# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 869203' #TrackingRef 'web_deposit_cif_file_0_Hui-ZhongKou_1330685378.kou-sub.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H81 Cu8 N11 O27' _chemical_formula_weight 2052.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.7644(13) _cell_length_b 15.3413(14) _cell_length_c 18.7449(19) _cell_angle_alpha 87.711(3) _cell_angle_beta 85.549(3) _cell_angle_gamma 75.531(3) _cell_volume 4097.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 2.119 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.833 _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 IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% 0 _diffrn_reflns_number 32422 _diffrn_reflns_av_R_equivalents 0.1657 _diffrn_reflns_av_sigmaI/netI 0.2295 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14282 _reflns_number_gt 4940 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.1109P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14282 _refine_ls_number_parameters 1069 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.2541 _refine_ls_R_factor_gt 0.0968 _refine_ls_wR_factor_ref 0.2629 _refine_ls_wR_factor_gt 0.2073 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.030 _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 0.09452(13) 0.61168(11) 0.48369(8) 0.0658(6) Uani 1 1 d . . . Cu2 Cu 0.09920(13) 0.65526(11) 0.29770(9) 0.0662(6) Uani 1 1 d . . . Cu3 Cu -0.39998(15) 1.21794(12) 0.04986(10) 0.0813(7) Uani 1 1 d . . . Cu4 Cu -0.18052(13) 1.13155(11) 0.11409(9) 0.0663(6) Uani 1 1 d . . . Cu5 Cu 0.07406(13) 0.81576(11) 0.39250(8) 0.0642(6) Uani 1 1 d . . . Cu6 Cu 0.10549(14) 0.85803(11) 0.21035(9) 0.0701(6) Uani 1 1 d . . . Cu7 Cu -0.33624(14) 1.21191(12) 0.22436(9) 0.0737(6) Uani 1 1 d . . . Cu8 Cu -0.11277(13) 1.13781(12) 0.28522(9) 0.0708(6) Uani 1 1 d . . . C1 C 0.2275(12) 0.5415(10) 0.3744(7) 0.067(4) Uani 1 1 d . . . C2 C 0.2763(13) 0.5575(11) 0.3074(8) 0.079(5) Uani 1 1 d . . . C3 C 0.3677(15) 0.5090(14) 0.2893(11) 0.119(7) Uani 1 1 d . . . H3A H 0.3993 0.5229 0.2472 0.143 Uiso 1 1 calc R . . C4 C 0.4119(13) 0.4393(12) 0.3345(9) 0.105(6) Uani 1 1 d . . . H4A H 0.4717 0.4046 0.3215 0.126 Uiso 1 1 calc R . . C5 C 0.3668(16) 0.4227(13) 0.3974(10) 0.113(7) Uani 1 1 d . . . H5A H 0.3972 0.3774 0.4279 0.135 Uiso 1 1 calc R . . C6 C 0.2761(12) 0.4718(10) 0.4175(8) 0.066(4) Uani 1 1 d . . . C7 C 0.2349(12) 0.4449(10) 0.4860(8) 0.071(4) Uani 1 1 d . . . H7A H 0.2659 0.3927 0.5095 0.085 Uiso 1 1 calc R . . C8 C 0.1111(11) 0.4609(11) 0.5796(8) 0.077(5) Uani 1 1 d . . . H8A H 0.1579 0.4229 0.6085 0.092 Uiso 1 1 calc R . . H8B H 0.0689 0.4256 0.5669 0.092 Uiso 1 1 calc R . . C9 C 0.0573(12) 0.5404(11) 0.6219(8) 0.084(5) Uani 1 1 d . . . H9A H 0.0085 0.5242 0.6534 0.101 Uiso 1 1 calc R . . H9B H 0.0987 0.5619 0.6508 0.101 Uiso 1 1 calc R . . C10 C -0.0671(12) 0.6556(10) 0.5796(7) 0.061(4) Uani 1 1 d . . . H10A H -0.1011 0.6421 0.6206 0.073 Uiso 1 1 calc R . . C11 C -0.1146(12) 0.7280(9) 0.5318(7) 0.065(4) Uani 1 1 d . . . C12 C -0.2108(13) 0.7649(10) 0.5403(8) 0.078(5) Uani 1 1 d . . . H12A H -0.2450 0.7437 0.5778 0.094 Uiso 1 1 calc R . . C13 C -0.2575(12) 0.8317(9) 0.4952(8) 0.079(5) Uani 1 1 d . . . H13A H -0.3220 0.8543 0.5028 0.095 Uiso 1 1 calc R . . C14 C -0.2082(12) 0.8663(9) 0.4377(7) 0.068(4) Uani 1 1 d . . . C15 C -0.1112(12) 0.8332(9) 0.4279(6) 0.060(4) Uani 1 1 d . . . C16 C -0.0616(12) 0.7615(8) 0.4739(7) 0.060(4) Uani 1 1 d . . . C17 C -0.2587(10) 0.9331(8) 0.3858(7) 0.058(4) Uani 1 1 d . . . C18 C -0.3306(11) 0.9163(10) 0.3511(8) 0.080(5) Uani 1 1 d . . . H18A H -0.3488 0.8635 0.3631 0.096 Uiso 1 1 calc R . . C19 C -0.3760(11) 0.9706(9) 0.3013(9) 0.086(6) Uani 1 1 d . . . H19A H -0.4268 0.9571 0.2818 0.103 Uiso 1 1 calc R . . C20 C -0.3467(10) 1.0494(11) 0.2780(8) 0.075(4) Uani 1 1 d . . . C21 C -0.2762(10) 1.0693(10) 0.3121(7) 0.073(5) Uani 1 1 d . . . C22 C -0.2298(10) 1.0140(9) 0.3677(7) 0.063(4) Uani 1 1 d . . . C23 C -0.1584(10) 1.0361(9) 0.4072(7) 0.062(4) Uani 1 1 d . . . H23A H -0.1462 1.0088 0.4519 0.074 Uiso 1 1 calc R . . C24 C -0.0354(11) 1.1153(10) 0.4200(7) 0.074(5) Uani 1 1 d . . . H24A H -0.0199 1.0759 0.4614 0.088 Uiso 1 1 calc R . . H24B H -0.0549 1.1770 0.4358 0.088 Uiso 1 1 calc R . . C25 C 0.0479(11) 1.1034(9) 0.3663(7) 0.070(5) Uani 1 1 d . . . H25A H 0.0942 1.1316 0.3828 0.084 Uiso 1 1 calc R . . H25B H 0.0769 1.0399 0.3595 0.084 Uiso 1 1 calc R . . C26 C 0.0611(11) 1.1823(9) 0.2524(9) 0.080(5) Uani 1 1 d . . . H26A H 0.1197 1.1854 0.2655 0.096 Uiso 1 1 calc R . . C27 C 0.0351(10) 1.2183(9) 0.1828(7) 0.060(4) Uani 1 1 d . . . C28 C 0.0925(11) 1.2672(10) 0.1410(8) 0.083(5) Uani 1 1 d . . . H28A H 0.1447 1.2787 0.1599 0.100 Uiso 1 1 calc R . . C29 C 0.0707(13) 1.2964(11) 0.0743(8) 0.096(6) Uani 1 1 d . . . H29A H 0.1105 1.3252 0.0471 0.116 Uiso 1 1 calc R . . C30 C -0.0079(12) 1.2854(11) 0.0450(9) 0.087(5) Uani 1 1 d . . . H30A H -0.0218 1.3078 -0.0008 0.105 Uiso 1 1 calc R . . C31 C -0.0661(11) 1.2406(8) 0.0842(7) 0.061(4) Uani 1 1 d . . . C32 C -0.0446(12) 1.2073(9) 0.1509(7) 0.072(5) Uani 1 1 d . . . C33 C 0.2053(10) 0.8930(8) 0.3265(7) 0.064(4) Uani 1 1 d . . . C34 C 0.2324(12) 0.8717(10) 0.3983(8) 0.078(5) Uani 1 1 d . . . C35 C 0.3018(12) 0.9024(12) 0.4245(8) 0.096(6) Uani 1 1 d . . . H35A H 0.3185 0.8883 0.4712 0.115 Uiso 1 1 calc R . . C36 C 0.3479(14) 0.9564(13) 0.3794(10) 0.121(7) Uani 1 1 d . . . H36A H 0.3963 0.9772 0.3959 0.145 Uiso 1 1 calc R . . C37 C 0.3207(12) 0.9785(11) 0.3097(9) 0.092(6) Uani 1 1 d . . . H37A H 0.3511 1.0150 0.2812 0.111 Uiso 1 1 calc R . . C38 C 0.2499(10) 0.9481(10) 0.2813(8) 0.069(4) Uani 1 1 d . . . C39 C 0.2216(11) 0.9818(9) 0.2120(7) 0.067(4) Uani 1 1 d . . . H39A H 0.2490 1.0249 0.1893 0.080 Uiso 1 1 calc R . . C40 C 0.1279(12) 0.9971(10) 0.1118(7) 0.088(5) Uani 1 1 d . . . H40A H 0.1743 1.0245 0.0870 0.105 Uiso 1 1 calc R . . H40B H 0.0701 1.0434 0.1201 0.105 Uiso 1 1 calc R . . C41 C 0.1112(11) 0.9227(9) 0.0674(6) 0.072(4) Uani 1 1 d . . . H41A H 0.0759 0.9477 0.0267 0.086 Uiso 1 1 calc R . . H41B H 0.1703 0.8830 0.0502 0.086 Uiso 1 1 calc R . . C42 C -0.0210(10) 0.8561(9) 0.1040(6) 0.056(4) Uani 1 1 d . . . H42A H -0.0441 0.8738 0.0595 0.067 Uiso 1 1 calc R . . C43 C -0.0748(11) 0.8103(8) 0.1551(6) 0.061(4) Uani 1 1 d . . . C44 C -0.1700(10) 0.8187(8) 0.1482(7) 0.057(4) Uani 1 1 d . . . C45 C -0.2156(10) 0.7702(9) 0.1961(7) 0.068(4) Uani 1 1 d . . . H45A H -0.2793 0.7753 0.1932 0.081 Uiso 1 1 calc R . . C46 C -0.1672(12) 0.7126(9) 0.2499(7) 0.074(5) Uani 1 1 d . . . H46A H -0.1992 0.6789 0.2799 0.089 Uiso 1 1 calc R . . C47 C -0.0757(12) 0.7063(9) 0.2577(7) 0.068(4) Uani 1 1 d . . . C48 C -0.0304(11) 0.7564(9) 0.2110(7) 0.059(4) Uani 1 1 d . . . C49 C -0.2230(10) 0.8838(9) 0.0960(7) 0.068(4) Uani 1 1 d . . . C50 C -0.2775(10) 0.8550(9) 0.0487(7) 0.070(4) Uani 1 1 d . . . H50A H -0.2740 0.7939 0.0459 0.084 Uiso 1 1 calc R . . C51 C -0.3377(11) 0.9167(9) 0.0052(8) 0.080(5) Uani 1 1 d . . . H51A H -0.3735 0.8962 -0.0260 0.096 Uiso 1 1 calc R . . C52 C -0.3436(10) 1.0099(9) 0.0089(7) 0.063(4) Uani 1 1 d . . . C53 C -0.2871(10) 1.0378(9) 0.0562(7) 0.066(4) Uani 1 1 d . . . C54 C -0.2251(10) 0.9786(8) 0.0982(7) 0.061(4) Uani 1 1 d . . . C55 C -0.4046(10) 1.0681(10) -0.0380(7) 0.069(4) Uani 1 1 d . . . H55A H -0.4271 1.0436 -0.0755 0.083 Uiso 1 1 calc R . . C56 C -0.4955(12) 1.2172(11) -0.0751(9) 0.085(5) Uani 1 1 d . . . H56A H -0.5302 1.1840 -0.1008 0.102 Uiso 1 1 calc R . . H56B H -0.4613 1.2478 -0.1097 0.102 Uiso 1 1 calc R . . C57 C -0.5633(12) 1.2860(12) -0.0261(9) 0.087(6) Uani 1 1 d . . . H57A H -0.5945 1.3383 -0.0536 0.105 Uiso 1 1 calc R . . H57B H -0.6104 1.2594 -0.0015 0.105 Uiso 1 1 calc R . . C58 C -0.5259(11) 1.3902(12) 0.0485(8) 0.074(5) Uani 1 1 d . . . H58A H -0.5748 1.4317 0.0283 0.089 Uiso 1 1 calc R . . C59 C -0.4794(10) 1.4221(10) 0.1051(8) 0.070(4) Uani 1 1 d . . . C60 C -0.4956(12) 1.5184(10) 0.1214(9) 0.088(5) Uani 1 1 d . . . H60A H -0.5380 1.5610 0.0959 0.106 Uiso 1 1 calc R . . C61 C -0.4514(12) 1.5451(11) 0.1710(8) 0.086(5) Uani 1 1 d . . . H61A H -0.4585 1.6062 0.1779 0.103 Uiso 1 1 calc R . . C62 C -0.3947(12) 1.4824(10) 0.2128(8) 0.081(5) Uani 1 1 d . . . H62A H -0.3663 1.5030 0.2490 0.098 Uiso 1 1 calc R . . C63 C -0.3771(11) 1.3909(10) 0.2044(8) 0.072(4) Uani 1 1 d . . . C64 C -0.4175(10) 1.3597(9) 0.1473(8) 0.065(4) Uani 1 1 d . . . C65 C -0.2261(15) 1.4474(15) 0.0807(10) 0.115(7) Uani 1 1 d . . . H65A H -0.2329 1.3936 0.1022 0.138 Uiso 1 1 calc R . . C66 C -0.1370(14) 1.4632(12) 0.1791(9) 0.119(7) Uani 1 1 d . . . H66A H -0.1028 1.5043 0.1937 0.179 Uiso 1 1 calc R . . H66B H -0.0954 1.4044 0.1735 0.179 Uiso 1 1 calc R . . H66C H -0.1865 1.4604 0.2148 0.179 Uiso 1 1 calc R . . C67 C -0.160(2) 1.5708(14) 0.0826(12) 0.186(13) Uani 1 1 d . . . H67A H -0.1908 1.5845 0.0389 0.279 Uiso 1 1 calc R . . H67B H -0.0936 1.5632 0.0726 0.279 Uiso 1 1 calc R . . H67C H -0.1835 1.6193 0.1152 0.279 Uiso 1 1 calc R . . C68 C -0.1373(19) 0.5532(18) 0.7694(13) 0.139(9) Uani 1 1 d . . . H68A H -0.0805 0.5188 0.7496 0.167 Uiso 1 1 calc R . . C69 C -0.1177(17) 0.4465(15) 0.8728(12) 0.157(9) Uani 1 1 d . . . H69A H -0.0580 0.4255 0.8468 0.236 Uiso 1 1 calc R . . H69B H -0.1501 0.3993 0.8766 0.236 Uiso 1 1 calc R . . H69C H -0.1084 0.4638 0.9198 0.236 Uiso 1 1 calc R . . C70 C -0.2705(17) 0.571(2) 0.8581(15) 0.226(17) Uani 1 1 d . . . H70A H -0.2939 0.6200 0.8254 0.340 Uiso 1 1 calc R . . H70B H -0.2715 0.5944 0.9051 0.340 Uiso 1 1 calc R . . H70C H -0.3095 0.5295 0.8595 0.340 Uiso 1 1 calc R . . C71 C 0.4670(14) 1.2008(12) 0.3480(9) 0.189(13) Uani 1 1 d D . . H71A H 0.4701 1.2480 0.3160 0.227 Uiso 1 1 calc R . . C72 C 0.5326(14) 1.1023(12) 0.4514(9) 0.223(13) Uani 1 1 d RDU . . H72A H 0.4874 1.0708 0.4396 0.334 Uiso 1 1 calc R . . H72B H 0.5214 1.1192 0.5007 0.334 Uiso 1 1 calc R . . H72C H 0.5946 1.0640 0.4438 0.334 Uiso 1 1 calc R . . C73 C 0.5910(17) 1.2379(14) 0.4164(12) 0.190(12) Uani 1 1 d D . . H73A H 0.5826 1.2872 0.3824 0.286 Uiso 1 1 calc R . . H73B H 0.6539 1.2010 0.4099 0.286 Uiso 1 1 calc R . . H73C H 0.5803 1.2609 0.4640 0.286 Uiso 1 1 calc R . . N1 N 0.1576(9) 0.4914(8) 0.5137(6) 0.061(3) Uani 1 1 d . . . N2 N 0.0154(10) 0.6113(8) 0.5689(6) 0.066(3) Uani 1 1 d . . . N3 N 0.0560(9) 0.8727(7) 0.1179(5) 0.060(3) Uani 1 1 d . . . N4 N 0.1616(8) 0.9559(6) 0.1805(6) 0.058(3) Uani 1 1 d . . . N5 N -0.4295(9) 1.1548(9) -0.0292(6) 0.076(4) Uani 1 1 d . . . N6 N -0.5050(9) 1.3114(8) 0.0252(6) 0.077(4) Uani 1 1 d . . . N7 N 0.0124(9) 1.1472(8) 0.2973(6) 0.074(4) Uani 1 1 d . . . N8 N -0.1116(9) 1.0918(7) 0.3830(5) 0.064(3) Uani 1 1 d . . . N9 N -0.1763(10) 1.4939(9) 0.1124(7) 0.090(4) Uani 1 1 d . . . N10 N -0.1743(16) 0.5252(13) 0.8342(9) 0.131(7) Uani 1 1 d . . . N11 N 0.5240(14) 1.1836(13) 0.4056(11) 0.192(10) Uani 1 1 d D . . O1 O 0.2257(7) 0.6234(7) 0.2653(5) 0.087(3) Uani 1 1 d . . . O2 O 0.1400(7) 0.5897(6) 0.3865(5) 0.062(3) Uani 1 1 d . . . O3 O 0.0321(8) 0.7327(6) 0.4606(5) 0.068(3) Uani 1 1 d . . . O4 O -0.0554(6) 0.8618(6) 0.3750(4) 0.064(3) Uani 1 1 d . . . O5 O 0.1314(7) 0.8632(6) 0.3092(4) 0.067(3) Uani 1 1 d . . . O6 O 0.1834(7) 0.8198(6) 0.4354(4) 0.078(3) Uani 1 1 d . . . O7 O 0.0590(7) 0.7509(5) 0.2251(4) 0.062(3) Uani 1 1 d . . . O8 O -0.0251(7) 0.6501(6) 0.3061(5) 0.071(3) Uani 1 1 d . . . O9 O -0.2864(6) 1.1246(6) 0.0628(4) 0.064(3) Uani 1 1 d . . . O10 O -0.1719(7) 1.0091(5) 0.1394(4) 0.065(3) Uani 1 1 d . . . O11 O -0.2469(6) 1.1462(5) 0.2874(5) 0.065(3) Uani 1 1 d . . . O12 O -0.3856(7) 1.1098(6) 0.2280(5) 0.082(3) Uani 1 1 d . . . O13 O -0.1419(7) 1.2236(6) 0.0573(5) 0.075(3) Uani 1 1 d . . . O14 O -0.1028(6) 1.1608(6) 0.1839(4) 0.067(3) Uani 1 1 d . . . O15 O -0.3961(7) 1.2700(6) 0.1403(5) 0.073(3) Uani 1 1 d . . . O16 O -0.3243(7) 1.3287(6) 0.2449(5) 0.079(3) Uani 1 1 d . . . O17 O -0.2641(9) 1.4719(8) 0.0238(7) 0.120(4) Uani 1 1 d . . . O18 O -0.1785(16) 0.6243(13) 0.7361(9) 0.186(9) Uani 1 1 d . . . O19 O 0.4108(15) 1.1520(14) 0.3391(11) 0.241(10) Uani 1 1 d D . . O1W O -0.0578(6) 0.9671(6) 0.2523(4) 0.068(3) Uani 1 1 d . . . O2W O -0.2890(8) 1.3041(7) -0.0205(5) 0.094(3) Uani 1 1 d . . . O3W O 0.2124(7) 0.6732(6) 0.5254(6) 0.087(3) Uani 1 1 d . . . O4W O -0.1679(10) 1.3051(8) 0.3193(6) 0.130(5) Uani 1 1 d . . . O5W O 0.2729(8) 0.7483(7) 0.1697(6) 0.102(4) Uani 1 1 d . . . O6W O -0.5252(11) 1.1167(11) 0.1366(8) 0.170(6) Uani 1 1 d . . . O7W O 0.3127(15) 1.2133(16) 0.2339(12) 0.248(10) Uani 1 1 d . . . O8W O -0.487(2) 1.680(2) 0.3555(16) 0.332(14) 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 0.0959(15) 0.0574(11) 0.0456(10) 0.0151(8) -0.0166(9) -0.0206(10) Cu2 0.0915(15) 0.0626(11) 0.0479(10) 0.0164(9) -0.0166(10) -0.0243(11) Cu3 0.1052(17) 0.0645(12) 0.0767(14) 0.0132(10) -0.0414(12) -0.0172(12) Cu4 0.0955(15) 0.0583(11) 0.0523(11) 0.0124(8) -0.0247(10) -0.0290(11) Cu5 0.0939(14) 0.0618(11) 0.0434(10) 0.0136(8) -0.0151(9) -0.0304(11) Cu6 0.1036(15) 0.0700(12) 0.0477(10) 0.0162(9) -0.0157(10) -0.0418(12) Cu7 0.0944(15) 0.0637(12) 0.0639(12) 0.0147(10) -0.0237(11) -0.0183(11) Cu8 0.0969(15) 0.0729(12) 0.0511(11) 0.0158(9) -0.0226(10) -0.0342(12) C1 0.093(13) 0.059(9) 0.054(9) 0.010(8) -0.030(9) -0.023(10) C2 0.096(14) 0.077(11) 0.053(10) 0.009(9) 0.001(10) -0.004(11) C3 0.115(18) 0.145(19) 0.091(15) 0.033(14) -0.028(14) -0.018(15) C4 0.092(14) 0.112(14) 0.080(13) 0.030(11) -0.009(11) 0.029(11) C5 0.136(19) 0.110(15) 0.088(15) 0.056(12) -0.028(13) -0.027(15) C6 0.074(12) 0.059(10) 0.061(10) 0.010(8) -0.012(9) -0.006(9) C7 0.077(12) 0.056(10) 0.073(11) 0.010(9) -0.022(10) -0.001(9) C8 0.084(12) 0.085(12) 0.069(11) 0.044(10) -0.014(9) -0.039(10) C9 0.127(15) 0.082(12) 0.046(9) 0.032(9) -0.032(10) -0.027(11) C10 0.077(12) 0.064(10) 0.041(8) -0.005(7) 0.003(8) -0.018(9) C11 0.091(13) 0.066(10) 0.034(8) 0.009(7) -0.019(8) -0.012(9) C12 0.120(15) 0.064(10) 0.059(10) 0.022(8) -0.023(10) -0.037(11) C13 0.106(13) 0.060(9) 0.064(10) 0.002(8) 0.021(9) -0.014(9) C14 0.095(13) 0.064(10) 0.051(9) 0.012(7) -0.006(9) -0.035(10) C15 0.097(13) 0.056(9) 0.027(7) 0.000(6) -0.008(8) -0.019(9) C16 0.107(13) 0.038(8) 0.034(8) -0.005(6) -0.024(8) -0.009(9) C17 0.070(10) 0.045(8) 0.053(9) 0.013(7) 0.000(7) -0.005(8) C18 0.072(11) 0.083(11) 0.087(12) 0.031(10) -0.014(9) -0.025(10) C19 0.088(12) 0.060(9) 0.121(14) 0.035(10) -0.056(11) -0.031(9) C20 0.054(10) 0.107(13) 0.060(10) -0.003(9) -0.019(8) -0.009(9) C21 0.077(11) 0.088(11) 0.057(9) 0.023(8) -0.022(8) -0.027(9) C22 0.083(11) 0.059(9) 0.045(8) -0.001(7) -0.011(8) -0.014(8) C23 0.078(11) 0.061(9) 0.042(8) 0.011(7) 0.001(7) -0.013(8) C24 0.109(13) 0.068(10) 0.049(9) 0.006(8) -0.006(9) -0.033(10) C25 0.100(13) 0.069(10) 0.054(9) 0.003(8) -0.039(9) -0.034(9) C26 0.082(12) 0.076(11) 0.096(13) 0.012(9) -0.035(10) -0.036(10) C27 0.077(11) 0.057(9) 0.037(8) 0.000(7) -0.010(7) 0.002(8) C28 0.093(13) 0.105(13) 0.065(11) 0.004(9) -0.017(9) -0.047(11) C29 0.133(17) 0.106(13) 0.059(11) 0.033(10) -0.004(11) -0.054(13) C30 0.108(14) 0.091(12) 0.068(11) 0.016(9) -0.030(10) -0.032(11) C31 0.086(11) 0.048(8) 0.052(9) 0.013(7) -0.019(8) -0.018(8) C32 0.120(13) 0.076(10) 0.037(8) 0.007(7) -0.030(8) -0.047(10) C33 0.085(11) 0.056(9) 0.049(9) 0.018(7) -0.011(8) -0.017(9) C34 0.100(13) 0.089(11) 0.051(9) 0.010(8) 0.007(9) -0.040(11) C35 0.108(14) 0.138(16) 0.060(11) -0.004(10) -0.019(10) -0.061(13) C36 0.134(17) 0.147(17) 0.113(16) 0.033(14) -0.035(13) -0.091(16) C37 0.098(14) 0.104(13) 0.080(13) 0.025(10) -0.023(10) -0.033(11) C38 0.075(11) 0.076(10) 0.062(10) 0.004(8) -0.015(8) -0.029(9) C39 0.093(12) 0.051(9) 0.052(9) 0.005(7) 0.011(8) -0.013(9) C40 0.145(16) 0.081(11) 0.054(10) 0.027(8) -0.024(10) -0.058(11) C41 0.111(13) 0.077(10) 0.034(8) -0.001(7) 0.012(8) -0.041(10) C42 0.075(10) 0.073(9) 0.027(7) 0.001(6) -0.012(7) -0.025(9) C43 0.107(13) 0.047(8) 0.032(7) 0.011(6) -0.023(8) -0.023(8) C44 0.071(10) 0.050(8) 0.054(9) 0.006(7) -0.019(8) -0.022(8) C45 0.065(10) 0.080(10) 0.060(9) 0.011(8) -0.019(8) -0.018(9) C46 0.103(13) 0.062(10) 0.064(10) 0.026(8) -0.004(9) -0.037(10) C47 0.109(14) 0.058(9) 0.050(9) 0.014(7) -0.016(9) -0.041(10) C48 0.085(12) 0.058(9) 0.043(8) -0.011(7) 0.000(8) -0.031(9) C49 0.067(10) 0.077(10) 0.065(10) 0.011(8) -0.036(8) -0.017(9) C50 0.095(12) 0.045(8) 0.070(10) 0.013(7) -0.026(9) -0.015(8) C51 0.104(13) 0.064(10) 0.080(11) -0.002(9) -0.022(10) -0.033(10) C52 0.088(11) 0.067(9) 0.046(8) 0.012(7) -0.028(8) -0.036(9) C53 0.095(12) 0.048(9) 0.054(9) 0.005(7) -0.025(8) -0.014(8) C54 0.078(11) 0.049(8) 0.065(9) 0.014(7) -0.011(8) -0.035(8) C55 0.089(12) 0.067(10) 0.062(10) 0.001(8) -0.019(8) -0.032(9) C56 0.107(14) 0.090(12) 0.068(11) 0.023(10) -0.042(11) -0.034(11) C57 0.099(14) 0.093(13) 0.084(13) 0.027(11) -0.043(11) -0.042(12) C58 0.079(12) 0.087(12) 0.061(10) 0.038(9) -0.023(9) -0.031(10) C59 0.069(11) 0.065(10) 0.063(10) 0.019(8) 0.002(8) 0.002(8) C60 0.123(15) 0.064(11) 0.066(11) 0.024(9) -0.004(10) -0.008(10) C61 0.143(16) 0.067(11) 0.049(10) 0.002(8) -0.024(10) -0.023(11) C62 0.119(15) 0.065(11) 0.052(10) -0.011(8) -0.017(9) -0.003(10) C63 0.077(11) 0.061(10) 0.076(11) -0.001(9) -0.013(9) -0.011(9) C64 0.074(11) 0.039(8) 0.069(10) 0.004(7) -0.001(8) 0.008(8) C65 0.15(2) 0.15(2) 0.053(12) 0.013(12) -0.010(12) -0.053(17) C66 0.18(2) 0.110(15) 0.071(13) -0.002(11) -0.039(13) -0.038(15) C67 0.35(4) 0.125(19) 0.13(2) 0.035(15) -0.05(2) -0.13(2) C68 0.19(3) 0.15(2) 0.11(2) -0.032(16) 0.014(18) -0.10(2) C69 0.20(3) 0.14(2) 0.12(2) 0.027(17) -0.027(18) -0.038(19) C70 0.10(2) 0.32(4) 0.24(4) -0.06(3) 0.10(2) -0.04(2) C71 0.15(3) 0.22(3) 0.21(3) -0.05(2) -0.07(2) -0.05(2) C72 0.221(16) 0.226(16) 0.219(16) 0.016(10) -0.018(10) -0.054(10) C73 0.18(3) 0.23(3) 0.20(3) -0.03(2) -0.05(2) -0.11(2) N1 0.076(9) 0.051(7) 0.058(8) 0.026(6) -0.022(7) -0.019(7) N2 0.099(10) 0.058(8) 0.043(7) 0.013(6) -0.009(7) -0.023(8) N3 0.095(9) 0.054(7) 0.034(6) 0.015(5) -0.010(6) -0.024(7) N4 0.089(9) 0.045(6) 0.046(7) 0.007(5) -0.005(6) -0.027(7) N5 0.087(10) 0.084(9) 0.064(8) 0.025(7) -0.037(7) -0.031(8) N6 0.117(12) 0.054(8) 0.069(9) 0.018(7) -0.032(8) -0.032(8) N7 0.109(11) 0.077(8) 0.044(7) 0.005(6) -0.011(7) -0.038(8) N8 0.105(10) 0.051(7) 0.038(6) 0.001(5) -0.012(6) -0.020(7) N9 0.110(12) 0.085(10) 0.076(10) 0.020(8) -0.022(9) -0.022(9) N10 0.19(2) 0.135(15) 0.092(13) 0.022(11) -0.020(13) -0.084(16) N11 0.14(2) 0.21(2) 0.21(3) 0.04(2) -0.059(18) -0.018(18) O1 0.096(8) 0.088(7) 0.074(7) 0.042(6) -0.019(6) -0.019(7) O2 0.067(7) 0.053(6) 0.057(6) 0.020(5) -0.014(5) 0.004(5) O3 0.084(8) 0.061(6) 0.060(6) 0.023(5) -0.025(6) -0.015(6) O4 0.076(7) 0.064(6) 0.050(6) 0.015(5) -0.004(5) -0.018(5) O5 0.091(7) 0.069(6) 0.055(6) 0.012(5) -0.026(5) -0.043(6) O6 0.105(8) 0.093(7) 0.041(6) 0.010(5) -0.006(5) -0.038(7) O7 0.092(8) 0.065(6) 0.041(5) 0.018(4) -0.010(5) -0.042(6) O8 0.090(7) 0.066(6) 0.061(6) 0.031(5) -0.020(5) -0.027(6) O9 0.086(7) 0.055(6) 0.058(6) 0.014(5) -0.029(5) -0.022(5) O10 0.102(8) 0.054(5) 0.049(6) 0.010(4) -0.029(5) -0.034(6) O11 0.075(7) 0.042(5) 0.083(7) 0.021(5) -0.018(5) -0.021(5) O12 0.104(8) 0.066(6) 0.084(7) 0.030(6) -0.038(6) -0.031(6) O13 0.120(9) 0.056(6) 0.054(6) 0.024(5) -0.020(6) -0.034(6) O14 0.082(7) 0.070(6) 0.055(6) 0.017(5) -0.017(5) -0.028(6) O15 0.100(8) 0.051(6) 0.063(6) -0.002(5) -0.029(6) -0.004(6) O16 0.107(8) 0.057(6) 0.074(7) 0.012(5) -0.035(6) -0.014(6) O17 0.154(12) 0.108(10) 0.100(10) 0.006(8) -0.030(9) -0.033(9) O18 0.31(3) 0.174(18) 0.101(13) 0.000(12) 0.008(13) -0.112(19) O19 0.21(2) 0.27(3) 0.27(3) 0.01(2) -0.060(19) -0.094(19) O1W 0.088(7) 0.064(6) 0.051(6) -0.015(5) 0.006(5) -0.019(6) O2W 0.127(10) 0.080(7) 0.080(8) 0.012(6) -0.026(7) -0.029(7) O3W 0.101(8) 0.065(6) 0.099(8) 0.007(6) -0.032(7) -0.023(6) O4W 0.211(14) 0.101(9) 0.107(10) 0.017(7) -0.063(9) -0.078(10) O5W 0.130(10) 0.089(8) 0.086(8) 0.019(6) -0.014(7) -0.028(7) O6W 0.182(15) 0.213(16) 0.129(13) -0.007(12) -0.069(11) -0.056(13) O7W 0.22(2) 0.30(3) 0.23(2) 0.08(2) -0.057(17) -0.07(2) O8W 0.354(16) 0.319(16) 0.325(16) -0.073(10) -0.038(10) -0.070(10) _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 O3 1.904(9) . ? Cu1 N2 1.905(12) . ? Cu1 O2 1.905(9) . ? Cu1 N1 1.931(11) . ? Cu1 O3W 2.371(9) . ? Cu2 O8 1.851(9) . ? Cu2 O1 1.867(11) . ? Cu2 O2 1.965(8) . ? Cu2 O7 1.972(7) . ? Cu2 Cu5 3.025(3) . ? Cu3 N6 1.903(13) . ? Cu3 O15 1.913(9) . ? Cu3 N5 1.938(12) . ? Cu3 O9 1.938(9) . ? Cu4 O10 1.895(7) . ? Cu4 O13 1.909(7) . ? Cu4 O9 1.925(8) . ? Cu4 O14 1.941(8) . ? Cu4 Cu7 3.021(3) . ? Cu5 O6 1.874(9) . ? Cu5 O4 1.914(9) . ? Cu5 O5 1.922(8) . ? Cu5 O3 1.944(8) . ? Cu6 N3 1.916(10) . ? Cu6 O5 1.930(8) . ? Cu6 N4 1.933(9) . ? Cu6 O7 1.936(7) . ? Cu7 O12 1.882(8) . ? Cu7 O16 1.901(9) . ? Cu7 O11 1.906(8) . ? Cu7 O15 1.941(8) . ? Cu8 O14 1.919(8) . ? Cu8 N7 1.921(12) . ? Cu8 N8 1.937(10) . ? Cu8 O11 1.950(9) . ? C1 O2 1.326(17) . ? C1 C6 1.397(18) . ? C1 C2 1.44(2) . ? C2 O1 1.361(17) . ? C2 C3 1.39(2) . ? C3 C4 1.40(2) . ? C3 H3A 0.9300 . ? C4 C5 1.36(2) . ? C4 H4A 0.9300 . ? C5 C6 1.39(2) . ? C5 H5A 0.9300 . ? C6 C7 1.465(19) . ? C7 N1 1.270(17) . ? C7 H7A 0.9300 . ? C8 N1 1.484(16) . ? C8 C9 1.50(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.491(15) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.243(16) . ? C10 C11 1.468(18) . ? C10 H10A 0.9300 . ? C11 C12 1.39(2) . ? C11 C16 1.441(18) . ? C12 C13 1.382(18) . ? C12 H12A 0.9300 . ? C13 C14 1.415(17) . ? C13 H13A 0.9300 . ? C14 C15 1.394(19) . ? C14 C17 1.484(17) . ? C15 O4 1.370(15) . ? C15 C16 1.452(17) . ? C16 O3 1.350(16) . ? C17 C18 1.368(17) . ? C17 C22 1.431(16) . ? C18 C19 1.330(17) . ? C18 H18A 0.9300 . ? C19 C20 1.424(18) . ? C19 H19A 0.9300 . ? C20 O12 1.347(15) . ? C20 C21 1.366(17) . ? C21 O11 1.405(14) . ? C21 C22 1.423(16) . ? C22 C23 1.448(17) . ? C23 N8 1.277(14) . ? C23 H23A 0.9300 . ? C24 N8 1.490(16) . ? C24 C25 1.507(19) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N7 1.502(14) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N7 1.257(16) . ? C26 C27 1.438(17) . ? C26 H26A 0.9300 . ? C27 C32 1.409(17) . ? C27 C28 1.438(17) . ? C28 C29 1.345(18) . ? C28 H28A 0.9300 . ? C29 C30 1.372(19) . ? C29 H29A 0.9300 . ? C30 C31 1.381(18) . ? C30 H30A 0.9300 . ? C31 O13 1.350(14) . ? C31 C32 1.362(16) . ? C32 O14 1.348(14) . ? C33 O5 1.350(14) . ? C33 C38 1.414(16) . ? C33 C34 1.435(17) . ? C34 O6 1.343(14) . ? C34 C35 1.362(18) . ? C35 C36 1.42(2) . ? C35 H35A 0.9300 . ? C36 C37 1.40(2) . ? C36 H36A 0.9300 . ? C37 C38 1.394(18) . ? C37 H37A 0.9300 . ? C38 C39 1.434(17) . ? C39 N4 1.251(15) . ? C39 H39A 0.9300 . ? C40 N4 1.478(14) . ? C40 C41 1.517(18) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 N3 1.512(14) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 N3 1.273(14) . ? C42 C43 1.465(16) . ? C42 H42A 0.9300 . ? C43 C44 1.395(17) . ? C43 C48 1.407(16) . ? C44 C45 1.384(16) . ? C44 C49 1.490(16) . ? C45 C46 1.425(17) . ? C45 H45A 0.9300 . ? C46 C47 1.350(18) . ? C46 H46A 0.9300 . ? C47 O8 1.359(15) . ? C47 C48 1.385(16) . ? C48 O7 1.347(14) . ? C49 C50 1.396(16) . ? C49 C54 1.449(17) . ? C50 C51 1.408(17) . ? C50 H50A 0.9300 . ? C51 C52 1.414(17) . ? C51 H51A 0.9300 . ? C52 C53 1.410(16) . ? C52 C55 1.428(17) . ? C53 O9 1.345(14) . ? C53 C54 1.386(16) . ? C54 O10 1.319(13) . ? C55 N5 1.301(17) . ? C55 H55A 0.9300 . ? C56 N5 1.485(16) . ? C56 C57 1.54(2) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 N6 1.462(16) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 N6 1.258(18) . ? C58 C59 1.469(19) . ? C58 H58A 0.9300 . ? C59 C64 1.411(17) . ? C59 C60 1.48(2) . ? C60 C61 1.310(19) . ? C60 H60A 0.9300 . ? C61 C62 1.371(19) . ? C61 H61A 0.9300 . ? C62 C63 1.374(19) . ? C62 H62A 0.9300 . ? C63 O16 1.326(15) . ? C63 C64 1.418(18) . ? C64 O15 1.343(15) . ? C65 O17 1.245(18) . ? C65 N9 1.33(2) . ? C65 H65A 0.9300 . ? C66 N9 1.433(17) . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 N9 1.354(18) . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 O18 1.27(3) . ? C68 N10 1.39(2) . ? C68 H68A 0.9300 . ? C69 N10 1.48(2) . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 N10 1.46(3) . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 O19 1.272(9) . ? C71 N11 1.397(7) . ? C71 H71A 0.9300 . ? C72 N11 1.470(8) . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C73 N11 1.474(8) . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cu1 N2 91.9(5) . . ? O3 Cu1 O2 91.4(4) . . ? N2 Cu1 O2 158.1(4) . . ? O3 Cu1 N1 176.1(5) . . ? N2 Cu1 N1 85.2(5) . . ? O2 Cu1 N1 92.2(5) . . ? O3 Cu1 O3W 85.8(4) . . ? N2 Cu1 O3W 101.0(4) . . ? O2 Cu1 O3W 100.8(4) . . ? N1 Cu1 O3W 92.1(4) . . ? O8 Cu2 O1 157.3(5) . . ? O8 Cu2 O2 98.8(4) . . ? O1 Cu2 O2 85.8(4) . . ? O8 Cu2 O7 85.3(3) . . ? O1 Cu2 O7 96.6(4) . . ? O2 Cu2 O7 163.5(4) . . ? O8 Cu2 Cu5 96.2(3) . . ? O1 Cu2 Cu5 106.5(3) . . ? O2 Cu2 Cu5 81.8(3) . . ? O7 Cu2 Cu5 81.9(3) . . ? N6 Cu3 O15 92.2(5) . . ? N6 Cu3 N5 85.1(5) . . ? O15 Cu3 N5 165.6(5) . . ? N6 Cu3 O9 172.8(5) . . ? O15 Cu3 O9 93.0(4) . . ? N5 Cu3 O9 91.2(5) . . ? O10 Cu4 O13 152.0(4) . . ? O10 Cu4 O9 85.6(3) . . ? O13 Cu4 O9 98.6(4) . . ? O10 Cu4 O14 100.0(3) . . ? O13 Cu4 O14 84.1(4) . . ? O9 Cu4 O14 163.0(4) . . ? O10 Cu4 Cu7 97.1(3) . . ? O13 Cu4 Cu7 110.9(3) . . ? O9 Cu4 Cu7 80.9(3) . . ? O14 Cu4 Cu7 82.5(3) . . ? O6 Cu5 O4 152.8(4) . . ? O6 Cu5 O5 84.6(3) . . ? O4 Cu5 O5 99.9(3) . . ? O6 Cu5 O3 97.8(4) . . ? O4 Cu5 O3 86.3(4) . . ? O5 Cu5 O3 161.9(4) . . ? O6 Cu5 Cu2 113.4(3) . . ? O4 Cu5 Cu2 93.8(3) . . ? O5 Cu5 Cu2 82.3(3) . . ? O3 Cu5 Cu2 80.3(3) . . ? N3 Cu6 O5 167.6(5) . . ? N3 Cu6 N4 85.6(4) . . ? O5 Cu6 N4 93.5(4) . . ? N3 Cu6 O7 88.3(4) . . ? O5 Cu6 O7 94.0(3) . . ? N4 Cu6 O7 170.3(4) . . ? O12 Cu7 O16 159.2(5) . . ? O12 Cu7 O11 86.3(3) . . ? O16 Cu7 O11 97.1(4) . . ? O12 Cu7 O15 97.7(4) . . ? O16 Cu7 O15 84.8(4) . . ? O11 Cu7 O15 163.4(4) . . ? O12 Cu7 Cu4 93.1(4) . . ? O16 Cu7 Cu4 107.7(3) . . ? O11 Cu7 Cu4 81.3(3) . . ? O15 Cu7 Cu4 82.4(3) . . ? O14 Cu8 N7 93.4(4) . . ? O14 Cu8 N8 169.4(4) . . ? N7 Cu8 N8 85.6(5) . . ? O14 Cu8 O11 93.2(4) . . ? N7 Cu8 O11 168.7(5) . . ? N8 Cu8 O11 89.6(4) . . ? O2 C1 C6 126.8(14) . . ? O2 C1 C2 117.3(13) . . ? C6 C1 C2 115.7(16) . . ? O1 C2 C3 124.2(14) . . ? O1 C2 C1 114.3(16) . . ? C3 C2 C1 121.5(15) . . ? C2 C3 C4 119.8(18) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C5 C4 C3 119.4(19) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? C4 C5 C6 121.8(15) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C5 C6 C1 121.6(15) . . ? C5 C6 C7 115.9(14) . . ? C1 C6 C7 122.4(16) . . ? N1 C7 C6 121.2(14) . . ? N1 C7 H7A 119.4 . . ? C6 C7 H7A 119.4 . . ? N1 C8 C9 110.1(11) . . ? N1 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? N1 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.2 . . ? N2 C9 C8 106.5(12) . . ? N2 C9 H9A 110.4 . . ? C8 C9 H9A 110.4 . . ? N2 C9 H9B 110.4 . . ? C8 C9 H9B 110.4 . . ? H9A C9 H9B 108.6 . . ? N2 C10 C11 124.4(14) . . ? N2 C10 H10A 117.8 . . ? C11 C10 H10A 117.8 . . ? C12 C11 C16 118.6(12) . . ? C12 C11 C10 121.4(13) . . ? C16 C11 C10 120.0(15) . . ? C13 C12 C11 122.6(14) . . ? C13 C12 H12A 118.7 . . ? C11 C12 H12A 118.7 . . ? C12 C13 C14 120.6(16) . . ? C12 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C15 C14 C13 119.0(13) . . ? C15 C14 C17 120.0(12) . . ? C13 C14 C17 120.9(15) . . ? O4 C15 C14 124.6(11) . . ? O4 C15 C16 114.5(14) . . ? C14 C15 C16 120.9(13) . . ? O3 C16 C11 124.4(12) . . ? O3 C16 C15 117.3(13) . . ? C11 C16 C15 118.3(15) . . ? C18 C17 C22 118.4(11) . . ? C18 C17 C14 120.7(11) . . ? C22 C17 C14 120.8(12) . . ? C19 C18 C17 124.3(13) . . ? C19 C18 H18A 117.9 . . ? C17 C18 H18A 117.9 . . ? C18 C19 C20 119.9(13) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? O12 C20 C21 116.0(13) . . ? O12 C20 C19 126.3(12) . . ? C21 C20 C19 117.5(13) . . ? C20 C21 O11 116.8(12) . . ? C20 C21 C22 123.1(13) . . ? O11 C21 C22 120.1(11) . . ? C21 C22 C17 116.7(12) . . ? C21 C22 C23 124.1(11) . . ? C17 C22 C23 119.2(11) . . ? N8 C23 C22 122.2(11) . . ? N8 C23 H23A 118.9 . . ? C22 C23 H23A 118.9 . . ? N8 C24 C25 106.5(11) . . ? N8 C24 H24A 110.4 . . ? C25 C24 H24A 110.4 . . ? N8 C24 H24B 110.4 . . ? C25 C24 H24B 110.4 . . ? H24A C24 H24B 108.6 . . ? N7 C25 C24 107.1(12) . . ? N7 C25 H25A 110.3 . . ? C24 C25 H25A 110.3 . . ? N7 C25 H25B 110.3 . . ? C24 C25 H25B 110.3 . . ? H25A C25 H25B 108.6 . . ? N7 C26 C27 126.3(13) . . ? N7 C26 H26A 116.8 . . ? C27 C26 H26A 116.8 . . ? C32 C27 C26 123.8(12) . . ? C32 C27 C28 116.1(11) . . ? C26 C27 C28 120.1(13) . . ? C29 C28 C27 119.9(13) . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.1 . . ? C28 C29 C30 122.6(15) . . ? C28 C29 H29A 118.7 . . ? C30 C29 H29A 118.7 . . ? C29 C30 C31 119.2(14) . . ? C29 C30 H30A 120.4 . . ? C31 C30 H30A 120.4 . . ? O13 C31 C32 117.7(12) . . ? O13 C31 C30 122.2(12) . . ? C32 C31 C30 120.0(13) . . ? O14 C32 C31 115.9(12) . . ? O14 C32 C27 121.9(11) . . ? C31 C32 C27 122.2(13) . . ? O5 C33 C38 124.3(11) . . ? O5 C33 C34 115.2(11) . . ? C38 C33 C34 120.3(13) . . ? O6 C34 C35 124.5(14) . . ? O6 C34 C33 113.9(13) . . ? C35 C34 C33 121.5(13) . . ? C34 C35 C36 118.6(15) . . ? C34 C35 H35A 120.7 . . ? C36 C35 H35A 120.7 . . ? C37 C36 C35 119.9(15) . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C38 C37 C36 122.7(14) . . ? C38 C37 H37A 118.6 . . ? C36 C37 H37A 118.6 . . ? C37 C38 C33 116.8(13) . . ? C37 C38 C39 117.9(13) . . ? C33 C38 C39 125.0(12) . . ? N4 C39 C38 122.9(12) . . ? N4 C39 H39A 118.6 . . ? C38 C39 H39A 118.6 . . ? N4 C40 C41 107.4(10) . . ? N4 C40 H40A 110.2 . . ? C41 C40 H40A 110.2 . . ? N4 C40 H40B 110.2 . . ? C41 C40 H40B 110.2 . . ? H40A C40 H40B 108.5 . . ? N3 C41 C40 104.8(10) . . ? N3 C41 H41A 110.8 . . ? C40 C41 H41A 110.8 . . ? N3 C41 H41B 110.8 . . ? C40 C41 H41B 110.8 . . ? H41A C41 H41B 108.9 . . ? N3 C42 C43 122.8(11) . . ? N3 C42 H42A 118.6 . . ? C43 C42 H42A 118.6 . . ? C44 C43 C48 119.4(12) . . ? C44 C43 C42 120.4(11) . . ? C48 C43 C42 120.2(13) . . ? C45 C44 C43 117.5(11) . . ? C45 C44 C49 120.8(13) . . ? C43 C44 C49 121.4(11) . . ? C44 C45 C46 121.6(13) . . ? C44 C45 H45A 119.2 . . ? C46 C45 H45A 119.2 . . ? C47 C46 C45 120.9(12) . . ? C47 C46 H46A 119.6 . . ? C45 C46 H46A 119.6 . . ? C46 C47 O8 123.5(11) . . ? C46 C47 C48 117.7(13) . . ? O8 C47 C48 118.7(14) . . ? O7 C48 C47 114.1(12) . . ? O7 C48 C43 123.1(11) . . ? C47 C48 C43 122.8(14) . . ? C50 C49 C54 119.5(11) . . ? C50 C49 C44 120.0(12) . . ? C54 C49 C44 120.3(11) . . ? C49 C50 C51 121.3(12) . . ? C49 C50 H50A 119.4 . . ? C51 C50 H50A 119.4 . . ? C50 C51 C52 119.9(12) . . ? C50 C51 H51A 120.0 . . ? C52 C51 H51A 120.0 . . ? C53 C52 C51 118.1(12) . . ? C53 C52 C55 125.2(12) . . ? C51 C52 C55 116.7(12) . . ? O9 C53 C54 113.8(11) . . ? O9 C53 C52 122.7(11) . . ? C54 C53 C52 123.4(12) . . ? O10 C54 C53 120.3(11) . . ? O10 C54 C49 122.1(11) . . ? C53 C54 C49 117.6(11) . . ? N5 C55 C52 121.3(13) . . ? N5 C55 H55A 119.3 . . ? C52 C55 H55A 119.3 . . ? N5 C56 C57 107.8(13) . . ? N5 C56 H56A 110.2 . . ? C57 C56 H56A 110.2 . . ? N5 C56 H56B 110.2 . . ? C57 C56 H56B 110.2 . . ? H56A C56 H56B 108.5 . . ? N6 C57 C56 105.6(14) . . ? N6 C57 H57A 110.6 . . ? C56 C57 H57A 110.6 . . ? N6 C57 H57B 110.6 . . ? C56 C57 H57B 110.6 . . ? H57A C57 H57B 108.7 . . ? N6 C58 C59 125.4(14) . . ? N6 C58 H58A 117.3 . . ? C59 C58 H58A 117.3 . . ? C64 C59 C58 120.0(14) . . ? C64 C59 C60 117.2(14) . . ? C58 C59 C60 122.7(13) . . ? C61 C60 C59 121.4(15) . . ? C61 C60 H60A 119.3 . . ? C59 C60 H60A 119.3 . . ? C60 C61 C62 119.6(15) . . ? C60 C61 H61A 120.2 . . ? C62 C61 H61A 120.2 . . ? C61 C62 C63 124.1(15) . . ? C61 C62 H62A 118.0 . . ? C63 C62 H62A 118.0 . . ? O16 C63 C62 125.4(14) . . ? O16 C63 C64 116.7(13) . . ? C62 C63 C64 117.9(14) . . ? O15 C64 C59 124.9(14) . . ? O15 C64 C63 115.5(12) . . ? C59 C64 C63 119.5(14) . . ? O17 C65 N9 123.7(18) . . ? O17 C65 H65A 118.2 . . ? N9 C65 H65A 118.2 . . ? N9 C66 H66A 109.5 . . ? N9 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N9 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N9 C67 H67A 109.5 . . ? N9 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? N9 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? O18 C68 N10 122(3) . . ? O18 C68 H68A 118.9 . . ? N10 C68 H68A 118.9 . . ? N10 C69 H69A 109.5 . . ? N10 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? N10 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N10 C70 H70A 109.5 . . ? N10 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? N10 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O19 C71 N11 120.2(7) . . ? O19 C71 H71A 119.9 . . ? N11 C71 H71A 119.9 . . ? N11 C72 H72A 109.5 . . ? N11 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? N11 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N11 C73 H73A 109.5 . . ? N11 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? N11 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C7 N1 C8 121.7(12) . . ? C7 N1 Cu1 125.7(10) . . ? C8 N1 Cu1 112.3(11) . . ? C10 N2 C9 119.9(13) . . ? C10 N2 Cu1 126.7(10) . . ? C9 N2 Cu1 112.9(11) . . ? C42 N3 C41 124.0(10) . . ? C42 N3 Cu6 124.8(8) . . ? C41 N3 Cu6 110.3(8) . . ? C39 N4 C40 121.8(10) . . ? C39 N4 Cu6 126.6(9) . . ? C40 N4 Cu6 111.5(8) . . ? C55 N5 C56 123.0(12) . . ? C55 N5 Cu3 125.8(9) . . ? C56 N5 Cu3 110.8(10) . . ? C58 N6 C57 119.8(14) . . ? C58 N6 Cu3 125.5(10) . . ? C57 N6 Cu3 114.7(11) . . ? C26 N7 C25 123.2(12) . . ? C26 N7 Cu8 125.0(10) . . ? C25 N7 Cu8 111.8(8) . . ? C23 N8 C24 124.8(10) . . ? C23 N8 Cu8 123.6(9) . . ? C24 N8 Cu8 110.5(8) . . ? C65 N9 C67 121.5(16) . . ? C65 N9 C66 120.8(14) . . ? C67 N9 C66 117.7(16) . . ? C68 N10 C70 118(2) . . ? C68 N10 C69 119(2) . . ? C70 N10 C69 123(2) . . ? C71 N11 C72 122.3(6) . . ? C71 N11 C73 121.4(8) . . ? C72 N11 C73 115.6(7) . . ? C2 O1 Cu2 111.6(9) . . ? C1 O2 Cu1 117.3(8) . . ? C1 O2 Cu2 108.4(8) . . ? Cu1 O2 Cu2 131.0(5) . . ? C16 O3 Cu1 120.0(7) . . ? C16 O3 Cu5 108.8(7) . . ? Cu1 O3 Cu5 128.3(6) . . ? C15 O4 Cu5 110.3(8) . . ? C33 O5 Cu5 110.6(7) . . ? C33 O5 Cu6 120.5(8) . . ? Cu5 O5 Cu6 128.4(4) . . ? C34 O6 Cu5 112.7(8) . . ? C48 O7 Cu6 118.0(8) . . ? C48 O7 Cu2 109.8(7) . . ? Cu6 O7 Cu2 125.6(4) . . ? C47 O8 Cu2 111.1(8) . . ? C53 O9 Cu4 109.5(8) . . ? C53 O9 Cu3 119.5(8) . . ? Cu4 O9 Cu3 127.8(5) . . ? C54 O10 Cu4 108.1(7) . . ? C21 O11 Cu7 107.8(7) . . ? C21 O11 Cu8 116.4(8) . . ? Cu7 O11 Cu8 128.7(4) . . ? C20 O12 Cu7 111.6(8) . . ? C31 O13 Cu4 109.2(7) . . ? C32 O14 Cu8 124.3(7) . . ? C32 O14 Cu4 109.2(7) . . ? Cu8 O14 Cu4 126.4(4) . . ? C64 O15 Cu3 120.9(8) . . ? C64 O15 Cu7 109.5(8) . . ? Cu3 O15 Cu7 128.0(5) . . ? C63 O16 Cu7 110.9(8) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.992 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.122 data_2 _database_code_depnum_ccdc_archive 'CCDC 869204' #TrackingRef 'web_deposit_cif_file_0_Hui-ZhongKou_1330685378.kou-sub.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H79 Cu4 Fe4 N11 O27' _chemical_formula_weight 2020.03 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' Fe Fe 0.3463 0.8444 '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 Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 29.714(3) _cell_length_b 29.714(3) _cell_length_c 16.2570(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12431(2) _cell_formula_units_Z 6 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 38274 _cell_measurement_theta_min 3.0150 _cell_measurement_theta_max 27.4978 _exptl_crystal_description Block _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6180 _exptl_absorpt_coefficient_mu 1.770 _exptl_absorpt_correction_type DTABSCOR _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7562 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_decay_% 0 _diffrn_reflns_number 91201 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 26.00 _reflns_number_total 16261 _reflns_number_gt 15213 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.0638P)^2^+88.8868P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16261 _refine_ls_number_parameters 1076 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0871 _refine_ls_wR_factor_ref 0.1983 _refine_ls_wR_factor_gt 0.1938 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.008 _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 0.08336(4) 0.47245(4) 0.51563(5) 0.0417(2) Uani 1 1 d . . . Cu2 Cu -0.09968(3) 0.25490(4) 0.46613(5) 0.0356(2) Uani 1 1 d . . . Cu3 Cu 0.06198(4) 0.23133(4) 0.16147(5) 0.0382(2) Uani 1 1 d . . . Cu4 Cu 0.14727(4) 0.45635(4) 0.09266(5) 0.0422(2) Uani 1 1 d . . . Fe1 Fe -0.01996(4) 0.23729(4) 0.31612(6) 0.0312(2) Uani 1 1 d . . . Fe2 Fe 0.11654(4) 0.47614(4) 0.29986(5) 0.0312(2) Uani 1 1 d . . . Fe3 Fe 0.02603(4) 0.36015(4) 0.38702(5) 0.0276(2) Uani 1 1 d . . . Fe4 Fe 0.07384(4) 0.35238(4) 0.23570(5) 0.0281(2) Uani 1 1 d . . . C1 C 0.1861(3) 0.5225(3) 0.4365(5) 0.0411(17) Uani 1 1 d . . . C2 C 0.2162(3) 0.5325(3) 0.3643(5) 0.0448(18) Uani 1 1 d . . . C3 C 0.2706(4) 0.5623(3) 0.3683(7) 0.063(2) Uani 1 1 d . . . H3A H 0.2900 0.5691 0.3204 0.075 Uiso 1 1 calc R . . C4 C 0.2955(4) 0.5817(4) 0.4422(7) 0.073(3) Uani 1 1 d . . . H4A H 0.3315 0.6010 0.4441 0.088 Uiso 1 1 calc R . . C5 C 0.2673(4) 0.5725(4) 0.5123(7) 0.074(3) Uani 1 1 d . . . H5A H 0.2847 0.5860 0.5617 0.089 Uiso 1 1 calc R . . C6 C 0.2120(4) 0.5429(3) 0.5126(5) 0.054(2) Uani 1 1 d . . . C7 C 0.1854(5) 0.5350(4) 0.5888(6) 0.067(3) Uani 1 1 d . . . H7A H 0.2055 0.5514 0.6350 0.080 Uiso 1 1 calc R . . C8 C 0.1142(5) 0.5030(4) 0.6816(5) 0.077(3) Uani 1 1 d . . . H8A H 0.1273 0.4986 0.7311 0.092 Uiso 1 1 calc R . . C9 C 0.0658(5) 0.5072(3) 0.6698(6) 0.076(3) Uani 1 1 d . . . H9A H 0.0438 0.4945 0.7183 0.091 Uiso 1 1 calc R . . H9B H 0.0752 0.5432 0.6612 0.091 Uiso 1 1 calc R . . C10 C -0.0429(4) 0.4289(3) 0.5213(5) 0.051(2) Uani 1 1 d . . . C11 C -0.0101(5) 0.4613(3) 0.5871(5) 0.062(3) Uani 1 1 d . . . H11A H -0.0253 0.4727 0.6257 0.074 Uiso 1 1 calc R . . C12 C -0.0959(4) 0.4138(4) 0.5211(6) 0.065(3) Uani 1 1 d . . . H12A H -0.1088 0.4261 0.5621 0.078 Uiso 1 1 calc R . . C13 C -0.1287(4) 0.3816(5) 0.4623(7) 0.072(3) Uani 1 1 d . . . H13A H -0.1634 0.3728 0.4632 0.086 Uiso 1 1 calc R . . C14 C -0.1105(3) 0.3610(4) 0.3990(5) 0.056(2) Uani 1 1 d . . . H14A H -0.1333 0.3381 0.3598 0.067 Uiso 1 1 calc R . . C15 C -0.0576(3) 0.3760(3) 0.3974(4) 0.0442(18) Uani 1 1 d . . . C16 C -0.0231(3) 0.4119(3) 0.4573(4) 0.0427(18) Uani 1 1 d . . . C17 C -0.1095(3) 0.1991(3) 0.2230(4) 0.0380(16) Uani 1 1 d . . . C18 C -0.1442(3) 0.1774(3) 0.1583(5) 0.0458(18) Uani 1 1 d . . . H18A H -0.1336 0.1685 0.1101 0.055 Uiso 1 1 calc R . . C19 C -0.1946(3) 0.1686(4) 0.1644(6) 0.063(2) Uani 1 1 d . . . H19A H -0.2178 0.1533 0.1210 0.075 Uiso 1 1 calc R . . C20 C -0.2101(3) 0.1826(3) 0.2346(6) 0.054(2) Uani 1 1 d . . . H20A H -0.2435 0.1777 0.2376 0.065 Uiso 1 1 calc R . . C21 C -0.1762(3) 0.2044(3) 0.3025(5) 0.0421(17) Uani 1 1 d . . . C22 C -0.1255(3) 0.2127(3) 0.2964(4) 0.0375(15) Uani 1 1 d . . . C23 C -0.2016(4) 0.2320(6) 0.5169(7) 0.099(5) Uani 1 1 d . . . H23A H -0.2339 0.2297 0.5136 0.118 Uiso 1 1 calc R . . C24 C -0.1750(4) 0.2397(6) 0.5876(7) 0.095(4) Uani 1 1 d . . . H24A H -0.1849 0.2062 0.6122 0.114 Uiso 1 1 calc R . . H24B H -0.1844 0.2587 0.6256 0.114 Uiso 1 1 calc R . . C25 C -0.1970(3) 0.2134(3) 0.3764(5) 0.0484(19) Uani 1 1 d . . . H25A H -0.2305 0.2084 0.3735 0.058 Uiso 1 1 calc R . . C26 C -0.0858(3) 0.2927(3) 0.6341(4) 0.0434(18) Uani 1 1 d . . . H26A H -0.0998 0.2937 0.6847 0.052 Uiso 1 1 calc R . . C27 C -0.0301(3) 0.3180(3) 0.6278(4) 0.0337(14) Uani 1 1 d . . . C28 C -0.0007(3) 0.3380(3) 0.7007(4) 0.0391(16) Uani 1 1 d . . . H28A H -0.0177 0.3342 0.7504 0.047 Uiso 1 1 calc R . . C29 C 0.0526(3) 0.3630(3) 0.6991(4) 0.0445(18) Uani 1 1 d . . . H29A H 0.0714 0.3742 0.7479 0.053 Uiso 1 1 calc R . . C30 C 0.0785(3) 0.3717(3) 0.6241(4) 0.0371(15) Uani 1 1 d . . . H30A H 0.1147 0.3894 0.6233 0.045 Uiso 1 1 calc R . . C31 C 0.0513(3) 0.3543(2) 0.5504(4) 0.0290(13) Uani 1 1 d . . . C32 C -0.0042(3) 0.3246(2) 0.5526(4) 0.0304(13) Uani 1 1 d . . . C33 C 0.0314(3) 0.1783(3) 0.3215(4) 0.0361(15) Uani 1 1 d . . . C34 C 0.0000(3) 0.1658(3) 0.3927(5) 0.0413(16) Uani 1 1 d . . . C35 C -0.0054(3) 0.1273(4) 0.4448(6) 0.057(2) Uani 1 1 d . . . H35A H -0.0263 0.1194 0.4912 0.068 Uiso 1 1 calc R . . C36 C 0.0204(4) 0.1001(4) 0.4289(6) 0.070(3) Uani 1 1 d . . . H36A H 0.0167 0.0741 0.4647 0.084 Uiso 1 1 calc R . . C37 C 0.0513(3) 0.1115(4) 0.3606(6) 0.057(2) Uani 1 1 d . . . H37A H 0.0686 0.0932 0.3506 0.069 Uiso 1 1 calc R . . C38 C 0.0572(3) 0.1509(3) 0.3050(5) 0.0424(17) Uani 1 1 d . . . C39 C 0.0877(3) 0.1581(3) 0.2318(5) 0.0441(18) Uani 1 1 d . . . H39A H 0.1041 0.1385 0.2274 0.053 Uiso 1 1 calc R . . C40 C 0.1224(4) 0.1896(4) 0.0993(6) 0.060(2) Uani 1 1 d . . . H40A H 0.1269 0.1595 0.0978 0.072 Uiso 1 1 calc R . . H40B H 0.1564 0.2207 0.0980 0.072 Uiso 1 1 calc R . . C41 C 0.0900(5) 0.1890(4) 0.0276(5) 0.070(3) Uani 1 1 d . . . H41A H 0.1100 0.1972 -0.0230 0.084 Uiso 1 1 calc R . . H41B H 0.0594 0.1549 0.0219 0.084 Uiso 1 1 calc R . . C42 C 0.0644(3) 0.2504(3) -0.0140(5) 0.053(2) Uani 1 1 d . . . H42A H 0.0672 0.2410 -0.0675 0.064 Uiso 1 1 calc R . . C43 C 0.0487(3) 0.2882(3) -0.0040(4) 0.0423(17) Uani 1 1 d . . . C44 C 0.0385(3) 0.3087(4) -0.0749(4) 0.051(2) Uani 1 1 d . . . H44A H 0.0404 0.2962 -0.1265 0.061 Uiso 1 1 calc R . . C45 C 0.0257(3) 0.3470(4) -0.0688(4) 0.054(2) Uani 1 1 d . . . H45A H 0.0180 0.3595 -0.1160 0.065 Uiso 1 1 calc R . . C46 C 0.0241(3) 0.3673(4) 0.0078(4) 0.0475(19) Uani 1 1 d . . . H46A H 0.0161 0.3938 0.0112 0.057 Uiso 1 1 calc R . . C47 C 0.0344(3) 0.3484(3) 0.0786(4) 0.0394(16) Uani 1 1 d . . . C48 C 0.0456(3) 0.3074(3) 0.0735(4) 0.0369(15) Uani 1 1 d . . . C49 C 0.0938(3) 0.5115(3) 0.1497(4) 0.0397(16) Uani 1 1 d . . . C50 C 0.0767(3) 0.5300(3) 0.2157(4) 0.0350(15) Uani 1 1 d . . . C51 C 0.0548(4) 0.5608(3) 0.2018(5) 0.050(2) Uani 1 1 d . . . H51A H 0.0445 0.5736 0.2458 0.060 Uiso 1 1 calc R . . C52 C 0.0482(4) 0.5728(4) 0.1211(5) 0.066(3) Uani 1 1 d . . . H52A H 0.0323 0.5925 0.1115 0.079 Uiso 1 1 calc R . . C53 C 0.0651(4) 0.5555(4) 0.0557(5) 0.068(3) Uani 1 1 d . . . H53A H 0.0609 0.5640 0.0023 0.081 Uiso 1 1 calc R . . C54 C 0.0885(4) 0.5252(3) 0.0687(4) 0.050(2) Uani 1 1 d . . . C55 C 0.2041(4) 0.4804(4) -0.0563(5) 0.064(3) Uani 1 1 d . . . H55A H 0.2162 0.4678 -0.1015 0.077 Uiso 1 1 calc R . . H55B H 0.2310 0.5156 -0.0432 0.077 Uiso 1 1 calc R . . C56 C 0.1546(4) 0.4792(4) -0.0793(5) 0.066(3) Uani 1 1 d . . . H56A H 0.1614 0.5063 -0.1188 0.079 Uiso 1 1 calc R . . H56B H 0.1301 0.4459 -0.1032 0.079 Uiso 1 1 calc R . . C57 C 0.1089(4) 0.5129(4) -0.0024(5) 0.059(2) Uani 1 1 d . . . H57A H 0.1038 0.5241 -0.0532 0.071 Uiso 1 1 calc R . . C58 C 0.2146(3) 0.4198(3) 0.0261(5) 0.052(2) Uani 1 1 d . . . H58A H 0.2376 0.4217 -0.0145 0.063 Uiso 1 1 calc R . . C59 C 0.2069(3) 0.3869(3) 0.0960(4) 0.0403(16) Uani 1 1 d . . . C60 C 0.2350(3) 0.3599(3) 0.0988(5) 0.0485(19) Uani 1 1 d . . . H60A H 0.2583 0.3645 0.0570 0.058 Uiso 1 1 calc R . . C61 C 0.2278(3) 0.3267(3) 0.1635(5) 0.0467(18) Uani 1 1 d . . . H61A H 0.2473 0.3101 0.1661 0.056 Uiso 1 1 calc R . . C62 C 0.1915(3) 0.3179(3) 0.2250(4) 0.0402(16) Uani 1 1 d . . . H62A H 0.1865 0.2951 0.2677 0.048 Uiso 1 1 calc R . . C63 C 0.1626(2) 0.3431(3) 0.2228(4) 0.0299(13) Uani 1 1 d . . . C64 C 0.1709(3) 0.3792(3) 0.1588(4) 0.0339(14) Uani 1 1 d . . . C100 C 0.2176(4) 0.2095(4) 0.2997(7) 0.071(3) Uani 1 1 d . . . H10A H 0.1993 0.2050 0.2491 0.106 Uiso 1 1 calc R . . H10B H 0.2531 0.2367 0.2934 0.106 Uiso 1 1 calc R . . H10C H 0.2015 0.2185 0.3427 0.106 Uiso 1 1 calc R . . C101 C 0.2398(4) 0.1596(4) 0.3969(5) 0.064(2) Uani 1 1 d . . . H10D H 0.2353 0.1255 0.4038 0.096 Uiso 1 1 calc R . . H10E H 0.2236 0.1670 0.4419 0.096 Uiso 1 1 calc R . . H10F H 0.2763 0.1848 0.3960 0.096 Uiso 1 1 calc R . . C102 C 0.1960(4) 0.1218(4) 0.2688(5) 0.056(2) Uani 1 1 d . . . H10N H 0.1973 0.0924 0.2850 0.067 Uiso 1 1 calc R . . C103 C -0.0902(4) 0.3195(3) 0.1595(6) 0.058(2) Uani 1 1 d . . . H10G H -0.1252 0.2913 0.1536 0.087 Uiso 1 1 calc R . . H10H H -0.0753 0.3147 0.2088 0.087 Uiso 1 1 calc R . . H10I H -0.0700 0.3203 0.1129 0.087 Uiso 1 1 calc R . . C104 C -0.0415(3) 0.4155(3) 0.1747(5) 0.053(2) Uani 1 1 d . . . H10J H -0.0475 0.4444 0.1770 0.079 Uiso 1 1 calc R . . H10K H -0.0191 0.4199 0.1291 0.079 Uiso 1 1 calc R . . H10L H -0.0253 0.4139 0.2249 0.079 Uiso 1 1 calc R . . C105 C -0.1338(4) 0.3691(4) 0.1660(6) 0.066(2) Uiso 1 1 d . . . H10M H -0.1645 0.3374 0.1619 0.079 Uiso 1 1 calc R . . C106 C 0.3545(19) 0.5214(15) 0.3038(18) 0.48(4) Uani 1 1 d DU . . H10O H 0.3830 0.5506 0.3305 0.727 Uiso 1 1 calc R . . H10P H 0.3615 0.4932 0.3013 0.727 Uiso 1 1 calc R . . H10Q H 0.3232 0.5109 0.3344 0.727 Uiso 1 1 calc R . . C107 C 0.3786(9) 0.5841(8) 0.1929(15) 0.192(10) Uani 1 1 d DU . . H107 H 0.3990 0.6102 0.2302 0.230 Uiso 1 1 calc R . . C108 C 0.3162(11) 0.4940(9) 0.1708(18) 0.276(16) Uani 1 1 d DU . . H10R H 0.3122 0.5066 0.1185 0.414 Uiso 1 1 calc R . . H10S H 0.2828 0.4741 0.1964 0.414 Uiso 1 1 calc R . . H10T H 0.3314 0.4724 0.1628 0.414 Uiso 1 1 calc R . . N1 N 0.1364(4) 0.5073(3) 0.5990(4) 0.0543(19) Uani 1 1 d . . . N2 N 0.0379(4) 0.4757(3) 0.5973(4) 0.0552(19) Uani 1 1 d . . . N3 N -0.1738(2) 0.2277(3) 0.4459(4) 0.0505(17) Uani 1 1 d . . . N4 N -0.1174(2) 0.2689(3) 0.5753(4) 0.0482(16) Uani 1 1 d . . . N5 N 0.0751(3) 0.2284(3) 0.0447(4) 0.0557(18) Uani 1 1 d . . . N6 N 0.0941(3) 0.1888(3) 0.1732(4) 0.0462(15) Uani 1 1 d . . . N7 N 0.1336(3) 0.4878(3) -0.0013(4) 0.0547(18) Uani 1 1 d . . . N8 N 0.1923(3) 0.4466(3) 0.0157(4) 0.0516(17) Uani 1 1 d . . . N100 N 0.2163(3) 0.1619(2) 0.3205(4) 0.0443(15) Uani 1 1 d . . . N101 N -0.0903(3) 0.3680(3) 0.1645(4) 0.0509(16) Uani 1 1 d . . . N102 N 0.3485(11) 0.5360(9) 0.2211(16) 0.300(14) Uani 1 1 d DU . . O1 O 0.13438(19) 0.49376(18) 0.4267(3) 0.0366(11) Uani 1 1 d . . . O2 O 0.0268(2) 0.42432(19) 0.4488(3) 0.0363(11) Uani 1 1 d . . . O3 O 0.1913(2) 0.5124(2) 0.2940(3) 0.0473(13) Uani 1 1 d . . . O4 O -0.0376(2) 0.3573(2) 0.3445(3) 0.0409(12) Uani 1 1 d . . . O5 O -0.02654(17) 0.30833(18) 0.4792(3) 0.0310(10) Uani 1 1 d . . . O6 O -0.08888(17) 0.23356(18) 0.3557(3) 0.0353(10) Uani 1 1 d . . . O7 O 0.07374(17) 0.36426(17) 0.4766(2) 0.0288(9) Uani 1 1 d . . . O8 O -0.06133(19) 0.2073(2) 0.2201(3) 0.0408(11) Uani 1 1 d . . . O9 O 0.03285(18) 0.21589(18) 0.2730(3) 0.0342(10) Uani 1 1 d . . . O10 O 0.05449(18) 0.29193(18) 0.1463(3) 0.0343(10) Uani 1 1 d . . . O11 O -0.02554(19) 0.19234(19) 0.4049(3) 0.0399(11) Uani 1 1 d . . . O12 O 0.0356(2) 0.3679(2) 0.1528(3) 0.0387(11) Uani 1 1 d . . . O13 O 0.1152(2) 0.48263(19) 0.1707(3) 0.0381(11) Uani 1 1 d . . . O14 O 0.14193(18) 0.40181(18) 0.1637(3) 0.0327(10) Uani 1 1 d . . . O15 O 0.0833(2) 0.51692(19) 0.2923(3) 0.0377(11) Uani 1 1 d . . . O16 O 0.12505(17) 0.33394(18) 0.2764(3) 0.0321(10) Uani 1 1 d . . . O17 O 0.02222(16) 0.30697(17) 0.3158(2) 0.0287(9) Uani 1 1 d . . . O18 O 0.08031(18) 0.40622(17) 0.3103(2) 0.0300(9) Uani 1 1 d . . . O100 O 0.1755(3) 0.1195(3) 0.2014(4) 0.0705(19) Uani 1 1 d . . . O101 O -0.1380(3) 0.4087(3) 0.1723(5) 0.085(2) Uani 1 1 d . . . O102 O 0.3807(7) 0.5961(10) 0.1171(11) 0.303(14) Uani 1 1 d D . . O1W O -0.0278(3) 0.1559(4) 0.1242(5) 0.096(3) Uani 1 1 d . . . O2W O 0.2308(3) 0.5284(3) 0.1405(5) 0.100(3) Uani 1 1 d . . . O3W O -0.08862(19) 0.1920(2) 0.5286(3) 0.0410(11) Uani 1 1 d . . . O4W O 0.1091(2) 0.2930(2) 0.4307(3) 0.0455(13) Uani 1 1 d . . . O5W O 0.2537(8) 0.5385(8) 0.7572(8) 0.236(9) Uani 1 1 d . . . O6W O 0.2350(17) 0.6510(17) -0.287(3) 0.263(18) Uani 0.50 1 d PU . . O7W O 0.0683(11) 0.0989(11) -0.1367(18) 0.170(10) Uani 0.50 1 d PU . . 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 0.0705(6) 0.0420(5) 0.0244(4) -0.0008(3) 0.0040(4) 0.0371(5) Cu2 0.0294(4) 0.0487(5) 0.0309(4) -0.0001(4) 0.0020(3) 0.0210(4) Cu3 0.0470(5) 0.0437(5) 0.0297(4) -0.0079(4) 0.0026(4) 0.0270(4) Cu4 0.0648(6) 0.0497(5) 0.0250(4) 0.0094(4) 0.0144(4) 0.0384(5) Fe1 0.0324(5) 0.0358(5) 0.0258(5) -0.0038(4) -0.0007(4) 0.0173(4) Fe2 0.0417(5) 0.0351(5) 0.0244(4) 0.0025(4) 0.0034(4) 0.0250(4) Fe3 0.0357(5) 0.0363(5) 0.0182(4) -0.0002(3) 0.0010(3) 0.0235(4) Fe4 0.0360(5) 0.0370(5) 0.0177(4) -0.0015(3) 0.0002(3) 0.0231(4) C1 0.056(5) 0.032(4) 0.048(4) -0.006(3) -0.010(3) 0.032(4) C2 0.050(4) 0.037(4) 0.053(5) -0.002(3) -0.002(4) 0.026(4) C3 0.056(5) 0.048(5) 0.083(7) -0.014(5) -0.005(5) 0.025(4) C4 0.057(6) 0.063(6) 0.092(8) -0.028(6) -0.020(6) 0.024(5) C5 0.081(7) 0.050(5) 0.087(8) -0.037(5) -0.034(6) 0.030(5) C6 0.072(6) 0.040(4) 0.055(5) -0.016(4) -0.013(4) 0.032(4) C7 0.105(9) 0.043(5) 0.050(5) -0.023(4) -0.020(5) 0.035(6) C8 0.136(10) 0.060(6) 0.023(4) -0.006(4) 0.002(5) 0.041(6) C9 0.116(9) 0.034(4) 0.052(5) -0.011(4) 0.035(6) 0.019(5) C10 0.079(6) 0.057(5) 0.045(4) 0.018(4) 0.028(4) 0.056(5) C11 0.130(9) 0.058(5) 0.031(4) 0.011(4) 0.034(5) 0.071(6) C12 0.085(7) 0.089(7) 0.058(6) 0.031(5) 0.034(5) 0.072(6) C13 0.069(6) 0.101(8) 0.083(7) 0.046(6) 0.034(6) 0.072(7) C14 0.054(5) 0.082(6) 0.054(5) 0.022(4) 0.014(4) 0.051(5) C15 0.057(5) 0.068(5) 0.031(4) 0.012(3) 0.011(3) 0.050(4) C16 0.068(5) 0.055(5) 0.030(4) 0.013(3) 0.010(3) 0.049(4) C17 0.041(4) 0.029(3) 0.034(4) -0.004(3) -0.004(3) 0.009(3) C18 0.043(4) 0.050(4) 0.039(4) -0.006(3) -0.014(3) 0.019(4) C19 0.051(5) 0.063(6) 0.058(6) -0.013(4) -0.029(4) 0.017(4) C20 0.032(4) 0.054(5) 0.063(5) -0.002(4) -0.015(4) 0.011(4) C21 0.032(4) 0.044(4) 0.044(4) 0.005(3) -0.001(3) 0.014(3) C22 0.038(4) 0.033(4) 0.037(4) 0.001(3) -0.009(3) 0.014(3) C23 0.038(5) 0.177(13) 0.079(7) -0.056(8) 0.000(5) 0.053(7) C24 0.048(6) 0.175(13) 0.059(6) 0.013(7) 0.022(5) 0.053(7) C25 0.031(4) 0.047(4) 0.067(5) 0.000(4) -0.002(4) 0.020(3) C26 0.049(4) 0.065(5) 0.023(3) 0.003(3) 0.011(3) 0.033(4) C27 0.042(4) 0.041(4) 0.024(3) 0.002(3) 0.003(3) 0.026(3) C28 0.053(4) 0.046(4) 0.022(3) 0.001(3) 0.004(3) 0.027(4) C29 0.059(5) 0.055(5) 0.020(3) 0.000(3) -0.006(3) 0.028(4) C30 0.043(4) 0.043(4) 0.026(3) 0.000(3) -0.005(3) 0.022(3) C31 0.042(4) 0.031(3) 0.021(3) -0.001(2) 0.000(3) 0.023(3) C32 0.041(4) 0.033(3) 0.023(3) 0.000(2) -0.001(3) 0.023(3) C33 0.031(3) 0.041(4) 0.036(4) -0.002(3) -0.005(3) 0.018(3) C34 0.039(4) 0.047(4) 0.042(4) 0.002(3) -0.002(3) 0.025(3) C35 0.057(5) 0.065(6) 0.062(5) 0.025(4) 0.009(4) 0.040(5) C36 0.069(6) 0.086(7) 0.076(7) 0.034(6) 0.018(5) 0.055(6) C37 0.058(5) 0.066(6) 0.071(6) 0.005(5) -0.001(4) 0.048(5) C38 0.035(4) 0.038(4) 0.054(5) -0.005(3) -0.007(3) 0.018(3) C39 0.042(4) 0.046(4) 0.052(5) -0.013(4) -0.001(3) 0.027(4) C40 0.073(6) 0.066(6) 0.060(5) -0.003(4) 0.017(5) 0.048(5) C41 0.106(8) 0.083(7) 0.042(5) -0.012(5) 0.016(5) 0.063(7) C42 0.062(5) 0.059(5) 0.034(4) -0.013(4) 0.009(4) 0.027(4) C43 0.042(4) 0.056(5) 0.025(3) -0.010(3) 0.001(3) 0.021(4) C44 0.052(5) 0.076(6) 0.019(3) -0.007(3) -0.002(3) 0.027(4) C45 0.059(5) 0.091(7) 0.021(3) -0.005(4) -0.013(3) 0.043(5) C46 0.059(5) 0.076(6) 0.025(3) 0.001(3) -0.006(3) 0.046(5) C47 0.044(4) 0.059(5) 0.019(3) -0.004(3) -0.003(3) 0.029(4) C48 0.033(4) 0.050(4) 0.022(3) -0.005(3) -0.001(3) 0.016(3) C49 0.056(5) 0.039(4) 0.030(3) 0.006(3) 0.004(3) 0.028(4) C50 0.045(4) 0.036(4) 0.033(3) 0.008(3) 0.005(3) 0.026(3) C51 0.076(6) 0.061(5) 0.035(4) 0.006(4) 0.004(4) 0.050(5) C52 0.095(7) 0.093(7) 0.048(5) 0.014(5) 0.004(5) 0.076(7) C53 0.111(8) 0.096(7) 0.038(4) 0.013(5) 0.003(5) 0.083(7) C54 0.079(6) 0.063(5) 0.028(4) 0.009(3) 0.003(4) 0.052(5) C55 0.102(8) 0.069(6) 0.035(4) 0.019(4) 0.031(5) 0.053(6) C56 0.110(8) 0.082(7) 0.027(4) 0.010(4) 0.020(4) 0.063(6) C57 0.095(7) 0.071(6) 0.029(4) 0.016(4) 0.010(4) 0.054(6) C58 0.062(5) 0.062(5) 0.041(4) 0.006(4) 0.019(4) 0.037(5) C59 0.049(4) 0.044(4) 0.033(4) 0.005(3) 0.013(3) 0.027(4) C60 0.047(4) 0.060(5) 0.047(4) 0.004(4) 0.020(4) 0.033(4) C61 0.046(4) 0.056(5) 0.049(4) -0.004(4) 0.002(3) 0.033(4) C62 0.041(4) 0.051(4) 0.036(4) 0.001(3) 0.004(3) 0.028(4) C63 0.029(3) 0.034(3) 0.026(3) -0.002(3) -0.002(2) 0.015(3) C64 0.033(3) 0.048(4) 0.028(3) -0.002(3) 0.002(3) 0.025(3) C100 0.076(7) 0.048(5) 0.077(7) 0.006(5) -0.013(5) 0.022(5) C101 0.076(6) 0.062(6) 0.048(5) 0.001(4) -0.016(5) 0.030(5) C102 0.066(6) 0.062(5) 0.053(5) -0.009(4) -0.011(4) 0.043(5) C103 0.066(6) 0.049(5) 0.060(5) -0.010(4) -0.015(4) 0.029(4) C104 0.069(6) 0.052(5) 0.041(4) -0.005(4) -0.006(4) 0.033(4) C106 0.49(4) 0.49(4) 0.49(4) 0.001(10) 0.001(10) 0.25(2) C107 0.183(13) 0.191(13) 0.210(14) 0.007(9) -0.002(9) 0.100(9) C108 0.273(18) 0.275(18) 0.287(18) -0.022(10) -0.008(10) 0.142(11) N1 0.102(6) 0.039(4) 0.027(3) -0.008(3) -0.001(4) 0.039(4) N2 0.095(6) 0.036(4) 0.039(4) 0.005(3) 0.023(4) 0.037(4) N3 0.030(3) 0.063(4) 0.058(4) -0.012(3) -0.002(3) 0.023(3) N4 0.038(3) 0.073(5) 0.035(3) 0.004(3) 0.009(3) 0.028(3) N5 0.079(5) 0.058(4) 0.041(4) -0.011(3) 0.011(3) 0.043(4) N6 0.049(4) 0.055(4) 0.042(4) -0.005(3) 0.006(3) 0.031(3) N7 0.086(5) 0.065(5) 0.028(3) 0.007(3) 0.013(3) 0.049(4) N8 0.074(5) 0.060(4) 0.031(3) 0.014(3) 0.020(3) 0.041(4) N100 0.052(4) 0.047(4) 0.034(3) 0.002(3) -0.004(3) 0.024(3) N101 0.061(4) 0.053(4) 0.046(4) 0.006(3) -0.002(3) 0.034(4) N102 0.292(16) 0.311(17) 0.313(17) 0.000(10) 0.002(10) 0.163(11) O1 0.047(3) 0.037(3) 0.033(2) -0.003(2) -0.002(2) 0.026(2) O2 0.055(3) 0.045(3) 0.024(2) 0.0032(19) 0.005(2) 0.037(3) O3 0.043(3) 0.056(3) 0.044(3) 0.001(2) 0.004(2) 0.025(3) O4 0.050(3) 0.062(3) 0.027(2) 0.005(2) -0.001(2) 0.041(3) O5 0.033(2) 0.041(3) 0.022(2) 0.0013(18) 0.0009(18) 0.021(2) O6 0.030(2) 0.042(3) 0.032(2) -0.003(2) -0.0029(19) 0.017(2) O7 0.034(2) 0.039(2) 0.019(2) 0.0015(17) 0.0010(17) 0.022(2) O8 0.040(3) 0.047(3) 0.034(3) -0.010(2) -0.006(2) 0.022(2) O9 0.038(3) 0.039(3) 0.032(2) -0.0033(19) -0.0013(19) 0.023(2) O10 0.044(3) 0.042(3) 0.020(2) -0.0052(19) -0.0017(19) 0.024(2) O11 0.038(3) 0.047(3) 0.037(3) 0.005(2) 0.006(2) 0.023(2) O12 0.052(3) 0.057(3) 0.019(2) -0.004(2) -0.005(2) 0.036(3) O13 0.062(3) 0.045(3) 0.025(2) 0.005(2) 0.008(2) 0.039(3) O14 0.041(3) 0.042(3) 0.025(2) 0.0023(19) 0.0073(19) 0.028(2) O15 0.058(3) 0.044(3) 0.025(2) 0.004(2) 0.004(2) 0.036(3) O16 0.036(2) 0.040(3) 0.024(2) 0.0027(18) 0.0041(18) 0.021(2) O17 0.029(2) 0.036(2) 0.021(2) -0.0037(17) 0.0011(17) 0.017(2) O18 0.041(3) 0.034(2) 0.023(2) 0.0016(18) 0.0036(18) 0.025(2) O100 0.087(5) 0.100(5) 0.053(4) -0.021(3) -0.024(3) 0.068(4) O101 0.098(6) 0.085(5) 0.095(6) -0.011(4) 0.000(4) 0.063(5) O102 0.238(19) 0.65(5) 0.183(16) -0.09(2) -0.070(14) 0.34(3) O1W 0.079(5) 0.141(7) 0.082(5) -0.080(5) -0.035(4) 0.066(5) O2W 0.084(5) 0.100(6) 0.087(6) -0.017(5) 0.029(4) 0.025(5) O3W 0.041(3) 0.045(3) 0.038(3) 0.001(2) 0.000(2) 0.022(2) O4W 0.057(3) 0.065(3) 0.030(3) 0.009(2) 0.002(2) 0.042(3) O5W 0.30(2) 0.38(3) 0.101(9) 0.065(13) -0.003(11) 0.22(2) O6W 0.26(2) 0.27(2) 0.26(2) -0.018(10) 0.008(10) 0.134(12) O7W 0.173(13) 0.185(13) 0.173(13) -0.005(9) -0.003(9) 0.105(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.910(5) . ? Cu1 N2 1.932(7) . ? Cu1 N1 1.940(8) . ? Cu1 O1 1.957(5) . ? Cu2 N4 1.955(6) . ? Cu2 N3 1.957(6) . ? Cu2 O5 1.959(5) . ? Cu2 O6 1.983(5) . ? Cu2 O3W 2.292(5) . ? Cu3 N6 1.936(7) . ? Cu3 O10 1.937(5) . ? Cu3 N5 1.948(7) . ? Cu3 O9 1.963(5) . ? Cu4 O14 1.931(4) . ? Cu4 N7 1.937(7) . ? Cu4 N8 1.957(6) . ? Cu4 O13 1.967(4) . ? Fe1 O17 1.806(4) . ? Fe1 O8 1.909(5) . ? Fe1 O11 1.917(5) . ? Fe1 O9 2.087(5) . ? Fe1 O6 2.096(5) . ? Fe2 O18 1.808(4) . ? Fe2 O15 1.912(5) . ? Fe2 O3 1.927(5) . ? Fe2 O13 2.111(4) . ? Fe2 O1 2.129(5) . ? Fe3 O17 1.916(4) . ? Fe3 O18 1.956(4) . ? Fe3 O4 1.974(5) . ? Fe3 O7 1.994(4) . ? Fe3 O2 2.145(5) . ? Fe3 O5 2.157(4) . ? Fe3 Fe4 2.9072(12) . ? Fe4 O18 1.939(4) . ? Fe4 O17 1.949(4) . ? Fe4 O12 1.962(5) . ? Fe4 O16 1.971(5) . ? Fe4 O10 2.153(4) . ? Fe4 O14 2.156(5) . ? C1 O1 1.343(9) . ? C1 C2 1.415(11) . ? C1 C6 1.421(11) . ? C2 O3 1.331(9) . ? C2 C3 1.401(12) . ? C3 C4 1.376(13) . ? C3 H3A 0.9300 . ? C4 C5 1.360(15) . ? C4 H4A 0.9300 . ? C5 C6 1.425(14) . ? C5 H5A 0.9300 . ? C6 C7 1.424(13) . ? C7 N1 1.276(13) . ? C7 H7A 0.9300 . ? C8 N1 1.473(11) . ? C8 C9 1.519(16) . ? C8 H8A 0.9300 . ? C9 N2 1.476(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C12 1.403(13) . ? C10 C16 1.410(10) . ? C10 C11 1.442(14) . ? C11 N2 1.277(13) . ? C11 H11A 0.9300 . ? C12 C13 1.358(15) . ? C12 H12A 0.9300 . ? C13 C14 1.435(13) . ? C13 H13A 0.9300 . ? C14 C15 1.404(11) . ? C14 H14A 0.9300 . ? C15 O4 1.317(8) . ? C15 C16 1.429(12) . ? C16 O2 1.344(9) . ? C17 O8 1.326(9) . ? C17 C18 1.386(9) . ? C17 C22 1.416(10) . ? C18 C19 1.390(12) . ? C18 H18A 0.9300 . ? C19 C20 1.370(13) . ? C19 H19A 0.9300 . ? C20 C21 1.416(10) . ? C20 H20A 0.9300 . ? C21 C22 1.403(10) . ? C21 C25 1.437(11) . ? C22 O6 1.349(8) . ? C23 C24 1.348(14) . ? C23 N3 1.461(11) . ? C23 H23A 0.9300 . ? C24 N4 1.493(11) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N3 1.280(10) . ? C25 H25A 0.9300 . ? C26 N4 1.277(10) . ? C26 C27 1.439(10) . ? C26 H26A 0.9300 . ? C27 C32 1.405(9) . ? C27 C28 1.416(9) . ? C28 C29 1.372(11) . ? C28 H28A 0.9300 . ? C29 C30 1.397(10) . ? C29 H29A 0.9300 . ? C30 C31 1.392(9) . ? C30 H30A 0.9300 . ? C31 O7 1.332(7) . ? C31 C32 1.430(9) . ? C32 O5 1.332(7) . ? C33 O9 1.349(8) . ? C33 C38 1.396(10) . ? C33 C34 1.415(10) . ? C34 O11 1.355(9) . ? C34 C35 1.366(11) . ? C35 C36 1.387(12) . ? C35 H35A 0.9300 . ? C36 C37 1.372(13) . ? C36 H36A 0.9300 . ? C37 C38 1.419(11) . ? C37 H37A 0.9300 . ? C38 C39 1.446(11) . ? C39 N6 1.265(10) . ? C39 H39A 0.9300 . ? C40 N6 1.460(10) . ? C40 C41 1.506(13) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 N5 1.471(11) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 N5 1.285(11) . ? C42 C43 1.425(11) . ? C42 H42A 0.9300 . ? C43 C48 1.404(9) . ? C43 C44 1.407(11) . ? C44 C45 1.372(12) . ? C44 H44A 0.9300 . ? C45 C46 1.394(10) . ? C45 H45A 0.9300 . ? C46 C47 1.381(10) . ? C46 H46A 0.9300 . ? C47 O12 1.332(8) . ? C47 C48 1.418(10) . ? C48 O10 1.343(8) . ? C49 O13 1.342(8) . ? C49 C54 1.410(9) . ? C49 C50 1.412(10) . ? C50 O15 1.348(8) . ? C50 C51 1.379(10) . ? C51 C52 1.398(11) . ? C51 H51A 0.9300 . ? C52 C53 1.380(12) . ? C52 H52A 0.9300 . ? C53 C54 1.402(11) . ? C53 H53A 0.9300 . ? C54 C57 1.434(11) . ? C55 N8 1.466(10) . ? C55 C56 1.501(14) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 N7 1.492(10) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 N7 1.283(11) . ? C57 H57A 0.9300 . ? C58 N8 1.275(10) . ? C58 C59 1.442(10) . ? C58 H58A 0.9300 . ? C59 C64 1.412(9) . ? C59 C60 1.418(10) . ? C60 C61 1.383(11) . ? C60 H60A 0.9300 . ? C61 C62 1.398(10) . ? C61 H61A 0.9300 . ? C62 C63 1.390(9) . ? C62 H62A 0.9300 . ? C63 O16 1.333(8) . ? C63 C64 1.426(9) . ? C64 O14 1.334(8) . ? C100 N100 1.435(11) . ? C100 H10A 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? C101 N100 1.444(10) . ? C101 H10D 0.9600 . ? C101 H10E 0.9600 . ? C101 H10F 0.9600 . ? C102 O100 1.238(10) . ? C102 N100 1.330(10) . ? C102 H10N 0.9300 . ? C103 N101 1.446(10) . ? C103 H10G 0.9600 . ? C103 H10H 0.9600 . ? C103 H10I 0.9600 . ? C104 N101 1.442(11) . ? C104 H10J 0.9600 . ? C104 H10K 0.9600 . ? C104 H10L 0.9600 . ? C105 O101 1.246(11) . ? C105 N101 1.309(12) . ? C105 H10M 0.9300 . ? C106 N102 1.450(17) . ? C106 H10O 0.9600 . ? C106 H10P 0.9600 . ? C106 H10Q 0.9600 . ? C107 O102 1.276(16) . ? C107 N102 1.333(15) . ? C107 H107 0.9300 . ? C108 N102 1.396(17) . ? C108 H10R 0.9600 . ? C108 H10S 0.9600 . ? C108 H10T 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 N2 93.0(3) . . ? O2 Cu1 N1 166.7(2) . . ? N2 Cu1 N1 84.0(4) . . ? O2 Cu1 O1 94.1(2) . . ? N2 Cu1 O1 160.1(2) . . ? N1 Cu1 O1 93.0(3) . . ? N4 Cu2 N3 82.7(3) . . ? N4 Cu2 O5 92.1(2) . . ? N3 Cu2 O5 156.4(3) . . ? N4 Cu2 O6 173.8(2) . . ? N3 Cu2 O6 92.5(2) . . ? O5 Cu2 O6 93.78(18) . . ? N4 Cu2 O3W 86.4(2) . . ? N3 Cu2 O3W 109.2(3) . . ? O5 Cu2 O3W 93.42(18) . . ? O6 Cu2 O3W 91.60(19) . . ? N6 Cu3 O10 160.4(3) . . ? N6 Cu3 N5 83.8(3) . . ? O10 Cu3 N5 92.1(2) . . ? N6 Cu3 O9 93.4(2) . . ? O10 Cu3 O9 95.32(18) . . ? N5 Cu3 O9 164.7(3) . . ? O14 Cu4 N7 158.1(3) . . ? O14 Cu4 N8 91.9(2) . . ? N7 Cu4 N8 83.8(3) . . ? O14 Cu4 O13 95.44(18) . . ? N7 Cu4 O13 93.2(2) . . ? N8 Cu4 O13 166.9(3) . . ? O17 Fe1 O8 116.6(2) . . ? O17 Fe1 O11 124.7(2) . . ? O8 Fe1 O11 118.7(2) . . ? O17 Fe1 O9 98.73(19) . . ? O8 Fe1 O9 89.5(2) . . ? O11 Fe1 O9 81.76(19) . . ? O17 Fe1 O6 99.27(19) . . ? O8 Fe1 O6 80.89(19) . . ? O11 Fe1 O6 89.44(19) . . ? O9 Fe1 O6 161.91(19) . . ? O18 Fe2 O15 122.3(2) . . ? O18 Fe2 O3 120.3(2) . . ? O15 Fe2 O3 117.3(2) . . ? O18 Fe2 O13 99.81(19) . . ? O15 Fe2 O13 80.74(18) . . ? O3 Fe2 O13 88.2(2) . . ? O18 Fe2 O1 97.13(19) . . ? O15 Fe2 O1 92.89(19) . . ? O3 Fe2 O1 80.5(2) . . ? O13 Fe2 O1 162.8(2) . . ? O17 Fe3 O18 83.08(18) . . ? O17 Fe3 O4 95.3(2) . . ? O18 Fe3 O4 104.10(19) . . ? O17 Fe3 O7 103.82(18) . . ? O18 Fe3 O7 96.38(18) . . ? O4 Fe3 O7 153.51(18) . . ? O17 Fe3 O2 170.39(18) . . ? O18 Fe3 O2 92.19(18) . . ? O4 Fe3 O2 77.7(2) . . ? O7 Fe3 O2 84.97(18) . . ? O17 Fe3 O5 96.20(18) . . ? O18 Fe3 O5 173.00(18) . . ? O4 Fe3 O5 82.91(19) . . ? O7 Fe3 O5 77.00(17) . . ? O2 Fe3 O5 89.50(17) . . ? O17 Fe3 Fe4 41.65(13) . . ? O18 Fe3 Fe4 41.48(12) . . ? O4 Fe3 Fe4 101.27(14) . . ? O7 Fe3 Fe4 105.21(12) . . ? O2 Fe3 Fe4 132.72(13) . . ? O5 Fe3 Fe4 137.69(13) . . ? O18 Fe4 O17 82.68(18) . . ? O18 Fe4 O12 93.73(19) . . ? O17 Fe4 O12 105.9(2) . . ? O18 Fe4 O16 104.35(19) . . ? O17 Fe4 O16 91.90(18) . . ? O12 Fe4 O16 156.17(19) . . ? O18 Fe4 O10 170.19(19) . . ? O17 Fe4 O10 94.82(18) . . ? O12 Fe4 O10 77.78(19) . . ? O16 Fe4 O10 85.17(18) . . ? O18 Fe4 O14 96.04(18) . . ? O17 Fe4 O14 168.47(18) . . ? O12 Fe4 O14 85.62(19) . . ? O16 Fe4 O14 77.27(17) . . ? O10 Fe4 O14 88.28(17) . . ? O18 Fe4 Fe3 41.93(13) . . ? O17 Fe4 Fe3 40.80(12) . . ? O12 Fe4 Fe3 101.46(14) . . ? O16 Fe4 Fe3 102.36(13) . . ? O10 Fe4 Fe3 134.44(13) . . ? O14 Fe4 Fe3 137.28(13) . . ? O1 C1 C2 115.9(7) . . ? O1 C1 C6 125.3(8) . . ? C2 C1 C6 118.8(8) . . ? O3 C2 C3 122.0(8) . . ? O3 C2 C1 117.9(7) . . ? C3 C2 C1 120.1(8) . . ? C4 C3 C2 120.9(10) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C5 C4 C3 120.0(10) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 122.0(9) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C1 C6 C7 123.4(9) . . ? C1 C6 C5 118.2(9) . . ? C7 C6 C5 118.5(9) . . ? N1 C7 C6 125.4(8) . . ? N1 C7 H7A 117.3 . . ? C6 C7 H7A 117.3 . . ? N1 C8 C9 106.3(8) . . ? N1 C8 H8A 126.9 . . ? C9 C8 H8A 126.9 . . ? N2 C9 C8 107.6(7) . . ? N2 C9 H9A 110.2 . . ? C8 C9 H9A 110.2 . . ? N2 C9 H9B 110.2 . . ? C8 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C12 C10 C16 119.1(9) . . ? C12 C10 C11 119.5(8) . . ? C16 C10 C11 121.4(8) . . ? N2 C11 C10 126.1(7) . . ? N2 C11 H11A 116.9 . . ? C10 C11 H11A 116.9 . . ? C13 C12 C10 121.6(8) . . ? C13 C12 H12A 119.2 . . ? C10 C12 H12A 119.2 . . ? C12 C13 C14 120.9(9) . . ? C12 C13 H13A 119.5 . . ? C14 C13 H13A 119.5 . . ? C15 C14 C13 118.6(9) . . ? C15 C14 H14A 120.7 . . ? C13 C14 H14A 120.7 . . ? O4 C15 C14 123.2(8) . . ? O4 C15 C16 117.0(7) . . ? C14 C15 C16 119.7(7) . . ? O2 C16 C10 125.4(8) . . ? O2 C16 C15 114.6(6) . . ? C10 C16 C15 119.9(8) . . ? O8 C17 C18 122.9(7) . . ? O8 C17 C22 117.5(6) . . ? C18 C17 C22 119.6(7) . . ? C17 C18 C19 121.0(8) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C20 C19 C18 119.8(7) . . ? C20 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C19 C20 C21 121.2(8) . . ? C19 C20 H20A 119.4 . . ? C21 C20 H20A 119.4 . . ? C22 C21 C20 118.8(7) . . ? C22 C21 C25 123.5(7) . . ? C20 C21 C25 117.6(7) . . ? O6 C22 C21 125.2(7) . . ? O6 C22 C17 115.2(6) . . ? C21 C22 C17 119.6(6) . . ? C24 C23 N3 112.2(8) . . ? C24 C23 H23A 123.9 . . ? N3 C23 H23A 123.9 . . ? C23 C24 N4 112.8(8) . . ? C23 C24 H24A 109.0 . . ? N4 C24 H24A 109.0 . . ? C23 C24 H24B 109.0 . . ? N4 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? N3 C25 C21 126.0(7) . . ? N3 C25 H25A 117.0 . . ? C21 C25 H25A 117.0 . . ? N4 C26 C27 124.9(6) . . ? N4 C26 H26A 117.5 . . ? C27 C26 H26A 117.5 . . ? C32 C27 C28 119.4(6) . . ? C32 C27 C26 122.8(6) . . ? C28 C27 C26 117.9(6) . . ? C29 C28 C27 121.0(6) . . ? C29 C28 H28A 119.5 . . ? C27 C28 H28A 119.5 . . ? C28 C29 C30 119.8(7) . . ? C28 C29 H29A 120.1 . . ? C30 C29 H29A 120.1 . . ? C31 C30 C29 121.2(7) . . ? C31 C30 H30A 119.4 . . ? C29 C30 H30A 119.4 . . ? O7 C31 C30 123.9(6) . . ? O7 C31 C32 117.0(5) . . ? C30 C31 C32 119.0(6) . . ? O5 C32 C27 126.2(6) . . ? O5 C32 C31 114.4(5) . . ? C27 C32 C31 119.3(6) . . ? O9 C33 C38 124.8(6) . . ? O9 C33 C34 116.1(6) . . ? C38 C33 C34 119.1(7) . . ? O11 C34 C35 122.1(7) . . ? O11 C34 C33 117.0(6) . . ? C35 C34 C33 120.9(7) . . ? C34 C35 C36 120.3(8) . . ? C34 C35 H35A 119.9 . . ? C36 C35 H35A 119.9 . . ? C37 C36 C35 120.3(8) . . ? C37 C36 H36A 119.8 . . ? C35 C36 H36A 119.8 . . ? C36 C37 C38 120.6(8) . . ? C36 C37 H37A 119.7 . . ? C38 C37 H37A 119.7 . . ? C33 C38 C37 118.9(7) . . ? C33 C38 C39 123.9(7) . . ? C37 C38 C39 117.1(7) . . ? N6 C39 C38 125.7(7) . . ? N6 C39 H39A 117.1 . . ? C38 C39 H39A 117.1 . . ? N6 C40 C41 106.2(7) . . ? N6 C40 H40A 110.5 . . ? C41 C40 H40A 110.5 . . ? N6 C40 H40B 110.5 . . ? C41 C40 H40B 110.5 . . ? H40A C40 H40B 108.7 . . ? N5 C41 C40 106.7(7) . . ? N5 C41 H41A 110.4 . . ? C40 C41 H41A 110.4 . . ? N5 C41 H41B 110.4 . . ? C40 C41 H41B 110.4 . . ? H41A C41 H41B 108.6 . . ? N5 C42 C43 125.4(7) . . ? N5 C42 H42A 117.3 . . ? C43 C42 H42A 117.3 . . ? C48 C43 C44 119.2(7) . . ? C48 C43 C42 122.4(7) . . ? C44 C43 C42 118.3(7) . . ? C45 C44 C43 120.6(7) . . ? C45 C44 H44A 119.7 . . ? C43 C44 H44A 119.7 . . ? C44 C45 C46 120.5(7) . . ? C44 C45 H45A 119.7 . . ? C46 C45 H45A 119.7 . . ? C47 C46 C45 120.3(8) . . ? C47 C46 H46A 119.8 . . ? C45 C46 H46A 119.8 . . ? O12 C47 C46 122.7(7) . . ? O12 C47 C48 117.4(6) . . ? C46 C47 C48 119.8(6) . . ? O10 C48 C43 126.1(7) . . ? O10 C48 C47 114.4(6) . . ? C43 C48 C47 119.5(7) . . ? O13 C49 C54 125.3(6) . . ? O13 C49 C50 115.8(6) . . ? C54 C49 C50 118.8(7) . . ? O15 C50 C51 121.9(6) . . ? O15 C50 C49 117.1(6) . . ? C51 C50 C49 121.0(6) . . ? C50 C51 C52 119.7(7) . . ? C50 C51 H51A 120.2 . . ? C52 C51 H51A 120.2 . . ? C53 C52 C51 120.3(8) . . ? C53 C52 H52A 119.8 . . ? C51 C52 H52A 119.8 . . ? C52 C53 C54 120.8(8) . . ? C52 C53 H53A 119.6 . . ? C54 C53 H53A 119.6 . . ? C53 C54 C49 119.3(7) . . ? C53 C54 C57 116.7(7) . . ? C49 C54 C57 123.9(7) . . ? N8 C55 C56 106.6(7) . . ? N8 C55 H55A 110.4 . . ? C56 C55 H55A 110.4 . . ? N8 C55 H55B 110.4 . . ? C56 C55 H55B 110.4 . . ? H55A C55 H55B 108.6 . . ? N7 C56 C55 106.0(7) . . ? N7 C56 H56A 110.5 . . ? C55 C56 H56A 110.5 . . ? N7 C56 H56B 110.5 . . ? C55 C56 H56B 110.5 . . ? H56A C56 H56B 108.7 . . ? N7 C57 C54 125.0(7) . . ? N7 C57 H57A 117.5 . . ? C54 C57 H57A 117.5 . . ? N8 C58 C59 124.9(7) . . ? N8 C58 H58A 117.5 . . ? C59 C58 H58A 117.5 . . ? C64 C59 C60 119.9(6) . . ? C64 C59 C58 122.0(7) . . ? C60 C59 C58 118.1(7) . . ? C61 C60 C59 120.3(7) . . ? C61 C60 H60A 119.9 . . ? C59 C60 H60A 119.9 . . ? C60 C61 C62 120.3(7) . . ? C60 C61 H61A 119.8 . . ? C62 C61 H61A 119.8 . . ? C63 C62 C61 120.6(7) . . ? C63 C62 H62A 119.7 . . ? C61 C62 H62A 119.7 . . ? O16 C63 C62 123.5(6) . . ? O16 C63 C64 116.3(6) . . ? C62 C63 C64 120.1(6) . . ? O14 C64 C59 126.2(6) . . ? O14 C64 C63 115.1(5) . . ? C59 C64 C63 118.8(6) . . ? N100 C100 H10A 109.5 . . ? N100 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? N100 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? N100 C101 H10D 109.5 . . ? N100 C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? N100 C101 H10F 109.5 . . ? H10D C101 H10F 109.5 . . ? H10E C101 H10F 109.5 . . ? O100 C102 N100 126.7(9) . . ? O100 C102 H10N 116.6 . . ? N100 C102 H10N 116.6 . . ? N101 C103 H10G 109.5 . . ? N101 C103 H10H 109.5 . . ? H10G C103 H10H 109.5 . . ? N101 C103 H10I 109.5 . . ? H10G C103 H10I 109.5 . . ? H10H C103 H10I 109.5 . . ? N101 C104 H10J 109.5 . . ? N101 C104 H10K 109.5 . . ? H10J C104 H10K 109.5 . . ? N101 C104 H10L 109.5 . . ? H10J C104 H10L 109.5 . . ? H10K C104 H10L 109.5 . . ? O101 C105 N101 126.2(10) . . ? O101 C105 H10M 116.9 . . ? N101 C105 H10M 116.9 . . ? N102 C106 H10O 109.5 . . ? N102 C106 H10P 109.5 . . ? H10O C106 H10P 109.5 . . ? N102 C106 H10Q 109.5 . . ? H10O C106 H10Q 109.5 . . ? H10P C106 H10Q 109.5 . . ? O102 C107 N102 123.0(19) . . ? O102 C107 H107 118.5 . . ? N102 C107 H107 118.5 . . ? N102 C108 H10R 109.5 . . ? N102 C108 H10S 109.5 . . ? H10R C108 H10S 109.5 . . ? N102 C108 H10T 109.5 . . ? H10R C108 H10T 109.5 . . ? H10S C108 H10T 109.5 . . ? C7 N1 C8 119.4(8) . . ? C7 N1 Cu1 127.9(6) . . ? C8 N1 Cu1 112.5(7) . . ? C11 N2 C9 119.7(8) . . ? C11 N2 Cu1 125.8(6) . . ? C9 N2 Cu1 113.3(7) . . ? C25 N3 C23 119.4(7) . . ? C25 N3 Cu2 126.4(6) . . ? C23 N3 Cu2 113.5(6) . . ? C26 N4 C24 122.3(7) . . ? C26 N4 Cu2 126.5(5) . . ? C24 N4 Cu2 110.4(6) . . ? C42 N5 C41 121.0(7) . . ? C42 N5 Cu3 126.5(6) . . ? C41 N5 Cu3 111.6(6) . . ? C39 N6 C40 120.6(7) . . ? C39 N6 Cu3 126.8(5) . . ? C40 N6 Cu3 112.1(5) . . ? C57 N7 C56 120.0(7) . . ? C57 N7 Cu4 127.7(5) . . ? C56 N7 Cu4 112.3(5) . . ? C58 N8 C55 120.8(7) . . ? C58 N8 Cu4 127.9(5) . . ? C55 N8 Cu4 110.9(5) . . ? C102 N100 C100 120.7(7) . . ? C102 N100 C101 121.0(7) . . ? C100 N100 C101 118.2(7) . . ? C105 N101 C104 119.8(8) . . ? C105 N101 C103 121.4(8) . . ? C104 N101 C103 118.7(7) . . ? C107 N102 C108 123.4(16) . . ? C107 N102 C106 121.5(18) . . ? C108 N102 C106 114.1(16) . . ? C1 O1 Cu1 125.0(4) . . ? C1 O1 Fe2 109.7(4) . . ? Cu1 O1 Fe2 125.4(2) . . ? C16 O2 Cu1 125.8(4) . . ? C16 O2 Fe3 106.5(4) . . ? Cu1 O2 Fe3 123.1(2) . . ? C2 O3 Fe2 115.8(5) . . ? C15 O4 Fe3 112.2(4) . . ? C32 O5 Cu2 122.7(4) . . ? C32 O5 Fe3 108.2(4) . . ? Cu2 O5 Fe3 128.1(2) . . ? C22 O6 Cu2 124.9(4) . . ? C22 O6 Fe1 110.3(4) . . ? Cu2 O6 Fe1 124.8(2) . . ? C31 O7 Fe3 112.5(4) . . ? C17 O8 Fe1 116.2(4) . . ? C33 O9 Cu3 124.2(4) . . ? C33 O9 Fe1 109.7(4) . . ? Cu3 O9 Fe1 123.3(2) . . ? C48 O10 Cu3 124.3(4) . . ? C48 O10 Fe4 109.0(4) . . ? Cu3 O10 Fe4 125.6(2) . . ? C34 O11 Fe1 114.7(4) . . ? C47 O12 Fe4 114.3(4) . . ? C49 O13 Cu4 124.6(4) . . ? C49 O13 Fe2 110.3(4) . . ? Cu4 O13 Fe2 124.8(2) . . ? C64 O14 Cu4 125.7(4) . . ? C64 O14 Fe4 108.2(4) . . ? Cu4 O14 Fe4 123.5(2) . . ? C50 O15 Fe2 116.0(4) . . ? C63 O16 Fe4 114.1(4) . . ? Fe1 O17 Fe3 131.6(2) . . ? Fe1 O17 Fe4 130.6(2) . . ? Fe3 O17 Fe4 97.5(2) . . ? Fe2 O18 Fe4 130.3(2) . . ? Fe2 O18 Fe3 132.3(2) . . ? Fe4 O18 Fe3 96.6(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.645 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.110 data_1 _database_code_depnum_ccdc_archive 'CCDC 894004' #TrackingRef '12899_web_deposit_cif_file_0_Hui-ZhongKou_1343381535.complex-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H86 Cu8 N8 O23' _chemical_formula_weight 1963.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 18.3819(10) _cell_length_b 43.1954(19) _cell_length_c 9.8247(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.251(2) _cell_angle_gamma 90.00 _cell_volume 7800.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6283 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 26.00 _exptl_crystal_description strip _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4008 _exptl_absorpt_coefficient_mu 2.218 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.133 _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 IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% 0 _diffrn_reflns_number 50899 _diffrn_reflns_av_R_equivalents 0.1543 _diffrn_reflns_av_sigmaI/netI 0.1567 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -52 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 26.00 _reflns_number_total 15067 _reflns_number_gt 6283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_cell_refinement 'crystalstructure 3.6.0 (Rigaku, 2004)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XP (Sheldrick, 1998)' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0024(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 15067 _refine_ls_number_parameters 1019 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1870 _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.2438 _refine_ls_wR_factor_gt 0.1947 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.28130(7) 0.63893(3) 0.65886(13) 0.0604(4) Uani 1 1 d . . . Cu2 Cu 0.31437(6) 0.62672(2) 1.00570(12) 0.0518(3) Uani 1 1 d . . . Cu3 Cu 0.47671(7) 0.61206(3) 1.18064(13) 0.0580(4) Uani 1 1 d . . . Cu4 Cu 0.44282(7) 0.62602(2) 0.83835(12) 0.0545(3) Uani 1 1 d . . . Cu5 Cu -0.22272(7) 0.62779(3) 1.69206(13) 0.0612(4) Uani 1 1 d . . . Cu6 Cu -0.05896(6) 0.63465(2) 1.51435(12) 0.0538(3) Uani 1 1 d . . . Cu7 Cu -0.02081(7) 0.63772(3) 1.16448(13) 0.0645(4) Uani 1 1 d . . . Cu8 Cu -0.18388(7) 0.62783(2) 1.34148(12) 0.0535(3) Uani 1 1 d . . . C1 C 0.2759(5) 0.6809(2) 0.8892(10) 0.052(2) Uani 1 1 d . . . C2 C 0.3061(5) 0.68815(19) 1.0168(10) 0.053(2) Uani 1 1 d . . . C3 C 0.3080(6) 0.7185(2) 1.0632(12) 0.075(3) Uani 1 1 d . . . H3A H 0.3305 0.7239 1.1446 0.090 Uiso 1 1 calc R . . C4 C 0.2726(8) 0.7410(2) 0.9766(15) 0.091(4) Uani 1 1 d . . . H4A H 0.2720 0.7614 1.0066 0.109 Uiso 1 1 calc R . . C5 C 0.2408(7) 0.7350(2) 0.8576(13) 0.075(3) Uani 1 1 d . . . H5A H 0.2187 0.7505 0.8066 0.090 Uiso 1 1 calc R . . C6 C 0.2421(6) 0.7045(2) 0.8129(11) 0.061(3) Uani 1 1 d . . . C7 C 0.2038(6) 0.6971(3) 0.6907(14) 0.079(4) Uani 1 1 d . . . H7A H 0.1709 0.7118 0.6588 0.094 Uiso 1 1 calc R . . C8 C 0.1651(7) 0.6692(4) 0.4898(13) 0.102(4) Uani 1 1 d . . . H8A H 0.1285 0.6532 0.5007 0.122 Uiso 1 1 calc R . . H8B H 0.1403 0.6887 0.4741 0.122 Uiso 1 1 calc R . . C9 C 0.2412(9) 0.6308(3) 0.3587(13) 0.097(4) Uani 1 1 d . . . H9A H 0.2765 0.6313 0.2856 0.116 Uiso 1 1 calc R . . H9B H 0.2024 0.6170 0.3309 0.116 Uiso 1 1 calc R . . C10 C 0.2939(5) 0.5884(3) 0.4708(11) 0.070(3) Uani 1 1 d . . . H10A H 0.2784 0.5780 0.3930 0.084 Uiso 1 1 calc R . . C11 C 0.3352(6) 0.5704(2) 0.5718(10) 0.062(3) Uani 1 1 d . . . C12 C 0.3400(7) 0.5381(3) 0.5601(13) 0.085(4) Uani 1 1 d . . . H12A H 0.3143 0.5283 0.4904 0.102 Uiso 1 1 calc R . . C13 C 0.3790(8) 0.5210(3) 0.6428(14) 0.092(4) Uani 1 1 d . . . H13A H 0.3780 0.4995 0.6360 0.110 Uiso 1 1 calc R . . C14 C 0.4224(8) 0.5356(2) 0.7422(13) 0.089(4) Uani 1 1 d . . . H14A H 0.4522 0.5238 0.7987 0.106 Uiso 1 1 calc R . . C15 C 0.4207(6) 0.5678(2) 0.7560(11) 0.067(3) Uani 1 1 d . . . C16 C 0.3738(5) 0.5850(2) 0.6726(10) 0.056(3) Uani 1 1 d . . . C17 C 0.3539(5) 0.57067(19) 1.1143(10) 0.051(2) Uani 1 1 d . . . C18 C 0.2981(5) 0.56540(19) 1.0238(10) 0.054(2) Uani 1 1 d . . . C19 C 0.2693(6) 0.5343(2) 1.0123(11) 0.069(3) Uani 1 1 d . . . H19A H 0.2313 0.5302 0.9523 0.083 Uiso 1 1 calc R . . C20 C 0.2979(7) 0.5110(2) 1.0891(12) 0.075(3) Uani 1 1 d . . . H20A H 0.2797 0.4910 1.0810 0.090 Uiso 1 1 calc R . . C21 C 0.3534(7) 0.5170(2) 1.1782(13) 0.083(4) Uani 1 1 d . . . H21A H 0.3715 0.5010 1.2318 0.099 Uiso 1 1 calc R . . C22 C 0.3837(6) 0.5467(2) 1.1907(10) 0.059(3) Uani 1 1 d . . . C23 C 0.4392(6) 0.5520(2) 1.2892(12) 0.069(3) Uani 1 1 d . . . H23A H 0.4506 0.5354 1.3452 0.082 Uiso 1 1 calc R . . C24 C 0.5286(6) 0.5763(3) 1.4259(13) 0.083(4) Uani 1 1 d . . . H24A H 0.5100 0.5622 1.4940 0.099 Uiso 1 1 calc R . . H24B H 0.5746 0.5681 1.3937 0.099 Uiso 1 1 calc R . . C25 C 0.5853(7) 0.6290(3) 1.4029(13) 0.091(4) Uani 1 1 d . . . H25A H 0.5973 0.6470 1.4578 0.109 Uiso 1 1 calc R . . H25B H 0.6306 0.6191 1.3768 0.109 Uiso 1 1 calc R . . C26 C 0.5540(6) 0.6678(2) 1.2464(11) 0.066(3) Uani 1 1 d . . . H26A H 0.5809 0.6798 1.3070 0.079 Uiso 1 1 calc R . . C27 C 0.5262(6) 0.6836(2) 1.1279(11) 0.061(3) Uani 1 1 d . . . C28 C 0.5364(6) 0.7161(2) 1.1252(12) 0.075(3) Uani 1 1 d . . . H28 H 0.5587 0.7262 1.1977 0.090 Uiso 1 1 calc R . . C29 C 0.5126(7) 0.7323(3) 1.0135(15) 0.092(4) Uani 1 1 d . . . H29A H 0.5160 0.7537 1.0133 0.110 Uiso 1 1 calc R . . C30 C 0.4828(6) 0.7168(2) 0.8977(14) 0.078(4) Uani 1 1 d . . . H30 H 0.4683 0.7281 0.8218 0.094 Uiso 1 1 calc R . . C31 C 0.4756(5) 0.6845(2) 0.8986(12) 0.062(3) Uani 1 1 d . . . C32 C 0.4970(5) 0.6688(2) 1.0202(10) 0.051(2) Uani 1 1 d . . . C33 C 0.5794(8) 0.5450(3) 1.0738(16) 0.118(5) Uani 1 1 d . . . C34 C 0.1534(7) 0.5735(3) 0.6721(15) 0.103(4) Uani 1 1 d . . . C35 C -0.1099(6) 0.5836(2) 1.2072(10) 0.062(3) Uani 1 1 d . . . C36 C -0.1598(6) 0.5677(2) 1.2967(11) 0.062(3) Uani 1 1 d . . . C37 C -0.1622(7) 0.5353(3) 1.2937(13) 0.086(4) Uani 1 1 d . . . H37A H -0.1931 0.5248 1.3526 0.104 Uiso 1 1 calc R . . C38 C -0.1193(8) 0.5188(3) 1.2041(16) 0.094(4) Uani 1 1 d . . . H38A H -0.1217 0.4973 1.2036 0.112 Uiso 1 1 calc R . . C39 C -0.0735(8) 0.5336(3) 1.1163(16) 0.097(4) Uani 1 1 d . . . H39A H -0.0459 0.5219 1.0559 0.116 Uiso 1 1 calc R . . C40 C -0.0671(7) 0.5659(3) 1.1153(13) 0.079(3) Uani 1 1 d . . . C41 C -0.0212(6) 0.5829(4) 1.0146(12) 0.085(4) Uani 1 1 d . . . H41A H -0.0028 0.5707 0.9448 0.102 Uiso 1 1 calc R . . C42 C 0.0334(10) 0.6181(4) 0.8817(16) 0.163(9) Uani 1 1 d . . . H42A H 0.0005 0.6145 0.8059 0.195 Uiso 1 1 calc R . . H42B H 0.0750 0.6045 0.8705 0.195 Uiso 1 1 calc R . . C43 C 0.1043(7) 0.6600(4) 0.9982(14) 0.105(5) Uani 1 1 d . . . H43A H 0.1373 0.6431 1.0184 0.126 Uiso 1 1 calc R . . H43B H 0.1333 0.6782 0.9776 0.126 Uiso 1 1 calc R . . C44 C 0.0652(6) 0.6928(3) 1.1728(14) 0.081(4) Uani 1 1 d . . . H44A H 0.0986 0.7063 1.1333 0.098 Uiso 1 1 calc R . . C45 C 0.0267(6) 0.7049(2) 1.2895(12) 0.069(3) Uani 1 1 d . . . C46 C 0.0305(7) 0.7370(3) 1.3237(15) 0.085(4) Uani 1 1 d . . . H46A H 0.0559 0.7506 1.2680 0.102 Uiso 1 1 calc R . . C47 C -0.0030(8) 0.7477(3) 1.4379(16) 0.093(4) Uani 1 1 d . . . H47A H -0.0007 0.7687 1.4583 0.111 Uiso 1 1 calc R . . C48 C -0.0402(7) 0.7281(3) 1.5240(13) 0.081(3) Uani 1 1 d . . . H48A H -0.0632 0.7362 1.6004 0.097 Uiso 1 1 calc R . . C49 C -0.0438(6) 0.6966(2) 1.4979(11) 0.061(3) Uani 1 1 d . . . C50 C -0.0137(5) 0.6852(2) 1.3758(12) 0.061(3) Uani 1 1 d . . . C51 C -0.1029(6) 0.58403(18) 1.6556(10) 0.054(3) Uani 1 1 d . . . C52 C -0.0478(5) 0.5744(2) 1.5675(11) 0.055(2) Uani 1 1 d . . . C53 C -0.0257(6) 0.5432(2) 1.5802(12) 0.073(3) Uani 1 1 d . . . H53A H 0.0122 0.5361 1.5263 0.088 Uiso 1 1 calc R . . C54 C -0.0577(8) 0.5232(2) 1.6679(13) 0.083(4) Uani 1 1 d . . . H54A H -0.0437 0.5025 1.6692 0.099 Uiso 1 1 calc R . . C55 C -0.1105(7) 0.5335(2) 1.7543(12) 0.075(3) Uani 1 1 d . . . H55A H -0.1305 0.5195 1.8158 0.090 Uiso 1 1 calc R . . C56 C -0.1358(5) 0.5643(2) 1.7541(10) 0.057(3) Uani 1 1 d . . . C57 C -0.1841(6) 0.5748(3) 1.8557(11) 0.069(3) Uani 1 1 d . . . H57A H -0.1924 0.5614 1.9281 0.083 Uiso 1 1 calc R . . C58 C -0.2587(6) 0.6084(3) 1.9845(12) 0.088(4) Uani 1 1 d . . . H58A H -0.2907 0.5911 2.0033 0.106 Uiso 1 1 calc R . . H58B H -0.2237 0.6096 2.0585 0.106 Uiso 1 1 calc R . . C59 C -0.3518(8) 0.6401(4) 1.8680(14) 0.127(6) Uani 1 1 d . . . H59A H -0.3886 0.6553 1.8906 0.152 Uiso 1 1 calc R . . H59B H -0.3761 0.6206 1.8482 0.152 Uiso 1 1 calc R . . C60 C -0.2617(6) 0.7143(2) 1.3157(12) 0.073(3) Uani 1 1 d . . . H60A H -0.2489 0.7230 1.2326 0.087 Uiso 1 1 calc R . . C61 C -0.3074(7) 0.7309(2) 1.4043(15) 0.083(4) Uani 1 1 d . . . H61A H -0.3232 0.7506 1.3801 0.099 Uiso 1 1 calc R . . C62 C -0.3287(6) 0.7185(2) 1.5244(14) 0.075(3) Uani 1 1 d . . . H62A H -0.3595 0.7295 1.5815 0.090 Uiso 1 1 calc R . . C63 C -0.3042(5) 0.6891(2) 1.5624(11) 0.056(3) Uani 1 1 d . . . C64 C -0.2575(5) 0.67300(19) 1.4763(11) 0.054(3) Uani 1 1 d . . . C65 C -0.2354(6) 0.6852(2) 1.3503(10) 0.057(3) Uani 1 1 d . . . C66 C 0.0592(10) 0.6519(4) 0.8784(15) 0.134(6) Uani 1 1 d . . . H66A H 0.0871 0.6554 0.7963 0.161 Uiso 1 1 calc R . . H66B H 0.0171 0.6655 0.8753 0.161 Uiso 1 1 calc R . . C67 C -0.3011(9) 0.6359(3) 1.9861(15) 0.113(5) Uani 1 1 d . . . H67A H -0.2684 0.6535 1.9893 0.136 Uiso 1 1 calc R . . H67B H -0.3295 0.6362 2.0691 0.136 Uiso 1 1 calc R . . C68 C -0.3307(6) 0.6753(3) 1.6848(11) 0.076(3) Uani 1 1 d . . . H68A H -0.3686 0.6858 1.7265 0.091 Uiso 1 1 calc R . . C69 C 0.2106(9) 0.6618(4) 0.3726(13) 0.130(6) Uani 1 1 d . . . H69A H 0.1821 0.6660 0.2913 0.156 Uiso 1 1 calc R . . H69B H 0.2509 0.6764 0.3726 0.156 Uiso 1 1 calc R . . C70 C 0.5411(7) 0.6065(3) 1.4885(12) 0.079(3) Uani 1 1 d . . . H70A H 0.5661 0.6034 1.5746 0.094 Uiso 1 1 calc R . . H70B H 0.4944 0.6158 1.5080 0.094 Uiso 1 1 calc R . . C71 C 0.1116(8) 0.5662(3) 1.2435(16) 0.110(5) Uani 1 1 d . . . C72 C -0.3117(7) 0.5508(3) 1.6268(15) 0.098(4) Uani 1 1 d . . . C73 C -0.1803(7) 0.7098(3) 1.8156(14) 0.098(4) Uani 1 1 d . . . C74 C 0.4252(14) 0.6848(4) 0.476(2) 0.197(12) Uani 1 1 d . . . N1 N 0.2100(5) 0.6714(2) 0.6180(9) 0.071(2) Uani 1 1 d . . . N2 N 0.2768(5) 0.6175(2) 0.4799(9) 0.067(2) Uani 1 1 d . . . N3 N 0.4769(4) 0.57784(18) 1.3112(8) 0.060(2) Uani 1 1 d . . . N4 N 0.5463(5) 0.63936(19) 1.2783(9) 0.065(2) Uani 1 1 d . . . N5 N -0.0038(6) 0.6102(3) 1.0091(12) 0.095(4) Uani 1 1 d . . . N6 N 0.0595(5) 0.6662(2) 1.1165(10) 0.074(3) Uani 1 1 d . . . N7 N -0.3103(5) 0.6506(2) 1.7450(10) 0.078(3) Uani 1 1 d . . . N8 N -0.2190(5) 0.6018(2) 1.8585(9) 0.073(3) Uani 1 1 d . . . O1 O 0.3338(4) 0.66437(14) 1.0922(7) 0.0604(17) Uani 1 1 d . . . O2 O 0.2786(4) 0.65088(12) 0.8498(6) 0.0552(16) Uani 1 1 d . . . O3 O 0.3717(3) 0.61553(14) 0.6986(6) 0.0559(16) Uani 1 1 d . . . O4 O 0.4619(4) 0.58288(14) 0.8483(7) 0.0671(19) Uani 1 1 d . . . O5 O 0.3776(3) 0.60046(13) 1.1209(6) 0.0546(16) Uani 1 1 d . . . O6 O 0.2691(4) 0.58929(14) 0.9566(7) 0.0640(19) Uani 1 1 d . . . O7 O 0.4490(4) 0.66781(14) 0.7948(7) 0.0644(19) Uani 1 1 d . . . O8 O 0.4838(3) 0.63726(13) 1.0156(6) 0.0557(16) Uani 1 1 d . . . O9 O 0.5558(5) 0.57614(16) 1.0446(8) 0.087(2) Uani 1 1 d . . . O10 O 0.1902(4) 0.59822(16) 0.7336(7) 0.072(2) Uani 1 1 d . . . O11 O -0.1080(4) 0.61361(14) 1.2166(7) 0.0624(18) Uani 1 1 d . . . O12 O -0.2016(4) 0.58550(14) 1.3728(7) 0.0656(19) Uani 1 1 d . . . O13 O -0.0200(3) 0.65375(14) 1.3522(6) 0.0569(17) Uani 1 1 d . . . O14 O -0.0753(4) 0.67576(15) 1.5777(7) 0.069(2) Uani 1 1 d . . . O15 O -0.1951(4) 0.66778(15) 1.2710(7) 0.0665(19) Uani 1 1 d . . . O16 O -0.2311(3) 0.64392(13) 1.5054(6) 0.0536(16) Uani 1 1 d . . . O17 O -0.0196(4) 0.59484(13) 1.4848(7) 0.0597(17) Uani 1 1 d . . . O18 O -0.1246(4) 0.61481(13) 1.6441(7) 0.0597(17) Uani 1 1 d . . . O19 O 0.0797(5) 0.5949(2) 1.2865(10) 0.108(3) Uani 1 1 d . . . O20 O -0.2906(4) 0.58101(15) 1.5798(8) 0.079(2) Uani 1 1 d . . . O21 O -0.1521(4) 0.67933(17) 1.7980(8) 0.085(2) Uani 1 1 d . . . O22 O 0.3713(6) 0.6837(2) 0.5798(13) 0.136(4) Uani 1 1 d . . . O1W O -0.0992(4) 0.67511(17) 1.0698(8) 0.084(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0608(8) 0.0679(7) 0.0525(9) -0.0009(6) -0.0059(6) 0.0060(6) Cu2 0.0543(8) 0.0491(6) 0.0520(8) 0.0038(5) -0.0026(6) -0.0019(5) Cu3 0.0576(8) 0.0575(7) 0.0587(9) 0.0107(6) -0.0081(6) -0.0072(6) Cu4 0.0572(8) 0.0526(6) 0.0536(8) 0.0026(5) -0.0008(6) 0.0008(5) Cu5 0.0533(8) 0.0755(8) 0.0549(8) 0.0097(6) 0.0101(6) 0.0127(6) Cu6 0.0536(8) 0.0548(7) 0.0532(8) 0.0041(5) 0.0071(6) 0.0026(5) Cu7 0.0563(8) 0.0842(9) 0.0531(9) -0.0014(6) 0.0112(6) -0.0028(6) Cu8 0.0548(8) 0.0522(6) 0.0537(8) 0.0017(5) 0.0063(6) 0.0024(5) C1 0.050(6) 0.056(6) 0.051(7) 0.003(4) 0.020(5) 0.003(4) C2 0.061(6) 0.043(5) 0.056(7) 0.006(4) 0.009(5) -0.001(4) C3 0.092(9) 0.054(6) 0.080(9) -0.017(5) 0.006(7) -0.009(6) C4 0.131(12) 0.050(6) 0.091(11) 0.003(6) 0.040(9) 0.012(7) C5 0.103(10) 0.060(6) 0.060(8) 0.009(5) 0.011(7) 0.022(6) C6 0.068(7) 0.058(6) 0.057(7) 0.013(5) 0.002(6) 0.008(5) C7 0.054(7) 0.083(8) 0.099(11) 0.027(7) 0.004(7) 0.022(6) C8 0.078(9) 0.172(13) 0.055(9) 0.035(8) -0.005(7) 0.022(8) C9 0.139(13) 0.086(8) 0.066(9) 0.011(6) -0.018(8) 0.014(8) C10 0.040(6) 0.107(9) 0.064(8) -0.019(6) 0.001(5) -0.007(6) C11 0.069(7) 0.065(6) 0.051(7) -0.010(5) 0.002(6) 0.001(5) C12 0.093(10) 0.084(8) 0.079(10) -0.027(7) 0.014(8) -0.009(7) C13 0.122(12) 0.055(7) 0.098(11) -0.016(7) -0.017(9) -0.003(7) C14 0.125(11) 0.056(7) 0.085(10) -0.003(6) 0.017(8) 0.008(7) C15 0.082(8) 0.065(6) 0.053(7) -0.002(5) 0.011(6) 0.001(6) C16 0.051(6) 0.065(6) 0.053(7) 0.000(5) -0.004(5) 0.009(5) C17 0.058(6) 0.042(5) 0.053(7) 0.003(4) 0.005(5) -0.004(4) C18 0.057(6) 0.040(5) 0.066(7) -0.002(4) 0.007(5) -0.008(4) C19 0.078(8) 0.072(7) 0.056(7) -0.001(5) -0.008(6) -0.012(6) C20 0.083(8) 0.049(6) 0.093(9) 0.004(6) -0.006(7) -0.018(6) C21 0.089(9) 0.060(7) 0.099(10) 0.032(6) 0.023(8) 0.004(6) C22 0.063(7) 0.059(6) 0.055(7) 0.010(5) -0.010(5) -0.009(5) C23 0.071(8) 0.054(6) 0.080(9) 0.021(5) 0.006(6) 0.009(5) C24 0.060(7) 0.099(9) 0.089(10) 0.023(7) -0.020(7) 0.001(6) C25 0.081(9) 0.116(10) 0.075(9) 0.013(7) -0.035(8) -0.012(7) C26 0.061(7) 0.070(7) 0.066(8) -0.002(6) -0.003(6) -0.021(5) C27 0.063(7) 0.056(6) 0.065(8) 0.004(5) 0.002(6) -0.012(5) C28 0.078(8) 0.063(6) 0.083(9) 0.013(6) -0.024(7) -0.020(6) C29 0.093(10) 0.062(7) 0.121(12) -0.008(7) -0.002(9) -0.031(7) C30 0.067(7) 0.051(6) 0.117(11) 0.029(6) -0.013(7) -0.011(5) C31 0.051(6) 0.055(6) 0.079(8) 0.014(5) 0.004(6) -0.001(5) C32 0.039(5) 0.049(5) 0.065(7) -0.002(5) 0.005(5) 0.003(4) C33 0.123(12) 0.096(9) 0.135(14) 0.024(8) -0.006(10) 0.063(9) C34 0.091(10) 0.104(9) 0.113(12) -0.023(8) -0.010(9) -0.025(8) C35 0.057(7) 0.083(7) 0.045(7) -0.025(5) -0.016(5) 0.013(5) C36 0.072(7) 0.058(6) 0.054(7) -0.008(5) -0.008(6) 0.001(5) C37 0.111(10) 0.062(7) 0.086(10) 0.001(6) -0.007(8) -0.002(7) C38 0.110(11) 0.064(7) 0.106(12) -0.027(7) -0.009(9) 0.016(8) C39 0.109(12) 0.075(8) 0.107(12) -0.018(7) -0.020(10) 0.032(8) C40 0.083(9) 0.091(8) 0.064(9) -0.017(6) -0.011(7) 0.018(7) C41 0.057(8) 0.146(12) 0.051(8) -0.025(8) 0.003(6) 0.035(8) C42 0.169(17) 0.213(18) 0.107(13) -0.087(13) 0.100(13) -0.115(15) C43 0.089(10) 0.166(13) 0.062(9) -0.001(9) 0.044(8) -0.038(9) C44 0.052(7) 0.109(10) 0.084(10) 0.034(8) 0.011(7) -0.003(7) C45 0.076(8) 0.076(7) 0.056(8) 0.021(6) -0.025(6) -0.011(6) C46 0.093(10) 0.073(8) 0.090(11) 0.021(7) -0.025(8) -0.031(7) C47 0.121(11) 0.048(6) 0.109(12) -0.001(7) -0.026(10) -0.025(7) C48 0.094(9) 0.066(7) 0.082(9) -0.002(6) -0.005(7) 0.000(6) C49 0.060(7) 0.067(7) 0.054(7) -0.002(5) 0.001(6) -0.003(5) C50 0.045(6) 0.068(6) 0.071(8) 0.028(5) -0.015(5) -0.011(5) C51 0.067(7) 0.037(5) 0.057(7) 0.003(4) -0.012(5) 0.004(4) C52 0.052(6) 0.052(5) 0.060(7) -0.001(5) 0.004(5) 0.012(5) C53 0.080(8) 0.061(6) 0.079(9) 0.007(6) 0.012(7) 0.011(6) C54 0.121(11) 0.043(6) 0.085(10) 0.001(6) -0.009(8) 0.003(6) C55 0.092(9) 0.055(6) 0.077(9) 0.012(6) -0.001(7) -0.006(6) C56 0.053(6) 0.057(6) 0.059(7) 0.017(5) -0.004(5) -0.002(5) C57 0.062(7) 0.090(8) 0.056(8) 0.014(6) 0.012(6) -0.011(6) C58 0.063(8) 0.151(12) 0.050(8) 0.024(7) 0.018(6) 0.033(8) C59 0.079(10) 0.230(18) 0.070(10) 0.055(11) 0.043(8) 0.041(10) C60 0.081(8) 0.065(6) 0.073(8) 0.010(6) 0.005(7) -0.013(6) C61 0.080(9) 0.047(6) 0.121(12) -0.011(7) 0.008(8) 0.006(6) C62 0.069(8) 0.061(7) 0.095(10) -0.011(6) 0.016(7) 0.010(6) C63 0.043(6) 0.058(6) 0.068(8) -0.009(5) -0.006(5) 0.008(5) C64 0.044(6) 0.044(5) 0.074(8) -0.002(5) 0.004(5) -0.002(4) C65 0.074(7) 0.049(5) 0.048(7) 0.009(5) 0.002(5) 0.003(5) C66 0.128(14) 0.209(19) 0.065(11) 0.003(11) 0.059(10) -0.006(13) C67 0.138(14) 0.124(11) 0.078(11) 0.003(8) 0.021(10) 0.015(10) C68 0.068(8) 0.114(10) 0.047(8) -0.019(7) 0.002(6) 0.024(7) C69 0.134(14) 0.207(18) 0.049(9) 0.024(10) -0.012(9) 0.058(13) C70 0.090(9) 0.085(8) 0.060(8) 0.010(6) -0.014(7) 0.004(7) C71 0.101(11) 0.092(9) 0.138(14) -0.037(9) 0.015(10) 0.021(8) C72 0.103(10) 0.069(7) 0.123(12) 0.042(7) 0.005(9) -0.014(7) C73 0.099(10) 0.082(8) 0.112(11) -0.014(7) -0.014(8) 0.040(7) C74 0.27(3) 0.128(13) 0.19(2) 0.049(13) 0.20(2) 0.038(15) N1 0.060(6) 0.099(7) 0.055(6) 0.020(5) -0.004(5) 0.001(5) N2 0.060(6) 0.086(6) 0.056(6) 0.003(5) -0.016(5) 0.002(5) N3 0.058(5) 0.064(5) 0.059(6) 0.002(4) 0.005(4) -0.002(4) N4 0.057(5) 0.071(6) 0.068(6) 0.005(4) 0.002(5) -0.014(4) N5 0.092(8) 0.096(7) 0.098(9) -0.017(7) 0.042(7) -0.021(7) N6 0.065(6) 0.093(7) 0.063(7) 0.017(5) 0.006(5) 0.004(5) N7 0.071(7) 0.105(7) 0.057(7) 0.006(5) -0.001(5) 0.013(5) N8 0.059(6) 0.109(7) 0.051(6) 0.010(5) 0.018(5) 0.001(5) O1 0.060(4) 0.062(4) 0.058(5) 0.000(3) -0.007(3) -0.003(3) O2 0.069(4) 0.043(3) 0.054(4) 0.003(3) 0.004(3) -0.003(3) O3 0.061(4) 0.057(4) 0.050(4) 0.002(3) 0.005(3) 0.003(3) O4 0.077(5) 0.060(4) 0.065(5) -0.006(3) -0.015(4) 0.011(3) O5 0.061(4) 0.048(3) 0.055(4) -0.002(3) -0.002(3) -0.003(3) O6 0.063(5) 0.061(4) 0.067(5) 0.006(3) -0.013(4) -0.009(3) O7 0.075(5) 0.060(4) 0.058(5) 0.007(3) -0.013(4) -0.012(3) O8 0.060(4) 0.051(3) 0.056(4) 0.007(3) 0.003(3) -0.005(3) O9 0.100(6) 0.077(5) 0.083(6) -0.003(4) -0.005(5) 0.008(4) O10 0.066(5) 0.077(5) 0.073(5) -0.008(4) -0.001(4) -0.016(4) O11 0.083(5) 0.052(4) 0.052(4) -0.012(3) 0.000(4) 0.003(3) O12 0.072(5) 0.066(4) 0.059(5) -0.016(3) 0.019(4) -0.011(4) O13 0.056(4) 0.054(4) 0.061(5) -0.003(3) 0.002(3) -0.002(3) O14 0.080(5) 0.067(4) 0.060(5) 0.008(4) 0.013(4) -0.013(4) O15 0.078(5) 0.067(4) 0.055(5) 0.003(3) 0.016(4) 0.019(4) O16 0.045(4) 0.058(4) 0.058(4) -0.003(3) -0.005(3) 0.005(3) O17 0.067(5) 0.052(4) 0.060(5) 0.007(3) 0.018(4) 0.002(3) O18 0.065(4) 0.054(4) 0.060(5) 0.008(3) 0.003(4) 0.010(3) O19 0.106(7) 0.115(7) 0.104(7) -0.018(6) 0.024(6) -0.010(6) O20 0.080(5) 0.071(5) 0.086(6) 0.018(4) -0.007(4) -0.013(4) O21 0.091(6) 0.081(5) 0.084(6) -0.001(4) 0.006(5) 0.024(4) O22 0.117(9) 0.127(8) 0.164(11) 0.014(7) -0.036(8) 0.004(6) O1W 0.076(5) 0.102(6) 0.075(6) 0.025(4) 0.001(4) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.947(6) . ? Cu1 N1 1.960(9) . ? Cu1 O3 1.982(6) . ? Cu1 N2 1.987(9) . ? Cu2 O1 1.869(6) . ? Cu2 O6 1.881(6) . ? Cu2 O2 1.964(6) . ? Cu2 O5 1.976(6) . ? Cu2 Cu4 2.8834(18) . ? Cu3 N3 1.957(8) . ? Cu3 O8 1.958(6) . ? Cu3 O5 1.977(6) . ? Cu3 N4 1.985(8) . ? Cu4 O7 1.859(6) . ? Cu4 O4 1.899(6) . ? Cu4 O3 1.945(6) . ? Cu4 O8 1.955(7) . ? Cu5 O18 1.949(7) . ? Cu5 N7 1.960(10) . ? Cu5 O16 1.967(6) . ? Cu5 N8 1.985(9) . ? Cu6 O17 1.888(6) . ? Cu6 O14 1.906(7) . ? Cu6 O13 1.934(7) . ? Cu6 O18 1.957(7) . ? Cu6 Cu8 2.8653(18) . ? Cu7 N5 1.962(11) . ? Cu7 O13 1.970(6) . ? Cu7 O11 1.980(7) . ? Cu7 N6 1.981(10) . ? Cu7 O1W 2.353(7) . ? Cu8 O15 1.870(6) . ? Cu8 O12 1.883(6) . ? Cu8 O16 1.960(6) . ? Cu8 O11 1.961(7) . ? C1 O2 1.353(10) . ? C1 C2 1.405(13) . ? C1 C6 1.407(12) . ? C2 O1 1.364(10) . ? C2 C3 1.387(12) . ? C3 C4 1.444(16) . ? C3 H3A 0.9300 . ? C4 C5 1.330(16) . ? C4 H4A 0.9300 . ? C5 C6 1.390(14) . ? C5 H5A 0.9300 . ? C6 C7 1.426(15) . ? C7 N1 1.323(14) . ? C7 H7A 0.9300 . ? C8 C69 1.461(17) . ? C8 N1 1.506(14) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C69 1.458(17) . ? C9 N2 1.474(13) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.300(13) . ? C10 C11 1.470(15) . ? C10 H10A 0.9300 . ? C11 C16 1.370(13) . ? C11 C12 1.404(14) . ? C12 C13 1.309(16) . ? C12 H12A 0.9300 . ? C13 C14 1.408(16) . ? C13 H13A 0.9300 . ? C14 C15 1.396(13) . ? C14 H14A 0.9300 . ? C15 O4 1.346(12) . ? C15 C16 1.402(13) . ? C16 O3 1.343(10) . ? C17 O5 1.360(10) . ? C17 C18 1.373(13) . ? C17 C22 1.389(12) . ? C18 O6 1.336(11) . ? C18 C19 1.449(12) . ? C19 C20 1.361(14) . ? C19 H19A 0.9300 . ? C20 C21 1.364(15) . ? C20 H20A 0.9300 . ? C21 C22 1.406(14) . ? C21 H21A 0.9300 . ? C22 C23 1.421(14) . ? C23 N3 1.330(12) . ? C23 H23A 0.9300 . ? C24 C70 1.458(15) . ? C24 N3 1.472(13) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N4 1.485(13) . ? C25 C70 1.523(15) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N4 1.277(11) . ? C26 C27 1.440(14) . ? C26 H26A 0.9300 . ? C27 C32 1.344(13) . ? C27 C28 1.417(13) . ? C28 C29 1.371(15) . ? C28 H28 0.9300 . ? C29 C30 1.426(16) . ? C29 H29A 0.9300 . ? C30 C31 1.400(13) . ? C30 H30 0.9300 . ? C31 O7 1.340(12) . ? C31 C32 1.427(13) . ? C32 O8 1.386(10) . ? C33 O9 1.443(13) . ? C34 O10 1.401(13) . ? C35 O11 1.302(11) . ? C35 C40 1.422(15) . ? C35 C36 1.445(15) . ? C36 O12 1.322(12) . ? C36 C37 1.400(14) . ? C37 C38 1.383(17) . ? C37 H37A 0.9300 . ? C38 C39 1.367(18) . ? C38 H38A 0.9300 . ? C39 C40 1.404(16) . ? C39 H39A 0.9300 . ? C40 C41 1.495(18) . ? C41 N5 1.222(15) . ? C41 H41A 0.9300 . ? C42 N5 1.469(16) . ? C42 C66 1.54(2) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 N6 1.452(14) . ? C43 C66 1.479(19) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 N6 1.280(15) . ? C44 C45 1.448(16) . ? C44 H44A 0.9300 . ? C45 C50 1.413(14) . ? C45 C46 1.426(15) . ? C46 C47 1.363(17) . ? C46 H46A 0.9300 . ? C47 C48 1.379(16) . ? C47 H47A 0.9300 . ? C48 C49 1.385(14) . ? C48 H48A 0.9300 . ? C49 O14 1.330(11) . ? C49 C50 1.412(14) . ? C50 O13 1.385(11) . ? C51 O18 1.392(10) . ? C51 C52 1.398(13) . ? C51 C56 1.427(13) . ? C52 O17 1.309(11) . ? C52 C53 1.413(13) . ? C53 C54 1.354(15) . ? C53 H53A 0.9300 . ? C54 C55 1.365(15) . ? C54 H54A 0.9300 . ? C55 C56 1.411(13) . ? C55 H55A 0.9300 . ? C56 C57 1.412(14) . ? C57 N8 1.333(13) . ? C57 H57A 0.9300 . ? C58 C67 1.420(16) . ? C58 N8 1.469(13) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C67 1.496(19) . ? C59 N7 1.503(14) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C65 1.390(13) . ? C60 C61 1.409(15) . ? C60 H60A 0.9300 . ? C61 C62 1.356(15) . ? C61 H61A 0.9300 . ? C62 C63 1.400(13) . ? C62 H62A 0.9300 . ? C63 C64 1.392(13) . ? C63 C68 1.430(15) . ? C64 O16 1.376(10) . ? C64 C65 1.407(13) . ? C65 O15 1.315(11) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 N7 1.273(13) . ? C68 H68A 0.9300 . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 O19 1.433(14) . ? C72 O20 1.440(12) . ? C73 O21 1.424(12) . ? C74 O22 1.429(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 N1 89.3(3) . . ? O2 Cu1 O3 88.3(3) . . ? N1 Cu1 O3 164.7(3) . . ? O2 Cu1 N2 167.1(3) . . ? N1 Cu1 N2 97.3(4) . . ? O3 Cu1 N2 88.2(3) . . ? O1 Cu2 O6 161.5(3) . . ? O1 Cu2 O2 87.4(3) . . ? O6 Cu2 O2 96.3(3) . . ? O1 Cu2 O5 97.4(3) . . ? O6 Cu2 O5 85.0(3) . . ? O2 Cu2 O5 161.0(3) . . ? O1 Cu2 Cu4 96.5(2) . . ? O6 Cu2 Cu4 102.0(2) . . ? O2 Cu2 Cu4 80.4(2) . . ? O5 Cu2 Cu4 80.78(19) . . ? N3 Cu3 O8 164.3(3) . . ? N3 Cu3 O5 90.1(3) . . ? O8 Cu3 O5 87.7(3) . . ? N3 Cu3 N4 97.6(4) . . ? O8 Cu3 N4 91.4(3) . . ? O5 Cu3 N4 152.4(3) . . ? O7 Cu4 O4 162.5(3) . . ? O7 Cu4 O3 96.1(3) . . ? O4 Cu4 O3 86.0(3) . . ? O7 Cu4 O8 86.6(3) . . ? O4 Cu4 O8 97.3(3) . . ? O3 Cu4 O8 160.3(3) . . ? O7 Cu4 Cu2 99.9(2) . . ? O4 Cu4 Cu2 97.6(2) . . ? O3 Cu4 Cu2 81.66(19) . . ? O8 Cu4 Cu2 78.63(19) . . ? O18 Cu5 N7 166.2(4) . . ? O18 Cu5 O16 86.9(3) . . ? N7 Cu5 O16 90.5(3) . . ? O18 Cu5 N8 90.5(3) . . ? N7 Cu5 N8 95.2(4) . . ? O16 Cu5 N8 166.1(3) . . ? O17 Cu6 O14 163.7(3) . . ? O17 Cu6 O13 96.8(3) . . ? O14 Cu6 O13 86.0(3) . . ? O17 Cu6 O18 86.5(3) . . ? O14 Cu6 O18 95.5(3) . . ? O13 Cu6 O18 162.7(3) . . ? O17 Cu6 Cu8 97.0(2) . . ? O14 Cu6 Cu8 99.3(2) . . ? O13 Cu6 Cu8 81.61(19) . . ? O18 Cu6 Cu8 81.2(2) . . ? N5 Cu7 O13 160.3(4) . . ? N5 Cu7 O11 90.8(4) . . ? O13 Cu7 O11 86.9(3) . . ? N5 Cu7 N6 94.0(5) . . ? O13 Cu7 N6 90.1(4) . . ? O11 Cu7 N6 173.3(4) . . ? N5 Cu7 O1W 102.0(4) . . ? O13 Cu7 O1W 97.5(3) . . ? O11 Cu7 O1W 88.2(3) . . ? N6 Cu7 O1W 86.3(3) . . ? O15 Cu8 O12 159.7(3) . . ? O15 Cu8 O16 85.9(3) . . ? O12 Cu8 O16 97.6(3) . . ? O15 Cu8 O11 97.7(3) . . ? O12 Cu8 O11 85.6(3) . . ? O16 Cu8 O11 160.8(3) . . ? O15 Cu8 Cu6 102.2(2) . . ? O12 Cu8 Cu6 98.1(2) . . ? O16 Cu8 Cu6 80.41(18) . . ? O11 Cu8 Cu6 80.4(2) . . ? O2 C1 C2 117.0(8) . . ? O2 C1 C6 123.9(9) . . ? C2 C1 C6 119.0(9) . . ? O1 C2 C3 121.6(10) . . ? O1 C2 C1 117.5(8) . . ? C3 C2 C1 120.9(9) . . ? C2 C3 C4 115.5(11) . . ? C2 C3 H3A 122.2 . . ? C4 C3 H3A 122.2 . . ? C5 C4 C3 125.6(10) . . ? C5 C4 H4A 117.2 . . ? C3 C4 H4A 117.2 . . ? C4 C5 C6 117.0(10) . . ? C4 C5 H5A 121.5 . . ? C6 C5 H5A 121.5 . . ? C5 C6 C1 121.8(10) . . ? C5 C6 C7 118.0(10) . . ? C1 C6 C7 120.1(9) . . ? N1 C7 C6 126.7(9) . . ? N1 C7 H7A 116.6 . . ? C6 C7 H7A 116.6 . . ? C69 C8 N1 111.1(11) . . ? C69 C8 H8A 109.4 . . ? N1 C8 H8A 109.4 . . ? C69 C8 H8B 109.4 . . ? N1 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C69 C9 N2 116.9(11) . . ? C69 C9 H9A 108.1 . . ? N2 C9 H9A 108.1 . . ? C69 C9 H9B 108.1 . . ? N2 C9 H9B 108.1 . . ? H9A C9 H9B 107.3 . . ? N2 C10 C11 126.1(10) . . ? N2 C10 H10A 116.9 . . ? C11 C10 H10A 116.9 . . ? C16 C11 C12 119.1(11) . . ? C16 C11 C10 120.5(9) . . ? C12 C11 C10 120.2(10) . . ? C13 C12 C11 123.0(12) . . ? C13 C12 H12A 118.5 . . ? C11 C12 H12A 118.5 . . ? C12 C13 C14 119.0(11) . . ? C12 C13 H13A 120.5 . . ? C14 C13 H13A 120.5 . . ? C15 C14 C13 120.1(12) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? O4 C15 C14 122.4(11) . . ? O4 C15 C16 118.6(9) . . ? C14 C15 C16 119.0(11) . . ? O3 C16 C11 125.1(9) . . ? O3 C16 C15 115.4(9) . . ? C11 C16 C15 119.5(9) . . ? O5 C17 C18 115.2(8) . . ? O5 C17 C22 123.6(9) . . ? C18 C17 C22 121.2(8) . . ? O6 C18 C17 119.2(8) . . ? O6 C18 C19 122.2(9) . . ? C17 C18 C19 118.4(9) . . ? C20 C19 C18 120.1(10) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? C19 C20 C21 120.1(10) . . ? C19 C20 H20A 119.9 . . ? C21 C20 H20A 119.9 . . ? C20 C21 C22 121.6(10) . . ? C20 C21 H21A 119.2 . . ? C22 C21 H21A 119.2 . . ? C17 C22 C21 118.5(10) . . ? C17 C22 C23 121.9(9) . . ? C21 C22 C23 119.4(9) . . ? N3 C23 C22 128.2(9) . . ? N3 C23 H23A 115.9 . . ? C22 C23 H23A 115.9 . . ? C70 C24 N3 112.5(9) . . ? C70 C24 H24A 109.1 . . ? N3 C24 H24A 109.1 . . ? C70 C24 H24B 109.1 . . ? N3 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? N4 C25 C70 113.0(9) . . ? N4 C25 H25A 109.0 . . ? C70 C25 H25A 109.0 . . ? N4 C25 H25B 109.0 . . ? C70 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? N4 C26 C27 127.8(10) . . ? N4 C26 H26A 116.1 . . ? C27 C26 H26A 116.1 . . ? C32 C27 C28 120.4(10) . . ? C32 C27 C26 123.6(9) . . ? C28 C27 C26 115.9(10) . . ? C29 C28 C27 118.6(10) . . ? C29 C28 H28 120.7 . . ? C27 C28 H28 120.7 . . ? C28 C29 C30 121.3(10) . . ? C28 C29 H29A 119.4 . . ? C30 C29 H29A 119.4 . . ? C31 C30 C29 119.8(11) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? O7 C31 C30 124.5(10) . . ? O7 C31 C32 118.6(8) . . ? C30 C31 C32 116.9(10) . . ? C27 C32 O8 124.1(9) . . ? C27 C32 C31 122.8(9) . . ? O8 C32 C31 113.1(8) . . ? O11 C35 C40 124.3(11) . . ? O11 C35 C36 116.6(9) . . ? C40 C35 C36 119.2(10) . . ? O12 C36 C37 125.0(11) . . ? O12 C36 C35 116.2(9) . . ? C37 C36 C35 118.8(10) . . ? C38 C37 C36 120.7(13) . . ? C38 C37 H37A 119.7 . . ? C36 C37 H37A 119.7 . . ? C39 C38 C37 121.1(13) . . ? C39 C38 H38A 119.5 . . ? C37 C38 H38A 119.5 . . ? C38 C39 C40 121.4(13) . . ? C38 C39 H39A 119.3 . . ? C40 C39 H39A 119.3 . . ? C39 C40 C35 118.9(13) . . ? C39 C40 C41 122.7(12) . . ? C35 C40 C41 118.3(11) . . ? N5 C41 C40 130.5(12) . . ? N5 C41 H41A 114.7 . . ? C40 C41 H41A 114.7 . . ? N5 C42 C66 112.6(11) . . ? N5 C42 H42A 109.1 . . ? C66 C42 H42A 109.1 . . ? N5 C42 H42B 109.1 . . ? C66 C42 H42B 109.1 . . ? H42A C42 H42B 107.8 . . ? N6 C43 C66 111.2(11) . . ? N6 C43 H43A 109.4 . . ? C66 C43 H43A 109.4 . . ? N6 C43 H43B 109.4 . . ? C66 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? N6 C44 C45 128.8(11) . . ? N6 C44 H44A 115.6 . . ? C45 C44 H44A 115.6 . . ? C50 C45 C46 117.9(12) . . ? C50 C45 C44 121.2(11) . . ? C46 C45 C44 120.9(12) . . ? C47 C46 C45 120.1(11) . . ? C47 C46 H46A 119.9 . . ? C45 C46 H46A 119.9 . . ? C46 C47 C48 121.5(11) . . ? C46 C47 H47A 119.2 . . ? C48 C47 H47A 119.2 . . ? C47 C48 C49 120.8(12) . . ? C47 C48 H48A 119.6 . . ? C49 C48 H48A 119.6 . . ? O14 C49 C48 125.3(11) . . ? O14 C49 C50 116.0(9) . . ? C48 C49 C50 118.7(10) . . ? O13 C50 C49 116.8(8) . . ? O13 C50 C45 122.3(11) . . ? C49 C50 C45 120.6(10) . . ? O18 C51 C52 116.3(8) . . ? O18 C51 C56 120.2(9) . . ? C52 C51 C56 123.5(8) . . ? O17 C52 C51 118.2(8) . . ? O17 C52 C53 125.7(9) . . ? C51 C52 C53 116.0(9) . . ? C54 C53 C52 122.5(11) . . ? C54 C53 H53A 118.8 . . ? C52 C53 H53A 118.8 . . ? C53 C54 C55 120.1(11) . . ? C53 C54 H54A 120.0 . . ? C55 C54 H54A 120.0 . . ? C54 C55 C56 122.7(10) . . ? C54 C55 H55A 118.6 . . ? C56 C55 H55A 118.6 . . ? C55 C56 C57 120.6(10) . . ? C55 C56 C51 115.1(10) . . ? C57 C56 C51 124.0(9) . . ? N8 C57 C56 126.8(10) . . ? N8 C57 H57A 116.6 . . ? C56 C57 H57A 116.6 . . ? C67 C58 N8 116.6(10) . . ? C67 C58 H58A 108.1 . . ? N8 C58 H58A 108.1 . . ? C67 C58 H58B 108.1 . . ? N8 C58 H58B 108.1 . . ? H58A C58 H58B 107.3 . . ? C67 C59 N7 110.1(12) . . ? C67 C59 H59A 109.6 . . ? N7 C59 H59A 109.6 . . ? C67 C59 H59B 109.6 . . ? N7 C59 H59B 109.6 . . ? H59A C59 H59B 108.2 . . ? C65 C60 C61 121.2(11) . . ? C65 C60 H60A 119.4 . . ? C61 C60 H60A 119.4 . . ? C62 C61 C60 120.8(10) . . ? C62 C61 H61A 119.6 . . ? C60 C61 H61A 119.6 . . ? C61 C62 C63 119.9(11) . . ? C61 C62 H62A 120.1 . . ? C63 C62 H62A 120.1 . . ? C64 C63 C62 119.3(10) . . ? C64 C63 C68 121.0(9) . . ? C62 C63 C68 119.5(10) . . ? O16 C64 C63 123.1(9) . . ? O16 C64 C65 114.9(8) . . ? C63 C64 C65 121.9(9) . . ? O15 C65 C60 124.8(9) . . ? O15 C65 C64 118.2(8) . . ? C60 C65 C64 116.9(10) . . ? C43 C66 C42 112.3(15) . . ? C43 C66 H66A 109.1 . . ? C42 C66 H66A 109.1 . . ? C43 C66 H66B 109.1 . . ? C42 C66 H66B 109.1 . . ? H66A C66 H66B 107.9 . . ? C58 C67 C59 115.6(13) . . ? C58 C67 H67A 108.4 . . ? C59 C67 H67A 108.4 . . ? C58 C67 H67B 108.4 . . ? C59 C67 H67B 108.4 . . ? H67A C67 H67B 107.4 . . ? N7 C68 C63 129.7(11) . . ? N7 C68 H68A 115.2 . . ? C63 C68 H68A 115.2 . . ? C9 C69 C8 119.6(14) . . ? C9 C69 H69A 107.4 . . ? C8 C69 H69A 107.4 . . ? C9 C69 H69B 107.4 . . ? C8 C69 H69B 107.4 . . ? H69A C69 H69B 106.9 . . ? C24 C70 C25 115.0(11) . . ? C24 C70 H70A 108.5 . . ? C25 C70 H70A 108.5 . . ? C24 C70 H70B 108.5 . . ? C25 C70 H70B 108.5 . . ? H70A C70 H70B 107.5 . . ? C7 N1 C8 117.2(10) . . ? C7 N1 Cu1 123.3(7) . . ? C8 N1 Cu1 119.2(8) . . ? C10 N2 C9 115.3(9) . . ? C10 N2 Cu1 120.2(7) . . ? C9 N2 Cu1 123.4(8) . . ? C23 N3 C24 114.9(9) . . ? C23 N3 Cu3 121.8(7) . . ? C24 N3 Cu3 122.3(7) . . ? C26 N4 C25 116.0(9) . . ? C26 N4 Cu3 121.7(7) . . ? C25 N4 Cu3 121.8(7) . . ? C41 N5 C42 112.6(12) . . ? C41 N5 Cu7 120.5(9) . . ? C42 N5 Cu7 126.7(9) . . ? C44 N6 C43 117.8(10) . . ? C44 N6 Cu7 121.0(8) . . ? C43 N6 Cu7 120.1(8) . . ? C68 N7 C59 118.5(11) . . ? C68 N7 Cu5 122.6(8) . . ? C59 N7 Cu5 118.8(8) . . ? C57 N8 C58 115.5(9) . . ? C57 N8 Cu5 119.6(7) . . ? C58 N8 Cu5 124.6(8) . . ? C2 O1 Cu2 109.7(6) . . ? C1 O2 Cu1 122.0(5) . . ? C1 O2 Cu2 107.4(6) . . ? Cu1 O2 Cu2 126.9(3) . . ? C16 O3 Cu4 110.1(6) . . ? C16 O3 Cu1 119.2(6) . . ? Cu4 O3 Cu1 125.5(3) . . ? C15 O4 Cu4 109.8(6) . . ? C17 O5 Cu2 109.2(5) . . ? C17 O5 Cu3 123.3(6) . . ? Cu2 O5 Cu3 124.3(3) . . ? C18 O6 Cu2 111.2(6) . . ? C31 O7 Cu4 111.8(6) . . ? C32 O8 Cu4 109.9(5) . . ? C32 O8 Cu3 122.1(6) . . ? Cu4 O8 Cu3 124.9(3) . . ? C35 O11 Cu8 109.7(6) . . ? C35 O11 Cu7 121.9(7) . . ? Cu8 O11 Cu7 125.2(3) . . ? C36 O12 Cu8 111.8(6) . . ? C50 O13 Cu6 108.2(6) . . ? C50 O13 Cu7 120.1(6) . . ? Cu6 O13 Cu7 128.3(3) . . ? C49 O14 Cu6 111.7(6) . . ? C65 O15 Cu8 111.7(6) . . ? C64 O16 Cu8 108.1(6) . . ? C64 O16 Cu5 122.9(6) . . ? Cu8 O16 Cu5 127.4(3) . . ? C52 O17 Cu6 111.5(6) . . ? C51 O18 Cu5 121.4(6) . . ? C51 O18 Cu6 107.1(6) . . ? Cu5 O18 Cu6 127.2(3) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.836 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.143