# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # 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_Cu2 #TrackingRef '18432_web_deposit_cif_file_0_DrScottJ.Dalgarno_1362935644.Cu2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common MonoOxaCu2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C198 H268 Cu4 N8 O23' _chemical_formula_weight 3382.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.02(3) _cell_length_b 17.80(3) _cell_length_c 19.23(4) _cell_angle_alpha 113.17(4) _cell_angle_beta 95.82(4) _cell_angle_gamma 106.81(4) _cell_volume 4679(14) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used . _cell_measurement_theta_min . _cell_measurement_theta_max . _exptl_crystal_description Needle _exptl_crystal_colour Brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1812 _exptl_absorpt_coefficient_mu 0.514 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8822 _exptl_absorpt_correction_T_max 0.9361 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 100(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 X8 Apex II CCD Diffractometer' _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 42073 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.1299 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.02 _reflns_number_total 17952 _reflns_number_gt 10088 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure showed disor- der in one tert-butyl group, one dmf of crystallisation that was modelled over three positions, and one dmf / MeCN of crystallisation, both modell- ed at 50% each. The restraints applied are listed below. The dmf of crystallissation that is disordered over three positions was refined isotropically, while the anisotropic displacement parameters of the disordered dmf / MeCN were restrained. The reported and calculated formulae differ due to partial occupancies of the badly disordered dmf of crystallisation. DFIX 1.54 0.02 C83 C86 DFIX 1.54 0.02 C83 C84 DFIX 1.54 0.02 C83 C88 DFIX 1.54 0.02 C83 C89 DFIX 1.54 0.02 C83 C85 DFIX 1.54 0.02 C83 C87 SIMU 0.01 C83 C84 C85 C86 C87 C88 C89 DFIX 1.45 0.02 C155 N156 DFIX 1.45 0.02 N156 C159 DFIX 1.45 0.02 N156 C160 DFIX 1.45 0.02 N156 C157 DFIX 1.45 0.02 N156 C164 DFIX 1.45 0.02 N156 C165 DFIX 1.45 0.02 N156 C166 DFIX 1.2 0.02 C159 O163 DFIX 1.2 0.02 C160 O162 DFIX 1.2 0.02 C157 O161 DFIX 1.45 0.02 N171 C172 DFIX 1.45 0.02 N171 C173 DFIX 1.45 0.02 N171 C170 DFIX 1.2 0.02 O174 C173 DFIX 1.1 0.02 C176 N177 DFIX 1.54 0.02 C175 C176 DANG 2.3 0.02 C170 C173 DANG 2.3 0.02 C172 C173 DANG 2.3 0.02 C170 C172 EADP C170 N171 C172 C173 O174 C175 C176 N177 EADP C90 C91 C92 C93 DFIX 1.54 0.02 C92 C90 DFIX 1.54 0.02 C90 C93 DFIX 1.54 0.02 C90 C91 ; _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^)+(0.0993P)^2^+3.3537P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17952 _refine_ls_number_parameters 1084 _refine_ls_number_restraints 88 _refine_ls_R_factor_all 0.1487 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.2071 _refine_ls_wR_factor_gt 0.1734 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.05176(4) 0.02821(4) 0.07949(3) 0.02100(17) Uani 1 1 d . . . O1 O 0.0917(2) 0.2316(2) 0.10210(18) 0.0272(8) Uani 1 1 d . . . H1O H 0.0870 0.2007 0.1262 0.033 Uiso 1 1 calc R . . N1 N 0.0402(4) 0.6779(4) 0.9959(4) 0.0645(17) Uani 1 1 d . . . C1 C 0.1916(3) 0.3499(3) 0.2239(3) 0.0237(12) Uani 1 1 d . . . Cu2 Cu 0.04817(4) 0.07991(4) 0.49224(3) 0.02009(17) Uani 1 1 d . . . O2 O 0.0761(2) 0.1172(2) -0.04976(19) 0.0250(8) Uani 1 1 d . . . H2O H 0.0752 0.1572 -0.0082 0.030 Uiso 1 1 calc R . . C157 C 0.0218(10) 0.4068(9) 0.6919(8) 0.018(4) Uiso 0.33 1 d PD A 3 H157 H 0.0558 0.3901 0.7227 0.022 Uiso 0.33 1 calc PR A 3 N156 N -0.0424(4) 0.3451(4) 0.6283(4) 0.0764(19) Uiso 1 1 d D . . C2 C 0.2664(3) 0.4264(3) 0.2611(3) 0.0278(12) Uani 1 1 d . . . H2 H 0.2836 0.4545 0.3165 0.033 Uiso 1 1 calc R . . O3 O 0.0473(2) -0.0446(2) -0.02731(17) 0.0205(7) Uani 1 1 d . . . C3 C 0.3172(4) 0.4637(3) 0.2210(3) 0.0317(13) Uani 1 1 d . . . O4 O 0.1403(2) -0.0109(2) 0.11931(17) 0.0204(7) Uani 1 1 d . . . C4 C 0.2868(4) 0.4226(3) 0.1398(3) 0.0348(14) Uani 1 1 d . . . H4 H 0.3187 0.4479 0.1107 0.042 Uiso 1 1 calc R . . O5 O 0.0766(2) 0.1291(2) 0.17466(17) 0.0204(7) Uani 1 1 d . . . C5 C 0.2113(4) 0.3454(3) 0.0996(3) 0.0296(13) Uani 1 1 d . . . O6 O 0.1332(2) 0.1706(2) 0.68385(18) 0.0246(8) Uani 1 1 d . . . H6O H 0.1520 0.1733 0.6454 0.030 Uiso 1 1 calc R . . C6 C 0.1657(3) 0.3089(3) 0.1433(3) 0.0262(12) Uani 1 1 d . . . O7 O -0.0361(2) 0.0464(2) 0.64094(18) 0.0224(8) Uani 1 1 d . . . H7O H 0.0177 0.0810 0.6578 0.027 Uiso 1 1 calc R . . C7 C 0.1770(4) 0.3058(3) 0.0108(3) 0.0305(13) Uani 1 1 d . . . H7A H 0.1104 0.2824 -0.0019 0.037 Uiso 1 1 calc R . . H7B H 0.1954 0.3538 -0.0048 0.037 Uiso 1 1 calc R . . O8 O -0.0733(2) -0.00030(19) 0.46922(17) 0.0178(7) Uani 1 1 d . . . C8 C 0.2073(3) 0.2338(3) -0.0390(3) 0.0262(12) Uani 1 1 d . . . O9 O 0.0079(2) 0.1388(2) 0.43616(18) 0.0222(8) Uani 1 1 d . . . C9 C 0.2871(3) 0.2555(4) -0.0625(3) 0.0347(14) Uani 1 1 d . . . H9 H 0.3239 0.3156 -0.0419 0.042 Uiso 1 1 calc R . . O10 O 0.1576(2) 0.1745(2) 0.54972(18) 0.0239(8) Uani 1 1 d . . . C10 C 0.3150(3) 0.1941(4) -0.1140(3) 0.0366(15) Uani 1 1 d . . . C11 C 0.2595(3) 0.1054(4) -0.1446(3) 0.0318(13) Uani 1 1 d . . . H11 H 0.2763 0.0619 -0.1815 0.038 Uiso 1 1 calc R . . C12 C 0.1810(3) 0.0803(3) -0.1219(3) 0.0232(12) Uani 1 1 d . . . C13 C 0.1562(3) 0.1445(3) -0.0694(3) 0.0244(12) Uani 1 1 d . . . C14 C 0.1235(3) -0.0173(3) -0.1559(3) 0.0266(12) Uani 1 1 d . . . H14A H 0.0599 -0.0238 -0.1563 0.032 Uiso 1 1 calc R . . H14B H 0.1270 -0.0473 -0.2105 0.032 Uiso 1 1 calc R . . C15 C 0.1538(3) -0.0606(3) -0.1096(3) 0.0222(11) Uani 1 1 d . . . C16 C 0.2251(3) -0.0881(3) -0.1257(3) 0.0242(12) Uani 1 1 d . . . H16 H 0.2468 -0.0854 -0.1691 0.029 Uiso 1 1 calc R . . C17 C 0.2667(3) -0.1192(3) -0.0824(3) 0.0254(12) Uani 1 1 d . . . C159 C -0.056(2) 0.3367(17) 0.5480(11) 0.015(6) Uiso 0.17 1 d PD A 1 H159 H -0.0830 0.2813 0.5037 0.018 Uiso 0.17 1 calc PR A 1 C18 C 0.2323(3) -0.1246(3) -0.0208(3) 0.0238(12) Uani 1 1 d . . . H18 H 0.2595 -0.1452 0.0106 0.029 Uiso 1 1 calc R . . C19 C 0.1596(3) -0.1007(3) -0.0034(3) 0.0204(11) Uani 1 1 d . . . C20 C 0.1179(3) -0.0695(3) -0.0482(3) 0.0225(11) Uani 1 1 d . . . C21 C 0.1289(3) -0.1022(3) 0.0672(3) 0.0206(11) Uani 1 1 d . . . H21A H 0.0651 -0.1409 0.0523 0.025 Uiso 1 1 calc R . . H21B H 0.1656 -0.1240 0.0936 0.025 Uiso 1 1 calc R . . C22 C 0.1458(3) 0.0073(3) 0.2008(3) 0.0216(11) Uani 1 1 d . . . H22A H 0.1831 -0.0219 0.2164 0.026 Uiso 1 1 calc R . . H22B H 0.0849 -0.0154 0.2083 0.026 Uiso 1 1 calc R . . C23 C 0.1873(3) 0.1050(3) 0.2501(3) 0.0168(10) Uani 1 1 d . . . C24 C 0.2641(3) 0.1415(3) 0.3103(3) 0.0205(11) Uani 1 1 d . . . H24 H 0.2908 0.1037 0.3191 0.025 Uiso 1 1 calc R . . C25 C 0.3037(3) 0.2319(3) 0.3586(3) 0.0223(11) Uani 1 1 d . . . C26 C 0.2596(3) 0.2836(3) 0.3459(3) 0.0220(11) Uani 1 1 d . . . H26 H 0.2826 0.3446 0.3797 0.026 Uiso 1 1 calc R . . C27 C 0.1840(3) 0.2505(3) 0.2865(3) 0.0178(11) Uani 1 1 d . . . C28 C 0.1481(3) 0.1598(3) 0.2354(3) 0.0193(11) Uani 1 1 d . . . C29 C 0.1436(3) 0.3119(3) 0.2731(3) 0.0242(12) Uani 1 1 d . . . H29A H 0.1485 0.3600 0.3239 0.029 Uiso 1 1 calc R . . H29B H 0.0791 0.2798 0.2463 0.029 Uiso 1 1 calc R . . C30 C 0.4020(4) 0.5470(4) 0.2671(3) 0.0359(14) Uani 1 1 d . . . C31 C 0.4715(4) 0.5207(4) 0.3039(4) 0.0496(18) Uani 1 1 d . . . H31A H 0.5263 0.5723 0.3339 0.074 Uiso 1 1 calc R . . H31B H 0.4859 0.4761 0.2627 0.074 Uiso 1 1 calc R . . H31C H 0.4466 0.4970 0.3386 0.074 Uiso 1 1 calc R . . C32 C 0.3810(4) 0.6189(4) 0.3308(4) 0.0519(18) Uani 1 1 d . . . H32A H 0.3599 0.5983 0.3684 0.078 Uiso 1 1 calc R . . H32B H 0.3341 0.6328 0.3070 0.078 Uiso 1 1 calc R . . H32C H 0.4354 0.6715 0.3575 0.078 Uiso 1 1 calc R . . C33 C 0.4428(4) 0.5828(4) 0.2131(4) 0.0532(19) Uani 1 1 d . . . H33A H 0.4956 0.6363 0.2439 0.080 Uiso 1 1 calc R . . H33B H 0.3982 0.5961 0.1860 0.080 Uiso 1 1 calc R . . H33C H 0.4610 0.5389 0.1748 0.080 Uiso 1 1 calc R . . C34 C 0.4021(4) 0.2175(5) -0.1412(4) 0.0478(18) Uani 1 1 d . . . C35 C 0.4540(4) 0.3189(5) -0.1003(4) 0.075(3) Uani 1 1 d . . . H35A H 0.4637 0.3407 -0.0437 0.113 Uiso 1 1 calc R . . H35B H 0.4186 0.3475 -0.1180 0.113 Uiso 1 1 calc R . . H35C H 0.5122 0.3322 -0.1137 0.113 Uiso 1 1 calc R . . C36 C 0.3772(4) 0.1868(5) -0.2289(4) 0.0514(18) Uani 1 1 d . . . H36A H 0.4318 0.2033 -0.2467 0.077 Uiso 1 1 calc R . . H36B H 0.3367 0.2144 -0.2411 0.077 Uiso 1 1 calc R . . H36C H 0.3470 0.1230 -0.2553 0.077 Uiso 1 1 calc R . . C37 C 0.4615(4) 0.1727(6) -0.1201(6) 0.089(3) Uani 1 1 d . . . H37A H 0.4763 0.1932 -0.0635 0.134 Uiso 1 1 calc R . . H37B H 0.5171 0.1869 -0.1373 0.134 Uiso 1 1 calc R . . H37C H 0.4295 0.1091 -0.1460 0.134 Uiso 1 1 calc R . . C38 C 0.3494(4) -0.1433(4) -0.1020(3) 0.0345(14) Uani 1 1 d . . . C39 C 0.3921(4) -0.1657(4) -0.0415(4) 0.0408(15) Uani 1 1 d . . . H39A H 0.4091 -0.1160 0.0103 0.061 Uiso 1 1 calc R . . H39B H 0.4458 -0.1779 -0.0547 0.061 Uiso 1 1 calc R . . H39C H 0.3488 -0.2174 -0.0414 0.061 Uiso 1 1 calc R . . C155 C -0.0573(7) 0.2535(6) 0.6064(6) 0.115(3) Uiso 1 1 d D A . H15A H -0.0056 0.2489 0.6341 0.172 Uiso 1 1 calc R . . H15B H -0.0645 0.2225 0.5500 0.172 Uiso 1 1 calc R . . H15C H -0.1118 0.2274 0.6203 0.172 Uiso 1 1 calc R . . O161 O 0.0364(9) 0.4824(8) 0.7101(8) 0.056(4) Uiso 0.33 1 d PD A 3 C40 C 0.4202(4) -0.0631(4) -0.1018(4) 0.0469(17) Uani 1 1 d . . . H40A H 0.3959 -0.0500 -0.1428 0.070 Uiso 1 1 calc R . . H40B H 0.4746 -0.0759 -0.1115 0.070 Uiso 1 1 calc R . . H40C H 0.4351 -0.0124 -0.0510 0.070 Uiso 1 1 calc R . . C41 C 0.3217(5) -0.2234(4) -0.1826(3) 0.0561(19) Uani 1 1 d . . . H41A H 0.2766 -0.2735 -0.1817 0.084 Uiso 1 1 calc R . . H41B H 0.3746 -0.2380 -0.1947 0.084 Uiso 1 1 calc R . . H41C H 0.2964 -0.2095 -0.2226 0.084 Uiso 1 1 calc R . . C42 C 0.3938(3) 0.2719(3) 0.4196(3) 0.0296(13) Uani 1 1 d . . . C43 C 0.3930(4) 0.2264(4) 0.4702(4) 0.0553(19) Uani 1 1 d . . . H43A H 0.3420 0.2270 0.4943 0.083 Uiso 1 1 calc R . . H43B H 0.4492 0.2566 0.5110 0.083 Uiso 1 1 calc R . . H43C H 0.3873 0.1657 0.4385 0.083 Uiso 1 1 calc R . . C44 C 0.4193(4) 0.3704(4) 0.4717(4) 0.0550(19) Uani 1 1 d . . . H44A H 0.3742 0.3796 0.5017 0.082 Uiso 1 1 calc R . . H44B H 0.4218 0.4012 0.4390 0.082 Uiso 1 1 calc R . . H44C H 0.4783 0.3933 0.5077 0.082 Uiso 1 1 calc R . . C45 C 0.4678(4) 0.2627(5) 0.3744(4) 0.067(2) Uani 1 1 d . . . H45A H 0.5267 0.2909 0.4115 0.101 Uiso 1 1 calc R . . H45B H 0.4665 0.2910 0.3399 0.101 Uiso 1 1 calc R . . H45C H 0.4569 0.2005 0.3432 0.101 Uiso 1 1 calc R . . C46 C 0.2256(3) 0.3262(3) 0.7468(3) 0.0253(12) Uani 1 1 d . . . C47 C 0.2421(3) 0.4089(3) 0.8077(3) 0.0260(12) Uani 1 1 d . . . H47 H 0.2898 0.4575 0.8109 0.031 Uiso 1 1 calc R . . C48 C 0.1927(3) 0.4235(3) 0.8635(3) 0.0219(11) Uani 1 1 d . . . C49 C 0.1251(3) 0.3502(3) 0.8582(3) 0.0213(11) Uani 1 1 d . . . H49 H 0.0902 0.3577 0.8958 0.026 Uiso 1 1 calc R . . C160 C -0.0911(19) 0.4054(16) 0.6346(18) 0.020(7) Uiso 0.17 1 d PD A 2 H160 H -0.1530 0.3775 0.6083 0.024 Uiso 0.17 1 calc PR A 2 C50 C 0.1068(3) 0.2650(3) 0.7989(3) 0.0197(11) Uani 1 1 d . . . C51 C 0.1554(3) 0.2546(3) 0.7427(3) 0.0199(11) Uani 1 1 d . . . C52 C 0.0368(3) 0.1872(3) 0.8000(3) 0.0202(11) Uani 1 1 d . . . H52A H 0.0572 0.1368 0.7810 0.024 Uiso 1 1 calc R . . H52B H 0.0338 0.2016 0.8547 0.024 Uiso 1 1 calc R . . C53 C -0.0571(3) 0.1591(3) 0.7517(3) 0.0176(10) Uani 1 1 d . . . C54 C -0.1139(3) 0.2010(3) 0.7845(3) 0.0208(11) Uani 1 1 d . . . H54 H -0.0913 0.2492 0.8350 0.025 Uiso 1 1 calc R . . C55 C -0.2039(3) 0.1744(3) 0.7456(3) 0.0208(11) Uani 1 1 d . . . C56 C -0.2345(3) 0.1016(3) 0.6726(3) 0.0210(11) Uani 1 1 d . . . H56 H -0.2959 0.0805 0.6461 0.025 Uiso 1 1 calc R . . C57 C -0.1797(3) 0.0583(3) 0.6367(3) 0.0185(11) Uani 1 1 d . . . C58 C -0.0903(3) 0.0893(3) 0.6767(3) 0.0171(10) Uani 1 1 d . . . C59 C -0.2179(3) -0.0198(3) 0.5557(3) 0.0205(11) Uani 1 1 d . . . H59A H -0.1815 -0.0576 0.5488 0.025 Uiso 1 1 calc R . . H59B H -0.2802 -0.0550 0.5518 0.025 Uiso 1 1 calc R . . C60 C -0.2179(3) 0.0091(3) 0.4915(3) 0.0204(11) Uani 1 1 d . . . N171 N 0.4002(14) 0.2364(14) 0.1330(11) 0.163(4) Uani 0.50 1 d PD B 1 C61 C -0.2897(3) 0.0312(3) 0.4718(3) 0.0283(12) Uani 1 1 d . . . H61 H -0.3389 0.0207 0.4948 0.034 Uiso 1 1 calc R . . C62 C -0.2939(4) 0.0681(4) 0.4201(3) 0.0333(13) Uani 1 1 d . C . C63 C -0.2211(4) 0.0823(3) 0.3878(3) 0.0276(12) Uani 1 1 d . . . H63 H -0.2204 0.1092 0.3537 0.033 Uiso 1 1 calc R . . C64 C -0.1491(3) 0.0584(3) 0.4035(3) 0.0226(11) Uani 1 1 d . . . C65 C -0.1476(3) 0.0200(3) 0.4550(3) 0.0199(11) Uani 1 1 d . . . C66 C -0.0709(3) 0.0806(3) 0.3702(3) 0.0255(12) Uani 1 1 d . . . H66A H -0.0611 0.0267 0.3368 0.031 Uiso 1 1 calc R . . H66B H -0.0818 0.1104 0.3382 0.031 Uiso 1 1 calc R . . C67 C 0.0810(3) 0.1908(3) 0.4164(3) 0.0266(12) Uani 1 1 d . . . H67A H 0.0566 0.2108 0.3803 0.032 Uiso 1 1 calc R . . H67B H 0.1158 0.1551 0.3902 0.032 Uiso 1 1 calc R . . C172 C 0.3111(14) 0.1843(16) 0.1038(14) 0.163(4) Uani 0.50 1 d PD B 1 H17A H 0.2921 0.1566 0.1374 0.244 Uiso 0.50 1 calc PR B 1 H17B H 0.3021 0.1390 0.0510 0.244 Uiso 0.50 1 calc PR B 1 H17C H 0.2753 0.2202 0.1021 0.244 Uiso 0.50 1 calc PR B 1 C68 C 0.1412(4) 0.2690(3) 0.4909(3) 0.0268(12) Uani 1 1 d . . . C94 C -0.0567(6) 0.5442(6) 0.8598(5) 0.088(3) Uani 1 1 d . . . H94A H -0.0514 0.4919 0.8627 0.132 Uiso 1 1 calc R . . H94B H -0.0379 0.5475 0.8138 0.132 Uiso 1 1 calc R . . H94C H -0.1193 0.5406 0.8556 0.132 Uiso 1 1 calc R . . C69 C 0.1596(4) 0.3539(3) 0.4988(3) 0.0369(15) Uani 1 1 d . . . H69 H 0.1317 0.3614 0.4573 0.044 Uiso 1 1 calc R . . C70 C 0.2168(5) 0.4279(4) 0.5645(3) 0.0453(17) Uani 1 1 d . . . C71 C 0.2558(4) 0.4128(3) 0.6228(3) 0.0389(15) Uani 1 1 d . . . H71 H 0.2970 0.4616 0.6679 0.047 Uiso 1 1 calc R . . C72 C 0.2378(4) 0.3289(3) 0.6187(3) 0.0271(12) Uani 1 1 d . . . C73 C 0.1777(3) 0.2562(3) 0.5528(3) 0.0251(12) Uani 1 1 d . . . C96 C 0.0805(6) 0.6839(6) 0.7741(6) 0.095(3) Uani 1 1 d . . . H96A H 0.0787 0.7274 0.8243 0.142 Uiso 1 1 calc R . . H96B H 0.1319 0.6661 0.7815 0.142 Uiso 1 1 calc R . . H96C H 0.0247 0.6326 0.7533 0.142 Uiso 1 1 calc R . . C74 C 0.2795(3) 0.3179(3) 0.6862(3) 0.0280(12) Uani 1 1 d . . . H74A H 0.3407 0.3628 0.7109 0.034 Uiso 1 1 calc R . . H74B H 0.2851 0.2596 0.6662 0.034 Uiso 1 1 calc R . . N2 N 0.0971(5) 0.7578(4) 0.6786(4) 0.071(2) Uani 1 1 d . . . C75 C 0.2143(4) 0.5170(3) 0.9275(3) 0.0317(13) Uani 1 1 d . . . C76 C 0.2086(4) 0.5779(4) 0.8899(3) 0.0430(15) Uani 1 1 d . . . H76A H 0.2535 0.5805 0.8591 0.065 Uiso 1 1 calc R . . H76B H 0.2202 0.6368 0.9308 0.065 Uiso 1 1 calc R . . H76C H 0.1484 0.5552 0.8558 0.065 Uiso 1 1 calc R . . C77 C 0.3086(4) 0.5514(4) 0.9790(3) 0.0482(17) Uani 1 1 d . . . H77A H 0.3130 0.5115 1.0015 0.072 Uiso 1 1 calc R . . H77B H 0.3207 0.6097 1.0210 0.072 Uiso 1 1 calc R . . H77C H 0.3527 0.5550 0.9476 0.072 Uiso 1 1 calc R . . C95 C 0.0063(8) 0.6297(8) 0.9367(6) 0.116(4) Uani 1 1 d . . . C78 C 0.1475(4) 0.5197(4) 0.9789(3) 0.0430(16) Uani 1 1 d . . . H78A H 0.0861 0.4939 0.9462 0.065 Uiso 1 1 calc R . . H78B H 0.1596 0.5806 1.0157 0.065 Uiso 1 1 calc R . . H78C H 0.1540 0.4863 1.0080 0.065 Uiso 1 1 calc R . . C79 C -0.2622(3) 0.2253(3) 0.7828(3) 0.0267(12) Uani 1 1 d . . . C80 C -0.2163(4) 0.3234(3) 0.8027(3) 0.0323(13) Uani 1 1 d . . . H80A H -0.1567 0.3469 0.8378 0.048 Uiso 1 1 calc R . . H80B H -0.2531 0.3561 0.8282 0.048 Uiso 1 1 calc R . . H80C H -0.2102 0.3290 0.7546 0.048 Uiso 1 1 calc R . . C81 C -0.2724(4) 0.2189(4) 0.8593(3) 0.0324(13) Uani 1 1 d . . . H81A H -0.3023 0.1575 0.8479 0.049 Uiso 1 1 calc R . . H81B H -0.3086 0.2529 0.8841 0.049 Uiso 1 1 calc R . . H81C H -0.2129 0.2423 0.8945 0.049 Uiso 1 1 calc R . . C82 C -0.3554(4) 0.1911(4) 0.7298(3) 0.0366(14) Uani 1 1 d . . . H82A H -0.3499 0.1944 0.6807 0.055 Uiso 1 1 calc R . . H82B H -0.3897 0.2268 0.7556 0.055 Uiso 1 1 calc R . . H82C H -0.3868 0.1300 0.7190 0.055 Uiso 1 1 calc R . . C83 C -0.3722(4) 0.0973(4) 0.4046(3) 0.0436(15) Uani 1 1 d DU . . C84 C -0.3386(9) 0.1931(8) 0.4356(10) 0.059(4) Uani 0.50 1 d PDU C 1 H84A H -0.3884 0.2121 0.4257 0.088 Uiso 0.50 1 calc PR C 1 H84B H -0.2923 0.2115 0.4100 0.088 Uiso 0.50 1 calc PR C 1 H84C H -0.3128 0.2199 0.4920 0.088 Uiso 0.50 1 calc PR C 1 C85 C -0.3636(11) 0.1797(10) 0.4816(8) 0.069(4) Uani 0.50 1 d PDU C 2 H85A H -0.3052 0.2261 0.4950 0.103 Uiso 0.50 1 calc PR C 2 H85B H -0.3685 0.1631 0.5243 0.103 Uiso 0.50 1 calc PR C 2 H85C H -0.4118 0.2011 0.4733 0.103 Uiso 0.50 1 calc PR C 2 C86 C -0.4511(9) 0.0634(10) 0.4389(9) 0.053(4) Uani 0.50 1 d PDU C 1 H86A H -0.4684 -0.0001 0.4201 0.079 Uiso 0.50 1 calc PR C 1 H86B H -0.5028 0.0765 0.4222 0.079 Uiso 0.50 1 calc PR C 1 H86C H -0.4318 0.0924 0.4960 0.079 Uiso 0.50 1 calc PR C 1 C87 C -0.4580(8) 0.0295(10) 0.3848(12) 0.077(5) Uani 0.50 1 d PDU C 2 H87A H -0.5061 0.0506 0.3753 0.115 Uiso 0.50 1 calc PR C 2 H87B H -0.4637 0.0137 0.4280 0.115 Uiso 0.50 1 calc PR C 2 H87C H -0.4629 -0.0221 0.3377 0.115 Uiso 0.50 1 calc PR C 2 C88 C -0.4137(8) 0.0509(8) 0.3142(6) 0.041(3) Uani 0.50 1 d PDU C 1 H88A H -0.4375 -0.0127 0.2959 0.061 Uiso 0.50 1 calc PR C 1 H88B H -0.3671 0.0662 0.2877 0.061 Uiso 0.50 1 calc PR C 1 H88C H -0.4625 0.0703 0.3026 0.061 Uiso 0.50 1 calc PR C 1 C89 C -0.3578(10) 0.1405(11) 0.3485(9) 0.066(4) Uani 0.50 1 d PDU C 2 H89A H -0.2983 0.1869 0.3683 0.100 Uiso 0.50 1 calc PR C 2 H89B H -0.4042 0.1655 0.3451 0.100 Uiso 0.50 1 calc PR C 2 H89C H -0.3619 0.0961 0.2966 0.100 Uiso 0.50 1 calc PR C 2 C97 C 0.0900(6) 0.7240(6) 0.7164(6) 0.084(3) Uani 1 1 d . . . C90 C 0.2338(7) 0.5196(5) 0.5719(4) 0.0936(17) Uani 1 1 d D . . C91 C 0.1414(7) 0.5338(5) 0.5640(5) 0.0936(17) Uani 1 1 d D . . H91A H 0.1166 0.5329 0.6083 0.140 Uiso 1 1 calc R . . H91B H 0.0993 0.4869 0.5153 0.140 Uiso 1 1 calc R . . H91C H 0.1510 0.5905 0.5635 0.140 Uiso 1 1 calc R . . C92 C 0.2672(7) 0.5290(5) 0.5036(4) 0.0936(17) Uani 1 1 d D . . H92A H 0.2764 0.5881 0.5091 0.140 Uiso 1 1 calc R . . H92B H 0.2226 0.4858 0.4548 0.140 Uiso 1 1 calc R . . H92C H 0.3243 0.5190 0.5027 0.140 Uiso 1 1 calc R . . C93 C 0.2931(7) 0.5908(4) 0.6454(4) 0.0936(17) Uani 1 1 d D . . H93A H 0.3533 0.5877 0.6503 0.140 Uiso 1 1 calc R . . H93B H 0.2693 0.5854 0.6890 0.140 Uiso 1 1 calc R . . H93C H 0.2963 0.6471 0.6465 0.140 Uiso 1 1 calc R . . O174 O 0.5125(13) 0.3561(13) 0.1424(10) 0.163(4) Uani 0.50 1 d PD B 1 C173 C 0.4480(15) 0.2920(16) 0.1087(14) 0.163(4) Uani 0.50 1 d PD B 1 H173 H 0.4264 0.2775 0.0555 0.195 Uiso 0.50 1 calc PR B 1 O162 O -0.0654(14) 0.4842(13) 0.6674(12) 0.114(7) Uiso 0.33 1 d PD A 2 C170 C 0.4228(16) 0.2660(17) 0.2127(10) 0.163(4) Uani 0.50 1 d PD B 1 H17D H 0.3826 0.2240 0.2268 0.244 Uiso 0.50 1 calc PR B 1 H17E H 0.4166 0.3231 0.2385 0.244 Uiso 0.50 1 calc PR B 1 H17F H 0.4851 0.2718 0.2295 0.244 Uiso 0.50 1 calc PR B 1 O163 O -0.031(2) 0.4042(17) 0.5417(17) 0.175(11) Uiso 0.33 1 d PD A 1 C164 C 0.0412(11) 0.3911(12) 0.6799(10) 0.031(5) Uiso 0.33 1 d PD A 1 H16A H 0.0550 0.4541 0.6976 0.047 Uiso 0.33 1 calc PR A 1 H16B H 0.0868 0.3741 0.6538 0.047 Uiso 0.33 1 calc PR A 1 H16C H 0.0412 0.3780 0.7248 0.047 Uiso 0.33 1 calc PR A 1 C165 C -0.087(2) 0.356(2) 0.5669(17) 0.024(7) Uiso 0.17 1 d PD A 3 H16D H -0.1424 0.3049 0.5368 0.036 Uiso 0.17 1 calc PR A 3 H16E H -0.0478 0.3628 0.5324 0.036 Uiso 0.17 1 calc PR A 3 H16F H -0.1030 0.4088 0.5893 0.036 Uiso 0.17 1 calc PR A 3 C166 C -0.113(2) 0.371(3) 0.605(3) 0.057(13) Uiso 0.17 1 d PD A 4 H16G H -0.0906 0.4347 0.6246 0.085 Uiso 0.17 1 calc PR A 4 H16H H -0.1639 0.3524 0.6257 0.085 Uiso 0.17 1 calc PR A 4 H16I H -0.1317 0.3433 0.5476 0.085 Uiso 0.17 1 calc PR A 4 C175 C 0.3652(17) 0.0571(17) 0.1587(14) 0.163(4) Uani 0.50 1 d PD D 2 H17G H 0.4303 0.0731 0.1747 0.244 Uiso 0.50 1 calc PR D 2 H17H H 0.3377 -0.0050 0.1214 0.244 Uiso 0.50 1 calc PR D 2 H17I H 0.3401 0.0676 0.2046 0.244 Uiso 0.50 1 calc PR D 2 C176 C 0.345(2) 0.1132(19) 0.1201(15) 0.163(4) Uani 0.50 1 d PD D 2 N177 N 0.3180(16) 0.1339(17) 0.0753(13) 0.163(4) Uani 0.50 1 d PD D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0212(3) 0.0260(4) 0.0122(3) 0.0079(3) 0.0008(2) 0.0054(3) O1 0.028(2) 0.0242(19) 0.0197(19) 0.0121(16) -0.0026(16) -0.0039(16) N1 0.055(4) 0.054(4) 0.062(4) 0.004(3) -0.002(3) 0.026(3) C1 0.026(3) 0.015(3) 0.023(3) 0.007(2) -0.003(2) 0.004(2) Cu2 0.0247(3) 0.0197(3) 0.0186(3) 0.0114(3) 0.0049(3) 0.0077(3) O2 0.0205(18) 0.030(2) 0.0201(19) 0.0120(16) 0.0058(15) 0.0015(16) C2 0.029(3) 0.023(3) 0.026(3) 0.013(2) -0.005(2) 0.003(2) O3 0.0183(18) 0.0262(19) 0.0143(17) 0.0102(15) 0.0022(14) 0.0033(15) C3 0.030(3) 0.027(3) 0.032(3) 0.018(3) -0.006(3) 0.000(2) O4 0.0288(19) 0.0185(18) 0.0106(16) 0.0062(14) 0.0031(14) 0.0050(15) C4 0.032(3) 0.030(3) 0.035(3) 0.023(3) -0.007(3) -0.006(3) O5 0.0176(18) 0.0216(18) 0.0165(17) 0.0082(15) -0.0017(14) 0.0019(14) C5 0.033(3) 0.028(3) 0.025(3) 0.016(3) -0.004(2) 0.004(2) O6 0.029(2) 0.0222(19) 0.0174(18) 0.0053(15) 0.0090(16) 0.0050(16) C6 0.022(3) 0.020(3) 0.030(3) 0.014(2) -0.004(2) -0.001(2) O7 0.0182(18) 0.0259(19) 0.0206(18) 0.0079(16) 0.0067(15) 0.0072(15) C7 0.032(3) 0.027(3) 0.028(3) 0.020(3) -0.001(2) -0.005(2) O8 0.0187(18) 0.0195(18) 0.0183(17) 0.0108(15) 0.0039(14) 0.0078(14) C8 0.020(3) 0.032(3) 0.027(3) 0.023(3) -0.004(2) 0.000(2) O9 0.0249(19) 0.0238(18) 0.0205(18) 0.0146(15) 0.0076(15) 0.0048(15) C9 0.022(3) 0.041(3) 0.043(4) 0.033(3) -0.002(3) -0.004(3) O10 0.028(2) 0.0192(18) 0.0233(19) 0.0103(15) 0.0088(15) 0.0053(15) C10 0.017(3) 0.056(4) 0.046(4) 0.039(3) 0.004(3) 0.004(3) C11 0.024(3) 0.048(4) 0.038(3) 0.034(3) 0.007(3) 0.012(3) C12 0.020(3) 0.035(3) 0.019(3) 0.021(2) 0.002(2) 0.004(2) C13 0.017(3) 0.037(3) 0.021(3) 0.023(3) 0.000(2) -0.001(2) C14 0.024(3) 0.038(3) 0.016(3) 0.013(2) 0.003(2) 0.007(2) C15 0.024(3) 0.020(3) 0.012(2) 0.004(2) 0.000(2) 0.000(2) C16 0.023(3) 0.030(3) 0.017(3) 0.012(2) 0.009(2) 0.003(2) C17 0.025(3) 0.024(3) 0.021(3) 0.006(2) 0.006(2) 0.004(2) C18 0.028(3) 0.016(3) 0.018(3) 0.004(2) 0.004(2) 0.003(2) C19 0.021(3) 0.021(3) 0.013(2) 0.005(2) 0.003(2) 0.001(2) C20 0.019(3) 0.022(3) 0.016(3) 0.006(2) 0.001(2) -0.001(2) C21 0.027(3) 0.018(3) 0.014(2) 0.007(2) 0.003(2) 0.005(2) C22 0.026(3) 0.027(3) 0.012(2) 0.010(2) 0.004(2) 0.007(2) C23 0.019(3) 0.018(2) 0.011(2) 0.007(2) 0.005(2) 0.002(2) C24 0.020(3) 0.027(3) 0.018(3) 0.013(2) 0.005(2) 0.009(2) C25 0.019(3) 0.029(3) 0.015(3) 0.010(2) 0.001(2) 0.005(2) C26 0.022(3) 0.021(3) 0.014(3) 0.004(2) 0.000(2) 0.001(2) C27 0.018(3) 0.022(3) 0.013(2) 0.010(2) 0.005(2) 0.003(2) C28 0.017(3) 0.024(3) 0.014(2) 0.011(2) 0.003(2) 0.001(2) C29 0.023(3) 0.026(3) 0.020(3) 0.008(2) 0.003(2) 0.007(2) C30 0.035(3) 0.034(3) 0.029(3) 0.020(3) -0.011(3) -0.004(3) C31 0.034(3) 0.054(4) 0.046(4) 0.034(3) -0.014(3) -0.011(3) C32 0.060(4) 0.026(3) 0.046(4) 0.015(3) -0.009(3) -0.008(3) C33 0.041(4) 0.043(4) 0.054(4) 0.032(3) -0.012(3) -0.022(3) C34 0.021(3) 0.079(5) 0.073(5) 0.065(4) 0.018(3) 0.012(3) C35 0.031(4) 0.107(7) 0.081(6) 0.064(5) 0.009(4) -0.016(4) C36 0.036(4) 0.074(5) 0.077(5) 0.057(4) 0.035(4) 0.025(3) C37 0.029(4) 0.162(9) 0.159(9) 0.140(8) 0.040(5) 0.042(5) C38 0.037(3) 0.044(4) 0.033(3) 0.021(3) 0.022(3) 0.020(3) C39 0.041(4) 0.047(4) 0.051(4) 0.030(3) 0.024(3) 0.023(3) C40 0.033(3) 0.078(5) 0.052(4) 0.047(4) 0.021(3) 0.023(3) C41 0.070(5) 0.069(5) 0.035(4) 0.011(3) 0.023(3) 0.046(4) C42 0.025(3) 0.027(3) 0.028(3) 0.010(2) -0.003(2) 0.006(2) C43 0.046(4) 0.057(4) 0.048(4) 0.026(4) -0.023(3) 0.005(3) C44 0.047(4) 0.036(4) 0.054(4) 0.008(3) -0.028(3) 0.006(3) C45 0.028(4) 0.079(5) 0.071(5) 0.021(4) -0.006(4) 0.011(4) C46 0.021(3) 0.028(3) 0.020(3) 0.009(2) 0.001(2) 0.001(2) C47 0.028(3) 0.025(3) 0.022(3) 0.011(2) 0.007(2) 0.005(2) C48 0.024(3) 0.020(3) 0.017(3) 0.007(2) 0.000(2) 0.006(2) C49 0.027(3) 0.027(3) 0.013(2) 0.010(2) 0.005(2) 0.011(2) C50 0.018(3) 0.024(3) 0.016(3) 0.011(2) 0.000(2) 0.006(2) C51 0.024(3) 0.021(3) 0.012(2) 0.006(2) 0.003(2) 0.008(2) C52 0.023(3) 0.020(3) 0.016(3) 0.010(2) 0.005(2) 0.005(2) C53 0.019(3) 0.020(3) 0.017(3) 0.010(2) 0.006(2) 0.008(2) C54 0.025(3) 0.020(3) 0.014(2) 0.007(2) 0.004(2) 0.004(2) C55 0.021(3) 0.024(3) 0.020(3) 0.010(2) 0.011(2) 0.009(2) C56 0.018(3) 0.025(3) 0.016(3) 0.008(2) 0.005(2) 0.004(2) C57 0.020(3) 0.021(3) 0.015(2) 0.010(2) 0.005(2) 0.006(2) C58 0.020(3) 0.020(3) 0.017(3) 0.011(2) 0.008(2) 0.008(2) C59 0.017(3) 0.022(3) 0.017(3) 0.005(2) 0.004(2) 0.005(2) C60 0.026(3) 0.017(3) 0.013(2) 0.004(2) 0.000(2) 0.007(2) N171 0.164(9) 0.219(11) 0.126(8) 0.059(7) 0.030(6) 0.123(8) C61 0.026(3) 0.032(3) 0.020(3) 0.006(2) 0.002(2) 0.010(2) C62 0.037(3) 0.040(3) 0.028(3) 0.014(3) 0.003(3) 0.023(3) C63 0.037(3) 0.034(3) 0.019(3) 0.015(2) 0.005(2) 0.019(3) C64 0.030(3) 0.022(3) 0.016(3) 0.008(2) 0.007(2) 0.012(2) C65 0.025(3) 0.015(2) 0.016(3) 0.005(2) 0.000(2) 0.007(2) C66 0.038(3) 0.025(3) 0.015(3) 0.010(2) 0.004(2) 0.013(2) C67 0.037(3) 0.032(3) 0.021(3) 0.020(2) 0.013(2) 0.013(3) C172 0.164(9) 0.219(11) 0.126(8) 0.059(7) 0.030(6) 0.123(8) C68 0.039(3) 0.026(3) 0.022(3) 0.014(2) 0.017(2) 0.012(2) C94 0.105(7) 0.099(7) 0.074(6) 0.047(6) 0.022(5) 0.045(6) C69 0.065(4) 0.029(3) 0.031(3) 0.020(3) 0.031(3) 0.021(3) C70 0.085(5) 0.024(3) 0.028(3) 0.012(3) 0.032(3) 0.014(3) C71 0.061(4) 0.020(3) 0.027(3) 0.007(3) 0.023(3) 0.003(3) C72 0.035(3) 0.024(3) 0.021(3) 0.009(2) 0.018(2) 0.006(2) C73 0.031(3) 0.023(3) 0.026(3) 0.013(2) 0.018(2) 0.010(2) C96 0.094(7) 0.101(7) 0.115(8) 0.070(7) 0.026(6) 0.039(6) C74 0.023(3) 0.026(3) 0.025(3) 0.005(2) 0.012(2) 0.002(2) N2 0.092(5) 0.073(5) 0.077(5) 0.055(4) 0.020(4) 0.037(4) C75 0.039(3) 0.023(3) 0.021(3) 0.003(2) 0.006(3) 0.005(3) C76 0.061(4) 0.029(3) 0.038(4) 0.012(3) 0.020(3) 0.016(3) C77 0.044(4) 0.037(4) 0.033(3) -0.005(3) -0.001(3) 0.007(3) C95 0.139(9) 0.159(10) 0.057(6) 0.011(7) 0.003(6) 0.120(9) C78 0.065(4) 0.033(3) 0.029(3) 0.009(3) 0.020(3) 0.018(3) C79 0.023(3) 0.025(3) 0.029(3) 0.008(2) 0.009(2) 0.010(2) C80 0.033(3) 0.031(3) 0.033(3) 0.012(3) 0.010(3) 0.016(3) C81 0.031(3) 0.037(3) 0.030(3) 0.012(3) 0.014(3) 0.016(3) C82 0.029(3) 0.039(3) 0.037(3) 0.009(3) 0.008(3) 0.016(3) C83 0.041(3) 0.069(4) 0.045(3) 0.034(3) 0.017(3) 0.039(3) C84 0.048(7) 0.069(7) 0.074(8) 0.027(7) 0.011(6) 0.049(6) C85 0.064(8) 0.079(9) 0.062(9) 0.010(7) 0.015(7) 0.057(7) C86 0.046(7) 0.068(9) 0.053(8) 0.022(7) 0.004(7) 0.041(7) C87 0.039(7) 0.082(10) 0.104(11) 0.030(9) -0.012(9) 0.039(7) C88 0.034(6) 0.074(7) 0.037(6) 0.037(6) 0.003(5) 0.033(6) C89 0.057(7) 0.092(8) 0.069(8) 0.041(7) 0.017(6) 0.046(7) C97 0.072(6) 0.069(6) 0.114(8) 0.042(6) 0.021(5) 0.026(5) C90 0.194(5) 0.034(2) 0.067(3) 0.0314(18) 0.055(3) 0.040(3) C91 0.194(5) 0.034(2) 0.067(3) 0.0314(18) 0.055(3) 0.040(3) C92 0.194(5) 0.034(2) 0.067(3) 0.0314(18) 0.055(3) 0.040(3) C93 0.194(5) 0.034(2) 0.067(3) 0.0314(18) 0.055(3) 0.040(3) O174 0.164(9) 0.219(11) 0.126(8) 0.059(7) 0.030(6) 0.123(8) C173 0.164(9) 0.219(11) 0.126(8) 0.059(7) 0.030(6) 0.123(8) C170 0.164(9) 0.219(11) 0.126(8) 0.059(7) 0.030(6) 0.123(8) C175 0.164(9) 0.219(11) 0.126(8) 0.059(7) 0.030(6) 0.123(8) C176 0.164(9) 0.219(11) 0.126(8) 0.059(7) 0.030(6) 0.123(8) N177 0.164(9) 0.219(11) 0.126(8) 0.059(7) 0.030(6) 0.123(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O5 1.893(4) . ? Cu1 O3 1.930(4) . ? Cu1 O3 1.945(4) 2 ? Cu1 O4 1.962(4) . ? Cu1 Cu1 2.949(5) 2 ? O1 C6 1.390(6) . ? N1 C95 1.079(10) . ? C1 C6 1.383(7) . ? C1 C2 1.385(7) . ? C1 C29 1.514(7) . ? Cu2 O10 1.887(4) . ? Cu2 O8 1.934(4) . ? Cu2 O8 1.953(4) 2_556 ? Cu2 O9 1.954(4) . ? Cu2 Cu2 2.964(4) 2_556 ? O2 C13 1.381(6) . ? C157 O161 1.192(14) . ? C157 N156 1.340(13) . ? N156 C164 1.380(14) . ? N156 C166 1.430(19) . ? N156 C165 1.432(17) . ? N156 C155 1.450(10) . ? N156 C160 1.476(17) . ? N156 C159 1.478(17) . ? C2 C3 1.384(7) . ? O3 C20 1.371(6) . ? O3 Cu1 1.945(4) 2 ? C3 C4 1.397(8) . ? C3 C30 1.545(7) . ? O4 C22 1.459(6) . ? O4 C21 1.479(6) . ? C4 C5 1.400(7) . ? O5 C28 1.356(6) . ? C5 C6 1.394(7) . ? C5 C7 1.533(7) . ? O6 C51 1.386(6) . ? O7 C58 1.378(6) . ? C7 C8 1.511(8) . ? O8 C65 1.373(6) . ? O8 Cu2 1.953(4) 2_556 ? C8 C13 1.399(7) . ? C8 C9 1.398(8) . ? O9 C67 1.454(6) . ? O9 C66 1.470(6) . ? C9 C10 1.375(8) . ? O10 C73 1.371(6) . ? C10 C11 1.407(8) . ? C10 C34 1.543(8) . ? C11 C12 1.382(7) . ? C12 C13 1.386(7) . ? C12 C14 1.533(7) . ? C14 C15 1.514(7) . ? C15 C16 1.383(7) . ? C15 C20 1.408(7) . ? C16 C17 1.382(7) . ? C17 C18 1.381(7) . ? C17 C38 1.544(8) . ? C159 O163 1.211(18) . ? C18 C19 1.378(7) . ? C19 C20 1.405(7) . ? C19 C21 1.496(7) . ? C22 C23 1.507(7) . ? C23 C24 1.392(7) . ? C23 C28 1.400(7) . ? C24 C25 1.404(7) . ? C25 C26 1.386(7) . ? C25 C42 1.540(7) . ? C26 C27 1.377(7) . ? C27 C28 1.415(7) . ? C27 C29 1.510(7) . ? C30 C33 1.525(8) . ? C30 C32 1.534(9) . ? C30 C31 1.538(8) . ? C34 C36 1.522(9) . ? C34 C37 1.524(9) . ? C34 C35 1.565(10) . ? C38 C39 1.529(8) . ? C38 C40 1.545(8) . ? C38 C41 1.545(8) . ? C42 C43 1.488(8) . ? C42 C44 1.538(8) . ? C42 C45 1.548(9) . ? C46 C47 1.401(7) . ? C46 C51 1.404(7) . ? C46 C74 1.506(7) . ? C47 C48 1.384(7) . ? C48 C49 1.393(7) . ? C48 C75 1.541(7) . ? C49 C50 1.414(7) . ? C160 O162 1.205(17) . ? C50 C51 1.380(7) . ? C50 C52 1.518(7) . ? C52 C53 1.512(7) . ? C53 C54 1.387(7) . ? C53 C58 1.400(7) . ? C54 C55 1.404(7) . ? C55 C56 1.397(7) . ? C55 C79 1.523(7) . ? C56 C57 1.393(7) . ? C57 C58 1.390(7) . ? C57 C59 1.531(7) . ? C59 C60 1.514(7) . ? C60 C61 1.383(7) . ? C60 C65 1.392(7) . ? N171 C173 1.334(16) . ? N171 C172 1.369(16) . ? N171 C170 1.379(16) . ? C61 C62 1.397(8) . ? C62 C63 1.383(8) . ? C62 C83 1.534(8) . ? C63 C64 1.384(7) . ? C64 C65 1.409(7) . ? C64 C66 1.487(7) . ? C67 C68 1.514(7) . ? C68 C69 1.394(7) . ? C68 C73 1.401(7) . ? C94 C95 1.600(14) . ? C69 C70 1.389(8) . ? C70 C71 1.383(8) . ? C70 C90 1.518(9) . ? C71 C72 1.403(7) . ? C72 C73 1.397(7) . ? C72 C74 1.505(8) . ? C96 C97 1.535(13) . ? N2 C97 1.107(10) . ? C75 C77 1.524(8) . ? C75 C78 1.526(8) . ? C75 C76 1.538(8) . ? C79 C82 1.522(8) . ? C79 C81 1.540(8) . ? C79 C80 1.552(7) . ? C83 C87 1.438(13) . ? C83 C84 1.468(12) . ? C83 C89 1.551(13) . ? C83 C86 1.562(13) . ? C83 C88 1.570(11) . ? C83 C85 1.580(12) . ? C90 C93 1.459(10) . ? C90 C92 1.518(9) . ? C90 C91 1.575(11) . ? O174 C173 1.180(16) . ? C175 C176 1.538(18) . ? C176 N177 1.155(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Cu1 O3 160.61(13) . . ? O5 Cu1 O3 95.00(17) . 2 ? O3 Cu1 O3 80.88(18) . 2 ? O5 Cu1 O4 94.21(17) . . ? O3 Cu1 O4 91.93(17) . . ? O3 Cu1 O4 169.63(13) 2 . ? O5 Cu1 Cu1 132.43(13) . 2 ? O3 Cu1 Cu1 40.63(13) . 2 ? O3 Cu1 Cu1 40.24(10) 2 2 ? O4 Cu1 Cu1 132.13(11) . 2 ? C6 C1 C2 119.1(5) . . ? C6 C1 C29 122.3(4) . . ? C2 C1 C29 118.6(5) . . ? O10 Cu2 O8 159.54(14) . . ? O10 Cu2 O8 96.06(18) . 2_556 ? O8 Cu2 O8 80.64(17) . 2_556 ? O10 Cu2 O9 93.96(18) . . ? O8 Cu2 O9 91.58(17) . . ? O8 Cu2 O9 168.90(13) 2_556 . ? O10 Cu2 Cu2 132.92(13) . 2_556 ? O8 Cu2 Cu2 40.56(9) . 2_556 ? O8 Cu2 Cu2 40.09(12) 2_556 2_556 ? O9 Cu2 Cu2 131.66(13) . 2_556 ? O161 C157 N156 120.4(14) . . ? C157 N156 C164 20.8(10) . . ? C157 N156 C166 116(2) . . ? C164 N156 C166 133(2) . . ? C157 N156 C165 127.6(15) . . ? C164 N156 C165 132.8(16) . . ? C166 N156 C165 35(2) . . ? C157 N156 C155 119.2(9) . . ? C164 N156 C155 105.4(10) . . ? C166 N156 C155 121(2) . . ? C165 N156 C155 111.7(15) . . ? C157 N156 C160 90.9(15) . . ? C164 N156 C160 109.2(15) . . ? C166 N156 C160 25(2) . . ? C165 N156 C160 52(2) . . ? C155 N156 C160 141.9(13) . . ? C157 N156 C159 128.6(13) . . ? C164 N156 C159 120.8(15) . . ? C166 N156 C159 64(2) . . ? C165 N156 C159 29.4(15) . . ? C155 N156 C159 96.2(12) . . ? C160 N156 C159 79.6(17) . . ? C3 C2 C1 122.8(5) . . ? C20 O3 Cu1 122.0(3) . . ? C20 O3 Cu1 135.4(3) . 2 ? Cu1 O3 Cu1 99.12(18) . 2 ? C2 C3 C4 116.5(5) . . ? C2 C3 C30 119.4(5) . . ? C4 C3 C30 124.1(5) . . ? C22 O4 C21 114.2(3) . . ? C22 O4 Cu1 112.3(3) . . ? C21 O4 Cu1 112.4(3) . . ? C3 C4 C5 122.7(5) . . ? C28 O5 Cu1 124.1(3) . . ? C6 C5 C4 117.8(5) . . ? C6 C5 C7 121.3(4) . . ? C4 C5 C7 120.8(4) . . ? C1 C6 O1 122.2(4) . . ? C1 C6 C5 120.9(5) . . ? O1 C6 C5 116.8(4) . . ? C8 C7 C5 117.6(4) . . ? C65 O8 Cu2 122.7(3) . . ? C65 O8 Cu2 134.6(3) . 2_556 ? Cu2 O8 Cu2 99.36(17) . 2_556 ? C13 C8 C9 116.5(5) . . ? C13 C8 C7 123.6(5) . . ? C9 C8 C7 119.6(5) . . ? C67 O9 C66 113.7(4) . . ? C67 O9 Cu2 112.7(3) . . ? C66 O9 Cu2 113.6(3) . . ? C10 C9 C8 123.2(5) . . ? C73 O10 Cu2 124.5(3) . . ? C9 C10 C11 117.8(5) . . ? C9 C10 C34 123.6(5) . . ? C11 C10 C34 118.5(6) . . ? C12 C11 C10 121.2(6) . . ? C11 C12 C13 118.8(5) . . ? C11 C12 C14 119.4(5) . . ? C13 C12 C14 121.9(4) . . ? O2 C13 C12 117.1(4) . . ? O2 C13 C8 120.5(5) . . ? C12 C13 C8 122.3(5) . . ? C15 C14 C12 112.2(4) . . ? C16 C15 C20 118.1(5) . . ? C16 C15 C14 117.6(4) . . ? C20 C15 C14 124.1(5) . . ? C17 C16 C15 124.0(5) . . ? C18 C17 C16 116.7(5) . . ? C18 C17 C38 123.1(5) . . ? C16 C17 C38 120.2(5) . . ? O163 C159 N156 116(2) . . ? C19 C18 C17 122.0(5) . . ? C18 C19 C20 120.6(4) . . ? C18 C19 C21 119.7(4) . . ? C20 C19 C21 119.6(4) . . ? O3 C20 C19 118.3(4) . . ? O3 C20 C15 123.1(4) . . ? C19 C20 C15 118.5(5) . . ? O4 C21 C19 106.5(4) . . ? O4 C22 C23 108.3(4) . . ? C24 C23 C28 119.5(4) . . ? C24 C23 C22 120.7(4) . . ? C28 C23 C22 119.8(4) . . ? C23 C24 C25 122.4(4) . . ? C26 C25 C24 116.5(4) . . ? C26 C25 C42 121.9(4) . . ? C24 C25 C42 121.6(4) . . ? C27 C26 C25 123.0(5) . . ? C26 C27 C28 119.7(4) . . ? C26 C27 C29 119.8(4) . . ? C28 C27 C29 120.3(4) . . ? O5 C28 C23 122.5(4) . . ? O5 C28 C27 118.9(4) . . ? C23 C28 C27 118.6(4) . . ? C27 C29 C1 110.5(4) . . ? C33 C30 C32 108.9(5) . . ? C33 C30 C31 107.9(5) . . ? C32 C30 C31 110.1(5) . . ? C33 C30 C3 111.2(4) . . ? C32 C30 C3 111.4(5) . . ? C31 C30 C3 107.3(5) . . ? C36 C34 C37 111.1(6) . . ? C36 C34 C10 108.6(5) . . ? C37 C34 C10 108.7(5) . . ? C36 C34 C35 108.7(5) . . ? C37 C34 C35 109.3(6) . . ? C10 C34 C35 110.5(6) . . ? C39 C38 C17 112.0(4) . . ? C39 C38 C40 107.9(5) . . ? C17 C38 C40 108.1(5) . . ? C39 C38 C41 108.2(5) . . ? C17 C38 C41 110.0(5) . . ? C40 C38 C41 110.6(5) . . ? C43 C42 C44 108.8(5) . . ? C43 C42 C25 111.7(4) . . ? C44 C42 C25 112.6(4) . . ? C43 C42 C45 109.9(5) . . ? C44 C42 C45 106.4(5) . . ? C25 C42 C45 107.2(5) . . ? C47 C46 C51 117.9(5) . . ? C47 C46 C74 119.4(4) . . ? C51 C46 C74 122.6(4) . . ? C48 C47 C46 123.5(5) . . ? C47 C48 C49 116.5(4) . . ? C47 C48 C75 120.1(4) . . ? C49 C48 C75 123.4(5) . . ? C48 C49 C50 122.3(5) . . ? O162 C160 N156 131(2) . . ? C51 C50 C49 118.8(4) . . ? C51 C50 C52 121.6(4) . . ? C49 C50 C52 119.6(4) . . ? C50 C51 O6 117.2(4) . . ? C50 C51 C46 120.8(4) . . ? O6 C51 C46 121.9(4) . . ? C53 C52 C50 115.6(4) . . ? C54 C53 C58 118.7(4) . . ? C54 C53 C52 118.8(4) . . ? C58 C53 C52 122.4(4) . . ? C53 C54 C55 122.1(5) . . ? C56 C55 C54 116.6(4) . . ? C56 C55 C79 123.5(4) . . ? C54 C55 C79 119.9(4) . . ? C57 C56 C55 123.4(5) . . ? C58 C57 C56 117.6(4) . . ? C58 C57 C59 122.2(4) . . ? C56 C57 C59 120.2(4) . . ? O7 C58 C57 117.5(4) . . ? O7 C58 C53 121.0(4) . . ? C57 C58 C53 121.5(4) . . ? C60 C59 C57 111.9(4) . . ? C61 C60 C65 118.4(5) . . ? C61 C60 C59 117.5(5) . . ? C65 C60 C59 124.0(4) . . ? C173 N171 C172 127.4(18) . . ? C173 N171 C170 113.7(17) . . ? C172 N171 C170 109.6(15) . . ? C60 C61 C62 123.8(5) . . ? C63 C62 C61 116.4(5) . . ? C63 C62 C83 121.8(5) . . ? C61 C62 C83 121.7(5) . . ? C64 C63 C62 121.9(5) . . ? C63 C64 C65 120.1(5) . . ? C63 C64 C66 118.7(4) . . ? C65 C64 C66 121.0(4) . . ? O8 C65 C60 123.7(4) . . ? O8 C65 C64 117.0(4) . . ? C60 C65 C64 119.2(4) . . ? O9 C66 C64 107.1(4) . . ? O9 C67 C68 108.4(4) . . ? C69 C68 C73 119.6(5) . . ? C69 C68 C67 120.5(5) . . ? C73 C68 C67 119.8(5) . . ? C70 C69 C68 123.2(5) . . ? C71 C70 C69 115.8(5) . . ? C71 C70 C90 122.4(6) . . ? C69 C70 C90 121.8(6) . . ? C70 C71 C72 123.4(5) . . ? C73 C72 C71 119.2(5) . . ? C73 C72 C74 120.4(5) . . ? C71 C72 C74 120.4(5) . . ? O10 C73 C72 119.4(5) . . ? O10 C73 C68 122.0(4) . . ? C72 C73 C68 118.6(5) . . ? C72 C74 C46 112.9(5) . . ? C77 C75 C78 108.5(5) . . ? C77 C75 C76 109.3(5) . . ? C78 C75 C76 107.6(5) . . ? C77 C75 C48 110.0(5) . . ? C78 C75 C48 111.6(4) . . ? C76 C75 C48 109.8(4) . . ? N1 C95 C94 165.2(13) . . ? C82 C79 C55 112.5(4) . . ? C82 C79 C81 108.6(4) . . ? C55 C79 C81 109.3(4) . . ? C82 C79 C80 108.3(4) . . ? C55 C79 C80 109.8(4) . . ? C81 C79 C80 108.1(4) . . ? C87 C83 C84 135.9(9) . . ? C87 C83 C62 112.0(8) . . ? C84 C83 C62 109.2(7) . . ? C87 C83 C89 116.3(10) . . ? C84 C83 C89 59.9(9) . . ? C62 C83 C89 111.1(7) . . ? C87 C83 C86 36.6(8) . . ? C84 C83 C86 112.0(9) . . ? C62 C83 C86 111.7(7) . . ? C89 C83 C86 136.4(8) . . ? C87 C83 C88 69.4(10) . . ? C84 C83 C88 111.7(9) . . ? C62 C83 C88 107.9(6) . . ? C89 C83 C88 53.9(7) . . ? C86 C83 C88 104.2(8) . . ? C87 C83 C85 109.4(11) . . ? C84 C83 C85 41.6(8) . . ? C62 C83 C85 107.3(7) . . ? C89 C83 C85 99.7(10) . . ? C86 C83 C85 75.2(9) . . ? C88 C83 C85 142.0(8) . . ? N2 C97 C96 175.5(10) . . ? C93 C90 C92 110.3(7) . . ? C93 C90 C70 115.4(7) . . ? C92 C90 C70 111.1(6) . . ? C93 C90 C91 106.8(7) . . ? C92 C90 C91 103.7(7) . . ? C70 C90 C91 108.9(7) . . ? O174 C173 N171 131(2) . . ? N177 C176 C175 162(3) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.262 _refine_diff_density_min -1.070 _refine_diff_density_rms 0.093 _database_code_depnum_ccdc_archive 'CCDC 928622' ####################################################################### # # 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_Cu4 #TrackingRef '18433_web_deposit_cif_file_1_DrScottJ.Dalgarno_1362935644.CU4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'MonOxaC4 Cu4' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H152 Cu4 N4 O18' _chemical_formula_weight 2024.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.021(3) _cell_length_b 12.9755(16) _cell_length_c 21.644(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.916(6) _cell_angle_gamma 90.00 _cell_volume 5433.1(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2560 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 19.19 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 0.836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7586 _exptl_absorpt_correction_T_max 0.8183 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex II CCD Diffractometer' _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 46243 _diffrn_reflns_av_R_equivalents 0.1470 _diffrn_reflns_av_sigmaI/netI 0.1362 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 22.72 _reflns_number_total 7128 _reflns_number_gt 3501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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. A number of restraints were appiled to the data due to disorder in an upper-rim tert-butyl group and to maintain chemical meaning with respect to a dmf of crystallisation. The crystals were foudn to be weakly diffracting but a satsifactory solution could be obtained. DFIX 1.45 0.02 C71 N3 DFIX 1.45 0.02 C72 N3 DFIX 1.45 0.02 C70 N3 DFIX 1.21 0.02 C70 O9 SIMU 0.01 C71 C72 C70 N3 O9 DFIX 1.54 0.02 C18 C38 DFIX 1.54 0.02 C39 C38 DFIX 1.54 0.02 C41 C38 DFIX 1.54 0.02 C40 C38 DFIX 1.54 0.02 C40A C38A DFIX 1.54 0.02 C41A C38A DFIX 1.54 0.02 C18 C38A DFIX 1.54 0.02 C38A C39A EADP C38 C39 C40 C41 C38A C39A C40A C41A DANG 2.54 0.02 C39 C40 DANG 2.54 0.02 C39 C41 DANG 2.54 0.02 C41 C40 EADP C30 C31 C32 C33 DANG 2.54 0.02 C39A C40A DANG 2.54 0.02 C39A C41A DANG 2.54 0.02 C41A C40A ; _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^)+(0.0819P)^2^+27.7234P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7128 _refine_ls_number_parameters 586 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1831 _refine_ls_R_factor_gt 0.0862 _refine_ls_wR_factor_ref 0.2307 _refine_ls_wR_factor_gt 0.1897 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.031 _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 Cu1 Cu 0.45937(6) 0.50082(9) 0.43294(6) 0.0384(4) Uani 1 1 d . . . O1 O 0.4189(3) 0.5993(4) 0.3658(3) 0.0343(17) Uani 1 1 d . . . N1 N 0.2669(4) 0.4922(7) 0.4687(5) 0.045(2) Uani 1 1 d . . . C1 C 0.5947(5) 0.5975(7) 0.3394(6) 0.039(3) Uani 1 1 d . . . Cu2 Cu 0.35294(6) 0.50593(9) 0.31201(6) 0.0319(4) Uani 1 1 d . . . O2 O 0.3206(3) 0.4036(4) 0.2490(3) 0.0295(17) Uani 1 1 d . . . C2 C 0.5680(5) 0.6603(7) 0.3864(5) 0.043(3) Uani 1 1 d . . . H2A H 0.6052 0.7064 0.4101 0.052 Uiso 1 1 calc R . . H2B H 0.5555 0.6134 0.4177 0.052 Uiso 1 1 calc R . . O3 O 0.4462(3) 0.3277(4) 0.2668(3) 0.0387(18) Uani 1 1 d . . . H3O H 0.4049 0.3473 0.2588 0.046 Uiso 1 1 calc R . . N3 N 0.4148(5) 0.6265(7) 0.1379(5) 0.058(3) Uani 1 1 d DU . . C3 C 0.5054(5) 0.7247(7) 0.3542(5) 0.039(3) Uani 1 1 d . . . O4 O 0.5359(3) 0.4470(5) 0.3622(4) 0.044(2) Uani 1 1 d . . . H4O H 0.5154 0.3960 0.3419 0.053 Uiso 1 1 calc R . . C4 C 0.5172(5) 0.8204(7) 0.3283(5) 0.040(3) Uani 1 1 d . . . H4 H 0.5637 0.8423 0.3341 0.048 Uiso 1 1 calc R . . O5 O 0.3092(3) 0.6209(4) 0.2557(3) 0.0295(17) Uani 1 1 d . . . C5 C 0.4655(5) 0.8837(7) 0.2951(5) 0.033(3) Uani 1 1 d . . . O6 O 0.4005(3) 0.4104(4) 0.3747(3) 0.0329(17) Uani 1 1 d . . . C6 C 0.3991(5) 0.8480(7) 0.2851(5) 0.035(3) Uani 1 1 d . . . H6 H 0.3622 0.8888 0.2608 0.042 Uiso 1 1 calc R . . O7 O 0.5000(4) 0.5932(4) 0.5003(4) 0.0424(17) Uani 1 1 d . . . C7 C 0.3840(5) 0.7542(7) 0.3091(5) 0.034(3) Uani 1 1 d . . . O8 O 0.2628(3) 0.5221(5) 0.3641(4) 0.0438(19) Uani 1 1 d . . . C8 C 0.3114(5) 0.7135(7) 0.2927(5) 0.040(3) Uani 1 1 d . . . H8A H 0.2971 0.6985 0.3323 0.047 Uiso 1 1 calc R . . H8B H 0.2794 0.7655 0.2677 0.047 Uiso 1 1 calc R . . O9 O 0.3337(6) 0.7479(8) 0.0906(6) 0.122(4) Uani 1 1 d DU . . C9 C 0.2402(5) 0.5886(7) 0.2191(5) 0.034(3) Uani 1 1 d . . . H9A H 0.2140 0.6495 0.1982 0.040 Uiso 1 1 calc R . . H9B H 0.2149 0.5585 0.2485 0.040 Uiso 1 1 calc R . . C10 C 0.2446(5) 0.5121(8) 0.1702(5) 0.034(3) Uani 1 1 d . . . C11 C 0.2094(5) 0.5265(7) 0.1080(5) 0.032(3) Uani 1 1 d . . . H11 H 0.1836 0.5883 0.0970 0.038 Uiso 1 1 calc R . . C12 C 0.2090(5) 0.4546(7) 0.0592(6) 0.039(3) Uani 1 1 d . . . C13 C 0.2506(5) 0.3693(8) 0.0774(6) 0.045(3) Uani 1 1 d . . . H13 H 0.2523 0.3189 0.0459 0.055 Uiso 1 1 calc R . . C14 C 0.2905(5) 0.3536(7) 0.1404(6) 0.038(3) Uani 1 1 d . . . C15 C 0.3362(5) 0.2569(7) 0.1569(5) 0.036(3) Uani 1 1 d . . . H15A H 0.3165 0.2020 0.1258 0.043 Uiso 1 1 calc R . . H15B H 0.3344 0.2322 0.1998 0.043 Uiso 1 1 calc R . . C16 C 0.4129(6) 0.2729(7) 0.1570(6) 0.039(3) Uani 1 1 d . . . C17 C 0.4316(6) 0.2525(7) 0.1004(6) 0.050(3) Uani 1 1 d . A . H17 H 0.3970 0.2365 0.0624 0.060 Uiso 1 1 calc R . . C18 C 0.5009(7) 0.2556(9) 0.0994(6) 0.060(4) Uani 1 1 d D . . C19 C 0.5485(7) 0.2769(8) 0.1560(7) 0.053(4) Uani 1 1 d . A . H19 H 0.5960 0.2752 0.1563 0.064 Uiso 1 1 calc R . . C20 C 0.5321(6) 0.3005(7) 0.2125(6) 0.042(3) Uani 1 1 d . . . C21 C 0.5862(5) 0.3219(7) 0.2727(6) 0.045(3) Uani 1 1 d . A . H21A H 0.6292 0.2856 0.2710 0.054 Uiso 1 1 calc R . . H21B H 0.5708 0.2935 0.3092 0.054 Uiso 1 1 calc R . . C22 C 0.6021(5) 0.4365(7) 0.2845(6) 0.041(3) Uani 1 1 d . . . C23 C 0.6436(5) 0.4863(8) 0.2503(6) 0.058(3) Uani 1 1 d . A . H23 H 0.6604 0.4488 0.2197 0.070 Uiso 1 1 calc R . . C24 C 0.6610(6) 0.5929(8) 0.2611(6) 0.054(4) Uani 1 1 d . . . C25 C 0.6368(5) 0.6425(7) 0.3072(6) 0.042(3) Uani 1 1 d . A . H25 H 0.6504 0.7120 0.3170 0.050 Uiso 1 1 calc R . . C26 C 0.5775(5) 0.4927(8) 0.3277(5) 0.039(3) Uani 1 1 d . A . C27 C 0.4364(5) 0.6917(7) 0.3443(5) 0.032(3) Uani 1 1 d . . . C28 C 0.2861(5) 0.4234(7) 0.1884(5) 0.026(2) Uani 1 1 d . . . C29 C 0.4621(6) 0.3029(7) 0.2113(6) 0.041(3) Uani 1 1 d . A . C30 C 0.4803(5) 0.9905(7) 0.2694(6) 0.0480(14) Uani 1 1 d . . . C31 C 0.4372(5) 1.0018(8) 0.2001(5) 0.0480(14) Uani 1 1 d . . . H31A H 0.4478 1.0679 0.1829 0.072 Uiso 1 1 calc R . . H31B H 0.3880 0.9991 0.1989 0.072 Uiso 1 1 calc R . . H31C H 0.4484 0.9454 0.1743 0.072 Uiso 1 1 calc R . . C32 C 0.4595(5) 1.0716(7) 0.3110(6) 0.0480(14) Uani 1 1 d . . . H32A H 0.4886 1.0655 0.3548 0.072 Uiso 1 1 calc R . . H32B H 0.4110 1.0617 0.3109 0.072 Uiso 1 1 calc R . . H32C H 0.4655 1.1402 0.2942 0.072 Uiso 1 1 calc R . . C33 C 0.5550(5) 1.0039(7) 0.2702(5) 0.0480(14) Uani 1 1 d . . . H33A H 0.5614 1.0707 0.2514 0.072 Uiso 1 1 calc R . . H33B H 0.5690 0.9486 0.2453 0.072 Uiso 1 1 calc R . . H33C H 0.5835 1.0010 0.3144 0.072 Uiso 1 1 calc R . . C34 C 0.1673(6) 0.4748(8) -0.0078(6) 0.050(3) Uani 1 1 d . . . C35 C 0.1975(7) 0.5674(9) -0.0359(7) 0.079(4) Uani 1 1 d . . . H35A H 0.2059 0.6242 -0.0050 0.118 Uiso 1 1 calc R . . H35B H 0.1646 0.5897 -0.0755 0.118 Uiso 1 1 calc R . . H35C H 0.2411 0.5473 -0.0452 0.118 Uiso 1 1 calc R . . C36 C 0.0925(6) 0.4993(10) -0.0078(7) 0.079(4) Uani 1 1 d . . . H36A H 0.0732 0.4416 0.0112 0.119 Uiso 1 1 calc R . . H36B H 0.0650 0.5102 -0.0518 0.119 Uiso 1 1 calc R . . H36C H 0.0914 0.5619 0.0173 0.119 Uiso 1 1 calc R . . C37 C 0.1657(6) 0.3796(9) -0.0522(6) 0.064(4) Uani 1 1 d . . . H37A H 0.2129 0.3622 -0.0536 0.096 Uiso 1 1 calc R . . H37B H 0.1380 0.3960 -0.0955 0.096 Uiso 1 1 calc R . . H37C H 0.1451 0.3208 -0.0355 0.096 Uiso 1 1 calc R . . C38 C 0.5288(13) 0.2389(18) 0.0412(10) 0.097(4) Uani 0.50 1 d PD A 1 C39 C 0.4853(14) 0.2971(19) -0.0178(13) 0.097(4) Uani 0.50 1 d PD A 1 H39A H 0.5053 0.2863 -0.0541 0.146 Uiso 0.50 1 calc PR A 1 H39B H 0.4853 0.3709 -0.0082 0.146 Uiso 0.50 1 calc PR A 1 H39C H 0.4377 0.2711 -0.0285 0.146 Uiso 0.50 1 calc PR A 1 C40 C 0.5245(15) 0.1220(15) 0.0293(14) 0.097(4) Uani 0.50 1 d PD A 1 H40A H 0.5389 0.1064 -0.0097 0.146 Uiso 0.50 1 calc PR A 1 H40B H 0.4768 0.0988 0.0242 0.146 Uiso 0.50 1 calc PR A 1 H40C H 0.5550 0.0864 0.0657 0.146 Uiso 0.50 1 calc PR A 1 C41 C 0.6061(11) 0.2727(19) 0.0508(14) 0.097(4) Uani 0.50 1 d PD A 1 H41A H 0.6195 0.2629 0.0107 0.146 Uiso 0.50 1 calc PR A 1 H41B H 0.6359 0.2308 0.0845 0.146 Uiso 0.50 1 calc PR A 1 H41C H 0.6111 0.3456 0.0631 0.146 Uiso 0.50 1 calc PR A 1 C42 C 0.7045(6) 0.6426(8) 0.2199(8) 0.060(4) Uani 1 1 d . A . C43 C 0.7155(7) 0.7569(8) 0.2344(9) 0.095(6) Uani 1 1 d . . . H43A H 0.7381 0.7883 0.2039 0.142 Uiso 1 1 calc R A . H43B H 0.7447 0.7659 0.2779 0.142 Uiso 1 1 calc R . . H43C H 0.6707 0.7903 0.2307 0.142 Uiso 1 1 calc R . . C44 C 0.7738(6) 0.5904(10) 0.2311(8) 0.101(6) Uani 1 1 d . . . H44A H 0.7672 0.5174 0.2197 0.151 Uiso 1 1 calc R A . H44B H 0.7987 0.5968 0.2763 0.151 Uiso 1 1 calc R . . H44C H 0.8008 0.6233 0.2046 0.151 Uiso 1 1 calc R . . C45 C 0.6672(8) 0.6353(13) 0.1516(9) 0.106(6) Uani 1 1 d . . . H45A H 0.6185 0.6535 0.1464 0.159 Uiso 1 1 calc R A . H45B H 0.6703 0.5647 0.1366 0.159 Uiso 1 1 calc R . . H45C H 0.6879 0.6829 0.1267 0.159 Uiso 1 1 calc R . . C49 C 0.4797(6) 0.6968(7) 0.5083(6) 0.051(3) Uani 1 1 d . . . H49A H 0.5148 0.7443 0.5007 0.076 Uiso 1 1 calc R . . H49B H 0.4750 0.7061 0.5519 0.076 Uiso 1 1 calc R . . H49C H 0.4353 0.7110 0.4776 0.076 Uiso 1 1 calc R . . C50 C 0.3691(6) 0.3169(7) 0.3885(6) 0.052(3) Uani 1 1 d . . . H50A H 0.3930 0.2578 0.3758 0.077 Uiso 1 1 calc R . . H50B H 0.3203 0.3159 0.3647 0.077 Uiso 1 1 calc R . . H50C H 0.3726 0.3132 0.4345 0.077 Uiso 1 1 calc R . . C70 C 0.3794(8) 0.7148(11) 0.1331(7) 0.087(4) Uani 1 1 d DU . . H70 H 0.3927 0.7586 0.1694 0.105 Uiso 1 1 calc R . . C71 C 0.3877(7) 0.5530(10) 0.0842(7) 0.085(4) Uani 1 1 d DU . . H71A H 0.3698 0.4913 0.1006 0.127 Uiso 1 1 calc R . . H71B H 0.4250 0.5334 0.0649 0.127 Uiso 1 1 calc R . . H71C H 0.3504 0.5860 0.0519 0.127 Uiso 1 1 calc R . . C72 C 0.4612(6) 0.5842(10) 0.1912(6) 0.077(4) Uani 1 1 d DU . . H72A H 0.4716 0.6350 0.2258 0.116 Uiso 1 1 calc R . . H72B H 0.5039 0.5651 0.1799 0.116 Uiso 1 1 calc R . . H72C H 0.4407 0.5227 0.2052 0.116 Uiso 1 1 calc R . . C73 C 0.2456(5) 0.4741(8) 0.4049(6) 0.045(3) Uani 1 1 d . . . H73 H 0.2142 0.4187 0.3913 0.054 Uiso 1 1 calc R . . C74 C 0.2442(6) 0.4315(10) 0.5148(6) 0.065(4) Uani 1 1 d . . . H74A H 0.2158 0.3740 0.4931 0.097 Uiso 1 1 calc R . . H74B H 0.2167 0.4745 0.5362 0.097 Uiso 1 1 calc R . . H74C H 0.2844 0.4045 0.5465 0.097 Uiso 1 1 calc R . . C75 C 0.3149(6) 0.5752(9) 0.4918(6) 0.069(4) Uani 1 1 d . . . H75A H 0.3192 0.6179 0.4556 0.103 Uiso 1 1 calc R . . H75B H 0.3602 0.5466 0.5133 0.103 Uiso 1 1 calc R . . H75C H 0.2978 0.6176 0.5219 0.103 Uiso 1 1 calc R . . C40A C 0.4668(13) 0.1545(18) -0.0084(13) 0.097(4) Uani 0.50 1 d PD A 2 H40D H 0.4828 0.1413 -0.0468 0.146 Uiso 0.50 1 calc PR A 2 H40E H 0.4195 0.1814 -0.0207 0.146 Uiso 0.50 1 calc PR A 2 H40F H 0.4677 0.0901 0.0155 0.146 Uiso 0.50 1 calc PR A 2 C41A C 0.5915(11) 0.208(2) 0.0417(14) 0.097(4) Uani 0.50 1 d PD A 2 H41D H 0.5986 0.1897 -0.0001 0.146 Uiso 0.50 1 calc PR A 2 H41E H 0.6044 0.1488 0.0708 0.146 Uiso 0.50 1 calc PR A 2 H41F H 0.6203 0.2671 0.0592 0.146 Uiso 0.50 1 calc PR A 2 C38A C 0.5150(13) 0.2343(19) 0.0342(9) 0.097(4) Uani 0.50 1 d PD A 2 C39A C 0.5013(16) 0.3407(15) -0.0019(15) 0.097(4) Uani 0.50 1 d PD A 2 H39D H 0.5130 0.3350 -0.0431 0.146 Uiso 0.50 1 calc PR A 2 H39E H 0.5300 0.3941 0.0241 0.146 Uiso 0.50 1 calc PR A 2 H39F H 0.4524 0.3591 -0.0093 0.146 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0456(8) 0.0180(6) 0.0462(9) 0.0058(7) 0.0018(6) -0.0054(6) O1 0.041(4) 0.025(4) 0.035(5) 0.004(3) 0.005(4) -0.012(3) N1 0.038(5) 0.041(5) 0.056(7) 0.014(6) 0.012(5) -0.003(5) C1 0.021(6) 0.027(6) 0.070(9) 0.009(6) 0.011(6) 0.004(5) Cu2 0.0379(7) 0.0173(6) 0.0399(8) 0.0052(7) 0.0091(6) -0.0017(6) O2 0.031(4) 0.017(3) 0.043(5) 0.001(3) 0.014(4) -0.003(3) C2 0.028(6) 0.024(6) 0.070(9) 0.016(6) 0.000(6) -0.013(5) O3 0.039(4) 0.024(4) 0.054(5) 0.007(4) 0.016(4) 0.001(3) N3 0.081(6) 0.043(5) 0.066(7) 0.012(5) 0.047(6) 0.024(5) C3 0.041(7) 0.025(6) 0.048(8) 0.001(5) 0.007(6) 0.002(5) O4 0.046(4) 0.017(3) 0.071(6) 0.009(4) 0.019(4) -0.004(3) C4 0.028(6) 0.023(6) 0.065(9) 0.012(6) 0.006(6) -0.006(5) O5 0.034(4) 0.017(3) 0.039(5) -0.005(3) 0.012(4) -0.002(3) C5 0.042(7) 0.016(5) 0.045(8) -0.005(5) 0.016(6) -0.004(5) O6 0.037(4) 0.014(3) 0.044(5) 0.009(3) 0.003(4) -0.008(3) C6 0.035(6) 0.021(5) 0.051(8) 0.003(5) 0.018(6) 0.007(5) O7 0.053(4) 0.027(4) 0.038(5) 0.004(4) -0.005(3) -0.002(4) C7 0.034(6) 0.020(5) 0.045(7) 0.000(5) 0.004(5) -0.005(5) O8 0.057(5) 0.023(4) 0.062(5) 0.007(4) 0.034(4) -0.001(3) C8 0.047(7) 0.015(5) 0.063(8) -0.001(5) 0.026(6) 0.001(5) O9 0.164(10) 0.107(8) 0.101(9) 0.039(7) 0.045(8) 0.088(7) C9 0.028(6) 0.030(6) 0.043(8) 0.007(5) 0.009(6) -0.003(5) C10 0.026(5) 0.036(6) 0.045(8) -0.003(6) 0.016(5) -0.002(5) C11 0.039(6) 0.020(6) 0.036(7) -0.001(5) 0.008(6) 0.003(4) C12 0.044(7) 0.017(5) 0.059(9) -0.001(6) 0.019(6) 0.004(5) C13 0.050(7) 0.038(7) 0.055(9) -0.010(6) 0.026(7) 0.002(6) C14 0.047(7) 0.024(6) 0.046(8) 0.008(6) 0.017(6) -0.001(5) C15 0.049(7) 0.015(5) 0.048(8) 0.002(5) 0.019(6) 0.003(5) C16 0.056(8) 0.019(5) 0.044(8) 0.009(5) 0.018(7) 0.010(5) C17 0.072(9) 0.024(6) 0.059(9) 0.015(6) 0.026(7) 0.012(6) C18 0.071(10) 0.050(8) 0.074(11) 0.011(7) 0.044(9) 0.010(7) C19 0.057(8) 0.031(6) 0.085(11) 0.023(7) 0.042(9) 0.015(6) C20 0.050(8) 0.008(5) 0.076(10) 0.003(6) 0.031(8) 0.003(5) C21 0.030(6) 0.024(6) 0.085(10) 0.012(6) 0.022(7) 0.010(5) C22 0.027(6) 0.016(5) 0.081(10) 0.017(6) 0.016(6) -0.001(5) C23 0.029(6) 0.041(7) 0.109(11) 0.018(7) 0.025(7) 0.018(6) C24 0.043(7) 0.029(6) 0.089(11) 0.028(7) 0.017(7) -0.005(5) C25 0.029(6) 0.023(6) 0.071(9) 0.012(6) 0.007(6) 0.002(5) C26 0.025(5) 0.031(6) 0.059(8) 0.024(7) 0.007(5) 0.002(5) C27 0.033(6) 0.016(5) 0.043(7) 0.003(5) 0.004(5) -0.003(5) C28 0.034(6) 0.017(5) 0.030(7) 0.006(5) 0.012(6) 0.004(4) C29 0.059(8) 0.016(5) 0.054(9) 0.012(6) 0.025(8) 0.007(5) C30 0.050(3) 0.023(3) 0.075(4) 0.013(3) 0.022(3) -0.003(3) C31 0.050(3) 0.023(3) 0.075(4) 0.013(3) 0.022(3) -0.003(3) C32 0.050(3) 0.023(3) 0.075(4) 0.013(3) 0.022(3) -0.003(3) C33 0.050(3) 0.023(3) 0.075(4) 0.013(3) 0.022(3) -0.003(3) C34 0.057(8) 0.042(7) 0.046(8) -0.003(6) 0.002(6) 0.011(6) C35 0.116(12) 0.053(8) 0.064(11) 0.019(8) 0.017(9) 0.002(8) C36 0.056(8) 0.091(10) 0.083(11) -0.032(9) 0.003(7) 0.017(8) C37 0.080(9) 0.058(8) 0.050(9) -0.004(7) 0.008(7) 0.014(7) C38 0.140(10) 0.083(8) 0.092(9) -0.003(7) 0.072(8) 0.027(7) C39 0.140(10) 0.083(8) 0.092(9) -0.003(7) 0.072(8) 0.027(7) C40 0.140(10) 0.083(8) 0.092(9) -0.003(7) 0.072(8) 0.027(7) C41 0.140(10) 0.083(8) 0.092(9) -0.003(7) 0.072(8) 0.027(7) C42 0.047(8) 0.045(7) 0.097(12) 0.007(8) 0.035(8) -0.008(6) C43 0.056(8) 0.045(8) 0.201(18) 0.032(10) 0.066(10) -0.001(7) C44 0.054(9) 0.055(8) 0.208(19) 0.037(10) 0.064(11) 0.012(7) C45 0.081(11) 0.122(14) 0.123(17) 0.026(12) 0.041(12) -0.021(10) C49 0.063(8) 0.021(6) 0.065(9) 0.010(6) 0.009(7) -0.003(5) C50 0.052(7) 0.024(6) 0.073(9) 0.005(6) 0.005(7) 0.003(5) C70 0.125(9) 0.083(8) 0.070(8) 0.026(7) 0.055(7) 0.035(7) C71 0.091(10) 0.070(9) 0.102(11) 0.001(8) 0.041(9) -0.001(8) C72 0.070(8) 0.083(9) 0.081(10) 0.033(8) 0.024(8) 0.026(7) C73 0.043(7) 0.037(7) 0.056(9) -0.007(7) 0.016(7) -0.004(5) C74 0.060(8) 0.080(9) 0.050(9) 0.015(7) 0.006(7) -0.014(7) C75 0.061(8) 0.052(8) 0.089(11) -0.023(7) 0.010(8) -0.023(7) C40A 0.140(10) 0.083(8) 0.092(9) -0.003(7) 0.072(8) 0.027(7) C41A 0.140(10) 0.083(8) 0.092(9) -0.003(7) 0.072(8) 0.027(7) C38A 0.140(10) 0.083(8) 0.092(9) -0.003(7) 0.072(8) 0.027(7) C39A 0.140(10) 0.083(8) 0.092(9) -0.003(7) 0.072(8) 0.027(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O6 1.895(6) . ? Cu1 O7 1.902(7) . ? Cu1 O7 1.906(7) 3_666 ? Cu1 O1 1.949(6) . ? Cu1 Cu1 2.940(2) 3_666 ? O1 C27 1.364(10) . ? O1 Cu2 1.943(6) . ? N1 C73 1.357(13) . ? N1 C74 1.433(13) . ? N1 C75 1.444(13) . ? C1 C25 1.358(13) . ? C1 C26 1.409(13) . ? C1 C2 1.503(14) . ? Cu2 O2 1.894(6) . ? Cu2 O6 1.902(6) . ? Cu2 O5 1.982(6) . ? Cu2 O8 2.370(7) . ? O2 C28 1.341(11) . ? C2 C3 1.519(13) . ? O3 C29 1.358(12) . ? N3 C70 1.337(12) . ? N3 C72 1.394(12) . ? N3 C71 1.494(13) . ? C3 C27 1.407(13) . ? C3 C4 1.407(13) . ? O4 C26 1.387(11) . ? C4 C5 1.371(13) . ? O5 C8 1.438(11) . ? O5 C9 1.465(11) . ? C5 C6 1.372(12) . ? C5 C30 1.550(13) . ? O6 C50 1.432(11) . ? C6 C7 1.388(12) . ? O7 C49 1.427(11) . ? O7 Cu1 1.906(7) 3_666 ? C7 C27 1.388(13) . ? C7 C8 1.500(13) . ? O8 C73 1.202(12) . ? O9 C70 1.198(13) . ? C9 C10 1.470(13) . ? C10 C11 1.362(13) . ? C10 C28 1.414(13) . ? C11 C12 1.409(13) . ? C12 C13 1.380(14) . ? C12 C34 1.498(15) . ? C13 C14 1.407(15) . ? C14 C28 1.398(14) . ? C14 C15 1.540(13) . ? C15 C16 1.549(14) . ? C16 C29 1.382(15) . ? C16 C17 1.395(15) . ? C17 C18 1.395(15) . ? C18 C19 1.371(17) . ? C18 C38 1.518(17) . ? C18 C38A 1.534(17) . ? C19 C20 1.380(15) . ? C20 C29 1.394(14) . ? C20 C21 1.490(15) . ? C21 C22 1.528(13) . ? C22 C26 1.375(14) . ? C22 C23 1.405(14) . ? C23 C24 1.430(14) . ? C24 C25 1.375(15) . ? C24 C42 1.540(15) . ? C30 C33 1.502(13) . ? C30 C32 1.511(14) . ? C30 C31 1.532(15) . ? C34 C36 1.532(15) . ? C34 C35 1.538(15) . ? C34 C37 1.561(15) . ? C38 C40 1.537(18) . ? C38 C39 1.546(18) . ? C38 C41 1.570(18) . ? C42 C45 1.477(19) . ? C42 C44 1.507(15) . ? C42 C43 1.521(15) . ? C40A C38A 1.547(18) . ? C41A C38A 1.539(17) . ? C38A C39A 1.575(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 O6 Cu1 O7 166.1(3) . . ? O6 Cu1 O7 100.3(3) . 3_666 ? O7 Cu1 O7 78.9(3) . 3_666 ? O6 Cu1 O1 80.9(2) . . ? O7 Cu1 O1 99.9(3) . . ? O7 Cu1 O1 178.8(3) 3_666 . ? O6 Cu1 Cu1 138.05(19) . 3_666 ? O7 Cu1 Cu1 39.50(19) . 3_666 ? O7 Cu1 Cu1 39.4(2) 3_666 3_666 ? O1 Cu1 Cu1 139.4(2) . 3_666 ? C27 O1 Cu2 122.6(6) . . ? C27 O1 Cu1 137.4(6) . . ? Cu2 O1 Cu1 97.2(3) . . ? C73 N1 C74 122.7(10) . . ? C73 N1 C75 119.1(9) . . ? C74 N1 C75 118.2(11) . . ? C25 C1 C26 118.6(10) . . ? C25 C1 C2 119.4(9) . . ? C26 C1 C2 122.1(9) . . ? O2 Cu2 O6 94.2(3) . . ? O2 Cu2 O1 157.2(3) . . ? O6 Cu2 O1 80.9(3) . . ? O2 Cu2 O5 94.0(3) . . ? O6 Cu2 O5 171.8(3) . . ? O1 Cu2 O5 91.3(3) . . ? O2 Cu2 O8 104.2(2) . . ? O6 Cu2 O8 91.2(3) . . ? O1 Cu2 O8 98.2(3) . . ? O5 Cu2 O8 87.5(2) . . ? C28 O2 Cu2 124.4(5) . . ? C1 C2 C3 112.6(9) . . ? C70 N3 C72 129.0(12) . . ? C70 N3 C71 114.0(11) . . ? C72 N3 C71 115.0(10) . . ? C27 C3 C4 117.8(9) . . ? C27 C3 C2 124.3(8) . . ? C4 C3 C2 117.7(9) . . ? C5 C4 C3 123.8(9) . . ? C8 O5 C9 115.5(7) . . ? C8 O5 Cu2 109.9(6) . . ? C9 O5 Cu2 108.8(5) . . ? C4 C5 C6 116.8(8) . . ? C4 C5 C30 122.4(9) . . ? C6 C5 C30 120.8(9) . . ? C50 O6 Cu1 128.1(6) . . ? C50 O6 Cu2 122.4(6) . . ? Cu1 O6 Cu2 100.5(3) . . ? C5 C6 C7 122.2(9) . . ? C49 O7 Cu1 127.4(7) . . ? C49 O7 Cu1 126.3(7) . 3_666 ? Cu1 O7 Cu1 101.1(3) . 3_666 ? C27 C7 C6 120.8(9) . . ? C27 C7 C8 118.3(8) . . ? C6 C7 C8 120.7(9) . . ? C73 O8 Cu2 134.6(7) . . ? O5 C8 C7 108.4(7) . . ? O5 C9 C10 111.0(7) . . ? C11 C10 C28 120.3(9) . . ? C11 C10 C9 120.4(9) . . ? C28 C10 C9 119.3(10) . . ? C10 C11 C12 123.5(9) . . ? C13 C12 C11 115.5(11) . . ? C13 C12 C34 124.1(10) . . ? C11 C12 C34 120.3(9) . . ? C12 C13 C14 122.9(10) . . ? C28 C14 C13 119.8(9) . . ? C28 C14 C15 120.2(10) . . ? C13 C14 C15 119.9(10) . . ? C14 C15 C16 114.9(7) . . ? C29 C16 C17 120.5(11) . . ? C29 C16 C15 121.9(10) . . ? C17 C16 C15 117.6(11) . . ? C18 C17 C16 120.0(12) . . ? C19 C18 C17 117.2(10) . . ? C19 C18 C38 116.8(15) . . ? C17 C18 C38 126.0(16) . . ? C19 C18 C38A 127.5(14) . . ? C17 C18 C38A 115.3(15) . . ? C38 C18 C38A 10.7(16) . . ? C18 C19 C20 124.6(11) . . ? C19 C20 C29 117.1(12) . . ? C19 C20 C21 122.1(11) . . ? C29 C20 C21 120.8(11) . . ? C20 C21 C22 113.6(9) . . ? C26 C22 C23 118.6(9) . . ? C26 C22 C21 122.3(9) . . ? C23 C22 C21 119.1(10) . . ? C22 C23 C24 120.7(11) . . ? C25 C24 C23 117.1(10) . . ? C25 C24 C42 125.5(10) . . ? C23 C24 C42 117.4(11) . . ? C1 C25 C24 123.5(10) . . ? C22 C26 O4 120.6(9) . . ? C22 C26 C1 121.4(9) . . ? O4 C26 C1 118.0(10) . . ? O1 C27 C7 118.4(8) . . ? O1 C27 C3 123.0(9) . . ? C7 C27 C3 118.6(8) . . ? O2 C28 C14 119.1(9) . . ? O2 C28 C10 123.1(9) . . ? C14 C28 C10 117.8(10) . . ? O3 C29 C16 122.7(10) . . ? O3 C29 C20 116.9(11) . . ? C16 C29 C20 120.2(11) . . ? C33 C30 C32 109.8(9) . . ? C33 C30 C31 108.0(9) . . ? C32 C30 C31 110.2(9) . . ? C33 C30 C5 112.4(8) . . ? C32 C30 C5 107.5(8) . . ? C31 C30 C5 109.0(9) . . ? C12 C34 C36 109.7(10) . . ? C12 C34 C35 110.0(9) . . ? C36 C34 C35 108.7(10) . . ? C12 C34 C37 112.1(9) . . ? C36 C34 C37 107.4(10) . . ? C35 C34 C37 108.9(10) . . ? C18 C38 C40 105.3(17) . . ? C18 C38 C39 111.5(19) . . ? C40 C38 C39 110.4(15) . . ? C18 C38 C41 114.3(19) . . ? C40 C38 C41 108.0(14) . . ? C39 C38 C41 107.3(14) . . ? C45 C42 C44 109.9(13) . . ? C45 C42 C43 106.2(13) . . ? C44 C42 C43 109.0(10) . . ? C45 C42 C24 109.7(11) . . ? C44 C42 C24 110.7(11) . . ? C43 C42 C24 111.3(11) . . ? O9 C70 N3 130.7(15) . . ? O8 C73 N1 125.7(10) . . ? C18 C38A C41A 110.9(18) . . ? C18 C38A C40A 115.8(19) . . ? C41A C38A C40A 111.3(14) . . ? C18 C38A C39A 104.5(19) . . ? C41A C38A C39A 106.9(15) . . ? C40A C38A C39A 106.8(15) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 22.72 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.672 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.097 _database_code_depnum_ccdc_archive 'CCDC 928623' ####################################################################### # # 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_Cu11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Cu11 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C114 H166 Cu11 N8 O36' _chemical_formula_weight 2923.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5485(7) _cell_length_b 14.4801(7) _cell_length_c 18.8246(10) _cell_angle_alpha 81.546(2) _cell_angle_beta 75.736(2) _cell_angle_gamma 62.611(2) _cell_volume 3175.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used . _cell_measurement_theta_min . _cell_measurement_theta_max . _exptl_crystal_description Needle _exptl_crystal_colour Brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1513 _exptl_absorpt_coefficient_mu 1.881 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6507 _exptl_absorpt_correction_T_max 0.7656 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 100(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 X8 Apex II CCD Diffractometer' _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 46912 _diffrn_reflns_av_R_equivalents 0.0737 _diffrn_reflns_av_sigmaI/netI 0.1386 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.11 _reflns_number_total 13470 _reflns_number_gt 7144 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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. A number of restraints were applied due to disorder present in upper rim tert-butyl groups, as well as DMF molecules that are disordered over two positions. All of this disorder has been modelled appropriately, also for the co-crystallised Et2O. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13470 _refine_ls_number_parameters 804 _refine_ls_number_restraints 177 _refine_ls_R_factor_all 0.1784 _refine_ls_R_factor_gt 0.0868 _refine_ls_wR_factor_ref 0.2404 _refine_ls_wR_factor_gt 0.2107 _refine_ls_goodness_of_fit_ref 1.271 _refine_ls_restrained_S_all 1.270 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.07180(8) 0.05691(7) 0.29447(5) 0.0227(3) Uani 1 1 d . . . O1 O 0.1003(4) -0.0823(4) 0.2776(3) 0.0237(12) Uani 1 1 d . . . N1 N 0.3844(13) 0.0177(12) 0.1743(8) 0.0375(11) Uani 0.50 1 d PD B 2 C1 C 0.1268(6) -0.0670(6) 0.1485(4) 0.0236(18) Uani 1 1 d . . . Cu2 Cu 0.22791(8) -0.03004(7) 0.40661(5) 0.0249(3) Uani 1 1 d . . . O2 O 0.2460(4) -0.1696(4) 0.3885(3) 0.0222(12) Uiso 1 1 d . . . N2 N 0.4312(13) -0.0229(12) 0.1968(8) 0.0375(11) Uani 0.50 1 d PD A 1 C2 C 0.1845(7) -0.1083(6) 0.0791(4) 0.0268(19) Uani 1 1 d . . . H2 H 0.1671 -0.0657 0.0362 0.032 Uiso 1 1 calc R . . Cu3 Cu 0.08933(9) -0.14107(9) 0.37577(6) 0.0407(3) Uani 1 1 d . . . O3 O 0.3885(4) -0.0874(4) 0.4143(3) 0.0243(12) Uani 1 1 d . . . N3 N -0.2759(13) 0.4379(11) 0.5169(10) 0.0436(13) Uani 0.50 1 d PD C 1 C3 C 0.2678(7) -0.2120(6) 0.0725(4) 0.0250(19) Uani 1 1 d . . . Cu4 Cu 0.0000 0.0000 0.5000 0.0376(4) Uani 1 2 d S . . O4 O 0.1996(4) 0.1043(4) 0.4413(3) 0.0248(13) Uani 1 1 d . . . N4 N -0.2327(12) 0.4403(12) 0.5285(8) 0.0436(13) Uani 0.50 1 d PD D 2 C4 C 0.2883(6) -0.2697(6) 0.1371(4) 0.0215(18) Uani 1 1 d . . . H4 H 0.3429 -0.3406 0.1336 0.026 Uiso 1 1 calc R . . Cu5 Cu -0.01694(8) 0.17497(7) 0.42456(5) 0.0263(3) Uani 1 1 d . . . O5 O 0.0260(4) 0.1968(4) 0.3198(3) 0.0287(13) Uani 1 1 d . . . N5 N 0.1755(6) -0.0833(5) 0.6114(4) 0.0267(16) Uani 1 1 d . . . C5 C 0.2346(6) -0.2314(6) 0.2071(4) 0.0223(18) Uani 1 1 d . . . Cu6 Cu 0.11969(8) 0.14154(8) 0.54297(5) 0.0254(3) Uani 1 1 d . . . O6 O 0.0601(4) 0.1063(4) 0.1882(3) 0.0246(12) Uani 1 1 d . . . N6 N 0.2152(8) 0.2658(9) 0.5527(5) 0.056(3) Uani 1 1 d . . . C6 C 0.1537(6) -0.1269(6) 0.2123(4) 0.0224(18) Uani 1 1 d . . . O7 O 0.2669(5) 0.0077(5) 0.2775(3) 0.0375(11) Uani 1 1 d D . . C7 C 0.2640(6) -0.3018(6) 0.2746(4) 0.0217(17) Uani 1 1 d . . . H7A H 0.1963 -0.2777 0.3149 0.026 Uiso 1 1 calc R . . H7B H 0.2813 -0.3731 0.2636 0.026 Uiso 1 1 calc R . . O8 O 0.0699(4) 0.0260(4) 0.3999(3) 0.0215(12) Uani 1 1 d . . . C8 C 0.3609(6) -0.3067(6) 0.3008(4) 0.0219(18) Uani 1 1 d . . . O9 O 0.0115(4) -0.1299(4) 0.4754(3) 0.0228(12) Uani 1 1 d . . . C9 C 0.4734(6) -0.3755(6) 0.2681(4) 0.0232(18) Uani 1 1 d . . . H9 H 0.4829 -0.4183 0.2309 0.028 Uiso 1 1 calc R . . O10 O 0.0182(5) 0.1882(5) 0.6356(3) 0.0400(16) Uani 1 1 d D . . C10 C 0.5700(7) -0.3847(6) 0.2865(5) 0.030(2) Uani 1 1 d . G . O11 O -0.1260(5) 0.3180(4) 0.4473(3) 0.0436(13) Uani 1 1 d D . . C11 C 0.5530(7) -0.3251(6) 0.3452(4) 0.0255(19) Uani 1 1 d . . . H11 H 0.6169 -0.3311 0.3614 0.031 Uiso 1 1 calc R . . O12 O 0.2223(5) -0.0226(5) 0.5985(3) 0.0437(16) Uani 1 1 d . . . C12 C 0.4470(6) -0.2592(6) 0.3792(4) 0.0218(18) Uani 1 1 d . . . O13 O 0.1774(5) -0.1281(5) 0.5593(4) 0.0487(18) Uani 1 1 d . . . C13 C 0.3493(6) -0.2431(5) 0.3561(4) 0.0205(17) Uani 1 1 d . . . O14 O 0.1354(4) -0.0985(4) 0.6738(3) 0.0318(14) Uani 1 1 d . . . C14 C 0.4316(7) -0.1951(6) 0.4410(4) 0.0247(18) Uani 1 1 d . . . H14A H 0.3772 -0.2037 0.4843 0.030 Uiso 1 1 calc R . . H14B H 0.5051 -0.2174 0.4555 0.030 Uiso 1 1 calc R . . O15 O 0.2418(5) 0.1669(6) 0.5625(3) 0.0428(17) Uani 1 1 d . . . C15 C 0.4245(7) -0.0255(6) 0.4478(4) 0.0269(19) Uani 1 1 d . . . H15A H 0.5076 -0.0618 0.4448 0.032 Uiso 1 1 calc R . . H15B H 0.3865 -0.0156 0.5002 0.032 Uiso 1 1 calc R . . O16 O 0.2825(7) 0.2963(7) 0.5619(5) 0.092(3) Uani 1 1 d . . . C16 C 0.3928(6) 0.0775(6) 0.4073(4) 0.0204(18) Uani 1 1 d . . . O17 O 0.1279(6) 0.3240(6) 0.5310(4) 0.058(2) Uani 1 1 d . . . C17 C 0.4743(6) 0.1098(6) 0.3695(4) 0.0248(19) Uani 1 1 d . . . H17 H 0.5521 0.0649 0.3694 0.030 Uiso 1 1 calc R . . O18 O 0.2139(13) 0.1097(12) -0.0302(10) 0.058(3) Uani 0.50 1 d PDU E 1 C18 C 0.4454(6) 0.2054(6) 0.3322(4) 0.0234(18) Uani 1 1 d . . . O19 O 0.2851(9) 0.1225(8) -0.1258(5) 0.035(3) Uani 0.50 1 d PDU F 2 C19 C 0.3300(6) 0.2687(6) 0.3344(4) 0.0265(19) Uani 1 1 d . . . H19 H 0.3079 0.3355 0.3104 0.032 Uiso 1 1 calc R . . C20 C 0.2457(7) 0.2390(6) 0.3700(4) 0.0268(19) Uani 1 1 d . . . C21 C 0.2777(6) 0.1423(6) 0.4064(4) 0.0234(18) Uani 1 1 d . . . C22 C 0.1235(6) 0.3150(6) 0.3689(5) 0.028(2) Uani 1 1 d . . . H22A H 0.0733 0.2901 0.4051 0.034 Uiso 1 1 calc R . . H22B H 0.1088 0.3833 0.3844 0.034 Uiso 1 1 calc R . . C23 C 0.0927(6) 0.3294(6) 0.2948(5) 0.031(2) Uani 1 1 d . . . C24 C 0.1141(7) 0.4013(6) 0.2436(5) 0.034(2) Uani 1 1 d . . . H24 H 0.1399 0.4449 0.2585 0.041 Uiso 1 1 calc R . . C25 C 0.0993(7) 0.4122(7) 0.1709(6) 0.040(2) Uani 1 1 d . H . C26 C 0.0581(7) 0.3513(6) 0.1517(5) 0.032(2) Uani 1 1 d . . . H26 H 0.0473 0.3570 0.1030 0.038 Uiso 1 1 calc R . . C27 C 0.0314(7) 0.2807(6) 0.2022(4) 0.030(2) Uani 1 1 d . . . C28 C 0.0503(6) 0.2675(6) 0.2733(5) 0.028(2) Uani 1 1 d . . . C29 C -0.0179(7) 0.2166(6) 0.1808(5) 0.0272(19) Uani 1 1 d . . . H29A H -0.0929 0.2314 0.2130 0.033 Uiso 1 1 calc R . . H29B H -0.0283 0.2347 0.1295 0.033 Uiso 1 1 calc R . . C30 C 0.0308(6) 0.0404(6) 0.1540(4) 0.0256(19) Uani 1 1 d . . . H30A H 0.0167 0.0695 0.1045 0.031 Uiso 1 1 calc R . . H30B H -0.0393 0.0379 0.1839 0.031 Uiso 1 1 calc R . . C31 C 0.3309(7) -0.2534(6) -0.0042(5) 0.034(2) Uani 1 1 d . . . C32 C 0.2451(9) -0.2450(7) -0.0492(5) 0.047(3) Uani 1 1 d . . . H32A H 0.2864 -0.2752 -0.0971 0.071 Uiso 1 1 calc R . . H32B H 0.1928 -0.1716 -0.0561 0.071 Uiso 1 1 calc R . . H32C H 0.2021 -0.2829 -0.0227 0.071 Uiso 1 1 calc R . . C33 C 0.4192(8) -0.3639(7) -0.0023(5) 0.048(3) Uani 1 1 d . . . H33A H 0.4761 -0.3693 0.0236 0.071 Uiso 1 1 calc R . . H33B H 0.4560 -0.3867 -0.0526 0.071 Uiso 1 1 calc R . . H33C H 0.3833 -0.4083 0.0232 0.071 Uiso 1 1 calc R . . C34 C 0.3914(9) -0.1863(7) -0.0442(5) 0.046(3) Uani 1 1 d . . . H34A H 0.4505 -0.1955 -0.0187 0.069 Uiso 1 1 calc R . . H34B H 0.3360 -0.1128 -0.0443 0.069 Uiso 1 1 calc R . . H34C H 0.4260 -0.2080 -0.0948 0.069 Uiso 1 1 calc R . . C35 C 0.6916(7) -0.4565(6) 0.2480(5) 0.0431(15) Uani 1 1 d D . . C36 C 0.6952(10) -0.5194(10) 0.1890(7) 0.0431(15) Uani 0.70 1 d PD G 2 H36A H 0.6520 -0.5592 0.2100 0.065 Uiso 0.70 1 calc PR G 2 H36B H 0.7742 -0.5674 0.1695 0.065 Uiso 0.70 1 calc PR G 2 H36C H 0.6618 -0.4724 0.1493 0.065 Uiso 0.70 1 calc PR G 2 C37 C 0.723(2) -0.5717(14) 0.2707(17) 0.0431(15) Uani 0.30 1 d PD G 1 H37A H 0.6690 -0.5912 0.2587 0.065 Uiso 0.30 1 calc PR G 1 H37B H 0.7208 -0.5820 0.3236 0.065 Uiso 0.30 1 calc PR G 1 H37C H 0.7999 -0.6153 0.2443 0.065 Uiso 0.30 1 calc PR G 1 C38 C 0.7499(10) -0.5375(9) 0.3066(7) 0.0431(15) Uani 0.70 1 d PD G 2 H38A H 0.7078 -0.5786 0.3265 0.065 Uiso 0.70 1 calc PR G 2 H38B H 0.7508 -0.5013 0.3464 0.065 Uiso 0.70 1 calc PR G 2 H38C H 0.8280 -0.5839 0.2840 0.065 Uiso 0.70 1 calc PR G 2 C39 C 0.782(2) -0.438(2) 0.2714(18) 0.0431(15) Uani 0.30 1 d PD G 1 H39A H 0.7689 -0.3660 0.2589 0.065 Uiso 0.30 1 calc PR G 1 H39B H 0.8572 -0.4854 0.2457 0.065 Uiso 0.30 1 calc PR G 1 H39C H 0.7761 -0.4514 0.3244 0.065 Uiso 0.30 1 calc PR G 1 C40 C 0.7571(10) -0.3943(10) 0.2171(8) 0.0431(15) Uani 0.70 1 d PD G 2 H40A H 0.7545 -0.3546 0.2560 0.065 Uiso 0.70 1 calc PR G 2 H40B H 0.7232 -0.3461 0.1779 0.065 Uiso 0.70 1 calc PR G 2 H40C H 0.8362 -0.4415 0.1971 0.065 Uiso 0.70 1 calc PR G 2 C41 C 0.699(2) -0.394(2) 0.1707(12) 0.0431(15) Uani 0.30 1 d PD G 1 H41A H 0.6451 -0.3942 0.1444 0.065 Uiso 0.30 1 calc PR G 1 H41B H 0.7761 -0.4274 0.1414 0.065 Uiso 0.30 1 calc PR G 1 H41C H 0.6802 -0.3220 0.1791 0.065 Uiso 0.30 1 calc PR G 1 C42 C 0.5372(6) 0.2407(6) 0.2937(4) 0.0246(18) Uani 1 1 d . . . C43 C 0.6414(7) 0.1527(6) 0.2503(4) 0.030(2) Uani 1 1 d . . . H43A H 0.6744 0.0936 0.2838 0.045 Uiso 1 1 calc R . . H43B H 0.6980 0.1779 0.2264 0.045 Uiso 1 1 calc R . . H43C H 0.6183 0.1308 0.2130 0.045 Uiso 1 1 calc R . . C44 C 0.5788(7) 0.2718(7) 0.3520(5) 0.037(2) Uani 1 1 d . . . H44A H 0.6096 0.2121 0.3856 0.055 Uiso 1 1 calc R . . H44B H 0.5150 0.3297 0.3796 0.055 Uiso 1 1 calc R . . H44C H 0.6381 0.2933 0.3275 0.055 Uiso 1 1 calc R . . C45 C 0.4920(7) 0.3338(7) 0.2399(5) 0.037(2) Uani 1 1 d . . . H45A H 0.5533 0.3525 0.2149 0.056 Uiso 1 1 calc R . . H45B H 0.4298 0.3933 0.2670 0.056 Uiso 1 1 calc R . . H45C H 0.4640 0.3150 0.2037 0.056 Uiso 1 1 calc R . . C46 C 0.1317(8) 0.4893(7) 0.1160(6) 0.051(2) Uani 1 1 d DU . . C47 C 0.2171(18) 0.4303(17) 0.0462(11) 0.071(6) Uani 0.50 1 d PDU H 2 H47A H 0.1863 0.3915 0.0275 0.107 Uiso 0.50 1 calc PR H 2 H47B H 0.2900 0.3819 0.0593 0.107 Uiso 0.50 1 calc PR H 2 H47C H 0.2282 0.4808 0.0083 0.107 Uiso 0.50 1 calc PR H 2 C48 C 0.2590(13) 0.4538(17) 0.1027(14) 0.061(5) Uani 0.50 1 d PDU H 1 H48A H 0.2827 0.4397 0.1498 0.092 Uiso 0.50 1 calc PR H 1 H48B H 0.2775 0.5085 0.0748 0.092 Uiso 0.50 1 calc PR H 1 H48C H 0.2989 0.3902 0.0748 0.092 Uiso 0.50 1 calc PR H 1 C49 C 0.183(2) 0.5472(17) 0.1399(13) 0.066(5) Uani 0.50 1 d PDU H 2 H49A H 0.1312 0.5888 0.1819 0.098 Uiso 0.50 1 calc PR H 2 H49B H 0.1976 0.5934 0.0994 0.098 Uiso 0.50 1 calc PR H 2 H49C H 0.2551 0.4978 0.1540 0.098 Uiso 0.50 1 calc PR H 2 C50 C 0.0834(17) 0.5928(12) 0.1590(10) 0.047(4) Uani 0.50 1 d PDU H 1 H50A H 0.1159 0.5769 0.2029 0.071 Uiso 0.50 1 calc PR H 1 H50B H 0.0006 0.6214 0.1734 0.071 Uiso 0.50 1 calc PR H 1 H50C H 0.1040 0.6438 0.1272 0.071 Uiso 0.50 1 calc PR H 1 C51 C 0.0293(17) 0.5585(18) 0.0797(13) 0.059(6) Uani 0.50 1 d PDU H 2 H51A H -0.0002 0.5150 0.0657 0.089 Uiso 0.50 1 calc PR H 2 H51B H 0.0534 0.5949 0.0360 0.089 Uiso 0.50 1 calc PR H 2 H51C H -0.0303 0.6096 0.1145 0.089 Uiso 0.50 1 calc PR H 2 C52 C 0.089(2) 0.5112(18) 0.0489(10) 0.052(5) Uani 0.50 1 d PDU H 1 H52A H 0.0067 0.5325 0.0612 0.078 Uiso 0.50 1 calc PR H 1 H52B H 0.1268 0.4485 0.0201 0.078 Uiso 0.50 1 calc PR H 1 H52C H 0.1034 0.5673 0.0201 0.078 Uiso 0.50 1 calc PR H 1 C53 C 0.3117(14) 0.0547(15) 0.2367(10) 0.0375(11) Uani 0.50 1 d PD B 2 H53 H 0.2945 0.1224 0.2494 0.045 Uiso 0.50 1 calc PR B 2 C54 C 0.4403(15) 0.0770(14) 0.1317(9) 0.0375(11) Uani 0.50 1 d P B 2 H54A H 0.4895 0.0404 0.0871 0.056 Uiso 0.50 1 calc PR B 2 H54B H 0.4863 0.0858 0.1606 0.056 Uiso 0.50 1 calc PR B 2 H54C H 0.3834 0.1455 0.1183 0.056 Uiso 0.50 1 calc PR B 2 C55 C 0.4203(16) -0.0846(15) 0.1498(10) 0.0375(11) Uani 0.50 1 d P B 2 H55A H 0.4723 -0.0942 0.1020 0.056 Uiso 0.50 1 calc PR B 2 H55B H 0.3539 -0.0922 0.1453 0.056 Uiso 0.50 1 calc PR B 2 H55C H 0.4592 -0.1371 0.1854 0.056 Uiso 0.50 1 calc PR B 2 C57 C 0.5376(15) -0.0036(14) 0.1749(10) 0.0375(11) Uani 0.50 1 d P A 1 H57A H 0.5942 -0.0532 0.1381 0.056 Uiso 0.50 1 calc PR A 1 H57B H 0.5695 -0.0127 0.2182 0.056 Uiso 0.50 1 calc PR A 1 H57C H 0.5169 0.0675 0.1542 0.056 Uiso 0.50 1 calc PR A 1 C58 C 0.4500(16) -0.1220(15) 0.1793(10) 0.0375(11) Uani 0.50 1 d P A 1 H58A H 0.5204 -0.1520 0.1425 0.056 Uiso 0.50 1 calc PR A 1 H58B H 0.3863 -0.1151 0.1596 0.056 Uiso 0.50 1 calc PR A 1 H58C H 0.4564 -0.1676 0.2236 0.056 Uiso 0.50 1 calc PR A 1 C59 C 0.0590(8) 0.1821(10) 0.6988(5) 0.068(4) Uani 1 1 d D . . H59A H 0.1163 0.1109 0.7063 0.102 Uiso 1 1 calc R . . H59B H -0.0041 0.2009 0.7414 0.102 Uiso 1 1 calc R . . H59C H 0.0932 0.2302 0.6927 0.102 Uiso 1 1 calc R . . C60 C -0.2153(13) 0.3469(12) 0.4855(9) 0.0436(13) Uani 0.50 1 d PD C 1 H60 H -0.2486 0.3001 0.4954 0.052 Uiso 0.50 1 calc PR C 1 C61 C -0.3958(13) 0.4731(14) 0.5390(11) 0.0436(13) Uani 0.50 1 d PD C 1 H61A H -0.4305 0.5415 0.5604 0.065 Uiso 0.50 1 calc PR C 1 H61B H -0.4118 0.4235 0.5755 0.065 Uiso 0.50 1 calc PR C 1 H61C H -0.4275 0.4786 0.4962 0.065 Uiso 0.50 1 calc PR C 1 C62 C -0.2350(15) 0.5063(14) 0.5307(11) 0.0436(13) Uani 0.50 1 d PD C 1 H62A H -0.2988 0.5682 0.5542 0.065 Uiso 0.50 1 calc PR C 1 H62B H -0.1975 0.5273 0.4842 0.065 Uiso 0.50 1 calc PR C 1 H62C H -0.1806 0.4709 0.5631 0.065 Uiso 0.50 1 calc PR C 1 C63 C -0.1378(14) 0.3648(12) 0.4966(9) 0.0436(13) Uani 0.50 1 d PD D 2 H63 H -0.0722 0.3465 0.5157 0.052 Uiso 0.50 1 calc PR D 2 C64 C -0.3381(16) 0.4698(15) 0.5052(11) 0.0436(13) Uani 0.50 1 d PD D 2 H64A H -0.3998 0.5273 0.5343 0.065 Uiso 0.50 1 calc PR D 2 H64B H -0.3556 0.4100 0.5124 0.065 Uiso 0.50 1 calc PR D 2 H64C H -0.3302 0.4918 0.4532 0.065 Uiso 0.50 1 calc PR D 2 C65 C -0.2374(16) 0.4957(13) 0.5871(10) 0.0436(13) Uani 0.50 1 d PD D 2 H65A H -0.3155 0.5483 0.6032 0.065 Uiso 0.50 1 calc PR D 2 H65B H -0.1874 0.5298 0.5702 0.065 Uiso 0.50 1 calc PR D 2 H65C H -0.2125 0.4469 0.6282 0.065 Uiso 0.50 1 calc PR D 2 C66 C 0.3206(19) 0.1052(18) 0.0498(12) 0.073(6) Uani 0.50 1 d PDU E 1 H66A H 0.3505 0.1444 0.0689 0.110 Uiso 0.50 1 calc PR E 1 H66B H 0.3839 0.0447 0.0244 0.110 Uiso 0.50 1 calc PR E 1 H66C H 0.2755 0.0817 0.0905 0.110 Uiso 0.50 1 calc PR E 1 C67 C 0.247(2) 0.1736(17) -0.0029(14) 0.061(5) Uani 0.50 1 d PDU E 1 H67A H 0.1801 0.2330 0.0224 0.073 Uiso 0.50 1 calc PR E 1 H67B H 0.2903 0.2011 -0.0432 0.073 Uiso 0.50 1 calc PR E 1 C68 C 0.137(2) 0.1656(16) -0.0766(12) 0.056(4) Uani 0.50 1 d PDU E 1 H68A H 0.1752 0.1918 -0.1210 0.067 Uiso 0.50 1 calc PR E 1 H68B H 0.0722 0.2261 -0.0511 0.067 Uiso 0.50 1 calc PR E 1 C69 C 0.096(2) 0.0952(18) -0.0981(13) 0.074(6) Uani 0.50 1 d PDU E 1 H69A H 0.0457 0.1329 -0.1327 0.111 Uiso 0.50 1 calc PR E 1 H69B H 0.0545 0.0730 -0.0543 0.111 Uiso 0.50 1 calc PR E 1 H69C H 0.1612 0.0339 -0.1213 0.111 Uiso 0.50 1 calc PR E 1 C70 C 0.3503(13) 0.1188(12) -0.2557(8) 0.029(4) Uani 0.50 1 d PDU F 2 H70A H 0.3266 0.1256 -0.3022 0.044 Uiso 0.50 1 calc PR F 2 H70B H 0.4135 0.0499 -0.2514 0.044 Uiso 0.50 1 calc PR F 2 H70C H 0.3746 0.1726 -0.2546 0.044 Uiso 0.50 1 calc PR F 2 C71 C 0.2514(13) 0.1316(13) -0.1924(7) 0.033(4) Uani 0.50 1 d PDU F 2 H71A H 0.1869 0.2007 -0.1970 0.040 Uiso 0.50 1 calc PR F 2 H71B H 0.2264 0.0776 -0.1935 0.040 Uiso 0.50 1 calc PR F 2 C72 C 0.1965(19) 0.138(2) -0.0630(10) 0.051(4) Uani 0.50 1 d PDU F 2 H72A H 0.1668 0.0861 -0.0605 0.061 Uiso 0.50 1 calc PR F 2 H72B H 0.1333 0.2084 -0.0654 0.061 Uiso 0.50 1 calc PR F 2 C73 C 0.248(2) 0.1240(19) 0.0052(12) 0.048(5) Uani 0.50 1 d PDU F 2 H73A H 0.1893 0.1315 0.0498 0.073 Uiso 0.50 1 calc PR F 2 H73B H 0.2740 0.1772 0.0029 0.073 Uiso 0.50 1 calc PR F 2 H73C H 0.3116 0.0547 0.0059 0.073 Uiso 0.50 1 calc PR F 2 C56 C 0.3399(13) 0.0345(15) 0.2453(10) 0.0375(11) Uani 0.50 1 d PD A 1 H56 H 0.3310 0.1006 0.2553 0.045 Uiso 0.50 1 calc PR A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0172(5) 0.0209(5) 0.0227(5) -0.0075(4) -0.0023(4) -0.0014(4) O1 0.026(3) 0.016(3) 0.021(3) -0.006(2) -0.005(2) -0.001(2) N1 0.035(3) 0.040(3) 0.031(3) -0.004(2) 0.001(2) -0.014(2) C1 0.021(4) 0.019(4) 0.029(5) -0.008(4) -0.006(4) -0.006(4) Cu2 0.0182(5) 0.0262(6) 0.0261(6) -0.0113(4) -0.0011(4) -0.0051(4) N2 0.035(3) 0.040(3) 0.031(3) -0.004(2) 0.001(2) -0.014(2) C2 0.033(5) 0.026(5) 0.015(4) 0.004(3) -0.009(4) -0.008(4) Cu3 0.0339(7) 0.0511(8) 0.0340(7) -0.0079(5) -0.0051(5) -0.0152(6) O3 0.025(3) 0.022(3) 0.025(3) -0.008(2) -0.009(2) -0.005(2) N3 0.039(3) 0.024(2) 0.044(3) -0.003(2) 0.011(2) -0.003(2) C3 0.023(4) 0.016(4) 0.029(5) -0.005(4) -0.002(4) -0.004(4) Cu4 0.0321(9) 0.0428(10) 0.0320(9) -0.0054(7) -0.0060(7) -0.0108(8) O4 0.017(3) 0.023(3) 0.030(3) -0.007(2) -0.003(2) -0.005(2) N4 0.039(3) 0.024(2) 0.044(3) -0.003(2) 0.011(2) -0.003(2) C4 0.025(4) 0.016(4) 0.020(4) -0.004(3) -0.003(3) -0.006(3) Cu5 0.0179(5) 0.0244(6) 0.0284(6) -0.0106(4) -0.0016(4) -0.0012(4) O5 0.028(3) 0.022(3) 0.031(3) -0.009(3) 0.002(3) -0.008(3) N5 0.020(4) 0.034(4) 0.027(4) 0.003(3) -0.010(3) -0.011(3) C5 0.014(4) 0.028(5) 0.024(4) -0.001(4) -0.005(3) -0.008(4) Cu6 0.0163(5) 0.0319(6) 0.0267(6) -0.0121(4) 0.0009(4) -0.0090(4) O6 0.021(3) 0.016(3) 0.026(3) 0.000(2) -0.010(2) 0.002(2) N6 0.042(6) 0.084(8) 0.058(6) -0.046(5) 0.010(5) -0.039(6) C6 0.023(4) 0.021(4) 0.027(5) -0.005(4) -0.009(4) -0.010(4) O7 0.035(3) 0.040(3) 0.031(3) -0.004(2) 0.001(2) -0.014(2) C7 0.021(4) 0.018(4) 0.022(4) 0.000(3) -0.001(3) -0.007(3) O8 0.014(3) 0.023(3) 0.021(3) -0.010(2) 0.001(2) -0.002(2) C8 0.026(4) 0.014(4) 0.020(4) 0.004(3) -0.008(3) -0.003(3) O9 0.015(3) 0.030(3) 0.022(3) -0.006(2) -0.002(2) -0.007(2) C9 0.022(4) 0.016(4) 0.019(4) 0.000(3) -0.006(3) 0.002(3) O10 0.032(3) 0.056(4) 0.040(4) -0.032(3) 0.015(3) -0.028(3) C10 0.020(4) 0.028(5) 0.033(5) -0.001(4) -0.006(4) -0.002(4) O11 0.039(3) 0.024(2) 0.044(3) -0.003(2) 0.011(2) -0.003(2) C11 0.025(5) 0.023(4) 0.020(4) 0.002(3) -0.009(4) -0.002(4) O12 0.028(4) 0.041(4) 0.047(4) 0.009(3) -0.007(3) -0.007(3) C12 0.026(5) 0.017(4) 0.019(4) -0.002(3) -0.005(3) -0.006(4) O13 0.015(3) 0.071(5) 0.052(4) -0.028(4) -0.008(3) -0.004(3) C13 0.022(4) 0.012(4) 0.018(4) 0.005(3) -0.004(3) 0.000(3) O14 0.023(3) 0.048(4) 0.021(3) 0.000(3) 0.000(3) -0.015(3) C14 0.026(4) 0.023(5) 0.022(4) -0.003(4) -0.009(4) -0.006(4) O15 0.023(3) 0.071(5) 0.035(4) -0.027(3) 0.005(3) -0.019(3) C15 0.030(5) 0.031(5) 0.020(4) -0.006(4) -0.012(4) -0.010(4) O16 0.048(5) 0.120(8) 0.136(8) -0.070(6) 0.002(5) -0.051(5) C16 0.022(4) 0.018(4) 0.020(4) -0.007(3) -0.007(3) -0.003(3) O17 0.047(5) 0.066(5) 0.070(5) -0.034(4) 0.010(4) -0.035(4) C17 0.015(4) 0.029(5) 0.023(4) -0.015(4) 0.000(3) -0.002(4) O18 0.054(6) 0.052(7) 0.056(7) 0.009(6) -0.011(6) -0.016(5) C18 0.024(4) 0.025(5) 0.018(4) -0.012(4) -0.003(3) -0.006(4) O19 0.033(5) 0.027(5) 0.024(5) 0.005(4) 0.005(4) -0.004(4) C19 0.019(4) 0.031(5) 0.026(5) -0.015(4) -0.001(3) -0.006(4) C20 0.024(5) 0.025(5) 0.029(5) -0.012(4) -0.005(4) -0.006(4) C21 0.020(4) 0.028(5) 0.021(4) -0.011(4) -0.001(3) -0.008(4) C22 0.013(4) 0.013(4) 0.050(6) -0.013(4) 0.004(4) 0.000(3) C23 0.010(4) 0.028(5) 0.046(6) -0.008(4) -0.005(4) 0.001(4) C24 0.021(5) 0.016(4) 0.062(7) -0.003(4) -0.011(4) -0.004(4) C25 0.014(4) 0.033(5) 0.064(7) 0.009(5) -0.009(4) -0.005(4) C26 0.025(5) 0.023(5) 0.039(5) 0.008(4) -0.007(4) -0.007(4) C27 0.019(4) 0.028(5) 0.028(5) -0.006(4) 0.000(4) 0.000(4) C28 0.012(4) 0.014(4) 0.043(5) -0.011(4) -0.001(4) 0.008(3) C29 0.021(4) 0.019(4) 0.030(5) 0.003(4) -0.001(4) -0.002(4) C30 0.022(4) 0.017(4) 0.023(4) -0.003(3) -0.005(3) 0.004(3) C31 0.044(6) 0.016(4) 0.030(5) -0.005(4) -0.003(4) -0.005(4) C32 0.062(7) 0.038(6) 0.037(6) -0.012(5) -0.002(5) -0.020(5) C33 0.051(6) 0.033(5) 0.033(5) -0.012(4) 0.013(5) -0.006(5) C34 0.060(7) 0.044(6) 0.028(5) -0.003(4) 0.006(5) -0.025(5) C35 0.021(3) 0.037(3) 0.058(4) -0.021(3) -0.002(3) 0.001(2) C36 0.021(3) 0.037(3) 0.058(4) -0.021(3) -0.002(3) 0.001(2) C37 0.021(3) 0.037(3) 0.058(4) -0.021(3) -0.002(3) 0.001(2) C38 0.021(3) 0.037(3) 0.058(4) -0.021(3) -0.002(3) 0.001(2) C39 0.021(3) 0.037(3) 0.058(4) -0.021(3) -0.002(3) 0.001(2) C40 0.021(3) 0.037(3) 0.058(4) -0.021(3) -0.002(3) 0.001(2) C41 0.021(3) 0.037(3) 0.058(4) -0.021(3) -0.002(3) 0.001(2) C42 0.019(4) 0.023(4) 0.024(4) -0.006(4) 0.000(3) -0.004(4) C43 0.030(5) 0.031(5) 0.026(5) -0.002(4) -0.004(4) -0.011(4) C44 0.036(5) 0.042(6) 0.033(5) -0.011(4) -0.004(4) -0.016(5) C45 0.020(5) 0.038(5) 0.040(5) -0.002(4) 0.005(4) -0.006(4) C46 0.038(5) 0.044(5) 0.069(6) 0.025(5) -0.017(5) -0.021(4) C47 0.053(10) 0.062(10) 0.074(11) 0.026(9) -0.001(9) -0.018(8) C48 0.042(9) 0.054(9) 0.087(11) 0.035(9) -0.025(8) -0.025(7) C49 0.060(10) 0.063(10) 0.071(10) 0.021(9) -0.024(9) -0.026(8) C50 0.059(10) 0.039(9) 0.067(10) 0.024(8) -0.046(9) -0.032(8) C51 0.063(12) 0.057(12) 0.058(11) 0.028(9) -0.016(10) -0.034(9) C52 0.057(10) 0.048(10) 0.051(10) 0.017(8) -0.014(9) -0.027(8) C53 0.035(3) 0.040(3) 0.031(3) -0.004(2) 0.001(2) -0.014(2) C54 0.035(3) 0.040(3) 0.031(3) -0.004(2) 0.001(2) -0.014(2) C55 0.035(3) 0.040(3) 0.031(3) -0.004(2) 0.001(2) -0.014(2) C57 0.035(3) 0.040(3) 0.031(3) -0.004(2) 0.001(2) -0.014(2) C58 0.035(3) 0.040(3) 0.031(3) -0.004(2) 0.001(2) -0.014(2) C59 0.041(6) 0.102(10) 0.049(7) -0.041(6) 0.029(5) -0.030(7) C60 0.039(3) 0.024(2) 0.044(3) -0.003(2) 0.011(2) -0.003(2) C61 0.039(3) 0.024(2) 0.044(3) -0.003(2) 0.011(2) -0.003(2) C62 0.039(3) 0.024(2) 0.044(3) -0.003(2) 0.011(2) -0.003(2) C63 0.039(3) 0.024(2) 0.044(3) -0.003(2) 0.011(2) -0.003(2) C64 0.039(3) 0.024(2) 0.044(3) -0.003(2) 0.011(2) -0.003(2) C65 0.039(3) 0.024(2) 0.044(3) -0.003(2) 0.011(2) -0.003(2) C66 0.064(11) 0.072(12) 0.066(12) -0.006(10) -0.006(10) -0.018(10) C67 0.064(8) 0.054(9) 0.058(9) 0.001(8) -0.011(7) -0.023(8) C68 0.055(8) 0.053(8) 0.051(8) 0.011(7) -0.016(7) -0.015(7) C69 0.069(13) 0.073(13) 0.079(14) 0.004(12) -0.030(11) -0.024(11) C70 0.045(10) 0.016(8) 0.022(8) 0.008(6) -0.007(7) -0.011(7) C71 0.035(7) 0.024(7) 0.024(7) 0.001(6) -0.004(6) -0.001(6) C72 0.047(7) 0.044(7) 0.041(7) 0.012(6) -0.004(6) -0.009(6) C73 0.059(9) 0.046(10) 0.037(9) 0.000(9) -0.005(7) -0.024(9) C56 0.035(3) 0.040(3) 0.031(3) -0.004(2) 0.001(2) -0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O5 1.922(5) . ? Cu1 O1 1.930(5) . ? Cu1 O8 1.965(5) . ? Cu1 O6 2.042(5) . ? Cu1 O7 2.349(6) . ? Cu1 Cu5 2.8730(13) . ? Cu1 Cu3 2.9799(15) . ? O1 C6 1.348(9) . ? O1 Cu3 1.919(5) . ? N1 C53 1.329(16) . ? N1 C54 1.43(2) . ? N1 C55 1.44(2) . ? C1 C6 1.396(11) . ? C1 C2 1.404(10) . ? C1 C30 1.497(10) . ? Cu2 O8 1.940(5) . ? Cu2 O3 1.976(5) . ? Cu2 O4 1.981(5) . ? Cu2 O2 1.992(5) . ? Cu2 O7 2.393(6) . ? Cu2 Cu4 3.0214(10) . ? O2 C13 1.365(8) . ? O2 Cu3 2.036(5) . ? N2 C56 1.332(15) . ? N2 C58 1.41(2) . ? N2 C57 1.54(2) . ? C2 C3 1.404(10) . ? Cu3 O9 1.901(5) . ? Cu3 O10 1.936(5) 2_556 ? Cu3 O8 2.409(5) . ? Cu3 Cu6 2.8705(15) 2_556 ? Cu3 Cu4 2.9735(11) . ? O3 C14 1.449(9) . ? O3 C15 1.469(9) . ? N3 C60 1.324(15) . ? N3 C62 1.416(16) . ? N3 C61 1.429(16) . ? C3 C4 1.380(10) . ? C3 C31 1.533(11) . ? Cu4 O9 1.930(5) 2_556 ? Cu4 O9 1.930(5) . ? Cu4 O8 1.957(5) . ? Cu4 O8 1.957(5) 2_556 ? Cu4 Cu5 2.6563(10) . ? Cu4 Cu5 2.6563(10) 2_556 ? Cu4 Cu3 2.9735(11) 2_556 ? Cu4 Cu2 3.0214(10) 2_556 ? O4 C21 1.392(9) . ? O4 Cu6 1.967(5) . ? N4 C63 1.314(15) . ? N4 C65 1.430(16) . ? N4 C64 1.452(16) . ? C4 C5 1.395(10) . ? Cu5 O9 1.908(5) 2_556 ? Cu5 O5 1.937(5) . ? Cu5 O11 1.946(6) . ? Cu5 O8 1.986(5) . ? O5 C28 1.352(10) . ? N5 O14 1.201(8) . ? N5 O13 1.243(8) . ? N5 O12 1.268(9) . ? C5 C6 1.401(10) . ? C5 C7 1.519(10) . ? Cu6 O10 1.923(5) . ? Cu6 O9 1.976(5) 2_556 ? Cu6 O15 1.977(6) . ? Cu6 O12 2.371(6) . ? Cu6 Cu3 2.8705(15) 2_556 ? O6 C30 1.462(9) . ? O6 C29 1.464(9) . ? N6 O17 1.222(11) . ? N6 O16 1.236(10) . ? N6 O15 1.302(11) . ? O7 C53 1.191(15) . ? O7 C56 1.218(15) . ? C7 C8 1.481(10) . ? C8 C9 1.420(10) . ? C8 C13 1.424(10) . ? O9 Cu5 1.908(5) 2_556 ? O9 Cu6 1.976(5) 2_556 ? C9 C10 1.378(11) . ? O10 C59 1.405(10) . ? O10 Cu3 1.936(5) 2_556 ? C10 C11 1.412(11) . ? C10 C35 1.541(11) . ? O11 C60 1.162(13) . ? O11 C63 1.166(14) . ? C11 C12 1.359(10) . ? C12 C13 1.401(10) . ? C12 C14 1.511(10) . ? C15 C16 1.493(11) . ? C16 C17 1.390(11) . ? C16 C21 1.406(10) . ? C17 C18 1.384(11) . ? O18 C67 1.400(17) . ? O18 C68 1.400(16) . ? C18 C19 1.396(11) . ? C18 C42 1.539(11) . ? O19 C71 1.406(14) . ? O19 C72 1.421(16) . ? C19 C20 1.388(11) . ? C20 C21 1.388(11) . ? C20 C22 1.512(11) . ? C22 C23 1.510(12) . ? C23 C24 1.393(12) . ? C23 C28 1.412(11) . ? C24 C25 1.408(13) . ? C25 C26 1.366(12) . ? C25 C46 1.547(13) . ? C26 C27 1.402(11) . ? C27 C28 1.393(11) . ? C27 C29 1.510(11) . ? C31 C33 1.496(12) . ? C31 C34 1.548(12) . ? C31 C32 1.551(12) . ? C35 C40 1.505(12) . ? C35 C36 1.516(12) . ? C35 C39 1.531(17) . ? C35 C37 1.540(17) . ? C35 C38 1.554(13) . ? C35 C41 1.604(17) . ? C42 C45 1.536(11) . ? C42 C43 1.539(10) . ? C42 C44 1.551(11) . ? C46 C52 1.453(15) . ? C46 C49 1.482(16) . ? C46 C48 1.521(15) . ? C46 C51 1.543(16) . ? C46 C47 1.571(16) . ? C46 C50 1.587(15) . ? C66 C67 1.499(18) . ? C68 C69 1.508(17) . ? C70 C71 1.516(15) . ? C72 C73 1.550(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Cu1 O1 172.7(2) . . ? O5 Cu1 O8 83.8(2) . . ? O1 Cu1 O8 92.6(2) . . ? O5 Cu1 O6 90.2(2) . . ? O1 Cu1 O6 93.1(2) . . ? O8 Cu1 O6 173.3(2) . . ? O5 Cu1 O7 94.5(2) . . ? O1 Cu1 O7 91.7(2) . . ? O8 Cu1 O7 87.7(2) . . ? O6 Cu1 O7 95.8(2) . . ? O5 Cu1 Cu5 42.08(16) . . ? O1 Cu1 Cu5 132.53(15) . . ? O8 Cu1 Cu5 43.63(14) . . ? O6 Cu1 Cu5 129.79(14) . . ? O7 Cu1 Cu5 101.54(14) . . ? O5 Cu1 Cu3 136.23(17) . . ? O1 Cu1 Cu3 39.12(15) . . ? O8 Cu1 Cu3 53.69(15) . . ? O6 Cu1 Cu3 131.54(15) . . ? O7 Cu1 Cu3 93.53(15) . . ? Cu5 Cu1 Cu3 94.18(4) . . ? C6 O1 Cu3 131.5(5) . . ? C6 O1 Cu1 122.8(5) . . ? Cu3 O1 Cu1 101.5(2) . . ? C53 N1 C54 119.3(15) . . ? C53 N1 C55 123.8(16) . . ? C54 N1 C55 116.6(14) . . ? C6 C1 C2 120.8(7) . . ? C6 C1 C30 119.6(7) . . ? C2 C1 C30 119.6(7) . . ? O8 Cu2 O3 179.5(2) . . ? O8 Cu2 O4 90.5(2) . . ? O3 Cu2 O4 89.4(2) . . ? O8 Cu2 O2 88.1(2) . . ? O3 Cu2 O2 91.9(2) . . ? O4 Cu2 O2 170.7(2) . . ? O8 Cu2 O7 87.0(2) . . ? O3 Cu2 O7 93.5(2) . . ? O4 Cu2 O7 98.2(2) . . ? O2 Cu2 O7 90.9(2) . . ? O8 Cu2 Cu4 39.38(15) . . ? O3 Cu2 Cu4 140.15(15) . . ? O4 Cu2 Cu4 87.90(15) . . ? O2 Cu2 Cu4 85.16(15) . . ? O7 Cu2 Cu4 126.25(15) . . ? C13 O2 Cu2 120.0(4) . . ? C13 O2 Cu3 128.3(4) . . ? Cu2 O2 Cu3 103.7(2) . . ? C56 N2 C58 121.0(16) . . ? C56 N2 C57 122.4(14) . . ? C58 N2 C57 114.1(13) . . ? C1 C2 C3 120.7(7) . . ? O9 Cu3 O1 149.7(2) . . ? O9 Cu3 O10 83.2(2) . 2_556 ? O1 Cu3 O10 93.2(2) . 2_556 ? O9 Cu3 O2 100.2(2) . . ? O1 Cu3 O2 97.2(2) . . ? O10 Cu3 O2 151.4(2) 2_556 . ? O9 Cu3 O8 80.37(19) . . ? O1 Cu3 O8 80.28(19) . . ? O10 Cu3 O8 132.9(2) 2_556 . ? O2 Cu3 O8 75.35(18) . . ? O9 Cu3 Cu6 43.26(15) . 2_556 ? O1 Cu3 Cu6 120.84(16) . 2_556 ? O10 Cu3 Cu6 41.76(16) 2_556 2_556 ? O2 Cu3 Cu6 141.41(15) . 2_556 ? O8 Cu3 Cu6 103.37(12) . 2_556 ? O9 Cu3 Cu4 39.45(15) . . ? O1 Cu3 Cu4 118.51(14) . . ? O10 Cu3 Cu4 112.42(16) 2_556 . ? O2 Cu3 Cu4 85.70(14) . . ? O8 Cu3 Cu4 40.99(12) . . ? Cu6 Cu3 Cu4 71.54(3) 2_556 . ? O9 Cu3 Cu1 116.44(16) . . ? O1 Cu3 Cu1 39.39(14) . . ? O10 Cu3 Cu1 115.7(2) 2_556 . ? O2 Cu3 Cu1 88.42(15) . . ? O8 Cu3 Cu1 41.08(12) . . ? Cu6 Cu3 Cu1 116.35(5) 2_556 . ? Cu4 Cu3 Cu1 79.66(3) . . ? C14 O3 C15 113.0(5) . . ? C14 O3 Cu2 111.5(4) . . ? C15 O3 Cu2 119.2(4) . . ? C60 N3 C62 127.1(16) . . ? C60 N3 C61 117.6(15) . . ? C62 N3 C61 115.3(14) . . ? C4 C3 C2 116.6(7) . . ? C4 C3 C31 124.4(7) . . ? C2 C3 C31 119.0(7) . . ? O9 Cu4 O9 180.0(3) 2_556 . ? O9 Cu4 O8 87.5(2) 2_556 . ? O9 Cu4 O8 92.5(2) . . ? O9 Cu4 O8 92.5(2) 2_556 2_556 ? O9 Cu4 O8 87.5(2) . 2_556 ? O8 Cu4 O8 180.000(1) . 2_556 ? O9 Cu4 Cu5 45.86(15) 2_556 . ? O9 Cu4 Cu5 134.14(15) . . ? O8 Cu4 Cu5 48.10(14) . . ? O8 Cu4 Cu5 131.90(14) 2_556 . ? O9 Cu4 Cu5 134.14(15) 2_556 2_556 ? O9 Cu4 Cu5 45.86(15) . 2_556 ? O8 Cu4 Cu5 131.90(14) . 2_556 ? O8 Cu4 Cu5 48.10(14) 2_556 2_556 ? Cu5 Cu4 Cu5 180.0 . 2_556 ? O9 Cu4 Cu3 141.26(15) 2_556 . ? O9 Cu4 Cu3 38.74(15) . . ? O8 Cu4 Cu3 53.85(14) . . ? O8 Cu4 Cu3 126.15(14) 2_556 . ? Cu5 Cu4 Cu3 99.04(3) . . ? Cu5 Cu4 Cu3 80.96(3) 2_556 . ? O9 Cu4 Cu3 38.74(15) 2_556 2_556 ? O9 Cu4 Cu3 141.26(15) . 2_556 ? O8 Cu4 Cu3 126.15(14) . 2_556 ? O8 Cu4 Cu3 53.85(14) 2_556 2_556 ? Cu5 Cu4 Cu3 80.96(3) . 2_556 ? Cu5 Cu4 Cu3 99.04(3) 2_556 2_556 ? Cu3 Cu4 Cu3 180.00(3) . 2_556 ? O9 Cu4 Cu2 85.16(15) 2_556 . ? O9 Cu4 Cu2 94.84(15) . . ? O8 Cu4 Cu2 38.97(14) . . ? O8 Cu4 Cu2 141.03(14) 2_556 . ? Cu5 Cu4 Cu2 69.69(3) . . ? Cu5 Cu4 Cu2 110.31(3) 2_556 . ? Cu3 Cu4 Cu2 63.79(3) . . ? Cu3 Cu4 Cu2 116.21(3) 2_556 . ? O9 Cu4 Cu2 94.84(15) 2_556 2_556 ? O9 Cu4 Cu2 85.16(15) . 2_556 ? O8 Cu4 Cu2 141.03(14) . 2_556 ? O8 Cu4 Cu2 38.97(14) 2_556 2_556 ? Cu5 Cu4 Cu2 110.31(3) . 2_556 ? Cu5 Cu4 Cu2 69.69(3) 2_556 2_556 ? Cu3 Cu4 Cu2 116.21(3) . 2_556 ? Cu3 Cu4 Cu2 63.79(3) 2_556 2_556 ? Cu2 Cu4 Cu2 180.0 . 2_556 ? C21 O4 Cu6 119.3(4) . . ? C21 O4 Cu2 115.4(4) . . ? Cu6 O4 Cu2 119.1(3) . . ? C63 N4 C65 122.3(15) . . ? C63 N4 C64 120.3(16) . . ? C65 N4 C64 117.4(14) . . ? C3 C4 C5 124.7(7) . . ? O9 Cu5 O5 162.9(2) 2_556 . ? O9 Cu5 O11 94.4(2) 2_556 . ? O5 Cu5 O11 97.8(2) . . ? O9 Cu5 O8 87.3(2) 2_556 . ? O5 Cu5 O8 82.8(2) . . ? O11 Cu5 O8 169.6(2) . . ? O9 Cu5 Cu4 46.55(15) 2_556 . ? O5 Cu5 Cu4 128.76(16) . . ? O11 Cu5 Cu4 129.04(18) . . ? O8 Cu5 Cu4 47.20(15) . . ? O9 Cu5 Cu1 130.38(15) 2_556 . ? O5 Cu5 Cu1 41.69(15) . . ? O11 Cu5 Cu1 134.12(19) . . ? O8 Cu5 Cu1 43.07(14) . . ? Cu4 Cu5 Cu1 87.11(3) . . ? C28 O5 Cu1 123.9(5) . . ? C28 O5 Cu5 137.8(5) . . ? Cu1 O5 Cu5 96.2(2) . . ? O14 N5 O13 122.7(8) . . ? O14 N5 O12 118.7(7) . . ? O13 N5 O12 118.4(7) . . ? C4 C5 C6 117.6(7) . . ? C4 C5 C7 120.3(7) . . ? C6 C5 C7 122.1(7) . . ? O10 Cu6 O4 170.2(2) . . ? O10 Cu6 O9 81.6(2) . 2_556 ? O4 Cu6 O9 89.9(2) . 2_556 ? O10 Cu6 O15 95.8(2) . . ? O4 Cu6 O15 92.2(2) . . ? O9 Cu6 O15 174.8(3) 2_556 . ? O10 Cu6 O12 90.3(3) . . ? O4 Cu6 O12 96.6(2) . . ? O9 Cu6 O12 103.3(2) 2_556 . ? O15 Cu6 O12 81.2(3) . . ? O10 Cu6 Cu3 42.11(16) . 2_556 ? O4 Cu6 Cu3 130.51(15) . 2_556 ? O9 Cu6 Cu3 41.23(14) 2_556 2_556 ? O15 Cu6 Cu3 137.15(16) . 2_556 ? O12 Cu6 Cu3 89.75(16) . 2_556 ? C30 O6 C29 111.8(5) . . ? C30 O6 Cu1 110.4(4) . . ? C29 O6 Cu1 113.0(4) . . ? O17 N6 O16 122.4(11) . . ? O17 N6 O15 119.1(8) . . ? O16 N6 O15 118.4(10) . . ? O1 C6 C1 118.7(6) . . ? O1 C6 C5 121.8(7) . . ? C1 C6 C5 119.5(7) . . ? C53 O7 C56 19.7(14) . . ? C53 O7 Cu1 122.3(10) . . ? C56 O7 Cu1 141.9(10) . . ? C53 O7 Cu2 137.8(11) . . ? C56 O7 Cu2 125.6(10) . . ? Cu1 O7 Cu2 81.00(18) . . ? C8 C7 C5 115.4(6) . . ? Cu2 O8 Cu4 101.6(2) . . ? Cu2 O8 Cu1 104.1(2) . . ? Cu4 O8 Cu1 152.9(3) . . ? Cu2 O8 Cu5 112.2(2) . . ? Cu4 O8 Cu5 84.70(18) . . ? Cu1 O8 Cu5 93.3(2) . . ? Cu2 O8 Cu3 92.85(19) . . ? Cu4 O8 Cu3 85.16(19) . . ? Cu1 O8 Cu3 85.23(17) . . ? Cu5 O8 Cu3 154.4(3) . . ? C9 C8 C13 116.4(7) . . ? C9 C8 C7 119.6(6) . . ? C13 C8 C7 123.9(7) . . ? Cu3 O9 Cu5 148.2(3) . 2_556 ? Cu3 O9 Cu4 101.8(2) . . ? Cu5 O9 Cu4 87.6(2) 2_556 . ? Cu3 O9 Cu6 95.5(2) . 2_556 ? Cu5 O9 Cu6 105.2(2) 2_556 2_556 ? Cu4 O9 Cu6 122.0(3) . 2_556 ? C10 C9 C8 124.8(7) . . ? C59 O10 Cu6 121.5(5) . . ? C59 O10 Cu3 128.3(6) . 2_556 ? Cu6 O10 Cu3 96.1(2) . 2_556 ? C9 C10 C11 116.2(7) . . ? C9 C10 C35 123.9(7) . . ? C11 C10 C35 119.9(7) . . ? C60 O11 C63 65.5(12) . . ? C60 O11 Cu5 127.7(9) . . ? C63 O11 Cu5 128.0(10) . . ? C12 C11 C10 121.3(7) . . ? N5 O12 Cu6 115.5(5) . . ? C11 C12 C13 122.3(7) . . ? C11 C12 C14 120.0(7) . . ? C13 C12 C14 117.5(6) . . ? O2 C13 C12 119.5(6) . . ? O2 C13 C8 121.9(7) . . ? C12 C13 C8 118.5(6) . . ? O3 C14 C12 107.1(6) . . ? N6 O15 Cu6 109.2(5) . . ? O3 C15 C16 108.2(6) . . ? C17 C16 C21 119.5(7) . . ? C17 C16 C15 121.7(7) . . ? C21 C16 C15 118.8(7) . . ? C18 C17 C16 121.9(7) . . ? C67 O18 C68 111.7(16) . . ? C17 C18 C19 116.8(8) . . ? C17 C18 C42 120.7(7) . . ? C19 C18 C42 122.5(7) . . ? C71 O19 C72 113.7(14) . . ? C20 C19 C18 123.4(8) . . ? C21 C20 C19 118.3(7) . . ? C21 C20 C22 123.4(7) . . ? C19 C20 C22 118.3(7) . . ? C20 C21 O4 122.4(7) . . ? C20 C21 C16 120.1(7) . . ? O4 C21 C16 117.6(7) . . ? C23 C22 C20 113.9(6) . . ? C24 C23 C28 118.3(8) . . ? C24 C23 C22 119.1(8) . . ? C28 C23 C22 122.4(8) . . ? C23 C24 C25 123.0(8) . . ? C26 C25 C24 117.3(8) . . ? C26 C25 C46 122.7(9) . . ? C24 C25 C46 119.9(8) . . ? C25 C26 C27 121.6(9) . . ? C28 C27 C26 120.7(8) . . ? C28 C27 C29 118.4(8) . . ? C26 C27 C29 120.9(7) . . ? O5 C28 C27 118.9(8) . . ? O5 C28 C23 122.1(8) . . ? C27 C28 C23 119.0(8) . . ? O6 C29 C27 108.7(6) . . ? O6 C30 C1 109.0(6) . . ? C33 C31 C3 112.8(7) . . ? C33 C31 C34 107.7(8) . . ? C3 C31 C34 109.0(7) . . ? C33 C31 C32 108.9(7) . . ? C3 C31 C32 109.9(7) . . ? C34 C31 C32 108.5(7) . . ? C40 C35 C36 110.5(9) . . ? C40 C35 C39 44.8(13) . . ? C36 C35 C39 133.8(13) . . ? C40 C35 C37 135.2(14) . . ? C36 C35 C37 65.9(13) . . ? C39 C35 C37 103.0(18) . . ? C40 C35 C10 110.3(8) . . ? C36 C35 C10 113.4(8) . . ? C39 C35 C10 112.3(12) . . ? C37 C35 C10 111.5(13) . . ? C40 C35 C38 109.4(9) . . ? C36 C35 C38 105.6(9) . . ? C39 C35 C38 66.2(14) . . ? C37 C35 C38 41.8(12) . . ? C10 C35 C38 107.5(8) . . ? C40 C35 C41 49.7(12) . . ? C36 C35 C41 71.4(13) . . ? C39 C35 C41 94.2(18) . . ? C37 C35 C41 134.0(17) . . ? C10 C35 C41 100.1(11) . . ? C38 C35 C41 150.6(13) . . ? C45 C42 C43 107.8(6) . . ? C45 C42 C18 111.5(6) . . ? C43 C42 C18 111.6(6) . . ? C45 C42 C44 109.2(7) . . ? C43 C42 C44 107.2(7) . . ? C18 C42 C44 109.5(6) . . ? C52 C46 C49 125.5(14) . . ? C52 C46 C48 113.5(15) . . ? C49 C46 C48 56.5(13) . . ? C52 C46 C51 35.3(11) . . ? C49 C46 C51 114.2(15) . . ? C48 C46 C51 140.3(14) . . ? C52 C46 C25 114.3(11) . . ? C49 C46 C25 119.3(11) . . ? C48 C46 C25 109.7(10) . . ? C51 C46 C25 107.6(10) . . ? C52 C46 C47 62.9(13) . . ? C49 C46 C47 106.0(15) . . ? C48 C46 C47 56.6(13) . . ? C51 C46 C47 98.0(14) . . ? C25 C46 C47 109.5(11) . . ? C52 C46 C50 110.8(12) . . ? C49 C46 C50 45.2(11) . . ? C48 C46 C50 101.7(13) . . ? C51 C46 C50 80.6(13) . . ? C25 C46 C50 106.0(10) . . ? C47 C46 C50 143.1(14) . . ? O7 C53 N1 123.6(18) . . ? O11 C60 N3 127.3(17) . . ? O11 C63 N4 126.7(17) . . ? O18 C67 C66 105.3(19) . . ? O18 C68 C69 109.2(17) . . ? O19 C71 C70 109.5(13) . . ? O19 C72 C73 107.1(18) . . ? O7 C56 N2 124.2(18) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 2.648 _refine_diff_density_min -2.230 _refine_diff_density_rms 0.169 _database_code_depnum_ccdc_archive 'CCDC 928624'