# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Adrian-Mihail Stadler' _publ_contact_author_email mstadler@unistra.fr _publ_author_name 'Adrian-Mihail Stadler' # Attachment '- Cu41b4.cif' data_st1541 _database_code_depnum_ccdc_archive 'CCDC 753682' #TrackingRef '- Cu41b4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C92 H84 Cu4 N36), 16(C F3 O3 S), 2(C2 H3 N), 6(C H Cl3), 3(H2 O)' _chemical_formula_sum 'C210 H186 Cl18 Cu8 F48 N74 O51 S16' _chemical_formula_weight 7133.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 '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' S S 0.1246 0.1234 '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' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 18.406(2) _cell_length_b 41.162(5) _cell_length_c 20.075(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.58(2) _cell_angle_gamma 90.00 _cell_volume 14498.6(32) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 42351 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 30.04 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7196 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9093 _exptl_absorpt_correction_T_max 0.9093 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42355 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0941 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 57 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 30.04 _reflns_number_total 42351 _reflns_number_gt 22234 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1514P)^2^+29.9174P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 42351 _refine_ls_number_parameters 1936 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1787 _refine_ls_R_factor_gt 0.0944 _refine_ls_wR_factor_ref 0.3015 _refine_ls_wR_factor_gt 0.2481 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.35169(4) 0.365826(14) 0.02831(3) 0.03050(15) Uani 1 1 d . . . Cu2 Cu 0.26022(4) 0.377331(14) 0.31888(3) 0.03158(15) Uani 1 1 d . . . Cu3 Cu 0.62341(4) 0.367054(14) 0.48041(3) 0.03029(15) Uani 1 1 d . . . Cu4 Cu 0.71765(4) 0.380975(14) 0.19330(3) 0.03159(15) Uani 1 1 d . . . N1 N 0.3809(3) 0.34823(10) -0.0679(2) 0.0385(11) Uani 1 1 d . . . C1 C 0.3888(4) 0.36540(15) -0.1224(3) 0.0506(15) Uani 1 1 d . . . H1 H 0.3923 0.3884 -0.1189 0.061 Uiso 1 1 calc R . . C2 C 0.3919(5) 0.35070(17) -0.1832(3) 0.062(2) Uani 1 1 d . . . H2 H 0.3970 0.3635 -0.2210 0.075 Uiso 1 1 calc R . . C3 C 0.3877(5) 0.31735(18) -0.1887(4) 0.063(2) Uani 1 1 d . . . H3 H 0.3906 0.3069 -0.2300 0.076 Uiso 1 1 calc R . . C4 C 0.3792(4) 0.29919(16) -0.1334(3) 0.0518(16) Uani 1 1 d . . . H4 H 0.3757 0.2762 -0.1359 0.062 Uiso 1 1 calc R . . C5 C 0.3760(3) 0.31592(13) -0.0739(3) 0.0379(12) Uani 1 1 d . . . C6 C 0.3646(3) 0.29810(12) -0.0144(3) 0.0340(11) Uani 1 1 d . . . H6 H 0.3632 0.2750 -0.0138 0.041 Uiso 1 1 calc R . . N2 N 0.3566(2) 0.31488(10) 0.0366(2) 0.0293(9) Uani 1 1 d . . . N3 N 0.3414(2) 0.29931(9) 0.0912(2) 0.0289(9) Uani 1 1 d . . . C7 C 0.3359(3) 0.26366(11) 0.0931(3) 0.0350(12) Uani 1 1 d . . . H7A H 0.3292 0.2569 0.1377 0.052 Uiso 1 1 calc R . . H7B H 0.3826 0.2540 0.0881 0.052 Uiso 1 1 calc R . . H7C H 0.2921 0.2563 0.0546 0.052 Uiso 1 1 calc R . . C8 C 0.3254(3) 0.31842(11) 0.1407(3) 0.0271(10) Uani 1 1 d . . . N4 N 0.3294(2) 0.35088(9) 0.1329(2) 0.0298(9) Uani 1 1 d . . . C9 C 0.3089(3) 0.36827(11) 0.1804(3) 0.0292(10) Uani 1 1 d . . . C10 C 0.3057(4) 0.40421(12) 0.1716(3) 0.0397(13) Uani 1 1 d . . . C11 C 0.3716(5) 0.42283(15) 0.1995(4) 0.061(2) Uani 1 1 d . . . H11 H 0.4185 0.4129 0.2243 0.073 Uiso 1 1 calc R . . C12 C 0.3663(8) 0.4568(2) 0.1900(5) 0.061(2) Uani 1 1 d . . . H12 H 0.4100 0.4700 0.2086 0.073 Uiso 1 1 calc R . . C13 C 0.2972(9) 0.4709(2) 0.1536(6) 0.061(2) Uani 1 1 d . . . H13 H 0.2937 0.4938 0.1476 0.073 Uiso 1 1 calc R . . C14 C 0.2374(8) 0.4528(2) 0.1276(5) 0.061(2) Uani 1 1 d . . . H14 H 0.1909 0.4631 0.1025 0.073 Uiso 1 1 calc R . . C15 C 0.2382(5) 0.41811(16) 0.1351(3) 0.061(2) Uani 1 1 d . . . H15 H 0.1938 0.4054 0.1154 0.073 Uiso 1 1 calc R . . N5 N 0.2892(2) 0.35591(9) 0.2339(2) 0.0290(9) Uani 1 1 d . . . C16 C 0.2882(3) 0.32301(11) 0.2357(2) 0.0278(10) Uani 1 1 d . . . N6 N 0.3076(2) 0.30360(9) 0.1918(2) 0.0274(8) Uani 1 1 d . . . N7 N 0.2651(2) 0.30906(9) 0.2878(2) 0.0290(9) Uani 1 1 d . . . C17 C 0.2532(3) 0.27415(11) 0.2932(3) 0.0354(12) Uani 1 1 d . . . H17A H 0.2740 0.2674 0.3421 0.053 Uiso 1 1 calc R . . H17B H 0.2790 0.2623 0.2646 0.053 Uiso 1 1 calc R . . H17C H 0.1985 0.2694 0.2767 0.053 Uiso 1 1 calc R . . N8 N 0.2451(2) 0.33054(10) 0.3303(2) 0.0306(9) Uani 1 1 d . . . C18 C 0.2150(3) 0.32195(12) 0.3778(3) 0.0317(11) Uani 1 1 d . . . H18 H 0.2037 0.2999 0.3845 0.038 Uiso 1 1 calc R . . C19 C 0.1993(3) 0.34795(12) 0.4207(3) 0.0309(10) Uani 1 1 d . . . C20 C 0.1632(3) 0.34255(14) 0.4706(3) 0.0384(12) Uani 1 1 d . . . H20 H 0.1478 0.3213 0.4789 0.046 Uiso 1 1 calc R . . C21 C 0.1498(4) 0.36906(15) 0.5087(3) 0.0462(14) Uani 1 1 d . . . H21 H 0.1241 0.3664 0.5429 0.055 Uiso 1 1 calc R . . C22 C 0.1751(4) 0.39934(15) 0.4950(3) 0.0479(15) Uani 1 1 d . . . H22 H 0.1670 0.4178 0.5204 0.057 Uiso 1 1 calc R . . C23 C 0.2118(3) 0.40298(13) 0.4453(3) 0.0421(13) Uani 1 1 d . . . H23 H 0.2294 0.4239 0.4376 0.050 Uiso 1 1 calc R . . N9 N 0.2233(3) 0.37814(10) 0.4077(2) 0.0352(10) Uani 1 1 d . . . N10 N 0.2373(3) 0.36469(10) -0.0251(2) 0.0366(10) Uani 1 1 d . . . C24 C 0.1899(3) 0.33946(14) -0.0394(3) 0.0422(13) Uani 1 1 d . . . H24 H 0.2080 0.3188 -0.0203 0.051 Uiso 1 1 calc R . . C25 C 0.1161(4) 0.34218(15) -0.0807(4) 0.0528(16) Uani 1 1 d . . . H25 H 0.0838 0.3237 -0.0902 0.063 Uiso 1 1 calc R . . C26 C 0.0887(4) 0.37207(17) -0.1087(4) 0.063(2) Uani 1 1 d . . . H26 H 0.0377 0.3743 -0.1380 0.076 Uiso 1 1 calc R . . C27 C 0.1365(4) 0.39858(16) -0.0934(4) 0.0590(19) Uani 1 1 d . . . H27 H 0.1191 0.4194 -0.1115 0.071 Uiso 1 1 calc R . . C28 C 0.2102(3) 0.39412(13) -0.0511(3) 0.0412(13) Uani 1 1 d . . . C29 C 0.2647(4) 0.42054(13) -0.0313(3) 0.0431(14) Uani 1 1 d . . . H29 H 0.2519 0.4423 -0.0460 0.052 Uiso 1 1 calc R . . N11 N 0.3313(2) 0.41251(10) 0.0072(2) 0.0324(9) Uani 1 1 d . . . N12 N 0.3882(3) 0.43432(10) 0.0334(2) 0.0337(10) Uani 1 1 d . . . C30 C 0.3787(4) 0.46887(12) 0.0151(3) 0.0438(14) Uani 1 1 d . . . H30A H 0.3781 0.4718 -0.0335 0.066 Uiso 1 1 calc R . . H30B H 0.4211 0.4812 0.0459 0.066 Uiso 1 1 calc R . . H30C H 0.3305 0.4767 0.0205 0.066 Uiso 1 1 calc R . . C31 C 0.4559(3) 0.42101(11) 0.0703(3) 0.0302(10) Uani 1 1 d . . . N13 N 0.4579(2) 0.38780(9) 0.0751(2) 0.0302(9) Uani 1 1 d . . . C32 C 0.5271(3) 0.37579(11) 0.1070(3) 0.0288(10) Uani 1 1 d . . . C33 C 0.5347(3) 0.33987(11) 0.1106(3) 0.0289(10) Uani 1 1 d . . . C34 C 0.5526(3) 0.32324(13) 0.0577(3) 0.0392(12) Uani 1 1 d . . . H34 H 0.5646 0.3348 0.0214 0.047 Uiso 1 1 calc R . . C35 C 0.5530(4) 0.28947(14) 0.0581(4) 0.0480(15) Uani 1 1 d . . . H35 H 0.5643 0.2779 0.0214 0.058 Uiso 1 1 calc R . . C36 C 0.5370(3) 0.27272(13) 0.1114(3) 0.0427(14) Uani 1 1 d . . . H36 H 0.5365 0.2496 0.1109 0.051 Uiso 1 1 calc R . . C37 C 0.5218(4) 0.28917(13) 0.1655(3) 0.0447(14) Uani 1 1 d . . . H37 H 0.5122 0.2775 0.2027 0.054 Uiso 1 1 calc R . . C38 C 0.5204(3) 0.32300(12) 0.1654(3) 0.0362(12) Uani 1 1 d . . . H38 H 0.5099 0.3345 0.2026 0.043 Uiso 1 1 calc R . . N14 N 0.5899(2) 0.39346(9) 0.1361(2) 0.0305(9) Uani 1 1 d . . . C39 C 0.5795(3) 0.42603(11) 0.1310(3) 0.0313(11) Uani 1 1 d . . . N15 N 0.5134(2) 0.44065(9) 0.0987(2) 0.0321(9) Uani 1 1 d . . . N16 N 0.6399(3) 0.44558(10) 0.1609(2) 0.0347(10) Uani 1 1 d . . . C40 C 0.6373(4) 0.48100(12) 0.1548(4) 0.0470(15) Uani 1 1 d . . . H40A H 0.5855 0.4878 0.1287 0.070 Uiso 1 1 calc R . . H40B H 0.6729 0.4882 0.1301 0.070 Uiso 1 1 calc R . . H40C H 0.6516 0.4907 0.2016 0.070 Uiso 1 1 calc R . . N17 N 0.7061(2) 0.43053(10) 0.1982(2) 0.0321(9) Uani 1 1 d . . . C41 C 0.7650(3) 0.44730(12) 0.2309(3) 0.0347(11) Uani 1 1 d . . . H41 H 0.7638 0.4704 0.2295 0.042 Uiso 1 1 calc R . . C42 C 0.8343(3) 0.42993(13) 0.2702(3) 0.0364(12) Uani 1 1 d . . . C43 C 0.8973(4) 0.44627(15) 0.3099(4) 0.0537(17) Uani 1 1 d . . . H43 H 0.8985 0.4693 0.3112 0.064 Uiso 1 1 calc R . . C44 C 0.9595(4) 0.42807(16) 0.3483(4) 0.061(2) Uani 1 1 d . . . H44 H 1.0040 0.4387 0.3766 0.074 Uiso 1 1 calc R . . C45 C 0.9566(4) 0.39497(16) 0.3450(4) 0.0581(18) Uani 1 1 d . . . H45 H 0.9987 0.3823 0.3712 0.070 Uiso 1 1 calc R . . C46 C 0.8907(3) 0.37999(14) 0.3027(3) 0.0424(13) Uani 1 1 d . . . H46 H 0.8888 0.3570 0.3000 0.051 Uiso 1 1 calc R . . N18 N 0.8305(3) 0.39711(10) 0.2661(2) 0.0361(10) Uani 1 1 d . . . N19 N 0.1429(3) 0.39042(10) 0.2519(2) 0.0367(10) Uani 1 1 d . . . C47 C 0.0827(4) 0.37235(13) 0.2193(3) 0.0449(14) Uani 1 1 d . . . H47 H 0.0889 0.3494 0.2190 0.054 Uiso 1 1 calc R . . C48 C 0.0118(4) 0.38518(15) 0.1860(4) 0.0560(18) Uani 1 1 d . . . H48 H -0.0299 0.3714 0.1640 0.067 Uiso 1 1 calc R . . C49 C 0.0026(4) 0.41844(16) 0.1852(4) 0.0604(19) Uani 1 1 d . . . H49 H -0.0454 0.4280 0.1622 0.072 Uiso 1 1 calc R . . C50 C 0.0643(4) 0.43758(15) 0.2184(4) 0.0534(17) Uani 1 1 d . . . H50 H 0.0592 0.4605 0.2189 0.064 Uiso 1 1 calc R . . C51 C 0.1334(3) 0.42306(12) 0.2511(3) 0.0380(12) Uani 1 1 d . . . C52 C 0.2008(3) 0.44183(12) 0.2853(3) 0.0367(12) Uani 1 1 d . . . H52 H 0.1989 0.4649 0.2866 0.044 Uiso 1 1 calc R . . N20 N 0.2636(3) 0.42633(10) 0.3140(2) 0.0321(9) Uani 1 1 d . . . N21 N 0.3296(2) 0.44308(10) 0.3477(2) 0.0318(9) Uani 1 1 d . . . C53 C 0.3303(3) 0.47836(12) 0.3525(3) 0.0412(13) Uani 1 1 d . . . H53A H 0.3811 0.4857 0.3799 0.062 Uiso 1 1 calc R . . H53B H 0.2928 0.4854 0.3753 0.062 Uiso 1 1 calc R . . H53C H 0.3173 0.4877 0.3054 0.062 Uiso 1 1 calc R . . C54 C 0.3930(3) 0.42461(12) 0.3762(3) 0.0316(11) Uani 1 1 d . . . N22 N 0.3849(2) 0.39193(9) 0.3702(2) 0.0293(9) Uani 1 1 d . . . C55 C 0.4483(3) 0.37499(10) 0.3974(2) 0.0263(10) Uani 1 1 d . . . C56 C 0.4427(3) 0.33912(11) 0.3945(3) 0.0287(10) Uani 1 1 d . . . C57 C 0.6852(6) 0.47236(17) 0.3666(5) 0.078(3) Uani 1 1 d . . . H57 H 0.6901 0.4951 0.3753 0.093 Uiso 1 1 calc R . . C58 C 0.6176(6) 0.46010(17) 0.3252(5) 0.071(2) Uani 1 1 d . . . H58 H 0.5760 0.4743 0.3058 0.086 Uiso 1 1 calc R . . C59 C 0.6091(4) 0.42662(14) 0.3110(4) 0.0511(16) Uani 1 1 d . . . H59 H 0.5622 0.4179 0.2824 0.061 Uiso 1 1 calc R . . C60 C 0.6717(3) 0.40656(12) 0.3404(3) 0.0361(12) Uani 1 1 d . . . C61 C 0.7400(4) 0.42009(14) 0.3824(3) 0.0472(15) Uani 1 1 d . . . H61 H 0.7830 0.4066 0.4023 0.057 Uiso 1 1 calc R . . C62 C 0.7444(5) 0.45292(16) 0.3949(4) 0.064(2) Uani 1 1 d . . . H62 H 0.7905 0.4619 0.4242 0.077 Uiso 1 1 calc R . . N23 N 0.5168(2) 0.38795(9) 0.4296(2) 0.0290(9) Uani 1 1 d . . . C63 C 0.5166(3) 0.42091(11) 0.4361(3) 0.0296(10) Uani 1 1 d . . . N24 N 0.4571(3) 0.43993(10) 0.4084(2) 0.0331(9) Uani 1 1 d . . . N25 N 0.5824(2) 0.43505(9) 0.4739(2) 0.0336(10) Uani 1 1 d . . . C64 C 0.5901(4) 0.46953(12) 0.4929(3) 0.0446(14) Uani 1 1 d . . . H64A H 0.5478 0.4817 0.4613 0.067 Uiso 1 1 calc R . . H64B H 0.6385 0.4778 0.4889 0.067 Uiso 1 1 calc R . . H64C H 0.5890 0.4721 0.5411 0.067 Uiso 1 1 calc R . . N26 N 0.6407(2) 0.41358(10) 0.5014(2) 0.0327(9) Uani 1 1 d . . . C65 C 0.7058(3) 0.42263(12) 0.5410(3) 0.0354(12) Uani 1 1 d . . . H65 H 0.7170 0.4445 0.5552 0.043 Uiso 1 1 calc R . . C66 C 0.7613(3) 0.39653(13) 0.5625(3) 0.0363(12) Uani 1 1 d . . . C67 C 0.8348(3) 0.40196(14) 0.6039(3) 0.0486(15) Uani 1 1 d . . . H67 H 0.8511 0.4232 0.6200 0.058 Uiso 1 1 calc R . . C68 C 0.8855(4) 0.37557(16) 0.6221(4) 0.0527(16) Uani 1 1 d . . . H68 H 0.9362 0.3784 0.6518 0.063 Uiso 1 1 calc R . . C69 C 0.8594(4) 0.34557(15) 0.5956(3) 0.0484(15) Uani 1 1 d . . . H69 H 0.8925 0.3273 0.6065 0.058 Uiso 1 1 calc R . . C70 C 0.7861(3) 0.34182(13) 0.5535(3) 0.0396(13) Uani 1 1 d . . . H70 H 0.7694 0.3208 0.5357 0.048 Uiso 1 1 calc R . . N27 N 0.7369(3) 0.36663(10) 0.5365(2) 0.0330(9) Uani 1 1 d . . . N28 N 0.5866(3) 0.35009(11) 0.5717(2) 0.0375(10) Uani 1 1 d . . . C71 C 0.5701(4) 0.36732(15) 0.6231(3) 0.0449(14) Uani 1 1 d . . . H71 H 0.5702 0.3904 0.6211 0.054 Uiso 1 1 calc R . . C72 C 0.5531(4) 0.35227(18) 0.6780(3) 0.0527(16) Uani 1 1 d . . . H72 H 0.5427 0.3649 0.7137 0.063 Uiso 1 1 calc R . . C73 C 0.5514(4) 0.31877(17) 0.6809(3) 0.0504(16) Uani 1 1 d . . . H73 H 0.5394 0.3082 0.7183 0.061 Uiso 1 1 calc R . . C74 C 0.5673(3) 0.30084(14) 0.6294(3) 0.0412(13) Uani 1 1 d . . . H74 H 0.5664 0.2778 0.6306 0.049 Uiso 1 1 calc R . . C75 C 0.5847(3) 0.31720(12) 0.5750(3) 0.0340(11) Uani 1 1 d . . . C76 C 0.6032(3) 0.29984(12) 0.5198(3) 0.0351(12) Uani 1 1 d . . . H76 H 0.6042 0.2768 0.5193 0.042 Uiso 1 1 calc R . . N29 N 0.6185(2) 0.31653(10) 0.4710(2) 0.0299(9) Uani 1 1 d . . . N30 N 0.6397(3) 0.30111(9) 0.4189(2) 0.0305(9) Uani 1 1 d . . . C77 C 0.6476(3) 0.26573(11) 0.4192(3) 0.0375(12) Uani 1 1 d . . . H77A H 0.6575 0.2587 0.3761 0.056 Uiso 1 1 calc R . . H77B H 0.6004 0.2556 0.4222 0.056 Uiso 1 1 calc R . . H77C H 0.6901 0.2591 0.4596 0.056 Uiso 1 1 calc R . . C78 C 0.6545(3) 0.32047(11) 0.3697(3) 0.0273(10) Uani 1 1 d . . . N31 N 0.6502(2) 0.35290(9) 0.3787(2) 0.0299(9) Uani 1 1 d . . . C79 C 0.6686(3) 0.37078(11) 0.3302(3) 0.0280(10) Uani 1 1 d . . . C80 C 0.4348(3) 0.27187(13) 0.3951(4) 0.0482(16) Uani 1 1 d . . . H80 H 0.4320 0.2488 0.3952 0.058 Uiso 1 1 calc R . . C81 C 0.4156(3) 0.28959(14) 0.4455(3) 0.0441(14) Uani 1 1 d . . . H81 H 0.4002 0.2786 0.4806 0.053 Uiso 1 1 calc R . . C82 C 0.4184(3) 0.32290(13) 0.4455(3) 0.0363(12) Uani 1 1 d . . . H82 H 0.4040 0.3349 0.4799 0.044 Uiso 1 1 calc R . . C83 C 0.4580(3) 0.28758(13) 0.3444(3) 0.0422(14) Uani 1 1 d . . . H83 H 0.4709 0.2753 0.3096 0.051 Uiso 1 1 calc R . . C84 C 0.4626(3) 0.32125(12) 0.3438(3) 0.0345(11) Uani 1 1 d . . . H84 H 0.4791 0.3320 0.3091 0.041 Uiso 1 1 calc R . . N32 N 0.6885(2) 0.35887(9) 0.2762(2) 0.0284(9) Uani 1 1 d . . . C85 C 0.6927(3) 0.32571(11) 0.2746(3) 0.0281(10) Uani 1 1 d . . . N33 N 0.6741(2) 0.30573(9) 0.3184(2) 0.0286(9) Uani 1 1 d . . . N34 N 0.7178(3) 0.31268(9) 0.2239(2) 0.0314(9) Uani 1 1 d . . . C86 C 0.7311(3) 0.27795(12) 0.2156(3) 0.0365(12) Uani 1 1 d . . . H86A H 0.7859 0.2740 0.2263 0.055 Uiso 1 1 calc R . . H86B H 0.7051 0.2713 0.1674 0.055 Uiso 1 1 calc R . . H86C H 0.7112 0.2653 0.2477 0.055 Uiso 1 1 calc R . . N35 N 0.7349(2) 0.33505(10) 0.1800(2) 0.0307(9) Uani 1 1 d . . . C87 C 0.7649(3) 0.32697(13) 0.1324(3) 0.0368(12) Uani 1 1 d . . . H87 H 0.7778 0.3052 0.1254 0.044 Uiso 1 1 calc R . . C88 C 0.7776(3) 0.35360(13) 0.0900(3) 0.0377(12) Uani 1 1 d . . . C89 C 0.8091(4) 0.34954(16) 0.0365(3) 0.0466(14) Uani 1 1 d . . . H89 H 0.8238 0.3285 0.0257 0.056 Uiso 1 1 calc R . . C90 C 0.8190(4) 0.37611(18) -0.0014(3) 0.0579(18) Uani 1 1 d . . . H90 H 0.8419 0.3737 -0.0376 0.069 Uiso 1 1 calc R . . C91 C 0.7952(5) 0.40635(17) 0.0140(4) 0.0614(19) Uani 1 1 d . . . H91 H 0.8009 0.4250 -0.0119 0.074 Uiso 1 1 calc R . . C92 C 0.7630(4) 0.40890(15) 0.0681(3) 0.0502(15) Uani 1 1 d . . . H92 H 0.7466 0.4296 0.0786 0.060 Uiso 1 1 calc R . . N36 N 0.7541(3) 0.38330(11) 0.1061(2) 0.0396(11) Uani 1 1 d . . . S1 S 0.11515(8) 0.29901(3) 0.10031(8) 0.0409(3) Uani 1 1 d . . . O1 O 0.1457(3) 0.33078(11) 0.1007(3) 0.0562(12) Uani 1 1 d . . . O2 O 0.1434(3) 0.27630(12) 0.0601(3) 0.0727(16) Uani 1 1 d . . . O3 O 0.1112(3) 0.28824(15) 0.1665(3) 0.0728(15) Uani 1 1 d . . . C93 C 0.0150(4) 0.30281(18) 0.0509(4) 0.0565(17) Uani 1 1 d . . . F1 F -0.0218(3) 0.27524(12) 0.0495(3) 0.0922(16) Uani 1 1 d . . . F2 F 0.0043(3) 0.3100(2) -0.0146(3) 0.133(3) Uani 1 1 d . . . F3 F -0.0193(3) 0.32486(15) 0.0769(4) 0.115(2) Uani 1 1 d . . . S2 S 0.41084(10) 0.43278(4) 0.56013(9) 0.0503(4) Uani 1 1 d . . . O4 O 0.3564(3) 0.45520(12) 0.5191(3) 0.0686(14) Uani 1 1 d . . . O5 O 0.4079(3) 0.40053(11) 0.5302(3) 0.0647(13) Uani 1 1 d . . . O6 O 0.4850(3) 0.44515(14) 0.5880(3) 0.0767(16) Uani 1 1 d . . . C94 C 0.3801(4) 0.42542(17) 0.6376(4) 0.0550(17) Uani 1 1 d . . . F4 F 0.3104(3) 0.41432(13) 0.6218(3) 0.0814(13) Uani 1 1 d . . . F5 F 0.3839(3) 0.45254(11) 0.6745(2) 0.0869(15) Uani 1 1 d . . . F6 F 0.4252(3) 0.40418(11) 0.6799(2) 0.0764(13) Uani 1 1 d . . . S3 S 0.86066(8) 0.30071(3) 0.41695(8) 0.0378(3) Uani 1 1 d . . . O7 O 0.8307(2) 0.33302(10) 0.4073(3) 0.0521(11) Uani 1 1 d . . . O8 O 0.8603(3) 0.28366(14) 0.3551(3) 0.0668(14) Uani 1 1 d . . . O9 O 0.8371(3) 0.28211(10) 0.4671(3) 0.0558(12) Uani 1 1 d . . . C95 C 0.9619(4) 0.30700(18) 0.4586(4) 0.0539(16) Uani 1 1 d . . . F7 F 0.9933(2) 0.32265(11) 0.4163(3) 0.0760(13) Uani 1 1 d . . . F8 F 0.9767(3) 0.32403(17) 0.5168(3) 0.112(2) Uani 1 1 d . . . F9 F 0.9990(3) 0.27850(13) 0.4730(3) 0.0902(16) Uani 1 1 d . . . S4 S 0.00817(9) 0.30152(3) 0.75114(8) 0.0462(4) Uani 1 1 d . . . O10 O -0.0176(2) 0.33359(10) 0.7595(2) 0.0501(11) Uani 1 1 d . . . O11 O -0.0370(3) 0.28443(11) 0.6905(3) 0.0709(16) Uani 1 1 d . . . O12 O 0.0321(3) 0.28285(12) 0.8142(3) 0.0711(15) Uani 1 1 d . . . C96 C 0.0964(5) 0.30937(18) 0.7321(5) 0.065(2) Uani 1 1 d . . . F10 F 0.1461(2) 0.32644(11) 0.7798(3) 0.0779(13) Uani 1 1 d . . . F11 F 0.0848(4) 0.32642(15) 0.6725(3) 0.1037(18) Uani 1 1 d . . . F12 F 0.1301(3) 0.28195(12) 0.7239(4) 0.109(2) Uani 1 1 d . . . S5 S 0.20535(10) 0.23216(4) 0.45750(8) 0.0467(4) Uani 1 1 d . . . O13 O 0.2788(3) 0.23331(14) 0.4478(3) 0.0713(15) Uani 1 1 d . . . O14 O 0.2041(3) 0.21753(12) 0.5222(2) 0.0590(12) Uani 1 1 d . . . O15 O 0.1611(3) 0.26156(11) 0.4394(3) 0.0688(15) Uani 1 1 d . . . C97 C 0.1531(4) 0.20362(16) 0.3906(4) 0.0552(17) Uani 1 1 d . . . F13 F 0.1516(3) 0.21403(11) 0.3274(2) 0.0739(12) Uani 1 1 d . . . F14 F 0.0803(3) 0.20137(12) 0.3909(3) 0.0851(14) Uani 1 1 d . . . F15 F 0.1821(3) 0.17441(10) 0.4005(3) 0.0881(15) Uani 1 1 d . . . S6 S 0.14207(10) 0.49438(4) 0.43350(11) 0.0571(5) Uani 1 1 d . . . O16 O 0.1243(3) 0.46824(11) 0.3845(3) 0.0654(14) Uani 1 1 d . . . O17 O 0.1944(3) 0.51705(12) 0.4218(4) 0.0848(19) Uani 1 1 d . . . O18 O 0.1577(4) 0.48409(16) 0.5063(3) 0.0901(19) Uani 1 1 d . . . C98 C 0.0556(5) 0.5169(2) 0.4188(5) 0.071(2) Uani 1 1 d . . . F16 F 0.0633(3) 0.54184(12) 0.4625(3) 0.1027(19) Uani 1 1 d . . . F17 F 0.0329(4) 0.52924(18) 0.3539(4) 0.127(2) Uani 1 1 d . . . F18 F -0.0017(3) 0.49904(12) 0.4247(3) 0.0836(14) Uani 1 1 d . . . S7 S 0.04524(17) 0.05611(6) 0.42353(16) 0.0907(8) Uani 1 1 d . . . O19 O 0.0396(5) 0.03094(17) 0.3644(4) 0.112(2) Uani 1 1 d . . . O20 O 0.1044(4) 0.04750(14) 0.4891(3) 0.0796(17) Uani 1 1 d . . . O21 O -0.0302(5) 0.06384(19) 0.4229(4) 0.120(3) Uani 1 1 d . . . C99 C 0.0823(9) 0.0904(3) 0.3899(8) 0.126(4) Uani 1 1 d . . . F19 F 0.1485(4) 0.0843(2) 0.3822(5) 0.145(3) Uani 1 1 d . . . F20 F 0.0887(7) 0.1132(2) 0.4418(6) 0.227(6) Uani 1 1 d . . . F21 F 0.0322(4) 0.09898(19) 0.3292(3) 0.131(3) Uani 1 1 d . . . S8 S 0.36080(13) 0.00108(4) 0.61504(14) 0.0724(6) Uani 1 1 d . . . O22 O 0.3631(3) 0.03145(13) 0.6435(3) 0.0791(17) Uani 1 1 d . . . O23 O 0.2893(5) -0.0039(4) 0.5659(12) 0.0791(17) Uani 1 1 d . . . O24 O 0.3756(11) -0.0262(2) 0.6502(7) 0.0791(17) Uani 1 1 d . . . C100 C 0.4169(8) 0.0016(3) 0.5598(6) 0.103(4) Uani 1 1 d . . . F22 F 0.4045(11) 0.0253(3) 0.5175(7) 0.300(10) Uani 1 1 d . . . F23 F 0.4196(5) -0.02590(17) 0.5282(4) 0.135(3) Uani 1 1 d . . . F24 F 0.4885(5) 0.0090(3) 0.5913(7) 0.193(5) Uani 1 1 d . . . C101 C 0.6831(6) 0.0598(2) 0.2388(5) 0.081(3) Uani 1 1 d . . . H101 H 0.6520 0.0491 0.2657 0.097 Uiso 1 1 calc R . . Cl1 Cl 0.67568(15) 0.03705(6) 0.16303(14) 0.0899(7) Uani 1 1 d . . . Cl2 Cl 0.6486(3) 0.09876(8) 0.2163(2) 0.174(2) Uani 1 1 d . . . Cl3 Cl 0.7785(2) 0.06122(7) 0.29111(15) 0.1079(9) Uani 1 1 d . . . C102 C 0.8048(4) 0.20492(16) 0.0928(4) 0.0538(16) Uani 1 1 d . . . H102 H 0.7817 0.2105 0.0423 0.065 Uiso 1 1 calc R . . Cl4 Cl 0.87010(11) 0.23563(5) 0.13190(11) 0.0665(5) Uani 1 1 d . . . Cl5 Cl 0.73161(12) 0.20320(5) 0.13144(12) 0.0721(5) Uani 1 1 d . . . Cl6 Cl 0.84935(11) 0.16727(4) 0.09770(10) 0.0619(4) Uani 1 1 d . . . C103 C 0.3156(5) 0.1688(2) 0.2615(5) 0.085(3) Uani 1 1 d . . . H103 H 0.3637 0.1641 0.2498 0.102 Uiso 1 1 calc R . . Cl7 Cl 0.26089(19) 0.13355(8) 0.2483(3) 0.1477(15) Uani 1 1 d . . . Cl8 Cl 0.26341(16) 0.19893(7) 0.20216(16) 0.1079(9) Uani 1 1 d . . . Cl9 Cl 0.33971(19) 0.18336(8) 0.34591(15) 0.1108(10) Uani 1 1 d . . . C104 C 0.5137(5) 0.2301(2) 0.7876(5) 0.076(2) Uani 1 1 d . . . H10A H 0.5415 0.2407 0.7590 0.113 Uiso 1 1 calc R . . H10B H 0.5502 0.2205 0.8291 0.113 Uiso 1 1 calc R . . H10C H 0.4823 0.2462 0.8021 0.113 Uiso 1 1 calc R . . C105 C 0.4657(4) 0.20497(18) 0.7476(4) 0.0547(17) Uani 1 1 d . . . N40 N 0.4275(4) 0.18574(17) 0.7144(4) 0.0747(19) Uani 1 1 d . . . O25 O 0.0568(7) 0.0236(3) 0.2249(5) 0.093(5) Uani 0.50 1 d P . . O26 O 0.1812(7) 0.0604(2) 0.1878(7) 0.092(4) Uani 0.50 1 d P . . O27 O 0.3425(10) 0.0311(3) 0.2461(6) 0.103(5) Uani 0.50 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 0.0339(3) 0.0245(3) 0.0308(3) 0.0022(2) 0.0064(3) 0.0015(2) Cu2 0.0351(4) 0.0295(3) 0.0296(3) 0.0009(2) 0.0090(3) 0.0041(2) Cu3 0.0318(3) 0.0245(3) 0.0324(3) -0.0011(2) 0.0066(3) -0.0038(2) Cu4 0.0360(4) 0.0263(3) 0.0327(3) -0.0020(2) 0.0108(3) -0.0036(2) N1 0.052(3) 0.029(2) 0.034(2) 0.0027(18) 0.012(2) -0.0024(19) C1 0.065(4) 0.042(3) 0.048(4) 0.008(3) 0.023(3) 0.002(3) C2 0.096(6) 0.059(4) 0.038(3) 0.011(3) 0.030(4) 0.004(4) C3 0.096(6) 0.065(4) 0.040(4) -0.009(3) 0.037(4) -0.004(4) C4 0.075(5) 0.047(3) 0.038(3) -0.007(3) 0.024(3) -0.002(3) C5 0.047(3) 0.037(3) 0.035(3) -0.003(2) 0.019(3) 0.001(2) C6 0.045(3) 0.027(2) 0.033(3) -0.002(2) 0.016(2) 0.000(2) N2 0.032(2) 0.028(2) 0.028(2) 0.0005(16) 0.0104(18) 0.0036(16) N3 0.038(2) 0.0215(18) 0.030(2) -0.0003(16) 0.0146(18) 0.0021(16) C7 0.044(3) 0.023(2) 0.040(3) -0.002(2) 0.016(2) 0.002(2) C8 0.027(2) 0.022(2) 0.029(2) -0.0017(18) 0.004(2) 0.0019(17) N4 0.033(2) 0.0233(19) 0.032(2) 0.0014(16) 0.0080(18) 0.0017(16) C9 0.030(3) 0.024(2) 0.030(2) 0.0001(19) 0.004(2) 0.0014(18) C10 0.070(4) 0.020(2) 0.033(3) 0.002(2) 0.022(3) 0.001(2) C11 0.102(6) 0.035(3) 0.055(4) -0.010(3) 0.038(4) -0.019(3) C12 0.091(6) 0.048(4) 0.043(4) 0.012(3) 0.020(4) 0.033(4) C13 0.091(6) 0.048(4) 0.043(4) 0.012(3) 0.020(4) 0.033(4) C14 0.091(6) 0.048(4) 0.043(4) 0.012(3) 0.020(4) 0.033(4) C15 0.091(6) 0.048(4) 0.043(4) 0.012(3) 0.020(4) 0.033(4) N5 0.036(2) 0.0218(18) 0.027(2) -0.0008(16) 0.0064(18) -0.0005(16) C16 0.032(3) 0.024(2) 0.026(2) -0.0004(18) 0.006(2) 0.0005(18) N6 0.033(2) 0.0229(18) 0.026(2) -0.0001(15) 0.0099(17) -0.0008(15) N7 0.038(2) 0.0216(18) 0.029(2) 0.0011(16) 0.0117(18) -0.0004(16) C17 0.048(3) 0.025(2) 0.037(3) 0.003(2) 0.017(2) -0.002(2) N8 0.028(2) 0.032(2) 0.030(2) -0.0010(17) 0.0063(18) 0.0039(16) C18 0.032(3) 0.033(3) 0.029(3) 0.000(2) 0.007(2) -0.003(2) C19 0.030(3) 0.034(3) 0.028(2) 0.002(2) 0.009(2) 0.0020(19) C20 0.040(3) 0.042(3) 0.035(3) 0.002(2) 0.014(2) 0.002(2) C21 0.042(3) 0.056(4) 0.045(3) -0.001(3) 0.020(3) 0.002(3) C22 0.057(4) 0.041(3) 0.047(3) -0.006(3) 0.018(3) 0.008(3) C23 0.048(3) 0.033(3) 0.045(3) 0.000(2) 0.014(3) 0.002(2) N9 0.035(2) 0.033(2) 0.037(2) 0.0027(18) 0.010(2) 0.0022(18) N10 0.041(3) 0.033(2) 0.034(2) 0.0027(18) 0.008(2) 0.0022(18) C24 0.041(3) 0.039(3) 0.044(3) 0.002(2) 0.008(3) -0.003(2) C25 0.048(4) 0.046(3) 0.056(4) -0.007(3) 0.003(3) -0.011(3) C26 0.045(4) 0.061(4) 0.066(5) -0.011(3) -0.010(3) -0.001(3) C27 0.048(4) 0.049(4) 0.060(4) -0.004(3) -0.013(3) 0.005(3) C28 0.042(3) 0.037(3) 0.037(3) -0.004(2) 0.000(2) 0.000(2) C29 0.051(4) 0.026(3) 0.043(3) 0.002(2) 0.001(3) 0.005(2) N11 0.033(2) 0.027(2) 0.035(2) 0.0025(17) 0.0074(19) 0.0016(17) N12 0.038(2) 0.024(2) 0.037(2) 0.0058(17) 0.0075(19) -0.0012(17) C30 0.047(3) 0.026(3) 0.053(4) 0.011(2) 0.006(3) 0.004(2) C31 0.038(3) 0.022(2) 0.030(2) 0.0014(18) 0.010(2) 0.0011(19) N13 0.031(2) 0.0240(19) 0.034(2) 0.0033(16) 0.0069(18) 0.0009(16) C32 0.036(3) 0.024(2) 0.028(2) 0.0015(18) 0.012(2) -0.0011(19) C33 0.028(2) 0.023(2) 0.033(3) 0.0041(19) 0.005(2) 0.0001(18) C34 0.048(3) 0.034(3) 0.040(3) 0.000(2) 0.020(3) 0.001(2) C35 0.049(4) 0.038(3) 0.059(4) -0.014(3) 0.020(3) 0.003(3) C36 0.040(3) 0.025(2) 0.056(4) 0.004(2) 0.005(3) 0.003(2) C37 0.051(4) 0.033(3) 0.049(3) 0.010(2) 0.013(3) 0.000(2) C38 0.043(3) 0.029(2) 0.037(3) 0.002(2) 0.011(2) -0.001(2) N14 0.031(2) 0.0250(19) 0.034(2) 0.0030(17) 0.0082(18) 0.0004(16) C39 0.039(3) 0.025(2) 0.027(2) 0.0038(19) 0.006(2) 0.000(2) N15 0.035(2) 0.0233(19) 0.036(2) 0.0016(17) 0.0074(19) -0.0033(16) N16 0.034(2) 0.024(2) 0.041(2) 0.0018(18) 0.0032(19) -0.0026(17) C40 0.050(4) 0.023(2) 0.063(4) 0.007(2) 0.010(3) -0.005(2) N17 0.034(2) 0.027(2) 0.033(2) 0.0002(17) 0.0086(19) -0.0044(17) C41 0.037(3) 0.027(2) 0.039(3) -0.003(2) 0.009(2) -0.007(2) C42 0.032(3) 0.034(3) 0.039(3) -0.002(2) 0.004(2) -0.005(2) C43 0.047(4) 0.035(3) 0.066(4) 0.003(3) -0.002(3) -0.009(3) C44 0.044(4) 0.048(4) 0.076(5) -0.003(3) -0.007(3) -0.014(3) C45 0.048(4) 0.051(4) 0.063(4) 0.006(3) -0.002(3) -0.007(3) C46 0.043(3) 0.037(3) 0.045(3) 0.002(2) 0.010(3) -0.008(2) N18 0.038(3) 0.032(2) 0.036(2) 0.0014(18) 0.009(2) -0.0052(18) N19 0.037(3) 0.031(2) 0.041(3) 0.0006(19) 0.011(2) 0.0064(18) C47 0.055(4) 0.031(3) 0.045(3) -0.010(2) 0.009(3) 0.001(2) C48 0.040(4) 0.047(3) 0.068(4) -0.010(3) -0.004(3) -0.003(3) C49 0.039(4) 0.052(4) 0.076(5) 0.000(3) -0.005(3) 0.011(3) C50 0.041(4) 0.040(3) 0.069(4) -0.001(3) 0.002(3) 0.013(3) C51 0.036(3) 0.027(2) 0.045(3) -0.001(2) 0.003(2) 0.008(2) C52 0.043(3) 0.027(2) 0.037(3) 0.002(2) 0.009(2) 0.005(2) N20 0.036(2) 0.028(2) 0.032(2) 0.0012(17) 0.0079(19) 0.0019(17) N21 0.036(2) 0.026(2) 0.032(2) -0.0041(17) 0.0073(18) 0.0044(17) C53 0.046(3) 0.024(2) 0.050(3) -0.003(2) 0.010(3) 0.001(2) C54 0.040(3) 0.027(2) 0.030(3) -0.0014(19) 0.014(2) 0.000(2) N22 0.033(2) 0.0246(19) 0.030(2) 0.0005(16) 0.0096(18) 0.0002(16) C55 0.033(3) 0.021(2) 0.025(2) -0.0003(17) 0.008(2) -0.0026(18) C56 0.030(3) 0.024(2) 0.030(2) 0.0005(18) 0.005(2) -0.0031(18) C57 0.137(9) 0.029(3) 0.090(6) -0.012(4) 0.069(6) -0.018(4) C58 0.110(7) 0.040(4) 0.086(6) 0.021(4) 0.062(5) 0.028(4) C59 0.062(4) 0.037(3) 0.062(4) 0.011(3) 0.031(3) 0.012(3) C60 0.054(3) 0.024(2) 0.036(3) -0.003(2) 0.022(3) -0.002(2) C61 0.066(4) 0.036(3) 0.044(3) -0.009(2) 0.023(3) -0.018(3) C62 0.101(6) 0.039(3) 0.059(4) -0.014(3) 0.035(4) -0.032(4) N23 0.034(2) 0.0233(18) 0.031(2) -0.0030(16) 0.0114(18) -0.0020(16) C63 0.035(3) 0.023(2) 0.031(3) -0.0009(19) 0.011(2) -0.0019(19) N24 0.037(2) 0.025(2) 0.036(2) -0.0053(17) 0.0106(19) -0.0030(17) N25 0.032(2) 0.0237(19) 0.038(2) -0.0035(17) 0.0013(19) -0.0017(16) C64 0.049(4) 0.026(3) 0.056(4) -0.009(2) 0.010(3) -0.006(2) N26 0.032(2) 0.030(2) 0.035(2) -0.0045(18) 0.0096(19) -0.0049(17) C65 0.037(3) 0.030(2) 0.038(3) -0.007(2) 0.009(2) -0.005(2) C66 0.034(3) 0.037(3) 0.035(3) 0.001(2) 0.005(2) -0.007(2) C67 0.040(3) 0.037(3) 0.059(4) -0.003(3) 0.000(3) -0.006(2) C68 0.034(3) 0.054(4) 0.059(4) 0.004(3) -0.002(3) -0.001(3) C69 0.041(3) 0.044(3) 0.053(4) 0.003(3) 0.004(3) 0.004(3) C70 0.043(3) 0.034(3) 0.038(3) -0.001(2) 0.006(2) -0.002(2) N27 0.037(2) 0.028(2) 0.034(2) -0.0027(17) 0.0096(19) -0.0052(17) N28 0.042(3) 0.036(2) 0.035(2) 0.0011(19) 0.013(2) -0.0056(19) C71 0.051(4) 0.042(3) 0.041(3) -0.004(3) 0.012(3) 0.000(3) C72 0.057(4) 0.070(4) 0.032(3) -0.004(3) 0.015(3) 0.002(3) C73 0.049(4) 0.069(4) 0.032(3) 0.011(3) 0.011(3) 0.002(3) C74 0.043(3) 0.043(3) 0.037(3) 0.007(2) 0.011(3) -0.004(2) C75 0.036(3) 0.033(3) 0.032(3) 0.004(2) 0.010(2) -0.001(2) C76 0.034(3) 0.029(2) 0.041(3) 0.001(2) 0.010(2) -0.005(2) N29 0.031(2) 0.028(2) 0.030(2) 0.0018(17) 0.0074(18) -0.0032(16) N30 0.038(2) 0.0221(19) 0.031(2) -0.0001(16) 0.0100(18) -0.0026(16) C77 0.048(3) 0.023(2) 0.040(3) 0.002(2) 0.012(3) -0.002(2) C78 0.027(2) 0.024(2) 0.029(2) 0.0016(18) 0.007(2) -0.0022(17) N31 0.035(2) 0.0227(19) 0.031(2) 0.0008(16) 0.0085(18) 0.0007(16) C79 0.029(3) 0.024(2) 0.030(2) 0.0006(18) 0.007(2) -0.0025(18) C80 0.040(3) 0.025(3) 0.066(4) 0.003(3) -0.004(3) -0.003(2) C81 0.039(3) 0.037(3) 0.053(4) 0.010(3) 0.009(3) -0.005(2) C82 0.037(3) 0.035(3) 0.037(3) 0.003(2) 0.013(2) 0.000(2) C83 0.040(3) 0.033(3) 0.045(3) -0.011(2) 0.001(3) 0.002(2) C84 0.039(3) 0.027(2) 0.036(3) -0.001(2) 0.009(2) 0.004(2) N32 0.035(2) 0.0207(18) 0.028(2) 0.0010(15) 0.0058(17) -0.0037(15) C85 0.027(2) 0.025(2) 0.030(2) -0.0010(19) 0.003(2) 0.0031(18) N33 0.031(2) 0.0225(18) 0.031(2) 0.0017(16) 0.0069(17) -0.0019(15) N34 0.040(3) 0.0217(19) 0.033(2) -0.0009(16) 0.0115(19) 0.0036(16) C86 0.046(3) 0.024(2) 0.040(3) -0.005(2) 0.014(2) 0.006(2) N35 0.032(2) 0.028(2) 0.029(2) -0.0020(17) 0.0063(18) -0.0019(16) C87 0.037(3) 0.037(3) 0.034(3) -0.007(2) 0.007(2) -0.001(2) C88 0.036(3) 0.040(3) 0.036(3) -0.007(2) 0.011(2) -0.003(2) C89 0.045(4) 0.054(4) 0.042(3) -0.010(3) 0.014(3) -0.003(3) C90 0.067(5) 0.076(5) 0.040(3) -0.009(3) 0.030(3) -0.017(4) C91 0.082(5) 0.054(4) 0.054(4) 0.004(3) 0.028(4) -0.016(4) C92 0.065(4) 0.042(3) 0.047(4) 0.000(3) 0.022(3) -0.012(3) N36 0.042(3) 0.040(2) 0.037(3) -0.004(2) 0.012(2) -0.007(2) S1 0.0378(8) 0.0404(7) 0.0414(8) -0.0076(6) 0.0072(6) 0.0017(6) O1 0.044(3) 0.048(2) 0.071(3) -0.008(2) 0.008(2) -0.0070(19) O2 0.057(3) 0.060(3) 0.105(4) -0.044(3) 0.031(3) -0.004(2) O3 0.054(3) 0.106(4) 0.055(3) 0.022(3) 0.011(2) 0.006(3) C93 0.046(4) 0.067(4) 0.051(4) -0.005(3) 0.007(3) -0.006(3) F1 0.052(3) 0.087(3) 0.127(4) -0.007(3) 0.012(3) -0.028(2) F2 0.069(4) 0.258(8) 0.055(3) 0.050(4) -0.008(3) -0.039(4) F3 0.046(3) 0.123(4) 0.151(5) -0.056(4) -0.009(3) 0.028(3) S2 0.0598(11) 0.0476(8) 0.0454(9) -0.0005(7) 0.0185(8) 0.0028(7) O4 0.092(4) 0.054(3) 0.058(3) 0.010(2) 0.018(3) 0.012(3) O5 0.093(4) 0.054(3) 0.054(3) -0.004(2) 0.031(3) 0.008(3) O6 0.080(4) 0.089(4) 0.065(3) 0.004(3) 0.028(3) -0.017(3) C94 0.068(5) 0.056(4) 0.045(4) -0.004(3) 0.022(3) 0.010(3) F4 0.068(3) 0.107(4) 0.079(3) -0.002(3) 0.037(3) -0.012(3) F5 0.125(4) 0.075(3) 0.071(3) -0.023(2) 0.045(3) 0.009(3) F6 0.098(4) 0.080(3) 0.053(2) 0.018(2) 0.024(2) 0.023(3) S3 0.0356(7) 0.0356(7) 0.0393(7) 0.0062(6) 0.0066(6) -0.0035(5) O7 0.042(2) 0.038(2) 0.071(3) 0.013(2) 0.009(2) 0.0007(17) O8 0.054(3) 0.089(4) 0.052(3) -0.019(3) 0.009(2) -0.002(3) O9 0.063(3) 0.042(2) 0.068(3) 0.019(2) 0.029(2) 0.000(2) C95 0.040(4) 0.072(4) 0.046(4) 0.006(3) 0.007(3) 0.002(3) F7 0.040(2) 0.080(3) 0.105(4) 0.021(3) 0.017(2) -0.008(2) F8 0.058(3) 0.175(6) 0.086(4) -0.059(4) -0.003(3) -0.009(3) F9 0.058(3) 0.095(3) 0.109(4) 0.041(3) 0.014(3) 0.032(3) S4 0.0434(8) 0.0294(7) 0.0570(9) -0.0009(6) 0.0022(7) 0.0000(6) O10 0.045(2) 0.036(2) 0.063(3) -0.0063(19) 0.008(2) 0.0019(17) O11 0.061(3) 0.048(3) 0.083(4) -0.022(2) -0.011(3) 0.004(2) O12 0.060(3) 0.055(3) 0.082(4) 0.027(3) -0.003(3) -0.009(2) C96 0.063(5) 0.056(4) 0.079(5) -0.017(4) 0.025(4) 0.005(3) F10 0.051(3) 0.075(3) 0.107(4) -0.027(3) 0.024(2) -0.021(2) F11 0.121(5) 0.124(5) 0.080(4) 0.008(3) 0.051(3) -0.010(4) F12 0.069(3) 0.076(3) 0.189(6) -0.053(4) 0.050(4) 0.006(2) S5 0.0550(10) 0.0441(8) 0.0391(8) 0.0061(6) 0.0112(7) -0.0101(7) O13 0.055(3) 0.107(4) 0.049(3) -0.002(3) 0.013(2) -0.031(3) O14 0.068(3) 0.063(3) 0.048(3) 0.018(2) 0.020(2) 0.003(2) O15 0.103(4) 0.041(2) 0.058(3) 0.008(2) 0.017(3) 0.002(2) C97 0.062(5) 0.043(3) 0.057(4) 0.003(3) 0.012(3) -0.005(3) F13 0.090(3) 0.079(3) 0.044(2) -0.006(2) 0.006(2) -0.005(2) F14 0.056(3) 0.092(3) 0.098(4) -0.002(3) 0.009(3) -0.021(2) F15 0.109(4) 0.048(2) 0.093(4) -0.009(2) 0.009(3) 0.003(2) S6 0.0459(9) 0.0426(8) 0.0838(13) -0.0174(8) 0.0209(9) -0.0088(7) O16 0.061(3) 0.049(3) 0.087(4) -0.024(2) 0.024(3) -0.007(2) O17 0.058(3) 0.050(3) 0.151(6) -0.013(3) 0.039(4) -0.020(2) O18 0.111(5) 0.093(4) 0.057(3) 0.002(3) 0.012(3) 0.011(4) C98 0.062(5) 0.064(5) 0.092(6) -0.006(4) 0.031(5) -0.001(4) F16 0.090(4) 0.072(3) 0.151(5) -0.040(3) 0.043(4) 0.004(3) F17 0.098(5) 0.162(6) 0.119(5) 0.061(5) 0.030(4) 0.036(4) F18 0.052(3) 0.094(3) 0.113(4) -0.029(3) 0.038(3) -0.019(2) S7 0.109(2) 0.0657(13) 0.117(2) 0.0254(13) 0.0629(17) 0.0195(13) O19 0.138(7) 0.084(5) 0.108(5) -0.013(4) 0.028(5) 0.014(4) O20 0.099(5) 0.077(4) 0.054(3) 0.008(3) 0.010(3) 0.016(3) O21 0.114(6) 0.130(6) 0.140(7) 0.065(5) 0.078(5) 0.057(5) C99 0.133(12) 0.114(10) 0.133(12) 0.033(9) 0.041(10) 0.012(8) F19 0.079(5) 0.182(8) 0.174(8) 0.019(6) 0.038(5) -0.015(5) F20 0.248(12) 0.143(7) 0.224(11) -0.109(8) -0.028(9) 0.021(7) F21 0.126(5) 0.180(7) 0.084(4) 0.063(4) 0.028(4) 0.040(5) S8 0.0763(14) 0.0384(9) 0.1211(18) -0.0188(10) 0.0575(13) -0.0146(8) O22 0.087(4) 0.059(3) 0.103(4) -0.038(3) 0.047(3) -0.013(3) O23 0.087(4) 0.059(3) 0.103(4) -0.038(3) 0.047(3) -0.013(3) O24 0.087(4) 0.059(3) 0.103(4) -0.038(3) 0.047(3) -0.013(3) C100 0.153(12) 0.077(6) 0.086(7) -0.015(6) 0.048(7) 0.010(7) F22 0.54(3) 0.233(11) 0.240(12) 0.153(10) 0.291(16) 0.231(14) F23 0.167(7) 0.132(5) 0.115(5) -0.056(4) 0.059(5) 0.023(5) F24 0.134(7) 0.207(10) 0.287(13) -0.121(9) 0.136(8) -0.067(7) C101 0.106(7) 0.061(5) 0.088(6) 0.009(4) 0.047(6) 0.010(4) Cl1 0.1026(18) 0.0723(13) 0.1117(19) -0.0225(12) 0.0576(15) -0.0203(12) Cl2 0.304(6) 0.0763(18) 0.151(3) 0.0176(19) 0.083(3) 0.079(3) Cl3 0.153(3) 0.0903(17) 0.0897(18) -0.0098(14) 0.0502(18) -0.0119(17) C102 0.059(4) 0.051(4) 0.054(4) -0.005(3) 0.020(3) 0.005(3) Cl4 0.0655(12) 0.0615(10) 0.0711(12) -0.0052(9) 0.0187(9) -0.0080(8) Cl5 0.0680(12) 0.0704(12) 0.0918(14) -0.0220(10) 0.0450(11) -0.0051(9) Cl6 0.0625(11) 0.0557(9) 0.0695(11) -0.0007(8) 0.0231(9) 0.0099(8) C103 0.048(5) 0.098(6) 0.108(7) -0.035(6) 0.022(5) -0.015(4) Cl7 0.094(2) 0.099(2) 0.241(5) -0.053(2) 0.036(2) -0.0283(16) Cl8 0.0887(18) 0.114(2) 0.117(2) -0.0485(17) 0.0254(16) 0.0100(15) Cl9 0.122(2) 0.128(2) 0.0921(18) -0.0315(16) 0.0475(17) -0.0424(18) C104 0.063(5) 0.083(6) 0.072(5) -0.007(4) 0.007(4) -0.012(4) C105 0.047(4) 0.057(4) 0.058(4) 0.005(3) 0.012(3) -0.002(3) N40 0.065(4) 0.063(4) 0.092(5) 0.000(4) 0.018(4) -0.001(3) O25 0.104(9) 0.132(10) 0.051(6) 0.028(6) 0.033(6) 0.095(8) O26 0.103(10) 0.034(5) 0.125(11) 0.006(6) 0.016(8) 0.017(5) O27 0.213(16) 0.047(6) 0.072(7) 0.009(5) 0.079(9) -0.009(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N11 1.979(4) . ? Cu1 N10 2.054(5) . ? Cu1 N13 2.101(4) . ? Cu1 N2 2.103(4) . ? Cu1 N1 2.274(5) . ? Cu1 N4 2.340(4) . ? Cu2 N8 1.969(4) . ? Cu2 N20 2.021(4) . ? Cu2 N9 2.091(5) . ? Cu2 N5 2.126(4) . ? Cu2 N19 2.237(5) . ? Cu2 N22 2.293(4) . ? Cu3 N26 1.966(4) . ? Cu3 N27 2.051(4) . ? Cu3 N29 2.088(4) . ? Cu3 N23 2.103(4) . ? Cu3 N28 2.249(5) . ? Cu3 N31 2.316(4) . ? Cu4 N35 1.948(4) . ? Cu4 N17 2.056(4) . ? Cu4 N36 2.057(5) . ? Cu4 N32 2.102(4) . ? Cu4 N18 2.248(4) . ? Cu4 N14 2.341(4) . ? N1 C5 1.336(7) . ? N1 C1 1.348(8) . ? C1 C2 1.378(9) . ? C1 H1 0.9500 . ? C2 C3 1.377(10) . ? C2 H2 0.9500 . ? C3 C4 1.386(9) . ? C3 H3 0.9500 . ? C4 C5 1.395(8) . ? C4 H4 0.9500 . ? C5 C6 1.470(8) . ? C6 N2 1.279(6) . ? C6 H6 0.9500 . ? N2 N3 1.370(6) . ? N3 C8 1.367(6) . ? N3 C7 1.472(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N6 1.318(6) . ? C8 N4 1.350(6) . ? N4 C9 1.334(7) . ? C9 N5 1.335(7) . ? C9 C10 1.489(7) . ? C10 C15 1.363(9) . ? C10 C11 1.400(9) . ? C11 C12 1.410(11) . ? C11 H11 0.9500 . ? C12 C13 1.388(17) . ? C12 H12 0.9500 . ? C13 C14 1.301(17) . ? C13 H13 0.9500 . ? C14 C15 1.437(10) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? N5 C16 1.355(6) . ? C16 N6 1.316(6) . ? C16 N7 1.368(6) . ? N7 N8 1.356(6) . ? N7 C17 1.463(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? N8 C18 1.288(7) . ? C18 C19 1.456(7) . ? C18 H18 0.9500 . ? C19 N9 1.370(7) . ? C19 C20 1.378(8) . ? C20 C21 1.397(8) . ? C20 H20 0.9500 . ? C21 C22 1.387(9) . ? C21 H21 0.9500 . ? C22 C23 1.372(9) . ? C22 H22 0.9500 . ? C23 N9 1.326(7) . ? C23 H23 0.9500 . ? N10 C24 1.331(7) . ? N10 C28 1.354(7) . ? C24 C25 1.366(9) . ? C24 H24 0.9500 . ? C25 C26 1.382(9) . ? C25 H25 0.9500 . ? C26 C27 1.377(10) . ? C26 H26 0.9500 . ? C27 C28 1.378(8) . ? C27 H27 0.9500 . ? C28 C29 1.451(8) . ? C29 N11 1.279(7) . ? C29 H29 0.9500 . ? N11 N12 1.358(6) . ? N12 C31 1.359(7) . ? N12 C30 1.466(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 N15 1.316(6) . ? C31 N13 1.370(6) . ? N13 C32 1.335(6) . ? C32 N14 1.340(6) . ? C32 C33 1.484(6) . ? C33 C34 1.386(8) . ? C33 C38 1.392(7) . ? C34 C35 1.390(8) . ? C34 H34 0.9500 . ? C35 C36 1.378(9) . ? C35 H35 0.9500 . ? C36 C37 1.379(9) . ? C36 H36 0.9500 . ? C37 C38 1.393(7) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? N14 C39 1.354(6) . ? C39 N15 1.337(6) . ? C39 N16 1.356(6) . ? N16 N17 1.372(6) . ? N16 C40 1.462(6) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? N17 C41 1.285(6) . ? C41 C42 1.466(8) . ? C41 H41 0.9500 . ? C42 N18 1.354(7) . ? C42 C43 1.370(8) . ? C43 C44 1.390(9) . ? C43 H43 0.9500 . ? C44 C45 1.364(9) . ? C44 H44 0.9500 . ? C45 C46 1.396(8) . ? C45 H45 0.9500 . ? C46 N18 1.332(7) . ? C46 H46 0.9500 . ? N19 C47 1.331(7) . ? N19 C51 1.354(6) . ? C47 C48 1.379(9) . ? C47 H47 0.9500 . ? C48 C49 1.379(9) . ? C48 H48 0.9500 . ? C49 C50 1.376(9) . ? C49 H49 0.9500 . ? C50 C51 1.380(8) . ? C50 H50 0.9500 . ? C51 C52 1.446(8) . ? C52 N20 1.294(7) . ? C52 H52 0.9500 . ? N20 N21 1.383(6) . ? N21 C54 1.366(7) . ? N21 C53 1.455(6) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 N24 1.322(7) . ? C54 N22 1.355(6) . ? N22 C55 1.328(6) . ? C55 N23 1.341(6) . ? C55 C56 1.480(6) . ? C56 C84 1.391(7) . ? C56 C82 1.404(7) . ? C57 C62 1.333(13) . ? C57 C58 1.367(13) . ? C57 H57 0.9500 . ? C58 C59 1.407(10) . ? C58 H58 0.9500 . ? C59 C60 1.396(8) . ? C59 H59 0.9500 . ? C60 C61 1.400(8) . ? C60 C79 1.486(6) . ? C61 C62 1.372(8) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? N23 C63 1.363(6) . ? C63 N24 1.324(6) . ? C63 N25 1.351(6) . ? N25 N26 1.371(6) . ? N25 C64 1.465(6) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? N26 C65 1.276(7) . ? C65 C66 1.455(8) . ? C65 H65 0.9500 . ? C66 N27 1.359(7) . ? C66 C67 1.376(8) . ? C67 C68 1.406(9) . ? C67 H67 0.9500 . ? C68 C69 1.373(9) . ? C68 H68 0.9500 . ? C69 C70 1.367(8) . ? C69 H69 0.9500 . ? C70 N27 1.339(7) . ? C70 H70 0.9500 . ? N28 C75 1.356(7) . ? N28 C71 1.359(8) . ? C71 C72 1.380(9) . ? C71 H71 0.9500 . ? C72 C73 1.381(10) . ? C72 H72 0.9500 . ? C73 C74 1.370(9) . ? C73 H73 0.9500 . ? C74 C75 1.400(8) . ? C74 H74 0.9500 . ? C75 C76 1.444(8) . ? C76 N29 1.296(7) . ? C76 H76 0.9500 . ? N29 N30 1.376(6) . ? N30 C78 1.359(6) . ? N30 C77 1.463(6) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 N33 1.336(7) . ? C78 N31 1.353(6) . ? N31 C79 1.341(6) . ? C79 N32 1.340(7) . ? C80 C83 1.377(9) . ? C80 C81 1.378(9) . ? C80 H80 0.9500 . ? C81 C82 1.372(8) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83 C84 1.389(7) . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? N32 C85 1.368(6) . ? C85 N33 1.323(6) . ? C85 N34 1.349(7) . ? N34 N35 1.375(6) . ? N34 C86 1.468(6) . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? N35 C87 1.285(7) . ? C87 C88 1.449(8) . ? C87 H87 0.9500 . ? C88 N36 1.368(7) . ? C88 C89 1.376(8) . ? C89 C90 1.375(9) . ? C89 H89 0.9500 . ? C90 C91 1.385(10) . ? C90 H90 0.9500 . ? C91 C92 1.390(10) . ? C91 H91 0.9500 . ? C92 N36 1.340(7) . ? C92 H92 0.9500 . ? S1 O1 1.422(5) . ? S1 O3 1.424(5) . ? S1 O2 1.431(5) . ? S1 C93 1.817(7) . ? C93 F2 1.304(9) . ? C93 F3 1.302(9) . ? C93 F1 1.318(8) . ? S2 O6 1.406(6) . ? S2 O4 1.427(5) . ? S2 O5 1.452(5) . ? S2 C94 1.834(7) . ? C94 F4 1.308(9) . ? C94 F6 1.322(8) . ? C94 F5 1.330(8) . ? S3 O8 1.424(5) . ? S3 O7 1.430(4) . ? S3 O9 1.432(4) . ? S3 C95 1.815(7) . ? C95 F8 1.318(8) . ? C95 F7 1.330(8) . ? C95 F9 1.345(8) . ? S4 O10 1.429(4) . ? S4 O12 1.431(5) . ? S4 O11 1.434(5) . ? S4 C96 1.807(9) . ? C96 F10 1.310(9) . ? C96 F12 1.321(8) . ? C96 F11 1.349(10) . ? S5 O13 1.423(6) . ? S5 O14 1.438(5) . ? S5 O15 1.442(5) . ? S5 C97 1.825(7) . ? C97 F15 1.306(8) . ? C97 F13 1.330(8) . ? C97 F14 1.345(9) . ? S6 O17 1.411(5) . ? S6 O16 1.428(5) . ? S6 O18 1.464(6) . ? S6 C98 1.787(8) . ? C98 F18 1.321(9) . ? C98 F16 1.330(9) . ? C98 F17 1.341(10) . ? S7 O21 1.421(7) . ? S7 O20 1.476(6) . ? S7 O19 1.556(7) . ? S7 C99 1.785(14) . ? C99 F19 1.299(15) . ? C99 F21 1.335(14) . ? C99 F20 1.382(16) . ? S8 O24 1.310(9) . ? S8 O22 1.370(5) . ? S8 O23 1.401(12) . ? S8 C100 1.728(13) . ? C100 F22 1.266(13) . ? C100 F23 1.307(11) . ? C100 F24 1.314(15) . ? C101 Cl2 1.733(8) . ? C101 Cl3 1.754(10) . ? C101 Cl1 1.757(9) . ? C101 H101 1.0000 . ? C102 Cl6 1.742(7) . ? C102 Cl5 1.747(7) . ? C102 Cl4 1.758(7) . ? C102 H102 1.0000 . ? C103 Cl9 1.725(9) . ? C103 Cl7 1.741(9) . ? C103 Cl8 1.785(11) . ? C103 H103 1.0000 . ? C104 C105 1.438(10) . ? C104 H10A 0.9800 . ? C104 H10B 0.9800 . ? C104 H10C 0.9800 . ? C105 N40 1.132(9) . ? 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 N11 Cu1 N10 79.18(17) . . ? N11 Cu1 N13 76.61(16) . . ? N10 Cu1 N13 155.76(16) . . ? N11 Cu1 N2 170.34(17) . . ? N10 Cu1 N2 91.80(17) . . ? N13 Cu1 N2 112.44(16) . . ? N11 Cu1 N1 101.89(17) . . ? N10 Cu1 N1 90.98(18) . . ? N13 Cu1 N1 95.17(17) . . ? N2 Cu1 N1 74.55(16) . . ? N11 Cu1 N4 111.95(16) . . ? N10 Cu1 N4 91.87(17) . . ? N13 Cu1 N4 95.95(16) . . ? N2 Cu1 N4 71.48(15) . . ? N1 Cu1 N4 145.98(14) . . ? N8 Cu2 N20 171.49(18) . . ? N8 Cu2 N9 79.75(17) . . ? N20 Cu2 N9 92.73(17) . . ? N8 Cu2 N5 76.52(16) . . ? N20 Cu2 N5 110.89(17) . . ? N9 Cu2 N5 156.26(16) . . ? N8 Cu2 N19 99.25(17) . . ? N20 Cu2 N19 76.62(17) . . ? N9 Cu2 N19 90.28(17) . . ? N5 Cu2 N19 92.80(16) . . ? N8 Cu2 N22 111.19(16) . . ? N20 Cu2 N22 73.69(16) . . ? N9 Cu2 N22 98.74(16) . . ? N5 Cu2 N22 90.53(16) . . ? N19 Cu2 N22 149.30(15) . . ? N26 Cu3 N27 79.53(17) . . ? N26 Cu3 N29 171.68(17) . . ? N27 Cu3 N29 92.89(16) . . ? N26 Cu3 N23 76.86(17) . . ? N27 Cu3 N23 156.31(16) . . ? N29 Cu3 N23 110.80(16) . . ? N26 Cu3 N28 101.34(18) . . ? N27 Cu3 N28 93.28(17) . . ? N29 Cu3 N28 75.48(17) . . ? N23 Cu3 N28 93.18(17) . . ? N26 Cu3 N31 111.74(16) . . ? N27 Cu3 N31 91.66(16) . . ? N29 Cu3 N31 71.60(15) . . ? N23 Cu3 N31 95.26(15) . . ? N28 Cu3 N31 146.91(15) . . ? N35 Cu4 N17 172.95(18) . . ? N35 Cu4 N36 79.64(18) . . ? N17 Cu4 N36 93.43(18) . . ? N35 Cu4 N32 77.26(17) . . ? N17 Cu4 N32 109.66(17) . . ? N36 Cu4 N32 156.90(17) . . ? N35 Cu4 N18 102.64(17) . . ? N17 Cu4 N18 76.36(16) . . ? N36 Cu4 N18 93.72(18) . . ? N32 Cu4 N18 91.12(16) . . ? N35 Cu4 N14 109.08(16) . . ? N17 Cu4 N14 72.73(15) . . ? N36 Cu4 N14 96.30(17) . . ? N32 Cu4 N14 91.42(16) . . ? N18 Cu4 N14 147.95(15) . . ? C5 N1 C1 118.0(5) . . ? C5 N1 Cu1 111.5(4) . . ? C1 N1 Cu1 129.4(4) . . ? N1 C1 C2 122.2(6) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.5(6) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 119.4(6) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 117.6(6) . . ? C3 C4 H4 121.2 . . ? C5 C4 H4 121.2 . . ? N1 C5 C4 123.4(5) . . ? N1 C5 C6 116.4(5) . . ? C4 C5 C6 120.2(5) . . ? N2 C6 C5 117.4(5) . . ? N2 C6 H6 121.3 . . ? C5 C6 H6 121.3 . . ? C6 N2 N3 119.2(4) . . ? C6 N2 Cu1 119.2(3) . . ? N3 N2 Cu1 121.0(3) . . ? C8 N3 N2 116.9(4) . . ? C8 N3 C7 121.5(4) . . ? N2 N3 C7 121.3(4) . . ? N3 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N6 C8 N4 125.6(4) . . ? N6 C8 N3 117.3(4) . . ? N4 C8 N3 117.1(4) . . ? C9 N4 C8 114.4(4) . . ? C9 N4 Cu1 131.6(3) . . ? C8 N4 Cu1 113.2(3) . . ? N4 C9 N5 125.1(4) . . ? N4 C9 C10 117.3(5) . . ? N5 C9 C10 117.6(4) . . ? C15 C10 C11 121.6(6) . . ? C15 C10 C9 118.5(6) . . ? C11 C10 C9 119.9(6) . . ? C10 C11 C12 118.2(9) . . ? C10 C11 H11 120.9 . . ? C12 C11 H11 120.9 . . ? C13 C12 C11 120.1(10) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 120.1(8) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 123.1(10) . . ? C13 C14 H14 118.5 . . ? C15 C14 H14 118.5 . . ? C10 C15 C14 117.0(9) . . ? C10 C15 H15 121.5 . . ? C14 C15 H15 121.5 . . ? C9 N5 C16 114.3(4) . . ? C9 N5 Cu2 133.1(3) . . ? C16 N5 Cu2 112.6(3) . . ? N6 C16 N5 125.5(5) . . ? N6 C16 N7 117.8(4) . . ? N5 C16 N7 116.7(4) . . ? C16 N6 C8 115.0(4) . . ? N8 N7 C16 114.5(4) . . ? N8 N7 C17 121.2(4) . . ? C16 N7 C17 123.9(4) . . ? N7 C17 H17A 109.5 . . ? N7 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N7 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C18 N8 N7 123.1(4) . . ? C18 N8 Cu2 117.6(3) . . ? N7 N8 Cu2 119.3(3) . . ? N8 C18 C19 116.2(5) . . ? N8 C18 H18 121.9 . . ? C19 C18 H18 121.9 . . ? N9 C19 C20 122.6(5) . . ? N9 C19 C18 114.9(5) . . ? C20 C19 C18 122.5(5) . . ? C19 C20 C21 118.5(5) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 120.8 . . ? C22 C21 C20 117.9(6) . . ? C22 C21 H21 121.1 . . ? C20 C21 H21 121.1 . . ? C23 C22 C21 120.7(6) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? N9 C23 C22 121.9(5) . . ? N9 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C23 N9 C19 118.3(5) . . ? C23 N9 Cu2 130.3(4) . . ? C19 N9 Cu2 110.8(3) . . ? C24 N10 C28 118.3(5) . . ? C24 N10 Cu1 129.2(4) . . ? C28 N10 Cu1 112.4(4) . . ? N10 C24 C25 122.3(5) . . ? N10 C24 H24 118.9 . . ? C25 C24 H24 118.9 . . ? C24 C25 C26 119.5(6) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C27 C26 C25 119.0(6) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C26 C27 C28 118.4(6) . . ? C26 C27 H27 120.8 . . ? C28 C27 H27 120.8 . . ? N10 C28 C27 122.4(5) . . ? N10 C28 C29 114.9(5) . . ? C27 C28 C29 122.6(5) . . ? N11 C29 C28 115.4(5) . . ? N11 C29 H29 122.3 . . ? C28 C29 H29 122.3 . . ? C29 N11 N12 123.3(4) . . ? C29 N11 Cu1 117.7(4) . . ? N12 N11 Cu1 119.0(3) . . ? N11 N12 C31 114.7(4) . . ? N11 N12 C30 121.7(4) . . ? C31 N12 C30 123.2(4) . . ? N12 C30 H30A 109.5 . . ? N12 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N12 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N15 C31 N12 118.3(4) . . ? N15 C31 N13 125.5(5) . . ? N12 C31 N13 116.2(4) . . ? C32 N13 C31 113.9(4) . . ? C32 N13 Cu1 132.8(3) . . ? C31 N13 Cu1 113.3(3) . . ? N13 C32 N14 125.4(4) . . ? N13 C32 C33 117.0(4) . . ? N14 C32 C33 117.6(4) . . ? C34 C33 C38 120.4(5) . . ? C34 C33 C32 119.7(5) . . ? C38 C33 C32 119.9(5) . . ? C33 C34 C35 119.5(5) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C36 C35 C34 120.2(6) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C37 C36 C35 120.6(5) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 119.9(6) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C33 C38 C37 119.5(5) . . ? C33 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C32 N14 C39 114.9(4) . . ? C32 N14 Cu4 134.5(3) . . ? C39 N14 Cu4 110.6(3) . . ? N15 C39 N14 124.7(5) . . ? N15 C39 N16 116.9(4) . . ? N14 C39 N16 118.5(4) . . ? C31 N15 C39 115.4(4) . . ? C39 N16 N17 116.6(4) . . ? C39 N16 C40 123.6(4) . . ? N17 N16 C40 119.8(4) . . ? N16 C40 H40A 109.5 . . ? N16 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N16 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C41 N17 N16 120.7(4) . . ? C41 N17 Cu4 118.3(4) . . ? N16 N17 Cu4 120.6(3) . . ? N17 C41 C42 118.3(5) . . ? N17 C41 H41 120.8 . . ? C42 C41 H41 120.8 . . ? N18 C42 C43 123.0(5) . . ? N18 C42 C41 115.7(4) . . ? C43 C42 C41 121.3(5) . . ? C42 C43 C44 118.0(6) . . ? C42 C43 H43 121.0 . . ? C44 C43 H43 121.0 . . ? C45 C44 C43 119.8(6) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 119.0(6) . . ? C44 C45 H45 120.5 . . ? C46 C45 H45 120.5 . . ? N18 C46 C45 121.8(5) . . ? N18 C46 H46 119.1 . . ? C45 C46 H46 119.1 . . ? C46 N18 C42 118.4(5) . . ? C46 N18 Cu4 130.8(4) . . ? C42 N18 Cu4 110.8(3) . . ? C47 N19 C51 117.6(5) . . ? C47 N19 Cu2 132.1(4) . . ? C51 N19 Cu2 110.1(3) . . ? N19 C47 C48 123.4(5) . . ? N19 C47 H47 118.3 . . ? C48 C47 H47 118.3 . . ? C47 C48 C49 118.7(6) . . ? C47 C48 H48 120.7 . . ? C49 C48 H48 120.7 . . ? C50 C49 C48 118.9(6) . . ? C50 C49 H49 120.6 . . ? C48 C49 H49 120.6 . . ? C49 C50 C51 119.3(6) . . ? C49 C50 H50 120.4 . . ? C51 C50 H50 120.4 . . ? N19 C51 C50 122.2(5) . . ? N19 C51 C52 115.8(5) . . ? C50 C51 C52 122.0(5) . . ? N20 C52 C51 118.1(5) . . ? N20 C52 H52 121.0 . . ? C51 C52 H52 121.0 . . ? C52 N20 N21 120.5(4) . . ? C52 N20 Cu2 118.5(4) . . ? N21 N20 Cu2 120.6(3) . . ? C54 N21 N20 116.2(4) . . ? C54 N21 C53 122.6(4) . . ? N20 N21 C53 121.3(4) . . ? N21 C53 H53A 109.5 . . ? N21 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N21 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N24 C54 N22 125.2(5) . . ? N24 C54 N21 117.6(4) . . ? N22 C54 N21 117.2(5) . . ? C55 N22 C54 115.1(4) . . ? C55 N22 Cu2 133.1(3) . . ? C54 N22 Cu2 111.7(3) . . ? N22 C55 N23 124.8(4) . . ? N22 C55 C56 117.8(4) . . ? N23 C55 C56 117.4(4) . . ? C84 C56 C82 119.6(5) . . ? C84 C56 C55 121.7(5) . . ? C82 C56 C55 118.6(5) . . ? C62 C57 C58 120.9(6) . . ? C62 C57 H57 119.5 . . ? C58 C57 H57 119.5 . . ? C57 C58 C59 120.7(7) . . ? C57 C58 H58 119.6 . . ? C59 C58 H58 119.7 . . ? C60 C59 C58 117.8(7) . . ? C60 C59 H59 121.1 . . ? C58 C59 H59 121.1 . . ? C59 C60 C61 119.7(5) . . ? C59 C60 C79 122.4(5) . . ? C61 C60 C79 117.9(5) . . ? C62 C61 C60 119.6(7) . . ? C62 C61 H61 120.2 . . ? C60 C61 H61 120.2 . . ? C57 C62 C61 121.2(7) . . ? C57 C62 H62 119.4 . . ? C61 C62 H62 119.4 . . ? C55 N23 C63 114.4(4) . . ? C55 N23 Cu3 132.4(3) . . ? C63 N23 Cu3 112.9(3) . . ? N24 C63 N25 117.9(4) . . ? N24 C63 N23 125.0(5) . . ? N25 C63 N23 117.1(4) . . ? C54 N24 C63 115.2(4) . . ? C63 N25 N26 114.1(4) . . ? C63 N25 C64 124.3(4) . . ? N26 N25 C64 121.2(4) . . ? N25 C64 H64A 109.5 . . ? N25 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N25 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C65 N26 N25 122.4(4) . . ? C65 N26 Cu3 118.6(4) . . ? N25 N26 Cu3 119.0(3) . . ? N26 C65 C66 114.3(5) . . ? N26 C65 H65 122.8 . . ? C66 C65 H65 122.8 . . ? N27 C66 C67 122.0(5) . . ? N27 C66 C65 115.7(5) . . ? C67 C66 C65 122.2(5) . . ? C66 C67 C68 119.1(5) . . ? C66 C67 H67 120.5 . . ? C68 C67 H67 120.5 . . ? C69 C68 C67 117.8(6) . . ? C69 C68 H68 121.1 . . ? C67 C68 H68 121.1 . . ? C70 C69 C68 120.4(6) . . ? C70 C69 H69 119.8 . . ? C68 C69 H69 119.8 . . ? N27 C70 C69 122.5(5) . . ? N27 C70 H70 118.8 . . ? C69 C70 H70 118.8 . . ? C70 N27 C66 118.2(5) . . ? C70 N27 Cu3 130.1(4) . . ? C66 N27 Cu3 111.5(3) . . ? C75 N28 C71 118.0(5) . . ? C75 N28 Cu3 111.6(4) . . ? C71 N28 Cu3 130.4(4) . . ? N28 C71 C72 121.9(6) . . ? N28 C71 H71 119.1 . . ? C72 C71 H71 119.1 . . ? C71 C72 C73 119.7(6) . . ? C71 C72 H72 120.2 . . ? C73 C72 H72 120.2 . . ? C74 C73 C72 119.6(6) . . ? C74 C73 H73 120.2 . . ? C72 C73 H73 120.2 . . ? C73 C74 C75 118.7(6) . . ? C73 C74 H74 120.7 . . ? C75 C74 H74 120.7 . . ? N28 C75 C74 122.2(5) . . ? N28 C75 C76 116.2(5) . . ? C74 C75 C76 121.6(5) . . ? N29 C76 C75 118.3(5) . . ? N29 C76 H76 120.9 . . ? C75 C76 H76 120.9 . . ? C76 N29 N30 120.4(4) . . ? C76 N29 Cu3 118.2(4) . . ? N30 N29 Cu3 120.9(3) . . ? C78 N30 N29 116.5(4) . . ? C78 N30 C77 123.0(4) . . ? N29 N30 C77 120.4(4) . . ? N30 C77 H77A 109.5 . . ? N30 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? N30 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? N33 C78 N31 126.2(4) . . ? N33 C78 N30 117.0(4) . . ? N31 C78 N30 116.7(4) . . ? C79 N31 C78 114.1(4) . . ? C79 N31 Cu3 132.0(3) . . ? C78 N31 Cu3 113.7(3) . . ? N32 C79 N31 125.3(4) . . ? N32 C79 C60 117.7(4) . . ? N31 C79 C60 116.9(4) . . ? C83 C80 C81 120.0(5) . . ? C83 C80 H80 120.0 . . ? C81 C80 H80 120.0 . . ? C82 C81 C80 120.7(6) . . ? C82 C81 H81 119.6 . . ? C80 C81 H81 119.6 . . ? C81 C82 C56 119.7(5) . . ? C81 C82 H82 120.2 . . ? C56 C82 H82 120.2 . . ? C80 C83 C84 120.6(6) . . ? C80 C83 H83 119.7 . . ? C84 C83 H83 119.7 . . ? C83 C84 C56 119.4(5) . . ? C83 C84 H84 120.3 . . ? C56 C84 H84 120.3 . . ? C79 N32 C85 114.5(4) . . ? C79 N32 Cu4 132.9(3) . . ? C85 N32 Cu4 112.6(3) . . ? N33 C85 N34 118.1(4) . . ? N33 C85 N32 125.2(5) . . ? N34 C85 N32 116.7(4) . . ? C85 N33 C78 114.5(4) . . ? C85 N34 N35 114.4(4) . . ? C85 N34 C86 125.4(4) . . ? N35 N34 C86 120.1(4) . . ? N34 C86 H86A 109.5 . . ? N34 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? N34 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C87 N35 N34 122.5(4) . . ? C87 N35 Cu4 118.5(4) . . ? N34 N35 Cu4 118.9(3) . . ? N35 C87 C88 115.0(5) . . ? N35 C87 H87 122.5 . . ? C88 C87 H87 122.5 . . ? N36 C88 C89 122.1(5) . . ? N36 C88 C87 114.8(5) . . ? C89 C88 C87 123.2(5) . . ? C90 C89 C88 119.5(6) . . ? C90 C89 H89 120.2 . . ? C88 C89 H89 120.2 . . ? C89 C90 C91 119.2(6) . . ? C89 C90 H90 120.4 . . ? C91 C90 H90 120.4 . . ? C90 C91 C92 118.7(6) . . ? C90 C91 H91 120.7 . . ? C92 C91 H91 120.7 . . ? N36 C92 C91 122.7(6) . . ? N36 C92 H92 118.7 . . ? C91 C92 H92 118.7 . . ? C92 N36 C88 117.8(5) . . ? C92 N36 Cu4 130.4(4) . . ? C88 N36 Cu4 111.6(4) . . ? O1 S1 O3 114.4(3) . . ? O1 S1 O2 113.2(3) . . ? O3 S1 O2 116.9(4) . . ? O1 S1 C93 104.9(3) . . ? O3 S1 C93 101.9(3) . . ? O2 S1 C93 103.3(3) . . ? F2 C93 F3 107.6(7) . . ? F2 C93 F1 104.8(6) . . ? F3 C93 F1 107.4(7) . . ? F2 C93 S1 113.0(5) . . ? F3 C93 S1 112.1(5) . . ? F1 C93 S1 111.6(5) . . ? O6 S2 O4 115.1(4) . . ? O6 S2 O5 114.0(4) . . ? O4 S2 O5 114.8(3) . . ? O6 S2 C94 103.5(3) . . ? O4 S2 C94 104.7(3) . . ? O5 S2 C94 102.6(3) . . ? F4 C94 F6 107.7(6) . . ? F4 C94 F5 108.1(6) . . ? F6 C94 F5 106.3(6) . . ? F4 C94 S2 112.6(5) . . ? F6 C94 S2 111.0(5) . . ? F5 C94 S2 110.8(5) . . ? O8 S3 O7 116.1(3) . . ? O8 S3 O9 115.2(3) . . ? O7 S3 O9 114.0(3) . . ? O8 S3 C95 101.9(3) . . ? O7 S3 C95 103.3(3) . . ? O9 S3 C95 103.8(3) . . ? F8 C95 F7 107.1(7) . . ? F8 C95 F9 108.5(6) . . ? F7 C95 F9 105.6(6) . . ? F8 C95 S3 113.2(5) . . ? F7 C95 S3 111.1(4) . . ? F9 C95 S3 111.0(5) . . ? O10 S4 O12 114.6(3) . . ? O10 S4 O11 115.1(3) . . ? O12 S4 O11 115.6(3) . . ? O10 S4 C96 102.2(3) . . ? O12 S4 C96 103.1(4) . . ? O11 S4 C96 103.7(4) . . ? F10 C96 F12 107.5(7) . . ? F10 C96 F11 105.0(7) . . ? F12 C96 F11 106.7(7) . . ? F10 C96 S4 114.5(6) . . ? F12 C96 S4 111.0(6) . . ? F11 C96 S4 111.6(6) . . ? O13 S5 O14 114.3(3) . . ? O13 S5 O15 115.2(3) . . ? O14 S5 O15 114.7(3) . . ? O13 S5 C97 103.4(3) . . ? O14 S5 C97 104.3(3) . . ? O15 S5 C97 102.9(3) . . ? F15 C97 F13 109.4(6) . . ? F15 C97 F14 107.3(6) . . ? F13 C97 F14 107.0(6) . . ? F15 C97 S5 112.3(5) . . ? F13 C97 S5 110.4(5) . . ? F14 C97 S5 110.2(5) . . ? O17 S6 O16 114.2(4) . . ? O17 S6 O18 114.8(4) . . ? O16 S6 O18 113.9(4) . . ? O17 S6 C98 104.3(4) . . ? O16 S6 C98 105.7(4) . . ? O18 S6 C98 102.2(4) . . ? F18 C98 F16 107.4(7) . . ? F18 C98 F17 105.9(7) . . ? F16 C98 F17 106.8(7) . . ? F18 C98 S6 113.0(6) . . ? F16 C98 S6 112.3(6) . . ? F17 C98 S6 111.0(6) . . ? O21 S7 O20 121.2(5) . . ? O21 S7 O19 107.6(5) . . ? O20 S7 O19 112.5(4) . . ? O21 S7 C99 107.7(6) . . ? O20 S7 C99 105.3(6) . . ? O19 S7 C99 100.5(6) . . ? F19 C99 F21 110.8(13) . . ? F19 C99 F20 110.6(14) . . ? F21 C99 F20 112.7(12) . . ? F19 C99 S7 111.9(9) . . ? F21 C99 S7 108.5(10) . . ? F20 C99 S7 102.1(11) . . ? O24 S8 O22 125.6(7) . . ? O24 S8 O23 104.5(11) . . ? O22 S8 O23 109.4(5) . . ? O24 S8 C100 106.8(6) . . ? O22 S8 C100 107.9(5) . . ? O23 S8 C100 99.6(10) . . ? F22 C100 F23 111.4(11) . . ? F22 C100 F24 95.5(14) . . ? F23 C100 F24 104.7(11) . . ? F22 C100 S8 114.8(10) . . ? F23 C100 S8 114.8(9) . . ? F24 C100 S8 113.6(8) . . ? Cl2 C101 Cl3 110.4(5) . . ? Cl2 C101 Cl1 109.9(5) . . ? Cl3 C101 Cl1 109.7(5) . . ? Cl2 C101 H101 108.9 . . ? Cl3 C101 H101 108.9 . . ? Cl1 C101 H101 108.9 . . ? Cl6 C102 Cl5 110.6(4) . . ? Cl6 C102 Cl4 111.6(4) . . ? Cl5 C102 Cl4 110.2(4) . . ? Cl6 C102 H102 108.1 . . ? Cl5 C102 H102 108.1 . . ? Cl4 C102 H102 108.1 . . ? Cl9 C103 Cl7 113.8(6) . . ? Cl9 C103 Cl8 110.0(5) . . ? Cl7 C103 Cl8 107.9(5) . . ? Cl9 C103 H103 108.3 . . ? Cl7 C103 H103 108.3 . . ? Cl8 C103 H103 108.3 . . ? C105 C104 H10A 109.5 . . ? C105 C104 H10B 109.5 . . ? H10A C104 H10B 109.5 . . ? C105 C104 H10C 109.5 . . ? H10A C104 H10C 109.5 . . ? H10B C104 H10C 109.5 . . ? N40 C105 C104 178.0(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.558 _refine_diff_density_min -1.031 _refine_diff_density_rms 0.171 data_stadler13 _database_code_depnum_ccdc_archive 'CCDC 753683' #TrackingRef '- Cu21a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H26 Cu2 F9 N10 O10 S3, C F3 O3 S' _chemical_formula_sum 'C26 H26 Cu2 F12 N10 O13 S4' _chemical_formula_weight 1169.89 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' S S 0.1246 0.1234 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3216(3) _cell_length_b 11.1123(3) _cell_length_c 19.8965(5) _cell_angle_alpha 87.112(2) _cell_angle_beta 82.405(2) _cell_angle_gamma 69.9080(10) _cell_volume 2124.35(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14856 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 1.322 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.65844 _exptl_absorpt_correction_T_max 0.92809 _exptl_absorpt_process_details 'MULscanABS in PLATON (Spek, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25866 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0687 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9689 _reflns_number_gt 6720 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material '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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0949P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9689 _refine_ls_number_parameters 608 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1640 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0720(4) 0.4547(3) 0.22468(17) 0.0232(7) Uani 1 1 d . . . H1 H 1.0656 0.4889 0.2683 0.028 Uiso 1 1 calc R . . C2 C 1.0347(4) 0.3091(3) 0.15831(17) 0.0224(7) Uani 1 1 d . . . C3 C 1.0936(4) 0.3560(3) 0.10131(17) 0.0236(8) Uani 1 1 d . . . H3 H 1.1027 0.3199 0.0579 0.028 Uiso 1 1 calc R . . C4 C 1.1389(4) 0.4571(3) 0.10950(17) 0.0217(7) Uani 1 1 d . . . C5 C 0.9740(4) 0.1445(4) 0.09872(19) 0.0310(9) Uani 1 1 d . . . H5A H 1.0047 0.1847 0.0576 0.047 Uiso 1 1 calc R . . H5B H 0.8776 0.1493 0.0979 0.047 Uiso 1 1 calc R . . H5C H 1.0338 0.0545 0.1007 0.047 Uiso 1 1 calc R . . C6 C 0.8859(4) 0.0862(3) 0.23408(19) 0.0273(8) Uani 1 1 d . . . H6 H 0.8793 0.0330 0.1997 0.033 Uiso 1 1 calc R . . C7 C 0.8448(4) 0.0684(3) 0.3061(2) 0.0285(8) Uani 1 1 d . . . C8 C 0.7963(4) -0.0275(4) 0.3306(2) 0.0392(10) Uani 1 1 d . . . H8 H 0.7859 -0.0866 0.3007 0.047 Uiso 1 1 calc R . . C9 C 0.7623(5) -0.0366(4) 0.4007(2) 0.0456(11) Uani 1 1 d . . . H9 H 0.7290 -0.1027 0.4191 0.055 Uiso 1 1 calc R . . C10 C 0.7773(5) 0.0505(4) 0.4425(2) 0.0437(11) Uani 1 1 d . . . H10 H 0.7540 0.0462 0.4902 0.052 Uiso 1 1 calc R . . C11 C 0.8269(4) 0.1450(4) 0.4142(2) 0.0385(10) Uani 1 1 d . . . H11 H 0.8381 0.2048 0.4434 0.046 Uiso 1 1 calc R . . C12 C 1.2315(5) 0.4715(4) -0.01259(19) 0.0350(9) Uani 1 1 d . . . H12A H 1.1901 0.5430 -0.0428 0.053 Uiso 1 1 calc R . . H12B H 1.1958 0.4021 -0.0183 0.053 Uiso 1 1 calc R . . H12C H 1.3328 0.4403 -0.0239 0.053 Uiso 1 1 calc R . . C13 C 1.2819(4) 0.6851(3) 0.03703(18) 0.0260(8) Uani 1 1 d . . . H13 H 1.3057 0.6697 -0.0103 0.031 Uiso 1 1 calc R . . C14 C 1.3031(4) 0.7904(3) 0.07050(18) 0.0251(8) Uani 1 1 d . . . C15 C 1.3473(4) 0.8825(4) 0.0359(2) 0.0305(8) Uani 1 1 d . . . H15 H 1.3702 0.8787 -0.0119 0.037 Uiso 1 1 calc R . . C16 C 1.3576(4) 0.9813(4) 0.0729(2) 0.0367(9) Uani 1 1 d . . . H16 H 1.3864 1.0468 0.0503 0.044 Uiso 1 1 calc R . . C17 C 1.3260(4) 0.9836(4) 0.1420(2) 0.0324(9) Uani 1 1 d . . . H17 H 1.3344 1.0496 0.1678 0.039 Uiso 1 1 calc R . . C18 C 1.2817(4) 0.8884(3) 0.17375(19) 0.0281(8) Uani 1 1 d . . . H18 H 1.2593 0.8908 0.2217 0.034 Uiso 1 1 calc R . . C19 C 1.3984(5) 0.0275(4) 0.3527(2) 0.0420(10) Uani 1 1 d . . . C20 C 1.5032(4) 0.2702(4) 0.2094(2) 0.0394(10) Uani 1 1 d . . . C21 C 0.7386(5) 0.7572(5) 0.1519(2) 0.0464(12) Uani 1 1 d . . . C22 C 1.4172(6) 0.3364(5) 0.4873(3) 0.0589(14) Uani 1 1 d . . . C23 C 0.6385(4) 0.5270(4) 0.3079(2) 0.0360(9) Uani 1 1 d . . . C24 C 0.5128(6) 0.6374(5) 0.3120(3) 0.0692(17) Uani 1 1 d . . . H24A H 0.5290 0.7093 0.3316 0.104 Uiso 1 1 calc R . . H24B H 0.4383 0.6169 0.3407 0.104 Uiso 1 1 calc R . . H24C H 0.4856 0.6607 0.2664 0.104 Uiso 1 1 calc R . . C25 C 1.1284(4) 0.6971(4) 0.3278(2) 0.0308(9) Uani 1 1 d . . . C26 C 1.0955(6) 0.7065(5) 0.4016(2) 0.0509(12) Uani 1 1 d . . . H26A H 1.0065 0.6933 0.4152 0.076 Uiso 1 1 calc R . . H26B H 1.0890 0.7915 0.4161 0.076 Uiso 1 1 calc R . . H26C H 1.1689 0.6408 0.4229 0.076 Uiso 1 1 calc R . . N1 N 1.0259(3) 0.3589(3) 0.22139(14) 0.0227(6) Uani 1 1 d . . . N2 N 1.1267(3) 0.5080(3) 0.17250(14) 0.0227(6) Uani 1 1 d . . . N3 N 0.9827(3) 0.2113(3) 0.15817(14) 0.0234(6) Uani 1 1 d . . . N4 N 0.9314(3) 0.1794(3) 0.22119(14) 0.0237(6) Uani 1 1 d . . . N5 N 0.8595(3) 0.1553(3) 0.34799(16) 0.0293(7) Uani 1 1 d . . . N6 N 1.1956(3) 0.5151(3) 0.05764(14) 0.0231(6) Uani 1 1 d . . . N7 N 1.2287(3) 0.6157(3) 0.07681(14) 0.0218(6) Uani 1 1 d . . . N8 N 1.2691(3) 0.7931(3) 0.13963(14) 0.0245(6) Uani 1 1 d . . . N9 N 0.7381(4) 0.4428(3) 0.30365(18) 0.0372(8) Uani 1 1 d . . . N10 N 1.1555(3) 0.6869(3) 0.27086(15) 0.0275(7) Uani 1 1 d . . . O1 O 1.1818(3) 0.1088(3) 0.29116(13) 0.0377(7) Uani 1 1 d . . . O2 O 1.1513(3) 0.0979(3) 0.41413(14) 0.0465(8) Uani 1 1 d . . . O3 O 1.2339(4) -0.0963(3) 0.34698(18) 0.0568(9) Uani 1 1 d . . . O4 O 1.4353(3) 0.5099(2) 0.17816(14) 0.0367(7) Uani 1 1 d . . . O5 O 1.6692(3) 0.3689(3) 0.13880(15) 0.0463(8) Uani 1 1 d . . . O6 O 1.4725(3) 0.3577(3) 0.08824(14) 0.0516(9) Uani 1 1 d . . . O7 O 0.9626(3) 0.8092(3) 0.15440(13) 0.0353(7) Uani 1 1 d . . . O8 O 0.9252(3) 0.7301(3) 0.04987(13) 0.0406(7) Uani 1 1 d . . . O9 O 0.7902(4) 0.9470(3) 0.08799(19) 0.0654(11) Uani 1 1 d . . . O10 O 1.2394(5) 0.3253(4) 0.5866(2) 0.0832(13) Uani 1 1 d . . . O11 O 1.2092(3) 0.5311(3) 0.52987(16) 0.0505(8) Uani 1 1 d . . . O12 O 1.1689(4) 0.3653(5) 0.4727(3) 0.116(2) Uani 1 1 d . . . O13 O 0.9944(3) 0.3580(2) 0.37085(12) 0.0319(6) Uani 1 1 d . . . F1 F 1.4514(3) -0.0403(3) 0.40604(15) 0.0719(9) Uani 1 1 d . . . F2 F 1.4789(3) -0.0295(3) 0.29718(15) 0.0761(10) Uani 1 1 d . . . F3 F 1.4083(4) 0.1419(3) 0.35497(15) 0.0682(9) Uani 1 1 d . . . F4 F 1.5778(3) 0.1531(2) 0.18845(18) 0.0727(9) Uani 1 1 d . . . F5 F 1.3710(3) 0.2750(3) 0.22062(15) 0.0593(8) Uani 1 1 d . . . F6 F 1.5434(3) 0.2868(3) 0.26728(13) 0.0600(8) Uani 1 1 d . . . F7 F 0.6394(3) 0.7631(3) 0.11512(16) 0.0669(9) Uani 1 1 d . . . F8 F 0.6784(4) 0.8245(4) 0.20722(17) 0.0971(13) Uani 1 1 d . . . F9 F 0.7959(3) 0.6358(3) 0.16819(17) 0.0727(9) Uani 1 1 d . . . F10 F 1.4376(4) 0.3880(4) 0.42729(18) 0.1043(14) Uani 1 1 d . . . F11 F 1.4601(4) 0.2102(3) 0.47971(19) 0.0942(13) Uani 1 1 d . . . F12 F 1.4971(4) 0.3620(4) 0.5266(2) 0.0967(13) Uani 1 1 d . . . S1 S 1.22158(10) 0.03477(9) 0.35144(5) 0.0299(2) Uani 1 1 d . . . S2 S 1.52256(10) 0.38964(9) 0.14677(5) 0.0328(2) Uani 1 1 d . . . S3 S 0.86777(10) 0.81872(9) 0.10558(5) 0.0297(2) Uani 1 1 d . . . S4 S 1.23717(12) 0.39578(11) 0.52136(7) 0.0527(3) Uani 1 1 d . . . Cu1 Cu 0.93950(5) 0.27922(4) 0.29843(2) 0.02561(14) Uani 1 1 d . . . Cu2 Cu 1.19587(5) 0.65412(4) 0.17335(2) 0.02532(14) Uani 1 1 d . . . H1W H 0.9285 0.4044 0.4055 0.050 Uiso 1 1 d . . . H2W H 1.0590 0.3095 0.3932 0.050 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 C1 0.0294(19) 0.0226(17) 0.0204(17) -0.0013(14) -0.0034(15) -0.0121(15) C2 0.0222(18) 0.0219(17) 0.0227(18) -0.0026(14) -0.0048(14) -0.0057(14) C3 0.0270(19) 0.0246(18) 0.0194(17) -0.0041(14) -0.0033(14) -0.0082(15) C4 0.0222(17) 0.0231(17) 0.0190(17) -0.0005(14) -0.0031(14) -0.0063(14) C5 0.035(2) 0.034(2) 0.028(2) -0.0074(16) -0.0052(17) -0.0166(17) C6 0.0274(19) 0.0251(18) 0.033(2) -0.0010(16) -0.0056(16) -0.0126(15) C7 0.0246(19) 0.0254(18) 0.037(2) 0.0064(16) -0.0091(16) -0.0098(15) C8 0.033(2) 0.036(2) 0.054(3) 0.009(2) -0.011(2) -0.0183(18) C9 0.037(2) 0.045(3) 0.059(3) 0.026(2) -0.006(2) -0.023(2) C10 0.037(2) 0.053(3) 0.040(2) 0.019(2) -0.001(2) -0.019(2) C11 0.037(2) 0.050(3) 0.030(2) 0.0088(19) -0.0036(18) -0.018(2) C12 0.050(3) 0.039(2) 0.0231(19) -0.0035(17) 0.0013(18) -0.025(2) C13 0.0270(19) 0.0306(19) 0.0201(18) 0.0011(15) -0.0015(15) -0.0099(16) C14 0.0211(18) 0.0258(18) 0.0273(19) 0.0030(15) -0.0040(15) -0.0065(15) C15 0.032(2) 0.031(2) 0.029(2) 0.0057(16) -0.0007(17) -0.0136(17) C16 0.039(2) 0.033(2) 0.044(2) 0.0050(18) -0.0021(19) -0.0203(18) C17 0.034(2) 0.0276(19) 0.040(2) -0.0036(17) -0.0030(18) -0.0163(17) C18 0.030(2) 0.0286(19) 0.0282(19) -0.0013(16) -0.0030(16) -0.0134(16) C19 0.034(2) 0.053(3) 0.039(2) 0.009(2) -0.008(2) -0.015(2) C20 0.027(2) 0.040(2) 0.050(3) 0.009(2) -0.0042(19) -0.0124(18) C21 0.034(2) 0.062(3) 0.041(3) -0.018(2) 0.002(2) -0.013(2) C22 0.054(3) 0.062(3) 0.050(3) -0.019(3) -0.004(3) -0.004(3) C23 0.033(2) 0.036(2) 0.039(2) -0.0036(18) -0.0115(18) -0.0099(19) C24 0.049(3) 0.062(3) 0.076(4) -0.010(3) -0.016(3) 0.013(3) C25 0.037(2) 0.033(2) 0.030(2) -0.0015(17) -0.0045(17) -0.0204(17) C26 0.068(3) 0.069(3) 0.024(2) -0.002(2) 0.001(2) -0.037(3) N1 0.0267(16) 0.0216(14) 0.0198(14) 0.0006(12) -0.0027(12) -0.0083(12) N2 0.0274(16) 0.0222(14) 0.0207(15) 0.0000(12) -0.0047(12) -0.0107(12) N3 0.0276(16) 0.0257(15) 0.0202(15) -0.0029(12) -0.0027(12) -0.0131(13) N4 0.0251(16) 0.0231(15) 0.0231(15) 0.0019(12) -0.0065(13) -0.0074(12) N5 0.0258(16) 0.0342(17) 0.0303(17) 0.0048(14) -0.0033(13) -0.0141(14) N6 0.0317(17) 0.0223(14) 0.0186(14) 0.0002(12) -0.0024(13) -0.0136(13) N7 0.0215(15) 0.0214(14) 0.0222(15) -0.0015(12) -0.0022(12) -0.0069(12) N8 0.0269(16) 0.0245(15) 0.0250(16) 0.0010(12) -0.0041(13) -0.0120(13) N9 0.0308(19) 0.0388(19) 0.040(2) 0.0040(16) -0.0081(16) -0.0089(17) N10 0.0344(18) 0.0299(16) 0.0220(16) -0.0013(13) -0.0004(14) -0.0169(14) O1 0.0336(15) 0.0453(16) 0.0273(14) 0.0022(12) -0.0077(12) -0.0035(13) O2 0.0370(17) 0.062(2) 0.0273(15) 0.0028(14) -0.0025(13) -0.0016(15) O3 0.077(3) 0.0365(17) 0.069(2) 0.0077(16) -0.0216(19) -0.0317(17) O4 0.0325(15) 0.0312(14) 0.0421(16) 0.0017(12) -0.0039(13) -0.0057(12) O5 0.0300(16) 0.0579(19) 0.0455(18) 0.0173(15) -0.0001(14) -0.0119(14) O6 0.0485(19) 0.063(2) 0.0299(16) -0.0099(14) -0.0087(14) 0.0014(16) O7 0.0317(15) 0.0379(15) 0.0353(15) -0.0137(12) -0.0094(12) -0.0067(12) O8 0.0403(17) 0.0596(19) 0.0265(14) -0.0133(13) 0.0028(12) -0.0237(15) O9 0.080(3) 0.0315(17) 0.087(3) 0.0129(17) -0.043(2) -0.0115(17) O10 0.116(4) 0.057(2) 0.080(3) 0.011(2) 0.015(3) -0.046(2) O11 0.061(2) 0.0356(16) 0.0465(18) -0.0064(14) 0.0038(16) -0.0093(15) O12 0.065(3) 0.117(4) 0.161(5) -0.084(4) -0.052(3) 0.000(3) O13 0.0317(15) 0.0388(15) 0.0246(13) -0.0043(11) -0.0045(11) -0.0103(12) F1 0.0424(16) 0.108(3) 0.0654(19) 0.0421(18) -0.0284(15) -0.0230(16) F2 0.0385(16) 0.110(3) 0.0618(19) -0.0064(18) 0.0137(14) -0.0081(17) F3 0.087(2) 0.090(2) 0.0599(18) 0.0176(16) -0.0232(17) -0.068(2) F4 0.063(2) 0.0317(14) 0.114(3) 0.0081(16) -0.0138(18) -0.0046(14) F5 0.0364(15) 0.0635(17) 0.082(2) 0.0302(15) -0.0107(14) -0.0257(13) F6 0.0662(19) 0.084(2) 0.0438(15) 0.0282(14) -0.0208(14) -0.0421(16) F7 0.0326(15) 0.079(2) 0.092(2) -0.0301(17) -0.0103(15) -0.0181(14) F8 0.077(2) 0.155(3) 0.067(2) -0.066(2) 0.0391(18) -0.058(2) F9 0.069(2) 0.071(2) 0.086(2) 0.0332(17) -0.0086(18) -0.0391(17) F10 0.109(3) 0.136(4) 0.056(2) -0.016(2) 0.027(2) -0.038(3) F11 0.083(2) 0.069(2) 0.095(3) -0.0322(19) -0.020(2) 0.0259(19) F12 0.055(2) 0.138(3) 0.101(3) -0.029(2) -0.029(2) -0.026(2) S1 0.0275(5) 0.0305(5) 0.0317(5) 0.0016(4) -0.0061(4) -0.0093(4) S2 0.0276(5) 0.0364(5) 0.0276(5) 0.0052(4) -0.0003(4) -0.0039(4) S3 0.0343(5) 0.0270(5) 0.0290(5) -0.0009(4) -0.0090(4) -0.0099(4) S4 0.0391(6) 0.0447(7) 0.0740(9) -0.0232(6) -0.0049(6) -0.0116(5) Cu1 0.0329(3) 0.0265(2) 0.0208(2) -0.00021(18) -0.00141(19) -0.0150(2) Cu2 0.0356(3) 0.0262(2) 0.0187(2) -0.00088(18) -0.00135(19) -0.0169(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.315(4) . ? C1 N2 1.326(4) . ? C1 H1 0.9500 . ? C2 N3 1.368(4) . ? C2 N1 1.377(4) . ? C2 C3 1.379(5) . ? C3 C4 1.381(5) . ? C3 H3 0.9500 . ? C4 N6 1.362(4) . ? C4 N2 1.374(4) . ? C5 N3 1.456(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N4 1.278(5) . ? C6 C7 1.463(5) . ? C6 H6 0.9500 . ? C7 N5 1.366(5) . ? C7 C8 1.369(5) . ? C8 C9 1.400(6) . ? C8 H8 0.9500 . ? C9 C10 1.368(7) . ? C9 H9 0.9500 . ? C10 C11 1.385(6) . ? C10 H10 0.9500 . ? C11 N5 1.325(5) . ? C11 H11 0.9500 . ? C12 N6 1.460(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N7 1.280(5) . ? C13 C14 1.468(5) . ? C13 H13 0.9500 . ? C14 N8 1.373(4) . ? C14 C15 1.377(5) . ? C15 C16 1.393(5) . ? C15 H15 0.9500 . ? C16 C17 1.370(6) . ? C16 H16 0.9500 . ? C17 C18 1.385(5) . ? C17 H17 0.9500 . ? C18 N8 1.338(4) . ? C18 H18 0.9500 . ? C19 F3 1.313(5) . ? C19 F2 1.333(5) . ? C19 F1 1.336(5) . ? C19 S1 1.803(5) . ? C20 F6 1.316(5) . ? C20 F4 1.320(5) . ? C20 F5 1.336(5) . ? C20 S2 1.818(4) . ? C21 F7 1.316(5) . ? C21 F9 1.318(6) . ? C21 F8 1.320(5) . ? C21 S3 1.825(5) . ? C22 F12 1.314(6) . ? C22 F10 1.322(6) . ? C22 F11 1.327(6) . ? C22 S4 1.794(5) . ? C23 N9 1.124(5) . ? C23 C24 1.444(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N10 1.131(5) . ? C25 C26 1.464(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? N1 Cu1 1.993(3) . ? N2 Cu2 1.987(3) . ? N3 N4 1.374(4) . ? N4 Cu1 1.967(3) . ? N5 Cu1 1.995(3) . ? N6 N7 1.361(4) . ? N7 Cu2 1.949(3) . ? N8 Cu2 1.992(3) . ? N9 Cu1 2.237(3) . ? N10 Cu2 1.955(3) . ? O1 S1 1.443(3) . ? O2 S1 1.440(3) . ? O3 S1 1.424(3) . ? O4 S2 1.447(3) . ? O5 S2 1.439(3) . ? O6 S2 1.441(3) . ? O7 S3 1.443(3) . ? O8 S3 1.444(3) . ? O9 S3 1.426(3) . ? O10 S4 1.481(4) . ? O11 S4 1.445(3) . ? O12 S4 1.387(4) . ? O13 Cu1 1.962(2) . ? O13 H1W 0.9353 . ? O13 H2W 0.8600 . ? 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 N1 C1 N2 125.8(3) . . ? N1 C1 H1 117.1 . . ? N2 C1 H1 117.1 . . ? N3 C2 N1 114.5(3) . . ? N3 C2 C3 124.6(3) . . ? N1 C2 C3 120.9(3) . . ? C2 C3 C4 117.7(3) . . ? C2 C3 H3 121.1 . . ? C4 C3 H3 121.1 . . ? N6 C4 N2 115.0(3) . . ? N6 C4 C3 124.1(3) . . ? N2 C4 C3 120.9(3) . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 C7 114.5(3) . . ? N4 C6 H6 122.8 . . ? C7 C6 H6 122.8 . . ? N5 C7 C8 121.8(4) . . ? N5 C7 C6 114.6(3) . . ? C8 C7 C6 123.6(4) . . ? C7 C8 C9 118.6(4) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C10 C9 C8 119.4(4) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 118.9(4) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? N5 C11 C10 122.6(4) . . ? N5 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? N6 C12 H12A 109.5 . . ? N6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N7 C13 C14 114.5(3) . . ? N7 C13 H13 122.7 . . ? C14 C13 H13 122.7 . . ? N8 C14 C15 122.3(3) . . ? N8 C14 C13 114.2(3) . . ? C15 C14 C13 123.4(3) . . ? C14 C15 C16 118.3(4) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? C17 C16 C15 119.8(4) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 119.1(3) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? N8 C18 C17 122.6(3) . . ? N8 C18 H18 118.7 . . ? C17 C18 H18 118.7 . . ? F3 C19 F2 107.0(4) . . ? F3 C19 F1 108.6(4) . . ? F2 C19 F1 107.3(4) . . ? F3 C19 S1 112.1(3) . . ? F2 C19 S1 110.9(3) . . ? F1 C19 S1 110.7(3) . . ? F6 C20 F4 107.5(4) . . ? F6 C20 F5 108.9(4) . . ? F4 C20 F5 106.7(4) . . ? F6 C20 S2 111.5(3) . . ? F4 C20 S2 111.4(3) . . ? F5 C20 S2 110.6(3) . . ? F7 C21 F9 106.6(4) . . ? F7 C21 F8 107.1(4) . . ? F9 C21 F8 109.6(4) . . ? F7 C21 S3 111.7(3) . . ? F9 C21 S3 110.8(3) . . ? F8 C21 S3 111.0(3) . . ? F12 C22 F10 107.3(5) . . ? F12 C22 F11 107.9(5) . . ? F10 C22 F11 107.9(4) . . ? F12 C22 S4 112.3(3) . . ? F10 C22 S4 111.0(4) . . ? F11 C22 S4 110.4(4) . . ? N9 C23 C24 178.2(6) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N10 C25 C26 178.4(5) . . ? 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 . . ? C1 N1 C2 117.4(3) . . ? C1 N1 Cu1 126.8(2) . . ? C2 N1 Cu1 115.8(2) . . ? C1 N2 C4 117.3(3) . . ? C1 N2 Cu2 128.1(2) . . ? C4 N2 Cu2 114.7(2) . . ? C2 N3 N4 114.3(3) . . ? C2 N3 C5 126.2(3) . . ? N4 N3 C5 119.5(3) . . ? C6 N4 N3 125.4(3) . . ? C6 N4 Cu1 117.5(3) . . ? N3 N4 Cu1 117.0(2) . . ? C11 N5 C7 118.7(3) . . ? C11 N5 Cu1 128.4(3) . . ? C7 N5 Cu1 112.9(3) . . ? N7 N6 C4 114.4(3) . . ? N7 N6 C12 120.0(3) . . ? C4 N6 C12 125.4(3) . . ? C13 N7 N6 125.5(3) . . ? C13 N7 Cu2 117.6(2) . . ? N6 N7 Cu2 116.9(2) . . ? C18 N8 C14 117.9(3) . . ? C18 N8 Cu2 129.5(3) . . ? C14 N8 Cu2 112.5(2) . . ? C23 N9 Cu1 177.6(3) . . ? C25 N10 Cu2 174.1(3) . . ? Cu1 O13 H1W 121.0 . . ? Cu1 O13 H2W 117.6 . . ? H1W O13 H2W 102.0 . . ? O3 S1 O2 115.9(2) . . ? O3 S1 O1 113.93(19) . . ? O2 S1 O1 114.69(17) . . ? O3 S1 C19 103.4(2) . . ? O2 S1 C19 103.2(2) . . ? O1 S1 C19 103.40(19) . . ? O5 S2 O6 114.66(19) . . ? O5 S2 O4 114.97(19) . . ? O6 S2 O4 114.27(17) . . ? O5 S2 C20 103.69(18) . . ? O6 S2 C20 103.6(2) . . ? O4 S2 C20 103.58(18) . . ? O9 S3 O7 114.18(18) . . ? O9 S3 O8 116.0(2) . . ? O7 S3 O8 114.19(17) . . ? O9 S3 C21 104.5(2) . . ? O7 S3 C21 103.39(19) . . ? O8 S3 C21 102.41(18) . . ? O12 S4 O11 115.3(3) . . ? O12 S4 O10 116.9(3) . . ? O11 S4 O10 112.9(2) . . ? O12 S4 C22 104.4(3) . . ? O11 S4 C22 103.6(2) . . ? O10 S4 C22 101.4(3) . . ? O13 Cu1 N4 166.60(11) . . ? O13 Cu1 N1 96.39(12) . . ? N4 Cu1 N1 78.42(12) . . ? O13 Cu1 N5 103.45(12) . . ? N4 Cu1 N5 80.54(13) . . ? N1 Cu1 N5 158.74(12) . . ? O13 Cu1 N9 89.48(12) . . ? N4 Cu1 N9 102.98(12) . . ? N1 Cu1 N9 92.33(12) . . ? N5 Cu1 N9 95.36(13) . . ? N7 Cu2 N10 176.62(12) . . ? N7 Cu2 N2 79.01(12) . . ? N10 Cu2 N2 97.77(12) . . ? N7 Cu2 N8 81.15(12) . . ? N10 Cu2 N8 102.02(12) . . ? N2 Cu2 N8 160.01(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 C2 C3 C4 178.6(3) . . . . ? N1 C2 C3 C4 -2.2(5) . . . . ? C2 C3 C4 N6 -178.2(3) . . . . ? C2 C3 C4 N2 0.7(5) . . . . ? N4 C6 C7 N5 1.0(5) . . . . ? N4 C6 C7 C8 -178.6(4) . . . . ? N5 C7 C8 C9 -0.6(6) . . . . ? C6 C7 C8 C9 178.9(4) . . . . ? C7 C8 C9 C10 0.5(6) . . . . ? C8 C9 C10 C11 -0.5(6) . . . . ? C9 C10 C11 N5 0.6(7) . . . . ? N7 C13 C14 N8 3.2(5) . . . . ? N7 C13 C14 C15 -174.0(3) . . . . ? N8 C14 C15 C16 0.1(5) . . . . ? C13 C14 C15 C16 177.1(4) . . . . ? C14 C15 C16 C17 1.0(6) . . . . ? C15 C16 C17 C18 -1.2(6) . . . . ? C16 C17 C18 N8 0.4(6) . . . . ? N2 C1 N1 C2 -0.1(5) . . . . ? N2 C1 N1 Cu1 -178.6(3) . . . . ? N3 C2 N1 C1 -178.8(3) . . . . ? C3 C2 N1 C1 1.9(5) . . . . ? N3 C2 N1 Cu1 -0.2(4) . . . . ? C3 C2 N1 Cu1 -179.5(3) . . . . ? N1 C1 N2 C4 -1.3(5) . . . . ? N1 C1 N2 Cu2 179.0(3) . . . . ? N6 C4 N2 C1 180.0(3) . . . . ? C3 C4 N2 C1 1.0(5) . . . . ? N6 C4 N2 Cu2 -0.3(4) . . . . ? C3 C4 N2 Cu2 -179.3(3) . . . . ? N1 C2 N3 N4 -0.4(4) . . . . ? C3 C2 N3 N4 178.9(3) . . . . ? N1 C2 N3 C5 177.6(3) . . . . ? C3 C2 N3 C5 -3.1(6) . . . . ? C7 C6 N4 N3 176.5(3) . . . . ? C7 C6 N4 Cu1 0.5(4) . . . . ? C2 N3 N4 C6 -175.3(3) . . . . ? C5 N3 N4 C6 6.6(5) . . . . ? C2 N3 N4 Cu1 0.8(4) . . . . ? C5 N3 N4 Cu1 -177.3(2) . . . . ? C10 C11 N5 C7 -0.7(6) . . . . ? C10 C11 N5 Cu1 -177.1(3) . . . . ? C8 C7 N5 C11 0.7(6) . . . . ? C6 C7 N5 C11 -178.9(3) . . . . ? C8 C7 N5 Cu1 177.7(3) . . . . ? C6 C7 N5 Cu1 -1.9(4) . . . . ? N2 C4 N6 N7 -1.1(4) . . . . ? C3 C4 N6 N7 177.9(3) . . . . ? N2 C4 N6 C12 173.8(3) . . . . ? C3 C4 N6 C12 -7.2(6) . . . . ? C14 C13 N7 N6 178.0(3) . . . . ? C14 C13 N7 Cu2 -3.5(4) . . . . ? C4 N6 N7 C13 -179.4(3) . . . . ? C12 N6 N7 C13 5.4(5) . . . . ? C4 N6 N7 Cu2 2.1(4) . . . . ? C12 N6 N7 Cu2 -173.1(3) . . . . ? C17 C18 N8 C14 0.6(5) . . . . ? C17 C18 N8 Cu2 -175.4(3) . . . . ? C15 C14 N8 C18 -0.8(5) . . . . ? C13 C14 N8 C18 -178.1(3) . . . . ? C15 C14 N8 Cu2 175.8(3) . . . . ? C13 C14 N8 Cu2 -1.5(4) . . . . ? F3 C19 S1 O3 178.3(3) . . . . ? F2 C19 S1 O3 58.7(4) . . . . ? F1 C19 S1 O3 -60.3(4) . . . . ? F3 C19 S1 O2 -60.5(3) . . . . ? F2 C19 S1 O2 179.9(3) . . . . ? F1 C19 S1 O2 60.9(4) . . . . ? F3 C19 S1 O1 59.3(3) . . . . ? F2 C19 S1 O1 -60.3(4) . . . . ? F1 C19 S1 O1 -179.3(3) . . . . ? F6 C20 S2 O5 60.7(3) . . . . ? F4 C20 S2 O5 -59.4(4) . . . . ? F5 C20 S2 O5 -178.0(3) . . . . ? F6 C20 S2 O6 -179.2(3) . . . . ? F4 C20 S2 O6 60.6(3) . . . . ? F5 C20 S2 O6 -57.9(3) . . . . ? F6 C20 S2 O4 -59.7(3) . . . . ? F4 C20 S2 O4 -179.8(3) . . . . ? F5 C20 S2 O4 61.7(3) . . . . ? F7 C21 S3 O9 58.0(3) . . . . ? F9 C21 S3 O9 176.7(3) . . . . ? F8 C21 S3 O9 -61.4(4) . . . . ? F7 C21 S3 O7 177.8(3) . . . . ? F9 C21 S3 O7 -63.6(3) . . . . ? F8 C21 S3 O7 58.3(4) . . . . ? F7 C21 S3 O8 -63.3(3) . . . . ? F9 C21 S3 O8 55.3(3) . . . . ? F8 C21 S3 O8 177.3(4) . . . . ? F12 C22 S4 O12 177.7(5) . . . . ? F10 C22 S4 O12 57.6(5) . . . . ? F11 C22 S4 O12 -61.9(5) . . . . ? F12 C22 S4 O11 56.7(5) . . . . ? F10 C22 S4 O11 -63.4(4) . . . . ? F11 C22 S4 O11 177.1(3) . . . . ? F12 C22 S4 O10 -60.5(5) . . . . ? F10 C22 S4 O10 179.4(4) . . . . ? F11 C22 S4 O10 59.9(4) . . . . ? C6 N4 Cu1 O13 107.4(5) . . . . ? N3 N4 Cu1 O13 -69.0(6) . . . . ? C6 N4 Cu1 N1 175.7(3) . . . . ? N3 N4 Cu1 N1 -0.7(2) . . . . ? C6 N4 Cu1 N5 -1.2(3) . . . . ? N3 N4 Cu1 N5 -177.6(2) . . . . ? C6 N4 Cu1 N9 -94.5(3) . . . . ? N3 N4 Cu1 N9 89.0(2) . . . . ? C1 N1 Cu1 O13 -13.6(3) . . . . ? C2 N1 Cu1 O13 168.0(2) . . . . ? C1 N1 Cu1 N4 178.9(3) . . . . ? C2 N1 Cu1 N4 0.5(2) . . . . ? C1 N1 Cu1 N5 -172.6(3) . . . . ? C2 N1 Cu1 N5 9.0(5) . . . . ? C1 N1 Cu1 N9 76.2(3) . . . . ? C2 N1 Cu1 N9 -102.3(2) . . . . ? C11 N5 Cu1 O13 11.3(4) . . . . ? C7 N5 Cu1 O13 -165.3(2) . . . . ? C11 N5 Cu1 N4 178.3(4) . . . . ? C7 N5 Cu1 N4 1.7(2) . . . . ? C11 N5 Cu1 N1 169.8(3) . . . . ? C7 N5 Cu1 N1 -6.8(5) . . . . ? C11 N5 Cu1 N9 -79.4(3) . . . . ? C7 N5 Cu1 N9 104.0(3) . . . . ? C13 N7 Cu2 N2 179.6(3) . . . . ? N6 N7 Cu2 N2 -1.7(2) . . . . ? C13 N7 Cu2 N8 2.1(3) . . . . ? N6 N7 Cu2 N8 -179.3(2) . . . . ? C1 N2 Cu2 N7 -179.3(3) . . . . ? C4 N2 Cu2 N7 1.1(2) . . . . ? C1 N2 Cu2 N10 -0.3(3) . . . . ? C4 N2 Cu2 N10 -179.9(2) . . . . ? C1 N2 Cu2 N8 -172.1(3) . . . . ? C4 N2 Cu2 N8 8.2(5) . . . . ? C18 N8 Cu2 N7 176.0(3) . . . . ? C14 N8 Cu2 N7 -0.2(2) . . . . ? C18 N8 Cu2 N10 -2.9(3) . . . . ? C14 N8 Cu2 N10 -179.0(2) . . . . ? C18 N8 Cu2 N2 168.8(3) . . . . ? C14 N8 Cu2 N2 -7.3(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H1W O11 0.94 1.76 2.684(4) 169.2 2_766 O13 H1W S4 0.94 2.65 3.541(3) 159.1 2_766 O13 H2W O2 0.86 2.25 2.936(4) 136.3 . O13 H2W O12 0.86 2.29 2.905(5) 128.9 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.319 _refine_diff_density_min -0.984 _refine_diff_density_rms 0.149 # Attachment '- Cu41a4.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 778853' #TrackingRef '- Cu41a4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Department of Chemistry University of Anywhere Sometown Somewhere, UK ; _chemical_name_common ;Department of Chemistry University of Anywhere Sometown Somewhere, UK ; _chemical_melting_point ? _chemical_formula_moiety 'C72 H72 Cu4 N32, 7(C F3 O3 S), 5(C2 H3 N)' _chemical_formula_sum 'C89 H87 Cu4 F21 N37 O21 S7' _chemical_formula_weight 2888.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 Orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 23.0185(4) _cell_length_b 20.8028(3) _cell_length_c 28.2909(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13547.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 113246 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5860 _exptl_absorpt_coefficient_mu 0.827 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Department of Chemistry University of Anywhere Sometown Somewhere, UK ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 84611 _diffrn_reflns_av_R_equivalents 0.0886 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15926 _reflns_number_gt 9041 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material '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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1771P)^2^+37.0514P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15926 _refine_ls_number_parameters 780 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1665 _refine_ls_R_factor_gt 0.1047 _refine_ls_wR_factor_ref 0.3277 _refine_ls_wR_factor_gt 0.2940 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7838(3) 0.0968(3) 0.4526(2) 0.0319(13) Uani 1 1 d . . . H1 H 0.7441 0.1001 0.4439 0.038 Uiso 1 1 calc R . . C2 C 0.8804(2) 0.0903(3) 0.4314(2) 0.0272(12) Uani 1 1 d . . . C3 C 0.8966(3) 0.0893(3) 0.4777(2) 0.0298(13) Uani 1 1 d . . . H3 H 0.9364 0.0882 0.4866 0.036 Uiso 1 1 calc R . . C4 C 0.8531(3) 0.0900(3) 0.5110(2) 0.0293(13) Uani 1 1 d . . . C5 C 0.9806(2) 0.0779(4) 0.3981(2) 0.0425(17) Uani 1 1 d . . . H5A H 1.0006 0.1163 0.3863 0.064 Uiso 1 1 calc R . . H5B H 0.9925 0.0405 0.3793 0.064 Uiso 1 1 calc R . . H5C H 0.9908 0.0709 0.4313 0.064 Uiso 1 1 calc R . . C6 C 0.9219(3) 0.0858(3) 0.3113(2) 0.0335(14) Uani 1 1 d . . . H6 H 0.9630 0.0821 0.3105 0.040 Uiso 1 1 calc R . . C7 C 0.8864(3) 0.0873(3) 0.2686(2) 0.0409(16) Uani 1 1 d . . . C8 C 0.9091(3) 0.0861(4) 0.2242(3) 0.056(2) Uani 1 1 d . . . H8 H 0.9500 0.0828 0.2201 0.068 Uiso 1 1 calc R . . C9 C 0.8732(4) 0.0897(6) 0.1853(3) 0.084(3) Uani 1 1 d . . . H9 H 0.8886 0.0923 0.1542 0.101 Uiso 1 1 calc R . . C10 C 0.8120(4) 0.0894(5) 0.1935(3) 0.081(3) Uani 1 1 d . . . H10 H 0.7854 0.0876 0.1679 0.098 Uiso 1 1 calc R . . C11 C 0.7923(3) 0.0919(4) 0.2396(3) 0.055(2) Uani 1 1 d . . . H11 H 0.7516 0.0948 0.2450 0.065 Uiso 1 1 calc R . . C12 C 0.9204(3) 0.0747(4) 0.5803(2) 0.0415(16) Uani 1 1 d . . . H12A H 0.9505 0.0757 0.5558 0.062 Uiso 1 1 calc R . . H12B H 0.9206 0.0327 0.5959 0.062 Uiso 1 1 calc R . . H12C H 0.9282 0.1084 0.6036 0.062 Uiso 1 1 calc R . . C13 C 0.8146(3) 0.0766(3) 0.6306(2) 0.0403(15) Uani 1 1 d . . . H13 H 0.8489 0.0677 0.6481 0.048 Uiso 1 1 calc R . . C14 C 0.7577(3) 0.0803(4) 0.6525(2) 0.0427(16) Uani 1 1 d . . . C15 C 0.7497(4) 0.0721(5) 0.7013(3) 0.065(2) Uani 1 1 d . . . H15 H 0.7810 0.0626 0.7220 0.078 Uiso 1 1 calc R . . C16 C 0.6913(4) 0.0789(5) 0.7181(3) 0.074(3) Uani 1 1 d . . . H16 H 0.6831 0.0747 0.7509 0.089 Uiso 1 1 calc R . . C17 C 0.6478(4) 0.0913(5) 0.6874(3) 0.084(3) Uani 1 1 d . . . H17 H 0.6088 0.0931 0.6982 0.100 Uiso 1 1 calc R . . C18 C 0.6603(3) 0.1014(4) 0.6396(3) 0.060(2) Uani 1 1 d . . . H18 H 0.6301 0.1146 0.6189 0.073 Uiso 1 1 calc R . . C19 C 0.7950(4) 0.2500 0.3463(3) 0.034(2) Uani 1 2 d S . . H19 H 0.8363 0.2500 0.3473 0.041 Uiso 1 2 calc SR . . C20 C 0.7117(2) 0.1928(3) 0.3457(2) 0.0306(13) Uani 1 1 d . . . C21 C 0.6799(3) 0.2500 0.3454(3) 0.038(2) Uani 1 2 d S . . H21 H 0.6386 0.2500 0.3450 0.046 Uiso 1 2 calc SR . . C22 C 0.6209(3) 0.1262(4) 0.3471(3) 0.054(2) Uani 1 1 d . . . H22A H 0.6064 0.1184 0.3150 0.081 Uiso 1 1 calc R . . H22B H 0.6032 0.1654 0.3598 0.081 Uiso 1 1 calc R . . H22C H 0.6109 0.0896 0.3673 0.081 Uiso 1 1 calc R . . C23 C 0.6989(3) 0.0243(3) 0.3408(3) 0.0406(16) Uani 1 1 d . . . H23 H 0.6582 0.0180 0.3382 0.049 Uiso 1 1 calc R . . C24 C 0.7376(3) -0.0306(4) 0.3410(3) 0.0493(18) Uani 1 1 d . . . C25 C 0.7154(5) -0.0923(4) 0.3377(5) 0.085(4) Uani 1 1 d . . . H25 H 0.6748 -0.0996 0.3355 0.102 Uiso 1 1 calc R . . C26 C 0.7542(5) -0.1430(5) 0.3377(5) 0.089(4) Uani 1 1 d . . . H26 H 0.7409 -0.1858 0.3332 0.107 Uiso 1 1 calc R . . C27 C 0.8113(5) -0.1308(4) 0.3441(4) 0.080(3) Uani 1 1 d . . . H27 H 0.8384 -0.1652 0.3457 0.096 Uiso 1 1 calc R . . C28 C 0.8303(3) -0.0668(4) 0.3483(3) 0.0464(17) Uani 1 1 d . . . H28 H 0.8704 -0.0583 0.3529 0.056 Uiso 1 1 calc R . . C29 C 0.7263(4) 0.2500 0.5502(3) 0.033(2) Uani 1 2 d S . . H29 H 0.7614 0.2500 0.5679 0.040 Uiso 1 2 calc SR . . C30 C 0.6541(2) 0.1941(3) 0.5138(2) 0.0328(14) Uani 1 1 d . . . C31 C 0.6281(4) 0.2500 0.4988(3) 0.038(2) Uani 1 2 d S . . H31 H 0.5943 0.2500 0.4794 0.045 Uiso 1 2 calc SR . . C32 C 0.5735(3) 0.1283(4) 0.4821(3) 0.055(2) Uani 1 1 d . . . H32A H 0.5736 0.0925 0.4595 0.083 Uiso 1 1 calc R . . H32B H 0.5640 0.1683 0.4655 0.083 Uiso 1 1 calc R . . H32C H 0.5444 0.1202 0.5067 0.083 Uiso 1 1 calc R . . C33 C 0.6363(3) 0.0250(3) 0.5186(3) 0.0452(17) Uani 1 1 d . . . H33 H 0.5981 0.0196 0.5064 0.054 Uiso 1 1 calc R . . C34 C 0.6702(3) -0.0306(4) 0.5357(3) 0.0492(18) Uani 1 1 d . . . C35 C 0.6474(5) -0.0901(4) 0.5365(4) 0.075(3) Uani 1 1 d . . . H35 H 0.6090 -0.0973 0.5253 0.090 Uiso 1 1 calc R . . C36 C 0.6797(5) -0.1401(4) 0.5535(4) 0.080(3) Uani 1 1 d . . . H36 H 0.6637 -0.1821 0.5555 0.096 Uiso 1 1 calc R . . C37 C 0.7360(4) -0.1285(4) 0.5678(3) 0.064(2) Uani 1 1 d . . . H37 H 0.7605 -0.1624 0.5781 0.077 Uiso 1 1 calc R . . C38 C 0.7552(4) -0.0663(4) 0.5668(3) 0.055(2) Uani 1 1 d . . . H38 H 0.7932 -0.0576 0.5781 0.066 Uiso 1 1 calc R . . C39 C 0.8676(5) 0.6349(9) 0.6867(6) 0.128(5) Uani 1 1 d . . . C40 C 0.8621(4) 0.8584(6) 0.4733(4) 0.078(3) Uani 1 1 d . . . C41 C 0.5066(7) 0.9807(6) 0.3905(5) 0.1046(10) Uani 1 1 d . . . C42 C 0.8440(7) 0.2500 0.7310(6) 0.082(4) Uani 1 2 d S . . C43 C 0.0082(6) 0.4224(6) 0.7297(4) 0.084(3) Uani 1 1 d . . . C44 C -0.0482(6) 0.4028(6) 0.7459(5) 0.112(5) Uani 1 1 d . . . H44A H -0.0444 0.3796 0.7758 0.168 Uiso 1 1 calc R . . H44B H -0.0661 0.3746 0.7222 0.168 Uiso 1 1 calc R . . H44C H -0.0727 0.4408 0.7505 0.168 Uiso 1 1 calc R . . C45 C 0.0444(12) 0.2500 0.8707(9) 0.136(7) Uiso 1 2 d S . . C46 C -0.0077(12) 0.2500 0.8421(9) 0.151(9) Uiso 1 2 d S . . C47 C 0.4337(10) 0.2500 0.2312(8) 0.127(7) Uiso 1 2 d SD . . C48 C 0.3746(10) 0.2500 0.2452(9) 0.147(8) Uiso 1 2 d SD . . C49 C 0.0108(8) 0.7500 0.5877(7) 0.104(5) Uiso 1 2 d SD . . C50 C 0.0629(8) 0.7500 0.6153(7) 0.115(6) Uiso 1 2 d SD . . N1 N 0.8219(2) 0.0948(2) 0.41792(18) 0.0318(11) Uani 1 1 d . . . N2 N 0.7956(2) 0.0947(2) 0.49858(18) 0.0299(11) Uani 1 1 d . . . N3 N 0.9180(2) 0.0868(2) 0.39394(18) 0.0288(11) Uani 1 1 d . . . N4 N 0.8933(2) 0.0899(2) 0.35006(18) 0.0291(11) Uani 1 1 d . . . N5 N 0.8277(2) 0.0904(3) 0.2765(2) 0.0402(13) Uani 1 1 d . . . N6 N 0.8637(2) 0.0858(3) 0.55868(18) 0.0338(12) Uani 1 1 d . . . N7 N 0.8152(2) 0.0862(2) 0.58608(18) 0.0307(11) Uani 1 1 d . . . N8 N 0.7139(3) 0.0931(3) 0.6224(2) 0.0409(13) Uani 1 1 d . . . N9 N 0.7694(2) 0.1929(3) 0.34568(19) 0.0334(12) Uani 1 1 d . . . N10 N 0.6845(2) 0.1338(3) 0.3457(2) 0.0395(13) Uani 1 1 d . . . N11 N 0.7193(2) 0.0806(3) 0.34424(19) 0.0353(12) Uani 1 1 d . . . N12 N 0.7941(2) -0.0192(3) 0.3460(2) 0.0407(13) Uani 1 1 d . . . N13 N 0.7044(2) 0.1931(2) 0.53919(18) 0.0309(11) Uani 1 1 d . . . N14 N 0.6304(2) 0.1340(3) 0.5036(2) 0.0398(13) Uani 1 1 d . . . N15 N 0.6600(2) 0.0817(3) 0.5209(2) 0.0378(13) Uani 1 1 d . . . N16 N 0.7242(3) -0.0182(3) 0.5511(2) 0.0437(14) Uani 1 1 d . . . N17 N 0.0503(6) 0.4431(6) 0.7204(4) 0.116(4) Uani 1 1 d . . . N18 N 0.0921(11) 0.2500 0.8881(8) 0.166(8) Uiso 1 2 d S . . N19 N 0.4875(11) 0.2500 0.2357(9) 0.177(8) Uiso 1 2 d S . . N20 N -0.0406(6) 0.7500 0.5705(5) 0.089(4) Uiso 1 2 d S . . O1 O 0.9102(4) 0.5274(5) 0.6685(4) 0.141(4) Uani 1 1 d . . . O2 O 0.9476(2) 0.5861(3) 0.7348(3) 0.078(2) Uani 1 1 d . . . O3 O 0.8518(3) 0.5376(4) 0.7375(3) 0.095(2) Uani 1 1 d . . . O4 O 0.9707(2) 0.8721(3) 0.4914(2) 0.0758(19) Uani 1 1 d . . . O5 O 0.9006(4) 0.9519(3) 0.5226(2) 0.091(2) Uani 1 1 d . . . O6 O 0.9258(3) 0.9491(3) 0.4371(2) 0.0786(19) Uani 1 1 d . . . O7 O 0.5410(5) 0.9135(6) 0.4489(4) 0.155(2) Uani 1 1 d . . . O8 O 0.6044(5) 0.9895(7) 0.4146(4) 0.155(2) Uani 1 1 d . . . O9 O 0.5745(5) 0.9001(6) 0.3685(4) 0.155(2) Uani 1 1 d . . . O10 O 0.8899(4) 0.1921(3) 0.6588(3) 0.104(3) Uani 1 1 d . . . O11 O 0.8012(6) 0.2500 0.6496(5) 0.129(5) Uani 1 2 d S . . F1 F 0.8507(4) 0.6762(4) 0.7253(4) 0.136(3) Uani 1 1 d . . . F2 F 0.8182(3) 0.6243(6) 0.6608(3) 0.150(4) Uani 1 1 d . . . F3 F 0.9028(3) 0.6700(4) 0.6611(3) 0.132(3) Uani 1 1 d . . . F4 F 0.8149(2) 0.8891(4) 0.4620(3) 0.116(2) Uani 1 1 d . . . F5 F 0.8754(3) 0.8189(3) 0.4380(3) 0.105(2) Uani 1 1 d . . . F6 F 0.8541(3) 0.8225(3) 0.5101(2) 0.097(2) Uani 1 1 d . . . F7 F 0.5106(5) 1.0203(8) 0.3463(6) 0.249(5) Uani 1 1 d . . . F8 F 0.4535(5) 0.9554(7) 0.3782(6) 0.249(5) Uani 1 1 d . . . F9 F 0.4811(5) 1.0281(8) 0.4223(6) 0.249(5) Uani 1 1 d . . . F10 F 0.8158(4) 0.2004(4) 0.7428(3) 0.138(3) Uani 1 1 d . . . F11 F 0.8971(5) 0.2500 0.7552(4) 0.128(4) Uani 1 2 d S . . S1 S 0.89552(10) 0.56579(12) 0.71145(9) 0.0669(6) Uani 1 1 d . . . S2 S 0.92252(10) 0.91430(10) 0.48198(8) 0.0606(6) Uani 1 1 d . . . S3 S 0.55742(18) 0.94261(16) 0.40694(13) 0.1046(10) Uani 1 1 d . . . S4 S 0.85890(15) 0.2500 0.66544(13) 0.0625(8) Uani 1 2 d S . . Cu1 Cu 0.80844(3) 0.09221(4) 0.34703(3) 0.0304(2) Uani 1 1 d . . . Cu2 Cu 0.73975(3) 0.09523(4) 0.55393(3) 0.0341(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(3) 0.044(4) 0.026(3) 0.002(3) -0.002(2) -0.006(3) C2 0.023(3) 0.029(3) 0.030(3) 0.002(2) -0.002(2) -0.002(2) C3 0.027(3) 0.033(3) 0.029(3) 0.001(3) -0.001(2) 0.002(2) C4 0.032(3) 0.030(3) 0.026(3) 0.003(2) -0.004(2) 0.001(2) C5 0.017(3) 0.076(5) 0.035(4) 0.004(3) 0.004(3) 0.002(3) C6 0.031(3) 0.042(4) 0.027(3) 0.000(3) 0.004(3) 0.003(3) C7 0.031(3) 0.058(4) 0.034(4) -0.005(3) 0.007(3) 0.006(3) C8 0.040(4) 0.096(6) 0.033(4) 0.001(4) 0.006(3) 0.021(4) C9 0.057(5) 0.163(11) 0.032(5) 0.008(6) 0.004(4) 0.018(6) C10 0.058(5) 0.152(10) 0.034(4) 0.013(5) -0.009(4) 0.041(6) C11 0.037(4) 0.096(6) 0.031(4) 0.010(4) -0.007(3) 0.007(4) C12 0.032(3) 0.069(5) 0.023(3) 0.001(3) -0.003(3) 0.006(3) C13 0.044(4) 0.048(4) 0.028(4) 0.005(3) 0.002(3) 0.001(3) C14 0.046(4) 0.057(4) 0.025(3) 0.008(3) 0.006(3) 0.000(3) C15 0.072(6) 0.094(6) 0.028(4) 0.015(4) 0.006(4) 0.010(5) C16 0.077(6) 0.111(8) 0.034(5) 0.015(5) 0.022(4) 0.002(5) C17 0.062(6) 0.140(10) 0.048(6) 0.004(6) 0.027(5) 0.011(6) C18 0.043(4) 0.100(7) 0.039(4) 0.001(4) 0.008(3) 0.009(4) C19 0.020(4) 0.039(5) 0.043(6) 0.000 -0.001(4) 0.000 C20 0.022(3) 0.046(4) 0.024(3) 0.001(3) 0.000(2) -0.001(3) C21 0.012(4) 0.054(6) 0.048(6) 0.000 -0.002(4) 0.000 C22 0.028(3) 0.063(5) 0.071(6) 0.007(4) 0.007(3) -0.018(3) C23 0.029(3) 0.038(4) 0.055(5) 0.001(3) -0.010(3) -0.005(3) C24 0.050(4) 0.044(4) 0.054(5) -0.006(3) -0.010(4) -0.007(3) C25 0.060(6) 0.037(5) 0.156(12) -0.006(5) -0.014(6) -0.002(4) C26 0.087(8) 0.046(5) 0.135(11) -0.013(6) -0.016(7) -0.005(5) C27 0.089(7) 0.050(5) 0.101(8) -0.008(5) -0.022(6) 0.009(5) C28 0.044(4) 0.049(4) 0.046(4) 0.000(3) -0.013(3) 0.009(3) C29 0.023(4) 0.036(5) 0.040(5) 0.000 -0.007(4) 0.000 C30 0.026(3) 0.050(4) 0.023(3) -0.003(3) -0.001(2) -0.007(3) C31 0.027(4) 0.059(6) 0.027(5) 0.000 -0.003(4) 0.000 C32 0.051(4) 0.063(5) 0.051(5) -0.001(4) -0.014(4) -0.014(4) C33 0.040(4) 0.049(4) 0.046(4) -0.004(3) -0.003(3) -0.005(3) C34 0.057(5) 0.049(4) 0.042(4) -0.006(3) 0.005(4) -0.006(4) C35 0.078(6) 0.050(5) 0.098(8) 0.002(5) -0.027(6) -0.017(5) C36 0.091(7) 0.043(5) 0.107(9) 0.000(5) -0.017(6) -0.006(5) C37 0.073(6) 0.053(5) 0.068(6) -0.001(4) 0.010(5) 0.004(4) C38 0.057(5) 0.052(5) 0.057(5) 0.000(4) 0.010(4) -0.001(4) C39 0.059(7) 0.177(15) 0.148(14) 0.025(12) 0.010(8) -0.033(9) C40 0.052(5) 0.107(8) 0.073(7) 0.026(6) 0.011(5) 0.026(5) C41 0.142(3) 0.084(2) 0.088(2) 0.0151(16) 0.025(2) 0.0063(19) C42 0.084(10) 0.078(10) 0.083(11) 0.000 -0.010(9) 0.000 C43 0.093(8) 0.093(8) 0.068(7) 0.018(6) 0.001(6) -0.020(7) C44 0.123(11) 0.095(9) 0.118(11) 0.028(7) -0.012(9) -0.028(8) N1 0.021(2) 0.045(3) 0.029(3) 0.000(2) -0.003(2) 0.003(2) N2 0.024(2) 0.041(3) 0.025(3) 0.001(2) 0.0013(19) -0.004(2) N3 0.021(2) 0.037(3) 0.028(3) 0.009(2) 0.0025(19) 0.002(2) N4 0.024(2) 0.034(3) 0.029(3) 0.001(2) -0.001(2) 0.004(2) N5 0.034(3) 0.054(4) 0.032(3) 0.005(3) 0.006(2) 0.004(2) N6 0.027(3) 0.051(3) 0.024(3) -0.003(2) -0.004(2) 0.004(2) N7 0.032(3) 0.037(3) 0.024(3) 0.004(2) 0.003(2) -0.003(2) N8 0.042(3) 0.050(3) 0.031(3) 0.009(3) 0.008(3) -0.003(3) N9 0.019(2) 0.045(3) 0.036(3) 0.001(2) -0.001(2) -0.002(2) N10 0.023(3) 0.050(3) 0.046(3) 0.002(3) 0.000(2) -0.003(2) N11 0.034(3) 0.041(3) 0.030(3) 0.005(2) 0.000(2) -0.007(2) N12 0.035(3) 0.050(3) 0.037(3) -0.004(3) -0.013(2) -0.006(3) N13 0.025(2) 0.041(3) 0.026(3) 0.000(2) 0.006(2) 0.006(2) N14 0.033(3) 0.046(3) 0.041(3) -0.004(3) -0.006(2) -0.009(2) N15 0.039(3) 0.039(3) 0.035(3) -0.003(2) 0.005(2) -0.010(2) N16 0.042(3) 0.046(4) 0.043(4) -0.001(3) 0.002(3) -0.005(3) N17 0.116(9) 0.112(8) 0.119(10) 0.016(7) 0.002(8) 0.003(7) O1 0.130(7) 0.136(7) 0.156(9) -0.086(7) 0.087(7) -0.055(6) O2 0.037(3) 0.083(4) 0.115(6) 0.000(4) 0.005(3) 0.004(3) O3 0.058(4) 0.120(6) 0.107(6) 0.020(5) 0.028(4) -0.024(4) O4 0.039(3) 0.099(5) 0.089(5) 0.044(4) -0.007(3) -0.011(3) O5 0.131(6) 0.087(5) 0.054(4) -0.024(4) -0.003(4) 0.006(4) O6 0.080(4) 0.090(5) 0.065(4) 0.035(4) -0.013(3) -0.008(4) O7 0.123(5) 0.203(7) 0.137(6) 0.024(5) 0.022(4) -0.001(4) O8 0.123(5) 0.203(7) 0.137(6) 0.024(5) 0.022(4) -0.001(4) O9 0.123(5) 0.203(7) 0.137(6) 0.024(5) 0.022(4) -0.001(4) O10 0.129(7) 0.062(4) 0.121(7) -0.005(4) 0.047(5) 0.009(4) O11 0.136(12) 0.125(10) 0.127(12) 0.000 -0.037(9) 0.000 F1 0.127(6) 0.105(5) 0.175(9) 0.014(5) 0.027(6) 0.033(5) F2 0.072(4) 0.273(11) 0.105(6) 0.053(7) -0.029(4) -0.010(6) F3 0.121(6) 0.140(6) 0.136(7) 0.070(5) 0.036(5) -0.006(5) F4 0.056(3) 0.196(7) 0.095(5) 0.025(5) -0.009(3) 0.029(4) F5 0.120(5) 0.092(4) 0.103(5) -0.037(4) -0.021(4) -0.011(4) F6 0.076(4) 0.110(5) 0.104(5) 0.035(4) -0.007(3) -0.031(3) F7 0.123(5) 0.295(10) 0.329(11) 0.117(9) -0.073(6) -0.042(5) F8 0.123(5) 0.295(10) 0.329(11) 0.117(9) -0.073(6) -0.042(5) F9 0.123(5) 0.295(10) 0.329(11) 0.117(9) -0.073(6) -0.042(5) F10 0.162(7) 0.120(6) 0.133(7) 0.015(5) 0.050(6) -0.055(5) F11 0.162(11) 0.135(8) 0.087(7) 0.000 -0.040(7) 0.000 S1 0.0605(13) 0.0734(15) 0.0668(15) -0.0151(12) 0.0133(11) -0.0259(11) S2 0.0676(13) 0.0529(12) 0.0614(14) 0.0149(10) -0.0258(11) -0.0157(10) S3 0.142(3) 0.084(2) 0.088(2) 0.0151(16) 0.025(2) 0.0063(19) S4 0.0638(19) 0.0543(18) 0.070(2) 0.000 -0.0030(16) 0.000 Cu1 0.0230(4) 0.0441(5) 0.0239(4) 0.0009(3) 0.0007(3) 0.0000(3) Cu2 0.0298(4) 0.0469(5) 0.0257(4) 0.0025(3) 0.0032(3) -0.0019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.317(8) . ? C1 N2 1.330(8) . ? C1 H1 0.9500 . ? C2 C3 1.363(8) . ? C2 N3 1.370(7) . ? C2 N1 1.401(7) . ? C3 C4 1.375(8) . ? C3 H3 0.9500 . ? C4 N6 1.372(8) . ? C4 N2 1.373(7) . ? C5 N3 1.458(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N4 1.281(8) . ? C6 C7 1.458(9) . ? C6 H6 0.9500 . ? C7 C8 1.361(10) . ? C7 N5 1.370(8) . ? C8 C9 1.380(11) . ? C8 H8 0.9500 . ? C9 C10 1.429(13) . ? C9 H9 0.9500 . ? C10 C11 1.381(12) . ? C10 H10 0.9500 . ? C11 N5 1.326(9) . ? C11 H11 0.9500 . ? C12 N6 1.459(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N7 1.275(8) . ? C13 C14 1.452(10) . ? C13 H13 0.9500 . ? C14 N8 1.347(9) . ? C14 C15 1.405(10) . ? C15 C16 1.432(12) . ? C15 H15 0.9500 . ? C16 C17 1.349(14) . ? C16 H16 0.9500 . ? C17 C18 1.397(12) . ? C17 H17 0.9500 . ? C18 N8 1.337(9) . ? C18 H18 0.9500 . ? C19 N9 1.327(6) . ? C19 N9 1.327(6) 8_565 ? C19 H19 0.9500 . ? C20 N9 1.328(7) . ? C20 N10 1.377(8) . ? C20 C21 1.397(7) . ? C21 C20 1.397(7) 8_565 ? C21 H21 0.9500 . ? C22 N10 1.471(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 N11 1.264(8) . ? C23 C24 1.448(10) . ? C23 H23 0.9500 . ? C24 N12 1.329(9) . ? C24 C25 1.384(11) . ? C25 C26 1.381(13) . ? C25 H25 0.9500 . ? C26 C27 1.351(14) . ? C26 H26 0.9500 . ? C27 C28 1.407(13) . ? C27 H27 0.9500 . ? C28 N12 1.296(9) . ? C28 H28 0.9500 . ? C29 N13 1.325(6) . ? C29 N13 1.325(6) 8_565 ? C29 H29 0.9500 . ? C30 N13 1.363(8) . ? C30 C31 1.375(8) . ? C30 N14 1.394(8) . ? C31 C30 1.375(8) 8_565 ? C31 H31 0.9500 . ? C32 N14 1.450(9) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 N15 1.300(9) . ? C33 C34 1.477(11) . ? C33 H33 0.9500 . ? C34 N16 1.341(10) . ? C34 C35 1.346(11) . ? C35 C36 1.367(13) . ? C35 H35 0.9500 . ? C36 C37 1.378(13) . ? C36 H36 0.9500 . ? C37 C38 1.367(12) . ? C37 H37 0.9500 . ? C38 N16 1.307(10) . ? C38 H38 0.9500 . ? C39 F3 1.310(14) . ? C39 F2 1.370(15) . ? C39 F1 1.443(19) . ? C39 S1 1.725(17) . ? C40 F6 1.295(11) . ? C40 F4 1.299(10) . ? C40 F5 1.331(12) . ? C40 S2 1.829(12) . ? C41 F8 1.375(17) . ? C41 F9 1.46(2) . ? C41 S3 1.488(15) . ? C41 F7 1.502(17) . ? C42 F10 1.264(11) . ? C42 F10 1.264(11) 8_565 ? C42 F11 1.401(18) . ? C42 S4 1.886(17) . ? C43 N17 1.092(14) . ? C43 C44 1.436(17) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 N18 1.20(3) . ? C45 C46 1.45(3) . ? C47 N19 1.25(3) . ? C47 C48 1.418(17) . ? C49 N20 1.279(19) . ? C49 C50 1.430(10) . ? N1 Cu1 2.030(5) . ? N2 Cu2 2.027(5) . ? N3 N4 1.366(7) . ? N4 Cu1 1.956(5) . ? N5 Cu1 2.045(6) . ? N6 N7 1.360(7) . ? N7 Cu2 1.969(5) . ? N8 Cu2 2.027(6) . ? N9 Cu1 2.280(5) . ? N10 N11 1.369(8) . ? N11 Cu1 2.067(5) . ? N12 Cu1 2.342(6) . ? N13 Cu2 2.232(5) . ? N14 N15 1.373(8) . ? N15 Cu2 2.080(6) . ? N16 Cu2 2.389(6) . ? O1 S1 1.492(8) . ? O2 S1 1.432(7) . ? O3 S1 1.379(6) . ? O4 S2 1.440(6) . ? O5 S2 1.479(7) . ? O6 S2 1.463(6) . ? O7 S3 1.387(11) . ? O8 S3 1.473(13) . ? O9 S3 1.456(13) . ? O10 S4 1.412(7) . ? O11 S4 1.401(14) . ? S4 O10 1.412(7) 8_565 ? 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 N1 C1 N2 126.2(6) . . ? N1 C1 H1 116.9 . . ? N2 C1 H1 116.9 . . ? C3 C2 N3 124.7(5) . . ? C3 C2 N1 121.8(5) . . ? N3 C2 N1 113.5(5) . . ? C2 C3 C4 117.3(5) . . ? C2 C3 H3 121.3 . . ? C4 C3 H3 121.3 . . ? N6 C4 N2 115.3(5) . . ? N6 C4 C3 122.9(5) . . ? N2 C4 C3 121.8(5) . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 C7 114.8(6) . . ? N4 C6 H6 122.6 . . ? C7 C6 H6 122.6 . . ? C8 C7 N5 122.0(7) . . ? C8 C7 C6 123.3(6) . . ? N5 C7 C6 114.7(6) . . ? C7 C8 C9 120.4(7) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C8 C9 C10 117.4(8) . . ? C8 C9 H9 121.3 . . ? C10 C9 H9 121.3 . . ? C11 C10 C9 118.6(8) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? N5 C11 C10 122.7(7) . . ? N5 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? N6 C12 H12A 109.5 . . ? N6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N7 C13 C14 114.9(6) . . ? N7 C13 H13 122.5 . . ? C14 C13 H13 122.5 . . ? N8 C14 C15 123.2(7) . . ? N8 C14 C13 114.6(6) . . ? C15 C14 C13 122.2(7) . . ? C14 C15 C16 115.9(8) . . ? C14 C15 H15 122.1 . . ? C16 C15 H15 122.1 . . ? C17 C16 C15 120.1(8) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 119.9(8) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? N8 C18 C17 121.5(8) . . ? N8 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? N9 C19 N9 127.1(8) . 8_565 ? N9 C19 H19 116.5 . . ? N9 C19 H19 116.5 8_565 . ? N9 C20 N10 117.1(6) . . ? N9 C20 C21 121.5(6) . . ? N10 C20 C21 121.3(5) . . ? C20 C21 C20 116.8(7) . 8_565 ? C20 C21 H21 121.6 . . ? C20 C21 H21 121.6 8_565 . ? N10 C22 H22A 109.5 . . ? N10 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N10 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N11 C23 C24 120.2(6) . . ? N11 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? N12 C24 C25 122.2(7) . . ? N12 C24 C23 117.4(6) . . ? C25 C24 C23 120.3(7) . . ? C26 C25 C24 118.0(9) . . ? C26 C25 H25 121.0 . . ? C24 C25 H25 121.0 . . ? C27 C26 C25 119.0(9) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C26 C27 C28 119.4(9) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? N12 C28 C27 121.3(7) . . ? N12 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? N13 C29 N13 126.7(8) . 8_565 ? N13 C29 H29 116.7 . . ? N13 C29 H29 116.7 8_565 . ? N13 C30 C31 123.0(6) . . ? N13 C30 N14 115.3(6) . . ? C31 C30 N14 121.7(6) . . ? C30 C31 C30 115.5(8) . 8_565 ? C30 C31 H31 122.2 . . ? C30 C31 H31 122.2 8_565 . ? N14 C32 H32A 109.5 . . ? N14 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N14 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N15 C33 C34 118.1(7) . . ? N15 C33 H33 120.9 . . ? C34 C33 H33 120.9 . . ? N16 C34 C35 122.2(8) . . ? N16 C34 C33 116.5(6) . . ? C35 C34 C33 121.3(8) . . ? C34 C35 C36 119.6(9) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C35 C36 C37 118.8(9) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? C38 C37 C36 117.7(9) . . ? C38 C37 H37 121.2 . . ? C36 C37 H37 121.2 . . ? N16 C38 C37 123.7(8) . . ? N16 C38 H38 118.2 . . ? C37 C38 H38 118.2 . . ? F3 C39 F2 108.0(13) . . ? F3 C39 F1 104.7(13) . . ? F2 C39 F1 106.1(12) . . ? F3 C39 S1 117.3(10) . . ? F2 C39 S1 113.1(12) . . ? F1 C39 S1 106.8(11) . . ? F6 C40 F4 111.3(8) . . ? F6 C40 F5 106.3(9) . . ? F4 C40 F5 108.2(9) . . ? F6 C40 S2 111.5(8) . . ? F4 C40 S2 110.9(8) . . ? F5 C40 S2 108.5(7) . . ? F8 C41 F9 93.4(13) . . ? F8 C41 S3 125.1(11) . . ? F9 C41 S3 119.0(11) . . ? F8 C41 F7 93.1(12) . . ? F9 C41 F7 99.6(12) . . ? S3 C41 F7 120.3(11) . . ? F10 C42 F10 109.4(15) . 8_565 ? F10 C42 F11 108.6(10) . . ? F10 C42 F11 108.6(10) 8_565 . ? F10 C42 S4 110.7(9) . . ? F10 C42 S4 110.7(9) 8_565 . ? F11 C42 S4 108.8(11) . . ? N17 C43 C44 172.3(16) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N18 C45 C46 170(3) . . ? N19 C47 C48 158(3) . . ? N20 C49 C50 169(2) . . ? C1 N1 C2 116.0(5) . . ? C1 N1 Cu1 129.4(4) . . ? C2 N1 Cu1 114.5(4) . . ? C1 N2 C4 116.8(5) . . ? C1 N2 Cu2 128.7(4) . . ? C4 N2 Cu2 114.5(4) . . ? N4 N3 C2 116.0(4) . . ? N4 N3 C5 119.3(5) . . ? C2 N3 C5 124.7(5) . . ? C6 N4 N3 124.1(5) . . ? C6 N4 Cu1 118.5(4) . . ? N3 N4 Cu1 117.1(4) . . ? C11 N5 C7 118.7(6) . . ? C11 N5 Cu1 129.4(5) . . ? C7 N5 Cu1 111.9(4) . . ? N7 N6 C4 114.5(5) . . ? N7 N6 C12 119.8(5) . . ? C4 N6 C12 125.4(5) . . ? C13 N7 N6 124.7(6) . . ? C13 N7 Cu2 117.6(5) . . ? N6 N7 Cu2 117.5(4) . . ? C18 N8 C14 119.1(6) . . ? C18 N8 Cu2 128.1(5) . . ? C14 N8 Cu2 112.9(4) . . ? C19 N9 C20 116.5(6) . . ? C19 N9 Cu1 130.3(4) . . ? C20 N9 Cu1 113.2(4) . . ? N11 N10 C20 117.0(5) . . ? N11 N10 C22 119.7(5) . . ? C20 N10 C22 123.2(6) . . ? C23 N11 N10 122.3(5) . . ? C23 N11 Cu1 118.7(5) . . ? N10 N11 Cu1 119.0(4) . . ? C28 N12 C24 119.9(6) . . ? C28 N12 Cu1 131.6(5) . . ? C24 N12 Cu1 108.5(5) . . ? C29 N13 C30 115.8(6) . . ? C29 N13 Cu2 129.2(4) . . ? C30 N13 Cu2 115.0(4) . . ? N15 N14 C30 116.3(5) . . ? N15 N14 C32 122.2(6) . . ? C30 N14 C32 120.8(6) . . ? C33 N15 N14 119.5(6) . . ? C33 N15 Cu2 121.0(5) . . ? N14 N15 Cu2 119.3(4) . . ? C38 N16 C34 118.0(7) . . ? C38 N16 Cu2 131.5(5) . . ? C34 N16 Cu2 109.8(5) . . ? O3 S1 O2 119.4(5) . . ? O3 S1 O1 111.9(5) . . ? O2 S1 O1 110.0(5) . . ? O3 S1 C39 107.4(5) . . ? O2 S1 C39 104.7(6) . . ? O1 S1 C39 101.6(8) . . ? O4 S2 O6 115.0(4) . . ? O4 S2 O5 116.3(4) . . ? O6 S2 O5 115.4(4) . . ? O4 S2 C40 102.9(4) . . ? O6 S2 C40 103.7(4) . . ? O5 S2 C40 100.4(5) . . ? O7 S3 O9 116.7(7) . . ? O7 S3 O8 111.3(7) . . ? O9 S3 O8 108.3(7) . . ? O7 S3 C41 106.6(7) . . ? O9 S3 C41 107.6(8) . . ? O8 S3 C41 105.8(7) . . ? O11 S4 O10 115.8(5) . 8_565 ? O11 S4 O10 115.8(5) . . ? O10 S4 O10 117.1(7) 8_565 . ? O11 S4 C42 98.2(8) . . ? O10 S4 C42 102.9(4) 8_565 . ? O10 S4 C42 102.9(4) . . ? N4 Cu1 N1 78.7(2) . . ? N4 Cu1 N5 79.9(2) . . ? N1 Cu1 N5 158.6(2) . . ? N4 Cu1 N11 171.8(2) . . ? N1 Cu1 N11 101.1(2) . . ? N5 Cu1 N11 100.1(2) . . ? N4 Cu1 N9 114.70(19) . . ? N1 Cu1 N9 93.0(2) . . ? N5 Cu1 N9 94.9(2) . . ? N11 Cu1 N9 73.47(19) . . ? N4 Cu1 N12 96.7(2) . . ? N1 Cu1 N12 93.4(2) . . ? N5 Cu1 N12 90.1(2) . . ? N11 Cu1 N12 75.1(2) . . ? N9 Cu1 N12 148.58(18) . . ? N7 Cu2 N8 79.4(2) . . ? N7 Cu2 N2 78.3(2) . . ? N8 Cu2 N2 157.6(2) . . ? N7 Cu2 N15 166.7(2) . . ? N8 Cu2 N15 99.6(2) . . ? N2 Cu2 N15 102.3(2) . . ? N7 Cu2 N13 119.7(2) . . ? N8 Cu2 N13 95.3(2) . . ? N2 Cu2 N13 95.31(19) . . ? N15 Cu2 N13 73.6(2) . . ? N7 Cu2 N16 93.1(2) . . ? N8 Cu2 N16 88.1(2) . . ? N2 Cu2 N16 93.6(2) . . ? N15 Cu2 N16 73.6(2) . . ? N13 Cu2 N16 147.2(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 C2 C3 C4 -176.9(5) . . . . ? N1 C2 C3 C4 2.9(8) . . . . ? C2 C3 C4 N6 176.4(5) . . . . ? C2 C3 C4 N2 -3.1(8) . . . . ? N4 C6 C7 C8 177.3(7) . . . . ? N4 C6 C7 N5 -2.3(9) . . . . ? N5 C7 C8 C9 1.6(13) . . . . ? C6 C7 C8 C9 -177.9(8) . . . . ? C7 C8 C9 C10 -4.9(15) . . . . ? C8 C9 C10 C11 6.2(16) . . . . ? C9 C10 C11 N5 -4.4(15) . . . . ? N7 C13 C14 N8 0.3(9) . . . . ? N7 C13 C14 C15 -178.9(7) . . . . ? N8 C14 C15 C16 -0.8(13) . . . . ? C13 C14 C15 C16 178.2(8) . . . . ? C14 C15 C16 C17 1.2(15) . . . . ? C15 C16 C17 C18 -4.0(17) . . . . ? C16 C17 C18 N8 6.6(16) . . . . ? N9 C20 C21 C20 -0.8(13) . . . 8_565 ? N10 C20 C21 C20 179.6(5) . . . 8_565 ? N11 C23 C24 N12 1.6(11) . . . . ? N11 C23 C24 C25 179.5(9) . . . . ? N12 C24 C25 C26 -2.7(17) . . . . ? C23 C24 C25 C26 179.5(10) . . . . ? C24 C25 C26 C27 4.4(19) . . . . ? C25 C26 C27 C28 -3.1(18) . . . . ? C26 C27 C28 N12 -0.2(15) . . . . ? N13 C30 C31 C30 -4.0(12) . . . 8_565 ? N14 C30 C31 C30 176.2(5) . . . 8_565 ? N15 C33 C34 N16 -1.8(10) . . . . ? N15 C33 C34 C35 176.7(8) . . . . ? N16 C34 C35 C36 0.0(16) . . . . ? C33 C34 C35 C36 -178.5(9) . . . . ? C34 C35 C36 C37 -2.3(17) . . . . ? C35 C36 C37 C38 3.8(15) . . . . ? C36 C37 C38 N16 -3.1(14) . . . . ? N2 C1 N1 C2 -0.3(9) . . . . ? N2 C1 N1 Cu1 175.8(4) . . . . ? C3 C2 N1 C1 -1.3(8) . . . . ? N3 C2 N1 C1 178.5(5) . . . . ? C3 C2 N1 Cu1 -178.0(4) . . . . ? N3 C2 N1 Cu1 1.8(6) . . . . ? N1 C1 N2 C4 0.1(9) . . . . ? N1 C1 N2 Cu2 -178.3(5) . . . . ? N6 C4 N2 C1 -177.9(5) . . . . ? C3 C4 N2 C1 1.6(8) . . . . ? N6 C4 N2 Cu2 0.7(6) . . . . ? C3 C4 N2 Cu2 -179.7(4) . . . . ? C3 C2 N3 N4 -178.6(5) . . . . ? N1 C2 N3 N4 1.6(7) . . . . ? C3 C2 N3 C5 3.6(9) . . . . ? N1 C2 N3 C5 -176.1(6) . . . . ? C7 C6 N4 N3 177.3(5) . . . . ? C7 C6 N4 Cu1 3.5(7) . . . . ? C2 N3 N4 C6 -178.3(5) . . . . ? C5 N3 N4 C6 -0.4(8) . . . . ? C2 N3 N4 Cu1 -4.5(6) . . . . ? C5 N3 N4 Cu1 173.4(4) . . . . ? C10 C11 N5 C7 1.0(12) . . . . ? C10 C11 N5 Cu1 -179.0(7) . . . . ? C8 C7 N5 C11 0.5(11) . . . . ? C6 C7 N5 C11 -179.9(6) . . . . ? C8 C7 N5 Cu1 -179.5(6) . . . . ? C6 C7 N5 Cu1 0.1(7) . . . . ? N2 C4 N6 N7 0.7(7) . . . . ? C3 C4 N6 N7 -178.9(5) . . . . ? N2 C4 N6 C12 174.2(6) . . . . ? C3 C4 N6 C12 -5.4(10) . . . . ? C14 C13 N7 N6 179.1(6) . . . . ? C14 C13 N7 Cu2 -6.1(8) . . . . ? C4 N6 N7 C13 173.0(6) . . . . ? C12 N6 N7 C13 -0.9(9) . . . . ? C4 N6 N7 Cu2 -1.8(6) . . . . ? C12 N6 N7 Cu2 -175.7(5) . . . . ? C17 C18 N8 C14 -6.1(13) . . . . ? C17 C18 N8 Cu2 172.5(7) . . . . ? C15 C14 N8 C18 3.3(12) . . . . ? C13 C14 N8 C18 -175.8(7) . . . . ? C15 C14 N8 Cu2 -175.6(7) . . . . ? C13 C14 N8 Cu2 5.3(8) . . . . ? N9 C19 N9 C20 -1.9(14) 8_565 . . . ? N9 C19 N9 Cu1 -179.6(5) 8_565 . . . ? N10 C20 N9 C19 -179.1(7) . . . . ? C21 C20 N9 C19 1.3(10) . . . . ? N10 C20 N9 Cu1 -1.1(7) . . . . ? C21 C20 N9 Cu1 179.4(6) . . . . ? N9 C20 N10 N11 -2.0(8) . . . . ? C21 C20 N10 N11 177.6(7) . . . . ? N9 C20 N10 C22 178.3(6) . . . . ? C21 C20 N10 C22 -2.2(10) . . . . ? C24 C23 N11 N10 -177.9(6) . . . . ? C24 C23 N11 Cu1 2.7(9) . . . . ? C20 N10 N11 C23 -175.0(6) . . . . ? C22 N10 N11 C23 4.8(10) . . . . ? C20 N10 N11 Cu1 4.4(7) . . . . ? C22 N10 N11 Cu1 -175.8(5) . . . . ? C27 C28 N12 C24 2.0(12) . . . . ? C27 C28 N12 Cu1 -176.0(6) . . . . ? C25 C24 N12 C28 -0.5(13) . . . . ? C23 C24 N12 C28 177.3(7) . . . . ? C25 C24 N12 Cu1 177.9(8) . . . . ? C23 C24 N12 Cu1 -4.2(8) . . . . ? N13 C29 N13 C30 0.2(13) 8_565 . . . ? N13 C29 N13 Cu2 177.6(5) 8_565 . . . ? C31 C30 N13 C29 2.0(10) . . . . ? N14 C30 N13 C29 -178.1(6) . . . . ? C31 C30 N13 Cu2 -175.7(6) . . . . ? N14 C30 N13 Cu2 4.1(7) . . . . ? N13 C30 N14 N15 0.9(8) . . . . ? C31 C30 N14 N15 -179.3(7) . . . . ? N13 C30 N14 C32 172.2(6) . . . . ? C31 C30 N14 C32 -8.0(10) . . . . ? C34 C33 N15 N14 177.4(6) . . . . ? C34 C33 N15 Cu2 -6.4(9) . . . . ? C30 N14 N15 C33 170.2(6) . . . . ? C32 N14 N15 C33 -0.9(10) . . . . ? C30 N14 N15 Cu2 -6.0(7) . . . . ? C32 N14 N15 Cu2 -177.2(5) . . . . ? C37 C38 N16 C34 0.8(12) . . . . ? C37 C38 N16 Cu2 170.7(6) . . . . ? C35 C34 N16 C38 0.8(12) . . . . ? C33 C34 N16 C38 179.4(7) . . . . ? C35 C34 N16 Cu2 -171.1(8) . . . . ? C33 C34 N16 Cu2 7.4(8) . . . . ? F3 C39 S1 O3 178.5(12) . . . . ? F2 C39 S1 O3 -54.8(13) . . . . ? F1 C39 S1 O3 61.5(9) . . . . ? F3 C39 S1 O2 50.7(15) . . . . ? F2 C39 S1 O2 177.4(10) . . . . ? F1 C39 S1 O2 -66.3(8) . . . . ? F3 C39 S1 O1 -63.9(14) . . . . ? F2 C39 S1 O1 62.8(12) . . . . ? F1 C39 S1 O1 179.1(8) . . . . ? F6 C40 S2 O4 58.5(8) . . . . ? F4 C40 S2 O4 -176.9(7) . . . . ? F5 C40 S2 O4 -58.3(7) . . . . ? F6 C40 S2 O6 178.7(7) . . . . ? F4 C40 S2 O6 -56.7(8) . . . . ? F5 C40 S2 O6 61.9(7) . . . . ? F6 C40 S2 O5 -61.7(8) . . . . ? F4 C40 S2 O5 62.9(8) . . . . ? F5 C40 S2 O5 -178.5(7) . . . . ? F8 C41 S3 O7 -63.0(16) . . . . ? F9 C41 S3 O7 55.0(13) . . . . ? F7 C41 S3 O7 178.0(12) . . . . ? F8 C41 S3 O9 62.8(16) . . . . ? F9 C41 S3 O9 -179.1(11) . . . . ? F7 C41 S3 O9 -56.2(14) . . . . ? F8 C41 S3 O8 178.4(14) . . . . ? F9 C41 S3 O8 -63.5(12) . . . . ? F7 C41 S3 O8 59.4(14) . . . . ? F10 C42 S4 O11 60.8(10) . . . . ? F10 C42 S4 O11 -60.8(10) 8_565 . . . ? F11 C42 S4 O11 180.000(3) . . . . ? F10 C42 S4 O10 179.8(10) . . . 8_565 ? F10 C42 S4 O10 58.2(11) 8_565 . . 8_565 ? F11 C42 S4 O10 -61.0(4) . . . 8_565 ? F10 C42 S4 O10 -58.2(11) . . . . ? F10 C42 S4 O10 -179.8(10) 8_565 . . . ? F11 C42 S4 O10 61.0(4) . . . . ? C6 N4 Cu1 N1 178.3(5) . . . . ? N3 N4 Cu1 N1 4.1(4) . . . . ? C6 N4 Cu1 N5 -2.7(5) . . . . ? N3 N4 Cu1 N5 -176.9(4) . . . . ? C6 N4 Cu1 N9 -93.5(5) . . . . ? N3 N4 Cu1 N9 92.3(4) . . . . ? C6 N4 Cu1 N12 86.2(5) . . . . ? N3 N4 Cu1 N12 -88.0(4) . . . . ? C1 N1 Cu1 N4 -179.3(6) . . . . ? C2 N1 Cu1 N4 -3.2(4) . . . . ? C1 N1 Cu1 N5 177.8(6) . . . . ? C2 N1 Cu1 N5 -6.0(8) . . . . ? C1 N1 Cu1 N11 -7.7(6) . . . . ? C2 N1 Cu1 N11 168.5(4) . . . . ? C1 N1 Cu1 N9 66.1(6) . . . . ? C2 N1 Cu1 N9 -117.8(4) . . . . ? C1 N1 Cu1 N12 -83.2(6) . . . . ? C2 N1 Cu1 N12 93.0(4) . . . . ? C11 N5 Cu1 N4 -178.7(7) . . . . ? C7 N5 Cu1 N4 1.3(5) . . . . ? C11 N5 Cu1 N1 -175.9(6) . . . . ? C7 N5 Cu1 N1 4.1(9) . . . . ? C11 N5 Cu1 N11 9.6(7) . . . . ? C7 N5 Cu1 N11 -170.4(5) . . . . ? C11 N5 Cu1 N9 -64.5(7) . . . . ? C7 N5 Cu1 N9 115.5(5) . . . . ? C11 N5 Cu1 N12 84.4(7) . . . . ? C7 N5 Cu1 N12 -95.6(5) . . . . ? C23 N11 Cu1 N1 -94.3(5) . . . . ? N10 N11 Cu1 N1 86.3(5) . . . . ? C23 N11 Cu1 N5 83.7(6) . . . . ? N10 N11 Cu1 N5 -95.7(5) . . . . ? C23 N11 Cu1 N9 175.9(6) . . . . ? N10 N11 Cu1 N9 -3.6(4) . . . . ? C23 N11 Cu1 N12 -3.6(5) . . . . ? N10 N11 Cu1 N12 176.9(5) . . . . ? C19 N9 Cu1 N4 0.5(7) . . . . ? C20 N9 Cu1 N4 -177.2(4) . . . . ? C19 N9 Cu1 N1 79.5(7) . . . . ? C20 N9 Cu1 N1 -98.3(4) . . . . ? C19 N9 Cu1 N5 -80.7(7) . . . . ? C20 N9 Cu1 N5 101.6(5) . . . . ? C19 N9 Cu1 N11 -179.8(7) . . . . ? C20 N9 Cu1 N11 2.4(4) . . . . ? C19 N9 Cu1 N12 -178.9(6) . . . . ? C20 N9 Cu1 N12 3.3(7) . . . . ? C28 N12 Cu1 N4 2.0(7) . . . . ? C24 N12 Cu1 N4 -176.2(5) . . . . ? C28 N12 Cu1 N1 -77.1(7) . . . . ? C24 N12 Cu1 N1 104.7(5) . . . . ? C28 N12 Cu1 N5 81.8(7) . . . . ? C24 N12 Cu1 N5 -96.4(5) . . . . ? C28 N12 Cu1 N11 -177.7(7) . . . . ? C24 N12 Cu1 N11 4.1(5) . . . . ? C28 N12 Cu1 N9 -178.6(6) . . . . ? C24 N12 Cu1 N9 3.2(7) . . . . ? C13 N7 Cu2 N8 7.0(5) . . . . ? N6 N7 Cu2 N8 -177.8(4) . . . . ? C13 N7 Cu2 N2 -173.5(5) . . . . ? N6 N7 Cu2 N2 1.7(4) . . . . ? C13 N7 Cu2 N15 -79.8(11) . . . . ? N6 N7 Cu2 N15 95.4(10) . . . . ? C13 N7 Cu2 N13 97.0(5) . . . . ? N6 N7 Cu2 N13 -87.8(4) . . . . ? C13 N7 Cu2 N16 -80.4(5) . . . . ? N6 N7 Cu2 N16 94.7(4) . . . . ? C18 N8 Cu2 N7 174.8(7) . . . . ? C14 N8 Cu2 N7 -6.5(5) . . . . ? C18 N8 Cu2 N2 173.4(6) . . . . ? C14 N8 Cu2 N2 -7.8(9) . . . . ? C18 N8 Cu2 N15 -18.6(7) . . . . ? C14 N8 Cu2 N15 160.1(5) . . . . ? C18 N8 Cu2 N13 55.6(7) . . . . ? C14 N8 Cu2 N13 -125.7(5) . . . . ? C18 N8 Cu2 N16 -91.7(7) . . . . ? C14 N8 Cu2 N16 87.0(5) . . . . ? C1 N2 Cu2 N7 177.2(5) . . . . ? C4 N2 Cu2 N7 -1.3(4) . . . . ? C1 N2 Cu2 N8 178.6(5) . . . . ? C4 N2 Cu2 N8 0.1(8) . . . . ? C1 N2 Cu2 N15 10.8(6) . . . . ? C4 N2 Cu2 N15 -167.7(4) . . . . ? C1 N2 Cu2 N13 -63.6(5) . . . . ? C4 N2 Cu2 N13 118.0(4) . . . . ? C1 N2 Cu2 N16 84.8(5) . . . . ? C4 N2 Cu2 N16 -93.6(4) . . . . ? C33 N15 Cu2 N7 7.0(13) . . . . ? N14 N15 Cu2 N7 -176.8(8) . . . . ? C33 N15 Cu2 N8 -77.5(6) . . . . ? N14 N15 Cu2 N8 98.7(5) . . . . ? C33 N15 Cu2 N2 97.8(6) . . . . ? N14 N15 Cu2 N2 -86.0(5) . . . . ? C33 N15 Cu2 N13 -170.2(6) . . . . ? N14 N15 Cu2 N13 6.0(4) . . . . ? C33 N15 Cu2 N16 7.6(5) . . . . ? N14 N15 Cu2 N16 -176.2(5) . . . . ? C29 N13 Cu2 N7 -2.0(7) . . . . ? C30 N13 Cu2 N7 175.4(4) . . . . ? C29 N13 Cu2 N8 78.7(7) . . . . ? C30 N13 Cu2 N8 -103.9(4) . . . . ? C29 N13 Cu2 N2 -81.5(6) . . . . ? C30 N13 Cu2 N2 95.9(4) . . . . ? C29 N13 Cu2 N15 177.2(7) . . . . ? C30 N13 Cu2 N15 -5.4(4) . . . . ? C29 N13 Cu2 N16 173.3(6) . . . . ? C30 N13 Cu2 N16 -9.3(6) . . . . ? C38 N16 Cu2 N7 1.5(7) . . . . ? C34 N16 Cu2 N7 172.0(5) . . . . ? C38 N16 Cu2 N8 -77.7(7) . . . . ? C34 N16 Cu2 N8 92.8(5) . . . . ? C38 N16 Cu2 N2 80.0(7) . . . . ? C34 N16 Cu2 N2 -109.6(5) . . . . ? C38 N16 Cu2 N15 -178.3(7) . . . . ? C34 N16 Cu2 N15 -7.8(5) . . . . ? C38 N16 Cu2 N13 -174.4(6) . . . . ? C34 N16 Cu2 N13 -3.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.514 _refine_diff_density_min -1.368 _refine_diff_density_rms 0.139 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.371 0.250 0.457 348.8 112.1 2 0.871 0.250 1.043 348.9 113.5 3 0.011 0.250 0.635 246.8 59.1 4 0.511 0.250 0.865 246.7 61.4 5 0.129 0.750 -0.043 348.9 113.6 6 0.629 0.750 0.543 348.9 114.6 7 0.489 0.750 0.135 246.7 57.7 8 0.989 0.750 0.365 246.8 59.2 _platon_squeeze_details ; The residual electron density was assigned to half a molecule of a triflate anion and two molecules of the acetonitrile solvent [691/8 = 86 e per asymmetric unit; half a molecule of CF3SO3 and two molecules of CH3CN would give 81e]. ;