# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;Self-Assembling of Nanoscopic Molecular Rectangles, Extended Helicates and Porous-like Materials Based on Macrocyclic Dicopper Building Blocks Under a Three-Level Supramolecular Control ; _publ_contact_author_name 'Miquel Costas' _publ_contact_author_email MIQUEL.COSTAS@UDG.ES loop_ _publ_author_name M.Costas A.Company X.Fontrodona L.Gomez X.Ribas # Attachment 'Gomezetal_CIF_revised.cif' data_lgl2p35g(3OTf)_CCDC648098 _database_code_depnum_ccdc_archive 'CCDC 648098' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H116 Cu4 N12 O8, 6(C3 H7 N O), 4(C F3 O3 S)' _chemical_formula_sum 'C110 H158 Cu4 F12 N18 O26 S4' _chemical_formula_weight 2759.02 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' Cu Cu 0.3201 1.2651 '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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.882(18) _cell_length_b 13.44(2) _cell_length_c 18.78(3) _cell_angle_alpha 70.93(3) _cell_angle_beta 79.53(3) _cell_angle_gamma 74.98(3) _cell_volume 2722(7) _cell_formula_units_Z 1 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 0.956 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(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 _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 46175 _diffrn_reflns_av_R_equivalents 0.1348 _diffrn_reflns_av_sigmaI/netI 0.2161 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 29.65 _reflns_number_total 14726 _reflns_number_gt 5963 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER Shelxtl' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997), Platon' _computing_molecular_graphics ? _computing_publication_material ? 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 0.000 0.000 0.000 14.7 3.2 2 0.000 0.000 0.500 176.7 44.9 _platon_squeeze_details ; ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The SUEEZE option of the PLATON Program (Spek, A. L. (2005). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, THe Netherlands) was used to eliminate electron density from disordered DMF solvent molecules. Those DMF molecules are, however, included in the reported chemical formula and derived values (reported crystal-data formula, formula weight,Dx, Mu and F(000)). The macrocyclic complex lies about an inversion center ; _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^)+(0.1043P)^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 14726 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1908 _refine_ls_R_factor_gt 0.0836 _refine_ls_wR_factor_ref 0.2266 _refine_ls_wR_factor_gt 0.1931 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.56461(6) 0.65558(5) 0.19151(4) 0.02507(19) Uani 1 1 d . . . Cu2 Cu -0.42272(6) 0.87303(5) -0.25092(4) 0.0272(2) Uani 1 1 d . . . O1 O 0.4383(3) 0.6932(3) 0.1358(2) 0.0276(9) Uani 1 1 d . . . O2 O 0.5032(3) 0.5485(3) 0.1038(2) 0.0359(10) Uani 1 1 d . . . O3 O -0.2410(4) 0.6785(3) -0.1945(2) 0.0402(11) Uani 1 1 d . . . O4 O -0.2998(3) 0.8416(3) -0.1930(2) 0.0288(9) Uani 1 1 d . . . N1 N 0.6883(4) 0.6945(3) 0.1077(3) 0.0265(11) Uani 1 1 d . . . N2 N 0.6808(4) 0.6407(3) 0.2553(3) 0.0296(11) Uani 1 1 d . . . N3 N 0.4808(4) 0.5769(3) 0.2863(3) 0.0295(11) Uani 1 1 d . . . N4 N 0.3303(4) 1.0844(3) 0.3484(3) 0.0317(12) Uani 1 1 d . . . N5 N 0.5567(4) 1.0641(3) 0.3082(3) 0.0263(11) Uani 1 1 d . . . N6 N 0.5318(4) 1.1981(3) 0.1709(3) 0.0278(11) Uani 1 1 d . . . C1 C 0.4291(5) 0.6290(4) 0.1042(3) 0.0273(13) Uani 1 1 d . . . C2 C 0.3267(5) 0.6510(4) 0.0661(3) 0.0233(12) Uani 1 1 d . . . C3 C 0.3254(5) 0.5969(4) 0.0187(3) 0.0276(13) Uani 1 1 d . . . H3A H 0.3907 0.5442 0.0111 0.033 Uiso 1 1 calc R . . C4 C 0.2340(5) 0.6159(4) -0.0180(3) 0.0277(13) Uani 1 1 d . . . H4A H 0.2362 0.5760 -0.0507 0.033 Uiso 1 1 calc R . . C5 C 0.1363(4) 0.6927(4) -0.0094(3) 0.0222(12) Uani 1 1 d . . . C6 C 0.1383(5) 0.7479(4) 0.0379(3) 0.0266(12) Uani 1 1 d . . . H6A H 0.0732 0.8006 0.0457 0.032 Uiso 1 1 calc R . . C7 C 0.2325(5) 0.7287(4) 0.0743(3) 0.0251(12) Uani 1 1 d . . . H7A H 0.2325 0.7697 0.1057 0.030 Uiso 1 1 calc R . . C8 C 0.0384(4) 0.7102(4) -0.0493(3) 0.0210(11) Uani 1 1 d . . . C9 C 0.0118(4) 0.6268(4) -0.0622(3) 0.0237(12) Uani 1 1 d . . . H9A H 0.0561 0.5577 -0.0432 0.028 Uiso 1 1 calc R . . C10 C -0.0761(5) 0.6409(4) -0.1014(3) 0.0264(12) Uani 1 1 d . . . H10A H -0.0930 0.5816 -0.1092 0.032 Uiso 1 1 calc R . . C11 C -0.1415(4) 0.7408(4) -0.1304(3) 0.0214(11) Uani 1 1 d . . . C12 C -0.1154(5) 0.8218(4) -0.1172(3) 0.0271(13) Uani 1 1 d . . . H12A H -0.1594 0.8909 -0.1365 0.033 Uiso 1 1 calc R . . C13 C -0.0282(5) 0.8083(4) -0.0771(3) 0.0316(14) Uani 1 1 d . . . H13A H -0.0132 0.8677 -0.0684 0.038 Uiso 1 1 calc R . . C14 C -0.2327(5) 0.7515(4) -0.1754(3) 0.0320(14) Uani 1 1 d . . . C15 C 0.6526(5) 0.7906(4) 0.0445(3) 0.0296(13) Uani 1 1 d . . . H15A H 0.7160 0.7944 0.0038 0.036 Uiso 1 1 calc R . . H15B H 0.5856 0.7826 0.0257 0.036 Uiso 1 1 calc R . . C16 C 0.7258(5) 0.6074(4) 0.0760(4) 0.0352(15) Uani 1 1 d . . . H16A H 0.7882 0.6217 0.0363 0.053 Uiso 1 1 calc R . . H16B H 0.6614 0.5991 0.0556 0.053 Uiso 1 1 calc R . . H16C H 0.7533 0.5423 0.1146 0.053 Uiso 1 1 calc R . . C17 C 0.7846(5) 0.7047(4) 0.1386(3) 0.0325(14) Uani 1 1 d . . . H17A H 0.7722 0.7771 0.1424 0.039 Uiso 1 1 calc R . . H17B H 0.8566 0.6910 0.1060 0.039 Uiso 1 1 calc R . . C18 C 0.7930(5) 0.6260(4) 0.2139(3) 0.0310(14) Uani 1 1 d . . . H18A H 0.8168 0.5533 0.2095 0.037 Uiso 1 1 calc R . . H18B H 0.8505 0.6373 0.2394 0.037 Uiso 1 1 calc R . . C19 C 0.6580(6) 0.7382(4) 0.2765(4) 0.0387(16) Uani 1 1 d . . . H19A H 0.7209 0.7367 0.3027 0.058 Uiso 1 1 calc R . . H19B H 0.5858 0.7439 0.3090 0.058 Uiso 1 1 calc R . . H19C H 0.6521 0.7991 0.2318 0.058 Uiso 1 1 calc R . . C20 C 0.6718(6) 0.5505(4) 0.3204(3) 0.0368(15) Uani 1 1 d . . . H20A H 0.7148 0.5514 0.3593 0.044 Uiso 1 1 calc R . . H20B H 0.7041 0.4839 0.3072 0.044 Uiso 1 1 calc R . . C21 C 0.5469(5) 0.5580(5) 0.3480(3) 0.0336(14) Uani 1 1 d . . . H21A H 0.5361 0.4916 0.3865 0.040 Uiso 1 1 calc R . . H21B H 0.5191 0.6165 0.3706 0.040 Uiso 1 1 calc R . . C22 C 0.4821(6) 0.4769(4) 0.2740(4) 0.0384(15) Uani 1 1 d . . . H22A H 0.4491 0.4307 0.3193 0.058 Uiso 1 1 calc R . . H22B H 0.5614 0.4426 0.2614 0.058 Uiso 1 1 calc R . . H22C H 0.4367 0.4903 0.2331 0.058 Uiso 1 1 calc R . . C23 C 0.3609(5) 0.6245(4) 0.3034(4) 0.0342(14) Uani 1 1 d . . . H23A H 0.3288 0.5746 0.3478 0.041 Uiso 1 1 calc R . . H23B H 0.3185 0.6329 0.2616 0.041 Uiso 1 1 calc R . . C24 C 0.3387(5) 0.7290(4) 0.3176(3) 0.0308(14) Uani 1 1 d . . . C25 C 0.3072(5) 0.7369(5) 0.3865(3) 0.0342(14) Uani 1 1 d . . . H25A H 0.3038 0.6750 0.4270 0.041 Uiso 1 1 calc R . . C26 C 0.2801(5) 0.8331(5) 0.3990(4) 0.0380(15) Uani 1 1 d . . . H26A H 0.2602 0.8379 0.4482 0.046 Uiso 1 1 calc R . . C27 C 0.2818(5) 0.9210(4) 0.3417(3) 0.0305(13) Uani 1 1 d . . . C28 C 0.3144(6) 0.9139(5) 0.2712(4) 0.0399(16) Uani 1 1 d . . . H28A H 0.3171 0.9759 0.2306 0.048 Uiso 1 1 calc R . . C29 C 0.3430(5) 0.8176(5) 0.2596(4) 0.0377(15) Uani 1 1 d . . . H29A H 0.3662 0.8121 0.2107 0.045 Uiso 1 1 calc R . . C30 C 0.2409(5) 1.0268(4) 0.3549(3) 0.0329(14) Uani 1 1 d . . . H30A H 0.1852 1.0711 0.3192 0.039 Uiso 1 1 calc R . . H30B H 0.1994 1.0171 0.4054 0.039 Uiso 1 1 calc R . . C31 C 0.2733(5) 1.1845(4) 0.3627(3) 0.0365(15) Uani 1 1 d . . . H31A H 0.2252 1.1711 0.4103 0.055 Uiso 1 1 calc R . . H31B H 0.2252 1.2279 0.3229 0.055 Uiso 1 1 calc R . . H31C H 0.3311 1.2218 0.3644 0.055 Uiso 1 1 calc R . . C32 C 0.4088(5) 1.0231(5) 0.4057(3) 0.0340(15) Uani 1 1 d . . . H32A H 0.4240 0.9470 0.4099 0.041 Uiso 1 1 calc R . . H32B H 0.3734 1.0327 0.4544 0.041 Uiso 1 1 calc R . . C33 C 0.5175(5) 1.0605(4) 0.3843(3) 0.0350(15) Uani 1 1 d . . . H33A H 0.5050 1.1318 0.3902 0.042 Uiso 1 1 calc R . . H33B H 0.5760 1.0121 0.4168 0.042 Uiso 1 1 calc R . . C34 C 0.6007(5) 0.9573(4) 0.3011(3) 0.0312(14) Uani 1 1 d . . . H34A H 0.6713 0.9249 0.3254 0.047 Uiso 1 1 calc R . . H34B H 0.6171 0.9611 0.2484 0.047 Uiso 1 1 calc R . . H34C H 0.5430 0.9147 0.3247 0.047 Uiso 1 1 calc R . . C35 C 0.6426(5) 1.1275(4) 0.2751(3) 0.0314(14) Uani 1 1 d . . . H35A H 0.7185 1.0872 0.2915 0.038 Uiso 1 1 calc R . . H35B H 0.6218 1.1926 0.2906 0.038 Uiso 1 1 calc R . . C36 C 0.6476(5) 1.1545(5) 0.1943(3) 0.0316(14) Uani 1 1 d . . . H36A H 0.6827 1.0906 0.1783 0.038 Uiso 1 1 calc R . . H36B H 0.6961 1.2070 0.1705 0.038 Uiso 1 1 calc R . . C37 C 0.5014(6) 1.3093(4) 0.1678(4) 0.0386(15) Uani 1 1 d . . . H37A H 0.5583 1.3460 0.1336 0.058 Uiso 1 1 calc R . . H37B H 0.5000 1.3157 0.2175 0.058 Uiso 1 1 calc R . . H37C H 0.4254 1.3411 0.1503 0.058 Uiso 1 1 calc R . . C38 C 0.5303(5) 1.1933(4) 0.0955(3) 0.0297(13) Uani 1 1 d . . . H38A H 0.5840 1.2351 0.0611 0.036 Uiso 1 1 calc R . . H38B H 0.4523 1.2271 0.0801 0.036 Uiso 1 1 calc R . . C39 C 0.5617(5) 1.0850(4) 0.0872(3) 0.0261(13) Uani 1 1 d . . . C40 C 0.6711(6) 1.0494(4) 0.0600(3) 0.0338(14) Uani 1 1 d . . . H40A H 0.7264 1.0917 0.0489 0.041 Uiso 1 1 calc R . . C41 C 0.7009(5) 0.9515(4) 0.0487(3) 0.0289(13) Uani 1 1 d . . . H41A H 0.7775 0.9260 0.0305 0.035 Uiso 1 1 calc R . . C42 C 0.6223(5) 0.8908(4) 0.0632(3) 0.0258(13) Uani 1 1 d . . . C43 C 0.5135(5) 0.9271(4) 0.0900(3) 0.0275(13) Uani 1 1 d . . . H43A H 0.4577 0.8855 0.1004 0.033 Uiso 1 1 calc R . . C44 C 0.4844(5) 1.0238(4) 0.1018(3) 0.0263(12) Uani 1 1 d . . . H44A H 0.4080 1.0486 0.1208 0.032 Uiso 1 1 calc R . . O1A O 0.7536(4) 0.3755(4) 0.2209(3) 0.0547(13) Uani 1 1 d . . . N1A N 0.8453(6) 0.2398(5) 0.3027(5) 0.073(2) Uani 1 1 d . . . C1A C 0.8296(5) 0.3029(5) 0.2374(4) 0.0329(14) Uani 1 1 d . . . H1A H 0.8858 0.2892 0.1983 0.040 Uiso 1 1 calc R . . C2A C 0.9449(8) 0.1646(8) 0.3109(7) 0.110(4) Uani 1 1 d . . . H7 H 0.9270 0.0949 0.3357 0.165 Uiso 1 1 calc R . . H8 H 0.9923 0.1793 0.3410 0.165 Uiso 1 1 calc R . . H9 H 0.9868 0.1657 0.2620 0.165 Uiso 1 1 calc R . . C3A C 0.7616(8) 0.2519(7) 0.3722(5) 0.076(3) Uani 1 1 d . . . H10 H 0.6905 0.3023 0.3567 0.114 Uiso 1 1 calc R . . H11 H 0.7972 0.2778 0.4026 0.114 Uiso 1 1 calc R . . H12 H 0.7441 0.1832 0.4013 0.114 Uiso 1 1 calc R . . O1C O -0.0248(9) 0.3710(8) 0.3655(7) 0.149(4) Uani 1 1 d . . . N1C N 0.0535(8) 0.5058(7) 0.2946(6) 0.090(3) Uani 1 1 d . . . C1C C 0.0248(10) 0.4199(9) 0.3090(7) 0.085(3) Uani 1 1 d . . . H1C H 0.0446 0.3877 0.2702 0.102 Uiso 1 1 calc R . . C2C C 0.0179(10) 0.5627(8) 0.3518(6) 0.114(4) Uani 1 1 d . . . H13 H -0.0265 0.6339 0.3300 0.171 Uiso 1 1 calc R . . H14 H 0.0863 0.5678 0.3698 0.171 Uiso 1 1 calc R . . H15 H -0.0294 0.5241 0.3933 0.171 Uiso 1 1 calc R . . C3C C 0.1166(8) 0.5475(8) 0.2291(6) 0.082(3) Uani 1 1 d . . . H16 H 0.1087 0.5161 0.1916 0.123 Uiso 1 1 calc R . . H17 H 0.1976 0.5318 0.2373 0.123 Uiso 1 1 calc R . . H18 H 0.0883 0.6241 0.2119 0.123 Uiso 1 1 calc R . . S1O S 0.0755(2) 0.10090(18) 0.80215(15) 0.0763(7) Uani 1 1 d . . . F1O F -0.1150(5) 0.0739(4) 0.8397(3) 0.0961(19) Uani 1 1 d . . . F2O F -0.0501(5) 0.0692(5) 0.7244(4) 0.115(2) Uani 1 1 d . . . F3O F -0.1024(5) 0.2157(4) 0.7455(4) 0.125(2) Uani 1 1 d . . . O1O O 0.0651(5) 0.1589(7) 0.8473(5) 0.123(3) Uani 1 1 d . . . O2O O 0.1250(5) -0.0030(5) 0.8199(4) 0.101(2) Uani 1 1 d . . . O3O O 0.1283(7) 0.1616(7) 0.7186(6) 0.172(4) Uani 1 1 d . . . C1O C -0.0512(9) 0.1126(7) 0.7764(7) 0.084(3) Uani 1 1 d . . . S1Q S 0.41376(17) 0.26684(15) 0.50032(11) 0.0499(5) Uani 1 1 d . . . F1Q F 0.2355(4) 0.3824(4) 0.4376(3) 0.0897(17) Uani 1 1 d . . . F2Q F 0.3205(5) 0.4591(3) 0.4826(3) 0.0878(16) Uani 1 1 d . . . F3Q F 0.2206(4) 0.3594(3) 0.5522(2) 0.0652(12) Uani 1 1 d . . . O1Q O 0.4612(5) 0.2660(4) 0.5616(3) 0.0732(17) Uani 1 1 d . . . O2Q O 0.4735(5) 0.2901(4) 0.4303(3) 0.0587(14) Uani 1 1 d . . . O3Q O 0.3641(6) 0.1762(4) 0.5159(3) 0.0753(17) Uani 1 1 d . . . C1Q C 0.2903(7) 0.3703(5) 0.4921(4) 0.0465(18) 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 Cu1 0.0296(4) 0.0136(3) 0.0320(4) -0.0094(3) -0.0124(3) 0.0053(3) Cu2 0.0316(4) 0.0154(3) 0.0345(4) -0.0116(3) -0.0152(3) 0.0088(3) O1 0.030(2) 0.0169(19) 0.039(2) -0.0123(17) -0.0150(18) 0.0023(16) O2 0.030(2) 0.021(2) 0.059(3) -0.019(2) -0.021(2) 0.0112(17) O3 0.044(3) 0.021(2) 0.060(3) -0.017(2) -0.033(2) 0.0116(18) O4 0.034(2) 0.0154(19) 0.037(2) -0.0109(17) -0.0161(18) 0.0087(16) N1 0.033(3) 0.012(2) 0.035(3) -0.010(2) -0.015(2) 0.0054(19) N2 0.040(3) 0.013(2) 0.036(3) -0.010(2) -0.012(2) 0.003(2) N3 0.040(3) 0.016(2) 0.037(3) -0.016(2) -0.008(2) -0.001(2) N4 0.036(3) 0.018(2) 0.043(3) -0.018(2) -0.016(2) 0.011(2) N5 0.034(3) 0.016(2) 0.033(3) -0.015(2) -0.010(2) 0.003(2) N6 0.040(3) 0.012(2) 0.034(3) -0.009(2) -0.017(2) 0.0042(19) C1 0.026(3) 0.021(3) 0.035(3) -0.011(3) -0.008(2) 0.003(2) C2 0.025(3) 0.015(3) 0.030(3) -0.010(2) -0.007(2) 0.002(2) C3 0.026(3) 0.018(3) 0.039(4) -0.014(3) -0.009(3) 0.004(2) C4 0.029(3) 0.023(3) 0.037(3) -0.017(3) -0.011(3) -0.001(2) C5 0.022(3) 0.020(3) 0.026(3) -0.008(2) -0.007(2) -0.003(2) C6 0.032(3) 0.017(3) 0.030(3) -0.011(2) -0.005(2) 0.003(2) C7 0.032(3) 0.015(3) 0.031(3) -0.010(2) -0.003(2) -0.004(2) C8 0.023(3) 0.017(3) 0.022(3) -0.004(2) -0.005(2) -0.002(2) C9 0.020(3) 0.019(3) 0.028(3) -0.007(2) -0.005(2) 0.004(2) C10 0.027(3) 0.016(3) 0.034(3) -0.010(2) -0.004(2) 0.002(2) C11 0.019(3) 0.022(3) 0.022(3) -0.005(2) -0.006(2) -0.001(2) C12 0.026(3) 0.018(3) 0.034(3) -0.008(2) -0.009(2) 0.005(2) C13 0.041(4) 0.021(3) 0.034(3) -0.013(3) -0.013(3) 0.004(3) C14 0.035(3) 0.015(3) 0.044(4) -0.010(3) -0.019(3) 0.011(2) C15 0.038(3) 0.021(3) 0.027(3) -0.010(2) -0.007(3) 0.004(2) C16 0.034(3) 0.020(3) 0.051(4) -0.019(3) -0.002(3) 0.005(2) C17 0.026(3) 0.022(3) 0.048(4) -0.010(3) -0.011(3) 0.003(2) C18 0.027(3) 0.018(3) 0.046(4) -0.008(3) -0.022(3) 0.008(2) C19 0.053(4) 0.020(3) 0.048(4) -0.017(3) -0.026(3) 0.006(3) C20 0.056(4) 0.020(3) 0.036(4) -0.009(3) -0.023(3) 0.004(3) C21 0.041(4) 0.027(3) 0.031(3) -0.013(3) -0.013(3) 0.007(3) C22 0.057(4) 0.017(3) 0.041(4) -0.010(3) -0.002(3) -0.007(3) C23 0.031(3) 0.025(3) 0.049(4) -0.020(3) 0.000(3) -0.001(3) C24 0.031(3) 0.019(3) 0.045(4) -0.014(3) -0.007(3) -0.002(2) C25 0.038(4) 0.026(3) 0.036(4) -0.010(3) -0.006(3) 0.001(3) C26 0.046(4) 0.035(4) 0.032(4) -0.017(3) 0.001(3) 0.000(3) C27 0.025(3) 0.024(3) 0.042(4) -0.015(3) -0.005(3) 0.003(2) C28 0.056(4) 0.023(3) 0.037(4) -0.012(3) -0.006(3) 0.003(3) C29 0.051(4) 0.024(3) 0.036(4) -0.017(3) 0.005(3) -0.001(3) C30 0.034(3) 0.025(3) 0.036(4) -0.013(3) -0.003(3) 0.006(3) C31 0.038(4) 0.026(3) 0.041(4) -0.015(3) -0.007(3) 0.011(3) C32 0.043(4) 0.025(3) 0.029(3) -0.007(3) -0.017(3) 0.010(3) C33 0.049(4) 0.021(3) 0.036(4) -0.014(3) -0.023(3) 0.011(3) C34 0.031(3) 0.016(3) 0.042(4) -0.010(3) -0.013(3) 0.011(2) C35 0.030(3) 0.024(3) 0.041(4) -0.014(3) -0.012(3) 0.004(2) C36 0.035(3) 0.024(3) 0.038(4) -0.009(3) -0.014(3) -0.004(3) C37 0.049(4) 0.021(3) 0.050(4) -0.015(3) -0.017(3) 0.000(3) C38 0.040(4) 0.014(3) 0.033(3) -0.007(2) -0.011(3) 0.004(2) C39 0.038(3) 0.014(3) 0.024(3) -0.006(2) -0.016(2) 0.007(2) C40 0.050(4) 0.017(3) 0.037(4) -0.009(3) -0.007(3) -0.010(3) C41 0.028(3) 0.019(3) 0.038(4) -0.009(3) -0.009(3) 0.003(2) C42 0.035(3) 0.015(3) 0.026(3) -0.005(2) -0.015(2) 0.003(2) C43 0.032(3) 0.016(3) 0.036(3) -0.009(2) -0.013(3) -0.001(2) C44 0.027(3) 0.018(3) 0.033(3) -0.009(2) -0.009(2) 0.003(2) O1A 0.070(4) 0.033(3) 0.053(3) -0.006(2) -0.022(3) 0.004(2) N1A 0.057(4) 0.051(4) 0.105(6) -0.024(4) -0.010(4) 0.000(3) C1A 0.036(4) 0.035(4) 0.025(3) -0.007(3) 0.000(3) -0.007(3) C2A 0.052(6) 0.078(7) 0.177(11) -0.046(7) 0.016(6) 0.016(5) C3A 0.094(7) 0.067(6) 0.078(6) -0.047(5) -0.036(5) 0.017(5) O1C 0.134(8) 0.106(7) 0.208(11) -0.026(7) -0.053(8) -0.029(6) N1C 0.087(6) 0.055(5) 0.127(8) -0.030(5) -0.051(6) 0.015(4) C1C 0.083(8) 0.049(6) 0.125(10) -0.033(6) -0.058(7) 0.024(5) C2C 0.123(9) 0.087(8) 0.141(10) -0.069(8) -0.042(8) 0.028(7) C3C 0.073(6) 0.082(7) 0.094(8) -0.037(6) 0.023(6) -0.030(5) S1O 0.0836(17) 0.0560(14) 0.1008(19) -0.0432(14) -0.0424(15) 0.0138(12) F1O 0.115(4) 0.040(3) 0.099(4) -0.012(3) 0.049(3) -0.012(3) F2O 0.085(4) 0.167(6) 0.141(5) -0.116(5) -0.037(4) -0.002(4) F3O 0.078(4) 0.060(3) 0.208(7) 0.006(4) -0.064(4) 0.009(3) O1O 0.058(4) 0.188(8) 0.189(8) -0.153(7) 0.002(4) -0.026(5) O2O 0.047(3) 0.062(4) 0.165(7) -0.011(4) -0.024(4) 0.020(3) O3O 0.110(7) 0.123(7) 0.225(10) -0.026(7) 0.094(7) -0.037(5) C1O 0.084(7) 0.048(5) 0.126(9) -0.036(6) -0.022(7) -0.003(5) S1Q 0.0582(12) 0.0463(11) 0.0449(11) -0.0231(9) -0.0204(9) 0.0119(9) F1Q 0.086(4) 0.099(4) 0.069(3) -0.035(3) -0.043(3) 0.043(3) F2Q 0.115(4) 0.024(2) 0.103(4) -0.020(2) 0.010(3) 0.010(2) F3Q 0.064(3) 0.065(3) 0.060(3) -0.025(2) -0.007(2) 0.006(2) O1Q 0.075(4) 0.081(4) 0.071(4) -0.050(3) -0.036(3) 0.027(3) O2Q 0.074(4) 0.037(3) 0.049(3) -0.013(2) -0.003(3) 0.014(2) O3Q 0.120(5) 0.036(3) 0.063(4) -0.009(3) -0.015(3) -0.008(3) C1Q 0.070(5) 0.030(4) 0.029(4) 0.000(3) -0.011(4) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.853(4) . ? Cu1 N2 1.920(5) . ? Cu1 N1 1.983(5) . ? Cu1 N3 1.987(5) . ? Cu1 C1 2.656(6) . ? Cu2 O4 1.858(4) . ? Cu2 N5 1.934(5) 2_575 ? Cu2 N4 1.948(6) 2_575 ? Cu2 N6 1.961(5) 2_575 ? Cu2 C31 2.674(7) 2_575 ? O1 C1 1.232(6) . ? O2 C1 1.206(6) . ? O3 C14 1.180(6) . ? O4 C14 1.243(6) . ? N1 C16 1.419(6) . ? N1 C17 1.428(7) . ? N1 C15 1.467(7) . ? N2 C18 1.417(7) . ? N2 C20 1.423(7) . ? N2 C19 1.437(7) . ? N3 C23 1.426(7) . ? N3 C22 1.432(7) . ? N3 C21 1.436(7) . ? N4 C31 1.428(7) . ? N4 C30 1.434(7) . ? N4 C32 1.448(7) . ? N4 Cu2 1.948(6) 2_575 ? N5 C33 1.409(7) . ? N5 C35 1.424(7) . ? N5 C34 1.436(6) . ? N5 Cu2 1.934(5) 2_575 ? N6 C37 1.428(7) . ? N6 C36 1.436(7) . ? N6 C38 1.444(7) . ? N6 Cu2 1.961(5) 2_575 ? C1 C2 1.439(7) . ? C2 C3 1.325(7) . ? C2 C7 1.342(7) . ? C3 C4 1.317(7) . ? C4 C5 1.363(7) . ? C5 C6 1.337(7) . ? C5 C8 1.424(7) . ? C6 C7 1.342(7) . ? C8 C13 1.340(7) . ? C8 C9 1.344(7) . ? C9 C10 1.325(7) . ? C10 C11 1.356(7) . ? C11 C12 1.312(7) . ? C11 C14 1.444(8) . ? C12 C13 1.331(7) . ? C15 C42 1.442(7) . ? C17 C18 1.465(8) . ? C20 C21 1.469(9) . ? C23 C24 1.464(7) . ? C24 C25 1.311(8) . ? C24 C29 1.331(8) . ? C25 C26 1.337(8) . ? C26 C27 1.314(8) . ? C27 C28 1.338(8) . ? C27 C30 1.465(7) . ? C28 C29 1.330(8) . ? C31 Cu2 2.674(7) 2_575 ? C32 C33 1.448(9) . ? C35 C36 1.434(8) . ? C38 C39 1.457(7) . ? C39 C44 1.323(8) . ? C39 C40 1.333(8) . ? C40 C41 1.347(7) . ? C41 C42 1.330(8) . ? C42 C43 1.326(8) . ? C43 C44 1.336(7) . ? O1A C1A 1.145(7) . ? N1A C1A 1.258(9) . ? N1A C2A 1.338(10) . ? N1A C3A 1.517(10) . ? O1C C1C 1.193(13) . ? N1C C1C 1.221(12) . ? N1C C3C 1.348(11) . ? N1C C2C 1.458(12) . ? S1O O1O 1.299(6) . ? S1O O2O 1.322(6) . ? S1O O3O 1.610(9) . ? S1O C1O 1.618(10) . ? F1O C1O 1.316(11) . ? F2O C1O 1.288(10) . ? F3O C1O 1.339(10) . ? S1Q O2Q 1.356(5) . ? S1Q O1Q 1.366(5) . ? S1Q O3Q 1.412(6) . ? S1Q C1Q 1.730(7) . ? F1Q C1Q 1.257(8) . ? F2Q C1Q 1.281(8) . ? F3Q C1Q 1.264(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 168.99(17) . . ? O1 Cu1 N1 99.3(2) . . ? N2 Cu1 N1 84.3(2) . . ? O1 Cu1 N3 94.0(2) . . ? N2 Cu1 N3 84.9(2) . . ? N1 Cu1 N3 162.06(18) . . ? O1 Cu1 C1 24.31(15) . . ? N2 Cu1 C1 166.52(17) . . ? N1 Cu1 C1 94.3(2) . . ? N3 Cu1 C1 92.9(2) . . ? O4 Cu2 N5 167.76(16) . 2_575 ? O4 Cu2 N4 95.4(2) . 2_575 ? N5 Cu2 N4 85.2(2) 2_575 2_575 ? O4 Cu2 N6 97.6(2) . 2_575 ? N5 Cu2 N6 85.2(2) 2_575 2_575 ? N4 Cu2 N6 160.48(18) 2_575 2_575 ? O4 Cu2 C31 90.4(2) . 2_575 ? N5 Cu2 C31 96.2(2) 2_575 2_575 ? N4 Cu2 C31 31.26(18) 2_575 2_575 ? N6 Cu2 C31 133.94(19) 2_575 2_575 ? C1 O1 Cu1 117.4(3) . . ? C14 O4 Cu2 123.0(4) . . ? C16 N1 C17 108.7(4) . . ? C16 N1 C15 105.8(4) . . ? C17 N1 C15 110.4(4) . . ? C16 N1 Cu1 106.7(4) . . ? C17 N1 Cu1 108.6(4) . . ? C15 N1 Cu1 116.4(4) . . ? C18 N2 C20 111.2(5) . . ? C18 N2 C19 109.7(5) . . ? C20 N2 C19 110.8(5) . . ? C18 N2 Cu1 108.8(4) . . ? C20 N2 Cu1 108.3(4) . . ? C19 N2 Cu1 107.9(3) . . ? C23 N3 C22 106.7(5) . . ? C23 N3 C21 110.7(5) . . ? C22 N3 C21 110.1(5) . . ? C23 N3 Cu1 116.9(4) . . ? C22 N3 Cu1 103.9(4) . . ? C21 N3 Cu1 108.3(4) . . ? C31 N4 C30 107.2(5) . . ? C31 N4 C32 108.8(4) . . ? C30 N4 C32 108.9(5) . . ? C31 N4 Cu2 103.7(4) . 2_575 ? C30 N4 Cu2 118.9(4) . 2_575 ? C32 N4 Cu2 108.9(4) . 2_575 ? C33 N5 C35 113.4(4) . . ? C33 N5 C34 110.8(4) . . ? C35 N5 C34 110.0(5) . . ? C33 N5 Cu2 107.7(4) . 2_575 ? C35 N5 Cu2 108.1(4) . 2_575 ? C34 N5 Cu2 106.5(3) . 2_575 ? C37 N6 C36 107.9(4) . . ? C37 N6 C38 107.1(4) . . ? C36 N6 C38 110.4(5) . . ? C37 N6 Cu2 106.5(4) . 2_575 ? C36 N6 Cu2 107.8(4) . 2_575 ? C38 N6 Cu2 116.8(4) . 2_575 ? O2 C1 O1 122.2(5) . . ? O2 C1 C2 118.9(5) . . ? O1 C1 C2 118.9(5) . . ? O2 C1 Cu1 84.1(3) . . ? O1 C1 Cu1 38.3(2) . . ? C2 C1 Cu1 156.8(4) . . ? C3 C2 C7 117.9(5) . . ? C3 C2 C1 119.9(5) . . ? C7 C2 C1 122.1(5) . . ? C4 C3 C2 121.7(5) . . ? C3 C4 C5 121.5(5) . . ? C6 C5 C4 116.7(5) . . ? C6 C5 C8 123.2(5) . . ? C4 C5 C8 120.1(5) . . ? C5 C6 C7 121.2(5) . . ? C6 C7 C2 120.9(5) . . ? C13 C8 C9 117.4(5) . . ? C13 C8 C5 122.8(5) . . ? C9 C8 C5 119.9(5) . . ? C10 C9 C8 121.4(5) . . ? C9 C10 C11 120.7(5) . . ? C12 C11 C10 117.6(5) . . ? C12 C11 C14 124.4(5) . . ? C10 C11 C14 118.0(5) . . ? C11 C12 C13 122.3(5) . . ? C12 C13 C8 120.8(5) . . ? O3 C14 O4 123.0(5) . . ? O3 C14 C11 121.1(5) . . ? O4 C14 C11 115.9(5) . . ? C42 C15 N1 114.7(5) . . ? N1 C17 C18 108.0(5) . . ? N2 C18 C17 107.5(4) . . ? N2 C20 C21 107.5(5) . . ? N3 C21 C20 109.8(5) . . ? N3 C23 C24 116.1(5) . . ? C25 C24 C29 119.8(5) . . ? C25 C24 C23 120.4(6) . . ? C29 C24 C23 119.7(6) . . ? C24 C25 C26 120.5(6) . . ? C27 C26 C25 120.0(6) . . ? C26 C27 C28 120.0(6) . . ? C26 C27 C30 119.7(6) . . ? C28 C27 C30 120.2(6) . . ? C29 C28 C27 119.5(6) . . ? C28 C29 C24 120.2(6) . . ? N4 C30 C27 115.7(5) . . ? N4 C31 Cu2 45.1(3) . 2_575 ? N4 C32 C33 108.7(5) . . ? N5 C33 C32 109.1(5) . . ? N5 C35 C36 108.3(5) . . ? C35 C36 N6 110.1(5) . . ? N6 C38 C39 115.0(4) . . ? C44 C39 C40 119.1(5) . . ? C44 C39 C38 122.4(5) . . ? C40 C39 C38 118.3(5) . . ? C39 C40 C41 119.4(6) . . ? C42 C41 C40 121.0(6) . . ? C43 C42 C41 119.2(5) . . ? C43 C42 C15 120.3(5) . . ? C41 C42 C15 120.3(5) . . ? C42 C43 C44 119.7(5) . . ? C39 C44 C43 121.5(5) . . ? C1A N1A C2A 117.6(8) . . ? C1A N1A C3A 122.7(7) . . ? C2A N1A C3A 119.5(8) . . ? O1A C1A N1A 126.9(7) . . ? C1C N1C C3C 122.4(11) . . ? C1C N1C C2C 117.2(11) . . ? C3C N1C C2C 120.4(9) . . ? O1C C1C N1C 129.7(13) . . ? O1O S1O O2O 123.0(6) . . ? O1O S1O O3O 109.9(6) . . ? O2O S1O O3O 109.7(5) . . ? O1O S1O C1O 109.8(5) . . ? O2O S1O C1O 106.3(4) . . ? O3O S1O C1O 94.1(6) . . ? F2O C1O F1O 113.6(8) . . ? F2O C1O F3O 102.7(9) . . ? F1O C1O F3O 108.4(8) . . ? F2O C1O S1O 115.5(7) . . ? F1O C1O S1O 104.7(8) . . ? F3O C1O S1O 112.0(7) . . ? O2Q S1Q O1Q 120.4(4) . . ? O2Q S1Q O3Q 112.2(3) . . ? O1Q S1Q O3Q 111.7(4) . . ? O2Q S1Q C1Q 103.5(3) . . ? O1Q S1Q C1Q 105.0(3) . . ? O3Q S1Q C1Q 101.6(4) . . ? F1Q C1Q F3Q 109.1(7) . . ? F1Q C1Q F2Q 108.1(6) . . ? F3Q C1Q F2Q 104.1(6) . . ? F1Q C1Q S1Q 113.3(5) . . ? F3Q C1Q S1Q 112.5(5) . . ? F2Q C1Q S1Q 109.3(6) . . ? 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 N2 Cu1 O1 C1 -172.1(9) . . . . ? N1 Cu1 O1 C1 79.8(4) . . . . ? N3 Cu1 O1 C1 -88.1(4) . . . . ? N5 Cu2 O4 C14 179.5(8) 2_575 . . . ? N4 Cu2 O4 C14 -88.2(5) 2_575 . . . ? N6 Cu2 O4 C14 77.2(5) 2_575 . . . ? C31 Cu2 O4 C14 -57.3(5) 2_575 . . . ? O1 Cu1 N1 C16 -81.3(4) . . . . ? N2 Cu1 N1 C16 109.2(4) . . . . ? N3 Cu1 N1 C16 56.3(7) . . . . ? C1 Cu1 N1 C16 -57.3(4) . . . . ? O1 Cu1 N1 C17 161.7(3) . . . . ? N2 Cu1 N1 C17 -7.8(3) . . . . ? N3 Cu1 N1 C17 -60.8(7) . . . . ? C1 Cu1 N1 C17 -174.4(3) . . . . ? O1 Cu1 N1 C15 36.4(4) . . . . ? N2 Cu1 N1 C15 -133.0(4) . . . . ? N3 Cu1 N1 C15 174.0(5) . . . . ? C1 Cu1 N1 C15 60.4(4) . . . . ? O1 Cu1 N2 C18 -130.2(9) . . . . ? N1 Cu1 N2 C18 -20.8(3) . . . . ? N3 Cu1 N2 C18 145.0(4) . . . . ? C1 Cu1 N2 C18 63.9(10) . . . . ? O1 Cu1 N2 C20 108.8(10) . . . . ? N1 Cu1 N2 C20 -141.7(4) . . . . ? N3 Cu1 N2 C20 24.0(4) . . . . ? C1 Cu1 N2 C20 -57.1(10) . . . . ? O1 Cu1 N2 C19 -11.3(12) . . . . ? N1 Cu1 N2 C19 98.2(4) . . . . ? N3 Cu1 N2 C19 -96.1(4) . . . . ? C1 Cu1 N2 C19 -177.1(7) . . . . ? O1 Cu1 N3 C23 -40.4(4) . . . . ? N2 Cu1 N3 C23 128.6(4) . . . . ? N1 Cu1 N3 C23 -178.5(5) . . . . ? C1 Cu1 N3 C23 -64.8(4) . . . . ? O1 Cu1 N3 C22 76.7(4) . . . . ? N2 Cu1 N3 C22 -114.3(4) . . . . ? N1 Cu1 N3 C22 -61.4(7) . . . . ? C1 Cu1 N3 C22 52.4(4) . . . . ? O1 Cu1 N3 C21 -166.2(3) . . . . ? N2 Cu1 N3 C21 2.8(3) . . . . ? N1 Cu1 N3 C21 55.7(7) . . . . ? C1 Cu1 N3 C21 169.5(3) . . . . ? Cu1 O1 C1 O2 -5.7(8) . . . . ? Cu1 O1 C1 C2 174.5(4) . . . . ? O1 Cu1 C1 O2 175.2(7) . . . . ? N2 Cu1 C1 O2 -11.3(10) . . . . ? N1 Cu1 C1 O2 72.1(4) . . . . ? N3 Cu1 C1 O2 -91.5(4) . . . . ? N2 Cu1 C1 O1 173.5(7) . . . . ? N1 Cu1 C1 O1 -103.1(4) . . . . ? N3 Cu1 C1 O1 93.4(4) . . . . ? O1 Cu1 C1 C2 -12.2(9) . . . . ? N2 Cu1 C1 C2 161.3(9) . . . . ? N1 Cu1 C1 C2 -115.3(10) . . . . ? N3 Cu1 C1 C2 81.2(10) . . . . ? O2 C1 C2 C3 -14.0(9) . . . . ? O1 C1 C2 C3 165.8(5) . . . . ? Cu1 C1 C2 C3 174.4(8) . . . . ? O2 C1 C2 C7 168.9(5) . . . . ? O1 C1 C2 C7 -11.3(8) . . . . ? Cu1 C1 C2 C7 -2.7(14) . . . . ? C7 C2 C3 C4 -1.8(9) . . . . ? C1 C2 C3 C4 -179.0(5) . . . . ? C2 C3 C4 C5 0.4(9) . . . . ? C3 C4 C5 C6 0.3(8) . . . . ? C3 C4 C5 C8 -179.2(5) . . . . ? C4 C5 C6 C7 0.4(8) . . . . ? C8 C5 C6 C7 -180.0(5) . . . . ? C5 C6 C7 C2 -1.9(9) . . . . ? C3 C2 C7 C6 2.6(8) . . . . ? C1 C2 C7 C6 179.7(5) . . . . ? C6 C5 C8 C13 36.9(8) . . . . ? C4 C5 C8 C13 -143.5(6) . . . . ? C6 C5 C8 C9 -145.1(6) . . . . ? C4 C5 C8 C9 34.4(8) . . . . ? C13 C8 C9 C10 0.5(8) . . . . ? C5 C8 C9 C10 -177.6(5) . . . . ? C8 C9 C10 C11 0.6(8) . . . . ? C9 C10 C11 C12 -0.9(8) . . . . ? C9 C10 C11 C14 177.4(5) . . . . ? C10 C11 C12 C13 0.2(9) . . . . ? C14 C11 C12 C13 -178.0(5) . . . . ? C11 C12 C13 C8 0.9(9) . . . . ? C9 C8 C13 C12 -1.3(9) . . . . ? C5 C8 C13 C12 176.8(5) . . . . ? Cu2 O4 C14 O3 0.7(9) . . . . ? Cu2 O4 C14 C11 179.8(4) . . . . ? C12 C11 C14 O3 168.8(6) . . . . ? C10 C11 C14 O3 -9.4(9) . . . . ? C12 C11 C14 O4 -10.4(9) . . . . ? C10 C11 C14 O4 171.4(5) . . . . ? C16 N1 C15 C42 -173.9(5) . . . . ? C17 N1 C15 C42 -56.5(7) . . . . ? Cu1 N1 C15 C42 67.8(6) . . . . ? C16 N1 C17 C18 -81.9(6) . . . . ? C15 N1 C17 C18 162.5(4) . . . . ? Cu1 N1 C17 C18 33.8(5) . . . . ? C20 N2 C18 C17 164.0(4) . . . . ? C19 N2 C18 C17 -73.1(6) . . . . ? Cu1 N2 C18 C17 44.8(5) . . . . ? N1 C17 C18 N2 -52.0(6) . . . . ? C18 N2 C20 C21 -165.0(5) . . . . ? C19 N2 C20 C21 72.7(6) . . . . ? Cu1 N2 C20 C21 -45.5(5) . . . . ? C23 N3 C21 C20 -157.8(5) . . . . ? C22 N3 C21 C20 84.5(6) . . . . ? Cu1 N3 C21 C20 -28.5(5) . . . . ? N2 C20 C21 N3 49.1(6) . . . . ? C22 N3 C23 C24 -179.5(5) . . . . ? C21 N3 C23 C24 60.6(7) . . . . ? Cu1 N3 C23 C24 -63.9(6) . . . . ? N3 C23 C24 C25 -107.0(7) . . . . ? N3 C23 C24 C29 77.3(8) . . . . ? C29 C24 C25 C26 -0.4(9) . . . . ? C23 C24 C25 C26 -176.0(6) . . . . ? C24 C25 C26 C27 1.9(10) . . . . ? C25 C26 C27 C28 -2.3(10) . . . . ? C25 C26 C27 C30 174.0(6) . . . . ? C26 C27 C28 C29 1.2(10) . . . . ? C30 C27 C28 C29 -175.1(6) . . . . ? C27 C28 C29 C24 0.3(10) . . . . ? C25 C24 C29 C28 -0.7(10) . . . . ? C23 C24 C29 C28 174.9(6) . . . . ? C31 N4 C30 C27 179.7(5) . . . . ? C32 N4 C30 C27 -62.7(6) . . . . ? Cu2 N4 C30 C27 62.7(6) 2_575 . . . ? C26 C27 C30 N4 108.3(7) . . . . ? C28 C27 C30 N4 -75.4(7) . . . . ? C30 N4 C31 Cu2 -126.5(5) . . . 2_575 ? C32 N4 C31 Cu2 115.8(5) . . . 2_575 ? C31 N4 C32 C33 -82.2(6) . . . . ? C30 N4 C32 C33 161.3(4) . . . . ? Cu2 N4 C32 C33 30.2(5) 2_575 . . . ? C35 N5 C33 C32 163.1(4) . . . . ? C34 N5 C33 C32 -72.5(6) . . . . ? Cu2 N5 C33 C32 43.6(5) 2_575 . . . ? N4 C32 C33 N5 -49.2(6) . . . . ? C33 N5 C35 C36 -161.4(5) . . . . ? C34 N5 C35 C36 73.9(5) . . . . ? Cu2 N5 C35 C36 -42.0(5) 2_575 . . . ? N5 C35 C36 N6 50.2(6) . . . . ? C37 N6 C36 C35 81.6(6) . . . . ? C38 N6 C36 C35 -161.6(5) . . . . ? Cu2 N6 C36 C35 -33.0(5) 2_575 . . . ? C37 N6 C38 C39 178.8(5) . . . . ? C36 N6 C38 C39 61.6(7) . . . . ? Cu2 N6 C38 C39 -61.9(6) 2_575 . . . ? N6 C38 C39 C44 85.3(7) . . . . ? N6 C38 C39 C40 -98.5(7) . . . . ? C44 C39 C40 C41 -0.7(9) . . . . ? C38 C39 C40 C41 -177.1(5) . . . . ? C39 C40 C41 C42 1.1(9) . . . . ? C40 C41 C42 C43 -0.7(9) . . . . ? C40 C41 C42 C15 174.4(5) . . . . ? N1 C15 C42 C43 -88.2(7) . . . . ? N1 C15 C42 C41 96.8(6) . . . . ? C41 C42 C43 C44 0.0(8) . . . . ? C15 C42 C43 C44 -175.0(5) . . . . ? C40 C39 C44 C43 0.1(8) . . . . ? C38 C39 C44 C43 176.3(5) . . . . ? C42 C43 C44 C39 0.3(8) . . . . ? C2A N1A C1A O1A -174.9(8) . . . . ? C3A N1A C1A O1A -0.2(12) . . . . ? C3C N1C C1C O1C 175.5(11) . . . . ? C2C N1C C1C O1C -3.8(17) . . . . ? O1O S1O C1O F2O 171.9(8) . . . . ? O2O S1O C1O F2O -52.9(10) . . . . ? O3O S1O C1O F2O 59.0(9) . . . . ? O1O S1O C1O F1O -62.3(8) . . . . ? O2O S1O C1O F1O 72.8(7) . . . . ? O3O S1O C1O F1O -175.2(6) . . . . ? O1O S1O C1O F3O 54.9(10) . . . . ? O2O S1O C1O F3O -170.0(8) . . . . ? O3O S1O C1O F3O -58.0(9) . . . . ? O2Q S1Q C1Q F1Q 52.9(7) . . . . ? O1Q S1Q C1Q F1Q 179.9(6) . . . . ? O3Q S1Q C1Q F1Q -63.7(6) . . . . ? O2Q S1Q C1Q F3Q 177.2(5) . . . . ? O1Q S1Q C1Q F3Q -55.7(7) . . . . ? O3Q S1Q C1Q F3Q 60.7(6) . . . . ? O2Q S1Q C1Q F2Q -67.7(6) . . . . ? O1Q S1Q C1Q F2Q 59.4(6) . . . . ? O3Q S1Q C1Q F2Q 175.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 29.65 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.948 _refine_diff_density_min -1.108 _refine_diff_density_rms 0.129 #===END data_lgl2p34g(4ClO4)_CCDC648099 _database_code_depnum_ccdc_archive 'CCDC 648099' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H111 Cu4 N12 O10, 6(C2 H3 N), 4(Cl O4), H2 O' _chemical_formula_sum 'C100 H131 Cl4 Cu4 N18 O27' _chemical_formula_weight 2413.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.585(4) _cell_length_b 19.674(6) _cell_length_c 22.666(7) _cell_angle_alpha 74.847(5) _cell_angle_beta 71.428(5) _cell_angle_gamma 69.732(5) _cell_volume 5699(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2514 _exptl_absorpt_coefficient_mu 0.909 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 87725 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.1335 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.52 _reflns_number_total 27652 _reflns_number_gt 12824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER Shelxtl' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997), platon' _computing_molecular_graphics ? _computing_publication_material ? 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 0.000 0.500 0.500 605.8 104.6 _platon_squeeze_details ; ? ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The SQUEEZE option of the PLATON Program (Spek, A. L. (2005). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, THe Netherlands) was used to eliminate electron density from disordered CH3CN solvent molecules. Those solvent molecule are, however, included in the reported chemical formula and derived values (reported crystal-data formula, formula weight,Dx, Mu and F(000)). The phenil ring geometry was fixed to a regular hexagon for the rings C10-C15, C25-C30, C40-C45, C55-C60, C63-C68, C77-82, C83-c88 ; _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^)+(0.1479P)^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 27652 _refine_ls_number_parameters 1197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1653 _refine_ls_R_factor_gt 0.0910 _refine_ls_wR_factor_ref 0.2790 _refine_ls_wR_factor_gt 0.2471 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.019 _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 1.13427(5) 0.20321(3) 0.45956(3) 0.03382(17) Uani 1 1 d . . . O1 O 1.0163(3) 0.1962(2) 0.52803(17) 0.0411(9) Uani 1 1 d . . . N1 N 1.1910(3) 0.0891(2) 0.4726(2) 0.0374(11) Uani 1 1 d . . . O1X O 1.2105(3) 0.2253(2) 0.51894(18) 0.0470(10) Uani 1 1 d . . . H1XA H 1.2222 0.2667 0.5038 0.056 Uiso 1 1 d R . . H1XB H 1.2667 0.1924 0.5190 0.056 Uiso 1 1 d R . . C1 C 1.1169(4) 0.0485(3) 0.4815(3) 0.0476(16) Uani 1 1 d . . . H1A H 1.0593 0.0645 0.5159 0.057 Uiso 1 1 calc R . . H1B H 1.1480 -0.0035 0.4940 0.057 Uiso 1 1 calc R . . Cu2 Cu 0.70521(5) 0.30544(3) 0.33771(3) 0.03575(17) Uani 1 1 d . . . N2 N 1.2450(3) 0.2043(2) 0.3785(2) 0.0372(11) Uani 1 1 d . . . O2 O 1.0520(3) 0.2132(3) 0.61008(19) 0.0548(11) Uani 1 1 d . . . C2 C 1.2298(5) 0.0632(3) 0.5320(3) 0.0491(16) Uani 1 1 d . . . H2A H 1.2675 0.0122 0.5344 0.074 Uiso 1 1 calc R . . H2B H 1.1736 0.0695 0.5685 0.074 Uiso 1 1 calc R . . H2C H 1.2726 0.0915 0.5306 0.074 Uiso 1 1 calc R . . Cu3 Cu 0.34719(5) 0.39610(4) 1.01788(3) 0.03846(18) Uani 1 1 d . . . N3 N 1.0634(3) 0.3068(2) 0.4161(2) 0.0401(11) Uani 1 1 d . . . O3 O 0.2905(4) 0.0874(3) 0.8295(2) 0.0701(14) Uani 1 1 d . . . C3 C 1.2784(4) 0.0706(3) 0.4158(3) 0.0439(14) Uani 1 1 d . . . H3A H 1.3413 0.0653 0.4250 0.053 Uiso 1 1 calc R . . H3B H 1.2823 0.0245 0.4058 0.053 Uiso 1 1 calc R . . Cu4 Cu 0.18935(5) 0.11044(4) 0.97501(4) 0.0457(2) Uani 1 1 d . . . O4 O 0.3098(3) 0.1202(2) 0.9109(2) 0.0489(11) Uani 1 1 d . . . N4 N 0.6646(4) 0.4168(2) 0.3023(2) 0.0452(12) Uani 1 1 d . . . C4 C 1.2621(4) 0.1318(3) 0.3602(3) 0.0419(14) Uani 1 1 d . . . H4A H 1.3208 0.1231 0.3247 0.050 Uiso 1 1 calc R . . H4B H 1.2040 0.1328 0.3475 0.050 Uiso 1 1 calc R . . O4X O 0.1298(3) 0.0667(3) 0.9182(3) 0.0851(17) Uani 1 1 d . . . H4XB H 0.0711 0.0943 0.9159 0.102 Uiso 1 1 d R . . H4XA H 0.1689 0.0655 0.8813 0.128 Uiso 1 1 d R . . O5 O 0.7101(3) 0.31591(19) 0.41823(17) 0.0416(9) Uani 1 1 d . . . N5 N 0.6880(4) 0.2895(3) 0.2600(2) 0.0421(12) Uani 1 1 d . . . C5 C 1.3410(4) 0.2092(3) 0.3836(3) 0.0486(15) Uani 1 1 d . . . H5A H 1.3347 0.2593 0.3839 0.073 Uiso 1 1 calc R . . H5B H 1.3944 0.1924 0.3482 0.073 Uiso 1 1 calc R . . H5C H 1.3561 0.1790 0.4220 0.073 Uiso 1 1 calc R . . N6 N 0.7938(3) 0.1976(2) 0.3461(2) 0.0344(10) Uani 1 1 d . . . O6 O 0.5628(3) 0.2980(2) 0.4321(2) 0.0508(11) Uani 1 1 d . . . C6 C 1.2083(4) 0.2657(3) 0.3290(3) 0.0438(14) Uani 1 1 d . . . H6A H 1.2273 0.2480 0.2894 0.053 Uiso 1 1 calc R . . H6B H 1.2391 0.3045 0.3223 0.053 Uiso 1 1 calc R . . O7 O 0.3591(3) 0.37233(19) 0.93850(17) 0.0404(9) Uani 1 1 d . . . N7 N 0.2420(3) 0.4981(2) 1.0070(2) 0.0387(11) Uani 1 1 d . . . C7 C 1.0954(4) 0.2954(3) 0.3495(3) 0.0426(14) Uani 1 1 d . . . H7A H 1.0730 0.3418 0.3225 0.051 Uiso 1 1 calc R . . H7B H 1.0642 0.2612 0.3454 0.051 Uiso 1 1 calc R . . O8 O 0.4907(3) 0.4113(2) 0.92373(18) 0.0493(11) Uani 1 1 d . . . N8 N 0.3510(3) 0.4194(2) 1.0964(2) 0.0379(11) Uani 1 1 d . . . C8 C 1.1015(5) 0.3635(3) 0.4237(3) 0.0482(15) Uani 1 1 d . . . H8A H 1.0779 0.4088 0.3968 0.072 Uiso 1 1 calc R . . H8B H 1.1740 0.3478 0.4124 0.072 Uiso 1 1 calc R . . H8C H 1.0774 0.3708 0.4669 0.072 Uiso 1 1 calc R . . N9 N 0.4050(3) 0.2872(2) 1.0546(2) 0.0403(11) Uani 1 1 d . . . C9 C 0.9505(4) 0.3281(3) 0.4395(3) 0.0422(14) Uani 1 1 d . . . H9A H 0.9323 0.3341 0.4833 0.051 Uiso 1 1 calc R . . H9B H 0.9268 0.2883 0.4380 0.051 Uiso 1 1 calc R . . N10 N 0.2717(4) 0.0090(2) 1.0177(3) 0.0532(14) Uani 1 1 d . . . N11 N 0.0799(4) 0.1067(3) 1.0541(3) 0.0582(16) Uani 1 1 d . . . N12 N 0.1151(3) 0.2234(2) 0.9595(2) 0.0429(12) Uani 1 1 d . . . C10 C 0.8958(3) 0.39987(18) 0.4012(2) 0.0565(18) Uani 1 1 d G . . C11 C 0.8558(3) 0.39417(16) 0.3553(2) 0.0452(15) Uani 1 1 d G . . H11A H 0.8696 0.3486 0.3443 0.054 Uiso 1 1 calc R . . C12 C 0.7950(4) 0.4565(2) 0.3258(2) 0.0577(18) Uani 1 1 d G . . C13 C 0.7743(4) 0.52457(17) 0.3422(3) 0.093(3) Uani 1 1 d G . . H13A H 0.7337 0.5663 0.3225 0.111 Uiso 1 1 calc R . . C14 C 0.8143(5) 0.53027(17) 0.3882(3) 0.103(3) Uani 1 1 d G . . H14A H 0.8004 0.5758 0.3992 0.124 Uiso 1 1 calc R . . C15 C 0.8750(4) 0.4679(2) 0.4177(2) 0.074(2) Uani 1 1 d G . . H15A H 0.9018 0.4717 0.4485 0.089 Uiso 1 1 calc R . . C16 C 0.7508(5) 0.4512(3) 0.2761(3) 0.0623(19) Uani 1 1 d . . . H16A H 0.8037 0.4222 0.2462 0.075 Uiso 1 1 calc R . . H16B H 0.7268 0.5001 0.2531 0.075 Uiso 1 1 calc R . . C17 C 0.5818(6) 0.4580(3) 0.3494(3) 0.074(2) Uani 1 1 d . . . H17A H 0.5326 0.4314 0.3694 0.111 Uiso 1 1 calc R . . H17B H 0.5503 0.5056 0.3285 0.111 Uiso 1 1 calc R . . H17C H 0.6089 0.4636 0.3807 0.111 Uiso 1 1 calc R . . C18 C 0.6237(5) 0.4218(3) 0.2490(3) 0.0538(17) Uani 1 1 d . . . H18A H 0.6254 0.4677 0.2202 0.065 Uiso 1 1 calc R . . H18B H 0.5541 0.4204 0.2645 0.065 Uiso 1 1 calc R . . C19 C 0.6869(5) 0.3580(3) 0.2153(3) 0.0532(17) Uani 1 1 d . . . H19A H 0.6590 0.3590 0.1814 0.064 Uiso 1 1 calc R . . H19B H 0.7552 0.3616 0.1970 0.064 Uiso 1 1 calc R . . C20 C 0.5895(4) 0.2715(4) 0.2736(3) 0.0511(16) Uani 1 1 d . . . H20A H 0.5343 0.3115 0.2895 0.077 Uiso 1 1 calc R . . H20B H 0.5901 0.2276 0.3046 0.077 Uiso 1 1 calc R . . H20C H 0.5818 0.2641 0.2355 0.077 Uiso 1 1 calc R . . C21 C 0.7756(5) 0.2261(3) 0.2373(3) 0.0499(16) Uani 1 1 d . . . H21A H 0.8364 0.2417 0.2184 0.060 Uiso 1 1 calc R . . H21B H 0.7620 0.2083 0.2059 0.060 Uiso 1 1 calc R . . C22 C 0.7894(5) 0.1661(3) 0.2938(3) 0.0460(15) Uani 1 1 d . . . H22A H 0.7335 0.1448 0.3080 0.055 Uiso 1 1 calc R . . H22B H 0.8514 0.1275 0.2821 0.055 Uiso 1 1 calc R . . C23 C 0.7615(4) 0.1524(3) 0.4071(3) 0.0434(14) Uani 1 1 d . . . H23A H 0.7716 0.1692 0.4401 0.065 Uiso 1 1 calc R . . H23B H 0.8007 0.1020 0.4061 0.065 Uiso 1 1 calc R . . H23C H 0.6913 0.1565 0.4150 0.065 Uiso 1 1 calc R . . C24 C 0.8956(4) 0.2039(3) 0.3390(3) 0.0371(13) Uani 1 1 d . . . H24A H 0.9087 0.2492 0.3262 0.045 Uiso 1 1 calc R . . C25 C 0.9768(2) 0.13416(15) 0.35328(16) 0.0374(13) Uani 1 1 d G . . C26 C 1.0035(2) 0.12100(16) 0.40976(15) 0.0346(12) Uani 1 1 d G . . H26A H 0.9704 0.1541 0.4379 0.042 Uiso 1 1 calc R . . C27 C 1.0797(3) 0.05842(18) 0.42425(16) 0.0412(14) Uani 1 1 d G . . C28 C 1.1292(3) 0.00900(16) 0.3823(2) 0.0535(17) Uani 1 1 d G . . H28A H 1.1801 -0.0329 0.3920 0.064 Uiso 1 1 calc R . . C29 C 1.1024(3) 0.02216(19) 0.32578(19) 0.070(2) Uani 1 1 d G . . H29A H 1.1356 -0.0109 0.2977 0.084 Uiso 1 1 calc R . . C30 C 1.0262(3) 0.0847(2) 0.31129(15) 0.0552(17) Uani 1 1 d G . . H30A H 1.0084 0.0935 0.2735 0.066 Uiso 1 1 calc R . . C31 C 0.1368(4) 0.4945(3) 1.0163(3) 0.0386(13) Uani 1 1 d . . . H31A H 0.0912 0.5440 1.0151 0.046 Uiso 1 1 calc R . . H31B H 0.1161 0.4668 1.0579 0.046 Uiso 1 1 calc R . . C32 C 0.2765(5) 0.5416(3) 0.9426(3) 0.0494(16) Uani 1 1 d . . . H32A H 0.2311 0.5905 0.9392 0.074 Uiso 1 1 calc R . . H32B H 0.2770 0.5179 0.9105 0.074 Uiso 1 1 calc R . . H32C H 0.3434 0.5440 0.9374 0.074 Uiso 1 1 calc R . . C33 C 0.2426(5) 0.5351(3) 1.0567(3) 0.0476(15) Uani 1 1 d . . . H33A H 0.2966 0.5583 1.0413 0.057 Uiso 1 1 calc R . . H33B H 0.1790 0.5728 1.0671 0.057 Uiso 1 1 calc R . . C34 C 0.2579(4) 0.4792(3) 1.1138(3) 0.0432(14) Uani 1 1 d . . . H34A H 0.2634 0.5017 1.1454 0.052 Uiso 1 1 calc R . . H34B H 0.2005 0.4595 1.1317 0.052 Uiso 1 1 calc R . . C35 C 0.4414(5) 0.4439(4) 1.0843(3) 0.0568(17) Uani 1 1 d . . . H35A H 0.5010 0.4050 1.0712 0.085 Uiso 1 1 calc R . . H35B H 0.4429 0.4561 1.1222 0.085 Uiso 1 1 calc R . . H35C H 0.4389 0.4863 1.0515 0.085 Uiso 1 1 calc R . . C36 C 0.3541(5) 0.3523(3) 1.1439(3) 0.0475(15) Uani 1 1 d . . . H36A H 0.2876 0.3448 1.1600 0.057 Uiso 1 1 calc R . . H36B H 0.3754 0.3563 1.1789 0.057 Uiso 1 1 calc R . . C37 C 0.4298(4) 0.2872(3) 1.1118(3) 0.0531(17) Uani 1 1 d . . . H37A H 0.4978 0.2912 1.1015 0.064 Uiso 1 1 calc R . . H37B H 0.4273 0.2413 1.1406 0.064 Uiso 1 1 calc R . . C38 C 0.4940(5) 0.2460(3) 1.0128(3) 0.0595(19) Uani 1 1 d . . . H38A H 0.5236 0.1997 1.0364 0.089 Uiso 1 1 calc R . . H38B H 0.5422 0.2736 0.9954 0.089 Uiso 1 1 calc R . . H38C H 0.4747 0.2375 0.9792 0.089 Uiso 1 1 calc R . . C39 C 0.3187(4) 0.2572(3) 1.0677(3) 0.0487(16) Uani 1 1 d . . . H39A H 0.2565 0.2877 1.0614 0.058 Uiso 1 1 calc R . . C40 C 0.3345(3) 0.17669(14) 1.09135(18) 0.0461(15) Uani 1 1 d G . . C41 C 0.3499(3) 0.13099(18) 1.04944(15) 0.0451(16) Uani 1 1 d G . . H41A H 0.3513 0.1505 1.0072 0.054 Uiso 1 1 calc R . . C42 C 0.3633(3) 0.05606(17) 1.0706(2) 0.0527(18) Uani 1 1 d G . . C43 C 0.3613(3) 0.02683(15) 1.1337(2) 0.062(2) Uani 1 1 d G . . H43A H 0.3703 -0.0233 1.1479 0.074 Uiso 1 1 calc R . . C44 C 0.3459(3) 0.0725(2) 1.17565(16) 0.069(2) Uani 1 1 d G . . H44A H 0.3446 0.0530 1.2179 0.083 Uiso 1 1 calc R . . C45 C 0.3325(3) 0.1475(2) 1.15446(17) 0.0574(18) Uani 1 1 d G . . H45A H 0.3222 0.1780 1.1825 0.069 Uiso 1 1 calc R . . C46 C 0.3708(4) 0.0080(3) 1.0247(4) 0.064(2) Uani 1 1 d . . . H46A H 0.4323 -0.0196 1.0028 0.077 Uiso 1 1 calc R . . C47 C 0.2958(6) -0.0475(3) 0.9795(4) 0.076(2) Uani 1 1 d . . . H47A H 0.3146 -0.0953 1.0044 0.114 Uiso 1 1 calc R . . H47B H 0.3509 -0.0418 0.9435 0.114 Uiso 1 1 calc R . . H47C H 0.2378 -0.0423 0.9656 0.114 Uiso 1 1 calc R . . C48 C 0.2019(5) -0.0101(3) 1.0802(3) 0.0610(19) Uani 1 1 d . . . H48A H 0.1639 -0.0394 1.0756 0.073 Uiso 1 1 calc R . . H48B H 0.2410 -0.0390 1.1105 0.073 Uiso 1 1 calc R . . C49 C 0.1308(5) 0.0585(4) 1.1037(3) 0.065(2) Uani 1 1 d . . . H49A H 0.0808 0.0461 1.1415 0.078 Uiso 1 1 calc R . . H49B H 0.1678 0.0842 1.1144 0.078 Uiso 1 1 calc R . . C50 C 0.0000(5) 0.0769(4) 1.0517(4) 0.083(3) Uani 1 1 d . . . H50A H -0.0518 0.0799 1.0905 0.125 Uiso 1 1 calc R . . H50B H 0.0294 0.0265 1.0459 0.125 Uiso 1 1 calc R . . H50C H -0.0288 0.1051 1.0170 0.125 Uiso 1 1 calc R . . C51 C 0.0315(6) 0.1829(4) 1.0679(4) 0.081(3) Uani 1 1 d . . . H51A H -0.0411 0.1914 1.0802 0.097 Uiso 1 1 calc R . . H51B H 0.0509 0.1859 1.1041 0.097 Uiso 1 1 calc R . . C52 C 0.0520(10) 0.2360(4) 1.0228(4) 0.172(7) Uani 1 1 d . . . H52A H 0.0256 0.2839 1.0310 0.207 Uiso 1 1 calc R . . C53 C 0.0581(7) 0.2423(5) 0.9133(5) 0.121(4) Uani 1 1 d . . . H53A H 0.0221 0.2069 0.9211 0.181 Uiso 1 1 calc R . . H53B H 0.1032 0.2424 0.8718 0.181 Uiso 1 1 calc R . . H53C H 0.0109 0.2903 0.9160 0.181 Uiso 1 1 calc R . . C54 C 0.1853(5) 0.2667(3) 0.9394(4) 0.070(2) Uani 1 1 d . . . H54A H 0.2544 0.2435 0.9315 0.083 Uiso 1 1 calc R . . C55 C 0.1467(3) 0.34974(13) 0.93130(17) 0.0455(15) Uani 1 1 d G . . C56 C 0.1473(3) 0.38373(16) 0.97772(14) 0.0422(14) Uani 1 1 d G . . H56A H 0.1618 0.3556 1.0153 0.051 Uiso 1 1 calc R . . C57 C 0.1261(3) 0.45975(17) 0.96794(15) 0.0394(14) Uani 1 1 d G . . C58 C 0.1044(3) 0.50179(13) 0.91173(17) 0.0411(14) Uani 1 1 d G . . H58A H 0.0903 0.5527 0.9052 0.049 Uiso 1 1 calc R . . C59 C 0.1038(3) 0.46780(18) 0.86530(14) 0.0475(15) Uani 1 1 d G . . H59A H 0.0893 0.4959 0.8277 0.057 Uiso 1 1 calc R . . C60 C 0.1250(3) 0.39178(19) 0.87508(16) 0.0491(16) Uani 1 1 d G . . H60A H 0.1246 0.3690 0.8440 0.059 Uiso 1 1 calc R . . C62 C 0.9959(4) 0.2028(3) 0.5858(3) 0.0403(14) Uani 1 1 d . . . C63 C 0.8952(2) 0.19189(19) 0.62583(14) 0.0397(13) Uani 1 1 d G . . C64 C 0.8245(2) 0.18909(19) 0.59812(11) 0.0382(13) Uani 1 1 d G . . H64A H 0.8378 0.1956 0.5544 0.046 Uiso 1 1 calc R . . C65 C 0.7339(2) 0.17654(19) 0.63576(15) 0.0414(14) Uani 1 1 d G . . H65A H 0.6866 0.1747 0.6172 0.050 Uiso 1 1 calc R . . C66 C 0.7140(2) 0.16679(19) 0.70112(15) 0.0359(13) Uani 1 1 d G . . C67 C 0.7848(3) 0.1696(2) 0.72884(11) 0.0411(14) Uani 1 1 d G . . H67A H 0.7715 0.1631 0.7726 0.049 Uiso 1 1 calc R . . C68 C 0.8754(2) 0.1821(2) 0.69120(15) 0.0459(15) Uani 1 1 d G . . H68A H 0.9227 0.1840 0.7097 0.055 Uiso 1 1 calc R . . C69 C 0.6165(2) 0.15165(17) 0.74213(15) 0.0357(13) Uani 1 1 d G . . C70 C 0.5712(3) 0.11433(19) 0.72084(16) 0.0454(15) Uani 1 1 d G . . H70A H 0.6014 0.0984 0.6821 0.054 Uiso 1 1 calc R . . C71 C 0.4806(3) 0.1008(2) 0.75743(17) 0.0479(15) Uani 1 1 d G . . H71A H 0.4503 0.0759 0.7432 0.057 Uiso 1 1 calc R . . C72 C 0.4353(3) 0.12469(19) 0.81535(17) 0.0400(14) Uani 1 1 d G . . C73 C 0.4806(3) 0.16202(18) 0.83663(16) 0.0383(13) Uani 1 1 d G . . H73A H 0.4503 0.1780 0.8753 0.046 Uiso 1 1 calc R . . C74 C 0.5712(2) 0.17550(18) 0.80002(16) 0.0377(13) Uani 1 1 d G . . H74A H 0.6015 0.2005 0.8143 0.045 Uiso 1 1 calc R . . C75 C 0.3364(5) 0.1108(3) 0.8528(3) 0.0541(18) Uani 1 1 d . . . C76 C 0.6235(5) 0.3108(3) 0.4528(3) 0.0439(15) Uani 1 1 d . . . C77 C 0.5940(3) 0.32275(18) 0.52014(12) 0.0407(14) Uani 1 1 d G . . C78 C 0.5130(3) 0.3016(2) 0.56396(16) 0.0448(15) Uani 1 1 d G . . H78A H 0.4749 0.2811 0.5516 0.054 Uiso 1 1 calc R . . C79 C 0.4890(2) 0.3111(2) 0.62631(15) 0.0487(15) Uani 1 1 d G . . H79A H 0.4349 0.2969 0.6556 0.058 Uiso 1 1 calc R . . C80 C 0.5461(3) 0.34167(19) 0.64486(12) 0.0337(12) Uani 1 1 d G . . C81 C 0.6271(3) 0.3628(2) 0.60104(15) 0.0440(14) Uani 1 1 d G . . H81A H 0.6652 0.3833 0.6134 0.053 Uiso 1 1 calc R . . C82 C 0.6510(2) 0.3534(2) 0.53868(14) 0.0449(14) Uani 1 1 d G . . H82A H 0.7052 0.3675 0.5094 0.054 Uiso 1 1 calc R . . C83 C 0.5204(2) 0.35136(17) 0.71291(11) 0.0342(12) Uani 1 1 d G . . C84 C 0.5868(2) 0.3694(2) 0.73449(14) 0.0402(13) Uani 1 1 d G . . H84A H 0.6483 0.3739 0.7075 0.048 Uiso 1 1 calc R . . C85 C 0.5612(2) 0.3807(2) 0.79644(15) 0.0417(14) Uani 1 1 d G . . H85A H 0.6056 0.3928 0.8109 0.050 Uiso 1 1 calc R . . C86 C 0.4692(3) 0.37392(18) 0.83682(12) 0.0347(13) Uani 1 1 d G . . C87 C 0.4029(2) 0.35586(18) 0.81524(14) 0.0377(13) Uani 1 1 d G . . H87A H 0.3414 0.3513 0.8423 0.045 Uiso 1 1 calc R . . C88 C 0.4285(2) 0.34458(18) 0.75329(15) 0.0348(12) Uani 1 1 d G . . H88A H 0.3841 0.3325 0.7389 0.042 Uiso 1 1 calc R . . C89 C 0.4410(4) 0.3876(3) 0.9037(3) 0.0439(15) Uani 1 1 d . . . Cl1S Cl 0.73366(12) 0.25847(9) 0.05383(9) 0.0575(4) Uani 1 1 d . . . O1S O 0.6761(12) 0.3102(7) 0.0186(8) 0.063(4) Uani 0.519(7) 1 d P A 1 O2S O 0.6720(9) 0.2562(8) 0.1161(4) 0.089(4) Uani 0.519(7) 1 d P A 1 O3S O 0.7559(14) 0.1985(6) 0.0308(7) 0.114(6) Uani 0.519(7) 1 d P A 1 O4S O 0.8140(9) 0.2880(8) 0.0365(13) 0.201(12) Uani 0.519(7) 1 d P A 1 O1S' O 0.6654(12) 0.3266(6) 0.0302(7) 0.042(3) Uani 0.481(7) 1 d P A 2 O2S' O 0.6863(11) 0.2017(9) 0.0918(14) 0.193(12) Uani 0.481(7) 1 d P A 2 O3S' O 0.8049(10) 0.2156(12) 0.0051(9) 0.146(8) Uani 0.481(7) 1 d P A 2 O4S' O 0.7980(6) 0.2676(5) 0.0861(4) 0.039(2) Uani 0.481(7) 1 d P A 2 Cl1T Cl 0.31426(15) 0.45438(10) 0.28989(10) 0.0675(5) Uani 1 1 d . . . O2T O 0.3522(8) 0.3905(7) 0.3315(6) 0.220(5) Uani 1 1 d . . . O1T O 0.3973(6) 0.4518(5) 0.2328(3) 0.148(3) Uani 1 1 d . . . O3T O 0.2366(7) 0.4335(5) 0.2845(5) 0.180(4) Uani 1 1 d . . . O4T O 0.2816(10) 0.5149(7) 0.3005(12) 0.504(16) Uani 1 1 d . . . Cl1U Cl 0.5764(2) 0.02096(17) 0.3710(2) 0.1483(14) Uani 1 1 d . . . O4U O 0.5224(6) 0.0150(6) 0.4412(5) 0.177(4) Uani 1 1 d . . . O3U O 0.5084(6) 0.0227(4) 0.3370(4) 0.140(3) Uani 1 1 d . . . O1U O 0.6602(6) -0.0377(7) 0.3537(5) 0.226(6) Uani 1 1 d . . . O2U O 0.6043(7) 0.0815(5) 0.3582(4) 0.162(3) Uani 1 1 d . . . Cl1V Cl 0.04716(11) 0.31432(8) 0.18299(7) 0.0446(4) Uani 1 1 d . . . O1V O -0.0565(7) 0.3375(7) 0.2147(8) 0.101(7) Uani 0.519(7) 1 d P A 1 O1V' O -0.0182(17) 0.3470(12) 0.2278(10) 0.145(9) Uani 0.481(7) 1 d P A 2 O2V O 0.0992(9) 0.3611(6) 0.1839(7) 0.096(4) Uani 0.519(7) 1 d P A 1 O2V' O 0.0959(9) 0.3581(7) 0.1298(6) 0.095(5) Uani 0.481(7) 1 d P A 2 O3V O 0.0960(14) 0.2522(10) 0.2205(7) 0.094(6) Uani 0.519(7) 1 d P A 1 O3V' O 0.0883(19) 0.2408(10) 0.1952(13) 0.176(13) Uani 0.481(7) 1 d P A 2 O4V O 0.0565(11) 0.3110(7) 0.1236(5) 0.080(4) Uani 0.519(7) 1 d P A 1 O4V' O -0.0159(16) 0.3145(13) 0.1458(10) 0.150(8) Uani 0.481(7) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0341(3) 0.0251(3) 0.0350(3) 0.0018(3) -0.0015(3) -0.0115(3) O1 0.036(2) 0.041(2) 0.039(2) 0.0036(17) -0.0051(17) -0.0128(17) N1 0.037(2) 0.030(2) 0.042(3) 0.002(2) -0.013(2) -0.0085(19) O1X 0.040(2) 0.046(2) 0.051(2) -0.0060(19) -0.0043(19) -0.0154(18) C1 0.048(3) 0.026(3) 0.061(4) 0.012(3) -0.018(3) -0.013(3) Cu2 0.0438(4) 0.0228(3) 0.0329(3) 0.0019(3) -0.0072(3) -0.0072(3) N2 0.040(2) 0.033(2) 0.040(2) 0.001(2) -0.007(2) -0.021(2) O2 0.051(2) 0.082(3) 0.039(2) -0.013(2) 0.001(2) -0.037(2) C2 0.047(3) 0.033(3) 0.063(4) 0.005(3) -0.017(3) -0.012(3) Cu3 0.0384(4) 0.0286(3) 0.0430(4) -0.0064(3) 0.0040(3) -0.0159(3) N3 0.043(3) 0.027(2) 0.046(3) -0.003(2) 0.000(2) -0.018(2) O3 0.061(3) 0.086(3) 0.073(3) -0.040(3) 0.015(2) -0.042(3) C3 0.035(3) 0.028(3) 0.061(4) -0.006(3) -0.006(3) -0.006(2) Cu4 0.0322(4) 0.0269(3) 0.0681(5) -0.0141(3) 0.0122(3) -0.0145(3) O4 0.039(2) 0.032(2) 0.069(3) -0.0207(19) 0.009(2) -0.0145(17) N4 0.057(3) 0.028(2) 0.039(3) 0.008(2) -0.013(2) -0.008(2) C4 0.037(3) 0.038(3) 0.049(3) -0.011(3) -0.003(3) -0.012(2) O4X 0.047(3) 0.079(3) 0.134(5) -0.059(3) 0.026(3) -0.039(2) O5 0.059(3) 0.0256(19) 0.035(2) -0.0018(16) -0.0062(19) -0.0135(18) N5 0.046(3) 0.041(3) 0.031(2) 0.003(2) -0.006(2) -0.011(2) C5 0.044(3) 0.045(3) 0.058(4) -0.009(3) 0.000(3) -0.025(3) N6 0.038(2) 0.026(2) 0.036(2) -0.0058(18) -0.002(2) -0.0106(19) O6 0.056(3) 0.039(2) 0.057(3) -0.017(2) -0.023(2) 0.0018(19) C6 0.053(4) 0.031(3) 0.040(3) -0.005(2) 0.001(3) -0.016(3) O7 0.040(2) 0.033(2) 0.045(2) -0.0135(17) 0.0114(17) -0.0216(17) N7 0.050(3) 0.030(2) 0.033(2) -0.0074(19) 0.007(2) -0.022(2) C7 0.056(4) 0.030(3) 0.041(3) 0.007(2) -0.017(3) -0.018(3) O8 0.059(3) 0.051(2) 0.043(2) -0.0172(19) 0.010(2) -0.036(2) N8 0.037(2) 0.024(2) 0.045(3) 0.0015(19) -0.003(2) -0.0117(19) C8 0.065(4) 0.031(3) 0.055(4) -0.005(3) -0.016(3) -0.023(3) N9 0.034(2) 0.029(2) 0.055(3) -0.010(2) -0.004(2) -0.0099(19) C9 0.049(3) 0.019(3) 0.057(4) -0.004(2) -0.015(3) -0.008(2) N10 0.040(3) 0.026(2) 0.082(4) -0.013(2) 0.010(3) -0.016(2) N11 0.033(3) 0.032(3) 0.087(4) -0.006(3) 0.018(3) -0.014(2) N12 0.036(3) 0.031(2) 0.048(3) -0.004(2) 0.000(2) -0.006(2) C10 0.057(4) 0.018(3) 0.085(5) -0.004(3) -0.019(4) -0.002(3) C11 0.060(4) 0.016(3) 0.062(4) -0.002(3) -0.027(3) -0.006(2) C12 0.072(4) 0.024(3) 0.082(5) 0.001(3) -0.040(4) -0.008(3) C13 0.133(7) 0.033(4) 0.120(7) -0.017(4) -0.073(6) 0.007(4) C14 0.140(8) 0.031(4) 0.151(8) -0.037(5) -0.088(7) 0.022(4) C15 0.086(5) 0.054(4) 0.097(6) -0.032(4) -0.042(5) -0.005(4) C16 0.081(5) 0.029(3) 0.079(5) 0.023(3) -0.043(4) -0.022(3) C17 0.095(6) 0.027(3) 0.072(5) -0.004(3) -0.019(4) 0.011(3) C18 0.059(4) 0.042(4) 0.055(4) 0.017(3) -0.023(3) -0.019(3) C19 0.061(4) 0.053(4) 0.044(3) 0.009(3) -0.017(3) -0.022(3) C20 0.039(3) 0.050(4) 0.059(4) -0.004(3) -0.004(3) -0.017(3) C21 0.046(3) 0.058(4) 0.042(3) -0.017(3) -0.011(3) -0.004(3) C22 0.054(4) 0.034(3) 0.056(4) -0.017(3) -0.023(3) -0.006(3) C23 0.048(3) 0.022(3) 0.049(3) -0.003(2) -0.007(3) -0.002(2) C24 0.040(3) 0.025(3) 0.048(3) 0.004(2) -0.016(3) -0.015(2) C25 0.035(3) 0.023(3) 0.054(3) -0.004(2) -0.009(3) -0.013(2) C26 0.035(3) 0.021(2) 0.045(3) -0.007(2) -0.003(2) -0.010(2) C27 0.032(3) 0.018(2) 0.073(4) -0.001(3) -0.016(3) -0.009(2) C28 0.040(3) 0.028(3) 0.094(5) -0.022(3) -0.018(3) -0.001(2) C29 0.061(4) 0.041(4) 0.114(6) -0.040(4) -0.025(4) 0.002(3) C30 0.057(4) 0.041(3) 0.073(4) -0.026(3) -0.016(3) -0.009(3) C31 0.043(3) 0.020(2) 0.039(3) -0.005(2) 0.002(2) -0.003(2) C32 0.073(4) 0.034(3) 0.041(3) 0.007(3) -0.007(3) -0.032(3) C33 0.064(4) 0.030(3) 0.045(3) -0.011(3) 0.002(3) -0.020(3) C34 0.050(3) 0.035(3) 0.042(3) -0.006(3) -0.003(3) -0.018(3) C35 0.061(4) 0.065(4) 0.055(4) -0.008(3) -0.001(3) -0.044(3) C36 0.050(3) 0.037(3) 0.049(3) 0.000(3) -0.004(3) -0.018(3) C37 0.036(3) 0.037(3) 0.079(5) -0.003(3) -0.014(3) -0.007(3) C38 0.045(4) 0.036(3) 0.087(5) -0.016(3) 0.002(3) -0.011(3) C39 0.031(3) 0.034(3) 0.078(4) -0.008(3) -0.003(3) -0.015(2) C40 0.037(3) 0.031(3) 0.062(4) 0.001(3) -0.007(3) -0.011(2) C41 0.025(3) 0.025(3) 0.068(4) 0.010(3) 0.000(3) -0.010(2) C42 0.031(3) 0.021(3) 0.091(5) -0.005(3) 0.001(3) -0.008(2) C43 0.049(4) 0.027(3) 0.086(5) 0.017(3) -0.008(4) -0.010(3) C44 0.056(4) 0.053(4) 0.087(5) 0.019(4) -0.021(4) -0.020(3) C45 0.064(4) 0.048(4) 0.060(4) 0.009(3) -0.019(3) -0.027(3) C46 0.027(3) 0.027(3) 0.119(6) -0.017(3) 0.012(3) -0.010(2) C47 0.078(5) 0.025(3) 0.112(6) -0.025(4) 0.010(4) -0.021(3) C48 0.050(4) 0.035(3) 0.085(5) 0.000(3) 0.004(3) -0.023(3) C49 0.037(3) 0.044(4) 0.083(5) -0.007(4) 0.017(3) -0.008(3) C50 0.046(4) 0.063(5) 0.116(7) 0.004(4) 0.012(4) -0.030(4) C51 0.077(5) 0.047(4) 0.071(5) -0.002(4) 0.021(4) -0.002(4) C52 0.239(13) 0.028(4) 0.097(7) 0.000(4) 0.113(8) -0.005(6) C53 0.154(7) 0.069(5) 0.203(10) 0.045(6) -0.147(7) -0.066(5) C54 0.034(3) 0.027(3) 0.149(7) -0.025(4) -0.013(4) -0.011(3) C55 0.032(3) 0.027(3) 0.073(4) -0.018(3) -0.003(3) -0.006(2) C56 0.034(3) 0.027(3) 0.056(4) -0.003(3) -0.009(3) -0.001(2) C57 0.039(3) 0.023(3) 0.043(3) -0.006(2) 0.003(3) -0.005(2) C58 0.038(3) 0.023(3) 0.055(4) 0.000(3) -0.006(3) -0.010(2) C59 0.045(3) 0.053(4) 0.040(3) -0.002(3) 0.000(3) -0.023(3) C60 0.041(3) 0.044(3) 0.058(4) -0.012(3) 0.004(3) -0.020(3) C62 0.044(3) 0.041(3) 0.035(3) -0.008(2) 0.000(3) -0.020(3) C63 0.044(3) 0.029(3) 0.041(3) 0.003(2) -0.003(3) -0.017(2) C64 0.041(3) 0.023(3) 0.038(3) 0.000(2) 0.001(3) -0.009(2) C65 0.045(3) 0.022(3) 0.046(3) -0.002(2) -0.003(3) -0.008(2) C66 0.041(3) 0.014(2) 0.036(3) 0.000(2) 0.008(2) -0.009(2) C67 0.055(4) 0.033(3) 0.030(3) -0.002(2) 0.001(3) -0.019(3) C68 0.039(3) 0.050(3) 0.047(3) -0.014(3) 0.008(3) -0.024(3) C69 0.026(3) 0.016(2) 0.047(3) 0.003(2) 0.007(2) -0.005(2) C70 0.044(3) 0.024(3) 0.056(4) 0.003(3) -0.004(3) -0.012(2) C71 0.047(3) 0.035(3) 0.057(4) -0.012(3) 0.003(3) -0.017(3) C72 0.032(3) 0.025(3) 0.048(3) -0.001(2) 0.008(2) -0.011(2) C73 0.030(3) 0.022(3) 0.047(3) 0.002(2) 0.003(2) -0.006(2) C74 0.036(3) 0.019(2) 0.047(3) 0.002(2) 0.004(2) -0.014(2) C75 0.042(3) 0.039(3) 0.072(5) -0.010(3) 0.006(3) -0.018(3) C76 0.069(4) 0.012(2) 0.041(3) 0.002(2) -0.021(3) 0.001(3) C77 0.045(3) 0.021(3) 0.046(3) -0.002(2) -0.011(3) 0.001(2) C78 0.040(3) 0.043(3) 0.047(3) -0.021(3) -0.005(3) -0.003(3) C79 0.045(3) 0.047(3) 0.047(3) -0.014(3) 0.004(3) -0.014(3) C80 0.035(3) 0.020(2) 0.036(3) -0.004(2) -0.001(2) -0.003(2) C81 0.058(4) 0.032(3) 0.038(3) 0.001(2) -0.005(3) -0.020(3) C82 0.062(4) 0.040(3) 0.035(3) -0.002(3) -0.011(3) -0.021(3) C83 0.035(3) 0.017(2) 0.043(3) -0.005(2) -0.002(2) -0.005(2) C84 0.043(3) 0.040(3) 0.039(3) -0.014(2) 0.002(3) -0.019(3) C85 0.038(3) 0.039(3) 0.048(3) -0.012(3) -0.002(3) -0.015(2) C86 0.039(3) 0.015(2) 0.040(3) -0.007(2) 0.007(2) -0.010(2) C87 0.037(3) 0.016(2) 0.052(3) -0.001(2) -0.004(3) -0.010(2) C88 0.035(3) 0.032(3) 0.033(3) 0.004(2) -0.005(2) -0.014(2) C89 0.046(3) 0.025(3) 0.044(3) 0.000(2) 0.008(3) -0.012(2) Cl1S 0.0438(8) 0.0496(9) 0.0811(12) -0.0216(9) -0.0036(8) -0.0192(7) O1S 0.058(7) 0.054(7) 0.086(8) -0.065(6) 0.025(6) -0.029(6) O2S 0.087(8) 0.124(10) 0.039(5) -0.027(6) -0.026(5) 0.007(7) O3S 0.172(15) 0.024(5) 0.110(10) -0.018(6) 0.020(10) -0.030(7) O4S 0.030(6) 0.066(9) 0.43(3) -0.009(14) 0.025(12) -0.017(6) O1S' 0.052(7) 0.012(5) 0.062(8) -0.021(5) -0.002(6) -0.008(4) O2S' 0.080(9) 0.104(12) 0.36(3) 0.118(15) -0.089(14) -0.073(9) O3S' 0.048(7) 0.235(18) 0.187(15) -0.183(14) -0.063(9) 0.058(9) O4S' 0.030(5) 0.049(5) 0.043(5) -0.030(4) -0.014(4) 0.003(4) Cl1T 0.0728(12) 0.0503(10) 0.0868(13) -0.0130(9) -0.0374(11) -0.0100(9) O2T 0.154(8) 0.262(13) 0.224(11) 0.094(9) -0.088(8) -0.100(8) O1T 0.174(7) 0.235(9) 0.074(4) 0.016(5) -0.018(4) -0.152(7) O3T 0.173(7) 0.189(8) 0.194(9) 0.039(6) -0.018(6) -0.150(7) O4T 0.259(13) 0.171(8) 0.99(4) -0.337(16) 0.274(19) -0.162(9) Cl1U 0.0720(16) 0.105(2) 0.291(5) -0.106(3) -0.032(2) -0.0131(15) O4U 0.098(6) 0.224(10) 0.202(9) -0.120(8) 0.060(6) -0.064(6) O3U 0.107(5) 0.122(5) 0.205(8) -0.119(5) -0.019(5) -0.002(4) O1U 0.084(6) 0.304(15) 0.231(11) -0.124(10) -0.025(7) 0.062(7) O2U 0.216(8) 0.182(8) 0.172(8) -0.030(6) -0.070(7) -0.141(7) Cl1V 0.0439(8) 0.0366(7) 0.0453(8) 0.0017(6) 0.0004(7) -0.0186(6) O1V 0.014(4) 0.063(7) 0.152(14) 0.057(8) 0.015(6) -0.008(4) O1V' 0.16(2) 0.127(14) 0.110(13) -0.058(11) 0.042(14) -0.032(15) O2V 0.104(8) 0.083(8) 0.122(11) 0.017(7) -0.031(8) -0.075(7) O2V' 0.060(7) 0.086(9) 0.060(7) 0.035(7) 0.028(6) 0.002(6) O3V 0.100(9) 0.084(10) 0.068(7) -0.025(6) -0.046(7) 0.041(7) O3V' 0.139(17) 0.034(8) 0.25(3) 0.023(14) 0.023(19) 0.004(9) O4V 0.104(10) 0.089(8) 0.040(6) 0.001(5) -0.012(6) -0.033(8) O4V' 0.131(15) 0.22(2) 0.138(16) -0.055(14) -0.020(14) -0.095(16) _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 O1 1.934(4) . ? Cu1 N2 2.025(4) . ? Cu1 N3 2.082(4) . ? Cu1 N1 2.083(4) . ? Cu1 O1X 2.198(4) . ? O1 C62 1.278(6) . ? N1 C1 1.491(7) . ? N1 C3 1.515(7) . ? N1 C2 1.522(7) . ? C1 C27 1.503(7) . ? Cu2 O5 1.915(4) . ? Cu2 N5 1.972(5) . ? Cu2 N6 2.062(4) . ? Cu2 N4 2.068(4) . ? Cu2 C76 2.513(6) . ? N2 C5 1.478(7) . ? N2 C6 1.494(7) . ? N2 C4 1.506(7) . ? O2 C62 1.216(7) . ? Cu3 O7 1.916(4) . ? Cu3 N8 1.972(5) . ? Cu3 N9 2.063(4) . ? Cu3 N7 2.071(5) . ? Cu3 C89 2.532(6) . ? N3 C8 1.473(7) . ? N3 C7 1.482(7) . ? N3 C9 1.499(7) . ? O3 C75 1.227(8) . ? C3 C4 1.514(8) . ? Cu4 O4 1.922(4) . ? Cu4 N11 1.989(5) . ? Cu4 N12 2.098(4) . ? Cu4 N10 2.105(5) . ? Cu4 O4X 2.229(5) . ? O4 C75 1.293(8) . ? N4 C18 1.478(8) . ? N4 C17 1.486(8) . ? N4 C16 1.515(8) . ? O5 C76 1.279(7) . ? N5 C19 1.458(7) . ? N5 C21 1.505(7) . ? N5 C20 1.516(7) . ? N6 C23 1.469(7) . ? N6 C24 1.486(7) . ? N6 C22 1.502(7) . ? O6 C76 1.244(7) . ? C6 C7 1.503(8) . ? O7 C89 1.290(6) . ? N7 C33 1.496(7) . ? N7 C31 1.505(7) . ? N7 C32 1.515(6) . ? O8 C89 1.226(7) . ? N8 C36 1.466(7) . ? N8 C34 1.476(7) . ? N8 C35 1.477(7) . ? N9 C37 1.454(8) . ? N9 C38 1.458(7) . ? N9 C39 1.485(7) . ? C9 C10 1.550(6) . ? N10 C47 1.464(8) . ? N10 C46 1.496(8) . ? N10 C48 1.500(8) . ? N11 C49 1.485(9) . ? N11 C51 1.490(8) . ? N11 C50 1.495(9) . ? N12 C53 1.436(9) . ? N12 C54 1.445(7) . ? N12 C52 1.469(9) . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C12 C16 1.507(8) . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C18 C19 1.502(9) . ? C21 C22 1.510(8) . ? C24 C25 1.508(6) . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C31 C57 1.506(6) . ? C33 C34 1.484(8) . ? C36 C37 1.544(8) . ? C39 C40 1.493(6) . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C42 C46 1.537(8) . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C48 C49 1.495(9) . ? C51 C52 1.298(10) . ? C54 C55 1.513(6) . ? C55 C56 1.3900 . ? C55 C60 1.3900 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? C58 C59 1.3900 . ? C59 C60 1.3900 . ? C62 C63 1.514(6) . ? C63 C64 1.3900 . ? C63 C68 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? C66 C67 1.3900 . ? C66 C69 1.511(4) . ? C67 C68 1.3900 . ? C69 C74 1.390(2) . ? C69 C70 1.390(2) . ? C70 C71 1.390(2) . ? C71 C72 1.391(2) . ? C72 C73 1.390(2) . ? C72 C75 1.499(7) . ? C73 C74 1.391(2) . ? C76 C77 1.507(6) . ? C77 C78 1.3900 . ? C77 C82 1.3900 . ? C78 C79 1.3900 . ? C79 C80 1.3900 . ? C80 C81 1.3900 . ? C80 C83 1.514(3) . ? C81 C82 1.3900 . ? C83 C84 1.3900 . ? C83 C88 1.3900 . ? C84 C85 1.3900 . ? C85 C86 1.3900 . ? C86 C87 1.3900 . ? C86 C89 1.509(7) . ? C87 C88 1.3900 . ? Cl1S O3S 1.310(12) . ? Cl1S O1S 1.337(17) . ? Cl1S O4S 1.387(13) . ? Cl1S O2S 1.410(10) . ? Cl1S O4S' 1.440(8) . ? Cl1S O1S' 1.454(13) . ? Cl1S O2S' 1.456(13) . ? Cl1S O3S' 1.470(13) . ? Cl1T O4T 1.178(9) . ? Cl1T O3T 1.380(8) . ? Cl1T O2T 1.417(10) . ? Cl1T O1T 1.462(7) . ? Cl1U O2U 1.322(8) . ? Cl1U O1U 1.390(9) . ? Cl1U O3U 1.425(8) . ? Cl1U O4U 1.526(9) . ? Cl1V O1V' 1.286(18) . ? Cl1V O4V 1.327(11) . ? Cl1V O3V' 1.351(18) . ? Cl1V O2V 1.389(10) . ? Cl1V O3V 1.402(15) . ? Cl1V O1V 1.418(11) . ? Cl1V O2V' 1.427(10) . ? Cl1V O4V' 1.430(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 169.01(18) . . ? O1 Cu1 N3 94.35(16) . . ? N2 Cu1 N3 84.12(17) . . ? O1 Cu1 N1 90.44(17) . . ? N2 Cu1 N1 86.71(17) . . ? N3 Cu1 N1 155.91(19) . . ? O1 Cu1 O1X 93.47(16) . . ? N2 Cu1 O1X 97.45(16) . . ? N3 Cu1 O1X 104.53(17) . . ? N1 Cu1 O1X 98.71(17) . . ? C62 O1 Cu1 130.5(4) . . ? C1 N1 C3 110.4(5) . . ? C1 N1 C2 106.2(4) . . ? C3 N1 C2 109.5(4) . . ? C1 N1 Cu1 115.6(3) . . ? C3 N1 Cu1 106.6(3) . . ? C2 N1 Cu1 108.5(3) . . ? N1 C1 C27 114.8(4) . . ? O5 Cu2 N5 173.60(18) . . ? O5 Cu2 N6 92.95(16) . . ? N5 Cu2 N6 86.20(18) . . ? O5 Cu2 N4 95.83(17) . . ? N5 Cu2 N4 87.16(19) . . ? N6 Cu2 N4 158.27(18) . . ? O5 Cu2 C76 29.88(19) . . ? N5 Cu2 C76 144.0(2) . . ? N6 Cu2 C76 98.69(16) . . ? N4 Cu2 C76 98.82(17) . . ? C5 N2 C6 108.7(4) . . ? C5 N2 C4 109.7(4) . . ? C6 N2 C4 109.6(4) . . ? C5 N2 Cu1 115.9(4) . . ? C6 N2 Cu1 110.2(3) . . ? C4 N2 Cu1 102.5(3) . . ? O7 Cu3 N8 173.69(17) . . ? O7 Cu3 N9 92.09(18) . . ? N8 Cu3 N9 86.73(18) . . ? O7 Cu3 N7 96.39(17) . . ? N8 Cu3 N7 86.87(18) . . ? N9 Cu3 N7 158.30(17) . . ? O7 Cu3 C89 29.81(18) . . ? N8 Cu3 C89 144.2(2) . . ? N9 Cu3 C89 96.85(18) . . ? N7 Cu3 C89 100.43(17) . . ? C8 N3 C7 111.6(4) . . ? C8 N3 C9 109.4(4) . . ? C7 N3 C9 110.9(5) . . ? C8 N3 Cu1 110.9(4) . . ? C7 N3 Cu1 100.5(3) . . ? C9 N3 Cu1 113.3(3) . . ? C4 C3 N1 109.0(4) . . ? O4 Cu4 N11 166.2(2) . . ? O4 Cu4 N12 93.41(17) . . ? N11 Cu4 N12 85.33(19) . . ? O4 Cu4 N10 90.31(18) . . ? N11 Cu4 N10 86.2(2) . . ? N12 Cu4 N10 159.1(2) . . ? O4 Cu4 O4X 96.17(18) . . ? N11 Cu4 O4X 97.5(2) . . ? N12 Cu4 O4X 102.3(2) . . ? N10 Cu4 O4X 97.8(2) . . ? C75 O4 Cu4 128.9(4) . . ? C18 N4 C17 107.6(5) . . ? C18 N4 C16 107.2(5) . . ? C17 N4 C16 111.3(6) . . ? C18 N4 Cu2 103.9(4) . . ? C17 N4 Cu2 111.0(4) . . ? C16 N4 Cu2 115.3(4) . . ? N2 C4 C3 109.5(5) . . ? C76 O5 Cu2 101.9(4) . . ? C19 N5 C21 112.5(5) . . ? C19 N5 C20 110.4(5) . . ? C21 N5 C20 110.0(5) . . ? C19 N5 Cu2 106.2(4) . . ? C21 N5 Cu2 107.3(3) . . ? C20 N5 Cu2 110.2(4) . . ? C23 N6 C24 110.0(4) . . ? C23 N6 C22 109.5(4) . . ? C24 N6 C22 113.0(4) . . ? C23 N6 Cu2 113.8(3) . . ? C24 N6 Cu2 103.4(3) . . ? C22 N6 Cu2 107.1(3) . . ? N2 C6 C7 109.6(4) . . ? C89 O7 Cu3 102.6(4) . . ? C33 N7 C31 109.4(4) . . ? C33 N7 C32 108.9(4) . . ? C31 N7 C32 110.2(4) . . ? C33 N7 Cu3 104.6(3) . . ? C31 N7 Cu3 113.9(3) . . ? C32 N7 Cu3 109.6(3) . . ? N3 C7 C6 110.4(5) . . ? C36 N8 C34 112.1(4) . . ? C36 N8 C35 111.4(5) . . ? C34 N8 C35 110.7(5) . . ? C36 N8 Cu3 107.2(4) . . ? C34 N8 Cu3 106.1(3) . . ? C35 N8 Cu3 109.1(4) . . ? C37 N9 C38 109.5(5) . . ? C37 N9 C39 112.6(5) . . ? C38 N9 C39 110.6(5) . . ? C37 N9 Cu3 106.1(3) . . ? C38 N9 Cu3 115.4(4) . . ? C39 N9 Cu3 102.6(3) . . ? N3 C9 C10 114.0(4) . . ? C47 N10 C46 105.6(5) . . ? C47 N10 C48 108.8(5) . . ? C46 N10 C48 112.0(6) . . ? C47 N10 Cu4 109.8(5) . . ? C46 N10 Cu4 115.1(3) . . ? C48 N10 Cu4 105.4(3) . . ? C49 N11 C51 110.9(6) . . ? C49 N11 C50 109.2(5) . . ? C51 N11 C50 108.6(6) . . ? C49 N11 Cu4 105.6(3) . . ? C51 N11 Cu4 107.7(4) . . ? C50 N11 Cu4 114.9(5) . . ? C53 N12 C54 108.9(6) . . ? C53 N12 C52 113.4(8) . . ? C54 N12 C52 108.6(7) . . ? C53 N12 Cu4 112.0(5) . . ? C54 N12 Cu4 111.6(4) . . ? C52 N12 Cu4 102.4(4) . . ? C11 C10 C15 120.0 . . ? C11 C10 C9 118.3(3) . . ? C15 C10 C9 121.1(3) . . ? C10 C11 C12 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 C16 120.6(3) . . ? C13 C12 C16 119.4(3) . . ? C14 C13 C12 120.0 . . ? C13 C14 C15 120.0 . . ? C14 C15 C10 120.0 . . ? C12 C16 N4 113.8(5) . . ? N4 C18 C19 108.6(5) . . ? N5 C19 C18 109.4(5) . . ? N5 C21 C22 107.8(5) . . ? N6 C22 C21 109.5(5) . . ? N6 C24 C25 117.7(4) . . ? C26 C25 C30 120.0 . . ? C26 C25 C24 117.9(3) . . ? C30 C25 C24 122.1(3) . . ? C27 C26 C25 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 C1 120.0(3) . . ? C28 C27 C1 119.6(3) . . ? C27 C28 C29 120.0 . . ? C28 C29 C30 120.0 . . ? C29 C30 C25 120.0 . . ? N7 C31 C57 114.3(4) . . ? C34 C33 N7 108.9(4) . . ? N8 C34 C33 109.3(5) . . ? N8 C36 C37 107.8(5) . . ? N9 C37 C36 109.9(5) . . ? N9 C39 C40 118.2(5) . . ? C41 C40 C45 120.0 . . ? C41 C40 C39 119.0(4) . . ? C45 C40 C39 121.0(3) . . ? C40 C41 C42 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 C46 118.8(4) . . ? C43 C42 C46 121.0(4) . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C44 C45 C40 120.0 . . ? N10 C46 C42 115.0(5) . . ? C49 C48 N10 110.1(5) . . ? N11 C49 C48 109.5(6) . . ? C52 C51 N11 117.1(7) . . ? C51 C52 N12 122.6(7) . . ? N12 C54 C55 120.2(5) . . ? C56 C55 C60 120.0 . . ? C56 C55 C54 118.2(4) . . ? C60 C55 C54 121.1(4) . . ? C55 C56 C57 120.0 . . ? C58 C57 C56 120.0 . . ? C58 C57 C31 120.9(3) . . ? C56 C57 C31 118.8(3) . . ? C59 C58 C57 120.0 . . ? C60 C59 C58 120.0 . . ? C59 C60 C55 120.0 . . ? O2 C62 O1 125.3(5) . . ? O2 C62 C63 119.8(5) . . ? O1 C62 C63 114.9(5) . . ? C64 C63 C68 120.0 . . ? C64 C63 C62 120.8(3) . . ? C68 C63 C62 119.1(3) . . ? C63 C64 C65 120.0 . . ? C66 C65 C64 120.0 . . ? C65 C66 C67 120.0 . . ? C65 C66 C69 120.0(3) . . ? C67 C66 C69 120.0(3) . . ? C68 C67 C66 120.0 . . ? C67 C68 C63 120.0 . . ? C74 C69 C70 120.0 . . ? C74 C69 C66 120.9(2) . . ? C70 C69 C66 119.1(2) . . ? C69 C70 C71 120.0 . . ? C70 C71 C72 120.0 . . ? C73 C72 C71 120.0 . . ? C73 C72 C75 121.5(4) . . ? C71 C72 C75 118.5(4) . . ? C72 C73 C74 120.0 . . ? C69 C74 C73 120.0 . . ? O3 C75 O4 124.7(6) . . ? O3 C75 C72 120.5(6) . . ? O4 C75 C72 114.7(6) . . ? O6 C76 O5 122.1(5) . . ? O6 C76 C77 119.6(6) . . ? O5 C76 C77 118.3(5) . . ? O6 C76 Cu2 73.9(3) . . ? O5 C76 Cu2 48.2(3) . . ? C77 C76 Cu2 165.9(5) . . ? C78 C77 C82 120.0 . . ? C78 C77 C76 120.9(3) . . ? C82 C77 C76 119.1(3) . . ? C79 C78 C77 120.0 . . ? C78 C79 C80 120.0 . . ? C81 C80 C79 120.0 . . ? C81 C80 C83 120.0(2) . . ? C79 C80 C83 120.0(2) . . ? C80 C81 C82 120.0 . . ? C81 C82 C77 120.0 . . ? C84 C83 C88 120.0 . . ? C84 C83 C80 120.3(2) . . ? C88 C83 C80 119.6(2) . . ? C85 C84 C83 120.0 . . ? C84 C85 C86 120.0 . . ? C85 C86 C87 120.0 . . ? C85 C86 C89 119.8(3) . . ? C87 C86 C89 120.2(3) . . ? C88 C87 C86 120.0 . . ? C87 C88 C83 120.0 . . ? O8 C89 O7 122.3(5) . . ? O8 C89 C86 123.6(5) . . ? O7 C89 C86 114.1(5) . . ? O8 C89 Cu3 74.7(3) . . ? O7 C89 Cu3 47.6(3) . . ? C86 C89 Cu3 161.7(4) . . ? O3S Cl1S O1S 104.4(10) . . ? O3S Cl1S O4S 112.9(11) . . ? O1S Cl1S O4S 97.8(11) . . ? O3S Cl1S O2S 113.9(8) . . ? O1S Cl1S O2S 104.8(7) . . ? O4S Cl1S O2S 119.9(13) . . ? O3S Cl1S O4S' 121.4(9) . . ? O1S Cl1S O4S' 128.1(7) . . ? O4S Cl1S O4S' 44.4(11) . . ? O2S Cl1S O4S' 79.2(6) . . ? O3S Cl1S O1S' 120.8(10) . . ? O1S Cl1S O1S' 16.8(9) . . ? O4S Cl1S O1S' 93.6(9) . . ? O2S Cl1S O1S' 93.2(7) . . ? O4S' Cl1S O1S' 114.6(7) . . ? O3S Cl1S O2S' 62.2(12) . . ? O1S Cl1S O2S' 112.8(10) . . ? O4S Cl1S O2S' 149.3(11) . . ? O2S Cl1S O2S' 51.9(11) . . ? O4S' Cl1S O2S' 109.6(11) . . ? O1S' Cl1S O2S' 115.3(9) . . ? O3S Cl1S O3S' 36.0(9) . . ? O1S Cl1S O3S' 99.5(9) . . ? O4S Cl1S O3S' 78.6(11) . . ? O2S Cl1S O3S' 146.3(11) . . ? O4S' Cl1S O3S' 103.5(6) . . ? O1S' Cl1S O3S' 114.8(9) . . ? O2S' Cl1S O3S' 97.1(14) . . ? O4T Cl1T O3T 108.4(10) . . ? O4T Cl1T O2T 126.1(15) . . ? O3T Cl1T O2T 96.8(6) . . ? O4T Cl1T O1T 108.9(9) . . ? O3T Cl1T O1T 112.9(5) . . ? O2T Cl1T O1T 103.3(6) . . ? O2U Cl1U O1U 109.7(7) . . ? O2U Cl1U O3U 114.9(6) . . ? O1U Cl1U O3U 104.2(6) . . ? O2U Cl1U O4U 103.9(6) . . ? O1U Cl1U O4U 116.1(7) . . ? O3U Cl1U O4U 108.4(5) . . ? O1V' Cl1V O4V 138.6(13) . . ? O1V' Cl1V O3V' 118.8(15) . . ? O4V Cl1V O3V' 90.6(14) . . ? O1V' Cl1V O2V 82.2(12) . . ? O4V Cl1V O2V 109.3(8) . . ? O3V' Cl1V O2V 119.7(14) . . ? O1V' Cl1V O3V 97.9(12) . . ? O4V Cl1V O3V 118.8(8) . . ? O3V' Cl1V O3V 30.2(15) . . ? O2V Cl1V O3V 97.5(10) . . ? O1V' Cl1V O1V 34.0(13) . . ? O4V Cl1V O1V 110.0(10) . . ? O3V' Cl1V O1V 113.1(11) . . ? O2V Cl1V O1V 111.9(9) . . ? O3V Cl1V O1V 108.9(9) . . ? O1V' Cl1V O2V' 117.7(11) . . ? O4V Cl1V O2V' 56.3(8) . . ? O3V' Cl1V O2V' 120.6(11) . . ? O2V Cl1V O2V' 53.2(8) . . ? O3V Cl1V O2V' 125.7(10) . . ? O1V Cl1V O2V' 123.8(6) . . ? O1V' Cl1V O4V' 101.5(14) . . ? O4V Cl1V O4V' 42.3(8) . . ? O3V' Cl1V O4V' 97.5(16) . . ? O2V Cl1V O4V' 135.5(10) . . ? O3V Cl1V O4V' 125.3(12) . . ? O1V Cl1V O4V' 68.8(11) . . ? O2V' Cl1V O4V' 88.1(10) . . ? 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 N2 Cu1 O1 C62 173.6(8) . . . . ? N3 Cu1 O1 C62 -104.9(5) . . . . ? N1 Cu1 O1 C62 98.7(5) . . . . ? O1X Cu1 O1 C62 0.0(5) . . . . ? O1 Cu1 N1 C1 44.8(4) . . . . ? N2 Cu1 N1 C1 -124.5(4) . . . . ? N3 Cu1 N1 C1 -56.9(6) . . . . ? O1X Cu1 N1 C1 138.4(4) . . . . ? O1 Cu1 N1 C3 167.9(4) . . . . ? N2 Cu1 N1 C3 -1.4(4) . . . . ? N3 Cu1 N1 C3 66.2(6) . . . . ? O1X Cu1 N1 C3 -98.5(4) . . . . ? O1 Cu1 N1 C2 -74.3(3) . . . . ? N2 Cu1 N1 C2 116.3(4) . . . . ? N3 Cu1 N1 C2 -176.0(4) . . . . ? O1X Cu1 N1 C2 19.3(4) . . . . ? C3 N1 C1 C27 -53.5(6) . . . . ? C2 N1 C1 C27 -172.1(4) . . . . ? Cu1 N1 C1 C27 67.6(5) . . . . ? O1 Cu1 N2 C5 -166.4(8) . . . . ? N3 Cu1 N2 C5 111.1(4) . . . . ? N1 Cu1 N2 C5 -91.2(4) . . . . ? O1X Cu1 N2 C5 7.1(4) . . . . ? O1 Cu1 N2 C6 69.6(10) . . . . ? N3 Cu1 N2 C6 -12.9(4) . . . . ? N1 Cu1 N2 C6 144.8(4) . . . . ? O1X Cu1 N2 C6 -116.8(4) . . . . ? O1 Cu1 N2 C4 -47.0(10) . . . . ? N3 Cu1 N2 C4 -129.5(3) . . . . ? N1 Cu1 N2 C4 28.2(3) . . . . ? O1X Cu1 N2 C4 126.6(3) . . . . ? O1 Cu1 N3 C8 108.2(4) . . . . ? N2 Cu1 N3 C8 -82.7(4) . . . . ? N1 Cu1 N3 C8 -150.9(4) . . . . ? O1X Cu1 N3 C8 13.5(4) . . . . ? O1 Cu1 N3 C7 -133.7(3) . . . . ? N2 Cu1 N3 C7 35.4(3) . . . . ? N1 Cu1 N3 C7 -32.8(6) . . . . ? O1X Cu1 N3 C7 131.6(3) . . . . ? O1 Cu1 N3 C9 -15.3(4) . . . . ? N2 Cu1 N3 C9 153.8(4) . . . . ? N1 Cu1 N3 C9 85.6(6) . . . . ? O1X Cu1 N3 C9 -110.0(4) . . . . ? C1 N1 C3 C4 99.8(5) . . . . ? C2 N1 C3 C4 -143.6(5) . . . . ? Cu1 N1 C3 C4 -26.5(5) . . . . ? N11 Cu4 O4 C75 179.3(7) . . . . ? N12 Cu4 O4 C75 -96.4(5) . . . . ? N10 Cu4 O4 C75 104.1(5) . . . . ? O4X Cu4 O4 C75 6.3(5) . . . . ? O5 Cu2 N4 C18 -161.5(4) . . . . ? N5 Cu2 N4 C18 12.8(4) . . . . ? N6 Cu2 N4 C18 85.1(6) . . . . ? C76 Cu2 N4 C18 -131.5(4) . . . . ? O5 Cu2 N4 C17 -46.1(5) . . . . ? N5 Cu2 N4 C17 128.2(5) . . . . ? N6 Cu2 N4 C17 -159.4(5) . . . . ? C76 Cu2 N4 C17 -16.1(5) . . . . ? O5 Cu2 N4 C16 81.6(4) . . . . ? N5 Cu2 N4 C16 -104.1(4) . . . . ? N6 Cu2 N4 C16 -31.8(8) . . . . ? C76 Cu2 N4 C16 111.6(4) . . . . ? C5 N2 C4 C3 72.3(5) . . . . ? C6 N2 C4 C3 -168.5(4) . . . . ? Cu1 N2 C4 C3 -51.5(5) . . . . ? N1 C3 C4 N2 53.6(6) . . . . ? N5 Cu2 O5 C76 -20.2(17) . . . . ? N6 Cu2 O5 C76 -102.3(3) . . . . ? N4 Cu2 O5 C76 97.6(3) . . . . ? O5 Cu2 N5 C19 134.3(15) . . . . ? N6 Cu2 N5 C19 -143.1(4) . . . . ? N4 Cu2 N5 C19 16.2(4) . . . . ? C76 Cu2 N5 C19 117.3(4) . . . . ? O5 Cu2 N5 C21 -105.1(16) . . . . ? N6 Cu2 N5 C21 -22.6(4) . . . . ? N4 Cu2 N5 C21 136.7(4) . . . . ? C76 Cu2 N5 C21 -122.1(4) . . . . ? O5 Cu2 N5 C20 14.7(18) . . . . ? N6 Cu2 N5 C20 97.3(4) . . . . ? N4 Cu2 N5 C20 -103.4(4) . . . . ? C76 Cu2 N5 C20 -2.3(5) . . . . ? O5 Cu2 N6 C23 48.1(4) . . . . ? N5 Cu2 N6 C23 -125.6(4) . . . . ? N4 Cu2 N6 C23 161.9(5) . . . . ? C76 Cu2 N6 C23 18.6(4) . . . . ? O5 Cu2 N6 C24 -71.2(3) . . . . ? N5 Cu2 N6 C24 115.1(3) . . . . ? N4 Cu2 N6 C24 42.6(7) . . . . ? C76 Cu2 N6 C24 -100.7(3) . . . . ? O5 Cu2 N6 C22 169.2(3) . . . . ? N5 Cu2 N6 C22 -4.4(3) . . . . ? N4 Cu2 N6 C22 -76.9(6) . . . . ? C76 Cu2 N6 C22 139.7(4) . . . . ? C5 N2 C6 C7 -141.5(5) . . . . ? C4 N2 C6 C7 98.7(5) . . . . ? Cu1 N2 C6 C7 -13.4(6) . . . . ? N8 Cu3 O7 C89 -21.1(16) . . . . ? N9 Cu3 O7 C89 -100.2(3) . . . . ? N7 Cu3 O7 C89 99.8(3) . . . . ? O7 Cu3 N7 C33 -165.2(3) . . . . ? N8 Cu3 N7 C33 9.4(3) . . . . ? N9 Cu3 N7 C33 82.4(6) . . . . ? C89 Cu3 N7 C33 -135.4(3) . . . . ? O7 Cu3 N7 C31 75.4(3) . . . . ? N8 Cu3 N7 C31 -110.1(3) . . . . ? N9 Cu3 N7 C31 -37.0(7) . . . . ? C89 Cu3 N7 C31 105.2(4) . . . . ? O7 Cu3 N7 C32 -48.5(4) . . . . ? N8 Cu3 N7 C32 126.0(4) . . . . ? N9 Cu3 N7 C32 -160.9(5) . . . . ? C89 Cu3 N7 C32 -18.7(4) . . . . ? C8 N3 C7 C6 64.3(6) . . . . ? C9 N3 C7 C6 -173.4(4) . . . . ? Cu1 N3 C7 C6 -53.3(5) . . . . ? N2 C6 C7 N3 46.4(6) . . . . ? O7 Cu3 N8 C36 -99.9(15) . . . . ? N9 Cu3 N8 C36 -20.5(3) . . . . ? N7 Cu3 N8 C36 138.7(4) . . . . ? C89 Cu3 N8 C36 -117.7(4) . . . . ? O7 Cu3 N8 C34 140.2(14) . . . . ? N9 Cu3 N8 C34 -140.5(3) . . . . ? N7 Cu3 N8 C34 18.8(3) . . . . ? C89 Cu3 N8 C34 122.3(4) . . . . ? O7 Cu3 N8 C35 20.9(17) . . . . ? N9 Cu3 N8 C35 100.2(4) . . . . ? N7 Cu3 N8 C35 -100.5(4) . . . . ? C89 Cu3 N8 C35 3.0(5) . . . . ? O7 Cu3 N9 C37 166.2(3) . . . . ? N8 Cu3 N9 C37 -7.6(4) . . . . ? N7 Cu3 N9 C37 -80.7(6) . . . . ? C89 Cu3 N9 C37 136.6(4) . . . . ? O7 Cu3 N9 C38 44.7(4) . . . . ? N8 Cu3 N9 C38 -129.1(4) . . . . ? N7 Cu3 N9 C38 157.9(5) . . . . ? C89 Cu3 N9 C38 15.2(5) . . . . ? O7 Cu3 N9 C39 -75.6(4) . . . . ? N8 Cu3 N9 C39 110.6(4) . . . . ? N7 Cu3 N9 C39 37.6(7) . . . . ? C89 Cu3 N9 C39 -105.1(4) . . . . ? C8 N3 C9 C10 63.9(6) . . . . ? C7 N3 C9 C10 -59.7(6) . . . . ? Cu1 N3 C9 C10 -171.8(3) . . . . ? O4 Cu4 N10 C47 -73.7(4) . . . . ? N11 Cu4 N10 C47 119.7(4) . . . . ? N12 Cu4 N10 C47 -174.1(5) . . . . ? O4X Cu4 N10 C47 22.6(4) . . . . ? O4 Cu4 N10 C46 45.3(5) . . . . ? N11 Cu4 N10 C46 -121.4(5) . . . . ? N12 Cu4 N10 C46 -55.1(7) . . . . ? O4X Cu4 N10 C46 141.6(4) . . . . ? O4 Cu4 N10 C48 169.3(4) . . . . ? N11 Cu4 N10 C48 2.6(4) . . . . ? N12 Cu4 N10 C48 68.8(7) . . . . ? O4X Cu4 N10 C48 -94.5(4) . . . . ? O4 Cu4 N11 C49 -51.5(10) . . . . ? N12 Cu4 N11 C49 -136.7(4) . . . . ? N10 Cu4 N11 C49 24.2(4) . . . . ? O4X Cu4 N11 C49 121.5(4) . . . . ? O4 Cu4 N11 C51 67.1(10) . . . . ? N12 Cu4 N11 C51 -18.2(5) . . . . ? N10 Cu4 N11 C51 142.7(5) . . . . ? O4X Cu4 N11 C51 -119.9(5) . . . . ? O4 Cu4 N11 C50 -171.8(7) . . . . ? N12 Cu4 N11 C50 102.9(5) . . . . ? N10 Cu4 N11 C50 -96.2(5) . . . . ? O4X Cu4 N11 C50 1.1(5) . . . . ? O4 Cu4 N12 C53 90.7(5) . . . . ? N11 Cu4 N12 C53 -103.0(6) . . . . ? N10 Cu4 N12 C53 -169.4(6) . . . . ? O4X Cu4 N12 C53 -6.4(6) . . . . ? O4 Cu4 N12 C54 -31.6(5) . . . . ? N11 Cu4 N12 C54 134.7(5) . . . . ? N10 Cu4 N12 C54 68.3(7) . . . . ? O4X Cu4 N12 C54 -128.7(5) . . . . ? O4 Cu4 N12 C52 -147.5(7) . . . . ? N11 Cu4 N12 C52 18.8(7) . . . . ? N10 Cu4 N12 C52 -47.6(9) . . . . ? O4X Cu4 N12 C52 115.4(7) . . . . ? N3 C9 C10 C11 98.8(5) . . . . ? N3 C9 C10 C15 -89.7(5) . . . . ? C15 C10 C11 C12 0.0 . . . . ? C9 C10 C11 C12 171.6(4) . . . . ? C10 C11 C12 C13 0.0 . . . . ? C10 C11 C12 C16 -179.8(5) . . . . ? C11 C12 C13 C14 0.0 . . . . ? C16 C12 C13 C14 179.8(5) . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C10 0.0 . . . . ? C11 C10 C15 C14 0.0 . . . . ? C9 C10 C15 C14 -171.4(4) . . . . ? C11 C12 C16 N4 73.8(6) . . . . ? C13 C12 C16 N4 -106.0(5) . . . . ? C18 N4 C16 C12 174.9(5) . . . . ? C17 N4 C16 C12 57.4(6) . . . . ? Cu2 N4 C16 C12 -70.1(6) . . . . ? C17 N4 C18 C19 -156.6(5) . . . . ? C16 N4 C18 C19 83.6(6) . . . . ? Cu2 N4 C18 C19 -38.8(5) . . . . ? C21 N5 C19 C18 -159.8(5) . . . . ? C20 N5 C19 C18 76.8(6) . . . . ? Cu2 N5 C19 C18 -42.6(6) . . . . ? N4 C18 C19 N5 56.5(6) . . . . ? C19 N5 C21 C22 161.9(5) . . . . ? C20 N5 C21 C22 -74.5(6) . . . . ? Cu2 N5 C21 C22 45.4(6) . . . . ? C23 N6 C22 C21 154.6(5) . . . . ? C24 N6 C22 C21 -82.4(5) . . . . ? Cu2 N6 C22 C21 30.8(5) . . . . ? N5 C21 C22 N6 -50.8(6) . . . . ? C23 N6 C24 C25 48.3(6) . . . . ? C22 N6 C24 C25 -74.3(5) . . . . ? Cu2 N6 C24 C25 170.2(3) . . . . ? N6 C24 C25 C26 -104.7(4) . . . . ? N6 C24 C25 C30 76.9(5) . . . . ? C30 C25 C26 C27 0.0 . . . . ? C24 C25 C26 C27 -178.4(4) . . . . ? C25 C26 C27 C28 0.0 . . . . ? C25 C26 C27 C1 172.9(4) . . . . ? N1 C1 C27 C26 -80.8(5) . . . . ? N1 C1 C27 C28 92.1(5) . . . . ? C26 C27 C28 C29 0.0 . . . . ? C1 C27 C28 C29 -172.9(4) . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C25 0.0 . . . . ? C26 C25 C30 C29 0.0 . . . . ? C24 C25 C30 C29 178.3(4) . . . . ? C33 N7 C31 C57 178.7(4) . . . . ? C32 N7 C31 C57 58.9(5) . . . . ? Cu3 N7 C31 C57 -64.7(5) . . . . ? C31 N7 C33 C34 86.4(5) . . . . ? C32 N7 C33 C34 -153.1(5) . . . . ? Cu3 N7 C33 C34 -36.0(5) . . . . ? C36 N8 C34 C33 -161.4(5) . . . . ? C35 N8 C34 C33 73.6(6) . . . . ? Cu3 N8 C34 C33 -44.7(5) . . . . ? N7 C33 C34 N8 55.3(6) . . . . ? C34 N8 C36 C37 159.4(5) . . . . ? C35 N8 C36 C37 -75.9(6) . . . . ? Cu3 N8 C36 C37 43.4(5) . . . . ? C38 N9 C37 C36 158.4(5) . . . . ? C39 N9 C37 C36 -78.2(6) . . . . ? Cu3 N9 C37 C36 33.2(5) . . . . ? N8 C36 C37 N9 -52.4(6) . . . . ? C37 N9 C39 C40 -70.3(6) . . . . ? C38 N9 C39 C40 52.5(7) . . . . ? Cu3 N9 C39 C40 176.1(4) . . . . ? N9 C39 C40 C41 -101.5(5) . . . . ? N9 C39 C40 C45 79.5(6) . . . . ? C45 C40 C41 C42 0.0 . . . . ? C39 C40 C41 C42 -179.0(4) . . . . ? C40 C41 C42 C43 0.0 . . . . ? C40 C41 C42 C46 174.6(4) . . . . ? C41 C42 C43 C44 0.0 . . . . ? C46 C42 C43 C44 -174.5(4) . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C40 0.0 . . . . ? C41 C40 C45 C44 0.0 . . . . ? C39 C40 C45 C44 179.0(4) . . . . ? C47 N10 C46 C42 -172.3(5) . . . . ? C48 N10 C46 C42 -54.0(6) . . . . ? Cu4 N10 C46 C42 66.4(6) . . . . ? C41 C42 C46 N10 -81.7(5) . . . . ? C43 C42 C46 N10 92.9(5) . . . . ? C47 N10 C48 C49 -147.1(6) . . . . ? C46 N10 C48 C49 96.5(6) . . . . ? Cu4 N10 C48 C49 -29.4(7) . . . . ? C51 N11 C49 C48 -164.1(5) . . . . ? C50 N11 C49 C48 76.3(6) . . . . ? Cu4 N11 C49 C48 -47.7(6) . . . . ? N10 C48 C49 N11 52.7(7) . . . . ? C49 N11 C51 C52 128.9(11) . . . . ? C50 N11 C51 C52 -111.1(12) . . . . ? Cu4 N11 C51 C52 13.9(12) . . . . ? N11 C51 C52 N12 3.4(19) . . . . ? C53 N12 C52 C51 103.4(14) . . . . ? C54 N12 C52 C51 -135.5(13) . . . . ? Cu4 N12 C52 C51 -17.4(16) . . . . ? C53 N12 C54 C55 61.4(9) . . . . ? C52 N12 C54 C55 -62.4(9) . . . . ? Cu4 N12 C54 C55 -174.5(5) . . . . ? N12 C54 C55 C56 103.6(6) . . . . ? N12 C54 C55 C60 -85.6(7) . . . . ? C60 C55 C56 C57 0.0 . . . . ? C54 C55 C56 C57 170.9(4) . . . . ? C55 C56 C57 C58 0.0 . . . . ? C55 C56 C57 C31 -174.3(4) . . . . ? N7 C31 C57 C58 -88.5(4) . . . . ? N7 C31 C57 C56 85.8(4) . . . . ? C56 C57 C58 C59 0.0 . . . . ? C31 C57 C58 C59 174.2(4) . . . . ? C57 C58 C59 C60 0.0 . . . . ? C58 C59 C60 C55 0.0 . . . . ? C56 C55 C60 C59 0.0 . . . . ? C54 C55 C60 C59 -170.6(4) . . . . ? Cu1 O1 C62 O2 -2.3(9) . . . . ? Cu1 O1 C62 C63 -178.8(3) . . . . ? O2 C62 C63 C64 171.8(4) . . . . ? O1 C62 C63 C64 -11.5(6) . . . . ? O2 C62 C63 C68 -10.4(7) . . . . ? O1 C62 C63 C68 166.3(3) . . . . ? C68 C63 C64 C65 0.0 . . . . ? C62 C63 C64 C65 177.8(4) . . . . ? C63 C64 C65 C66 0.0 . . . . ? C64 C65 C66 C67 0.0 . . . . ? C64 C65 C66 C69 -178.8(3) . . . . ? C65 C66 C67 C68 0.0 . . . . ? C69 C66 C67 C68 178.8(3) . . . . ? C66 C67 C68 C63 0.0 . . . . ? C64 C63 C68 C67 0.0 . . . . ? C62 C63 C68 C67 -177.8(4) . . . . ? C65 C66 C69 C74 -148.8(2) . . . . ? C67 C66 C69 C74 32.4(3) . . . . ? C65 C66 C69 C70 30.2(3) . . . . ? C67 C66 C69 C70 -148.6(2) . . . . ? C74 C69 C70 C71 0.0 . . . . ? C66 C69 C70 C71 -179.0(3) . . . . ? C69 C70 C71 C72 0.0 . . . . ? C70 C71 C72 C73 0.0 . . . . ? C70 C71 C72 C75 178.6(4) . . . . ? C71 C72 C73 C74 0.0 . . . . ? C75 C72 C73 C74 -178.5(4) . . . . ? C70 C69 C74 C73 0.0 . . . . ? C66 C69 C74 C73 179.0(3) . . . . ? C72 C73 C74 C69 0.0 . . . . ? Cu4 O4 C75 O3 -6.2(9) . . . . ? Cu4 O4 C75 C72 178.8(3) . . . . ? C73 C72 C75 O3 169.5(5) . . . . ? C71 C72 C75 O3 -9.1(7) . . . . ? C73 C72 C75 O4 -15.3(6) . . . . ? C71 C72 C75 O4 166.2(4) . . . . ? Cu2 O5 C76 O6 3.3(6) . . . . ? Cu2 O5 C76 C77 -175.0(3) . . . . ? O5 Cu2 C76 O6 -177.1(5) . . . . ? N5 Cu2 C76 O6 -0.8(5) . . . . ? N6 Cu2 C76 O6 -96.4(3) . . . . ? N4 Cu2 C76 O6 96.6(3) . . . . ? N5 Cu2 C76 O5 176.2(3) . . . . ? N6 Cu2 C76 O5 80.7(3) . . . . ? N4 Cu2 C76 O5 -86.4(3) . . . . ? O5 Cu2 C76 C77 18.5(12) . . . . ? N5 Cu2 C76 C77 -165.3(13) . . . . ? N6 Cu2 C76 C77 99.2(14) . . . . ? N4 Cu2 C76 C77 -67.9(14) . . . . ? O6 C76 C77 C78 16.7(6) . . . . ? O5 C76 C77 C78 -164.9(3) . . . . ? Cu2 C76 C77 C78 179.5(12) . . . . ? O6 C76 C77 C82 -165.2(4) . . . . ? O5 C76 C77 C82 13.1(5) . . . . ? Cu2 C76 C77 C82 -2.5(15) . . . . ? C82 C77 C78 C79 0.0 . . . . ? C76 C77 C78 C79 178.0(3) . . . . ? C77 C78 C79 C80 0.0 . . . . ? C78 C79 C80 C81 0.0 . . . . ? C78 C79 C80 C83 -179.5(3) . . . . ? C79 C80 C81 C82 0.0 . . . . ? C83 C80 C81 C82 179.5(3) . . . . ? C80 C81 C82 C77 0.0 . . . . ? C78 C77 C82 C81 0.0 . . . . ? C76 C77 C82 C81 -178.0(3) . . . . ? C81 C80 C83 C84 -11.0(3) . . . . ? C79 C80 C83 C84 168.5(2) . . . . ? C81 C80 C83 C88 166.8(2) . . . . ? C79 C80 C83 C88 -13.7(3) . . . . ? C88 C83 C84 C85 0.0 . . . . ? C80 C83 C84 C85 177.8(3) . . . . ? C83 C84 C85 C86 0.0 . . . . ? C84 C85 C86 C87 0.0 . . . . ? C84 C85 C86 C89 -178.9(3) . . . . ? C85 C86 C87 C88 0.0 . . . . ? C89 C86 C87 C88 178.9(3) . . . . ? C86 C87 C88 C83 0.0 . . . . ? C84 C83 C88 C87 0.0 . . . . ? C80 C83 C88 C87 -177.8(3) . . . . ? Cu3 O7 C89 O8 -0.1(6) . . . . ? Cu3 O7 C89 C86 -179.8(3) . . . . ? C85 C86 C89 O8 7.0(6) . . . . ? C87 C86 C89 O8 -171.9(4) . . . . ? C85 C86 C89 O7 -173.2(3) . . . . ? C87 C86 C89 O7 7.9(6) . . . . ? C85 C86 C89 Cu3 -173.6(10) . . . . ? C87 C86 C89 Cu3 7.5(12) . . . . ? O7 Cu3 C89 O8 180.0(5) . . . . ? N8 Cu3 C89 O8 -3.9(5) . . . . ? N9 Cu3 C89 O8 -97.9(3) . . . . ? N7 Cu3 C89 O8 95.3(3) . . . . ? N8 Cu3 C89 O7 176.1(3) . . . . ? N9 Cu3 C89 O7 82.2(3) . . . . ? N7 Cu3 C89 O7 -84.6(3) . . . . ? O7 Cu3 C89 C86 0.5(9) . . . . ? N8 Cu3 C89 C86 176.6(10) . . . . ? N9 Cu3 C89 C86 82.7(11) . . . . ? N7 Cu3 C89 C86 -84.2(11) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 28.52 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.568 _refine_diff_density_min -1.555 _refine_diff_density_rms 0.119 #===END data_mc1(5OTf)_CCDC648100 _database_code_depnum_ccdc_archive 'CCDC 648100' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H112 Cu4 N12 O8, 6(C3 H7 N O), 4(C F3 O3 S)' _chemical_formula_sum 'C106 H154 Cu4 F12 N18 O26 S4' _chemical_formula_weight 2708.94 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' Cu Cu 0.3201 1.2651 '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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 47.459(6) _cell_length_b 10.8410(13) _cell_length_c 25.399(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.066(2) _cell_angle_gamma 90.00 _cell_volume 12424(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5327 _exptl_absorpt_coefficient_mu 0.831 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ccd area detector' _diffrn_measurement_method 'phi and omega scnas' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 94392 _diffrn_reflns_av_R_equivalents 0.1294 _diffrn_reflns_av_sigmaI/netI 0.1264 _diffrn_reflns_limit_h_min -63 _diffrn_reflns_limit_h_max 63 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 28.39 _reflns_number_total 15381 _reflns_number_gt 8330 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER Shelxtl' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)/PLATON' _computing_molecular_graphics ? _computing_publication_material ? 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 0.000 0.187 0.250 272.5 246.4 2 0.000 -0.187 0.750 272.5 283.9 3 0.250 0.250 0.500 156.7 157.1 4 0.500 0.313 0.750 272.5 284.0 5 0.750 0.250 1.000 156.8 161.2 6 0.500 0.687 0.250 272.5 246.4 7 0.250 0.750 1.000 156.8 161.2 8 0.750 0.750 0.500 156.7 157.1 _platon_squeeze_details ; ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A considerable amount of electron density attibutable to partially disordered solvent was removed with the SQUEEZE option of PLATON (Spek, A. L. (2005). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, THe Netherlands. The SQUEEZE option of the PLATON Program (Spek, A. L. (2005). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, THe Netherlands) was used to eliminate electron density from disordered DMF solvent molecules. This DMF molecules are, however, included in the reported chemical formula and derived values (reported crystal-data formula, formula weight,Dx, Mu and F(000)). The macrocyclic complex lies about an inversion center ; _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^)+(0.1091P)^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 15381 _refine_ls_number_parameters 729 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1410 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.2078 _refine_ls_wR_factor_gt 0.1865 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.173453(11) 0.59489(5) 0.20136(2) 0.01716(14) Uani 1 1 d . . . Cu2 Cu -0.109661(12) 0.61077(5) 0.06559(2) 0.01985(15) Uani 1 1 d . . . O1 O 0.13386(6) 0.6260(3) 0.20047(12) 0.0204(7) Uani 1 1 d . . . O2 O 0.13260(7) 0.6873(3) 0.28400(12) 0.0283(8) Uani 1 1 d . . . O3 O -0.06106(7) 0.5215(4) 0.02171(15) 0.0428(10) Uani 1 1 d . . . O4 O -0.06770(7) 0.6017(3) 0.09734(13) 0.0319(8) Uani 1 1 d . . . N1 N 0.17613(8) 0.4255(3) 0.23714(14) 0.0226(8) Uani 1 1 d . . . N2 N 0.21082(8) 0.5474(3) 0.18570(14) 0.0208(8) Uani 1 1 d . . . N3 N 0.18373(8) 0.7725(3) 0.18679(15) 0.0221(8) Uani 1 1 d . . . N4 N 0.10846(9) 0.2034(4) -0.04549(16) 0.0290(9) Uani 1 1 d . . . N5 N 0.15306(8) 0.3644(4) -0.04916(15) 0.0246(9) Uani 1 1 d . . . N6 N 0.11691(8) 0.5603(3) -0.09671(14) 0.0225(8) Uani 1 1 d . . . C1 C 0.14862(10) 0.3471(4) 0.22304(18) 0.0245(10) Uani 1 1 d . . . H1A H 0.1331 0.3937 0.2313 0.029 Uiso 1 1 calc R . . H1B H 0.1527 0.2751 0.2469 0.029 Uiso 1 1 calc R . . C2 C 0.18415(11) 0.4588(5) 0.29655(18) 0.0312(12) Uani 1 1 d . . . H2A H 0.1859 0.3851 0.3183 0.047 Uiso 1 1 calc R . . H2B H 0.1690 0.5106 0.3025 0.047 Uiso 1 1 calc R . . H2C H 0.2027 0.5021 0.3074 0.047 Uiso 1 1 calc R . . C3 C 0.20097(10) 0.3554(4) 0.2263(2) 0.0279(11) Uani 1 1 d . . . H3A H 0.1937 0.3113 0.1915 0.033 Uiso 1 1 calc R . . H3B H 0.2090 0.2957 0.2556 0.033 Uiso 1 1 calc R . . C4 C 0.22477(10) 0.4449(5) 0.22387(19) 0.0286(11) Uani 1 1 d . . . H4A H 0.2347 0.4773 0.2606 0.034 Uiso 1 1 calc R . . H4B H 0.2394 0.4035 0.2106 0.034 Uiso 1 1 calc R . . C5 C 0.20314(10) 0.5070(4) 0.12738(17) 0.0230(10) Uani 1 1 d . . . H5A H 0.2210 0.4946 0.1178 0.035 Uiso 1 1 calc R . . H5B H 0.1912 0.5690 0.1038 0.035 Uiso 1 1 calc R . . H5C H 0.1922 0.4310 0.1227 0.035 Uiso 1 1 calc R . . C6 C 0.22988(10) 0.6596(4) 0.1950(2) 0.0275(11) Uani 1 1 d . . . H6A H 0.2457 0.6487 0.1787 0.033 Uiso 1 1 calc R . . H6B H 0.2387 0.6741 0.2344 0.033 Uiso 1 1 calc R . . C7 C 0.21051(10) 0.7683(4) 0.1683(2) 0.0294(11) Uani 1 1 d . . . H7A H 0.2216 0.8444 0.1785 0.035 Uiso 1 1 calc R . . H7B H 0.2046 0.7603 0.1283 0.035 Uiso 1 1 calc R . . C8 C 0.19056(11) 0.8288(5) 0.2429(2) 0.0323(12) Uani 1 1 d . . . H8A H 0.1973 0.9119 0.2419 0.048 Uiso 1 1 calc R . . H8B H 0.2057 0.7816 0.2689 0.048 Uiso 1 1 calc R . . H8C H 0.1730 0.8291 0.2541 0.048 Uiso 1 1 calc R . . C9 C 0.16040(10) 0.8519(4) 0.14864(19) 0.0249(10) Uani 1 1 d . . . H9A H 0.1687 0.9330 0.1470 0.030 Uiso 1 1 calc R . . H9B H 0.1442 0.8616 0.1641 0.030 Uiso 1 1 calc R . . C10 C 0.14811(10) 0.8022(4) 0.09050(18) 0.0217(10) Uani 1 1 d . . . C11 C 0.12453(10) 0.7188(4) 0.07761(18) 0.0229(10) Uani 1 1 d . . . H11A H 0.1173 0.6916 0.1057 0.027 Uiso 1 1 calc R . . C11X C 0.15755(11) 0.8433(4) 0.0465(2) 0.0280(11) Uani 1 1 d . . . H11B H 0.1729 0.9002 0.0533 0.034 Uiso 1 1 calc R . . C12 C 0.11157(10) 0.6754(4) 0.02425(18) 0.0232(10) Uani 1 1 d . . . H12A H 0.0962 0.6186 0.0172 0.028 Uiso 1 1 calc R . . C12X C 0.11015(11) 0.2185(4) 0.0547(2) 0.0282(11) Uani 1 1 d . . . C13X C 0.11396(11) 0.3445(4) 0.06631(19) 0.0268(11) Uani 1 1 d . . . H13A H 0.1074 0.4015 0.0377 0.032 Uiso 1 1 calc R . . C14X C 0.12738(10) 0.3857(4) 0.11974(18) 0.0227(10) Uani 1 1 d . . . H14A H 0.1299 0.4700 0.1264 0.027 Uiso 1 1 calc R . . C15X C 0.13721(10) 0.3042(4) 0.16356(18) 0.0226(10) Uani 1 1 d . . . C16X C 0.13385(11) 0.1785(4) 0.1517(2) 0.0297(11) Uani 1 1 d . . . H16A H 0.1407 0.1218 0.1802 0.036 Uiso 1 1 calc R . . C17X C 0.12081(11) 0.1369(4) 0.0990(2) 0.0309(11) Uani 1 1 d . . . H17A H 0.1190 0.0524 0.0925 0.037 Uiso 1 1 calc R . . C20 C 0.12068(9) 0.6545(4) 0.23596(18) 0.0193(9) Uani 1 1 d . . . C21 C 0.08724(10) 0.6435(4) 0.21315(17) 0.0213(10) Uani 1 1 d . . . C22 C 0.07423(10) 0.5822(5) 0.16525(19) 0.0283(11) Uani 1 1 d . . . H22A H 0.0862 0.5454 0.1469 0.034 Uiso 1 1 calc R . . C23 C 0.04333(10) 0.5721(5) 0.14236(19) 0.0286(11) Uani 1 1 d . . . C24 C 0.03001(12) 0.5085(6) 0.0925(2) 0.0442(15) Uani 1 1 d . . . H24A H 0.0418 0.4688 0.0744 0.053 Uiso 1 1 calc R . . C25 C -0.00018(11) 0.5047(6) 0.0704(2) 0.0428(14) Uani 1 1 d . . . H25A H -0.0087 0.4636 0.0371 0.051 Uiso 1 1 calc R . . C26 C -0.01865(10) 0.5623(5) 0.0974(2) 0.0309(12) Uani 1 1 d . . . C27 C -0.00620(10) 0.6222(5) 0.14621(19) 0.0280(11) Uani 1 1 d . . . H27A H -0.0185 0.6593 0.1638 0.034 Uiso 1 1 calc R . . C28 C 0.02488(10) 0.6299(4) 0.17095(18) 0.0248(10) Uani 1 1 d . . . C29 C 0.03893(11) 0.6914(5) 0.22040(19) 0.0299(11) Uani 1 1 d . . . H29A H 0.0273 0.7291 0.2393 0.036 Uiso 1 1 calc R . . C30 C 0.06894(10) 0.6983(4) 0.24206(18) 0.0258(10) Uani 1 1 d . . . H30A H 0.0775 0.7385 0.2756 0.031 Uiso 1 1 calc R . . C31 C -0.05153(11) 0.5616(5) 0.0694(2) 0.0335(12) Uani 1 1 d . . . C32 C 0.09406(13) 0.1724(4) -0.0027(2) 0.0346(12) Uani 1 1 d . . . H32A H 0.0922 0.0834 -0.0013 0.041 Uiso 1 1 calc R . . H32B H 0.0742 0.2066 -0.0142 0.041 Uiso 1 1 calc R . . C33 C 0.09110(13) 0.1435(5) -0.0984(2) 0.0423(14) Uani 1 1 d . . . H33A H 0.0902 0.0562 -0.0928 0.063 Uiso 1 1 calc R . . H33B H 0.1005 0.1591 -0.1262 0.063 Uiso 1 1 calc R . . H33C H 0.0714 0.1767 -0.1103 0.063 Uiso 1 1 calc R . . C34 C 0.13969(12) 0.1564(4) -0.0286(2) 0.0330(12) Uani 1 1 d . . . H34A H 0.1398 0.0699 -0.0383 0.040 Uiso 1 1 calc R . . H34B H 0.1485 0.1642 0.0112 0.040 Uiso 1 1 calc R . . C35 C 0.15736(11) 0.2301(4) -0.0579(2) 0.0328(12) Uani 1 1 d . . . H35A H 0.1782 0.2091 -0.0431 0.039 Uiso 1 1 calc R . . H35B H 0.1507 0.2112 -0.0971 0.039 Uiso 1 1 calc R . . C36 C 0.16978(11) 0.4009(5) 0.00786(19) 0.0302(11) Uani 1 1 d . . . H36A H 0.1906 0.4022 0.0120 0.045 Uiso 1 1 calc R . . H36B H 0.1661 0.3427 0.0335 0.045 Uiso 1 1 calc R . . H36C H 0.1636 0.4815 0.0153 0.045 Uiso 1 1 calc R . . C37 C 0.16169(11) 0.4412(5) -0.0901(2) 0.0307(12) Uani 1 1 d . . . H37A H 0.1538 0.4058 -0.1269 0.037 Uiso 1 1 calc R . . H37B H 0.1831 0.4450 -0.0806 0.037 Uiso 1 1 calc R . . C38 C 0.14924(10) 0.5683(4) -0.0891(2) 0.0272(11) Uani 1 1 d . . . H38A H 0.1593 0.6077 -0.0539 0.033 Uiso 1 1 calc R . . H38B H 0.1525 0.6180 -0.1184 0.033 Uiso 1 1 calc R . . C39 C 0.10087(11) 0.5473(5) -0.15715(18) 0.0308(12) Uani 1 1 d . . . H39A H 0.1053 0.6166 -0.1767 0.046 Uiso 1 1 calc R . . H39B H 0.0799 0.5441 -0.1629 0.046 Uiso 1 1 calc R . . H39C H 0.1071 0.4727 -0.1707 0.046 Uiso 1 1 calc R . . C40 C 0.10611(11) 0.6780(4) -0.0779(2) 0.0304(11) Uani 1 1 d . . . H40A H 0.1080 0.7440 -0.1023 0.036 Uiso 1 1 calc R . . H40B H 0.0852 0.6687 -0.0822 0.036 Uiso 1 1 calc R . . C41 C 0.12163(10) 0.7169(4) -0.01926(19) 0.0227(10) Uani 1 1 d . . . C42 C 0.14458(11) 0.8016(4) -0.0065(2) 0.0279(11) Uani 1 1 d . . . H42A H 0.1514 0.8310 -0.0347 0.042 Uiso 1 1 calc R . . O1O O 0.0898(2) -0.0809(6) 0.1566(4) 0.140(3) Uani 1 1 d . . . N1O N 0.0752(2) 0.0733(11) 0.2026(6) 0.184(6) Uani 1 1 d . . . C1O C 0.0915(2) -0.0320(9) 0.2032(5) 0.111(4) Uani 1 1 d . . . H22 H 0.1033 -0.0662 0.2363 0.134 Uiso 1 1 calc R . . C2O C 0.0810(3) 0.127(2) 0.2581(7) 0.322(16) Uani 1 1 d . . . H2O1 H 0.0692 0.1997 0.2558 0.483 Uiso 1 1 calc R . . H2O2 H 0.1016 0.1472 0.2731 0.483 Uiso 1 1 calc R . . H2O3 H 0.0758 0.0677 0.2818 0.483 Uiso 1 1 calc R . . C3O C 0.0581(3) 0.151(2) 0.1538(8) 0.298(15) Uani 1 1 d . . . H3OA H 0.0560 0.1074 0.1200 0.446 Uiso 1 1 calc R . . H3OB H 0.0685 0.2272 0.1537 0.446 Uiso 1 1 calc R . . H3OC H 0.0388 0.1693 0.1567 0.446 Uiso 1 1 calc R . . O1M O -0.0173(2) 0.9023(10) 0.0829(7) 0.238(8) Uani 1 1 d . . . N1M N 0.0142(3) 0.8355(8) 0.0311(6) 0.133(4) Uani 1 1 d . . . C1M C 0.0081(5) 0.8734(12) 0.0806(8) 0.185(7) Uani 1 1 d . . . H1MA H 0.0239 0.8769 0.1132 0.222 Uiso 1 1 calc R . . C2M C -0.0126(3) 0.8241(11) -0.0189(6) 0.170(6) Uani 1 1 d . . . H30 H -0.0073 0.8419 -0.0516 0.255 Uiso 1 1 calc R . . H31 H -0.0275 0.8815 -0.0160 0.255 Uiso 1 1 calc R . . H32 H -0.0203 0.7417 -0.0211 0.255 Uiso 1 1 calc R . . C3M C 0.0436(2) 0.8091(9) 0.0315(5) 0.140(5) Uani 1 1 d . . . H33 H 0.0574 0.8495 0.0626 0.209 Uiso 1 1 calc R . . H34 H 0.0464 0.8384 -0.0022 0.209 Uiso 1 1 calc R . . H35 H 0.0469 0.7217 0.0345 0.209 Uiso 1 1 calc R . . S1V S 0.16380(5) 0.07686(14) 0.34110(7) 0.0618(5) Uani 1 1 d . . . F1V F 0.20313(12) 0.0209(7) 0.4324(2) 0.149(3) Uani 1 1 d . . . F2V F 0.19203(12) -0.1266(5) 0.3631(2) 0.1019(16) Uani 1 1 d . . . F3V F 0.21909(14) 0.0231(7) 0.3602(3) 0.168(3) Uani 1 1 d . . . O1V O 0.1641(3) 0.1933(5) 0.3546(3) 0.222(6) Uani 1 1 d . . . O2V O 0.16038(18) 0.0624(5) 0.2849(2) 0.138(3) Uani 1 1 d . . . O3V O 0.14275(16) 0.0147(7) 0.3645(3) 0.145(3) Uani 1 1 d . . . C1V C 0.1984(3) -0.0027(11) 0.3770(4) 0.118(4) Uani 1 1 d . . . S1W S 0.22736(3) 0.13092(11) 0.12192(5) 0.0294(3) Uani 1 1 d . . . F1W F 0.24158(8) 0.3077(3) 0.06544(16) 0.0626(11) Uani 1 1 d . . . F2W F 0.27166(8) 0.1573(4) 0.08462(17) 0.0747(13) Uani 1 1 d . . . F3W F 0.22963(10) 0.1409(5) 0.02212(15) 0.0925(15) Uani 1 1 d . . . O1W O 0.24341(10) 0.1956(5) 0.17113(16) 0.0670(14) Uani 1 1 d . . . O2W O 0.19689(9) 0.1727(5) 0.10228(18) 0.0713(15) Uani 1 1 d . . . O3W O 0.23326(15) 0.0044(4) 0.1247(2) 0.102(2) Uani 1 1 d . . . C1W C 0.24434(13) 0.1877(5) 0.0724(2) 0.0374(13) 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 Cu1 0.0134(3) 0.0223(3) 0.0164(3) -0.0019(2) 0.0054(2) 0.0026(2) Cu2 0.0158(3) 0.0266(3) 0.0180(3) -0.0004(2) 0.0064(2) 0.0018(2) O1 0.0144(16) 0.0309(17) 0.0164(15) -0.0025(13) 0.0056(12) 0.0026(13) O2 0.0217(18) 0.043(2) 0.0183(16) -0.0071(15) 0.0039(14) 0.0006(15) O3 0.020(2) 0.064(3) 0.037(2) -0.0140(19) -0.0015(17) -0.0038(18) O4 0.0146(17) 0.051(2) 0.0304(18) 0.0020(17) 0.0078(14) 0.0006(16) N1 0.024(2) 0.031(2) 0.0156(18) 0.0049(16) 0.0100(16) 0.0097(17) N2 0.019(2) 0.0234(19) 0.0195(19) -0.0043(16) 0.0057(16) 0.0039(16) N3 0.016(2) 0.0255(19) 0.026(2) -0.0078(17) 0.0086(17) 0.0002(16) N4 0.034(3) 0.028(2) 0.023(2) -0.0032(18) 0.0049(18) -0.0014(18) N5 0.026(2) 0.032(2) 0.0156(19) -0.0028(16) 0.0065(16) 0.0082(17) N6 0.021(2) 0.033(2) 0.0170(19) 0.0007(16) 0.0110(16) 0.0058(17) C1 0.028(3) 0.028(2) 0.021(2) 0.008(2) 0.012(2) 0.003(2) C2 0.037(3) 0.042(3) 0.014(2) 0.005(2) 0.007(2) 0.010(2) C3 0.025(3) 0.033(3) 0.027(3) 0.006(2) 0.010(2) 0.014(2) C4 0.021(3) 0.043(3) 0.022(2) 0.004(2) 0.008(2) 0.016(2) C5 0.016(2) 0.031(2) 0.021(2) -0.001(2) 0.0035(19) -0.0005(19) C6 0.019(3) 0.035(3) 0.029(3) -0.015(2) 0.009(2) -0.008(2) C7 0.022(3) 0.030(3) 0.041(3) -0.011(2) 0.017(2) -0.011(2) C8 0.024(3) 0.033(3) 0.038(3) -0.015(2) 0.006(2) -0.004(2) C9 0.022(3) 0.019(2) 0.034(3) -0.001(2) 0.009(2) -0.0008(19) C10 0.019(2) 0.019(2) 0.028(2) -0.0010(19) 0.009(2) 0.0043(18) C11 0.025(3) 0.022(2) 0.025(2) 0.0058(19) 0.013(2) 0.0034(19) C11X 0.026(3) 0.023(2) 0.039(3) 0.003(2) 0.016(2) -0.002(2) C12 0.023(3) 0.022(2) 0.028(3) 0.000(2) 0.012(2) 0.0026(19) C12X 0.034(3) 0.023(2) 0.031(3) 0.002(2) 0.015(2) -0.004(2) C13X 0.033(3) 0.021(2) 0.027(3) 0.007(2) 0.010(2) 0.000(2) C14X 0.033(3) 0.017(2) 0.024(2) 0.0045(19) 0.017(2) 0.0018(19) C15X 0.022(3) 0.026(2) 0.023(2) 0.005(2) 0.011(2) 0.0027(19) C16X 0.036(3) 0.024(2) 0.034(3) 0.009(2) 0.018(2) 0.007(2) C17X 0.039(3) 0.023(2) 0.032(3) 0.000(2) 0.013(2) -0.005(2) C20 0.014(2) 0.021(2) 0.021(2) 0.0038(19) 0.0021(18) 0.0023(17) C21 0.016(2) 0.033(2) 0.018(2) 0.0012(19) 0.0101(18) 0.0043(19) C22 0.015(2) 0.048(3) 0.023(2) -0.006(2) 0.0075(19) 0.001(2) C23 0.014(2) 0.049(3) 0.025(2) -0.009(2) 0.0102(19) 0.002(2) C24 0.028(3) 0.072(4) 0.036(3) -0.025(3) 0.015(3) -0.002(3) C25 0.024(3) 0.065(4) 0.038(3) -0.027(3) 0.008(2) -0.011(3) C26 0.015(3) 0.050(3) 0.030(3) 0.001(2) 0.010(2) -0.001(2) C27 0.013(2) 0.050(3) 0.024(2) 0.002(2) 0.0093(19) 0.004(2) C28 0.017(2) 0.038(3) 0.021(2) -0.001(2) 0.0093(19) 0.000(2) C29 0.023(3) 0.046(3) 0.026(3) -0.002(2) 0.015(2) 0.009(2) C30 0.022(3) 0.036(3) 0.019(2) -0.002(2) 0.006(2) 0.006(2) C31 0.024(3) 0.041(3) 0.034(3) 0.003(2) 0.007(2) -0.002(2) C32 0.052(4) 0.024(2) 0.028(3) 0.002(2) 0.012(2) -0.009(2) C33 0.052(4) 0.037(3) 0.030(3) -0.010(2) 0.002(3) -0.011(3) C34 0.052(4) 0.025(2) 0.021(2) -0.004(2) 0.011(2) 0.011(2) C35 0.035(3) 0.036(3) 0.023(3) -0.007(2) 0.004(2) 0.020(2) C36 0.025(3) 0.039(3) 0.025(2) -0.008(2) 0.005(2) 0.004(2) C37 0.021(3) 0.044(3) 0.033(3) -0.009(2) 0.018(2) 0.004(2) C38 0.019(3) 0.035(3) 0.033(3) -0.003(2) 0.016(2) -0.002(2) C39 0.037(3) 0.040(3) 0.016(2) 0.004(2) 0.008(2) 0.009(2) C40 0.034(3) 0.029(3) 0.031(3) 0.007(2) 0.014(2) 0.008(2) C41 0.025(3) 0.019(2) 0.026(2) 0.0020(19) 0.011(2) 0.0065(19) C42 0.032(3) 0.025(2) 0.031(3) 0.002(2) 0.017(2) -0.001(2) O1O 0.224(9) 0.068(4) 0.185(8) -0.006(4) 0.148(7) -0.035(5) N1O 0.129(9) 0.178(10) 0.299(16) -0.171(11) 0.146(10) -0.064(8) C1O 0.143(10) 0.072(6) 0.157(10) -0.032(6) 0.103(8) -0.044(6) C2O 0.108(11) 0.61(4) 0.235(18) -0.31(2) 0.039(11) -0.002(16) C3O 0.060(9) 0.51(4) 0.31(3) 0.14(2) 0.048(12) 0.115(15) O1M 0.165(10) 0.158(9) 0.46(2) 0.137(10) 0.199(13) 0.068(7) N1M 0.142(9) 0.068(5) 0.224(13) 0.032(7) 0.105(10) 0.023(6) C1M 0.27(2) 0.090(9) 0.231(19) 0.051(10) 0.123(19) 0.012(12) C2M 0.186(15) 0.100(9) 0.192(15) 0.001(9) 0.012(13) 0.029(9) C3M 0.085(7) 0.114(8) 0.255(14) -0.019(9) 0.105(9) 0.007(6) S1V 0.1178(17) 0.0329(8) 0.0510(10) 0.0161(7) 0.0499(11) 0.0208(9) F1V 0.118(5) 0.240(7) 0.063(3) 0.050(4) -0.012(3) -0.091(5) F2V 0.123(4) 0.106(4) 0.086(4) 0.016(3) 0.045(3) 0.004(3) F3V 0.107(5) 0.182(7) 0.243(8) 0.006(6) 0.096(5) -0.048(5) O1V 0.574(18) 0.042(3) 0.109(5) 0.025(3) 0.192(9) 0.090(6) O2V 0.280(9) 0.100(4) 0.046(3) 0.039(3) 0.071(4) 0.131(5) O3V 0.128(6) 0.176(7) 0.123(6) 0.108(5) 0.026(5) -0.006(5) C1V 0.174(12) 0.129(9) 0.076(6) 0.039(6) 0.077(7) -0.036(8) S1W 0.0295(7) 0.0323(6) 0.0253(6) 0.0065(5) 0.0068(5) -0.0048(5) F1W 0.051(2) 0.052(2) 0.101(3) 0.041(2) 0.046(2) 0.0142(17) F2W 0.041(2) 0.097(3) 0.102(3) 0.045(3) 0.047(2) 0.038(2) F3W 0.102(4) 0.146(4) 0.035(2) -0.017(2) 0.030(2) 0.000(3) O1W 0.075(3) 0.101(4) 0.028(2) -0.022(2) 0.021(2) -0.011(3) O2W 0.035(3) 0.122(4) 0.057(3) 0.033(3) 0.013(2) -0.005(3) O3W 0.173(6) 0.027(2) 0.132(5) 0.021(3) 0.087(5) 0.010(3) C1W 0.040(3) 0.041(3) 0.033(3) 0.000(3) 0.015(3) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.902(3) . ? Cu1 N2 2.001(4) . ? Cu1 N1 2.035(4) . ? Cu1 N3 2.048(4) . ? Cu2 O4 1.905(3) . ? Cu2 N5 1.989(4) 5_565 ? Cu2 N4 2.084(4) 5_565 ? Cu2 N6 2.086(4) 5_565 ? O1 C20 1.284(5) . ? O2 C20 1.228(5) . ? O3 C31 1.233(6) . ? O4 C31 1.272(6) . ? N1 C2 1.482(5) . ? N1 C3 1.498(5) . ? N1 C1 1.505(6) . ? N2 C5 1.478(5) . ? N2 C4 1.488(6) . ? N2 C6 1.490(6) . ? N3 C7 1.486(5) . ? N3 C8 1.491(6) . ? N3 C9 1.497(6) . ? N4 C33 1.490(6) . ? N4 C32 1.490(6) . ? N4 C34 1.498(6) . ? N4 Cu2 2.084(4) 5_565 ? N5 C36 1.473(5) . ? N5 C37 1.486(6) . ? N5 C35 1.496(6) . ? N5 Cu2 1.989(4) 5_565 ? N6 C38 1.488(6) . ? N6 C39 1.494(5) . ? N6 C40 1.507(6) . ? N6 Cu2 2.086(4) 5_565 ? C1 C15X 1.511(6) . ? C3 C4 1.505(7) . ? C6 C7 1.519(7) . ? C9 C10 1.509(6) . ? C10 C11 1.396(6) . ? C10 C11X 1.400(6) . ? C11 C12 1.386(6) . ? C11X C42 1.372(7) . ? C12 C41 1.407(6) . ? C12X C17X 1.398(7) . ? C12X C13X 1.398(6) . ? C12X C32 1.506(7) . ? C13X C14X 1.382(6) . ? C14X C15X 1.384(6) . ? C15X C16X 1.394(6) . ? C16X C17X 1.365(7) . ? C20 C21 1.516(6) . ? C21 C22 1.355(6) . ? C21 C30 1.429(6) . ? C22 C23 1.404(6) . ? C23 C24 1.409(7) . ? C23 C28 1.443(6) . ? C24 C25 1.368(7) . ? C25 C26 1.413(7) . ? C26 C27 1.362(7) . ? C26 C31 1.500(7) . ? C27 C28 1.415(6) . ? C28 C29 1.395(6) . ? C29 C30 1.360(6) . ? C34 C35 1.510(7) . ? C37 C38 1.503(6) . ? C40 C41 1.502(6) . ? C41 C42 1.384(6) . ? O1O C1O 1.277(11) . ? N1O C1O 1.375(15) . ? N1O C2O 1.471(15) . ? N1O C3O 1.51(2) . ? O1M C1M 1.262(19) . ? N1M C3M 1.421(12) . ? N1M C1M 1.434(18) . ? N1M C2M 1.500(14) . ? S1V O1V 1.307(5) . ? S1V O2V 1.395(5) . ? S1V O3V 1.474(6) . ? S1V C1V 1.829(13) . ? F1V C1V 1.379(10) . ? F2V C1V 1.398(11) . ? F3V C1V 1.218(10) . ? S1W O3W 1.397(4) . ? S1W O1W 1.430(4) . ? S1W O2W 1.448(4) . ? S1W C1W 1.801(5) . ? F1W C1W 1.314(6) . ? F2W C1W 1.279(6) . ? F3W C1W 1.349(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 167.44(13) . . ? O1 Cu1 N1 95.16(14) . . ? N2 Cu1 N1 85.41(14) . . ? O1 Cu1 N3 96.95(13) . . ? N2 Cu1 N3 86.03(14) . . ? N1 Cu1 N3 160.65(15) . . ? O4 Cu2 N5 166.99(14) . 5_565 ? O4 Cu2 N4 92.81(15) . 5_565 ? N5 Cu2 N4 85.57(16) 5_565 5_565 ? O4 Cu2 N6 93.87(14) . 5_565 ? N5 Cu2 N6 85.31(15) 5_565 5_565 ? N4 Cu2 N6 166.61(15) 5_565 5_565 ? C20 O1 Cu1 136.8(3) . . ? C31 O4 Cu2 120.9(3) . . ? C2 N1 C3 110.0(4) . . ? C2 N1 C1 108.0(3) . . ? C3 N1 C1 110.1(4) . . ? C2 N1 Cu1 101.3(3) . . ? C3 N1 Cu1 108.6(3) . . ? C1 N1 Cu1 118.3(3) . . ? C5 N2 C4 110.7(3) . . ? C5 N2 C6 110.5(3) . . ? C4 N2 C6 112.3(4) . . ? C5 N2 Cu1 108.5(3) . . ? C4 N2 Cu1 107.8(3) . . ? C6 N2 Cu1 106.8(3) . . ? C7 N3 C8 111.2(4) . . ? C7 N3 C9 110.3(4) . . ? C8 N3 C9 106.4(3) . . ? C7 N3 Cu1 107.6(3) . . ? C8 N3 Cu1 101.8(3) . . ? C9 N3 Cu1 119.2(3) . . ? C33 N4 C32 108.0(4) . . ? C33 N4 C34 109.4(4) . . ? C32 N4 C34 110.6(4) . . ? C33 N4 Cu2 104.5(3) . 5_565 ? C32 N4 Cu2 116.7(3) . 5_565 ? C34 N4 Cu2 107.4(3) . 5_565 ? C36 N5 C37 110.9(4) . . ? C36 N5 C35 110.5(4) . . ? C37 N5 C35 111.2(3) . . ? C36 N5 Cu2 112.1(3) . 5_565 ? C37 N5 Cu2 105.6(3) . 5_565 ? C35 N5 Cu2 106.3(3) . 5_565 ? C38 N6 C39 108.4(3) . . ? C38 N6 C40 110.3(4) . . ? C39 N6 C40 107.0(3) . . ? C38 N6 Cu2 106.7(3) . 5_565 ? C39 N6 Cu2 102.3(3) . 5_565 ? C40 N6 Cu2 121.3(3) . 5_565 ? N1 C1 C15X 115.3(3) . . ? N1 C3 C4 108.9(4) . . ? N2 C4 C3 108.6(4) . . ? N2 C6 C7 108.0(4) . . ? N3 C7 C6 109.9(4) . . ? N3 C9 C10 114.3(4) . . ? C11 C10 C11X 116.8(4) . . ? C11 C10 C9 119.9(4) . . ? C11X C10 C9 123.1(4) . . ? C12 C11 C10 122.0(4) . . ? C42 C11X C10 121.4(4) . . ? C11 C12 C41 120.3(4) . . ? C17X C12X C13X 117.2(4) . . ? C17X C12X C32 121.2(4) . . ? C13X C12X C32 121.5(4) . . ? C14X C13X C12X 120.9(4) . . ? C13X C14X C15X 121.4(4) . . ? C14X C15X C16X 117.5(4) . . ? C14X C15X C1 122.3(4) . . ? C16X C15X C1 120.0(4) . . ? C17X C16X C15X 121.5(4) . . ? C16X C17X C12X 121.4(4) . . ? O2 C20 O1 126.3(4) . . ? O2 C20 C21 120.5(4) . . ? O1 C20 C21 113.1(4) . . ? C22 C21 C30 119.0(4) . . ? C22 C21 C20 120.9(4) . . ? C30 C21 C20 120.1(4) . . ? C21 C22 C23 122.5(4) . . ? C22 C23 C24 122.0(4) . . ? C22 C23 C28 118.5(4) . . ? C24 C23 C28 119.5(4) . . ? C25 C24 C23 120.2(5) . . ? C24 C25 C26 121.1(5) . . ? C27 C26 C25 119.5(4) . . ? C27 C26 C31 121.8(4) . . ? C25 C26 C31 118.6(5) . . ? C26 C27 C28 122.0(4) . . ? C29 C28 C27 124.7(4) . . ? C29 C28 C23 117.7(4) . . ? C27 C28 C23 117.6(4) . . ? C30 C29 C28 122.6(4) . . ? C29 C30 C21 119.8(4) . . ? O3 C31 O4 124.6(5) . . ? O3 C31 C26 118.5(5) . . ? O4 C31 C26 116.9(5) . . ? N4 C32 C12X 114.9(4) . . ? N4 C34 C35 109.3(4) . . ? N5 C35 C34 108.7(4) . . ? N5 C37 C38 107.8(3) . . ? N6 C38 C37 109.9(4) . . ? C41 C40 N6 116.3(4) . . ? C42 C41 C12 117.6(4) . . ? C42 C41 C40 121.8(4) . . ? C12 C41 C40 120.5(4) . . ? C11X C42 C41 122.0(4) . . ? C1O N1O C2O 112.2(16) . . ? C1O N1O C3O 129.3(13) . . ? C2O N1O C3O 117.2(14) . . ? O1O C1O N1O 117.3(12) . . ? C3M N1M C1M 121.1(16) . . ? C3M N1M C2M 124.4(13) . . ? C1M N1M C2M 114.5(13) . . ? O1M C1M N1M 125(2) . . ? O1V S1V O2V 111.5(4) . . ? O1V S1V O3V 106.7(6) . . ? O2V S1V O3V 118.8(5) . . ? O1V S1V C1V 113.0(7) . . ? O2V S1V C1V 105.0(4) . . ? O3V S1V C1V 101.5(4) . . ? F3V C1V F1V 114.9(11) . . ? F3V C1V F2V 105.5(10) . . ? F1V C1V F2V 112.9(6) . . ? F3V C1V S1V 114.5(7) . . ? F1V C1V S1V 104.9(8) . . ? F2V C1V S1V 103.7(8) . . ? O3W S1W O1W 113.2(3) . . ? O3W S1W O2W 119.2(4) . . ? O1W S1W O2W 110.6(3) . . ? O3W S1W C1W 104.1(3) . . ? O1W S1W C1W 102.2(3) . . ? O2W S1W C1W 105.5(3) . . ? F2W C1W F1W 109.8(5) . . ? F2W C1W F3W 108.8(5) . . ? F1W C1W F3W 104.2(5) . . ? F2W C1W S1W 112.4(4) . . ? F1W C1W S1W 112.6(4) . . ? F3W C1W S1W 108.7(4) . . ? 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 N2 Cu1 O1 C20 166.3(6) . . . . ? N1 Cu1 O1 C20 74.2(4) . . . . ? N3 Cu1 O1 C20 -90.7(4) . . . . ? N5 Cu2 O4 C31 -179.3(6) 5_565 . . . ? N4 Cu2 O4 C31 -96.8(4) 5_565 . . . ? N6 Cu2 O4 C31 94.8(4) 5_565 . . . ? O1 Cu1 N1 C2 -83.7(3) . . . . ? N2 Cu1 N1 C2 108.9(3) . . . . ? N3 Cu1 N1 C2 44.9(5) . . . . ? O1 Cu1 N1 C3 160.5(3) . . . . ? N2 Cu1 N1 C3 -6.9(3) . . . . ? N3 Cu1 N1 C3 -71.0(5) . . . . ? O1 Cu1 N1 C1 34.1(3) . . . . ? N2 Cu1 N1 C1 -133.3(3) . . . . ? N3 Cu1 N1 C1 162.7(4) . . . . ? O1 Cu1 N2 C5 7.1(8) . . . . ? N1 Cu1 N2 C5 100.2(3) . . . . ? N3 Cu1 N2 C5 -97.2(3) . . . . ? O1 Cu1 N2 C4 -112.8(6) . . . . ? N1 Cu1 N2 C4 -19.7(3) . . . . ? N3 Cu1 N2 C4 142.9(3) . . . . ? O1 Cu1 N2 C6 126.2(6) . . . . ? N1 Cu1 N2 C6 -140.6(3) . . . . ? N3 Cu1 N2 C6 22.0(3) . . . . ? O1 Cu1 N3 C7 -162.8(3) . . . . ? N2 Cu1 N3 C7 5.0(3) . . . . ? N1 Cu1 N3 C7 68.9(5) . . . . ? O1 Cu1 N3 C8 80.2(3) . . . . ? N2 Cu1 N3 C8 -112.0(3) . . . . ? N1 Cu1 N3 C8 -48.1(5) . . . . ? O1 Cu1 N3 C9 -36.3(3) . . . . ? N2 Cu1 N3 C9 131.4(3) . . . . ? N1 Cu1 N3 C9 -164.7(4) . . . . ? C2 N1 C1 C15X -179.9(4) . . . . ? C3 N1 C1 C15X -59.7(5) . . . . ? Cu1 N1 C1 C15X 66.0(4) . . . . ? C2 N1 C3 C4 -78.0(5) . . . . ? C1 N1 C3 C4 163.1(3) . . . . ? Cu1 N1 C3 C4 32.1(4) . . . . ? C5 N2 C4 C3 -75.7(4) . . . . ? C6 N2 C4 C3 160.2(4) . . . . ? Cu1 N2 C4 C3 42.8(4) . . . . ? N1 C3 C4 N2 -49.8(5) . . . . ? C5 N2 C6 C7 73.5(4) . . . . ? C4 N2 C6 C7 -162.3(4) . . . . ? Cu1 N2 C6 C7 -44.4(4) . . . . ? C8 N3 C7 C6 79.8(5) . . . . ? C9 N3 C7 C6 -162.5(4) . . . . ? Cu1 N3 C7 C6 -30.9(4) . . . . ? N2 C6 C7 N3 50.7(5) . . . . ? C7 N3 C9 C10 65.5(5) . . . . ? C8 N3 C9 C10 -173.8(4) . . . . ? Cu1 N3 C9 C10 -59.7(4) . . . . ? N3 C9 C10 C11 86.5(5) . . . . ? N3 C9 C10 C11X -99.0(5) . . . . ? C11X C10 C11 C12 2.0(6) . . . . ? C9 C10 C11 C12 176.7(4) . . . . ? C11 C10 C11X C42 -1.3(7) . . . . ? C9 C10 C11X C42 -175.9(4) . . . . ? C10 C11 C12 C41 -1.3(7) . . . . ? C17X C12X C13X C14X -0.9(7) . . . . ? C32 C12X C13X C14X 176.5(5) . . . . ? C12X C13X C14X C15X -0.7(7) . . . . ? C13X C14X C15X C16X 1.8(7) . . . . ? C13X C14X C15X C1 -172.6(4) . . . . ? N1 C1 C15X C14X -63.1(6) . . . . ? N1 C1 C15X C16X 122.6(5) . . . . ? C14X C15X C16X C17X -1.4(7) . . . . ? C1 C15X C16X C17X 173.2(4) . . . . ? C15X C16X C17X C12X -0.2(8) . . . . ? C13X C12X C17X C16X 1.3(7) . . . . ? C32 C12X C17X C16X -176.1(5) . . . . ? Cu1 O1 C20 O2 11.0(7) . . . . ? Cu1 O1 C20 C21 -168.7(3) . . . . ? O2 C20 C21 C22 -165.2(4) . . . . ? O1 C20 C21 C22 14.5(6) . . . . ? O2 C20 C21 C30 14.9(6) . . . . ? O1 C20 C21 C30 -165.4(4) . . . . ? C30 C21 C22 C23 1.1(7) . . . . ? C20 C21 C22 C23 -178.8(4) . . . . ? C21 C22 C23 C24 179.8(5) . . . . ? C21 C22 C23 C28 0.3(8) . . . . ? C22 C23 C24 C25 -177.5(6) . . . . ? C28 C23 C24 C25 2.0(9) . . . . ? C23 C24 C25 C26 -1.1(9) . . . . ? C24 C25 C26 C27 -0.2(9) . . . . ? C24 C25 C26 C31 176.3(5) . . . . ? C25 C26 C27 C28 0.6(8) . . . . ? C31 C26 C27 C28 -175.9(5) . . . . ? C26 C27 C28 C29 179.0(5) . . . . ? C26 C27 C28 C23 0.4(7) . . . . ? C22 C23 C28 C29 -0.8(7) . . . . ? C24 C23 C28 C29 179.6(5) . . . . ? C22 C23 C28 C27 177.9(5) . . . . ? C24 C23 C28 C27 -1.6(7) . . . . ? C27 C28 C29 C30 -178.7(5) . . . . ? C23 C28 C29 C30 0.0(7) . . . . ? C28 C29 C30 C21 1.5(7) . . . . ? C22 C21 C30 C29 -2.0(7) . . . . ? C20 C21 C30 C29 177.9(4) . . . . ? Cu2 O4 C31 O3 -2.9(7) . . . . ? Cu2 O4 C31 C26 177.9(3) . . . . ? C27 C26 C31 O3 169.5(5) . . . . ? C25 C26 C31 O3 -6.9(8) . . . . ? C27 C26 C31 O4 -11.2(7) . . . . ? C25 C26 C31 O4 172.3(5) . . . . ? C33 N4 C32 C12X 175.8(4) . . . . ? C34 N4 C32 C12X 56.2(5) . . . . ? Cu2 N4 C32 C12X -66.9(5) 5_565 . . . ? C17X C12X C32 N4 -119.2(5) . . . . ? C13X C12X C32 N4 63.5(6) . . . . ? C33 N4 C34 C35 84.4(5) . . . . ? C32 N4 C34 C35 -156.8(4) . . . . ? Cu2 N4 C34 C35 -28.4(4) 5_565 . . . ? C36 N5 C35 C34 74.2(5) . . . . ? C37 N5 C35 C34 -162.2(4) . . . . ? Cu2 N5 C35 C34 -47.7(4) 5_565 . . . ? N4 C34 C35 N5 51.0(5) . . . . ? C36 N5 C37 C38 -71.8(5) . . . . ? C35 N5 C37 C38 164.9(4) . . . . ? Cu2 N5 C37 C38 49.9(4) 5_565 . . . ? C39 N6 C38 C37 -81.3(4) . . . . ? C40 N6 C38 C37 161.9(4) . . . . ? Cu2 N6 C38 C37 28.3(4) 5_565 . . . ? N5 C37 C38 N6 -52.8(5) . . . . ? C38 N6 C40 C41 -56.1(5) . . . . ? C39 N6 C40 C41 -173.9(4) . . . . ? Cu2 N6 C40 C41 69.6(5) 5_565 . . . ? C11 C12 C41 C42 -0.1(6) . . . . ? C11 C12 C41 C40 -175.2(4) . . . . ? N6 C40 C41 C42 96.2(5) . . . . ? N6 C40 C41 C12 -89.0(5) . . . . ? C10 C11X C42 C41 0.0(7) . . . . ? C12 C41 C42 C11X 0.7(7) . . . . ? C40 C41 C42 C11X 175.8(4) . . . . ? C2O N1O C1O O1O -175.1(11) . . . . ? C3O N1O C1O O1O -8.6(17) . . . . ? C3M N1M C1M O1M 177.5(12) . . . . ? C2M N1M C1M O1M -3.9(18) . . . . ? O1V S1V C1V F3V -73.7(10) . . . . ? O2V S1V C1V F3V 48.0(11) . . . . ? O3V S1V C1V F3V 172.3(9) . . . . ? O1V S1V C1V F1V 53.2(7) . . . . ? O2V S1V C1V F1V 174.9(6) . . . . ? O3V S1V C1V F1V -60.8(7) . . . . ? O1V S1V C1V F2V 171.8(5) . . . . ? O2V S1V C1V F2V -66.5(6) . . . . ? O3V S1V C1V F2V 57.9(6) . . . . ? O3W S1W C1W F2W -53.7(5) . . . . ? O1W S1W C1W F2W 64.3(5) . . . . ? O2W S1W C1W F2W 180.0(4) . . . . ? O3W S1W C1W F1W -178.4(5) . . . . ? O1W S1W C1W F1W -60.4(5) . . . . ? O2W S1W C1W F1W 55.3(5) . . . . ? O3W S1W C1W F3W 66.8(5) . . . . ? O1W S1W C1W F3W -175.2(4) . . . . ? O2W S1W C1W F3W -59.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.39 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.360 _refine_diff_density_min -0.955 _refine_diff_density_rms 0.114 #===END data_mc2baf1g(5BArF)_CCDC648101 _database_code_depnum_ccdc_archive 'CCDC 648101' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H110 Fe4 N12 O8, 4(C32 H12 B F24), 4(C4 H10 O), 2(C H2 Cl2)' _chemical_formula_sum 'C230 H202 B4 Cl4 F96 Fe4 N12 O12' _chemical_formula_weight 5558.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.427(3) _cell_length_b 19.209(3) _cell_length_c 19.274(3) _cell_angle_alpha 88.204(3) _cell_angle_beta 72.320(2) _cell_angle_gamma 76.923(2) _cell_volume 6326.4(17) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2818 _exptl_absorpt_coefficient_mu 0.396 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 97776 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0734 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.70 _reflns_number_total 29315 _reflns_number_gt 19494 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER Shelxtl' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)/PLATON' _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. A considerable amount of electron density attibutable to partially disordered solvent molecules (CH2Cl2 and CH3CH2OCH2CH3) were removed with the SQUEEZE option of PLATON (Spek, A. L. (2005). PLATON, A Multipurpose Crystallographic Tool,Utrecht University, Utrecht, THe Netherlands. Those solvent molecules are, however, included in the reported chemical formula and derived values (e.g. formula weight, F_000, etc). The macrocyclic coordination complex lies about an inversion centre. ; 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 0.000 0.000 0.500 1293.3 139.0 2 0.393 0.334 0.372 18.9 1.1 3 0.484 0.281 0.063 7.3 0.2 4 0.516 0.719 0.938 7.3 0.2 5 0.607 0.666 0.628 18.9 0.4 _platon_squeeze_details ; ; _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^)+(0.1075P)^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 29315 _refine_ls_number_parameters 1570 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1927 _refine_ls_wR_factor_gt 0.1799 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.082 _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 Fe1 Fe 0.34059(2) 0.138445(18) 0.866290(18) 0.01604(9) Uani 1 1 d . . . Fe2 Fe 0.52847(2) -0.377675(19) 0.388440(18) 0.01540(9) Uani 1 1 d . . . O1 O 0.38400(12) 0.06962(11) 0.78631(11) 0.0314(5) Uani 1 1 d . . . O2 O 0.34521(13) -0.00813(11) 0.86933(11) 0.0378(5) Uani 1 1 d . . . O3 O 0.45479(13) -0.39133(12) 0.55018(11) 0.0365(5) Uani 1 1 d . . . O4 O 0.48865(12) -0.30981(11) 0.46805(11) 0.0318(5) Uani 1 1 d . . . N1 N 0.22584(14) 0.15765(14) 0.86249(13) 0.0315(6) Uani 1 1 d . . . N2 N 0.30462(14) 0.22861(13) 0.92784(13) 0.0301(5) Uani 1 1 d . . . N3 N 0.43654(14) 0.11977(13) 0.90477(13) 0.0296(5) Uani 1 1 d . . . N4 N 0.57798(15) 0.36882(14) 0.63134(13) 0.0323(6) Uani 1 1 d . . . N5 N 0.42596(14) 0.43829(13) 0.70323(13) 0.0288(5) Uani 1 1 d . . . N6 N 0.36250(14) 0.41503(13) 0.59626(13) 0.0278(5) Uani 1 1 d . . . C1 C 0.21692(18) 0.15420(17) 0.78811(17) 0.0341(7) Uani 1 1 d . . . H1A H 0.1618 0.1604 0.7933 0.041 Uiso 1 1 calc R . . H1B H 0.2434 0.1068 0.7663 0.041 Uiso 1 1 calc R . . C2 C 0.18914(19) 0.10100(18) 0.90578(19) 0.0420(8) Uani 1 1 d . . . H2A H 0.1352 0.1097 0.9076 0.063 Uiso 1 1 calc R . . H2B H 0.1926 0.1024 0.9544 0.063 Uiso 1 1 calc R . . H2C H 0.2162 0.0548 0.8829 0.063 Uiso 1 1 calc R . . C3 C 0.18423(18) 0.22863(17) 0.90073(18) 0.0372(7) Uani 1 1 d . . . H3A H 0.1289 0.2299 0.9216 0.045 Uiso 1 1 calc R . . H3B H 0.1898 0.2663 0.8661 0.045 Uiso 1 1 calc R . . C4 C 0.21830(18) 0.24087(18) 0.96076(17) 0.0366(7) Uani 1 1 d . . . H4A H 0.1968 0.2894 0.9812 0.044 Uiso 1 1 calc R . . H4B H 0.2056 0.2080 0.9995 0.044 Uiso 1 1 calc R . . C5 C 0.32503(19) 0.28776(16) 0.88030(17) 0.0347(7) Uani 1 1 d . . . H5A H 0.3077 0.3318 0.9089 0.052 Uiso 1 1 calc R . . H5B H 0.2999 0.2915 0.8429 0.052 Uiso 1 1 calc R . . H5C H 0.3807 0.2783 0.8583 0.052 Uiso 1 1 calc R . . C6 C 0.34609(18) 0.22026(17) 0.98424(16) 0.0336(7) Uani 1 1 d . . . H6A H 0.3233 0.1905 1.0225 0.040 Uiso 1 1 calc R . . H6B H 0.3414 0.2666 1.0059 0.040 Uiso 1 1 calc R . . C7 C 0.43150(18) 0.18563(17) 0.94736(17) 0.0342(7) Uani 1 1 d . . . H7A H 0.4564 0.2189 0.9150 0.041 Uiso 1 1 calc R . . H7B H 0.4584 0.1730 0.9837 0.041 Uiso 1 1 calc R . . C8 C 0.4263(2) 0.06034(17) 0.95631(18) 0.0387(7) Uani 1 1 d . . . H8A H 0.4672 0.0515 0.9789 0.058 Uiso 1 1 calc R . . H8B H 0.4287 0.0178 0.9300 0.058 Uiso 1 1 calc R . . H8C H 0.3764 0.0736 0.9931 0.058 Uiso 1 1 calc R . . C9 C 0.51580(17) 0.09668(17) 0.84898(17) 0.0339(7) Uani 1 1 d . . . H9A H 0.5163 0.0545 0.8223 0.041 Uiso 1 1 calc R . . H9B H 0.5546 0.0830 0.8744 0.041 Uiso 1 1 calc R . . C10 C 0.53995(17) 0.15198(16) 0.79488(16) 0.0307(6) Uani 1 1 d . . . C11 C 0.50384(19) 0.17389(19) 0.74153(19) 0.0411(8) Uani 1 1 d . . . H11A H 0.4607 0.1567 0.7410 0.049 Uiso 1 1 calc R . . C12 C 0.53086(19) 0.22072(19) 0.68944(19) 0.0415(8) Uani 1 1 d . . . H12A H 0.5056 0.2342 0.6544 0.050 Uiso 1 1 calc R . . C13 C 0.59446(16) 0.24799(16) 0.68817(16) 0.0305(6) Uani 1 1 d . . . C14 C 0.6303(2) 0.2257(2) 0.7413(2) 0.0478(9) Uani 1 1 d . . . H14A H 0.6735 0.2428 0.7420 0.057 Uiso 1 1 calc R . . C15 C 0.6033(2) 0.1787(2) 0.79332(19) 0.0458(9) Uani 1 1 d . . . H68A H 0.6262 0.1642 0.8268 0.079(14) Uiso 1 1 d R . . C16 C 0.62761(17) 0.29498(17) 0.62967(17) 0.0354(7) Uani 1 1 d . . . H16A H 0.6759 0.2795 0.5945 0.042 Uiso 1 1 calc R . . C17 C 0.6225(2) 0.40842(19) 0.57203(18) 0.0411(8) Uani 1 1 d . . . H17A H 0.6715 0.4095 0.5795 0.062 Uiso 1 1 calc R . . H17B H 0.5927 0.4565 0.5726 0.062 Uiso 1 1 calc R . . H17C H 0.6321 0.3849 0.5259 0.062 Uiso 1 1 calc R . . C18 C 0.56186(19) 0.40838(18) 0.70269(17) 0.0363(7) Uani 1 1 d . . . H18A H 0.6063 0.4277 0.7022 0.044 Uiso 1 1 calc R . . H18B H 0.5533 0.3760 0.7425 0.044 Uiso 1 1 calc R . . C19 C 0.48959(19) 0.46869(17) 0.71328(17) 0.0359(7) Uani 1 1 d . . . H19A H 0.4737 0.4907 0.7618 0.043 Uiso 1 1 calc R . . H19B H 0.5008 0.5050 0.6781 0.043 Uiso 1 1 calc R . . C20 C 0.3961(2) 0.39498(17) 0.76527(16) 0.0366(7) Uani 1 1 d . . . H20A H 0.3741 0.4248 0.8090 0.055 Uiso 1 1 calc R . . H20B H 0.4382 0.3574 0.7704 0.055 Uiso 1 1 calc R . . H20C H 0.3565 0.3745 0.7568 0.055 Uiso 1 1 calc R . . C21 C 0.36055(19) 0.49572(17) 0.69331(17) 0.0356(7) Uani 1 1 d . . . H21A H 0.3811 0.5304 0.6599 0.043 Uiso 1 1 calc R . . H21B H 0.3294 0.5202 0.7396 0.043 Uiso 1 1 calc R . . C22 C 0.31065(18) 0.45952(16) 0.66242(17) 0.0333(7) Uani 1 1 d . . . H22A H 0.2847 0.4296 0.6986 0.040 Uiso 1 1 calc R . . H22B H 0.2709 0.4954 0.6497 0.040 Uiso 1 1 calc R . . C23 C 0.37538(19) 0.46395(16) 0.53407(16) 0.0339(7) Uani 1 1 d . . . H23A H 0.3260 0.4870 0.5277 0.051 Uiso 1 1 calc R . . H23B H 0.4081 0.4368 0.4903 0.051 Uiso 1 1 calc R . . H23C H 0.4004 0.4995 0.5442 0.051 Uiso 1 1 calc R . . C24 C 0.32457(18) 0.36107(16) 0.57648(16) 0.0297(6) Uani 1 1 d . . . H24A H 0.3606 0.3339 0.5333 0.036 Uiso 1 1 calc R . . H24B H 0.2787 0.3863 0.5638 0.036 Uiso 1 1 calc R . . C25 C 0.29994(16) 0.30923(16) 0.63446(15) 0.0274(6) Uani 1 1 d . . . C26 C 0.22382(17) 0.32224(18) 0.68061(17) 0.0367(7) Uani 1 1 d . . . H26A H 0.1892 0.3652 0.6784 0.044 Uiso 1 1 calc R . . C27 C 0.19845(18) 0.27254(19) 0.72981(18) 0.0393(8) Uani 1 1 d . . . H27A H 0.1467 0.2821 0.7593 0.047 Uiso 1 1 calc R . . C28 C 0.24845(17) 0.20904(16) 0.73612(16) 0.0300(6) Uani 1 1 d . . . C29 C 0.32503(17) 0.19532(16) 0.69041(16) 0.0296(6) Uani 1 1 d . . . H29A H 0.3596 0.1526 0.6936 0.036 Uiso 1 1 calc R . . C30 C 0.35071(17) 0.24471(16) 0.63991(15) 0.0280(6) Uani 1 1 d . . . H30A H 0.4021 0.2347 0.6095 0.034 Uiso 1 1 calc R . . C31 C 0.37314(17) 0.00673(16) 0.80546(16) 0.0308(6) Uani 1 1 d . . . C32 C 0.39476(17) -0.04833(16) 0.74437(16) 0.0310(6) Uani 1 1 d . . . C33 C 0.38341(16) -0.11531(16) 0.76043(15) 0.0280(6) Uani 1 1 d . . . H33A H 0.3635 -0.1263 0.8088 0.034 Uiso 1 1 calc R . . C34 C 0.40137(16) -0.16820(15) 0.70503(15) 0.0265(6) Uani 1 1 d . . . C35 C 0.39086(19) -0.23847(16) 0.72090(16) 0.0340(7) Uani 1 1 d . . . H35A H 0.3708 -0.2501 0.7691 0.041 Uiso 1 1 calc R . . C36 C 0.40967(19) -0.28942(17) 0.66653(17) 0.0353(7) Uani 1 1 d . . . H36A H 0.4025 -0.3353 0.6779 0.042 Uiso 1 1 calc R . . C37 C 0.44009(16) -0.27241(16) 0.59287(15) 0.0282(6) Uani 1 1 d . . . C38 C 0.45003(18) -0.20510(16) 0.57628(16) 0.0325(7) Uani 1 1 d . . . H38A H 0.4690 -0.1940 0.5277 0.039 Uiso 1 1 calc R . . C39 C 0.43205(18) -0.15185(16) 0.63158(16) 0.0316(7) Uani 1 1 d . . . C40 C 0.4437(2) -0.08114(19) 0.61629(18) 0.0487(9) Uani 1 1 d . . . H40A H 0.4638 -0.0691 0.5682 0.058 Uiso 1 1 calc R . . C41 C 0.4259(2) -0.03127(18) 0.67107(18) 0.0456(9) Uani 1 1 d . . . H41A H 0.4342 0.0143 0.6602 0.055 Uiso 1 1 calc R . . C42 C 0.46160(17) -0.32998(16) 0.53439(16) 0.0299(6) Uani 1 1 d . . . F1B F 0.92732(17) 0.51267(15) 0.07356(14) 0.0838(9) Uani 1 1 d . . . F2B F 0.9123(2) 0.53434(16) 0.18367(16) 0.0958(10) Uani 1 1 d . . . F3B F 0.82420(15) 0.58119(13) 0.1378(2) 0.0916(10) Uani 1 1 d . . . F4B F 0.74272(13) 0.35795(12) 0.36359(10) 0.0579(6) Uani 1 1 d . . . F5B F 0.80350(16) 0.26058(12) 0.30377(12) 0.0673(7) Uani 1 1 d . . . F6B F 0.86821(13) 0.32983(16) 0.32780(12) 0.0736(8) Uani 1 1 d . . . F7B F 0.78125(13) 0.33551(15) -0.26059(11) 0.0723(8) Uani 1 1 d . . . F8B F 0.66966(12) 0.35580(13) -0.17729(11) 0.0580(6) Uani 1 1 d . . . F9B F 0.72269(15) 0.44268(14) -0.21724(13) 0.0719(7) Uani 1 1 d . . . F10B F 1.01160(12) 0.34972(13) -0.08133(13) 0.0614(6) Uani 1 1 d . . . F11B F 1.01292(12) 0.25404(13) -0.13445(16) 0.0720(7) Uani 1 1 d . . . F12B F 1.01695(13) 0.35216(16) -0.19251(13) 0.0739(7) Uani 1 1 d . . . F13B F 0.46793(11) 0.61009(10) 0.03133(11) 0.0442(5) Uani 1 1 d . . . F14B F 0.51746(14) 0.64040(10) 0.10904(11) 0.0530(5) Uani 1 1 d . . . F15B F 0.59125(11) 0.60311(11) 0.00096(12) 0.0558(6) Uani 1 1 d . . . F16B F 0.39288(15) 0.43096(15) 0.26168(13) 0.0768(8) Uani 1 1 d . . . F17B F 0.36305(13) 0.40875(17) 0.16960(14) 0.0825(8) Uani 1 1 d . . . F18B F 0.43877(14) 0.32893(14) 0.2087(2) 0.1057(12) Uani 1 1 d . . . F19B F 0.88618(15) 0.03043(13) 0.0500(2) 0.1029(12) Uani 1 1 d . . . F20B F 0.93395(16) 0.11666(14) 0.0587(3) 0.1235(15) Uani 1 1 d . . . F21B F 0.8601(3) 0.0841(3) 0.1507(2) 0.199(3) Uani 1 1 d . . . F22B F 0.56769(11) 0.13060(12) 0.05428(11) 0.0512(5) Uani 1 1 d . . . F23B F 0.66198(14) 0.07886(15) -0.03478(15) 0.0823(9) Uani 1 1 d . . . F24B F 0.60313(16) 0.18863(14) -0.04080(13) 0.0732(8) Uani 1 1 d . . . C1B C 0.76375(16) 0.38011(16) 0.12810(16) 0.0277(6) Uani 1 1 d . . . C2B C 0.79967(16) 0.43795(16) 0.11318(16) 0.0292(6) Uani 1 1 d . . . H2BA H 0.7983 0.4630 0.0714 0.035 Uiso 1 1 calc R . . C3B C 0.83755(17) 0.45956(17) 0.15859(16) 0.0311(6) Uani 1 1 d . . . C4B C 0.84176(17) 0.42248(17) 0.22162(16) 0.0331(7) Uani 1 1 d . . . H4BA H 0.8687 0.4355 0.2510 0.040 Uiso 1 1 calc R . . C5B C 0.80536(17) 0.36675(17) 0.23888(15) 0.0314(7) Uani 1 1 d . . . C6B C 0.76646(17) 0.34595(16) 0.19363(16) 0.0303(6) Uani 1 1 d . . . H6BA H 0.7416 0.3084 0.2072 0.036 Uiso 1 1 calc R . . C7B C 0.8751(2) 0.52163(19) 0.13808(19) 0.0394(8) Uani 1 1 d . . . C8B C 0.8057(2) 0.32819(19) 0.30769(17) 0.0406(8) Uani 1 1 d . . . C9B C 0.77123(16) 0.36229(15) -0.01291(15) 0.0248(6) Uani 1 1 d . . . C10B C 0.73654(17) 0.37056(16) -0.06871(16) 0.0293(6) Uani 1 1 d . . . H10A H 0.6823 0.3804 -0.0563 0.035 Uiso 1 1 calc R . . C11B C 0.78010(17) 0.36456(16) -0.14217(16) 0.0300(6) Uani 1 1 d . . . C12B C 0.86063(18) 0.35039(17) -0.16343(16) 0.0343(7) Uani 1 1 d . . . H12B H 0.8900 0.3461 -0.2124 0.041 Uiso 1 1 calc R . . C13B C 0.89634(17) 0.34265(17) -0.10820(16) 0.0331(7) Uani 1 1 d . . . C14B C 0.85253(16) 0.34794(16) -0.03546(16) 0.0289(6) Uani 1 1 d . . . H14B H 0.8784 0.3417 -0.0003 0.035 Uiso 1 1 calc R . . C15B C 0.7399(2) 0.3735(2) -0.19939(18) 0.0467(9) Uani 1 1 d . . . C16B C 0.98378(19) 0.3249(2) -0.12853(18) 0.0452(9) Uani 1 1 d . . . C17B C 0.63226(16) 0.40411(16) 0.09228(15) 0.0274(6) Uani 1 1 d . . . C18B C 0.61835(16) 0.47351(16) 0.06648(15) 0.0264(6) Uani 1 1 d . . . H18C H 0.6607 0.4914 0.0391 0.032 Uiso 1 1 calc R . . C19B C 0.54261(16) 0.51677(16) 0.08071(15) 0.0283(6) Uani 1 1 d . . . C20B C 0.47843(17) 0.49129(17) 0.12094(16) 0.0326(7) Uani 1 1 d . . . H20D H 0.4280 0.5191 0.1291 0.039 Uiso 1 1 calc R . . C21B C 0.49066(17) 0.42357(17) 0.14887(17) 0.0329(7) Uani 1 1 d . . . C22B C 0.56614(16) 0.38159(17) 0.13527(15) 0.0295(6) Uani 1 1 d . . . H22C H 0.5729 0.3369 0.1555 0.035 Uiso 1 1 calc R . . C23B C 0.53031(17) 0.59089(17) 0.05486(16) 0.0328(7) Uani 1 1 d . . . C24B C 0.42245(18) 0.39718(19) 0.1958(2) 0.0437(8) Uani 1 1 d . . . C25B C 0.72601(16) 0.26856(16) 0.07295(15) 0.0266(6) Uani 1 1 d . . . C26B C 0.78935(18) 0.21834(16) 0.08360(17) 0.0330(7) Uani 1 1 d . . . H26B H 0.8250 0.2343 0.1007 0.040 Uiso 1 1 calc R . . C27B C 0.80092(19) 0.14531(18) 0.06949(19) 0.0389(7) Uani 1 1 d . . . C28B C 0.74943(19) 0.11855(18) 0.04350(18) 0.0377(7) Uani 1 1 d . . . H28A H 0.7571 0.0698 0.0339 0.045 Uiso 1 1 calc R . . C29B C 0.68649(17) 0.16725(17) 0.03256(16) 0.0322(7) Uani 1 1 d . . . C30B C 0.67516(17) 0.23952(16) 0.04703(15) 0.0290(6) Uani 1 1 d . . . H30B H 0.6318 0.2705 0.0393 0.035 Uiso 1 1 calc R . . C31B C 0.8701(3) 0.0954(2) 0.0813(3) 0.0641(12) Uani 1 1 d . . . C32B C 0.6301(2) 0.14165(19) 0.00367(18) 0.0413(8) Uani 1 1 d . . . B1B B 0.72166(18) 0.35415(18) 0.07260(18) 0.0265(7) Uani 1 1 d . . . F1D F 0.76640(14) 0.46131(14) 0.62538(13) 0.0679(7) Uani 1 1 d . . . F2D F 0.83447(16) 0.45480(14) 0.51367(13) 0.0728(7) Uani 1 1 d . . . F3D F 0.74951(16) 0.54999(13) 0.55838(16) 0.0792(8) Uani 1 1 d . . . F4D F 1.11200(13) 0.48640(13) 0.63415(14) 0.0669(7) Uani 1 1 d . . . F5D F 1.04172(13) 0.41322(13) 0.67891(13) 0.0693(7) Uani 1 1 d . . . F6D F 1.09601(13) 0.41132(13) 0.56439(12) 0.0639(6) Uani 1 1 d . . . F7D F 0.8030(2) 0.53232(16) 0.87055(15) 0.0984(11) Uani 1 1 d . . . F8D F 0.88358(18) 0.51705(17) 0.9271(2) 0.1053(11) Uani 1 1 d . . . F9D F 0.77795(19) 0.59286(15) 0.96664(16) 0.1053(12) Uani 1 1 d . . . F10D F 0.94996(12) 0.79626(13) 0.93207(13) 0.0654(7) Uani 1 1 d . . . F11D F 1.04657(13) 0.77525(14) 0.83330(11) 0.0596(6) Uani 1 1 d . . . F12D F 1.03965(13) 0.70139(14) 0.91806(13) 0.0672(7) Uani 1 1 d . . . F13D F 1.1091(3) 0.6920(2) 0.41948(19) 0.1335(16) Uani 1 1 d . . . F14D F 1.1537(2) 0.7857(2) 0.4153(2) 0.164(2) Uani 1 1 d . . . F15D F 1.18341(19) 0.7010(2) 0.4839(3) 0.1391(16) Uani 1 1 d . . . F21D F 0.6284(2) 0.7874(3) 0.53712(17) 0.1444(18) Uani 1 1 d . . . F19D F 0.6618(4) 0.88279(19) 0.5297(2) 0.212(3) Uani 1 1 d . . . F20D F 0.74077(18) 0.7884(2) 0.48374(14) 0.1351(17) Uani 1 1 d . . . F22F F 0.6165(6) 0.8318(6) 0.8652(6) 0.064(3) Uiso 0.340(9) 1 d P A 1 F23F F 0.5599(4) 0.9043(4) 0.8123(4) 0.043(2) Uiso 0.340(9) 1 d P A 1 F24F F 0.5304(5) 0.8099(4) 0.8131(5) 0.048(2) Uiso 0.340(9) 1 d P A 1 F22D F 0.6050(3) 0.8016(4) 0.8672(2) 0.0675(16) Uani 0.660(9) 1 d PD A 2 F23D F 0.6151(7) 0.9084(4) 0.8326(4) 0.231(7) Uani 0.660(9) 1 d PD A 2 F24D F 0.5325(3) 0.8617(9) 0.8072(3) 0.266(9) Uani 0.660(9) 1 d PD A 2 C1D C 0.90210(17) 0.62707(18) 0.63759(15) 0.0323(7) Uani 1 1 d . . . C2D C 0.84914(19) 0.59892(17) 0.61554(16) 0.0343(7) Uani 1 1 d . . . H2DA H 0.8020 0.6290 0.6152 0.041 Uiso 1 1 calc R . . C3D C 0.8641(2) 0.52697(18) 0.59386(17) 0.0392(8) Uani 1 1 d . . . C4D C 0.9327(2) 0.48010(19) 0.59447(17) 0.0399(8) Uani 1 1 d . . . H4DA H 0.9425 0.4321 0.5807 0.048 Uiso 1 1 calc R . . C5D C 0.98706(19) 0.50663(18) 0.61629(17) 0.0377(7) Uani 1 1 d . . . C6D C 0.97196(18) 0.57812(18) 0.63713(16) 0.0345(7) Uani 1 1 d . . . H6DA H 1.0093 0.5944 0.6513 0.041 Uiso 1 1 calc R . . C7D C 0.8040(2) 0.4994(2) 0.5736(2) 0.0517(10) Uani 1 1 d . . . C8D C 1.0585(2) 0.4552(2) 0.62278(19) 0.0440(8) Uani 1 1 d . . . C9D C 0.89327(17) 0.69539(16) 0.75461(16) 0.0308(6) Uani 1 1 d . . . C10D C 0.85835(17) 0.64371(17) 0.79788(16) 0.0312(7) Uani 1 1 d . . . H10B H 0.8258 0.6225 0.7812 0.037 Uiso 1 1 calc R . . C11D C 0.87042(18) 0.62320(17) 0.86386(16) 0.0337(7) Uani 1 1 d . . . C12D C 0.91863(17) 0.65473(17) 0.89048(16) 0.0350(7) Uani 1 1 d . . . H12C H 0.9286 0.6404 0.9339 0.042 Uiso 1 1 calc R . . C13D C 0.95126(16) 0.70764(17) 0.85108(16) 0.0320(7) Uani 1 1 d . . . C14D C 0.93886(16) 0.72721(17) 0.78443(16) 0.0304(6) Uani 1 1 d . . . H14C H 0.9617 0.7627 0.7590 0.036 Uiso 1 1 calc R . . C15D C 0.8345(2) 0.56734(19) 0.90562(18) 0.0417(8) Uani 1 1 d . . . C16D C 0.99664(18) 0.7450(2) 0.88246(18) 0.0412(8) Uani 1 1 d . . . C17D C 0.94331(19) 0.75601(18) 0.62410(17) 0.0361(7) Uani 1 1 d . . . C18D C 1.0093(2) 0.7289(2) 0.5649(2) 0.0487(9) Uani 1 1 d . . . H18D H 1.0225 0.6802 0.5529 0.058 Uiso 1 1 calc R . . C19D C 1.0556(2) 0.7724(2) 0.5237(2) 0.0627(11) Uani 1 1 d . . . C20D C 1.0378(3) 0.8450(3) 0.5398(3) 0.0679(12) Uani 1 1 d . B . H20E H 1.0687 0.8742 0.5121 0.082 Uiso 1 1 calc R . . C21D C 0.9740(3) 0.8729(2) 0.5971(3) 0.0743(14) Uani 1 1 d . . . C22D C 0.9294(3) 0.8285(2) 0.6386(2) 0.0628(11) Uani 1 1 d . B . H22D H 0.8875 0.8488 0.6787 0.075 Uiso 1 1 calc R . . C23D C 1.1256(3) 0.7381(3) 0.4586(4) 0.0940(19) Uani 1 1 d . . . C25D C 0.79502(18) 0.75261(17) 0.67753(16) 0.0328(7) Uani 1 1 d . . . C26D C 0.77643(19) 0.76842(18) 0.61167(17) 0.0372(7) Uani 1 1 d . . . H26C H 0.8149 0.7535 0.5675 0.045 Uiso 1 1 calc R . . C27D C 0.70312(19) 0.80529(18) 0.61108(18) 0.0385(7) Uani 1 1 d . . . C28D C 0.6450(2) 0.8294(2) 0.67530(19) 0.0484(9) Uani 1 1 d . . . H28B H 0.5957 0.8547 0.6749 0.058 Uiso 1 1 calc R . . C29D C 0.6617(2) 0.8152(2) 0.74071(19) 0.0500(9) Uani 1 1 d . A . C30D C 0.73560(19) 0.77733(18) 0.74050(18) 0.0402(8) Uani 1 1 d . . . H30C H 0.7453 0.7683 0.7849 0.048 Uiso 1 1 calc R . . C31D C 0.6866(2) 0.8177(2) 0.5401(2) 0.0586(11) Uani 1 1 d . . . C32D C 0.5986(3) 0.8402(3) 0.8102(2) 0.0867(19) Uani 1 1 d . . . B1D B 0.8837(2) 0.7083(2) 0.67294(19) 0.0321(7) Uani 1 1 d . . . C24D C 0.9649(7) 0.9465(5) 0.6213(6) 0.075(4) Uani 0.606(14) 1 d P B 1 F18D F 1.0098(11) 0.9826(6) 0.5839(8) 0.157(7) Uani 0.606(14) 1 d P B 1 F17D F 0.8875(8) 0.9787(4) 0.6405(14) 0.181(8) Uani 0.606(14) 1 d P B 1 F16D F 0.9727(18) 0.9588(8) 0.6780(11) 0.309(13) Uani 0.606(14) 1 d P B 1 C24A C 0.9262(11) 0.9633(12) 0.5937(11) 0.072(5) Uani 0.394(14) 1 d P B 2 F18A F 0.9744(17) 0.9925(9) 0.5793(13) 0.149(10) Uani 0.394(14) 1 d P B 2 F17A F 0.8883(7) 0.9834(4) 0.5555(9) 0.123(6) Uani 0.394(14) 1 d P B 2 F16A F 0.925(3) 0.9670(12) 0.6834(12) 0.43(3) Uani 0.394(14) 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01820(18) 0.01579(19) 0.01344(18) -0.00009(13) -0.00526(14) -0.00182(14) Fe2 0.01999(18) 0.01794(19) 0.01028(17) -0.00161(13) -0.00549(14) -0.00686(14) O1 0.0369(11) 0.0272(11) 0.0290(11) -0.0015(9) -0.0092(9) -0.0060(9) O2 0.0536(14) 0.0320(12) 0.0266(11) -0.0018(9) -0.0089(10) -0.0113(10) O3 0.0427(12) 0.0367(13) 0.0294(11) -0.0070(9) -0.0043(10) -0.0157(10) O4 0.0352(11) 0.0361(12) 0.0253(11) -0.0048(9) -0.0085(9) -0.0110(9) N1 0.0313(13) 0.0365(15) 0.0272(13) 0.0062(11) -0.0097(11) -0.0082(11) N2 0.0327(13) 0.0305(14) 0.0248(13) 0.0018(10) -0.0078(11) -0.0040(11) N3 0.0329(13) 0.0275(13) 0.0272(13) 0.0002(10) -0.0111(11) -0.0016(10) N4 0.0361(14) 0.0394(15) 0.0273(13) 0.0034(11) -0.0124(11) -0.0168(12) N5 0.0368(13) 0.0288(13) 0.0236(12) -0.0005(10) -0.0116(11) -0.0095(11) N6 0.0339(13) 0.0288(13) 0.0226(12) 0.0001(10) -0.0107(10) -0.0079(10) C1 0.0341(16) 0.0404(18) 0.0328(17) 0.0062(14) -0.0137(14) -0.0141(14) C2 0.0371(17) 0.043(2) 0.043(2) 0.0101(16) -0.0059(15) -0.0132(15) C3 0.0333(16) 0.0385(18) 0.0358(18) 0.0042(14) -0.0103(14) -0.0013(14) C4 0.0349(16) 0.0402(19) 0.0284(16) -0.0010(14) -0.0064(14) 0.0000(14) C5 0.0441(18) 0.0286(16) 0.0283(16) 0.0018(13) -0.0096(14) -0.0042(14) C6 0.0410(17) 0.0354(17) 0.0247(15) -0.0041(13) -0.0126(13) -0.0047(14) C7 0.0373(16) 0.0369(18) 0.0302(16) -0.0005(13) -0.0150(14) -0.0051(14) C8 0.0490(19) 0.0358(18) 0.0347(17) 0.0105(14) -0.0204(16) -0.0073(15) C9 0.0279(15) 0.0353(17) 0.0353(17) -0.0014(14) -0.0100(13) 0.0000(13) C10 0.0279(14) 0.0307(16) 0.0321(16) -0.0020(13) -0.0112(13) -0.0008(12) C11 0.0385(17) 0.048(2) 0.048(2) 0.0138(16) -0.0228(16) -0.0197(15) C12 0.0405(18) 0.050(2) 0.045(2) 0.0143(16) -0.0261(16) -0.0173(16) C13 0.0254(14) 0.0335(17) 0.0315(16) -0.0034(13) -0.0082(12) -0.0048(12) C14 0.047(2) 0.065(2) 0.047(2) 0.0145(18) -0.0272(18) -0.0287(18) C15 0.047(2) 0.067(2) 0.0360(18) 0.0146(17) -0.0266(17) -0.0202(18) C16 0.0262(15) 0.0425(19) 0.0342(17) 0.0031(14) -0.0061(13) -0.0058(13) C17 0.0428(18) 0.053(2) 0.0354(18) 0.0075(15) -0.0121(15) -0.0276(16) C18 0.0430(18) 0.0459(19) 0.0304(16) 0.0011(14) -0.0201(14) -0.0187(15) C19 0.053(2) 0.0332(17) 0.0291(16) 0.0002(13) -0.0197(15) -0.0161(15) C20 0.0463(18) 0.0386(18) 0.0260(16) 0.0025(13) -0.0114(14) -0.0117(15) C21 0.0447(18) 0.0307(17) 0.0305(16) -0.0047(13) -0.0124(14) -0.0049(14) C22 0.0334(16) 0.0308(17) 0.0340(17) -0.0063(13) -0.0121(14) -0.0002(13) C23 0.0421(17) 0.0345(17) 0.0287(16) 0.0050(13) -0.0148(14) -0.0109(14) C24 0.0343(15) 0.0339(17) 0.0254(15) 0.0022(12) -0.0138(13) -0.0105(13) C25 0.0283(14) 0.0330(16) 0.0228(14) 0.0002(12) -0.0106(12) -0.0066(12) C26 0.0284(15) 0.0409(19) 0.0387(18) 0.0100(15) -0.0112(14) -0.0035(14) C27 0.0284(15) 0.050(2) 0.0372(18) 0.0106(15) -0.0078(14) -0.0091(14) C28 0.0300(15) 0.0353(17) 0.0291(15) 0.0012(13) -0.0137(13) -0.0094(13) C29 0.0327(15) 0.0312(16) 0.0270(15) 0.0017(12) -0.0127(13) -0.0065(13) C30 0.0278(14) 0.0333(16) 0.0247(14) -0.0006(12) -0.0095(12) -0.0084(12) C31 0.0322(15) 0.0293(16) 0.0304(16) -0.0006(13) -0.0098(13) -0.0053(13) C32 0.0334(15) 0.0273(16) 0.0300(16) -0.0037(12) -0.0086(13) -0.0030(12) C33 0.0302(14) 0.0325(16) 0.0211(14) -0.0014(12) -0.0064(12) -0.0082(12) C34 0.0270(14) 0.0246(15) 0.0285(15) -0.0002(12) -0.0097(12) -0.0050(11) C35 0.0467(18) 0.0332(17) 0.0217(14) 0.0009(12) -0.0051(13) -0.0158(14) C36 0.0451(18) 0.0303(17) 0.0301(16) -0.0034(13) -0.0053(14) -0.0155(14) C37 0.0272(14) 0.0320(16) 0.0268(15) -0.0050(12) -0.0078(12) -0.0092(12) C38 0.0399(17) 0.0336(17) 0.0209(14) -0.0011(12) -0.0048(13) -0.0079(14) C39 0.0391(17) 0.0307(16) 0.0242(15) -0.0007(12) -0.0085(13) -0.0074(13) C40 0.081(3) 0.039(2) 0.0230(16) 0.0017(14) -0.0057(17) -0.0218(19) C41 0.071(2) 0.0309(18) 0.0315(18) 0.0024(14) -0.0069(17) -0.0165(17) C42 0.0308(15) 0.0349(17) 0.0262(15) -0.0027(13) -0.0078(13) -0.0125(13) F1B 0.0946(19) 0.0868(19) 0.0646(16) -0.0155(14) 0.0158(15) -0.0626(16) F2B 0.148(3) 0.109(2) 0.091(2) 0.0352(17) -0.082(2) -0.094(2) F3B 0.0655(16) 0.0371(14) 0.172(3) 0.0109(16) -0.0349(18) -0.0147(12) F4B 0.0610(13) 0.0707(15) 0.0269(10) 0.0063(10) -0.0027(10) -0.0001(11) F5B 0.116(2) 0.0450(13) 0.0430(13) 0.0091(10) -0.0358(13) -0.0075(13) F6B 0.0572(14) 0.126(2) 0.0512(14) 0.0308(14) -0.0356(12) -0.0257(14) F7B 0.0488(13) 0.125(2) 0.0296(11) -0.0284(12) -0.0144(10) 0.0148(13) F8B 0.0428(11) 0.0978(18) 0.0398(12) -0.0072(11) -0.0238(10) -0.0120(11) F9B 0.0837(17) 0.0774(17) 0.0564(15) 0.0240(13) -0.0391(13) 0.0001(14) F10B 0.0346(11) 0.0818(17) 0.0730(16) 0.0005(13) -0.0180(11) -0.0211(11) F11B 0.0366(11) 0.0625(16) 0.111(2) -0.0227(14) -0.0258(13) 0.0078(11) F12B 0.0419(12) 0.120(2) 0.0535(15) 0.0207(14) -0.0039(11) -0.0226(13) F13B 0.0435(11) 0.0462(12) 0.0510(12) 0.0000(9) -0.0303(10) -0.0044(9) F14B 0.0826(15) 0.0390(11) 0.0512(12) -0.0054(9) -0.0418(12) -0.0109(10) F15B 0.0399(11) 0.0503(13) 0.0669(15) 0.0188(11) -0.0070(10) -0.0044(9) F16B 0.0714(16) 0.109(2) 0.0438(13) -0.0086(14) 0.0127(12) -0.0487(15) F17B 0.0478(13) 0.144(3) 0.0721(17) 0.0126(17) -0.0202(13) -0.0541(16) F18B 0.0481(14) 0.0525(16) 0.183(3) 0.0213(18) 0.0166(17) -0.0186(12) F19B 0.0601(16) 0.0381(14) 0.220(4) -0.0135(18) -0.060(2) -0.0032(12) F20B 0.0606(17) 0.0502(16) 0.287(5) 0.000(2) -0.093(2) -0.0102(13) F21B 0.184(4) 0.239(5) 0.099(3) 0.039(3) -0.056(3) 0.118(4) F22B 0.0412(11) 0.0698(15) 0.0515(13) 0.0103(11) -0.0158(10) -0.0293(10) F23B 0.0615(15) 0.0915(19) 0.096(2) -0.0568(16) -0.0152(14) -0.0246(14) F24B 0.112(2) 0.0934(18) 0.0620(15) 0.0358(13) -0.0637(15) -0.0718(16) C1B 0.0239(13) 0.0305(16) 0.0281(15) -0.0012(12) -0.0086(12) -0.0036(12) C2B 0.0293(14) 0.0324(16) 0.0265(15) 0.0003(12) -0.0102(12) -0.0062(12) C3B 0.0279(14) 0.0363(17) 0.0289(15) -0.0071(13) -0.0089(13) -0.0052(13) C4B 0.0281(15) 0.0436(19) 0.0279(15) -0.0071(13) -0.0104(13) -0.0050(13) C5B 0.0299(15) 0.0420(18) 0.0219(14) -0.0007(13) -0.0099(12) -0.0042(13) C6B 0.0285(14) 0.0342(17) 0.0284(15) 0.0007(13) -0.0095(12) -0.0063(12) C7B 0.0400(18) 0.044(2) 0.0400(19) -0.0051(15) -0.0182(16) -0.0131(15) C8B 0.0462(19) 0.047(2) 0.0292(17) -0.0033(15) -0.0178(15) -0.0036(16) C9B 0.0247(13) 0.0243(14) 0.0251(14) 0.0001(11) -0.0072(12) -0.0056(11) C10B 0.0242(14) 0.0339(17) 0.0283(15) -0.0042(12) -0.0084(12) -0.0021(12) C11B 0.0321(15) 0.0299(16) 0.0262(15) -0.0019(12) -0.0113(13) 0.0005(12) C12B 0.0336(16) 0.0402(18) 0.0233(15) 0.0003(13) -0.0041(13) -0.0028(14) C13B 0.0258(14) 0.0424(18) 0.0288(16) 0.0047(13) -0.0066(13) -0.0060(13) C14B 0.0258(14) 0.0369(17) 0.0258(15) 0.0020(12) -0.0106(12) -0.0065(12) C15B 0.0422(19) 0.065(3) 0.0248(17) -0.0048(16) -0.0115(15) 0.0070(17) C16B 0.0328(17) 0.066(3) 0.0305(18) 0.0031(17) -0.0036(15) -0.0060(17) C17B 0.0265(14) 0.0375(17) 0.0203(14) -0.0036(12) -0.0084(12) -0.0089(12) C18B 0.0221(13) 0.0343(16) 0.0239(14) -0.0032(12) -0.0074(11) -0.0072(12) C19B 0.0272(14) 0.0343(16) 0.0252(14) -0.0051(12) -0.0114(12) -0.0053(12) C20B 0.0237(14) 0.0418(18) 0.0334(16) -0.0107(14) -0.0111(13) -0.0046(13) C21B 0.0262(14) 0.0400(18) 0.0319(16) -0.0085(14) -0.0064(13) -0.0085(13) C22B 0.0275(14) 0.0355(17) 0.0247(15) -0.0030(12) -0.0069(12) -0.0064(12) C23B 0.0306(15) 0.0401(18) 0.0290(16) -0.0030(13) -0.0114(13) -0.0070(13) C24B 0.0271(16) 0.044(2) 0.055(2) -0.0054(17) -0.0017(16) -0.0121(15) C25B 0.0276(14) 0.0338(16) 0.0182(13) -0.0013(11) -0.0040(11) -0.0100(12) C26B 0.0336(16) 0.0322(17) 0.0386(17) 0.0012(13) -0.0144(14) -0.0133(13) C27B 0.0358(17) 0.0363(18) 0.0450(19) 0.0048(15) -0.0109(15) -0.0111(14) C28B 0.0395(17) 0.0341(18) 0.0400(18) -0.0013(14) -0.0068(15) -0.0158(14) C29B 0.0332(15) 0.0398(18) 0.0223(15) -0.0007(13) -0.0005(13) -0.0164(14) C30B 0.0275(14) 0.0394(17) 0.0218(14) 0.0017(12) -0.0072(12) -0.0116(13) C31B 0.064(3) 0.038(2) 0.099(4) 0.003(2) -0.040(3) -0.0083(19) C32B 0.0480(19) 0.047(2) 0.0341(18) -0.0032(15) -0.0110(16) -0.0236(17) B1B 0.0238(15) 0.0318(18) 0.0245(16) 0.0018(13) -0.0075(13) -0.0076(13) F1D 0.0749(16) 0.0979(19) 0.0530(14) 0.0197(13) -0.0309(12) -0.0503(15) F2D 0.0969(19) 0.0884(18) 0.0495(14) -0.0147(13) -0.0292(13) -0.0417(15) F3D 0.0934(19) 0.0665(16) 0.117(2) 0.0114(15) -0.0850(18) -0.0253(14) F4D 0.0491(13) 0.0675(16) 0.0901(18) -0.0011(13) -0.0391(13) -0.0002(11) F5D 0.0571(14) 0.0763(17) 0.0573(15) 0.0244(13) -0.0130(12) 0.0103(12) F6D 0.0645(14) 0.0649(15) 0.0453(13) -0.0159(11) -0.0147(11) 0.0191(12) F7D 0.183(3) 0.091(2) 0.0660(17) 0.0264(15) -0.061(2) -0.090(2) F8D 0.093(2) 0.095(2) 0.141(3) 0.076(2) -0.053(2) -0.0341(18) F9D 0.124(2) 0.0716(18) 0.084(2) -0.0231(15) 0.0465(18) -0.0538(18) F10D 0.0415(11) 0.0855(17) 0.0677(15) -0.0428(13) -0.0114(11) -0.0129(11) F11D 0.0541(13) 0.0942(18) 0.0440(12) -0.0001(12) -0.0159(10) -0.0420(12) F12D 0.0611(14) 0.0882(18) 0.0725(16) 0.0090(13) -0.0486(13) -0.0191(13) F13D 0.156(4) 0.104(3) 0.074(2) -0.008(2) 0.049(2) -0.010(3) F14D 0.139(3) 0.097(3) 0.158(4) 0.034(3) 0.090(3) -0.017(2) F15D 0.0555(18) 0.117(3) 0.196(4) 0.018(3) 0.018(2) -0.0009(19) F21D 0.103(3) 0.296(6) 0.068(2) -0.011(3) -0.0486(19) -0.079(3) F19D 0.474(9) 0.079(2) 0.119(3) 0.004(2) -0.209(5) 0.024(4) F20D 0.088(2) 0.244(4) 0.0327(14) -0.014(2) -0.0251(14) 0.055(2) F22D 0.053(2) 0.107(5) 0.0266(19) 0.006(2) -0.0031(16) 0.000(3) F23D 0.307(15) 0.147(7) 0.119(6) -0.081(5) 0.046(7) 0.045(7) F24D 0.049(3) 0.61(2) 0.054(3) -0.025(9) -0.020(3) 0.099(8) C1D 0.0278(14) 0.0490(19) 0.0194(14) -0.0026(13) -0.0078(12) -0.0059(13) C2D 0.0379(17) 0.0426(19) 0.0262(15) 0.0046(13) -0.0161(14) -0.0083(14) C3D 0.051(2) 0.047(2) 0.0277(16) 0.0021(14) -0.0199(15) -0.0172(16) C4D 0.053(2) 0.0404(19) 0.0277(16) -0.0035(14) -0.0162(15) -0.0069(16) C5D 0.0420(18) 0.0424(19) 0.0254(16) -0.0042(14) -0.0125(14) 0.0008(15) C6D 0.0320(15) 0.047(2) 0.0256(15) -0.0004(14) -0.0104(13) -0.0083(14) C7D 0.072(3) 0.055(2) 0.044(2) 0.0062(18) -0.037(2) -0.021(2) C8D 0.048(2) 0.048(2) 0.0336(18) 0.0012(16) -0.0163(16) -0.0020(17) C9D 0.0269(14) 0.0358(17) 0.0286(15) -0.0014(13) -0.0103(12) -0.0020(12) C10D 0.0285(15) 0.0382(17) 0.0271(15) -0.0059(13) -0.0094(13) -0.0058(13) C11D 0.0341(16) 0.0345(17) 0.0273(16) -0.0041(13) -0.0063(13) -0.0010(13) C12D 0.0327(16) 0.0441(19) 0.0240(15) -0.0034(13) -0.0090(13) 0.0006(14) C13D 0.0234(14) 0.0428(18) 0.0277(15) -0.0079(13) -0.0079(12) -0.0019(13) C14D 0.0253(14) 0.0396(18) 0.0263(15) -0.0053(13) -0.0083(12) -0.0059(13) C15D 0.053(2) 0.044(2) 0.0286(17) -0.0003(15) -0.0113(16) -0.0118(16) C16D 0.0282(16) 0.062(2) 0.0335(18) -0.0079(16) -0.0109(14) -0.0070(15) C17D 0.0373(17) 0.045(2) 0.0273(16) 0.0009(14) -0.0119(14) -0.0084(14) C18D 0.0407(19) 0.052(2) 0.042(2) 0.0088(17) -0.0022(16) -0.0043(17) C19D 0.048(2) 0.060(3) 0.062(3) 0.018(2) 0.005(2) -0.009(2) C20D 0.062(3) 0.073(3) 0.065(3) 0.015(2) -0.003(2) -0.032(2) C21D 0.091(3) 0.054(3) 0.063(3) -0.006(2) 0.012(3) -0.035(3) C22D 0.073(3) 0.058(3) 0.047(2) -0.007(2) 0.006(2) -0.027(2) C23D 0.072(4) 0.073(4) 0.107(5) 0.022(4) 0.017(3) -0.019(3) C25D 0.0354(16) 0.0373(18) 0.0299(16) 0.0016(13) -0.0152(13) -0.0098(13) C26D 0.0355(16) 0.047(2) 0.0277(16) -0.0016(14) -0.0118(14) -0.0035(14) C27D 0.0375(17) 0.044(2) 0.0340(17) -0.0019(14) -0.0175(15) -0.0004(15) C28D 0.0361(18) 0.065(2) 0.040(2) 0.0012(17) -0.0167(16) 0.0052(17) C29D 0.0403(19) 0.066(3) 0.0349(19) -0.0026(17) -0.0123(16) 0.0078(17) C30D 0.0391(17) 0.048(2) 0.0286(16) -0.0009(14) -0.0125(14) 0.0028(15) C31D 0.051(2) 0.075(3) 0.043(2) -0.003(2) -0.0242(19) 0.014(2) C32D 0.062(3) 0.127(5) 0.040(2) -0.004(3) -0.015(2) 0.041(3) B1D 0.0312(17) 0.040(2) 0.0269(17) -0.0019(15) -0.0103(14) -0.0090(15) C24D 0.089(7) 0.066(6) 0.062(6) -0.010(5) 0.007(6) -0.041(6) F18D 0.226(15) 0.086(7) 0.132(9) -0.039(7) 0.047(8) -0.112(9) F17D 0.158(9) 0.050(4) 0.31(3) -0.015(9) -0.055(13) 0.000(5) F16D 0.60(4) 0.139(11) 0.179(16) -0.015(10) -0.11(2) -0.082(16) C24A 0.050(8) 0.115(15) 0.054(9) -0.007(9) 0.000(7) -0.043(9) F18A 0.20(2) 0.079(8) 0.142(13) 0.062(9) -0.030(14) -0.022(10) F17A 0.116(8) 0.055(5) 0.185(14) 0.026(6) -0.042(8) -0.002(5) F16A 0.83(7) 0.120(14) 0.134(15) -0.118(12) 0.31(3) -0.28(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 Fe1 O1 1.914(2) . ? Fe1 N2 1.995(2) . ? Fe1 N3 2.073(2) . ? Fe1 N1 2.086(2) . ? Fe2 O4 1.898(2) . ? Fe2 N5 1.992(2) 2_656 ? Fe2 N4 2.079(2) 2_656 ? Fe2 N6 2.082(2) 2_656 ? O1 C31 1.293(4) . ? O2 C31 1.233(4) . ? O3 C42 1.232(4) . ? O4 C42 1.305(4) . ? N1 C3 1.496(4) . ? N1 C1 1.497(4) . ? N1 C2 1.507(4) . ? N2 C5 1.480(4) . ? N2 C4 1.488(4) . ? N2 C6 1.493(4) . ? N3 C8 1.496(4) . ? N3 C7 1.499(4) . ? N3 C9 1.506(4) . ? N4 C17 1.489(4) . ? N4 C16 1.499(4) . ? N4 C18 1.508(4) . ? N4 Fe2 2.079(2) 2_656 ? N5 C20 1.473(4) . ? N5 C19 1.486(4) . ? N5 C21 1.494(4) . ? N5 Fe2 1.992(2) 2_656 ? N6 C24 1.491(4) . ? N6 C22 1.493(4) . ? N6 C23 1.495(4) . ? N6 Fe2 2.082(2) 2_656 ? C1 C28 1.519(4) . ? C3 C4 1.521(4) . ? C6 C7 1.517(4) . ? C9 C10 1.509(4) . ? C10 C15 1.370(4) . ? C10 C11 1.393(4) . ? C11 C12 1.381(5) . ? C12 C13 1.381(4) . ? C13 C14 1.387(4) . ? C13 C16 1.492(4) . ? C14 C15 1.383(5) . ? C18 C19 1.519(5) . ? C21 C22 1.527(4) . ? C24 C25 1.508(4) . ? C25 C26 1.385(4) . ? C25 C30 1.396(4) . ? C26 C27 1.380(4) . ? C27 C28 1.379(4) . ? C28 C29 1.389(4) . ? C29 C30 1.392(4) . ? C31 C32 1.505(4) . ? C32 C33 1.361(4) . ? C32 C41 1.413(4) . ? C33 C34 1.408(4) . ? C34 C39 1.410(4) . ? C34 C35 1.418(4) . ? C35 C36 1.366(4) . ? C36 C37 1.417(4) . ? C37 C38 1.361(4) . ? C37 C42 1.503(4) . ? C38 C39 1.412(4) . ? C39 C40 1.431(5) . ? C40 C41 1.360(5) . ? F1B C7B 1.309(4) . ? F2B C7B 1.325(4) . ? F3B C7B 1.306(4) . ? F4B C8B 1.347(4) . ? F5B C8B 1.314(4) . ? F6B C8B 1.329(4) . ? F7B C15B 1.327(4) . ? F8B C15B 1.353(4) . ? F9B C15B 1.353(4) . ? F10B C16B 1.319(4) . ? F11B C16B 1.340(4) . ? F12B C16B 1.347(4) . ? F13B C23B 1.333(3) . ? F14B C23B 1.364(3) . ? F15B C23B 1.338(4) . ? F16B C24B 1.343(4) . ? F17B C24B 1.311(4) . ? F18B C24B 1.311(4) . ? F19B C31B 1.335(5) . ? F20B C31B 1.278(5) . ? F21B C31B 1.312(6) . ? F22B C32B 1.317(4) . ? F23B C32B 1.349(4) . ? F24B C32B 1.343(4) . ? C1B C2B 1.397(4) . ? C1B C6B 1.414(4) . ? C1B B1B 1.645(4) . ? C2B C3B 1.397(4) . ? C3B C4B 1.403(4) . ? C3B C7B 1.495(4) . ? C4B C5B 1.369(4) . ? C5B C6B 1.402(4) . ? C5B C8B 1.500(4) . ? C9B C14B 1.391(4) . ? C9B C10B 1.397(4) . ? C9B B1B 1.646(4) . ? C10B C11B 1.393(4) . ? C11B C12B 1.378(4) . ? C11B C15B 1.490(4) . ? C12B C13B 1.400(4) . ? C13B C14B 1.383(4) . ? C13B C16B 1.497(4) . ? C17B C22B 1.400(4) . ? C17B C18B 1.404(4) . ? C17B B1B 1.645(4) . ? C18B C19B 1.404(4) . ? C19B C20B 1.386(4) . ? C19B C23B 1.485(4) . ? C20B C21B 1.389(5) . ? C21B C22B 1.392(4) . ? C21B C24B 1.491(4) . ? C25B C26B 1.400(4) . ? C25B C30B 1.406(4) . ? C25B B1B 1.628(4) . ? C26B C27B 1.393(4) . ? C27B C28B 1.393(4) . ? C27B C31B 1.486(5) . ? C28B C29B 1.382(5) . ? C29B C30B 1.381(4) . ? C29B C32B 1.494(4) . ? F1D C7D 1.331(4) . ? F2D C7D 1.354(4) . ? F3D C7D 1.326(4) . ? F4D C8D 1.336(4) . ? F5D C8D 1.331(4) . ? F6D C8D 1.334(4) . ? F7D C15D 1.300(4) . ? F8D C15D 1.316(4) . ? F9D C15D 1.330(4) . ? F10D C16D 1.342(4) . ? F11D C16D 1.327(4) . ? F12D C16D 1.340(4) . ? F13D C23D 1.323(7) . ? F14D C23D 1.305(6) . ? F15D C23D 1.352(7) . ? F21D C31D 1.346(6) . ? F19D C31D 1.263(5) . ? F20D C31D 1.273(5) . ? F22F C32D 1.199(12) . ? F23F C32D 1.272(9) . ? F24F C32D 1.485(10) . ? F22D C32D 1.326(6) . ? F23D C32D 1.514(12) . ? F24D C32D 1.213(6) . ? C1D C2D 1.390(4) . ? C1D C6D 1.410(4) . ? C1D B1D 1.643(5) . ? C2D C3D 1.398(5) . ? C3D C4D 1.380(5) . ? C3D C7D 1.484(5) . ? C4D C5D 1.392(5) . ? C5D C6D 1.385(5) . ? C5D C8D 1.492(5) . ? C9D C14D 1.399(4) . ? C9D C10D 1.417(4) . ? C9D B1D 1.641(4) . ? C10D C11D 1.387(4) . ? C11D C12D 1.400(4) . ? C11D C15D 1.477(5) . ? C12D C13D 1.386(5) . ? C13D C14D 1.398(4) . ? C13D C16D 1.478(4) . ? C17D C22D 1.379(5) . ? C17D C18D 1.399(5) . ? C17D B1D 1.645(5) . ? C18D C19D 1.388(5) . ? C19D C20D 1.382(6) . ? C19D C23D 1.536(7) . ? C20D C21D 1.362(6) . ? C21D C22D 1.385(6) . ? C21D C24D 1.461(10) . ? C21D C24A 1.77(3) . ? C25D C30D 1.375(4) . ? C25D C26D 1.419(4) . ? C25D B1D 1.640(5) . ? C26D C27D 1.379(4) . ? C27D C28D 1.379(5) . ? C27D C31D 1.490(5) . ? C28D C29D 1.391(5) . ? C29D C30D 1.391(4) . ? C29D C32D 1.488(6) . ? C24D F16D 1.18(2) . ? C24D F18D 1.244(15) . ? C24D F17D 1.360(16) . ? C24A F18A 1.12(3) . ? C24A F17A 1.16(3) . ? C24A F16A 1.73(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 N2 164.07(9) . . ? O1 Fe1 N3 97.38(9) . . ? N2 Fe1 N3 85.17(10) . . ? O1 Fe1 N1 95.89(9) . . ? N2 Fe1 N1 85.42(10) . . ? N3 Fe1 N1 161.97(10) . . ? O4 Fe2 N5 172.45(9) . 2_656 ? O4 Fe2 N4 95.34(9) . 2_656 ? N5 Fe2 N4 85.33(10) 2_656 2_656 ? O4 Fe2 N6 95.77(9) . 2_656 ? N5 Fe2 N6 84.99(9) 2_656 2_656 ? N4 Fe2 N6 164.92(10) 2_656 2_656 ? C31 O1 Fe1 112.21(18) . . ? C42 O4 Fe2 120.49(19) . . ? C3 N1 C1 111.6(2) . . ? C3 N1 C2 108.2(2) . . ? C1 N1 C2 107.1(2) . . ? C3 N1 Fe1 106.83(18) . . ? C1 N1 Fe1 115.70(18) . . ? C2 N1 Fe1 107.07(18) . . ? C5 N2 C4 110.5(2) . . ? C5 N2 C6 109.9(2) . . ? C4 N2 C6 112.2(2) . . ? C5 N2 Fe1 108.18(18) . . ? C4 N2 Fe1 107.62(19) . . ? C6 N2 Fe1 108.36(18) . . ? C8 N3 C7 108.4(2) . . ? C8 N3 C9 107.3(2) . . ? C7 N3 C9 111.1(2) . . ? C8 N3 Fe1 105.41(18) . . ? C7 N3 Fe1 107.68(17) . . ? C9 N3 Fe1 116.66(18) . . ? C17 N4 C16 107.5(2) . . ? C17 N4 C18 108.1(2) . . ? C16 N4 C18 111.2(2) . . ? C17 N4 Fe2 104.60(18) . 2_656 ? C16 N4 Fe2 117.28(18) . 2_656 ? C18 N4 Fe2 107.60(18) . 2_656 ? C20 N5 C19 110.9(2) . . ? C20 N5 C21 110.0(2) . . ? C19 N5 C21 111.4(2) . . ? C20 N5 Fe2 110.27(18) . 2_656 ? C19 N5 Fe2 106.78(18) . 2_656 ? C21 N5 Fe2 107.36(17) . 2_656 ? C24 N6 C22 111.8(2) . . ? C24 N6 C23 106.5(2) . . ? C22 N6 C23 107.3(2) . . ? C24 N6 Fe2 117.37(18) . 2_656 ? C22 N6 Fe2 107.63(17) . 2_656 ? C23 N6 Fe2 105.60(18) . 2_656 ? N1 C1 C28 115.4(2) . . ? N1 C3 C4 109.8(2) . . ? N2 C4 C3 107.6(2) . . ? N2 C6 C7 108.0(2) . . ? N3 C7 C6 109.0(2) . . ? N3 C9 C10 115.5(2) . . ? C15 C10 C11 117.2(3) . . ? C15 C10 C9 120.1(3) . . ? C11 C10 C9 122.5(3) . . ? C12 C11 C10 121.2(3) . . ? C11 C12 C13 121.6(3) . . ? C12 C13 C14 116.9(3) . . ? C12 C13 C16 122.4(3) . . ? C14 C13 C16 120.6(3) . . ? C15 C14 C13 121.5(3) . . ? C10 C15 C14 121.6(3) . . ? C13 C16 N4 115.5(3) . . ? N4 C18 C19 108.6(2) . . ? N5 C19 C18 108.3(2) . . ? N5 C21 C22 107.1(2) . . ? N6 C22 C21 108.7(2) . . ? N6 C24 C25 115.8(2) . . ? C26 C25 C30 118.0(3) . . ? C26 C25 C24 120.3(3) . . ? C30 C25 C24 121.5(3) . . ? C27 C26 C25 121.1(3) . . ? C28 C27 C26 121.2(3) . . ? C27 C28 C29 118.3(3) . . ? C27 C28 C1 119.4(3) . . ? C29 C28 C1 122.1(3) . . ? C28 C29 C30 120.7(3) . . ? C29 C30 C25 120.6(3) . . ? O2 C31 O1 123.2(3) . . ? O2 C31 C32 120.9(3) . . ? O1 C31 C32 115.9(3) . . ? C33 C32 C41 119.9(3) . . ? C33 C32 C31 119.1(3) . . ? C41 C32 C31 121.0(3) . . ? C32 C33 C34 121.1(3) . . ? C33 C34 C39 119.6(3) . . ? C33 C34 C35 121.8(3) . . ? C39 C34 C35 118.5(3) . . ? C36 C35 C34 121.1(3) . . ? C35 C36 C37 120.0(3) . . ? C38 C37 C36 119.9(3) . . ? C38 C37 C42 121.3(3) . . ? C36 C37 C42 118.8(3) . . ? C37 C38 C39 121.0(3) . . ? C34 C39 C38 119.4(3) . . ? C34 C39 C40 118.0(3) . . ? C38 C39 C40 122.6(3) . . ? C41 C40 C39 120.9(3) . . ? C40 C41 C32 120.4(3) . . ? O3 C42 O4 124.3(3) . . ? O3 C42 C37 120.8(3) . . ? O4 C42 C37 114.9(3) . . ? C2B C1B C6B 115.3(3) . . ? C2B C1B B1B 121.7(3) . . ? C6B C1B B1B 122.9(3) . . ? C3B C2B C1B 122.6(3) . . ? C2B C3B C4B 120.4(3) . . ? C2B C3B C7B 119.0(3) . . ? C4B C3B C7B 120.6(3) . . ? C5B C4B C3B 118.5(3) . . ? C4B C5B C6B 120.8(3) . . ? C4B C5B C8B 119.8(3) . . ? C6B C5B C8B 119.4(3) . . ? C5B C6B C1B 122.3(3) . . ? F3B C7B F1B 106.9(3) . . ? F3B C7B F2B 105.5(3) . . ? F1B C7B F2B 105.6(3) . . ? F3B C7B C3B 112.3(3) . . ? F1B C7B C3B 113.0(3) . . ? F2B C7B C3B 113.0(3) . . ? F5B C8B F6B 106.7(3) . . ? F5B C8B F4B 105.5(3) . . ? F6B C8B F4B 106.6(3) . . ? F5B C8B C5B 113.9(3) . . ? F6B C8B C5B 112.5(3) . . ? F4B C8B C5B 111.1(3) . . ? C14B C9B C10B 115.6(3) . . ? C14B C9B B1B 121.0(2) . . ? C10B C9B B1B 122.4(2) . . ? C11B C10B C9B 122.5(3) . . ? C12B C11B C10B 121.0(3) . . ? C12B C11B C15B 118.7(3) . . ? C10B C11B C15B 120.2(3) . . ? C11B C12B C13B 117.2(3) . . ? C14B C13B C12B 121.3(3) . . ? C14B C13B C16B 119.5(3) . . ? C12B C13B C16B 119.2(3) . . ? C13B C14B C9B 122.4(3) . . ? F7B C15B F8B 106.8(3) . . ? F7B C15B F9B 107.2(3) . . ? F8B C15B F9B 103.8(3) . . ? F7B C15B C11B 113.6(3) . . ? F8B C15B C11B 113.0(3) . . ? F9B C15B C11B 111.7(3) . . ? F10B C16B F11B 106.0(3) . . ? F10B C16B F12B 105.0(3) . . ? F11B C16B F12B 107.4(3) . . ? F10B C16B C13B 114.2(3) . . ? F11B C16B C13B 111.5(3) . . ? F12B C16B C13B 112.3(3) . . ? C22B C17B C18B 115.9(3) . . ? C22B C17B B1B 123.4(3) . . ? C18B C17B B1B 120.7(2) . . ? C19B C18B C17B 122.1(3) . . ? C20B C19B C18B 120.2(3) . . ? C20B C19B C23B 119.2(3) . . ? C18B C19B C23B 120.6(3) . . ? C19B C20B C21B 118.9(3) . . ? C20B C21B C22B 120.4(3) . . ? C20B C21B C24B 119.4(3) . . ? C22B C21B C24B 120.2(3) . . ? C21B C22B C17B 122.5(3) . . ? F13B C23B F15B 106.5(2) . . ? F13B C23B F14B 104.4(2) . . ? F15B C23B F14B 105.6(3) . . ? F13B C23B C19B 113.9(2) . . ? F15B C23B C19B 113.7(3) . . ? F14B C23B C19B 112.0(2) . . ? F18B C24B F17B 107.4(3) . . ? F18B C24B F16B 105.3(3) . . ? F17B C24B F16B 104.1(3) . . ? F18B C24B C21B 114.1(3) . . ? F17B C24B C21B 113.4(3) . . ? F16B C24B C21B 111.9(3) . . ? C26B C25B C30B 114.8(3) . . ? C26B C25B B1B 122.6(2) . . ? C30B C25B B1B 121.3(3) . . ? C27B C26B C25B 122.4(3) . . ? C26B C27B C28B 121.2(3) . . ? C26B C27B C31B 119.2(3) . . ? C28B C27B C31B 119.6(3) . . ? C29B C28B C27B 117.4(3) . . ? C30B C29B C28B 121.2(3) . . ? C30B C29B C32B 119.2(3) . . ? C28B C29B C32B 119.6(3) . . ? C29B C30B C25B 123.1(3) . . ? F20B C31B F21B 105.3(5) . . ? F20B C31B F19B 105.3(4) . . ? F21B C31B F19B 104.8(4) . . ? F20B C31B C27B 115.0(4) . . ? F21B C31B C27B 111.6(4) . . ? F19B C31B C27B 114.0(3) . . ? F22B C32B F24B 105.8(3) . . ? F22B C32B F23B 104.9(3) . . ? F24B C32B F23B 106.6(3) . . ? F22B C32B C29B 114.3(3) . . ? F24B C32B C29B 111.8(3) . . ? F23B C32B C29B 112.8(3) . . ? C25B B1B C17B 114.0(2) . . ? C25B B1B C1B 113.3(2) . . ? C17B B1B C1B 107.6(2) . . ? C25B B1B C9B 100.4(2) . . ? C17B B1B C9B 110.7(2) . . ? C1B B1B C9B 110.7(2) . . ? C2D C1D C6D 115.5(3) . . ? C2D C1D B1D 124.6(3) . . ? C6D C1D B1D 119.4(3) . . ? C1D C2D C3D 122.4(3) . . ? C4D C3D C2D 120.8(3) . . ? C4D C3D C7D 119.2(3) . . ? C2D C3D C7D 120.0(3) . . ? C3D C4D C5D 118.2(3) . . ? C6D C5D C4D 120.5(3) . . ? C6D C5D C8D 120.8(3) . . ? C4D C5D C8D 118.5(3) . . ? C5D C6D C1D 122.5(3) . . ? F3D C7D F1D 106.5(3) . . ? F3D C7D F2D 105.0(3) . . ? F1D C7D F2D 104.8(3) . . ? F3D C7D C3D 113.9(3) . . ? F1D C7D C3D 112.9(3) . . ? F2D C7D C3D 112.9(3) . . ? F5D C8D F6D 105.9(3) . . ? F5D C8D F4D 104.8(3) . . ? F6D C8D F4D 105.7(3) . . ? F5D C8D C5D 111.8(3) . . ? F6D C8D C5D 113.8(3) . . ? F4D C8D C5D 114.1(3) . . ? C14D C9D C10D 115.3(3) . . ? C14D C9D B1D 125.6(3) . . ? C10D C9D B1D 118.9(3) . . ? C11D C10D C9D 123.1(3) . . ? C10D C11D C12D 119.6(3) . . ? C10D C11D C15D 120.8(3) . . ? C12D C11D C15D 119.6(3) . . ? C13D C12D C11D 118.9(3) . . ? C12D C13D C14D 120.6(3) . . ? C12D C13D C16D 118.6(3) . . ? C14D C13D C16D 120.7(3) . . ? C13D C14D C9D 122.3(3) . . ? F7D C15D F8D 104.0(3) . . ? F7D C15D F9D 105.2(3) . . ? F8D C15D F9D 104.5(3) . . ? F7D C15D C11D 114.8(3) . . ? F8D C15D C11D 114.2(3) . . ? F9D C15D C11D 113.1(3) . . ? F11D C16D F12D 105.6(3) . . ? F11D C16D F10D 107.3(3) . . ? F12D C16D F10D 105.0(3) . . ? F11D C16D C13D 113.8(3) . . ? F12D C16D C13D 112.8(3) . . ? F10D C16D C13D 111.8(3) . . ? C22D C17D C18D 114.7(3) . . ? C22D C17D B1D 120.7(3) . . ? C18D C17D B1D 124.6(3) . . ? C19D C18D C17D 122.1(4) . . ? C20D C19D C18D 120.7(4) . . ? C20D C19D C23D 120.9(4) . . ? C18D C19D C23D 118.4(4) . . ? C21D C20D C19D 118.4(4) . . ? C20D C21D C22D 120.1(4) . . ? C20D C21D C24D 117.0(5) . . ? C22D C21D C24D 121.7(5) . . ? C20D C21D C24A 117.4(6) . . ? C22D C21D C24A 117.1(6) . . ? C24D C21D C24A 34.6(6) . . ? C17D C22D C21D 123.9(4) . . ? F14D C23D F13D 108.4(6) . . ? F14D C23D F15D 107.5(5) . . ? F13D C23D F15D 106.6(5) . . ? F14D C23D C19D 112.3(5) . . ? F13D C23D C19D 113.0(5) . . ? F15D C23D C19D 108.8(5) . . ? C30D C25D C26D 115.7(3) . . ? C30D C25D B1D 125.7(3) . . ? C26D C25D B1D 118.6(3) . . ? C27D C26D C25D 122.0(3) . . ? C28D C27D C26D 120.7(3) . . ? C28D C27D C31D 120.0(3) . . ? C26D C27D C31D 119.3(3) . . ? C27D C28D C29D 118.5(3) . . ? C30D C29D C28D 120.1(3) . . ? C30D C29D C32D 121.2(3) . . ? C28D C29D C32D 118.7(3) . . ? C25D C30D C29D 122.9(3) . . ? F19D C31D F20D 110.0(5) . . ? F19D C31D F21D 103.4(4) . . ? F20D C31D F21D 100.7(4) . . ? F19D C31D C27D 113.6(4) . . ? F20D C31D C27D 116.4(3) . . ? F21D C31D C27D 111.2(4) . . ? F22F C32D F24D 125.1(7) . . ? F22F C32D F23F 107.5(8) . . ? F24D C32D F23F 51.3(8) . . ? F22F C32D F22D 29.6(5) . . ? F24D C32D F22D 115.4(7) . . ? F23F C32D F22D 126.1(6) . . ? F22F C32D F24F 112.3(7) . . ? F24D C32D F24F 42.2(9) . . ? F23F C32D F24F 93.1(5) . . ? F22D C32D F24F 87.0(6) . . ? F22F C32D C29D 116.9(7) . . ? F24D C32D C29D 117.7(5) . . ? F23F C32D C29D 115.7(5) . . ? F22D C32D C29D 115.0(4) . . ? F24F C32D C29D 109.0(5) . . ? F22F C32D F23D 70.2(7) . . ? F24D C32D F23D 100.9(7) . . ? F23F C32D F23D 50.7(5) . . ? F22D C32D F23D 99.3(6) . . ? F24F C32D F23D 139.0(6) . . ? C29D C32D F23D 104.8(5) . . ? C25D B1D C9D 111.1(2) . . ? C25D B1D C1D 111.2(2) . . ? C9D B1D C1D 104.0(3) . . ? C25D B1D C17D 106.1(3) . . ? C9D B1D C17D 112.0(2) . . ? C1D B1D C17D 112.4(3) . . ? F16D C24D F18D 96.9(16) . . ? F16D C24D F17D 95.1(16) . . ? F18D C24D F17D 115.5(14) . . ? F16D C24D C21D 120.3(13) . . ? F18D C24D C21D 118.9(9) . . ? F17D C24D C21D 107.8(10) . . ? F18A C24A F17A 106(2) . . ? F18A C24A F16A 88(2) . . ? F17A C24A F16A 142(3) . . ? F18A C24A C21D 104.3(18) . . ? F17A C24A C21D 124.1(13) . . ? F16A C24A C21D 83.2(17) . . ? 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 N2 Fe1 O1 C31 -174.9(3) . . . . ? N3 Fe1 O1 C31 86.8(2) . . . . ? N1 Fe1 O1 C31 -80.9(2) . . . . ? N5 Fe2 O4 C42 -175.6(6) 2_656 . . . ? N4 Fe2 O4 C42 89.7(2) 2_656 . . . ? N6 Fe2 O4 C42 -80.1(2) 2_656 . . . ? O1 Fe1 N1 C3 -159.27(19) . . . . ? N2 Fe1 N1 C3 4.79(19) . . . . ? N3 Fe1 N1 C3 63.5(4) . . . . ? O1 Fe1 N1 C1 -34.3(2) . . . . ? N2 Fe1 N1 C1 129.8(2) . . . . ? N3 Fe1 N1 C1 -171.5(3) . . . . ? O1 Fe1 N1 C2 85.0(2) . . . . ? N2 Fe1 N1 C2 -111.0(2) . . . . ? N3 Fe1 N1 C2 -52.2(4) . . . . ? O1 Fe1 N2 C5 -1.1(4) . . . . ? N3 Fe1 N2 C5 98.90(19) . . . . ? N1 Fe1 N2 C5 -96.50(19) . . . . ? O1 Fe1 N2 C4 118.3(3) . . . . ? N3 Fe1 N2 C4 -141.74(19) . . . . ? N1 Fe1 N2 C4 22.86(18) . . . . ? O1 Fe1 N2 C6 -120.2(3) . . . . ? N3 Fe1 N2 C6 -20.25(19) . . . . ? N1 Fe1 N2 C6 144.3(2) . . . . ? O1 Fe1 N3 C8 -87.53(19) . . . . ? N2 Fe1 N3 C8 108.29(19) . . . . ? N1 Fe1 N3 C8 49.5(4) . . . . ? O1 Fe1 N3 C7 156.96(18) . . . . ? N2 Fe1 N3 C7 -7.22(19) . . . . ? N1 Fe1 N3 C7 -66.0(4) . . . . ? O1 Fe1 N3 C9 31.4(2) . . . . ? N2 Fe1 N3 C9 -132.8(2) . . . . ? N1 Fe1 N3 C9 168.4(3) . . . . ? C3 N1 C1 C28 60.0(3) . . . . ? C2 N1 C1 C28 178.3(3) . . . . ? Fe1 N1 C1 C28 -62.4(3) . . . . ? C1 N1 C3 C4 -158.7(3) . . . . ? C2 N1 C3 C4 83.7(3) . . . . ? Fe1 N1 C3 C4 -31.3(3) . . . . ? C5 N2 C4 C3 72.0(3) . . . . ? C6 N2 C4 C3 -165.0(3) . . . . ? Fe1 N2 C4 C3 -45.9(3) . . . . ? N1 C3 C4 N2 51.8(3) . . . . ? C5 N2 C6 C7 -74.2(3) . . . . ? C4 N2 C6 C7 162.5(3) . . . . ? Fe1 N2 C6 C7 43.8(3) . . . . ? C8 N3 C7 C6 -80.6(3) . . . . ? C9 N3 C7 C6 161.9(2) . . . . ? Fe1 N3 C7 C6 33.0(3) . . . . ? N2 C6 C7 N3 -51.1(3) . . . . ? C8 N3 C9 C10 -175.6(2) . . . . ? C7 N3 C9 C10 -57.4(3) . . . . ? Fe1 N3 C9 C10 66.5(3) . . . . ? N3 C9 C10 C15 116.0(3) . . . . ? N3 C9 C10 C11 -69.1(4) . . . . ? C15 C10 C11 C12 -0.2(5) . . . . ? C9 C10 C11 C12 -175.2(3) . . . . ? C10 C11 C12 C13 -0.3(6) . . . . ? C11 C12 C13 C14 0.5(5) . . . . ? C11 C12 C13 C16 176.1(3) . . . . ? C12 C13 C14 C15 -0.3(5) . . . . ? C16 C13 C14 C15 -176.0(3) . . . . ? C11 C10 C15 C14 0.3(5) . . . . ? C9 C10 C15 C14 175.5(3) . . . . ? C13 C14 C15 C10 -0.1(6) . . . . ? C12 C13 C16 N4 70.7(4) . . . . ? C14 C13 C16 N4 -113.9(3) . . . . ? C17 N4 C16 C13 176.8(2) . . . . ? C18 N4 C16 C13 58.7(3) . . . . ? Fe2 N4 C16 C13 -65.8(3) 2_656 . . . ? C17 N4 C18 C19 83.2(3) . . . . ? C16 N4 C18 C19 -159.0(2) . . . . ? Fe2 N4 C18 C19 -29.2(3) 2_656 . . . ? C20 N5 C19 C18 72.0(3) . . . . ? C21 N5 C19 C18 -165.0(2) . . . . ? Fe2 N5 C19 C18 -48.1(3) 2_656 . . . ? N4 C18 C19 N5 51.7(3) . . . . ? C20 N5 C21 C22 -72.3(3) . . . . ? C19 N5 C21 C22 164.2(2) . . . . ? Fe2 N5 C21 C22 47.7(3) 2_656 . . . ? C24 N6 C22 C21 162.1(2) . . . . ? C23 N6 C22 C21 -81.4(3) . . . . ? Fe2 N6 C22 C21 31.8(3) 2_656 . . . ? N5 C21 C22 N6 -53.0(3) . . . . ? C22 N6 C24 C25 -58.3(3) . . . . ? C23 N6 C24 C25 -175.2(2) . . . . ? Fe2 N6 C24 C25 66.8(3) 2_656 . . . ? N6 C24 C25 C26 95.7(3) . . . . ? N6 C24 C25 C30 -89.1(3) . . . . ? C30 C25 C26 C27 -1.0(5) . . . . ? C24 C25 C26 C27 174.4(3) . . . . ? C25 C26 C27 C28 1.7(5) . . . . ? C26 C27 C28 C29 -1.4(5) . . . . ? C26 C27 C28 C1 -176.7(3) . . . . ? N1 C1 C28 C27 -94.6(3) . . . . ? N1 C1 C28 C29 90.2(3) . . . . ? C27 C28 C29 C30 0.5(4) . . . . ? C1 C28 C29 C30 175.6(3) . . . . ? C28 C29 C30 C25 0.2(4) . . . . ? C26 C25 C30 C29 0.0(4) . . . . ? C24 C25 C30 C29 -175.3(2) . . . . ? Fe1 O1 C31 O2 -7.0(4) . . . . ? Fe1 O1 C31 C32 171.43(19) . . . . ? O2 C31 C32 C33 -0.3(4) . . . . ? O1 C31 C32 C33 -178.7(3) . . . . ? O2 C31 C32 C41 179.2(3) . . . . ? O1 C31 C32 C41 0.8(4) . . . . ? C41 C32 C33 C34 -0.7(5) . . . . ? C31 C32 C33 C34 178.8(3) . . . . ? C32 C33 C34 C39 0.3(4) . . . . ? C32 C33 C34 C35 179.2(3) . . . . ? C33 C34 C35 C36 -179.0(3) . . . . ? C39 C34 C35 C36 -0.2(5) . . . . ? C34 C35 C36 C37 -0.1(5) . . . . ? C35 C36 C37 C38 -0.5(5) . . . . ? C35 C36 C37 C42 178.9(3) . . . . ? C36 C37 C38 C39 1.4(5) . . . . ? C42 C37 C38 C39 -178.0(3) . . . . ? C33 C34 C39 C38 179.9(3) . . . . ? C35 C34 C39 C38 1.1(4) . . . . ? C33 C34 C39 C40 0.0(4) . . . . ? C35 C34 C39 C40 -178.9(3) . . . . ? C37 C38 C39 C34 -1.7(5) . . . . ? C37 C38 C39 C40 178.3(3) . . . . ? C34 C39 C40 C41 0.1(5) . . . . ? C38 C39 C40 C41 -179.8(3) . . . . ? C39 C40 C41 C32 -0.5(6) . . . . ? C33 C32 C41 C40 0.8(5) . . . . ? C31 C32 C41 C40 -178.7(3) . . . . ? Fe2 O4 C42 O3 -5.0(4) . . . . ? Fe2 O4 C42 C37 173.63(18) . . . . ? C38 C37 C42 O3 177.6(3) . . . . ? C36 C37 C42 O3 -1.8(4) . . . . ? C38 C37 C42 O4 -1.1(4) . . . . ? C36 C37 C42 O4 179.5(3) . . . . ? C6B C1B C2B C3B 1.7(4) . . . . ? B1B C1B C2B C3B -178.2(3) . . . . ? C1B C2B C3B C4B 0.8(5) . . . . ? C1B C2B C3B C7B 179.4(3) . . . . ? C2B C3B C4B C5B -2.5(4) . . . . ? C7B C3B C4B C5B 178.9(3) . . . . ? C3B C4B C5B C6B 1.6(4) . . . . ? C3B C4B C5B C8B -177.2(3) . . . . ? C4B C5B C6B C1B 1.0(5) . . . . ? C8B C5B C6B C1B 179.9(3) . . . . ? C2B C1B C6B C5B -2.6(4) . . . . ? B1B C1B C6B C5B 177.3(3) . . . . ? C2B C3B C7B F3B 64.0(4) . . . . ? C4B C3B C7B F3B -117.5(3) . . . . ? C2B C3B C7B F1B -57.1(4) . . . . ? C4B C3B C7B F1B 121.5(3) . . . . ? C2B C3B C7B F2B -176.8(3) . . . . ? C4B C3B C7B F2B 1.7(5) . . . . ? C4B C5B C8B F5B -150.2(3) . . . . ? C6B C5B C8B F5B 31.0(4) . . . . ? C4B C5B C8B F6B -28.6(4) . . . . ? C6B C5B C8B F6B 152.6(3) . . . . ? C4B C5B C8B F4B 90.9(4) . . . . ? C6B C5B C8B F4B -88.0(4) . . . . ? C14B C9B C10B C11B 0.3(4) . . . . ? B1B C9B C10B C11B -168.1(3) . . . . ? C9B C10B C11B C12B -0.4(5) . . . . ? C9B C10B C11B C15B 179.7(3) . . . . ? C10B C11B C12B C13B -0.3(5) . . . . ? C15B C11B C12B C13B 179.7(3) . . . . ? C11B C12B C13B C14B 1.0(5) . . . . ? C11B C12B C13B C16B 178.1(3) . . . . ? C12B C13B C14B C9B -1.1(5) . . . . ? C16B C13B C14B C9B -178.2(3) . . . . ? C10B C9B C14B C13B 0.4(4) . . . . ? B1B C9B C14B C13B 169.0(3) . . . . ? C12B C11B C15B F7B 30.5(5) . . . . ? C10B C11B C15B F7B -149.5(3) . . . . ? C12B C11B C15B F8B 152.4(3) . . . . ? C10B C11B C15B F8B -27.6(5) . . . . ? C12B C11B C15B F9B -90.9(4) . . . . ? C10B C11B C15B F9B 89.0(4) . . . . ? C14B C13B C16B F10B -32.4(5) . . . . ? C12B C13B C16B F10B 150.5(3) . . . . ? C14B C13B C16B F11B 87.7(4) . . . . ? C12B C13B C16B F11B -89.4(4) . . . . ? C14B C13B C16B F12B -151.7(3) . . . . ? C12B C13B C16B F12B 31.1(5) . . . . ? C22B C17B C18B C19B -2.1(4) . . . . ? B1B C17B C18B C19B 178.3(2) . . . . ? C17B C18B C19B C20B -0.5(4) . . . . ? C17B C18B C19B C23B 177.7(3) . . . . ? C18B C19B C20B C21B 2.3(4) . . . . ? C23B C19B C20B C21B -176.0(3) . . . . ? C19B C20B C21B C22B -1.3(4) . . . . ? C19B C20B C21B C24B 176.5(3) . . . . ? C20B C21B C22B C17B -1.5(4) . . . . ? C24B C21B C22B C17B -179.3(3) . . . . ? C18B C17B C22B C21B 3.1(4) . . . . ? B1B C17B C22B C21B -177.3(3) . . . . ? C20B C19B C23B F13B -40.1(4) . . . . ? C18B C19B C23B F13B 141.7(3) . . . . ? C20B C19B C23B F15B -162.4(3) . . . . ? C18B C19B C23B F15B 19.4(4) . . . . ? C20B C19B C23B F14B 78.0(3) . . . . ? C18B C19B C23B F14B -100.2(3) . . . . ? C20B C21B C24B F18B 168.9(3) . . . . ? C22B C21B C24B F18B -13.2(5) . . . . ? C20B C21B C24B F17B 45.7(4) . . . . ? C22B C21B C24B F17B -136.5(3) . . . . ? C20B C21B C24B F16B -71.7(4) . . . . ? C22B C21B C24B F16B 106.2(4) . . . . ? C30B C25B C26B C27B 0.1(4) . . . . ? B1B C25B C26B C27B -166.7(3) . . . . ? C25B C26B C27B C28B 0.3(5) . . . . ? C25B C26B C27B C31B 179.2(3) . . . . ? C26B C27B C28B C29B -0.2(5) . . . . ? C31B C27B C28B C29B -179.2(3) . . . . ? C27B C28B C29B C30B -0.1(5) . . . . ? C27B C28B C29B C32B 179.1(3) . . . . ? C28B C29B C30B C25B 0.5(5) . . . . ? C32B C29B C30B C25B -178.7(3) . . . . ? C26B C25B C30B C29B -0.4(4) . . . . ? B1B C25B C30B C29B 166.5(3) . . . . ? C26B C27B C31B F20B -42.8(6) . . . . ? C28B C27B C31B F20B 136.2(4) . . . . ? C26B C27B C31B F21B 77.0(5) . . . . ? C28B C27B C31B F21B -104.0(5) . . . . ? C26B C27B C31B F19B -164.5(4) . . . . ? C28B C27B C31B F19B 14.5(6) . . . . ? C30B C29B C32B F22B -85.5(4) . . . . ? C28B C29B C32B F22B 95.2(4) . . . . ? C30B C29B C32B F24B 34.6(4) . . . . ? C28B C29B C32B F24B -144.6(3) . . . . ? C30B C29B C32B F23B 154.8(3) . . . . ? C28B C29B C32B F23B -24.4(4) . . . . ? C26B C25B B1B C17B -156.6(3) . . . . ? C30B C25B B1B C17B 37.5(4) . . . . ? C26B C25B B1B C1B -33.1(4) . . . . ? C30B C25B B1B C1B 161.0(3) . . . . ? C26B C25B B1B C9B 85.0(3) . . . . ? C30B C25B B1B C9B -80.9(3) . . . . ? C22B C17B B1B C25B 26.9(4) . . . . ? C18B C17B B1B C25B -153.6(2) . . . . ? C22B C17B B1B C1B -99.6(3) . . . . ? C18B C17B B1B C1B 79.9(3) . . . . ? C22B C17B B1B C9B 139.3(3) . . . . ? C18B C17B B1B C9B -41.2(3) . . . . ? C2B C1B B1B C25B 148.8(3) . . . . ? C6B C1B B1B C25B -31.1(4) . . . . ? C2B C1B B1B C17B -84.2(3) . . . . ? C6B C1B B1B C17B 95.9(3) . . . . ? C2B C1B B1B C9B 36.9(4) . . . . ? C6B C1B B1B C9B -143.0(3) . . . . ? C14B C9B B1B C25B -82.9(3) . . . . ? C10B C9B B1B C25B 84.8(3) . . . . ? C14B C9B B1B C17B 156.2(3) . . . . ? C10B C9B B1B C17B -36.0(4) . . . . ? C14B C9B B1B C1B 37.0(4) . . . . ? C10B C9B B1B C1B -155.2(3) . . . . ? C6D C1D C2D C3D -0.4(4) . . . . ? B1D C1D C2D C3D -172.2(3) . . . . ? C1D C2D C3D C4D 0.9(5) . . . . ? C1D C2D C3D C7D 177.6(3) . . . . ? C2D C3D C4D C5D -0.8(5) . . . . ? C7D C3D C4D C5D -177.6(3) . . . . ? C3D C4D C5D C6D 0.3(5) . . . . ? C3D C4D C5D C8D 175.2(3) . . . . ? C4D C5D C6D C1D 0.2(5) . . . . ? C8D C5D C6D C1D -174.6(3) . . . . ? C2D C1D C6D C5D -0.1(4) . . . . ? B1D C1D C6D C5D 172.1(3) . . . . ? C4D C3D C7D F3D -165.2(3) . . . . ? C2D C3D C7D F3D 18.0(5) . . . . ? C4D C3D C7D F1D 73.2(4) . . . . ? C2D C3D C7D F1D -103.6(4) . . . . ? C4D C3D C7D F2D -45.5(4) . . . . ? C2D C3D C7D F2D 137.7(3) . . . . ? C6D C5D C8D F5D 104.8(4) . . . . ? C4D C5D C8D F5D -70.1(4) . . . . ? C6D C5D C8D F6D -135.3(3) . . . . ? C4D C5D C8D F6D 49.8(5) . . . . ? C6D C5D C8D F4D -13.9(5) . . . . ? C4D C5D C8D F4D 171.3(3) . . . . ? C14D C9D C10D C11D -2.6(4) . . . . ? B1D C9D C10D C11D 172.5(3) . . . . ? C9D C10D C11D C12D 0.6(5) . . . . ? C9D C10D C11D C15D -178.0(3) . . . . ? C10D C11D C12D C13D 2.1(4) . . . . ? C15D C11D C12D C13D -179.3(3) . . . . ? C11D C12D C13D C14D -2.6(4) . . . . ? C11D C12D C13D C16D 174.9(3) . . . . ? C12D C13D C14D C9D 0.4(5) . . . . ? C16D C13D C14D C9D -177.0(3) . . . . ? C10D C9D C14D C13D 2.1(4) . . . . ? B1D C9D C14D C13D -172.6(3) . . . . ? C10D C11D C15D F7D 10.7(5) . . . . ? C12D C11D C15D F7D -167.9(3) . . . . ? C10D C11D C15D F8D 130.7(3) . . . . ? C12D C11D C15D F8D -48.0(4) . . . . ? C10D C11D C15D F9D -110.0(4) . . . . ? C12D C11D C15D F9D 71.3(4) . . . . ? C12D C13D C16D F11D 158.0(3) . . . . ? C14D C13D C16D F11D -24.5(4) . . . . ? C12D C13D C16D F12D 37.8(4) . . . . ? C14D C13D C16D F12D -144.7(3) . . . . ? C12D C13D C16D F10D -80.2(4) . . . . ? C14D C13D C16D F10D 97.3(4) . . . . ? C22D C17D C18D C19D -1.3(5) . . . . ? B1D C17D C18D C19D 177.1(4) . . . . ? C17D C18D C19D C20D -0.1(7) . . . . ? C17D C18D C19D C23D -178.5(5) . . . . ? C18D C19D C20D C21D 0.1(7) . . . . ? C23D C19D C20D C21D 178.5(5) . . . . ? C19D C20D C21D C22D 1.2(8) . . . . ? C19D C20D C21D C24D 168.8(9) . . . . ? C19D C20D C21D C24A -152.0(8) . . . . ? C18D C17D C22D C21D 2.7(6) . . . . ? B1D C17D C22D C21D -175.7(4) . . . . ? C20D C21D C22D C17D -2.8(8) . . . . ? C24D C21D C22D C17D -169.8(9) . . . . ? C24A C21D C22D C17D 150.6(9) . . . . ? C20D C19D C23D F14D -12.5(9) . . . . ? C18D C19D C23D F14D 165.9(5) . . . . ? C20D C19D C23D F13D -135.5(5) . . . . ? C18D C19D C23D F13D 43.0(7) . . . . ? C20D C19D C23D F15D 106.3(5) . . . . ? C18D C19D C23D F15D -75.3(6) . . . . ? C30D C25D C26D C27D -0.9(5) . . . . ? B1D C25D C26D C27D 179.8(3) . . . . ? C25D C26D C27D C28D 1.1(5) . . . . ? C25D C26D C27D C31D -177.6(4) . . . . ? C26D C27D C28D C29D -0.6(6) . . . . ? C31D C27D C28D C29D 178.2(4) . . . . ? C27D C28D C29D C30D -0.1(6) . . . . ? C27D C28D C29D C32D -179.0(4) . . . . ? C26D C25D C30D C29D 0.2(5) . . . . ? B1D C25D C30D C29D 179.4(3) . . . . ? C28D C29D C30D C25D 0.3(6) . . . . ? C32D C29D C30D C25D 179.1(4) . . . . ? C28D C27D C31D F19D 56.8(6) . . . . ? C26D C27D C31D F19D -124.4(5) . . . . ? C28D C27D C31D F20D -173.9(4) . . . . ? C26D C27D C31D F20D 4.9(6) . . . . ? C28D C27D C31D F21D -59.4(5) . . . . ? C26D C27D C31D F21D 119.4(4) . . . . ? C30D C29D C32D F22F 6.5(10) . . . . ? C28D C29D C32D F22F -174.6(8) . . . . ? C30D C29D C32D F24D -167.4(11) . . . . ? C28D C29D C32D F24D 11.4(13) . . . . ? C30D C29D C32D F23F 134.7(6) . . . . ? C28D C29D C32D F23F -46.5(8) . . . . ? C30D C29D C32D F22D -26.4(9) . . . . ? C28D C29D C32D F22D 152.5(6) . . . . ? C30D C29D C32D F24F -122.1(5) . . . . ? C28D C29D C32D F24F 56.7(6) . . . . ? C30D C29D C32D F23D 81.5(7) . . . . ? C28D C29D C32D F23D -99.7(7) . . . . ? C30D C25D B1D C9D 0.9(4) . . . . ? C26D C25D B1D C9D -179.9(3) . . . . ? C30D C25D B1D C1D 116.3(3) . . . . ? C26D C25D B1D C1D -64.6(4) . . . . ? C30D C25D B1D C17D -121.2(3) . . . . ? C26D C25D B1D C17D 58.0(4) . . . . ? C14D C9D B1D C25D -111.2(3) . . . . ? C10D C9D B1D C25D 74.2(3) . . . . ? C14D C9D B1D C1D 129.0(3) . . . . ? C10D C9D B1D C1D -45.5(3) . . . . ? C14D C9D B1D C17D 7.3(4) . . . . ? C10D C9D B1D C17D -167.2(3) . . . . ? C2D C1D B1D C25D -1.0(4) . . . . ? C6D C1D B1D C25D -172.6(3) . . . . ? C2D C1D B1D C9D 118.6(3) . . . . ? C6D C1D B1D C9D -52.9(3) . . . . ? C2D C1D B1D C17D -119.9(3) . . . . ? C6D C1D B1D C17D 68.5(4) . . . . ? C22D C17D B1D C25D 47.9(4) . . . . ? C18D C17D B1D C25D -130.3(3) . . . . ? C22D C17D B1D C9D -73.5(4) . . . . ? C18D C17D B1D C9D 108.2(3) . . . . ? C22D C17D B1D C1D 169.7(3) . . . . ? C18D C17D B1D C1D -8.5(4) . . . . ? C20D C21D C24D F16D -110.5(19) . . . . ? C22D C21D C24D F16D 57(2) . . . . ? C24A C21D C24D F16D 150(2) . . . . ? C20D C21D C24D F18D 8.3(19) . . . . ? C22D C21D C24D F18D 175.7(13) . . . . ? C24A C21D C24D F18D -91.6(18) . . . . ? C20D C21D C24D F17D 142.2(13) . . . . ? C22D C21D C24D F17D -50.4(17) . . . . ? C24A C21D C24D F17D 42.4(14) . . . . ? C20D C21D C24A F18A -49(2) . . . . ? C22D C21D C24A F18A 156.7(16) . . . . ? C24D C21D C24A F18A 49.4(17) . . . . ? C20D C21D C24A F17A 72.4(16) . . . . ? C22D C21D C24A F17A -81.7(16) . . . . ? C24D C21D C24A F17A 171(2) . . . . ? C20D C21D C24A F16A -135.9(16) . . . . ? C22D C21D C24A F16A 70.1(17) . . . . ? C24D C21D C24A F16A -37.2(16) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.70 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.039 _refine_diff_density_min -0.770 _refine_diff_density_rms 0.079 #===END data_mc2(6OTf)_CCDC648102 _database_code_depnum_ccdc_archive 'CCDC 648102' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C84 H116 Cu4 N12 O10), 4(C F3 O3 S), 4.5(OH2)' _chemical_formula_sum 'C88 H125 Cu4 F12 N12 O26.50 S4' _chemical_formula_weight 2385.40 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 Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 36.414(11) _cell_length_b 11.889(4) _cell_length_c 25.772(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11158(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4948 _exptl_absorpt_coefficient_mu 0.920 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 170433 _diffrn_reflns_av_R_equivalents 0.1515 _diffrn_reflns_av_sigmaI/netI 0.1357 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.55 _reflns_number_total 27839 _reflns_number_gt 14941 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER Shelxtl' _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. A considerable amount of electron density attibutable to partially disordered water of solvation was seen in the channels between the host molecules. Some of this could be modeled by oxygen atoms at full occupancy and some at 0.75 occupancy. The hydrogen atoms associated with the solvent waters could not be located and so are omitted from the final refinement and structure factor calculations. They are, however, included in the reported chemical formula and derived values (e.g. formula weight, etc) ; _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^)+(0.1758P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(8) _refine_ls_number_reflns 27839 _refine_ls_number_parameters 1324 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1837 _refine_ls_R_factor_gt 0.0964 _refine_ls_wR_factor_ref 0.2962 _refine_ls_wR_factor_gt 0.2450 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 4.870 _refine_ls_shift/su_max 0.015 _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 0.50417(12) -0.2190(4) 0.7876(2) 0.0323(12) Uani 1 1 d . . . N1 N 0.4697(10) -0.357(4) 0.8043(16) 0.045(10) Uani 1 1 d . . . O1 O 0.5194(9) -0.259(3) 0.7088(13) 0.048(8) Uani 1 1 d D . . H1XB H 0.5371 -0.3090 0.7018 0.058 Uiso 1 1 d RD . . H1XA H 0.5072 -0.2230 0.6833 0.058 Uiso 1 1 d RD . . C1 C 0.4365(11) -0.326(4) 0.835(2) 0.045(12) Uani 1 1 d . . . H1C H 0.4199 -0.3897 0.8364 0.054 Uiso 1 1 calc R . . H1D H 0.4238 -0.2647 0.8182 0.054 Uiso 1 1 calc R . . Cu2 Cu 0.48397(14) 0.1967(5) 0.9846(2) 0.0419(14) Uani 1 1 d . . . O2 O 0.4623(8) -0.129(3) 0.7689(12) 0.037(7) Uani 1 1 d . . . N2 N 0.5432(10) -0.303(3) 0.8259(16) 0.039(9) Uani 1 1 d . . . C2 C 0.4541(13) -0.396(4) 0.752(2) 0.050(13) Uani 1 1 d . . . H2A H 0.4381 -0.4587 0.7579 0.074 Uiso 1 1 calc R . . H2B H 0.4739 -0.4176 0.7299 0.074 Uiso 1 1 calc R . . H2C H 0.4406 -0.3353 0.7368 0.074 Uiso 1 1 calc R . . Cu3 Cu 0.32018(13) 0.6260(4) 0.5975(2) 0.0343(12) Uani 1 1 d . . . O3 O 0.4667(9) -0.108(3) 0.6829(14) 0.048(8) Uani 1 1 d . . . N3 N 0.5384(8) -0.077(3) 0.7952(14) 0.034(8) Uani 1 1 d . . . C3 C 0.4920(14) -0.439(4) 0.828(2) 0.050(12) Uani 1 1 d . . . H3A H 0.5023 -0.4876 0.8010 0.060 Uiso 1 1 calc R . . H3B H 0.4771 -0.4858 0.8503 0.060 Uiso 1 1 calc R . . Cu4 Cu 0.20748(12) 0.3418(4) 0.7782(2) 0.0366(13) Uani 1 1 d . . . N4 N 0.5279(10) 0.311(3) 0.9872(15) 0.040(8) Uani 1 1 d . . . O4 O 0.2447(9) 0.220(3) 0.8249(17) 0.056(10) Uani 1 1 d . . . C4 C 0.5232(11) -0.388(4) 0.859(2) 0.039(11) Uani 1 1 d . . . H4A H 0.5134 -0.3506 0.8897 0.047 Uiso 1 1 calc R . . H4B H 0.5400 -0.4459 0.8704 0.047 Uiso 1 1 calc R . . O5 O 0.2523(8) 0.284(3) 0.7456(15) 0.043(8) Uani 1 1 d . . . N5 N 0.4883(10) 0.184(4) 1.0597(16) 0.044(10) Uani 1 1 d . . . C5 C 0.5694(12) -0.361(4) 0.792(2) 0.044(12) Uani 1 1 d . . . H5A H 0.5873 -0.3994 0.8124 0.066 Uiso 1 1 calc R . . H5B H 0.5815 -0.3061 0.7702 0.066 Uiso 1 1 calc R . . H5C H 0.5566 -0.4137 0.7703 0.066 Uiso 1 1 calc R . . O6 O 0.4697(8) 0.219(3) 0.9144(14) 0.054(10) Uani 1 1 d . . . N6 N 0.4556(10) 0.049(4) 0.9883(16) 0.046(10) Uani 1 1 d . . . C6 C 0.5621(12) -0.216(4) 0.8573(19) 0.039(10) Uani 1 1 d . . . H6A H 0.5844 -0.2466 0.8721 0.047 Uiso 1 1 calc R . . H6B H 0.5463 -0.1919 0.8856 0.047 Uiso 1 1 calc R . . O7 O 0.4316(9) 0.322(4) 0.9623(14) 0.059(10) Uani 1 1 d . . . N7 N 0.1698(11) 0.237(3) 0.7415(17) 0.042(9) Uani 1 1 d . . . C7 C 0.5714(10) -0.116(4) 0.8238(19) 0.037(10) Uani 1 1 d . . . H7A H 0.5808 -0.0559 0.8452 0.044 Uiso 1 1 calc R . . H7B H 0.5904 -0.1374 0.7992 0.044 Uiso 1 1 calc R . . O8 O 0.3604(8) 0.600(3) 0.5341(13) 0.042(8) Uani 1 1 d D . . H8XA H 0.3785 0.5499 0.5397 0.051 Uiso 1 1 d RD . . H8XB H 0.3600 0.6351 0.5032 0.051 Uiso 1 1 d RD . . N8 N 0.1668(9) 0.394(3) 0.8246(17) 0.040(9) Uani 1 1 d . . . C8 C 0.5488(11) -0.032(4) 0.7437(18) 0.037(10) Uani 1 1 d . . . H8C H 0.5644 0.0321 0.7480 0.056 Uiso 1 1 calc R . . H8D H 0.5271 -0.0107 0.7250 0.056 Uiso 1 1 calc R . . H8E H 0.5617 -0.0892 0.7245 0.056 Uiso 1 1 calc R . . O9 O 0.3900(10) 0.457(4) 0.5985(16) 0.066(11) Uani 1 1 d . . . C9 C 0.5179(11) 0.005(4) 0.8271(18) 0.033(9) Uani 1 1 d . . . H9A H 0.5114 -0.0324 0.8593 0.039 Uiso 1 1 calc R . . H9B H 0.4951 0.0211 0.8091 0.039 Uiso 1 1 calc R . . N9 N 0.2333(8) 0.494(3) 0.7992(15) 0.037(9) Uani 1 1 d . . . O10 O 0.3467(7) 0.537(3) 0.6473(13) 0.040(8) Uani 1 1 d . . . N10 N 0.3407(9) 0.772(4) 0.6331(17) 0.043(10) Uani 1 1 d . . . N11 N 0.2859(11) 0.729(3) 0.5598(17) 0.045(10) Uani 1 1 d . . . C11 C 0.5351(10) 0.114(4) 0.8406(19) 0.038(11) Uani 1 1 d . . . N12 N 0.2806(9) 0.501(3) 0.5819(14) 0.034(8) Uani 1 1 d . . . C12 C 0.5452(10) 0.136(4) 0.8909(19) 0.034(10) Uani 1 1 d . . . H12A H 0.5441 0.0793 0.9158 0.041 Uiso 1 1 calc R . . C13 C 0.5571(11) 0.244(4) 0.905(2) 0.039(11) Uani 1 1 d . . . C14 C 0.5618(11) 0.325(4) 0.868(2) 0.040(11) Uani 1 1 d . . . H14A H 0.5715 0.3944 0.8777 0.048 Uiso 1 1 calc R . . C15 C 0.5527(11) 0.305(4) 0.819(2) 0.041(11) Uani 1 1 d . . . H15A H 0.5568 0.3603 0.7941 0.049 Uiso 1 1 calc R . . C16 C 0.5371(11) 0.203(4) 0.8030(18) 0.037(10) Uani 1 1 d . . . H16A H 0.5284 0.1927 0.7694 0.044 Uiso 1 1 calc R . . C17 C 0.5625(12) 0.269(4) 0.962(2) 0.040(11) Uani 1 1 d . . . H17A H 0.5704 0.2009 0.9798 0.048 Uiso 1 1 calc R . . H17B H 0.5817 0.3247 0.9662 0.048 Uiso 1 1 calc R . . C18 C 0.5167(14) 0.421(4) 0.965(2) 0.051(13) Uani 1 1 d . . . H18A H 0.5369 0.4729 0.9675 0.077 Uiso 1 1 calc R . . H18B H 0.4963 0.4505 0.9848 0.077 Uiso 1 1 calc R . . H18C H 0.5097 0.4119 0.9298 0.077 Uiso 1 1 calc R . . C19 C 0.5351(17) 0.325(5) 1.045(2) 0.056(14) Uani 1 1 d . . . H19A H 0.5606 0.3457 1.0498 0.067 Uiso 1 1 calc R . . H19B H 0.5199 0.3856 1.0580 0.067 Uiso 1 1 calc R . . C20 C 0.5271(12) 0.221(5) 1.073(2) 0.047(12) Uani 1 1 d . . . H20A H 0.5292 0.2345 1.1100 0.057 Uiso 1 1 calc R . . H20B H 0.5446 0.1633 1.0633 0.057 Uiso 1 1 calc R . . C21 C 0.4605(15) 0.253(5) 1.082(2) 0.059(15) Uani 1 1 d . . . H21A H 0.4618 0.2491 1.1189 0.088 Uiso 1 1 calc R . . H21B H 0.4368 0.2277 1.0703 0.088 Uiso 1 1 calc R . . H21C H 0.4641 0.3297 1.0709 0.088 Uiso 1 1 calc R . . C22 C 0.4815(14) 0.063(4) 1.0724(19) 0.046(12) Uani 1 1 d . . . H22A H 0.5031 0.0187 1.0640 0.056 Uiso 1 1 calc R . . H22B H 0.4768 0.0550 1.1093 0.056 Uiso 1 1 calc R . . C23 C 0.4503(17) 0.022(5) 1.043(2) 0.060(15) Uani 1 1 d . . . H23A H 0.4280 0.0569 1.0558 0.072 Uiso 1 1 calc R . . H23B H 0.4481 -0.0588 1.0474 0.072 Uiso 1 1 calc R . . C33 C 0.4176(12) 0.047(5) 0.961(2) 0.058(15) Uani 1 1 d . . . H33A H 0.4066 -0.0257 0.9657 0.088 Uiso 1 1 calc R . . H33B H 0.4205 0.0627 0.9251 0.088 Uiso 1 1 calc R . . H33C H 0.4020 0.1032 0.9767 0.088 Uiso 1 1 calc R . . C34 C 0.4804(12) -0.030(4) 0.960(2) 0.045(12) Uani 1 1 d . . . H34A H 0.5033 -0.0342 0.9793 0.054 Uiso 1 1 calc R . . H34B H 0.4858 0.0024 0.9266 0.054 Uiso 1 1 calc R . . C35 C 0.4671(12) -0.151(5) 0.9512(19) 0.047(12) Uani 1 1 d . . . C36 C 0.4556(12) -0.181(4) 0.901(2) 0.042(11) Uani 1 1 d . . . H36A H 0.4551 -0.1271 0.8750 0.051 Uiso 1 1 calc R . . C37 C 0.4452(12) -0.290(4) 0.8913(19) 0.044(12) Uani 1 1 d . . . C38 C 0.4446(13) -0.371(5) 0.932(2) 0.047(12) Uani 1 1 d . . . H38A H 0.4368 -0.4441 0.9260 0.056 Uiso 1 1 calc R . . C39 C 0.4557(14) -0.338(5) 0.980(2) 0.052(13) Uani 1 1 d . . . H39A H 0.4550 -0.3895 1.0072 0.062 Uiso 1 1 calc R . . C40 C 0.4682(13) -0.229(5) 0.990(2) 0.054(14) Uani 1 1 d . . . H40A H 0.4772 -0.2105 1.0226 0.065 Uiso 1 1 calc R . . C41 C 0.4519(10) -0.087(4) 0.7254(18) 0.034(10) Uani 1 1 d . . . C42 C 0.4189(11) -0.014(3) 0.7279(19) 0.036(10) Uani 1 1 d . . . C43 C 0.4001(11) -0.002(4) 0.773(2) 0.040(11) Uani 1 1 d . . . H43A H 0.4091 -0.0372 0.8029 0.049 Uiso 1 1 calc R . . C44 C 0.3677(11) 0.063(4) 0.778(2) 0.040(10) Uani 1 1 d . . . C45 C 0.3490(13) 0.072(5) 0.825(2) 0.054(14) Uani 1 1 d . . . H45A H 0.3589 0.0406 0.8547 0.065 Uiso 1 1 calc R . . C46 C 0.3160(13) 0.126(4) 0.826(2) 0.053(13) Uani 1 1 d . . . H46A H 0.3033 0.1316 0.8574 0.063 Uiso 1 1 calc R . . C47 C 0.3010(10) 0.175(4) 0.781(2) 0.040(10) Uani 1 1 d . . . C48 C 0.3181(11) 0.168(4) 0.736(2) 0.038(10) Uani 1 1 d . . . H48A H 0.3071 0.1992 0.7065 0.046 Uiso 1 1 calc R . . C49 C 0.3545(11) 0.113(4) 0.731(2) 0.038(11) Uani 1 1 d . . . C50 C 0.3726(11) 0.105(4) 0.686(2) 0.039(11) Uani 1 1 d . . . H50A H 0.3636 0.1398 0.6564 0.046 Uiso 1 1 calc R . . C51 C 0.4054(11) 0.043(4) 0.6841(18) 0.035(10) Uani 1 1 d . . . H51A H 0.4185 0.0388 0.6532 0.042 Uiso 1 1 calc R . . C52 C 0.2642(12) 0.228(4) 0.784(2) 0.041(10) Uani 1 1 d . . . C53 C 0.1611(12) 0.269(4) 0.687(2) 0.041(11) Uani 1 1 d . . . H53A H 0.1538 0.3476 0.6858 0.049 Uiso 1 1 calc R . . H53B H 0.1404 0.2246 0.6749 0.049 Uiso 1 1 calc R . . C54 C 0.1839(13) 0.116(4) 0.744(2) 0.047(12) Uani 1 1 d . . . H54A H 0.1668 0.0668 0.7265 0.071 Uiso 1 1 calc R . . H54B H 0.1865 0.0927 0.7792 0.071 Uiso 1 1 calc R . . H54C H 0.2073 0.1111 0.7267 0.071 Uiso 1 1 calc R . . C55 C 0.1373(12) 0.248(4) 0.773(2) 0.046(11) Uani 1 1 d . . . H55A H 0.1389 0.1946 0.8019 0.055 Uiso 1 1 calc R . . H55B H 0.1159 0.2287 0.7529 0.055 Uiso 1 1 calc R . . C56 C 0.1328(10) 0.362(4) 0.7946(19) 0.037(10) Uani 1 1 d . . . H56A H 0.1115 0.3649 0.8173 0.044 Uiso 1 1 calc R . . H56B H 0.1289 0.4153 0.7665 0.044 Uiso 1 1 calc R . . C57 C 0.1680(13) 0.332(5) 0.8747(19) 0.047(12) Uani 1 1 d . . . H57A H 0.1483 0.3573 0.8965 0.070 Uiso 1 1 calc R . . H57B H 0.1911 0.3458 0.8915 0.070 Uiso 1 1 calc R . . H57C H 0.1654 0.2529 0.8682 0.070 Uiso 1 1 calc R . . C58 C 0.1708(11) 0.514(4) 0.8333(19) 0.038(10) Uani 1 1 d . . . H58A H 0.1567 0.5356 0.8636 0.045 Uiso 1 1 calc R . . H58B H 0.1610 0.5546 0.8037 0.045 Uiso 1 1 calc R . . C59 C 0.2114(11) 0.547(4) 0.8412(18) 0.039(10) Uani 1 1 d . . . H59A H 0.2141 0.6278 0.8400 0.047 Uiso 1 1 calc R . . H59B H 0.2199 0.5204 0.8747 0.047 Uiso 1 1 calc R . . C60 C 0.2714(11) 0.481(5) 0.816(2) 0.049(13) Uani 1 1 d . . . H60A H 0.2812 0.5537 0.8252 0.074 Uiso 1 1 calc R . . H60B H 0.2857 0.4485 0.7891 0.074 Uiso 1 1 calc R . . H60C H 0.2721 0.4332 0.8464 0.074 Uiso 1 1 calc R . . C61 C 0.2311(11) 0.559(3) 0.7484(16) 0.030(9) Uani 1 1 d . . . H61A H 0.2404 0.5106 0.7211 0.036 Uiso 1 1 calc R . . H61B H 0.2054 0.5727 0.7410 0.036 Uiso 1 1 calc R . . C62 C 0.2507(10) 0.668(4) 0.7449(17) 0.031(9) Uani 1 1 d . . . C63 C 0.2861(10) 0.671(4) 0.7207(18) 0.033(9) Uani 1 1 d . . . H63A H 0.2965 0.6056 0.7078 0.039 Uiso 1 1 calc R . . C64 C 0.3046(11) 0.771(4) 0.7165(19) 0.037(10) Uani 1 1 d . . . C65 C 0.2900(13) 0.868(4) 0.737(2) 0.043(11) Uani 1 1 d . . . H65A H 0.3035 0.9342 0.7354 0.052 Uiso 1 1 calc R . . C66 C 0.2546(14) 0.869(4) 0.760(2) 0.049(13) Uani 1 1 d . . . H66A H 0.2443 0.9349 0.7722 0.059 Uiso 1 1 calc R . . C67 C 0.2355(12) 0.766(4) 0.7625(19) 0.040(11) Uani 1 1 d . . . H67A H 0.2120 0.7646 0.7767 0.048 Uiso 1 1 calc R . . C68 C 0.3425(12) 0.774(5) 0.690(2) 0.047(12) Uani 1 1 d . . . H68A H 0.3552 0.8421 0.7011 0.056 Uiso 1 1 calc R . . H68B H 0.3568 0.7104 0.7021 0.056 Uiso 1 1 calc R . . C69 C 0.3806(12) 0.779(5) 0.617(2) 0.053(14) Uani 1 1 d . . . H69A H 0.3917 0.8441 0.6325 0.079 Uiso 1 1 calc R . . H69B H 0.3821 0.7849 0.5798 0.079 Uiso 1 1 calc R . . H69C H 0.3933 0.7126 0.6282 0.079 Uiso 1 1 calc R . . C70 C 0.3199(12) 0.867(3) 0.613(2) 0.041(11) Uani 1 1 d . . . H70A H 0.3325 0.8996 0.5839 0.049 Uiso 1 1 calc R . . H70B H 0.3176 0.9238 0.6401 0.049 Uiso 1 1 calc R . . C71 C 0.2805(13) 0.825(4) 0.596(2) 0.049(12) Uani 1 1 d . . . H71A H 0.2666 0.8006 0.6265 0.058 Uiso 1 1 calc R . . H71B H 0.2672 0.8850 0.5795 0.058 Uiso 1 1 calc R . . C72 C 0.2992(15) 0.774(5) 0.509(2) 0.052(13) Uani 1 1 d . . . H72A H 0.2809 0.8227 0.4947 0.079 Uiso 1 1 calc R . . H72B H 0.3036 0.7122 0.4857 0.079 Uiso 1 1 calc R . . H72C H 0.3216 0.8145 0.5144 0.079 Uiso 1 1 calc R . . C73 C 0.2487(12) 0.670(4) 0.552(2) 0.046(12) Uani 1 1 d . . . H73A H 0.2289 0.7216 0.5605 0.055 Uiso 1 1 calc R . . H73B H 0.2460 0.6466 0.5164 0.055 Uiso 1 1 calc R . . C74 C 0.2468(10) 0.570(4) 0.5869(18) 0.036(10) Uani 1 1 d . . . H74A H 0.2255 0.5251 0.5779 0.044 Uiso 1 1 calc R . . H74B H 0.2440 0.5947 0.6226 0.044 Uiso 1 1 calc R . . C75 C 0.2861(14) 0.453(4) 0.530(2) 0.047(12) Uani 1 1 d . . . H75A H 0.2678 0.3960 0.5241 0.071 Uiso 1 1 calc R . . H75B H 0.3101 0.4198 0.5283 0.071 Uiso 1 1 calc R . . H75C H 0.2839 0.5109 0.5046 0.071 Uiso 1 1 calc R . . C76 C 0.2814(13) 0.408(4) 0.6191(18) 0.040(10) Uani 1 1 d . . . H76A H 0.2807 0.4400 0.6537 0.048 Uiso 1 1 calc R . . H76B H 0.3047 0.3698 0.6154 0.048 Uiso 1 1 calc R . . C77 C 0.2519(13) 0.323(4) 0.6152(19) 0.043(11) Uani 1 1 d . . . C78 C 0.2202(11) 0.338(4) 0.6449(18) 0.036(10) Uani 1 1 d . . . H78A H 0.2167 0.4057 0.6621 0.043 Uiso 1 1 calc R . . C79 C 0.1929(15) 0.252(4) 0.650(2) 0.049(13) Uani 1 1 d . . . C80 C 0.1967(14) 0.157(5) 0.620(2) 0.058(15) Uani 1 1 d . . . H80A H 0.1784 0.1027 0.6200 0.069 Uiso 1 1 calc R . . C81 C 0.2277(18) 0.142(4) 0.590(3) 0.064(17) Uani 1 1 d . . . H81A H 0.2301 0.0762 0.5708 0.077 Uiso 1 1 calc R . . C82 C 0.2548(15) 0.221(4) 0.586(2) 0.051(13) Uani 1 1 d . . . H82A H 0.2752 0.2081 0.5653 0.061 Uiso 1 1 calc R . . C83 C 0.4410(13) 0.284(5) 0.920(2) 0.050(13) Uani 1 1 d . . . C84 C 0.4208(11) 0.315(5) 0.872(2) 0.044(12) Uani 1 1 d . . . C85 C 0.4365(11) 0.285(4) 0.825(2) 0.047(13) Uani 1 1 d . . . H85A H 0.4578 0.2421 0.8238 0.056 Uiso 1 1 calc R . . C86 C 0.4196(11) 0.322(4) 0.777(2) 0.039(10) Uani 1 1 d . . . C87 C 0.4356(12) 0.304(4) 0.730(2) 0.041(11) Uani 1 1 d . . . H87A H 0.4566 0.2596 0.7270 0.049 Uiso 1 1 calc R . . C88 C 0.4214(12) 0.350(4) 0.6873(19) 0.040(11) Uani 1 1 d . . . H88A H 0.4334 0.3397 0.6558 0.048 Uiso 1 1 calc R . . C89 C 0.3880(11) 0.415(4) 0.688(2) 0.038(11) Uani 1 1 d . . . C90 C 0.3717(11) 0.432(4) 0.7345(17) 0.036(10) Uani 1 1 d . . . H90A H 0.3504 0.4755 0.7359 0.044 Uiso 1 1 calc R . . C91 C 0.3860(11) 0.385(4) 0.781(2) 0.045(11) Uani 1 1 d . . . C92 C 0.3698(11) 0.407(4) 0.8309(19) 0.040(11) Uani 1 1 d . . . H92A H 0.3473 0.4433 0.8330 0.048 Uiso 1 1 calc R . . C93 C 0.3874(12) 0.374(4) 0.875(2) 0.046(12) Uani 1 1 d . . . H93A H 0.3773 0.3900 0.9071 0.055 Uiso 1 1 calc R . . C94 C 0.3750(14) 0.472(4) 0.641(2) 0.047(12) Uani 1 1 d . . . S1A S 0.6439(3) 0.5201(10) 0.8979(5) 0.038(3) Uani 1 1 d . . . O1A O 0.6427(12) 0.480(3) 0.8460(14) 0.060(10) Uani 1 1 d . . . C1A C 0.6725(13) 0.647(5) 0.891(2) 0.057(15) Uani 1 1 d . . . F1A F 0.6568(9) 0.718(3) 0.8591(15) 0.068(9) Uani 1 1 d . . . O2A O 0.6096(9) 0.561(3) 0.9173(15) 0.052(9) Uani 1 1 d . . . F2A F 0.7047(9) 0.623(4) 0.8727(19) 0.101(15) Uani 1 1 d . . . O3A O 0.6646(9) 0.449(3) 0.9329(14) 0.054(9) Uani 1 1 d . . . F3A F 0.6761(14) 0.696(4) 0.9362(17) 0.102(16) Uani 1 1 d . . . S1B S 0.3987(3) 0.0425(11) 0.4943(5) 0.046(3) Uani 1 1 d . . . O1B O 0.371(2) -0.011(6) 0.521(3) 0.14(3) Uani 1 1 d . . . F1B F 0.4095(15) 0.178(4) 0.5721(15) 0.102(15) Uani 1 1 d . . . C1B C 0.402(2) 0.183(7) 0.524(3) 0.08(2) Uani 1 1 d . . . F2B F 0.363(3) 0.214(11) 0.526(4) 0.33(9) Uani 1 1 d . . . O2B O 0.3931(13) 0.062(4) 0.4413(17) 0.077(13) Uani 1 1 d . . . O3B O 0.4339(12) -0.001(5) 0.506(2) 0.11(2) Uani 1 1 d . . . F3B F 0.419(4) 0.246(5) 0.500(3) 0.29(8) Uani 1 1 d . . . S1D S 0.3616(4) 0.1214(15) 0.1624(7) 0.067(4) Uani 1 1 d . . . C1D C 0.357(3) 0.269(11) 0.160(5) 0.14(4) Uani 1 1 d . . . F1D F 0.395(2) 0.304(8) 0.180(4) 0.21(4) Uani 1 1 d . . . O1D O 0.3596(11) 0.096(5) 0.2148(19) 0.084(15) Uani 1 1 d . . . O2D O 0.3978(13) 0.098(6) 0.143(2) 0.104(19) Uani 1 1 d . . . F2D F 0.326(4) 0.299(7) 0.174(4) 0.30(8) Uani 1 1 d . . . F3D F 0.3600(16) 0.313(6) 0.115(3) 0.17(3) Uani 1 1 d . . . O3D O 0.332(2) 0.083(6) 0.134(4) 0.16(3) Uani 1 1 d . . . S1C S 0.4440(5) 0.5497(14) 0.1541(6) 0.068(4) Uani 1 1 d . . . F1C F 0.4938(12) 0.661(4) 0.1070(19) 0.099(13) Uani 1 1 d . . . C1C C 0.4677(19) 0.670(6) 0.143(3) 0.074(18) Uani 1 1 d U . . O1C O 0.4739(12) 0.477(4) 0.173(2) 0.094(17) Uani 1 1 d . . . F2C F 0.4798(16) 0.727(5) 0.181(2) 0.122(18) Uani 1 1 d . . . O2C O 0.4149(19) 0.574(5) 0.188(2) 0.13(3) Uani 1 1 d . . . O3C O 0.4280(17) 0.513(4) 0.104(2) 0.097(16) Uani 1 1 d . . . F3C F 0.4447(17) 0.756(4) 0.120(2) 0.123(19) Uani 1 1 d . . . O1W O 0.2432(14) 0.105(5) 0.914(2) 0.071(16) Uani 0.75 1 d P . . O2W O 0.3849(14) 0.474(6) 0.016(2) 0.11(2) Uani 1 1 d . . . O3W O 0.3150(19) 0.381(7) 0.009(3) 0.13(2) Uani 1 1 d . . . O4W O 0.309(4) 0.023(14) 0.956(4) 0.36(12) Uani 1 1 d . . . O6W O 0.266(3) 0.38(2) 0.931(4) 0.36(16) Uani 0.75 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 0.018(2) 0.036(3) 0.043(3) -0.003(2) -0.002(2) 0.0056(18) N1 0.022(17) 0.06(3) 0.06(3) -0.01(2) 0.000(17) 0.000(17) O1 0.037(18) 0.06(2) 0.05(2) -0.006(17) -0.003(15) 0.018(16) C1 0.013(17) 0.05(3) 0.07(3) 0.00(2) -0.01(2) 0.005(18) Cu2 0.023(2) 0.057(4) 0.045(3) -0.004(3) -0.004(2) 0.003(2) O2 0.027(14) 0.048(18) 0.036(17) -0.010(14) 0.002(12) 0.008(12) N2 0.028(17) 0.04(2) 0.05(2) -0.001(18) 0.003(16) 0.006(16) C2 0.03(2) 0.05(3) 0.06(3) -0.02(3) -0.01(2) -0.01(2) Cu3 0.020(2) 0.036(3) 0.046(3) 0.001(2) 0.003(2) -0.002(2) O3 0.032(16) 0.05(2) 0.06(2) -0.011(17) -0.003(16) 0.016(14) N3 0.019(14) 0.039(19) 0.04(2) 0.000(16) -0.005(14) 0.012(14) C3 0.05(3) 0.03(3) 0.07(4) 0.00(2) 0.01(3) 0.00(2) Cu4 0.017(2) 0.035(3) 0.058(4) 0.009(3) 0.007(2) 0.0065(18) N4 0.037(19) 0.05(2) 0.03(2) -0.006(18) -0.005(17) 0.011(16) O4 0.025(15) 0.05(2) 0.09(3) 0.03(2) 0.013(17) 0.014(14) C4 0.022(19) 0.04(3) 0.05(3) 0.01(2) -0.010(19) -0.002(17) O5 0.023(14) 0.033(16) 0.07(2) 0.009(16) 0.003(14) 0.005(12) N5 0.03(2) 0.05(2) 0.05(2) 0.00(2) -0.002(17) 0.000(17) C5 0.03(2) 0.04(2) 0.06(3) 0.01(2) 0.00(2) 0.013(18) O6 0.014(13) 0.09(3) 0.05(2) -0.007(19) -0.010(14) 0.012(16) N6 0.027(18) 0.06(3) 0.05(2) -0.01(2) -0.003(18) 0.009(17) C6 0.03(2) 0.04(3) 0.05(3) 0.00(2) -0.016(19) 0.004(19) O7 0.032(17) 0.10(3) 0.04(2) 0.00(2) -0.006(15) 0.015(19) N7 0.04(2) 0.03(2) 0.06(3) -0.007(18) 0.014(18) 0.001(16) C7 0.014(17) 0.04(3) 0.05(3) -0.01(2) -0.001(18) -0.001(16) O8 0.027(15) 0.047(19) 0.05(2) -0.007(15) 0.011(13) 0.000(13) N8 0.017(15) 0.04(2) 0.06(3) 0.002(19) 0.007(16) 0.002(14) C8 0.024(19) 0.04(3) 0.04(3) 0.01(2) 0.003(18) -0.003(18) O9 0.05(2) 0.09(3) 0.05(2) -0.01(2) 0.000(19) 0.04(2) C9 0.022(18) 0.04(2) 0.04(2) 0.000(19) 0.004(17) 0.003(16) N9 0.012(14) 0.04(2) 0.06(2) 0.003(17) 0.005(14) 0.000(13) O10 0.015(13) 0.038(17) 0.07(2) 0.002(15) 0.005(13) 0.004(12) N10 0.016(16) 0.06(3) 0.05(2) -0.02(2) 0.012(15) -0.005(16) N11 0.04(2) 0.04(2) 0.05(2) 0.002(19) 0.013(18) 0.002(17) C11 0.015(17) 0.04(2) 0.06(3) 0.01(2) 0.008(19) 0.005(16) N12 0.030(17) 0.032(19) 0.04(2) 0.000(16) 0.001(15) 0.000(14) C12 0.016(17) 0.03(2) 0.05(3) 0.01(2) -0.009(18) 0.003(15) C13 0.018(18) 0.04(3) 0.06(3) 0.00(2) 0.000(19) 0.002(17) C14 0.019(19) 0.04(3) 0.06(3) 0.00(2) 0.003(19) 0.001(17) C15 0.03(2) 0.04(3) 0.06(3) 0.00(2) 0.01(2) 0.005(18) C16 0.018(17) 0.05(3) 0.05(3) 0.00(2) -0.005(17) 0.009(17) C17 0.03(2) 0.03(2) 0.06(3) 0.00(2) 0.00(2) 0.006(18) C18 0.04(3) 0.04(3) 0.07(4) 0.00(2) 0.01(3) 0.00(2) C19 0.06(3) 0.06(3) 0.05(3) 0.01(3) 0.00(3) 0.00(3) C20 0.02(2) 0.06(3) 0.06(3) 0.01(3) -0.02(2) -0.01(2) C21 0.04(3) 0.08(4) 0.06(3) -0.02(3) 0.00(2) 0.00(3) C22 0.05(3) 0.05(3) 0.03(3) 0.01(2) 0.01(2) 0.00(2) C23 0.07(4) 0.06(4) 0.05(3) -0.02(3) 0.02(3) -0.01(3) C33 0.02(2) 0.08(4) 0.08(4) -0.02(3) 0.00(2) 0.00(2) C34 0.02(2) 0.07(3) 0.04(3) -0.01(2) 0.000(19) -0.01(2) C35 0.03(2) 0.08(4) 0.04(3) -0.01(3) 0.008(19) 0.00(2) C36 0.03(2) 0.04(3) 0.05(3) -0.01(2) 0.01(2) -0.001(19) C37 0.03(2) 0.06(3) 0.04(3) -0.01(2) 0.01(2) 0.00(2) C38 0.03(2) 0.05(3) 0.06(3) 0.00(3) 0.01(2) -0.01(2) C39 0.04(3) 0.06(3) 0.05(3) 0.01(3) 0.02(3) 0.01(2) C40 0.03(2) 0.08(4) 0.05(3) -0.01(3) 0.01(2) -0.01(2) C41 0.019(18) 0.03(2) 0.05(3) -0.01(2) -0.014(19) 0.004(16) C42 0.023(18) 0.03(2) 0.06(3) -0.02(2) 0.001(19) 0.009(16) C43 0.03(2) 0.04(2) 0.05(3) 0.00(2) -0.01(2) 0.017(18) C44 0.022(18) 0.05(2) 0.05(3) -0.01(2) 0.00(2) 0.012(17) C45 0.04(2) 0.07(4) 0.06(3) -0.02(3) -0.02(2) 0.02(2) C46 0.04(2) 0.05(3) 0.07(4) 0.00(3) 0.01(2) 0.02(2) C47 0.023(18) 0.04(2) 0.06(3) 0.00(2) -0.01(2) 0.003(16) C48 0.023(19) 0.03(2) 0.06(3) 0.00(2) 0.00(2) 0.006(17) C49 0.017(18) 0.03(2) 0.07(3) -0.01(2) -0.02(2) 0.003(16) C50 0.023(19) 0.03(2) 0.06(3) 0.01(2) -0.01(2) -0.003(16) C51 0.025(19) 0.04(2) 0.04(3) -0.01(2) -0.002(18) 0.000(17) C52 0.03(2) 0.04(2) 0.05(3) 0.00(2) 0.00(2) -0.006(18) C53 0.03(2) 0.03(2) 0.06(3) 0.00(2) 0.00(2) -0.002(18) C54 0.04(3) 0.03(2) 0.07(4) 0.00(2) 0.01(2) 0.005(19) C55 0.03(2) 0.06(3) 0.05(3) 0.00(2) 0.01(2) 0.00(2) C56 0.016(16) 0.04(2) 0.06(3) 0.00(2) 0.002(18) 0.000(15) C57 0.04(2) 0.06(3) 0.04(3) 0.01(2) 0.00(2) 0.01(2) C58 0.021(18) 0.04(3) 0.05(3) 0.00(2) 0.002(18) 0.008(17) C59 0.03(2) 0.05(3) 0.04(3) 0.00(2) 0.000(18) 0.003(19) C60 0.019(19) 0.06(3) 0.07(3) 0.00(3) -0.01(2) 0.006(19) C61 0.029(19) 0.03(2) 0.03(2) 0.004(17) 0.004(17) -0.002(16) C62 0.020(18) 0.03(2) 0.04(2) -0.002(19) 0.007(17) 0.010(16) C63 0.018(18) 0.03(2) 0.05(3) -0.002(19) 0.001(17) -0.002(15) C64 0.024(19) 0.04(3) 0.04(3) 0.00(2) 0.005(18) -0.004(18) C65 0.04(3) 0.03(3) 0.06(3) 0.00(2) 0.01(2) 0.00(2) C66 0.05(3) 0.04(3) 0.07(3) 0.00(2) 0.03(2) 0.00(2) C67 0.03(2) 0.03(2) 0.05(3) 0.01(2) 0.01(2) 0.000(18) C68 0.03(2) 0.06(3) 0.05(3) -0.01(2) 0.02(2) -0.02(2) C69 0.03(2) 0.07(3) 0.07(3) -0.02(3) 0.01(2) -0.02(2) C70 0.04(2) 0.02(2) 0.06(3) 0.00(2) 0.02(2) -0.004(17) C71 0.04(2) 0.03(2) 0.08(4) 0.01(2) 0.00(3) 0.004(19) C72 0.05(3) 0.05(3) 0.06(3) 0.01(3) 0.00(2) -0.01(2) C73 0.02(2) 0.05(3) 0.07(3) 0.00(2) 0.00(2) 0.006(19) C74 0.019(18) 0.05(3) 0.04(3) 0.00(2) -0.002(17) -0.004(17) C75 0.04(3) 0.04(3) 0.06(3) 0.00(2) 0.00(2) 0.00(2) C76 0.04(2) 0.05(3) 0.03(2) 0.01(2) 0.002(19) 0.00(2) C77 0.04(2) 0.04(3) 0.04(3) 0.01(2) 0.00(2) 0.00(2) C78 0.03(2) 0.04(2) 0.04(3) 0.00(2) 0.004(18) -0.001(18) C79 0.05(3) 0.03(3) 0.06(4) -0.01(2) 0.00(3) -0.01(2) C80 0.04(3) 0.05(3) 0.08(4) 0.00(3) 0.00(3) -0.01(2) C81 0.08(4) 0.04(3) 0.08(4) -0.01(3) 0.02(3) -0.02(3) C82 0.06(3) 0.03(3) 0.06(3) -0.01(2) 0.02(3) 0.00(2) C83 0.03(2) 0.07(4) 0.06(3) -0.01(3) -0.01(2) -0.01(2) C84 0.018(19) 0.06(3) 0.05(3) 0.00(2) -0.013(19) -0.01(2) C85 0.017(18) 0.05(3) 0.08(4) -0.01(3) -0.02(2) 0.002(18) C86 0.027(19) 0.03(2) 0.06(3) 0.00(2) -0.01(2) -0.006(16) C87 0.03(2) 0.03(2) 0.06(3) -0.01(2) -0.01(2) 0.003(18) C88 0.03(2) 0.04(3) 0.05(3) -0.02(2) -0.01(2) 0.005(19) C89 0.03(2) 0.03(2) 0.06(3) 0.00(2) -0.02(2) -0.002(17) C90 0.022(19) 0.05(3) 0.04(2) 0.00(2) -0.009(18) -0.007(18) C91 0.020(18) 0.06(3) 0.06(3) -0.01(3) 0.00(2) -0.004(18) C92 0.016(18) 0.05(3) 0.06(3) 0.00(2) -0.006(19) 0.000(18) C93 0.03(2) 0.06(3) 0.05(3) 0.00(2) 0.00(2) 0.01(2) C94 0.04(3) 0.04(3) 0.06(3) -0.01(2) -0.01(2) 0.01(2) S1A 0.032(5) 0.036(6) 0.047(7) -0.003(5) 0.000(5) 0.004(4) O1A 0.09(3) 0.05(2) 0.04(2) -0.003(18) -0.008(19) 0.00(2) C1A 0.03(2) 0.08(4) 0.07(4) 0.00(3) 0.00(2) -0.02(2) F1A 0.050(18) 0.06(2) 0.09(3) 0.034(18) 0.000(17) 0.000(15) O2A 0.032(16) 0.05(2) 0.07(3) 0.001(18) 0.015(16) 0.000(15) F2A 0.042(19) 0.13(4) 0.13(4) 0.05(3) 0.03(2) 0.02(2) O3A 0.041(19) 0.07(2) 0.05(2) 0.016(18) -0.006(16) 0.004(17) F3A 0.13(4) 0.09(3) 0.08(3) 0.00(2) -0.01(3) -0.07(3) S1B 0.036(6) 0.048(7) 0.054(8) 0.004(6) 0.007(5) 0.005(5) O1B 0.16(6) 0.14(6) 0.12(5) 0.00(4) 0.06(4) -0.08(5) F1B 0.17(5) 0.08(3) 0.06(2) -0.01(2) -0.02(3) 0.04(3) C1B 0.10(6) 0.07(5) 0.07(5) 0.01(4) -0.02(4) 0.01(4) F2B 0.29(11) 0.43(16) 0.26(10) -0.24(11) -0.17(9) 0.31(12) O2B 0.09(3) 0.07(3) 0.06(3) -0.02(2) 0.00(2) 0.00(2) O3B 0.05(2) 0.13(4) 0.15(5) -0.07(4) -0.01(3) 0.04(3) F3B 0.7(2) 0.05(3) 0.11(5) 0.02(3) -0.10(9) -0.11(7) S1D 0.044(7) 0.084(11) 0.074(10) 0.026(9) 0.000(7) -0.014(7) C1D 0.07(6) 0.18(11) 0.15(10) 0.07(9) 0.03(6) 0.04(7) F1D 0.15(6) 0.22(8) 0.25(9) 0.12(7) -0.08(6) -0.09(6) O1D 0.04(2) 0.12(4) 0.09(3) 0.04(3) 0.01(2) 0.01(2) O2D 0.06(3) 0.17(5) 0.08(3) 0.03(4) 0.02(2) 0.04(3) F2D 0.38(15) 0.18(8) 0.33(13) 0.15(8) 0.25(12) 0.20(9) F3D 0.11(4) 0.19(6) 0.21(7) 0.15(6) -0.05(4) -0.06(4) O3D 0.15(6) 0.11(5) 0.20(7) -0.02(5) -0.09(6) 0.02(5) S1C 0.076(10) 0.063(10) 0.066(10) 0.001(8) -0.004(8) 0.010(8) F1C 0.08(3) 0.11(4) 0.11(3) 0.01(3) 0.02(2) 0.02(2) C1C 0.07(3) 0.09(4) 0.06(3) 0.00(3) -0.03(3) -0.01(3) O1C 0.06(3) 0.07(3) 0.15(5) 0.05(3) -0.01(3) 0.01(2) F2C 0.13(5) 0.14(4) 0.09(3) -0.01(3) -0.03(3) -0.02(3) O2C 0.17(6) 0.08(3) 0.14(5) 0.03(3) 0.11(5) 0.06(4) O3C 0.13(5) 0.08(3) 0.08(3) -0.01(3) 0.00(3) -0.01(3) F3C 0.16(5) 0.05(2) 0.16(5) 0.01(3) 0.00(4) 0.00(3) O1W 0.05(3) 0.10(4) 0.06(3) 0.04(3) 0.02(3) 0.00(3) O2W 0.06(3) 0.16(5) 0.11(4) 0.03(4) 0.03(3) 0.04(3) O3W 0.12(5) 0.16(6) 0.12(5) 0.03(4) -0.03(4) -0.01(4) O4W 0.5(2) 0.5(2) 0.15(8) -0.09(11) -0.07(11) 0.38(19) O6W 0.08(6) 0.9(4) 0.14(9) 0.26(17) -0.07(6) -0.13(14) _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 O2 1.92(3) . ? Cu1 N2 2.00(4) . ? Cu1 N3 2.11(4) . ? Cu1 N1 2.11(4) . ? Cu1 O1 2.16(3) . ? N1 C3 1.41(7) . ? N1 C1 1.50(6) . ? N1 C2 1.52(6) . ? C1 C37 1.53(7) . ? Cu2 O6 1.90(4) . ? Cu2 N5 1.95(4) . ? Cu2 N6 2.04(4) . ? Cu2 N4 2.10(4) . ? Cu2 C83 2.51(5) . ? O2 C41 1.29(5) . ? N2 C5 1.47(6) . ? N2 C6 1.49(6) . ? N2 C4 1.50(6) . ? Cu3 O10 1.93(3) . ? Cu3 N11 2.00(4) . ? Cu3 N10 2.10(4) . ? Cu3 N12 2.11(4) . ? Cu3 O8 2.21(3) . ? O3 C41 1.25(6) . ? N3 C9 1.47(5) . ? N3 C8 1.48(6) . ? N3 C7 1.49(5) . ? C3 C4 1.52(7) . ? Cu4 O5 1.96(3) . ? Cu4 N8 2.00(4) . ? Cu4 N7 2.08(4) . ? Cu4 N9 2.11(4) . ? Cu4 O4 2.32(3) . ? Cu4 C52 2.47(4) . ? N4 C18 1.48(7) . ? N4 C17 1.50(6) . ? N4 C19 1.51(7) . ? O4 C52 1.27(6) . ? O5 C52 1.27(6) . ? N5 C21 1.43(7) . ? N5 C22 1.50(7) . ? N5 C20 1.52(6) . ? O6 C83 1.31(6) . ? N6 C23 1.46(7) . ? N6 C34 1.49(6) . ? N6 C33 1.55(6) . ? C6 C7 1.50(7) . ? O7 C83 1.23(6) . ? N7 C55 1.45(6) . ? N7 C53 1.50(6) . ? N7 C54 1.54(6) . ? N8 C58 1.45(6) . ? N8 C57 1.49(6) . ? N8 C56 1.51(5) . ? O9 C94 1.23(7) . ? C9 C11 1.48(6) . ? N9 C60 1.46(5) . ? N9 C59 1.48(6) . ? N9 C61 1.52(5) . ? O10 C94 1.30(6) . ? N10 C70 1.45(6) . ? N10 C68 1.48(6) . ? N10 C69 1.52(5) . ? N11 C72 1.49(7) . ? N11 C71 1.50(7) . ? N11 C73 1.54(6) . ? C11 C12 1.37(7) . ? C11 C16 1.44(7) . ? N12 C76 1.46(6) . ? N12 C75 1.46(6) . ? N12 C74 1.49(5) . ? C12 C13 1.40(6) . ? C13 C14 1.36(7) . ? C13 C17 1.52(7) . ? C14 C15 1.34(7) . ? C15 C16 1.40(7) . ? C19 C20 1.46(8) . ? C22 C23 1.45(8) . ? C34 C35 1.53(7) . ? C35 C40 1.37(8) . ? C35 C36 1.40(7) . ? C36 C37 1.38(7) . ? C37 C38 1.42(7) . ? C38 C39 1.36(8) . ? C39 C40 1.39(8) . ? C41 C42 1.48(5) . ? C42 C43 1.36(7) . ? C42 C51 1.40(7) . ? C43 C44 1.41(5) . ? C44 C45 1.40(8) . ? C44 C49 1.42(7) . ? C45 C46 1.37(6) . ? C46 C47 1.40(7) . ? C47 C48 1.33(7) . ? C47 C52 1.49(6) . ? C48 C49 1.48(6) . ? C49 C50 1.34(7) . ? C50 C51 1.41(6) . ? C53 C79 1.51(7) . ? C55 C56 1.48(7) . ? C58 C59 1.54(6) . ? C61 C62 1.48(6) . ? C62 C67 1.37(6) . ? C62 C63 1.43(5) . ? C63 C64 1.37(6) . ? C64 C65 1.37(7) . ? C64 C68 1.54(6) . ? C65 C66 1.42(6) . ? C66 C67 1.41(7) . ? C70 C71 1.58(7) . ? C73 C74 1.48(7) . ? C76 C77 1.48(7) . ? C77 C78 1.40(6) . ? C77 C82 1.43(7) . ? C78 C79 1.43(6) . ? C79 C80 1.37(7) . ? C80 C81 1.38(8) . ? C81 C82 1.36(8) . ? C83 C84 1.48(7) . ? C84 C85 1.39(7) . ? C84 C93 1.40(6) . ? C85 C86 1.44(7) . ? C86 C87 1.37(7) . ? C86 C91 1.44(6) . ? C87 C88 1.32(7) . ? C88 C89 1.45(6) . ? C89 C90 1.34(7) . ? C89 C94 1.48(7) . ? C90 C91 1.43(7) . ? C91 C92 1.43(7) . ? C92 C93 1.36(7) . ? S1A O1A 1.42(4) . ? S1A O2A 1.43(3) . ? S1A O3A 1.45(4) . ? S1A C1A 1.84(5) . ? C1A F2A 1.30(6) . ? C1A F3A 1.30(7) . ? C1A F1A 1.32(7) . ? S1B O1B 1.36(5) . ? S1B O2B 1.40(5) . ? S1B O3B 1.41(4) . ? S1B C1B 1.85(8) . ? F1B C1B 1.27(8) . ? C1B F3B 1.14(12) . ? C1B F2B 1.47(12) . ? S1D O3D 1.36(7) . ? S1D O1D 1.39(5) . ? S1D O2D 1.44(5) . ? S1D C1D 1.76(13) . ? C1D F2D 1.21(11) . ? C1D F3D 1.29(11) . ? C1D F1D 1.53(13) . ? S1C O2C 1.41(5) . ? S1C O1C 1.48(4) . ? S1C O3C 1.48(5) . ? S1C C1C 1.70(8) . ? F1C C1C 1.32(8) . ? C1C F2C 1.28(8) . ? C1C F3C 1.44(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 O2 Cu1 N2 165.0(14) . . ? O2 Cu1 N3 92.8(13) . . ? N2 Cu1 N3 86.4(14) . . ? O2 Cu1 N1 90.6(14) . . ? N2 Cu1 N1 86.0(16) . . ? N3 Cu1 N1 163.0(16) . . ? O2 Cu1 O1 95.1(12) . . ? N2 Cu1 O1 99.9(14) . . ? N3 Cu1 O1 96.4(14) . . ? N1 Cu1 O1 99.9(15) . . ? C3 N1 C1 114(4) . . ? C3 N1 C2 113(4) . . ? C1 N1 C2 104(3) . . ? C3 N1 Cu1 107(3) . . ? C1 N1 Cu1 113(3) . . ? C2 N1 Cu1 106(3) . . ? N1 C1 C37 114(3) . . ? O6 Cu2 N5 168.2(15) . . ? O6 Cu2 N6 91.5(17) . . ? N5 Cu2 N6 85.8(17) . . ? O6 Cu2 N4 98.6(16) . . ? N5 Cu2 N4 87.5(16) . . ? N6 Cu2 N4 160.4(14) . . ? O6 Cu2 C83 30.7(16) . . ? N5 Cu2 C83 138.0(18) . . ? N6 Cu2 C83 94.1(16) . . ? N4 Cu2 C83 103.1(16) . . ? C41 O2 Cu1 132(3) . . ? C5 N2 C6 110(4) . . ? C5 N2 C4 110(4) . . ? C6 N2 C4 112(4) . . ? C5 N2 Cu1 114(3) . . ? C6 N2 Cu1 104(3) . . ? C4 N2 Cu1 106(2) . . ? O10 Cu3 N11 166.9(15) . . ? O10 Cu3 N10 89.2(15) . . ? N11 Cu3 N10 85.9(17) . . ? O10 Cu3 N12 94.7(13) . . ? N11 Cu3 N12 84.9(15) . . ? N10 Cu3 N12 155.2(13) . . ? O10 Cu3 O8 94.8(13) . . ? N11 Cu3 O8 98.1(15) . . ? N10 Cu3 O8 101.8(13) . . ? N12 Cu3 O8 102.3(13) . . ? C9 N3 C8 113(3) . . ? C9 N3 C7 110(3) . . ? C8 N3 C7 110(3) . . ? C9 N3 Cu1 106(2) . . ? C8 N3 Cu1 111(3) . . ? C7 N3 Cu1 106(3) . . ? N1 C3 C4 112(4) . . ? O5 Cu4 N8 168.7(16) . . ? O5 Cu4 N7 98.3(14) . . ? N8 Cu4 N7 88.2(15) . . ? O5 Cu4 N9 92.4(13) . . ? N8 Cu4 N9 84.9(14) . . ? N7 Cu4 N9 157.4(15) . . ? O5 Cu4 O4 61.1(13) . . ? N8 Cu4 O4 108.4(15) . . ? N7 Cu4 O4 104.3(15) . . ? N9 Cu4 O4 98.3(14) . . ? O5 Cu4 C52 30.6(16) . . ? N8 Cu4 C52 138.6(18) . . ? N7 Cu4 C52 104.7(15) . . ? N9 Cu4 C52 94.7(13) . . ? O4 Cu4 C52 30.6(15) . . ? C18 N4 C17 111(4) . . ? C18 N4 C19 109(4) . . ? C17 N4 C19 108(4) . . ? C18 N4 Cu2 111(3) . . ? C17 N4 Cu2 114(3) . . ? C19 N4 Cu2 104(3) . . ? C52 O4 Cu4 81(3) . . ? N2 C4 C3 109(4) . . ? C52 O5 Cu4 98(3) . . ? C21 N5 C22 111(4) . . ? C21 N5 C20 114(4) . . ? C22 N5 C20 113(4) . . ? C21 N5 Cu2 107(3) . . ? C22 N5 Cu2 106(3) . . ? C20 N5 Cu2 106(3) . . ? C83 O6 Cu2 102(3) . . ? C23 N6 C34 114(4) . . ? C23 N6 C33 108(4) . . ? C34 N6 C33 108(4) . . ? C23 N6 Cu2 108(3) . . ? C34 N6 Cu2 102(3) . . ? C33 N6 Cu2 116(3) . . ? N2 C6 C7 110(4) . . ? C55 N7 C53 110(4) . . ? C55 N7 C54 110(4) . . ? C53 N7 C54 110(4) . . ? C55 N7 Cu4 103(3) . . ? C53 N7 Cu4 115(3) . . ? C54 N7 Cu4 109(3) . . ? N3 C7 C6 111(3) . . ? C58 N8 C57 111(4) . . ? C58 N8 C56 114(3) . . ? C57 N8 C56 110(4) . . ? C58 N8 Cu4 109(3) . . ? C57 N8 Cu4 110(3) . . ? C56 N8 Cu4 103(3) . . ? N3 C9 C11 120(3) . . ? C60 N9 C59 109(4) . . ? C60 N9 C61 111(3) . . ? C59 N9 C61 113(3) . . ? C60 N9 Cu4 114(3) . . ? C59 N9 Cu4 108(3) . . ? C61 N9 Cu4 101(2) . . ? C94 O10 Cu3 129(3) . . ? C70 N10 C68 111(4) . . ? C70 N10 C69 111(4) . . ? C68 N10 C69 103(4) . . ? C70 N10 Cu3 108(3) . . ? C68 N10 Cu3 118(3) . . ? C69 N10 Cu3 105(3) . . ? C72 N11 C71 109(4) . . ? C72 N11 C73 110(4) . . ? C71 N11 C73 108(4) . . ? C72 N11 Cu3 116(3) . . ? C71 N11 Cu3 104(3) . . ? C73 N11 Cu3 110(3) . . ? C12 C11 C16 119(4) . . ? C12 C11 C9 120(4) . . ? C16 C11 C9 120(4) . . ? C76 N12 C75 107(4) . . ? C76 N12 C74 112(3) . . ? C75 N12 C74 114(3) . . ? C76 N12 Cu3 113(3) . . ? C75 N12 Cu3 111(3) . . ? C74 N12 Cu3 99(2) . . ? C11 C12 C13 120(4) . . ? C14 C13 C12 121(5) . . ? C14 C13 C17 121(4) . . ? C12 C13 C17 118(4) . . ? C15 C14 C13 120(5) . . ? C14 C15 C16 122(5) . . ? C15 C16 C11 118(4) . . ? N4 C17 C13 112(4) . . ? C20 C19 N4 111(5) . . ? C19 C20 N5 109(4) . . ? C23 C22 N5 110(4) . . ? C22 C23 N6 109(4) . . ? N6 C34 C35 118(4) . . ? C40 C35 C36 120(5) . . ? C40 C35 C34 121(5) . . ? C36 C35 C34 118(5) . . ? C37 C36 C35 119(5) . . ? C36 C37 C38 120(5) . . ? C36 C37 C1 119(5) . . ? C38 C37 C1 120(5) . . ? C39 C38 C37 118(5) . . ? C38 C39 C40 122(5) . . ? C35 C40 C39 119(5) . . ? O3 C41 O2 124(4) . . ? O3 C41 C42 120(4) . . ? O2 C41 C42 115(4) . . ? C43 C42 C51 118(4) . . ? C43 C42 C41 120(4) . . ? C51 C42 C41 122(4) . . ? C42 C43 C44 123(4) . . ? C45 C44 C43 121(5) . . ? C45 C44 C49 122(4) . . ? C43 C44 C49 117(4) . . ? C46 C45 C44 119(5) . . ? C45 C46 C47 121(5) . . ? C48 C47 C46 121(4) . . ? C48 C47 C52 119(5) . . ? C46 C47 C52 119(5) . . ? C47 C48 C49 121(4) . . ? C50 C49 C44 122(4) . . ? C50 C49 C48 123(4) . . ? C44 C49 C48 115(4) . . ? C49 C50 C51 119(4) . . ? C42 C51 C50 121(4) . . ? O5 C52 O4 120(4) . . ? O5 C52 C47 120(4) . . ? O4 C52 C47 121(5) . . ? O5 C52 Cu4 52(2) . . ? O4 C52 Cu4 68(2) . . ? C47 C52 Cu4 170(4) . . ? N7 C53 C79 113(4) . . ? N7 C55 C56 112(4) . . ? C55 C56 N8 109(3) . . ? N8 C58 C59 111(3) . . ? N9 C59 C58 108(4) . . ? C62 C61 N9 118(4) . . ? C67 C62 C63 119(4) . . ? C67 C62 C61 122(4) . . ? C63 C62 C61 119(4) . . ? C64 C63 C62 120(4) . . ? C63 C64 C65 121(4) . . ? C63 C64 C68 120(4) . . ? C65 C64 C68 119(4) . . ? C64 C65 C66 121(4) . . ? C67 C66 C65 118(4) . . ? C62 C67 C66 122(4) . . ? N10 C68 C64 113(4) . . ? N10 C70 C71 109(3) . . ? N11 C71 C70 107(4) . . ? C74 C73 N11 109(4) . . ? C73 C74 N12 111(3) . . ? N12 C76 C77 117(4) . . ? C78 C77 C82 117(4) . . ? C78 C77 C76 119(4) . . ? C82 C77 C76 124(5) . . ? C77 C78 C79 122(4) . . ? C80 C79 C78 118(5) . . ? C80 C79 C53 123(4) . . ? C78 C79 C53 119(4) . . ? C79 C80 C81 120(5) . . ? C82 C81 C80 123(5) . . ? C81 C82 C77 120(5) . . ? O7 C83 O6 122(5) . . ? O7 C83 C84 121(5) . . ? O6 C83 C84 117(5) . . ? O7 C83 Cu2 75(3) . . ? O6 C83 Cu2 48(2) . . ? C84 C83 Cu2 164(4) . . ? C85 C84 C93 122(4) . . ? C85 C84 C83 118(4) . . ? C93 C84 C83 120(5) . . ? C84 C85 C86 120(4) . . ? C87 C86 C85 122(4) . . ? C87 C86 C91 121(4) . . ? C85 C86 C91 117(5) . . ? C88 C87 C86 120(4) . . ? C87 C88 C89 122(5) . . ? C90 C89 C88 118(4) . . ? C90 C89 C94 122(4) . . ? C88 C89 C94 120(5) . . ? C89 C90 C91 122(4) . . ? C92 C91 C90 122(4) . . ? C92 C91 C86 121(4) . . ? C90 C91 C86 116(4) . . ? C93 C92 C91 120(4) . . ? C92 C93 C84 120(5) . . ? O9 C94 O10 124(5) . . ? O9 C94 C89 122(4) . . ? O10 C94 C89 114(5) . . ? O1A S1A O2A 115(2) . . ? O1A S1A O3A 114(2) . . ? O2A S1A O3A 116(2) . . ? O1A S1A C1A 102(3) . . ? O2A S1A C1A 104(2) . . ? O3A S1A C1A 104(2) . . ? F2A C1A F3A 110(5) . . ? F2A C1A F1A 108(5) . . ? F3A C1A F1A 108(6) . . ? F2A C1A S1A 111(5) . . ? F3A C1A S1A 110(4) . . ? F1A C1A S1A 110(3) . . ? O1B S1B O2B 117(4) . . ? O1B S1B O3B 113(5) . . ? O2B S1B O3B 114(3) . . ? O1B S1B C1B 105(4) . . ? O2B S1B C1B 105(3) . . ? O3B S1B C1B 100(3) . . ? F3B C1B F1B 117(8) . . ? F3B C1B F2B 112(10) . . ? F1B C1B F2B 101(7) . . ? F3B C1B S1B 114(7) . . ? F1B C1B S1B 112(5) . . ? F2B C1B S1B 100(6) . . ? O3D S1D O1D 114(5) . . ? O3D S1D O2D 117(5) . . ? O1D S1D O2D 111(3) . . ? O3D S1D C1D 104(5) . . ? O1D S1D C1D 104(5) . . ? O2D S1D C1D 106(4) . . ? F2D C1D F3D 103(9) . . ? F2D C1D F1D 130(10) . . ? F3D C1D F1D 96(8) . . ? F2D C1D S1D 113(9) . . ? F3D C1D S1D 115(10) . . ? F1D C1D S1D 100(6) . . ? O2C S1C O1C 118(4) . . ? O2C S1C O3C 108(4) . . ? O1C S1C O3C 114(3) . . ? O2C S1C C1C 108(4) . . ? O1C S1C C1C 100(3) . . ? O3C S1C C1C 107(3) . . ? F2C C1C F1C 110(6) . . ? F2C C1C F3C 98(6) . . ? F1C C1C F3C 101(6) . . ? F2C C1C S1C 119(6) . . ? F1C C1C S1C 115(6) . . ? F3C C1C S1C 112(5) . . ? 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 O2 Cu1 N1 C3 -171(3) . . . . ? N2 Cu1 N1 C3 -6(3) . . . . ? N3 Cu1 N1 C3 -70(6) . . . . ? O1 Cu1 N1 C3 93(3) . . . . ? O2 Cu1 N1 C1 -45(3) . . . . ? N2 Cu1 N1 C1 120(3) . . . . ? N3 Cu1 N1 C1 56(6) . . . . ? O1 Cu1 N1 C1 -140(3) . . . . ? O2 Cu1 N1 C2 68(3) . . . . ? N2 Cu1 N1 C2 -126(3) . . . . ? N3 Cu1 N1 C2 170(4) . . . . ? O1 Cu1 N1 C2 -27(3) . . . . ? C3 N1 C1 C37 54(6) . . . . ? C2 N1 C1 C37 177(4) . . . . ? Cu1 N1 C1 C37 -69(5) . . . . ? N2 Cu1 O2 C41 169(5) . . . . ? N3 Cu1 O2 C41 83(4) . . . . ? N1 Cu1 O2 C41 -114(4) . . . . ? O1 Cu1 O2 C41 -14(4) . . . . ? O2 Cu1 N2 C5 179(5) . . . . ? N3 Cu1 N2 C5 -94(3) . . . . ? N1 Cu1 N2 C5 101(3) . . . . ? O1 Cu1 N2 C5 2(3) . . . . ? O2 Cu1 N2 C6 -61(7) . . . . ? N3 Cu1 N2 C6 26(3) . . . . ? N1 Cu1 N2 C6 -139(3) . . . . ? O1 Cu1 N2 C6 122(3) . . . . ? O2 Cu1 N2 C4 57(7) . . . . ? N3 Cu1 N2 C4 145(3) . . . . ? N1 Cu1 N2 C4 -20(3) . . . . ? O1 Cu1 N2 C4 -120(3) . . . . ? O2 Cu1 N3 C9 48(3) . . . . ? N2 Cu1 N3 C9 -117(3) . . . . ? N1 Cu1 N3 C9 -53(6) . . . . ? O1 Cu1 N3 C9 144(3) . . . . ? O2 Cu1 N3 C8 -75(3) . . . . ? N2 Cu1 N3 C8 120(3) . . . . ? N1 Cu1 N3 C8 -177(4) . . . . ? O1 Cu1 N3 C8 20(3) . . . . ? O2 Cu1 N3 C7 165(3) . . . . ? N2 Cu1 N3 C7 0(3) . . . . ? N1 Cu1 N3 C7 64(6) . . . . ? O1 Cu1 N3 C7 -100(3) . . . . ? C1 N1 C3 C4 -94(5) . . . . ? C2 N1 C3 C4 147(4) . . . . ? Cu1 N1 C3 C4 32(5) . . . . ? O6 Cu2 N4 C18 49(3) . . . . ? N5 Cu2 N4 C18 -121(3) . . . . ? N6 Cu2 N4 C18 169(4) . . . . ? C83 Cu2 N4 C18 18(3) . . . . ? O6 Cu2 N4 C17 -78(3) . . . . ? N5 Cu2 N4 C17 112(3) . . . . ? N6 Cu2 N4 C17 43(6) . . . . ? C83 Cu2 N4 C17 -109(3) . . . . ? O6 Cu2 N4 C19 165(3) . . . . ? N5 Cu2 N4 C19 -5(3) . . . . ? N6 Cu2 N4 C19 -75(6) . . . . ? C83 Cu2 N4 C19 134(3) . . . . ? O5 Cu4 O4 C52 3(3) . . . . ? N8 Cu4 O4 C52 -172(3) . . . . ? N7 Cu4 O4 C52 95(3) . . . . ? N9 Cu4 O4 C52 -85(3) . . . . ? C5 N2 C4 C3 -81(5) . . . . ? C6 N2 C4 C3 155(4) . . . . ? Cu1 N2 C4 C3 42(4) . . . . ? N1 C3 C4 N2 -51(5) . . . . ? N8 Cu4 O5 C52 20(9) . . . . ? N7 Cu4 O5 C52 -105(3) . . . . ? N9 Cu4 O5 C52 95(3) . . . . ? O4 Cu4 O5 C52 -3(3) . . . . ? O6 Cu2 N5 C21 -21(11) . . . . ? N6 Cu2 N5 C21 -98(3) . . . . ? N4 Cu2 N5 C21 100(3) . . . . ? C83 Cu2 N5 C21 -7(5) . . . . ? O6 Cu2 N5 C22 97(9) . . . . ? N6 Cu2 N5 C22 20(3) . . . . ? N4 Cu2 N5 C22 -142(3) . . . . ? C83 Cu2 N5 C22 111(3) . . . . ? O6 Cu2 N5 C20 -143(8) . . . . ? N6 Cu2 N5 C20 140(3) . . . . ? N4 Cu2 N5 C20 -22(3) . . . . ? C83 Cu2 N5 C20 -129(3) . . . . ? N5 Cu2 O6 C83 19(10) . . . . ? N6 Cu2 O6 C83 96(3) . . . . ? N4 Cu2 O6 C83 -101(3) . . . . ? O6 Cu2 N6 C23 -162(3) . . . . ? N5 Cu2 N6 C23 6(3) . . . . ? N4 Cu2 N6 C23 77(6) . . . . ? C83 Cu2 N6 C23 -132(3) . . . . ? O6 Cu2 N6 C34 77(3) . . . . ? N5 Cu2 N6 C34 -114(3) . . . . ? N4 Cu2 N6 C34 -44(6) . . . . ? C83 Cu2 N6 C34 108(3) . . . . ? O6 Cu2 N6 C33 -40(3) . . . . ? N5 Cu2 N6 C33 128(3) . . . . ? N4 Cu2 N6 C33 -162(4) . . . . ? C83 Cu2 N6 C33 -10(4) . . . . ? C5 N2 C6 C7 74(4) . . . . ? C4 N2 C6 C7 -163(3) . . . . ? Cu1 N2 C6 C7 -49(4) . . . . ? O5 Cu4 N7 C55 163(3) . . . . ? N8 Cu4 N7 C55 -8(3) . . . . ? N9 Cu4 N7 C55 -80(5) . . . . ? O4 Cu4 N7 C55 101(3) . . . . ? C52 Cu4 N7 C55 133(3) . . . . ? O5 Cu4 N7 C53 -77(3) . . . . ? N8 Cu4 N7 C53 112(3) . . . . ? N9 Cu4 N7 C53 40(5) . . . . ? O4 Cu4 N7 C53 -139(3) . . . . ? C52 Cu4 N7 C53 -108(3) . . . . ? O5 Cu4 N7 C54 47(3) . . . . ? N8 Cu4 N7 C54 -124(3) . . . . ? N9 Cu4 N7 C54 164(3) . . . . ? O4 Cu4 N7 C54 -15(3) . . . . ? C52 Cu4 N7 C54 16(3) . . . . ? C9 N3 C7 C6 88(4) . . . . ? C8 N3 C7 C6 -147(4) . . . . ? Cu1 N3 C7 C6 -27(4) . . . . ? N2 C6 C7 N3 52(5) . . . . ? O5 Cu4 N8 C58 94(8) . . . . ? N7 Cu4 N8 C58 -141(3) . . . . ? N9 Cu4 N8 C58 18(3) . . . . ? O4 Cu4 N8 C58 115(3) . . . . ? C52 Cu4 N8 C58 109(3) . . . . ? O5 Cu4 N8 C57 -27(9) . . . . ? N7 Cu4 N8 C57 98(3) . . . . ? N9 Cu4 N8 C57 -104(3) . . . . ? O4 Cu4 N8 C57 -7(3) . . . . ? C52 Cu4 N8 C57 -12(4) . . . . ? O5 Cu4 N8 C56 -145(7) . . . . ? N7 Cu4 N8 C56 -20(3) . . . . ? N9 Cu4 N8 C56 139(3) . . . . ? O4 Cu4 N8 C56 -124(3) . . . . ? C52 Cu4 N8 C56 -130(3) . . . . ? C8 N3 C9 C11 -60(5) . . . . ? C7 N3 C9 C11 64(5) . . . . ? Cu1 N3 C9 C11 179(3) . . . . ? O5 Cu4 N9 C60 -39(3) . . . . ? N8 Cu4 N9 C60 130(3) . . . . ? N7 Cu4 N9 C60 -157(4) . . . . ? O4 Cu4 N9 C60 22(3) . . . . ? C52 Cu4 N9 C60 -8(3) . . . . ? O5 Cu4 N9 C59 -161(3) . . . . ? N8 Cu4 N9 C59 8(3) . . . . ? N7 Cu4 N9 C59 81(5) . . . . ? O4 Cu4 N9 C59 -99(3) . . . . ? C52 Cu4 N9 C59 -130(3) . . . . ? O5 Cu4 N9 C61 81(2) . . . . ? N8 Cu4 N9 C61 -110(2) . . . . ? N7 Cu4 N9 C61 -37(5) . . . . ? O4 Cu4 N9 C61 142(2) . . . . ? C52 Cu4 N9 C61 111(2) . . . . ? N11 Cu3 O10 C94 -179(100) . . . . ? N10 Cu3 O10 C94 -111(4) . . . . ? N12 Cu3 O10 C94 93(4) . . . . ? O8 Cu3 O10 C94 -9(4) . . . . ? O10 Cu3 N10 C70 -167(3) . . . . ? N11 Cu3 N10 C70 1(3) . . . . ? N12 Cu3 N10 C70 -68(5) . . . . ? O8 Cu3 N10 C70 98(3) . . . . ? O10 Cu3 N10 C68 -40(3) . . . . ? N11 Cu3 N10 C68 127(3) . . . . ? N12 Cu3 N10 C68 59(5) . . . . ? O8 Cu3 N10 C68 -135(3) . . . . ? O10 Cu3 N10 C69 74(3) . . . . ? N11 Cu3 N10 C69 -118(3) . . . . ? N12 Cu3 N10 C69 174(4) . . . . ? O8 Cu3 N10 C69 -21(4) . . . . ? O10 Cu3 N11 C72 159(6) . . . . ? N10 Cu3 N11 C72 90(4) . . . . ? N12 Cu3 N11 C72 -113(4) . . . . ? O8 Cu3 N11 C72 -11(4) . . . . ? O10 Cu3 N11 C71 39(8) . . . . ? N10 Cu3 N11 C71 -29(3) . . . . ? N12 Cu3 N11 C71 128(3) . . . . ? O8 Cu3 N11 C71 -131(3) . . . . ? O10 Cu3 N11 C73 -76(8) . . . . ? N10 Cu3 N11 C73 -145(3) . . . . ? N12 Cu3 N11 C73 12(3) . . . . ? O8 Cu3 N11 C73 114(3) . . . . ? N3 C9 C11 C12 -111(5) . . . . ? N3 C9 C11 C16 77(5) . . . . ? O10 Cu3 N12 C76 12(3) . . . . ? N11 Cu3 N12 C76 -155(3) . . . . ? N10 Cu3 N12 C76 -86(5) . . . . ? O8 Cu3 N12 C76 108(3) . . . . ? O10 Cu3 N12 C75 -108(3) . . . . ? N11 Cu3 N12 C75 85(3) . . . . ? N10 Cu3 N12 C75 153(4) . . . . ? O8 Cu3 N12 C75 -12(3) . . . . ? O10 Cu3 N12 C74 131(3) . . . . ? N11 Cu3 N12 C74 -36(3) . . . . ? N10 Cu3 N12 C74 33(5) . . . . ? O8 Cu3 N12 C74 -133(2) . . . . ? C16 C11 C12 C13 0(6) . . . . ? C9 C11 C12 C13 -172(4) . . . . ? C11 C12 C13 C14 -6(6) . . . . ? C11 C12 C13 C17 171(4) . . . . ? C12 C13 C14 C15 5(6) . . . . ? C17 C13 C14 C15 -172(4) . . . . ? C13 C14 C15 C16 2(6) . . . . ? C14 C15 C16 C11 -7(6) . . . . ? C12 C11 C16 C15 6(6) . . . . ? C9 C11 C16 C15 178(4) . . . . ? C18 N4 C17 C13 -65(5) . . . . ? C19 N4 C17 C13 176(4) . . . . ? Cu2 N4 C17 C13 61(4) . . . . ? C14 C13 C17 N4 88(5) . . . . ? C12 C13 C17 N4 -89(5) . . . . ? C18 N4 C19 C20 150(4) . . . . ? C17 N4 C19 C20 -89(5) . . . . ? Cu2 N4 C19 C20 32(5) . . . . ? N4 C19 C20 N5 -53(6) . . . . ? C21 N5 C20 C19 -72(6) . . . . ? C22 N5 C20 C19 162(4) . . . . ? Cu2 N5 C20 C19 46(5) . . . . ? C21 N5 C22 C23 72(5) . . . . ? C20 N5 C22 C23 -160(4) . . . . ? Cu2 N5 C22 C23 -44(5) . . . . ? N5 C22 C23 N6 51(6) . . . . ? C34 N6 C23 C22 81(5) . . . . ? C33 N6 C23 C22 -159(5) . . . . ? Cu2 N6 C23 C22 -32(5) . . . . ? C23 N6 C34 C35 68(6) . . . . ? C33 N6 C34 C35 -52(6) . . . . ? Cu2 N6 C34 C35 -176(4) . . . . ? N6 C34 C35 C40 -78(6) . . . . ? N6 C34 C35 C36 105(5) . . . . ? C40 C35 C36 C37 0(7) . . . . ? C34 C35 C36 C37 177(4) . . . . ? C35 C36 C37 C38 3(7) . . . . ? C35 C36 C37 C1 -174(4) . . . . ? N1 C1 C37 C36 84(6) . . . . ? N1 C1 C37 C38 -93(5) . . . . ? C36 C37 C38 C39 -2(7) . . . . ? C1 C37 C38 C39 174(4) . . . . ? C37 C38 C39 C40 -1(7) . . . . ? C36 C35 C40 C39 -4(7) . . . . ? C34 C35 C40 C39 180(4) . . . . ? C38 C39 C40 C35 4(7) . . . . ? Cu1 O2 C41 O3 8(7) . . . . ? Cu1 O2 C41 C42 -175(3) . . . . ? O3 C41 C42 C43 172(4) . . . . ? O2 C41 C42 C43 -4(6) . . . . ? O3 C41 C42 C51 -7(6) . . . . ? O2 C41 C42 C51 177(4) . . . . ? C51 C42 C43 C44 2(7) . . . . ? C41 C42 C43 C44 -177(4) . . . . ? C42 C43 C44 C45 179(5) . . . . ? C42 C43 C44 C49 1(7) . . . . ? C43 C44 C45 C46 -174(5) . . . . ? C49 C44 C45 C46 3(8) . . . . ? C44 C45 C46 C47 -1(8) . . . . ? C45 C46 C47 C48 1(8) . . . . ? C45 C46 C47 C52 177(5) . . . . ? C46 C47 C48 C49 -2(7) . . . . ? C52 C47 C48 C49 -178(4) . . . . ? C45 C44 C49 C50 180(5) . . . . ? C43 C44 C49 C50 -3(7) . . . . ? C45 C44 C49 C48 -4(7) . . . . ? C43 C44 C49 C48 173(4) . . . . ? C47 C48 C49 C50 180(4) . . . . ? C47 C48 C49 C44 4(6) . . . . ? C44 C49 C50 C51 1(6) . . . . ? C48 C49 C50 C51 -175(4) . . . . ? C43 C42 C51 C50 -4(6) . . . . ? C41 C42 C51 C50 175(4) . . . . ? C49 C50 C51 C42 2(6) . . . . ? Cu4 O5 C52 O4 5(5) . . . . ? Cu4 O5 C52 C47 -174(4) . . . . ? Cu4 O4 C52 O5 -5(4) . . . . ? Cu4 O4 C52 C47 174(4) . . . . ? C48 C47 C52 O5 -12(6) . . . . ? C46 C47 C52 O5 172(4) . . . . ? C48 C47 C52 O4 169(5) . . . . ? C46 C47 C52 O4 -7(7) . . . . ? C48 C47 C52 Cu4 -42(23) . . . . ? C46 C47 C52 Cu4 141(20) . . . . ? N8 Cu4 C52 O5 -174(3) . . . . ? N7 Cu4 C52 O5 81(3) . . . . ? N9 Cu4 C52 O5 -87(3) . . . . ? O4 Cu4 C52 O5 175(5) . . . . ? O5 Cu4 C52 O4 -175(5) . . . . ? N8 Cu4 C52 O4 11(4) . . . . ? N7 Cu4 C52 O4 -93(3) . . . . ? N9 Cu4 C52 O4 98(3) . . . . ? O5 Cu4 C52 C47 34(21) . . . . ? N8 Cu4 C52 C47 -140(21) . . . . ? N7 Cu4 C52 C47 115(21) . . . . ? N9 Cu4 C52 C47 -53(22) . . . . ? O4 Cu4 C52 C47 -151(23) . . . . ? C55 N7 C53 C79 -176(4) . . . . ? C54 N7 C53 C79 -55(5) . . . . ? Cu4 N7 C53 C79 68(4) . . . . ? C53 N7 C55 C56 -87(5) . . . . ? C54 N7 C55 C56 151(4) . . . . ? Cu4 N7 C55 C56 35(5) . . . . ? N7 C55 C56 N8 -56(5) . . . . ? C58 N8 C56 C55 162(4) . . . . ? C57 N8 C56 C55 -73(5) . . . . ? Cu4 N8 C56 C55 44(4) . . . . ? C57 N8 C58 C59 80(4) . . . . ? C56 N8 C58 C59 -155(4) . . . . ? Cu4 N8 C58 C59 -41(5) . . . . ? C60 N9 C59 C58 -156(4) . . . . ? C61 N9 C59 C58 80(4) . . . . ? Cu4 N9 C59 C58 -31(4) . . . . ? N8 C58 C59 N9 48(5) . . . . ? C60 N9 C61 C62 -51(5) . . . . ? C59 N9 C61 C62 72(4) . . . . ? Cu4 N9 C61 C62 -173(3) . . . . ? N9 C61 C62 C67 -84(5) . . . . ? N9 C61 C62 C63 98(5) . . . . ? C67 C62 C63 C64 2(7) . . . . ? C61 C62 C63 C64 179(4) . . . . ? C62 C63 C64 C65 2(7) . . . . ? C62 C63 C64 C68 -180(4) . . . . ? C63 C64 C65 C66 -4(8) . . . . ? C68 C64 C65 C66 178(5) . . . . ? C64 C65 C66 C67 2(8) . . . . ? C63 C62 C67 C66 -3(7) . . . . ? C61 C62 C67 C66 179(5) . . . . ? C65 C66 C67 C62 1(8) . . . . ? C70 N10 C68 C64 59(5) . . . . ? C69 N10 C68 C64 179(4) . . . . ? Cu3 N10 C68 C64 -66(5) . . . . ? C63 C64 C68 N10 78(6) . . . . ? C65 C64 C68 N10 -103(5) . . . . ? C68 N10 C70 C71 -104(4) . . . . ? C69 N10 C70 C71 142(4) . . . . ? Cu3 N10 C70 C71 27(4) . . . . ? C72 N11 C71 C70 -73(5) . . . . ? C73 N11 C71 C70 168(4) . . . . ? Cu3 N11 C71 C70 51(4) . . . . ? N10 C70 C71 N11 -53(5) . . . . ? C72 N11 C73 C74 144(4) . . . . ? C71 N11 C73 C74 -98(5) . . . . ? Cu3 N11 C73 C74 15(5) . . . . ? N11 C73 C74 N12 -49(5) . . . . ? C76 N12 C74 C73 174(4) . . . . ? C75 N12 C74 C73 -63(5) . . . . ? Cu3 N12 C74 C73 55(4) . . . . ? C75 N12 C76 C77 -64(5) . . . . ? C74 N12 C76 C77 62(5) . . . . ? Cu3 N12 C76 C77 173(3) . . . . ? N12 C76 C77 C78 -92(5) . . . . ? N12 C76 C77 C82 93(6) . . . . ? C82 C77 C78 C79 5(7) . . . . ? C76 C77 C78 C79 -170(5) . . . . ? C77 C78 C79 C80 -7(8) . . . . ? C77 C78 C79 C53 174(5) . . . . ? N7 C53 C79 C80 96(6) . . . . ? N7 C53 C79 C78 -84(6) . . . . ? C78 C79 C80 C81 5(8) . . . . ? C53 C79 C80 C81 -175(6) . . . . ? C79 C80 C81 C82 -3(10) . . . . ? C80 C81 C82 C77 0(10) . . . . ? C78 C77 C82 C81 -2(8) . . . . ? C76 C77 C82 C81 173(5) . . . . ? Cu2 O6 C83 O7 6(6) . . . . ? Cu2 O6 C83 C84 -177(4) . . . . ? O6 Cu2 C83 O7 -175(5) . . . . ? N5 Cu2 C83 O7 11(5) . . . . ? N6 Cu2 C83 O7 99(3) . . . . ? N4 Cu2 C83 O7 -90(3) . . . . ? N5 Cu2 C83 O6 -174(3) . . . . ? N6 Cu2 C83 O6 -86(3) . . . . ? N4 Cu2 C83 O6 85(3) . . . . ? O6 Cu2 C83 C84 11(12) . . . . ? N5 Cu2 C83 C84 -163(13) . . . . ? N6 Cu2 C83 C84 -75(14) . . . . ? N4 Cu2 C83 C84 96(14) . . . . ? O7 C83 C84 C85 169(5) . . . . ? O6 C83 C84 C85 -9(7) . . . . ? Cu2 C83 C84 C85 -18(16) . . . . ? O7 C83 C84 C93 -10(8) . . . . ? O6 C83 C84 C93 173(5) . . . . ? Cu2 C83 C84 C93 164(11) . . . . ? C93 C84 C85 C86 4(7) . . . . ? C83 C84 C85 C86 -175(4) . . . . ? C84 C85 C86 C87 174(5) . . . . ? C84 C85 C86 C91 -2(6) . . . . ? C85 C86 C87 C88 -172(4) . . . . ? C91 C86 C87 C88 3(7) . . . . ? C86 C87 C88 C89 -3(7) . . . . ? C87 C88 C89 C90 2(7) . . . . ? C87 C88 C89 C94 175(4) . . . . ? C88 C89 C90 C91 -1(6) . . . . ? C94 C89 C90 C91 -175(4) . . . . ? C89 C90 C91 C92 177(4) . . . . ? C89 C90 C91 C86 2(6) . . . . ? C87 C86 C91 C92 -178(4) . . . . ? C85 C86 C91 C92 -2(6) . . . . ? C87 C86 C91 C90 -3(6) . . . . ? C85 C86 C91 C90 173(4) . . . . ? C90 C91 C92 C93 -171(5) . . . . ? C86 C91 C92 C93 5(7) . . . . ? C91 C92 C93 C84 -2(7) . . . . ? C85 C84 C93 C92 -2(8) . . . . ? C83 C84 C93 C92 177(5) . . . . ? Cu3 O10 C94 O9 0(7) . . . . ? Cu3 O10 C94 C89 -180(3) . . . . ? C90 C89 C94 O9 179(5) . . . . ? C88 C89 C94 O9 6(7) . . . . ? C90 C89 C94 O10 0(6) . . . . ? C88 C89 C94 O10 -174(4) . . . . ? O1A S1A C1A F2A -59(5) . . . . ? O2A S1A C1A F2A -178(4) . . . . ? O3A S1A C1A F2A 60(5) . . . . ? O1A S1A C1A F3A 179(4) . . . . ? O2A S1A C1A F3A 60(5) . . . . ? O3A S1A C1A F3A -62(5) . . . . ? O1A S1A C1A F1A 60(5) . . . . ? O2A S1A C1A F1A -59(5) . . . . ? O3A S1A C1A F1A 179(4) . . . . ? O1B S1B C1B F3B -166(10) . . . . ? O2B S1B C1B F3B -41(10) . . . . ? O3B S1B C1B F3B 77(10) . . . . ? O1B S1B C1B F1B 60(7) . . . . ? O2B S1B C1B F1B -176(6) . . . . ? O3B S1B C1B F1B -57(7) . . . . ? O1B S1B C1B F2B -47(8) . . . . ? O2B S1B C1B F2B 78(7) . . . . ? O3B S1B C1B F2B -164(7) . . . . ? O3D S1D C1D F2D 53(13) . . . . ? O1D S1D C1D F2D -66(12) . . . . ? O2D S1D C1D F2D 177(11) . . . . ? O3D S1D C1D F3D -65(9) . . . . ? O1D S1D C1D F3D 176(7) . . . . ? O2D S1D C1D F3D 59(8) . . . . ? O3D S1D C1D F1D -166(7) . . . . ? O1D S1D C1D F1D 75(7) . . . . ? O2D S1D C1D F1D -42(8) . . . . ? O2C S1C C1C F2C 54(7) . . . . ? O1C S1C C1C F2C -70(7) . . . . ? O3C S1C C1C F2C 170(6) . . . . ? O2C S1C C1C F1C -174(5) . . . . ? O1C S1C C1C F1C 62(6) . . . . ? O3C S1C C1C F1C -57(6) . . . . ? O2C S1C C1C F3C -59(6) . . . . ? O1C S1C C1C F3C 176(5) . . . . ? O3C S1C C1C F3C 57(6) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.55 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.878 _refine_diff_density_min -1.167 _refine_diff_density_rms 0.160 #===END