# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 loop_ _publ_author_name _publ_author_address 'Xuan Jiang.' ; Indiana University Department of Chemistry Bloomington, Indiana 47405-7102 U.S.A. ; J.C.Bollinger ; Indiana University Department of Chemistry Bloomington, Indiana 47405-7102 U.S.A. ; 'Mu-Hyun Baik.' ; Indiana University Department of Chemistry Bloomington, Indiana 47405-7102 U.S.A. ; 'Dongwhan Lee.' ; Indiana University Department of Chemistry Bloomington, Indiana 47405-7102 U.S.A. ; _publ_contact_author 'Professor Dongwhan Lee' _publ_contact_author_address ; Indiana University Department of Chemistry Bloomington, Indiana 47405-7102 U.S.A. ; _publ_contact_author_email dongwhan@indiana.edu _publ_contact_author_name 'Professor Dongwhan Lee' data_04021 _database_code_depnum_ccdc_archive 'CCDC 247397' _audit_creation_method SHELXL-97 _chemical_formula_moiety '2(C76 H64 Cu4 N4), C H2 Cl2, C5 H12' _chemical_formula_sum 'C158 H142 Cl2 Cu8 N8' _chemical_formula_weight 2732.20 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.666(3) _cell_length_b 14.295(2) _cell_length_c 19.401(5) _cell_angle_alpha 83.271(12) _cell_angle_beta 74.874(14) _cell_angle_gamma 74.361(12) _cell_volume 3518.8(14) _cell_formula_units_Z 1 _cell_measurement_temperature 112(2) _cell_measurement_reflns_used 994 _cell_measurement_theta_min 2.372 _cell_measurement_theta_max 29.062 _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.054 0 0 1 0.083 2 0 -1 0.148 -2 0 1 0.121 0 -1 -1 0.178 -1 -2 -1 0.266 0 1 1 0.424 _exptl_absorpt_coefficient_mu 1.275 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.487 _exptl_absorpt_correction_T_max 0.864 _exptl_absorpt_process_details ; Gaussian integration from crystal shape, via Bruker XPREP 6.12 ; _diffrn_ambient_temperature 112(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_measurement_method '\w scans' _diffrn_measurement_details ' 0.30 degree frames measured for 5.17 seconds each' _diffrn_standards_number 304 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 313 _diffrn_standards_decay_% 0 _diffrn_reflns_number 97467 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 30.04 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 20526 _reflns_number_gt 14974 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'SMART (Bruker, 2003)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SHELXTL (Bruker, 2003)' _computing_structure_refinement 'SHELXTL (Bruker, 2003)' _computing_molecular_graphics 'XTEL (local library)' _computing_publication_material 'XTEL (local library)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. The model contains a moderate-sized region of disordered, partially resolved solvent, modeled by use of partially-occupied atomic positions Cl01 and C102 through C116. The solvent molecules in this region are expected to be a combination of dichloromethane and one or more isomers of pentane; the formulae and derived parameters on this file use an estimate of one half methylene chloride and one half pentane per copper cluster. The atomic positions in this group do not represent atoms of resolved chemical moieties; they are an explicit model of the electron density contributions from an indeterminate number of disordered conformations of pentane and dichloromethane in that region of the structure. As such, no interatomic distances or angles are reported herein, as they would not be meaningful in any chemical sense. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc w = [\s^2^(Fo^2^)+(0.06Fo^2^)^2^]^-1^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20526 _refine_ls_number_parameters 937 _refine_ls_number_restraints 198 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1333 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 1.248 _refine_ls_restrained_S_all 1.252 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.006 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.095 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 0.77998(2) 0.698919(19) 0.360449(14) 0.01936(7) Uani 1 1 d . . . Cu2 Cu 0.64724(2) 0.860877(19) 0.336514(14) 0.01843(7) Uani 1 1 d . . . Cu3 Cu 0.70848(2) 0.93894(2) 0.207910(15) 0.01938(7) Uani 1 1 d . . . Cu4 Cu 0.84900(2) 0.792413(19) 0.239396(16) 0.02220(7) Uani 1 1 d . . . N5 N 0.75257(15) 0.76618(13) 0.44326(10) 0.0197(4) Uani 1 1 d . . . C6 C 0.75383(19) 0.69856(16) 0.50396(12) 0.0215(4) Uani 1 1 d . . . C7 C 0.8443(2) 0.62571(18) 0.50610(14) 0.0286(5) Uani 1 1 d . . . H7A H 0.9060 0.6242 0.4692 0.034 Uiso 1 1 calc R . . C8 C 0.8449(2) 0.55566(19) 0.56137(16) 0.0367(6) Uani 1 1 d . . . H8A H 0.9074 0.5069 0.5628 0.044 Uiso 1 1 calc R . . C9 C 0.7552(3) 0.5560(2) 0.61481(17) 0.0483(8) Uani 1 1 d . . . H9A H 0.7556 0.5073 0.6526 0.058 Uiso 1 1 calc R . . C10 C 0.6653(3) 0.6277(2) 0.61278(19) 0.0533(9) Uani 1 1 d . . . H10A H 0.6036 0.6285 0.6496 0.064 Uiso 1 1 calc R . . C11 C 0.6639(2) 0.6988(2) 0.55742(15) 0.0355(6) Uani 1 1 d . . . H11A H 0.6014 0.7476 0.5562 0.043 Uiso 1 1 calc R . . C12 C 0.72599(16) 0.86179(15) 0.45158(11) 0.0171(4) Uani 1 1 d . . . C13 C 0.73227(17) 0.89720(15) 0.51936(11) 0.0173(4) Uani 1 1 d . . . C14 C 0.64650(18) 0.96061(17) 0.56020(12) 0.0222(5) Uani 1 1 d . . . H14A H 0.5833 0.9827 0.5447 0.027 Uiso 1 1 calc R . . C15 C 0.65304(19) 0.99177(18) 0.62367(13) 0.0265(5) Uani 1 1 d . . . H15A H 0.5941 1.0347 0.6516 0.032 Uiso 1 1 calc R . . C16 C 0.7452(2) 0.96040(18) 0.64645(13) 0.0272(5) Uani 1 1 d . . . H16A H 0.7496 0.9820 0.6898 0.033 Uiso 1 1 calc R . . C17 C 0.83189(19) 0.89673(18) 0.60539(13) 0.0261(5) Uani 1 1 d . . . H17A H 0.8952 0.8752 0.6208 0.031 Uiso 1 1 calc R . . C18 C 0.82513(17) 0.86519(16) 0.54245(12) 0.0209(4) Uani 1 1 d . . . H18A H 0.8838 0.8216 0.5148 0.025 Uiso 1 1 calc R . . N19 N 0.69343(15) 0.92135(13) 0.39942(10) 0.0192(4) Uani 1 1 d . . . C20 C 0.68935(18) 1.02206(16) 0.39275(12) 0.0204(4) Uani 1 1 d . . . C21 C 0.7570(2) 1.06372(18) 0.41484(13) 0.0270(5) Uani 1 1 d . . . H21A H 0.8086 1.0237 0.4374 0.032 Uiso 1 1 calc R . . C22 C 0.7494(2) 1.16293(19) 0.40413(15) 0.0364(6) Uani 1 1 d . . . H22A H 0.7952 1.1902 0.4202 0.044 Uiso 1 1 calc R . . C23 C 0.6757(3) 1.2226(2) 0.37025(15) 0.0408(7) Uani 1 1 d . . . H23A H 0.6703 1.2905 0.3635 0.049 Uiso 1 1 calc R . . C24 C 0.6104(2) 1.18184(19) 0.34651(15) 0.0370(6) Uani 1 1 d . . . H24A H 0.5605 1.2219 0.3225 0.044 Uiso 1 1 calc R . . C25 C 0.61709(19) 1.08258(18) 0.35751(13) 0.0271(5) Uani 1 1 d . . . H25A H 0.5717 1.0556 0.3407 0.033 Uiso 1 1 calc R . . N26 N 0.56550(15) 0.80489(14) 0.29647(10) 0.0193(4) Uani 1 1 d . . . C27 C 0.53354(17) 0.72209(17) 0.33358(12) 0.0214(4) Uani 1 1 d . . . C28 C 0.54223(19) 0.63852(17) 0.29974(13) 0.0255(5) Uani 1 1 d . . . H28A H 0.5706 0.6352 0.2496 0.031 Uiso 1 1 calc R . . C29 C 0.5097(2) 0.56019(19) 0.33876(15) 0.0334(6) Uani 1 1 d . . . H29A H 0.5144 0.5042 0.3149 0.040 Uiso 1 1 calc R . . C30 C 0.4704(2) 0.5626(2) 0.41214(15) 0.0371(6) Uani 1 1 d . . . H30A H 0.4476 0.5089 0.4386 0.045 Uiso 1 1 calc R . . C31 C 0.4646(2) 0.6436(2) 0.44621(15) 0.0378(6) Uani 1 1 d . . . H31A H 0.4388 0.6454 0.4966 0.045 Uiso 1 1 calc R . . C32 C 0.4964(2) 0.72309(19) 0.40753(13) 0.0289(5) Uani 1 1 d . . . H32A H 0.4926 0.7784 0.4318 0.035 Uiso 1 1 calc R . . C33 C 0.53895(17) 0.84368(16) 0.23627(11) 0.0176(4) Uani 1 1 d . . . C34 C 0.45480(17) 0.81756(15) 0.21170(11) 0.0180(4) Uani 1 1 d . . . C35 C 0.35845(18) 0.81704(17) 0.25803(12) 0.0218(4) Uani 1 1 d . . . H35A H 0.3452 0.8330 0.3063 0.026 Uiso 1 1 calc R . . C36 C 0.28137(19) 0.79319(19) 0.23396(13) 0.0280(5) Uani 1 1 d . . . H36A H 0.2151 0.7943 0.2656 0.034 Uiso 1 1 calc R . . C37 C 0.3008(2) 0.7679(2) 0.16422(14) 0.0309(6) Uani 1 1 d . . . H37A H 0.2484 0.7505 0.1482 0.037 Uiso 1 1 calc R . . C38 C 0.3970(2) 0.76795(19) 0.11751(13) 0.0274(5) Uani 1 1 d . . . H38A H 0.4102 0.7508 0.0695 0.033 Uiso 1 1 calc R . . C39 C 0.47415(18) 0.79318(17) 0.14100(12) 0.0223(5) Uani 1 1 d . . . H39A H 0.5398 0.7938 0.1089 0.027 Uiso 1 1 calc R . . N40 N 0.58794(14) 0.90840(14) 0.19834(10) 0.0194(4) Uani 1 1 d . . . C41 C 0.54568(17) 0.97633(16) 0.14683(12) 0.0199(4) Uani 1 1 d . . . C42 C 0.4496(2) 1.0430(2) 0.16704(16) 0.0385(7) Uani 1 1 d . . . H42A H 0.4068 1.0385 0.2139 0.046 Uiso 1 1 calc R . . C43 C 0.4164(2) 1.1162(2) 0.11824(18) 0.0474(8) Uani 1 1 d . . . H43A H 0.3508 1.1619 0.1320 0.057 Uiso 1 1 calc R . . C44 C 0.4781(2) 1.1230(2) 0.04992(15) 0.0353(6) Uani 1 1 d . . . H44A H 0.4549 1.1731 0.0168 0.042 Uiso 1 1 calc R . . C45 C 0.5737(2) 1.0567(2) 0.02983(14) 0.0314(6) Uani 1 1 d . . . H45A H 0.6162 1.0613 -0.0171 0.038 Uiso 1 1 calc R . . C46 C 0.6075(2) 0.98361(18) 0.07803(13) 0.0260(5) Uani 1 1 d . . . H46A H 0.6733 0.9382 0.0640 0.031 Uiso 1 1 calc R . . N47 N 0.82078(14) 0.99700(13) 0.19356(10) 0.0199(4) Uani 1 1 d . . . C48 C 0.81418(19) 1.07130(16) 0.13765(13) 0.0227(5) Uani 1 1 d . . . C49 C 0.8924(2) 1.0700(2) 0.07533(14) 0.0316(6) Uani 1 1 d . . . H49A H 0.9576 1.0230 0.0711 0.038 Uiso 1 1 calc R . . C50 C 0.8755(3) 1.1372(2) 0.01903(16) 0.0451(8) Uani 1 1 d . . . H50A H 0.9293 1.1359 -0.0235 0.054 Uiso 1 1 calc R . . C51 C 0.7816(3) 1.2056(2) 0.02447(17) 0.0467(8) Uani 1 1 d . . . H51A H 0.7705 1.2512 -0.0142 0.056 Uiso 1 1 calc R . . C52 C 0.7042(3) 1.2075(2) 0.08579(18) 0.0417(7) Uani 1 1 d . . . H52A H 0.6392 1.2546 0.0894 0.050 Uiso 1 1 calc R . . C53 C 0.7196(2) 1.14147(18) 0.14278(15) 0.0307(5) Uani 1 1 d . . . H53A H 0.6656 1.1441 0.1854 0.037 Uiso 1 1 calc R . . C54 C 0.90188(17) 0.96879(16) 0.22309(12) 0.0189(4) Uani 1 1 d . . . C55 C 0.97764(17) 1.03048(16) 0.21373(12) 0.0203(4) Uani 1 1 d . . . C56 C 1.08410(19) 0.99152(19) 0.18624(13) 0.0266(5) Uani 1 1 d . . . H56A H 1.1083 0.9266 0.1713 0.032 Uiso 1 1 calc R . . C57 C 1.1546(2) 1.0472(2) 0.18065(14) 0.0345(6) Uani 1 1 d . . . H57A H 1.2272 1.0210 0.1613 0.041 Uiso 1 1 calc R . . C58 C 1.1189(2) 1.1413(2) 0.20339(14) 0.0359(6) Uani 1 1 d . . . H58A H 1.1675 1.1787 0.2013 0.043 Uiso 1 1 calc R . . C59 C 1.0127(2) 1.1814(2) 0.22922(14) 0.0331(6) Uani 1 1 d . . . H59A H 0.9888 1.2466 0.2436 0.040 Uiso 1 1 calc R . . C60 C 0.9412(2) 1.12612(17) 0.23408(12) 0.0238(5) Uani 1 1 d . . . H60A H 0.8683 1.1535 0.2511 0.029 Uiso 1 1 calc R . . N61 N 0.91461(15) 0.88317(14) 0.26057(11) 0.0220(4) Uani 1 1 d . . . C62 C 0.97998(18) 0.85480(18) 0.30989(14) 0.0266(5) Uani 1 1 d . . . C63 C 1.0023(2) 0.9182(2) 0.34956(13) 0.0302(5) Uani 1 1 d . . . H63A H 0.9740 0.9863 0.3437 0.036 Uiso 1 1 calc R . . C64 C 1.0653(2) 0.8838(2) 0.39740(15) 0.0403(7) Uani 1 1 d . . . H64A H 1.0807 0.9288 0.4228 0.048 Uiso 1 1 calc R . . C65 C 1.1056(2) 0.7863(3) 0.40871(17) 0.0454(8) Uani 1 1 d . . . H65A H 1.1493 0.7634 0.4412 0.054 Uiso 1 1 calc R . . C66 C 1.0815(2) 0.7222(2) 0.37201(18) 0.0485(9) Uani 1 1 d . . . H66A H 1.1075 0.6543 0.3803 0.058 Uiso 1 1 calc R . . C67 C 1.0193(2) 0.7549(2) 0.32265(17) 0.0371(7) Uani 1 1 d . . . H67A H 1.0038 0.7093 0.2978 0.044 Uiso 1 1 calc R . . N68 N 0.82770(16) 0.69257(14) 0.19381(10) 0.0220(4) Uani 1 1 d . . . C69 C 0.81618(19) 0.71160(17) 0.12235(12) 0.0244(5) Uani 1 1 d . . . C70 C 0.7481(2) 0.67608(18) 0.09600(13) 0.0284(5) Uani 1 1 d . . . H70A H 0.7070 0.6364 0.1262 0.034 Uiso 1 1 calc R . . C71 C 0.7403(2) 0.6985(2) 0.02590(14) 0.0346(6) Uani 1 1 d . . . H71A H 0.6950 0.6728 0.0080 0.042 Uiso 1 1 calc R . . C72 C 0.7978(2) 0.7580(2) -0.01839(14) 0.0402(7) Uani 1 1 d . . . H72A H 0.7920 0.7730 -0.0664 0.048 Uiso 1 1 calc R . . C73 C 0.8636(2) 0.7956(2) 0.00734(14) 0.0369(6) Uani 1 1 d . . . H73A H 0.9027 0.8369 -0.0228 0.044 Uiso 1 1 calc R . . C74 C 0.8726(2) 0.77291(18) 0.07715(14) 0.0310(6) Uani 1 1 d . . . H74A H 0.9176 0.7993 0.0947 0.037 Uiso 1 1 calc R . . C75 C 0.83224(17) 0.60487(15) 0.22704(12) 0.0197(4) Uani 1 1 d . . . C76 C 0.8522(2) 0.51631(16) 0.18691(12) 0.0234(5) Uani 1 1 d . . . C77 C 0.9341(2) 0.49759(19) 0.12583(14) 0.0336(6) Uani 1 1 d . . . H77A H 0.9773 0.5417 0.1095 0.040 Uiso 1 1 calc R . . C78 C 0.9524(3) 0.4147(2) 0.08885(16) 0.0468(8) Uani 1 1 d . . . H78A H 1.0087 0.4021 0.0476 0.056 Uiso 1 1 calc R . . C79 C 0.8898(3) 0.3505(2) 0.11145(19) 0.0517(9) Uani 1 1 d . . . H79A H 0.9028 0.2939 0.0859 0.062 Uiso 1 1 calc R . . C80 C 0.8078(3) 0.3689(2) 0.17145(19) 0.0458(8) Uani 1 1 d . . . H80A H 0.7640 0.3251 0.1865 0.055 Uiso 1 1 calc R . . C81 C 0.7887(2) 0.45079(17) 0.21014(15) 0.0293(5) Uani 1 1 d . . . H81A H 0.7332 0.4622 0.2519 0.035 Uiso 1 1 calc R . . N82 N 0.82102(15) 0.59759(13) 0.29739(10) 0.0196(4) Uani 1 1 d . . . C83 C 0.85513(18) 0.50665(15) 0.33370(12) 0.0202(4) Uani 1 1 d . . . C84 C 0.95899(19) 0.45232(17) 0.31477(13) 0.0241(5) Uani 1 1 d . . . H84A H 1.0066 0.4729 0.2746 0.029 Uiso 1 1 calc R . . C85 C 0.9925(2) 0.36807(18) 0.35483(14) 0.0292(5) Uani 1 1 d . . . H85A H 1.0631 0.3310 0.3417 0.035 Uiso 1 1 calc R . . C86 C 0.9243(2) 0.33787(18) 0.41346(14) 0.0314(6) Uani 1 1 d . . . H86A H 0.9476 0.2802 0.4406 0.038 Uiso 1 1 calc R . . C87 C 0.8219(2) 0.39199(18) 0.43255(14) 0.0306(5) Uani 1 1 d . . . H87A H 0.7747 0.3714 0.4730 0.037 Uiso 1 1 calc R . . C88 C 0.7873(2) 0.47638(17) 0.39298(13) 0.0252(5) Uani 1 1 d . . . H88A H 0.7168 0.5133 0.4067 0.030 Uiso 1 1 calc R . . Cl01 Cl 0.8666(3) 0.4011(4) 0.8520(3) 0.1330(19) Uani 0.50 1 d PU . . C102 C 0.7557(6) 0.6370(6) 0.8028(4) 0.078(2) Uani 0.90 1 d PU . . C103 C 0.4621(10) 0.4741(8) 0.8639(7) 0.130(4) Uani 0.75 1 d PU . . C104 C 0.4307(8) 0.4977(6) 0.9259(6) 0.121(3) Uani 0.75 1 d PU . . C105 C 0.7986(9) 0.4575(8) 0.9416(8) 0.145(4) Uani 0.65 1 d PU . . C106 C 0.6817(7) 0.4660(7) 0.9643(10) 0.173(6) Uani 0.60 1 d PU . . C107 C 0.8286(14) 0.4305(13) 0.8160(8) 0.157(7) Uani 0.60 1 d PU . . C108 C 0.7910(10) 0.5390(14) 0.8715(8) 0.121(5) Uani 0.50 1 d PU . . C109 C 0.5290(17) 0.4990(13) 0.9471(11) 0.146(6) Uani 0.40 1 d PU . . C110 C 0.7728(12) 0.6041(10) 0.8376(8) 0.107(5) Uani 0.60 1 d PU . . C111 C 0.6028(16) 0.4389(9) 0.9876(9) 0.135(6) Uani 0.45 1 d PU . . C112 C 0.601(6) 0.499(4) 0.825(3) 0.182(16) Uani 0.15 1 d PU . . C113 C 0.7473(18) 0.6874(16) 0.7698(13) 0.120(9) Uani 0.30 1 d PU . . C114 C 0.483(3) 0.534(2) 0.8498(15) 0.162(8) Uani 0.40 1 d PU . . C115 C 0.565(2) 0.5918(15) 0.8153(8) 0.253(9) Uani 0.70 1 d PU . . C116 C 0.5313(9) 0.6577(10) 0.7957(4) 0.219(8) Uani 0.85 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02443(15) 0.01489(13) 0.01840(13) -0.00399(10) -0.00499(11) -0.00311(10) Cu2 0.02021(14) 0.01877(13) 0.01812(13) -0.00182(10) -0.00764(10) -0.00456(10) Cu3 0.01690(13) 0.02074(14) 0.02281(14) 0.00149(11) -0.00659(11) -0.00787(10) Cu4 0.02389(15) 0.01484(13) 0.02669(15) -0.00016(11) -0.00365(12) -0.00554(11) N5 0.0229(9) 0.0181(9) 0.0185(9) -0.0032(7) -0.0060(7) -0.0039(7) C6 0.0286(12) 0.0166(10) 0.0216(11) -0.0027(8) -0.0080(9) -0.0069(9) C7 0.0290(13) 0.0235(12) 0.0291(13) -0.0006(10) -0.0054(10) -0.0012(10) C8 0.0399(16) 0.0247(13) 0.0402(16) 0.0055(11) -0.0128(13) 0.0008(11) C9 0.059(2) 0.0309(15) 0.0418(17) 0.0148(13) -0.0048(15) -0.0039(14) C10 0.0474(19) 0.0434(18) 0.0495(19) 0.0168(15) 0.0102(15) -0.0079(15) C11 0.0306(14) 0.0284(13) 0.0380(15) 0.0040(11) -0.0001(12) -0.0019(11) C12 0.0158(10) 0.0186(10) 0.0171(10) -0.0036(8) -0.0032(8) -0.0044(8) C13 0.0192(10) 0.0161(9) 0.0172(10) -0.0026(8) -0.0042(8) -0.0047(8) C14 0.0208(11) 0.0232(11) 0.0221(11) -0.0052(9) -0.0061(9) -0.0023(9) C15 0.0261(12) 0.0278(12) 0.0230(12) -0.0092(10) -0.0030(9) -0.0017(10) C16 0.0324(13) 0.0313(13) 0.0189(11) -0.0062(9) -0.0087(10) -0.0049(10) C17 0.0262(12) 0.0290(12) 0.0259(12) -0.0046(10) -0.0121(10) -0.0044(10) C18 0.0192(10) 0.0205(10) 0.0222(11) -0.0050(9) -0.0046(9) -0.0027(8) N19 0.0219(9) 0.0173(9) 0.0187(9) -0.0038(7) -0.0059(7) -0.0035(7) C20 0.0231(11) 0.0177(10) 0.0171(10) -0.0042(8) 0.0007(8) -0.0035(8) C21 0.0330(13) 0.0240(12) 0.0251(12) -0.0026(9) -0.0044(10) -0.0107(10) C22 0.0508(17) 0.0275(13) 0.0328(14) -0.0069(11) -0.0009(12) -0.0194(12) C23 0.0579(19) 0.0199(12) 0.0325(15) -0.0018(11) 0.0084(13) -0.0078(12) C24 0.0413(16) 0.0236(13) 0.0322(14) 0.0017(11) -0.0001(12) 0.0052(11) C25 0.0251(12) 0.0264(12) 0.0257(12) -0.0020(10) -0.0031(10) -0.0020(10) N26 0.0199(9) 0.0211(9) 0.0184(9) -0.0003(7) -0.0053(7) -0.0072(7) C27 0.0186(10) 0.0242(11) 0.0226(11) 0.0025(9) -0.0069(9) -0.0068(9) C28 0.0272(12) 0.0248(12) 0.0251(12) -0.0002(9) -0.0069(10) -0.0073(10) C29 0.0376(15) 0.0260(13) 0.0395(15) 0.0029(11) -0.0115(12) -0.0127(11) C30 0.0414(16) 0.0360(15) 0.0375(15) 0.0152(12) -0.0126(13) -0.0197(12) C31 0.0455(17) 0.0435(16) 0.0239(13) 0.0096(12) -0.0068(12) -0.0163(13) C32 0.0362(14) 0.0322(13) 0.0207(11) 0.0009(10) -0.0077(10) -0.0128(11) C33 0.0171(10) 0.0191(10) 0.0167(10) -0.0036(8) -0.0032(8) -0.0045(8) C34 0.0189(10) 0.0196(10) 0.0180(10) -0.0007(8) -0.0064(8) -0.0072(8) C35 0.0221(11) 0.0259(11) 0.0178(10) -0.0010(9) -0.0038(9) -0.0076(9) C36 0.0192(11) 0.0389(14) 0.0274(12) 0.0017(11) -0.0039(9) -0.0127(10) C37 0.0271(13) 0.0440(15) 0.0311(13) 0.0019(11) -0.0137(11) -0.0196(11) C38 0.0300(13) 0.0379(14) 0.0206(11) -0.0032(10) -0.0084(10) -0.0163(11) C39 0.0205(11) 0.0306(12) 0.0180(10) -0.0019(9) -0.0044(9) -0.0096(9) N40 0.0166(9) 0.0228(9) 0.0208(9) 0.0022(7) -0.0071(7) -0.0068(7) C41 0.0206(10) 0.0216(10) 0.0211(11) 0.0030(8) -0.0085(9) -0.0095(9) C42 0.0212(12) 0.0453(16) 0.0353(15) 0.0172(12) 0.0018(11) -0.0021(11) C43 0.0230(13) 0.055(2) 0.0504(19) 0.0223(15) -0.0056(13) -0.0004(13) C44 0.0300(13) 0.0396(15) 0.0378(15) 0.0185(12) -0.0161(12) -0.0123(12) C45 0.0392(15) 0.0345(14) 0.0211(12) 0.0042(10) -0.0068(11) -0.0127(12) C46 0.0277(12) 0.0273(12) 0.0217(11) -0.0014(9) -0.0039(9) -0.0062(10) N47 0.0189(9) 0.0191(9) 0.0237(10) 0.0016(7) -0.0065(7) -0.0079(7) C48 0.0297(12) 0.0212(11) 0.0248(11) 0.0025(9) -0.0137(10) -0.0136(9) C49 0.0361(14) 0.0384(14) 0.0249(12) 0.0006(11) -0.0079(11) -0.0173(12) C50 0.063(2) 0.058(2) 0.0269(14) 0.0093(13) -0.0142(14) -0.0373(17) C51 0.071(2) 0.0434(17) 0.0448(18) 0.0206(14) -0.0384(17) -0.0326(17) C52 0.0504(18) 0.0291(14) 0.0563(19) 0.0095(13) -0.0340(16) -0.0124(13) C53 0.0350(14) 0.0243(12) 0.0382(14) 0.0029(10) -0.0178(12) -0.0095(10) C54 0.0171(10) 0.0180(10) 0.0212(11) -0.0028(8) -0.0029(8) -0.0047(8) C55 0.0209(11) 0.0229(11) 0.0204(11) 0.0045(8) -0.0082(9) -0.0101(9) C56 0.0234(12) 0.0344(13) 0.0230(12) 0.0038(10) -0.0081(9) -0.0085(10) C57 0.0241(12) 0.0569(18) 0.0270(13) 0.0096(12) -0.0082(10) -0.0204(12) C58 0.0418(16) 0.0505(17) 0.0297(14) 0.0118(12) -0.0168(12) -0.0332(14) C59 0.0493(17) 0.0314(13) 0.0306(13) 0.0052(11) -0.0176(12) -0.0250(12) C60 0.0288(12) 0.0228(11) 0.0223(11) 0.0020(9) -0.0081(9) -0.0101(9) N61 0.0178(9) 0.0178(9) 0.0299(10) 0.0020(8) -0.0060(8) -0.0049(7) C62 0.0168(11) 0.0267(12) 0.0317(13) 0.0104(10) -0.0031(9) -0.0055(9) C63 0.0270(13) 0.0386(14) 0.0238(12) 0.0079(11) -0.0060(10) -0.0102(11) C64 0.0306(14) 0.063(2) 0.0255(13) 0.0104(13) -0.0066(11) -0.0141(14) C65 0.0268(14) 0.067(2) 0.0372(16) 0.0261(15) -0.0106(12) -0.0115(14) C66 0.0221(13) 0.0443(17) 0.062(2) 0.0350(16) -0.0034(13) -0.0019(12) C67 0.0202(12) 0.0290(13) 0.0555(18) 0.0166(12) -0.0063(12) -0.0059(10) N68 0.0275(10) 0.0170(9) 0.0189(9) -0.0005(7) -0.0026(8) -0.0041(8) C69 0.0263(12) 0.0189(11) 0.0205(11) -0.0015(9) -0.0008(9) 0.0026(9) C70 0.0267(12) 0.0268(12) 0.0254(12) 0.0018(10) -0.0048(10) 0.0012(10) C71 0.0307(14) 0.0383(15) 0.0292(13) -0.0050(11) -0.0098(11) 0.0047(11) C72 0.0390(16) 0.0446(17) 0.0213(13) 0.0049(12) -0.0024(11) 0.0082(13) C73 0.0374(15) 0.0345(14) 0.0261(13) 0.0073(11) 0.0019(11) -0.0008(12) C74 0.0336(14) 0.0255(12) 0.0272(13) 0.0019(10) -0.0014(11) -0.0035(10) C75 0.0223(11) 0.0164(10) 0.0191(10) -0.0024(8) -0.0040(9) -0.0030(8) C76 0.0334(13) 0.0160(10) 0.0215(11) -0.0034(8) -0.0125(10) -0.0005(9) C77 0.0433(16) 0.0271(13) 0.0235(12) -0.0047(10) -0.0076(11) 0.0040(11) C78 0.059(2) 0.0386(16) 0.0321(15) -0.0185(13) -0.0150(14) 0.0159(15) C79 0.074(2) 0.0302(15) 0.056(2) -0.0251(14) -0.0376(19) 0.0103(15) C80 0.061(2) 0.0250(13) 0.066(2) -0.0089(14) -0.0398(18) -0.0068(13) C81 0.0359(14) 0.0213(11) 0.0356(14) -0.0045(10) -0.0191(11) -0.0042(10) N82 0.0239(9) 0.0151(8) 0.0195(9) -0.0023(7) -0.0053(7) -0.0034(7) C83 0.0290(12) 0.0138(9) 0.0200(10) -0.0020(8) -0.0081(9) -0.0061(8) C84 0.0264(12) 0.0228(11) 0.0228(11) -0.0020(9) -0.0059(9) -0.0052(9) C85 0.0304(13) 0.0271(12) 0.0293(13) -0.0026(10) -0.0124(10) -0.0004(10) C86 0.0431(15) 0.0217(12) 0.0296(13) 0.0035(10) -0.0149(11) -0.0042(11) C87 0.0368(14) 0.0265(12) 0.0274(13) 0.0045(10) -0.0061(11) -0.0101(11) C88 0.0271(12) 0.0212(11) 0.0259(12) -0.0002(9) -0.0047(10) -0.0055(9) Cl01 0.093(2) 0.159(4) 0.168(4) -0.072(3) 0.021(2) -0.090(3) C102 0.063(4) 0.084(6) 0.077(6) -0.029(4) -0.002(4) -0.007(4) C103 0.161(9) 0.131(8) 0.160(9) -0.033(7) -0.114(8) -0.054(7) C104 0.127(7) 0.071(5) 0.170(9) 0.002(6) -0.046(7) -0.028(5) C105 0.111(8) 0.127(8) 0.194(11) -0.070(8) 0.028(8) -0.058(7) C106 0.047(5) 0.061(5) 0.374(17) -0.030(8) 0.034(8) -0.024(4) C107 0.216(15) 0.205(14) 0.127(11) 0.031(9) -0.053(9) -0.188(13) C108 0.072(7) 0.178(15) 0.099(10) -0.040(10) 0.010(7) -0.024(10) C109 0.172(15) 0.090(10) 0.202(15) -0.004(11) -0.129(13) 0.002(10) C110 0.114(10) 0.078(9) 0.101(11) -0.033(7) 0.004(9) 0.007(7) C111 0.215(15) 0.063(7) 0.167(12) -0.015(8) -0.148(12) 0.001(9) C112 0.25(3) 0.09(2) 0.14(2) -0.02(2) -0.05(2) 0.10(2) C113 0.102(12) 0.126(14) 0.132(15) -0.118(12) 0.090(11) -0.096(12) C114 0.211(18) 0.146(16) 0.133(15) -0.043(14) -0.085(14) 0.007(14) C115 0.33(2) 0.244(18) 0.094(10) -0.050(11) 0.008(12) 0.041(16) C116 0.183(8) 0.327(15) 0.054(4) -0.091(7) -0.076(5) 0.170(10) _geom_special_details ; All esds are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances and angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. ; 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 N5 1.8708(19) . ? Cu1 N82 1.8785(18) . ? Cu1 Cu2 2.6057(6) . ? Cu1 Cu4 2.6419(7) . ? Cu2 N26 1.8900(19) . ? Cu2 N19 1.8917(19) . ? Cu2 Cu3 2.6330(7) . ? Cu2 Cu4 2.8942(8) . ? Cu3 N40 1.8722(19) . ? Cu3 N47 1.8790(19) . ? Cu3 Cu4 2.5674(6) . ? Cu4 N68 1.886(2) . ? Cu4 N61 1.897(2) . ? N5 C12 1.334(3) . ? N5 C6 1.434(3) . ? C6 C11 1.385(4) . ? C6 C7 1.392(3) . ? C7 C8 1.379(4) . ? C8 C9 1.383(4) . ? C9 C10 1.378(5) . ? C10 C11 1.390(4) . ? C12 N19 1.333(3) . ? C12 C13 1.494(3) . ? C13 C14 1.391(3) . ? C13 C18 1.398(3) . ? C14 C15 1.389(3) . ? C15 C16 1.386(3) . ? C16 C17 1.401(3) . ? C17 C18 1.383(3) . ? N19 C20 1.417(3) . ? C20 C25 1.394(3) . ? C20 C21 1.398(3) . ? C21 C22 1.389(3) . ? C22 C23 1.387(4) . ? C23 C24 1.381(5) . ? C24 C25 1.391(4) . ? N26 C33 1.328(3) . ? N26 C27 1.423(3) . ? C27 C32 1.392(3) . ? C27 C28 1.393(3) . ? C28 C29 1.385(3) . ? C29 C30 1.385(4) . ? C30 C31 1.374(4) . ? C31 C32 1.392(4) . ? C33 N40 1.328(3) . ? C33 C34 1.499(3) . ? C34 C35 1.388(3) . ? C34 C39 1.395(3) . ? C35 C36 1.390(3) . ? C36 C37 1.381(4) . ? C37 C38 1.388(4) . ? C38 C39 1.395(3) . ? N40 C41 1.431(3) . ? C41 C42 1.389(3) . ? C41 C46 1.390(3) . ? C42 C43 1.391(4) . ? C43 C44 1.381(4) . ? C44 C45 1.382(4) . ? C45 C46 1.384(3) . ? N47 C54 1.325(3) . ? N47 C48 1.429(3) . ? C48 C49 1.387(4) . ? C48 C53 1.394(4) . ? C49 C50 1.391(4) . ? C50 C51 1.375(5) . ? C51 C52 1.367(5) . ? C52 C53 1.389(4) . ? C54 N61 1.342(3) . ? C54 C55 1.496(3) . ? C55 C60 1.389(3) . ? C55 C56 1.392(3) . ? C56 C57 1.383(4) . ? C57 C58 1.384(4) . ? C58 C59 1.388(4) . ? C59 C60 1.393(3) . ? N61 C62 1.428(3) . ? C62 C63 1.394(4) . ? C62 C67 1.401(3) . ? C63 C64 1.387(4) . ? C64 C65 1.368(5) . ? C65 C66 1.376(5) . ? C66 C67 1.401(4) . ? N68 C75 1.334(3) . ? N68 C69 1.422(3) . ? C69 C70 1.396(4) . ? C69 C74 1.401(3) . ? C70 C71 1.385(4) . ? C71 C72 1.385(4) . ? C72 C73 1.379(5) . ? C73 C74 1.384(4) . ? C75 N82 1.328(3) . ? C75 C76 1.489(3) . ? C76 C77 1.396(4) . ? C76 C81 1.403(4) . ? C77 C78 1.388(4) . ? C78 C79 1.379(5) . ? C79 C80 1.382(5) . ? C80 C81 1.393(4) . ? N82 C83 1.426(3) . ? C83 C88 1.383(3) . ? C83 C84 1.397(3) . ? C84 C85 1.391(3) . ? C85 C86 1.378(4) . ? C86 C87 1.381(4) . ? C87 C88 1.390(3) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C42 H42A 0.9500 . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 H51A 0.9500 . ? C52 H52A 0.9500 . ? C53 H53A 0.9500 . ? C56 H56A 0.9500 . ? C57 H57A 0.9500 . ? C58 H58A 0.9500 . ? C59 H59A 0.9500 . ? C60 H60A 0.9500 . ? C63 H63A 0.9500 . ? C64 H64A 0.9500 . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C67 H67A 0.9500 . ? C70 H70A 0.9500 . ? C71 H71A 0.9500 . ? C72 H72A 0.9500 . ? C73 H73A 0.9500 . ? C74 H74A 0.9500 . ? C77 H77A 0.9500 . ? C78 H78A 0.9500 . ? C79 H79A 0.9500 . ? C80 H80A 0.9500 . ? C81 H81A 0.9500 . ? C84 H84A 0.9500 . ? C85 H85A 0.9500 . ? C86 H86A 0.9500 . ? C87 H87A 0.9500 . ? C88 H88A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Cu1 N82 161.50(8) . . ? N5 Cu1 Cu2 76.67(6) . . ? N82 Cu1 Cu2 120.53(6) . . ? N5 Cu1 Cu4 115.40(6) . . ? N82 Cu1 Cu4 79.99(6) . . ? Cu2 Cu1 Cu4 66.939(19) . . ? N26 Cu2 N19 162.95(8) . . ? N26 Cu2 Cu1 96.58(6) . . ? N19 Cu2 Cu1 88.73(6) . . ? N26 Cu2 Cu3 86.73(6) . . ? N19 Cu2 Cu3 106.38(6) . . ? Cu1 Cu2 Cu3 111.75(2) . . ? N26 Cu2 Cu4 99.22(6) . . ? N19 Cu2 Cu4 97.27(6) . . ? Cu1 Cu2 Cu4 57.129(18) . . ? Cu3 Cu2 Cu4 55.113(16) . . ? N40 Cu3 N47 162.03(8) . . ? N40 Cu3 Cu4 114.58(6) . . ? N47 Cu3 Cu4 80.04(6) . . ? N40 Cu3 Cu2 79.93(6) . . ? N47 Cu3 Cu2 116.60(6) . . ? Cu4 Cu3 Cu2 67.618(19) . . ? N68 Cu4 N61 160.04(9) . . ? N68 Cu4 Cu3 101.21(6) . . ? N61 Cu4 Cu3 87.19(6) . . ? N68 Cu4 Cu1 85.88(6) . . ? N61 Cu4 Cu1 107.73(6) . . ? Cu3 Cu4 Cu1 112.70(2) . . ? N68 Cu4 Cu2 102.70(6) . . ? N61 Cu4 Cu2 97.09(6) . . ? Cu3 Cu4 Cu2 57.269(19) . . ? Cu1 Cu4 Cu2 55.932(16) . . ? C12 N5 C6 120.72(18) . . ? C12 N5 Cu1 129.42(16) . . ? C6 N5 Cu1 109.62(14) . . ? C11 C6 C7 119.2(2) . . ? C11 C6 N5 121.1(2) . . ? C7 C6 N5 119.5(2) . . ? C8 C7 C6 120.4(2) . . ? C7 C8 C9 120.4(3) . . ? C10 C9 C8 119.4(3) . . ? C9 C10 C11 120.6(3) . . ? C6 C11 C10 120.0(3) . . ? N5 C12 N19 118.42(19) . . ? N5 C12 C13 118.61(19) . . ? N19 C12 C13 122.97(19) . . ? C14 C13 C18 119.7(2) . . ? C14 C13 C12 120.79(19) . . ? C18 C13 C12 119.55(19) . . ? C15 C14 C13 120.1(2) . . ? C16 C15 C14 120.3(2) . . ? C15 C16 C17 119.8(2) . . ? C18 C17 C16 119.9(2) . . ? C17 C18 C13 120.2(2) . . ? C12 N19 C20 123.48(19) . . ? C12 N19 Cu2 114.06(14) . . ? C20 N19 Cu2 122.41(15) . . ? C25 C20 C21 117.9(2) . . ? C25 C20 N19 117.3(2) . . ? C21 C20 N19 124.6(2) . . ? C22 C21 C20 120.7(3) . . ? C23 C22 C21 120.7(3) . . ? C24 C23 C22 119.1(2) . . ? C23 C24 C25 120.5(3) . . ? C24 C25 C20 121.1(3) . . ? C33 N26 C27 122.46(19) . . ? C33 N26 Cu2 119.95(15) . . ? C27 N26 Cu2 117.59(15) . . ? C32 C27 C28 118.5(2) . . ? C32 C27 N26 118.4(2) . . ? C28 C27 N26 123.0(2) . . ? C29 C28 C27 120.4(2) . . ? C30 C29 C28 120.8(3) . . ? C31 C30 C29 119.2(2) . . ? C30 C31 C32 120.6(3) . . ? C31 C32 C27 120.5(2) . . ? N40 C33 N26 118.09(19) . . ? N40 C33 C34 120.17(19) . . ? N26 C33 C34 121.73(19) . . ? C35 C34 C39 119.6(2) . . ? C35 C34 C33 121.20(19) . . ? C39 C34 C33 119.17(19) . . ? C36 C35 C34 120.2(2) . . ? C37 C36 C35 120.2(2) . . ? C36 C37 C38 120.0(2) . . ? C37 C38 C39 120.1(2) . . ? C38 C39 C34 119.8(2) . . ? C33 N40 C41 122.57(18) . . ? C33 N40 Cu3 128.82(15) . . ? C41 N40 Cu3 108.22(14) . . ? C42 C41 C46 119.6(2) . . ? C42 C41 N40 120.7(2) . . ? C46 C41 N40 119.1(2) . . ? C41 C42 C43 119.6(3) . . ? C44 C43 C42 120.5(3) . . ? C43 C44 C45 119.8(2) . . ? C44 C45 C46 120.1(2) . . ? C45 C46 C41 120.3(2) . . ? C54 N47 C48 122.86(19) . . ? C54 N47 Cu3 127.21(16) . . ? C48 N47 Cu3 109.49(14) . . ? C49 C48 C53 118.8(2) . . ? C49 C48 N47 123.0(2) . . ? C53 C48 N47 117.8(2) . . ? C48 C49 C50 120.1(3) . . ? C51 C50 C49 120.6(3) . . ? C52 C51 C50 119.7(3) . . ? C51 C52 C53 120.7(3) . . ? C52 C53 C48 120.2(3) . . ? N47 C54 N61 118.1(2) . . ? N47 C54 C55 120.58(19) . . ? N61 C54 C55 121.3(2) . . ? C60 C55 C56 120.4(2) . . ? C60 C55 C54 119.5(2) . . ? C56 C55 C54 120.1(2) . . ? C57 C56 C55 120.1(3) . . ? C58 C57 C56 119.6(3) . . ? C57 C58 C59 120.6(2) . . ? C58 C59 C60 120.0(3) . . ? C55 C60 C59 119.2(2) . . ? C54 N61 C62 124.2(2) . . ? C54 N61 Cu4 116.30(16) . . ? C62 N61 Cu4 119.35(15) . . ? C63 C62 C67 117.5(2) . . ? C63 C62 N61 125.2(2) . . ? C67 C62 N61 117.2(2) . . ? C64 C63 C62 121.2(3) . . ? C65 C64 C63 121.3(3) . . ? C66 C65 C64 118.5(3) . . ? C65 C66 C67 121.5(3) . . ? C66 C67 C62 120.0(3) . . ? C75 N68 C69 122.2(2) . . ? C75 N68 Cu4 119.37(16) . . ? C69 N68 Cu4 118.21(15) . . ? C70 C69 C74 118.4(2) . . ? C70 C69 N68 123.4(2) . . ? C74 C69 N68 118.1(2) . . ? C71 C70 C69 120.2(3) . . ? C72 C71 C70 120.7(3) . . ? C73 C72 C71 119.9(3) . . ? C72 C73 C74 119.9(3) . . ? C73 C74 C69 121.0(3) . . ? N82 C75 N68 118.25(19) . . ? N82 C75 C76 120.13(19) . . ? N68 C75 C76 121.6(2) . . ? C77 C76 C81 119.3(2) . . ? C77 C76 C75 120.5(2) . . ? C81 C76 C75 120.2(2) . . ? C78 C77 C76 120.1(3) . . ? C79 C78 C77 120.6(3) . . ? C78 C79 C80 119.7(3) . . ? C79 C80 C81 120.8(3) . . ? C80 C81 C76 119.4(3) . . ? C75 N82 C83 121.43(18) . . ? C75 N82 Cu1 127.80(15) . . ? C83 N82 Cu1 110.20(14) . . ? C88 C83 C84 119.3(2) . . ? C88 C83 N82 119.4(2) . . ? C84 C83 N82 121.0(2) . . ? C85 C84 C83 119.9(2) . . ? C86 C85 C84 120.5(2) . . ? C85 C86 C87 119.6(2) . . ? C86 C87 C88 120.5(2) . . ? C83 C88 C87 120.2(2) . . ? C8 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? C7 C8 H8A 119.8 . . ? C9 C8 H8A 119.8 . . ? C10 C9 H9A 120.3 . . ? C8 C9 H9A 120.3 . . ? C9 C10 H10A 119.7 . . ? C11 C10 H10A 119.7 . . ? C6 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C17 C18 H18A 119.9 . . ? C13 C18 H18A 119.9 . . ? C22 C21 H21A 119.6 . . ? C20 C21 H21A 119.6 . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C24 C25 H25A 119.5 . . ? C20 C25 H25A 119.5 . . ? C29 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C30 C29 H29A 119.6 . . ? C28 C29 H29A 119.6 . . ? C31 C30 H30A 120.4 . . ? C29 C30 H30A 120.4 . . ? C30 C31 H31A 119.7 . . ? C32 C31 H31A 119.7 . . ? C31 C32 H32A 119.8 . . ? C27 C32 H32A 119.8 . . ? C36 C35 H35A 119.9 . . ? C34 C35 H35A 119.9 . . ? C37 C36 H36A 119.9 . . ? C35 C36 H36A 119.9 . . ? C36 C37 H37A 120.0 . . ? C38 C37 H37A 120.0 . . ? C37 C38 H38A 120.0 . . ? C39 C38 H38A 120.0 . . ? C38 C39 H39A 120.1 . . ? C34 C39 H39A 120.1 . . ? C41 C42 H42A 120.2 . . ? C43 C42 H42A 120.2 . . ? C44 C43 H43A 119.7 . . ? C42 C43 H43A 119.7 . . ? C43 C44 H44A 120.1 . . ? C45 C44 H44A 120.1 . . ? C44 C45 H45A 120.0 . . ? C46 C45 H45A 120.0 . . ? C45 C46 H46A 119.8 . . ? C41 C46 H46A 119.8 . . ? C48 C49 H49A 120.0 . . ? C50 C49 H49A 120.0 . . ? C51 C50 H50A 119.7 . . ? C49 C50 H50A 119.7 . . ? C52 C51 H51A 120.2 . . ? C50 C51 H51A 120.2 . . ? C51 C52 H52A 119.7 . . ? C53 C52 H52A 119.7 . . ? C52 C53 H53A 119.9 . . ? C48 C53 H53A 119.9 . . ? C57 C56 H56A 119.9 . . ? C55 C56 H56A 119.9 . . ? C58 C57 H57A 120.2 . . ? C56 C57 H57A 120.2 . . ? C57 C58 H58A 119.7 . . ? C59 C58 H58A 119.7 . . ? C58 C59 H59A 120.0 . . ? C60 C59 H59A 120.0 . . ? C55 C60 H60A 120.4 . . ? C59 C60 H60A 120.4 . . ? C64 C63 H63A 119.4 . . ? C62 C63 H63A 119.4 . . ? C65 C64 H64A 119.3 . . ? C63 C64 H64A 119.3 . . ? C66 C65 H65A 120.8 . . ? C64 C65 H65A 120.8 . . ? C65 C66 H66A 119.3 . . ? C67 C66 H66A 119.3 . . ? C66 C67 H67A 120.0 . . ? C62 C67 H67A 120.0 . . ? C71 C70 H70A 119.9 . . ? C69 C70 H70A 119.9 . . ? C72 C71 H71A 119.7 . . ? C70 C71 H71A 119.7 . . ? C73 C72 H72A 120.1 . . ? C71 C72 H72A 120.1 . . ? C72 C73 H73A 120.1 . . ? C74 C73 H73A 120.1 . . ? C73 C74 H74A 119.5 . . ? C69 C74 H74A 119.5 . . ? C78 C77 H77A 119.9 . . ? C76 C77 H77A 119.9 . . ? C79 C78 H78A 119.7 . . ? C77 C78 H78A 119.7 . . ? C78 C79 H79A 120.1 . . ? C80 C79 H79A 120.1 . . ? C79 C80 H80A 119.6 . . ? C81 C80 H80A 119.6 . . ? C80 C81 H81A 120.3 . . ? C76 C81 H81A 120.3 . . ? C85 C84 H84A 120.1 . . ? C83 C84 H84A 120.1 . . ? C86 C85 H85A 119.7 . . ? C84 C85 H85A 119.7 . . ? C85 C86 H86A 120.2 . . ? C87 C86 H86A 120.2 . . ? C86 C87 H87A 119.8 . . ? C88 C87 H87A 119.8 . . ? C83 C88 H88A 119.9 . . ? C87 C88 H88A 119.9 . . ? #==== END OF CIF === #===END data_04026 _database_code_depnum_ccdc_archive 'CCDC 247398' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C46 H46 Cu2 N4' _chemical_formula_sum 'C46 H46 Cu2 N4' _chemical_formula_weight 781.95 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' 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 'P 21/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 10.9223(8) _cell_length_b 14.8184(11) _cell_length_c 11.8480(9) _cell_angle_alpha 90.00 _cell_angle_beta 91.315(2) _cell_angle_gamma 90.00 _cell_volume 1917.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 119(2) _cell_measurement_reflns_used 1006 _cell_measurement_theta_min 4.11 _cell_measurement_theta_max 39.72 _exptl_crystal_description block _exptl_crystal_colour colorless _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 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.147 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.616 _exptl_absorpt_correction_T_max 0.748 _exptl_absorpt_process_details 'SADABS 2.10' _diffrn_ambient_temperature 119(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 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_measurement_method '\w scans' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_number 1 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 215 _diffrn_standards_decay_% 0. _diffrn_reflns_number 75170 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 40.02 _diffrn_reflns_theta_full 40.02 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measurement_details ' 0.30 degree frames measured for 5.17 seconds each' _reflns_number_total 11896 _reflns_number_gt 10140 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'SMART (Bruker, 2003)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XTEL (local library)' _computing_publication_material 'XTEL (local library)' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc w = [\s^2^(Fo^2^)+0.22*Fo^2^+(0.0430Fo^2^)^2^]^-1^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11896 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0777 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.698 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.069 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 0.502145(7) 0.531085(5) 0.596154(6) 0.01353(2) Uani 1 1 d . . . N2 N 0.37418(5) 0.45102(4) 0.62903(5) 0.01416(8) Uani 1 1 d . . . C3 C 0.31570(6) 0.46408(4) 0.73433(5) 0.01466(9) Uani 1 1 d . . . C4 C 0.38159(7) 0.44228(5) 0.83434(6) 0.01865(11) Uani 1 1 d . . . C5 C 0.50765(8) 0.40201(7) 0.82934(7) 0.02573(14) Uani 1 1 d . . . C6 C 0.32831(9) 0.45905(6) 0.93811(6) 0.02616(15) Uani 1 1 d . . . C7 C 0.21278(10) 0.49772(7) 0.94353(7) 0.02965(17) Uani 1 1 d . . . C8 C 0.14988(8) 0.52072(6) 0.84452(8) 0.02578(15) Uani 1 1 d . . . C9 C 0.20018(7) 0.50518(5) 0.73894(6) 0.01884(11) Uani 1 1 d . . . C10 C 0.13270(9) 0.53673(7) 0.63402(9) 0.02813(16) Uani 1 1 d . . . C11 C 0.33082(5) 0.39119(4) 0.55376(5) 0.01297(9) Uani 1 1 d . . . C12 C 0.23498(6) 0.32476(4) 0.58787(5) 0.01481(9) Uani 1 1 d . . . C13 C 0.25475(7) 0.26970(4) 0.68229(6) 0.01816(11) Uani 1 1 d . . . C14 C 0.16616(8) 0.20752(5) 0.71376(7) 0.02384(14) Uani 1 1 d . . . C15 C 0.05749(8) 0.19987(6) 0.65151(8) 0.02659(15) Uani 1 1 d . . . C16 C 0.03633(7) 0.25505(6) 0.55823(7) 0.02548(15) Uani 1 1 d . . . C17 C 0.12481(6) 0.31686(5) 0.52617(6) 0.01959(11) Uani 1 1 d . . . N18 N 0.37354(5) 0.39006(4) 0.44907(4) 0.01383(8) Uani 1 1 d . . . C19 C 0.34120(6) 0.31889(4) 0.37252(5) 0.01316(9) Uani 1 1 d . . . C20 C 0.39637(6) 0.23355(4) 0.38372(5) 0.01616(10) Uani 1 1 d . . . C21 C 0.48945(8) 0.21544(6) 0.47616(7) 0.02279(13) Uani 1 1 d . . . C22 C 0.36659(8) 0.16676(5) 0.30458(6) 0.02209(13) Uani 1 1 d . . . C23 C 0.28564(9) 0.18397(6) 0.21553(7) 0.02573(15) Uani 1 1 d . . . C24 C 0.23477(7) 0.26933(6) 0.20293(6) 0.02296(13) Uani 1 1 d . . . C25 C 0.26230(6) 0.33785(5) 0.28015(5) 0.01670(10) Uani 1 1 d . . . C26 C 0.20948(8) 0.43058(6) 0.26301(7) 0.02399(13) Uani 1 1 d . . . H5A H 0.5417(14) 0.3968(11) 0.9015(12) 0.037(4) Uiso 1 1 d . . . H5B H 0.5550(17) 0.4443(13) 0.7865(16) 0.054(5) Uiso 1 1 d . . . H5C H 0.5051(18) 0.3461(15) 0.7968(16) 0.068(6) Uiso 1 1 d . . . H6 H 0.3759(13) 0.4413(10) 1.0067(12) 0.033(3) Uiso 1 1 d . . . H7 H 0.1760(15) 0.5080(12) 1.0202(14) 0.043(4) Uiso 1 1 d . . . H8 H 0.0781(13) 0.5456(9) 0.8484(12) 0.025(3) Uiso 1 1 d . . . H10A H 0.0856(14) 0.5882(11) 0.6542(13) 0.040(4) Uiso 1 1 d . . . H10B H 0.0821(15) 0.4916(13) 0.6033(14) 0.044(4) Uiso 1 1 d . . . H10C H 0.1827(15) 0.5515(11) 0.5788(14) 0.040(4) Uiso 1 1 d . . . H13 H 0.3279(12) 0.2750(9) 0.7246(11) 0.025(3) Uiso 1 1 d . . . H14 H 0.1869(12) 0.1695(10) 0.7780(11) 0.031(3) Uiso 1 1 d . . . H15 H -0.0028(12) 0.1622(10) 0.6732(11) 0.029(3) Uiso 1 1 d . . . H16 H -0.0373(14) 0.2522(10) 0.5146(12) 0.034(3) Uiso 1 1 d . . . H17 H 0.1093(12) 0.3535(9) 0.4639(11) 0.028(3) Uiso 1 1 d . . . H21A H 0.5324(12) 0.1603(10) 0.4657(11) 0.030(3) Uiso 1 1 d . . . H21B H 0.4534(13) 0.2099(10) 0.5469(13) 0.033(3) Uiso 1 1 d . . . H21C H 0.5419(15) 0.2650(11) 0.4802(13) 0.044(4) Uiso 1 1 d . . . H22 H 0.4069(12) 0.1086(9) 0.3137(11) 0.025(3) Uiso 1 1 d . . . H23 H 0.2657(13) 0.1354(10) 0.1609(12) 0.035(4) Uiso 1 1 d . . . H24 H 0.1826(12) 0.2843(9) 0.1413(11) 0.027(3) Uiso 1 1 d . . . H26A H 0.1826(17) 0.4536(12) 0.3255(17) 0.051(5) Uiso 1 1 d . . . H26B H 0.1477(17) 0.4311(13) 0.1979(16) 0.055(5) Uiso 1 1 d . . . H26C H 0.2666(15) 0.4727(9) 0.2418(14) 0.035(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01546(4) 0.01414(4) 0.01105(3) -0.00148(2) 0.00174(2) -0.00460(2) N2 0.0157(2) 0.01525(19) 0.01164(18) -0.00168(15) 0.00182(15) -0.00380(16) C3 0.0170(2) 0.0145(2) 0.0125(2) -0.00133(17) 0.00252(18) -0.00325(18) C4 0.0230(3) 0.0195(3) 0.0134(2) 0.00049(19) 0.0008(2) -0.0037(2) C5 0.0237(3) 0.0319(4) 0.0214(3) 0.0050(3) -0.0036(2) -0.0003(3) C6 0.0370(4) 0.0287(4) 0.0130(2) -0.0011(2) 0.0038(3) -0.0056(3) C7 0.0397(5) 0.0299(4) 0.0200(3) -0.0061(3) 0.0137(3) -0.0055(3) C8 0.0251(3) 0.0254(3) 0.0273(3) -0.0077(3) 0.0107(3) -0.0019(3) C9 0.0184(3) 0.0178(3) 0.0205(3) -0.0039(2) 0.0031(2) -0.0015(2) C10 0.0239(3) 0.0309(4) 0.0294(4) -0.0044(3) -0.0043(3) 0.0071(3) C11 0.0136(2) 0.0130(2) 0.0123(2) 0.00001(16) 0.00040(16) -0.00177(17) C12 0.0154(2) 0.0143(2) 0.0148(2) -0.00168(17) 0.00295(18) -0.00353(18) C13 0.0212(3) 0.0140(2) 0.0194(3) 0.00142(19) 0.0049(2) -0.0016(2) C14 0.0303(4) 0.0153(3) 0.0265(3) 0.0012(2) 0.0131(3) -0.0030(2) C15 0.0270(3) 0.0232(3) 0.0302(4) -0.0064(3) 0.0143(3) -0.0110(3) C16 0.0197(3) 0.0321(4) 0.0250(3) -0.0091(3) 0.0075(2) -0.0109(3) C17 0.0163(2) 0.0250(3) 0.0175(3) -0.0034(2) 0.0025(2) -0.0060(2) N18 0.0158(2) 0.01430(19) 0.01145(18) -0.00107(15) 0.00081(15) -0.00406(16) C19 0.0141(2) 0.0141(2) 0.0112(2) -0.00051(16) 0.00018(16) -0.00285(17) C20 0.0191(3) 0.0146(2) 0.0148(2) 0.00033(18) 0.00130(19) -0.00130(19) C21 0.0249(3) 0.0233(3) 0.0201(3) 0.0038(2) -0.0020(2) 0.0053(3) C22 0.0305(3) 0.0156(3) 0.0204(3) -0.0033(2) 0.0046(2) -0.0048(2) C23 0.0328(4) 0.0249(3) 0.0194(3) -0.0071(2) 0.0010(3) -0.0117(3) C24 0.0230(3) 0.0301(3) 0.0156(2) -0.0019(2) -0.0045(2) -0.0091(3) C25 0.0154(2) 0.0204(3) 0.0142(2) 0.00154(19) -0.00184(18) -0.0036(2) C26 0.0213(3) 0.0259(3) 0.0246(3) 0.0073(3) -0.0032(2) 0.0019(3) _geom_special_details ; All esds are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances and angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. ; 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 N18 1.8786(5) 3_666 ? Cu1 N2 1.8809(6) . ? Cu1 Cu1 2.4571(2) 3_666 ? N2 C11 1.3365(8) . ? N2 C3 1.4278(8) . ? C3 C9 1.4032(10) . ? C3 C4 1.4097(10) . ? C4 C6 1.3946(11) . ? C4 C5 1.5031(12) . ? C6 C7 1.3888(15) . ? C7 C8 1.3882(15) . ? C8 C9 1.3968(11) . ? C9 C10 1.5050(12) . ? C11 N18 1.3353(8) . ? C11 C12 1.4992(8) . ? C12 C13 1.3974(10) . ? C12 C17 1.3985(10) . ? C13 C14 1.3931(10) . ? C14 C15 1.3876(14) . ? C15 C16 1.3899(14) . ? C16 C17 1.3906(10) . ? N18 C19 1.4300(8) . ? N18 Cu1 1.8787(5) 3_666 ? C19 C25 1.4057(9) . ? C19 C20 1.4059(9) . ? C20 C22 1.3966(10) . ? C20 C21 1.5014(10) . ? C22 C23 1.3846(12) . ? C23 C24 1.3883(13) . ? C24 C25 1.3949(10) . ? C25 C26 1.5024(11) . ? C5 H5A 0.928(14) . ? C5 H5B 0.96(2) . ? C5 H5C 0.91(2) . ? C6 H6 0.990(14) . ? C7 H7 1.013(17) . ? C8 H8 0.869(14) . ? C10 H10A 0.953(16) . ? C10 H10B 0.936(18) . ? C10 H10C 0.889(18) . ? C13 H13 0.937(13) . ? C14 H14 0.970(14) . ? C15 H15 0.904(14) . ? C16 H16 0.947(15) . ? C17 H17 0.929(13) . ? C21 H21A 0.952(14) . ? C21 H21B 0.937(15) . ? C21 H21C 0.933(16) . ? C22 H22 0.973(14) . ? C23 H23 0.989(15) . ? C24 H24 0.942(13) . ? C26 H26A 0.87(2) . ? C26 H26B 1.013(18) . ? C26 H26C 0.921(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N18 Cu1 N2 175.37(2) 3_666 . ? N18 Cu1 Cu1 88.126(17) 3_666 3_666 ? N2 Cu1 Cu1 87.541(17) . 3_666 ? C11 N2 C3 120.95(5) . . ? C11 N2 Cu1 122.27(4) . . ? C3 N2 Cu1 116.42(4) . . ? C9 C3 C4 120.59(6) . . ? C9 C3 N2 120.90(6) . . ? C4 C3 N2 118.25(6) . . ? C6 C4 C3 119.01(7) . . ? C6 C4 C5 120.44(7) . . ? C3 C4 C5 120.56(6) . . ? C7 C6 C4 120.81(8) . . ? C8 C7 C6 119.66(7) . . ? C7 C8 C9 121.27(8) . . ? C8 C9 C3 118.61(7) . . ? C8 C9 C10 119.56(8) . . ? C3 C9 C10 121.76(7) . . ? N18 C11 N2 120.14(5) . . ? N18 C11 C12 120.21(5) . . ? N2 C11 C12 119.65(5) . . ? C13 C12 C17 119.00(6) . . ? C13 C12 C11 120.21(6) . . ? C17 C12 C11 120.79(6) . . ? C14 C13 C12 120.33(7) . . ? C15 C14 C13 120.18(8) . . ? C14 C15 C16 119.94(7) . . ? C15 C16 C17 120.05(8) . . ? C16 C17 C12 120.49(7) . . ? C11 N18 C19 120.79(5) . . ? C11 N18 Cu1 121.83(4) . 3_666 ? C19 N18 Cu1 116.58(4) . 3_666 ? C25 C19 C20 120.46(6) . . ? C25 C19 N18 118.99(6) . . ? C20 C19 N18 120.29(6) . . ? C22 C20 C19 118.77(6) . . ? C22 C20 C21 120.43(7) . . ? C19 C20 C21 120.75(6) . . ? C23 C22 C20 121.06(7) . . ? C22 C23 C24 119.78(7) . . ? C23 C24 C25 120.86(7) . . ? C24 C25 C19 118.97(7) . . ? C24 C25 C26 120.05(6) . . ? C19 C25 C26 120.97(6) . . ? C4 C5 H5A 110.2(9) . . ? C4 C5 H5B 105.4(11) . . ? H5A C5 H5B 109.3(15) . . ? C4 C5 H5C 110.9(12) . . ? H5A C5 H5C 108.8(15) . . ? H5B C5 H5C 112.2(16) . . ? C7 C6 H6 122.1(9) . . ? C4 C6 H6 117.1(9) . . ? C8 C7 H7 121.4(10) . . ? C6 C7 H7 118.9(10) . . ? C7 C8 H8 119.3(9) . . ? C9 C8 H8 119.5(9) . . ? C9 C10 H10A 107.3(9) . . ? C9 C10 H10B 111.9(11) . . ? H10A C10 H10B 110.6(14) . . ? C9 C10 H10C 112.8(11) . . ? H10A C10 H10C 109.4(14) . . ? H10B C10 H10C 104.8(15) . . ? C14 C13 H13 120.1(8) . . ? C12 C13 H13 119.6(8) . . ? C15 C14 H14 123.5(8) . . ? C13 C14 H14 116.3(8) . . ? C14 C15 H15 121.3(8) . . ? C16 C15 H15 118.6(9) . . ? C15 C16 H16 122.1(9) . . ? C17 C16 H16 117.9(9) . . ? C16 C17 H17 119.1(8) . . ? C12 C17 H17 120.4(8) . . ? C20 C21 H21A 112.7(8) . . ? C20 C21 H21B 112.1(9) . . ? H21A C21 H21B 105.1(12) . . ? C20 C21 H21C 107.6(10) . . ? H21A C21 H21C 112.3(12) . . ? H21B C21 H21C 107.0(13) . . ? C23 C22 H22 121.8(8) . . ? C20 C22 H22 117.1(8) . . ? C22 C23 H23 119.5(8) . . ? C24 C23 H23 120.7(8) . . ? C23 C24 H24 122.1(8) . . ? C25 C24 H24 117.1(8) . . ? C25 C26 H26A 112.3(12) . . ? C25 C26 H26B 110.9(11) . . ? H26A C26 H26B 114.3(16) . . ? C25 C26 H26C 113.3(10) . . ? H26A C26 H26C 102.1(15) . . ? H26B C26 H26C 103.3(14) . . ? #===END data_04069 _database_code_depnum_ccdc_archive 'CCDC 247399' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C50 H52 Cu2 N6 +, F6 Sb -, C2 H4 Cl2' _chemical_formula_sum 'C52 H56 Cl2 Cu2 F6 N6 Sb' _chemical_formula_weight 1198.80 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'I 2/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z' 'x+1/2, y+1/2, z+1/2' 'x+1, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y, -z' '-x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z+1/2' _cell_length_a 22.385(4) _cell_length_b 10.4127(18) _cell_length_c 22.665(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.516(4) _cell_angle_gamma 90.00 _cell_volume 5136.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 115(2) _cell_measurement_reflns_used 883 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 24.18 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2452 _exptl_absorpt_coefficient_mu 1.510 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .584 _exptl_absorpt_correction_T_max .927 _exptl_absorpt_process_details ; Absorption correction for the twinned crystal studied was performed with the use of program TWINABS (Sheldrick, 2004). ; _exptl_special_details ; The reported cell setting (in which the space group is I2/a) was chosen over the one leading to space group C2/c because it has a monoclinic angle much closer to 90 degrees, and hence less correlation between atomic x and z coordinates. ; _diffrn_ambient_temperature 115(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_measurement_method '\w scans' _diffrn_measurement_details ' 0.30 degree frames measured for 15.19 seconds each' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 29600 _diffrn_reflns_av_R_equivalents 0.0939 _diffrn_reflns_av_sigmaI/netI 0.2462 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.09 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 8469 _reflns_number_gt 3979 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'SMART (Bruker, 2003)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT (Bruker, 2004), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. The crystal was twinned by a 180-degree rotation around the reciprocal c axis. Determination of the initial orientation matrices and twin law was performed with the use of CELL_NOW (Sheldrick, 2004). The twin domain ratio was determined during structure refinement as 0.5969(8):0.4031(8). Reflections with contributions from equivalent collections of twin domains were averaged with the use of local program TwinMerge (Bollinger, 2004). This procedure leaves more "unique" reflections than for a single crystal because some observations are distinguished from others by having contributions from inequivalent _sets_ of individual twin domain reflections. The structure model contains a region of partially resolved solvent, disordered in multiple configurations and also disordered around a crystallographic two-fold axis. Formulae and derived parameters are computed based on the assumption that this region contains exactly one 1,2-dichloroethane per cation. It is possible, however, that some of the time, pentane is present at that site instead; pentane was present in the crystallization solution, and the region would easilly accommodate a pentane molecule. Attempts to model such a mixture produced no better model of the observed electron density, so the simpler (and less restrained) model presented herein was used for the final refinements. The "atomic" positions and thermal parameters in this region (C(34) - C(37)) should be interpreted as modelling the composite electron density rather than as modelling individual atomic positions. Anisotropic thermal parameters for the fluorine atoms of the SbF6 anion are very elongated, probably indicating an unresolved minor orientational disorder. Such disorders are common for SbF6-, AsF6-, and PF6- anions. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [\s^2^(Fo^2^)+(0.08Fo^2^)^2^]^-1^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8469 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1053 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 0.486 _refine_ls_restrained_S_all 0.486 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.915 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.109 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 0.30386(3) 0.22133(6) 0.27157(3) 0.02364(18) Uani 1 1 d . . . N2 N 0.32458(17) 0.3494(4) 0.2196(2) 0.0210(11) Uani 1 1 d . . . C3 C 0.3900(2) 0.3674(5) 0.2222(3) 0.0252(14) Uani 1 1 d . . . C4 C 0.4153(3) 0.2980(6) 0.1813(3) 0.0393(17) Uani 1 1 d . . . C5 C 0.3783(3) 0.2130(7) 0.1337(3) 0.052(2) Uani 1 1 d . . . H5A H 0.3565 0.1494 0.1526 0.079 Uiso 1 1 calc R . . H5B H 0.4056 0.1689 0.1121 0.079 Uiso 1 1 calc R . . H5C H 0.3485 0.2648 0.1048 0.079 Uiso 1 1 calc R . . C6 C 0.4791(3) 0.3082(8) 0.1871(4) 0.060(3) Uani 1 1 d . . . H6A H 0.4977 0.2670 0.1586 0.072 Uiso 1 1 calc R . . C7 C 0.5140(3) 0.3766(8) 0.2333(4) 0.067(3) Uani 1 1 d . . . H7A H 0.5572 0.3792 0.2374 0.081 Uiso 1 1 calc R . . C8 C 0.4896(3) 0.4414(7) 0.2736(4) 0.054(2) Uani 1 1 d . . . H8A H 0.5156 0.4896 0.3050 0.065 Uiso 1 1 calc R . . C9 C 0.4250(3) 0.4378(6) 0.2693(3) 0.0381(16) Uani 1 1 d . . . C10 C 0.3983(3) 0.5002(6) 0.3156(3) 0.0543(19) Uani 1 1 d . . . H10A H 0.3565 0.5294 0.2969 0.081 Uiso 1 1 calc R . . H10B H 0.4236 0.5741 0.3327 0.081 Uiso 1 1 calc R . . H10C H 0.3969 0.4387 0.3480 0.081 Uiso 1 1 calc R . . C11 C 0.2840(2) 0.4153(5) 0.1794(2) 0.0226(13) Uani 1 1 d . . . C12 C 0.3045(2) 0.5172(5) 0.1413(2) 0.0223(13) Uani 1 1 d . . . C13 C 0.3303(3) 0.6298(6) 0.1694(3) 0.0359(16) Uani 1 1 d . . . H13A H 0.3349 0.6410 0.2118 0.043 Uiso 1 1 calc R . . C14 C 0.3493(2) 0.7258(6) 0.1352(3) 0.0405(17) Uani 1 1 d . . . H14A H 0.3658 0.8035 0.1542 0.049 Uiso 1 1 calc R . . C15 C 0.3445(2) 0.7094(6) 0.0753(3) 0.0403(17) Uani 1 1 d . . . H15A H 0.3591 0.7743 0.0527 0.048 Uiso 1 1 calc R . . C16 C 0.3186(2) 0.5989(6) 0.0465(3) 0.0348(16) Uani 1 1 d . . . H16A H 0.3148 0.5877 0.0042 0.042 Uiso 1 1 calc R . . C17 C 0.2985(2) 0.5058(6) 0.0799(3) 0.0301(14) Uani 1 1 d . . . H17 H 0.2797 0.4309 0.0598 0.036 Uiso 1 1 calc R . . N18 N 0.22460(18) 0.3913(4) 0.1738(2) 0.0227(11) Uani 1 1 d . . . C19 C 0.1785(2) 0.4574(5) 0.1290(2) 0.0221(13) Uani 1 1 d . . . C20 C 0.1499(2) 0.3904(5) 0.0770(2) 0.0278(14) Uani 1 1 d . . . C21 C 0.1699(3) 0.2560(6) 0.0653(3) 0.0454(18) Uani 1 1 d . . . H21A H 0.1666 0.2001 0.0992 0.068 Uiso 1 1 calc R . . H21B H 0.2127 0.2578 0.0615 0.068 Uiso 1 1 calc R . . H21C H 0.1435 0.2230 0.0277 0.068 Uiso 1 1 calc R . . C22 C 0.0993(3) 0.4449(7) 0.0361(3) 0.0407(18) Uani 1 1 d . . . H22A H 0.0781 0.3980 0.0016 0.049 Uiso 1 1 calc R . . C23 C 0.0807(3) 0.5674(8) 0.0466(3) 0.0407(18) Uani 1 1 d . . . H23A H 0.0476 0.6061 0.0181 0.049 Uiso 1 1 calc R . . C24 C 0.1092(2) 0.6336(6) 0.0973(3) 0.0343(16) Uani 1 1 d . . . H24A H 0.0952 0.7175 0.1037 0.041 Uiso 1 1 calc R . . C25 C 0.1588(2) 0.5805(5) 0.1405(3) 0.0300(14) Uani 1 1 d . . . C26 C 0.1857(3) 0.6503(6) 0.1976(3) 0.0445(18) Uani 1 1 d . . . H26A H 0.1937 0.5897 0.2316 0.067 Uiso 1 1 calc R . . H26B H 0.1568 0.7163 0.2045 0.067 Uiso 1 1 calc R . . H26C H 0.2243 0.6910 0.1945 0.067 Uiso 1 1 calc R . . N27 N 0.3936(2) 0.1582(5) 0.3005(2) 0.0371(14) Uani 1 1 d . . . C28 C 0.4431(2) 0.1448(6) 0.3281(3) 0.0296(15) Uani 1 1 d . . . C29 C 0.5059(2) 0.1301(6) 0.3627(3) 0.0356(16) Uani 1 1 d . . . H29A H 0.5336 0.1303 0.3350 0.053 Uiso 1 1 calc R . . H29B H 0.5101 0.0486 0.3849 0.053 Uiso 1 1 calc R . . H29C H 0.5166 0.2013 0.3915 0.053 Uiso 1 1 calc R . . Sb30 Sb 0.5000 0.5000 0.5000 0.02056(13) Uani 1 2 d S . . F31 F 0.41805(17) 0.5319(4) 0.4851(4) 0.133(3) Uani 1 1 d . . . F32 F 0.4829(3) 0.3724(4) 0.4422(2) 0.1020(19) Uani 1 1 d . . . F33 F 0.5037(2) 0.6236(4) 0.4437(2) 0.0851(16) Uani 1 1 d . . . C34 C 0.2251(14) -0.083(3) 0.0781(13) 0.150(14) Uani 0.50 1 d P . . Cl35 Cl 0.25369(16) -0.0053(4) 0.1488(2) 0.0770(12) Uani 0.55 1 d P . . Cl36 Cl 0.2435(3) -0.0405(5) 0.0426(3) 0.0672(18) Uani 0.45 1 d P . . C37 C 0.2243(7) 0.0168(12) -0.0347(6) 0.101(5) Uani 0.80 1 d P . . 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 0.0106(3) 0.0286(4) 0.0312(4) 0.0007(4) 0.0038(3) 0.0029(3) N2 0.006(2) 0.031(3) 0.023(3) 0.002(2) -0.0013(19) 0.0019(19) C3 0.012(3) 0.033(4) 0.028(4) 0.007(3) 0.000(3) -0.003(2) C4 0.016(3) 0.059(5) 0.045(4) 0.022(4) 0.010(3) 0.014(3) C5 0.039(4) 0.082(6) 0.036(4) -0.002(4) 0.008(3) 0.038(4) C6 0.031(4) 0.095(7) 0.068(6) 0.052(5) 0.038(4) 0.035(4) C7 0.019(4) 0.085(7) 0.095(7) 0.057(6) 0.009(4) 0.007(4) C8 0.036(4) 0.047(4) 0.064(5) 0.033(4) -0.020(4) -0.017(4) C9 0.027(3) 0.040(4) 0.039(4) 0.015(4) -0.011(3) -0.013(3) C10 0.072(5) 0.032(4) 0.043(4) -0.002(4) -0.017(4) -0.013(4) C11 0.016(3) 0.022(3) 0.027(3) -0.018(3) 0.000(2) -0.001(2) C12 0.008(2) 0.023(3) 0.033(3) -0.001(3) -0.001(2) 0.000(2) C13 0.030(3) 0.033(4) 0.040(4) -0.008(3) -0.002(3) 0.004(3) C14 0.023(3) 0.017(3) 0.073(5) 0.003(4) -0.005(3) -0.005(3) C15 0.014(3) 0.038(4) 0.066(5) 0.021(4) 0.004(3) 0.008(3) C16 0.020(3) 0.039(4) 0.048(4) 0.003(4) 0.014(3) 0.001(3) C17 0.017(3) 0.028(3) 0.045(4) -0.011(4) 0.009(3) 0.000(3) N18 0.013(2) 0.023(3) 0.030(3) -0.001(2) 0.002(2) 0.002(2) C19 0.011(3) 0.028(3) 0.027(3) 0.002(3) 0.003(2) 0.000(2) C20 0.018(3) 0.032(3) 0.032(3) 0.001(3) 0.003(3) -0.010(3) C21 0.054(4) 0.038(4) 0.046(4) -0.013(3) 0.013(3) -0.011(3) C22 0.027(4) 0.071(5) 0.023(4) 0.008(4) 0.006(3) -0.016(4) C23 0.019(3) 0.071(5) 0.031(4) 0.024(4) 0.001(3) 0.013(4) C24 0.020(3) 0.033(4) 0.050(5) 0.011(3) 0.010(3) 0.010(3) C25 0.019(3) 0.033(4) 0.038(4) 0.001(3) 0.008(3) 0.007(3) C26 0.036(4) 0.035(4) 0.060(5) -0.018(4) 0.005(4) 0.010(3) N27 0.017(3) 0.042(3) 0.053(4) 0.013(3) 0.011(3) 0.007(2) C28 0.019(3) 0.031(4) 0.039(4) 0.004(3) 0.008(3) 0.005(3) C29 0.018(3) 0.046(4) 0.040(4) -0.002(3) 0.000(3) -0.001(3) Sb30 0.0150(2) 0.0195(3) 0.0257(3) -0.0017(3) 0.0016(3) 0.0008(3) F31 0.020(2) 0.056(3) 0.317(9) 0.027(4) 0.029(4) 0.009(2) F32 0.181(5) 0.053(3) 0.056(3) -0.023(3) -0.006(4) 0.017(4) F33 0.121(4) 0.065(3) 0.068(3) 0.025(3) 0.018(3) -0.016(3) C34 0.14(3) 0.13(2) 0.13(3) 0.03(2) -0.07(2) 0.003(19) Cl35 0.057(2) 0.071(3) 0.107(3) 0.034(3) 0.028(2) 0.016(2) Cl36 0.060(4) 0.035(3) 0.088(5) -0.008(3) -0.020(3) 0.022(3) C37 0.110(13) 0.101(11) 0.099(11) 0.067(9) 0.035(9) 0.040(9) _geom_special_details ; All esds are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances and angles; correlations between esds in cell parameters are only used where they are defined by crystal symmetry. ; 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 N2 1.906(4) . ? Cu1 N18 1.918(5) 7 ? Cu1 N27 2.070(5) . ? Cu1 Cu1 2.4547(13) 7 ? N2 C11 1.319(6) . ? N2 C3 1.465(6) . ? C3 C9 1.379(8) . ? C3 C4 1.395(8) . ? C4 C6 1.407(8) . ? C4 C5 1.490(8) . ? C6 C7 1.352(11) . ? C7 C8 1.349(10) . ? C8 C9 1.427(9) . ? C9 C10 1.476(9) . ? C11 N18 1.329(6) . ? C11 C12 1.507(7) . ? C12 C17 1.373(7) . ? C12 C13 1.394(7) . ? C13 C14 1.392(8) . ? C14 C15 1.347(8) . ? C15 C16 1.382(8) . ? C16 C17 1.368(8) . ? N18 C19 1.443(6) . ? N18 Cu1 1.919(5) 7 ? C19 C20 1.391(7) . ? C19 C25 1.399(7) . ? C20 C22 1.404(8) . ? C20 C21 1.512(8) . ? C22 C23 1.379(9) . ? C23 C24 1.363(8) . ? C24 C25 1.410(7) . ? C25 C26 1.484(7) . ? N27 C28 1.146(7) . ? C28 C29 1.450(7) . ? Sb30 F31 1.817(4) . ? Sb30 F31 1.817(4) 5_666 ? Sb30 F33 1.828(4) 5_666 ? Sb30 F33 1.828(4) . ? Sb30 F32 1.842(4) 5_666 ? Sb30 F32 1.842(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 H17 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? 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 N2 Cu1 N18 172.39(18) . 7 ? N2 Cu1 N27 93.43(19) . . ? N18 Cu1 N27 92.60(19) 7 . ? N2 Cu1 Cu1 86.67(12) . 7 ? N18 Cu1 Cu1 87.84(13) 7 7 ? N27 Cu1 Cu1 173.78(16) . 7 ? C11 N2 C3 118.8(4) . . ? C11 N2 Cu1 124.2(3) . . ? C3 N2 Cu1 116.8(3) . . ? C9 C3 C4 123.0(5) . . ? C9 C3 N2 118.7(5) . . ? C4 C3 N2 117.7(5) . . ? C3 C4 C6 117.3(7) . . ? C3 C4 C5 123.1(5) . . ? C6 C4 C5 119.6(7) . . ? C7 C6 C4 120.2(7) . . ? C8 C7 C6 122.3(7) . . ? C7 C8 C9 120.4(7) . . ? C3 C9 C8 116.7(7) . . ? C3 C9 C10 122.3(5) . . ? C8 C9 C10 120.9(6) . . ? N2 C11 N18 118.7(5) . . ? N2 C11 C12 120.6(4) . . ? N18 C11 C12 120.7(5) . . ? C17 C12 C13 117.9(6) . . ? C17 C12 C11 123.4(5) . . ? C13 C12 C11 118.7(5) . . ? C14 C13 C12 119.9(6) . . ? C15 C14 C13 120.5(6) . . ? C14 C15 C16 120.5(6) . . ? C17 C16 C15 119.0(6) . . ? C16 C17 C12 122.2(6) . . ? C11 N18 C19 120.8(5) . . ? C11 N18 Cu1 121.9(4) . 7 ? C19 N18 Cu1 117.1(3) . 7 ? C20 C19 C25 121.0(5) . . ? C20 C19 N18 118.0(5) . . ? C25 C19 N18 120.7(5) . . ? C19 C20 C22 119.7(6) . . ? C19 C20 C21 121.1(5) . . ? C22 C20 C21 119.1(6) . . ? C23 C22 C20 119.4(6) . . ? C24 C23 C22 120.7(6) . . ? C23 C24 C25 121.6(6) . . ? C19 C25 C24 117.4(6) . . ? C19 C25 C26 122.0(5) . . ? C24 C25 C26 120.5(5) . . ? C28 N27 Cu1 162.6(5) . . ? N27 C28 C29 179.0(7) . . ? F31 Sb30 F31 179.996(1) . 5_666 ? F31 Sb30 F33 92.8(3) . 5_666 ? F31 Sb30 F33 87.2(3) 5_666 5_666 ? F31 Sb30 F33 87.2(3) . . ? F31 Sb30 F33 92.8(3) 5_666 . ? F33 Sb30 F33 179.996(1) 5_666 . ? F31 Sb30 F32 91.9(3) . 5_666 ? F31 Sb30 F32 88.1(3) 5_666 5_666 ? F33 Sb30 F32 92.7(2) 5_666 5_666 ? F33 Sb30 F32 87.3(2) . 5_666 ? F31 Sb30 F32 88.1(3) . . ? F31 Sb30 F32 91.9(3) 5_666 . ? F33 Sb30 F32 87.3(2) 5_666 . ? F33 Sb30 F32 92.7(2) . . ? F32 Sb30 F32 179.996(2) 5_666 . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 119.9 . . ? C4 C6 H6A 119.9 . . ? C8 C7 H7A 118.9 . . ? C6 C7 H7A 118.9 . . ? C7 C8 H8A 119.8 . . ? C9 C8 H8A 119.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 H15A 119.7 . . ? C16 C15 H15A 119.7 . . ? C17 C16 H16A 120.5 . . ? C15 C16 H16A 120.5 . . ? C16 C17 H17 118.9 . . ? C12 C17 H17 118.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 H22A 120.3 . . ? C20 C22 H22A 120.3 . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C23 C24 H24A 119.2 . . ? C25 C24 H24A 119.2 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? data_04097 _database_code_depnum_ccdc_archive 'CCDC 247400' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C54 H62 Cu2 N4 O2 +, F6 Sb -, 2(C H2 Cl2)' _chemical_formula_sum 'C56 H66 Cl2 Cu2 F6 N4 O2 Sb' _chemical_formula_weight 1260.91 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 12.562(3) _cell_length_b 21.015(4) _cell_length_c 21.138(5) _cell_angle_alpha 90.899(6) _cell_angle_beta 104.009(8) _cell_angle_gamma 91.598(7) _cell_volume 5411(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 1768 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 25.05 _exptl_crystal_description plate _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2572 _exptl_absorpt_coefficient_mu 1.439 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.611 _exptl_absorpt_correction_T_max 0.931 _exptl_absorpt_process_details 'TwinAbs (Sheldrick, 2004)' _exptl_special_details ; The experimental crystal was twinned, as were all others from the sample that were considered. The twin law corresponds to a 180-degree rotation around the reciprocal (0 1 0) axis. The twinning solution and initial orientation for integration were determined with the use of program CELL_NOW (Sheldrick, 2004). ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_measurement_details ' 0.30 degree frames measured for 10.17 seconds each' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 78414 _diffrn_reflns_av_R_equivalents 0.087 _diffrn_reflns_av_sigmaI/netI 0.2371 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.26 _diffrn_reflns_theta_full 25.26 _diffrn_measured_fraction_theta_max 0.979 _diffrn_measured_fraction_theta_full 0.979 _reflns_number_total 33033 _reflns_number_gt 15012 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'SMART (Bruker, 2003)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XTEL (local library)' _computing_publication_material 'XTEL (local library)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. Partially resolved disordered solvent in the structure is modeled with the use of partially occupied carbon atom and chlorine atom positions C(88) through C(95). Formulae and derived parameters are calculated as if this space contains one disordered dichloromethane molecule. The atomic positions in this group do not represent atoms of resolved chemical moieties; they are an explicit model of the electron density contributions from an indeterminate number of disordered conformations of dichloromethane in that region of the structure. As such, no interatomic distances or angles are reported herein, as they would not be meaningful in any chemical sense. Reflections with the same combination of contributing components from the two recognized twin domains were averaged. Other reflections were not averaged, hence the number of unique reflections is greater than would be correct for an untwinned crystal of the same unit cell and diffraction limits. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [\s^2^(Fo^2^)+(0.05Fo^2^)^2^]^-1^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 33033 _refine_ls_number_parameters 1378 _refine_ls_number_restraints 374 _refine_ls_R_factor_all 0.1181 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1450 _refine_ls_wR_factor_gt 0.1254 _refine_ls_goodness_of_fit_ref 0.707 _refine_ls_restrained_S_all 0.706 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.011 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.098 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 0.29691(6) 0.74312(4) 0.04591(3) 0.01718(19) Uani 1 1 d . . . Cu2 Cu 0.17027(6) 0.74650(4) 0.11437(3) 0.01683(18) Uani 1 1 d . . . N3 N 0.3348(4) 0.8288(2) 0.0723(2) 0.0179(12) Uani 1 1 d . . . C4 C 0.4368(5) 0.8543(3) 0.0622(3) 0.0230(16) Uani 1 1 d . . . C5 C 0.4379(6) 0.8946(3) 0.0110(3) 0.0242(16) Uani 1 1 d . . . C6 C 0.3330(6) 0.9146(3) -0.0351(3) 0.0322(18) Uani 1 1 d . . . H6A H 0.2699 0.8964 -0.0213 0.048 Uiso 1 1 calc R . . H6B H 0.3311 0.8992 -0.0794 0.048 Uiso 1 1 calc R . . H6C H 0.3301 0.9611 -0.0345 0.048 Uiso 1 1 calc R . . C7 C 0.5378(7) 0.9133(4) 0.0011(4) 0.040(2) Uani 1 1 d . . . H7A H 0.5398 0.9413 -0.0336 0.048 Uiso 1 1 calc R . . C8 C 0.6347(7) 0.8935(4) 0.0389(4) 0.047(2) Uani 1 1 d . . . H8A H 0.7023 0.9068 0.0299 0.057 Uiso 1 1 calc R . . C9 C 0.6336(6) 0.8546(3) 0.0894(4) 0.038(2) Uani 1 1 d . . . H9A H 0.7011 0.8416 0.1164 0.045 Uiso 1 1 calc R . . C10 C 0.5343(6) 0.8335(3) 0.1025(4) 0.0302(18) Uani 1 1 d . . . C11 C 0.5353(6) 0.7885(3) 0.1578(3) 0.0356(19) Uani 1 1 d . . . H11A H 0.4599 0.7797 0.1612 0.053 Uiso 1 1 calc R . . H11B H 0.5784 0.8080 0.1987 0.053 Uiso 1 1 calc R . . H11C H 0.5684 0.7486 0.1492 0.053 Uiso 1 1 calc R . . C12 C 0.2685(5) 0.8641(3) 0.0986(3) 0.0128(14) Uani 1 1 d . . . C13 C 0.3004(5) 0.9317(3) 0.1210(3) 0.0154(14) Uani 1 1 d . . . C14 C 0.2480(5) 0.9838(3) 0.0917(3) 0.0235(16) Uani 1 1 d . . . H14A H 0.1894 0.9783 0.0538 0.028 Uiso 1 1 calc R . . C15 C 0.2799(6) 1.0442(3) 0.1170(3) 0.0280(17) Uani 1 1 d . . . H15A H 0.2442 1.0802 0.0961 0.034 Uiso 1 1 calc R . . C16 C 0.3635(6) 1.0524(3) 0.1725(3) 0.0285(18) Uani 1 1 d . . . H16A H 0.3852 1.0940 0.1900 0.034 Uiso 1 1 calc R . . C17 C 0.4155(6) 1.0004(3) 0.2025(3) 0.0306(18) Uani 1 1 d . . . H17A H 0.4724 1.0059 0.2412 0.037 Uiso 1 1 calc R . . C18 C 0.3852(5) 0.9403(3) 0.1765(3) 0.0229(16) Uani 1 1 d . . . H18A H 0.4226 0.9045 0.1968 0.027 Uiso 1 1 calc R . . N19 N 0.1785(4) 0.8359(2) 0.1078(2) 0.0171(12) Uani 1 1 d . . . C20 C 0.0911(5) 0.8757(3) 0.1176(3) 0.0206(16) Uani 1 1 d . . . C21 C 0.0802(5) 0.8880(3) 0.1809(3) 0.0273(17) Uani 1 1 d . . . C22 C 0.1608(6) 0.8643(4) 0.2404(3) 0.0353(19) Uani 1 1 d . . . H22A H 0.1395 0.8785 0.2798 0.053 Uiso 1 1 calc R . . H22B H 0.2346 0.8814 0.2413 0.053 Uiso 1 1 calc R . . H22C H 0.1607 0.8177 0.2385 0.053 Uiso 1 1 calc R . . C23 C -0.0063(6) 0.9264(3) 0.1881(4) 0.037(2) Uani 1 1 d . . . H23A H -0.0145 0.9371 0.2304 0.045 Uiso 1 1 calc R . . C24 C -0.0795(6) 0.9486(3) 0.1335(4) 0.039(2) Uani 1 1 d . . . H24A H -0.1389 0.9734 0.1389 0.047 Uiso 1 1 calc R . . C25 C -0.0678(6) 0.9354(4) 0.0719(4) 0.039(2) Uani 1 1 d . . . H25A H -0.1178 0.9519 0.0352 0.047 Uiso 1 1 calc R . . C26 C 0.0181(5) 0.8975(3) 0.0629(3) 0.0256(17) Uani 1 1 d . . . C27 C 0.0282(5) 0.8808(3) -0.0042(3) 0.0332(19) Uani 1 1 d . . . H27A H 0.0905 0.8531 -0.0015 0.050 Uiso 1 1 calc R . . H27B H 0.0400 0.9198 -0.0267 0.050 Uiso 1 1 calc R . . H27C H -0.0394 0.8586 -0.0284 0.050 Uiso 1 1 calc R . . N28 N 0.2820(4) 0.6533(2) 0.0445(2) 0.0190(12) Uani 1 1 d . . . C29 C 0.3065(6) 0.6136(3) -0.0052(3) 0.0221(16) Uani 1 1 d . . . C30 C 0.4147(5) 0.5992(3) -0.0029(3) 0.0250(17) Uani 1 1 d . . . C31 C 0.5098(5) 0.6216(3) 0.0526(3) 0.0312(18) Uani 1 1 d . . . H31A H 0.4823 0.6477 0.0837 0.047 Uiso 1 1 calc R . . H31B H 0.5625 0.6469 0.0353 0.047 Uiso 1 1 calc R . . H31C H 0.5460 0.5845 0.0748 0.047 Uiso 1 1 calc R . . C32 C 0.4364(6) 0.5620(3) -0.0540(3) 0.0308(18) Uani 1 1 d . . . H32A H 0.5097 0.5514 -0.0533 0.037 Uiso 1 1 calc R . . C33 C 0.3510(6) 0.5407(3) -0.1052(3) 0.0308(18) Uani 1 1 d . . . H33A H 0.3660 0.5157 -0.1397 0.037 Uiso 1 1 calc R . . C34 C 0.2448(6) 0.5555(3) -0.1063(3) 0.0259(17) Uani 1 1 d . . . H34A H 0.1873 0.5405 -0.1418 0.031 Uiso 1 1 calc R . . C35 C 0.2191(5) 0.5919(3) -0.0571(3) 0.0201(15) Uani 1 1 d . . . C36 C 0.1022(5) 0.6068(3) -0.0571(3) 0.0231(16) Uani 1 1 d . . . H36A H 0.1016 0.6336 -0.0188 0.035 Uiso 1 1 calc R . . H36B H 0.0603 0.5670 -0.0556 0.035 Uiso 1 1 calc R . . H36C H 0.0688 0.6293 -0.0968 0.035 Uiso 1 1 calc R . . C37 C 0.2549(5) 0.6257(3) 0.0961(3) 0.0146(14) Uani 1 1 d . . . C38 C 0.2863(5) 0.5594(3) 0.1143(3) 0.0207(16) Uani 1 1 d . . . C39 C 0.2425(5) 0.5058(3) 0.0765(3) 0.0226(16) Uani 1 1 d . . . H39A H 0.1877 0.5105 0.0373 0.027 Uiso 1 1 calc R . . C40 C 0.2774(6) 0.4459(3) 0.0951(3) 0.0312(18) Uani 1 1 d . . . H40A H 0.2451 0.4096 0.0697 0.037 Uiso 1 1 calc R . . C41 C 0.3595(6) 0.4389(3) 0.1510(4) 0.0340(19) Uani 1 1 d . . . H41A H 0.3847 0.3976 0.1633 0.041 Uiso 1 1 calc R . . C42 C 0.4049(6) 0.4908(4) 0.1887(4) 0.0356(19) Uani 1 1 d . . . H42A H 0.4605 0.4854 0.2274 0.043 Uiso 1 1 calc R . . C43 C 0.3694(5) 0.5520(3) 0.1703(3) 0.0240(16) Uani 1 1 d . . . H43A H 0.4019 0.5882 0.1960 0.029 Uiso 1 1 calc R . . N44 N 0.2085(4) 0.6608(2) 0.1330(2) 0.0173(12) Uani 1 1 d . . . C45 C 0.1806(5) 0.6365(3) 0.1903(3) 0.0210(16) Uani 1 1 d . . . C46 C 0.2408(6) 0.6604(3) 0.2514(3) 0.0269(17) Uani 1 1 d . . . C47 C 0.3357(6) 0.7077(3) 0.2572(3) 0.0337(19) Uani 1 1 d . . . H47A H 0.3661 0.7194 0.3033 0.051 Uiso 1 1 calc R . . H47B H 0.3099 0.7458 0.2328 0.051 Uiso 1 1 calc R . . H47C H 0.3928 0.6884 0.2394 0.051 Uiso 1 1 calc R . . C48 C 0.2095(6) 0.6405(4) 0.3060(3) 0.040(2) Uani 1 1 d . . . H48A H 0.2470 0.6575 0.3475 0.048 Uiso 1 1 calc R . . C49 C 0.1250(6) 0.5963(4) 0.3018(4) 0.042(2) Uani 1 1 d . . . H49A H 0.1071 0.5815 0.3403 0.050 Uiso 1 1 calc R . . C50 C 0.0660(6) 0.5735(3) 0.2412(3) 0.0312(18) Uani 1 1 d . . . H50A H 0.0065 0.5439 0.2383 0.037 Uiso 1 1 calc R . . C51 C 0.0927(5) 0.5934(3) 0.1853(3) 0.0221(16) Uani 1 1 d . . . C52 C 0.0223(5) 0.5696(3) 0.1198(3) 0.0270(17) Uani 1 1 d . . . H52A H -0.0353 0.5400 0.1268 0.040 Uiso 1 1 calc R . . H52B H 0.0682 0.5476 0.0955 0.040 Uiso 1 1 calc R . . H52C H -0.0116 0.6058 0.0948 0.040 Uiso 1 1 calc R . . O53 O 0.3381(3) 0.7532(2) -0.04392(19) 0.0237(11) Uani 1 1 d . . . C54 C 0.4416(5) 0.7468(3) -0.0630(3) 0.0272(17) Uani 1 1 d . . . H54A H 0.4857 0.7130 -0.0383 0.033 Uiso 1 1 calc R . . H54B H 0.4852 0.7874 -0.0557 0.033 Uiso 1 1 calc R . . C55 C 0.4065(7) 0.7295(5) -0.1341(4) 0.071(3) Uani 1 1 d . . . H55A H 0.4605 0.7464 -0.1573 0.085 Uiso 1 1 calc R . . H55B H 0.3995 0.6827 -0.1406 0.085 Uiso 1 1 calc R . . C56 C 0.3002(6) 0.7585(4) -0.1578(3) 0.042(2) Uani 1 1 d . . . H56A H 0.2560 0.7352 -0.1969 0.050 Uiso 1 1 calc R . . H56B H 0.3095 0.8036 -0.1687 0.050 Uiso 1 1 calc R . . C57 C 0.2472(5) 0.7528(4) -0.1010(3) 0.0271(17) Uani 1 1 d . . . H57A H 0.1994 0.7891 -0.0993 0.033 Uiso 1 1 calc R . . H57B H 0.2027 0.7127 -0.1046 0.033 Uiso 1 1 calc R . . O58 O 0.0116(3) 0.7350(2) 0.1337(2) 0.0262(11) Uani 1 1 d . . . C59 C -0.0316(6) 0.7358(3) 0.1916(3) 0.0326(19) Uani 1 1 d . . . H59A H -0.0412 0.7800 0.2055 0.039 Uiso 1 1 calc R . . H59B H 0.0182 0.7143 0.2280 0.039 Uiso 1 1 calc R . . C60 C -0.1415(6) 0.6999(4) 0.1710(3) 0.043(2) Uani 1 1 d . . . H60A H -0.1960 0.7194 0.1915 0.052 Uiso 1 1 calc R . . H60B H -0.1340 0.6548 0.1837 0.052 Uiso 1 1 calc R . . C61 C -0.1767(5) 0.7050(4) 0.0963(4) 0.037(2) Uani 1 1 d . . . H61A H -0.1851 0.6623 0.0747 0.045 Uiso 1 1 calc R . . H61B H -0.2467 0.7273 0.0825 0.045 Uiso 1 1 calc R . . C62 C -0.0822(5) 0.7435(4) 0.0809(3) 0.0329(19) Uani 1 1 d . . . H62A H -0.0677 0.7281 0.0393 0.040 Uiso 1 1 calc R . . H62B H -0.0999 0.7891 0.0769 0.040 Uiso 1 1 calc R . . Cu1' Cu 0.20772(6) 0.75541(4) 0.60942(4) 0.01860(19) Uani 1 1 d . . . Cu2' Cu 0.03458(6) 0.75808(4) 0.64250(4) 0.0213(2) Uani 1 1 d . A . N3' N 0.2295(4) 0.8436(3) 0.6317(2) 0.0221(13) Uani 1 1 d . A . C4' C 0.3254(5) 0.8763(3) 0.6215(3) 0.0185(15) Uani 1 1 d . . . C5' C 0.4288(5) 0.8626(3) 0.6610(3) 0.0238(16) Uani 1 1 d . A . C6' C 0.4386(6) 0.8148(4) 0.7133(4) 0.043(2) Uani 1 1 d . . . H6'A H 0.3653 0.7981 0.7141 0.064 Uiso 1 1 calc R A . H6'B H 0.4734 0.8351 0.7556 0.064 Uiso 1 1 calc R . . H6'C H 0.4834 0.7798 0.7046 0.064 Uiso 1 1 calc R . . C7' C 0.5218(6) 0.8944(4) 0.6498(3) 0.0331(18) Uani 1 1 d . . . H7'A H 0.5919 0.8870 0.6775 0.040 Uiso 1 1 calc R A . C8' C 0.5138(6) 0.9349(4) 0.6008(3) 0.037(2) Uani 1 1 d . A . H8'A H 0.5779 0.9560 0.5940 0.045 Uiso 1 1 calc R . . C9' C 0.4130(6) 0.9461(3) 0.5603(3) 0.035(2) Uani 1 1 d . . . H9'A H 0.4088 0.9747 0.5255 0.042 Uiso 1 1 calc R A . C10' C 0.3174(6) 0.9171(3) 0.5688(3) 0.0287(17) Uani 1 1 d . A . C11' C 0.2093(6) 0.9312(4) 0.5226(3) 0.045(2) Uani 1 1 d . . . H11D H 0.2222 0.9601 0.4890 0.068 Uiso 1 1 calc R A . H11E H 0.1613 0.9513 0.5468 0.068 Uiso 1 1 calc R . . H11F H 0.1742 0.8914 0.5018 0.068 Uiso 1 1 calc R . . C12' C 0.1582(5) 0.8761(3) 0.6552(3) 0.0194(15) Uani 1 1 d . . . C13' C 0.1876(5) 0.9425(3) 0.6836(3) 0.0214(16) Uani 1 1 d . A . C14' C 0.2678(5) 0.9498(3) 0.7418(3) 0.0268(17) Uani 1 1 d . . . H14B H 0.3023 0.9133 0.7624 0.032 Uiso 1 1 calc R A . C15' C 0.2978(6) 1.0090(4) 0.7699(4) 0.038(2) Uani 1 1 d . A . H15B H 0.3537 1.0133 0.8093 0.046 Uiso 1 1 calc R . . C16' C 0.2474(7) 1.0619(4) 0.7414(4) 0.043(2) Uani 1 1 d . . . H16B H 0.2679 1.1027 0.7613 0.051 Uiso 1 1 calc R A . C17' C 0.1670(6) 1.0563(4) 0.6838(4) 0.040(2) Uani 1 1 d . A . H17B H 0.1327 1.0931 0.6637 0.048 Uiso 1 1 calc R . . C18' C 0.1373(6) 0.9971(3) 0.6562(3) 0.0300(18) Uani 1 1 d . . . H18B H 0.0808 0.9932 0.6172 0.036 Uiso 1 1 calc R A . N19' N 0.0639(4) 0.8468(3) 0.6594(2) 0.0198(13) Uani 1 1 d . A . C20' C -0.0194(5) 0.8857(3) 0.6757(3) 0.0227(16) Uani 1 1 d . . . C21' C -0.0243(5) 0.8938(3) 0.7410(3) 0.0234(16) Uani 1 1 d . A . C22' C 0.0565(5) 0.8648(3) 0.7955(3) 0.0299(18) Uani 1 1 d . . . H22D H 0.1097 0.8413 0.7779 0.045 Uiso 1 1 calc R A . H22E H 0.0179 0.8355 0.8186 0.045 Uiso 1 1 calc R . . H22F H 0.0950 0.8984 0.8257 0.045 Uiso 1 1 calc R . . C23' C -0.1080(6) 0.9301(3) 0.7536(4) 0.0291(18) Uani 1 1 d . . . H23B H -0.1135 0.9358 0.7974 0.035 Uiso 1 1 calc R A . C24' C -0.1835(6) 0.9580(3) 0.7041(4) 0.0364(19) Uani 1 1 d . A . H24B H -0.2392 0.9832 0.7140 0.044 Uiso 1 1 calc R . . C25' C -0.1777(6) 0.9490(3) 0.6408(4) 0.0333(19) Uani 1 1 d . . . H25B H -0.2302 0.9680 0.6069 0.040 Uiso 1 1 calc R A . C26' C -0.0957(5) 0.9125(3) 0.6249(3) 0.0229(16) Uani 1 1 d . A . C27' C -0.0895(6) 0.9048(3) 0.5545(3) 0.0332(19) Uani 1 1 d . . . H27D H -0.1507 0.9264 0.5262 0.050 Uiso 1 1 calc R A . H27E H -0.0940 0.8594 0.5424 0.050 Uiso 1 1 calc R . . H27F H -0.0199 0.9235 0.5493 0.050 Uiso 1 1 calc R . . N28' N 0.2018(4) 0.6659(2) 0.6165(2) 0.0180(12) Uani 1 1 d . A . C29' C 0.2914(5) 0.6305(3) 0.6023(3) 0.0212(16) Uani 1 1 d . . . C30' C 0.3879(6) 0.6236(3) 0.6495(3) 0.0263(17) Uani 1 1 d . A . C31' C 0.4008(6) 0.6455(4) 0.7197(3) 0.039(2) Uani 1 1 d . . . H31D H 0.4748 0.6365 0.7451 0.059 Uiso 1 1 calc R A . H31E H 0.3465 0.6227 0.7380 0.059 Uiso 1 1 calc R . . H31F H 0.3893 0.6914 0.7213 0.059 Uiso 1 1 calc R . . C32' C 0.4746(6) 0.5947(4) 0.6328(4) 0.041(2) Uani 1 1 d . . . H32B H 0.5413 0.5904 0.6650 0.050 Uiso 1 1 calc R A . C33' C 0.4663(7) 0.5716(4) 0.5697(4) 0.050(2) Uani 1 1 d . A . H33B H 0.5266 0.5518 0.5586 0.060 Uiso 1 1 calc R . . C34' C 0.3691(7) 0.5781(4) 0.5237(4) 0.045(2) Uani 1 1 d . . . H34B H 0.3627 0.5622 0.4806 0.053 Uiso 1 1 calc R A . C35' C 0.2799(6) 0.6073(3) 0.5385(3) 0.0287(17) Uani 1 1 d . A . C36' C 0.1755(6) 0.6150(4) 0.4851(3) 0.041(2) Uani 1 1 d . . . H36D H 0.1841 0.5952 0.4444 0.061 Uiso 1 1 calc R A . H36E H 0.1618 0.6604 0.4784 0.061 Uiso 1 1 calc R . . H36F H 0.1133 0.5943 0.4980 0.061 Uiso 1 1 calc R . . C37' C 0.1225(5) 0.6353(3) 0.6365(3) 0.0148(14) Uani 1 1 d . . . C38' C 0.1321(5) 0.5648(3) 0.6499(3) 0.0215(16) Uani 1 1 d . A . C39' C 0.1757(5) 0.5469(3) 0.7134(3) 0.0228(16) Uani 1 1 d . . . H39B H 0.1973 0.5782 0.7473 0.027 Uiso 1 1 calc R A . C40' C 0.1874(6) 0.4824(3) 0.7269(3) 0.0318(18) Uani 1 1 d . A . H40B H 0.2198 0.4701 0.7702 0.038 Uiso 1 1 calc R . . C41' C 0.1535(6) 0.4367(3) 0.6794(3) 0.0342(19) Uani 1 1 d . . . H41B H 0.1592 0.3929 0.6898 0.041 Uiso 1 1 calc R A . C42' C 0.1109(6) 0.4546(3) 0.6160(3) 0.041(2) Uani 1 1 d . A . H42B H 0.0881 0.4231 0.5822 0.049 Uiso 1 1 calc R . . C43' C 0.1016(6) 0.5186(3) 0.6018(3) 0.040(2) Uani 1 1 d . . . H43B H 0.0736 0.5308 0.5579 0.047 Uiso 1 1 calc R A . N44' N 0.0374(4) 0.6674(3) 0.6462(2) 0.0226(13) Uani 1 1 d . A . C45' C -0.0486(5) 0.6314(3) 0.6650(3) 0.0212(16) Uani 1 1 d . . . C46' C -0.1262(6) 0.5958(3) 0.6191(3) 0.0302(18) Uani 1 1 d . A . C47' C -0.1318(6) 0.5929(4) 0.5479(3) 0.045(2) Uani 1 1 d . . . H47D H -0.1925 0.5640 0.5260 0.068 Uiso 1 1 calc R A . H47E H -0.0627 0.5772 0.5410 0.068 Uiso 1 1 calc R . . H47F H -0.1440 0.6355 0.5300 0.068 Uiso 1 1 calc R . . C48' C -0.2055(6) 0.5594(4) 0.6407(4) 0.040(2) Uani 1 1 d . . . H48B H -0.2564 0.5329 0.6104 0.048 Uiso 1 1 calc R A . C49' C -0.2111(6) 0.5614(3) 0.7055(4) 0.0344(19) Uani 1 1 d . A . H49B H -0.2663 0.5371 0.7190 0.041 Uiso 1 1 calc R . . C50' C -0.1368(6) 0.5983(4) 0.7496(3) 0.0325(19) Uani 1 1 d . . . H50B H -0.1413 0.5997 0.7938 0.039 Uiso 1 1 calc R A . C51' C -0.0541(5) 0.6342(3) 0.7312(3) 0.0250(17) Uani 1 1 d . A . C52' C 0.0269(6) 0.6759(4) 0.7796(3) 0.0341(19) Uani 1 1 d . . . H52D H 0.0762 0.6982 0.7572 0.051 Uiso 1 1 calc R A . H52E H 0.0699 0.6495 0.8137 0.051 Uiso 1 1 calc R . . H52F H -0.0127 0.7071 0.7993 0.051 Uiso 1 1 calc R . . O53' O 0.2920(4) 0.7575(2) 0.5358(2) 0.0220(14) Uani 0.857(6) 1 d PD A 1 C54' C 0.3925(9) 0.7518(5) 0.5279(5) 0.085(4) Uani 0.857(6) 1 d PD A 1 H54C H 0.4227 0.7122 0.5489 0.102 Uiso 0.857(6) 1 calc PR A 1 H54D H 0.4388 0.7879 0.5511 0.102 Uiso 0.857(6) 1 calc PR A 1 C55' C 0.4024(8) 0.7501(5) 0.4573(4) 0.047(3) Uani 0.857(6) 1 d PD A 1 H55C H 0.4752 0.7664 0.4534 0.056 Uiso 0.857(6) 1 calc PR A 1 H55D H 0.3879 0.7068 0.4374 0.056 Uiso 0.857(6) 1 calc PR A 1 C56' C 0.3201(8) 0.7908(5) 0.4308(4) 0.060(3) Uani 0.857(6) 1 d PD A 1 H56C H 0.2862 0.7798 0.3845 0.072 Uiso 0.857(6) 1 calc PR A 1 H56D H 0.3474 0.8357 0.4346 0.072 Uiso 0.857(6) 1 calc PR A 1 C57' C 0.2403(11) 0.7786(5) 0.4737(5) 0.100(5) Uani 0.857(6) 1 d PD A 1 H57C H 0.2022 0.8183 0.4784 0.121 Uiso 0.857(6) 1 calc PR A 1 H57D H 0.1841 0.7462 0.4519 0.121 Uiso 0.857(6) 1 calc PR A 1 O58' O -0.1360(3) 0.7606(2) 0.6336(2) 0.0245(11) Uani 1 1 d . . . C59' C -0.2000(6) 0.7696(3) 0.6806(3) 0.0300(18) Uani 1 1 d . A . H59C H -0.2142 0.8153 0.6853 0.036 Uiso 1 1 calc R . . H59D H -0.1608 0.7539 0.7236 0.036 Uiso 1 1 calc R . . C60' C -0.3039(6) 0.7331(4) 0.6558(4) 0.048(2) Uani 1 1 d . . . H60C H -0.3647 0.7531 0.6702 0.058 Uiso 1 1 calc R A . H60D H -0.2976 0.6888 0.6712 0.058 Uiso 1 1 calc R . . C61' C -0.3224(7) 0.7346(5) 0.5832(4) 0.071(3) Uani 1 1 d . A . H61C H -0.3773 0.7665 0.5649 0.085 Uiso 1 1 calc R . . H61D H -0.3491 0.6923 0.5634 0.085 Uiso 1 1 calc R . . C62' C -0.2130(6) 0.7523(4) 0.5700(3) 0.051(2) Uani 1 1 d . A . H62C H -0.1893 0.7181 0.5442 0.062 Uiso 1 1 calc R . . H62D H -0.2176 0.7922 0.5455 0.062 Uiso 1 1 calc R . . Sb63 Sb -0.24262(4) 0.75467(2) 0.88444(2) 0.03344(14) Uani 1 1 d . . . F64 F -0.3249(3) 0.70233(19) 0.9265(2) 0.0469(12) Uani 1 1 d . . . F65 F -0.1210(4) 0.7082(3) 0.9168(2) 0.0705(16) Uani 1 1 d . . . F66 F -0.2043(3) 0.80934(19) 0.95850(18) 0.0414(11) Uani 1 1 d . . . F67 F -0.3657(4) 0.8011(2) 0.8527(3) 0.0785(18) Uani 1 1 d . . . F68 F -0.2833(5) 0.7020(2) 0.8108(2) 0.088(2) Uani 1 1 d . . . F69 F -0.1610(5) 0.8079(2) 0.8440(2) 0.0807(18) Uani 1 1 d . . . Sb70 Sb -0.09272(18) 0.75802(6) 0.40031(5) 0.0291(4) Uani 0.627(4) 1 d PD B 1 F71 F -0.1711(6) 0.7636(4) 0.3147(3) 0.057(2) Uani 0.627(4) 1 d PD B 1 F72 F -0.1841(7) 0.8177(4) 0.4243(4) 0.046(3) Uani 0.627(4) 1 d PD B 1 F73 F -0.1871(5) 0.6928(3) 0.4138(3) 0.047(2) Uani 0.627(4) 1 d PD B 1 F74 F -0.0018(6) 0.6980(3) 0.3777(4) 0.054(3) Uani 0.627(4) 1 d PD B 1 F75 F 0.0042(5) 0.8237(3) 0.3897(3) 0.044(2) Uani 0.627(4) 1 d PD B 1 F76 F -0.0152(6) 0.7533(4) 0.4882(3) 0.033(2) Uani 0.627(4) 1 d PD B 1 Sb77 Sb -0.0267(3) 0.77560(10) 0.41025(8) 0.0303(8) Uani 0.373(4) 1 d PD B 2 F78 F -0.1653(8) 0.7884(7) 0.4253(7) 0.070(7) Uani 0.373(4) 1 d PD B 2 F79 F -0.0866(9) 0.7833(5) 0.3206(4) 0.055(4) Uani 0.373(4) 1 d PD B 2 F80 F 0.0020(10) 0.8636(4) 0.4167(5) 0.063(5) Uani 0.373(4) 1 d PD B 2 F81 F 0.0329(9) 0.7698(6) 0.4993(4) 0.042(5) Uani 0.373(4) 1 d PD B 2 F82 F -0.0552(12) 0.6890(4) 0.4043(6) 0.092(7) Uani 0.373(4) 1 d PD B 2 F83 F 0.1106(7) 0.7649(6) 0.3945(5) 0.070(5) Uani 0.373(4) 1 d PD B 2 C84A C 0.6131(7) 0.8917(5) 0.3870(4) 0.063(3) Uani 0.64(5) 1 d PDU C 1 H84A H 0.6132 0.9373 0.3761 0.075 Uiso 0.64(5) 1 calc PR C 1 H84B H 0.6850 0.8750 0.3846 0.075 Uiso 0.64(5) 1 calc PR C 1 C84B C 0.6131(7) 0.8917(5) 0.3870(4) 0.063(3) Uani 0.36(5) 1 d PDU C 2 H84C H 0.6612 0.8584 0.3770 0.075 Uiso 0.36(5) 1 calc PR C 2 H84D H 0.6458 0.9339 0.3810 0.075 Uiso 0.36(5) 1 calc PR C 2 Cl85 Cl 0.59903(18) 0.88496(11) 0.46649(10) 0.0557(6) Uani 1 1 d U . . Cl86 Cl 0.511(2) 0.8515(18) 0.3294(5) 0.135(7) Uani 0.64(5) 1 d PDU C 1 Cl87 Cl 0.4799(16) 0.8823(16) 0.3353(14) 0.088(8) Uani 0.36(5) 1 d PDU C 2 C88 C 0.5377(11) 0.6135(6) 0.4085(7) 0.105(4) Uiso 1 1 d . . . Cl89 Cl 0.4665(5) 0.5804(3) 0.3539(3) 0.1130(19) Uiso 0.60 1 d P . . C90 C 0.6512(11) 0.6614(7) 0.4005(6) 0.104(4) Uiso 0.90 1 d P . . C91 C 0.5822(11) 0.6010(7) 0.4531(7) 0.114(5) Uiso 1 1 d . . . Cl92 Cl 0.6068(6) 0.6371(4) 0.2777(4) 0.121(2) Uiso 0.50 1 d P . . C93 C 0.6228(13) 0.5820(8) 0.3801(8) 0.102(5) Uiso 0.75 1 d P . . C94 C 0.5705(13) 0.5886(8) 0.3091(8) 0.106(5) Uiso 0.75 1 d P . . C95 C 0.647(3) 0.708(2) 0.3020(19) 0.157(15) Uiso 0.40 1 d P . . 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 0.0233(5) 0.0155(5) 0.0148(4) -0.0022(3) 0.0090(3) -0.0016(4) Cu2 0.0216(5) 0.0133(5) 0.0177(4) -0.0008(3) 0.0090(4) -0.0014(4) N3 0.018(3) 0.019(3) 0.021(3) -0.002(2) 0.014(2) -0.009(2) C4 0.025(4) 0.019(4) 0.030(4) -0.014(3) 0.017(3) -0.006(3) C5 0.030(4) 0.016(4) 0.031(4) -0.011(3) 0.016(3) -0.007(3) C6 0.050(5) 0.024(4) 0.029(4) -0.004(3) 0.021(4) -0.004(4) C7 0.051(6) 0.029(5) 0.049(5) -0.008(4) 0.031(5) -0.018(4) C8 0.034(5) 0.047(6) 0.067(6) -0.020(5) 0.027(5) -0.017(4) C9 0.032(5) 0.026(5) 0.057(5) -0.018(4) 0.019(4) -0.009(4) C10 0.024(4) 0.021(4) 0.048(5) -0.022(3) 0.014(4) 0.000(3) C11 0.030(5) 0.029(5) 0.046(5) -0.006(4) 0.005(4) 0.009(4) C12 0.016(4) 0.012(4) 0.010(3) 0.004(3) 0.003(3) -0.001(3) C13 0.021(4) 0.012(4) 0.017(3) 0.001(3) 0.011(3) -0.004(3) C14 0.024(4) 0.027(4) 0.021(4) -0.003(3) 0.008(3) 0.004(3) C15 0.033(5) 0.017(4) 0.036(4) 0.004(3) 0.014(4) 0.004(3) C16 0.034(5) 0.013(4) 0.043(5) -0.008(3) 0.019(4) -0.005(3) C17 0.028(4) 0.028(5) 0.036(4) -0.010(3) 0.009(3) 0.001(4) C18 0.026(4) 0.009(4) 0.030(4) -0.002(3) 0.000(3) -0.004(3) N19 0.018(3) 0.014(3) 0.021(3) -0.007(2) 0.007(2) -0.003(2) C20 0.016(4) 0.010(4) 0.036(4) -0.001(3) 0.008(3) -0.008(3) C21 0.020(4) 0.023(4) 0.042(5) -0.013(3) 0.012(4) -0.002(3) C22 0.038(5) 0.041(5) 0.029(4) -0.015(4) 0.013(4) -0.004(4) C23 0.028(5) 0.026(5) 0.062(6) -0.019(4) 0.020(4) -0.005(4) C24 0.026(5) 0.020(4) 0.076(6) 0.003(4) 0.021(4) 0.008(4) C25 0.018(4) 0.040(5) 0.058(6) 0.011(4) 0.006(4) -0.005(4) C26 0.011(4) 0.021(4) 0.045(5) 0.007(3) 0.008(3) -0.004(3) C27 0.025(4) 0.039(5) 0.032(4) 0.014(4) 0.000(3) -0.007(4) N28 0.023(3) 0.020(3) 0.014(3) 0.000(2) 0.005(2) 0.000(3) C29 0.038(5) 0.014(4) 0.016(4) 0.005(3) 0.011(3) 0.002(3) C30 0.024(4) 0.029(4) 0.026(4) -0.003(3) 0.012(3) 0.003(3) C31 0.024(4) 0.042(5) 0.027(4) 0.004(3) 0.005(3) 0.006(4) C32 0.030(5) 0.036(5) 0.030(4) -0.002(3) 0.015(4) 0.003(4) C33 0.043(5) 0.028(5) 0.024(4) -0.009(3) 0.015(4) 0.005(4) C34 0.032(4) 0.026(4) 0.018(4) 0.001(3) 0.003(3) -0.005(3) C35 0.026(4) 0.015(4) 0.017(4) 0.005(3) 0.001(3) -0.002(3) C36 0.028(4) 0.023(4) 0.019(4) 0.004(3) 0.007(3) -0.001(3) C37 0.018(4) 0.009(3) 0.016(3) 0.000(3) 0.004(3) 0.000(3) C38 0.021(4) 0.018(4) 0.024(4) 0.008(3) 0.007(3) 0.005(3) C39 0.034(4) 0.011(4) 0.025(4) 0.004(3) 0.012(3) 0.001(3) C40 0.044(5) 0.014(4) 0.040(5) -0.002(3) 0.019(4) -0.001(4) C41 0.048(5) 0.018(4) 0.043(5) 0.009(4) 0.023(4) 0.010(4) C42 0.039(5) 0.035(5) 0.037(5) 0.017(4) 0.015(4) 0.008(4) C43 0.033(4) 0.022(4) 0.020(4) -0.001(3) 0.013(3) 0.005(3) N44 0.023(3) 0.008(3) 0.021(3) 0.005(2) 0.007(3) 0.000(2) C45 0.035(4) 0.013(4) 0.018(4) 0.005(3) 0.010(3) 0.006(3) C46 0.038(5) 0.024(4) 0.022(4) 0.003(3) 0.012(3) 0.004(3) C47 0.052(5) 0.032(5) 0.013(4) -0.004(3) 0.002(3) 0.001(4) C48 0.056(6) 0.048(6) 0.018(4) -0.006(4) 0.012(4) -0.005(4) C49 0.060(6) 0.044(6) 0.030(5) 0.013(4) 0.027(4) 0.001(4) C50 0.048(5) 0.023(4) 0.028(4) -0.001(3) 0.021(4) -0.007(4) C51 0.027(4) 0.018(4) 0.023(4) -0.003(3) 0.009(3) -0.009(3) C52 0.030(4) 0.025(4) 0.030(4) -0.002(3) 0.016(3) -0.007(3) O53 0.024(3) 0.036(3) 0.014(2) 0.004(2) 0.010(2) 0.000(2) C54 0.021(4) 0.040(5) 0.021(4) -0.007(3) 0.007(3) 0.001(3) C55 0.048(6) 0.146(11) 0.024(5) 0.001(5) 0.016(4) 0.024(6) C56 0.044(5) 0.066(6) 0.019(4) 0.015(4) 0.014(4) -0.001(4) C57 0.020(4) 0.040(5) 0.020(4) -0.001(3) 0.002(3) -0.002(3) O58 0.017(3) 0.031(3) 0.032(3) 0.005(2) 0.010(2) -0.001(2) C59 0.043(5) 0.032(5) 0.030(4) -0.005(3) 0.025(4) -0.004(4) C60 0.026(5) 0.065(6) 0.043(5) 0.012(4) 0.017(4) -0.002(4) C61 0.019(4) 0.038(5) 0.055(5) -0.005(4) 0.010(4) -0.008(4) C62 0.026(4) 0.031(5) 0.042(5) 0.011(4) 0.005(4) 0.005(4) Cu1' 0.0237(5) 0.0150(5) 0.0192(4) -0.0003(3) 0.0093(4) -0.0004(4) Cu2' 0.0262(5) 0.0173(5) 0.0224(4) -0.0018(4) 0.0104(4) -0.0021(4) N3' 0.025(3) 0.022(3) 0.024(3) 0.002(2) 0.013(3) 0.004(3) C4' 0.020(4) 0.017(4) 0.022(4) -0.005(3) 0.013(3) -0.001(3) C5' 0.022(4) 0.024(4) 0.029(4) -0.007(3) 0.012(3) -0.002(3) C6' 0.021(4) 0.053(6) 0.056(5) 0.023(4) 0.008(4) 0.011(4) C7' 0.031(5) 0.041(5) 0.029(4) -0.011(4) 0.011(4) -0.002(4) C8' 0.029(5) 0.057(6) 0.031(4) 0.004(4) 0.019(4) -0.017(4) C9' 0.050(5) 0.036(5) 0.027(4) 0.003(3) 0.024(4) -0.016(4) C10' 0.031(5) 0.030(5) 0.027(4) 0.000(3) 0.012(3) -0.003(4) C11' 0.040(5) 0.063(6) 0.036(5) 0.009(4) 0.015(4) -0.004(4) C12' 0.027(4) 0.013(4) 0.020(4) 0.006(3) 0.008(3) -0.003(3) C13' 0.021(4) 0.016(4) 0.029(4) 0.005(3) 0.011(3) 0.000(3) C14' 0.026(4) 0.022(4) 0.037(4) 0.002(3) 0.014(4) 0.004(3) C15' 0.037(5) 0.043(6) 0.039(5) -0.015(4) 0.019(4) -0.004(4) C16' 0.041(5) 0.031(5) 0.066(6) -0.022(4) 0.034(5) -0.008(4) C17' 0.047(6) 0.018(5) 0.062(6) 0.005(4) 0.029(5) 0.000(4) C18' 0.030(5) 0.026(5) 0.034(4) 0.001(3) 0.010(3) -0.004(4) N19' 0.012(3) 0.025(3) 0.021(3) -0.002(2) 0.003(2) -0.003(3) C20' 0.018(4) 0.019(4) 0.032(4) -0.006(3) 0.010(3) -0.006(3) C21' 0.029(4) 0.020(4) 0.025(4) -0.005(3) 0.015(3) -0.006(3) C22' 0.035(5) 0.023(4) 0.034(4) -0.003(3) 0.015(4) -0.007(3) C23' 0.032(5) 0.023(4) 0.040(5) -0.007(3) 0.026(4) -0.004(4) C24' 0.022(4) 0.029(5) 0.064(6) -0.011(4) 0.022(4) 0.007(4) C25' 0.025(5) 0.021(4) 0.053(5) 0.001(4) 0.007(4) 0.005(3) C26' 0.021(4) 0.022(4) 0.027(4) 0.000(3) 0.006(3) -0.003(3) C27' 0.031(5) 0.038(5) 0.028(4) 0.003(3) 0.003(3) 0.004(4) N28' 0.024(3) 0.016(3) 0.014(3) 0.001(2) 0.006(2) -0.004(3) C29' 0.022(4) 0.014(4) 0.028(4) -0.003(3) 0.008(3) -0.006(3) C30' 0.028(4) 0.017(4) 0.033(4) 0.002(3) 0.005(3) 0.004(3) C31' 0.037(5) 0.043(5) 0.030(4) 0.012(4) -0.007(4) -0.001(4) C32' 0.031(5) 0.027(5) 0.064(6) 0.011(4) 0.006(4) 0.007(4) C33' 0.048(6) 0.042(6) 0.069(6) -0.010(5) 0.031(5) 0.017(5) C34' 0.062(6) 0.029(5) 0.050(5) -0.019(4) 0.029(5) 0.000(4) C35' 0.026(4) 0.031(5) 0.031(4) -0.007(3) 0.011(3) 0.000(3) C36' 0.050(6) 0.040(5) 0.028(4) -0.009(4) 0.005(4) -0.007(4) C37' 0.028(4) 0.010(4) 0.003(3) -0.005(2) -0.002(3) -0.001(3) C38' 0.035(4) 0.012(4) 0.019(4) 0.001(3) 0.011(3) -0.003(3) C39' 0.031(4) 0.018(4) 0.019(4) -0.002(3) 0.006(3) 0.000(3) C40' 0.043(5) 0.032(5) 0.021(4) 0.002(3) 0.009(4) 0.001(4) C41' 0.067(6) 0.006(4) 0.034(4) 0.000(3) 0.021(4) 0.004(4) C42' 0.072(6) 0.029(5) 0.020(4) -0.012(3) 0.011(4) -0.012(4) C43' 0.069(6) 0.021(5) 0.022(4) 0.003(3) -0.001(4) 0.001(4) N44' 0.029(4) 0.026(4) 0.011(3) -0.001(2) 0.001(3) -0.003(3) C45' 0.025(4) 0.016(4) 0.027(4) 0.001(3) 0.015(3) -0.001(3) C46' 0.041(5) 0.015(4) 0.033(4) -0.004(3) 0.007(4) -0.005(3) C47' 0.056(6) 0.050(6) 0.028(4) -0.009(4) 0.011(4) -0.017(4) C48' 0.038(5) 0.030(5) 0.053(5) -0.007(4) 0.013(4) -0.007(4) C49' 0.037(5) 0.025(5) 0.043(5) 0.013(4) 0.013(4) -0.003(4) C50' 0.032(5) 0.040(5) 0.029(4) 0.016(4) 0.013(4) 0.003(4) C51' 0.021(4) 0.025(4) 0.031(4) 0.007(3) 0.011(3) 0.005(3) C52' 0.037(5) 0.049(5) 0.019(4) 0.000(3) 0.012(3) 0.005(4) O53' 0.018(3) 0.025(3) 0.028(3) 0.005(3) 0.016(3) 0.004(2) C54' 0.135(12) 0.022(7) 0.129(11) -0.019(7) 0.095(10) -0.026(7) C55' 0.048(7) 0.045(7) 0.053(6) -0.023(5) 0.027(5) -0.009(5) C56' 0.076(9) 0.072(9) 0.037(6) 0.011(5) 0.023(6) -0.021(7) C57' 0.211(17) 0.039(8) 0.074(9) -0.004(6) 0.079(11) -0.009(9) O58' 0.016(3) 0.030(3) 0.028(3) -0.002(2) 0.007(2) -0.002(2) C59' 0.036(5) 0.024(4) 0.032(4) -0.004(3) 0.012(4) 0.002(4) C60' 0.040(5) 0.051(6) 0.056(6) -0.012(4) 0.017(4) -0.010(4) C61' 0.039(6) 0.121(10) 0.044(6) 0.027(6) -0.006(4) -0.025(6) C62' 0.048(6) 0.072(7) 0.027(4) 0.000(4) -0.003(4) -0.026(5) Sb63 0.0448(4) 0.0254(3) 0.0306(3) 0.0002(2) 0.0109(2) -0.0061(3) F64 0.060(3) 0.022(3) 0.070(3) 0.008(2) 0.038(3) -0.002(2) F65 0.048(3) 0.085(4) 0.087(4) 0.005(3) 0.033(3) 0.016(3) F66 0.041(3) 0.042(3) 0.035(2) -0.012(2) -0.001(2) -0.001(2) F67 0.058(3) 0.053(4) 0.096(4) 0.026(3) -0.036(3) -0.012(3) F68 0.184(6) 0.041(3) 0.035(3) -0.015(2) 0.027(3) -0.051(4) F69 0.127(5) 0.057(4) 0.077(4) -0.012(3) 0.067(4) -0.039(3) Sb70 0.0362(11) 0.0269(6) 0.0239(5) -0.0006(4) 0.0064(5) 0.0024(6) F71 0.067(6) 0.072(6) 0.025(4) -0.004(4) -0.003(4) -0.001(5) F72 0.048(6) 0.050(6) 0.041(5) -0.004(4) 0.013(4) 0.027(5) F73 0.049(5) 0.039(5) 0.054(5) -0.009(3) 0.017(4) -0.008(4) F74 0.062(6) 0.042(6) 0.062(6) -0.009(4) 0.017(5) 0.018(4) F75 0.046(5) 0.035(5) 0.050(5) 0.016(4) 0.009(4) -0.001(4) F76 0.036(6) 0.036(5) 0.028(4) 0.009(4) 0.005(4) 0.004(4) Sb77 0.0397(18) 0.0290(11) 0.0191(8) -0.0045(7) 0.0013(8) -0.0001(11) F78 0.034(9) 0.12(2) 0.047(10) -0.005(11) -0.004(7) 0.031(11) F79 0.078(11) 0.058(10) 0.025(7) 0.016(6) 0.005(7) 0.012(8) F80 0.099(12) 0.018(8) 0.049(9) -0.003(6) -0.022(8) -0.007(8) F81 0.035(10) 0.037(9) 0.039(8) -0.014(6) -0.021(7) -0.004(7) F82 0.18(2) 0.031(9) 0.053(11) 0.007(7) -0.004(11) -0.021(11) F83 0.065(10) 0.097(13) 0.047(8) 0.015(8) 0.007(7) 0.001(9) C84A 0.067(6) 0.079(8) 0.045(5) 0.008(5) 0.020(4) -0.016(5) C84B 0.067(6) 0.079(8) 0.045(5) 0.008(5) 0.020(4) -0.016(5) Cl85 0.0604(15) 0.0688(17) 0.0357(12) -0.0020(11) 0.0083(11) -0.0081(12) Cl86 0.197(10) 0.174(17) 0.023(3) -0.015(5) 0.018(5) -0.104(11) Cl87 0.100(9) 0.109(14) 0.035(7) 0.026(7) -0.017(6) -0.042(9) _geom_special_details ; All esds are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances and angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. ; 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 N3 1.890(5) . ? Cu1 N28 1.890(5) . ? Cu1 O53 2.098(4) . ? Cu1 Cu2 2.3974(11) . ? Cu2 N19 1.888(5) . ? Cu2 N44 1.900(5) . ? Cu2 O58 2.138(4) . ? N3 C12 1.341(7) . ? N3 C4 1.440(7) . ? C4 C5 1.387(9) . ? C4 C10 1.398(9) . ? C5 C7 1.370(9) . ? C5 C6 1.511(9) . ? C7 C8 1.364(10) . ? C8 C9 1.357(10) . ? C9 C10 1.404(9) . ? C10 C11 1.512(9) . ? C12 N19 1.319(7) . ? C12 C13 1.502(8) . ? C13 C14 1.372(8) . ? C13 C18 1.388(8) . ? C14 C15 1.380(9) . ? C15 C16 1.377(9) . ? C16 C17 1.373(9) . ? C17 C18 1.375(9) . ? N19 C20 1.450(8) . ? C20 C26 1.384(9) . ? C20 C21 1.399(9) . ? C21 C23 1.406(9) . ? C21 C22 1.512(9) . ? C23 C24 1.387(10) . ? C24 C25 1.370(10) . ? C25 C26 1.406(9) . ? C26 C27 1.490(9) . ? N28 C37 1.352(7) . ? N28 C29 1.429(8) . ? C29 C30 1.389(9) . ? C29 C35 1.411(8) . ? C30 C32 1.408(9) . ? C30 C31 1.515(9) . ? C32 C33 1.385(9) . ? C33 C34 1.374(9) . ? C34 C35 1.386(9) . ? C35 C36 1.510(8) . ? C37 N44 1.311(7) . ? C37 C38 1.489(8) . ? C38 C43 1.390(8) . ? C38 C39 1.391(9) . ? C39 C40 1.375(9) . ? C40 C41 1.379(9) . ? C41 C42 1.367(10) . ? C42 C43 1.403(9) . ? N44 C45 1.436(7) . ? C45 C51 1.392(8) . ? C45 C46 1.406(9) . ? C46 C48 1.374(9) . ? C46 C47 1.511(9) . ? C48 C49 1.376(10) . ? C49 C50 1.386(10) . ? C50 C51 1.372(8) . ? C51 C52 1.520(8) . ? O53 C57 1.447(7) . ? O53 C54 1.460(7) . ? C54 C55 1.496(9) . ? C55 C56 1.461(10) . ? C56 C57 1.512(8) . ? O58 C62 1.431(7) . ? O58 C59 1.453(7) . ? C59 C60 1.518(9) . ? C60 C61 1.539(9) . ? C61 C62 1.522(8) . ? Cu1' N28' 1.891(5) . ? Cu1' N3' 1.900(5) . ? Cu1' O53' 2.083(5) . ? Cu1' Cu2' 2.4423(12) . ? Cu2' N19' 1.901(5) . ? Cu2' N44' 1.908(5) . ? Cu2' O58' 2.108(4) . ? N3' C12' 1.324(8) . ? N3' C4' 1.434(7) . ? C4' C10' 1.402(9) . ? C4' C5' 1.404(8) . ? C5' C7' 1.401(9) . ? C5' C6' 1.492(9) . ? C7' C8' 1.337(9) . ? C8' C9' 1.375(9) . ? C9' C10' 1.383(9) . ? C10' C11' 1.508(9) . ? C12' N19' 1.342(7) . ? C12' C13' 1.510(9) . ? C13' C18' 1.392(9) . ? C13' C14' 1.393(9) . ? C14' C15' 1.374(9) . ? C15' C16' 1.369(10) . ? C16' C17' 1.382(10) . ? C17' C18' 1.369(10) . ? N19' C20' 1.448(8) . ? C20' C26' 1.392(9) . ? C20' C21' 1.405(9) . ? C21' C23' 1.391(9) . ? C21' C22' 1.489(9) . ? C23' C24' 1.381(10) . ? C24' C25' 1.369(10) . ? C25' C26' 1.403(9) . ? C26' C27' 1.516(9) . ? N28' C37' 1.327(7) . ? N28' C29' 1.454(8) . ? C29' C30' 1.384(8) . ? C29' C35' 1.398(9) . ? C30' C32' 1.377(9) . ? C30' C31' 1.515(9) . ? C32' C33' 1.391(11) . ? C33' C34' 1.377(10) . ? C34' C35' 1.390(9) . ? C35' C36' 1.525(9) . ? C37' N44' 1.336(8) . ? C37' C38' 1.514(8) . ? C38' C43' 1.373(9) . ? C38' C39' 1.383(8) . ? C39' C40' 1.395(9) . ? C40' C41' 1.362(9) . ? C41' C42' 1.381(9) . ? C42' C43' 1.386(9) . ? N44' C45' 1.438(7) . ? C45' C46' 1.390(9) . ? C45' C51' 1.420(8) . ? C46' C48' 1.405(9) . ? C46' C47' 1.488(9) . ? C48' C49' 1.388(10) . ? C49' C50' 1.362(10) . ? C50' C51' 1.400(9) . ? C51' C52' 1.505(9) . ? O53' C54' 1.322(10) . ? O53' C57' 1.401(11) . ? C54' C55' 1.528(11) . ? C55' C56' 1.379(13) . ? C56' C57' 1.526(11) . ? O58' C59' 1.434(7) . ? O58' C62' 1.457(7) . ? C59' C60' 1.472(9) . ? C60' C61' 1.496(10) . ? C61' C62' 1.505(10) . ? Sb63 F65 1.831(5) . ? Sb63 F67 1.843(5) . ? Sb63 F69 1.850(4) . ? Sb63 F68 1.855(4) . ? Sb63 F64 1.866(4) . ? Sb63 F66 1.884(4) . ? Sb70 F71 1.847(5) . ? Sb70 F73 1.858(5) . ? Sb70 F74 1.858(6) . ? Sb70 F75 1.866(6) . ? Sb70 F72 1.867(6) . ? Sb70 F76 1.883(6) . ? Sb77 F82 1.840(8) . ? Sb77 F83 1.853(8) . ? Sb77 F81 1.857(8) . ? Sb77 F78 1.869(9) . ? Sb77 F79 1.872(7) . ? Sb77 F80 1.870(8) . ? C84A Cl86 1.733(11) . ? C84A Cl85 1.739(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 H43A 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9500 . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C6' H6'A 0.9800 . ? C6' H6'B 0.9800 . ? C6' H6'C 0.9800 . ? C7' H7'A 0.9500 . ? C8' H8'A 0.9500 . ? C9' H9'A 0.9500 . ? C11' H11D 0.9800 . ? C11' H11E 0.9800 . ? C11' H11F 0.9800 . ? C14' H14B 0.9500 . ? C15' H15B 0.9500 . ? C16' H16B 0.9500 . ? C17' H17B 0.9500 . ? C18' H18B 0.9500 . ? C22' H22D 0.9800 . ? C22' H22E 0.9800 . ? C22' H22F 0.9800 . ? C23' H23B 0.9500 . ? C24' H24B 0.9500 . ? C25' H25B 0.9500 . ? C27' H27D 0.9800 . ? C27' H27E 0.9800 . ? C27' H27F 0.9800 . ? C31' H31D 0.9800 . ? C31' H31E 0.9800 . ? C31' H31F 0.9800 . ? C32' H32B 0.9500 . ? C33' H33B 0.9500 . ? C34' H34B 0.9500 . ? C36' H36D 0.9800 . ? C36' H36E 0.9800 . ? C36' H36F 0.9800 . ? C39' H39B 0.9500 . ? C40' H40B 0.9500 . ? C41' H41B 0.9500 . ? C42' H42B 0.9500 . ? C43' H43B 0.9500 . ? C47' H47D 0.9800 . ? C47' H47E 0.9800 . ? C47' H47F 0.9800 . ? C48' H48B 0.9500 . ? C49' H49B 0.9500 . ? C50' H50B 0.9500 . ? C52' H52D 0.9800 . ? C52' H52E 0.9800 . ? C52' H52F 0.9800 . ? C54' H54C 0.9900 . ? C54' H54D 0.9900 . ? C55' H55C 0.9900 . ? C55' H55D 0.9900 . ? C56' H56C 0.9900 . ? C56' H56D 0.9900 . ? C57' H57C 0.9900 . ? C57' H57D 0.9900 . ? C59' H59C 0.9900 . ? C59' H59D 0.9900 . ? C60' H60C 0.9900 . ? C60' H60D 0.9900 . ? C61' H61C 0.9900 . ? C61' H61D 0.9900 . ? C62' H62C 0.9900 . ? C62' H62D 0.9900 . ? C84A H84A 0.9900 . ? C84A H84B 0.9900 . ? 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 N3 Cu1 N28 163.4(2) . . ? N3 Cu1 O53 93.76(19) . . ? N28 Cu1 O53 97.98(19) . . ? N3 Cu1 Cu2 86.68(14) . . ? N28 Cu1 Cu2 88.28(15) . . ? O53 Cu1 Cu2 152.55(12) . . ? N19 Cu2 N44 162.4(2) . . ? N19 Cu2 O58 100.01(19) . . ? N44 Cu2 O58 94.28(19) . . ? N19 Cu2 Cu1 86.44(15) . . ? N44 Cu2 Cu1 85.23(15) . . ? O58 Cu2 Cu1 153.84(13) . . ? C12 N3 C4 121.9(5) . . ? C12 N3 Cu1 121.0(4) . . ? C4 N3 Cu1 117.1(4) . . ? C5 C4 C10 121.3(6) . . ? C5 C4 N3 120.7(6) . . ? C10 C4 N3 117.8(6) . . ? C7 C5 C4 117.8(7) . . ? C7 C5 C6 120.4(7) . . ? C4 C5 C6 121.7(6) . . ? C8 C7 C5 122.7(7) . . ? C9 C8 C7 119.5(7) . . ? C8 C9 C10 121.0(8) . . ? C4 C10 C9 117.8(7) . . ? C4 C10 C11 122.3(6) . . ? C9 C10 C11 119.9(7) . . ? N19 C12 N3 117.5(5) . . ? N19 C12 C13 121.6(5) . . ? N3 C12 C13 120.8(5) . . ? C14 C13 C18 119.3(6) . . ? C14 C13 C12 124.1(6) . . ? C18 C13 C12 116.5(5) . . ? C13 C14 C15 120.3(6) . . ? C16 C15 C14 120.1(6) . . ? C17 C16 C15 119.9(6) . . ? C16 C17 C18 120.0(7) . . ? C17 C18 C13 120.4(6) . . ? C12 N19 C20 118.2(5) . . ? C12 N19 Cu2 120.0(4) . . ? C20 N19 Cu2 121.6(4) . . ? C26 C20 C21 122.5(6) . . ? C26 C20 N19 117.9(6) . . ? C21 C20 N19 119.5(6) . . ? C20 C21 C23 117.6(7) . . ? C20 C21 C22 122.1(6) . . ? C23 C21 C22 120.2(6) . . ? C24 C23 C21 120.2(7) . . ? C25 C24 C23 121.1(7) . . ? C24 C25 C26 120.3(7) . . ? C20 C26 C25 118.2(7) . . ? C20 C26 C27 121.5(6) . . ? C25 C26 C27 120.3(6) . . ? C37 N28 C29 118.8(5) . . ? C37 N28 Cu1 117.6(4) . . ? C29 N28 Cu1 123.3(4) . . ? C30 C29 C35 121.8(6) . . ? C30 C29 N28 119.9(6) . . ? C35 C29 N28 118.2(6) . . ? C29 C30 C32 118.5(6) . . ? C29 C30 C31 122.7(6) . . ? C32 C30 C31 118.8(6) . . ? C33 C32 C30 120.1(7) . . ? C34 C33 C32 120.3(7) . . ? C33 C34 C35 121.9(6) . . ? C34 C35 C29 117.5(6) . . ? C34 C35 C36 122.1(6) . . ? C29 C35 C36 120.4(6) . . ? N44 C37 N28 117.9(5) . . ? N44 C37 C38 120.6(5) . . ? N28 C37 C38 121.2(5) . . ? C43 C38 C39 119.0(6) . . ? C43 C38 C37 117.0(6) . . ? C39 C38 C37 123.9(6) . . ? C40 C39 C38 121.0(7) . . ? C39 C40 C41 119.7(7) . . ? C42 C41 C40 120.6(7) . . ? C41 C42 C43 120.1(7) . . ? C38 C43 C42 119.6(6) . . ? C37 N44 C45 122.1(5) . . ? C37 N44 Cu2 123.0(4) . . ? C45 N44 Cu2 114.9(4) . . ? C51 C45 C46 121.0(6) . . ? C51 C45 N44 120.9(5) . . ? C46 C45 N44 118.0(6) . . ? C48 C46 C45 118.1(6) . . ? C48 C46 C47 120.6(6) . . ? C45 C46 C47 121.4(6) . . ? C46 C48 C49 121.4(7) . . ? C48 C49 C50 119.7(6) . . ? C51 C50 C49 120.7(7) . . ? C50 C51 C45 118.9(6) . . ? C50 C51 C52 118.9(6) . . ? C45 C51 C52 122.2(5) . . ? C57 O53 C54 110.3(4) . . ? C57 O53 Cu1 116.1(3) . . ? C54 O53 Cu1 132.0(4) . . ? O53 C54 C55 103.7(5) . . ? C56 C55 C54 105.6(7) . . ? C55 C56 C57 103.5(6) . . ? O53 C57 C56 104.7(5) . . ? C62 O58 C59 104.6(5) . . ? C62 O58 Cu2 117.7(4) . . ? C59 O58 Cu2 135.7(4) . . ? O58 C59 C60 104.6(5) . . ? C59 C60 C61 105.5(5) . . ? C62 C61 C60 102.8(6) . . ? O58 C62 C61 106.7(5) . . ? N28' Cu1' N3' 161.6(2) . . ? N28' Cu1' O53' 96.6(2) . . ? N3' Cu1' O53' 95.7(2) . . ? N28' Cu1' Cu2' 88.03(16) . . ? N3' Cu1' Cu2' 88.37(16) . . ? O53' Cu1' Cu2' 149.51(14) . . ? N19' Cu2' N44' 164.3(2) . . ? N19' Cu2' O58' 96.3(2) . . ? N44' Cu2' O58' 93.8(2) . . ? N19' Cu2' Cu1' 87.14(15) . . ? N44' Cu2' Cu1' 87.67(17) . . ? O58' Cu2' Cu1' 158.90(12) . . ? C12' N3' C4' 118.9(5) . . ? C12' N3' Cu1' 122.3(4) . . ? C4' N3' Cu1' 118.8(4) . . ? C10' C4' C5' 120.0(6) . . ? C10' C4' N3' 120.4(6) . . ? C5' C4' N3' 119.3(5) . . ? C7' C5' C4' 118.6(6) . . ? C7' C5' C6' 121.2(6) . . ? C4' C5' C6' 120.3(6) . . ? C8' C7' C5' 121.3(7) . . ? C7' C8' C9' 120.1(6) . . ? C8' C9' C10' 122.0(6) . . ? C9' C10' C4' 117.9(6) . . ? C9' C10' C11' 119.4(6) . . ? C4' C10' C11' 122.6(6) . . ? N3' C12' N19' 118.8(6) . . ? N3' C12' C13' 120.5(6) . . ? N19' C12' C13' 120.3(6) . . ? C18' C13' C14' 117.5(6) . . ? C18' C13' C12' 124.1(6) . . ? C14' C13' C12' 118.4(6) . . ? C15' C14' C13' 121.0(7) . . ? C16' C15' C14' 120.1(7) . . ? C15' C16' C17' 120.5(7) . . ? C18' C17' C16' 119.1(7) . . ? C17' C18' C13' 121.9(7) . . ? C12' N19' C20' 117.5(5) . . ? C12' N19' Cu2' 123.0(4) . . ? C20' N19' Cu2' 119.4(4) . . ? C26' C20' C21' 121.7(6) . . ? C26' C20' N19' 118.1(6) . . ? C21' C20' N19' 120.2(6) . . ? C23' C21' C20' 117.7(6) . . ? C23' C21' C22' 120.4(6) . . ? C20' C21' C22' 121.9(6) . . ? C24' C23' C21' 121.7(7) . . ? C25' C24' C23' 119.7(7) . . ? C24' C25' C26' 121.3(7) . . ? C20' C26' C25' 118.0(6) . . ? C20' C26' C27' 121.8(6) . . ? C25' C26' C27' 120.2(6) . . ? C37' N28' C29' 119.7(5) . . ? C37' N28' Cu1' 122.6(4) . . ? C29' N28' Cu1' 117.6(4) . . ? C30' C29' C35' 121.1(6) . . ? C30' C29' N28' 120.7(6) . . ? C35' C29' N28' 118.0(6) . . ? C32' C30' C29' 119.2(7) . . ? C32' C30' C31' 118.6(7) . . ? C29' C30' C31' 122.2(6) . . ? C30' C32' C33' 121.2(7) . . ? C34' C33' C32' 118.7(7) . . ? C33' C34' C35' 121.9(7) . . ? C34' C35' C29' 117.9(7) . . ? C34' C35' C36' 119.6(7) . . ? C29' C35' C36' 122.5(6) . . ? N28' C37' N44' 119.5(6) . . ? N28' C37' C38' 119.2(6) . . ? N44' C37' C38' 121.2(6) . . ? C43' C38' C39' 119.2(6) . . ? C43' C38' C37' 122.9(6) . . ? C39' C38' C37' 118.0(6) . . ? C38' C39' C40' 119.2(6) . . ? C41' C40' C39' 121.4(6) . . ? C40' C41' C42' 119.3(7) . . ? C41' C42' C43' 119.7(7) . . ? C38' C43' C42' 121.2(6) . . ? C37' N44' C45' 117.1(5) . . ? C37' N44' Cu2' 121.8(4) . . ? C45' N44' Cu2' 120.9(4) . . ? C46' C45' C51' 120.6(6) . . ? C46' C45' N44' 120.8(6) . . ? C51' C45' N44' 118.6(6) . . ? C45' C46' C48' 118.3(6) . . ? C45' C46' C47' 124.8(6) . . ? C48' C46' C47' 117.0(7) . . ? C49' C48' C46' 121.5(7) . . ? C50' C49' C48' 119.5(7) . . ? C49' C50' C51' 121.6(7) . . ? C50' C51' C45' 118.4(6) . . ? C50' C51' C52' 121.7(6) . . ? C45' C51' C52' 119.8(6) . . ? C54' O53' C57' 99.2(8) . . ? C54' O53' Cu1' 140.0(6) . . ? C57' O53' Cu1' 120.1(6) . . ? O53' C54' C55' 115.6(9) . . ? C56' C55' C54' 99.1(8) . . ? C55' C56' C57' 101.0(8) . . ? O53' C57' C56' 113.0(9) . . ? C59' O58' C62' 107.0(5) . . ? C59' O58' Cu2' 132.3(4) . . ? C62' O58' Cu2' 120.7(4) . . ? O58' C59' C60' 106.5(6) . . ? C59' C60' C61' 104.3(6) . . ? C60' C61' C62' 106.1(6) . . ? O58' C62' C61' 106.2(6) . . ? F65 Sb63 F67 179.3(2) . . ? F65 Sb63 F69 90.1(2) . . ? F67 Sb63 F69 90.5(3) . . ? F65 Sb63 F68 91.4(3) . . ? F67 Sb63 F68 88.9(3) . . ? F69 Sb63 F68 91.5(2) . . ? F65 Sb63 F64 90.2(2) . . ? F67 Sb63 F64 89.2(2) . . ? F69 Sb63 F64 178.8(2) . . ? F68 Sb63 F64 89.6(2) . . ? F65 Sb63 F66 90.0(2) . . ? F67 Sb63 F66 89.7(2) . . ? F69 Sb63 F66 88.5(2) . . ? F68 Sb63 F66 178.6(2) . . ? F64 Sb63 F66 90.36(18) . . ? F71 Sb70 F73 90.6(3) . . ? F71 Sb70 F74 91.5(3) . . ? F73 Sb70 F74 89.7(3) . . ? F71 Sb70 F75 91.3(3) . . ? F73 Sb70 F75 178.1(3) . . ? F74 Sb70 F75 90.6(3) . . ? F71 Sb70 F72 89.2(3) . . ? F73 Sb70 F72 89.7(3) . . ? F74 Sb70 F72 179.1(4) . . ? F75 Sb70 F72 90.0(3) . . ? F71 Sb70 F76 178.8(3) . . ? F73 Sb70 F76 89.1(3) . . ? F74 Sb70 F76 89.7(3) . . ? F75 Sb70 F76 89.0(3) . . ? F72 Sb70 F76 89.6(3) . . ? F82 Sb77 F83 91.1(5) . . ? F82 Sb77 F81 90.1(4) . . ? F83 Sb77 F81 90.3(4) . . ? F82 Sb77 F78 90.1(5) . . ? F83 Sb77 F78 178.6(6) . . ? F81 Sb77 F78 90.4(5) . . ? F82 Sb77 F79 91.1(4) . . ? F83 Sb77 F79 89.9(4) . . ? F81 Sb77 F79 178.8(5) . . ? F78 Sb77 F79 89.5(5) . . ? F82 Sb77 F80 179.7(5) . . ? F83 Sb77 F80 89.0(5) . . ? F81 Sb77 F80 89.7(4) . . ? F78 Sb77 F80 89.7(5) . . ? F79 Sb77 F80 89.1(4) . . ? Cl86 C84A Cl85 113.7(6) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 H7A 118.6 . . ? C5 C7 H7A 118.6 . . ? C9 C8 H8A 120.3 . . ? C7 C8 H8A 120.3 . . ? C8 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.9 . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C17 C18 H18A 119.8 . . ? C13 C18 H18A 119.8 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 119.9 . . ? C21 C23 H23A 119.9 . . ? C25 C24 H24A 119.4 . . ? C23 C24 H24A 119.4 . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 H32A 120.0 . . ? C30 C32 H32A 120.0 . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C33 C34 H34A 119.0 . . ? C35 C34 H34A 119.0 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C40 C39 H39A 119.5 . . ? C38 C39 H39A 119.5 . . ? C39 C40 H40A 120.1 . . ? C41 C40 H40A 120.1 . . ? C42 C41 H41A 119.7 . . ? C40 C41 H41A 119.7 . . ? C41 C42 H42A 119.9 . . ? C43 C42 H42A 119.9 . . ? C38 C43 H43A 120.2 . . ? C42 C43 H43A 120.2 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 119.3 . . ? C49 C48 H48A 119.3 . . ? C48 C49 H49A 120.1 . . ? C50 C49 H49A 120.1 . . ? C51 C50 H50A 119.6 . . ? C49 C50 H50A 119.6 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O53 C54 H54A 111.0 . . ? C55 C54 H54A 111.0 . . ? O53 C54 H54B 111.0 . . ? C55 C54 H54B 111.0 . . ? H54A C54 H54B 109.0 . . ? C56 C55 H55A 110.6 . . ? C54 C55 H55A 110.6 . . ? C56 C55 H55B 110.6 . . ? C54 C55 H55B 110.6 . . ? H55A C55 H55B 108.8 . . ? C55 C56 H56A 111.1 . . ? C57 C56 H56A 111.1 . . ? C55 C56 H56B 111.1 . . ? C57 C56 H56B 111.1 . . ? H56A C56 H56B 109.0 . . ? O53 C57 H57A 110.8 . . ? C56 C57 H57A 110.8 . . ? O53 C57 H57B 110.8 . . ? C56 C57 H57B 110.8 . . ? H57A C57 H57B 108.9 . . ? O58 C59 H59A 110.8 . . ? C60 C59 H59A 110.8 . . ? O58 C59 H59B 110.8 . . ? C60 C59 H59B 110.8 . . ? H59A C59 H59B 108.9 . . ? C59 C60 H60A 110.7 . . ? C61 C60 H60A 110.7 . . ? C59 C60 H60B 110.7 . . ? C61 C60 H60B 110.7 . . ? H60A C60 H60B 108.8 . . ? C62 C61 H61A 111.2 . . ? C60 C61 H61A 111.2 . . ? C62 C61 H61B 111.2 . . ? C60 C61 H61B 111.2 . . ? H61A C61 H61B 109.1 . . ? O58 C62 H62A 110.4 . . ? C61 C62 H62A 110.4 . . ? O58 C62 H62B 110.4 . . ? C61 C62 H62B 110.4 . . ? H62A C62 H62B 108.6 . . ? C5' C6' H6'A 109.5 . . ? C5' C6' H6'B 109.5 . . ? H6'A C6' H6'B 109.5 . . ? C5' C6' H6'C 109.5 . . ? H6'A C6' H6'C 109.5 . . ? H6'B C6' H6'C 109.5 . . ? C8' C7' H7'A 119.4 . . ? C5' C7' H7'A 119.4 . . ? C7' C8' H8'A 120.0 . . ? C9' C8' H8'A 120.0 . . ? C8' C9' H9'A 119.0 . . ? C10' C9' H9'A 119.0 . . ? C10' C11' H11D 109.5 . . ? C10' C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? C10' C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C15' C14' H14B 119.5 . . ? C13' C14' H14B 119.5 . . ? C16' C15' H15B 120.0 . . ? C14' C15' H15B 120.0 . . ? C15' C16' H16B 119.8 . . ? C17' C16' H16B 119.8 . . ? C18' C17' H17B 120.5 . . ? C16' C17' H17B 120.5 . . ? C17' C18' H18B 119.0 . . ? C13' C18' H18B 119.0 . . ? C21' C22' H22D 109.5 . . ? C21' C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C21' C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? C24' C23' H23B 119.2 . . ? C21' C23' H23B 119.2 . . ? C25' C24' H24B 120.2 . . ? C23' C24' H24B 120.2 . . ? C24' C25' H25B 119.3 . . ? C26' C25' H25B 119.3 . . ? C26' C27' H27D 109.5 . . ? C26' C27' H27E 109.5 . . ? H27D C27' H27E 109.5 . . ? C26' C27' H27F 109.5 . . ? H27D C27' H27F 109.5 . . ? H27E C27' H27F 109.5 . . ? C30' C31' H31D 109.5 . . ? C30' C31' H31E 109.5 . . ? H31D C31' H31E 109.5 . . ? C30' C31' H31F 109.5 . . ? H31D C31' H31F 109.5 . . ? H31E C31' H31F 109.5 . . ? C30' C32' H32B 119.4 . . ? C33' C32' H32B 119.4 . . ? C34' C33' H33B 120.7 . . ? C32' C33' H33B 120.7 . . ? C33' C34' H34B 119.0 . . ? C35' C34' H34B 119.0 . . ? C35' C36' H36D 109.5 . . ? C35' C36' H36E 109.5 . . ? H36D C36' H36E 109.5 . . ? C35' C36' H36F 109.5 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? C38' C39' H39B 120.4 . . ? C40' C39' H39B 120.4 . . ? C41' C40' H40B 119.3 . . ? C39' C40' H40B 119.3 . . ? C40' C41' H41B 120.3 . . ? C42' C41' H41B 120.3 . . ? C41' C42' H42B 120.2 . . ? C43' C42' H42B 120.2 . . ? C38' C43' H43B 119.4 . . ? C42' C43' H43B 119.4 . . ? C46' C47' H47D 109.5 . . ? C46' C47' H47E 109.5 . . ? H47D C47' H47E 109.5 . . ? C46' C47' H47F 109.5 . . ? H47D C47' H47F 109.5 . . ? H47E C47' H47F 109.5 . . ? C49' C48' H48B 119.2 . . ? C46' C48' H48B 119.2 . . ? C50' C49' H49B 120.3 . . ? C48' C49' H49B 120.3 . . ? C49' C50' H50B 119.2 . . ? C51' C50' H50B 119.2 . . ? C51' C52' H52D 109.5 . . ? C51' C52' H52E 109.5 . . ? H52D C52' H52E 109.5 . . ? C51' C52' H52F 109.5 . . ? H52D C52' H52F 109.5 . . ? H52E C52' H52F 109.5 . . ? O53' C54' H54C 108.4 . . ? C55' C54' H54C 108.4 . . ? O53' C54' H54D 108.4 . . ? C55' C54' H54D 108.4 . . ? H54C C54' H54D 107.4 . . ? C56' C55' H55C 111.9 . . ? C54' C55' H55C 111.9 . . ? C56' C55' H55D 111.9 . . ? C54' C55' H55D 111.9 . . ? H55C C55' H55D 109.6 . . ? C55' C56' H56C 111.6 . . ? C57' C56' H56C 111.6 . . ? C55' C56' H56D 111.6 . . ? C57' C56' H56D 111.6 . . ? H56C C56' H56D 109.4 . . ? O53' C57' H57C 109.0 . . ? C56' C57' H57C 109.0 . . ? O53' C57' H57D 109.0 . . ? C56' C57' H57D 109.0 . . ? H57C C57' H57D 107.8 . . ? O58' C59' H59C 110.4 . . ? C60' C59' H59C 110.4 . . ? O58' C59' H59D 110.4 . . ? C60' C59' H59D 110.4 . . ? H59C C59' H59D 108.6 . . ? C59' C60' H60C 110.9 . . ? C61' C60' H60C 110.9 . . ? C59' C60' H60D 110.9 . . ? C61' C60' H60D 110.9 . . ? H60C C60' H60D 108.9 . . ? C60' C61' H61C 110.5 . . ? C62' C61' H61C 110.5 . . ? C60' C61' H61D 110.5 . . ? C62' C61' H61D 110.5 . . ? H61C C61' H61D 108.7 . . ? O58' C62' H62C 110.5 . . ? C61' C62' H62C 110.5 . . ? O58' C62' H62D 110.5 . . ? C61' C62' H62D 110.5 . . ? H62C C62' H62D 108.7 . . ? Cl86 C84A H84A 108.8 . . ? Cl85 C84A H84A 108.8 . . ? Cl86 C84A H84B 108.8 . . ? Cl85 C84A H84B 108.8 . . ? H84A C84A H84B 107.7 . . ? #==== END OF CIF ====