# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'George Christou' _publ_contact_author_email CHRISTOU@CHEM.UFL.EDU _publ_section_title ; Initial employment of ?-benzoin oxime as a route to high-nuclearity metal clusters: Decanuclear CuII complexes with a wheel topology ; loop_ _publ_author_name 'George Christou' 'Spyros Perlepes' 'Catherine Raptopoulou' 'Theocharis Stamatatos' ; G.C.Vlahopoulou ; # Attachment 'Cu10_complex_11.cif' data_pegv427 _database_code_depnum_ccdc_archive 'CCDC 717731' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C188 H226 Cu10 N26 O38' _chemical_formula_weight 4093.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 '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 17.6557(3) _cell_length_b 17.9324(3) _cell_length_c 18.0189(3) _cell_angle_alpha 67.5200(10) _cell_angle_beta 85.5750(10) _cell_angle_gamma 65.9770(10) _cell_volume 4793.97(14) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parall _exptl_crystal_colour dark _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2130 _exptl_absorpt_coefficient_mu 1.831 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.613 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IPDS' _diffrn_measurement_method '\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.2 _diffrn_reflns_number 64502 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 6.82 _diffrn_reflns_theta_max 65.00 _reflns_number_total 15688 _reflns_number_gt 13346 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Rigaku MSC, 2005' _computing_cell_refinement 'CrystalClear, Rigaku MSC, 2005' _computing_data_reduction 'CrystalClear, Rigaku MSC, 2005' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1048P)^2^+5.6241P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15688 _refine_ls_number_parameters 1378 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.0751 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.1959 _refine_ls_wR_factor_gt 0.1892 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.034 _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 0.70742(3) 0.60865(4) -0.05606(4) 0.03719(17) Uani 1 1 d . . . Cu2 Cu 0.71896(3) 0.65074(4) 0.09809(4) 0.03893(17) Uani 1 1 d . . . Cu3 Cu 0.84088(3) 0.60768(4) 0.24219(4) 0.04165(18) Uani 1 1 d . . . Cu4 Cu 1.03449(3) 0.54230(4) 0.26816(4) 0.03707(17) Uani 1 1 d . . . Cu5 Cu 1.21236(3) 0.44092(4) 0.20947(4) 0.03685(17) Uani 1 1 d . . . N1 N 0.7437(2) 0.5452(2) 0.1957(2) 0.0408(8) Uani 1 1 d . . . O1 O 0.68220(17) 0.58833(18) 0.05414(17) 0.0391(6) Uani 1 1 d . . . O2 O 0.78373(18) 0.5305(2) 0.26422(18) 0.0478(7) Uani 1 1 d . . . C1 C 0.7234(2) 0.4850(3) 0.1920(3) 0.0419(10) Uani 1 1 d . . . C2 C 0.6788(3) 0.5097(3) 0.1122(3) 0.0416(10) Uani 1 1 d . . . C3 C 0.7369(3) 0.3990(3) 0.2592(3) 0.0476(11) Uani 1 1 d . . . C4 C 0.7141(4) 0.3950(4) 0.3355(3) 0.0568(13) Uani 1 1 d . . . C5 C 0.7258(4) 0.3132(5) 0.3957(4) 0.0745(19) Uani 1 1 d . . . C6 C 0.7593(4) 0.2378(4) 0.3803(4) 0.0750(19) Uani 1 1 d . . . C7 C 0.7817(4) 0.2418(4) 0.3055(4) 0.0754(17) Uani 1 1 d . . . C8 C 0.7702(3) 0.3221(3) 0.2447(4) 0.0604(13) Uani 1 1 d . . . C9 C 0.5890(3) 0.5204(3) 0.1222(3) 0.0450(10) Uani 1 1 d . . . C10 C 0.5374(3) 0.5771(4) 0.1573(4) 0.0651(14) Uani 1 1 d . . . C11 C 0.4550(4) 0.5890(5) 0.1657(4) 0.0766(18) Uani 1 1 d . . . C12 C 0.4238(4) 0.5435(4) 0.1385(4) 0.0736(17) Uani 1 1 d . . . C13 C 0.4744(4) 0.4875(5) 0.1045(4) 0.0780(18) Uani 1 1 d . . . H13 H 0.4531 0.4560 0.0862 0.101 Uiso 1 1 calc R . . C14 C 0.5572(4) 0.4755(4) 0.0963(4) 0.0666(15) Uani 1 1 d . . . N21 N 0.7042(2) 0.7228(2) -0.0666(2) 0.0386(8) Uani 1 1 d . . . O21 O 0.72482(17) 0.65007(17) -0.16806(17) 0.0412(6) Uani 1 1 d . . . O22 O 0.69928(19) 0.7469(2) -0.00248(18) 0.0471(7) Uani 1 1 d . . . C21 C 0.7195(3) 0.7385(3) -0.2021(3) 0.0387(9) Uani 1 1 d . . . C22 C 0.7149(2) 0.7721(3) -0.1366(3) 0.0372(9) Uani 1 1 d . . . C23 C 0.6445(3) 0.7975(3) -0.2644(3) 0.0420(10) Uani 1 1 d . . . C24 C 0.6542(3) 0.8166(3) -0.3454(3) 0.0520(11) Uani 1 1 d . . . C25 C 0.5858(4) 0.8653(4) -0.4034(4) 0.0701(15) Uani 1 1 d . . . C26 C 0.5073(4) 0.8972(4) -0.3782(4) 0.0731(17) Uani 1 1 d . . . C27 C 0.4966(3) 0.8793(4) -0.2986(4) 0.0666(15) Uani 1 1 d . . . C28 C 0.5642(3) 0.8301(3) -0.2409(3) 0.0519(11) Uani 1 1 d . . . C29 C 0.7215(3) 0.8570(3) -0.1536(3) 0.0444(10) Uani 1 1 d . . . C30 C 0.7848(4) 0.8749(4) -0.1960(4) 0.0649(14) Uani 1 1 d . . . C31 C 0.7926(5) 0.9529(5) -0.2085(5) 0.088(2) Uani 1 1 d . . . C32 C 0.7350(5) 1.0150(4) -0.1830(4) 0.0832(19) Uani 1 1 d . . . C33 C 0.6702(4) 0.9991(4) -0.1432(4) 0.0707(15) Uani 1 1 d . . . C34 C 0.6639(3) 0.9202(3) -0.1276(3) 0.0536(12) Uani 1 1 d . . . N41 N 1.22605(19) 0.5285(2) 0.1077(2) 0.0389(8) Uani 1 1 d . . . O41 O 1.13636(16) 0.54657(17) 0.22463(18) 0.0410(7) Uani 1 1 d . . . O42 O 1.26885(18) 0.50825(18) 0.04646(18) 0.0435(7) Uani 1 1 d . . . C41 C 1.1350(3) 0.6273(3) 0.1650(3) 0.0413(10) Uani 1 1 d . . . C42 C 1.1799(2) 0.6101(3) 0.0939(3) 0.0400(9) Uani 1 1 d . . . C43 C 1.1739(3) 0.6705(3) 0.1994(3) 0.0448(10) Uani 1 1 d . . . C44 C 1.1417(4) 0.7624(3) 0.1718(4) 0.0606(13) Uani 1 1 d . . . C45 C 1.1752(5) 0.8021(4) 0.2054(4) 0.0779(18) Uani 1 1 d . . . C46 C 1.2396(4) 0.7526(4) 0.2633(4) 0.0733(17) Uani 1 1 d . . . C47 C 1.2730(3) 0.6617(4) 0.2905(4) 0.0610(14) Uani 1 1 d . . . C48 C 1.2396(3) 0.6215(4) 0.2582(3) 0.0517(12) Uani 1 1 d . . . C49 C 1.1660(3) 0.6864(3) 0.0171(3) 0.0450(10) Uani 1 1 d . . . C50 C 1.0857(4) 0.7496(3) -0.0131(3) 0.0592(13) Uani 1 1 d . . . C51 C 1.0707(4) 0.8204(4) -0.0870(4) 0.0767(17) Uani 1 1 d . . . H51 H 1.0152 0.8619 -0.1077 0.100 Uiso 1 1 calc R . . C52 C 1.1355(5) 0.8301(4) -0.1295(4) 0.0795(18) Uani 1 1 d . . . C53 C 1.2160(5) 0.7696(4) -0.1001(4) 0.0703(16) Uani 1 1 d . . . C54 C 1.2317(3) 0.6970(3) -0.0275(3) 0.0555(12) Uani 1 1 d . . . N61 N 1.08734(19) 0.4130(2) 0.3036(2) 0.0369(7) Uani 1 1 d . . . O61 O 0.93993(15) 0.52053(17) 0.31419(17) 0.0393(6) Uani 1 1 d . . . O62 O 1.16476(16) 0.36733(17) 0.28735(18) 0.0420(7) Uani 1 1 d . . . C61 C 0.9534(2) 0.4295(3) 0.3483(3) 0.0399(9) Uani 1 1 d . . . C62 C 1.0383(2) 0.3736(3) 0.3310(3) 0.0372(9) Uani 1 1 d . . . C63 C 0.9453(3) 0.3990(3) 0.4386(3) 0.0451(10) Uani 1 1 d . . . C64 C 0.8799(5) 0.3774(6) 0.4695(5) 0.101(3) Uani 1 1 d . . . C65 C 0.8724(7) 0.3510(8) 0.5513(6) 0.141(4) Uani 1 1 d . . . H65 H 0.8251 0.3400 0.5716 0.183 Uiso 1 1 calc R . . C66 C 0.9308(6) 0.3404(5) 0.6032(5) 0.100(3) Uani 1 1 d . . . C67 C 0.9959(4) 0.3623(4) 0.5745(4) 0.0795(18) Uani 1 1 d . . . H67 H 1.0353 0.3589 0.6101 0.103 Uiso 1 1 calc R . . C68 C 1.0033(3) 0.3898(4) 0.4916(3) 0.0679(16) Uani 1 1 d . . . C69 C 1.0584(3) 0.2804(3) 0.3449(3) 0.0449(10) Uani 1 1 d . . . C70 C 1.0056(3) 0.2607(3) 0.3090(3) 0.0562(12) Uani 1 1 d . . . C71 C 1.0245(4) 0.1747(4) 0.3198(4) 0.0712(16) Uani 1 1 d . . . C72 C 1.0937(4) 0.1071(4) 0.3680(4) 0.0750(17) Uani 1 1 d . . . C73 C 1.1461(4) 0.1255(3) 0.4054(4) 0.0691(16) Uani 1 1 d . . . C74 C 1.1283(3) 0.2110(3) 0.3939(3) 0.0518(12) Uani 1 1 d . . . N81 N 0.89474(19) 0.6901(2) 0.2025(2) 0.0387(8) Uani 1 1 d . . . O81 O 0.75691(16) 0.69915(18) 0.15702(17) 0.0402(6) Uani 1 1 d . . . O82 O 0.97393(16) 0.66838(18) 0.22951(18) 0.0430(7) Uani 1 1 d . . . C81 C 0.8523(2) 0.7672(3) 0.1479(3) 0.0388(9) Uani 1 1 d . . . C82 C 0.7670(2) 0.7800(3) 0.1211(3) 0.0394(9) Uani 1 1 d . . . C83 C 0.8775(2) 0.8414(3) 0.1115(3) 0.0480(11) Uani 1 1 d . . . C84 C 0.9215(3) 0.8618(4) 0.1562(4) 0.0610(14) Uani 1 1 d . . . C85 C 0.9361(4) 0.9376(4) 0.1226(4) 0.0712(16) Uani 1 1 d . . . C86 C 0.9097(4) 0.9936(4) 0.0454(5) 0.0783(19) Uani 1 1 d . . . C87 C 0.8702(5) 0.9725(4) -0.0019(5) 0.085(2) Uani 1 1 d . . . C88 C 0.8528(4) 0.8977(4) 0.0318(4) 0.0674(15) Uani 1 1 d . . . C89 C 0.6972(2) 0.8517(3) 0.1407(3) 0.0436(10) Uani 1 1 d . . . C90 C 0.6978(3) 0.8604(4) 0.2134(4) 0.0669(15) Uani 1 1 d . . . C91 C 0.6312(4) 0.9231(5) 0.2317(5) 0.0784(19) Uani 1 1 d . . . C92 C 0.5628(4) 0.9776(4) 0.1772(5) 0.0780(19) Uani 1 1 d . . . C93 C 0.5604(4) 0.9714(5) 0.1054(5) 0.088(2) Uani 1 1 d . . . C94 C 0.6278(3) 0.9086(4) 0.0861(4) 0.0679(15) Uani 1 1 d . . . N101 N 1.4683(2) 0.3577(3) 0.3135(3) 0.0687(13) Uani 1 1 d D . . O101 O 1.32898(18) 0.4083(2) 0.2894(2) 0.0536(8) Uani 1 1 d D . . C101 C 1.4006(3) 0.3663(3) 0.2779(3) 0.0535(12) Uani 1 1 d D . . H101 H 1.4079 0.3381 0.2411 0.070 Uiso 1 1 calc R . . C102 C 1.4627(5) 0.4078(5) 0.3625(5) 0.101(2) Uani 1 1 d D . . H10A H 1.5104 0.3750 0.4034 0.132 Uiso 1 1 calc R . . H10B H 1.4110 0.4170 0.3891 0.132 Uiso 1 1 calc R . . H10C H 1.4629 0.4653 0.3280 0.132 Uiso 1 1 calc R . . C103 C 1.5509(3) 0.3098(5) 0.2934(5) 0.093(2) Uani 1 1 d D . . H10D H 1.5846 0.2619 0.3426 0.120 Uiso 1 1 calc R . . H10E H 1.5779 0.3505 0.2687 0.120 Uiso 1 1 calc R . . H10F H 1.5455 0.2848 0.2553 0.120 Uiso 1 1 calc R . . N111 N 0.7604(3) 0.6387(4) 0.4839(4) 0.0818(15) Uani 1 1 d . . . O111 O 0.7786(4) 0.6640(4) 0.3471(4) 0.1185(18) Uani 1 1 d . . . C111 C 0.7984(4) 0.6240(5) 0.4197(4) 0.0815(18) Uani 1 1 d . . . H111 H 0.8498 0.5733 0.4335 0.106 Uiso 1 1 calc R . . C112 C 0.7887(6) 0.5682(8) 0.5627(5) 0.140(4) Uani 1 1 d . . . H11A H 0.7809 0.5936 0.6036 0.182 Uiso 1 1 calc R . . H11B H 0.8478 0.5309 0.5643 0.182 Uiso 1 1 calc R . . H11C H 0.7564 0.5324 0.5737 0.182 Uiso 1 1 calc R . . C113 C 0.6977(9) 0.7322(11) 0.4735(10) 0.286(11) Uani 1 1 d . . . H11D H 0.6957 0.7390 0.5251 0.371 Uiso 1 1 calc R . . H11E H 0.6424 0.7414 0.4557 0.371 Uiso 1 1 calc R . . H11F H 0.7151 0.7758 0.4331 0.371 Uiso 1 1 calc R . . N121 N 0.5370(4) 0.6953(5) 0.2956(5) 0.132(3) Uani 1 1 d D . . O121 O 0.5422 0.5818 0.3992 0.317 Uani 1 1 d D . . C121 C 0.5841 0.6178 0.3580 0.155 Uani 1 1 d D . . H121 H 0.6428 0.5953 0.3674 0.202 Uiso 1 1 calc R . . C122 C 0.5797(7) 0.7389(8) 0.2403(8) 0.209(7) Uani 1 1 d D . . H12A H 0.5576 0.7555 0.1853 0.271 Uiso 1 1 calc R . . H12B H 0.6391 0.6996 0.2480 0.271 Uiso 1 1 calc R . . H12C H 0.5725 0.7922 0.2486 0.271 Uiso 1 1 calc R . . C123 C 0.4487(5) 0.7308(10) 0.2879(9) 0.244(9) Uani 1 1 d D . . H12D H 0.4297 0.6918 0.3321 0.317 Uiso 1 1 calc R . . H12E H 0.4291 0.7356 0.2362 0.317 Uiso 1 1 calc R . . H12F H 0.4264 0.7896 0.2902 0.317 Uiso 1 1 calc R . . N131 N 0.0257(4) 0.9226(4) 0.3997(4) 0.0953(18) Uani 1 1 d . . . O131 O 0.0188(5) 0.9899(5) 0.2648(4) 0.149(3) Uani 1 1 d . . . C131 C 0.0549(7) 0.9278(7) 0.3319(6) 0.128(3) Uani 1 1 d . . . H131 H 0.1070 0.8824 0.3314 0.166 Uiso 1 1 calc R . . C132 C 0.0614(7) 0.8582(7) 0.4762(6) 0.179(6) Uani 1 1 d . . . H13A H 0.0312 0.8201 0.4957 0.233 Uiso 1 1 calc R . . H13B H 0.0582 0.8871 0.5136 0.233 Uiso 1 1 calc R . . H13C H 0.1199 0.8224 0.4731 0.233 Uiso 1 1 calc R . . C133 C -0.0557(6) 0.9945(7) 0.3958(8) 0.156(4) Uani 1 1 d . . . H13D H -0.0957 0.9692 0.4206 0.203 Uiso 1 1 calc R . . H13E H -0.0756 1.0337 0.3394 0.203 Uiso 1 1 calc R . . H13F H -0.0498 1.0283 0.4251 0.203 Uiso 1 1 calc R . . N171 N 0.9853(3) 0.4281(4) 0.0941(3) 0.0842(15) Uani 1 1 d . . . O171 O 0.9596(12) 0.5444(6) 0.1241(7) 0.291(10) Uani 1 1 d . . . C171 C 1.0012(14) 0.4786(13) 0.1246(6) 0.235(11) Uani 1 1 d . . . H171 H 1.0558 0.4542 0.1502 0.306 Uiso 1 1 calc R . . C172 C 0.9092(5) 0.4355(7) 0.0719(6) 0.137(4) Uani 1 1 d . . . H17A H 0.9065 0.3776 0.0967 0.178 Uiso 1 1 calc R . . H17B H 0.9015 0.4562 0.0130 0.178 Uiso 1 1 calc R . . H17C H 0.8651 0.4779 0.0900 0.178 Uiso 1 1 calc R . . C173 C 1.0560(6) 0.3489(8) 0.0849(8) 0.192(6) Uani 1 1 d . . . H17D H 1.0461 0.2955 0.1142 0.249 Uiso 1 1 calc R . . H17E H 1.1087 0.3416 0.1070 0.249 Uiso 1 1 calc R . . H17F H 1.0588 0.3585 0.0277 0.249 Uiso 1 1 calc R . . N181 N 0.3925(4) 0.8829(4) 0.4085(4) 0.110(2) Uani 1 1 d D . . O181 O 0.2709(9) 0.8784(12) 0.4266(9) 0.416(15) Uani 1 1 d D . . C181 C 0.3100(8) 0.9258(9) 0.4067(12) 0.41(2) Uani 1 1 d D . . H181 H 0.2834 0.9881 0.3913 0.528 Uiso 1 1 calc R . . C182 C 0.4402(11) 0.7994(7) 0.4666(10) 0.308(13) Uani 1 1 d D . . H18A H 0.4891 0.7688 0.4432 0.401 Uiso 1 1 calc R . . H18B H 0.4065 0.7647 0.4844 0.401 Uiso 1 1 calc R . . H18C H 0.4582 0.8061 0.5129 0.401 Uiso 1 1 calc R . . C183 C 0.4394(11) 0.9315(10) 0.3596(9) 0.277(11) Uani 1 1 d D . . H18D H 0.4644 0.9076 0.3187 0.360 Uiso 1 1 calc R . . H18E H 0.4835 0.9256 0.3942 0.360 Uiso 1 1 calc R . . H18F H 0.4020 0.9942 0.3331 0.360 Uiso 1 1 calc R . . OW1 O 0.4080(8) 0.5805(10) 0.4730(6) 0.269(6) Uani 1 1 d . . . N141 N 0.5805 1.1944 0.0211 0.142 Uani 1 1 d . . . O141 O 0.5453 1.1764 -0.0852 0.601 Uani 1 1 d . . . C141 C 0.5198 1.1948 -0.0291 0.287 Uani 1 1 d . . . H141 H 0.4634 1.2090 -0.0177 0.373 Uiso 1 1 d . . . C142 C 0.6637 1.1394 0.0222 0.277 Uani 1 1 d . . . H14A H 0.6851 1.0957 0.0777 0.360 Uiso 1 1 d . . . H14B H 0.6969 1.1736 0.0030 0.360 Uiso 1 1 d . . . H14C H 0.6678 1.1067 -0.0126 0.360 Uiso 1 1 d . . . C143 C 0.5565 1.2547 0.0641 0.174 Uani 1 1 d . . . H14D H 0.5814 1.2215 0.1200 0.226 Uiso 1 1 d . . . H14E H 0.4957 1.2814 0.0634 0.226 Uiso 1 1 d . . . H14F H 0.5764 1.3014 0.0375 0.226 Uiso 1 1 d . . . N95 N 0.7823(7) 0.9459(9) 0.3458(8) 0.074(4) Uani 0.557(13) 1 d PD A 1 O95 O 0.7062(7) 0.9163(11) 0.4502(8) 0.152(6) Uani 0.557(13) 1 d PD A 1 C95 C 0.7252(9) 0.9702(15) 0.3959(9) 0.130(11) Uani 0.557(13) 1 d PD A 1 H95 H 0.6992 1.0307 0.3887 0.169 Uiso 0.557(13) 1 calc PR A 1 C96 C 0.8446(10) 0.8567(12) 0.3705(13) 0.115(6) Uani 0.557(13) 1 d PD A 1 C97 C 0.777(2) 1.0086(18) 0.2651(10) 0.197(18) Uani 0.557(13) 1 d PD A 1 N95A N 0.760(2) 0.9926(16) 0.322(2) 0.28(4) Uani 0.443(13) 1 d PD A 2 O95A O 0.6828(17) 1.1142(12) 0.2091(18) 0.31(2) Uani 0.443(13) 1 d PD A 2 C95A C 0.739(2) 1.040(2) 0.2412(18) 0.43(7) Uani 0.443(13) 1 d PD A 2 H95A H 0.7705 1.0134 0.2062 0.555 Uiso 0.443(13) 1 calc PR A 2 C96A C 0.797(4) 0.8991(18) 0.360(3) 0.29(4) Uani 0.443(13) 1 d PD A 2 C97A C 0.727(2) 1.044(3) 0.372(3) 0.25(2) Uani 0.443(13) 1 d PD A 2 H2 H 0.705(3) 0.465(3) 0.099(3) 0.042(13) Uiso 1 1 d . . . H4 H 0.688(4) 0.449(4) 0.336(4) 0.078(19) Uiso 1 1 d . . . H5 H 0.712(4) 0.311(5) 0.441(5) 0.10(3) Uiso 1 1 d . . . H6 H 0.769(4) 0.184(4) 0.430(4) 0.088(19) Uiso 1 1 d . . . H7 H 0.808(3) 0.188(4) 0.300(3) 0.066(16) Uiso 1 1 d . . . H8 H 0.788(3) 0.326(3) 0.198(3) 0.054(16) Uiso 1 1 d . . . H10 H 0.564(3) 0.608(4) 0.172(3) 0.068(16) Uiso 1 1 d . . . H11 H 0.419(4) 0.623(4) 0.190(4) 0.09(2) Uiso 1 1 d . . . H12 H 0.360(5) 0.550(5) 0.1575 0.13(3) Uiso 1 1 d . . . H14 H 0.589(4) 0.439(4) 0.072(4) 0.09(2) Uiso 1 1 d . . . H21 H 0.766(3) 0.736(3) -0.229(3) 0.034(10) Uiso 1 1 d . . . H24 H 0.710(3) 0.794(3) -0.366(3) 0.046(12) Uiso 1 1 d . . . H25 H 0.584(4) 0.874(4) -0.461(4) 0.076(18) Uiso 1 1 d . . . H26 H 0.467(3) 0.925(4) -0.420(3) 0.065(16) Uiso 1 1 d . . . H27 H 0.448(4) 0.891(4) -0.278(4) 0.071(17) Uiso 1 1 d . . . H28 H 0.558(3) 0.814(3) -0.183(3) 0.049(13) Uiso 1 1 d . . . H30 H 0.823(3) 0.835(4) -0.214(3) 0.062(16) Uiso 1 1 d . . . H31 H 0.827(5) 0.966(5) -0.245(5) 0.12(3) Uiso 1 1 d . . . H32 H 0.738(4) 1.073(4) -0.192(4) 0.090(19) Uiso 1 1 d . . . H33 H 0.627(4) 1.041(5) -0.111(4) 0.11(2) Uiso 1 1 d . . . H34 H 0.616(3) 0.911(3) -0.103(3) 0.045(12) Uiso 1 1 d . . . H41 H 1.082(3) 0.664(3) 0.147(2) 0.035(11) Uiso 1 1 d . . . H44 H 1.096(3) 0.796(3) 0.132(3) 0.058(15) Uiso 1 1 d . . . H45 H 1.153(4) 0.857(4) 0.187(3) 0.069(17) Uiso 1 1 d . . . H46 H 1.258(3) 0.788(4) 0.280(3) 0.067(15) Uiso 1 1 d . . . H47 H 1.314(4) 0.637(4) 0.329(4) 0.08(2) Uiso 1 1 d . . . H48 H 1.261(3) 0.575(3) 0.272(3) 0.045(15) Uiso 1 1 d . . . H50 H 1.047(3) 0.743(3) 0.014(3) 0.037(12) Uiso 1 1 d . . . H52 H 1.120(4) 0.885(4) -0.184(4) 0.087(19) Uiso 1 1 d . . . H53 H 1.258(4) 0.778(4) -0.127(4) 0.078(19) Uiso 1 1 d . . . H54 H 1.290(3) 0.654(3) -0.013(3) 0.055(14) Uiso 1 1 d . . . H61 H 0.914(2) 0.420(2) 0.325(2) 0.026(9) Uiso 1 1 d . . . H64 H 0.850(4) 0.372(4) 0.438(4) 0.09(2) Uiso 1 1 d . . . H66 H 0.928(4) 0.330(4) 0.648(4) 0.065(18) Uiso 1 1 d . . . H68 H 1.057(4) 0.394(4) 0.473(4) 0.09(2) Uiso 1 1 d . . . H70 H 0.957(4) 0.312(4) 0.277(4) 0.09(2) Uiso 1 1 d . . . H71 H 0.983(4) 0.160(4) 0.305(4) 0.086(19) Uiso 1 1 d . . . H72 H 1.098(4) 0.041(4) 0.378(4) 0.10(2) Uiso 1 1 d . . . H73 H 1.199(5) 0.076(6) 0.437(5) 0.14(3) Uiso 1 1 d . . . H74 H 1.159(3) 0.223(3) 0.422(3) 0.058(15) Uiso 1 1 d . . . H82 H 0.765(2) 0.790(2) 0.069(3) 0.026(10) Uiso 1 1 d . . . H84 H 0.934(4) 0.834(4) 0.207(4) 0.08(2) Uiso 1 1 d . . . H85 H 0.969(4) 0.946(4) 0.160(4) 0.075(17) Uiso 1 1 d . . . H86 H 0.905(3) 1.053(3) 0.021(3) 0.059(14) Uiso 1 1 d . . . H87 H 0.833(6) 1.022(6) -0.038(6) 0.14(3) Uiso 1 1 d . . . H88 H 0.825(4) 0.882(4) 0.003(4) 0.078(19) Uiso 1 1 d . . . H90 H 0.739(4) 0.820(4) 0.250(4) 0.078(19) Uiso 1 1 d . . . H91 H 0.627(6) 0.917(6) 0.280(6) 0.14(4) Uiso 1 1 d . . . H92 H 0.526(4) 1.020(4) 0.188(3) 0.066(17) Uiso 1 1 d . . . H93 H 0.507(6) 0.980(6) 0.073(6) 0.17(4) Uiso 1 1 d . . . H94 H 0.626(3) 0.908(3) 0.038(3) 0.047(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0343(3) 0.0403(3) 0.0395(4) -0.0138(3) 0.0058(2) -0.0196(3) Cu2 0.0367(3) 0.0433(3) 0.0412(4) -0.0148(3) 0.0046(3) -0.0221(3) Cu3 0.0349(3) 0.0452(3) 0.0450(4) -0.0104(3) -0.0010(3) -0.0223(3) Cu4 0.0276(3) 0.0391(3) 0.0466(4) -0.0151(3) 0.0057(2) -0.0173(2) Cu5 0.0299(3) 0.0387(3) 0.0426(4) -0.0147(3) 0.0067(2) -0.0162(2) N1 0.0321(17) 0.056(2) 0.040(2) -0.0164(16) 0.0056(14) -0.0246(16) O1 0.0457(15) 0.0479(15) 0.0346(16) -0.0172(12) 0.0092(12) -0.0292(13) O2 0.0447(16) 0.0553(17) 0.0447(18) -0.0071(14) -0.0055(13) -0.0314(14) C1 0.035(2) 0.046(2) 0.045(3) -0.0123(19) 0.0075(18) -0.0224(18) C2 0.042(2) 0.043(2) 0.044(3) -0.0124(19) 0.0035(18) -0.0240(19) C3 0.037(2) 0.051(2) 0.052(3) -0.006(2) -0.0036(19) -0.0272(19) C4 0.070(3) 0.062(3) 0.043(3) -0.011(2) 0.002(2) -0.040(3) C5 0.090(4) 0.091(5) 0.050(4) -0.003(3) -0.006(3) -0.064(4) C6 0.067(3) 0.060(3) 0.079(5) 0.009(3) -0.022(3) -0.037(3) C7 0.074(4) 0.050(3) 0.083(5) -0.007(3) 0.005(3) -0.023(3) C8 0.059(3) 0.049(3) 0.069(4) -0.015(3) 0.006(3) -0.025(2) C9 0.042(2) 0.055(2) 0.040(3) -0.0107(19) 0.0075(18) -0.029(2) C10 0.045(3) 0.086(4) 0.082(4) -0.043(3) 0.018(3) -0.036(3) C11 0.045(3) 0.096(5) 0.089(5) -0.036(4) 0.018(3) -0.032(3) C12 0.051(3) 0.101(4) 0.064(4) -0.010(3) 0.002(3) -0.047(3) C13 0.062(3) 0.117(5) 0.087(5) -0.047(4) 0.015(3) -0.061(4) C14 0.061(3) 0.096(4) 0.071(4) -0.041(3) 0.013(3) -0.052(3) N21 0.0381(17) 0.0459(18) 0.038(2) -0.0187(15) 0.0057(14) -0.0215(15) O21 0.0417(15) 0.0370(14) 0.0437(17) -0.0125(12) 0.0071(12) -0.0182(12) O22 0.0568(18) 0.0530(17) 0.0418(18) -0.0215(14) 0.0076(14) -0.0295(15) C21 0.035(2) 0.041(2) 0.040(2) -0.0132(18) 0.0084(18) -0.0192(17) C22 0.0301(19) 0.042(2) 0.039(2) -0.0144(17) 0.0051(16) -0.0162(17) C23 0.038(2) 0.037(2) 0.048(3) -0.0137(18) 0.0029(18) -0.0143(17) C24 0.047(3) 0.056(3) 0.043(3) -0.014(2) 0.003(2) -0.017(2) C25 0.063(3) 0.078(4) 0.056(4) -0.020(3) -0.006(3) -0.019(3) C26 0.057(3) 0.075(4) 0.069(4) -0.026(3) -0.019(3) -0.006(3) C27 0.038(3) 0.077(4) 0.073(4) -0.032(3) -0.001(3) -0.008(3) C28 0.043(2) 0.060(3) 0.048(3) -0.025(2) 0.007(2) -0.013(2) C29 0.040(2) 0.041(2) 0.047(3) -0.0106(18) 0.0018(19) -0.0171(18) C30 0.072(3) 0.062(3) 0.074(4) -0.031(3) 0.031(3) -0.040(3) C31 0.101(5) 0.080(4) 0.111(6) -0.040(4) 0.049(4) -0.067(4) C32 0.113(5) 0.059(3) 0.092(5) -0.025(3) 0.020(4) -0.055(4) C33 0.085(4) 0.049(3) 0.077(4) -0.024(3) 0.009(3) -0.028(3) C34 0.055(3) 0.046(2) 0.057(3) -0.018(2) 0.006(2) -0.020(2) N41 0.0310(16) 0.0449(19) 0.047(2) -0.0220(16) 0.0101(15) -0.0180(15) O41 0.0349(14) 0.0405(14) 0.0492(18) -0.0148(13) 0.0093(12) -0.0201(12) O42 0.0471(16) 0.0421(15) 0.0476(18) -0.0187(13) 0.0137(13) -0.0246(13) C41 0.033(2) 0.039(2) 0.051(3) -0.0143(19) 0.0110(19) -0.0172(18) C42 0.035(2) 0.045(2) 0.045(3) -0.0145(18) 0.0064(17) -0.0233(18) C43 0.041(2) 0.049(2) 0.055(3) -0.025(2) 0.020(2) -0.027(2) C44 0.070(3) 0.050(3) 0.066(4) -0.021(2) 0.011(3) -0.033(3) C45 0.099(5) 0.054(3) 0.092(5) -0.023(3) 0.006(4) -0.045(3) C46 0.088(4) 0.079(4) 0.088(5) -0.040(3) 0.020(4) -0.062(4) C47 0.054(3) 0.075(3) 0.073(4) -0.034(3) 0.014(3) -0.041(3) C48 0.044(3) 0.051(3) 0.068(4) -0.026(3) 0.014(2) -0.026(2) C49 0.050(2) 0.041(2) 0.048(3) -0.0148(19) 0.004(2) -0.024(2) C50 0.058(3) 0.049(3) 0.056(3) -0.010(2) 0.004(3) -0.018(2) C51 0.086(4) 0.053(3) 0.066(4) -0.011(3) -0.009(3) -0.012(3) C52 0.110(5) 0.054(3) 0.065(4) -0.011(3) 0.004(4) -0.035(4) C53 0.094(4) 0.061(3) 0.064(4) -0.018(3) 0.025(3) -0.048(3) C54 0.062(3) 0.050(3) 0.057(3) -0.016(2) 0.012(2) -0.031(2) N61 0.0283(16) 0.0407(17) 0.039(2) -0.0136(14) 0.0030(14) -0.0132(14) O61 0.0298(13) 0.0424(14) 0.0456(17) -0.0123(12) 0.0049(11) -0.0193(12) O62 0.0299(13) 0.0406(14) 0.0526(18) -0.0160(13) 0.0104(12) -0.0147(12) C61 0.0282(19) 0.043(2) 0.052(3) -0.0176(19) 0.0066(18) -0.0192(17) C62 0.0325(19) 0.044(2) 0.039(2) -0.0157(17) 0.0043(16) -0.0194(17) C63 0.039(2) 0.044(2) 0.049(3) -0.0144(19) 0.0135(19) -0.0193(18) C64 0.118(6) 0.185(8) 0.077(5) -0.073(5) 0.059(4) -0.124(6) C65 0.195(10) 0.245(12) 0.089(6) -0.086(7) 0.087(7) -0.184(10) C66 0.152(8) 0.111(6) 0.045(4) -0.027(4) 0.043(5) -0.071(5) C67 0.062(3) 0.100(5) 0.047(3) -0.018(3) 0.006(3) -0.015(3) C68 0.041(3) 0.099(4) 0.048(3) -0.018(3) 0.009(2) -0.024(3) C69 0.041(2) 0.047(2) 0.052(3) -0.021(2) 0.0154(19) -0.0238(19) C70 0.054(3) 0.059(3) 0.069(4) -0.027(3) 0.008(2) -0.034(2) C71 0.075(4) 0.070(4) 0.095(5) -0.041(3) 0.022(3) -0.048(3) C72 0.094(4) 0.055(3) 0.091(5) -0.032(3) 0.036(4) -0.046(3) C73 0.065(3) 0.045(3) 0.080(4) -0.013(3) 0.020(3) -0.020(3) C74 0.043(2) 0.046(2) 0.061(3) -0.014(2) 0.006(2) -0.019(2) N81 0.0290(16) 0.0460(19) 0.047(2) -0.0194(16) 0.0057(14) -0.0195(14) O81 0.0367(14) 0.0452(15) 0.0432(17) -0.0146(12) -0.0016(12) -0.0223(12) O82 0.0280(13) 0.0425(15) 0.0576(19) -0.0145(13) -0.0009(12) -0.0172(12) C81 0.032(2) 0.042(2) 0.044(3) -0.0178(18) 0.0049(17) -0.0161(17) C82 0.034(2) 0.043(2) 0.047(3) -0.0203(19) 0.0041(18) -0.0176(17) C83 0.032(2) 0.040(2) 0.068(3) -0.018(2) 0.006(2) -0.0144(18) C84 0.057(3) 0.054(3) 0.080(4) -0.025(3) 0.002(3) -0.031(2) C85 0.067(3) 0.057(3) 0.102(5) -0.032(3) 0.004(3) -0.035(3) C86 0.059(3) 0.048(3) 0.120(6) -0.017(3) 0.014(3) -0.030(3) C87 0.087(4) 0.063(4) 0.092(5) 0.002(3) -0.008(4) -0.045(3) C88 0.067(3) 0.057(3) 0.071(4) -0.006(3) -0.002(3) -0.036(3) C89 0.035(2) 0.044(2) 0.056(3) -0.022(2) 0.0054(19) -0.0162(18) C90 0.048(3) 0.074(4) 0.073(4) -0.036(3) -0.010(3) -0.010(3) C91 0.058(3) 0.095(5) 0.090(5) -0.059(4) 0.006(3) -0.016(3) C92 0.049(3) 0.078(4) 0.106(6) -0.055(4) 0.006(3) -0.006(3) C93 0.052(3) 0.091(5) 0.085(5) -0.038(4) -0.010(3) 0.011(3) C94 0.049(3) 0.074(4) 0.060(4) -0.030(3) -0.005(3) -0.001(3) N101 0.044(2) 0.079(3) 0.078(3) -0.020(3) -0.005(2) -0.028(2) O101 0.0378(16) 0.0621(19) 0.063(2) -0.0247(16) 0.0009(14) -0.0212(15) C101 0.040(2) 0.057(3) 0.066(3) -0.020(2) 0.001(2) -0.024(2) C102 0.094(5) 0.130(6) 0.093(5) -0.035(5) -0.014(4) -0.062(5) C103 0.042(3) 0.099(5) 0.120(6) -0.024(4) -0.001(3) -0.029(3) N111 0.072(3) 0.097(4) 0.082(4) -0.040(3) 0.027(3) -0.039(3) O111 0.111(4) 0.113(4) 0.114(5) -0.045(4) 0.016(3) -0.029(3) C111 0.081(4) 0.101(5) 0.046(4) -0.022(3) 0.012(3) -0.029(4) C112 0.109(6) 0.224(11) 0.065(5) -0.043(6) 0.018(5) -0.059(7) C113 0.206(14) 0.32(2) 0.260(18) -0.146(16) 0.181(14) -0.037(14) N121 0.106(5) 0.158(7) 0.175(8) -0.090(6) 0.054(5) -0.077(5) O121 0.508 0.253 0.269 -0.140 0.177 -0.220 C121 0.096 0.136 0.200 -0.086 -0.038 0.012 C122 0.175(11) 0.283(17) 0.33(2) -0.211(16) 0.141(13) -0.176(13) C123 0.063(6) 0.39(2) 0.35(2) -0.25(2) 0.019(9) -0.066(9) N131 0.094(4) 0.116(5) 0.070(4) -0.018(3) 0.005(3) -0.054(4) O131 0.186(7) 0.142(5) 0.098(5) -0.011(4) -0.019(4) -0.075(5) C131 0.162(9) 0.161(9) 0.089(7) -0.033(6) 0.008(6) -0.106(8) C132 0.179(11) 0.154(9) 0.079(6) -0.026(6) -0.005(6) 0.036(8) C133 0.094(6) 0.130(8) 0.238(13) -0.042(8) -0.004(7) -0.063(6) N171 0.068(3) 0.107(4) 0.088(4) -0.041(3) 0.008(3) -0.042(3) O171 0.59(3) 0.106(6) 0.139(8) -0.056(6) 0.032(10) -0.093(10) C171 0.43(3) 0.30(2) 0.065(6) 0.011(10) -0.031(11) -0.31(2) C172 0.096(6) 0.197(11) 0.146(9) -0.071(8) 0.017(6) -0.083(7) C173 0.105(7) 0.157(10) 0.177(11) -0.002(8) 0.015(7) 0.016(7) N181 0.118(5) 0.077(4) 0.082(4) -0.007(3) 0.019(4) -0.012(4) O181 0.293(16) 0.42(2) 0.247(15) 0.178(15) 0.018(12) -0.151(16) C181 0.44(4) 0.159(15) 0.206(19) 0.041(13) 0.06(2) 0.16(2) C182 0.40(3) 0.104(9) 0.26(2) -0.042(11) -0.006(19) 0.032(13) C183 0.51(4) 0.247(18) 0.160(13) -0.034(13) 0.013(18) -0.27(2) OW1 0.291(14) 0.385(17) 0.160(9) -0.101(10) 0.031(9) -0.170(13) N141 0.113 0.105 0.199 -0.039 0.020 -0.057 O141 0.510 0.382 0.491 -0.106 0.079 0.147 C141 0.103 0.266 0.286 0.152 -0.087 -0.102 C142 0.091 0.256 0.542 -0.206 -0.012 -0.070 C143 0.150 0.128 0.253 -0.088 0.105 -0.068 N95 0.048(6) 0.100(10) 0.085(8) -0.037(7) 0.011(5) -0.039(7) O95 0.101(8) 0.225(16) 0.110(10) -0.065(10) 0.006(7) -0.047(9) C95 0.062(9) 0.23(3) 0.061(9) -0.024(12) 0.004(7) -0.056(12) C96 0.082(10) 0.158(15) 0.106(14) -0.062(12) 0.000(10) -0.039(10) C97 0.35(5) 0.36(4) 0.076(13) -0.108(19) 0.10(2) -0.32(4) N95A 0.19(4) 0.089(18) 0.55(10) -0.12(3) -0.20(5) 0.00(2) O95A 0.39(4) 0.159(18) 0.49(5) -0.18(3) 0.32(4) -0.21(2) C95A 0.39(7) 0.92(16) 0.07(2) -0.01(5) -0.02(3) -0.53(10) C96A 0.33(9) 0.34(9) 0.27(6) -0.14(6) -0.13(7) -0.17(6) C97A 0.11(2) 0.21(4) 0.43(7) -0.10(4) 0.03(3) -0.09(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O42 1.902(3) 2_765 ? Cu1 O21 1.914(3) . ? Cu1 O1 1.928(3) . ? Cu1 N21 1.959(3) . ? Cu2 O22 1.897(3) . ? Cu2 O81 1.902(3) . ? Cu2 O1 1.910(3) . ? Cu2 N1 1.940(3) . ? Cu3 O81 1.921(3) . ? Cu3 O2 1.935(3) . ? Cu3 O61 1.938(3) . ? Cu3 N81 1.958(3) . ? Cu4 O82 1.919(3) . ? Cu4 O61 1.923(3) . ? Cu4 O41 1.925(3) . ? Cu4 N61 1.962(3) . ? Cu5 O62 1.929(3) . ? Cu5 O41 1.932(3) . ? Cu5 O21 1.944(3) 2_765 ? Cu5 N41 1.981(4) . ? Cu5 O101 2.343(3) . ? N1 C1 1.293(5) . ? N1 O2 1.352(4) . ? O1 C2 1.420(5) . ? C1 C3 1.490(6) . ? C1 C2 1.513(6) . ? C2 C9 1.522(6) . ? C2 H2 0.86(5) . ? C3 C8 1.380(7) . ? C3 C4 1.386(7) . ? C4 C5 1.393(7) . ? C4 H4 0.90(6) . ? C5 C6 1.365(10) . ? C5 H5 0.83(7) . ? C6 C7 1.358(10) . ? C6 H6 1.00(6) . ? C7 C8 1.381(8) . ? C7 H7 0.94(6) . ? C8 H8 0.87(5) . ? C9 C14 1.370(7) . ? C9 C10 1.383(7) . ? C10 C11 1.388(7) . ? C10 H10 0.98(6) . ? C11 C12 1.387(9) . ? C11 H11 0.90(7) . ? C12 C13 1.355(9) . ? C12 H12 1.13(8) . ? C13 C14 1.394(8) . ? C13 H13 0.9500 . ? C14 H14 0.90(7) . ? N21 C22 1.286(5) . ? N21 O22 1.366(4) . ? O21 C21 1.430(5) . ? O21 Cu5 1.944(3) 2_765 ? C21 C22 1.501(6) . ? C21 C23 1.521(6) . ? C21 H21 0.91(4) . ? C22 C29 1.487(6) . ? C23 C24 1.381(7) . ? C23 C28 1.398(6) . ? C24 C25 1.396(7) . ? C24 H24 1.01(5) . ? C25 C26 1.382(8) . ? C25 H25 0.99(6) . ? C26 C27 1.361(9) . ? C26 H26 0.91(6) . ? C27 C28 1.385(7) . ? C27 H27 0.88(6) . ? C28 H28 0.97(5) . ? C29 C30 1.381(7) . ? C29 C34 1.390(7) . ? C30 C31 1.392(8) . ? C30 H30 0.91(6) . ? C31 C32 1.371(10) . ? C31 H31 0.89(8) . ? C32 C33 1.374(9) . ? C32 H32 1.02(6) . ? C33 C34 1.383(7) . ? C33 H33 1.13(7) . ? C34 H34 0.97(5) . ? N41 C42 1.284(5) . ? N41 O42 1.369(4) . ? O41 C41 1.427(5) . ? O42 Cu1 1.902(3) 2_765 ? C41 C42 1.521(6) . ? C41 C43 1.523(6) . ? C41 H41 0.89(4) . ? C42 C49 1.476(6) . ? C43 C48 1.374(7) . ? C43 C44 1.394(7) . ? C44 C45 1.396(8) . ? C44 H44 0.95(5) . ? C45 C46 1.350(9) . ? C45 H45 0.83(6) . ? C46 C47 1.378(8) . ? C46 H46 0.96(6) . ? C47 C48 1.388(7) . ? C47 H47 0.88(6) . ? C48 H48 0.70(5) . ? C49 C50 1.388(7) . ? C49 C54 1.395(7) . ? C50 C51 1.394(7) . ? C50 H50 0.83(5) . ? C51 C52 1.361(9) . ? C51 H51 0.9500 . ? C52 C53 1.377(9) . ? C52 H52 1.05(6) . ? C53 C54 1.394(7) . ? C53 H53 0.88(6) . ? C54 H54 0.98(5) . ? N61 C62 1.287(5) . ? N61 O62 1.355(4) . ? O61 C61 1.428(5) . ? C61 C62 1.515(5) . ? C61 C63 1.520(6) . ? C61 H61 0.95(4) . ? C62 C69 1.481(6) . ? C63 C68 1.372(7) . ? C63 C64 1.377(7) . ? C64 C65 1.378(11) . ? C64 H64 0.87(7) . ? C65 C66 1.353(12) . ? C65 H65 0.9500 . ? C66 C67 1.364(10) . ? C66 H66 0.76(6) . ? C67 C68 1.398(8) . ? C67 H67 0.9500 . ? C68 H68 1.00(7) . ? C69 C74 1.389(6) . ? C69 C70 1.395(6) . ? C70 C71 1.376(7) . ? C70 H70 0.97(6) . ? C71 C72 1.368(9) . ? C71 H71 0.96(6) . ? C72 C73 1.390(9) . ? C72 H72 1.11(7) . ? C73 C74 1.367(7) . ? C73 H73 1.00(9) . ? C74 H74 0.90(5) . ? N81 C81 1.292(5) . ? N81 O82 1.364(4) . ? O81 C82 1.423(5) . ? C81 C83 1.472(6) . ? C81 C82 1.518(5) . ? C82 C89 1.512(6) . ? C82 H82 0.89(4) . ? C83 C88 1.379(7) . ? C83 C84 1.392(7) . ? C84 C85 1.383(7) . ? C84 H84 0.85(6) . ? C85 C86 1.346(9) . ? C85 H85 1.02(6) . ? C86 C87 1.382(10) . ? C86 H86 0.95(5) . ? C87 C88 1.394(8) . ? C87 H87 0.89(9) . ? C88 H88 0.94(6) . ? C89 C90 1.379(7) . ? C89 C94 1.382(7) . ? C90 C91 1.379(8) . ? C90 H90 0.87(6) . ? C91 C92 1.365(9) . ? C91 H91 0.84(9) . ? C92 C93 1.346(9) . ? C92 H92 0.85(6) . ? C93 C94 1.396(8) . ? C93 H93 1.07(10) . ? C94 H94 0.87(5) . ? N101 C101 1.326(6) . ? N101 C102 1.455(8) . ? N101 C103 1.460(7) . ? O101 C101 1.230(5) . ? C101 H101 0.9500 . ? C102 H10A 0.9800 . ? C102 H10B 0.9800 . ? C102 H10C 0.9800 . ? C103 H10D 0.9800 . ? C103 H10E 0.9800 . ? C103 H10F 0.9800 . ? N111 C111 1.351(8) . ? N111 C112 1.444(10) . ? N111 C113 1.534(15) . ? O111 C111 1.224(8) . ? C111 H111 0.9500 . ? C112 H11A 0.9800 . ? C112 H11B 0.9800 . ? C112 H11C 0.9800 . ? C113 H11D 0.9800 . ? C113 H11E 0.9800 . ? C113 H11F 0.9800 . ? N121 C121 1.376(8) . ? N121 C122 1.393(10) . ? N121 C123 1.419(9) . ? O121 C121 1.2039 . ? C121 H121 0.9500 . ? C122 H12A 0.9800 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C123 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? N131 C131 1.273(11) . ? N131 C132 1.399(10) . ? N131 C133 1.473(11) . ? O131 C131 1.274(10) . ? C131 H131 0.9500 . ? C132 H13A 0.9800 . ? C132 H13B 0.9800 . ? C132 H13C 0.9800 . ? C133 H13D 0.9800 . ? C133 H13E 0.9800 . ? C133 H13F 0.9800 . ? N171 C171 1.348(14) . ? N171 C172 1.372(9) . ? N171 C173 1.518(12) . ? O171 C171 1.10(2) . ? C171 H171 0.9500 . ? C172 H17A 0.9800 . ? C172 H17B 0.9800 . ? C172 H17C 0.9800 . ? C173 H17D 0.9800 . ? C173 H17E 0.9800 . ? C173 H17F 0.9800 . ? N181 C181 1.338(12) . ? N181 C182 1.399(10) . ? N181 C183 1.452(11) . ? O181 C181 1.238(15) . ? C181 H181 0.9500 . ? C182 H18A 0.9800 . ? C182 H18B 0.9800 . ? C182 H18C 0.9800 . ? C183 H18D 0.9800 . ? C183 H18E 0.9800 . ? C183 H18F 0.9800 . ? N141 C142 1.3939 . ? N141 C141 1.4490 . ? N141 C143 1.4727 . ? O141 C141 1.1813 . ? C141 H141 0.9500 . ? C142 H14A 0.9867 . ? C142 H14B 0.9686 . ? C142 H14C 0.9902 . ? C143 H14D 0.9800 . ? C143 H14E 0.9800 . ? C143 H14F 0.9800 . ? N95 C95 1.350(15) . ? N95 C96 1.436(15) . ? N95 C97 1.438(15) . ? O95 C95 1.222(15) . ? C95 H95 0.9500 . ? N95A C95A 1.361(16) . ? N95A C96A 1.417(16) . ? N95A C97A 1.457(17) . ? O95A C95A 1.226(17) . ? C95A H95A 0.9500 . ? 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 O42 Cu1 O21 94.84(12) 2_765 . ? O42 Cu1 O1 94.99(12) 2_765 . ? O21 Cu1 O1 170.01(12) . . ? O42 Cu1 N21 169.89(13) 2_765 . ? O21 Cu1 N21 82.40(13) . . ? O1 Cu1 N21 88.21(13) . . ? O22 Cu2 O81 95.33(12) . . ? O22 Cu2 O1 93.19(12) . . ? O81 Cu2 O1 171.44(12) . . ? O22 Cu2 N1 174.72(14) . . ? O81 Cu2 N1 88.48(13) . . ? O1 Cu2 N1 83.06(13) . . ? O81 Cu3 O2 91.33(11) . . ? O81 Cu3 O61 169.45(12) . . ? O2 Cu3 O61 96.14(11) . . ? O81 Cu3 N81 82.23(12) . . ? O2 Cu3 N81 171.24(14) . . ? O61 Cu3 N81 89.52(12) . . ? O82 Cu4 O61 93.10(11) . . ? O82 Cu4 O41 94.85(11) . . ? O61 Cu4 O41 171.88(12) . . ? O82 Cu4 N61 174.62(12) . . ? O61 Cu4 N61 83.13(12) . . ? O41 Cu4 N61 88.83(12) . . ? O62 Cu5 O41 93.08(11) . . ? O62 Cu5 O21 92.96(12) . 2_765 ? O41 Cu5 O21 166.14(12) . 2_765 ? O62 Cu5 N41 160.49(13) . . ? O41 Cu5 N41 82.37(13) . . ? O21 Cu5 N41 87.80(13) 2_765 . ? O62 Cu5 O101 99.60(12) . . ? O41 Cu5 O101 98.82(12) . . ? O21 Cu5 O101 92.45(12) 2_765 . ? N41 Cu5 O101 99.85(12) . . ? C1 N1 O2 119.6(3) . . ? C1 N1 Cu2 116.6(3) . . ? O2 N1 Cu2 123.7(2) . . ? C2 O1 Cu2 114.3(3) . . ? C2 O1 Cu1 126.3(3) . . ? Cu2 O1 Cu1 112.15(13) . . ? N1 O2 Cu3 110.5(2) . . ? N1 C1 C3 125.8(4) . . ? N1 C1 C2 114.4(4) . . ? C3 C1 C2 119.8(4) . . ? O1 C2 C1 110.3(3) . . ? O1 C2 C9 110.9(3) . . ? C1 C2 C9 110.8(4) . . ? O1 C2 H2 112(3) . . ? C1 C2 H2 105(3) . . ? C9 C2 H2 108(3) . . ? C8 C3 C4 119.3(5) . . ? C8 C3 C1 119.5(5) . . ? C4 C3 C1 121.1(4) . . ? C3 C4 C5 119.0(6) . . ? C3 C4 H4 111(4) . . ? C5 C4 H4 130(4) . . ? C6 C5 C4 120.9(7) . . ? C6 C5 H5 120(5) . . ? C4 C5 H5 119(5) . . ? C7 C6 C5 120.0(6) . . ? C7 C6 H6 128(4) . . ? C5 C6 H6 112(4) . . ? C6 C7 C8 120.2(6) . . ? C6 C7 H7 116(3) . . ? C8 C7 H7 124(4) . . ? C3 C8 C7 120.6(6) . . ? C3 C8 H8 117(3) . . ? C7 C8 H8 122(3) . . ? C14 C9 C10 118.6(5) . . ? C14 C9 C2 121.4(5) . . ? C10 C9 C2 119.9(4) . . ? C9 C10 C11 120.9(6) . . ? C9 C10 H10 113(3) . . ? C11 C10 H10 126(3) . . ? C12 C11 C10 119.6(7) . . ? C12 C11 H11 115(4) . . ? C10 C11 H11 125(5) . . ? C13 C12 C11 119.6(5) . . ? C13 C12 H12 127(4) . . ? C11 C12 H12 113(4) . . ? C12 C13 C14 120.7(6) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C9 C14 C13 120.6(6) . . ? C9 C14 H14 121(4) . . ? C13 C14 H14 119(4) . . ? C22 N21 O22 120.1(3) . . ? C22 N21 Cu1 116.6(3) . . ? O22 N21 Cu1 123.0(2) . . ? C21 O21 Cu1 115.1(3) . . ? C21 O21 Cu5 124.4(3) . 2_765 ? Cu1 O21 Cu5 115.86(13) . 2_765 ? N21 O22 Cu2 112.6(2) . . ? O21 C21 C22 109.9(3) . . ? O21 C21 C23 109.8(3) . . ? C22 C21 C23 111.4(3) . . ? O21 C21 H21 106(3) . . ? C22 C21 H21 112(3) . . ? C23 C21 H21 107(3) . . ? N21 C22 C29 123.7(4) . . ? N21 C22 C21 115.2(3) . . ? C29 C22 C21 121.1(4) . . ? C24 C23 C28 118.6(4) . . ? C24 C23 C21 120.3(4) . . ? C28 C23 C21 121.0(4) . . ? C23 C24 C25 121.5(5) . . ? C23 C24 H24 122(3) . . ? C25 C24 H24 117(3) . . ? C26 C25 C24 118.5(6) . . ? C26 C25 H25 113(3) . . ? C24 C25 H25 128(3) . . ? C27 C26 C25 120.8(5) . . ? C27 C26 H26 127(4) . . ? C25 C26 H26 112(4) . . ? C26 C27 C28 120.9(5) . . ? C26 C27 H27 125(4) . . ? C28 C27 H27 113(4) . . ? C27 C28 C23 119.7(5) . . ? C27 C28 H28 122(3) . . ? C23 C28 H28 118(3) . . ? C30 C29 C34 118.7(4) . . ? C30 C29 C22 120.6(4) . . ? C34 C29 C22 120.7(4) . . ? C29 C30 C31 120.2(6) . . ? C29 C30 H30 120(3) . . ? C31 C30 H30 120(3) . . ? C32 C31 C30 120.5(6) . . ? C32 C31 H31 122(5) . . ? C30 C31 H31 116(5) . . ? C31 C32 C33 119.8(5) . . ? C31 C32 H32 123(4) . . ? C33 C32 H32 118(4) . . ? C32 C33 C34 120.1(6) . . ? C32 C33 H33 123(4) . . ? C34 C33 H33 115(4) . . ? C33 C34 C29 120.7(5) . . ? C33 C34 H34 120(3) . . ? C29 C34 H34 119(3) . . ? C42 N41 O42 118.2(3) . . ? C42 N41 Cu5 116.0(3) . . ? O42 N41 Cu5 124.8(2) . . ? C41 O41 Cu4 119.6(2) . . ? C41 O41 Cu5 114.8(2) . . ? Cu4 O41 Cu5 115.12(13) . . ? N41 O42 Cu1 112.9(2) . 2_765 ? O41 C41 C42 109.8(3) . . ? O41 C41 C43 111.7(4) . . ? C42 C41 C43 110.5(3) . . ? O41 C41 H41 108(3) . . ? C42 C41 H41 108(3) . . ? C43 C41 H41 109(3) . . ? N41 C42 C49 126.7(4) . . ? N41 C42 C41 115.1(4) . . ? C49 C42 C41 118.2(4) . . ? C48 C43 C44 118.4(5) . . ? C48 C43 C41 122.0(4) . . ? C44 C43 C41 119.6(4) . . ? C43 C44 C45 119.7(6) . . ? C43 C44 H44 118(3) . . ? C45 C44 H44 123(3) . . ? C46 C45 C44 120.9(6) . . ? C46 C45 H45 124(4) . . ? C44 C45 H45 115(4) . . ? C45 C46 C47 120.2(5) . . ? C45 C46 H46 113(3) . . ? C47 C46 H46 127(3) . . ? C46 C47 C48 119.4(6) . . ? C46 C47 H47 112(4) . . ? C48 C47 H47 129(4) . . ? C43 C48 C47 121.4(5) . . ? C43 C48 H48 123(4) . . ? C47 C48 H48 115(4) . . ? C50 C49 C54 118.1(4) . . ? C50 C49 C42 120.1(4) . . ? C54 C49 C42 121.8(4) . . ? C49 C50 C51 121.2(6) . . ? C49 C50 H50 118(3) . . ? C51 C50 H50 121(3) . . ? C52 C51 C50 119.9(6) . . ? C52 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C51 C52 C53 120.2(6) . . ? C51 C52 H52 116(3) . . ? C53 C52 H52 124(3) . . ? C52 C53 C54 120.4(6) . . ? C52 C53 H53 120(4) . . ? C54 C53 H53 120(4) . . ? C53 C54 C49 120.1(5) . . ? C53 C54 H54 116(3) . . ? C49 C54 H54 124(3) . . ? C62 N61 O62 119.4(3) . . ? C62 N61 Cu4 115.2(3) . . ? O62 N61 Cu4 124.1(2) . . ? C61 O61 Cu4 114.8(2) . . ? C61 O61 Cu3 119.9(2) . . ? Cu4 O61 Cu3 108.68(13) . . ? N61 O62 Cu5 113.9(2) . . ? O61 C61 C62 109.7(3) . . ? O61 C61 C63 111.1(4) . . ? C62 C61 C63 110.7(3) . . ? O61 C61 H61 111(2) . . ? C62 C61 H61 106(2) . . ? C63 C61 H61 107(2) . . ? N61 C62 C69 125.2(4) . . ? N61 C62 C61 115.8(3) . . ? C69 C62 C61 118.9(3) . . ? C68 C63 C64 118.0(5) . . ? C68 C63 C61 121.7(4) . . ? C64 C63 C61 120.2(5) . . ? C63 C64 C65 119.9(7) . . ? C63 C64 H64 118(5) . . ? C65 C64 H64 122(5) . . ? C66 C65 C64 121.5(7) . . ? C66 C65 H65 119.2 . . ? C64 C65 H65 119.2 . . ? C65 C66 C67 120.0(7) . . ? C65 C66 H66 126(5) . . ? C67 C66 H66 113(5) . . ? C66 C67 C68 118.4(7) . . ? C66 C67 H67 120.8 . . ? C68 C67 H67 120.8 . . ? C63 C68 C67 121.9(5) . . ? C63 C68 H68 120(4) . . ? C67 C68 H68 118(4) . . ? C74 C69 C70 118.4(4) . . ? C74 C69 C62 121.8(4) . . ? C70 C69 C62 119.8(4) . . ? C71 C70 C69 120.4(5) . . ? C71 C70 H70 126(4) . . ? C69 C70 H70 113(4) . . ? C72 C71 C70 120.4(6) . . ? C72 C71 H71 118(4) . . ? C70 C71 H71 120(4) . . ? C71 C72 C73 119.9(5) . . ? C71 C72 H72 113(3) . . ? C73 C72 H72 127(3) . . ? C74 C73 C72 119.9(6) . . ? C74 C73 H73 121(5) . . ? C72 C73 H73 119(5) . . ? C73 C74 C69 120.9(5) . . ? C73 C74 H74 121(3) . . ? C69 C74 H74 118(3) . . ? C81 N81 O82 120.3(3) . . ? C81 N81 Cu3 117.1(3) . . ? O82 N81 Cu3 122.5(2) . . ? C82 O81 Cu2 123.7(3) . . ? C82 O81 Cu3 114.8(2) . . ? Cu2 O81 Cu3 111.18(14) . . ? N81 O82 Cu4 109.0(2) . . ? N81 C81 C83 127.3(4) . . ? N81 C81 C82 114.2(3) . . ? C83 C81 C82 118.5(4) . . ? O81 C82 C89 109.8(3) . . ? O81 C82 C81 110.4(3) . . ? C89 C82 C81 112.4(4) . . ? O81 C82 H82 103(2) . . ? C89 C82 H82 113(2) . . ? C81 C82 H82 109(3) . . ? C88 C83 C84 117.1(5) . . ? C88 C83 C81 120.4(4) . . ? C84 C83 C81 122.4(5) . . ? C85 C84 C83 121.0(6) . . ? C85 C84 H84 115(4) . . ? C83 C84 H84 123(4) . . ? C86 C85 C84 121.5(6) . . ? C86 C85 H85 124(3) . . ? C84 C85 H85 115(3) . . ? C85 C86 C87 118.9(5) . . ? C85 C86 H86 127(3) . . ? C87 C86 H86 113(3) . . ? C86 C87 C88 120.1(6) . . ? C86 C87 H87 110(6) . . ? C88 C87 H87 119(6) . . ? C83 C88 C87 121.3(6) . . ? C83 C88 H88 115(4) . . ? C87 C88 H88 123(4) . . ? C90 C89 C94 117.8(5) . . ? C90 C89 C82 122.5(4) . . ? C94 C89 C82 119.7(5) . . ? C89 C90 C91 121.3(5) . . ? C89 C90 H90 117(4) . . ? C91 C90 H90 121(4) . . ? C92 C91 C90 119.7(7) . . ? C92 C91 H91 119(6) . . ? C90 C91 H91 118(6) . . ? C93 C92 C91 120.5(6) . . ? C93 C92 H92 122(4) . . ? C91 C92 H92 117(4) . . ? C92 C93 C94 120.2(6) . . ? C92 C93 H93 127(5) . . ? C94 C93 H93 105(5) . . ? C89 C94 C93 120.5(6) . . ? C89 C94 H94 121(3) . . ? C93 C94 H94 119(3) . . ? C101 N101 C102 121.1(5) . . ? C101 N101 C103 120.5(5) . . ? C102 N101 C103 117.6(5) . . ? C101 O101 Cu5 122.6(3) . . ? O101 C101 N101 124.4(5) . . ? O101 C101 H101 117.8 . . ? N101 C101 H101 117.8 . . ? N101 C102 H10A 109.5 . . ? N101 C102 H10B 109.5 . . ? H10A C102 H10B 109.5 . . ? N101 C102 H10C 109.5 . . ? H10A C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? N101 C103 H10D 109.5 . . ? N101 C103 H10E 109.5 . . ? H10D C103 H10E 109.5 . . ? N101 C103 H10F 109.5 . . ? H10D C103 H10F 109.5 . . ? H10E C103 H10F 109.5 . . ? C111 N111 C112 118.4(6) . . ? C111 N111 C113 119.6(7) . . ? C112 N111 C113 121.4(8) . . ? O111 C111 N111 131.7(7) . . ? O111 C111 H111 114.1 . . ? N111 C111 H111 114.1 . . ? N111 C112 H11A 109.5 . . ? N111 C112 H11B 109.5 . . ? H11A C112 H11B 109.5 . . ? N111 C112 H11C 109.5 . . ? H11A C112 H11C 109.5 . . ? H11B C112 H11C 109.5 . . ? N111 C113 H11D 109.5 . . ? N111 C113 H11E 109.5 . . ? H11D C113 H11E 109.5 . . ? N111 C113 H11F 109.5 . . ? H11D C113 H11F 109.5 . . ? H11E C113 H11F 109.5 . . ? C121 N121 C122 117.2(8) . . ? C121 N121 C123 122.0(8) . . ? C122 N121 C123 120.8(10) . . ? O121 C121 N121 112.3(3) . . ? O121 C121 H121 123.8 . . ? N121 C121 H121 123.8 . . ? N121 C122 H12A 109.5 . . ? N121 C122 H12B 109.5 . . ? H12A C122 H12B 109.5 . . ? N121 C122 H12C 109.5 . . ? H12A C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? N121 C123 H12D 109.5 . . ? N121 C123 H12E 109.5 . . ? H12D C123 H12E 109.5 . . ? N121 C123 H12F 109.5 . . ? H12D C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C131 N131 C132 128.2(9) . . ? C131 N131 C133 115.0(9) . . ? C132 N131 C133 116.8(8) . . ? N131 C131 O131 124.2(12) . . ? N131 C131 H131 117.9 . . ? O131 C131 H131 117.9 . . ? N131 C132 H13A 109.5 . . ? N131 C132 H13B 109.5 . . ? H13A C132 H13B 109.5 . . ? N131 C132 H13C 109.5 . . ? H13A C132 H13C 109.5 . . ? H13B C132 H13C 109.5 . . ? N131 C133 H13D 109.5 . . ? N131 C133 H13E 109.5 . . ? H13D C133 H13E 109.5 . . ? N131 C133 H13F 109.5 . . ? H13D C133 H13F 109.5 . . ? H13E C133 H13F 109.5 . . ? C171 N171 C172 127.9(12) . . ? C171 N171 C173 120.4(12) . . ? C172 N171 C173 111.6(8) . . ? O171 C171 N171 129(2) . . ? O171 C171 H171 115.5 . . ? N171 C171 H171 115.5 . . ? N171 C172 H17A 109.5 . . ? N171 C172 H17B 109.5 . . ? H17A C172 H17B 109.5 . . ? N171 C172 H17C 109.5 . . ? H17A C172 H17C 109.5 . . ? H17B C172 H17C 109.5 . . ? N171 C173 H17D 109.5 . . ? N171 C173 H17E 109.5 . . ? H17D C173 H17E 109.5 . . ? N171 C173 H17F 109.5 . . ? H17D C173 H17F 109.5 . . ? H17E C173 H17F 109.5 . . ? C181 N181 C182 124.2(10) . . ? C181 N181 C183 118.9(9) . . ? C182 N181 C183 115.5(11) . . ? O181 C181 N181 115.3(13) . . ? O181 C181 H181 122.4 . . ? N181 C181 H181 122.4 . . ? N181 C182 H18A 109.5 . . ? N181 C182 H18B 109.5 . . ? H18A C182 H18B 109.5 . . ? N181 C182 H18C 109.5 . . ? H18A C182 H18C 109.5 . . ? H18B C182 H18C 109.5 . . ? N181 C183 H18D 109.5 . . ? N181 C183 H18E 109.5 . . ? H18D C183 H18E 109.5 . . ? N181 C183 H18F 109.5 . . ? H18D C183 H18F 109.5 . . ? H18E C183 H18F 109.5 . . ? C142 N141 C141 117.4 . . ? C142 N141 C143 120.9 . . ? C141 N141 C143 121.6 . . ? O141 C141 N141 115.5 . . ? O141 C141 H141 122.2 . . ? N141 C141 H141 122.2 . . ? N141 C142 H14A 109.5 . . ? N141 C142 H14B 110.7 . . ? H14A C142 H14B 109.9 . . ? N141 C142 H14C 109.1 . . ? H14A C142 H14C 108.1 . . ? H14B C142 H14C 109.6 . . ? N141 C143 H14D 109.5 . . ? N141 C143 H14E 109.5 . . ? H14D C143 H14E 109.5 . . ? N141 C143 H14F 109.5 . . ? H14D C143 H14F 109.5 . . ? H14E C143 H14F 109.5 . . ? C95 N95 C96 120.6(14) . . ? C95 N95 C97 119.2(16) . . ? C96 N95 C97 120.0(16) . . ? O95 C95 N95 121.7(19) . . ? O95 C95 H95 119.1 . . ? N95 C95 H95 119.1 . . ? C95A N95A C96A 126(2) . . ? C95A N95A C97A 115(2) . . ? C96A N95A C97A 119(2) . . ? O95A C95A N95A 127(3) . . ? O95A C95A H95A 116.6 . . ? N95A C95A H95A 116.6 . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.858 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.086 # start Validation Reply Form # PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.73 Ratio # RESPONSE: This is due to the large thermal motion of the methyl groups # of the coordinated dmf molecules. # PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 10.00 Ratio # RESPONSE: This is due to the large thermal motion of the methyl hydrogens # of the coordinated dmf molecules. These H-atoms were introduced at # calculated positions as riding on bonded atoms and were refined with # Ueq = 1.3 times the Ueq of their respective carbon atoms. # PROBLEM: Check High Ueq as Compared to Neighbors for O111 # RESPONSE: No action taken. Atom O111 belongs to a coordinated dmf # molecule and is coordinated to a copper atom. # PROBLEM: Check Low Ueq as Compared to Neighbors for N111 # RESPONSE: No action taken. Atom N111 belongs to a coordinated dmf # molecule whose methyl groups showed large thermal motion. # PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... OW1 # RESPONSE: No H-atoms for the solvate water molecule were included in # the refinement. # PROBLEM: Ueq(Rep) and Ueq(Calc) differ by 0.010 Ang**2 . C95A # RESPONSE: No action taken. Atom C95A belongs to a disordered dmf molecule. # end Validation Reply Form # Attachment 'Cu10_complex_21.cif' data_st412 _database_code_depnum_ccdc_archive 'CCDC 717732' _audit_update_record ; 2008-11-25 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C156 H146 Cl16 Cu10 N10 O22' _chemical_formula_weight 3715.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.9401(11) _cell_length_b 27.9757(18) _cell_length_c 16.9907(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.464(1) _cell_angle_gamma 90.00 _cell_volume 8049.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 448 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description plates _exptl_crystal_colour green _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3780 _exptl_absorpt_coefficient_mu 1.626 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6772 _exptl_absorpt_correction_T_max 0.7925 _exptl_absorpt_process_details 'based on measured indexed crystal faces, Bruker SHELXTL v6.12 (Bruker 1998)' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 53932 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.50 _reflns_number_total 18359 _reflns_number_gt 14412 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART v5.624 (Bruker 1998)' _computing_cell_refinement 'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL v6.14 (Bruker 2000)' _computing_structure_solution 'Bruker SHELXTL v6.14' _computing_structure_refinement 'Bruker SHELXTL v6.14' _computing_molecular_graphics 'Bruker SHELXTL v6.14' _computing_publication_material 'Bruker SHELXTL v6.14' _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. The asymmetric unit consists of a half Cu10 ring cluster, four dichloromethane and one ether solvent molecules. All solvent molecules were disordered and could not be modeled properly, thus program SQUEEZE, a part of the PLATON package of crystallographic software, was used to calculate the solvent disorder area and remove its contribution to the overall intensity data. It is important to note that one of the disordered dichloromethane molecules is located at the center of the Cu10 ring cluster. ; _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^)+(0.0428P)] 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 18359 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.884210(14) -0.118741(8) 0.288323(14) 0.02953(6) Uani 1 1 d . . . Cu2 Cu 0.820038(13) -0.011590(8) 0.316356(13) 0.02547(6) Uani 1 1 d . . . Cu3 Cu 0.797320(13) 0.088190(8) 0.408410(12) 0.02560(6) Uani 1 1 d . . . Cu4 Cu 0.859849(13) 0.172076(8) 0.518674(13) 0.02504(6) Uani 1 1 d . . . Cu5 Cu 0.973968(13) 0.185621(8) 0.662278(13) 0.02715(6) Uani 1 1 d . . . N1 N 0.92763(9) -0.06347(5) 0.23401(9) 0.0294(3) Uani 1 1 d . . . N2 N 0.75649(9) -0.00715(5) 0.41041(9) 0.0270(3) Uani 1 1 d . . . N3 N 0.87117(9) 0.13642(5) 0.36987(9) 0.0274(3) Uani 1 1 d . . . N4 N 0.82475(9) 0.16025(6) 0.62568(9) 0.0272(3) Uani 1 1 d . . . N5 N 1.07919(9) 0.19283(5) 0.61897(9) 0.0272(3) Uani 1 1 d . . . O1 O 0.97895(8) -0.14914(5) 0.25208(7) 0.0305(3) Uani 1 1 d . . . O2 O 0.89574(8) -0.01888(5) 0.23678(8) 0.0340(3) Uani 1 1 d . . . O3 O 0.80212(7) -0.07816(4) 0.32706(7) 0.0279(3) Uani 1 1 d . . . O4 O 0.74336(8) 0.03416(4) 0.45007(8) 0.0320(3) Uani 1 1 d . . . O5 O 0.82585(8) 0.05582(4) 0.31525(7) 0.0302(3) Uani 1 1 d . . . O6 O 0.89651(8) 0.17443(5) 0.41354(7) 0.0313(3) Uani 1 1 d . . . O7 O 0.77361(7) 0.13064(4) 0.49219(7) 0.0274(3) Uani 1 1 d . . . O8 O 0.86669(8) 0.17505(5) 0.69065(7) 0.0333(3) Uani 1 1 d . . . O9 O 0.94208(7) 0.21253(5) 0.56177(7) 0.0280(3) Uani 1 1 d . . . O10 O 1.14527(8) 0.17393(5) 0.65319(8) 0.0337(3) Uani 1 1 d . . . C1 C 0.99499(12) -0.06944(7) 0.20206(11) 0.0304(4) Uani 1 1 d . . . C2 C 1.02459(12) -0.12032(7) 0.20127(11) 0.0306(4) Uani 1 1 d . . . H2A H 1.0808 -0.1207 0.2206 0.037 Uiso 1 1 calc R . . C3 C 1.02085(12) -0.13831(7) 0.11672(11) 0.0301(4) Uani 1 1 d . . . C4 C 0.94915(14) -0.14933(8) 0.08011(13) 0.0438(5) Uani 1 1 d . . . H4A H 0.9019 -0.1475 0.1089 0.053 Uiso 1 1 calc R . . C5 C 0.94602(16) -0.16304(9) 0.00174(15) 0.0555(7) Uani 1 1 d . . . H5A H 0.8967 -0.1710 -0.0227 0.067 Uiso 1 1 calc R . . C6 C 1.01392(16) -0.16518(8) -0.04104(14) 0.0499(6) Uani 1 1 d . . . H6A H 1.0115 -0.1746 -0.0948 0.060 Uiso 1 1 calc R . . C7 C 1.08461(15) -0.15368(8) -0.00584(14) 0.0480(6) Uani 1 1 d . . . H7A H 1.1315 -0.1548 -0.0353 0.058 Uiso 1 1 calc R . . C8 C 1.08847(13) -0.14036(8) 0.07296(13) 0.0405(5) Uani 1 1 d . . . H8A H 1.1381 -0.1326 0.0970 0.049 Uiso 1 1 calc R . . C9 C 1.04163(12) -0.03076(7) 0.16556(12) 0.0342(4) Uani 1 1 d . . . C10 C 1.12082(15) -0.02585(10) 0.18409(18) 0.0600(7) Uani 1 1 d . . . H10A H 1.1461 -0.0477 0.2194 0.072 Uiso 1 1 calc R . . C11 C 1.16375(17) 0.01108(11) 0.1511(2) 0.0783(10) Uani 1 1 d . . . H11A H 1.2180 0.0148 0.1652 0.094 Uiso 1 1 calc R . . C12 C 1.12901(18) 0.04204(10) 0.09869(18) 0.0653(8) Uani 1 1 d . . . H12A H 1.1590 0.0671 0.0763 0.078 Uiso 1 1 calc R . . C13 C 1.05138(17) 0.03690(9) 0.07875(15) 0.0558(7) Uani 1 1 d . . . H13A H 1.0272 0.0582 0.0418 0.067 Uiso 1 1 calc R . . C14 C 1.00712(15) 0.00065(8) 0.11211(13) 0.0438(5) Uani 1 1 d . . . H14A H 0.9527 -0.0026 0.0981 0.053 Uiso 1 1 calc R . . C15C C 0.73533(11) -0.04747(7) 0.44076(11) 0.0265(4) Uani 1 1 d . . . C16C C 0.74808(11) -0.09016(6) 0.38730(11) 0.0263(4) Uani 1 1 d . . . H16A H 0.7712 -0.1169 0.4196 0.032 Uiso 1 1 calc R . . C17C C 0.66991(11) -0.10679(7) 0.35077(11) 0.0284(4) Uani 1 1 d . . . C18A C 0.60558(13) -0.07707(8) 0.34095(15) 0.0469(6) Uani 1 1 d . . . H18A H 0.6090 -0.0449 0.3589 0.056 Uiso 1 1 calc R . . C19C C 0.53594(14) -0.09313(9) 0.30547(16) 0.0541(7) Uani 1 1 d . . . H19A H 0.4924 -0.0719 0.2992 0.065 Uiso 1 1 calc R . . C20C C 0.52955(14) -0.13861(9) 0.27972(15) 0.0516(6) Uani 1 1 d . . . H20A H 0.4820 -0.1495 0.2550 0.062 Uiso 1 1 calc R . . C21C C 0.59248(17) -0.16872(10) 0.2898(2) 0.0771(10) Uani 1 1 d . . . H21A H 0.5882 -0.2009 0.2723 0.092 Uiso 1 1 calc R . . C22C C 0.66253(14) -0.15302(9) 0.32521(18) 0.0592(8) Uani 1 1 d . . . H22A H 0.7056 -0.1745 0.3318 0.071 Uiso 1 1 calc R . . C23A C 0.69775(12) -0.05407(7) 0.51726(12) 0.0345(5) Uani 1 1 d . . . C24A C 0.63997(15) -0.02330(8) 0.54332(15) 0.0498(6) Uani 1 1 d . . . H24A H 0.6239 0.0030 0.5114 0.060 Uiso 1 1 calc R . . C25A C 0.60515(18) -0.03035(10) 0.61562(17) 0.0669(8) Uani 1 1 d . . . H25A H 0.5655 -0.0089 0.6325 0.080 Uiso 1 1 calc R . . C26A C 0.6276(2) -0.06793(11) 0.66249(16) 0.0703(9) Uani 1 1 d . . . H26A H 0.6040 -0.0725 0.7121 0.084 Uiso 1 1 calc R . . C27A C 0.68442(19) -0.09911(12) 0.63762(16) 0.0703(8) Uani 1 1 d . . . H27A H 0.6999 -0.1253 0.6700 0.084 Uiso 1 1 calc R . . C28C C 0.71946(15) -0.09242(9) 0.56510(14) 0.0515(6) Uani 1 1 d . . . H28A H 0.7585 -0.1143 0.5482 0.062 Uiso 1 1 calc R . . C29A C 0.90562(11) 0.12624(6) 0.30492(10) 0.0263(4) Uani 1 1 d . . . C30 C 0.87147(12) 0.08351(7) 0.26207(10) 0.0288(4) Uani 1 1 d . . . H30A H 0.9158 0.0633 0.2430 0.035 Uiso 1 1 calc R . . C31 C 0.81885(12) 0.09750(7) 0.19193(11) 0.0331(4) Uani 1 1 d . . . C32 C 0.81403(15) 0.06761(9) 0.12628(12) 0.0458(6) Uani 1 1 d . . . H32A H 0.8472 0.0403 0.1238 0.055 Uiso 1 1 calc R . . C33A C 0.76156(17) 0.07726(11) 0.06480(14) 0.0603(7) Uani 1 1 d . . . H33A H 0.7588 0.0565 0.0206 0.072 Uiso 1 1 calc R . . C34A C 0.71343(16) 0.11661(11) 0.06717(14) 0.0597(7) Uani 1 1 d . . . H34A H 0.6772 0.1230 0.0249 0.072 Uiso 1 1 calc R . . C35 C 0.71779(16) 0.14683(10) 0.13101(15) 0.0561(7) Uani 1 1 d . . . H35A H 0.6846 0.1742 0.1327 0.067 Uiso 1 1 calc R . . C36 C 0.77083(14) 0.13743(8) 0.19325(13) 0.0430(5) Uani 1 1 d . . . H36A H 0.7740 0.1586 0.2369 0.052 Uiso 1 1 calc R . . C37 C 0.97348(12) 0.15274(7) 0.2736(1) 0.0303(4) Uani 1 1 d . . . C38 C 1.03899(13) 0.12758(8) 0.24785(13) 0.0414(5) Uani 1 1 d . . . H38A H 1.0391 0.0936 0.2494 0.050 Uiso 1 1 calc R . . C39 C 1.10394(14) 0.15172(9) 0.22011(14) 0.0493(6) Uani 1 1 d . . . H39A H 1.1486 0.1342 0.2034 0.059 Uiso 1 1 calc R . . C40 C 1.10430(14) 0.20077(9) 0.21650(13) 0.0482(6) Uani 1 1 d . . . H40A H 1.1490 0.2171 0.1973 0.058 Uiso 1 1 calc R . . C41 C 1.03935(14) 0.22631(8) 0.24100(13) 0.0442(5) Uani 1 1 d . . . H41A H 1.0392 0.2602 0.2379 0.053 Uiso 1 1 calc R . . C42 C 0.97446(13) 0.20238(7) 0.27014(12) 0.0363(5) Uani 1 1 d . . . H42A H 0.9304 0.2201 0.2878 0.044 Uiso 1 1 calc R . . C43 C 0.76217(11) 0.13486(7) 0.63305(11) 0.0262(4) Uani 1 1 d . . . C44A C 0.72402(10) 0.11849(7) 0.5561(1) 0.0258(4) Uani 1 1 d . . . H44A H 0.7191 0.0829 0.5578 0.031 Uiso 1 1 calc R . . C45 C 0.64191(11) 0.13939(7) 0.54222(10) 0.0272(4) Uani 1 1 d . . . C46 C 0.62288(14) 0.18510(8) 0.56524(14) 0.0480(6) Uani 1 1 d . . . H46A H 0.6611 0.2041 0.5925 0.058 Uiso 1 1 calc R . . C47 C 0.54810(17) 0.20352(10) 0.54886(16) 0.0640(8) Uani 1 1 d . . . H47A H 0.5357 0.2352 0.5644 0.077 Uiso 1 1 calc R . . C48 C 0.49238(15) 0.17641(11) 0.51061(16) 0.0603(7) Uani 1 1 d . . . H48A H 0.4411 0.1890 0.5003 0.072 Uiso 1 1 calc R . . C49 C 0.51042(16) 0.13132(11) 0.48729(19) 0.0722(9) Uani 1 1 d . . . H49A H 0.4717 0.1125 0.4604 0.087 Uiso 1 1 calc R . . C50 C 0.58507(14) 0.11280(9) 0.50267(16) 0.0546(7) Uani 1 1 d . . . H50A H 0.5972 0.0814 0.4857 0.066 Uiso 1 1 calc R . . C51 C 0.72674(11) 0.12088(7) 0.70842(11) 0.0302(4) Uani 1 1 d . . . C52 C 0.72250(13) 0.15269(8) 0.77148(12) 0.0406(5) Uani 1 1 d . . . H52A H 0.7446 0.1838 0.7671 0.049 Uiso 1 1 calc R . . C53 C 0.68636(14) 0.13945(10) 0.84032(13) 0.0508(6) Uani 1 1 d . . . H53A H 0.6828 0.1617 0.8824 0.061 Uiso 1 1 calc R . . C54A C 0.65555(14) 0.09415(10) 0.84799(13) 0.0512(6) Uani 1 1 d . . . H54A H 0.6314 0.0850 0.8956 0.061 Uiso 1 1 calc R . . C55A C 0.65973(13) 0.06195(9) 0.78636(13) 0.0458(6) Uani 1 1 d . . . H55A H 0.6388 0.0306 0.7918 0.055 Uiso 1 1 calc R . . C56 C 0.69455(12) 0.07547(8) 0.71651(12) 0.0380(5) Uani 1 1 d . . . H56A H 0.6964 0.0535 0.6740 0.046 Uiso 1 1 calc R . . C57 C 1.08378(11) 0.21387(6) 0.55149(11) 0.0275(4) Uani 1 1 d . . . C58 C 1.00509(11) 0.23065(7) 0.51658(11) 0.0286(4) Uani 1 1 d . . . H58A H 0.9993 0.2179 0.4618 0.034 Uiso 1 1 calc R . . C59A C 1.00176(11) 0.28505(7) 0.51305(11) 0.0299(4) Uani 1 1 d . . . C60 C 0.98427(15) 0.30846(9) 0.44315(13) 0.0464(6) Uani 1 1 d . . . H60A H 0.9759 0.2906 0.3961 0.056 Uiso 1 1 calc R . . C61A C 0.97880(16) 0.35818(9) 0.44125(17) 0.0587(7) Uani 1 1 d . . . H61A H 0.9675 0.3739 0.3927 0.070 Uiso 1 1 calc R . . C62 C 0.98938(15) 0.38440(9) 0.50773(18) 0.0561(7) Uani 1 1 d . . . H62A H 0.9840 0.4182 0.5062 0.067 Uiso 1 1 calc R . . C63 C 1.00809(16) 0.36144(9) 0.57797(16) 0.0559(7) Uani 1 1 d . . . H63A H 1.0168 0.3795 0.6247 0.067 Uiso 1 1 calc R . . C64 C 1.01417(14) 0.31197(8) 0.58000(14) 0.0449(6) Uani 1 1 d . . . H64A H 1.0271 0.2965 0.6284 0.054 Uiso 1 1 calc R . . C65 C 1.15710(12) 0.22203(7) 0.50872(12) 0.0320(4) Uani 1 1 d . . . C66 C 1.15859(13) 0.21691(8) 0.42742(13) 0.0434(5) Uani 1 1 d . . . H66A H 1.1125 0.2070 0.3988 0.052 Uiso 1 1 calc R . . C67 C 1.22849(15) 0.22648(10) 0.38789(16) 0.0572(7) Uani 1 1 d . . . H67A H 1.2297 0.2228 0.3324 0.069 Uiso 1 1 calc R . . C68 C 1.29478(15) 0.24104(10) 0.42824(17) 0.0598(7) Uani 1 1 d . . . H68A H 1.3416 0.2478 0.4007 0.072 Uiso 1 1 calc R . . C69 C 1.29399(14) 0.24594(9) 0.50802(18) 0.0562(7) Uani 1 1 d . . . H69A H 1.3404 0.2559 0.5359 0.067 Uiso 1 1 calc R . . C70 C 1.22593(13) 0.23642(8) 0.54882(14) 0.0428(5) Uani 1 1 d . . . H70A H 1.2262 0.2397 0.6045 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.03009(13) 0.02746(12) 0.03149(13) 0.00282(9) 0.00952(9) 0.00401(10) Cu2 0.02855(12) 0.02281(11) 0.02524(12) -0.00201(9) 0.00473(9) -0.00167(9) Cu3 0.03066(12) 0.02392(11) 0.02244(11) -0.00393(9) 0.00465(9) -0.00345(9) Cu4 0.02467(12) 0.02702(12) 0.02357(11) -0.00322(9) 0.00318(9) -0.00520(9) Cu5 0.02403(12) 0.03185(13) 0.02563(12) 0.00108(9) 0.00179(9) -0.00382(9) N1 0.0332(9) 0.0259(8) 0.0292(8) -0.0012(6) 0.0057(7) 0.0028(7) N2 0.0295(8) 0.0245(8) 0.0271(8) -0.0056(6) 0.0024(6) -0.0021(7) N3 0.0327(9) 0.0259(8) 0.0237(8) -0.0027(6) 0.0026(6) -0.0040(7) N4 0.0242(8) 0.0325(8) 0.0250(8) -0.0042(6) 0.0028(6) -0.0027(7) N5 0.0246(8) 0.0242(8) 0.0326(9) -0.0002(6) 0.0004(6) 0.0004(6) O1 0.0289(7) 0.0318(7) 0.0312(7) 0.0057(6) 0.0093(5) 0.0056(6) O2 0.0415(8) 0.0246(7) 0.0364(8) 0.0020(6) 0.0136(6) 0.0033(6) O3 0.0283(7) 0.0226(6) 0.0332(7) -0.0023(5) 0.0106(5) -0.0015(5) O4 0.0421(8) 0.0235(7) 0.0310(7) -0.0073(5) 0.0116(6) -0.0054(6) O5 0.0463(8) 0.0231(6) 0.0215(6) -0.0007(5) 0.0085(6) -0.0052(6) O6 0.0381(8) 0.0292(7) 0.0268(7) -0.0078(5) 0.0067(6) -0.0121(6) O7 0.0287(7) 0.0283(7) 0.0255(7) -0.0073(5) 0.0077(5) -0.0075(5) O8 0.0264(7) 0.0502(9) 0.0234(7) -0.0047(6) -0.0003(5) -0.0105(6) O9 0.0244(7) 0.0346(7) 0.0251(7) 0.0001(5) 0.0021(5) -0.0084(6) O10 0.0265(7) 0.0330(7) 0.0416(8) 0.0095(6) 0.0041(6) 0.0049(6) C1 0.0342(11) 0.032(1) 0.0253(10) -0.0006(8) 0.0041(8) 0.0003(8) C2 0.0292(10) 0.0342(10) 0.0288(10) 0.0039(8) 0.0078(8) 0.0020(8) C3 0.0342(11) 0.0262(9) 0.0303(10) 0.0027(8) 0.0091(8) 0.0039(8) C4 0.0392(12) 0.0526(14) 0.0401(12) -0.0063(10) 0.0095(10) -0.0049(11) C5 0.0572(16) 0.0641(17) 0.0450(14) -0.0071(12) -0.0002(12) -0.0096(13) C6 0.0734(18) 0.0430(13) 0.0337(12) -0.0055(10) 0.0112(12) -0.0065(12) C7 0.0562(15) 0.0479(14) 0.0410(13) -0.0019(10) 0.0235(11) 0.0041(12) C8 0.0373(12) 0.0441(13) 0.0405(12) -0.0012(10) 0.0095(9) 0.0035(10) C9 0.0385(12) 0.0308(10) 0.0337(11) -0.0017(8) 0.0122(9) -0.0038(9) C10 0.0428(14) 0.0529(15) 0.084(2) 0.0150(14) 0.0021(13) -0.0083(12) C11 0.0450(16) 0.066(2) 0.124(3) 0.0183(19) 0.0148(17) -0.0185(14) C12 0.070(2) 0.0432(15) 0.084(2) 0.0038(14) 0.0360(16) -0.0159(14) C13 0.080(2) 0.0432(14) 0.0453(14) 0.0088(11) 0.0222(13) -0.0042(13) C14 0.0505(14) 0.0440(13) 0.0374(12) 0.0056(10) 0.0116(10) -0.0031(11) C15C 0.0246(9) 0.0260(9) 0.0289(10) -0.0028(7) 0.0041(7) -0.0031(7) C16C 0.0243(9) 0.0251(9) 0.0296(10) -0.0003(7) 0.0044(7) -0.0007(7) C17C 0.027(1) 0.0275(9) 0.0309(10) -0.0004(8) 0.0037(8) -0.0024(8) C18A 0.0380(12) 0.0344(12) 0.0677(16) -0.0109(11) -0.0104(11) 0.0033(10) C19C 0.0361(13) 0.0527(15) 0.0727(18) -0.0019(13) -0.0156(12) 0.0050(11) C20C 0.0375(13) 0.0524(15) 0.0642(16) 0.0008(12) -0.0135(11) -0.0122(11) C21C 0.0557(17) 0.0428(15) 0.131(3) -0.0373(17) -0.0256(18) -0.0056(13) C22C 0.0379(13) 0.0363(13) 0.102(2) -0.0224(13) -0.0174(14) 0.0059(10) C23A 0.0377(11) 0.0335(11) 0.0327(11) -0.0065(9) 0.0099(8) -0.0127(9) C24A 0.0586(15) 0.0335(12) 0.0589(15) -0.0052(11) 0.0321(12) -0.0070(11) C25A 0.083(2) 0.0459(15) 0.0747(19) -0.0215(14) 0.0525(16) -0.0178(14) C26A 0.099(2) 0.070(2) 0.0432(15) -0.0112(14) 0.0327(15) -0.0295(18) C27A 0.085(2) 0.085(2) 0.0425(15) 0.0181(14) 0.0151(14) -0.0046(18) C28C 0.0557(15) 0.0588(16) 0.0403(13) 0.0104(11) 0.0093(11) 0.0022(12) C29A 0.0323(10) 0.0242(9) 0.0223(9) 0.0017(7) 0.0015(7) 0.0007(8) C30 0.0382(11) 0.0262(9) 0.0225(9) -0.0003(7) 0.0085(8) -0.0020(8) C31 0.0398(12) 0.0357(11) 0.0238(10) 0.0018(8) 0.0028(8) -0.0091(9) C32 0.0568(15) 0.0507(14) 0.0301(11) -0.0054(10) 0.0014(10) -0.0062(11) C33A 0.0672(18) 0.085(2) 0.0281(12) -0.0093(12) -0.0036(11) -0.0131(16) C34A 0.0560(16) 0.090(2) 0.0327(13) 0.0146(13) -0.0086(11) -0.0108(15) C35 0.0553(16) 0.0608(16) 0.0518(16) 0.0124(13) -0.0082(12) 0.0043(13) C36 0.0488(14) 0.0427(12) 0.0373(12) -0.0002(10) -0.0031(10) 0.0003(11) C37 0.0379(11) 0.0329(10) 0.0202(9) 0.0014(8) 0.0015(8) -0.0055(9) C38 0.0464(13) 0.0355(12) 0.0429(13) -0.0002(9) 0.0106(10) -0.0007(10) C39 0.0397(13) 0.0554(15) 0.0535(15) -0.0013(12) 0.0162(11) -0.0022(11) C40 0.0455(14) 0.0604(16) 0.0392(13) 0.0023(11) 0.0111(10) -0.0167(12) C41 0.0584(15) 0.0360(12) 0.0387(12) 0.0034(9) 0.0087(11) -0.0115(11) C42 0.0459(13) 0.0322(11) 0.0311(11) 0.0013(8) 0.0064(9) -0.0025(9) C43 0.0235(9) 0.0282(9) 0.0270(9) -0.0026(7) 0.0026(7) -0.0002(8) C44A 0.0248(9) 0.0267(9) 0.0261(9) -0.0051(7) 0.0032(7) -0.0041(7) C45 0.0271(10) 0.0311(10) 0.0235(9) -0.0003(7) 0.0033(7) -0.0004(8) C46 0.0472(14) 0.0451(13) 0.0509(14) -0.0143(11) -0.0124(11) 0.0114(11) C47 0.0723(19) 0.0617(17) 0.0576(17) -0.0138(13) -0.0070(14) 0.0343(15) C48 0.0384(14) 0.083(2) 0.0592(17) 0.0098(14) -0.0009(12) 0.0241(14) C49 0.0414(15) 0.072(2) 0.102(2) 0.0053(17) -0.0270(15) -0.0030(14) C50 0.0410(13) 0.0385(13) 0.0832(19) -0.0086(12) -0.0200(13) -0.0026(11) C51 0.0191(9) 0.0438(12) 0.0277(10) 0.0010(8) 0.0020(7) -0.0024(8) C52 0.0383(12) 0.0522(13) 0.0316(11) -0.005(1) 0.0085(9) -0.0065(10) C53 0.0449(14) 0.0767(18) 0.0312(12) -0.0092(11) 0.0084(10) -0.0098(13) C54A 0.0377(13) 0.0848(19) 0.0313(12) 0.0090(12) 0.0060(9) -0.0110(13) C55A 0.0341(12) 0.0610(15) 0.0422(13) 0.0129(11) 0.0032(9) -0.0125(11) C56 0.0331(11) 0.0480(13) 0.0330(11) 0.0017(9) 0.0007(9) -0.009(1) C57 0.028(1) 0.0231(9) 0.0317(10) -0.0022(8) 0.0051(8) -0.0034(8) C58 0.0275(10) 0.0311(10) 0.0272(10) 0.0009(8) 0.0024(7) -0.0067(8) C59A 0.0219(9) 0.0311(10) 0.0368(11) 0.0040(8) -0.0003(8) -0.0039(8) C60 0.0563(15) 0.0472(13) 0.0356(12) 0.005(1) 0.0013(10) 0.0041(11) C61A 0.0647(17) 0.0505(15) 0.0611(17) 0.0250(13) 0.0033(13) 0.0070(13) C62 0.0507(15) 0.0331(12) 0.085(2) 0.0118(13) 0.0041(14) -0.0002(11) C63 0.0617(17) 0.0365(13) 0.0688(18) -0.0067(12) -0.0109(13) -0.0038(12) C64 0.0543(14) 0.0365(12) 0.0434(13) 0.0015(10) -0.0081(11) -0.0043(11) C65 0.0292(10) 0.0258(10) 0.0413(11) 0.0072(8) 0.0079(8) 0.0009(8) C66 0.0358(12) 0.0543(14) 0.0406(12) 0.0097(10) 0.0099(9) 0.0029(10) C67 0.0477(15) 0.0743(18) 0.0504(15) 0.0225(13) 0.0203(12) 0.0085(13) C68 0.0358(14) 0.0669(18) 0.078(2) 0.0289(15) 0.0227(13) 0.0070(12) C69 0.0286(12) 0.0544(15) 0.086(2) 0.0153(14) 0.0077(12) -0.0063(11) C70 0.0346(12) 0.0401(12) 0.0540(14) 0.0063(10) 0.0036(10) -0.0067(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 O10 1.9094(13) 3_756 ? Cu1 O3 1.9242(12) . ? Cu1 O1 1.9310(13) . ? Cu1 N1 1.9541(16) . ? Cu2 O5 1.8885(13) . ? Cu2 O3 1.8965(12) . ? Cu2 O2 1.8981(14) . ? Cu2 N2 1.9534(16) . ? Cu3 O5 1.8969(12) . ? Cu3 O7 1.9045(12) . ? Cu3 O4 1.9116(13) . ? Cu3 N3 1.9638(16) . ? Cu4 O6 1.9072(13) . ? Cu4 O7 1.9098(12) . ? Cu4 O9 1.9249(12) . ? Cu4 N4 1.9555(16) . ? Cu5 O8 1.9149(13) . ? Cu5 O9 1.9307(12) . ? Cu5 O1 1.9327(13) 3_756 ? Cu5 N5 1.9561(16) . ? N1 C1 1.287(2) . ? N1 O2 1.3607(19) . ? N2 C15C 1.295(2) . ? N2 O4 1.3589(19) . ? N3 C29A 1.293(2) . ? N3 O6 1.3600(19) . ? N4 C43 1.285(2) . ? N4 O8 1.3618(19) . ? N5 C57 1.293(2) . ? N5 O10 1.3555(19) . ? O1 C2 1.424(2) . ? O1 Cu5 1.9327(13) 3_756 ? O3 C16C 1.430(2) . ? O5 C30 1.432(2) . ? O7 C44A 1.431(2) . ? O9 C58 1.424(2) . ? O10 Cu1 1.9094(13) 3_756 ? C1 C9 1.485(3) . ? C1 C2 1.509(3) . ? C2 C3 1.522(3) . ? C2 H2A 1.0000 . ? C3 C8 1.383(3) . ? C3 C4 1.385(3) . ? C4 C5 1.385(3) . ? C4 H4A 0.9500 . ? C5 C6 1.378(4) . ? C5 H5A 0.9500 . ? C6 C7 1.363(4) . ? C6 H6A 0.9500 . ? C7 C8 1.390(3) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 C10 1.377(3) . ? C9 C14 1.382(3) . ? C10 C11 1.390(4) . ? C10 H10A 0.9500 . ? C11 C12 1.365(4) . ? C11 H11A 0.9500 . ? C12 C13 1.357(4) . ? C12 H12A 0.9500 . ? C13 C14 1.391(3) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15C C23A 1.473(3) . ? C15C C16C 1.519(2) . ? C16C C17C 1.521(2) . ? C16C H16A 1.0000 . ? C17C C22C 1.369(3) . ? C17C C18A 1.378(3) . ? C18A C19C 1.386(3) . ? C18A H18A 0.9500 . ? C19C C20C 1.349(3) . ? C19C H19A 0.9500 . ? C20C C21C 1.366(4) . ? C20C H20A 0.9500 . ? C21C C22C 1.388(3) . ? C21C H21A 0.9500 . ? C22C H22A 0.9500 . ? C23A C24A 1.385(3) . ? C23A C28C 1.390(3) . ? C24A C25A 1.390(3) . ? C24A H24A 0.9500 . ? C25A C26A 1.367(4) . ? C25A H25A 0.9500 . ? C26A C27A 1.374(4) . ? C26A H26A 0.9500 . ? C27A C28C 1.394(3) . ? C27A H27A 0.9500 . ? C28C H28A 0.9500 . ? C29A C37 1.478(3) . ? C29A C30 1.507(3) . ? C30 C31 1.521(3) . ? C30 H30A 1.0000 . ? C31 C36 1.382(3) . ? C31 C32 1.395(3) . ? C32 C33A 1.381(3) . ? C32 H32A 0.9500 . ? C33A C34A 1.371(4) . ? C33A H33A 0.9500 . ? C34A C35 1.376(4) . ? C34A H34A 0.9500 . ? C35 C36 1.395(3) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C42 1.390(3) . ? C37 C38 1.394(3) . ? C38 C39 1.384(3) . ? C38 H38A 0.9500 . ? C39 C40 1.373(3) . ? C39 H39A 0.9500 . ? C40 C41 1.385(3) . ? C40 H40A 0.9500 . ? C41 C42 1.389(3) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 C51 1.481(3) . ? C43 C44A 1.514(2) . ? C44A C45 1.522(3) . ? C44A H44A 1.0000 . ? C45 C46 1.378(3) . ? C45 C50 1.378(3) . ? C46 C47 1.389(3) . ? C46 H46A 0.9500 . ? C47 C48 1.363(4) . ? C47 H47A 0.9500 . ? C48 C49 1.359(4) . ? C48 H48A 0.9500 . ? C49 C50 1.385(3) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 C56 1.391(3) . ? C51 C52 1.396(3) . ? C52 C53 1.385(3) . ? C52 H52A 0.9500 . ? C53 C54A 1.378(4) . ? C53 H53A 0.9500 . ? C54A C55A 1.384(3) . ? C54A H54A 0.9500 . ? C55A C56 1.391(3) . ? C55A H55A 0.9500 . ? C56 H56A 0.9500 . ? C57 C65 1.473(3) . ? C57 C58 1.520(3) . ? C58 C59A 1.524(3) . ? C58 H58A 1.0000 . ? C59A C64 1.376(3) . ? C59A C60 1.382(3) . ? C60 C61A 1.395(3) . ? C60 H60A 0.9500 . ? C61A C62 1.355(4) . ? C61A H61A 0.9500 . ? C62 C63 1.385(4) . ? C62 H62A 0.9500 . ? C63 C64 1.388(3) . ? C63 H63A 0.9500 . ? C64 H64A 0.9500 . ? C65 C66 1.390(3) . ? C65 C70 1.395(3) . ? C66 C67 1.402(3) . ? C66 H66A 0.9500 . ? C67 C68 1.363(4) . ? C67 H67A 0.9500 . ? C68 C69 1.363(4) . ? C68 H68A 0.9500 . ? C69 C70 1.386(3) . ? C69 H69A 0.9500 . ? C70 H70A 0.9500 . ? 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 O10 Cu1 O3 95.63(6) 3_756 . ? O10 Cu1 O1 92.31(6) 3_756 . ? O3 Cu1 O1 169.34(6) . . ? O10 Cu1 N1 172.86(6) 3_756 . ? O3 Cu1 N1 88.78(6) . . ? O1 Cu1 N1 82.65(6) . . ? O5 Cu2 O3 171.93(6) . . ? O5 Cu2 O2 93.66(6) . . ? O3 Cu2 O2 94.33(5) . . ? O5 Cu2 N2 88.54(6) . . ? O3 Cu2 N2 83.75(6) . . ? O2 Cu2 N2 170.41(6) . . ? O5 Cu3 O7 169.89(5) . . ? O5 Cu3 O4 93.78(5) . . ? O7 Cu3 O4 95.99(5) . . ? O5 Cu3 N3 82.63(6) . . ? O7 Cu3 N3 88.23(6) . . ? O4 Cu3 N3 168.96(6) . . ? O6 Cu4 O7 93.77(5) . . ? O6 Cu4 O9 94.94(5) . . ? O7 Cu4 O9 171.24(5) . . ? O6 Cu4 N4 172.17(6) . . ? O7 Cu4 N4 82.38(6) . . ? O9 Cu4 N4 88.86(6) . . ? O8 Cu5 O9 92.12(5) . . ? O8 Cu5 O1 96.02(6) . 3_756 ? O9 Cu5 O1 166.54(6) . 3_756 ? O8 Cu5 N5 172.03(6) . . ? O9 Cu5 N5 82.19(6) . . ? O1 Cu5 N5 88.58(6) 3_756 . ? C1 N1 O2 119.39(16) . . ? C1 N1 Cu1 116.42(13) . . ? O2 N1 Cu1 123.68(12) . . ? C15C N2 O4 119.54(15) . . ? C15C N2 Cu2 115.74(13) . . ? O4 N2 Cu2 124.08(11) . . ? C29A N3 O6 119.65(15) . . ? C29A N3 Cu3 116.00(12) . . ? O6 N3 Cu3 123.38(11) . . ? C43 N4 O8 120.26(15) . . ? C43 N4 Cu4 117.08(12) . . ? O8 N4 Cu4 122.51(11) . . ? C57 N5 O10 119.36(16) . . ? C57 N5 Cu5 117.17(13) . . ? O10 N5 Cu5 123.29(11) . . ? C2 O1 Cu1 114.36(11) . . ? C2 O1 Cu5 122.38(11) . 3_756 ? Cu1 O1 Cu5 108.84(6) . 3_756 ? N1 O2 Cu2 113.53(10) . . ? C16C O3 Cu2 113.95(10) . . ? C16C O3 Cu1 125.99(11) . . ? Cu2 O3 Cu1 115.32(6) . . ? N2 O4 Cu3 113.77(10) . . ? C30 O5 Cu2 125.15(11) . . ? C30 O5 Cu3 114.93(11) . . ? Cu2 O5 Cu3 117.00(6) . . ? N3 O6 Cu4 112.22(10) . . ? C44A O7 Cu3 123.94(10) . . ? C44A O7 Cu4 115.2(1) . . ? Cu3 O7 Cu4 112.33(6) . . ? N4 O8 Cu5 108.77(10) . . ? C58 O9 Cu4 123.32(11) . . ? C58 O9 Cu5 114.77(10) . . ? Cu4 O9 Cu5 106.90(6) . . ? N5 O10 Cu1 108.34(10) . 3_756 ? N1 C1 C9 124.64(18) . . ? N1 C1 C2 115.12(17) . . ? C9 C1 C2 120.21(17) . . ? O1 C2 C1 110.07(15) . . ? O1 C2 C3 112.01(16) . . ? C1 C2 C3 108.33(15) . . ? O1 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2A 108.8 . . ? C8 C3 C4 118.57(19) . . ? C8 C3 C2 120.41(19) . . ? C4 C3 C2 120.83(18) . . ? C3 C4 C5 120.3(2) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C6 C5 C4 120.5(2) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C7 C6 C5 119.6(2) . . ? C7 C6 H6A 120.2 . . ? C5 C6 H6A 120.2 . . ? C6 C7 C8 120.3(2) . . ? C6 C7 H7A 119.8 . . ? C8 C7 H7A 119.8 . . ? C3 C8 C7 120.7(2) . . ? C3 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C10 C9 C14 118.7(2) . . ? C10 C9 C1 120.2(2) . . ? C14 C9 C1 121.13(19) . . ? C9 C10 C11 119.9(3) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C12 C11 C10 120.9(3) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C13 C12 C11 119.6(2) . . ? C13 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C12 C13 C14 120.3(3) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C9 C14 C13 120.5(2) . . ? C9 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? N2 C15C C23A 126.21(17) . . ? N2 C15C C16C 113.69(16) . . ? C23A C15C C16C 120.01(16) . . ? O3 C16C C15C 110.29(14) . . ? O3 C16C C17C 110.25(15) . . ? C15C C16C C17C 110.41(15) . . ? O3 C16C H16A 108.6 . . ? C15C C16C H16A 108.6 . . ? C17C C16C H16A 108.6 . . ? C22C C17C C18A 117.79(19) . . ? C22C C17C C16C 119.34(18) . . ? C18A C17C C16C 122.87(17) . . ? C17C C18A C19C 121.3(2) . . ? C17C C18A H18A 119.4 . . ? C19C C18A H18A 119.4 . . ? C20C C19C C18A 120.5(2) . . ? C20C C19C H19A 119.8 . . ? C18A C19C H19A 119.8 . . ? C19C C20C C21C 119.0(2) . . ? C19C C20C H20A 120.5 . . ? C21C C20C H20A 120.5 . . ? C20C C21C C22C 121.0(2) . . ? C20C C21C H21A 119.5 . . ? C22C C21C H21A 119.5 . . ? C17C C22C C21C 120.4(2) . . ? C17C C22C H22A 119.8 . . ? C21C C22C H22A 119.8 . . ? C24A C23A C28C 118.1(2) . . ? C24A C23A C15C 121.9(2) . . ? C28C C23A C15C 119.9(2) . . ? C23A C24A C25A 120.9(2) . . ? C23A C24A H24A 119.5 . . ? C25A C24A H24A 119.5 . . ? C26A C25A C24A 120.4(3) . . ? C26A C25A H25A 119.8 . . ? C24A C25A H25A 119.8 . . ? C25A C26A C27A 119.7(3) . . ? C25A C26A H26A 120.1 . . ? C27A C26A H26A 120.1 . . ? C26A C27A C28C 120.3(3) . . ? C26A C27A H27A 119.9 . . ? C28C C27A H27A 119.9 . . ? C23A C28C C27A 120.6(3) . . ? C23A C28C H28A 119.7 . . ? C27A C28C H28A 119.7 . . ? N3 C29A C37 124.67(16) . . ? N3 C29A C30 114.26(16) . . ? C37 C29A C30 121.07(16) . . ? O5 C30 C29A 109.32(15) . . ? O5 C30 C31 108.58(16) . . ? C29A C30 C31 112.61(15) . . ? O5 C30 H30A 108.8 . . ? C29A C30 H30A 108.8 . . ? C31 C30 H30A 108.8 . . ? C36 C31 C32 118.35(19) . . ? C36 C31 C30 121.91(17) . . ? C32 C31 C30 119.57(19) . . ? C33A C32 C31 120.7(2) . . ? C33A C32 H32A 119.6 . . ? C31 C32 H32A 119.6 . . ? C34A C33A C32 120.4(2) . . ? C34A C33A H33A 119.8 . . ? C32 C33A H33A 119.8 . . ? C33A C34A C35 119.8(2) . . ? C33A C34A H34A 120.1 . . ? C35 C34A H34A 120.1 . . ? C34A C35 C36 120.2(3) . . ? C34A C35 H35A 119.9 . . ? C36 C35 H35A 119.9 . . ? C31 C36 C35 120.5(2) . . ? C31 C36 H36A 119.7 . . ? C35 C36 H36A 119.7 . . ? C42 C37 C38 118.72(19) . . ? C42 C37 C29A 121.76(18) . . ? C38 C37 C29A 119.51(18) . . ? C39 C38 C37 120.4(2) . . ? C39 C38 H38A 119.8 . . ? C37 C38 H38A 119.8 . . ? C40 C39 C38 120.5(2) . . ? C40 C39 H39A 119.8 . . ? C38 C39 H39A 119.8 . . ? C39 C40 C41 119.8(2) . . ? C39 C40 H40A 120.1 . . ? C41 C40 H40A 120.1 . . ? C40 C41 C42 120.0(2) . . ? C40 C41 H41A 120.0 . . ? C42 C41 H41A 120.0 . . ? C41 C42 C37 120.5(2) . . ? C41 C42 H42A 119.8 . . ? C37 C42 H42A 119.8 . . ? N4 C43 C51 125.73(16) . . ? N4 C43 C44A 114.72(16) . . ? C51 C43 C44A 119.55(16) . . ? O7 C44A C43 109.72(14) . . ? O7 C44A C45 110.08(14) . . ? C43 C44A C45 112.70(15) . . ? O7 C44A H44A 108.1 . . ? C43 C44A H44A 108.1 . . ? C45 C44A H44A 108.1 . . ? C46 C45 C50 118.27(19) . . ? C46 C45 C44A 122.15(17) . . ? C50 C45 C44A 119.53(18) . . ? C45 C46 C47 120.4(2) . . ? C45 C46 H46A 119.8 . . ? C47 C46 H46A 119.8 . . ? C48 C47 C46 120.4(2) . . ? C48 C47 H47A 119.8 . . ? C46 C47 H47A 119.8 . . ? C49 C48 C47 119.8(2) . . ? C49 C48 H48A 120.1 . . ? C47 C48 H48A 120.1 . . ? C48 C49 C50 120.2(3) . . ? C48 C49 H49A 119.9 . . ? C50 C49 H49A 119.9 . . ? C45 C50 C49 120.9(2) . . ? C45 C50 H50A 119.6 . . ? C49 C50 H50A 119.6 . . ? C56 C51 C52 118.59(19) . . ? C56 C51 C43 119.70(18) . . ? C52 C51 C43 121.68(18) . . ? C53 C52 C51 120.7(2) . . ? C53 C52 H52A 119.7 . . ? C51 C52 H52A 119.7 . . ? C54A C53 C52 120.2(2) . . ? C54A C53 H53A 119.9 . . ? C52 C53 H53A 119.9 . . ? C53 C54A C55A 120.0(2) . . ? C53 C54A H54A 120.0 . . ? C55A C54A H54A 120.0 . . ? C54A C55A C56 120.0(2) . . ? C54A C55A H55A 120.0 . . ? C56 C55A H55A 120.0 . . ? C51 C56 C55A 120.6(2) . . ? C51 C56 H56A 119.7 . . ? C55A C56 H56A 119.7 . . ? N5 C57 C65 125.37(17) . . ? N5 C57 C58 114.50(16) . . ? C65 C57 C58 120.13(16) . . ? O9 C58 C57 109.98(15) . . ? O9 C58 C59A 110.44(16) . . ? C57 C58 C59A 110.80(15) . . ? O9 C58 H58A 108.5 . . ? C57 C58 H58A 108.5 . . ? C59A C58 H58A 108.5 . . ? C64 C59A C60 118.4(2) . . ? C64 C59A C58 120.61(18) . . ? C60 C59A C58 120.94(18) . . ? C59A C60 C61A 120.4(2) . . ? C59A C60 H60A 119.8 . . ? C61A C60 H60A 119.8 . . ? C62 C61A C60 120.9(2) . . ? C62 C61A H61A 119.6 . . ? C60 C61A H61A 119.6 . . ? C61A C62 C63 119.3(2) . . ? C61A C62 H62A 120.3 . . ? C63 C62 H62A 120.3 . . ? C62 C63 C64 119.9(2) . . ? C62 C63 H63A 120.0 . . ? C64 C63 H63A 120.0 . . ? C59A C64 C63 121.0(2) . . ? C59A C64 H64A 119.5 . . ? C63 C64 H64A 119.5 . . ? C66 C65 C70 118.6(2) . . ? C66 C65 C57 120.77(18) . . ? C70 C65 C57 120.58(19) . . ? C65 C66 C67 119.6(2) . . ? C65 C66 H66A 120.2 . . ? C67 C66 H66A 120.2 . . ? C68 C67 C66 120.7(2) . . ? C68 C67 H67A 119.6 . . ? C66 C67 H67A 119.6 . . ? C69 C68 C67 120.1(2) . . ? C69 C68 H68A 120.0 . . ? C67 C68 H68A 120.0 . . ? C68 C69 C70 120.5(2) . . ? C68 C69 H69A 119.8 . . ? C70 C69 H69A 119.8 . . ? C69 C70 C65 120.5(2) . . ? C69 C70 H70A 119.8 . . ? C65 C70 H70A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.356 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.057