# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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 915725' #TrackingRef '1-3 new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H49 Cl Cu2 N4 O14' _chemical_formula_weight 1068.44 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4873(15) _cell_length_b 13.908(2) _cell_length_c 17.158(3) _cell_angle_alpha 67.376(5) _cell_angle_beta 89.533(5) _cell_angle_gamma 81.192(5) _cell_volume 2279.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Rectangular _exptl_crystal_colour Brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 1.067 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7992 _exptl_absorpt_correction_T_max 0.8564 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 28452 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8810 _reflns_number_gt 5719 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+0.6415P] 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 8810 _refine_ls_number_parameters 641 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1098 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 Cu2 Cu 0.52717(4) 0.39794(3) 0.10885(3) 0.03789(13) Uani 1 1 d . . . Cu1 Cu 0.85613(4) 0.19455(3) 0.41212(3) 0.03986(13) Uani 1 1 d . . . N1 N 1.0061(3) 0.2038(2) 0.47364(17) 0.0430(7) Uani 1 1 d . . . N2 N 0.7648(3) 0.2939(2) 0.45623(16) 0.0392(7) Uani 1 1 d . . . N3 N 0.5044(3) 0.4896(2) 0.17071(16) 0.0383(7) Uani 1 1 d . . . N4 N 0.3470(3) 0.4556(2) 0.07116(17) 0.0409(7) Uani 1 1 d . . . O1 O 0.9526(2) 0.09661(18) 0.37147(14) 0.0464(6) Uani 1 1 d . . . O2 O 0.7044(2) 0.18919(17) 0.35305(14) 0.0414(6) Uani 1 1 d . . . O3 O 1.0367(2) -0.03936(19) 0.30694(16) 0.0537(7) Uani 1 1 d . . . O4 O 0.5244(2) 0.1504(2) 0.27094(16) 0.0533(7) Uani 1 1 d . . . O5 O 0.7075(2) 0.35736(18) 0.13658(14) 0.0443(6) Uani 1 1 d . . . O6 O 0.5390(2) 0.30230(18) 0.05325(14) 0.0461(6) Uani 1 1 d . . . O8 O 0.6055(3) 0.1631(2) -0.01211(16) 0.0589(7) Uani 1 1 d . . . O7 O 0.9529(2) 0.2891(2) 0.14999(16) 0.0554(7) Uani 1 1 d . . . C1 C 1.0741(3) 0.0520(3) 0.3918(2) 0.0411(8) Uani 1 1 d . . . C6 C 1.1578(3) 0.0733(3) 0.4448(2) 0.0442(9) Uani 1 1 d . . . C7 C 1.1201(4) 0.1474(3) 0.4823(2) 0.0473(9) Uani 1 1 d . . . H7 H 1.1824 0.1566 0.5159 0.057 Uiso 1 1 calc R . . C8 C 0.9777(4) 0.2771(3) 0.5131(2) 0.0453(9) Uani 1 1 d . . . C14 C 0.6432(3) 0.3310(3) 0.4440(2) 0.0439(9) Uani 1 1 d . . . H14 H 0.6114 0.3781 0.4688 0.053 Uiso 1 1 calc R . . C15 C 0.5524(3) 0.3063(3) 0.3954(2) 0.0407(8) Uani 1 1 d . . . C20 C 0.5854(3) 0.2375(3) 0.3531(2) 0.0390(8) Uani 1 1 d . . . C19 C 0.4852(3) 0.2198(3) 0.3082(2) 0.0420(9) Uani 1 1 d . . . C18 C 0.3602(4) 0.2690(3) 0.3053(2) 0.0545(10) Uani 1 1 d . . . H18 H 0.2959 0.2564 0.2752 0.065 Uiso 1 1 calc R . . C13 C 0.8480(3) 0.3243(3) 0.5053(2) 0.0431(9) Uani 1 1 d . . . C12 C 0.8089(4) 0.3945(3) 0.5432(2) 0.0585(11) Uani 1 1 d . . . H12 H 0.7229 0.4261 0.5377 0.070 Uiso 1 1 calc R . . C9 C 1.0664(4) 0.3029(3) 0.5589(2) 0.0580(11) Uani 1 1 d . . . H9 H 1.1530 0.2725 0.5643 0.070 Uiso 1 1 calc R . . C26 C 0.9121(3) 0.3504(3) 0.1947(2) 0.0431(9) Uani 1 1 d . . . C25 C 0.7762(3) 0.3867(3) 0.1847(2) 0.0374(8) Uani 1 1 d . . . C27 C 0.9895(4) 0.3777(3) 0.2433(2) 0.0541(10) Uani 1 1 d . . . H27 H 1.0778 0.3528 0.2490 0.065 Uiso 1 1 calc R . . C30 C 0.7256(3) 0.4528(3) 0.2266(2) 0.0373(8) Uani 1 1 d . . . C29 C 0.8098(4) 0.4790(3) 0.2769(2) 0.0469(9) Uani 1 1 d . . . H29 H 0.7763 0.5219 0.3050 0.056 Uiso 1 1 calc R . . C31 C 0.5937(3) 0.5013(3) 0.2169(2) 0.0430(9) Uani 1 1 d . . . H31 H 0.5694 0.5449 0.2460 0.052 Uiso 1 1 calc R . . C32 C 0.3760(3) 0.5467(3) 0.1603(2) 0.0417(8) Uani 1 1 d . . . C37 C 0.2928(3) 0.5298(3) 0.1052(2) 0.0430(9) Uani 1 1 d . . . C33 C 0.3322(4) 0.6147(3) 0.1993(2) 0.0556(10) Uani 1 1 d . . . H33 H 0.3876 0.6256 0.2360 0.067 Uiso 1 1 calc R . . C38 C 0.2799(3) 0.4292(3) 0.0209(2) 0.0437(9) Uani 1 1 d . . . H38 H 0.1951 0.4638 0.0062 0.052 Uiso 1 1 calc R . . C39 C 0.3241(3) 0.3529(3) -0.0131(2) 0.0429(9) Uani 1 1 d . . . C44 C 0.4503(3) 0.2930(3) 0.0047(2) 0.0409(8) Uani 1 1 d . . . C43 C 0.4823(4) 0.2192(3) -0.0340(2) 0.0480(9) Uani 1 1 d . . . C40 C 0.2365(4) 0.3376(3) -0.0684(2) 0.0519(10) Uani 1 1 d . . . H40 H 0.1533 0.3762 -0.0796 0.062 Uiso 1 1 calc R . . C41 C 0.2721(4) 0.2679(3) -0.1050(2) 0.0603(11) Uani 1 1 d . . . H41 H 0.2137 0.2599 -0.1417 0.072 Uiso 1 1 calc R . . C17 C 0.3281(4) 0.3377(3) 0.3468(3) 0.0589(11) Uani 1 1 d . . . H17 H 0.2433 0.3708 0.3440 0.071 Uiso 1 1 calc R . . C16 C 0.4223(4) 0.3555(3) 0.3912(2) 0.0536(10) Uani 1 1 d . . . H16 H 0.4011 0.4007 0.4192 0.064 Uiso 1 1 calc R . . C45 C 1.0831(3) 0.2373(3) 0.1643(2) 0.0510(10) Uani 1 1 d . . . H45A H 1.1019 0.1947 0.2241 0.061 Uiso 1 1 calc R . . H45B H 1.1412 0.2888 0.1463 0.061 Uiso 1 1 calc R . . C46 C 1.1009(4) 0.1685(3) 0.1143(3) 0.0625(11) Uani 1 1 d . . . H46A H 1.0469 0.1150 0.1351 0.094 Uiso 1 1 calc R . . H46B H 1.1897 0.1357 0.1202 0.094 Uiso 1 1 calc R . . H46C H 1.0774 0.2108 0.0558 0.094 Uiso 1 1 calc R . . C23 C 0.4284(4) 0.1219(3) 0.2288(2) 0.0542(10) Uani 1 1 d . . . H23A H 0.3926 0.1819 0.1783 0.065 Uiso 1 1 calc R . . H23B H 0.3587 0.1000 0.2658 0.065 Uiso 1 1 calc R . . C10 C 1.0269(4) 0.3725(3) 0.5959(3) 0.0683(13) Uani 1 1 d . . . H10 H 1.0868 0.3900 0.6259 0.082 Uiso 1 1 calc R . . C42 C 0.3957(4) 0.2078(3) -0.0883(2) 0.0574(11) Uani 1 1 d . . . H42 H 0.4193 0.1601 -0.1138 0.069 Uiso 1 1 calc R . . C2 C 1.1243(4) -0.0237(3) 0.3574(2) 0.0457(9) Uani 1 1 d . . . C3 C 1.2504(4) -0.0749(3) 0.3758(2) 0.0508(10) Uani 1 1 d . . . H3 H 1.2817 -0.1239 0.3528 0.061 Uiso 1 1 calc R . . C4 C 1.3313(4) -0.0528(3) 0.4291(2) 0.0561(10) Uani 1 1 d . . . H4 H 1.4161 -0.0879 0.4417 0.067 Uiso 1 1 calc R . . C5 C 1.2880(4) 0.0186(3) 0.4625(2) 0.0542(10) Uani 1 1 d . . . H5 H 1.3435 0.0325 0.4975 0.065 Uiso 1 1 calc R . . C24 C 0.4909(4) 0.0332(4) 0.2056(3) 0.0726(13) Uani 1 1 d . . . H24A H 0.5544 0.0574 0.1651 0.109 Uiso 1 1 calc R . . H24B H 0.4265 0.0090 0.1815 0.109 Uiso 1 1 calc R . . H24C H 0.5319 -0.0237 0.2553 0.109 Uiso 1 1 calc R . . C11 C 0.8976(4) 0.4176(3) 0.5890(3) 0.0700(13) Uani 1 1 d . . . H11 H 0.8711 0.4637 0.6156 0.084 Uiso 1 1 calc R . . C36 C 0.1685(4) 0.5858(3) 0.0881(3) 0.0686(13) Uani 1 1 d . . . H36 H 0.1133 0.5776 0.0498 0.082 Uiso 1 1 calc R . . C35 C 0.1255(4) 0.6537(4) 0.1275(3) 0.0768(14) Uani 1 1 d . . . H35 H 0.0417 0.6909 0.1159 0.092 Uiso 1 1 calc R . . C34 C 0.2072(4) 0.6661(3) 0.1839(3) 0.0671(12) Uani 1 1 d . . . H34 H 0.1772 0.7098 0.2120 0.081 Uiso 1 1 calc R . . C47 C 0.6522(4) 0.0941(3) -0.0534(3) 0.0658(12) Uani 1 1 d . . . H47A H 0.6506 0.1334 -0.1140 0.079 Uiso 1 1 calc R . . H47B H 0.5982 0.0400 -0.0424 0.079 Uiso 1 1 calc R . . C48 C 0.7877(5) 0.0447(4) -0.0192(3) 0.0909(16) Uani 1 1 d . . . H48A H 0.8389 0.0991 -0.0272 0.136 Uiso 1 1 calc R . . H48B H 0.8239 0.0013 -0.0485 0.136 Uiso 1 1 calc R . . H48C H 0.7874 0.0021 0.0401 0.136 Uiso 1 1 calc R . . C28 C 0.9382(4) 0.4425(3) 0.2847(2) 0.0558(11) Uani 1 1 d . . . H28 H 0.9923 0.4606 0.3177 0.067 Uiso 1 1 calc R . . C21 C 1.0761(4) -0.1119(3) 0.2677(2) 0.0598(11) Uani 1 1 d . . . H21A H 1.1067 -0.1816 0.3103 0.072 Uiso 1 1 calc R . . H21B H 1.1458 -0.0894 0.2309 0.072 Uiso 1 1 calc R . . C22 C 0.9615(4) -0.1148(3) 0.2173(3) 0.0782(14) Uani 1 1 d . . . H22A H 0.8933 -0.1375 0.2543 0.117 Uiso 1 1 calc R . . H22B H 0.9857 -0.1632 0.1902 0.117 Uiso 1 1 calc R . . H22C H 0.9321 -0.0455 0.1752 0.117 Uiso 1 1 calc R . . Cl1 Cl 0.44329(11) 0.29400(9) 0.64820(7) 0.0669(3) Uani 1 1 d . . . O9 O 0.4272(4) 0.2385(3) 0.5975(2) 0.1196(14) Uani 1 1 d . . . O10 O 0.4438(5) 0.4005(3) 0.6003(3) 0.169(2) Uani 1 1 d . . . O11 O 0.5603(4) 0.2473(3) 0.6967(3) 0.1521(19) Uani 1 1 d . . . O12 O 0.3450(4) 0.2851(4) 0.7030(3) 0.1509(18) Uani 1 1 d . . . O1W O 0.7805(3) 0.0673(3) 0.2735(2) 0.0624(9) Uani 1 1 d D . . H1WA H 0.849(2) 0.052(4) 0.298(3) 0.094 Uiso 1 1 d D . . H1WB H 0.737(4) 0.097(3) 0.297(3) 0.094 Uiso 1 1 d D . . H1WC H 0.777(5) 0.101(4) 0.223(3) 0.094 Uiso 1 1 d . . . O2W O 0.7781(3) 0.1674(2) 0.1191(2) 0.0619(8) Uani 1 1 d D . . H2WA H 0.788(4) 0.2270(19) 0.110(3) 0.093 Uiso 1 1 d D . . H2WB H 0.710(3) 0.179(3) 0.093(3) 0.093 Uiso 1 1 d 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 Cu2 0.0340(2) 0.0419(3) 0.0414(2) -0.0202(2) -0.00301(18) -0.00566(19) Cu1 0.0379(3) 0.0424(3) 0.0430(3) -0.0221(2) -0.00281(19) -0.0026(2) N1 0.0420(19) 0.0445(18) 0.0451(17) -0.0207(15) -0.0016(14) -0.0062(15) N2 0.0413(18) 0.0387(16) 0.0405(16) -0.0195(14) -0.0031(13) -0.0041(14) N3 0.0346(16) 0.0378(17) 0.0412(16) -0.0161(14) -0.0022(13) 0.0003(13) N4 0.0373(17) 0.0426(17) 0.0432(16) -0.0174(14) -0.0039(13) -0.0052(14) O1 0.0390(15) 0.0515(15) 0.0541(15) -0.0301(13) -0.0026(12) 0.0028(12) O2 0.0339(14) 0.0459(14) 0.0510(14) -0.0287(12) -0.0033(11) 0.0006(11) O3 0.0509(16) 0.0543(16) 0.0619(16) -0.0349(14) -0.0016(13) 0.0075(13) O4 0.0418(15) 0.0672(18) 0.0655(17) -0.0414(15) -0.0035(12) -0.0093(13) O5 0.0357(14) 0.0524(15) 0.0549(15) -0.0330(13) -0.0062(11) -0.0029(11) O6 0.0371(14) 0.0569(16) 0.0521(15) -0.0312(13) -0.0071(11) -0.0029(12) O8 0.0653(19) 0.0652(18) 0.0603(17) -0.0435(15) -0.0099(14) 0.0004(15) O7 0.0361(15) 0.0698(18) 0.0737(18) -0.0471(15) -0.0094(12) 0.0042(13) C1 0.042(2) 0.037(2) 0.0387(19) -0.0095(16) 0.0037(16) -0.0014(17) C6 0.041(2) 0.044(2) 0.043(2) -0.0124(18) 0.0024(17) -0.0058(17) C7 0.043(2) 0.053(2) 0.046(2) -0.0179(19) -0.0009(17) -0.0107(19) C8 0.048(2) 0.046(2) 0.047(2) -0.0223(18) -0.0015(17) -0.0083(18) C14 0.043(2) 0.043(2) 0.050(2) -0.0258(18) -0.0043(17) 0.0021(17) C15 0.037(2) 0.045(2) 0.0407(19) -0.0186(17) -0.0009(16) -0.0046(17) C20 0.038(2) 0.039(2) 0.0384(19) -0.0126(16) -0.0025(16) -0.0052(17) C19 0.039(2) 0.045(2) 0.047(2) -0.0225(18) 0.0000(16) -0.0076(17) C18 0.041(2) 0.063(3) 0.066(3) -0.031(2) -0.0073(19) -0.010(2) C13 0.048(2) 0.040(2) 0.046(2) -0.0210(18) -0.0057(17) -0.0109(18) C12 0.055(3) 0.058(3) 0.074(3) -0.040(2) -0.011(2) -0.001(2) C9 0.046(2) 0.065(3) 0.072(3) -0.036(2) -0.009(2) -0.008(2) C26 0.039(2) 0.047(2) 0.050(2) -0.0259(18) -0.0046(16) -0.0043(17) C25 0.035(2) 0.036(2) 0.0409(19) -0.0156(16) -0.0046(15) -0.0053(16) C27 0.035(2) 0.063(3) 0.075(3) -0.039(2) -0.0111(19) -0.0030(19) C30 0.040(2) 0.036(2) 0.0357(18) -0.0137(16) -0.0048(15) -0.0062(16) C29 0.048(2) 0.049(2) 0.051(2) -0.0284(19) -0.0058(18) -0.0041(18) C31 0.046(2) 0.040(2) 0.047(2) -0.0216(18) -0.0020(17) -0.0060(17) C32 0.036(2) 0.042(2) 0.044(2) -0.0144(17) 0.0032(16) -0.0055(17) C37 0.038(2) 0.042(2) 0.047(2) -0.0147(18) 0.0031(17) -0.0066(17) C33 0.052(3) 0.055(2) 0.065(3) -0.034(2) -0.006(2) 0.004(2) C38 0.034(2) 0.048(2) 0.044(2) -0.0120(18) -0.0026(16) -0.0086(17) C39 0.039(2) 0.049(2) 0.042(2) -0.0150(18) 0.0013(16) -0.0172(18) C44 0.048(2) 0.046(2) 0.0316(18) -0.0139(17) -0.0001(16) -0.0186(18) C43 0.055(3) 0.051(2) 0.043(2) -0.0213(19) -0.0001(18) -0.014(2) C40 0.047(2) 0.065(3) 0.045(2) -0.020(2) -0.0037(18) -0.021(2) C41 0.062(3) 0.073(3) 0.056(2) -0.031(2) -0.013(2) -0.023(2) C17 0.036(2) 0.073(3) 0.076(3) -0.042(2) -0.009(2) 0.005(2) C16 0.049(2) 0.056(3) 0.063(2) -0.034(2) -0.0015(19) -0.001(2) C45 0.037(2) 0.057(3) 0.061(2) -0.027(2) 0.0029(18) -0.0034(19) C46 0.047(2) 0.068(3) 0.083(3) -0.042(3) 0.004(2) -0.004(2) C23 0.052(2) 0.065(3) 0.057(2) -0.030(2) -0.0012(19) -0.024(2) C10 0.064(3) 0.075(3) 0.086(3) -0.052(3) -0.015(2) -0.015(2) C42 0.072(3) 0.060(3) 0.051(2) -0.030(2) -0.004(2) -0.018(2) C2 0.048(2) 0.038(2) 0.046(2) -0.0115(18) 0.0026(18) -0.0032(18) C3 0.048(2) 0.044(2) 0.056(2) -0.0176(19) 0.0084(19) -0.0002(19) C4 0.041(2) 0.051(2) 0.064(3) -0.013(2) 0.002(2) 0.0038(19) C5 0.044(2) 0.057(3) 0.054(2) -0.017(2) -0.0073(18) 0.001(2) C24 0.067(3) 0.087(3) 0.091(3) -0.060(3) 0.007(2) -0.025(3) C11 0.071(3) 0.073(3) 0.090(3) -0.060(3) -0.010(2) -0.005(2) C36 0.043(3) 0.079(3) 0.097(3) -0.052(3) -0.010(2) 0.000(2) C35 0.040(3) 0.086(3) 0.116(4) -0.060(3) -0.007(2) 0.009(2) C34 0.054(3) 0.069(3) 0.088(3) -0.048(3) 0.002(2) 0.011(2) C47 0.087(3) 0.061(3) 0.062(3) -0.039(2) -0.002(2) -0.009(2) C48 0.093(4) 0.096(4) 0.100(4) -0.068(3) -0.010(3) 0.021(3) C28 0.048(2) 0.064(3) 0.069(3) -0.041(2) -0.015(2) -0.008(2) C21 0.072(3) 0.053(3) 0.056(2) -0.030(2) 0.002(2) 0.009(2) C22 0.085(3) 0.071(3) 0.089(3) -0.052(3) -0.019(3) 0.015(3) Cl1 0.0682(8) 0.0714(8) 0.0693(7) -0.0429(6) 0.0017(6) 0.0067(6) O9 0.164(4) 0.122(3) 0.092(3) -0.073(2) -0.012(2) 0.008(3) O10 0.248(6) 0.059(3) 0.175(4) -0.026(3) 0.029(4) 0.000(3) O11 0.104(3) 0.140(4) 0.241(5) -0.121(4) -0.064(3) 0.028(3) O12 0.145(4) 0.191(5) 0.125(3) -0.081(3) 0.066(3) -0.003(3) O1W 0.0467(18) 0.072(2) 0.081(2) -0.0483(19) -0.0095(17) 0.0045(16) O2W 0.0494(18) 0.0654(19) 0.084(2) -0.0469(18) -0.0128(15) -0.0005(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu2 O5 1.898(2) . ? Cu2 O6 1.902(2) . ? Cu2 N3 1.937(3) . ? Cu2 N4 1.946(3) . ? Cu1 O1 1.914(2) . ? Cu1 O2 1.920(2) . ? Cu1 N2 1.946(3) . ? Cu1 N1 1.949(3) . ? N1 C7 1.301(4) . ? N1 C8 1.422(4) . ? N2 C14 1.287(4) . ? N2 C13 1.430(4) . ? N3 C31 1.300(4) . ? N3 C32 1.430(4) . ? N4 C38 1.306(4) . ? N4 C37 1.417(4) . ? O1 C1 1.315(4) . ? O2 C20 1.324(4) . ? O3 C2 1.364(4) . ? O3 C21 1.426(4) . ? O4 C19 1.364(4) . ? O4 C23 1.431(4) . ? O5 C25 1.314(4) . ? O6 C44 1.307(4) . ? O8 C43 1.376(4) . ? O8 C47 1.427(4) . ? O7 C26 1.373(4) . ? O7 C45 1.418(4) . ? C1 C6 1.410(5) . ? C1 C2 1.427(5) . ? C6 C7 1.418(5) . ? C6 C5 1.431(5) . ? C7 H7 0.9300 . ? C8 C9 1.394(5) . ? C8 C13 1.400(5) . ? C14 C15 1.433(4) . ? C14 H14 0.9300 . ? C15 C20 1.411(4) . ? C15 C16 1.418(5) . ? C20 C19 1.413(4) . ? C19 C18 1.374(5) . ? C18 C17 1.396(5) . ? C18 H18 0.9300 . ? C13 C12 1.382(5) . ? C12 C11 1.372(5) . ? C12 H12 0.9300 . ? C9 C10 1.363(5) . ? C9 H9 0.9300 . ? C26 C27 1.359(5) . ? C26 C25 1.426(4) . ? C25 C30 1.413(4) . ? C27 C28 1.395(5) . ? C27 H27 0.9300 . ? C30 C29 1.418(4) . ? C30 C31 1.424(5) . ? C29 C28 1.352(5) . ? C29 H29 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.378(5) . ? C32 C37 1.399(5) . ? C37 C36 1.383(5) . ? C33 C34 1.369(5) . ? C33 H33 0.9300 . ? C38 C39 1.416(5) . ? C38 H38 0.9300 . ? C39 C44 1.418(5) . ? C39 C40 1.422(4) . ? C44 C43 1.422(5) . ? C43 C42 1.374(5) . ? C40 C41 1.351(5) . ? C40 H40 0.9300 . ? C41 C42 1.397(5) . ? C41 H41 0.9300 . ? C17 C16 1.360(5) . ? C17 H17 0.9300 . ? C16 H16 0.9300 . ? C45 C46 1.504(5) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C23 C24 1.496(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C10 C11 1.389(6) . ? C10 H10 0.9300 . ? C42 H42 0.9300 . ? C2 C3 1.379(5) . ? C3 C4 1.400(5) . ? C3 H3 0.9300 . ? C4 C5 1.347(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C11 H11 0.9300 . ? C36 C35 1.382(5) . ? C36 H36 0.9300 . ? C35 C34 1.373(6) . ? C35 H35 0.9300 . ? C34 H34 0.9300 . ? C47 C48 1.497(6) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C28 H28 0.9300 . ? C21 C22 1.501(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? Cl1 O12 1.377(4) . ? Cl1 O10 1.391(4) . ? Cl1 O9 1.393(3) . ? Cl1 O11 1.406(4) . ? O1W H1WA 0.797(19) . ? O1W H1WB 0.788(19) . ? O1W H1WC 0.82(5) . ? O2W H2WA 0.805(18) . ? O2W H2WB 0.810(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Cu2 O6 88.65(9) . . ? O5 Cu2 N3 94.04(10) . . ? O6 Cu2 N3 175.39(11) . . ? O5 Cu2 N4 173.19(11) . . ? O6 Cu2 N4 93.60(10) . . ? N3 Cu2 N4 84.16(11) . . ? O1 Cu1 O2 88.90(9) . . ? O1 Cu1 N2 177.50(10) . . ? O2 Cu1 N2 93.60(10) . . ? O1 Cu1 N1 93.32(11) . . ? O2 Cu1 N1 177.78(10) . . ? N2 Cu1 N1 84.19(11) . . ? C7 N1 C8 121.7(3) . . ? C7 N1 Cu1 125.5(2) . . ? C8 N1 Cu1 112.8(2) . . ? C14 N2 C13 121.5(3) . . ? C14 N2 Cu1 125.7(2) . . ? C13 N2 Cu1 112.7(2) . . ? C31 N3 C32 121.5(3) . . ? C31 N3 Cu2 125.5(2) . . ? C32 N3 Cu2 112.9(2) . . ? C38 N4 C37 122.1(3) . . ? C38 N4 Cu2 125.0(2) . . ? C37 N4 Cu2 112.9(2) . . ? C1 O1 Cu1 126.8(2) . . ? C20 O2 Cu1 127.1(2) . . ? C2 O3 C21 119.1(3) . . ? C19 O4 C23 118.2(3) . . ? C25 O5 Cu2 126.7(2) . . ? C44 O6 Cu2 127.6(2) . . ? C43 O8 C47 118.4(3) . . ? C26 O7 C45 117.8(3) . . ? O1 C1 C6 124.9(3) . . ? O1 C1 C2 117.2(3) . . ? C6 C1 C2 117.9(3) . . ? C1 C6 C7 123.4(3) . . ? C1 C6 C5 119.3(3) . . ? C7 C6 C5 117.3(3) . . ? N1 C7 C6 125.8(3) . . ? N1 C7 H7 117.1 . . ? C6 C7 H7 117.1 . . ? C9 C8 C13 119.1(3) . . ? C9 C8 N1 125.7(3) . . ? C13 C8 N1 115.3(3) . . ? N2 C14 C15 125.7(3) . . ? N2 C14 H14 117.1 . . ? C15 C14 H14 117.1 . . ? C20 C15 C16 119.8(3) . . ? C20 C15 C14 124.1(3) . . ? C16 C15 C14 116.2(3) . . ? O2 C20 C15 123.7(3) . . ? O2 C20 C19 118.6(3) . . ? C15 C20 C19 117.7(3) . . ? O4 C19 C18 125.0(3) . . ? O4 C19 C20 114.1(3) . . ? C18 C19 C20 120.9(3) . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C12 C13 C8 120.2(3) . . ? C12 C13 N2 124.9(3) . . ? C8 C13 N2 114.9(3) . . ? C11 C12 C13 119.8(4) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C10 C9 C8 120.3(4) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C27 C26 O7 125.5(3) . . ? C27 C26 C25 121.2(3) . . ? O7 C26 C25 113.3(3) . . ? O5 C25 C30 124.9(3) . . ? O5 C25 C26 117.8(3) . . ? C30 C25 C26 117.4(3) . . ? C26 C27 C28 120.9(3) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C25 C30 C29 119.6(3) . . ? C25 C30 C31 123.3(3) . . ? C29 C30 C31 117.0(3) . . ? C28 C29 C30 121.0(3) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? N3 C31 C30 125.3(3) . . ? N3 C31 H31 117.3 . . ? C30 C31 H31 117.3 . . ? C33 C32 C37 120.2(3) . . ? C33 C32 N3 125.1(3) . . ? C37 C32 N3 114.7(3) . . ? C36 C37 C32 118.7(3) . . ? C36 C37 N4 126.1(3) . . ? C32 C37 N4 115.2(3) . . ? C34 C33 C32 120.0(4) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? N4 C38 C39 126.0(3) . . ? N4 C38 H38 117.0 . . ? C39 C38 H38 117.0 . . ? C38 C39 C44 123.3(3) . . ? C38 C39 C40 117.3(3) . . ? C44 C39 C40 119.4(3) . . ? O6 C44 C39 124.3(3) . . ? O6 C44 C43 118.2(3) . . ? C39 C44 C43 117.5(3) . . ? C42 C43 O8 124.8(3) . . ? C42 C43 C44 121.5(4) . . ? O8 C43 C44 113.7(3) . . ? C41 C40 C39 121.0(4) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C40 C41 C42 120.7(3) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C16 C17 C18 119.2(3) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C17 C16 C15 121.2(3) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? O7 C45 C46 107.8(3) . . ? O7 C45 H45A 110.2 . . ? C46 C45 H45A 110.2 . . ? O7 C45 H45B 110.2 . . ? C46 C45 H45B 110.2 . . ? H45A C45 H45B 108.5 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O4 C23 C24 108.2(3) . . ? O4 C23 H23A 110.1 . . ? C24 C23 H23A 110.1 . . ? O4 C23 H23B 110.1 . . ? C24 C23 H23B 110.1 . . ? H23A C23 H23B 108.4 . . ? C9 C10 C11 120.3(4) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C43 C42 C41 119.9(4) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? O3 C2 C3 125.0(3) . . ? O3 C2 C1 113.9(3) . . ? C3 C2 C1 121.1(3) . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.9(4) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 120.9(4) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C12 C11 C10 120.4(4) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C35 C36 C37 120.6(4) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C34 C35 C36 119.7(4) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C33 C34 C35 120.7(4) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? O8 C47 C48 107.5(3) . . ? O8 C47 H47A 110.2 . . ? C48 C47 H47A 110.2 . . ? O8 C47 H47B 110.2 . . ? C48 C47 H47B 110.2 . . ? H47A C47 H47B 108.5 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C29 C28 C27 120.0(3) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? O3 C21 C22 107.9(3) . . ? O3 C21 H21A 110.1 . . ? C22 C21 H21A 110.1 . . ? O3 C21 H21B 110.1 . . ? C22 C21 H21B 110.1 . . ? H21A C21 H21B 108.4 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O12 Cl1 O10 108.7(3) . . ? O12 Cl1 O9 110.0(3) . . ? O10 Cl1 O9 111.8(3) . . ? O12 Cl1 O11 107.9(3) . . ? O10 Cl1 O11 110.6(3) . . ? O9 Cl1 O11 107.7(2) . . ? H1WA O1W H1WB 104(4) . . ? H1WA O1W H1WC 118(5) . . ? H1WB O1W H1WC 112(5) . . ? H2WA O2W H2WB 100(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WC O2W 0.82(5) 1.66(5) 2.473(5) 177(5) . O1W H1WA O1 0.797(19) 1.99(3) 2.655(4) 140(4) . O1W H1WA O3 0.797(19) 2.14(3) 2.810(4) 142(4) . O1W H1WB O2 0.788(19) 1.86(3) 2.592(3) 154(5) . O1W H1WB O4 0.788(19) 2.23(4) 2.750(4) 124(4) . O2W H2WA O5 0.805(18) 2.09(3) 2.762(3) 141(5) . O2W H2WA O7 0.805(18) 2.27(3) 2.858(4) 130(4) . O2W H2WB O6 0.810(18) 2.19(3) 2.839(3) 137(4) . O2W H2WB O8 0.810(18) 2.21(3) 2.923(4) 147(4) . _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.353 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.064 data_2 _database_code_depnum_ccdc_archive 'CCDC 915726' #TrackingRef '1-3 new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H61 Cl Cu2 N4 O14' _chemical_formula_weight 1080.54 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 Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.973(2) _cell_length_b 14.052(3) _cell_length_c 17.507(4) _cell_angle_alpha 111.320(2) _cell_angle_beta 95.487(2) _cell_angle_gamma 103.616(3) _cell_volume 2394.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3352 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 21.32 _exptl_crystal_description Cubic _exptl_crystal_colour Brown _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.016 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8709 _exptl_absorpt_correction_T_max 0.9232 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16285 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8164 _reflns_number_gt 4880 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.9592P] 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 8164 _refine_ls_number_parameters 646 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1031 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1476 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4021(5) 0.5553(4) 0.6008(3) 0.0528(13) Uani 1 1 d . . . C2 C 0.3392(5) 0.4901(4) 0.6398(3) 0.0571(14) Uani 1 1 d . . . C3 C 0.2100(5) 0.4387(4) 0.6148(4) 0.0679(16) Uani 1 1 d . . . H3 H 0.1709 0.3952 0.6401 0.081 Uiso 1 1 calc R . . C4 C 0.1378(6) 0.4517(5) 0.5515(4) 0.0754(18) Uani 1 1 d . . . H4 H 0.0505 0.4170 0.5350 0.090 Uiso 1 1 calc R . . C5 C 0.1930(5) 0.5140(5) 0.5137(4) 0.0704(16) Uani 1 1 d . . . H5 H 0.1431 0.5224 0.4719 0.085 Uiso 1 1 calc R . . C6 C 0.3259(5) 0.5669(4) 0.5367(3) 0.0576(14) Uani 1 1 d . . . C7 C 0.3767(6) 0.6315(4) 0.4938(3) 0.0627(15) Uani 1 1 d . . . H7 H 0.3190 0.6345 0.4528 0.075 Uiso 1 1 calc R . . C8 C 0.5360(5) 0.7445(5) 0.4534(3) 0.0655(15) Uani 1 1 d . . . H8 H 0.5655 0.6964 0.4078 0.079 Uiso 1 1 calc R . . C9 C 0.4343(6) 0.7787(5) 0.4130(4) 0.0777(18) Uani 1 1 d . . . H9A H 0.3672 0.7160 0.3745 0.093 Uiso 1 1 calc R . . H9B H 0.3963 0.8209 0.4558 0.093 Uiso 1 1 calc R . . C10 C 0.4935(6) 0.8441(6) 0.3659(4) 0.092(2) Uani 1 1 d . . . H10A H 0.5149 0.7972 0.3163 0.111 Uiso 1 1 calc R . . H10B H 0.4304 0.8736 0.3477 0.111 Uiso 1 1 calc R . . C11 C 0.6100(7) 0.9326(5) 0.4161(4) 0.088(2) Uani 1 1 d . . . H11A H 0.5858 0.9864 0.4598 0.106 Uiso 1 1 calc R . . H11B H 0.6474 0.9653 0.3803 0.106 Uiso 1 1 calc R . . C12 C 0.7102(6) 0.8970(5) 0.4559(3) 0.0684(16) Uani 1 1 d . . . H12A H 0.7451 0.8518 0.4129 0.082 Uiso 1 1 calc R . . H12B H 0.7796 0.9588 0.4931 0.082 Uiso 1 1 calc R . . C13 C 0.6497(5) 0.8367(4) 0.5042(3) 0.0626(15) Uani 1 1 d . . . H13 H 0.6180 0.8866 0.5472 0.075 Uiso 1 1 calc R . . C14 C 0.8542(5) 0.8275(4) 0.5594(3) 0.0571(14) Uani 1 1 d . . . H14 H 0.8890 0.8757 0.5368 0.068 Uiso 1 1 calc R . . C15 C 0.9417(5) 0.7940(4) 0.6034(3) 0.0497(12) Uani 1 1 d . . . C16 C 1.0711(5) 0.8238(4) 0.5980(3) 0.0630(15) Uani 1 1 d . . . H16 H 1.0972 0.8670 0.5695 0.076 Uiso 1 1 calc R . . C17 C 1.1578(5) 0.7909(5) 0.6334(3) 0.0666(15) Uani 1 1 d . . . H17 H 1.2428 0.8108 0.6288 0.080 Uiso 1 1 calc R . . C18 C 1.1212(5) 0.7280(4) 0.6764(3) 0.0633(15) Uani 1 1 d . . . H18 H 1.1815 0.7046 0.7000 0.076 Uiso 1 1 calc R . . C19 C 0.9956(5) 0.6990(4) 0.6850(3) 0.0506(13) Uani 1 1 d . . . C20 C 0.9014(5) 0.7294(4) 0.6467(3) 0.0491(12) Uani 1 1 d . . . C21 C 0.3630(6) 0.4205(4) 0.7445(4) 0.0721(17) Uani 1 1 d . . . H21A H 0.3197 0.3478 0.7051 0.086 Uiso 1 1 calc R . . H21B H 0.3010 0.4502 0.7735 0.086 Uiso 1 1 calc R . . C22 C 0.4683(6) 0.4221(5) 0.8051(4) 0.087(2) Uani 1 1 d . . . H22A H 0.5245 0.3863 0.7754 0.131 Uiso 1 1 calc R . . H22B H 0.4332 0.3863 0.8389 0.131 Uiso 1 1 calc R . . H22C H 0.5153 0.4947 0.8403 0.131 Uiso 1 1 calc R . . C23 C 1.0349(6) 0.6013(5) 0.7668(4) 0.0763(18) Uani 1 1 d . . . H23A H 1.0962 0.6624 0.8115 0.092 Uiso 1 1 calc R . . H23B H 1.0816 0.5640 0.7276 0.092 Uiso 1 1 calc R . . C24 C 0.9623(6) 0.5290(5) 0.8016(4) 0.089(2) Uani 1 1 d . . . H24A H 0.9201 0.5675 0.8426 0.133 Uiso 1 1 calc R . . H24B H 1.0201 0.5026 0.8273 0.133 Uiso 1 1 calc R . . H24C H 0.8997 0.4702 0.7573 0.133 Uiso 1 1 calc R . . C25 C 0.7084(4) 0.8818(4) 0.8171(3) 0.0440(12) Uani 1 1 d . . . C26 C 0.5734(5) 0.8471(4) 0.8097(3) 0.0490(12) Uani 1 1 d . . . C27 C 0.4932(5) 0.8714(4) 0.7594(3) 0.0593(14) Uani 1 1 d . . . H27 H 0.4051 0.8460 0.7536 0.071 Uiso 1 1 calc R . . C28 C 0.5420(5) 0.9334(4) 0.7169(3) 0.0633(15) Uani 1 1 d . . . H28 H 0.4869 0.9500 0.6833 0.076 Uiso 1 1 calc R . . C29 C 0.6708(5) 0.9698(4) 0.7247(3) 0.0561(14) Uani 1 1 d . . . H29 H 0.7029 1.0124 0.6969 0.067 Uiso 1 1 calc R . . C30 C 0.7569(5) 0.9445(4) 0.7742(3) 0.0457(12) Uani 1 1 d . . . C31 C 0.8898(5) 0.9888(4) 0.7816(3) 0.0494(12) Uani 1 1 d . . . H31 H 0.9143 1.0330 0.7536 0.059 Uiso 1 1 calc R . . C32 C 1.1154(5) 1.0162(5) 0.8239(4) 0.0731(17) Uani 1 1 d . . . H32 H 1.1400 0.9563 0.7856 0.088 Uiso 1 1 calc R . . C33 C 1.1484(5) 1.1033(4) 0.7918(3) 0.0659(15) Uani 1 1 d . . . H33A H 1.1180 1.1624 0.8236 0.079 Uiso 1 1 calc R . . H33B H 1.1065 1.0762 0.7336 0.079 Uiso 1 1 calc R . . C34 C 1.2915(6) 1.1417(6) 0.7997(5) 0.104(2) Uani 1 1 d . . . H34A H 1.3172 1.0865 0.7582 0.125 Uiso 1 1 calc R . . H34B H 1.3112 1.2042 0.7865 0.125 Uiso 1 1 calc R . . C35 C 1.3662(6) 1.1680(6) 0.8795(5) 0.105(2) Uani 1 1 d . . . H35A H 1.3547 1.2330 0.9191 0.126 Uiso 1 1 calc R . . H35B H 1.4558 1.1826 0.8757 0.126 Uiso 1 1 calc R . . C36 C 1.3337(5) 1.0815(5) 0.9137(4) 0.0706(16) Uani 1 1 d . . . H36A H 1.3637 1.0218 0.8824 0.085 Uiso 1 1 calc R . . H36B H 1.3761 1.1096 0.9719 0.085 Uiso 1 1 calc R . . C37 C 1.1900(5) 1.0440(5) 0.9061(4) 0.0750(17) Uani 1 1 d . . . H37 H 1.1673 1.1050 0.9444 0.090 Uiso 1 1 calc R . . C38 C 1.2113(5) 0.9332(4) 0.9822(3) 0.0543(13) Uani 1 1 d . . . H38 H 1.2971 0.9730 0.9991 0.065 Uiso 1 1 calc R . . C39 C 1.1715(5) 0.8548(4) 1.0154(3) 0.0466(12) Uani 1 1 d . . . C40 C 1.2626(5) 0.8449(4) 1.0721(3) 0.0594(14) Uani 1 1 d . . . H40 H 1.3471 0.8869 1.0847 0.071 Uiso 1 1 calc R . . C41 C 1.2293(6) 0.7752(5) 1.1086(3) 0.0695(16) Uani 1 1 d . . . H41 H 1.2907 0.7702 1.1463 0.083 Uiso 1 1 calc R . . C42 C 1.1050(6) 0.7116(4) 1.0902(3) 0.0661(15) Uani 1 1 d . . . H42 H 1.0827 0.6644 1.1159 0.079 Uiso 1 1 calc R . . C43 C 1.0133(5) 0.7176(4) 1.0340(3) 0.0526(13) Uani 1 1 d . . . C44 C 1.0436(5) 0.7912(4) 0.9959(3) 0.0476(12) Uani 1 1 d . . . C45 C 0.4003(5) 0.7423(4) 0.8439(3) 0.0596(14) Uani 1 1 d . . . H45A H 0.3665 0.6916 0.7865 0.072 Uiso 1 1 calc R . . H45B H 0.3559 0.7966 0.8562 0.072 Uiso 1 1 calc R . . C46 C 0.3819(5) 0.6866(4) 0.9024(4) 0.0696(16) Uani 1 1 d . . . H46A H 0.4284 0.6347 0.8908 0.104 Uiso 1 1 calc R . . H46B H 0.2925 0.6516 0.8946 0.104 Uiso 1 1 calc R . . H46C H 0.4130 0.7379 0.9591 0.104 Uiso 1 1 calc R . . C47 C 0.8472(6) 0.5786(5) 1.0431(4) 0.0763(18) Uani 1 1 d . . . H47A H 0.8523 0.6118 1.1030 0.092 Uiso 1 1 calc R . . H47B H 0.9016 0.5318 1.0327 0.092 Uiso 1 1 calc R . . C48 C 0.7121(6) 0.5165(6) 0.9995(5) 0.103(2) Uani 1 1 d . . . H48A H 0.6598 0.5641 1.0087 0.154 Uiso 1 1 calc R . . H48B H 0.6809 0.4638 1.0213 0.154 Uiso 1 1 calc R . . H48C H 0.7088 0.4819 0.9406 0.154 Uiso 1 1 calc R . . Cl1 Cl 0.05518(17) 0.79021(15) 0.34765(11) 0.0812(5) Uani 1 1 d . . . Cu1 Cu 0.63338(6) 0.69330(5) 0.58576(4) 0.0508(2) Uani 1 1 d . . . Cu2 Cu 0.95925(5) 0.89025(4) 0.89086(3) 0.04385(19) Uani 1 1 d . . . H1WA H 0.622(3) 0.576(4) 0.706(3) 0.08(2) Uiso 1 1 d D . . H2WA H 0.700(5) 0.7217(18) 0.884(3) 0.08(2) Uiso 1 1 d D . . H1WB H 0.733(5) 0.612(5) 0.714(5) 0.14(4) Uiso 1 1 d D . . H2WB H 0.766(2) 0.682(3) 0.912(2) 0.049(16) Uiso 1 1 d D . . H1WC H 0.686(6) 0.615(5) 0.793(5) 0.13(3) Uiso 1 1 d . . . N1 N 0.4928(4) 0.6856(3) 0.5058(2) 0.0560(11) Uani 1 1 d . . . N2 N 0.7321(4) 0.7959(3) 0.5490(2) 0.0538(11) Uani 1 1 d . . . N3 N 0.9796(4) 0.9726(3) 0.8243(2) 0.0474(10) Uani 1 1 d . . . N4 N 1.1417(4) 0.9547(3) 0.9318(3) 0.0533(11) Uani 1 1 d . . . O1 O 0.5266(3) 0.6004(3) 0.6265(2) 0.0553(9) Uani 1 1 d . . . O2 O 0.7813(3) 0.6936(3) 0.65301(19) 0.0506(8) Uani 1 1 d . . . O3 O 0.4186(3) 0.4830(3) 0.7015(2) 0.0626(10) Uani 1 1 d . . . O4 O 0.9486(3) 0.6362(3) 0.7256(2) 0.0643(10) Uani 1 1 d . . . O5 O 0.7784(3) 0.8530(2) 0.86598(19) 0.0465(8) Uani 1 1 d . . . O6 O 0.9497(3) 0.7952(2) 0.94499(19) 0.0504(8) Uani 1 1 d . . . O7 O 0.5336(3) 0.7898(3) 0.8555(2) 0.0591(9) Uani 1 1 d . . . O8 O 0.8871(3) 0.6578(3) 1.0111(2) 0.0645(10) Uani 1 1 d . . . O9 O -0.0477(6) 0.7245(5) 0.2819(4) 0.175(3) Uani 1 1 d . . . O10 O 0.1449(7) 0.8266(9) 0.3160(6) 0.261(5) Uani 1 1 d . . . O11 O 0.0907(6) 0.7338(5) 0.3918(4) 0.152(2) Uani 1 1 d . . . O12 O 0.0150(10) 0.8700(8) 0.3977(5) 0.268(5) Uani 1 1 d . . . O1W O 0.6861(4) 0.5705(4) 0.7265(3) 0.0661(10) Uani 1 1 d D . . O2W O 0.6991(4) 0.6633(3) 0.8802(3) 0.0629(10) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.053(3) 0.047(3) 0.059(3) 0.018(3) 0.015(3) 0.018(3) C2 0.055(3) 0.045(3) 0.064(4) 0.010(3) 0.016(3) 0.017(3) C3 0.060(4) 0.048(3) 0.084(4) 0.016(3) 0.021(3) 0.010(3) C4 0.047(4) 0.067(4) 0.087(5) 0.007(4) 0.010(3) 0.010(3) C5 0.057(4) 0.069(4) 0.071(4) 0.012(3) 0.002(3) 0.020(3) C6 0.052(3) 0.058(3) 0.056(3) 0.012(3) 0.007(3) 0.022(3) C7 0.063(4) 0.073(4) 0.051(3) 0.023(3) 0.001(3) 0.023(3) C8 0.071(4) 0.081(4) 0.061(4) 0.039(3) 0.011(3) 0.034(3) C9 0.076(4) 0.092(4) 0.081(4) 0.048(4) 0.003(3) 0.038(4) C10 0.092(5) 0.115(6) 0.098(5) 0.071(5) 0.002(4) 0.040(4) C11 0.108(5) 0.098(5) 0.092(5) 0.064(4) 0.028(4) 0.046(4) C12 0.089(4) 0.073(4) 0.064(4) 0.043(3) 0.015(3) 0.036(3) C13 0.075(4) 0.070(4) 0.060(4) 0.038(3) 0.014(3) 0.034(3) C14 0.071(4) 0.057(3) 0.053(3) 0.032(3) 0.016(3) 0.021(3) C15 0.050(3) 0.053(3) 0.045(3) 0.020(3) 0.006(2) 0.014(2) C16 0.055(4) 0.075(4) 0.053(3) 0.027(3) 0.006(3) 0.007(3) C17 0.046(3) 0.088(4) 0.062(4) 0.035(3) 0.006(3) 0.008(3) C18 0.052(3) 0.078(4) 0.058(3) 0.027(3) 0.002(3) 0.020(3) C19 0.052(3) 0.059(3) 0.046(3) 0.027(3) 0.004(2) 0.019(3) C20 0.048(3) 0.054(3) 0.044(3) 0.018(3) 0.007(2) 0.015(2) C21 0.082(4) 0.058(3) 0.071(4) 0.024(3) 0.029(3) 0.006(3) C22 0.106(5) 0.069(4) 0.081(5) 0.040(4) 0.012(4) 0.002(4) C23 0.079(4) 0.110(5) 0.078(4) 0.058(4) 0.020(3) 0.060(4) C24 0.103(5) 0.106(5) 0.101(5) 0.069(4) 0.033(4) 0.063(4) C25 0.043(3) 0.048(3) 0.041(3) 0.014(2) 0.006(2) 0.020(2) C26 0.055(3) 0.050(3) 0.052(3) 0.029(3) 0.009(3) 0.021(2) C27 0.050(3) 0.067(3) 0.068(4) 0.037(3) 0.000(3) 0.019(3) C28 0.060(4) 0.073(4) 0.072(4) 0.045(3) 0.000(3) 0.026(3) C29 0.078(4) 0.053(3) 0.046(3) 0.031(3) 0.006(3) 0.020(3) C30 0.056(3) 0.043(3) 0.044(3) 0.023(2) 0.006(2) 0.016(2) C31 0.056(3) 0.053(3) 0.048(3) 0.028(3) 0.016(3) 0.014(3) C32 0.061(4) 0.091(4) 0.082(4) 0.057(4) 0.016(3) 0.013(3) C33 0.070(4) 0.067(4) 0.073(4) 0.045(3) 0.024(3) 0.012(3) C34 0.085(5) 0.131(6) 0.127(6) 0.099(5) 0.031(5) 0.009(4) C35 0.067(4) 0.119(6) 0.135(7) 0.087(5) 0.006(4) -0.013(4) C36 0.048(3) 0.086(4) 0.088(4) 0.049(4) 0.017(3) 0.013(3) C37 0.060(4) 0.079(4) 0.089(5) 0.049(4) 0.008(3) 0.004(3) C38 0.044(3) 0.057(3) 0.058(3) 0.023(3) 0.003(3) 0.012(2) C39 0.047(3) 0.055(3) 0.047(3) 0.022(3) 0.012(2) 0.026(2) C40 0.052(3) 0.069(4) 0.058(3) 0.022(3) 0.002(3) 0.028(3) C41 0.074(4) 0.078(4) 0.057(4) 0.027(3) -0.005(3) 0.032(3) C42 0.084(4) 0.072(4) 0.058(4) 0.037(3) 0.003(3) 0.035(3) C43 0.059(3) 0.059(3) 0.050(3) 0.031(3) 0.012(3) 0.022(3) C44 0.061(3) 0.055(3) 0.039(3) 0.023(2) 0.014(3) 0.030(3) C45 0.050(3) 0.066(3) 0.073(4) 0.037(3) 0.014(3) 0.021(3) C46 0.059(4) 0.079(4) 0.083(4) 0.041(3) 0.023(3) 0.024(3) C47 0.098(5) 0.080(4) 0.083(4) 0.063(4) 0.022(4) 0.031(4) C48 0.093(5) 0.111(5) 0.135(6) 0.093(5) 0.023(5) 0.015(4) Cl1 0.0826(12) 0.0908(12) 0.0759(11) 0.0486(10) 0.0164(9) 0.0106(9) Cu1 0.0526(4) 0.0570(4) 0.0511(4) 0.0279(3) 0.0089(3) 0.0212(3) Cu2 0.0458(4) 0.0490(4) 0.0460(4) 0.0268(3) 0.0107(3) 0.0170(3) N1 0.058(3) 0.062(3) 0.053(3) 0.028(2) 0.007(2) 0.021(2) N2 0.061(3) 0.059(3) 0.051(3) 0.030(2) 0.009(2) 0.023(2) N3 0.046(2) 0.053(2) 0.054(3) 0.030(2) 0.017(2) 0.0162(19) N4 0.049(3) 0.062(3) 0.060(3) 0.038(2) 0.011(2) 0.015(2) O1 0.044(2) 0.063(2) 0.065(2) 0.0345(19) 0.0067(17) 0.0122(17) O2 0.049(2) 0.063(2) 0.054(2) 0.0349(18) 0.0121(17) 0.0226(17) O3 0.056(2) 0.061(2) 0.074(3) 0.038(2) 0.013(2) 0.0059(18) O4 0.058(2) 0.084(3) 0.072(2) 0.050(2) 0.0102(19) 0.029(2) O5 0.0400(18) 0.0538(19) 0.059(2) 0.0368(17) 0.0066(16) 0.0147(15) O6 0.047(2) 0.060(2) 0.055(2) 0.0355(18) 0.0072(17) 0.0179(16) O7 0.038(2) 0.078(2) 0.080(3) 0.054(2) 0.0099(18) 0.0148(17) O8 0.070(3) 0.076(2) 0.073(2) 0.057(2) 0.013(2) 0.023(2) O9 0.176(6) 0.140(5) 0.161(6) 0.070(4) -0.067(5) -0.019(4) O10 0.146(6) 0.434(14) 0.310(10) 0.302(11) 0.084(7) 0.015(7) O11 0.172(6) 0.192(6) 0.132(5) 0.118(5) 0.023(4) 0.046(5) O12 0.334(12) 0.272(10) 0.166(7) -0.013(7) 0.004(7) 0.209(10) O1W 0.056(3) 0.079(3) 0.080(3) 0.050(3) 0.012(2) 0.021(2) O2W 0.058(3) 0.060(3) 0.077(3) 0.041(2) 0.000(2) 0.015(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.318(6) . ? C1 C6 1.413(7) . ? C1 C2 1.425(7) . ? C2 O3 1.369(6) . ? C2 C3 1.375(7) . ? C3 C4 1.391(8) . ? C3 H3 0.9300 . ? C4 C5 1.350(8) . ? C4 H4 0.9300 . ? C5 C6 1.414(7) . ? C5 H5 0.9300 . ? C6 C7 1.429(7) . ? C7 N1 1.273(6) . ? C7 H7 0.9300 . ? C8 N1 1.483(6) . ? C8 C13 1.488(7) . ? C8 C9 1.526(7) . ? C8 H8 0.9800 . ? C9 C10 1.523(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.481(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.520(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.495(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N2 1.483(6) . ? C13 H13 0.9800 . ? C14 N2 1.280(6) . ? C14 C15 1.440(7) . ? C14 H14 0.9300 . ? C15 C20 1.403(6) . ? C15 C16 1.405(7) . ? C16 C17 1.344(7) . ? C16 H16 0.9300 . ? C17 C18 1.373(7) . ? C17 H17 0.9300 . ? C18 C19 1.381(7) . ? C18 H18 0.9300 . ? C19 O4 1.364(6) . ? C19 C20 1.409(6) . ? C20 O2 1.326(5) . ? C21 O3 1.423(6) . ? C21 C22 1.483(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 O4 1.415(6) . ? C23 C24 1.483(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 O5 1.326(5) . ? C25 C30 1.401(6) . ? C25 C26 1.424(6) . ? C26 O7 1.361(5) . ? C26 C27 1.370(6) . ? C27 C28 1.388(7) . ? C27 H27 0.9300 . ? C28 C29 1.359(7) . ? C28 H28 0.9300 . ? C29 C30 1.411(6) . ? C29 H29 0.9300 . ? C30 C31 1.418(6) . ? C31 N3 1.292(6) . ? C31 H31 0.9300 . ? C32 C37 1.453(7) . ? C32 N3 1.474(6) . ? C32 C33 1.508(7) . ? C32 H32 0.9800 . ? C33 C34 1.510(8) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.422(8) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.526(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.517(7) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 N4 1.484(6) . ? C37 H37 0.9800 . ? C38 N4 1.276(6) . ? C38 C39 1.424(7) . ? C38 H38 0.9300 . ? C39 C44 1.407(7) . ? C39 C40 1.408(6) . ? C40 C41 1.354(7) . ? C40 H40 0.9300 . ? C41 C42 1.377(7) . ? C41 H41 0.9300 . ? C42 C43 1.379(7) . ? C42 H42 0.9300 . ? C43 O8 1.373(6) . ? C43 C44 1.417(6) . ? C44 O6 1.322(5) . ? C45 O7 1.418(5) . ? C45 C46 1.499(7) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 O8 1.420(6) . ? C47 C48 1.494(8) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? Cl1 O10 1.269(6) . ? Cl1 O12 1.347(7) . ? Cl1 O11 1.383(5) . ? Cl1 O9 1.393(5) . ? Cu1 O2 1.910(3) . ? Cu1 O1 1.924(3) . ? Cu1 N2 1.934(4) . ? Cu1 N1 1.936(4) . ? Cu2 O6 1.889(3) . ? Cu2 O5 1.893(3) . ? Cu2 N3 1.913(4) . ? Cu2 N4 1.935(4) . ? O1W H1WA 0.796(10) . ? O1W H1WB 0.799(10) . ? O1W H1WC 1.11(8) . ? O2W H2WA 0.797(10) . ? O2W H2WB 0.798(10) . ? O2W H1WC 1.40(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C6 124.6(5) . . ? O1 C1 C2 118.1(5) . . ? C6 C1 C2 117.3(5) . . ? O3 C2 C3 124.7(5) . . ? O3 C2 C1 114.2(5) . . ? C3 C2 C1 121.2(6) . . ? C2 C3 C4 120.0(6) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.8(6) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 120.8(6) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 119.8(5) . . ? C1 C6 C7 122.9(5) . . ? C5 C6 C7 117.3(5) . . ? N1 C7 C6 126.8(5) . . ? N1 C7 H7 116.6 . . ? C6 C7 H7 116.6 . . ? N1 C8 C13 108.4(4) . . ? N1 C8 C9 115.9(5) . . ? C13 C8 C9 111.7(5) . . ? N1 C8 H8 106.8 . . ? C13 C8 H8 106.8 . . ? C9 C8 H8 106.8 . . ? C10 C9 C8 110.3(5) . . ? C10 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? C10 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 113.7(5) . . ? C11 C10 H10A 108.8 . . ? C9 C10 H10A 108.8 . . ? C11 C10 H10B 108.8 . . ? C9 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C10 C11 C12 113.4(5) . . ? C10 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? C10 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C13 C12 C11 109.2(5) . . ? C13 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? C13 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? N2 C13 C8 106.3(4) . . ? N2 C13 C12 117.8(5) . . ? C8 C13 C12 113.7(5) . . ? N2 C13 H13 106.1 . . ? C8 C13 H13 106.1 . . ? C12 C13 H13 106.1 . . ? N2 C14 C15 125.0(5) . . ? N2 C14 H14 117.5 . . ? C15 C14 H14 117.5 . . ? C20 C15 C16 120.0(5) . . ? C20 C15 C14 122.6(5) . . ? C16 C15 C14 117.3(5) . . ? C17 C16 C15 121.0(5) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 120.3(5) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C19 120.6(5) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? O4 C19 C18 125.6(5) . . ? O4 C19 C20 113.7(4) . . ? C18 C19 C20 120.7(5) . . ? O2 C20 C15 125.0(4) . . ? O2 C20 C19 117.7(5) . . ? C15 C20 C19 117.3(5) . . ? O3 C21 C22 107.3(5) . . ? O3 C21 H21A 110.3 . . ? C22 C21 H21A 110.3 . . ? O3 C21 H21B 110.3 . . ? C22 C21 H21B 110.3 . . ? H21A C21 H21B 108.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O4 C23 C24 109.2(5) . . ? O4 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? O4 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O5 C25 C30 125.3(4) . . ? O5 C25 C26 116.5(4) . . ? C30 C25 C26 118.2(4) . . ? O7 C26 C27 124.5(5) . . ? O7 C26 C25 114.9(4) . . ? C27 C26 C25 120.6(5) . . ? C26 C27 C28 120.8(5) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C29 C28 C27 119.7(5) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 121.5(5) . . ? C28 C29 H29 119.2 . . ? C30 C29 H29 119.2 . . ? C25 C30 C29 119.1(5) . . ? C25 C30 C31 122.7(4) . . ? C29 C30 C31 118.1(5) . . ? N3 C31 C30 125.0(4) . . ? N3 C31 H31 117.5 . . ? C30 C31 H31 117.5 . . ? C37 C32 N3 108.2(4) . . ? C37 C32 C33 113.4(5) . . ? N3 C32 C33 117.3(5) . . ? C37 C32 H32 105.7 . . ? N3 C32 H32 105.7 . . ? C33 C32 H32 105.7 . . ? C32 C33 C34 110.0(5) . . ? C32 C33 H33A 109.7 . . ? C34 C33 H33A 109.7 . . ? C32 C33 H33B 109.7 . . ? C34 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? C35 C34 C33 115.6(6) . . ? C35 C34 H34A 108.4 . . ? C33 C34 H34A 108.4 . . ? C35 C34 H34B 108.4 . . ? C33 C34 H34B 108.4 . . ? H34A C34 H34B 107.4 . . ? C34 C35 C36 114.4(6) . . ? C34 C35 H35A 108.7 . . ? C36 C35 H35A 108.7 . . ? C34 C35 H35B 108.7 . . ? C36 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? C37 C36 C35 109.4(5) . . ? C37 C36 H36A 109.8 . . ? C35 C36 H36A 109.8 . . ? C37 C36 H36B 109.8 . . ? C35 C36 H36B 109.8 . . ? H36A C36 H36B 108.2 . . ? C32 C37 N4 107.4(4) . . ? C32 C37 C36 114.6(5) . . ? N4 C37 C36 116.1(5) . . ? C32 C37 H37 105.9 . . ? N4 C37 H37 105.9 . . ? C36 C37 H37 105.9 . . ? N4 C38 C39 126.9(5) . . ? N4 C38 H38 116.6 . . ? C39 C38 H38 116.6 . . ? C44 C39 C40 119.7(5) . . ? C44 C39 C38 121.9(4) . . ? C40 C39 C38 118.3(5) . . ? C41 C40 C39 121.1(5) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C40 C41 C42 120.4(5) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C43 120.4(5) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? O8 C43 C42 125.1(5) . . ? O8 C43 C44 113.9(4) . . ? C42 C43 C44 121.0(5) . . ? O6 C44 C39 124.9(4) . . ? O6 C44 C43 117.6(5) . . ? C39 C44 C43 117.4(4) . . ? O7 C45 C46 107.5(4) . . ? O7 C45 H45A 110.2 . . ? C46 C45 H45A 110.2 . . ? O7 C45 H45B 110.2 . . ? C46 C45 H45B 110.2 . . ? H45A C45 H45B 108.5 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O8 C47 C48 107.3(4) . . ? O8 C47 H47A 110.3 . . ? C48 C47 H47A 110.3 . . ? O8 C47 H47B 110.3 . . ? C48 C47 H47B 110.3 . . ? H47A C47 H47B 108.5 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O10 Cl1 O12 110.4(7) . . ? O10 Cl1 O11 112.4(5) . . ? O12 Cl1 O11 109.8(5) . . ? O10 Cl1 O9 107.1(5) . . ? O12 Cl1 O9 106.6(5) . . ? O11 Cl1 O9 110.3(4) . . ? O2 Cu1 O1 89.84(14) . . ? O2 Cu1 N2 92.84(16) . . ? O1 Cu1 N2 174.74(16) . . ? O2 Cu1 N1 172.86(16) . . ? O1 Cu1 N1 93.73(17) . . ? N2 Cu1 N1 84.11(18) . . ? O6 Cu2 O5 89.99(13) . . ? O6 Cu2 N3 171.50(15) . . ? O5 Cu2 N3 93.53(15) . . ? O6 Cu2 N4 93.55(15) . . ? O5 Cu2 N4 168.73(16) . . ? N3 Cu2 N4 84.47(17) . . ? C7 N1 C8 122.0(5) . . ? C7 N1 Cu1 125.6(4) . . ? C8 N1 Cu1 112.3(3) . . ? C14 N2 C13 121.1(4) . . ? C14 N2 Cu1 126.7(4) . . ? C13 N2 Cu1 112.2(3) . . ? C31 N3 C32 121.3(4) . . ? C31 N3 Cu2 127.0(3) . . ? C32 N3 Cu2 111.7(3) . . ? C38 N4 C37 122.7(4) . . ? C38 N4 Cu2 125.6(4) . . ? C37 N4 Cu2 111.3(3) . . ? C1 O1 Cu1 126.4(3) . . ? C20 O2 Cu1 125.5(3) . . ? C2 O3 C21 117.7(4) . . ? C19 O4 C23 118.6(4) . . ? C25 O5 Cu2 126.3(3) . . ? C44 O6 Cu2 127.0(3) . . ? C26 O7 C45 118.0(4) . . ? C43 O8 C47 118.6(4) . . ? H1WA O1W H1WB 96(4) . . ? H1WA O1W H1WC 99(5) . . ? H1WB O1W H1WC 105(6) . . ? H2WA O2W H2WB 96(4) . . ? H2WA O2W H1WC 98(5) . . ? H2WB O2W H1WC 123(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WC O2W 1.11(8) 1.40(8) 2.501(6) 171(6) . O1W H1WA O1 0.796(10) 1.83(3) 2.569(5) 153(6) . O1W H1WA O3 0.796(10) 2.28(4) 2.826(6) 126(5) . O1W H1WB O2 0.799(10) 1.85(3) 2.600(5) 156(7) . O1W H1WB O4 0.799(10) 2.28(5) 2.814(6) 124(6) . O2W H2WA O5 0.797(10) 1.99(3) 2.713(5) 150(5) . O2W H2WA O7 0.797(10) 2.35(4) 2.929(5) 131(5) . O2W H2WB O6 0.798(10) 2.13(3) 2.785(5) 139(4) . O2W H2WB O8 0.798(10) 2.26(3) 2.968(5) 149(4) . _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.648 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.069 data_3 _database_code_depnum_ccdc_archive 'CCDC 915727' #TrackingRef '1-3 new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H98 Cl2 Cu4 N8 O28' _chemical_formula_weight 1944.72 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 13.8039(7) _cell_length_b 44.740(2) _cell_length_c 15.9315(7) _cell_angle_alpha 90.00 _cell_angle_beta 120.633(3) _cell_angle_gamma 90.00 _cell_volume 8466.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9969 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 23.51 _exptl_crystal_description Cubic _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4032 _exptl_absorpt_coefficient_mu 1.140 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8753 _exptl_absorpt_correction_T_max 0.9143 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 103992 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -56 _diffrn_reflns_limit_k_max 55 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.72 _reflns_number_total 17824 _reflns_number_gt 11278 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+6.2014P] 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 17824 _refine_ls_number_parameters 1123 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.0962 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1282 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1674(3) 1.03447(7) 0.6016(2) 0.0412(8) Uani 1 1 d . . . C2 C -0.2573(3) 1.02079(8) 0.6064(3) 0.0495(9) Uani 1 1 d . . . C3 C -0.3484(3) 1.03728(9) 0.5940(3) 0.0578(10) Uani 1 1 d . . . H3 H -0.4063 1.0279 0.5977 0.069 Uiso 1 1 calc R . . C4 C -0.3540(3) 1.06783(10) 0.5760(3) 0.0643(11) Uani 1 1 d . . . H4 H -0.4158 1.0788 0.5669 0.077 Uiso 1 1 calc R . . C5 C -0.2695(3) 1.08147(9) 0.5716(3) 0.0558(10) Uani 1 1 d . . . H5 H -0.2739 1.1019 0.5597 0.067 Uiso 1 1 calc R . . C6 C -0.1744(3) 1.06539(7) 0.5848(2) 0.0448(8) Uani 1 1 d . . . C7 C -0.0868(3) 1.08205(7) 0.5833(2) 0.0480(9) Uani 1 1 d . . . H6 H -0.0956 1.1027 0.5763 0.058 Uiso 1 1 calc R . . C8 C 0.0900(3) 1.09055(8) 0.5945(3) 0.0545(9) Uani 1 1 d . . . H8A H 0.1438 1.0959 0.6615 0.065 Uiso 1 1 calc R . . H8B H 0.0563 1.1087 0.5580 0.065 Uiso 1 1 calc R . . C9 C 0.1483(3) 1.07375(7) 0.5503(3) 0.0535(9) Uani 1 1 d . . . H9A H 0.1033 1.0745 0.4797 0.064 Uiso 1 1 calc R . . H9B H 0.2210 1.0827 0.5708 0.064 Uiso 1 1 calc R . . C10 C 0.2499(3) 1.02791(8) 0.6009(3) 0.0494(9) Uani 1 1 d . . . H10 H 0.3050 1.0382 0.5954 0.059 Uiso 1 1 calc R . . C11 C 0.2707(3) 0.99707(8) 0.6279(2) 0.0470(9) Uani 1 1 d . . . C12 C 0.3747(3) 0.98520(10) 0.6473(3) 0.0612(10) Uani 1 1 d . . . H12 H 0.4274 0.9977 0.6454 0.073 Uiso 1 1 calc R . . C13 C 0.3993(3) 0.95585(10) 0.6688(3) 0.0670(12) Uani 1 1 d . . . H13 H 0.4682 0.9484 0.6811 0.080 Uiso 1 1 calc R . . C14 C 0.3217(3) 0.93698(9) 0.6724(3) 0.0592(10) Uani 1 1 d . . . H14 H 0.3385 0.9168 0.6868 0.071 Uiso 1 1 calc R . . C15 C 0.2201(3) 0.94795(8) 0.6550(2) 0.0480(9) Uani 1 1 d . . . C16 C 0.1913(3) 0.97837(7) 0.6323(2) 0.0422(8) Uani 1 1 d . . . C17 C -0.3310(4) 0.97424(10) 0.6232(3) 0.0721(12) Uani 1 1 d . . . H17A H -0.4010 0.9775 0.5623 0.087 Uiso 1 1 calc R . . H17B H -0.3413 0.9806 0.6764 0.087 Uiso 1 1 calc R . . C18 C -0.3007(4) 0.94224(10) 0.6341(4) 0.0863(15) Uani 1 1 d . . . H18A H -0.2336 0.9390 0.6960 0.129 Uiso 1 1 calc R . . H18B H -0.2876 0.9363 0.5827 0.129 Uiso 1 1 calc R . . H18C H -0.3611 0.9306 0.6305 0.129 Uiso 1 1 calc R . . C19 C 0.1601(4) 0.90046(8) 0.6819(3) 0.0700(12) Uani 1 1 d . . . H19A H 0.2305 0.8983 0.7433 0.084 Uiso 1 1 calc R . . H19B H 0.1667 0.8899 0.6318 0.084 Uiso 1 1 calc R . . C20 C 0.0665(4) 0.88760(9) 0.6907(3) 0.0807(14) Uani 1 1 d . . . H20B H -0.0023 0.8889 0.6289 0.121 Uiso 1 1 calc R . . H20A H 0.0586 0.8986 0.7387 0.121 Uiso 1 1 calc R . . H20C H 0.0826 0.8670 0.7102 0.121 Uiso 1 1 calc R . . C21 C -0.1650(3) 0.96138(8) 0.8997(2) 0.0451(8) Uani 1 1 d . . . C22 C -0.1699(3) 0.92992(8) 0.9081(3) 0.0520(9) Uani 1 1 d . . . C23 C -0.2593(4) 0.91665(9) 0.9085(3) 0.0654(11) Uani 1 1 d . . . H23 H -0.2609 0.8960 0.9141 0.078 Uiso 1 1 calc R . . C24 C -0.3471(4) 0.93369(11) 0.9006(3) 0.0732(13) Uani 1 1 d . . . H24 H -0.4071 0.9245 0.9012 0.088 Uiso 1 1 calc R . . C25 C -0.3460(3) 0.96373(10) 0.8920(3) 0.0621(11) Uani 1 1 d . . . H25 H -0.4058 0.9750 0.8861 0.075 Uiso 1 1 calc R . . C26 C -0.2553(3) 0.97817(8) 0.8920(2) 0.0476(9) Uani 1 1 d . . . C27 C -0.2562(3) 1.01056(9) 0.8891(2) 0.0500(9) Uani 1 1 d . . . H27 H -0.3167 1.0203 0.8875 0.060 Uiso 1 1 calc R . . C28 C -0.1849(3) 1.05951(8) 0.8948(3) 0.0566(10) Uani 1 1 d . . . H28A H -0.1390 1.0659 0.9621 0.068 Uiso 1 1 calc R . . H28B H -0.2617 1.0661 0.8706 0.068 Uiso 1 1 calc R . . C29 C -0.1408(3) 1.07277(8) 0.8340(3) 0.0605(10) Uani 1 1 d . . . H29A H -0.1985 1.0722 0.7654 0.073 Uiso 1 1 calc R . . H29B H -0.1192 1.0934 0.8524 0.073 Uiso 1 1 calc R . . C30 C 0.0362(3) 1.06695(9) 0.8420(3) 0.0577(10) Uani 1 1 d . . . H30 H 0.0306 1.0873 0.8283 0.069 Uiso 1 1 calc R . . C31 C 0.1321(3) 1.05161(9) 0.8514(3) 0.0540(10) Uani 1 1 d . . . C32 C 0.2123(4) 1.06876(11) 0.8418(3) 0.0773(14) Uani 1 1 d . . . H32 H 0.2019 1.0893 0.8321 0.093 Uiso 1 1 calc R . . C33 C 0.3035(4) 1.05596(14) 0.8465(3) 0.0893(16) Uani 1 1 d . . . H33 H 0.3545 1.0676 0.8389 0.107 Uiso 1 1 calc R . . C34 C 0.3210(4) 1.02553(14) 0.8627(3) 0.0809(15) Uani 1 1 d . . . H34 H 0.3831 1.0166 0.8649 0.097 Uiso 1 1 calc R . . C35 C 0.2465(3) 1.00829(10) 0.8757(3) 0.0604(11) Uani 1 1 d . . . C36 C 0.1488(3) 1.02073(9) 0.8694(2) 0.0507(9) Uani 1 1 d . . . C37 C -0.0685(4) 0.88405(8) 0.9344(3) 0.0726(12) Uani 1 1 d . . . H37A H -0.1341 0.8736 0.8841 0.087 Uiso 1 1 calc R . . H37B H -0.0627 0.8802 0.9967 0.087 Uiso 1 1 calc R . . C38 C 0.0354(4) 0.87323(9) 0.9363(4) 0.0953(16) Uani 1 1 d . . . H38A H 0.0990 0.8848 0.9825 0.143 Uiso 1 1 calc R . . H38B H 0.0260 0.8754 0.8726 0.143 Uiso 1 1 calc R . . H38C H 0.0477 0.8526 0.9550 0.143 Uiso 1 1 calc R . . C39 C 0.3619(4) 0.96435(13) 0.9197(4) 0.0873(16) Uani 1 1 d . . . H39A H 0.4247 0.9756 0.9703 0.105 Uiso 1 1 calc R . . H39B H 0.3700 0.9636 0.8627 0.105 Uiso 1 1 calc R . . C40 C 0.3606(4) 0.93350(13) 0.9545(4) 0.110(2) Uani 1 1 d . . . H40A H 0.2971 0.9228 0.9045 0.164 Uiso 1 1 calc R . . H40B H 0.3550 0.9345 1.0121 0.164 Uiso 1 1 calc R . . H40C H 0.4288 0.9233 0.9693 0.164 Uiso 1 1 calc R . . C41 C 0.6672(3) 0.78601(8) 0.4033(2) 0.0432(8) Uani 1 1 d . . . C42 C 0.7592(3) 0.77239(8) 0.4016(3) 0.0521(9) Uani 1 1 d . . . C43 C 0.8442(3) 0.78932(10) 0.4038(3) 0.0649(11) Uani 1 1 d . . . H43 H 0.9031 0.7799 0.4019 0.078 Uiso 1 1 calc R . . C44 C 0.8420(4) 0.82006(10) 0.4088(3) 0.0727(12) Uani 1 1 d . . . H44 H 0.8999 0.8313 0.4109 0.087 Uiso 1 1 calc R . . C45 C 0.7558(4) 0.83393(9) 0.4106(3) 0.0656(11) Uani 1 1 d . . . H45 H 0.7554 0.8547 0.4141 0.079 Uiso 1 1 calc R . . C46 C 0.6665(3) 0.81752(8) 0.4072(3) 0.0492(9) Uani 1 1 d . . . C47 C 0.5775(3) 0.83394(8) 0.4059(3) 0.0517(9) Uani 1 1 d . . . H47 H 0.5821 0.8547 0.4054 0.062 Uiso 1 1 calc R . . C48 C 0.4019(3) 0.84250(8) 0.3979(3) 0.0571(10) Uani 1 1 d . . . H48A H 0.3461 0.8460 0.3299 0.068 Uiso 1 1 calc R . . H48B H 0.4333 0.8616 0.4285 0.068 Uiso 1 1 calc R . . C49 C 0.3483(3) 0.82725(8) 0.4487(3) 0.0557(10) Uani 1 1 d . . . H49A H 0.3942 0.8302 0.5186 0.067 Uiso 1 1 calc R . . H49B H 0.2743 0.8356 0.4266 0.067 Uiso 1 1 calc R . . C50 C 0.2542(3) 0.78040(8) 0.4138(3) 0.0487(9) Uani 1 1 d . . . H50 H 0.1963 0.7910 0.4141 0.058 Uiso 1 1 calc R . . C51 C 0.2405(3) 0.74883(8) 0.4005(2) 0.0464(8) Uani 1 1 d . . . C52 C 0.1416(3) 0.73631(9) 0.3897(3) 0.0606(10) Uani 1 1 d . . . H52 H 0.0863 0.7489 0.3867 0.073 Uiso 1 1 calc R . . C53 C 0.1246(3) 0.70648(10) 0.3835(3) 0.0692(12) Uani 1 1 d . . . H53 H 0.0589 0.6987 0.3774 0.083 Uiso 1 1 calc R . . C54 C 0.2064(3) 0.68747(9) 0.3863(3) 0.0613(11) Uani 1 1 d . . . H54 H 0.1955 0.6669 0.3828 0.074 Uiso 1 1 calc R . . C55 C 0.3032(3) 0.69902(8) 0.3943(2) 0.0481(9) Uani 1 1 d . . . C56 C 0.3240(3) 0.73008(7) 0.4023(2) 0.0416(8) Uani 1 1 d . . . C57 C 0.8473(4) 0.72565(10) 0.4086(3) 0.0718(12) Uani 1 1 d . . . H57A H 0.9163 0.7320 0.4663 0.086 Uiso 1 1 calc R . . H57B H 0.8548 0.7290 0.3520 0.086 Uiso 1 1 calc R . . C58 C 0.8260(4) 0.69361(11) 0.4163(4) 0.0976(17) Uani 1 1 d . . . H58A H 0.8230 0.6904 0.4745 0.146 Uiso 1 1 calc R . . H58B H 0.8856 0.6818 0.4189 0.146 Uiso 1 1 calc R . . H58C H 0.7556 0.6878 0.3604 0.146 Uiso 1 1 calc R . . C59 C 0.3748(4) 0.65084(8) 0.3894(4) 0.0752(13) Uani 1 1 d . . . H59A H 0.3026 0.6457 0.3330 0.090 Uiso 1 1 calc R . . H59B H 0.3777 0.6429 0.4472 0.090 Uiso 1 1 calc R . . C60 C 0.4684(4) 0.63805(10) 0.3791(4) 0.1001(18) Uani 1 1 d . . . H60A H 0.4687 0.6473 0.3248 0.150 Uiso 1 1 calc R . . H60B H 0.4576 0.6169 0.3681 0.150 Uiso 1 1 calc R . . H60C H 0.5391 0.6417 0.4377 0.150 Uiso 1 1 calc R . . C61 C 0.6909(3) 0.78620(9) 0.6381(2) 0.0497(9) Uani 1 1 d . . . C62 C 0.7093(3) 0.81744(9) 0.6506(3) 0.0546(10) Uani 1 1 d . . . C63 C 0.8062(4) 0.82993(11) 0.6613(3) 0.0740(13) Uani 1 1 d . . . H63 H 0.8169 0.8505 0.6691 0.089 Uiso 1 1 calc R . . C64 C 0.8879(4) 0.81201(13) 0.6606(3) 0.0858(15) Uani 1 1 d . . . H64 H 0.9527 0.8207 0.6673 0.103 Uiso 1 1 calc R . . C65 C 0.8739(4) 0.78192(12) 0.6502(3) 0.0754(13) Uani 1 1 d . . . H65 H 0.9297 0.7701 0.6509 0.090 Uiso 1 1 calc R . . C66 C 0.7753(3) 0.76838(10) 0.6385(3) 0.0575(10) Uani 1 1 d . . . C67 C 0.7652(3) 0.73635(10) 0.6246(3) 0.0622(11) Uani 1 1 d . . . H67 H 0.8227 0.7264 0.6218 0.075 Uiso 1 1 calc R . . C68 C 0.6794(4) 0.68829(9) 0.5974(3) 0.0731(12) Uani 1 1 d . . . H68A H 0.7545 0.6807 0.6194 0.088 Uiso 1 1 calc R . . H68B H 0.6325 0.6843 0.5281 0.088 Uiso 1 1 calc R . . C69 C 0.6313(4) 0.67344(9) 0.6523(3) 0.0749(13) Uani 1 1 d . . . H69A H 0.6046 0.6536 0.6264 0.090 Uiso 1 1 calc R . . H69B H 0.6886 0.6716 0.7207 0.090 Uiso 1 1 calc R . . C70 C 0.4566(4) 0.68009(9) 0.6472(3) 0.0651(11) Uani 1 1 d . . . H70 H 0.4574 0.6594 0.6534 0.078 Uiso 1 1 calc R . . C71 C 0.3651(4) 0.69577(9) 0.6448(3) 0.0601(10) Uani 1 1 d . . . C72 C 0.2794(4) 0.67863(11) 0.6473(3) 0.0774(14) Uani 1 1 d . . . H72 H 0.2839 0.6579 0.6482 0.093 Uiso 1 1 calc R . . C73 C 0.1930(4) 0.69161(13) 0.6485(3) 0.0868(16) Uani 1 1 d . . . H73 H 0.1386 0.6799 0.6505 0.104 Uiso 1 1 calc R . . C74 C 0.1838(4) 0.72285(12) 0.6466(3) 0.0780(14) Uani 1 1 d . . . H74 H 0.1245 0.7319 0.6489 0.094 Uiso 1 1 calc R . . C75 C 0.2634(3) 0.74010(10) 0.6413(3) 0.0608(10) Uani 1 1 d . . . C76 C 0.3567(3) 0.72711(9) 0.6403(2) 0.0526(9) Uani 1 1 d . . . C77 C 0.6356(4) 0.86448(9) 0.6639(4) 0.0798(14) Uani 1 1 d . . . H77A H 0.6348 0.8736 0.6083 0.096 Uiso 1 1 calc R . . H77B H 0.7062 0.8695 0.7222 0.096 Uiso 1 1 calc R . . C78 C 0.5392(5) 0.87574(10) 0.6723(4) 0.0953(17) Uani 1 1 d . . . H78A H 0.4700 0.8720 0.6125 0.143 Uiso 1 1 calc R . . H78B H 0.5476 0.8968 0.6850 0.143 Uiso 1 1 calc R . . H78C H 0.5379 0.8656 0.7249 0.143 Uiso 1 1 calc R . . C79 C 0.1661(4) 0.78588(12) 0.6265(3) 0.0807(14) Uani 1 1 d . . . H79A H 0.1614 0.7828 0.6846 0.097 Uiso 1 1 calc R . . H79B H 0.0977 0.7783 0.5708 0.097 Uiso 1 1 calc R . . C80 C 0.1791(4) 0.81845(12) 0.6132(4) 0.1010(17) Uani 1 1 d . . . H80A H 0.2448 0.8260 0.6701 0.152 Uiso 1 1 calc R . . H80B H 0.1138 0.8291 0.6038 0.152 Uiso 1 1 calc R . . H80C H 0.1868 0.8212 0.5571 0.152 Uiso 1 1 calc R . . Cl1 Cl 0.50912(8) 0.91050(2) 0.27225(9) 0.0650(3) Uani 1 1 d . . . Cl2 Cl 1.0057(5) 0.84272(12) 0.2614(6) 0.0696(9) Uani 0.709(4) 1 d PDU A 1 O21 O 1.0598(5) 0.84103(13) 0.3666(4) 0.1165(17) Uani 0.709(4) 1 d PDU A 1 O22 O 0.9027(6) 0.85792(19) 0.2299(6) 0.102(2) Uani 0.709(4) 1 d PDU A 1 O23 O 1.0815(5) 0.85892(15) 0.2429(5) 0.105(2) Uani 0.709(4) 1 d PDU A 1 O24 O 0.9871(5) 0.81397(12) 0.2214(5) 0.105(2) Uani 0.709(4) 1 d PDU A 1 Cl2' Cl 0.9949(12) 0.8438(3) 0.2474(16) 0.0696(9) Uani 0.291(4) 1 d PDU A 2 O21' O 0.9502(10) 0.8455(3) 0.1444(8) 0.1165(17) Uani 0.291(4) 1 d PDU A 2 O22' O 0.9211(16) 0.8608(5) 0.2655(17) 0.102(2) Uani 0.291(4) 1 d PDU A 2 O23' O 1.1049(13) 0.8560(4) 0.2922(11) 0.105(2) Uani 0.291(4) 1 d PDU A 2 O24' O 1.0013(15) 0.8142(3) 0.2772(11) 0.105(2) Uani 0.291(4) 1 d PDU A 2 Cu1 Cu 0.04046(3) 1.028630(9) 0.59957(3) 0.04191(11) Uani 1 1 d . . . Cu2 Cu -0.05086(3) 1.013832(9) 0.88330(3) 0.04487(12) Uani 1 1 d . . . Cu3 Cu 0.46321(3) 0.780757(9) 0.41337(3) 0.04244(12) Uani 1 1 d . . . Cu4 Cu 0.55703(4) 0.734080(10) 0.62631(3) 0.05025(13) Uani 1 1 d . . . N1 N 0.0027(2) 1.07089(6) 0.5907(2) 0.0443(7) Uani 1 1 d . . . N2 N 0.1627(2) 1.04261(6) 0.5838(2) 0.0453(7) Uani 1 1 d . . . N3 N -0.1811(2) 1.02675(6) 0.8885(2) 0.0467(7) Uani 1 1 d . . . N4 N -0.0428(3) 1.05514(6) 0.8509(2) 0.0503(7) Uani 1 1 d . . . N6 N 0.3388(2) 0.79538(6) 0.4256(2) 0.0479(7) Uani 1 1 d . . . N5 N 0.4917(3) 0.82281(6) 0.4054(2) 0.0472(7) Uani 1 1 d . . . N7 N 0.6836(3) 0.72069(7) 0.6159(2) 0.0578(8) Uani 1 1 d . . . N8 N 0.5375(3) 0.69185(7) 0.6417(2) 0.0590(8) Uani 1 1 d . . . O1 O -0.08432(18) 1.01725(5) 0.61348(16) 0.0445(5) Uani 1 1 d . . . O2 O 0.09067(19) 0.98743(5) 0.61451(17) 0.0475(6) Uani 1 1 d . . . O3 O -0.2433(2) 0.99085(6) 0.6241(2) 0.0612(7) Uani 1 1 d . . . O4 O 0.1377(2) 0.93109(5) 0.65731(19) 0.0581(7) Uani 1 1 d . . . O5 O -0.0751(2) 0.97271(5) 0.90307(18) 0.0531(6) Uani 1 1 d . . . O6 O 0.08128(19) 1.00305(5) 0.88140(17) 0.0507(6) Uani 1 1 d . . . O7 O -0.0792(2) 0.91518(5) 0.9149(2) 0.0664(7) Uani 1 1 d . . . O8 O 0.2588(2) 0.97820(7) 0.8960(2) 0.0729(8) Uani 1 1 d . . . O9 O 0.58883(18) 0.76865(5) 0.40108(17) 0.0449(6) Uani 1 1 d . . . O10 O 0.42069(19) 0.73963(5) 0.41326(18) 0.0485(6) Uani 1 1 d . . . O11 O 0.7542(2) 0.74192(6) 0.3996(2) 0.0629(7) Uani 1 1 d . . . O12 O 0.3884(2) 0.68229(5) 0.39688(19) 0.0595(7) Uani 1 1 d . . . O13 O 0.5946(2) 0.77566(5) 0.62519(19) 0.0554(6) Uani 1 1 d . . . O14 O 0.4297(2) 0.74516(5) 0.63563(17) 0.0532(6) Uani 1 1 d . . . O15 O 0.6249(2) 0.83299(6) 0.6518(2) 0.0638(7) Uani 1 1 d . . . O16 O 0.2611(2) 0.77058(7) 0.6355(2) 0.0705(8) Uani 1 1 d . . . O17 O 0.5852(3) 0.89558(8) 0.2521(3) 0.1158(13) Uani 1 1 d . . . O18 O 0.4880(3) 0.93971(7) 0.2351(3) 0.1059(12) Uani 1 1 d . . . O19 O 0.5660(3) 0.91188(8) 0.3781(3) 0.1026(11) Uani 1 1 d . . . O20 O 0.4090(3) 0.89432(7) 0.2408(3) 0.0993(11) Uani 1 1 d . . . O1W O -0.0397(2) 0.96110(5) 0.66397(17) 0.0537(6) Uani 1 1 d D . . H1WB H 0.0171 0.9634 0.6625 0.081 Uiso 1 1 d RD . . H1WC H 0.0053 0.9549 0.7440 0.081 Uiso 1 1 d R . . H1WA H -0.0688 0.9769 0.6589 0.081 Uiso 1 1 d RD . . O2W O 0.0509(2) 0.94497(6) 0.83674(18) 0.0623(7) Uani 1 1 d D . . H2WB H 0.0989 0.9574 0.8536 0.093 Uiso 1 1 d RD . . H2WA H 0.0089 0.9490 0.8563 0.093 Uiso 1 1 d RD . . O3W O 0.5518(2) 0.78818(5) 0.86485(18) 0.0546(6) Uani 1 1 d D . . H3WB H 0.4967 0.7857 0.8676 0.082 Uiso 1 1 d RD . . H3WA H 0.5896 0.7735 0.8749 0.082 Uiso 1 1 d RD . . H3WC H 0.5262 0.7955 0.7961 0.082 Uiso 1 1 d R . . O4W O 0.4677(2) 0.80191(6) 0.69274(18) 0.0613(7) Uani 1 1 d D . . H4WA H 0.5086 0.7998 0.6712 0.092 Uiso 1 1 d RD . . H4WB H 0.4312 0.7873 0.6672 0.092 Uiso 1 1 d RD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.043(2) 0.0433(19) 0.0360(18) 0.0001(15) 0.0191(15) 0.0060(16) C2 0.046(2) 0.051(2) 0.049(2) 0.0030(17) 0.0227(18) 0.0028(17) C3 0.045(2) 0.071(3) 0.062(2) -0.003(2) 0.0306(19) 0.0048(19) C4 0.055(3) 0.076(3) 0.062(3) 0.003(2) 0.029(2) 0.022(2) C5 0.064(3) 0.052(2) 0.051(2) 0.0032(18) 0.029(2) 0.021(2) C6 0.054(2) 0.044(2) 0.0390(19) 0.0001(15) 0.0252(17) 0.0071(17) C7 0.064(2) 0.0346(18) 0.044(2) 0.0029(15) 0.0258(18) 0.0094(17) C8 0.064(2) 0.038(2) 0.064(2) 0.0015(17) 0.034(2) -0.0047(18) C9 0.056(2) 0.043(2) 0.065(2) 0.0048(18) 0.033(2) -0.0062(17) C10 0.046(2) 0.051(2) 0.051(2) -0.0023(17) 0.0246(18) -0.0046(17) C11 0.040(2) 0.056(2) 0.0386(19) -0.0002(16) 0.0157(16) 0.0079(17) C12 0.047(2) 0.074(3) 0.059(2) -0.007(2) 0.024(2) 0.003(2) C13 0.048(2) 0.072(3) 0.071(3) -0.004(2) 0.022(2) 0.018(2) C14 0.061(3) 0.052(2) 0.056(2) 0.0024(18) 0.024(2) 0.024(2) C15 0.054(2) 0.046(2) 0.0378(19) 0.0021(15) 0.0193(17) 0.0104(18) C16 0.044(2) 0.0432(19) 0.0341(18) 0.0003(14) 0.0161(16) 0.0090(15) C17 0.065(3) 0.080(3) 0.076(3) -0.001(2) 0.040(2) -0.017(2) C18 0.086(3) 0.070(3) 0.112(4) 0.002(3) 0.058(3) -0.023(3) C19 0.087(3) 0.040(2) 0.071(3) 0.0105(19) 0.031(2) 0.018(2) C20 0.117(4) 0.041(2) 0.094(4) 0.020(2) 0.060(3) 0.016(2) C21 0.046(2) 0.048(2) 0.0372(19) 0.0033(15) 0.0184(16) -0.0056(17) C22 0.056(2) 0.051(2) 0.048(2) -0.0023(17) 0.0256(19) -0.0094(19) C23 0.072(3) 0.056(2) 0.063(3) -0.005(2) 0.030(2) -0.023(2) C24 0.063(3) 0.083(3) 0.073(3) -0.010(2) 0.035(2) -0.031(3) C25 0.043(2) 0.084(3) 0.057(2) -0.009(2) 0.0247(19) -0.010(2) C26 0.042(2) 0.060(2) 0.0353(19) -0.0042(16) 0.0157(16) -0.0046(17) C27 0.041(2) 0.066(3) 0.039(2) 0.0011(17) 0.0176(17) 0.0067(18) C28 0.059(2) 0.047(2) 0.056(2) 0.0036(18) 0.024(2) 0.0116(18) C29 0.064(3) 0.051(2) 0.053(2) 0.0084(18) 0.020(2) 0.0106(19) C30 0.073(3) 0.051(2) 0.041(2) 0.0043(17) 0.023(2) -0.014(2) C31 0.058(2) 0.062(2) 0.040(2) 0.0033(17) 0.0232(18) -0.014(2) C32 0.076(3) 0.098(4) 0.055(3) 0.008(2) 0.031(2) -0.029(3) C33 0.081(4) 0.125(5) 0.067(3) 0.006(3) 0.042(3) -0.035(3) C34 0.052(3) 0.142(5) 0.057(3) -0.011(3) 0.033(2) -0.021(3) C35 0.051(2) 0.088(3) 0.042(2) -0.008(2) 0.0233(19) -0.014(2) C36 0.042(2) 0.072(3) 0.0357(19) -0.0055(17) 0.0178(16) -0.0120(18) C37 0.089(3) 0.043(2) 0.075(3) 0.001(2) 0.034(3) -0.012(2) C38 0.118(4) 0.045(3) 0.133(5) 0.000(3) 0.071(4) 0.005(3) C39 0.051(3) 0.128(5) 0.083(3) -0.026(3) 0.033(3) 0.007(3) C40 0.080(4) 0.112(5) 0.123(5) -0.022(4) 0.041(3) 0.028(3) C41 0.041(2) 0.048(2) 0.0386(19) 0.0026(15) 0.0196(16) -0.0011(16) C42 0.050(2) 0.057(2) 0.048(2) 0.0000(18) 0.0243(18) -0.0001(18) C43 0.051(2) 0.080(3) 0.071(3) 0.009(2) 0.037(2) -0.001(2) C44 0.068(3) 0.077(3) 0.084(3) 0.007(2) 0.046(3) -0.017(2) C45 0.073(3) 0.059(3) 0.070(3) 0.010(2) 0.040(2) -0.008(2) C46 0.055(2) 0.047(2) 0.046(2) 0.0046(16) 0.0261(18) -0.0064(17) C47 0.067(3) 0.0378(19) 0.051(2) 0.0083(16) 0.031(2) 0.0009(18) C48 0.069(3) 0.040(2) 0.062(2) 0.0077(17) 0.032(2) 0.0138(18) C49 0.055(2) 0.047(2) 0.063(2) -0.0050(18) 0.029(2) 0.0060(18) C50 0.041(2) 0.051(2) 0.051(2) 0.0010(17) 0.0219(17) 0.0071(17) C51 0.041(2) 0.051(2) 0.0408(19) -0.0036(16) 0.0165(16) -0.0072(16) C52 0.041(2) 0.074(3) 0.066(3) -0.005(2) 0.026(2) -0.005(2) C53 0.051(2) 0.084(3) 0.074(3) -0.012(2) 0.032(2) -0.023(2) C54 0.064(3) 0.054(2) 0.067(3) -0.0120(19) 0.034(2) -0.026(2) C55 0.053(2) 0.047(2) 0.043(2) -0.0110(16) 0.0245(18) -0.0114(17) C56 0.0377(19) 0.0435(19) 0.0366(18) -0.0063(15) 0.0139(15) -0.0094(15) C57 0.059(3) 0.081(3) 0.085(3) -0.005(2) 0.044(2) 0.015(2) C58 0.097(4) 0.075(3) 0.137(5) -0.005(3) 0.072(4) 0.022(3) C59 0.095(3) 0.037(2) 0.103(4) -0.016(2) 0.058(3) -0.014(2) C60 0.122(4) 0.044(3) 0.158(5) -0.018(3) 0.089(4) -0.005(3) C61 0.045(2) 0.063(2) 0.0363(19) 0.0013(17) 0.0170(16) -0.0050(18) C62 0.051(2) 0.064(3) 0.043(2) -0.0025(18) 0.0195(18) -0.015(2) C63 0.064(3) 0.079(3) 0.071(3) -0.003(2) 0.028(2) -0.023(2) C64 0.054(3) 0.114(4) 0.083(3) -0.005(3) 0.030(3) -0.030(3) C65 0.048(3) 0.108(4) 0.063(3) 0.002(3) 0.023(2) -0.002(3) C66 0.038(2) 0.085(3) 0.041(2) -0.002(2) 0.0131(17) -0.005(2) C67 0.043(2) 0.086(3) 0.053(2) 0.008(2) 0.0211(19) 0.014(2) C68 0.071(3) 0.069(3) 0.073(3) 0.007(2) 0.032(2) 0.019(2) C69 0.087(3) 0.056(3) 0.073(3) 0.019(2) 0.035(3) 0.020(2) C70 0.091(3) 0.045(2) 0.055(3) 0.0107(18) 0.034(2) -0.007(2) C71 0.071(3) 0.066(3) 0.044(2) 0.0034(19) 0.029(2) -0.015(2) C72 0.096(4) 0.072(3) 0.067(3) 0.006(2) 0.044(3) -0.030(3) C73 0.088(4) 0.104(4) 0.081(3) 0.000(3) 0.052(3) -0.039(3) C74 0.066(3) 0.110(4) 0.069(3) -0.006(3) 0.042(2) -0.025(3) C75 0.054(2) 0.082(3) 0.048(2) -0.006(2) 0.027(2) -0.012(2) C76 0.056(2) 0.061(2) 0.0323(19) -0.0049(17) 0.0166(17) -0.0167(19) C77 0.097(4) 0.047(2) 0.094(4) -0.019(2) 0.048(3) -0.025(2) C78 0.136(5) 0.053(3) 0.124(4) -0.027(3) 0.086(4) -0.021(3) C79 0.058(3) 0.115(4) 0.074(3) -0.018(3) 0.037(2) 0.002(3) C80 0.090(4) 0.103(4) 0.121(5) -0.023(4) 0.061(4) 0.015(3) Cl1 0.0580(6) 0.0502(6) 0.0921(8) 0.0139(5) 0.0422(6) 0.0023(4) Cl2 0.0607(13) 0.0502(7) 0.105(3) -0.0074(10) 0.0476(16) -0.0017(7) O21 0.110(4) 0.139(4) 0.100(3) 0.003(3) 0.053(3) 0.015(3) O22 0.081(3) 0.088(3) 0.131(6) -0.009(4) 0.049(4) 0.015(2) O23 0.107(3) 0.097(3) 0.138(5) 0.006(4) 0.082(4) -0.012(3) O24 0.109(3) 0.061(2) 0.142(5) -0.028(3) 0.061(4) -0.006(2) Cl2' 0.0607(13) 0.0502(7) 0.105(3) -0.0074(10) 0.0476(16) -0.0017(7) O21' 0.110(4) 0.139(4) 0.100(3) 0.003(3) 0.053(3) 0.015(3) O22' 0.081(3) 0.088(3) 0.131(6) -0.009(4) 0.049(4) 0.015(2) O23' 0.107(3) 0.097(3) 0.138(5) 0.006(4) 0.082(4) -0.012(3) O24' 0.109(3) 0.061(2) 0.142(5) -0.028(3) 0.061(4) -0.006(2) Cu1 0.0416(2) 0.0337(2) 0.0501(3) 0.00464(18) 0.0230(2) 0.00324(18) Cu2 0.0428(2) 0.0430(2) 0.0476(3) 0.00668(19) 0.0221(2) 0.00135(19) Cu3 0.0414(2) 0.0347(2) 0.0507(3) -0.00185(18) 0.0231(2) -0.00034(18) Cu4 0.0486(3) 0.0482(3) 0.0507(3) 0.0038(2) 0.0229(2) 0.0007(2) N1 0.0524(18) 0.0326(15) 0.0489(17) 0.0000(12) 0.0265(15) -0.0009(13) N2 0.0439(17) 0.0413(16) 0.0479(17) 0.0015(13) 0.0213(14) -0.0023(13) N3 0.0457(18) 0.0467(17) 0.0434(17) 0.0064(13) 0.0195(14) 0.0072(14) N4 0.0592(19) 0.0432(17) 0.0417(17) 0.0038(13) 0.0207(15) -0.0012(15) N6 0.0473(18) 0.0428(17) 0.0506(18) -0.0012(13) 0.0227(15) 0.0044(14) N5 0.0553(19) 0.0364(15) 0.0520(18) 0.0052(13) 0.0288(15) 0.0043(14) N7 0.051(2) 0.063(2) 0.055(2) 0.0071(16) 0.0237(16) 0.0115(17) N8 0.070(2) 0.0514(19) 0.0503(19) 0.0104(15) 0.0267(17) 0.0084(17) O1 0.0435(13) 0.0375(12) 0.0542(14) 0.0047(11) 0.0261(12) 0.0061(11) O2 0.0444(14) 0.0366(13) 0.0606(15) 0.0106(11) 0.0261(12) 0.0088(11) O3 0.0490(15) 0.0580(17) 0.0827(19) 0.0080(14) 0.0381(14) -0.0035(13) O4 0.0682(17) 0.0381(14) 0.0686(17) 0.0135(12) 0.0352(15) 0.0178(12) O5 0.0503(15) 0.0435(14) 0.0713(17) 0.0112(12) 0.0351(13) 0.0030(11) O6 0.0464(14) 0.0532(15) 0.0578(15) -0.0001(12) 0.0303(12) -0.0047(12) O7 0.0778(19) 0.0401(14) 0.091(2) 0.0080(14) 0.0499(17) -0.0014(14) O8 0.0475(17) 0.092(2) 0.084(2) -0.0103(17) 0.0368(16) 0.0012(15) O9 0.0401(13) 0.0420(13) 0.0566(15) -0.0038(11) 0.0275(12) -0.0030(10) O10 0.0445(14) 0.0360(12) 0.0677(16) -0.0069(11) 0.0304(13) -0.0037(11) O11 0.0524(16) 0.0547(17) 0.089(2) -0.0038(14) 0.0419(15) 0.0049(13) O12 0.0708(18) 0.0341(13) 0.0818(19) -0.0134(12) 0.0449(16) -0.0125(12) O13 0.0458(15) 0.0528(15) 0.0688(17) -0.0050(12) 0.0300(13) -0.0085(12) O14 0.0521(15) 0.0519(15) 0.0579(16) -0.0015(12) 0.0298(13) -0.0093(12) O15 0.0683(18) 0.0486(15) 0.0778(19) -0.0051(13) 0.0397(16) -0.0118(13) O16 0.0557(17) 0.077(2) 0.087(2) -0.0096(16) 0.0425(16) -0.0038(15) O17 0.133(3) 0.099(3) 0.169(4) 0.014(3) 0.116(3) 0.022(2) O18 0.092(2) 0.0538(19) 0.148(3) 0.031(2) 0.044(2) 0.0038(17) O19 0.097(3) 0.111(3) 0.094(3) -0.004(2) 0.045(2) -0.016(2) O20 0.067(2) 0.079(2) 0.131(3) 0.015(2) 0.036(2) -0.0192(17) O1W 0.0570(15) 0.0457(14) 0.0626(16) 0.0038(12) 0.0334(13) 0.0064(12) O2W 0.0664(17) 0.0619(17) 0.0678(17) 0.0115(13) 0.0409(15) 0.0030(13) O3W 0.0553(15) 0.0503(15) 0.0658(17) -0.0004(12) 0.0364(14) 0.0050(12) O4W 0.0655(17) 0.0594(17) 0.0659(17) 0.0068(13) 0.0385(14) -0.0028(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.314(4) . ? C1 C6 1.403(5) . ? C1 C2 1.420(5) . ? C2 O3 1.362(4) . ? C2 C3 1.382(5) . ? C3 C4 1.391(5) . ? C3 H3 0.9300 . ? C4 C5 1.349(5) . ? C4 H4 0.9300 . ? C5 C6 1.417(5) . ? C5 H5 0.9300 . ? C6 C7 1.431(5) . ? C7 N1 1.280(4) . ? C7 H6 0.9300 . ? C8 N1 1.468(4) . ? C8 C9 1.512(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.469(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.273(4) . ? C10 C11 1.430(5) . ? C10 H10 0.9300 . ? C11 C16 1.409(5) . ? C11 C12 1.410(5) . ? C12 C13 1.356(5) . ? C12 H12 0.9300 . ? C13 C14 1.389(6) . ? C13 H13 0.9300 . ? C14 C15 1.374(5) . ? C14 H14 0.9300 . ? C15 O4 1.381(4) . ? C15 C16 1.412(4) . ? C16 O2 1.331(4) . ? C17 O3 1.415(4) . ? C17 C18 1.477(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O4 1.416(4) . ? C19 C20 1.485(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20B 0.9600 . ? C20 H20A 0.9600 . ? C20 H20C 0.9600 . ? C21 O5 1.317(4) . ? C21 C26 1.406(5) . ? C21 C22 1.419(5) . ? C22 O7 1.369(4) . ? C22 C23 1.372(5) . ? C23 C24 1.382(6) . ? C23 H23 0.9300 . ? C24 C25 1.352(6) . ? C24 H24 0.9300 . ? C25 C26 1.409(5) . ? C25 H25 0.9300 . ? C26 C27 1.450(5) . ? C27 N3 1.269(4) . ? C27 H27 0.9300 . ? C28 N3 1.472(4) . ? C28 C29 1.505(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N4 1.468(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N4 1.282(5) . ? C30 C31 1.430(5) . ? C30 H30 0.9300 . ? C31 C36 1.406(5) . ? C31 C32 1.418(5) . ? C32 C33 1.350(7) . ? C32 H32 0.9300 . ? C33 C34 1.384(7) . ? C33 H33 0.9300 . ? C34 C35 1.382(6) . ? C34 H34 0.9300 . ? C35 O8 1.375(5) . ? C35 C36 1.415(5) . ? C36 O6 1.308(4) . ? C37 O7 1.418(4) . ? C37 C38 1.499(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 O8 1.417(5) . ? C39 C40 1.491(7) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 O9 1.317(4) . ? C41 C46 1.412(5) . ? C41 C42 1.422(5) . ? C42 O11 1.365(4) . ? C42 C43 1.381(5) . ? C43 C44 1.379(6) . ? C43 H43 0.9300 . ? C44 C45 1.355(6) . ? C44 H44 0.9300 . ? C45 C46 1.412(5) . ? C45 H45 0.9300 . ? C46 C47 1.423(5) . ? C47 N5 1.281(4) . ? C47 H47 0.9300 . ? C48 N5 1.474(4) . ? C48 C49 1.510(5) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 N6 1.462(4) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 N6 1.276(4) . ? C50 C51 1.427(5) . ? C50 H50 0.9300 . ? C51 C52 1.402(5) . ? C51 C56 1.414(5) . ? C52 C53 1.350(5) . ? C52 H52 0.9300 . ? C53 C54 1.395(6) . ? C53 H53 0.9300 . ? C54 C55 1.377(5) . ? C54 H54 0.9300 . ? C55 O12 1.376(4) . ? C55 C56 1.412(4) . ? C56 O10 1.325(4) . ? C57 O11 1.419(4) . ? C57 C58 1.481(6) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 O12 1.416(4) . ? C59 C60 1.496(6) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 O13 1.324(4) . ? C61 C66 1.409(5) . ? C61 C62 1.416(5) . ? C62 O15 1.365(5) . ? C62 C63 1.377(5) . ? C63 C64 1.389(6) . ? C63 H63 0.9300 . ? C64 C65 1.358(6) . ? C64 H64 0.9300 . ? C65 C66 1.412(5) . ? C65 H65 0.9300 . ? C66 C67 1.446(6) . ? C67 N7 1.272(5) . ? C67 H67 0.9300 . ? C68 N7 1.475(5) . ? C68 C69 1.497(6) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 N8 1.469(5) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 N8 1.278(5) . ? C70 C71 1.429(6) . ? C70 H70 0.9300 . ? C71 C76 1.406(5) . ? C71 C72 1.427(5) . ? C72 C73 1.335(6) . ? C72 H72 0.9300 . ? C73 C74 1.402(7) . ? C73 H73 0.9300 . ? C74 C75 1.380(5) . ? C74 H74 0.9300 . ? C75 O16 1.366(5) . ? C75 C76 1.420(5) . ? C76 O14 1.323(4) . ? C77 O15 1.419(4) . ? C77 C78 1.493(6) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 O16 1.420(5) . ? C79 C80 1.496(7) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? Cl1 O18 1.403(3) . ? Cl1 O20 1.407(3) . ? Cl1 O17 1.412(3) . ? Cl1 O19 1.454(4) . ? Cl2 O24 1.400(6) . ? Cl2 O22 1.418(5) . ? Cl2 O23 1.421(6) . ? Cl2 O21 1.448(11) . ? Cl2' O24' 1.396(9) . ? Cl2' O22' 1.413(9) . ? Cl2' O23' 1.418(9) . ? Cl2' O21' 1.431(17) . ? Cu1 O1 1.914(2) . ? Cu1 N2 1.931(3) . ? Cu1 O2 1.941(2) . ? Cu1 N1 1.947(3) . ? Cu2 O6 1.902(2) . ? Cu2 O5 1.924(2) . ? Cu2 N3 1.930(3) . ? Cu2 N4 1.938(3) . ? Cu3 O9 1.920(2) . ? Cu3 O10 1.931(2) . ? Cu3 N6 1.937(3) . ? Cu3 N5 1.940(3) . ? Cu4 O14 1.903(2) . ? Cu4 N7 1.933(3) . ? Cu4 O13 1.934(2) . ? Cu4 N8 1.941(3) . ? O1W H1WB 0.8021 . ? O1W H1WC 1.1327 . ? O1W H1WA 0.7957 . ? O2W H1WC 1.3514 . ? O2W H2WB 0.7990 . ? O2W H2WA 0.8051 . ? O3W H3WB 0.7921 . ? O3W H3WA 0.8007 . ? O3W H3WC 1.0189 . ? O4W H3WC 1.4455 . ? O4W H4WA 0.8011 . ? O4W H4WB 0.7992 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C6 125.1(3) . . ? O1 C1 C2 117.5(3) . . ? C6 C1 C2 117.3(3) . . ? O3 C2 C3 125.3(3) . . ? O3 C2 C1 113.5(3) . . ? C3 C2 C1 121.2(3) . . ? C2 C3 C4 120.3(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.8(4) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.5(4) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C1 C6 C5 119.8(3) . . ? C1 C6 C7 122.7(3) . . ? C5 C6 C7 117.4(3) . . ? N1 C7 C6 125.4(3) . . ? N1 C7 H6 117.3 . . ? C6 C7 H6 117.3 . . ? N1 C8 C9 107.7(3) . . ? N1 C8 H8A 110.2 . . ? C9 C8 H8A 110.2 . . ? N1 C8 H8B 110.2 . . ? C9 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? N2 C9 C8 107.9(3) . . ? N2 C9 H9A 110.1 . . ? C8 C9 H9A 110.1 . . ? N2 C9 H9B 110.1 . . ? C8 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? N2 C10 C11 125.9(3) . . ? N2 C10 H10 117.1 . . ? C11 C10 H10 117.1 . . ? C16 C11 C12 119.8(3) . . ? C16 C11 C10 123.1(3) . . ? C12 C11 C10 117.1(4) . . ? C13 C12 C11 121.1(4) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 120.0(4) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.3(4) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 O4 124.7(3) . . ? C14 C15 C16 121.4(4) . . ? O4 C15 C16 113.9(3) . . ? O2 C16 C11 124.2(3) . . ? O2 C16 C15 118.4(3) . . ? C11 C16 C15 117.4(3) . . ? O3 C17 C18 108.5(4) . . ? O3 C17 H17A 110.0 . . ? C18 C17 H17A 110.0 . . ? O3 C17 H17B 110.0 . . ? C18 C17 H17B 110.0 . . ? H17A C17 H17B 108.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 C20 108.9(3) . . ? O4 C19 H19A 109.9 . . ? C20 C19 H19A 109.9 . . ? O4 C19 H19B 109.9 . . ? C20 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20A 109.5 . . ? H20B C20 H20A 109.5 . . ? C19 C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? O5 C21 C26 125.0(3) . . ? O5 C21 C22 117.9(3) . . ? C26 C21 C22 117.1(3) . . ? O7 C22 C23 125.4(4) . . ? O7 C22 C21 113.5(3) . . ? C23 C22 C21 121.1(4) . . ? C22 C23 C24 120.6(4) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 120.2(4) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.8(4) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C21 C26 C25 120.2(4) . . ? C21 C26 C27 122.0(3) . . ? C25 C26 C27 117.8(4) . . ? N3 C27 C26 125.3(3) . . ? N3 C27 H27 117.4 . . ? C26 C27 H27 117.4 . . ? N3 C28 C29 108.0(3) . . ? N3 C28 H28A 110.1 . . ? C29 C28 H28A 110.1 . . ? N3 C28 H28B 110.1 . . ? C29 C28 H28B 110.1 . . ? H28A C28 H28B 108.4 . . ? N4 C29 C28 107.9(3) . . ? N4 C29 H29A 110.1 . . ? C28 C29 H29A 110.1 . . ? N4 C29 H29B 110.1 . . ? C28 C29 H29B 110.1 . . ? H29A C29 H29B 108.4 . . ? N4 C30 C31 125.8(4) . . ? N4 C30 H30 117.1 . . ? C31 C30 H30 117.1 . . ? C36 C31 C32 119.9(4) . . ? C36 C31 C30 122.7(3) . . ? C32 C31 C30 117.5(4) . . ? C33 C32 C31 121.5(5) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C32 C33 C34 119.8(5) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C35 C34 C33 120.3(5) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? O8 C35 C34 124.7(4) . . ? O8 C35 C36 113.6(3) . . ? C34 C35 C36 121.7(5) . . ? O6 C36 C31 124.7(4) . . ? O6 C36 C35 118.4(4) . . ? C31 C36 C35 116.9(4) . . ? O7 C37 C38 108.3(3) . . ? O7 C37 H37A 110.0 . . ? C38 C37 H37A 110.0 . . ? O7 C37 H37B 110.0 . . ? C38 C37 H37B 110.0 . . ? H37A C37 H37B 108.4 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O8 C39 C40 107.6(4) . . ? O8 C39 H39A 110.2 . . ? C40 C39 H39A 110.2 . . ? O8 C39 H39B 110.2 . . ? C40 C39 H39B 110.2 . . ? H39A C39 H39B 108.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O9 C41 C46 124.5(3) . . ? O9 C41 C42 118.5(3) . . ? C46 C41 C42 117.1(3) . . ? O11 C42 C43 125.5(4) . . ? O11 C42 C41 113.1(3) . . ? C43 C42 C41 121.3(4) . . ? C44 C43 C42 120.4(4) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C45 C44 C43 120.2(4) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 121.3(4) . . ? C44 C45 H45 119.3 . . ? C46 C45 H45 119.3 . . ? C45 C46 C41 119.7(4) . . ? C45 C46 C47 117.6(4) . . ? C41 C46 C47 122.7(3) . . ? N5 C47 C46 126.0(3) . . ? N5 C47 H47 117.0 . . ? C46 C47 H47 117.0 . . ? N5 C48 C49 107.9(3) . . ? N5 C48 H48A 110.1 . . ? C49 C48 H48A 110.1 . . ? N5 C48 H48B 110.1 . . ? C49 C48 H48B 110.1 . . ? H48A C48 H48B 108.4 . . ? N6 C49 C48 108.1(3) . . ? N6 C49 H49A 110.1 . . ? C48 C49 H49A 110.1 . . ? N6 C49 H49B 110.1 . . ? C48 C49 H49B 110.1 . . ? H49A C49 H49B 108.4 . . ? N6 C50 C51 125.7(3) . . ? N6 C50 H50 117.1 . . ? C51 C50 H50 117.1 . . ? C52 C51 C56 119.9(3) . . ? C52 C51 C50 117.4(3) . . ? C56 C51 C50 122.7(3) . . ? C53 C52 C51 121.7(4) . . ? C53 C52 H52 119.1 . . ? C51 C52 H52 119.1 . . ? C52 C53 C54 119.5(4) . . ? C52 C53 H53 120.2 . . ? C54 C53 H53 120.2 . . ? C55 C54 C53 120.3(4) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? O12 C55 C54 124.9(3) . . ? O12 C55 C56 113.7(3) . . ? C54 C55 C56 121.4(4) . . ? O10 C56 C55 118.3(3) . . ? O10 C56 C51 124.6(3) . . ? C55 C56 C51 117.1(3) . . ? O11 C57 C58 107.3(4) . . ? O11 C57 H57A 110.3 . . ? C58 C57 H57A 110.3 . . ? O11 C57 H57B 110.3 . . ? C58 C57 H57B 110.3 . . ? H57A C57 H57B 108.5 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O12 C59 C60 107.8(3) . . ? O12 C59 H59A 110.2 . . ? C60 C59 H59A 110.2 . . ? O12 C59 H59B 110.2 . . ? C60 C59 H59B 110.2 . . ? H59A C59 H59B 108.5 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O13 C61 C66 124.1(4) . . ? O13 C61 C62 117.8(3) . . ? C66 C61 C62 118.0(4) . . ? O15 C62 C63 125.0(4) . . ? O15 C62 C61 114.3(3) . . ? C63 C62 C61 120.7(4) . . ? C62 C63 C64 120.4(4) . . ? C62 C63 H63 119.8 . . ? C64 C63 H63 119.8 . . ? C65 C64 C63 120.4(4) . . ? C65 C64 H64 119.8 . . ? C63 C64 H64 119.8 . . ? C64 C65 C66 120.7(5) . . ? C64 C65 H65 119.7 . . ? C66 C65 H65 119.7 . . ? C61 C66 C65 119.7(4) . . ? C61 C66 C67 123.1(4) . . ? C65 C66 C67 117.2(4) . . ? N7 C67 C66 125.0(4) . . ? N7 C67 H67 117.5 . . ? C66 C67 H67 117.5 . . ? N7 C68 C69 107.7(4) . . ? N7 C68 H68A 110.2 . . ? C69 C68 H68A 110.2 . . ? N7 C68 H68B 110.2 . . ? C69 C68 H68B 110.2 . . ? H68A C68 H68B 108.5 . . ? N8 C69 C68 108.1(3) . . ? N8 C69 H69A 110.1 . . ? C68 C69 H69A 110.1 . . ? N8 C69 H69B 110.1 . . ? C68 C69 H69B 110.1 . . ? H69A C69 H69B 108.4 . . ? N8 C70 C71 126.0(4) . . ? N8 C70 H70 117.0 . . ? C71 C70 H70 117.0 . . ? C76 C71 C72 119.3(4) . . ? C76 C71 C70 122.7(4) . . ? C72 C71 C70 118.0(4) . . ? C73 C72 C71 121.7(5) . . ? C73 C72 H72 119.1 . . ? C71 C72 H72 119.1 . . ? C72 C73 C74 120.3(4) . . ? C72 C73 H73 119.8 . . ? C74 C73 H73 119.8 . . ? C75 C74 C73 119.5(5) . . ? C75 C74 H74 120.2 . . ? C73 C74 H74 120.2 . . ? O16 C75 C74 124.8(4) . . ? O16 C75 C76 113.4(3) . . ? C74 C75 C76 121.8(4) . . ? O14 C76 C71 124.5(4) . . ? O14 C76 C75 118.2(4) . . ? C71 C76 C75 117.3(4) . . ? O15 C77 C78 108.2(3) . . ? O15 C77 H77A 110.1 . . ? C78 C77 H77A 110.1 . . ? O15 C77 H77B 110.1 . . ? C78 C77 H77B 110.1 . . ? H77A C77 H77B 108.4 . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? O16 C79 C80 108.2(4) . . ? O16 C79 H79A 110.1 . . ? C80 C79 H79A 110.1 . . ? O16 C79 H79B 110.1 . . ? C80 C79 H79B 110.1 . . ? H79A C79 H79B 108.4 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? O18 Cl1 O20 111.9(2) . . ? O18 Cl1 O17 111.3(2) . . ? O20 Cl1 O17 112.6(2) . . ? O18 Cl1 O19 108.9(2) . . ? O20 Cl1 O19 106.6(2) . . ? O17 Cl1 O19 105.0(2) . . ? O24 Cl2 O22 111.2(5) . . ? O24 Cl2 O23 111.0(6) . . ? O22 Cl2 O23 113.2(5) . . ? O24 Cl2 O21 110.2(5) . . ? O22 Cl2 O21 105.5(6) . . ? O23 Cl2 O21 105.4(5) . . ? O24' Cl2' O22' 111.6(12) . . ? O24' Cl2' O23' 109.2(12) . . ? O22' Cl2' O23' 112.9(12) . . ? O24' Cl2' O21' 111.0(12) . . ? O22' Cl2' O21' 105.7(13) . . ? O23' Cl2' O21' 106.3(12) . . ? O1 Cu1 N2 176.44(11) . . ? O1 Cu1 O2 91.10(9) . . ? N2 Cu1 O2 92.44(11) . . ? O1 Cu1 N1 92.48(11) . . ? N2 Cu1 N1 84.00(12) . . ? O2 Cu1 N1 175.41(11) . . ? O6 Cu2 O5 90.46(10) . . ? O6 Cu2 N3 176.95(12) . . ? O5 Cu2 N3 92.06(11) . . ? O6 Cu2 N4 92.95(12) . . ? O5 Cu2 N4 173.75(12) . . ? N3 Cu2 N4 84.69(13) . . ? O9 Cu3 O10 91.20(9) . . ? O9 Cu3 N6 176.65(11) . . ? O10 Cu3 N6 92.14(11) . . ? O9 Cu3 N5 92.49(11) . . ? O10 Cu3 N5 174.83(11) . . ? N6 Cu3 N5 84.17(12) . . ? O14 Cu4 N7 177.01(13) . . ? O14 Cu4 O13 90.75(10) . . ? N7 Cu4 O13 92.21(13) . . ? O14 Cu4 N8 92.91(13) . . ? N7 Cu4 N8 84.19(15) . . ? O13 Cu4 N8 172.94(12) . . ? C7 N1 C8 120.2(3) . . ? C7 N1 Cu1 126.5(2) . . ? C8 N1 Cu1 113.3(2) . . ? C10 N2 C9 120.3(3) . . ? C10 N2 Cu1 126.7(3) . . ? C9 N2 Cu1 112.9(2) . . ? C27 N3 C28 120.7(3) . . ? C27 N3 Cu2 127.7(3) . . ? C28 N3 Cu2 111.6(2) . . ? C30 N4 C29 121.0(3) . . ? C30 N4 Cu2 126.2(3) . . ? C29 N4 Cu2 112.8(2) . . ? C50 N6 C49 120.4(3) . . ? C50 N6 Cu3 126.9(2) . . ? C49 N6 Cu3 112.6(2) . . ? C47 N5 C48 120.3(3) . . ? C47 N5 Cu3 126.4(2) . . ? C48 N5 Cu3 113.3(2) . . ? C67 N7 C68 120.4(4) . . ? C67 N7 Cu4 127.5(3) . . ? C68 N7 Cu4 112.1(3) . . ? C70 N8 C69 120.7(4) . . ? C70 N8 Cu4 126.3(3) . . ? C69 N8 Cu4 112.9(3) . . ? C1 O1 Cu1 126.8(2) . . ? C16 O2 Cu1 125.7(2) . . ? C2 O3 C17 118.9(3) . . ? C15 O4 C19 118.0(3) . . ? C21 O5 Cu2 126.9(2) . . ? C36 O6 Cu2 127.5(2) . . ? C22 O7 C37 118.7(3) . . ? C35 O8 C39 118.5(4) . . ? C41 O9 Cu3 127.1(2) . . ? C56 O10 Cu3 126.3(2) . . ? C42 O11 C57 118.5(3) . . ? C55 O12 C59 117.7(3) . . ? C61 O13 Cu4 126.5(2) . . ? C76 O14 Cu4 127.3(2) . . ? C62 O15 C77 118.5(3) . . ? C75 O16 C79 118.4(3) . . ? H1WB O1W H1WC 94.7 . . ? H1WB O1W H1WA 109.4 . . ? H1WC O1W H1WA 106.9 . . ? H1WC O2W H2WB 89.1 . . ? H1WC O2W H2WA 108.9 . . ? H2WB O2W H2WA 110.6 . . ? H3WB O3W H3WA 114.9 . . ? H3WB O3W H3WC 106.7 . . ? H3WA O3W H3WC 108.2 . . ? H3WC O4W H4WA 110.9 . . ? H3WC O4W H4WB 105.0 . . ? H4WA O4W H4WB 94.7 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.72 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.493 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.060