step-like di- and trimerizations of [Cu(OH)2Cu] units ; loop_ _publ_author_name 'Yue-Qing Zheng' 'De-Yi Cheng' 'Jian-Li Lin' 'Wei Xu' #================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 725663' #TrackingRef '_CuOH_n1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H62 Cu4 N10 O24' _chemical_formula_weight 1383.05 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 0.2630 1.2660 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2992(19) _cell_length_b 15.585(3) _cell_length_c 19.286(4) _cell_angle_alpha 91.20(3) _cell_angle_beta 100.97(3) _cell_angle_gamma 93.38(3) _cell_volume 2737.8(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17436 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 1.592 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.42 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26321 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11846 _reflns_number_gt 7767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku,1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC,2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Johnson,1976)' _computing_publication_material SHELXTL97 _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^)+(0.0750P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11846 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 0.30989(4) 0.62995(2) 0.354940(19) 0.02348(10) Uani 1 1 d . . . Cu2 Cu 0.10552(4) 0.69412(2) 0.236260(19) 0.02341(10) Uani 1 1 d . . . Cu3 Cu 0.41065(4) 0.80253(2) 0.259895(19) 0.02392(10) Uani 1 1 d . . . Cu4 Cu 0.20945(4) 0.86513(2) 0.137871(19) 0.02435(10) Uani 1 1 d . . . O1 O 0.2057(2) 0.59267(13) 0.26252(11) 0.0275(5) Uani 1 1 d . . . H1 H 0.1418 0.5507 0.2586 0.033 Uiso 1 1 d . . . O2 O 0.2406(2) 0.74102(13) 0.32149(11) 0.0256(4) Uani 1 1 d . . . H2 H 0.2100 0.7727 0.3475 0.031 Uiso 1 1 d . . . O3 O 0.2752(2) 0.75475(13) 0.17646(10) 0.0229(4) Uani 1 1 d . . . H3 H 0.3044 0.7206 0.1521 0.027 Uiso 1 1 d . . . O4 O 0.3199(2) 0.90569(14) 0.22773(12) 0.0338(5) Uani 1 1 d . . . H4 H 0.3748 0.9489 0.2377 0.041 Uiso 1 1 d . . . O5 O 0.1346(3) 0.57566(17) 0.41059(13) 0.0469(7) Uani 1 1 d . . . H5 H 0.0907 0.5991 0.4398 0.056 Uiso 1 1 d . . . H6 H 0.0863 0.5268 0.4028 0.056 Uiso 1 1 d . . . O6 O 0.3907(3) 0.88285(16) 0.07530(13) 0.0444(6) Uani 1 1 d . . . H8 H 0.4053 0.8541 0.0410 0.053 Uiso 1 1 d . . . H7 H 0.4131 0.9366 0.0743 0.053 Uiso 1 1 d . . . N6 N 0.5478(3) 0.85837(17) 0.34202(14) 0.0285(6) Uani 1 1 d . . . N5 N 0.5568(3) 0.71116(17) 0.27748(14) 0.0263(6) Uani 1 1 d . . . C1 C 0.4576(4) 0.7467(2) 0.47772(17) 0.0339(7) Uani 1 1 d . . . H1A H 0.3828 0.7834 0.4638 0.051 Uiso 1 1 calc R . . C2 C 0.5674(4) 0.7707(3) 0.5350(2) 0.0448(9) Uani 1 1 d . . . H2A H 0.5654 0.8221 0.5600 0.067 Uiso 1 1 calc R . . C3 C 0.6797(4) 0.7171(3) 0.5544(2) 0.0484(10) Uani 1 1 d . . . H3A H 0.7562 0.7330 0.5918 0.073 Uiso 1 1 calc R . . C4 C 0.6784(4) 0.6405(3) 0.51858(19) 0.0407(9) Uani 1 1 d . . . H4A H 0.7529 0.6034 0.5317 0.061 Uiso 1 1 calc R . . C5 C 0.5643(3) 0.6189(2) 0.46224(16) 0.0291(7) Uani 1 1 d . . . C6 C 0.5517(3) 0.5375(2) 0.42096(16) 0.0271(7) Uani 1 1 d . . . C7 C 0.6501(4) 0.4740(2) 0.43352(19) 0.0383(8) Uani 1 1 d . . . H7A H 0.7321 0.4814 0.4697 0.058 Uiso 1 1 calc R . . C8 C 0.6255(4) 0.3997(2) 0.3920(2) 0.0404(9) Uani 1 1 d . . . H8A H 0.6894 0.3557 0.4005 0.061 Uiso 1 1 calc R . . C9 C 0.5049(4) 0.3912(2) 0.3376(2) 0.0434(9) Uani 1 1 d . . . H9A H 0.4868 0.3420 0.3084 0.065 Uiso 1 1 calc R . . C10 C 0.4121(4) 0.4570(2) 0.32759(19) 0.0362(8) Uani 1 1 d . . . H10A H 0.3306 0.4513 0.2911 0.054 Uiso 1 1 calc R . . N8 N 0.0806(3) 0.96505(17) 0.12455(14) 0.0291(6) Uani 1 1 d . . . N7 N 0.0606(3) 0.81905(17) 0.05476(14) 0.0271(6) Uani 1 1 d . . . C11 C -0.0269(4) 0.5642(2) 0.12363(19) 0.0401(8) Uani 1 1 d . . . H11A H 0.0586 0.5357 0.1373 0.060 Uiso 1 1 calc R . . C12 C -0.1361(5) 0.5268(3) 0.0709(2) 0.0504(10) Uani 1 1 d . . . H12A H -0.1250 0.4744 0.0492 0.076 Uiso 1 1 calc R . . C13 C -0.2619(4) 0.5702(3) 0.0516(2) 0.0528(11) Uani 1 1 d . . . H13A H -0.3386 0.5459 0.0174 0.079 Uiso 1 1 calc R . . C14 C -0.2751(4) 0.6485(3) 0.08220(19) 0.0419(9) Uani 1 1 d . . . H14A H -0.3584 0.6787 0.0681 0.063 Uiso 1 1 calc R . . C15 C -0.1613(3) 0.6817(2) 0.13485(17) 0.0296(7) Uani 1 1 d . . . C16 C -0.1615(3) 0.7649(2) 0.17245(16) 0.0270(7) Uani 1 1 d . . . C17 C -0.2757(3) 0.8184(2) 0.16046(19) 0.0382(8) Uani 1 1 d . . . H17A H -0.3597 0.8029 0.1270 0.057 Uiso 1 1 calc R . . C18 C -0.2645(4) 0.8958(2) 0.19868(19) 0.0399(9) Uani 1 1 d . . . H18A H -0.3409 0.9326 0.1912 0.060 Uiso 1 1 calc R . . C19 C -0.1393(4) 0.9174(2) 0.2475(2) 0.0397(8) Uani 1 1 d . . . H19A H -0.1292 0.9690 0.2736 0.060 Uiso 1 1 calc R . . C20 C -0.0291(4) 0.8615(2) 0.25729(18) 0.0331(7) Uani 1 1 d . . . H20A H 0.0555 0.8762 0.2907 0.050 Uiso 1 1 calc R . . N2 N 0.4341(3) 0.52866(17) 0.36801(14) 0.0285(6) Uani 1 1 d . . . N1 N 0.4562(3) 0.67193(17) 0.44171(13) 0.0271(6) Uani 1 1 d . . . C21 C 0.5510(4) 0.6359(2) 0.24170(18) 0.0320(7) Uani 1 1 d . . . H21A H 0.4684 0.6200 0.2075 0.048 Uiso 1 1 calc R . . C22 C 0.6642(4) 0.5816(2) 0.2542(2) 0.0393(8) Uani 1 1 d . . . H22A H 0.6577 0.5295 0.2290 0.059 Uiso 1 1 calc R . . C23 C 0.7867(4) 0.6053(3) 0.3043(2) 0.0434(9) Uani 1 1 d . . . H23A H 0.8649 0.5699 0.3128 0.065 Uiso 1 1 calc R . . C24 C 0.7930(3) 0.6822(3) 0.34222(19) 0.0401(9) Uani 1 1 d . . . H24A H 0.8742 0.6983 0.3772 0.060 Uiso 1 1 calc R . . C25 C 0.6775(3) 0.7351(2) 0.32761(16) 0.0274(7) Uani 1 1 d . . . C26 C 0.6714(3) 0.8174(2) 0.36399(16) 0.0300(7) Uani 1 1 d . . . C27 C 0.7809(4) 0.8537(3) 0.41748(19) 0.0430(9) Uani 1 1 d . . . H27A H 0.8667 0.8258 0.4320 0.065 Uiso 1 1 calc R . . C28 C 0.7617(4) 0.9308(3) 0.4486(2) 0.0545(11) Uani 1 1 d . . . H28A H 0.8355 0.9563 0.4836 0.082 Uiso 1 1 calc R . . C29 C 0.6321(5) 0.9709(3) 0.4279(2) 0.0508(10) Uani 1 1 d . . . H29A H 0.6156 1.0221 0.4498 0.061 Uiso 1 1 calc R . . C30 C 0.5283(4) 0.9325(2) 0.3736(2) 0.0415(9) Uani 1 1 d . . . H30A H 0.4416 0.9593 0.3586 0.062 Uiso 1 1 calc R . . N4 N -0.0392(3) 0.63861(17) 0.15527(14) 0.0286(6) Uani 1 1 d . . . N3 N -0.0381(3) 0.78665(17) 0.22080(14) 0.0264(6) Uani 1 1 d . . . C31 C 0.0623(4) 0.7446(2) 0.02006(18) 0.0343(8) Uani 1 1 d . . . H31A H 0.1415 0.7108 0.0332 0.051 Uiso 1 1 calc R . . C32 C -0.0495(4) 0.7156(2) -0.0350(2) 0.0429(9) Uani 1 1 d . . . H32A H -0.0446 0.6640 -0.0593 0.064 Uiso 1 1 calc R . . C33 C -0.1686(4) 0.7651(3) -0.0528(2) 0.0452(9) Uani 1 1 d . . . H33A H -0.2469 0.7461 -0.0884 0.068 Uiso 1 1 calc R . . C34 C -0.1707(4) 0.8424(2) -0.01783(19) 0.0403(9) Uani 1 1 d . . . H34A H -0.2498 0.8767 -0.0296 0.060 Uiso 1 1 calc R . . C35 C -0.0531(3) 0.8686(2) 0.03540(17) 0.0284(7) Uani 1 1 d . . . C36 C -0.0427(3) 0.9509(2) 0.07518(17) 0.0272(7) Uani 1 1 d . . . C37 C -0.1491(4) 1.0096(2) 0.0645(2) 0.0381(8) Uani 1 1 d . . . H37A H -0.2334 0.9988 0.0301 0.057 Uiso 1 1 calc R . . C38 C -0.1291(4) 1.0849(2) 0.1055(2) 0.0449(9) Uani 1 1 d . . . H38A H -0.1990 1.1258 0.0986 0.067 Uiso 1 1 calc R . . C39 C -0.0048(4) 1.0982(2) 0.1565(2) 0.0464(9) Uani 1 1 d . . . H39A H 0.0096 1.1478 0.1853 0.070 Uiso 1 1 calc R . . C40 C 0.0983(4) 1.0378(2) 0.16487(19) 0.0372(8) Uani 1 1 d . . . H40A H 0.1828 1.0475 0.1993 0.056 Uiso 1 1 calc R . . O7 O -0.0146(3) 0.42111(18) 0.36082(14) 0.0526(7) Uani 1 1 d . . . O8 O 0.0254(3) 0.44644(16) 0.25458(14) 0.0471(6) Uani 1 1 d . . . C41 C -0.0355(4) 0.4051(2) 0.2964(2) 0.0350(8) Uani 1 1 d . . . C42 C -0.1474(4) 0.3320(3) 0.26535(19) 0.0438(9) Uani 1 1 d . . . H42A H -0.1014 0.2780 0.2741 0.066 Uiso 1 1 calc R . . H42B H -0.2283 0.3318 0.2905 0.066 Uiso 1 1 calc R . . C43 C -0.2093(4) 0.3356(2) 0.1869(2) 0.0464(9) Uani 1 1 d . . . H43A H -0.2361 0.3938 0.1764 0.070 Uiso 1 1 calc R . . H43B H -0.1326 0.3231 0.1611 0.070 Uiso 1 1 calc R . . C44 C -0.3404(4) 0.2751(2) 0.16018(19) 0.0414(9) Uani 1 1 d . . . H44A H -0.4195 0.2896 0.1837 0.062 Uiso 1 1 calc R . . H44B H -0.3156 0.2171 0.1726 0.062 Uiso 1 1 calc R . . C45 C -0.3946(3) 0.2770(2) 0.08037(18) 0.0339(8) Uani 1 1 d . . . O9 O -0.4114(3) 0.20792(17) 0.04599(14) 0.0515(7) Uani 1 1 d . . . O10 O -0.4190(3) 0.34901(18) 0.05436(14) 0.0519(7) Uani 1 1 d . . . N9 N 0.1169(4) 0.0703(3) 0.3645(2) 0.0607(10) Uani 1 1 d . . . O11 O 0.0806(4) 0.1435(2) 0.3477(2) 0.0880(11) Uani 1 1 d . . . O12 O 0.2272(5) 0.0439(3) 0.3501(3) 0.1226(17) Uani 1 1 d . . . O13 O 0.0401(4) 0.0251(3) 0.39570(19) 0.0916(13) Uani 1 1 d . . . N10 N 0.5820(4) 1.1107(2) 0.2783(2) 0.0578(9) Uani 1 1 d . . . O14 O 0.5783(4) 1.1646(2) 0.32542(19) 0.0793(10) Uani 1 1 d . . . O15 O 0.7007(5) 1.0822(3) 0.2735(2) 0.1135(16) Uani 1 1 d . . . O16 O 0.4707(4) 1.0877(3) 0.23428(19) 0.0905(13) Uani 1 1 d . . . OW1 O 0.1582(3) 0.8302(2) 0.56870(16) 0.0685(9) Uani 1 1 d . . . H9 H 0.1065 0.8544 0.5946 0.082 Uiso 1 1 d . . . H10 H 0.2276 0.8319 0.5963 0.082 Uiso 1 1 d . . . OW2 O 0.2111(3) 0.3692(2) 0.18141(15) 0.0627(8) Uani 1 1 d . . . H11 H 0.1400 0.3948 0.1970 0.075 Uiso 1 1 d . . . H12 H 0.2282 0.3354 0.2122 0.075 Uiso 1 1 d . . . OW3 O -0.5679(3) 0.46628(18) 0.12654(16) 0.0587(8) Uani 1 1 d . . . H13 H -0.6288 0.4407 0.1449 0.070 Uiso 1 1 d . . . H14 H -0.5282 0.4284 0.1055 0.070 Uiso 1 1 d . . . OW4 O 0.4805(3) 1.05472(18) 0.09143(15) 0.0564(7) Uani 1 1 d . . . H15 H 0.4862 1.0826 0.1320 0.068 Uiso 1 1 d . . . H16 H 0.5137 1.0923 0.0708 0.068 Uiso 1 1 d . . . OW5 O -0.0398(3) 0.33755(19) 0.48184(15) 0.0541(7) Uani 1 1 d . . . H17 H -0.0414 0.3617 0.4459 0.065 Uiso 1 1 d . . . H18 H -0.0759 0.2877 0.4668 0.065 Uiso 1 1 d . . . OW6 O 0.1626(4) 0.8581(2) 0.42667(16) 0.0690(9) Uani 1 1 d . . . H19 H 0.1647 0.8567 0.4694 0.083 Uiso 1 1 d . . . H20 H 0.1714 0.9081 0.4187 0.083 Uiso 1 1 d . . . OW7 O -0.3462(3) 0.37113(18) -0.07690(14) 0.0508(7) Uani 1 1 d . . . H21 H -0.3663 0.3551 -0.0404 0.061 Uiso 1 1 d . . . H22 H -0.3709 0.4189 -0.0909 0.061 Uiso 1 1 d . . . OW8 O 0.2642(4) 0.2208(2) 0.2583(2) 0.0845(11) Uani 1 1 d . . . H23 H 0.2324 0.1807 0.2835 0.101 Uiso 1 1 d . . . H24 H 0.3285 0.1887 0.2570 0.101 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 0.02391(19) 0.0243(2) 0.0199(2) 0.00181(15) -0.00248(14) 0.00369(14) Cu2 0.02283(19) 0.0224(2) 0.0223(2) 0.00193(15) -0.00281(14) 0.00236(14) Cu3 0.02293(19) 0.0229(2) 0.0233(2) 0.00032(15) -0.00258(14) 0.00289(14) Cu4 0.0252(2) 0.0229(2) 0.0228(2) 0.00164(16) -0.00208(15) 0.00493(14) O1 0.0300(11) 0.0232(11) 0.0263(12) 0.0012(9) -0.0022(9) 0.0023(8) O2 0.0277(11) 0.0247(11) 0.0224(11) -0.0017(9) -0.0007(8) 0.0049(8) O3 0.0268(10) 0.0213(11) 0.0191(11) 0.0003(8) 0.0003(8) 0.0035(8) O4 0.0362(12) 0.0254(12) 0.0334(13) -0.0009(10) -0.0099(10) 0.0051(9) O5 0.0429(14) 0.0588(18) 0.0403(15) -0.0081(13) 0.0168(12) -0.0125(12) O6 0.0482(14) 0.0453(16) 0.0418(15) -0.0025(12) 0.0169(12) -0.0050(11) N6 0.0266(13) 0.0300(15) 0.0268(15) 0.0000(12) 0.0006(11) -0.0014(10) N5 0.0240(13) 0.0302(15) 0.0233(14) 0.0028(11) 0.0004(10) 0.0034(10) C1 0.0411(18) 0.034(2) 0.0257(18) -0.0030(15) 0.0043(14) -0.0002(14) C2 0.056(2) 0.044(2) 0.031(2) -0.0048(17) 0.0048(17) -0.0080(18) C3 0.042(2) 0.063(3) 0.035(2) -0.006(2) -0.0034(16) -0.0053(18) C4 0.0294(18) 0.056(2) 0.033(2) -0.0010(18) -0.0035(14) 0.0002(15) C5 0.0264(16) 0.0387(19) 0.0215(16) 0.0048(14) 0.0034(12) -0.0013(13) C6 0.0262(16) 0.0327(18) 0.0221(16) 0.0038(13) 0.0038(12) 0.0020(12) C7 0.0319(18) 0.049(2) 0.034(2) 0.0106(17) 0.0014(14) 0.0111(15) C8 0.0390(19) 0.043(2) 0.042(2) 0.0077(17) 0.0107(16) 0.0190(15) C9 0.049(2) 0.032(2) 0.049(2) -0.0037(17) 0.0081(18) 0.0100(16) C10 0.0378(19) 0.035(2) 0.0323(19) -0.0072(15) -0.0041(14) 0.0070(14) N8 0.0282(14) 0.0284(15) 0.0297(15) 0.0063(12) 0.0012(11) 0.0071(11) N7 0.0258(13) 0.0297(15) 0.0240(14) 0.0029(11) -0.0001(10) 0.0036(10) C11 0.049(2) 0.034(2) 0.033(2) 0.0022(16) -0.0038(16) 0.0038(15) C12 0.069(3) 0.039(2) 0.034(2) -0.0050(18) -0.0106(18) -0.0070(19) C13 0.048(2) 0.056(3) 0.044(2) 0.000(2) -0.0132(18) -0.0135(19) C14 0.0337(19) 0.050(2) 0.037(2) 0.0001(18) -0.0055(15) -0.0032(15) C15 0.0245(16) 0.038(2) 0.0249(17) 0.0057(14) 0.0014(12) -0.0002(13) C16 0.0226(15) 0.0352(18) 0.0234(16) 0.0073(14) 0.0042(12) 0.0018(12) C17 0.0249(17) 0.050(2) 0.039(2) 0.0128(17) 0.0030(14) 0.0079(14) C18 0.0359(19) 0.046(2) 0.041(2) 0.0077(18) 0.0100(16) 0.0185(15) C19 0.044(2) 0.038(2) 0.041(2) 0.0036(17) 0.0154(17) 0.0088(15) C20 0.0356(18) 0.0320(19) 0.0317(19) 0.0019(15) 0.0048(14) 0.0065(13) N2 0.0257(13) 0.0318(15) 0.0263(15) 0.0032(12) -0.0008(11) 0.0059(10) N1 0.0252(13) 0.0332(16) 0.0213(14) 0.0040(11) 0.0004(10) 0.0006(10) C21 0.0346(17) 0.0300(19) 0.0315(19) 0.0031(15) 0.0056(14) 0.0058(13) C22 0.047(2) 0.035(2) 0.041(2) 0.0085(16) 0.0159(17) 0.0118(15) C23 0.037(2) 0.050(2) 0.047(2) 0.0105(19) 0.0102(17) 0.0214(16) C24 0.0255(17) 0.058(2) 0.037(2) 0.0143(18) 0.0014(14) 0.0088(15) C25 0.0216(15) 0.0371(19) 0.0246(17) 0.0065(14) 0.0066(12) 0.0015(12) C26 0.0252(16) 0.041(2) 0.0221(17) 0.0048(14) 0.0025(12) -0.0043(13) C27 0.0334(19) 0.055(3) 0.036(2) -0.0052(18) -0.0029(15) -0.0067(16) C28 0.050(2) 0.065(3) 0.039(2) -0.006(2) -0.0058(18) -0.022(2) C29 0.070(3) 0.036(2) 0.041(2) -0.0084(18) 0.003(2) -0.0100(19) C30 0.047(2) 0.037(2) 0.037(2) -0.0037(17) 0.0021(16) -0.0007(16) N4 0.0302(14) 0.0286(15) 0.0246(14) 0.0035(11) -0.0013(11) 0.0014(11) N3 0.0256(13) 0.0288(15) 0.0243(14) 0.0046(11) 0.0021(10) 0.0042(10) C31 0.0416(19) 0.0326(19) 0.0279(18) -0.0033(15) 0.0029(14) 0.0091(14) C32 0.049(2) 0.041(2) 0.034(2) -0.0073(17) -0.0019(16) 0.0027(16) C33 0.037(2) 0.056(3) 0.036(2) -0.0071(19) -0.0079(16) 0.0060(17) C34 0.0319(18) 0.051(2) 0.035(2) -0.0002(17) -0.0052(14) 0.0098(15) C35 0.0267(16) 0.0335(19) 0.0255(17) 0.0053(14) 0.0048(13) 0.0059(12) C36 0.0275(16) 0.0286(18) 0.0253(17) 0.0061(14) 0.0030(13) 0.0048(12) C37 0.0339(18) 0.038(2) 0.042(2) 0.0065(17) 0.0021(15) 0.0132(14) C38 0.041(2) 0.039(2) 0.058(3) 0.0067(19) 0.0113(18) 0.0182(16) C39 0.056(2) 0.028(2) 0.054(3) -0.0050(18) 0.0066(19) 0.0103(16) C40 0.0426(19) 0.0260(19) 0.040(2) -0.0054(15) -0.0014(15) 0.0066(14) O7 0.0653(17) 0.0524(18) 0.0361(16) -0.0018(13) 0.0059(13) -0.0149(14) O8 0.0557(15) 0.0381(15) 0.0464(16) -0.0003(12) 0.0122(13) -0.0138(12) C41 0.0391(18) 0.0262(18) 0.040(2) -0.0020(15) 0.0082(15) 0.0043(14) C42 0.053(2) 0.044(2) 0.033(2) 0.0012(17) 0.0104(16) -0.0123(17) C43 0.059(2) 0.040(2) 0.037(2) -0.0009(17) 0.0034(17) -0.0087(18) C44 0.050(2) 0.041(2) 0.033(2) -0.0010(16) 0.0093(16) -0.0058(16) C45 0.0311(17) 0.035(2) 0.035(2) -0.0017(16) 0.0060(14) 0.0010(14) O9 0.0780(19) 0.0364(16) 0.0400(16) -0.0077(13) 0.0124(14) 0.0011(13) O10 0.0766(18) 0.0406(16) 0.0385(16) 0.0073(13) 0.0080(13) 0.0118(13) N9 0.059(2) 0.068(3) 0.050(2) -0.007(2) 0.0008(18) 0.000(2) O11 0.083(2) 0.058(2) 0.121(3) -0.004(2) 0.015(2) 0.0038(19) O12 0.122(3) 0.113(4) 0.151(5) 0.008(3) 0.059(3) 0.053(3) O13 0.081(2) 0.121(3) 0.062(2) 0.022(2) -0.0027(19) -0.032(2) N10 0.074(3) 0.048(2) 0.055(2) 0.0061(19) 0.021(2) 0.0042(19) O14 0.084(2) 0.080(3) 0.075(2) -0.031(2) 0.0192(19) 0.0137(18) O15 0.114(3) 0.122(4) 0.104(3) -0.024(3) 0.007(3) 0.067(3) O16 0.083(2) 0.123(3) 0.058(2) -0.006(2) 0.0077(19) -0.037(2) OW1 0.079(2) 0.074(2) 0.052(2) -0.0082(17) 0.0143(16) 0.0009(17) OW2 0.0739(19) 0.070(2) 0.0429(17) -0.0157(15) 0.0138(14) -0.0055(16) OW3 0.080(2) 0.0431(17) 0.058(2) 0.0041(14) 0.0209(16) 0.0140(14) OW4 0.0694(18) 0.0445(17) 0.0533(19) -0.0027(14) 0.0114(14) -0.0101(13) OW5 0.0554(16) 0.063(2) 0.0440(17) -0.0020(14) 0.0119(13) 0.0024(14) OW6 0.092(2) 0.072(2) 0.0452(18) -0.0026(16) 0.0104(16) 0.0347(18) OW7 0.0666(17) 0.0504(17) 0.0400(16) 0.0077(13) 0.0143(13) 0.0276(13) OW8 0.084(2) 0.068(2) 0.099(3) 0.007(2) 0.011(2) 0.0020(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.920(2) . ? Cu1 O2 1.962(2) . ? Cu1 N2 2.003(3) . ? Cu1 N1 2.016(3) . ? Cu1 O5 2.251(2) . ? Cu1 Cu2 2.9180(11) . ? Cu1 Cu3 3.4691(11) . ? Cu2 O1 1.911(2) . ? Cu2 O2 1.967(2) . ? Cu2 N4 2.002(3) . ? Cu2 N3 2.011(3) . ? Cu2 O3 2.296(2) . ? Cu2 Cu3 3.1661(11) . ? Cu2 Cu4 3.4990(11) . ? Cu2 H1 2.3180 . ? Cu3 O4 1.919(2) . ? Cu3 O3 1.949(2) . ? Cu3 N6 1.984(3) . ? Cu3 N5 2.016(3) . ? Cu3 O2 2.327(2) . ? Cu3 Cu4 2.9370(11) . ? Cu4 O4 1.913(2) . ? Cu4 O3 1.973(2) . ? Cu4 N7 1.998(3) . ? Cu4 N8 2.012(3) . ? Cu4 O6 2.260(2) . ? O1 H1 0.8495 . ? O2 H2 0.7975 . ? O3 H3 0.7966 . ? O4 H4 0.8170 . ? O5 H5 0.8444 . ? O5 H6 0.8560 . ? O6 H8 0.8289 . ? O6 H7 0.8518 . ? N6 C30 1.333(4) . ? N6 C26 1.350(4) . ? N5 C21 1.341(4) . ? N5 C25 1.362(4) . ? C1 N1 1.342(4) . ? C1 C2 1.382(5) . ? C1 H1A 0.9300 . ? C2 C3 1.377(6) . ? C2 H2A 0.9300 . ? C3 C4 1.364(5) . ? C3 H3A 0.9300 . ? C4 C5 1.388(5) . ? C4 H4A 0.9300 . ? C5 N1 1.345(4) . ? C5 C6 1.470(5) . ? C6 N2 1.345(4) . ? C6 C7 1.381(5) . ? C7 C8 1.376(5) . ? C7 H7A 0.9300 . ? C8 C9 1.380(5) . ? C8 H8A 0.9300 . ? C9 C10 1.372(5) . ? C9 H9A 0.9300 . ? C10 N2 1.331(4) . ? C10 H10A 0.9300 . ? N8 C40 1.346(4) . ? N8 C36 1.347(4) . ? N7 C31 1.330(4) . ? N7 C35 1.345(4) . ? C11 N4 1.321(4) . ? C11 C12 1.385(5) . ? C11 H11A 0.9300 . ? C12 C13 1.379(6) . ? C12 H12A 0.9300 . ? C13 C14 1.366(6) . ? C13 H13A 0.9300 . ? C14 C15 1.387(5) . ? C14 H14A 0.9300 . ? C15 N4 1.351(4) . ? C15 C16 1.473(5) . ? C16 N3 1.355(4) . ? C16 C17 1.377(4) . ? C17 C18 1.389(5) . ? C17 H17A 0.9300 . ? C18 C19 1.371(5) . ? C18 H18A 0.9300 . ? C19 C20 1.372(5) . ? C19 H19A 0.9300 . ? C20 N3 1.340(4) . ? C20 H20A 0.9300 . ? C21 C22 1.379(4) . ? C21 H21A 0.9300 . ? C22 C23 1.373(5) . ? C22 H22A 0.9300 . ? C23 C24 1.384(5) . ? C23 H23A 0.9300 . ? C24 C25 1.382(4) . ? C24 H24A 0.9300 . ? C25 C26 1.459(5) . ? C26 C27 1.389(5) . ? C27 C28 1.369(6) . ? C27 H27A 0.9300 . ? C28 C29 1.385(6) . ? C28 H28A 0.9300 . ? C29 C30 1.381(5) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 C32 1.384(5) . ? C31 H31A 0.9300 . ? C32 C33 1.381(5) . ? C32 H32A 0.9300 . ? C33 C34 1.372(5) . ? C33 H33A 0.9300 . ? C34 C35 1.385(5) . ? C34 H34A 0.9300 . ? C35 C36 1.470(5) . ? C36 C37 1.377(4) . ? C37 C38 1.386(5) . ? C37 H37A 0.9300 . ? C38 C39 1.370(5) . ? C38 H38A 0.9300 . ? C39 C40 1.372(5) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? O7 C41 1.237(4) . ? O8 C41 1.241(4) . ? C41 C42 1.528(5) . ? C42 C43 1.517(5) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.499(5) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.527(5) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 O9 1.239(4) . ? C45 O10 1.254(4) . ? N9 O12 1.205(5) . ? N9 O13 1.221(5) . ? N9 O11 1.241(5) . ? N10 O14 1.232(4) . ? N10 O15 1.232(5) . ? N10 O16 1.237(5) . ? OW1 H9 0.8536 . ? OW1 H10 0.7535 . ? OW2 H11 0.8885 . ? OW2 H12 0.8023 . ? OW3 H13 0.8118 . ? OW3 H14 0.8508 . ? OW4 H15 0.8776 . ? OW4 H16 0.7947 . ? OW5 H17 0.7939 . ? OW5 H18 0.8504 . ? OW6 H19 0.8210 . ? OW6 H20 0.7998 . ? OW7 H21 0.8021 . ? OW7 H22 0.8276 . ? OW8 H23 0.8721 . ? OW8 H24 0.8056 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O2 81.38(9) . . ? O1 Cu1 N2 94.77(10) . . ? O2 Cu1 N2 159.31(10) . . ? O1 Cu1 N1 167.81(9) . . ? O2 Cu1 N1 98.99(10) . . ? N2 Cu1 N1 80.57(11) . . ? O1 Cu1 O5 94.23(9) . . ? O2 Cu1 O5 104.31(10) . . ? N2 Cu1 O5 96.22(11) . . ? N1 Cu1 O5 97.45(10) . . ? O1 Cu1 Cu2 40.27(6) . . ? O2 Cu1 Cu2 42.10(6) . . ? N2 Cu1 Cu2 134.31(8) . . ? N1 Cu1 Cu2 141.06(8) . . ? O5 Cu1 Cu2 95.14(7) . . ? O1 Cu1 Cu3 81.02(7) . . ? O2 Cu1 Cu3 39.73(6) . . ? N2 Cu1 Cu3 119.66(8) . . ? N1 Cu1 Cu3 91.45(8) . . ? O5 Cu1 Cu3 144.02(8) . . ? Cu2 Cu1 Cu3 58.68(3) . . ? O1 Cu2 O2 81.47(9) . . ? O1 Cu2 N4 95.86(10) . . ? O2 Cu2 N4 174.72(9) . . ? O1 Cu2 N3 165.56(9) . . ? O2 Cu2 N3 100.46(10) . . ? N4 Cu2 N3 80.99(11) . . ? O1 Cu2 O3 96.67(8) . . ? O2 Cu2 O3 84.85(8) . . ? N4 Cu2 O3 100.03(9) . . ? N3 Cu2 O3 97.76(9) . . ? O1 Cu2 Cu1 40.50(7) . . ? O2 Cu2 Cu1 41.96(6) . . ? N4 Cu2 Cu1 134.46(8) . . ? N3 Cu2 Cu1 136.94(8) . . ? O3 Cu2 Cu1 98.06(5) . . ? O1 Cu2 Cu3 89.84(6) . . ? O2 Cu2 Cu3 47.11(6) . . ? N4 Cu2 Cu3 137.75(8) . . ? N3 Cu2 Cu3 102.00(7) . . ? O3 Cu2 Cu3 37.74(5) . . ? Cu1 Cu2 Cu3 69.39(3) . . ? O1 Cu2 Cu4 128.68(6) . . ? O2 Cu2 Cu4 90.90(7) . . ? N4 Cu2 Cu4 94.32(8) . . ? N3 Cu2 Cu4 65.74(7) . . ? O3 Cu2 Cu4 32.02(5) . . ? Cu1 Cu2 Cu4 121.37(3) . . ? Cu3 Cu2 Cu4 52.00(3) . . ? O1 Cu2 H1 20.4 . . ? O2 Cu2 H1 96.2 . . ? N4 Cu2 H1 80.2 . . ? N3 Cu2 H1 146.9 . . ? O3 Cu2 H1 112.1 . . ? Cu1 Cu2 H1 54.3 . . ? Cu3 Cu2 H1 110.2 . . ? Cu4 Cu2 H1 142.6 . . ? O4 Cu3 O3 81.02(9) . . ? O4 Cu3 N6 95.63(10) . . ? O3 Cu3 N6 176.37(10) . . ? O4 Cu3 N5 161.14(10) . . ? O3 Cu3 N5 101.59(10) . . ? N6 Cu3 N5 81.12(11) . . ? O4 Cu3 O2 101.49(9) . . ? O3 Cu3 O2 84.41(8) . . ? N6 Cu3 O2 97.68(9) . . ? N5 Cu3 O2 97.36(9) . . ? O4 Cu3 Cu4 39.88(7) . . ? O3 Cu3 Cu4 41.81(6) . . ? N6 Cu3 Cu4 134.67(8) . . ? N5 Cu3 Cu4 136.77(8) . . ? O2 Cu3 Cu4 99.63(6) . . ? O4 Cu3 Cu2 92.54(7) . . ? O3 Cu3 Cu2 46.15(6) . . ? N6 Cu3 Cu2 135.86(8) . . ? N5 Cu3 Cu2 102.76(7) . . ? O2 Cu3 Cu2 38.26(5) . . ? Cu4 Cu3 Cu2 69.85(3) . . ? O4 Cu3 Cu1 134.04(7) . . ? O3 Cu3 Cu1 89.29(6) . . ? N6 Cu3 Cu1 94.07(8) . . ? N5 Cu3 Cu1 64.83(7) . . ? O2 Cu3 Cu1 32.60(5) . . ? Cu4 Cu3 Cu1 121.76(3) . . ? Cu2 Cu3 Cu1 51.93(3) . . ? O4 Cu4 O3 80.59(9) . . ? O4 Cu4 N7 168.29(10) . . ? O3 Cu4 N7 98.49(10) . . ? O4 Cu4 N8 95.21(11) . . ? O3 Cu4 N8 155.61(9) . . ? N7 Cu4 N8 80.77(11) . . ? O4 Cu4 O6 97.69(10) . . ? O3 Cu4 O6 94.23(9) . . ? N7 Cu4 O6 94.02(10) . . ? N8 Cu4 O6 110.16(10) . . ? O4 Cu4 Cu3 40.05(7) . . ? O3 Cu4 Cu3 41.20(6) . . ? N7 Cu4 Cu3 139.61(8) . . ? N8 Cu4 Cu3 133.41(8) . . ? O6 Cu4 Cu3 92.18(7) . . ? O4 Cu4 Cu2 82.90(7) . . ? O3 Cu4 Cu2 38.11(6) . . ? N7 Cu4 Cu2 89.21(8) . . ? N8 Cu4 Cu2 117.68(8) . . ? O6 Cu4 Cu2 131.93(7) . . ? Cu3 Cu4 Cu2 58.15(3) . . ? Cu2 O1 Cu1 99.23(10) . . ? Cu2 O1 H1 107.9 . . ? Cu1 O1 H1 119.1 . . ? Cu1 O2 Cu2 95.93(9) . . ? Cu1 O2 Cu3 107.67(9) . . ? Cu2 O2 Cu3 94.63(9) . . ? Cu1 O2 H2 119.8 . . ? Cu2 O2 H2 118.5 . . ? Cu3 O2 H2 116.0 . . ? Cu3 O3 Cu4 96.99(9) . . ? Cu3 O3 Cu2 96.10(8) . . ? Cu4 O3 Cu2 109.87(9) . . ? Cu3 O3 H3 118.0 . . ? Cu4 O3 H3 120.0 . . ? Cu2 O3 H3 112.5 . . ? Cu4 O4 Cu3 100.07(10) . . ? Cu4 O4 H4 129.4 . . ? Cu3 O4 H4 112.9 . . ? Cu1 O5 H5 130.5 . . ? Cu1 O5 H6 127.8 . . ? H5 O5 H6 101.2 . . ? Cu4 O6 H8 129.1 . . ? Cu4 O6 H7 107.9 . . ? H8 O6 H7 115.0 . . ? C30 N6 C26 119.8(3) . . ? C30 N6 Cu3 125.1(2) . . ? C26 N6 Cu3 115.1(2) . . ? C21 N5 C25 119.5(3) . . ? C21 N5 Cu3 126.9(2) . . ? C25 N5 Cu3 113.4(2) . . ? N1 C1 C2 121.7(3) . . ? N1 C1 H1A 119.1 . . ? C2 C1 H1A 119.1 . . ? C3 C2 C1 118.9(4) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? C4 C3 C2 119.8(3) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C3 C4 C5 119.0(4) . . ? C3 C4 H4A 120.5 . . ? C5 C4 H4A 120.5 . . ? N1 C5 C4 121.6(3) . . ? N1 C5 C6 115.3(3) . . ? C4 C5 C6 123.2(3) . . ? N2 C6 C7 121.1(3) . . ? N2 C6 C5 114.3(3) . . ? C7 C6 C5 124.5(3) . . ? C8 C7 C6 119.3(3) . . ? C8 C7 H7A 120.3 . . ? C6 C7 H7A 120.3 . . ? C7 C8 C9 119.2(3) . . ? C7 C8 H8A 120.4 . . ? C9 C8 H8A 120.4 . . ? C10 C9 C8 118.5(3) . . ? C10 C9 H9A 120.7 . . ? C8 C9 H9A 120.7 . . ? N2 C10 C9 122.7(3) . . ? N2 C10 H10A 118.7 . . ? C9 C10 H10A 118.7 . . ? C40 N8 C36 118.9(3) . . ? C40 N8 Cu4 126.2(2) . . ? C36 N8 Cu4 114.4(2) . . ? C31 N7 C35 119.0(3) . . ? C31 N7 Cu4 126.2(2) . . ? C35 N7 Cu4 114.8(2) . . ? N4 C11 C12 122.7(3) . . ? N4 C11 H11A 118.7 . . ? C12 C11 H11A 118.7 . . ? C13 C12 C11 117.5(4) . . ? C13 C12 H12A 121.2 . . ? C11 C12 H12A 121.2 . . ? C14 C13 C12 120.7(3) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C13 C14 C15 118.4(3) . . ? C13 C14 H14A 120.8 . . ? C15 C14 H14A 120.8 . . ? N4 C15 C14 121.3(3) . . ? N4 C15 C16 114.7(3) . . ? C14 C15 C16 124.1(3) . . ? N3 C16 C17 121.0(3) . . ? N3 C16 C15 114.8(3) . . ? C17 C16 C15 124.1(3) . . ? C16 C17 C18 119.5(3) . . ? C16 C17 H17A 120.2 . . ? C18 C17 H17A 120.2 . . ? C19 C18 C17 119.1(3) . . ? C19 C18 H18A 120.5 . . ? C17 C18 H18A 120.5 . . ? C18 C19 C20 118.9(3) . . ? C18 C19 H19A 120.6 . . ? C20 C19 H19A 120.6 . . ? N3 C20 C19 122.8(3) . . ? N3 C20 H20A 118.6 . . ? C19 C20 H20A 118.6 . . ? C10 N2 C6 119.1(3) . . ? C10 N2 Cu1 125.5(2) . . ? C6 N2 Cu1 115.3(2) . . ? C1 N1 C5 119.0(3) . . ? C1 N1 Cu1 126.6(2) . . ? C5 N1 Cu1 114.3(2) . . ? N5 C21 C22 121.8(3) . . ? N5 C21 H21A 119.1 . . ? C22 C21 H21A 119.1 . . ? C23 C22 C21 119.2(3) . . ? C23 C22 H22A 120.4 . . ? C21 C22 H22A 120.4 . . ? C22 C23 C24 119.5(3) . . ? C22 C23 H23A 120.3 . . ? C24 C23 H23A 120.3 . . ? C25 C24 C23 119.4(3) . . ? C25 C24 H24A 120.3 . . ? C23 C24 H24A 120.3 . . ? N5 C25 C24 120.6(3) . . ? N5 C25 C26 115.0(3) . . ? C24 C25 C26 124.4(3) . . ? N6 C26 C27 120.4(3) . . ? N6 C26 C25 114.8(3) . . ? C27 C26 C25 124.8(3) . . ? C28 C27 C26 119.5(4) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C27 C28 C29 119.9(4) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C30 C29 C28 117.9(4) . . ? C30 C29 H29A 121.0 . . ? C28 C29 H29A 121.0 . . ? N6 C30 C29 122.4(4) . . ? N6 C30 H30A 118.8 . . ? C29 C30 H30A 118.8 . . ? C11 N4 C15 119.4(3) . . ? C11 N4 Cu2 125.8(2) . . ? C15 N4 Cu2 114.8(2) . . ? C20 N3 C16 118.7(3) . . ? C20 N3 Cu2 126.8(2) . . ? C16 N3 Cu2 114.2(2) . . ? N7 C31 C32 122.4(3) . . ? N7 C31 H31A 118.8 . . ? C32 C31 H31A 118.8 . . ? C33 C32 C31 118.3(3) . . ? C33 C32 H32A 120.8 . . ? C31 C32 H32A 120.8 . . ? C34 C33 C32 119.7(3) . . ? C34 C33 H33A 120.2 . . ? C32 C33 H33A 120.2 . . ? C33 C34 C35 118.8(3) . . ? C33 C34 H34A 120.6 . . ? C35 C34 H34A 120.6 . . ? N7 C35 C34 121.7(3) . . ? N7 C35 C36 115.0(3) . . ? C34 C35 C36 123.3(3) . . ? N8 C36 C37 121.6(3) . . ? N8 C36 C35 114.6(3) . . ? C37 C36 C35 123.9(3) . . ? C36 C37 C38 119.2(3) . . ? C36 C37 H37A 120.4 . . ? C38 C37 H37A 120.4 . . ? C39 C38 C37 118.9(3) . . ? C39 C38 H38A 120.5 . . ? C37 C38 H38A 120.6 . . ? C38 C39 C40 119.6(3) . . ? C38 C39 H39A 120.2 . . ? C40 C39 H39A 120.2 . . ? N8 C40 C39 121.8(3) . . ? N8 C40 H40A 119.1 . . ? C39 C40 H40A 119.1 . . ? O7 C41 O8 124.2(3) . . ? O7 C41 C42 118.5(3) . . ? O8 C41 C42 117.2(3) . . ? C43 C42 C41 115.7(3) . . ? C43 C42 H42A 108.3 . . ? C41 C42 H42A 108.3 . . ? C43 C42 H42B 108.3 . . ? C41 C42 H42B 108.3 . . ? H42A C42 H42B 107.4 . . ? C44 C43 C42 115.1(3) . . ? C44 C43 H43A 108.5 . . ? C42 C43 H43A 108.5 . . ? C44 C43 H43B 108.5 . . ? C42 C43 H43B 108.5 . . ? H43A C43 H43B 107.5 . . ? C43 C44 C45 113.6(3) . . ? C43 C44 H44A 108.8 . . ? C45 C44 H44A 108.8 . . ? C43 C44 H44B 108.8 . . ? C45 C44 H44B 108.8 . . ? H44A C44 H44B 107.7 . . ? O9 C45 O10 124.7(3) . . ? O9 C45 C44 118.1(3) . . ? O10 C45 C44 117.2(3) . . ? O12 N9 O13 120.1(5) . . ? O12 N9 O11 120.3(5) . . ? O13 N9 O11 119.6(4) . . ? O14 N10 O15 118.8(4) . . ? O14 N10 O16 121.3(4) . . ? O15 N10 O16 119.8(4) . . ? H9 OW1 H10 95.7 . . ? H11 OW2 H12 97.7 . . ? H13 OW3 H14 106.5 . . ? H15 OW4 H16 98.1 . . ? H17 OW5 H18 101.4 . . ? H19 OW6 H20 104.8 . . ? H21 OW7 H22 118.8 . . ? H23 OW8 H24 83.1 . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.497 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.111 #================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 725664' #TrackingRef '_CuOH_n1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H84 Cu4 N8 O30' _chemical_formula_weight 1533.25 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 0.2630 1.2660 '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/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.771(3) _cell_length_b 14.274(3) _cell_length_c 27.846(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.90(3) _cell_angle_gamma 90.00 _cell_volume 6650(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 31030 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 27.62 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 1.324 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.30 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 59457 _diffrn_reflns_av_R_equivalents 0.1495 _diffrn_reflns_av_sigmaI/netI 0.1322 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.48 _reflns_number_total 14730 _reflns_number_gt 8437 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO Rigaku,1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure Rigaku/MSC,2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Johnson,1976)' _computing_publication_material SHELXTL97 _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^)+(0.0326P)^2^+94.5453P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0022(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 14730 _refine_ls_number_parameters 827 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.1746 _refine_ls_R_factor_gt 0.1097 _refine_ls_wR_factor_ref 0.2713 _refine_ls_wR_factor_gt 0.2449 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 5.196 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.0875(3) 0.1652(4) 0.4898(2) 0.0381(15) Uani 1 1 d . . . Cu2 Cu 0.0613(3) 0.0661(4) 0.4760(2) 0.0367(15) Uani 1 1 d . . . Cu3 Cu 0.4106(3) 0.3348(4) 0.5103(2) 0.0339(14) Uani 1 1 d . . . Cu4 Cu 0.5622(3) 0.4328(4) 0.52703(19) 0.0320(14) Uani 1 1 d . . . O1 O -0.0256(19) 0.124(2) 0.4385(11) 0.042(8) Uani 1 1 d . . . H1 H -0.0123 0.1711 0.4220 0.050 Uiso 1 1 d . . . O2 O -0.0102(18) 0.084(2) 0.5275(11) 0.034(7) Uani 1 1 d . . . H2 H 0.0086 0.0982 0.5559 0.041 Uiso 1 1 d . . . O3 O -0.020(2) 0.301(3) 0.4960(14) 0.059(10) Uani 1 1 d . . . H3 H -0.0249 0.3374 0.4719 0.071 Uiso 1 1 d . . . H4 H -0.0197 0.3341 0.5213 0.071 Uiso 1 1 d . . . N1 N -0.165(3) 0.185(3) 0.5400(15) 0.042(10) Uani 1 1 d . . . N2 N -0.185(3) 0.195(3) 0.4468(15) 0.047(11) Uani 1 1 d . . . C1 C -0.150(3) 0.186(4) 0.587(2) 0.051(14) Uani 1 1 d . . . H1A H -0.0967 0.1802 0.5987 0.062 Uiso 1 1 calc R . . C2 C -0.209(4) 0.194(4) 0.620(2) 0.056(15) Uani 1 1 d . . . H2A H -0.1961 0.1894 0.6524 0.067 Uiso 1 1 calc R . . C3 C -0.284(3) 0.210(4) 0.603(2) 0.055(15) Uani 1 1 d . . . H3A H -0.3242 0.2190 0.6241 0.065 Uiso 1 1 calc R . . C4 C -0.303(3) 0.213(4) 0.552(2) 0.056(15) Uani 1 1 d . . . H4A H -0.3557 0.2218 0.5402 0.067 Uiso 1 1 calc R . . C5 C -0.243(3) 0.202(3) 0.521(2) 0.042(12) Uani 1 1 d . . . C6 C -0.253(3) 0.206(3) 0.470(2) 0.045(12) Uani 1 1 d . . . C7 C -0.327(3) 0.217(4) 0.444(2) 0.053(14) Uani 1 1 d . . . H7A H -0.3738 0.2232 0.4595 0.063 Uiso 1 1 calc R . . C8 C -0.328(4) 0.220(5) 0.395(3) 0.07(2) Uani 1 1 d . . . H8A H -0.3764 0.2270 0.3767 0.087 Uiso 1 1 calc R . . C9 C -0.258(4) 0.212(5) 0.371(2) 0.065(17) Uani 1 1 d . . . H9A H -0.2581 0.2159 0.3376 0.078 Uiso 1 1 calc R . . C10 C -0.189(4) 0.198(4) 0.399(2) 0.058(15) Uani 1 1 d . . . H10A H -0.1415 0.1889 0.3840 0.070 Uiso 1 1 calc R . . N3 N 0.132(2) 0.058(3) 0.4221(15) 0.043(10) Uani 1 1 d . . . N4 N 0.166(2) 0.044(3) 0.5142(13) 0.038(9) Uani 1 1 d . . . C11 C 0.110(3) 0.061(4) 0.3760(19) 0.048(13) Uani 1 1 d . . . H11A H 0.0561 0.0651 0.3670 0.058 Uiso 1 1 calc R . . C12 C 0.163(4) 0.057(5) 0.340(2) 0.068(18) Uani 1 1 d . . . H12A H 0.1449 0.0604 0.3079 0.082 Uiso 1 1 calc R . . C13 C 0.242(4) 0.050(5) 0.353(2) 0.08(2) Uani 1 1 d . . . H13A H 0.2793 0.0457 0.3299 0.092 Uiso 1 1 calc R . . C14 C 0.269(3) 0.048(4) 0.402(2) 0.053(14) Uani 1 1 d . . . H14A H 0.3228 0.0457 0.4118 0.064 Uiso 1 1 calc R . . C15 C 0.212(3) 0.051(3) 0.4361(18) 0.040(11) Uani 1 1 d . . . C16 C 0.231(3) 0.045(3) 0.488(2) 0.047(13) Uani 1 1 d . . . C17 C 0.308(3) 0.042(4) 0.510(2) 0.059(15) Uani 1 1 d . . . H17A H 0.3517 0.0438 0.4914 0.070 Uiso 1 1 calc R . . C18 C 0.317(4) 0.036(4) 0.558(2) 0.063(16) Uani 1 1 d . . . H18A H 0.3687 0.0347 0.5731 0.076 Uiso 1 1 calc R . . C19 C 0.252(4) 0.032(4) 0.586(2) 0.054(14) Uani 1 1 d . . . H19A H 0.2582 0.0253 0.6192 0.064 Uiso 1 1 calc R . . C20 C 0.179(3) 0.038(3) 0.5625(19) 0.046(12) Uani 1 1 d . . . H20A H 0.1342 0.0371 0.5807 0.055 Uiso 1 1 calc R . . O4 O 0.4810(19) 0.376(2) 0.5630(11) 0.036(7) Uani 1 1 d . . . H5 H 0.4989 0.3286 0.5789 0.043 Uiso 1 1 d . . . O5 O 0.4813(18) 0.414(2) 0.4738(10) 0.034(7) Uani 1 1 d . . . H6 H 0.4956 0.4230 0.4453 0.041 Uiso 1 1 d . . . O6 O 0.479(3) 0.201(2) 0.5034(13) 0.057(10) Uani 1 1 d . . . H7 H 0.4795 0.1747 0.5291 0.068 Uiso 1 1 d . . . H8 H 0.4744 0.1641 0.4812 0.068 Uiso 1 1 d . . . N5 N 0.319(2) 0.304(3) 0.5509(14) 0.037(9) Uani 1 1 d . . . N6 N 0.325(2) 0.313(3) 0.4576(14) 0.036(9) Uani 1 1 d . . . C21 C 0.321(4) 0.303(4) 0.598(2) 0.052(14) Uani 1 1 d . . . H21A H 0.3710 0.3090 0.6149 0.078 Uiso 1 1 calc R . . C22 C 0.255(4) 0.292(4) 0.624(2) 0.056(15) Uani 1 1 d . . . H22A H 0.2604 0.2918 0.6577 0.084 Uiso 1 1 calc R . . C23 C 0.183(4) 0.283(4) 0.600(2) 0.066(17) Uani 1 1 d . . . H23A H 0.1372 0.2746 0.6171 0.098 Uiso 1 1 calc R . . C24 C 0.176(3) 0.285(4) 0.549(2) 0.053(14) Uani 1 1 d . . . H24A H 0.1266 0.2795 0.5315 0.079 Uiso 1 1 calc R . . C25 C 0.246(3) 0.297(3) 0.5264(18) 0.041(12) Uani 1 1 d . . . C26 C 0.251(3) 0.300(3) 0.4732(17) 0.038(11) Uani 1 1 d . . . C27 C 0.184(3) 0.290(4) 0.440(2) 0.053(14) Uani 1 1 d . . . H27A H 0.1334 0.2809 0.4504 0.080 Uiso 1 1 calc R . . C28 C 0.197(3) 0.294(4) 0.392(2) 0.054(15) Uani 1 1 d . . . H28A H 0.1534 0.2879 0.3694 0.081 Uiso 1 1 calc R . . C29 C 0.270(4) 0.306(4) 0.3766(19) 0.054(15) Uani 1 1 d . . . H29A H 0.2783 0.3081 0.3439 0.081 Uiso 1 1 calc R . . C30 C 0.334(3) 0.315(4) 0.4103(18) 0.045(12) Uani 1 1 d . . . H30A H 0.3855 0.3233 0.3999 0.067 Uiso 1 1 calc R . . N7 N 0.661(2) 0.454(2) 0.4898(13) 0.033(8) Uani 1 1 d . . . N8 N 0.643(2) 0.443(3) 0.5821(13) 0.033(8) Uani 1 1 d . . . C31 C 0.663(3) 0.459(3) 0.4422(18) 0.045(12) Uani 1 1 d . . . H31A H 0.6151 0.4619 0.4234 0.067 Uiso 1 1 calc R . . C32 C 0.733(3) 0.461(4) 0.420(2) 0.048(13) Uani 1 1 d . . . H32A H 0.7320 0.4637 0.3865 0.073 Uiso 1 1 calc R . . C33 C 0.803(4) 0.460(4) 0.447(2) 0.061(16) Uani 1 1 d . . . H33A H 0.8511 0.4626 0.4322 0.092 Uiso 1 1 calc R . . C34 C 0.803(3) 0.455(4) 0.499(2) 0.057(15) Uani 1 1 d . . . H34A H 0.8506 0.4541 0.5182 0.085 Uiso 1 1 calc R . . C35 C 0.729(3) 0.453(3) 0.5173(19) 0.043(12) Uani 1 1 d . . . C36 C 0.720(3) 0.450(3) 0.5699(17) 0.040(11) Uani 1 1 d . . . C37 C 0.783(4) 0.454(4) 0.605(2) 0.053(14) Uani 1 1 d . . . H37A H 0.8357 0.4574 0.5957 0.079 Uiso 1 1 calc R . . C38 C 0.768(4) 0.452(4) 0.652(2) 0.067(18) Uani 1 1 d . . . H38A H 0.8091 0.4544 0.6761 0.100 Uiso 1 1 calc R . . C39 C 0.689(4) 0.447(4) 0.6642(19) 0.057(15) Uani 1 1 d . . . H39A H 0.6769 0.4462 0.6963 0.086 Uiso 1 1 calc R . . C40 C 0.629(3) 0.443(3) 0.6284(17) 0.045(12) Uani 1 1 d . . . H40A H 0.5760 0.4406 0.6368 0.067 Uiso 1 1 calc R . . O7 O 0.702(3) 0.643(4) 0.755(2) 0.094(17) Uani 1 1 d . A . O8 O 0.701(3) 0.502(3) 0.7870(15) 0.073(12) Uani 1 1 d . A . C41 C 0.667(4) 0.581(6) 0.778(2) 0.070(18) Uani 1 1 d D . . C42A C 0.587(5) 0.616(7) 0.792(4) 0.06(3) Uiso 0.60(9) 1 d PD A 1 H42A H 0.5601 0.6443 0.7639 0.077 Uiso 0.60(9) 1 calc PR A 1 H42D H 0.5965 0.6653 0.8160 0.077 Uiso 0.60(9) 1 calc PR A 1 C42B C 0.604(7) 0.584(12) 0.816(5) 0.07(5) Uiso 0.40(9) 1 d PD A 2 H42B H 0.6059 0.5260 0.8338 0.080 Uiso 0.40(9) 1 calc PR A 2 H42C H 0.6162 0.6350 0.8382 0.080 Uiso 0.40(9) 1 calc PR A 2 C43A C 0.533(5) 0.545(6) 0.812(3) 0.05(3) Uiso 0.60(9) 1 d PD A 1 H43A H 0.5607 0.5120 0.8385 0.062 Uiso 0.60(9) 1 calc PR A 1 H43B H 0.5176 0.4992 0.7871 0.062 Uiso 0.60(9) 1 calc PR A 1 C43B C 0.522(7) 0.598(15) 0.793(5) 0.08(6) Uiso 0.40(9) 1 d PD A 2 H43C H 0.5116 0.5503 0.7682 0.101 Uiso 0.40(9) 1 calc PR A 2 H43D H 0.5186 0.6585 0.7774 0.101 Uiso 0.40(9) 1 calc PR A 2 C44 C 0.458(3) 0.591(4) 0.8290(19) 0.053(14) Uani 1 1 d D . . H44A H 0.4354 0.6321 0.8040 0.080 Uiso 1 1 calc R A 1 H44B H 0.4192 0.5433 0.8351 0.080 Uiso 1 1 calc R A 1 C45 C 0.477(3) 0.647(4) 0.8742(18) 0.044(12) Uani 1 1 d . A . O9 O 0.485(3) 0.606(3) 0.9129(13) 0.061(11) Uani 1 1 d . . . O10 O 0.480(2) 0.735(2) 0.8713(13) 0.052(9) Uani 1 1 d . . . O11 O -0.280(4) 0.449(4) 0.275(2) 0.11(2) Uani 1 1 d . A . O12 O -0.224(3) 0.586(3) 0.2726(18) 0.076(13) Uani 1 1 d . A . C46 C -0.221(4) 0.499(6) 0.277(2) 0.071(19) Uani 1 1 d D . . C47A C -0.154(7) 0.435(9) 0.298(6) 0.06(4) Uiso 0.40(9) 1 d PD A 1 H47A H -0.1723 0.4022 0.3256 0.073 Uiso 0.40(9) 1 calc PR A 1 H47B H -0.1433 0.3881 0.2739 0.073 Uiso 0.40(9) 1 calc PR A 1 C47B C -0.135(5) 0.464(8) 0.275(3) 0.06(3) Uiso 0.60(9) 1 d PD A 2 H47C H -0.1328 0.4123 0.2527 0.074 Uiso 0.60(9) 1 calc PR A 2 H47D H -0.1007 0.5138 0.2649 0.074 Uiso 0.60(9) 1 calc PR A 2 C48A C -0.076(6) 0.483(8) 0.313(5) 0.05(4) Uiso 0.40(9) 1 d PD A 1 H48A H -0.0849 0.5274 0.3386 0.063 Uiso 0.40(9) 1 calc PR A 1 H48B H -0.0578 0.5181 0.2859 0.063 Uiso 0.40(9) 1 calc PR A 1 C48B C -0.107(5) 0.432(9) 0.325(4) 0.08(4) Uiso 0.60(9) 1 d PD A 2 H48C H -0.1356 0.3754 0.3322 0.093 Uiso 0.60(9) 1 calc PR A 2 H48D H -0.1199 0.4798 0.3477 0.093 Uiso 0.60(9) 1 calc PR A 2 C49 C -0.015(4) 0.412(5) 0.330(2) 0.070(19) Uani 1 1 d D . . H49A H 0.0364 0.4436 0.3289 0.104 Uiso 1 1 calc R A 1 H49B H -0.0158 0.3647 0.3049 0.104 Uiso 1 1 calc R A 1 C50 C -0.010(3) 0.358(5) 0.377(2) 0.053(14) Uani 1 1 d . A . O13 O -0.004(2) 0.271(3) 0.3756(14) 0.058(10) Uani 1 1 d . . . O14 O -0.011(3) 0.404(3) 0.4154(15) 0.072(13) Uani 1 1 d . . . OW1 O 0.865(4) 0.299(5) 0.7214(18) 0.11(2) Uani 1 1 d D . . H9 H 0.8950 0.2938 0.7496 0.131 Uiso 1 1 d D . . H10 H 0.8223 0.2958 0.7378 0.131 Uiso 1 1 d D . . OW2 O -0.416(4) 0.480(4) 0.324(2) 0.11(2) Uani 1 1 d D . . H11 H -0.4313 0.5170 0.3085 0.135 Uiso 1 1 d D . . H12 H -0.3737 0.4664 0.3115 0.135 Uiso 1 1 d D . . OW3 O 0.872(3) 0.496(4) 0.808(2) 0.101(18) Uani 1 1 d D . . H13 H 0.8192 0.4872 0.8012 0.121 Uiso 1 1 d D . . H14 H 0.9035 0.4477 0.8109 0.121 Uiso 1 1 d D . . OW4 O 0.853(3) 0.633(4) 0.7303(18) 0.088(15) Uani 1 1 d D . . H15 H 0.8787 0.5869 0.7442 0.105 Uiso 1 1 d D . . H16 H 0.8050 0.6495 0.7408 0.105 Uiso 1 1 d D . . OW5 O -0.279(3) 0.276(3) 0.2355(19) 0.090(15) Uani 1 1 d D . . H17 H -0.2738 0.3347 0.2467 0.108 Uiso 1 1 d D . . H18 H -0.3195 0.2446 0.2455 0.108 Uiso 1 1 d D . . OW6 O -0.097(3) 0.700(3) 0.2638(18) 0.088(15) Uani 1 1 d D . . H19 H -0.1198 0.7040 0.2916 0.106 Uiso 1 1 d D . . H20 H -0.1338 0.6709 0.2437 0.106 Uiso 1 1 d D . . OW7 O -0.012(3) 0.297(3) 0.6625(15) 0.077(13) Uani 1 1 d . . . H21 H -0.0378 0.2817 0.6826 0.092 Uiso 1 1 d . . . H22 H -0.0428 0.3090 0.6409 0.092 Uiso 1 1 d . . . OW8 O -0.360(3) 0.683(3) 0.2431(15) 0.065(11) Uani 1 1 d D . . H23 H -0.3409 0.7389 0.2528 0.079 Uiso 1 1 d D . . H24 H -0.3163 0.6525 0.2529 0.079 Uiso 1 1 d D . . OW9 O -0.026(3) 0.159(3) 0.2986(16) 0.079(13) Uani 1 1 d . . . H25 H 0.0100 0.1724 0.2839 0.095 Uiso 1 1 d . . . H26 H -0.0334 0.1952 0.3186 0.095 Uiso 1 1 d . . . OW10 O 0.037(3) 0.117(3) 0.6277(16) 0.075(13) Uani 1 1 d D . . H27 H 0.0712 0.0993 0.6515 0.090 Uiso 1 1 d D . . H28 H 0.0299 0.1611 0.6495 0.090 Uiso 1 1 d D . . OW11 O 0.507(3) 0.850(3) 0.7955(14) 0.062(11) Uani 1 1 d D . . H29 H 0.4977 0.8085 0.8183 0.074 Uiso 1 1 d D . . H30 H 0.5457 0.8511 0.7763 0.074 Uiso 1 1 d D . . OW12 O 0.472(3) 0.319(3) 0.8348(14) 0.068(12) Uani 1 1 d . . . H31 H 0.5140 0.3243 0.8265 0.081 Uiso 1 1 d . . . H32 H 0.4476 0.3061 0.8104 0.081 Uiso 1 1 d . . . OW13 O -0.020(3) 0.409(3) 0.5771(15) 0.072(12) Uani 1 1 d D . . H33 H 0.0031 0.4559 0.5931 0.086 Uiso 1 1 d D . . H34 H -0.0440 0.3816 0.6010 0.086 Uiso 1 1 d D . . OW14 O 0.491(3) 0.641(3) 0.6233(14) 0.063(11) Uani 1 1 d . . . H35 H 0.4993 0.6932 0.6310 0.075 Uiso 1 1 d . . . H36 H 0.4593 0.6182 0.6402 0.075 Uiso 1 1 d . . . OW15 O 0.471(3) 0.415(3) 0.9242(13) 0.067(12) Uani 1 1 d . . . H37 H 0.4906 0.4609 0.9132 0.081 Uiso 1 1 d . . . H38 H 0.4385 0.4003 0.9001 0.081 Uiso 1 1 d . . . OW16 O 0.608(3) 0.341(3) 0.7789(14) 0.063(11) Uani 1 1 d . . . H39 H 0.5700 0.3376 0.7600 0.076 Uiso 1 1 d . . . H40 H 0.6342 0.3830 0.7710 0.076 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 0.029(3) 0.047(3) 0.038(3) -0.003(3) 0.001(2) 0.005(3) Cu2 0.027(3) 0.046(3) 0.037(3) -0.001(3) 0.003(2) 0.002(2) Cu3 0.029(3) 0.039(3) 0.033(3) -0.001(2) 0.003(2) -0.005(2) Cu4 0.027(3) 0.038(3) 0.031(3) 0.002(2) 0.002(2) -0.002(2) O1 0.030(19) 0.05(2) 0.040(19) 0.008(15) 0.000(14) 0.006(15) O2 0.033(18) 0.032(17) 0.037(17) -0.003(13) 0.002(13) 0.000(13) O3 0.07(3) 0.05(2) 0.06(2) -0.005(18) 0.00(2) -0.010(19) N1 0.04(3) 0.04(2) 0.05(2) -0.006(18) 0.001(19) 0.004(18) N2 0.04(3) 0.06(3) 0.04(2) 0.002(19) 0.00(2) 0.00(2) C1 0.03(3) 0.07(4) 0.05(3) -0.01(3) 0.01(2) 0.01(2) C2 0.05(4) 0.06(4) 0.06(4) -0.01(3) 0.02(3) 0.00(3) C3 0.04(4) 0.06(3) 0.07(4) -0.01(3) 0.03(3) 0.00(2) C4 0.03(3) 0.05(3) 0.09(5) -0.01(3) 0.01(3) 0.00(2) C5 0.02(3) 0.04(3) 0.07(4) -0.01(2) 0.01(2) -0.007(18) C6 0.04(3) 0.03(3) 0.06(3) 0.00(2) 0.00(3) 0.00(2) C7 0.03(3) 0.05(3) 0.07(4) 0.00(3) 0.01(3) 0.00(2) C8 0.07(5) 0.07(4) 0.08(5) 0.00(3) -0.04(4) 0.01(3) C9 0.05(4) 0.08(5) 0.06(4) 0.00(3) -0.02(3) 0.01(3) C10 0.05(4) 0.08(4) 0.05(3) 0.00(3) 0.00(3) 0.00(3) N3 0.03(2) 0.04(2) 0.05(3) 0.004(19) 0.002(19) 0.001(18) N4 0.03(2) 0.05(3) 0.03(2) -0.001(17) 0.002(17) 0.004(17) C11 0.04(3) 0.05(3) 0.05(3) 0.01(2) 0.01(2) 0.00(2) C12 0.06(4) 0.10(5) 0.05(3) 0.00(3) 0.02(3) 0.02(4) C13 0.06(4) 0.11(6) 0.06(4) 0.02(4) 0.03(3) 0.02(4) C14 0.03(3) 0.07(4) 0.06(3) 0.01(3) 0.02(2) 0.01(2) C15 0.03(3) 0.04(3) 0.05(3) 0.00(2) 0.00(2) 0.00(2) C16 0.04(3) 0.04(3) 0.06(3) 0.00(2) 0.00(3) 0.00(2) C17 0.03(3) 0.08(4) 0.07(4) -0.01(3) 0.00(3) -0.01(3) C18 0.05(4) 0.07(4) 0.08(4) -0.01(3) -0.01(3) 0.00(3) C19 0.05(4) 0.07(4) 0.04(3) 0.00(3) -0.01(3) 0.00(3) C20 0.04(3) 0.05(3) 0.05(3) 0.00(2) 0.00(2) 0.00(2) O4 0.04(2) 0.035(17) 0.033(17) 0.003(13) 0.000(14) -0.011(13) O5 0.026(17) 0.043(18) 0.034(17) 0.001(13) 0.003(13) -0.002(13) O6 0.08(3) 0.04(2) 0.05(2) -0.004(17) 0.00(2) 0.013(19) N5 0.03(2) 0.04(2) 0.04(2) -0.001(17) 0.000(17) -0.003(16) N6 0.03(2) 0.04(2) 0.04(2) 0.000(16) 0.000(17) -0.001(16) C21 0.05(3) 0.06(3) 0.05(3) 0.01(3) 0.01(3) 0.00(3) C22 0.06(4) 0.07(4) 0.05(3) 0.00(3) 0.02(3) -0.01(3) C23 0.05(4) 0.07(4) 0.08(5) -0.01(3) 0.03(3) -0.01(3) C24 0.04(3) 0.05(3) 0.07(4) 0.00(3) 0.02(3) 0.00(2) C25 0.04(3) 0.03(3) 0.05(3) 0.00(2) 0.00(2) -0.01(2) C26 0.04(3) 0.03(2) 0.04(3) 0.00(2) 0.00(2) -0.007(19) C27 0.03(3) 0.06(4) 0.07(4) 0.00(3) -0.01(3) 0.00(2) C28 0.04(3) 0.07(4) 0.06(4) 0.01(3) -0.02(3) -0.01(3) C29 0.06(4) 0.06(4) 0.04(3) 0.00(2) -0.01(3) 0.00(3) C30 0.03(3) 0.06(3) 0.04(3) 0.00(2) 0.01(2) -0.01(2) N7 0.03(2) 0.03(2) 0.04(2) -0.002(15) 0.005(17) -0.004(15) N8 0.03(2) 0.04(2) 0.03(2) 0.003(16) -0.001(16) 0.001(15) C31 0.05(3) 0.05(3) 0.04(3) 0.00(2) 0.01(2) 0.00(2) C32 0.05(3) 0.06(3) 0.04(3) -0.01(2) 0.02(3) 0.00(2) C33 0.05(4) 0.07(4) 0.07(4) 0.00(3) 0.03(3) 0.00(3) C34 0.03(3) 0.07(4) 0.06(4) -0.01(3) 0.00(3) 0.00(3) C35 0.04(3) 0.03(3) 0.06(3) 0.00(2) 0.01(2) 0.00(2) C36 0.04(3) 0.04(3) 0.04(3) 0.01(2) -0.01(2) -0.01(2) C37 0.05(4) 0.06(3) 0.05(3) 0.01(3) -0.01(3) 0.01(3) C38 0.06(4) 0.08(4) 0.06(4) 0.01(3) -0.03(3) 0.00(3) C39 0.07(5) 0.06(4) 0.03(3) 0.01(2) 0.00(3) 0.00(3) C40 0.05(3) 0.04(3) 0.04(3) 0.00(2) 0.00(2) -0.01(2) O7 0.08(4) 0.09(4) 0.12(4) 0.01(3) 0.04(3) 0.02(3) O8 0.08(3) 0.08(3) 0.06(3) 0.00(2) 0.01(2) 0.00(3) C41 0.06(4) 0.09(5) 0.07(4) -0.02(4) 0.02(3) 0.00(4) C44 0.06(4) 0.06(3) 0.05(3) -0.01(3) 0.01(3) 0.00(3) C45 0.04(3) 0.05(3) 0.04(3) -0.01(2) 0.00(2) 0.00(2) O9 0.08(3) 0.06(2) 0.04(2) -0.004(18) 0.00(2) 0.00(2) O10 0.06(3) 0.04(2) 0.05(2) -0.004(16) 0.001(18) 0.003(17) O11 0.08(4) 0.07(3) 0.18(6) 0.01(4) 0.05(4) 0.00(3) O12 0.06(3) 0.06(3) 0.10(4) -0.02(3) 0.01(3) 0.00(2) C46 0.04(4) 0.10(6) 0.07(4) -0.02(4) 0.00(3) 0.00(4) C49 0.06(4) 0.09(5) 0.05(4) 0.00(3) -0.01(3) 0.03(4) C50 0.03(3) 0.08(4) 0.05(3) 0.00(3) 0.00(2) 0.01(3) O13 0.06(3) 0.05(3) 0.06(3) 0.004(19) 0.01(2) 0.002(19) O14 0.10(4) 0.06(3) 0.05(2) 0.00(2) 0.01(2) 0.01(2) OW1 0.11(5) 0.15(5) 0.07(3) 0.00(3) 0.00(3) -0.02(4) OW2 0.10(5) 0.10(4) 0.15(5) 0.05(4) 0.04(4) 0.03(3) OW3 0.08(4) 0.07(3) 0.15(5) -0.02(3) -0.01(3) 0.00(3) OW4 0.08(4) 0.10(4) 0.09(4) 0.00(3) 0.02(3) -0.01(3) OW5 0.08(4) 0.09(3) 0.11(4) 0.00(3) 0.04(3) -0.01(3) OW6 0.09(4) 0.08(3) 0.09(4) 0.00(3) -0.01(3) -0.02(3) OW7 0.09(4) 0.08(3) 0.06(3) 0.00(2) 0.00(2) 0.00(3) OW8 0.06(3) 0.06(3) 0.08(3) 0.00(2) 0.01(2) 0.00(2) OW9 0.08(3) 0.09(3) 0.07(3) -0.01(2) -0.01(2) 0.01(3) OW10 0.07(3) 0.08(3) 0.07(3) -0.02(2) -0.01(2) 0.02(2) OW11 0.07(3) 0.05(2) 0.06(2) 0.007(18) 0.01(2) 0.01(2) OW12 0.07(3) 0.08(3) 0.05(2) 0.00(2) 0.00(2) -0.01(2) OW13 0.09(4) 0.07(3) 0.06(3) -0.01(2) 0.01(2) -0.01(2) OW14 0.06(3) 0.07(3) 0.06(2) -0.01(2) 0.02(2) -0.01(2) OW15 0.10(4) 0.06(3) 0.04(2) 0.012(18) 0.00(2) 0.00(2) OW16 0.07(3) 0.06(2) 0.06(3) 0.00(2) -0.01(2) 0.00(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.91(3) . ? Cu1 O2 1.99(3) . ? Cu1 N1 1.99(4) . ? Cu1 N2 2.01(4) . ? Cu1 O3 2.25(4) . ? Cu1 Cu2 2.917(8) . ? Cu1 Cu2 3.456(8) 3_556 ? Cu2 O1 1.92(3) . ? Cu2 O2 1.95(3) . ? Cu2 N3 1.98(4) . ? Cu2 N4 2.02(4) . ? Cu2 O2 2.31(3) 3_556 ? Cu2 Cu2 3.155(12) 3_556 ? Cu2 Cu1 3.456(8) 3_556 ? Cu3 O4 1.91(3) . ? Cu3 O5 1.97(3) . ? Cu3 N6 2.01(4) . ? Cu3 N5 2.02(4) . ? Cu3 O6 2.24(4) . ? Cu3 Cu4 2.913(8) . ? Cu4 O4 1.92(3) . ? Cu4 O5 1.96(3) . ? Cu4 N8 1.99(4) . ? Cu4 N7 2.03(4) . ? Cu4 O5 2.30(3) 3_666 ? Cu4 Cu4 3.143(11) 3_666 ? O1 H1 0.8514 . ? O2 Cu2 2.31(3) 3_556 ? O2 H2 0.8555 . ? O3 H3 0.8502 . ? O3 H4 0.8503 . ? N1 C1 1.30(6) . ? N1 C5 1.41(6) . ? N2 C10 1.32(7) . ? N2 C6 1.35(7) . ? C1 C2 1.40(7) . ? C1 H1A 0.9300 . ? C2 C3 1.33(8) . ? C2 H2A 0.9300 . ? C3 C4 1.42(8) . ? C3 H3A 0.9300 . ? C4 C5 1.37(7) . ? C4 H4A 0.9300 . ? C5 C6 1.43(8) . ? C6 C7 1.40(7) . ? C7 C8 1.37(8) . ? C7 H7A 0.9300 . ? C8 C9 1.39(10) . ? C8 H8A 0.9300 . ? C9 C10 1.37(8) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? N3 C11 1.31(6) . ? N3 C15 1.37(6) . ? N4 C20 1.35(6) . ? N4 C16 1.35(7) . ? C11 C12 1.38(7) . ? C11 H11A 0.9300 . ? C12 C13 1.36(9) . ? C12 H12A 0.9300 . ? C13 C14 1.40(8) . ? C13 H13A 0.9300 . ? C14 C15 1.38(7) . ? C14 H14A 0.9300 . ? C15 C16 1.46(7) . ? C16 C17 1.38(7) . ? C17 C18 1.35(8) . ? C17 H17A 0.9300 . ? C18 C19 1.38(8) . ? C18 H18A 0.9300 . ? C19 C20 1.36(7) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? O4 H5 0.8527 . ? O5 Cu4 2.30(3) 3_666 ? O5 H6 0.8547 . ? O6 H7 0.8101 . ? O6 H8 0.8103 . ? N5 C21 1.31(6) . ? N5 C25 1.36(6) . ? N6 C30 1.34(6) . ? N6 C26 1.36(6) . ? C21 C22 1.37(8) . ? C21 H21A 0.9300 . ? C22 C23 1.36(9) . ? C22 H22A 0.9300 . ? C23 C24 1.42(8) . ? C23 H23A 0.9300 . ? C24 C25 1.38(7) . ? C24 H24A 0.9300 . ? C25 C26 1.49(7) . ? C26 C27 1.40(7) . ? C27 C28 1.37(8) . ? C27 H27A 0.9300 . ? C28 C29 1.35(8) . ? C28 H28A 0.9300 . ? C29 C30 1.38(7) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? N7 C31 1.33(6) . ? N7 C35 1.33(6) . ? N8 C40 1.33(6) . ? N8 C36 1.36(6) . ? C31 C32 1.36(7) . ? C31 H31A 0.9300 . ? C32 C33 1.36(8) . ? C32 H32A 0.9300 . ? C33 C34 1.44(8) . ? C33 H33A 0.9300 . ? C34 C35 1.39(7) . ? C34 H34A 0.9300 . ? C35 C36 1.48(7) . ? C36 C37 1.39(7) . ? C37 C38 1.37(8) . ? C37 H37A 0.9300 . ? C38 C39 1.39(9) . ? C38 H38A 0.9300 . ? C39 C40 1.37(7) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? O7 C41 1.26(8) . ? O8 C41 1.28(8) . ? C41 C42A 1.50(8) . ? C41 C42B 1.54(9) . ? C42A C43A 1.50(8) . ? C42A H42A 0.9700 . ? C42A H42D 0.9700 . ? C42B C43B 1.49(9) . ? C42B H42B 0.9700 . ? C42B H42C 0.9700 . ? C43A C44 1.52(7) . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C43B C44 1.52(9) . ? C43B H43C 0.9700 . ? C43B H43D 0.9700 . ? C44 C45 1.50(7) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 O9 1.23(6) . ? C45 O10 1.27(6) . ? O11 C46 1.23(8) . ? O12 C46 1.25(8) . ? C46 C47B 1.53(8) . ? C46 C47A 1.53(9) . ? C47A C48A 1.50(9) . ? C47A H47A 0.9700 . ? C47A H47B 0.9700 . ? C47B C48B 1.49(8) . ? C47B H47C 0.9700 . ? C47B H47D 0.9700 . ? C48A C49 1.51(8) . ? C48A H48A 0.9700 . ? C48A H48B 0.9700 . ? C48B C49 1.57(8) . ? C48B H48C 0.9700 . ? C48B H48D 0.9700 . ? C49 C50 1.52(8) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 O13 1.25(7) . ? C50 O14 1.25(7) . ? OW1 H9 0.9065 . ? OW1 H10 0.8756 . ? OW2 H11 0.7147 . ? OW2 H12 0.8313 . ? OW3 H13 0.9062 . ? OW3 H14 0.8638 . ? OW4 H15 0.8648 . ? OW4 H16 0.9030 . ? OW5 H17 0.9034 . ? OW5 H18 0.8695 . ? OW6 H19 0.8913 . ? OW6 H20 0.9094 . ? OW7 H21 0.7577 . ? OW7 H22 0.7836 . ? OW8 H23 0.8936 . ? OW8 H24 0.8774 . ? OW9 H25 0.7811 . ? OW9 H26 0.7751 . ? OW10 H27 0.8784 . ? OW10 H28 0.8926 . ? OW11 H29 0.8938 . ? OW11 H30 0.8681 . ? OW12 H31 0.7627 . ? OW12 H32 0.7879 . ? OW13 H33 0.8732 . ? OW13 H34 0.8962 . ? OW14 H35 0.7842 . ? OW14 H36 0.8012 . ? OW15 H37 0.8030 . ? OW15 H38 0.8658 . ? OW16 H39 0.7995 . ? OW16 H40 0.7806 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O2 81.2(13) . . ? O1 Cu1 N1 168.6(16) . . ? O2 Cu1 N1 98.2(15) . . ? O1 Cu1 N2 94.7(16) . . ? O2 Cu1 N2 156.5(16) . . ? N1 Cu1 N2 81.2(18) . . ? O1 Cu1 O3 91.3(15) . . ? O2 Cu1 O3 98.8(14) . . ? N1 Cu1 O3 100.0(16) . . ? N2 Cu1 O3 104.5(16) . . ? O1 Cu1 Cu2 40.6(9) . . ? O2 Cu1 Cu2 41.7(9) . . ? N1 Cu1 Cu2 139.9(12) . . ? N2 Cu1 Cu2 134.0(13) . . ? O3 Cu1 Cu2 89.6(11) . . ? O1 Cu1 Cu2 81.2(10) . 3_556 ? O2 Cu1 Cu2 39.6(9) . 3_556 ? N1 Cu1 Cu2 91.0(12) . 3_556 ? N2 Cu1 Cu2 116.9(13) . 3_556 ? O3 Cu1 Cu2 138.3(11) . 3_556 ? Cu2 Cu1 Cu2 58.6(2) . 3_556 ? O1 Cu2 O2 82.1(13) . . ? O1 Cu2 N3 95.1(15) . . ? O2 Cu2 N3 175.7(15) . . ? O1 Cu2 N4 162.8(16) . . ? O2 Cu2 N4 100.9(14) . . ? N3 Cu2 N4 80.9(16) . . ? O1 Cu2 O2 96.4(13) . 3_556 ? O2 Cu2 O2 84.6(12) . 3_556 ? N3 Cu2 O2 98.9(14) . 3_556 ? N4 Cu2 O2 100.7(14) . 3_556 ? O1 Cu2 Cu1 40.4(10) . . ? O2 Cu2 Cu1 42.7(9) . . ? N3 Cu2 Cu1 133.9(12) . . ? N4 Cu2 Cu1 136.7(11) . . ? O2 Cu2 Cu1 97.9(8) 3_556 . ? O1 Cu2 Cu2 89.8(10) . 3_556 ? O2 Cu2 Cu2 46.7(9) . 3_556 ? N3 Cu2 Cu2 136.8(12) . 3_556 ? N4 Cu2 Cu2 104.6(12) . 3_556 ? O2 Cu2 Cu2 37.9(8) 3_556 3_556 ? Cu1 Cu2 Cu2 69.3(2) . 3_556 ? O1 Cu2 Cu1 129.7(11) . 3_556 ? O2 Cu2 Cu1 89.7(9) . 3_556 ? N3 Cu2 Cu1 94.6(12) . 3_556 ? N4 Cu2 Cu1 67.4(12) . 3_556 ? O2 Cu2 Cu1 33.3(8) 3_556 3_556 ? Cu1 Cu2 Cu1 121.4(2) . 3_556 ? Cu2 Cu2 Cu1 52.1(2) 3_556 3_556 ? O4 Cu3 O5 81.7(12) . . ? O4 Cu3 N6 169.4(15) . . ? O5 Cu3 N6 98.1(14) . . ? O4 Cu3 N5 95.3(14) . . ? O5 Cu3 N5 157.2(14) . . ? N6 Cu3 N5 80.7(16) . . ? O4 Cu3 O6 92.0(14) . . ? O5 Cu3 O6 96.6(14) . . ? N6 Cu3 O6 98.5(15) . . ? N5 Cu3 O6 106.1(15) . . ? O4 Cu3 Cu4 40.7(9) . . ? O5 Cu3 Cu4 42.0(9) . . ? N6 Cu3 Cu4 140.1(11) . . ? N5 Cu3 Cu4 134.9(11) . . ? O6 Cu3 Cu4 88.6(11) . . ? O4 Cu4 O5 81.8(13) . . ? O4 Cu4 N8 95.8(14) . . ? O5 Cu4 N8 176.3(14) . . ? O4 Cu4 N7 163.2(14) . . ? O5 Cu4 N7 100.4(14) . . ? N8 Cu4 N7 81.1(15) . . ? O4 Cu4 O5 99.8(12) . 3_666 ? O5 Cu4 O5 85.3(12) . 3_666 ? N8 Cu4 O5 97.9(13) . 3_666 ? N7 Cu4 O5 97.0(13) . 3_666 ? O4 Cu4 Cu3 40.5(9) . . ? O5 Cu4 Cu3 42.3(9) . . ? N8 Cu4 Cu3 134.8(11) . . ? N7 Cu4 Cu3 136.1(10) . . ? O5 Cu4 Cu3 100.4(8) 3_666 . ? O4 Cu4 Cu4 92.0(10) . 3_666 ? O5 Cu4 Cu4 46.9(9) . 3_666 ? N8 Cu4 Cu4 136.2(11) . 3_666 ? N7 Cu4 Cu4 101.6(11) . 3_666 ? O5 Cu4 Cu4 38.4(7) 3_666 3_666 ? Cu3 Cu4 Cu4 70.9(2) . 3_666 ? Cu1 O1 Cu2 99.1(14) . . ? Cu1 O1 H1 109.6 . . ? Cu2 O1 H1 114.6 . . ? Cu2 O2 Cu1 95.7(13) . . ? Cu2 O2 Cu2 95.4(12) . 3_556 ? Cu1 O2 Cu2 107.0(13) . 3_556 ? Cu2 O2 H2 120.4 . . ? Cu1 O2 H2 122.3 . . ? Cu2 O2 H2 112.0 3_556 . ? Cu1 O3 H3 116.3 . . ? Cu1 O3 H4 121.2 . . ? H3 O3 H4 107.5 . . ? C1 N1 C5 119(5) . . ? C1 N1 Cu1 128(4) . . ? C5 N1 Cu1 114(3) . . ? C10 N2 C6 119(5) . . ? C10 N2 Cu1 126(4) . . ? C6 N2 Cu1 115(3) . . ? N1 C1 C2 123(5) . . ? N1 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C3 C2 C1 119(6) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 119(5) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 120(5) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C4 C5 N1 119(5) . . ? C4 C5 C6 126(5) . . ? N1 C5 C6 115(4) . . ? N2 C6 C7 121(5) . . ? N2 C6 C5 115(5) . . ? C7 C6 C5 124(5) . . ? C8 C7 C6 118(6) . . ? C8 C7 H7A 121.0 . . ? C6 C7 H7A 121.0 . . ? C7 C8 C9 121(6) . . ? C7 C8 H8A 119.4 . . ? C9 C8 H8A 119.4 . . ? C10 C9 C8 117(6) . . ? C10 C9 H9A 121.6 . . ? C8 C9 H9A 121.6 . . ? N2 C10 C9 124(6) . . ? N2 C10 H10A 118.2 . . ? C9 C10 H10A 118.2 . . ? C11 N3 C15 119(5) . . ? C11 N3 Cu2 126(4) . . ? C15 N3 Cu2 115(3) . . ? C20 N4 C16 118(4) . . ? C20 N4 Cu2 127(3) . . ? C16 N4 Cu2 115(3) . . ? N3 C11 C12 124(5) . . ? N3 C11 H11A 118.1 . . ? C12 C11 H11A 118.1 . . ? C13 C12 C11 118(6) . . ? C13 C12 H12A 120.9 . . ? C11 C12 H12A 120.9 . . ? C12 C13 C14 120(6) . . ? C12 C13 H13A 120.1 . . ? C14 C13 H13A 120.1 . . ? C15 C14 C13 119(5) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? C14 C15 N3 121(5) . . ? C14 C15 C16 124(5) . . ? N3 C15 C16 115(4) . . ? N4 C16 C17 121(5) . . ? N4 C16 C15 114(4) . . ? C17 C16 C15 125(5) . . ? C18 C17 C16 119(6) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C17 C18 C19 121(6) . . ? C17 C18 H18A 119.6 . . ? C19 C18 H18A 119.6 . . ? C20 C19 C18 117(5) . . ? C20 C19 H19A 121.4 . . ? C18 C19 H19A 121.4 . . ? N4 C20 C19 124(5) . . ? N4 C20 H20A 118.1 . . ? C19 C20 H20A 118.1 . . ? Cu3 O4 Cu4 98.8(14) . . ? Cu3 O4 H5 109.4 . . ? Cu4 O4 H5 111.7 . . ? Cu4 O5 Cu3 95.7(13) . . ? Cu4 O5 Cu4 94.7(12) . 3_666 ? Cu3 O5 Cu4 110.4(14) . 3_666 ? Cu4 O5 H6 117.4 . . ? Cu3 O5 H6 141.3 . . ? Cu4 O5 H6 87.6 3_666 . ? Cu3 O6 H7 107.1 . . ? Cu3 O6 H8 126.6 . . ? H7 O6 H8 111.5 . . ? C21 N5 C25 118(5) . . ? C21 N5 Cu3 126(4) . . ? C25 N5 Cu3 115(3) . . ? C30 N6 C26 120(4) . . ? C30 N6 Cu3 126(3) . . ? C26 N6 Cu3 114(3) . . ? N5 C21 C22 124(6) . . ? N5 C21 H21A 118.1 . . ? C22 C21 H21A 118.1 . . ? C23 C22 C21 119(6) . . ? C23 C22 H22A 120.7 . . ? C21 C22 H22A 120.7 . . ? C22 C23 C24 120(5) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C25 C24 C23 116(5) . . ? C25 C24 H24A 121.8 . . ? C23 C24 H24A 121.8 . . ? N5 C25 C24 123(5) . . ? N5 C25 C26 113(4) . . ? C24 C25 C26 124(5) . . ? N6 C26 C27 120(5) . . ? N6 C26 C25 116(4) . . ? C27 C26 C25 124(5) . . ? C28 C27 C26 118(5) . . ? C28 C27 H27A 120.9 . . ? C26 C27 H27A 120.9 . . ? C29 C28 C27 121(5) . . ? C29 C28 H28A 119.4 . . ? C27 C28 H28A 119.4 . . ? C28 C29 C30 119(5) . . ? C28 C29 H29A 120.5 . . ? C30 C29 H29A 120.5 . . ? N6 C30 C29 122(5) . . ? N6 C30 H30A 119.2 . . ? C29 C30 H30A 119.2 . . ? C31 N7 C35 120(4) . . ? C31 N7 Cu4 127(3) . . ? C35 N7 Cu4 113(3) . . ? C40 N8 C36 119(4) . . ? C40 N8 Cu4 126(3) . . ? C36 N8 Cu4 115(3) . . ? N7 C31 C32 123(5) . . ? N7 C31 H31A 118.7 . . ? C32 C31 H31A 118.7 . . ? C31 C32 C33 119(5) . . ? C31 C32 H32A 120.4 . . ? C33 C32 H32A 120.4 . . ? C32 C33 C34 120(5) . . ? C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C35 C34 C33 116(5) . . ? C35 C34 H34A 122.2 . . ? C33 C34 H34A 122.2 . . ? N7 C35 C34 123(5) . . ? N7 C35 C36 116(4) . . ? C34 C35 C36 121(5) . . ? N8 C36 C37 121(5) . . ? N8 C36 C35 114(4) . . ? C37 C36 C35 125(5) . . ? C38 C37 C36 119(6) . . ? C38 C37 H37A 120.5 . . ? C36 C37 H37A 120.5 . . ? C37 C38 C39 119(5) . . ? C37 C38 H38A 120.6 . . ? C39 C38 H38A 120.6 . . ? C40 C39 C38 120(5) . . ? C40 C39 H39A 120.2 . . ? C38 C39 H39A 120.2 . . ? N8 C40 C39 122(5) . . ? N8 C40 H40A 119.0 . . ? C39 C40 H40A 119.0 . . ? O7 C41 O8 120(6) . . ? O7 C41 C42A 111(7) . . ? O8 C41 C42A 129(7) . . ? O7 C41 C42B 135(9) . . ? O8 C41 C42B 102(8) . . ? C42A C41 C42B 32(6) . . ? C41 C42A C43A 117(7) . . ? C41 C42A H42A 108.1 . . ? C43A C42A H42A 108.2 . . ? C41 C42A H42D 108.1 . . ? C43A C42A H42D 108.1 . . ? H42A C42A H42D 107.3 . . ? C43B C42B C41 112(9) . . ? C43B C42B H42B 109.1 . . ? C41 C42B H42B 109.1 . . ? C43B C42B H42C 109.3 . . ? C41 C42B H42C 109.3 . . ? H42B C42B H42C 107.9 . . ? C42A C43A C44 111(6) . . ? C42A C43A H43A 109.5 . . ? C44 C43A H43A 109.5 . . ? C42A C43A H43B 109.4 . . ? C44 C43A H43B 109.5 . . ? H43A C43A H43B 108.1 . . ? C42B C43B C44 112(9) . . ? C42B C43B H43C 109.3 . . ? C44 C43B H43C 109.2 . . ? C42B C43B H43D 109.0 . . ? C44 C43B H43D 109.2 . . ? H43C C43B H43D 107.9 . . ? C45 C44 C43A 111(6) . . ? C45 C44 C43B 114(8) . . ? C43A C44 C43B 36(7) . . ? C45 C44 H44A 109.4 . . ? C43A C44 H44A 109.4 . . ? C43B C44 H44A 75.4 . . ? C45 C44 H44B 109.4 . . ? C43A C44 H44B 109.4 . . ? C43B C44 H44B 132.4 . . ? H44A C44 H44B 108.0 . . ? O9 C45 O10 122(5) . . ? O9 C45 C44 119(5) . . ? O10 C45 C44 119(5) . . ? O11 C46 O12 123(6) . . ? O11 C46 C47B 125(8) . . ? O12 C46 C47B 110(7) . . ? O11 C46 C47A 104(8) . . ? O12 C46 C47A 131(7) . . ? C47B C46 C47A 32(6) . . ? C48A C47A C46 115(9) . . ? C48A C47A H47A 108.5 . . ? C46 C47A H47A 108.5 . . ? C48A C47A H47B 108.4 . . ? C46 C47A H47B 108.4 . . ? H47A C47A H47B 107.5 . . ? C48B C47B C46 107(7) . . ? C48B C47B H47C 110.3 . . ? C46 C47B H47C 110.3 . . ? C48B C47B H47D 110.1 . . ? C46 C47B H47D 110.2 . . ? H47C C47B H47D 108.5 . . ? C47A C48A C49 110(8) . . ? C47A C48A H48A 109.7 . . ? C49 C48A H48A 109.7 . . ? C47A C48A H48B 109.7 . . ? C49 C48A H48B 109.7 . . ? H48A C48A H48B 108.2 . . ? C47B C48B C49 113(7) . . ? C47B C48B H48C 109.0 . . ? C49 C48B H48C 109.0 . . ? C47B C48B H48D 109.1 . . ? C49 C48B H48D 109.1 . . ? H48C C48B H48D 107.8 . . ? C48A C49 C50 128(7) . . ? C48A C49 C48B 36(6) . . ? C50 C49 C48B 100(6) . . ? C48A C49 H49A 105.4 . . ? C50 C49 H49A 105.4 . . ? C48B C49 H49A 141.1 . . ? C48A C49 H49B 105.4 . . ? C50 C49 H49B 105.4 . . ? C48B C49 H49B 95.1 . . ? H49A C49 H49B 106.0 . . ? O13 C50 O14 123(6) . . ? O13 C50 C49 119(5) . . ? O14 C50 C49 118(6) . . ? H9 OW1 H10 88.2 . . ? H11 OW2 H12 102.1 . . ? H13 OW3 H14 119.4 . . ? H15 OW4 H16 118.9 . . ? H17 OW5 H18 115.0 . . ? H19 OW6 H20 104.1 . . ? H21 OW7 H22 104.9 . . ? H23 OW8 H24 94.5 . . ? H25 OW9 H26 112.2 . . ? H27 OW10 H28 78.5 . . ? H29 OW11 H30 128.3 . . ? H31 OW12 H32 101.3 . . ? H33 OW13 H34 99.4 . . ? H35 OW14 H36 110.0 . . ? H37 OW15 H38 98.5 . . ? H39 OW16 H40 107.8 . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.947 _refine_diff_density_min -0.837 _refine_diff_density_rms 0.183 # Attachment '_CuOH_n1.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 725665' #TrackingRef '_CuOH_n1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H62 Cu4 N10 O22' _chemical_formula_weight 1459.14 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 0.2630 1.2660 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5976(19) _cell_length_b 12.781(3) _cell_length_c 13.532(3) _cell_angle_alpha 79.90(3) _cell_angle_beta 75.40(3) _cell_angle_gamma 76.63(3) _cell_volume 1550.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11728 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.46 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.784 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15452 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7047 _reflns_number_gt 5530 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku,1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC,2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Johnson,1976)' _computing_publication_material SHELXTL97 _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^)+(0.0670P)^2^+1.3187P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary PATTERSON _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 7047 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1628 _refine_ls_wR_factor_gt 0.1545 _refine_ls_goodness_of_fit_ref 1.332 _refine_ls_restrained_S_all 1.332 _refine_ls_shift/su_max 0.014 _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 0.91893(5) 0.70753(3) 0.56486(3) 0.02970(14) Uani 1 1 d . . . Cu2 Cu 0.82631(5) 0.51311(3) 0.54563(3) 0.02910(14) Uani 1 1 d . . . O1 O 0.8267(3) 0.5953(2) 0.6514(2) 0.0350(6) Uani 1 1 d . . . H1 H 0.7452 0.6240 0.6802 0.042 Uiso 1 1 d . . . O2 O 0.9549(3) 0.60904(19) 0.46006(18) 0.0291(5) Uani 1 1 d . . . H2 H 0.9422 0.6432 0.4062 0.035 Uiso 1 1 d . . . O3 O 0.6999(4) 0.7985(3) 0.5336(2) 0.0540(8) Uani 1 1 d . . . H3 H 0.6813 0.8495 0.4911 0.065 Uiso 1 1 d . . . H4 H 0.6536 0.8212 0.5890 0.065 Uiso 1 1 d . . . N1 N 1.0494(4) 0.8094(2) 0.4835(3) 0.0336(7) Uani 1 1 d . . . N2 N 0.9548(4) 0.7685(3) 0.6817(3) 0.0364(7) Uani 1 1 d . . . C1 C 1.0893(5) 0.8267(3) 0.3817(3) 0.0423(9) Uani 1 1 d . . . H1A H 1.0518 0.7915 0.3427 0.051 Uiso 1 1 calc R . . C2 C 1.1851(5) 0.8956(4) 0.3312(4) 0.0507(11) Uani 1 1 d . . . H2A H 1.2119 0.9063 0.2597 0.061 Uiso 1 1 calc R . . C3 C 1.2391(5) 0.9474(4) 0.3897(4) 0.0541(12) Uani 1 1 d . . . H3A H 1.3030 0.9942 0.3580 0.065 Uiso 1 1 calc R . . C4 C 1.1983(5) 0.9300(4) 0.4955(4) 0.0489(11) Uani 1 1 d . . . H4A H 1.2347 0.9646 0.5357 0.059 Uiso 1 1 calc R . . C5 C 1.1029(4) 0.8607(3) 0.5410(3) 0.0358(8) Uani 1 1 d . . . C6 C 1.0501(4) 0.8364(3) 0.6533(3) 0.0363(8) Uani 1 1 d . . . C7 C 1.0942(5) 0.8772(4) 0.7263(4) 0.0511(11) Uani 1 1 d . . . H7A H 1.1607 0.9236 0.7057 0.061 Uiso 1 1 calc R . . C8 C 1.0405(6) 0.8493(4) 0.8279(4) 0.0567(13) Uani 1 1 d . . . H8A H 1.0682 0.8775 0.8772 0.068 Uiso 1 1 calc R . . C9 C 0.9439(6) 0.7785(5) 0.8571(4) 0.0576(13) Uani 1 1 d . . . H9A H 0.9074 0.7570 0.9264 0.069 Uiso 1 1 calc R . . C10 C 0.9026(5) 0.7401(4) 0.7818(3) 0.0491(11) Uani 1 1 d . . . H10A H 0.8367 0.6932 0.8013 0.059 Uiso 1 1 calc R . . N3 N 0.6859(4) 0.4233(3) 0.6326(3) 0.0363(7) Uani 1 1 d . . . N4 N 0.7711(4) 0.4565(3) 0.4338(3) 0.0349(7) Uani 1 1 d . . . C11 C 0.6544(5) 0.4078(4) 0.7358(4) 0.0465(10) Uani 1 1 d . . . H11A H 0.7039 0.4380 0.7710 0.056 Uiso 1 1 calc R . . C12 C 0.5508(5) 0.3483(4) 0.7911(4) 0.0580(13) Uani 1 1 d . . . H12A H 0.5298 0.3391 0.8627 0.070 Uiso 1 1 calc R . . C13 C 0.4787(6) 0.3028(4) 0.7384(5) 0.0633(14) Uani 1 1 d . . . H13A H 0.4083 0.2626 0.7742 0.076 Uiso 1 1 calc R . . C14 C 0.5117(5) 0.3174(4) 0.6332(5) 0.0559(13) Uani 1 1 d . . . H14A H 0.4645 0.2862 0.5972 0.067 Uiso 1 1 calc R . . C15 C 0.6164(4) 0.3791(3) 0.5797(4) 0.0392(9) Uani 1 1 d . . . C16 C 0.6632(4) 0.3993(3) 0.4675(3) 0.0378(9) Uani 1 1 d . . . C17 C 0.6044(5) 0.3626(4) 0.3991(4) 0.0516(12) Uani 1 1 d . . . H17A H 0.5299 0.3230 0.4231 0.062 Uiso 1 1 calc R . . C18 C 0.6590(6) 0.3861(4) 0.2947(4) 0.0572(13) Uani 1 1 d . . . H18A H 0.6202 0.3630 0.2477 0.069 Uiso 1 1 calc R . . C19 C 0.7709(6) 0.4438(4) 0.2600(4) 0.0509(11) Uani 1 1 d . . . H19A H 0.8085 0.4598 0.1899 0.061 Uiso 1 1 calc R . . C20 C 0.8256(5) 0.4771(3) 0.3315(3) 0.0421(9) Uani 1 1 d . . . H20A H 0.9022 0.5148 0.3088 0.051 Uiso 1 1 calc R . . C27 C 0.5145(5) 0.8057(3) 0.7837(3) 0.0409(9) Uani 1 1 d . . . O4 O 0.5709(3) 0.7068(2) 0.7871(2) 0.0462(7) Uani 1 1 d . . . O5 O 0.5354(4) 0.8741(3) 0.7057(3) 0.0647(10) Uani 1 1 d . . . O6A O 0.8498(11) 0.7746(13) 0.1311(8) 0.091(4) Uiso 0.54(2) 1 d P A 1 O6B O 0.8639(10) 0.7215(12) 0.1232(7) 0.066(4) Uiso 0.46(2) 1 d P A 2 N5 N 0.8987(5) 0.7303(4) 0.2035(4) 0.0607(11) Uani 1 1 d . . . O7 O 1.0114(6) 0.6672(5) 0.2143(5) 0.1167(19) Uani 1 1 d . A . O8 O 0.8301(6) 0.7561(5) 0.2875(4) 0.119(2) Uani 1 1 d . A . OW1 O 0.6529(5) 0.9447(3) 0.3600(3) 0.0738(11) Uani 1 1 d . . . H9 H 0.5980 1.0023 0.3335 0.089 Uiso 1 1 d . . . H10 H 0.6552 0.8869 0.3322 0.089 Uiso 1 1 d . . . OW2 O 0.6165(5) 0.5468(4) 0.9537(4) 0.1037(17) Uani 1 1 d . . . H5 H 0.5934 0.5931 0.9014 0.124 Uiso 1 1 d . . . H6 H 0.7099 0.5159 0.9425 0.124 Uiso 1 1 d . . . OW3A O 1.1116(12) 0.5551(10) 0.0117(11) 0.090(4) Uiso 0.54(2) 1 d P A 1 OW3B O 1.0908(14) 0.5157(13) 0.0555(13) 0.094(5) Uiso 0.46(2) 1 d P A 2 H7 H 1.0659 0.5793 0.0709 0.113 Uiso 1 1 d . . . H8 H 1.1045 0.4927 -0.0035 0.113 Uiso 1 1 d . . . C26 C 0.4075(4) 0.8424(3) 0.8797(3) 0.0547(12) Uiso 1 1 d G . . C24 C 0.3356(5) 0.7680(2) 0.9495(3) 0.0689(15) Uiso 1 1 d G . . H24A H 0.3599 0.6951 0.9400 0.083 Uiso 1 1 calc R . . C21 C 0.2275(5) 0.8025(4) 1.0335(3) 0.098(2) Uiso 1 1 d G . . H21A H 0.1794 0.7527 1.0801 0.117 Uiso 1 1 calc R . . C22 C 0.1912(5) 0.9114(4) 1.0477(3) 0.112(3) Uiso 1 1 d G . . H22A H 0.1189 0.9345 1.1039 0.134 Uiso 1 1 calc R . . C23 C 0.2631(6) 0.9858(3) 0.9779(4) 0.126(3) Uiso 1 1 d G . . H23A H 0.2389 1.0587 0.9874 0.151 Uiso 1 1 calc R . . C25 C 0.3713(5) 0.9513(3) 0.8940(3) 0.094(2) Uiso 1 1 d G . . H25A H 0.4194 1.0011 0.8473 0.113 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 0.0331(3) 0.0273(2) 0.0310(2) -0.00650(18) -0.00632(18) -0.00929(18) Cu2 0.0277(2) 0.0293(2) 0.0326(3) -0.00494(19) -0.00631(18) -0.00977(18) O1 0.0374(15) 0.0346(14) 0.0326(13) -0.0073(11) -0.0014(11) -0.0110(11) O2 0.0331(13) 0.0276(12) 0.0273(12) -0.0033(10) -0.0065(10) -0.0077(10) O3 0.0495(19) 0.0523(18) 0.0487(18) -0.0006(15) -0.0098(15) 0.0077(15) N1 0.0346(17) 0.0284(15) 0.0403(17) -0.0048(14) -0.0104(14) -0.0084(13) N2 0.0389(18) 0.0364(17) 0.0354(17) -0.0086(14) -0.0104(14) -0.0050(14) C1 0.047(2) 0.040(2) 0.042(2) 0.0022(18) -0.0129(19) -0.0154(18) C2 0.054(3) 0.047(2) 0.048(3) 0.006(2) -0.008(2) -0.016(2) C3 0.050(3) 0.043(2) 0.071(3) 0.001(2) -0.010(2) -0.023(2) C4 0.050(3) 0.041(2) 0.064(3) -0.009(2) -0.016(2) -0.019(2) C5 0.033(2) 0.0258(17) 0.050(2) -0.0074(17) -0.0133(17) -0.0027(14) C6 0.035(2) 0.0293(18) 0.048(2) -0.0114(17) -0.0152(17) -0.0020(15) C7 0.052(3) 0.049(3) 0.064(3) -0.023(2) -0.022(2) -0.010(2) C8 0.061(3) 0.064(3) 0.055(3) -0.030(3) -0.027(2) 0.001(2) C9 0.063(3) 0.072(3) 0.040(2) -0.019(2) -0.014(2) -0.004(3) C10 0.051(3) 0.061(3) 0.037(2) -0.014(2) -0.0072(19) -0.011(2) N3 0.0291(16) 0.0339(16) 0.0451(19) -0.0022(15) -0.0072(14) -0.0077(13) N4 0.0325(17) 0.0319(16) 0.0448(18) -0.0073(14) -0.0158(14) -0.0053(13) C11 0.041(2) 0.046(2) 0.049(2) 0.001(2) -0.0094(19) -0.0088(19) C12 0.044(3) 0.061(3) 0.056(3) 0.012(2) 0.000(2) -0.012(2) C13 0.040(3) 0.061(3) 0.081(4) 0.011(3) 0.000(3) -0.023(2) C14 0.032(2) 0.044(2) 0.093(4) -0.004(3) -0.016(2) -0.0133(19) C15 0.0260(19) 0.0305(19) 0.062(3) -0.0054(18) -0.0135(18) -0.0036(15) C16 0.0313(19) 0.0294(18) 0.057(2) -0.0074(18) -0.0181(18) -0.0045(15) C17 0.043(2) 0.043(2) 0.082(4) -0.018(2) -0.030(2) -0.0088(19) C18 0.060(3) 0.053(3) 0.073(3) -0.026(3) -0.037(3) -0.001(2) C19 0.061(3) 0.048(2) 0.049(3) -0.013(2) -0.025(2) -0.002(2) C20 0.047(2) 0.037(2) 0.046(2) -0.0076(18) -0.0175(19) -0.0045(18) C27 0.037(2) 0.043(2) 0.042(2) -0.0071(19) -0.0055(17) -0.0109(18) O4 0.0450(17) 0.0439(16) 0.0442(16) -0.0055(14) 0.0002(13) -0.0091(13) O5 0.074(2) 0.0477(19) 0.055(2) 0.0000(17) 0.0095(18) -0.0074(17) N5 0.052(3) 0.076(3) 0.053(2) -0.011(2) -0.006(2) -0.014(2) O7 0.081(4) 0.105(4) 0.150(5) 0.023(4) -0.038(4) -0.005(3) O8 0.093(4) 0.162(6) 0.114(4) -0.075(4) -0.022(3) -0.007(4) OW1 0.103(3) 0.060(2) 0.057(2) -0.0043(18) -0.031(2) -0.003(2) OW2 0.077(3) 0.102(4) 0.106(4) 0.037(3) -0.019(3) -0.003(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 Cu1 O1 1.921(3) . ? Cu1 O2 1.973(2) . ? Cu1 N1 2.008(3) . ? Cu1 N2 2.014(3) . ? Cu1 O3 2.257(3) . ? Cu1 Cu2 2.8978(8) . ? Cu1 H1 2.2985 . ? Cu2 O1 1.920(3) . ? Cu2 O2 1.962(3) . ? Cu2 N3 1.990(3) . ? Cu2 N4 2.015(3) . ? Cu2 O2 2.301(3) 2_766 ? Cu2 Cu2 3.2104(13) 2_766 ? O1 H1 0.8135 . ? O2 Cu2 2.301(3) 2_766 ? O2 H2 0.8040 . ? O3 H3 0.8086 . ? O3 H4 0.8329 . ? N1 C1 1.326(5) . ? N1 C5 1.354(5) . ? N2 C10 1.337(5) . ? N2 C6 1.346(5) . ? C1 C2 1.392(6) . ? C1 H1A 0.9300 . ? C2 C3 1.372(7) . ? C2 H2A 0.9300 . ? C3 C4 1.378(7) . ? C3 H3A 0.9300 . ? C4 C5 1.380(6) . ? C4 H4A 0.9300 . ? C5 C6 1.477(6) . ? C6 C7 1.386(6) . ? C7 C8 1.355(7) . ? C7 H7A 0.9300 . ? C8 C9 1.383(8) . ? C8 H8A 0.9300 . ? C9 C10 1.380(6) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? N3 C11 1.341(6) . ? N3 C15 1.355(5) . ? N4 C16 1.346(5) . ? N4 C20 1.352(5) . ? C11 C12 1.379(6) . ? C11 H11A 0.9300 . ? C12 C13 1.380(8) . ? C12 H12A 0.9300 . ? C13 C14 1.367(8) . ? C13 H13A 0.9300 . ? C14 C15 1.398(6) . ? C14 H14A 0.9300 . ? C15 C16 1.466(6) . ? C16 C17 1.390(6) . ? C17 C18 1.382(8) . ? C17 H17A 0.9300 . ? C18 C19 1.382(7) . ? C18 H18A 0.9300 . ? C19 C20 1.377(6) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C27 O4 1.252(5) . ? C27 O5 1.253(5) . ? C27 C26 1.511(5) . ? O6A N5 1.190(11) . ? O6B N5 1.245(11) . ? N5 O7 1.215(7) . ? N5 O8 1.220(6) . ? OW1 H9 0.8791 . ? OW1 H10 0.8788 . ? OW2 H5 0.8788 . ? OW2 H6 0.8778 . ? OW3A H7 0.8817 . ? OW3A H8 0.8795 . ? OW3B H7 0.8409 . ? OW3B H8 0.8667 . ? C26 C24 1.3900 . ? C26 C25 1.3900 . ? C24 C21 1.3900 . ? C24 H24A 0.9300 . ? C21 C22 1.3900 . ? C21 H21A 0.9300 . ? C22 C23 1.3900 . ? C22 H22A 0.9300 . ? C23 C25 1.3900 . ? C23 H23A 0.9300 . ? C25 H25A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O2 82.45(11) . . ? O1 Cu1 N1 169.19(13) . . ? O2 Cu1 N1 97.67(12) . . ? O1 Cu1 N2 94.93(13) . . ? O2 Cu1 N2 157.46(12) . . ? N1 Cu1 N2 80.79(13) . . ? O1 Cu1 O3 90.32(13) . . ? O2 Cu1 O3 94.70(12) . . ? N1 Cu1 O3 100.42(13) . . ? N2 Cu1 O3 107.73(13) . . ? O1 Cu1 Cu2 41.00(8) . . ? O2 Cu1 Cu2 42.43(7) . . ? N1 Cu1 Cu2 140.09(9) . . ? N2 Cu1 Cu2 134.81(10) . . ? O3 Cu1 Cu2 86.28(10) . . ? O1 Cu1 H1 19.7 . . ? O2 Cu1 H1 95.0 . . ? N1 Cu1 H1 166.6 . . ? N2 Cu1 H1 89.2 . . ? O3 Cu1 H1 74.1 . . ? Cu2 Cu1 H1 52.7 . . ? O1 Cu2 O2 82.77(11) . . ? O1 Cu2 N3 96.15(13) . . ? O2 Cu2 N3 176.59(12) . . ? O1 Cu2 N4 163.62(13) . . ? O2 Cu2 N4 99.30(12) . . ? N3 Cu2 N4 80.83(14) . . ? O1 Cu2 O2 101.51(11) . 2_766 ? O2 Cu2 O2 82.62(10) . 2_766 ? N3 Cu2 O2 100.78(12) . 2_766 ? N4 Cu2 O2 94.87(11) . 2_766 ? O1 Cu2 Cu1 41.03(8) . . ? O2 Cu2 Cu1 42.72(7) . . ? N3 Cu2 Cu1 135.55(10) . . ? N4 Cu2 Cu1 135.73(10) . . ? O2 Cu2 Cu1 99.77(6) 2_766 . ? O1 Cu2 Cu2 93.79(9) . 2_766 ? O2 Cu2 Cu2 45.31(8) . 2_766 ? N3 Cu2 Cu2 138.08(10) . 2_766 ? N4 Cu2 Cu2 99.18(10) . 2_766 ? O2 Cu2 Cu2 37.31(6) 2_766 2_766 ? Cu1 Cu2 Cu2 70.89(3) . 2_766 ? Cu2 O1 Cu1 97.97(12) . . ? Cu2 O1 H1 113.8 . . ? Cu1 O1 H1 107.4 . . ? Cu2 O2 Cu1 94.85(11) . . ? Cu2 O2 Cu2 97.38(10) . 2_766 ? Cu1 O2 Cu2 112.15(11) . 2_766 ? Cu2 O2 H2 124.0 . . ? Cu1 O2 H2 110.1 . . ? Cu2 O2 H2 116.2 2_766 . ? Cu1 O3 H3 129.8 . . ? Cu1 O3 H4 104.6 . . ? H3 O3 H4 103.2 . . ? C1 N1 C5 119.2(3) . . ? C1 N1 Cu1 126.0(3) . . ? C5 N1 Cu1 114.7(3) . . ? C10 N2 C6 119.2(4) . . ? C10 N2 Cu1 125.7(3) . . ? C6 N2 Cu1 114.8(3) . . ? N1 C1 C2 122.4(4) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C3 C2 C1 118.2(4) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? C2 C3 C4 119.9(4) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C3 C4 C5 119.1(4) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? N1 C5 C4 121.2(4) . . ? N1 C5 C6 114.7(3) . . ? C4 C5 C6 124.1(4) . . ? N2 C6 C7 120.9(4) . . ? N2 C6 C5 114.7(3) . . ? C7 C6 C5 124.4(4) . . ? C8 C7 C6 120.0(4) . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C9 119.2(4) . . ? C7 C8 H8A 120.4 . . ? C9 C8 H8A 120.4 . . ? C10 C9 C8 118.9(5) . . ? C10 C9 H9A 120.6 . . ? C8 C9 H9A 120.6 . . ? N2 C10 C9 121.8(5) . . ? N2 C10 H10A 119.1 . . ? C9 C10 H10A 119.1 . . ? C11 N3 C15 120.0(4) . . ? C11 N3 Cu2 125.1(3) . . ? C15 N3 Cu2 114.8(3) . . ? C16 N4 C20 119.5(3) . . ? C16 N4 Cu2 114.4(3) . . ? C20 N4 Cu2 126.0(3) . . ? N3 C11 C12 121.9(4) . . ? N3 C11 H11A 119.1 . . ? C12 C11 H11A 119.1 . . ? C11 C12 C13 118.8(5) . . ? C11 C12 H12A 120.6 . . ? C13 C12 H12A 120.6 . . ? C14 C13 C12 119.5(4) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C13 C14 C15 120.0(5) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? N3 C15 C14 119.7(4) . . ? N3 C15 C16 114.9(3) . . ? C14 C15 C16 125.4(4) . . ? N4 C16 C17 121.3(4) . . ? N4 C16 C15 114.6(3) . . ? C17 C16 C15 124.1(4) . . ? C18 C17 C16 118.6(4) . . ? C18 C17 H17A 120.7 . . ? C16 C17 H17A 120.7 . . ? C17 C18 C19 120.2(4) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? C20 C19 C18 118.5(5) . . ? C20 C19 H19A 120.8 . . ? C18 C19 H19A 120.8 . . ? N4 C20 C19 121.9(4) . . ? N4 C20 H20A 119.0 . . ? C19 C20 H20A 119.0 . . ? O4 C27 O5 124.8(4) . . ? O4 C27 C26 116.7(4) . . ? O5 C27 C26 118.4(4) . . ? O6A N5 O7 134.3(8) . . ? O6A N5 O8 116.8(8) . . ? O7 N5 O8 108.6(6) . . ? O6A N5 O6B 32.5(6) . . ? O7 N5 O6B 111.5(8) . . ? O8 N5 O6B 134.3(7) . . ? H9 OW1 H10 111.3 . . ? H5 OW2 H6 112.9 . . ? H7 OW3A H8 122.8 . . ? H7 OW3B H8 129.8 . . ? C24 C26 C25 120.0 . . ? C24 C26 C27 119.4(3) . . ? C25 C26 C27 120.4(3) . . ? C21 C24 C26 120.0 . . ? C21 C24 H24A 120.0 . . ? C26 C24 H24A 120.0 . . ? C24 C21 C22 120.0 . . ? C24 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C21 C22 C23 120.0 . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C25 120.0 . . ? C22 C23 H23A 120.0 . . ? C25 C23 H23A 120.0 . . ? C23 C25 C26 120.0 . . ? C23 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.115 _refine_diff_density_min -0.912 _refine_diff_density_rms 0.112 #================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 725666' #TrackingRef '_CuOH_n1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H54 Cu6 N18 O32' _chemical_formula_weight 1923.21 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 0.2630 1.2660 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' __symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.900(2) _cell_length_b 11.965(2) _cell_length_c 15.477(3) _cell_angle_alpha 98.08(3) _cell_angle_beta 108.35(3) _cell_angle_gamma 94.36(3) _cell_volume 1881.4(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11615 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 27.52 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 1.727 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.716 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; __diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18551 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8507 _reflns_number_gt 5187 _reflns_threshold_expression >2sigma(I) __computing_data_collection 'RAPID-AUTO (Rigaku,1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure Rigaku/MSC,2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Johnson,1976)' _computing_publication_material SHELXTL97 _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^)+(0.1591P)^2^+1.6787P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8507 _refine_ls_number_parameters 500 _refine_ls_number_restraints 74 _refine_ls_R_factor_all 0.1175 _refine_ls_R_factor_gt 0.0754 _refine_ls_wR_factor_ref 0.2722 _refine_ls_wR_factor_gt 0.2368 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.067 _refine_ls_shift/su_mean 0.003 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 0.21189(7) 1.06034(6) 0.23815(5) 0.0422(3) Uani 1 1 d . . . Cu2 Cu 0.35962(7) 1.19565(6) 0.41516(5) 0.0409(2) Uani 1 1 d . . . Cu3 Cu 0.42563(6) 0.93390(6) 0.40590(4) 0.0357(2) Uani 1 1 d . . . O1 O 0.1823(4) 1.1368(4) 0.3449(3) 0.0481(11) Uani 1 1 d . . . H1 H 0.1464 1.1907 0.3459 0.058 Uiso 1 1 d . . . O2 O 0.3925(4) 1.0794(3) 0.3240(3) 0.0402(9) Uani 1 1 d . . . H2 H 0.4421 1.1126 0.3069 0.048 Uiso 1 1 d . . . O3 O 0.6016(4) 0.9655(4) 0.4932(3) 0.0428(10) Uani 1 1 d . . . H3 H 0.6591 0.9827 0.4764 0.051 Uiso 1 1 d . . . N1 N 0.2344(6) 0.9597(4) 0.1302(3) 0.0453(12) Uani 1 1 d . . . N2 N 0.0264(6) 0.9956(5) 0.1728(4) 0.0476(13) Uani 1 1 d . . . C1 C 0.1190(9) 0.8256(7) -0.0072(5) 0.068(2) Uani 1 1 d . . . H1A H 0.0417 0.7836 -0.0470 0.081 Uiso 1 1 calc R . . C2 C 0.1212(7) 0.8995(5) 0.0709(4) 0.0492(16) Uani 1 1 d . . . C3 C 0.0050(7) 0.9164(5) 0.0962(4) 0.0486(16) Uani 1 1 d . . . C4 C -0.1173(8) 0.8589(7) 0.0476(5) 0.066(2) Uani 1 1 d . . . H4A H -0.1293 0.8033 -0.0038 0.079 Uiso 1 1 calc R . . C5 C -0.2193(8) 0.8837(7) 0.0748(6) 0.075(3) Uani 1 1 d . . . H5A H -0.3023 0.8472 0.0405 0.090 Uiso 1 1 calc R . . C6 C -0.2013(8) 0.9660(7) 0.1566(6) 0.072(2) Uani 1 1 d . . . H6A H -0.2701 0.9827 0.1775 0.087 Uiso 1 1 calc R . . C7 C -0.0747(7) 1.0188(6) 0.2024(5) 0.0586(19) Uani 1 1 d . . . H7A H -0.0588 1.0725 0.2556 0.070 Uiso 1 1 calc R . . C8 C 0.3426(8) 0.9504(6) 0.1124(5) 0.0564(18) Uani 1 1 d . . . H8A H 0.4188 0.9934 0.1531 0.068 Uiso 1 1 calc R . . C9 C 0.3495(9) 0.8795(7) 0.0358(6) 0.067(2) Uani 1 1 d . . . H9A H 0.4286 0.8749 0.0254 0.080 Uiso 1 1 calc R . . C10 C 0.2375(10) 0.8160(7) -0.0244(6) 0.077(3) Uani 1 1 d . . . H10A H 0.2398 0.7672 -0.0761 0.092 Uiso 1 1 calc R . . N3 N 0.5378(5) 1.2775(4) 0.4783(3) 0.0402(11) Uani 1 1 d . . . N4 N 0.3219(5) 1.3049(4) 0.5104(4) 0.0436(12) Uani 1 1 d . . . C11 C 0.6461(6) 1.2590(6) 0.4561(5) 0.0517(16) Uani 1 1 d . . . H11A H 0.6404 1.1986 0.4096 0.062 Uiso 1 1 calc R . . C12 C 0.7653(7) 1.3263(7) 0.4998(5) 0.0607(19) Uani 1 1 d . . . H12A H 0.8380 1.3113 0.4831 0.073 Uiso 1 1 calc R . . C13 C 0.7732(7) 1.4161(7) 0.5689(6) 0.064(2) Uani 1 1 d . . . H13A H 0.8515 1.4630 0.5994 0.076 Uiso 1 1 calc R . . C14 C 0.6655(7) 1.4350(6) 0.5916(5) 0.0521(17) Uani 1 1 d . . . H14A H 0.6703 1.4948 0.6384 0.063 Uiso 1 1 calc R . . C15 C 0.5479(6) 1.3660(5) 0.5459(4) 0.0432(14) Uani 1 1 d . . . C16 C 0.4251(6) 1.3811(5) 0.5654(4) 0.0422(14) Uani 1 1 d . . . C17 C 0.4143(8) 1.4630(6) 0.6327(5) 0.0550(18) Uani 1 1 d . . . H17A H 0.4860 1.5145 0.6698 0.066 Uiso 1 1 calc R . . C18 C 0.2926(8) 1.4675(6) 0.6445(5) 0.0595(19) Uani 1 1 d . . . H18A H 0.2813 1.5230 0.6888 0.071 Uiso 1 1 calc R . . C19 C 0.1908(8) 1.3887(6) 0.5895(6) 0.0598(18) Uani 1 1 d . . . H19A H 0.1103 1.3879 0.5984 0.072 Uiso 1 1 calc R . . C20 C 0.2068(7) 1.3114(6) 0.5217(5) 0.0518(16) Uani 1 1 d . . . H20A H 0.1350 1.2619 0.4822 0.062 Uiso 1 1 calc R . . N5 N 0.4594(5) 0.8234(4) 0.3076(3) 0.0406(11) Uani 1 1 d . . . N6 N 0.2430(5) 0.8523(4) 0.3410(3) 0.0412(11) Uani 1 1 d . . . C21 C 0.5725(7) 0.8204(6) 0.2918(5) 0.0512(16) Uani 1 1 d . . . H21A H 0.6435 0.8727 0.3286 0.061 Uiso 1 1 calc R . . C22 C 0.5873(8) 0.7425(7) 0.2229(6) 0.0621(19) Uani 1 1 d . . . H22A H 0.6677 0.7409 0.2139 0.075 Uiso 1 1 calc R . . C23 C 0.4821(9) 0.6673(7) 0.1678(6) 0.068(2) Uani 1 1 d . . . H23A H 0.4901 0.6142 0.1205 0.081 Uiso 1 1 calc R . . C24 C 0.3631(8) 0.6703(6) 0.1825(5) 0.0551(18) Uani 1 1 d . . . H24A H 0.2907 0.6194 0.1456 0.066 Uiso 1 1 calc R . . C25 C 0.3544(6) 0.7503(5) 0.2529(4) 0.0419(14) Uani 1 1 d . . . C26 C 0.2337(6) 0.7658(5) 0.2726(4) 0.0419(14) Uani 1 1 d . . . C27 C 0.1149(7) 0.6973(6) 0.2246(5) 0.0565(18) Uani 1 1 d . . . H27A H 0.1094 0.6378 0.1773 0.068 Uiso 1 1 calc R . . C28 C 0.0082(8) 0.7185(7) 0.2479(6) 0.065(2) Uani 1 1 d . . . H28A H -0.0710 0.6734 0.2162 0.079 Uiso 1 1 calc R . . C29 C 0.0157(7) 0.8088(7) 0.3201(6) 0.063(2) Uani 1 1 d . . . H29A H -0.0567 0.8239 0.3371 0.075 Uiso 1 1 calc R . . C30 C 0.1347(6) 0.8729(6) 0.3637(5) 0.0513(16) Uani 1 1 d . . . H30A H 0.1419 0.9331 0.4108 0.062 Uiso 1 1 calc R . . N7 N 0.2794(9) 1.3096(6) 0.2105(5) 0.085(2) Uani 1 1 d . . . O4 O 0.2164(9) 1.2180(5) 0.1698(4) 0.106(3) Uani 1 1 d . . . O5 O 0.3523(7) 1.3202(5) 0.2916(4) 0.087(2) Uani 1 1 d . . . O6 O 0.2762(14) 1.3942(7) 0.1731(7) 0.194(6) Uani 1 1 d . . . N8 N 0.8443 1.0181 0.4229 0.117(4) Uani 1 1 d DU . . O7 O 0.7785 1.0495 0.3808 0.211(6) Uani 1 1 d DU . . O8 O 0.8498 0.9411 0.4496 0.292(9) Uani 1 1 d DU . . O9 O 0.9783 1.0935 0.4596 0.223(6) Uani 1 1 d DU . . N9 N 1.0492 1.6414 0.7184 0.362(17) Uani 1 1 d DU . . O10 O 1.1666 1.7102 0.7470 0.70(3) Uani 1 1 d DU . . O11 O 1.0635 1.5432 0.7342 0.266(8) Uani 1 1 d DU . . O12 O 0.9602 1.6656 0.6823 0.218(6) Uani 1 1 d DU . . OW1 O -0.0968(19) 0.5453(17) -0.0165(15) 0.289(9) Uani 1 1 d U . . OW2 O 1.4149(7) 1.8480(8) 0.7691(6) 0.130(3) Uani 1 1 d U . . OW3 O -0.2678(18) 0.5077(17) 0.1088(14) 0.272(9) Uani 1 1 d U . . OW4 O -0.493(2) 0.660(2) -0.0789(15) 0.310(10) Uani 1 1 d U . . 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 0.0459(5) 0.0376(4) 0.0312(4) -0.0026(3) 0.0006(3) 0.0012(3) Cu2 0.0407(4) 0.0336(4) 0.0376(4) -0.0060(3) 0.0042(3) -0.0011(3) Cu3 0.0371(4) 0.0331(4) 0.0286(4) -0.0027(3) 0.0039(3) 0.0000(3) O1 0.043(2) 0.047(3) 0.042(2) -0.0097(19) 0.0046(19) 0.0034(19) O2 0.045(2) 0.033(2) 0.033(2) -0.0002(16) 0.0037(17) -0.0005(17) O3 0.037(2) 0.051(3) 0.035(2) -0.0035(18) 0.0085(17) -0.0001(18) N1 0.057(3) 0.039(3) 0.031(2) 0.004(2) 0.005(2) 0.003(2) N2 0.053(3) 0.041(3) 0.035(3) -0.002(2) 0.002(2) -0.001(2) C1 0.090(6) 0.057(5) 0.042(4) -0.010(3) 0.011(4) 0.003(4) C2 0.067(4) 0.036(3) 0.032(3) 0.004(2) 0.001(3) 0.001(3) C3 0.054(4) 0.042(3) 0.035(3) 0.003(3) -0.003(3) -0.001(3) C4 0.062(5) 0.067(5) 0.049(4) -0.006(4) 0.002(4) -0.008(4) C5 0.055(5) 0.070(5) 0.068(5) 0.002(4) -0.017(4) -0.014(4) C6 0.055(5) 0.073(5) 0.076(6) 0.011(4) 0.004(4) 0.008(4) C7 0.049(4) 0.057(4) 0.055(4) -0.004(3) 0.003(3) 0.002(3) C8 0.065(5) 0.061(4) 0.038(3) 0.002(3) 0.013(3) 0.003(3) C9 0.072(5) 0.073(5) 0.052(4) 0.004(4) 0.019(4) 0.012(4) C10 0.117(8) 0.064(5) 0.050(4) -0.008(4) 0.034(5) 0.021(5) N3 0.045(3) 0.035(3) 0.034(2) 0.005(2) 0.006(2) 0.003(2) N4 0.051(3) 0.033(3) 0.040(3) -0.001(2) 0.008(2) 0.003(2) C11 0.047(4) 0.051(4) 0.048(4) 0.003(3) 0.006(3) 0.003(3) C12 0.046(4) 0.064(5) 0.061(5) 0.011(4) 0.005(3) -0.004(3) C13 0.049(4) 0.056(4) 0.067(5) 0.013(4) -0.003(4) -0.016(3) C14 0.057(4) 0.038(3) 0.044(4) 0.003(3) -0.002(3) -0.007(3) C15 0.053(4) 0.026(3) 0.039(3) 0.002(2) 0.001(3) -0.005(2) C16 0.052(4) 0.030(3) 0.036(3) 0.000(2) 0.006(3) 0.003(2) C17 0.075(5) 0.035(3) 0.041(3) -0.008(3) 0.009(3) -0.005(3) C18 0.077(5) 0.045(4) 0.054(4) -0.009(3) 0.024(4) 0.011(3) C19 0.064(5) 0.051(4) 0.067(5) 0.006(3) 0.028(4) 0.012(3) C20 0.056(4) 0.041(3) 0.049(4) -0.003(3) 0.010(3) 0.000(3) N5 0.045(3) 0.037(3) 0.034(3) 0.002(2) 0.006(2) 0.005(2) N6 0.046(3) 0.039(3) 0.032(2) 0.003(2) 0.005(2) 0.000(2) C21 0.057(4) 0.046(4) 0.045(4) 0.004(3) 0.011(3) 0.004(3) C22 0.070(5) 0.065(5) 0.056(4) 0.002(4) 0.027(4) 0.019(4) C23 0.094(6) 0.053(4) 0.051(4) -0.009(3) 0.023(4) 0.018(4) C24 0.068(5) 0.041(4) 0.043(4) -0.010(3) 0.011(3) -0.001(3) C25 0.052(4) 0.030(3) 0.034(3) 0.002(2) 0.005(3) 0.003(3) C26 0.047(3) 0.032(3) 0.036(3) 0.005(2) 0.001(3) -0.003(2) C27 0.055(4) 0.046(4) 0.050(4) -0.006(3) 0.001(3) -0.009(3) C28 0.049(4) 0.060(5) 0.068(5) 0.005(4) 0.001(4) -0.015(3) C29 0.048(4) 0.072(5) 0.061(5) 0.015(4) 0.008(3) -0.004(4) C30 0.042(4) 0.057(4) 0.047(4) 0.005(3) 0.008(3) -0.001(3) N7 0.136(7) 0.046(4) 0.058(4) 0.009(3) 0.015(4) -0.007(4) O4 0.183(7) 0.043(3) 0.047(3) 0.003(2) -0.013(4) -0.025(4) O5 0.107(5) 0.055(3) 0.069(4) 0.002(3) -0.003(3) -0.020(3) O6 0.305(14) 0.073(5) 0.124(7) 0.049(5) -0.041(8) -0.048(7) N8 0.152(7) 0.117(7) 0.078(5) 0.004(5) 0.037(5) 0.026(6) O7 0.211(10) 0.201(9) 0.205(10) 0.030(8) 0.045(8) 0.037(8) O8 0.295(12) 0.285(12) 0.295(12) 0.077(9) 0.088(9) 0.022(9) O9 0.197(9) 0.222(9) 0.236(10) 0.039(8) 0.059(8) -0.009(7) N9 0.344(19) 0.359(19) 0.367(19) 0.040(10) 0.099(11) 0.068(10) O10 0.70(4) 0.69(4) 0.70(4) 0.102(12) 0.241(15) 0.090(11) O11 0.265(11) 0.240(11) 0.277(11) 0.050(9) 0.071(8) 0.013(8) O12 0.201(9) 0.194(9) 0.235(10) 0.026(8) 0.039(7) 0.044(7) OW1 0.293(12) 0.279(12) 0.271(12) 0.067(9) 0.050(9) 0.053(9) OW2 0.078(4) 0.162(6) 0.127(6) -0.052(5) 0.040(4) -0.011(4) OW3 0.264(11) 0.279(12) 0.278(12) 0.023(9) 0.104(9) 0.060(9) OW4 0.301(13) 0.333(13) 0.295(13) 0.028(9) 0.101(9) 0.059(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.904(4) . ? Cu1 O2 1.973(4) . ? Cu1 N2 1.992(5) . ? Cu1 N1 2.010(5) . ? Cu1 O4 2.294(6) . ? Cu1 Cu2 2.8809(16) . ? Cu2 O1 1.915(4) . ? Cu2 O2 1.974(4) . ? Cu2 N3 1.983(5) . ? Cu2 N4 1.993(5) . ? Cu2 O3 2.534(5) 2_676 ? Cu2 O5 2.571(7) . ? Cu2 Cu3 3.2601(13) . ? Cu2 H1 2.2242 . ? Cu2 H2 2.2846 . ? Cu3 O3 1.940(4) . ? Cu3 O3 1.947(4) 2_676 ? Cu3 N5 2.014(5) . ? Cu3 N6 2.023(5) . ? Cu3 O2 2.279(4) . ? Cu3 Cu3 2.9928(17) 2_676 ? O1 H1 0.7805 . ? O2 H2 0.7799 . ? O3 Cu3 1.947(4) 2_676 ? O3 Cu2 2.534(5) 2_676 ? O3 H3 0.7758 . ? N1 C8 1.301(10) . ? N1 C2 1.360(8) . ? N2 C7 1.353(10) . ? N2 C3 1.355(8) . ? C1 C2 1.387(10) . ? C1 C10 1.408(13) . ? C1 H1A 0.9300 . ? C2 C3 1.458(10) . ? C3 C4 1.379(10) . ? C4 C5 1.346(13) . ? C4 H4A 0.9300 . ? C5 C6 1.441(12) . ? C5 H5A 0.9300 . ? C6 C7 1.390(11) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.384(10) . ? C8 H8A 0.9300 . ? C9 C10 1.371(12) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? N3 C15 1.351(8) . ? N3 C11 1.354(9) . ? N4 C20 1.326(9) . ? N4 C16 1.358(7) . ? C11 C12 1.389(9) . ? C11 H11A 0.9300 . ? C12 C13 1.383(11) . ? C12 H12A 0.9300 . ? C13 C14 1.352(11) . ? C13 H13A 0.9300 . ? C14 C15 1.389(9) . ? C14 H14A 0.9300 . ? C15 C16 1.480(9) . ? C16 C17 1.367(9) . ? C17 C18 1.398(11) . ? C17 H17A 0.9300 . ? C18 C19 1.366(10) . ? C18 H18A 0.9300 . ? C19 C20 1.361(10) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? N5 C21 1.332(9) . ? N5 C25 1.349(8) . ? N6 C26 1.345(8) . ? N6 C30 1.363(9) . ? C21 C22 1.373(10) . ? C21 H21A 0.9300 . ? C22 C23 1.366(11) . ? C22 H22A 0.9300 . ? C23 C24 1.388(11) . ? C23 H23A 0.9300 . ? C24 C25 1.378(9) . ? C24 H24A 0.9300 . ? C25 C26 1.461(9) . ? C26 C27 1.401(8) . ? C27 C28 1.353(12) . ? C27 H27A 0.9300 . ? C28 C29 1.419(12) . ? C28 H28A 0.9300 . ? C29 C30 1.370(10) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? N7 O4 1.220(8) . ? N7 O6 1.232(10) . ? N7 O5 1.239(9) . ? N8 O7 0.9468(3) . ? N8 O8 1.0593(2) . ? N8 O9 1.5503(6) . ? N9 O12 1.0412(3) . ? N9 O11 1.2447(3) . ? N9 O10 1.3756(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O2 81.95(18) . . ? O1 Cu1 N2 95.3(2) . . ? O2 Cu1 N2 160.4(2) . . ? O1 Cu1 N1 172.1(2) . . ? O2 Cu1 N1 99.1(2) . . ? N2 Cu1 N1 81.1(2) . . ? O1 Cu1 O4 95.7(2) . . ? O2 Cu1 O4 100.8(2) . . ? N2 Cu1 O4 98.8(3) . . ? N1 Cu1 O4 91.9(2) . . ? O1 Cu1 Cu2 41.18(13) . . ? O2 Cu1 Cu2 43.13(12) . . ? N2 Cu1 Cu2 136.38(17) . . ? N1 Cu1 Cu2 141.56(16) . . ? O4 Cu1 Cu2 89.95(13) . . ? O1 Cu2 O2 81.65(18) . . ? O1 Cu2 N3 171.1(2) . . ? O2 Cu2 N3 100.7(2) . . ? O1 Cu2 N4 96.9(2) . . ? O2 Cu2 N4 176.27(19) . . ? N3 Cu2 N4 81.2(2) . . ? O1 Cu2 O3 94.83(18) . 2_676 ? O2 Cu2 O3 80.16(16) . 2_676 ? N3 Cu2 O3 94.07(17) . 2_676 ? N4 Cu2 O3 96.58(19) . 2_676 ? O1 Cu2 O5 87.1(2) . . ? O2 Cu2 O5 82.66(19) . . ? N3 Cu2 O5 84.6(2) . . ? N4 Cu2 O5 100.7(2) . . ? O3 Cu2 O5 162.23(19) 2_676 . ? O1 Cu2 Cu1 40.89(13) . . ? O2 Cu2 Cu1 43.11(12) . . ? N3 Cu2 Cu1 138.23(16) . . ? N4 Cu2 Cu1 136.32(16) . . ? O3 Cu2 Cu1 97.58(10) 2_676 . ? O5 Cu2 Cu1 72.50(12) . . ? O1 Cu2 Cu3 88.01(14) . . ? O2 Cu2 Cu3 43.54(13) . . ? N3 Cu2 Cu3 99.67(15) . . ? N4 Cu2 Cu3 133.17(16) . . ? O3 Cu2 Cu3 36.63(10) 2_676 . ? O5 Cu2 Cu3 126.08(15) . . ? Cu1 Cu2 Cu3 69.31(4) . . ? O1 Cu2 H1 20.0 . . ? O2 Cu2 H1 98.0 . . ? N3 Cu2 H1 152.5 . . ? N4 Cu2 H1 81.2 . . ? O3 Cu2 H1 108.9 2_676 . ? O5 Cu2 H1 77.9 . . ? Cu1 Cu2 H1 55.1 . . ? Cu3 Cu2 H1 107.8 . . ? O1 Cu2 H2 94.5 . . ? O2 Cu2 H2 19.4 . . ? N3 Cu2 H2 85.8 . . ? N4 Cu2 H2 164.1 . . ? O3 Cu2 H2 93.5 2_676 . ? O5 Cu2 H2 68.8 . . ? Cu1 Cu2 H2 53.6 . . ? Cu3 Cu2 H2 58.2 . . ? H1 Cu2 H2 107.1 . . ? O3 Cu3 O3 79.3(2) . 2_676 ? O3 Cu3 N5 98.5(2) . . ? O3 Cu3 N5 176.22(19) 2_676 . ? O3 Cu3 N6 158.5(2) . . ? O3 Cu3 N6 100.6(2) 2_676 . ? N5 Cu3 N6 80.4(2) . . ? O3 Cu3 O2 107.58(18) . . ? O3 Cu3 O2 87.58(17) 2_676 . ? N5 Cu3 O2 96.02(19) . . ? N6 Cu3 O2 93.83(18) . . ? O3 Cu3 Cu3 39.73(13) . 2_676 ? O3 Cu3 Cu3 39.55(12) 2_676 2_676 ? N5 Cu3 Cu3 138.12(15) . 2_676 ? N6 Cu3 Cu3 136.28(16) . 2_676 ? O2 Cu3 Cu3 99.69(10) . 2_676 ? O3 Cu3 Cu2 97.45(14) . . ? O3 Cu3 Cu2 50.96(14) 2_676 . ? N5 Cu3 Cu2 132.64(15) . . ? N6 Cu3 Cu2 98.94(16) . . ? O2 Cu3 Cu2 36.62(10) . . ? Cu3 Cu3 Cu2 70.99(4) 2_676 . ? Cu1 O1 Cu2 97.9(2) . . ? Cu1 O1 H1 124.3 . . ? Cu2 O1 H1 103.0 . . ? Cu1 O2 Cu2 93.76(19) . . ? Cu1 O2 Cu3 110.86(18) . . ? Cu2 O2 Cu3 99.84(18) . . ? Cu1 O2 H2 113.3 . . ? Cu2 O2 H2 103.4 . . ? Cu3 O2 H2 127.9 . . ? Cu3 O3 Cu3 100.7(2) . 2_676 ? Cu3 O3 Cu2 108.04(19) . 2_676 ? Cu3 O3 Cu2 92.41(17) 2_676 2_676 ? Cu3 O3 H3 119.7 . . ? Cu3 O3 H3 119.0 2_676 . ? Cu2 O3 H3 113.1 2_676 . ? C8 N1 C2 119.7(6) . . ? C8 N1 Cu1 126.6(5) . . ? C2 N1 Cu1 113.6(5) . . ? C7 N2 C3 119.3(6) . . ? C7 N2 Cu1 125.3(4) . . ? C3 N2 Cu1 115.3(5) . . ? C2 C1 C10 118.0(7) . . ? C2 C1 H1A 121.0 . . ? C10 C1 H1A 121.0 . . ? N1 C2 C1 121.2(8) . . ? N1 C2 C3 115.7(6) . . ? C1 C2 C3 123.0(6) . . ? N2 C3 C4 121.6(7) . . ? N2 C3 C2 114.1(5) . . ? C4 C3 C2 124.3(6) . . ? C5 C4 C3 119.7(7) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C4 C5 C6 120.8(7) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C7 C6 C5 115.8(8) . . ? C7 C6 H6A 122.1 . . ? C5 C6 H6A 122.1 . . ? N2 C7 C6 122.8(7) . . ? N2 C7 H7A 118.6 . . ? C6 C7 H7A 118.6 . . ? N1 C8 C9 123.0(7) . . ? N1 C8 H8A 118.5 . . ? C9 C8 H8A 118.5 . . ? C10 C9 C8 118.7(8) . . ? C10 C9 H9A 120.6 . . ? C8 C9 H9A 120.6 . . ? C9 C10 C1 119.3(7) . . ? C9 C10 H10A 120.3 . . ? C1 C10 H10A 120.3 . . ? C15 N3 C11 117.7(5) . . ? C15 N3 Cu2 115.3(4) . . ? C11 N3 Cu2 126.8(4) . . ? C20 N4 C16 118.9(5) . . ? C20 N4 Cu2 126.1(4) . . ? C16 N4 Cu2 114.9(4) . . ? N3 C11 C12 122.9(7) . . ? N3 C11 H11A 118.5 . . ? C12 C11 H11A 118.5 . . ? C13 C12 C11 118.3(7) . . ? C13 C12 H12A 120.9 . . ? C11 C12 H12A 120.9 . . ? C14 C13 C12 119.1(6) . . ? C14 C13 H13A 120.4 . . ? C12 C13 H13A 120.4 . . ? C13 C14 C15 120.8(7) . . ? C13 C14 H14A 119.6 . . ? C15 C14 H14A 119.6 . . ? N3 C15 C14 121.2(7) . . ? N3 C15 C16 114.3(5) . . ? C14 C15 C16 124.5(6) . . ? N4 C16 C17 122.0(6) . . ? N4 C16 C15 114.0(5) . . ? C17 C16 C15 124.0(6) . . ? C16 C17 C18 118.3(6) . . ? C16 C17 H17A 120.8 . . ? C18 C17 H17A 120.8 . . ? C19 C18 C17 118.6(6) . . ? C19 C18 H18A 120.7 . . ? C17 C18 H18A 120.7 . . ? C20 C19 C18 120.2(7) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? N4 C20 C19 121.9(6) . . ? N4 C20 H20A 119.1 . . ? C19 C20 H20A 119.1 . . ? C21 N5 C25 119.6(5) . . ? C21 N5 Cu3 125.6(4) . . ? C25 N5 Cu3 114.8(4) . . ? C26 N6 C30 119.1(5) . . ? C26 N6 Cu3 114.4(4) . . ? C30 N6 Cu3 126.4(4) . . ? N5 C21 C22 122.0(6) . . ? N5 C21 H21A 119.0 . . ? C22 C21 H21A 119.0 . . ? C23 C22 C21 118.8(7) . . ? C23 C22 H22A 120.6 . . ? C21 C22 H22A 120.6 . . ? C22 C23 C24 119.9(7) . . ? C22 C23 H23A 120.1 . . ? C24 C23 H23A 120.1 . . ? C25 C24 C23 118.6(6) . . ? C25 C24 H24A 120.7 . . ? C23 C24 H24A 120.7 . . ? N5 C25 C24 121.1(6) . . ? N5 C25 C26 115.0(5) . . ? C24 C25 C26 123.9(6) . . ? N6 C26 C27 121.1(6) . . ? N6 C26 C25 115.3(5) . . ? C27 C26 C25 123.6(6) . . ? C28 C27 C26 119.2(7) . . ? C28 C27 H27A 120.4 . . ? C26 C27 H27A 120.4 . . ? C27 C28 C29 120.7(7) . . ? C27 C28 H28A 119.6 . . ? C29 C28 H28A 119.6 . . ? C30 C29 C28 116.9(7) . . ? C30 C29 H29A 121.5 . . ? C28 C29 H29A 121.5 . . ? N6 C30 C29 123.0(7) . . ? N6 C30 H30A 118.5 . . ? C29 C30 H30A 118.5 . . ? O4 N7 O6 122.2(8) . . ? O4 N7 O5 120.6(7) . . ? O6 N7 O5 117.1(7) . . ? N7 O4 Cu1 123.5(5) . . ? N7 O5 Cu2 130.8(5) . . ? O7 N8 O8 135.16(2) . . ? O7 N8 O9 113.75(2) . . ? O8 N8 O9 111.04(3) . . ? O12 N9 O11 123.66(3) . . ? O12 N9 O10 124.487(19) . . ? O11 N9 O10 111.61(3) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.527 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.151 #============================================================================ # END OF CIF #================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 751292' #TrackingRef '_CuOH_n1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H124 Cu6 N12 O32' _chemical_formula_weight 2483.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.725(3) _cell_length_b 17.232(3) _cell_length_c 21.155(4) _cell_angle_alpha 92.81(3) _cell_angle_beta 90.63(3) _cell_angle_gamma 118.60(3) _cell_volume 5342.3(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 41350 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2572 _exptl_absorpt_coefficient_mu 1.261 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4373 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50248 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 23854 _reflns_number_gt 18876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku,1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure Rigaku/MSC,2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Johnson,1976)' _computing_publication_material SHELXTL97 _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^)+(0.0903P)^2^+2.6326P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary PATTERSON _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef NONE _refine_ls_number_reflns 23854 _refine_ls_number_parameters 1381 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1784 _refine_ls_wR_factor_gt 0.1689 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.220 _refine_ls_shift/su_max 0.352 _refine_ls_shift/su_mean 0.008 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 0.36706(3) 0.48500(3) 0.179812(18) 0.01446(10) Uani 1 1 d . . . N1 N 0.23393(19) 0.4243(2) 0.19979(13) 0.0193(6) Uani 1 1 d . . . C1 C 0.1786(2) 0.3366(3) 0.19910(18) 0.0261(8) Uani 1 1 d . . . H1 H 0.2032 0.2986 0.1935 0.031 Uiso 1 1 calc R . . C2 C 0.0852(3) 0.3011(3) 0.20647(18) 0.0310(9) Uani 1 1 d . . . H2 H 0.0482 0.2400 0.2060 0.037 Uiso 1 1 calc R . . C3 C 0.0483(3) 0.3565(3) 0.21441(19) 0.0354(10) Uani 1 1 d . . . H3 H -0.0142 0.3335 0.2186 0.043 Uiso 1 1 calc R . . C4 C 0.1048(3) 0.4469(3) 0.21609(18) 0.0287(9) Uani 1 1 d . . . H4 H 0.0810 0.4855 0.2222 0.034 Uiso 1 1 calc R . . C5 C 0.1979(2) 0.4797(3) 0.20856(15) 0.0207(7) Uani 1 1 d . . . C6 C 0.2645(2) 0.5742(3) 0.20897(16) 0.0212(7) Uani 1 1 d . . . C7 C 0.2452(3) 0.6420(3) 0.2262(2) 0.0337(10) Uani 1 1 d . . . H7 H 0.1867 0.6289 0.2375 0.040 Uiso 1 1 calc R . . C8 C 0.3124(4) 0.7279(3) 0.2266(3) 0.0485(14) Uani 1 1 d . . . H8 H 0.3000 0.7737 0.2382 0.058 Uiso 1 1 calc R . . C9 C 0.3993(3) 0.7462(3) 0.2096(3) 0.0472(13) Uani 1 1 d . . . H9 H 0.4462 0.8043 0.2096 0.057 Uiso 1 1 calc R . . C10 C 0.4146(3) 0.6757(3) 0.19248(19) 0.0279(8) Uani 1 1 d . . . H10 H 0.4724 0.6876 0.1801 0.033 Uiso 1 1 calc R . . N2 N 0.3497(2) 0.5914(2) 0.19313(13) 0.0192(6) Uani 1 1 d . . . O1 O 0.37550(16) 0.38137(16) 0.15475(11) 0.0191(5) Uani 1 1 d . . . HW11 H 0.3493 0.3324 0.1717 0.023 Uiso 1 1 d R . . O2 O 0.47536(15) 0.53592(15) 0.12628(10) 0.0151(5) Uani 1 1 d . . . HW21 H 0.5134 0.5886 0.1306 0.018 Uiso 1 1 d R . . Cu2 Cu 0.49577(3) 0.43239(3) 0.124360(18) 0.01430(10) Uani 1 1 d . . . N3 N 0.63215(19) 0.4942(2) 0.12075(12) 0.0171(6) Uani 1 1 d . . . C11 C 0.6865(2) 0.5812(2) 0.11688(16) 0.0205(7) Uani 1 1 d . . . H11 H 0.6603 0.6178 0.1134 0.025 Uiso 1 1 calc R . . C12 C 0.7803(2) 0.6186(3) 0.11794(17) 0.0261(8) Uani 1 1 d . . . H12 H 0.8165 0.6793 0.1151 0.031 Uiso 1 1 calc R . . C13 C 0.8196(3) 0.5645(3) 0.12324(18) 0.0291(9) Uani 1 1 d . . . H13 H 0.8826 0.5883 0.1241 0.035 Uiso 1 1 calc R . . C14 C 0.7640(2) 0.4746(3) 0.12721(17) 0.0256(8) Uani 1 1 d . . . H14 H 0.7892 0.4371 0.1306 0.031 Uiso 1 1 calc R . . C15 C 0.6696(2) 0.4407(2) 0.12615(15) 0.0196(7) Uani 1 1 d . . . C16 C 0.6042(3) 0.3466(2) 0.13017(16) 0.0210(7) Uani 1 1 d . . . C17 C 0.6283(3) 0.2807(3) 0.13709(18) 0.0291(8) Uani 1 1 d . . . H17 H 0.6892 0.2946 0.1407 0.035 Uiso 1 1 calc R . . C18 C 0.5600(3) 0.1941(3) 0.1385(2) 0.0357(10) Uani 1 1 d . . . H18 H 0.5749 0.1492 0.1440 0.043 Uiso 1 1 calc R . . C19 C 0.4701(3) 0.1738(3) 0.13175(19) 0.0330(9) Uani 1 1 d . . . H19 H 0.4239 0.1154 0.1312 0.040 Uiso 1 1 calc R . . C20 C 0.4497(3) 0.2423(2) 0.12581(17) 0.0241(8) Uani 1 1 d . . . H20 H 0.3891 0.2293 0.1216 0.029 Uiso 1 1 calc R . . N4 N 0.5157(2) 0.3273(2) 0.12594(13) 0.0194(6) Uani 1 1 d . . . O3 O 0.54088(15) 0.57925(15) -0.01676(10) 0.0147(4) Uani 1 1 d . . . HW31 H 0.5737 0.6245 0.0036 0.018 Uiso 1 1 d R . . O4 O 0.44498(17) 0.50642(17) 0.26982(11) 0.0234(5) Uani 1 1 d . . . HW41 H 0.4217 0.4561 0.2846 0.028 Uiso 1 1 d R . . HW42 H 0.4698 0.5519 0.2962 0.028 Uiso 1 1 d R . . Cu3 Cu 0.42567(3) 0.51540(3) 0.024328(17) 0.01341(10) Uani 1 1 d . . . N5 N 0.29239(19) 0.4409(2) 0.03645(13) 0.0183(6) Uani 1 1 d . . . C21 C 0.2491(2) 0.3533(2) 0.03928(16) 0.0225(7) Uani 1 1 d . . . H21 H 0.2831 0.3236 0.0390 0.027 Uiso 1 1 calc R . . C22 C 0.1551(3) 0.3046(3) 0.04265(18) 0.0288(8) Uani 1 1 d . . . H22 H 0.1264 0.2432 0.0437 0.035 Uiso 1 1 calc R . . C23 C 0.1049(3) 0.3499(3) 0.04442(18) 0.0321(9) Uani 1 1 d . . . H23 H 0.0419 0.3191 0.0470 0.039 Uiso 1 1 calc R . . C24 C 0.1496(3) 0.4405(3) 0.04237(18) 0.0278(8) Uani 1 1 d . . . H24 H 0.1171 0.4717 0.0436 0.033 Uiso 1 1 calc R . . C25 C 0.2438(2) 0.4850(3) 0.03851(15) 0.0204(7) Uani 1 1 d . . . C26 C 0.2987(2) 0.5816(3) 0.03657(16) 0.0212(7) Uani 1 1 d . . . C27 C 0.2631(3) 0.6397(3) 0.04332(18) 0.0301(9) Uani 1 1 d . . . H27 H 0.2010 0.6184 0.0484 0.036 Uiso 1 1 calc R . . C28 C 0.3208(3) 0.7290(3) 0.0423(2) 0.0370(10) Uani 1 1 d . . . H28 H 0.2982 0.7688 0.0471 0.044 Uiso 1 1 calc R . . C29 C 0.4138(3) 0.7600(3) 0.03420(19) 0.0321(9) Uani 1 1 d . . . H29 H 0.4539 0.8203 0.0337 0.039 Uiso 1 1 calc R . . C30 C 0.4449(3) 0.6983(3) 0.02684(16) 0.0230(7) Uani 1 1 d . . . H30 H 0.5065 0.7183 0.0208 0.028 Uiso 1 1 calc R . . Cu4 Cu -0.17389(3) 0.42067(3) 0.32328(2) 0.02451(12) Uani 1 1 d . . . N7 N -0.3086(2) 0.3385(2) 0.30577(16) 0.0296(7) Uani 1 1 d . . . C31 C -0.3512(3) 0.2506(3) 0.3089(2) 0.0361(10) Uani 1 1 d . . . H31 H -0.3169 0.2223 0.3161 0.043 Uiso 1 1 calc R . . C32 C -0.4450(3) 0.2004(3) 0.3015(2) 0.0431(11) Uani 1 1 d . . . H32 H -0.4730 0.1392 0.3033 0.052 Uiso 1 1 calc R . . C33 C -0.4963(3) 0.2416(3) 0.2916(2) 0.0398(11) Uani 1 1 d . . . H33 H -0.5594 0.2088 0.2871 0.048 Uiso 1 1 calc R . . C34 C -0.4525(3) 0.3336(3) 0.28823(19) 0.0335(10) Uani 1 1 d . . . H34 H -0.4858 0.3631 0.2812 0.040 Uiso 1 1 calc R . . C35 C -0.3583(3) 0.3799(3) 0.29567(17) 0.0277(9) Uani 1 1 d . . . C36 C -0.3049(3) 0.4769(3) 0.29421(16) 0.0256(8) Uani 1 1 d . . . C37 C -0.3425(3) 0.5317(3) 0.28184(17) 0.0313(9) Uani 1 1 d . . . H37 H -0.4050 0.5076 0.2745 0.038 Uiso 1 1 calc R . . C38 C -0.2864(3) 0.6216(3) 0.28059(19) 0.0349(10) Uani 1 1 d . . . H38 H -0.3105 0.6589 0.2722 0.042 Uiso 1 1 calc R . . C39 C -0.1939(3) 0.6558(3) 0.29198(18) 0.0325(9) Uani 1 1 d . . . H39 H -0.1546 0.7162 0.2906 0.039 Uiso 1 1 calc R . . C40 C -0.1604(3) 0.5984(3) 0.30556(17) 0.0272(8) Uani 1 1 d . . . H40 H -0.0982 0.6216 0.3142 0.033 Uiso 1 1 calc R . . N8 N -0.2145(2) 0.5107(2) 0.30671(14) 0.0236(7) Uani 1 1 d . . . O5 O -0.14410(17) 0.33079(18) 0.34771(13) 0.0271(6) Uani 1 1 d . . . HW51 H -0.1908 0.2855 0.3606 0.033 Uiso 1 1 d R . . O6 O -0.05358(16) 0.50036(17) 0.36772(12) 0.0210(5) Uani 1 1 d . . . HW61 H -0.0285 0.5408 0.3455 0.025 Uiso 1 1 d R . . Cu5 Cu -0.01897(3) 0.40638(3) 0.37400(2) 0.02111(11) Uani 1 1 d . . . N9 N 0.11714(19) 0.4816(2) 0.37911(14) 0.0208(6) Uani 1 1 d . . . C41 C 0.1632(2) 0.5691(3) 0.38257(17) 0.0237(7) Uani 1 1 d . . . H41 H 0.1308 0.6003 0.3853 0.028 Uiso 1 1 calc R . . C42 C 0.2574(2) 0.6165(3) 0.38226(18) 0.0252(8) Uani 1 1 d . . . H42 H 0.2875 0.6781 0.3842 0.030 Uiso 1 1 calc R . . C43 C 0.3059(2) 0.5696(3) 0.37902(17) 0.0257(8) Uani 1 1 d . . . H43 H 0.3692 0.5994 0.3790 0.031 Uiso 1 1 calc R . . C44 C 0.2585(2) 0.4781(3) 0.37577(17) 0.0238(8) Uani 1 1 d . . . H44 H 0.2897 0.4455 0.3739 0.029 Uiso 1 1 calc R . . C45 C 0.1640(2) 0.4352(2) 0.37530(16) 0.0194(7) Uani 1 1 d . . . C46 C 0.1065(2) 0.3378(2) 0.36945(17) 0.0213(7) Uani 1 1 d . . . C47 C 0.1412(3) 0.2795(3) 0.36155(18) 0.0258(8) Uani 1 1 d . . . H47 H 0.2038 0.3003 0.3628 0.031 Uiso 1 1 calc R . . C48 C 0.0815(3) 0.1899(3) 0.35180(19) 0.0298(9) Uani 1 1 d . . . H48 H 0.1037 0.1500 0.3453 0.036 Uiso 1 1 calc R . . C49 C -0.0115(3) 0.1601(3) 0.3518(2) 0.0311(9) Uani 1 1 d . . . H49 H -0.0528 0.1002 0.3453 0.037 Uiso 1 1 calc R . . C50 C -0.0413(3) 0.2223(3) 0.3618(2) 0.0302(9) Uani 1 1 d . . . H50 H -0.1037 0.2027 0.3630 0.036 Uiso 1 1 calc R . . N10 N 0.0160(2) 0.3094(2) 0.36977(15) 0.0224(6) Uani 1 1 d . . . O7 O 0.04724(15) 0.58004(16) 0.51739(11) 0.0189(5) Uani 1 1 d . . . HW71 H 0.0884 0.6296 0.5056 0.023 Uiso 1 1 d R . . O8 O -0.1024(2) 0.4365(2) 0.23496(14) 0.0366(7) Uani 1 1 d . . . HW81 H -0.0766 0.4845 0.2195 0.044 Uiso 1 1 d R . . HW82 H -0.1224 0.3994 0.2026 0.044 Uiso 1 1 d R . . Cu6 Cu -0.07172(3) 0.51896(3) 0.47241(2) 0.01716(10) Uani 1 1 d . . . N11 N -0.20981(19) 0.45464(19) 0.46567(14) 0.0188(6) Uani 1 1 d . . . C51 C -0.2639(2) 0.3678(2) 0.46563(18) 0.0226(7) Uani 1 1 d . . . H51 H -0.2377 0.3313 0.4703 0.027 Uiso 1 1 calc R . . C52 C -0.3588(2) 0.3289(2) 0.45883(18) 0.0246(8) Uani 1 1 d . . . H52 H -0.3952 0.2678 0.4589 0.030 Uiso 1 1 calc R . . C53 C -0.3972(2) 0.3836(3) 0.45203(17) 0.0228(7) Uani 1 1 d . . . H53 H -0.4600 0.3596 0.4465 0.027 Uiso 1 1 calc R . . C54 C -0.3413(2) 0.4745(2) 0.45357(16) 0.0194(7) Uani 1 1 d . . . H54 H -0.3661 0.5123 0.4499 0.023 Uiso 1 1 calc R . . C55 C -0.2472(2) 0.5083(2) 0.46067(15) 0.0168(7) Uani 1 1 d . . . C56 C -0.1816(2) 0.6031(2) 0.46248(16) 0.0174(7) Uani 1 1 d . . . C57 C -0.2066(2) 0.6690(2) 0.45951(19) 0.0252(8) Uani 1 1 d . . . H57 H -0.2678 0.6544 0.4572 0.030 Uiso 1 1 calc R . . N6 N 0.3885(2) 0.6109(2) 0.02814(12) 0.0177(6) Uani 1 1 d . . . C58 C -0.1396(3) 0.7561(3) 0.4600(2) 0.0308(9) Uani 1 1 d . . . H58 H -0.1553 0.8009 0.4577 0.037 Uiso 1 1 calc R . . C59 C -0.0488(3) 0.7767(2) 0.46391(19) 0.0261(8) Uani 1 1 d . . . H59 H -0.0027 0.8352 0.4645 0.031 Uiso 1 1 calc R . . C60 C -0.0285(2) 0.7080(2) 0.46698(18) 0.0222(7) Uani 1 1 d . . . H60 H 0.0324 0.7214 0.4692 0.027 Uiso 1 1 calc R . . N12 N -0.09281(19) 0.62309(19) 0.46693(14) 0.0182(6) Uani 1 1 d . . . O9 O 0.05732(18) 0.65339(19) 0.30014(14) 0.0312(6) Uani 1 1 d . . . O10 O 0.0036(2) 0.6030(2) 0.20163(16) 0.0441(8) Uani 1 1 d . . . C61 C 0.0502(3) 0.6640(3) 0.2423(2) 0.0308(9) Uani 1 1 d . . . C62 C 0.1004(3) 0.7592(3) 0.2205(2) 0.0331(9) Uani 1 1 d . . . H62A H 0.1566 0.7930 0.2456 0.040 Uiso 1 1 calc R . . H62B H 0.1159 0.7577 0.1765 0.040 Uiso 1 1 calc R . . C63 C 0.0417(3) 0.8042(3) 0.2272(2) 0.0310(9) Uani 1 1 d . . . C64 C 0.0324(3) 0.8382(3) 0.2852(2) 0.0373(10) Uani 1 1 d . . . H64A H 0.0627 0.8340 0.3209 0.045 Uiso 1 1 calc R . . C65 C -0.0221(3) 0.8789(3) 0.2908(3) 0.0430(11) Uani 1 1 d . . . H65A H -0.0280 0.9013 0.3304 0.052 Uiso 1 1 calc R . . C66 C -0.0668(3) 0.8866(3) 0.2393(3) 0.0457(12) Uani 1 1 d . . . H66A H -0.1028 0.9140 0.2435 0.055 Uiso 1 1 calc R . . C67 C -0.0581(3) 0.8526(3) 0.1798(3) 0.0455(12) Uani 1 1 d . . . H67A H -0.0881 0.8576 0.1443 0.055 Uiso 1 1 calc R . . C68 C -0.0039(3) 0.8110(3) 0.1741(2) 0.0362(10) Uani 1 1 d . . . H68A H 0.0016 0.7879 0.1348 0.043 Uiso 1 1 calc R . . O11 O 0.5458(2) 0.59936(18) 0.43509(12) 0.0303(6) Uani 1 1 d . . . O12 O 0.53227(17) 0.65801(17) 0.34636(11) 0.0247(5) Uani 1 1 d . . . C69 C 0.5650(2) 0.6645(2) 0.40103(16) 0.0201(7) Uani 1 1 d . . . C70 C 0.6319(3) 0.7564(3) 0.42988(19) 0.0272(8) Uani 1 1 d . . . H70A H 0.6753 0.7511 0.4578 0.033 Uiso 1 1 calc R . . H70B H 0.6656 0.7931 0.3961 0.033 Uiso 1 1 calc R . . C71 C 0.5885(3) 0.8025(3) 0.46678(17) 0.0472(12) Uiso 1 1 d G . . C72 C 0.5297(3) 0.8281(3) 0.43921(15) 0.0728(18) Uiso 1 1 d G . . H72A H 0.5117 0.8129 0.3967 0.087 Uiso 1 1 calc R . . C73 C 0.4977(3) 0.8764(3) 0.4752(2) 0.084(2) Uiso 1 1 d G . . H73A H 0.4583 0.8936 0.4568 0.101 Uiso 1 1 calc R . . C74 C 0.5246(4) 0.8991(3) 0.5388(2) 0.086(2) Uiso 1 1 d G . . H74A H 0.5032 0.9314 0.5630 0.103 Uiso 1 1 calc R . . C75 C 0.5835(4) 0.8735(3) 0.56641(15) 0.112(3) Uiso 1 1 d G . . H75A H 0.6015 0.8887 0.6090 0.134 Uiso 1 1 calc R . . C76 C 0.6154(3) 0.8252(3) 0.53038(18) 0.0745(18) Uiso 1 1 d G . . H76A H 0.6548 0.8081 0.5488 0.089 Uiso 1 1 calc R . . O13 O 0.61634(16) 0.72307(16) 0.14127(11) 0.0215(5) Uani 1 1 d . . . O14 O 0.65913(17) 0.74097(17) 0.04109(12) 0.0241(5) Uani 1 1 d . . . C77 C 0.6629(2) 0.7698(2) 0.09743(16) 0.0177(7) Uani 1 1 d . . . C78 C 0.7246(2) 0.8688(2) 0.11265(17) 0.0204(7) Uani 1 1 d . . . H78A H 0.7459 0.8794 0.1567 0.025 Uiso 1 1 calc R . . H78B H 0.7772 0.8904 0.0863 0.025 Uiso 1 1 calc R . . C79 C 0.6715(2) 0.9167(2) 0.10040(16) 0.0199(7) Uani 1 1 d . . . C80 C 0.6629(3) 0.9407(3) 0.03919(18) 0.0274(8) Uani 1 1 d . . . H80A H 0.6931 0.9298 0.0062 0.033 Uiso 1 1 calc R . . C81 C 0.6093(3) 0.9806(3) 0.02767(19) 0.0336(9) Uani 1 1 d . . . H81A H 0.6039 0.9960 -0.0130 0.040 Uiso 1 1 calc R . . C82 C 0.5639(3) 0.9976(3) 0.0764(2) 0.0326(9) Uani 1 1 d . . . H82A H 0.5276 1.0236 0.0685 0.039 Uiso 1 1 calc R . . C83 C 0.5733(3) 0.9753(3) 0.1374(2) 0.0315(9) Uani 1 1 d . . . H83A H 0.5438 0.9874 0.1704 0.038 Uiso 1 1 calc R . . C84 C 0.6269(3) 0.9349(3) 0.14929(18) 0.0253(8) Uani 1 1 d . . . H84A H 0.6327 0.9202 0.1902 0.030 Uiso 1 1 calc R . . O15 O 0.9076(3) 0.3357(3) 0.0619(2) 0.0724(12) Uani 1 1 d . . . O16 O 0.8302(2) 0.3019(2) 0.14663(15) 0.0451(8) Uani 1 1 d . . . C85 C 0.8497(3) 0.2787(4) 0.0979(2) 0.0449(12) Uani 1 1 d . . . C86 C 0.8035(3) 0.1806(4) 0.0767(3) 0.0604(17) Uani 1 1 d . . . H86A H 0.7526 0.1487 0.1035 0.072 Uiso 1 1 calc R . . H86B H 0.7792 0.1731 0.0336 0.072 Uiso 1 1 calc R . . C87 C 0.8662(3) 0.1401(3) 0.0791(3) 0.0433(12) Uani 1 1 d . . . C88 C 0.8811(3) 0.1083(3) 0.1347(3) 0.0550(15) Uani 1 1 d . . . H88A H 0.8516 0.1114 0.1710 0.066 Uiso 1 1 calc R . . C89 C 0.9393(4) 0.0717(3) 0.1369(3) 0.0546(14) Uani 1 1 d . . . H89A H 0.9496 0.0517 0.1745 0.066 Uiso 1 1 calc R . . C90 C 0.9813(3) 0.0654(3) 0.0831(3) 0.0535(14) Uani 1 1 d . . . H90A H 1.0210 0.0419 0.0843 0.064 Uiso 1 1 calc R . . C91 C 0.9647(3) 0.0939(3) 0.0280(3) 0.0476(13) Uani 1 1 d . . . H91A H 0.9916 0.0875 -0.0088 0.057 Uiso 1 1 calc R . . C92 C 0.9087(3) 0.1320(3) 0.0258(3) 0.0442(11) Uani 1 1 d . . . H92A H 0.8995 0.1524 -0.0120 0.053 Uiso 1 1 calc R . . O17 O 0.75674(19) 0.18808(18) 0.41596(14) 0.0302(6) Uani 1 1 d . . . O18 O 0.82046(17) 0.24466(17) 0.51174(13) 0.0253(6) Uani 1 1 d . . . C93 C 0.7686(2) 0.1808(2) 0.4737(2) 0.0255(8) Uani 1 1 d . . . C94 C 0.7168(3) 0.0884(2) 0.4993(2) 0.0291(9) Uani 1 1 d . . . H94A H 0.6885 0.0923 0.5382 0.035 Uiso 1 1 calc R . . H94B H 0.6688 0.0495 0.4688 0.035 Uiso 1 1 calc R . . C95 C 0.7784(3) 0.0488(2) 0.5120(2) 0.0272(8) Uani 1 1 d . . . C96 C 0.7991(3) 0.0371(3) 0.5730(2) 0.0325(9) Uani 1 1 d . . . H96A H 0.7779 0.0571 0.6071 0.039 Uiso 1 1 calc R . . C97 C 0.8513(3) -0.0045(3) 0.5839(2) 0.0363(10) Uani 1 1 d . . . H97A H 0.8632 -0.0134 0.6252 0.044 Uiso 1 1 calc R . . C98 C 0.8856(3) -0.0326(3) 0.5339(2) 0.0352(10) Uani 1 1 d . . . H98A H 0.9214 -0.0594 0.5413 0.042 Uiso 1 1 calc R . . C99 C 0.8655(3) -0.0200(3) 0.4722(2) 0.0322(9) Uani 1 1 d . . . H99A H 0.8882 -0.0385 0.4381 0.039 Uiso 1 1 calc R . . C100 C 0.8123(3) 0.0196(3) 0.4616(2) 0.0289(8) Uani 1 1 d . . . H10A H 0.7989 0.0269 0.4203 0.035 Uiso 1 1 calc R . . O19 O 0.2664(2) 0.1796(2) 0.28549(14) 0.0405(7) Uani 1 1 d . . . O20 O 0.2650(2) 0.20658(18) 0.18348(13) 0.0318(6) Uani 1 1 d . . . C101 C 0.2414(3) 0.1556(2) 0.22899(18) 0.0253(8) Uani 1 1 d . . . C102 C 0.1784(3) 0.0575(3) 0.2127(2) 0.0285(8) Uani 1 1 d . . . H10B H 0.1434 0.0304 0.2492 0.034 Uiso 1 1 calc R . . H10C H 0.1361 0.0504 0.1784 0.034 Uiso 1 1 calc R . . C103 C 0.2326(2) 0.0120(2) 0.19345(18) 0.0239(8) Uani 1 1 d . . . C104 C 0.2231(3) -0.0254(3) 0.13195(19) 0.0289(8) Uani 1 1 d . . . H10D H 0.1838 -0.0212 0.1026 0.035 Uiso 1 1 calc R . . C105 C 0.2721(3) -0.0691(3) 0.1141(2) 0.0399(11) Uani 1 1 d . . . H10E H 0.2641 -0.0950 0.0733 0.048 Uiso 1 1 calc R . . C106 C 0.3316(3) -0.0739(3) 0.1564(3) 0.0427(11) Uani 1 1 d . . . H10F H 0.3644 -0.1026 0.1440 0.051 Uiso 1 1 calc R . . C107 C 0.3436(3) -0.0363(3) 0.2176(2) 0.0410(11) Uani 1 1 d . . . H10G H 0.3851 -0.0388 0.2460 0.049 Uiso 1 1 calc R . . C108 C 0.2932(3) 0.0053(3) 0.2363(2) 0.0320(9) Uani 1 1 d . . . H10H H 0.2999 0.0289 0.2777 0.038 Uiso 1 1 calc R . . O21 O 0.7825(2) 0.21702(19) 0.63919(15) 0.0359(7) Uani 1 1 d . . . H211 H 0.8294 0.2575 0.6610 0.043 Uiso 1 1 d R . . H212 H 0.7790 0.2154 0.5976 0.043 Uiso 1 1 d R . . O22 O 0.36182(19) 0.34990(18) 0.32219(12) 0.0284(6) Uani 1 1 d . . . H221 H 0.3326 0.2961 0.3040 0.034 Uiso 1 1 d R . . H222 H 0.3801 0.3666 0.3621 0.034 Uiso 1 1 d R . . O23 O 0.58292(19) 0.58100(19) 0.55794(12) 0.0294(6) Uani 1 1 d . . . H231 H 0.5711 0.5939 0.5204 0.035 Uiso 1 1 d R . . H232 H 0.5420 0.5266 0.5624 0.035 Uiso 1 1 d R . . O24 O 0.7909(2) 0.9553(2) 0.30103(16) 0.0465(8) Uani 1 1 d . . . H241 H 0.7482 0.9008 0.2908 0.056 Uiso 1 1 d R . . H242 H 0.7704 0.9930 0.3016 0.056 Uiso 1 1 d R . . O25 O 0.2118(2) 0.1422(2) 0.05142(14) 0.0377(7) Uani 1 1 d . . . H251 H 0.2490 0.1750 0.0234 0.045 Uiso 1 1 d R . . H252 H 0.2202 0.1630 0.0912 0.045 Uiso 1 1 d R . . O26 O 0.7061(2) 0.0656(2) 0.31508(18) 0.0526(9) Uani 1 1 d . . . H261 H 0.7285 0.1014 0.2841 0.063 Uiso 1 1 d R . . H262 H 0.7193 0.0993 0.3498 0.063 Uiso 1 1 d R . . O27 O 0.8103(3) 0.2066(2) 0.24866(19) 0.0579(10) Uani 1 1 d . . . H271 H 0.8090 0.2223 0.2101 0.070 Uiso 1 1 d R . . H272 H 0.8270 0.2538 0.2745 0.070 Uiso 1 1 d R . . O28 O 0.6290(3) 0.7923(2) 0.26689(14) 0.0568(11) Uani 1 1 d U . . H281 H 0.6481 0.7650 0.2398 0.068 Uiso 1 1 d R . . H282 H 0.5971 0.7477 0.2901 0.068 Uiso 1 1 d R . . O29 O 0.0080(4) 0.5170(4) 0.0860(3) 0.105(2) Uani 1 1 d . . . H291 H -0.0309 0.4637 0.0707 0.126 Uiso 1 1 d R . . H292 H -0.0236 0.5292 0.1140 0.126 Uiso 1 1 d R . . O30 O 0.6010(4) 0.0756(4) 0.6407(3) 0.112(2) Uani 1 1 d . . . H301 H 0.6571 0.1194 0.6398 0.134 Uiso 1 1 d R . . H302 H 0.5567 0.0781 0.6613 0.134 Uiso 1 1 d R . . O31 O 0.9090(4) 0.3001(3) 0.9350(2) 0.0839(14) Uani 1 1 d . . . H311 H 0.9087 0.3107 0.9741 0.101 Uiso 1 1 d R . . H312 H 0.9348 0.3562 0.9284 0.101 Uiso 1 1 d R . . O32 O 0.5348(3) 0.9234(5) 0.2950(2) 0.137(3) Uani 1 1 d U . . H321 H 0.5863 0.9714 0.3019 0.165 Uiso 1 1 d R . . H322 H 0.5609 0.8901 0.2876 0.165 Uiso 1 1 d 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 0.01328(19) 0.0148(2) 0.01771(19) 0.00046(15) 0.00168(16) 0.00873(16) N1 0.0154(13) 0.0229(16) 0.0220(13) -0.0001(11) 0.0017(12) 0.0111(12) C1 0.0193(17) 0.024(2) 0.0320(19) -0.0004(15) 0.0046(16) 0.0083(15) C2 0.0229(19) 0.030(2) 0.0314(19) -0.0014(16) 0.0038(17) 0.0057(16) C3 0.0152(17) 0.054(3) 0.035(2) -0.0010(19) 0.0011(17) 0.0149(18) C4 0.0206(18) 0.042(3) 0.0293(18) 0.0023(17) 0.0022(16) 0.0198(18) C5 0.0193(17) 0.030(2) 0.0184(15) 0.0020(14) 0.0018(14) 0.0163(15) C6 0.0218(17) 0.031(2) 0.0202(15) 0.0045(14) 0.0033(14) 0.0197(16) C7 0.037(2) 0.037(2) 0.043(2) 0.0143(19) 0.020(2) 0.029(2) C8 0.061(3) 0.035(3) 0.072(3) 0.019(2) 0.039(3) 0.039(3) C9 0.050(3) 0.017(2) 0.077(3) 0.011(2) 0.034(3) 0.017(2) C10 0.0279(19) 0.022(2) 0.038(2) 0.0041(16) 0.0115(17) 0.0151(16) N2 0.0226(15) 0.0209(16) 0.0208(13) 0.0023(11) 0.0047(12) 0.0156(13) O1 0.0213(12) 0.0115(12) 0.0265(12) 0.0027(9) 0.0064(10) 0.0091(10) O2 0.0153(11) 0.0141(12) 0.0181(10) 0.0015(9) 0.0029(9) 0.0087(9) Cu2 0.01450(19) 0.0136(2) 0.01810(19) 0.00158(15) 0.00053(16) 0.00936(16) N3 0.0189(14) 0.0202(16) 0.0168(12) -0.0005(11) -0.0010(11) 0.0133(12) C11 0.0187(16) 0.0193(18) 0.0251(16) -0.0009(13) -0.0032(14) 0.0107(14) C12 0.0174(17) 0.027(2) 0.0294(18) -0.0001(15) -0.0027(15) 0.0071(15) C13 0.0168(17) 0.042(3) 0.0300(19) -0.0009(17) -0.0044(16) 0.0153(17) C14 0.0206(17) 0.036(2) 0.0275(17) 0.0042(16) -0.0020(15) 0.0191(17) C15 0.0207(17) 0.027(2) 0.0164(14) 0.0000(13) -0.0005(14) 0.0160(15) C16 0.0257(18) 0.025(2) 0.0212(15) 0.0005(14) 0.0008(15) 0.0190(16) C17 0.035(2) 0.030(2) 0.0349(19) 0.0021(16) 0.0002(18) 0.0252(18) C18 0.053(3) 0.029(2) 0.042(2) 0.0070(18) 0.004(2) 0.033(2) C19 0.045(2) 0.019(2) 0.038(2) 0.0019(16) 0.006(2) 0.0176(19) C20 0.0270(18) 0.0186(19) 0.0289(17) 0.0027(14) 0.0029(16) 0.0125(15) N4 0.0250(15) 0.0176(15) 0.0210(13) 0.0032(11) 0.0033(12) 0.0143(13) O3 0.0136(10) 0.0138(12) 0.0167(10) -0.0018(8) -0.0003(9) 0.0068(9) O4 0.0242(13) 0.0213(14) 0.0212(11) 0.0002(10) -0.0055(10) 0.0084(11) Cu3 0.01282(19) 0.0138(2) 0.01640(18) 0.00028(14) 0.00049(16) 0.00872(16) N5 0.0170(14) 0.0243(16) 0.0173(12) -0.0012(11) -0.0008(12) 0.0131(12) C21 0.0188(17) 0.024(2) 0.0239(16) 0.0002(14) 0.0024(15) 0.0091(15) C22 0.0205(18) 0.027(2) 0.0313(19) 0.0002(16) 0.0027(16) 0.0058(16) C23 0.0141(17) 0.045(3) 0.0316(19) 0.0003(17) 0.0024(16) 0.0096(17) C24 0.0194(17) 0.038(2) 0.0299(18) -0.0004(16) 0.0001(16) 0.0173(17) C25 0.0182(16) 0.030(2) 0.0171(15) -0.0013(13) -0.0006(14) 0.0155(15) C26 0.0216(17) 0.029(2) 0.0193(15) -0.0038(14) -0.0045(14) 0.0182(16) C27 0.030(2) 0.040(3) 0.0330(19) -0.0071(17) -0.0052(17) 0.0282(19) C28 0.044(2) 0.039(3) 0.045(2) -0.0118(19) -0.010(2) 0.036(2) C29 0.041(2) 0.022(2) 0.040(2) -0.0068(16) -0.0076(19) 0.0209(19) C30 0.0280(19) 0.022(2) 0.0224(16) -0.0015(14) -0.0019(15) 0.0155(16) Cu4 0.0166(2) 0.0255(3) 0.0358(2) -0.00932(19) -0.00960(19) 0.01486(19) N7 0.0208(15) 0.035(2) 0.0371(17) -0.0122(15) -0.0103(14) 0.0180(15) C31 0.0215(19) 0.035(3) 0.051(2) -0.016(2) -0.0127(19) 0.0155(18) C32 0.027(2) 0.037(3) 0.057(3) -0.017(2) -0.014(2) 0.011(2) C33 0.0170(18) 0.054(3) 0.044(2) -0.015(2) -0.0090(18) 0.0147(19) C34 0.0196(18) 0.054(3) 0.032(2) -0.0098(19) -0.0054(17) 0.0235(19) C35 0.0202(18) 0.048(3) 0.0215(17) -0.0092(16) -0.0080(15) 0.0227(18) C36 0.0237(18) 0.044(2) 0.0194(16) -0.0047(15) -0.0034(15) 0.0251(18) C37 0.028(2) 0.053(3) 0.0256(18) 0.0040(17) 0.0006(17) 0.030(2) C38 0.039(2) 0.052(3) 0.033(2) 0.0126(19) 0.0062(19) 0.036(2) C39 0.040(2) 0.041(3) 0.0324(19) 0.0099(18) 0.0099(19) 0.031(2) C40 0.0284(19) 0.038(2) 0.0255(17) 0.0012(16) 0.0020(16) 0.0244(18) N8 0.0228(15) 0.0338(19) 0.0225(14) -0.0033(13) -0.0032(13) 0.0208(14) O5 0.0156(12) 0.0218(14) 0.0452(15) -0.0101(12) -0.0112(11) 0.0113(11) O6 0.0146(11) 0.0211(14) 0.0305(12) -0.0028(10) -0.0050(10) 0.0117(10) Cu5 0.0128(2) 0.0165(2) 0.0367(2) -0.00541(18) -0.00470(18) 0.00997(17) N9 0.0149(13) 0.0247(17) 0.0274(14) 0.0005(12) -0.0022(12) 0.0134(13) C41 0.0200(17) 0.021(2) 0.0327(18) 0.0006(15) -0.0029(15) 0.0125(15) C42 0.0181(17) 0.022(2) 0.0340(19) 0.0018(15) 0.0002(16) 0.0088(15) C43 0.0127(16) 0.030(2) 0.0301(18) 0.0015(15) -0.0002(15) 0.0068(15) C44 0.0207(17) 0.030(2) 0.0284(17) 0.0008(15) 0.0013(15) 0.0185(16) C45 0.0179(16) 0.0219(19) 0.0226(16) 0.0009(13) -0.0002(14) 0.0128(14) C46 0.0194(17) 0.0230(19) 0.0271(17) 0.0014(14) 0.0016(15) 0.0145(15) C47 0.0235(18) 0.028(2) 0.0342(19) 0.0079(16) 0.0058(16) 0.0186(16) C48 0.034(2) 0.028(2) 0.040(2) 0.0072(17) 0.0102(18) 0.0238(18) C49 0.031(2) 0.020(2) 0.044(2) 0.0004(17) 0.0070(19) 0.0138(17) C50 0.0223(18) 0.026(2) 0.046(2) -0.0016(17) 0.0024(18) 0.0155(16) N10 0.0171(14) 0.0200(16) 0.0333(16) -0.0048(12) -0.0021(13) 0.0122(12) O7 0.0105(10) 0.0121(12) 0.0346(13) 0.0017(10) -0.0031(10) 0.0058(9) O8 0.0326(15) 0.0353(18) 0.0446(16) -0.0136(13) -0.0012(14) 0.0199(14) Cu6 0.01011(19) 0.0105(2) 0.0327(2) -0.00020(16) -0.00285(17) 0.00656(16) N11 0.0148(13) 0.0145(15) 0.0287(14) -0.0004(11) -0.0017(12) 0.0084(11) C51 0.0157(16) 0.0141(18) 0.0384(19) 0.0011(14) -0.0035(15) 0.0076(14) C52 0.0161(16) 0.0147(18) 0.040(2) -0.0011(15) -0.0037(16) 0.0053(14) C53 0.0121(15) 0.026(2) 0.0297(18) -0.0005(15) -0.0016(14) 0.0089(14) C54 0.0170(16) 0.0225(19) 0.0238(16) 0.0012(13) 0.0031(14) 0.0136(14) C55 0.0148(15) 0.0171(17) 0.0206(15) 0.0009(12) -0.0006(13) 0.0095(13) C56 0.0143(15) 0.0173(18) 0.0228(15) -0.0001(13) 0.0006(13) 0.0094(13) C57 0.0191(17) 0.0194(19) 0.043(2) 0.0003(16) 0.0024(16) 0.0138(15) N6 0.0203(14) 0.0229(16) 0.0151(12) -0.0003(11) -0.0008(11) 0.0148(12) C58 0.0281(19) 0.0166(19) 0.055(2) 0.0012(17) 0.0024(19) 0.0165(16) C59 0.0210(17) 0.0132(18) 0.044(2) 0.0020(15) -0.0012(17) 0.0083(14) C60 0.0141(15) 0.0155(18) 0.0378(19) 0.0019(14) 0.0010(15) 0.0076(14) N12 0.0142(13) 0.0136(15) 0.0287(14) 0.0006(11) -0.0003(12) 0.0083(11) O9 0.0245(13) 0.0264(16) 0.0431(16) 0.0001(12) -0.0073(13) 0.0128(12) O10 0.0408(18) 0.044(2) 0.0513(18) -0.0153(15) -0.0142(15) 0.0257(16) C61 0.0208(18) 0.032(2) 0.048(2) -0.0045(18) -0.0019(18) 0.0204(17) C62 0.0235(19) 0.040(3) 0.041(2) 0.0046(18) 0.0028(18) 0.0184(18) C63 0.0192(18) 0.030(2) 0.046(2) 0.0115(18) 0.0019(17) 0.0131(16) C64 0.031(2) 0.036(3) 0.052(3) 0.007(2) 0.006(2) 0.021(2) C65 0.033(2) 0.031(2) 0.068(3) 0.004(2) 0.012(2) 0.018(2) C66 0.025(2) 0.022(2) 0.092(4) 0.011(2) 0.006(2) 0.0124(18) C67 0.024(2) 0.032(3) 0.076(3) 0.016(2) -0.009(2) 0.0094(19) C68 0.026(2) 0.030(2) 0.050(2) 0.0095(19) -0.0043(19) 0.0107(18) O11 0.0397(16) 0.0233(15) 0.0283(13) 0.0068(11) -0.0013(12) 0.0151(13) O12 0.0237(13) 0.0232(14) 0.0253(12) 0.0061(10) -0.0030(11) 0.0094(11) C69 0.0174(16) 0.0191(18) 0.0268(17) 0.0034(14) 0.0025(14) 0.0111(14) C70 0.0252(18) 0.023(2) 0.0350(19) -0.0041(15) -0.0030(16) 0.0136(16) O13 0.0191(12) 0.0167(13) 0.0272(12) -0.0003(10) 0.0010(10) 0.0075(10) O14 0.0224(12) 0.0201(14) 0.0274(12) -0.0021(10) 0.0020(11) 0.0086(11) C77 0.0147(15) 0.0158(17) 0.0246(16) 0.0008(13) -0.0016(14) 0.0091(13) C78 0.0192(16) 0.0163(18) 0.0249(16) -0.0001(13) 0.0001(14) 0.0080(14) C79 0.0189(16) 0.0116(17) 0.0261(16) -0.0015(13) -0.0012(14) 0.0051(13) C80 0.032(2) 0.022(2) 0.0285(18) 0.0013(15) 0.0003(17) 0.0128(17) C81 0.043(2) 0.025(2) 0.0320(19) 0.0020(16) -0.0097(18) 0.0161(19) C82 0.032(2) 0.021(2) 0.051(2) -0.0034(18) -0.0084(19) 0.0183(18) C83 0.033(2) 0.023(2) 0.042(2) -0.0066(17) -0.0008(18) 0.0178(18) C84 0.0293(19) 0.021(2) 0.0282(18) -0.0020(14) -0.0011(16) 0.0145(16) O15 0.055(2) 0.082(3) 0.078(3) -0.008(2) 0.013(2) 0.033(2) O16 0.0419(18) 0.051(2) 0.0498(18) -0.0210(16) -0.0124(15) 0.0308(17) C85 0.030(2) 0.057(3) 0.052(3) -0.005(2) -0.004(2) 0.025(2) C86 0.029(2) 0.060(4) 0.090(4) -0.042(3) -0.022(3) 0.025(2) C87 0.0170(18) 0.028(2) 0.075(3) -0.024(2) -0.011(2) 0.0051(17) C88 0.039(3) 0.032(3) 0.070(3) -0.025(2) 0.008(3) 0.001(2) C89 0.050(3) 0.023(3) 0.074(4) -0.012(2) -0.013(3) 0.006(2) C90 0.036(2) 0.023(3) 0.100(4) -0.012(3) -0.009(3) 0.015(2) C91 0.027(2) 0.034(3) 0.075(3) -0.014(2) 0.004(2) 0.011(2) C92 0.032(2) 0.033(3) 0.062(3) -0.015(2) -0.008(2) 0.013(2) O17 0.0276(14) 0.0188(14) 0.0435(16) -0.0030(12) -0.0036(13) 0.0110(12) O18 0.0176(12) 0.0147(13) 0.0418(14) 0.0029(11) -0.0042(11) 0.0064(10) C93 0.0117(15) 0.0130(18) 0.053(2) 0.0000(16) -0.0007(16) 0.0073(14) C94 0.0191(17) 0.0144(19) 0.051(2) 0.0008(16) 0.0060(17) 0.0060(15) C95 0.0217(17) 0.0096(17) 0.047(2) 0.0039(15) 0.0078(17) 0.0046(14) C96 0.039(2) 0.018(2) 0.043(2) 0.0043(16) 0.015(2) 0.0156(18) C97 0.049(3) 0.025(2) 0.038(2) 0.0042(17) 0.005(2) 0.020(2) C98 0.040(2) 0.021(2) 0.053(2) 0.0044(18) 0.006(2) 0.0210(19) C99 0.039(2) 0.023(2) 0.041(2) 0.0029(17) 0.0106(19) 0.0195(18) C100 0.030(2) 0.0163(19) 0.040(2) 0.0030(16) 0.0042(18) 0.0112(16) O19 0.0518(19) 0.0250(17) 0.0392(16) -0.0032(13) -0.0026(15) 0.0145(15) O20 0.0375(16) 0.0182(14) 0.0376(15) 0.0045(11) 0.0116(13) 0.0112(12) C101 0.0240(18) 0.0163(19) 0.037(2) 0.0009(15) 0.0068(17) 0.0104(15) C102 0.0252(18) 0.020(2) 0.040(2) 0.0024(16) 0.0071(17) 0.0101(16) C103 0.0213(17) 0.0118(17) 0.0340(18) 0.0049(14) 0.0035(16) 0.0040(14) C104 0.031(2) 0.022(2) 0.0333(19) 0.0017(16) -0.0037(17) 0.0126(16) C105 0.040(2) 0.029(2) 0.047(2) -0.0065(19) 0.007(2) 0.014(2) C106 0.032(2) 0.022(2) 0.077(3) 0.002(2) 0.006(2) 0.0156(19) C107 0.033(2) 0.025(2) 0.062(3) 0.010(2) -0.011(2) 0.0108(19) C108 0.030(2) 0.019(2) 0.040(2) 0.0053(16) -0.0036(18) 0.0069(16) O21 0.0305(15) 0.0263(16) 0.0457(16) -0.0023(13) -0.0024(13) 0.0100(13) O22 0.0358(15) 0.0244(15) 0.0243(12) -0.0010(10) -0.0050(12) 0.0141(12) O23 0.0347(15) 0.0277(16) 0.0255(12) -0.0019(11) -0.0052(12) 0.0151(13) O24 0.0354(17) 0.038(2) 0.061(2) -0.0177(16) -0.0053(16) 0.0153(15) O25 0.0404(17) 0.0312(17) 0.0349(15) 0.0040(12) 0.0065(14) 0.0117(14) O26 0.049(2) 0.034(2) 0.070(2) -0.0210(17) -0.0102(18) 0.0194(17) O27 0.056(2) 0.040(2) 0.069(2) -0.0209(18) 0.0006(19) 0.0183(18) O28 0.087(3) 0.0236(17) 0.0265(14) 0.0027(12) -0.0005(16) -0.0002(17) O29 0.115(4) 0.102(4) 0.133(5) 0.019(4) 0.059(4) 0.078(4) O30 0.089(4) 0.123(5) 0.118(4) -0.011(4) 0.009(4) 0.048(4) O31 0.112(4) 0.079(3) 0.062(3) 0.007(2) 0.010(3) 0.046(3) O32 0.055(3) 0.211(6) 0.054(3) 0.023(3) -0.006(2) -0.012(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 Cu1 O1 1.908(2) . ? Cu1 O2 1.988(2) . ? Cu1 N2 1.997(3) . ? Cu1 N1 2.016(3) . ? Cu1 O4 2.208(3) . ? Cu1 Cu2 2.9413(9) . ? N1 C1 1.341(5) . ? N1 C5 1.357(4) . ? C1 C2 1.391(5) . ? C1 H1 0.9300 . ? C2 C3 1.370(6) . ? C2 H2 0.9300 . ? C3 C4 1.380(6) . ? C3 H3 0.9300 . ? C4 C5 1.394(5) . ? C4 H4 0.9300 . ? C5 C6 1.468(5) . ? C6 N2 1.358(4) . ? C6 C7 1.388(5) . ? C7 C8 1.363(7) . ? C7 H7 0.9300 . ? C8 C9 1.389(6) . ? C8 H8 0.9300 . ? C9 C10 1.389(5) . ? C9 H9 0.9300 . ? C10 N2 1.334(5) . ? C10 H10 0.9300 . ? O1 Cu2 1.903(2) . ? O1 HW11 0.8439 . ? O2 Cu2 1.969(2) . ? O2 Cu3 2.252(2) . ? O2 HW21 0.8211 . ? Cu2 N4 1.995(3) . ? Cu2 N3 2.007(3) . ? Cu2 O3 2.325(2) 2_665 ? N3 C11 1.338(5) . ? N3 C15 1.349(4) . ? C11 C12 1.380(5) . ? C11 H11 0.9300 . ? C12 C13 1.382(6) . ? C12 H12 0.9300 . ? C13 C14 1.381(6) . ? C13 H13 0.9300 . ? C14 C15 1.396(5) . ? C14 H14 0.9300 . ? C15 C16 1.466(5) . ? C16 N4 1.353(5) . ? C16 C17 1.389(5) . ? C17 C18 1.380(6) . ? C17 H17 0.9300 . ? C18 C19 1.376(6) . ? C18 H18 0.9300 . ? C19 C20 1.387(5) . ? C19 H19 0.9300 . ? C20 N4 1.347(5) . ? C20 H20 0.9300 . ? O3 Cu3 1.944(2) . ? O3 Cu3 1.962(2) 2_665 ? O3 Cu2 2.325(2) 2_665 ? O3 HW31 0.8041 . ? O4 HW41 0.8412 . ? O4 HW42 0.8599 . ? Cu3 O3 1.962(2) 2_665 ? Cu3 N5 1.997(3) . ? Cu3 N6 2.018(3) . ? Cu3 Cu3 2.9646(10) 2_665 ? N5 C21 1.330(5) . ? N5 C25 1.353(4) . ? C21 C22 1.387(5) . ? C21 H21 0.9300 . ? C22 C23 1.393(6) . ? C22 H22 0.9300 . ? C23 C24 1.374(6) . ? C23 H23 0.9300 . ? C24 C25 1.389(5) . ? C24 H24 0.9300 . ? C25 C26 1.470(5) . ? C26 N6 1.353(4) . ? C26 C27 1.393(5) . ? C27 C28 1.371(6) . ? C27 H27 0.9300 . ? C28 C29 1.397(6) . ? C28 H28 0.9300 . ? C29 C30 1.391(5) . ? C29 H29 0.9300 . ? C30 N6 1.343(5) . ? C30 H30 0.9300 . ? Cu4 O5 1.930(3) . ? Cu4 O6 2.001(3) . ? Cu4 N8 2.012(3) . ? Cu4 N7 2.024(3) . ? Cu4 O8 2.187(3) . ? Cu4 Cu5 2.9155(9) . ? N7 C31 1.336(6) . ? N7 C35 1.350(5) . ? C31 C32 1.384(6) . ? C31 H31 0.9300 . ? C32 C33 1.370(7) . ? C32 H32 0.9300 . ? C33 C34 1.399(7) . ? C33 H33 0.9300 . ? C34 C35 1.387(5) . ? C34 H34 0.9300 . ? C35 C36 1.473(6) . ? C36 N8 1.352(5) . ? C36 C37 1.393(5) . ? C37 C38 1.377(7) . ? C37 H37 0.9300 . ? C38 C39 1.379(6) . ? C38 H38 0.9300 . ? C39 C40 1.389(5) . ? C39 H39 0.9300 . ? C40 N8 1.342(5) . ? C40 H40 0.9300 . ? O5 Cu5 1.918(3) . ? O5 HW51 0.8579 . ? O6 Cu5 1.973(2) . ? O6 Cu6 2.267(2) . ? O6 HW61 0.7997 . ? Cu5 N9 2.007(3) . ? Cu5 N10 2.017(3) . ? Cu5 O7 2.374(2) 2_566 ? N9 C41 1.323(5) . ? N9 C45 1.361(4) . ? C41 C42 1.384(5) . ? C41 H41 0.9300 . ? C42 C43 1.393(5) . ? C42 H42 0.9300 . ? C43 C44 1.382(5) . ? C43 H43 0.9300 . ? C44 C45 1.388(5) . ? C44 H44 0.9300 . ? C45 C46 1.480(5) . ? C46 N10 1.349(4) . ? C46 C47 1.386(5) . ? C47 C48 1.382(6) . ? C47 H47 0.9300 . ? C48 C49 1.385(6) . ? C48 H48 0.9300 . ? C49 C50 1.392(5) . ? C49 H49 0.9300 . ? C50 N10 1.339(5) . ? C50 H50 0.9300 . ? O7 Cu6 1.956(2) . ? O7 Cu6 1.956(2) 2_566 ? O7 Cu5 2.374(2) 2_566 ? O7 HW71 0.8524 . ? O8 HW81 0.8163 . ? O8 HW82 0.8578 . ? Cu6 O7 1.956(2) 2_566 ? Cu6 N12 1.996(3) . ? Cu6 N11 2.027(3) . ? Cu6 Cu6 3.0097(11) 2_566 ? N11 C51 1.328(5) . ? N11 C55 1.349(4) . ? C51 C52 1.398(5) . ? C51 H51 0.9300 . ? C52 C53 1.383(5) . ? C52 H52 0.9300 . ? C53 C54 1.385(5) . ? C53 H53 0.9300 . ? C54 C55 1.396(5) . ? C54 H54 0.9300 . ? C55 C56 1.466(5) . ? C56 N12 1.356(4) . ? C56 C57 1.389(5) . ? C57 C58 1.378(5) . ? C57 H57 0.9300 . ? C58 C59 1.385(5) . ? C58 H58 0.9300 . ? C59 C60 1.383(5) . ? C59 H59 0.9300 . ? C60 N12 1.338(4) . ? C60 H60 0.9300 . ? O9 C61 1.258(5) . ? O10 C61 1.251(5) . ? C61 C62 1.540(6) . ? C62 C63 1.518(5) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.376(6) . ? C63 C68 1.392(6) . ? C64 C65 1.395(6) . ? C64 H64A 0.9300 . ? C65 C66 1.363(7) . ? C65 H65A 0.9300 . ? C66 C67 1.399(8) . ? C66 H66A 0.9300 . ? C67 C68 1.401(6) . ? C67 H67A 0.9300 . ? C68 H68A 0.9300 . ? O11 C69 1.273(4) . ? O12 C69 1.251(4) . ? C69 C70 1.525(5) . ? C70 C71 1.507(5) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C72 H72A 0.9300 . ? C73 C74 1.3900 . ? C73 H73A 0.9300 . ? C74 C75 1.3900 . ? C74 H74A 0.9300 . ? C75 C76 1.3900 . ? C75 H75A 0.9300 . ? C76 H76A 0.9300 . ? O13 C77 1.267(4) . ? O14 C77 1.258(4) . ? C77 C78 1.527(5) . ? C78 C79 1.501(5) . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? C79 C84 1.391(5) . ? C79 C80 1.405(5) . ? C80 C81 1.392(6) . ? C80 H80A 0.9300 . ? C81 C82 1.388(6) . ? C81 H81A 0.9300 . ? C82 C83 1.390(6) . ? C82 H82A 0.9300 . ? C83 C84 1.401(5) . ? C83 H83A 0.9300 . ? C84 H84A 0.9300 . ? O15 C85 1.288(7) . ? O16 C85 1.192(6) . ? C85 C86 1.525(8) . ? C86 C87 1.515(7) . ? C86 H86A 0.9700 . ? C86 H86B 0.9700 . ? C87 C92 1.376(7) . ? C87 C88 1.390(8) . ? C88 C89 1.391(8) . ? C88 H88A 0.9300 . ? C89 C90 1.369(8) . ? C89 H89A 0.9300 . ? C90 C91 1.363(8) . ? C90 H90A 0.9300 . ? C91 C92 1.380(7) . ? C91 H91A 0.9300 . ? C92 H92A 0.9300 . ? O17 C93 1.256(5) . ? O18 C93 1.263(5) . ? C93 C94 1.535(5) . ? C94 C95 1.510(5) . ? C94 H94A 0.9700 . ? C94 H94B 0.9700 . ? C95 C96 1.382(6) . ? C95 C100 1.395(5) . ? C96 C97 1.393(6) . ? C96 H96A 0.9300 . ? C97 C98 1.382(6) . ? C97 H97A 0.9300 . ? C98 C99 1.397(6) . ? C98 H98A 0.9300 . ? C99 C100 1.379(6) . ? C99 H99A 0.9300 . ? C100 H10A 0.9300 . ? O19 C101 1.245(5) . ? O20 C101 1.270(5) . ? C101 C102 1.522(5) . ? C102 C103 1.503(5) . ? C102 H10B 0.9700 . ? C102 H10C 0.9700 . ? C103 C104 1.396(5) . ? C103 C108 1.402(6) . ? C104 C105 1.395(6) . ? C104 H10D 0.9300 . ? C105 C106 1.365(7) . ? C105 H10E 0.9300 . ? C106 C107 1.388(7) . ? C106 H10F 0.9300 . ? C107 C108 1.392(6) . ? C107 H10G 0.9300 . ? C108 H10H 0.9300 . ? O21 H211 0.8669 . ? O21 H212 0.8799 . ? O22 H221 0.8801 . ? O22 H222 0.8800 . ? O23 H231 0.8799 . ? O23 H232 0.8671 . ? O24 H241 0.8800 . ? O24 H242 0.8670 . ? O25 H251 0.8741 . ? O25 H252 0.8801 . ? O26 H261 0.8801 . ? O26 H262 0.8701 . ? O27 H271 0.8749 . ? O27 H272 0.8800 . ? O28 H281 0.8799 . ? O28 H282 0.8751 . ? O29 H291 0.8750 . ? O29 H292 0.8800 . ? O30 H301 0.8800 . ? O30 H302 0.8801 . ? O31 H311 0.8378 . ? O31 H312 0.8697 . ? O32 H321 0.8671 . ? O32 H322 0.8800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O2 79.15(10) . . ? O1 Cu1 N2 171.40(11) . . ? O2 Cu1 N2 99.04(11) . . ? O1 Cu1 N1 97.58(12) . . ? O2 Cu1 N1 157.35(11) . . ? N2 Cu1 N1 80.83(12) . . ? O1 Cu1 O4 92.92(11) . . ? O2 Cu1 O4 95.52(9) . . ? N2 Cu1 O4 95.63(11) . . ? N1 Cu1 O4 107.07(11) . . ? O1 Cu1 Cu2 39.44(7) . . ? O2 Cu1 Cu2 41.74(7) . . ? N2 Cu1 Cu2 140.41(9) . . ? N1 Cu1 Cu2 136.61(9) . . ? O4 Cu1 Cu2 85.58(7) . . ? C1 N1 C5 119.0(3) . . ? C1 N1 Cu1 126.2(2) . . ? C5 N1 Cu1 114.5(2) . . ? N1 C1 C2 121.7(4) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C3 C2 C1 119.6(4) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.2(4) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 119.3(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 121.2(4) . . ? N1 C5 C6 114.6(3) . . ? C4 C5 C6 124.3(3) . . ? N2 C6 C7 121.3(4) . . ? N2 C6 C5 114.6(3) . . ? C7 C6 C5 124.1(3) . . ? C8 C7 C6 119.8(4) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 119.3(4) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C8 C9 C10 118.4(4) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? N2 C10 C9 122.6(4) . . ? N2 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C10 N2 C6 118.6(3) . . ? C10 N2 Cu1 126.1(2) . . ? C6 N2 Cu1 115.1(2) . . ? Cu2 O1 Cu1 101.02(11) . . ? Cu2 O1 HW11 124.4 . . ? Cu1 O1 HW11 126.0 . . ? Cu2 O2 Cu1 96.01(10) . . ? Cu2 O2 Cu3 95.16(9) . . ? Cu1 O2 Cu3 108.06(10) . . ? Cu2 O2 HW21 128.3 . . ? Cu1 O2 HW21 121.1 . . ? Cu3 O2 HW21 104.6 . . ? O1 Cu2 O2 79.74(10) . . ? O1 Cu2 N4 99.14(11) . . ? O2 Cu2 N4 177.82(10) . . ? O1 Cu2 N3 162.45(11) . . ? O2 Cu2 N3 99.47(11) . . ? N4 Cu2 N3 81.01(12) . . ? O1 Cu2 O3 98.36(10) . 2_665 ? O2 Cu2 O3 84.47(9) . 2_665 ? N4 Cu2 O3 97.56(10) . 2_665 ? N3 Cu2 O3 99.02(10) . 2_665 ? O1 Cu2 Cu1 39.54(7) . . ? O2 Cu2 Cu1 42.25(7) . . ? N4 Cu2 Cu1 136.18(8) . . ? N3 Cu2 Cu1 132.84(8) . . ? O3 Cu2 Cu1 101.87(6) 2_665 . ? C11 N3 C15 119.3(3) . . ? C11 N3 Cu2 126.3(2) . . ? C15 N3 Cu2 114.3(2) . . ? N3 C11 C12 122.3(3) . . ? N3 C11 H11 118.9 . . ? C12 C11 H11 118.8 . . ? C11 C12 C13 119.0(4) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C12 C13 C14 119.1(3) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C13 C14 C15 119.3(4) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? N3 C15 C14 121.0(3) . . ? N3 C15 C16 115.0(3) . . ? C14 C15 C16 124.0(3) . . ? N4 C16 C17 121.1(4) . . ? N4 C16 C15 114.6(3) . . ? C17 C16 C15 124.3(3) . . ? C18 C17 C16 118.8(4) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C19 C18 C17 120.2(4) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 118.7(4) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? N4 C20 C19 121.5(4) . . ? N4 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 N4 C16 119.6(3) . . ? C20 N4 Cu2 125.6(2) . . ? C16 N4 Cu2 114.7(2) . . ? Cu3 O3 Cu3 98.75(11) . 2_665 ? Cu3 O3 Cu2 105.95(10) . 2_665 ? Cu3 O3 Cu2 93.11(9) 2_665 2_665 ? Cu3 O3 HW31 110.1 . . ? Cu3 O3 HW31 119.4 2_665 . ? Cu2 O3 HW31 125.5 2_665 . ? Cu1 O4 HW41 104.2 . . ? Cu1 O4 HW42 130.4 . . ? HW41 O4 HW42 117.7 . . ? O3 Cu3 O3 81.25(11) . 2_665 ? O3 Cu3 N5 160.85(11) . . ? O3 Cu3 N5 98.59(11) 2_665 . ? O3 Cu3 N6 98.65(11) . . ? O3 Cu3 N6 177.39(10) 2_665 . ? N5 Cu3 N6 80.65(12) . . ? O3 Cu3 O2 100.36(9) . . ? O3 Cu3 O2 86.61(9) 2_665 . ? N5 Cu3 O2 98.74(10) . . ? N6 Cu3 O2 95.96(10) . . ? O3 Cu3 Cu3 40.85(7) . 2_665 ? O3 Cu3 Cu3 40.40(7) 2_665 2_665 ? N5 Cu3 Cu3 135.92(9) . 2_665 ? N6 Cu3 Cu3 139.43(9) . 2_665 ? O2 Cu3 Cu3 94.52(6) . 2_665 ? C21 N5 C25 119.2(3) . . ? C21 N5 Cu3 125.4(2) . . ? C25 N5 Cu3 115.3(2) . . ? N5 C21 C22 122.5(4) . . ? N5 C21 H21 118.7 . . ? C22 C21 H21 118.7 . . ? C21 C22 C23 118.3(4) . . ? C21 C22 H22 120.8 . . ? C23 C22 H22 120.8 . . ? C24 C23 C22 119.3(4) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C23 C24 C25 119.3(4) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? N5 C25 C24 121.3(4) . . ? N5 C25 C26 114.6(3) . . ? C24 C25 C26 124.1(3) . . ? N6 C26 C27 121.7(4) . . ? N6 C26 C25 114.6(3) . . ? C27 C26 C25 123.8(3) . . ? C28 C27 C26 119.0(4) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C27 C28 C29 119.8(4) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C30 C29 C28 118.4(4) . . ? C30 C29 H29 120.8 . . ? C28 C29 H29 120.8 . . ? N6 C30 C29 121.9(4) . . ? N6 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? O5 Cu4 O6 81.87(11) . . ? O5 Cu4 N8 173.18(12) . . ? O6 Cu4 N8 99.27(12) . . ? O5 Cu4 N7 96.35(13) . . ? O6 Cu4 N7 162.39(12) . . ? N8 Cu4 N7 80.51(14) . . ? O5 Cu4 O8 91.56(12) . . ? O6 Cu4 O8 88.46(11) . . ? N8 Cu4 O8 95.19(12) . . ? N7 Cu4 O8 109.14(13) . . ? O5 Cu4 Cu5 40.59(8) . . ? O6 Cu4 Cu5 42.43(7) . . ? N8 Cu4 Cu5 141.51(10) . . ? N7 Cu4 Cu5 136.64(11) . . ? O8 Cu4 Cu5 82.49(8) . . ? C31 N7 C35 119.3(4) . . ? C31 N7 Cu4 125.9(3) . . ? C35 N7 Cu4 114.6(3) . . ? N7 C31 C32 121.8(4) . . ? N7 C31 H31 119.1 . . ? C32 C31 H31 119.1 . . ? C33 C32 C31 119.5(5) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C34 119.2(4) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C35 C34 C33 118.4(4) . . ? C35 C34 H34 120.8 . . ? C33 C34 H34 120.8 . . ? N7 C35 C34 121.8(4) . . ? N7 C35 C36 115.0(3) . . ? C34 C35 C36 123.3(4) . . ? N8 C36 C37 121.2(4) . . ? N8 C36 C35 114.7(3) . . ? C37 C36 C35 124.1(4) . . ? C38 C37 C36 119.5(4) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C37 C38 C39 119.2(4) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C38 C39 C40 118.8(4) . . ? C38 C39 H39 120.6 . . ? C40 C39 H39 120.6 . . ? N8 C40 C39 122.3(4) . . ? N8 C40 H40 118.8 . . ? C39 C40 H40 118.8 . . ? C40 N8 C36 118.8(3) . . ? C40 N8 Cu4 126.0(3) . . ? C36 N8 Cu4 115.1(3) . . ? Cu5 O5 Cu4 98.51(13) . . ? Cu5 O5 HW51 138.3 . . ? Cu4 O5 HW51 111.7 . . ? Cu5 O6 Cu4 94.39(11) . . ? Cu5 O6 Cu6 97.25(11) . . ? Cu4 O6 Cu6 110.55(11) . . ? Cu5 O6 HW61 122.9 . . ? Cu4 O6 HW61 105.1 . . ? Cu6 O6 HW61 123.1 . . ? O5 Cu5 O6 82.92(11) . . ? O5 Cu5 N9 165.98(12) . . ? O6 Cu5 N9 99.24(11) . . ? O5 Cu5 N10 95.29(12) . . ? O6 Cu5 N10 173.61(11) . . ? N9 Cu5 N10 81.02(12) . . ? O5 Cu5 O7 95.68(11) . 2_566 ? O6 Cu5 O7 82.50(9) . 2_566 ? N9 Cu5 O7 98.34(11) . 2_566 ? N10 Cu5 O7 103.81(11) . 2_566 ? O5 Cu5 Cu4 40.90(8) . . ? O6 Cu5 Cu4 43.18(8) . . ? N9 Cu5 Cu4 136.71(9) . . ? N10 Cu5 Cu4 133.62(9) . . ? O7 Cu5 Cu4 96.58(6) 2_566 . ? C41 N9 C45 118.8(3) . . ? C41 N9 Cu5 126.5(2) . . ? C45 N9 Cu5 114.6(2) . . ? N9 C41 C42 123.2(3) . . ? N9 C41 H41 118.4 . . ? C42 C41 H41 118.4 . . ? C41 C42 C43 118.3(4) . . ? C41 C42 H42 120.9 . . ? C43 C42 H42 120.9 . . ? C44 C43 C42 119.1(3) . . ? C44 C43 H43 120.5 . . ? C42 C43 H43 120.5 . . ? C43 C44 C45 119.3(3) . . ? C43 C44 H44 120.4 . . ? C45 C44 H44 120.4 . . ? N9 C45 C44 121.3(3) . . ? N9 C45 C46 114.9(3) . . ? C44 C45 C46 123.8(3) . . ? N10 C46 C47 121.8(4) . . ? N10 C46 C45 114.6(3) . . ? C47 C46 C45 123.6(3) . . ? C48 C47 C46 119.1(4) . . ? C48 C47 H47 120.4 . . ? C46 C47 H47 120.4 . . ? C47 C48 C49 119.5(4) . . ? C47 C48 H48 120.3 . . ? C49 C48 H48 120.3 . . ? C48 C49 C50 118.2(4) . . ? C48 C49 H49 120.9 . . ? C50 C49 H49 120.9 . . ? N10 C50 C49 122.6(4) . . ? N10 C50 H50 118.7 . . ? C49 C50 H50 118.7 . . ? C50 N10 C46 118.7(3) . . ? C50 N10 Cu5 126.2(3) . . ? C46 N10 Cu5 114.8(2) . . ? Cu6 O7 Cu6 100.57(11) . 2_566 ? Cu6 O7 Cu5 106.67(10) . 2_566 ? Cu6 O7 Cu5 94.30(10) 2_566 2_566 ? Cu6 O7 HW71 120.3 . . ? Cu6 O7 HW71 121.2 2_566 . ? Cu5 O7 HW71 110.1 2_566 . ? Cu4 O8 HW81 120.9 . . ? Cu4 O8 HW82 124.6 . . ? HW81 O8 HW82 103.6 . . ? O7 Cu6 O7 79.43(11) . 2_566 ? O7 Cu6 N12 97.75(11) . . ? O7 Cu6 N12 176.61(11) 2_566 . ? O7 Cu6 N11 154.92(11) . . ? O7 Cu6 N11 100.88(11) 2_566 . ? N12 Cu6 N11 80.87(12) . . ? O7 Cu6 O6 109.96(10) . . ? O7 Cu6 O6 85.72(10) 2_566 . ? N12 Cu6 O6 97.05(11) . . ? N11 Cu6 O6 95.01(11) . . ? O7 Cu6 Cu6 39.71(7) . 2_566 ? O7 Cu6 Cu6 39.71(7) 2_566 2_566 ? N12 Cu6 Cu6 137.44(9) . 2_566 ? N11 Cu6 Cu6 135.35(9) . 2_566 ? O6 Cu6 Cu6 99.98(7) . 2_566 ? C51 N11 C55 119.3(3) . . ? C51 N11 Cu6 126.5(2) . . ? C55 N11 Cu6 114.2(2) . . ? N11 C51 C52 122.6(3) . . ? N11 C51 H51 118.7 . . ? C52 C51 H51 118.7 . . ? C53 C52 C51 118.3(3) . . ? C53 C52 H52 120.9 . . ? C51 C52 H52 120.9 . . ? C54 C53 C52 119.5(3) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C53 C54 C55 118.9(3) . . ? C53 C54 H54 120.5 . . ? C55 C54 H54 120.5 . . ? N11 C55 C54 121.5(3) . . ? N11 C55 C56 114.9(3) . . ? C54 C55 C56 123.6(3) . . ? N12 C56 C57 121.3(3) . . ? N12 C56 C55 115.1(3) . . ? C57 C56 C55 123.6(3) . . ? C58 C57 C56 119.1(3) . . ? C58 C57 H57 120.4 . . ? C56 C57 H57 120.4 . . ? C30 N6 C26 119.2(3) . . ? C30 N6 Cu3 126.0(2) . . ? C26 N6 Cu3 114.7(2) . . ? C57 C58 C59 119.8(3) . . ? C57 C58 H58 120.1 . . ? C59 C58 H58 120.1 . . ? C60 C59 C58 118.2(3) . . ? C60 C59 H59 120.9 . . ? C58 C59 H59 120.9 . . ? N12 C60 C59 122.7(3) . . ? N12 C60 H60 118.6 . . ? C59 C60 H60 118.6 . . ? C60 N12 C56 118.9(3) . . ? C60 N12 Cu6 126.2(2) . . ? C56 N12 Cu6 114.9(2) . . ? O10 C61 O9 124.6(4) . . ? O10 C61 C62 117.7(4) . . ? O9 C61 C62 117.6(4) . . ? C63 C62 C61 111.1(3) . . ? C63 C62 H62A 109.4 . . ? C61 C62 H62A 109.4 . . ? C63 C62 H62B 109.4 . . ? C61 C62 H62B 109.4 . . ? H62A C62 H62B 108.0 . . ? C64 C63 C68 119.2(4) . . ? C64 C63 C62 121.0(4) . . ? C68 C63 C62 119.8(4) . . ? C63 C64 C65 120.5(4) . . ? C63 C64 H64A 119.8 . . ? C65 C64 H64A 119.8 . . ? C66 C65 C64 121.0(5) . . ? C66 C65 H65A 119.5 . . ? C64 C65 H65A 119.5 . . ? C65 C66 C67 119.3(4) . . ? C65 C66 H66A 120.3 . . ? C67 C66 H66A 120.3 . . ? C66 C67 C68 119.7(5) . . ? C66 C67 H67A 120.1 . . ? C68 C67 H67A 120.1 . . ? C63 C68 C67 120.3(5) . . ? C63 C68 H68A 119.9 . . ? C67 C68 H68A 119.9 . . ? O12 C69 O11 124.6(3) . . ? O12 C69 C70 118.4(3) . . ? O11 C69 C70 117.0(3) . . ? C71 C70 C69 114.6(3) . . ? C71 C70 H70A 108.6 . . ? C69 C70 H70A 108.6 . . ? C71 C70 H70B 108.6 . . ? C69 C70 H70B 108.6 . . ? H70A C70 H70B 107.6 . . ? C72 C71 C76 120.0 . . ? C72 C71 C70 123.2(3) . . ? C76 C71 C70 116.6(3) . . ? C73 C72 C71 120.0 . . ? C73 C72 H72A 120.0 . . ? C71 C72 H72A 120.0 . . ? C72 C73 C74 120.0 . . ? C72 C73 H73A 120.0 . . ? C74 C73 H73A 120.0 . . ? C73 C74 C75 120.0 . . ? C73 C74 H74A 120.0 . . ? C75 C74 H74A 120.0 . . ? C76 C75 C74 120.0 . . ? C76 C75 H75A 120.0 . . ? C74 C75 H75A 120.0 . . ? C75 C76 C71 120.0 . . ? C75 C76 H76A 120.0 . . ? C71 C76 H76A 120.0 . . ? O14 C77 O13 124.4(3) . . ? O14 C77 C78 117.2(3) . . ? O13 C77 C78 118.3(3) . . ? C79 C78 C77 108.9(3) . . ? C79 C78 H78A 109.9 . . ? C77 C78 H78A 109.9 . . ? C79 C78 H78B 109.9 . . ? C77 C78 H78B 109.9 . . ? H78A C78 H78B 108.3 . . ? C84 C79 C80 118.8(3) . . ? C84 C79 C78 120.2(3) . . ? C80 C79 C78 120.9(3) . . ? C81 C80 C79 120.4(4) . . ? C81 C80 H80A 119.8 . . ? C79 C80 H80A 119.8 . . ? C82 C81 C80 120.6(4) . . ? C82 C81 H81A 119.7 . . ? C80 C81 H81A 119.7 . . ? C81 C82 C83 119.4(4) . . ? C81 C82 H82A 120.3 . . ? C83 C82 H82A 120.3 . . ? C82 C83 C84 120.4(4) . . ? C82 C83 H83A 119.8 . . ? C84 C83 H83A 119.8 . . ? C79 C84 C83 120.4(4) . . ? C79 C84 H84A 119.8 . . ? C83 C84 H84A 119.8 . . ? O16 C85 O15 121.0(5) . . ? O16 C85 C86 119.6(5) . . ? O15 C85 C86 119.4(5) . . ? C87 C86 C85 113.7(4) . . ? C87 C86 H86A 108.8 . . ? C85 C86 H86A 108.8 . . ? C87 C86 H86B 108.8 . . ? C85 C86 H86B 108.8 . . ? H86A C86 H86B 107.7 . . ? C92 C87 C88 118.0(5) . . ? C92 C87 C86 120.8(5) . . ? C88 C87 C86 121.2(5) . . ? C87 C88 C89 121.1(5) . . ? C87 C88 H88A 119.5 . . ? C89 C88 H88A 119.5 . . ? C90 C89 C88 119.5(6) . . ? C90 C89 H89A 120.2 . . ? C88 C89 H89A 120.2 . . ? C91 C90 C89 119.7(5) . . ? C91 C90 H90A 120.1 . . ? C89 C90 H90A 120.1 . . ? C90 C91 C92 121.0(5) . . ? C90 C91 H91A 119.5 . . ? C92 C91 H91A 119.5 . . ? C87 C92 C91 120.6(5) . . ? C87 C92 H92A 119.7 . . ? C91 C92 H92A 119.7 . . ? O17 C93 O18 124.2(3) . . ? O17 C93 C94 117.7(4) . . ? O18 C93 C94 118.1(4) . . ? C95 C94 C93 112.2(3) . . ? C95 C94 H94A 109.2 . . ? C93 C94 H94A 109.2 . . ? C95 C94 H94B 109.2 . . ? C93 C94 H94B 109.2 . . ? H94A C94 H94B 107.9 . . ? C96 C95 C100 118.6(4) . . ? C96 C95 C94 121.3(4) . . ? C100 C95 C94 120.1(4) . . ? C95 C96 C97 120.7(4) . . ? C95 C96 H96A 119.6 . . ? C97 C96 H96A 119.6 . . ? C98 C97 C96 120.6(4) . . ? C98 C97 H97A 119.7 . . ? C96 C97 H97A 119.7 . . ? C97 C98 C99 118.8(4) . . ? C97 C98 H98A 120.6 . . ? C99 C98 H98A 120.6 . . ? C100 C99 C98 120.4(4) . . ? C100 C99 H99A 119.8 . . ? C98 C99 H99A 119.8 . . ? C99 C100 C95 120.9(4) . . ? C99 C100 H10A 119.5 . . ? C95 C100 H10A 119.5 . . ? O19 C101 O20 125.1(4) . . ? O19 C101 C102 117.7(4) . . ? O20 C101 C102 117.1(3) . . ? C103 C102 C101 110.5(3) . . ? C103 C102 H10B 109.6 . . ? C101 C102 H10B 109.6 . . ? C103 C102 H10C 109.6 . . ? C101 C102 H10C 109.6 . . ? H10B C102 H10C 108.1 . . ? C104 C103 C108 118.2(4) . . ? C104 C103 C102 120.4(4) . . ? C108 C103 C102 121.4(4) . . ? C103 C104 C105 120.6(4) . . ? C103 C104 H10D 119.7 . . ? C105 C104 H10D 119.7 . . ? C106 C105 C104 120.3(4) . . ? C106 C105 H10E 119.9 . . ? C104 C105 H10E 119.9 . . ? C105 C106 C107 120.5(4) . . ? C105 C106 H10F 119.7 . . ? C107 C106 H10F 119.7 . . ? C106 C107 C108 119.6(4) . . ? C106 C107 H10G 120.2 . . ? C108 C107 H10G 120.2 . . ? C107 C108 C103 120.7(4) . . ? C107 C108 H10H 119.6 . . ? C103 C108 H10H 119.6 . . ? H211 O21 H212 121.9 . . ? H221 O22 H222 129.1 . . ? H231 O23 H232 105.8 . . ? H241 O24 H242 112.7 . . ? H251 O25 H252 118.9 . . ? H261 O26 H262 106.3 . . ? H271 O27 H272 107.4 . . ? H281 O28 H282 98.0 . . ? H291 O29 H292 103.1 . . ? H301 O30 H302 125.0 . . ? H311 O31 H312 91.5 . . ? H321 O32 H322 93.5 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 2.771 _refine_diff_density_min -1.887 _refine_diff_density_rms 0.140