# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2009 data_global _journal_name_full 'New J. Chem.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Pei Yu' _publ_contact_author_email YUPEI@ICMO.U-PSUD.FR _publ_section_title ; Photo-controlled release and uptake of Cu(hfac)2 in a binuclear copper complex with a photochromic dithiazolylethene bridging ligand ; loop_ _publ_author_name 'Pei Yu' 'Pierre Dorlet' 'Marion Giraud' 'Regis Guillot' 'Anne Leaustic' 'R Metivier' ; K.Nakatani ; # Attachment 'B901201J_CIFS.cif' data_(hfac)2Cu-1o-Cu(hfac)2 _database_code_depnum_ccdc_archive 'CCDC 715795' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C43 H18 Cu2 F30 N4 O8 S2' _chemical_formula_sum 'C43 H18 Cu2 F30 N4 O8 S2' _chemical_melting_point ? _exptl_crystal_description cube _exptl_crystal_colour green _diffrn_ambient_temperature 150(1) _chemical_formula_weight 1479.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0031 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 0.0109 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0176 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1250 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3221 1.2697 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n' _symmetry_int_tables_number 86 _chemical_absolute_configuration . loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 17.879(8) _cell_length_b 17.879(8) _cell_length_c 17.607(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5628(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 3010 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 23.15 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912 _exptl_absorpt_coefficient_mu 0.982 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.781 _exptl_absorpt_correction_T_max 0.801 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Nonius kappa CCD' _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 113444 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 31.46 _reflns_number_total 8920 _reflns_number_gt 6423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis RED' _computing_data_reduction 'CrysAlis RED' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 8920 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.1034 _refine_ls_wR_factor_ref 0.0729 _refine_ls_wR_factor_gt 0.1000 _refine_ls_goodness_of_fit_ref 1.222 _refine_ls_restrained_S_all 1.222 _refine_ls_shift/su_max 0.004 _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 C1 C 0.8575(2) 0.23903(18) 0.5641(2) 0.0404(8) Uani 1 1 d . . . C3 C 0.8518(3) 0.3216(2) 0.5794(3) 0.0562(12) Uani 1 1 d . . . H3A H 0.8410 0.3475 0.5329 0.084 Uiso 1 1 calc R . . H3B H 0.8983 0.3394 0.5998 0.084 Uiso 1 1 calc R . . H3C H 0.8124 0.3307 0.6154 0.084 Uiso 1 1 calc R . . C4 C 0.82394(19) 0.19728(17) 0.50826(19) 0.0302(6) Uani 1 1 d . . . C5 C 0.88930(18) 0.10656(17) 0.56192(18) 0.0309(6) Uani 1 1 d . . . C6 C 0.91867(17) 0.03070(17) 0.57148(18) 0.0298(6) Uani 1 1 d . . . C7 C 0.98430(19) 0.01533(19) 0.6107(2) 0.0351(7) Uani 1 1 d . . . H7 H 1.0104 0.0532 0.6355 0.042 Uiso 1 1 calc R . . C8 C 1.01024(19) -0.05859(19) 0.6120(2) 0.0380(7) Uani 1 1 d . . . H8 H 1.0541 -0.0705 0.6377 0.046 Uiso 1 1 calc R . . C9 C 0.9705(2) -0.11342(18) 0.5751(2) 0.0379(7) Uani 1 1 d . . . H9 H 0.9873 -0.1626 0.5748 0.045 Uiso 1 1 calc R . . C10 C 0.9043(2) -0.09385(18) 0.5379(2) 0.0382(7) Uani 1 1 d . . . H10 H 0.8768 -0.1310 0.5137 0.046 Uiso 1 1 calc R . . C11 C 0.77937(17) 0.22638(16) 0.44492(18) 0.0295(6) Uani 1 1 d . . . C12 C 0.8037(2) 0.20906(18) 0.3652(2) 0.0363(7) Uani 1 1 d . . . C13 C 0.7659(5) 0.2635(4) 0.3143(4) 0.0367(17) Uani 0.50 1 d P . . C14 C 0.5804(2) 0.0459(3) 0.3688(3) 0.0527(10) Uani 1 1 d . . . C15 C 0.6628(2) 0.0259(2) 0.3824(2) 0.0385(7) Uani 1 1 d . . . C16 C 0.7015(2) -0.0108(2) 0.3241(2) 0.0404(8) Uani 1 1 d . . . H16 H 0.6761 -0.0239 0.2800 0.049 Uiso 1 1 calc R . . C17 C 0.7758(2) -0.0280(2) 0.3305(2) 0.0369(7) Uani 1 1 d . . . C18 C 0.8158(3) -0.0585(3) 0.2603(3) 0.0557(11) Uani 1 1 d . . . C19 C 0.6289(6) -0.1931(4) 0.5068(6) 0.111(3) Uani 1 1 d . . . C20 C 0.6786(3) -0.1264(2) 0.5320(3) 0.0564(11) Uani 1 1 d . . . C21 C 0.6625(4) -0.0930(3) 0.6011(3) 0.0753(17) Uani 1 1 d . . . H21 H 0.6265 -0.1150 0.6320 0.090 Uiso 1 1 calc R . . C22 C 0.6977(3) -0.0277(2) 0.6268(3) 0.0571(12) Uani 1 1 d . . . C23 C 0.6810(6) -0.0030(4) 0.7085(4) 0.101(3) Uani 1 1 d . . . N1 N 0.87927(15) -0.02338(15) 0.53596(17) 0.0324(6) Uani 1 1 d . . . N2 N 0.84197(15) 0.12214(14) 0.50803(15) 0.0283(5) Uani 1 1 d . . . O1 O 0.68633(14) 0.04241(14) 0.44689(15) 0.0381(5) Uani 1 1 d . . . O2 O 0.81888(13) -0.02059(13) 0.38717(14) 0.0353(5) Uani 1 1 d . . . O3 O 0.72531(17) -0.10910(15) 0.48608(16) 0.0445(6) Uani 1 1 d . . . O4 O 0.74089(15) 0.01609(15) 0.59264(15) 0.0412(6) Uani 1 1 d . . . F1 F 0.8029(2) 0.13717(13) 0.34794(14) 0.0673(9) Uani 1 1 d . . . F2 F 0.8734(2) 0.2312(3) 0.3537(2) 0.1184(19) Uani 1 1 d . . . F3 F 0.7458(7) 0.2323(3) 0.2483(3) 0.067(3) Uani 0.50 1 d P . . F4 F 0.8101(3) 0.3226(2) 0.2986(3) 0.0506(11) Uani 0.50 1 d P . . F5 F 0.56454(18) 0.1116(2) 0.3982(2) 0.0855(11) Uani 1 1 d . . . F6 F 0.53634(18) -0.0024(3) 0.4011(3) 0.1059(14) Uani 1 1 d . . . F7 F 0.56244(19) 0.0492(3) 0.2962(2) 0.0964(13) Uani 1 1 d . . . F8 F 0.77380(19) -0.0746(3) 0.2049(2) 0.1047(15) Uani 1 1 d . . . F9 F 0.8622(4) -0.0074(4) 0.2338(3) 0.158(3) Uani 1 1 d . . . F10 F 0.8597(4) -0.1124(4) 0.2759(3) 0.161(3) Uani 1 1 d . . . F11 F 0.6569(3) -0.2374(2) 0.4624(3) 0.1066(15) Uani 1 1 d . . . F12 F 0.5702(4) -0.1669(5) 0.4641(7) 0.220(6) Uani 1 1 d . . . F13 F 0.5873(4) -0.2183(3) 0.5602(4) 0.171(3) Uani 1 1 d . . . F14 F 0.7359(8) -0.0083(6) 0.7501(4) 0.257(7) Uani 1 1 d . . . F15 F 0.6350(8) -0.0499(4) 0.7434(4) 0.230(5) Uani 1 1 d . . . F16 F 0.6551(4) 0.0609(3) 0.7147(2) 0.135(2) Uani 1 1 d . . . S S 0.91398(6) 0.18140(5) 0.61754(6) 0.0436(3) Uani 1 1 d . . . Cu Cu 0.78064(2) 0.00423(2) 0.48866(3) 0.03061(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0493(19) 0.0270(14) 0.045(2) 0.0005(13) -0.0128(15) 0.0041(13) C3 0.077(3) 0.0269(16) 0.064(3) -0.0063(16) -0.027(2) 0.0075(17) C4 0.0327(15) 0.0223(13) 0.0354(16) -0.0019(11) 0.0009(12) 0.0029(11) C5 0.0341(15) 0.0275(13) 0.0310(15) -0.0016(11) -0.0011(12) 0.0020(11) C6 0.0327(14) 0.0251(13) 0.0316(15) 0.0027(11) -0.0009(12) 0.0012(10) C7 0.0344(15) 0.0323(15) 0.0386(17) 0.0035(13) -0.0052(13) 0.0007(12) C8 0.0325(15) 0.0344(16) 0.047(2) 0.0111(14) -0.0010(13) 0.0034(12) C9 0.0393(17) 0.0279(14) 0.046(2) 0.0110(13) 0.0058(14) 0.0056(12) C10 0.0378(17) 0.0264(14) 0.050(2) 0.0041(14) -0.0019(15) 0.0014(12) C11 0.0340(15) 0.0223(12) 0.0320(15) -0.0016(11) -0.0005(12) 0.0019(11) C12 0.0426(17) 0.0280(14) 0.0383(17) 0.0013(12) 0.0062(14) 0.0069(12) C13 0.054(6) 0.030(4) 0.027(3) 0.003(2) -0.003(3) 0.008(3) C14 0.0386(19) 0.061(3) 0.059(3) -0.010(2) -0.0101(18) 0.0113(17) C15 0.0344(16) 0.0376(17) 0.0436(19) -0.0065(14) -0.0034(14) 0.0015(13) C16 0.0421(18) 0.0412(18) 0.0380(18) -0.0100(14) -0.0046(15) 0.0004(14) C17 0.0411(18) 0.0337(16) 0.0359(17) -0.0061(13) 0.0029(13) -0.0012(13) C18 0.049(2) 0.071(3) 0.047(2) -0.010(2) 0.0006(18) 0.002(2) C19 0.104(6) 0.064(4) 0.166(9) -0.032(5) 0.056(6) -0.034(4) C20 0.067(3) 0.0350(19) 0.068(3) -0.0077(19) 0.018(2) -0.0090(18) C21 0.103(4) 0.051(3) 0.072(3) 0.001(2) 0.046(3) -0.010(3) C22 0.087(3) 0.042(2) 0.042(2) 0.0030(17) 0.022(2) 0.010(2) C23 0.181(8) 0.078(4) 0.045(3) 0.012(3) 0.045(4) 0.031(4) N1 0.0340(13) 0.0262(12) 0.0369(14) 0.0040(10) -0.0002(11) 0.0020(10) N2 0.0293(13) 0.0229(11) 0.0327(13) 0.0001(9) -0.0002(10) 0.0040(10) O1 0.0364(12) 0.0363(12) 0.0415(14) -0.0103(10) -0.0003(10) 0.0048(9) O2 0.0342(11) 0.0347(11) 0.0370(12) -0.0025(9) 0.0005(9) 0.0017(9) O3 0.0505(16) 0.0316(13) 0.0513(16) -0.0066(10) 0.0079(12) -0.0077(11) O4 0.0453(14) 0.0415(13) 0.0369(13) -0.0062(10) 0.0000(11) 0.0014(11) F1 0.136(3) 0.0288(11) 0.0373(12) -0.0082(9) 0.0052(15) 0.0094(13) F2 0.087(2) 0.200(5) 0.068(2) -0.044(3) 0.043(2) -0.078(3) F3 0.090(4) 0.074(6) 0.037(2) -0.014(2) -0.021(3) 0.041(6) F4 0.058(3) 0.040(2) 0.055(3) 0.019(2) 0.016(2) 0.010(2) F5 0.0584(18) 0.084(2) 0.114(3) -0.027(2) -0.0215(18) 0.0337(16) F6 0.0446(16) 0.111(3) 0.162(4) 0.033(3) -0.002(2) -0.0125(18) F7 0.0646(19) 0.148(3) 0.076(2) -0.022(2) -0.0328(17) 0.042(2) F8 0.075(2) 0.173(4) 0.065(2) -0.068(3) -0.0034(17) 0.016(2) F9 0.166(5) 0.187(5) 0.120(4) -0.057(4) 0.101(4) -0.079(4) F10 0.203(6) 0.203(6) 0.078(3) -0.041(3) 0.003(3) 0.148(5) F11 0.115(3) 0.0564(19) 0.148(4) -0.042(2) 0.031(3) -0.027(2) F12 0.113(5) 0.166(7) 0.380(16) -0.113(9) -0.068(7) -0.025(4) F13 0.196(6) 0.121(4) 0.195(7) -0.018(4) 0.085(6) -0.103(5) F14 0.395(14) 0.307(11) 0.069(3) -0.080(5) -0.099(6) 0.236(11) F15 0.446(15) 0.131(5) 0.112(5) -0.018(4) 0.159(8) -0.067(7) F16 0.255(6) 0.095(3) 0.056(2) -0.0075(19) 0.039(3) 0.087(3) S 0.0559(6) 0.0294(4) 0.0456(5) -0.0037(3) -0.0200(4) 0.0040(3) Cu 0.0308(3) 0.0282(2) 0.0328(3) -0.00262(14) -0.00085(14) 0.00181(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C4 1.372(5) . ? C1 C3 1.505(5) . ? C1 S 1.723(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 N2 1.382(4) . ? C4 C11 1.466(5) . ? C5 N2 1.301(4) . ? C5 C6 1.464(4) . ? C5 S 1.716(3) . ? C6 N1 1.350(4) . ? C6 C7 1.389(5) . ? C7 C8 1.401(5) . ? C7 H7 0.9300 . ? C8 C9 1.374(5) . ? C8 H8 0.9300 . ? C9 C10 1.396(5) . ? C9 H9 0.9300 . ? C10 N1 1.338(4) . ? C10 H10 0.9300 . ? C11 C11 1.348(6) 2_655 ? C11 C12 1.502(5) . ? C12 F1 1.321(4) . ? C12 F2 1.324(5) . ? C12 C13 1.486(8) . ? C12 C13 1.610(9) 2_655 ? C13 C13 0.745(13) 2_655 ? C13 F3 1.182(9) 2_655 ? C13 F3 1.337(8) . ? C13 F4 1.349(8) . ? C13 C12 1.610(9) 2_655 ? C14 F6 1.299(6) . ? C14 F5 1.314(6) . ? C14 F7 1.321(6) . ? C14 C15 1.535(5) . ? C15 O1 1.247(5) . ? C15 C16 1.401(5) . ? C16 C17 1.368(5) . ? C16 H16 0.9300 . ? C17 O2 1.268(4) . ? C17 C18 1.528(6) . ? C18 F8 1.265(6) . ? C18 F10 1.273(7) . ? C18 F9 1.319(7) . ? C19 F11 1.219(9) . ? C19 F13 1.281(10) . ? C19 F12 1.374(14) . ? C19 C20 1.553(9) . ? C20 O3 1.202(5) . ? C20 C21 1.386(7) . ? C21 C22 1.401(8) . ? C21 H21 0.9300 . ? C22 O4 1.252(6) . ? C22 C23 1.534(7) . ? C23 F14 1.229(13) . ? C23 F16 1.237(7) . ? C23 F15 1.325(11) . ? N1 Cu 2.012(3) . ? N2 Cu 2.401(3) . ? O1 Cu 1.962(3) . ? O2 Cu 1.964(3) . ? O3 Cu 2.255(3) . ? O4 Cu 1.975(3) . ? F3 F3 0.652(15) 2_655 ? F3 C13 1.182(9) 2_655 ? F3 F4 1.657(13) 2_655 ? F4 F3 1.657(13) 2_655 ? 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 C4 C1 C3 129.3(3) . . ? C4 C1 S 108.8(2) . . ? C3 C1 S 121.9(3) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 N2 115.4(3) . . ? C1 C4 C11 126.1(3) . . ? N2 C4 C11 118.0(3) . . ? N2 C5 C6 121.0(3) . . ? N2 C5 S 114.6(2) . . ? C6 C5 S 124.4(2) . . ? N1 C6 C7 122.0(3) . . ? N1 C6 C5 115.0(3) . . ? C7 C6 C5 122.9(3) . . ? C6 C7 C8 118.3(3) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C9 C8 C7 119.6(3) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 118.8(3) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N1 C10 C9 122.1(3) . . ? N1 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C4 C11 C12 118.7(3) . . ? F1 C12 F2 105.4(4) . . ? F1 C12 C13 119.6(4) . . ? F2 C12 C13 98.1(4) . . ? F1 C12 C11 114.4(3) . . ? F2 C12 C11 110.7(3) . . ? C13 C12 C11 107.3(4) . . ? F3 C13 F4 107.9(7) . . ? F3 C13 C12 111.9(6) . . ? F4 C13 C12 111.7(6) . . ? F6 C14 F5 107.0(4) . . ? F6 C14 F7 107.9(4) . . ? F5 C14 F7 106.7(4) . . ? F6 C14 C15 111.0(4) . . ? F5 C14 C15 110.7(4) . . ? F7 C14 C15 113.2(4) . . ? O1 C15 C16 127.6(3) . . ? O1 C15 C14 114.2(3) . . ? C16 C15 C14 118.1(3) . . ? C17 C16 C15 121.7(3) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? O2 C17 C16 129.1(3) . . ? O2 C17 C18 113.0(3) . . ? C16 C17 C18 117.9(3) . . ? F8 C18 F10 111.1(5) . . ? F8 C18 F9 105.0(5) . . ? F10 C18 F9 102.2(6) . . ? F8 C18 C17 115.3(4) . . ? F10 C18 C17 112.6(4) . . ? F9 C18 C17 109.4(4) . . ? F11 C19 F13 118.7(7) . . ? F11 C19 F12 100.6(10) . . ? F13 C19 F12 94.4(8) . . ? F11 C19 C20 116.6(6) . . ? F13 C19 C20 113.1(8) . . ? F12 C19 C20 109.3(7) . . ? O3 C20 C21 128.6(4) . . ? O3 C20 C19 113.8(5) . . ? C21 C20 C19 117.6(5) . . ? C20 C21 C22 123.3(4) . . ? C20 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? O4 C22 C21 130.0(4) . . ? O4 C22 C23 113.0(5) . . ? C21 C22 C23 117.0(5) . . ? F14 C23 F16 108.5(9) . . ? F14 C23 F15 99.8(8) . . ? F16 C23 F15 108.1(8) . . ? F14 C23 C22 112.4(7) . . ? F16 C23 C22 114.9(5) . . ? F15 C23 C22 112.0(7) . . ? C10 N1 C6 119.2(3) . . ? C10 N1 Cu 122.4(2) . . ? C6 N1 Cu 118.3(2) . . ? C5 N2 C4 111.0(3) . . ? C5 N2 Cu 102.27(19) . . ? C4 N2 Cu 138.4(2) . . ? C15 O1 Cu 123.3(2) . . ? C17 O2 Cu 121.9(2) . . ? C20 O3 Cu 121.5(3) . . ? C22 O4 Cu 126.8(3) . . ? C5 S C1 90.21(16) . . ? O1 Cu O2 92.10(11) . . ? O1 Cu O4 90.05(11) . . ? O2 Cu O4 173.10(11) . . ? O1 Cu N1 173.64(11) . . ? O2 Cu N1 90.92(11) . . ? O4 Cu N1 87.60(12) . . ? O1 Cu O3 85.87(11) . . ? O2 Cu O3 86.06(10) . . ? O4 Cu O3 87.56(11) . . ? N1 Cu O3 99.93(11) . . ? O1 Cu N2 98.06(10) . . ? O2 Cu N2 99.71(10) . . ? O4 Cu N2 86.47(10) . . ? N1 Cu N2 75.89(10) . . ? O3 Cu N2 172.84(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 C3 C1 C4 N2 178.4(4) . . . . ? S C1 C4 N2 0.4(4) . . . . ? C3 C1 C4 C11 6.5(7) . . . . ? S C1 C4 C11 -171.6(3) . . . . ? N2 C5 C6 N1 -17.2(5) . . . . ? S C5 C6 N1 163.8(3) . . . . ? N2 C5 C6 C7 159.5(3) . . . . ? S C5 C6 C7 -19.4(5) . . . . ? N1 C6 C7 C8 0.9(5) . . . . ? C5 C6 C7 C8 -175.6(3) . . . . ? C6 C7 C8 C9 -0.2(5) . . . . ? C7 C8 C9 C10 -0.9(5) . . . . ? C8 C9 C10 N1 1.3(6) . . . . ? C1 C4 C11 C11 -51.8(6) . . . 2_655 ? N2 C4 C11 C11 136.4(4) . . . 2_655 ? C1 C4 C11 C12 121.7(4) . . . . ? N2 C4 C11 C12 -50.1(4) . . . . ? C11 C11 C12 F1 -122.3(4) 2_655 . . . ? C4 C11 C12 F1 63.0(4) . . . . ? C11 C11 C12 F2 118.8(5) 2_655 . . . ? C4 C11 C12 F2 -55.9(5) . . . . ? C11 C11 C12 C13 12.8(5) 2_655 . . . ? C4 C11 C12 C13 -161.9(4) . . . . ? C11 C11 C12 C13 -15.4(5) 2_655 . . 2_655 ? C4 C11 C12 C13 169.9(3) . . . 2_655 ? F1 C12 C13 C13 46.2(10) . . . 2_655 ? F2 C12 C13 C13 159.2(8) . . . 2_655 ? C11 C12 C13 C13 -86.1(8) . . . 2_655 ? F1 C12 C13 F3 -31.5(14) . . . 2_655 ? F2 C12 C13 F3 81.4(12) . . . 2_655 ? C11 C12 C13 F3 -163.9(11) . . . 2_655 ? C13 C12 C13 F3 -77.8(12) 2_655 . . 2_655 ? F1 C12 C13 F3 -10.8(9) . . . . ? F2 C12 C13 F3 102.1(8) . . . . ? C11 C12 C13 F3 -143.2(7) . . . . ? C13 C12 C13 F3 -57.1(9) 2_655 . . . ? F1 C12 C13 F4 -131.9(5) . . . . ? F2 C12 C13 F4 -19.0(6) . . . . ? C11 C12 C13 F4 95.7(6) . . . . ? C13 C12 C13 F4 -178.2(12) 2_655 . . . ? F1 C12 C13 C12 111.4(5) . . . 2_655 ? F2 C12 C13 C12 -135.6(4) . . . 2_655 ? C11 C12 C13 C12 -20.9(4) . . . 2_655 ? C13 C12 C13 C12 65.2(8) 2_655 . . 2_655 ? F6 C14 C15 O1 -77.5(5) . . . . ? F5 C14 C15 O1 41.1(6) . . . . ? F7 C14 C15 O1 160.9(4) . . . . ? F6 C14 C15 C16 99.8(5) . . . . ? F5 C14 C15 C16 -141.5(4) . . . . ? F7 C14 C15 C16 -21.7(6) . . . . ? O1 C15 C16 C17 -5.7(7) . . . . ? C14 C15 C16 C17 177.4(4) . . . . ? C15 C16 C17 O2 6.1(7) . . . . ? C15 C16 C17 C18 -172.0(4) . . . . ? O2 C17 C18 F8 172.5(4) . . . . ? C16 C17 C18 F8 -9.1(7) . . . . ? O2 C17 C18 F10 43.6(6) . . . . ? C16 C17 C18 F10 -138.0(6) . . . . ? O2 C17 C18 F9 -69.4(6) . . . . ? C16 C17 C18 F9 109.0(5) . . . . ? F11 C19 C20 O3 27.1(13) . . . . ? F13 C19 C20 O3 170.0(8) . . . . ? F12 C19 C20 O3 -86.2(9) . . . . ? F11 C19 C20 C21 -155.3(9) . . . . ? F13 C19 C20 C21 -12.3(13) . . . . ? F12 C19 C20 C21 91.4(10) . . . . ? O3 C20 C21 C22 4.1(11) . . . . ? C19 C20 C21 C22 -173.1(7) . . . . ? C20 C21 C22 O4 8.9(11) . . . . ? C20 C21 C22 C23 -172.7(6) . . . . ? O4 C22 C23 F14 -68.9(10) . . . . ? C21 C22 C23 F14 112.4(10) . . . . ? O4 C22 C23 F16 55.8(10) . . . . ? C21 C22 C23 F16 -122.8(9) . . . . ? O4 C22 C23 F15 179.7(8) . . . . ? C21 C22 C23 F15 1.0(11) . . . . ? C9 C10 N1 C6 -0.5(6) . . . . ? C9 C10 N1 Cu -175.8(3) . . . . ? C7 C6 N1 C10 -0.6(5) . . . . ? C5 C6 N1 C10 176.2(3) . . . . ? C7 C6 N1 Cu 174.9(3) . . . . ? C5 C6 N1 Cu -8.4(4) . . . . ? C6 C5 N2 C4 -178.0(3) . . . . ? S C5 N2 C4 1.1(4) . . . . ? C6 C5 N2 Cu 27.5(3) . . . . ? S C5 N2 Cu -153.46(17) . . . . ? C1 C4 N2 C5 -0.9(4) . . . . ? C11 C4 N2 C5 171.7(3) . . . . ? C1 C4 N2 Cu 139.8(3) . . . . ? C11 C4 N2 Cu -47.5(5) . . . . ? C16 C15 O1 Cu -11.2(6) . . . . ? C14 C15 O1 Cu 165.8(3) . . . . ? C16 C17 O2 Cu 10.4(5) . . . . ? C18 C17 O2 Cu -171.5(3) . . . . ? C21 C20 O3 Cu -16.5(8) . . . . ? C19 C20 O3 Cu 160.8(5) . . . . ? C21 C22 O4 Cu -4.3(8) . . . . ? C23 C22 O4 Cu 177.3(4) . . . . ? C13 C13 F3 F3 138(3) 2_655 . . 2_655 ? F4 C13 F3 F3 -26(2) . . . 2_655 ? C12 C13 F3 F3 -150(2) . . . 2_655 ? C12 C13 F3 F3 95(2) 2_655 . . 2_655 ? F3 C13 F3 C13 -138(3) 2_655 . . 2_655 ? F4 C13 F3 C13 -164.8(18) . . . 2_655 ? C12 C13 F3 C13 71.9(11) . . . 2_655 ? C12 C13 F3 C13 -43.6(11) 2_655 . . 2_655 ? C13 C13 F3 F4 -8.6(13) 2_655 . . 2_655 ? F3 C13 F3 F4 -147(2) 2_655 . . 2_655 ? F4 C13 F3 F4 -173.3(6) . . . 2_655 ? C12 C13 F3 F4 63.4(7) . . . 2_655 ? C12 C13 F3 F4 -52.1(5) 2_655 . . 2_655 ? C13 C13 F4 F3 -38(4) 2_655 . . 2_655 ? F3 C13 F4 F3 12.6(9) . . . 2_655 ? C12 C13 F4 F3 136.0(9) . . . 2_655 ? C12 C13 F4 F3 -111.5(8) 2_655 . . 2_655 ? N2 C5 S C1 -0.7(3) . . . . ? C6 C5 S C1 178.3(3) . . . . ? C4 C1 S C5 0.2(3) . . . . ? C3 C1 S C5 -178.1(4) . . . . ? C15 O1 Cu O2 20.0(3) . . . . ? C15 O1 Cu O4 -153.5(3) . . . . ? C15 O1 Cu O3 -65.9(3) . . . . ? C15 O1 Cu N2 120.1(3) . . . . ? C17 O2 Cu O1 -19.4(3) . . . . ? C17 O2 Cu N1 166.2(3) . . . . ? C17 O2 Cu O3 66.3(3) . . . . ? C17 O2 Cu N2 -117.9(3) . . . . ? C22 O4 Cu O1 80.5(4) . . . . ? C22 O4 Cu N1 -105.4(4) . . . . ? C22 O4 Cu O3 -5.4(4) . . . . ? C22 O4 Cu N2 178.5(4) . . . . ? C10 N1 Cu O2 -68.1(3) . . . . ? C6 N1 Cu O2 116.6(2) . . . . ? C10 N1 Cu O4 105.1(3) . . . . ? C6 N1 Cu O4 -70.2(3) . . . . ? C10 N1 Cu O3 18.0(3) . . . . ? C6 N1 Cu O3 -157.3(2) . . . . ? C10 N1 Cu N2 -167.9(3) . . . . ? C6 N1 Cu N2 16.8(2) . . . . ? C20 O3 Cu O1 -75.1(4) . . . . ? C20 O3 Cu O2 -167.5(4) . . . . ? C20 O3 Cu O4 15.1(4) . . . . ? C20 O3 Cu N1 102.2(4) . . . . ? C5 N2 Cu O1 155.0(2) . . . . ? C4 N2 Cu O1 12.2(3) . . . . ? C5 N2 Cu O2 -111.5(2) . . . . ? C4 N2 Cu O2 105.7(3) . . . . ? C5 N2 Cu O4 65.4(2) . . . . ? C4 N2 Cu O4 -77.4(3) . . . . ? C5 N2 Cu N1 -23.0(2) . . . . ? C4 N2 Cu N1 -165.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.180 _refine_diff_density_min -0.897 _refine_diff_density_rms 0.186 data_(hfac)2Cu-1c-Cu(hfac)2 _database_code_depnum_ccdc_archive 'CCDC 715796' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H18 Cu2 F30 N4 O8 S2' _chemical_formula_sum 'C43 H18 Cu2 F30 N4 O8 S2' _chemical_formula_weight 1479.85 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.699(5) _cell_length_b 17.418(5) _cell_length_c 17.916(5) _cell_angle_alpha 90. _cell_angle_beta 106.609(5) _cell_angle_gamma 90. _cell_volume 5293(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 8777 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 30.48 _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.857 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912 _exptl_absorpt_coefficient_mu 1.044 _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(1) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'X8 APEX II Bruker' _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 86102 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 30.63 _reflns_number_total 12886 _reflns_number_gt 11090 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The C1-C2 bond is disordered over two orientations. Occupancies were constrained to add to unity and were fixed after convergence to 0.6912(10)(A) and 0.3088(10)(B). New cif file and ORTEP view were generated. ; _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^)+(0.1038P)^2^+16.9688P] 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 12883 _refine_ls_number_parameters 861 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1926 _refine_ls_wR_factor_gt 0.1812 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.002 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 C1A C 0.6966(3) 0.3057(3) 0.6887(3) 0.0242(10) Uani 0.6912(10) 1 d P A 1 C2A C 0.7467(3) 0.3740(3) 0.7226(3) 0.0234(10) Uani 0.6912(10) 1 d P A 1 C3A C 0.7352(5) 0.2524(4) 0.6394(4) 0.0308(12) Uani 0.6912(10) 1 d P A 1 H3A1 H 0.7394 0.2797 0.5942 0.046 Uiso 0.6912(10) 1 calc PR A 1 H3A2 H 0.7032 0.2075 0.6235 0.046 Uiso 0.6912(10) 1 calc PR A 1 H3A3 H 0.7869 0.2373 0.6703 0.046 Uiso 0.6912(10) 1 calc PR A 1 S1A S 0.5995(4) 0.3261(4) 0.6248(4) 0.0204(8) Uani 0.6912(10) 1 d P A 1 S2A S 0.7870(4) 0.4287(3) 0.6572(4) 0.0190(7) Uani 0.6912(10) 1 d P A 1 C43A C 0.7033(4) 0.4317(3) 0.7623(4) 0.0270(11) Uani 0.6912(10) 1 d P A 1 H43A H 0.6595 0.4538 0.7238 0.041 Uiso 0.6912(10) 1 calc PR A 1 H43B H 0.7392 0.4716 0.7872 0.041 Uiso 0.6912(10) 1 calc PR A 1 H43C H 0.6846 0.4053 0.8006 0.041 Uiso 0.6912(10) 1 calc PR A 1 C1B C 0.6839(6) 0.3403(5) 0.7161(6) 0.0140(17) Uani 0.3088(10) 1 d P A 2 C2B C 0.7613(6) 0.3401(6) 0.7021(6) 0.0133(17) Uani 0.3088(10) 1 d P A 2 C3B C 0.7720(8) 0.2674(8) 0.6482(7) 0.022(2) Uani 0.3088(10) 1 d P A 2 H3B1 H 0.7613 0.2205 0.6714 0.033 Uiso 0.3088(10) 1 calc PR A 2 H3B2 H 0.8250 0.2665 0.6445 0.033 Uiso 0.3088(10) 1 calc PR A 2 H3B3 H 0.7358 0.2726 0.5971 0.033 Uiso 0.3088(10) 1 calc PR A 2 S2B S 0.7930(11) 0.4148(8) 0.6486(11) 0.0212(17) Uani 0.3088(10) 1 d P A 2 S1B S 0.5935(9) 0.3354(9) 0.6372(9) 0.0137(13) Uani 0.3088(10) 1 d P A 2 C43B C 0.6710(7) 0.4122(6) 0.7632(7) 0.019(2) Uani 0.3088(10) 1 d P A 2 H43D H 0.7074 0.4107 0.8145 0.029 Uiso 0.3088(10) 1 calc PR A 2 H43E H 0.6180 0.4121 0.7671 0.029 Uiso 0.3088(10) 1 calc PR A 2 H43F H 0.6797 0.4580 0.7371 0.029 Uiso 0.3088(10) 1 calc PR A 2 C4 C 0.6791(2) 0.2591(2) 0.7559(2) 0.0295(8) Uani 1 1 d . . . C5 C 0.56207(19) 0.2519(2) 0.6715(2) 0.0229(7) Uani 1 1 d . . . C6 C 0.48231(19) 0.2220(2) 0.6332(2) 0.0228(6) Uani 1 1 d . A . C7 C 0.4259(2) 0.2662(2) 0.5817(2) 0.0286(7) Uani 1 1 d . . . H7 H 0.4376 0.3158 0.5692 0.034 Uiso 1 1 calc R A . C8 C 0.3515(2) 0.2349(2) 0.5490(3) 0.0334(8) Uani 1 1 d . A . H8 H 0.3126 0.2632 0.5139 0.040 Uiso 1 1 calc R . . C9 C 0.3361(2) 0.1617(2) 0.5691(3) 0.0368(9) Uani 1 1 d . . . H9 H 0.2865 0.1400 0.5486 0.044 Uiso 1 1 calc R A . C10 C 0.3958(2) 0.1206(2) 0.6203(3) 0.0345(9) Uani 1 1 d . A . H10 H 0.3853 0.0709 0.6334 0.041 Uiso 1 1 calc R . . C11 C 0.73820(19) 0.24913(18) 0.8214(2) 0.0194(6) Uani 1 1 d . A . C12 C 0.7441(2) 0.1963(2) 0.8886(2) 0.0260(7) Uani 1 1 d . . . C13 C 0.8160(2) 0.2275(2) 0.9518(2) 0.0318(8) Uani 1 1 d . A . C14 C 0.8707(2) 0.25879(19) 0.9049(2) 0.0231(7) Uani 1 1 d . . . C15 C 0.81320(18) 0.28833(18) 0.8328(2) 0.0194(6) Uani 1 1 d . A . C16 C 0.8237(2) 0.3404(2) 0.7815(2) 0.0292(8) Uani 1 1 d . . . C17 C 0.8838(2) 0.4168(2) 0.7185(2) 0.0248(7) Uani 1 1 d . . . C18 C 0.9505(2) 0.4543(2) 0.6994(2) 0.0268(7) Uani 1 1 d . A . C19 C 0.9389(2) 0.5101(3) 0.6420(3) 0.0385(10) Uani 1 1 d . . . H19 H 0.8882 0.5252 0.6143 0.046 Uiso 1 1 calc R A . C20 C 1.0042(3) 0.5429(3) 0.6267(3) 0.0461(12) Uani 1 1 d . A . H20 H 0.9981 0.5801 0.5882 0.055 Uiso 1 1 calc R . . C21 C 1.0784(3) 0.5193(3) 0.6695(3) 0.0438(11) Uani 1 1 d . . . H21 H 1.1230 0.5410 0.6605 0.053 Uiso 1 1 calc R A . C22 C 1.0857(2) 0.4633(2) 0.7258(3) 0.0344(9) Uani 1 1 d . A . H22 H 1.1359 0.4474 0.7540 0.041 Uiso 1 1 calc R . . C23 C 0.4894(3) -0.1517(3) 0.6234(4) 0.0535(14) Uani 1 1 d . . . C24 C 0.5243(3) -0.0698(2) 0.6373(3) 0.0405(10) Uani 1 1 d . A . C25 C 0.5907(3) -0.0549(3) 0.6104(3) 0.0442(11) Uani 1 1 d . . . H25 H 0.6105 -0.0944 0.5865 0.053 Uiso 1 1 calc R . . C26 C 0.6274(3) 0.0159(3) 0.6183(3) 0.0395(10) Uani 1 1 d . A . C27 C 0.6985(3) 0.0241(3) 0.5853(4) 0.0529(14) Uani 1 1 d . . . C28 C 0.7087(3) -0.0407(3) 0.9081(4) 0.0519(13) Uani 1 1 d . . . C29 C 0.6369(2) 0.0085(2) 0.8627(3) 0.0365(10) Uani 1 1 d . A . C30 C 0.5852(2) 0.0295(2) 0.9042(3) 0.0364(9) Uani 1 1 d . . . H30 H 0.5958 0.0160 0.9565 0.044 Uiso 1 1 calc R . . C31 C 0.5174(2) 0.0706(2) 0.8679(2) 0.0275(7) Uani 1 1 d . A . C32 C 0.4599(2) 0.0893(2) 0.9151(2) 0.0300(8) Uani 1 1 d . . . C33 C 1.25675(16) 0.2169(2) 0.8170(2) 0.139(6) Uani 1 1 d . . . C34 C 1.1729(3) 0.2537(3) 0.7885(3) 0.0474(12) Uani 1 1 d . A . C35 C 1.1168(3) 0.2001(3) 0.7480(3) 0.0462(12) Uani 1 1 d . . . H35 H 1.1346 0.1535 0.7340 0.055 Uiso 1 1 calc R . . C36 C 1.0374(3) 0.2132(2) 0.7281(2) 0.0351(9) Uani 1 1 d . A . C37 C 0.9819(4) 0.1551(3) 0.6746(3) 0.0484(12) Uani 1 1 d . . . C38 C 1.1129(2) 0.2054(2) 1.0231(3) 0.0351(9) Uani 1 1 d . . . C39 C 1.0958(2) 0.2797(2) 0.9746(2) 0.0289(8) Uani 1 1 d . A . C40 C 1.1167(2) 0.3492(2) 1.0131(3) 0.0294(8) Uani 1 1 d . . . H40 H 1.1403 0.3497 1.0666 0.035 Uiso 1 1 calc R . . C41 C 1.1026(2) 0.4181(2) 0.9722(2) 0.0267(7) Uani 1 1 d . A . C42 C 1.1268(2) 0.4925(2) 1.0206(3) 0.0330(8) Uani 1 1 d . . . N1 N 0.60673(16) 0.22201(18) 0.7342(2) 0.0271(6) Uani 1 1 d . A . N2 N 0.46747(18) 0.14934(18) 0.6514(2) 0.0273(6) Uani 1 1 d . . . N3 N 0.89395(17) 0.37493(19) 0.78030(19) 0.0275(6) Uani 1 1 d . A . N4 N 1.02273(17) 0.43093(18) 0.7412(2) 0.0259(6) Uani 1 1 d . . . O1 O 0.49113(18) -0.02608(17) 0.6717(2) 0.0421(8) Uani 1 1 d . . . O2 O 0.61137(17) 0.07749(17) 0.6469(2) 0.0368(7) Uani 1 1 d . . . O3 O 0.63435(16) 0.02398(16) 0.7937(2) 0.0368(7) Uani 1 1 d . . . O4 O 0.49390(15) 0.09481(17) 0.79925(18) 0.0323(6) Uani 1 1 d . . . O5 O 1.16268(17) 0.31774(19) 0.8129(2) 0.0418(7) Uani 1 1 d . . . O6 O 0.99998(18) 0.26911(16) 0.74444(18) 0.0334(6) Uani 1 1 d . . . O7 O 1.06365(15) 0.26787(15) 0.90356(17) 0.0302(6) Uani 1 1 d . . . O8 O 1.07339(15) 0.42856(15) 0.90121(17) 0.0272(5) Uani 1 1 d . . . F1 F 0.75972(15) 0.12301(13) 0.87200(16) 0.0388(6) Uani 1 1 d . A . F2 F 0.67976(15) 0.19399(16) 0.91425(15) 0.0375(6) Uani 1 1 d . A . F3 F 0.85087(16) 0.17437(16) 1.00502(16) 0.0451(7) Uani 1 1 d . . . F4 F 0.79310(15) 0.28630(15) 0.98899(14) 0.0373(5) Uani 1 1 d . . . F5 F 0.92162(12) 0.31142(12) 0.94568(13) 0.0259(4) Uani 1 1 d . A . F6 F 0.91359(13) 0.19937(12) 0.88976(14) 0.0320(5) Uani 1 1 d . A . F7 F 0.5251(2) -0.19592(19) 0.6839(3) 0.0741(11) Uani 1 1 d . . . F8 F 0.4141(2) -0.15236(19) 0.6174(3) 0.0775(13) Uani 1 1 d . . . F9 F 0.5002(3) -0.1849(2) 0.5605(3) 0.0800(12) Uani 1 1 d . . . F10 F 0.6843(3) 0.0707(4) 0.5280(3) 0.118(2) Uani 1 1 d . . . F11 F 0.7592(2) 0.0536(2) 0.6396(3) 0.0777(12) Uani 1 1 d . . . F12 F 0.7261(2) -0.0418(2) 0.5677(3) 0.0787(12) Uani 1 1 d . . . F13 F 0.76485(18) -0.0412(2) 0.8738(2) 0.0662(10) Uani 1 1 d . . . F14 F 0.7468(3) -0.0075(4) 0.9765(3) 0.128(3) Uani 1 1 d . . . F15 F 0.6900(2) -0.1019(3) 0.9235(7) 0.272(7) Uani 1 1 d . . . F16 F 0.39730(14) 0.04245(17) 0.89418(16) 0.0405(6) Uani 1 1 d . . . F17 F 0.49128(16) 0.08014(15) 0.99165(16) 0.0402(6) Uani 1 1 d . . . F18 F 0.43409(18) 0.16077(15) 0.90334(19) 0.0475(7) Uani 1 1 d . . . F19 F 1.30941(18) 0.26997(19) 0.8486(2) 0.0806(13) Uani 1 1 d . . . F21 F 1.2781(2) 0.1868(3) 0.7585(2) 0.1052(18) Uani 1 1 d . . . F22 F 1.0172(3) 0.08846(19) 0.6693(2) 0.0817(13) Uani 1 1 d . . . F23 F 0.9560(3) 0.1837(2) 0.60433(19) 0.0724(11) Uani 1 1 d . . . F24 F 0.9212(3) 0.1386(2) 0.6995(2) 0.0766(12) Uani 1 1 d . . . F25 F 1.04753(17) 0.17769(17) 1.0349(2) 0.0511(7) Uani 1 1 d . . . F26 F 1.16548(18) 0.21563(16) 1.09235(18) 0.0521(8) Uani 1 1 d . . . F27 F 1.14227(19) 0.15182(15) 0.98635(19) 0.0518(8) Uani 1 1 d . . . F28 F 1.0771(3) 0.5096(2) 1.0578(4) 0.119(2) Uani 1 1 d . . . F29 F 1.1981(2) 0.48449(19) 1.0709(2) 0.0785(13) Uani 1 1 d . . . F30 F 1.1350(2) 0.55102(16) 0.97776(19) 0.0562(8) Uani 1 1 d . . . Cu1 Cu 0.55126(3) 0.08442(3) 0.72253(3) 0.03049(14) Uani 1 1 d . A . Cu2 Cu 1.03999(2) 0.34810(2) 0.82310(3) 0.02561(13) Uani 1 1 d . A . F20 F 1.2640(3) 0.1621(3) 0.8696(3) 0.173(4) 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 C1A 0.020(2) 0.028(3) 0.024(3) 0.006(2) 0.0059(19) -0.0015(19) C2A 0.023(2) 0.027(3) 0.022(3) 0.005(2) 0.008(2) 0.001(2) C3A 0.031(3) 0.038(3) 0.026(3) -0.004(2) 0.013(3) -0.003(3) S1A 0.0175(14) 0.0284(19) 0.016(2) 0.0039(13) 0.0057(10) -0.0010(11) S2A 0.0159(11) 0.0212(19) 0.0199(19) 0.0078(13) 0.0050(9) 0.0009(12) C43A 0.027(3) 0.021(3) 0.029(3) 0.001(2) 0.003(2) 0.004(2) C1B 0.017(4) 0.012(4) 0.013(5) -0.002(4) 0.003(4) 0.001(3) C2B 0.012(4) 0.021(5) 0.006(5) 0.004(4) 0.001(3) -0.001(4) C3B 0.018(5) 0.032(6) 0.016(6) -0.005(4) 0.006(5) -0.003(5) S2B 0.020(3) 0.022(4) 0.023(3) 0.000(3) 0.0095(18) 0.001(3) S1B 0.012(2) 0.022(3) 0.010(4) -0.001(2) 0.0067(19) 0.0022(16) C43B 0.014(5) 0.014(5) 0.029(6) 0.005(4) 0.006(4) -0.002(4) C4 0.0179(15) 0.0312(18) 0.037(2) 0.0151(15) 0.0032(14) -0.0034(13) C5 0.0162(13) 0.0264(15) 0.0263(19) 0.0051(13) 0.0066(12) -0.0001(12) C6 0.0186(14) 0.0270(16) 0.0235(18) -0.0009(13) 0.0070(12) -0.0012(12) C7 0.0216(15) 0.0311(18) 0.031(2) 0.0007(15) 0.0046(14) -0.0033(13) C8 0.0196(15) 0.037(2) 0.039(2) -0.0002(16) 0.0007(15) 0.0008(14) C9 0.0197(16) 0.035(2) 0.052(3) -0.0077(18) 0.0032(16) -0.0055(14) C10 0.0239(16) 0.0282(18) 0.051(3) 0.0000(17) 0.0100(16) -0.0044(14) C11 0.0199(14) 0.0183(13) 0.0211(17) 0.0029(11) 0.0076(12) 0.0009(11) C12 0.0290(16) 0.0215(15) 0.0256(19) 0.0074(13) 0.0051(14) -0.0037(13) C13 0.0349(19) 0.0303(18) 0.026(2) 0.0125(15) 0.0020(15) -0.0056(15) C14 0.0229(15) 0.0208(15) 0.0233(18) 0.0037(12) 0.0029(13) 0.0001(12) C15 0.0183(13) 0.0192(14) 0.0191(17) 0.0028(11) 0.0029(11) 0.0001(11) C16 0.0193(15) 0.0364(19) 0.026(2) 0.0120(15) -0.0026(13) -0.0081(13) C17 0.0183(14) 0.0260(16) 0.0281(19) 0.0060(13) 0.0034(13) -0.0022(12) C18 0.0213(15) 0.0286(17) 0.030(2) 0.0041(14) 0.0072(13) -0.0057(13) C19 0.0263(17) 0.043(2) 0.045(3) 0.0173(19) 0.0071(17) -0.0086(16) C20 0.034(2) 0.052(3) 0.052(3) 0.021(2) 0.012(2) -0.0117(19) C21 0.0284(19) 0.049(3) 0.058(3) 0.009(2) 0.0193(19) -0.0108(18) C22 0.0207(16) 0.0340(19) 0.050(3) -0.0005(17) 0.0121(16) -0.0042(14) C23 0.046(3) 0.032(2) 0.086(4) 0.000(2) 0.024(3) -0.0008(19) C24 0.036(2) 0.0280(19) 0.059(3) 0.0068(18) 0.015(2) 0.0026(16) C25 0.039(2) 0.035(2) 0.064(3) -0.001(2) 0.024(2) 0.0022(18) C26 0.034(2) 0.040(2) 0.049(3) 0.0074(19) 0.0197(19) 0.0053(17) C27 0.044(3) 0.047(3) 0.081(4) 0.008(3) 0.040(3) 0.003(2) C28 0.032(2) 0.050(3) 0.073(4) 0.025(3) 0.014(2) 0.012(2) C29 0.0224(16) 0.0246(17) 0.063(3) 0.0156(18) 0.0132(17) 0.0050(13) C30 0.0257(17) 0.034(2) 0.048(3) 0.0139(18) 0.0086(17) 0.0047(15) C31 0.0205(15) 0.0230(15) 0.037(2) 0.0045(14) 0.0059(14) -0.0015(12) C32 0.0293(17) 0.0264(17) 0.032(2) -0.0030(14) 0.0054(15) -0.0014(13) C33 0.044(4) 0.167(10) 0.177(11) -0.122(9) -0.012(5) 0.045(5) C34 0.036(2) 0.057(3) 0.044(3) -0.011(2) 0.0022(19) 0.018(2) C35 0.058(3) 0.039(2) 0.034(3) -0.0095(18) 0.001(2) 0.018(2) C36 0.053(2) 0.0268(18) 0.019(2) 0.0025(14) -0.0010(16) 0.0014(16) C37 0.073(3) 0.030(2) 0.031(3) -0.0045(17) -0.002(2) -0.008(2) C38 0.0301(18) 0.0270(18) 0.039(2) 0.0005(16) -0.0054(16) 0.0064(14) C39 0.0176(14) 0.0253(16) 0.039(2) -0.0015(15) -0.0003(14) 0.0047(12) C40 0.0221(15) 0.0261(17) 0.035(2) -0.0020(14) 0.0003(14) 0.0031(13) C41 0.0172(14) 0.0235(16) 0.039(2) -0.0060(14) 0.0074(14) 0.0024(12) C42 0.037(2) 0.0258(17) 0.036(2) -0.0064(15) 0.0118(17) 0.0016(15) N1 0.0157(12) 0.0307(15) 0.0337(18) 0.0105(13) 0.0051(11) -0.0027(11) N2 0.0197(13) 0.0263(15) 0.0375(19) 0.0025(12) 0.0109(12) -0.0009(11) N3 0.0202(13) 0.0303(15) 0.0280(17) 0.0079(12) 0.0004(11) -0.0065(11) N4 0.0197(13) 0.0247(14) 0.0327(18) 0.0002(12) 0.0065(12) -0.0039(11) O1 0.0344(15) 0.0289(14) 0.070(2) 0.0033(14) 0.0262(15) -0.0019(12) O2 0.0314(14) 0.0316(14) 0.055(2) 0.0075(13) 0.0246(14) 0.0009(11) O3 0.0248(12) 0.0285(13) 0.061(2) 0.0131(13) 0.0193(13) 0.0060(10) O4 0.0222(12) 0.0338(14) 0.0421(18) 0.0080(12) 0.0110(11) 0.0066(10) O5 0.0244(13) 0.0432(17) 0.055(2) -0.0107(15) 0.0078(13) 0.0040(12) O6 0.0357(14) 0.0268(13) 0.0313(16) -0.0018(11) -0.0009(11) -0.0038(11) O7 0.0245(12) 0.0245(12) 0.0349(16) -0.0006(11) -0.0026(11) 0.0022(10) O8 0.0245(12) 0.0227(11) 0.0328(16) -0.0034(10) 0.0053(10) 0.0013(9) F1 0.0432(13) 0.0175(10) 0.0465(15) 0.0073(9) -0.0018(11) -0.0007(9) F2 0.0366(12) 0.0482(14) 0.0297(13) 0.0080(10) 0.0125(10) -0.0155(11) F3 0.0462(14) 0.0463(14) 0.0322(14) 0.0237(11) -0.0058(11) -0.0089(12) F4 0.0442(13) 0.0448(14) 0.0253(13) -0.0031(10) 0.0141(10) -0.0116(11) F5 0.0247(9) 0.0259(10) 0.0222(11) 0.0008(8) -0.0012(8) -0.0034(8) F6 0.0304(11) 0.0213(10) 0.0388(14) 0.0034(9) 0.0010(9) 0.0072(8) F7 0.074(2) 0.0368(16) 0.115(3) 0.0214(18) 0.034(2) -0.0006(16) F8 0.0466(18) 0.0387(17) 0.149(4) -0.0148(19) 0.031(2) -0.0115(13) F9 0.096(3) 0.0434(18) 0.110(3) -0.025(2) 0.045(3) -0.0167(19) F10 0.084(3) 0.167(5) 0.131(4) 0.092(4) 0.078(3) 0.049(3) F11 0.0457(18) 0.082(3) 0.120(3) -0.025(2) 0.048(2) -0.0137(17) F12 0.065(2) 0.064(2) 0.129(4) -0.026(2) 0.064(2) -0.0053(17) F13 0.0402(15) 0.065(2) 0.096(3) 0.0235(19) 0.0236(17) 0.0259(15) F14 0.114(4) 0.183(6) 0.070(3) 0.012(3) -0.003(3) 0.095(4) F15 0.0333(19) 0.112(4) 0.640(19) 0.240(8) 0.048(5) 0.028(2) F16 0.0294(11) 0.0548(16) 0.0399(15) -0.0139(12) 0.0140(10) -0.0135(11) F17 0.0433(14) 0.0377(13) 0.0344(14) -0.0084(10) 0.0025(11) 0.0035(10) F18 0.0523(16) 0.0323(13) 0.062(2) 0.0061(12) 0.0230(14) 0.0177(11) F19 0.0319(15) 0.068(2) 0.135(4) -0.023(2) 0.0138(19) 0.0074(15) F21 0.067(2) 0.151(5) 0.100(4) -0.045(3) 0.028(2) 0.043(3) F22 0.123(4) 0.0339(16) 0.066(2) -0.0206(15) -0.008(2) 0.0042(18) F23 0.106(3) 0.060(2) 0.0280(17) 0.0013(14) -0.0182(17) -0.0111(19) F24 0.099(3) 0.055(2) 0.071(3) -0.0144(17) 0.016(2) -0.044(2) F25 0.0430(14) 0.0406(14) 0.064(2) 0.0224(13) 0.0055(13) 0.0005(12) F26 0.0539(16) 0.0349(13) 0.0456(17) 0.0031(12) -0.0210(13) 0.0073(12) F27 0.0607(18) 0.0322(13) 0.0528(18) 0.0008(12) 0.0008(14) 0.0233(12) F28 0.147(4) 0.066(2) 0.205(6) -0.081(3) 0.149(5) -0.054(3) F29 0.091(3) 0.0420(17) 0.068(2) -0.0220(16) -0.032(2) 0.0059(17) F30 0.077(2) 0.0323(14) 0.0527(19) -0.0048(12) 0.0085(16) -0.0160(14) Cu1 0.0207(2) 0.0274(2) 0.0462(3) 0.00894(19) 0.0141(2) 0.00297(16) Cu2 0.0204(2) 0.0208(2) 0.0317(3) -0.00129(16) 0.00120(17) -0.00029(14) F20 0.099(4) 0.166(7) 0.236(9) 0.101(7) 0.018(5) 0.065(5) _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 C1A C2A 1.504(8) . ? C1A C4 1.554(6) . ? C1A C3A 1.568(8) . ? C1A S1A 1.807(10) . ? C2A C43A 1.555(8) . ? C2A C16 1.578(6) . ? C2A S2A 1.809(9) . ? C3A H3A1 0.9600 . ? C3A H3A2 0.9600 . ? C3A H3A3 0.9600 . ? S1A C5 1.768(9) . ? S2A C17 1.763(8) . ? C43A H43A 0.9600 . ? C43A H43B 0.9600 . ? C43A H43C 0.9600 . ? C1B C2B 1.463(13) . ? C1B C43B 1.564(15) . ? C1B C4 1.597(10) . ? C1B S1B 1.81(2) . ? C2B C16 1.531(10) . ? C2B C3B 1.636(16) . ? C2B S2B 1.80(2) . ? C3B H3B1 0.9600 . ? C3B H3B2 0.9600 . ? C3B H3B3 0.9600 . ? S2B C17 1.73(2) . ? S1B C5 1.732(18) . ? C43B H43D 0.9600 . ? C43B H43E 0.9600 . ? C43B H43F 0.9600 . ? C4 C11 1.341(5) . ? C4 N1 1.387(4) . ? C5 N1 1.284(5) . ? C5 C6 1.477(5) . ? C6 N2 1.351(5) . ? C6 C7 1.383(5) . ? C7 C8 1.391(5) . ? C7 H7 0.9300 . ? C8 C9 1.373(6) . ? C8 H8 0.9300 . ? C9 C10 1.384(6) . ? C9 H9 0.9300 . ? C10 N2 1.329(5) . ? C10 H10 0.9300 . ? C11 C15 1.454(4) . ? C11 C12 1.496(5) . ? C12 F2 1.345(4) . ? C12 F1 1.357(4) . ? C12 C13 1.540(5) . ? C13 F3 1.345(4) . ? C13 F4 1.346(5) . ? C13 C14 1.552(5) . ? C14 F5 1.345(4) . ? C14 F6 1.356(4) . ? C14 C15 1.489(5) . ? C15 C16 1.342(5) . ? C16 N3 1.386(4) . ? C17 N3 1.295(5) . ? C17 C18 1.472(5) . ? C18 N4 1.347(5) . ? C18 C19 1.387(5) . ? C19 C20 1.385(5) . ? C19 H19 0.9300 . ? C20 C21 1.380(7) . ? C20 H20 0.9300 . ? C21 C22 1.383(7) . ? C21 H21 0.9300 . ? C22 N4 1.347(5) . ? C22 H22 0.9300 . ? C23 F8 1.306(6) . ? C23 F9 1.329(8) . ? C23 F7 1.333(7) . ? C23 C24 1.547(7) . ? C24 O1 1.230(6) . ? C24 C25 1.416(6) . ? C25 C26 1.382(7) . ? C25 H25 0.9300 . ? C26 O2 1.255(6) . ? C26 C27 1.544(6) . ? C27 F10 1.276(7) . ? C27 F12 1.320(6) . ? C27 F11 1.331(8) . ? C28 F15 1.171(7) . ? C28 F13 1.310(6) . ? C28 F14 1.350(9) . ? C28 C29 1.556(6) . ? C29 O3 1.254(6) . ? C29 C30 1.384(6) . ? C30 C31 1.390(5) . ? C30 H30 0.9300 . ? C31 O4 1.254(5) . ? C31 C32 1.532(6) . ? C32 F18 1.322(4) . ? C32 F17 1.334(5) . ? C32 F16 1.340(4) . ? C33 F19 1.320(5) . ? C33 F21 1.320(5) . ? C33 F20 1.322(6) . ? C33 C34 1.562(5) . ? C34 O5 1.230(6) . ? C34 C35 1.405(7) . ? C35 C36 1.367(7) . ? C35 H35 0.9300 . ? C36 O6 1.258(5) . ? C36 C37 1.539(6) . ? C37 F24 1.307(8) . ? C37 F23 1.309(6) . ? C37 F22 1.335(6) . ? C38 F25 1.325(5) . ? C38 F27 1.332(5) . ? C38 F26 1.332(5) . ? C38 C39 1.540(6) . ? C39 O7 1.254(5) . ? C39 C40 1.391(5) . ? C40 C41 1.391(5) . ? C40 H40 0.9300 . ? C41 O8 1.242(5) . ? C41 C42 1.548(5) . ? C42 F28 1.281(5) . ? C42 F30 1.309(5) . ? C42 F29 1.333(5) . ? N2 Cu1 2.005(3) . ? N4 Cu2 2.018(3) . ? O1 Cu1 2.261(3) . ? O2 Cu1 1.951(3) . ? O3 Cu1 1.955(3) . ? O4 Cu1 1.937(3) . ? O5 Cu2 2.292(3) . ? O6 Cu2 1.952(3) . ? O7 Cu2 1.965(3) . ? O8 Cu2 1.949(3) . ? 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 C2A C1A C4 109.0(4) . . ? C2A C1A C3A 113.2(5) . . ? C4 C1A C3A 110.1(4) . . ? C2A C1A S1A 116.4(4) . . ? C4 C1A S1A 103.3(4) . . ? C3A C1A S1A 104.4(4) . . ? C1A C2A C43A 112.6(5) . . ? C1A C2A C16 105.9(4) . . ? C43A C2A C16 112.2(4) . . ? C1A C2A S2A 116.9(5) . . ? C43A C2A S2A 107.0(4) . . ? C16 C2A S2A 101.7(4) . . ? C5 S1A C1A 88.5(4) . . ? C17 S2A C2A 91.5(4) . . ? C2B C1B C43B 112.5(9) . . ? C2B C1B C4 104.2(7) . . ? C43B C1B C4 115.7(8) . . ? C2B C1B S1B 121.9(8) . . ? C43B C1B S1B 103.1(7) . . ? C4 C1B S1B 99.2(8) . . ? C1B C2B C16 107.7(8) . . ? C1B C2B C3B 112.0(9) . . ? C16 C2B C3B 112.2(8) . . ? C1B C2B S2B 122.7(8) . . ? C16 C2B S2B 103.9(8) . . ? C3B C2B S2B 98.0(8) . . ? C2B C3B H3B1 109.5 . . ? C2B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C2B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C17 S2B C2B 89.7(10) . . ? C5 S1B C1B 93.7(9) . . ? C1B C43B H43D 109.5 . . ? C1B C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C1B C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? C11 C4 N1 127.7(3) . . ? C11 C4 C1A 117.8(3) . . ? N1 C4 C1A 113.4(3) . . ? C11 C4 C1B 112.2(4) . . ? N1 C4 C1B 116.7(4) . . ? N1 C5 C6 122.1(3) . . ? N1 C5 S1B 118.1(6) . . ? C6 C5 S1B 119.6(6) . . ? N1 C5 S1A 119.3(4) . . ? C6 C5 S1A 118.4(4) . . ? N2 C6 C7 122.0(3) . . ? N2 C6 C5 116.4(3) . . ? C7 C6 C5 121.6(3) . . ? C6 C7 C8 118.6(4) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? C9 C8 C7 119.2(4) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 118.9(4) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N2 C10 C9 122.7(4) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? C4 C11 C15 121.0(3) . . ? C4 C11 C12 129.9(3) . . ? C15 C11 C12 108.9(3) . . ? F2 C12 F1 107.0(3) . . ? F2 C12 C11 115.0(3) . . ? F1 C12 C11 112.0(3) . . ? F2 C12 C13 111.2(3) . . ? F1 C12 C13 108.4(3) . . ? C11 C12 C13 103.2(3) . . ? F3 C13 F4 108.4(3) . . ? F3 C13 C12 113.2(3) . . ? F4 C13 C12 109.3(3) . . ? F3 C13 C14 113.2(3) . . ? F4 C13 C14 108.9(3) . . ? C12 C13 C14 103.8(3) . . ? F5 C14 F6 107.6(3) . . ? F5 C14 C15 114.9(3) . . ? F6 C14 C15 111.9(3) . . ? F5 C14 C13 111.7(3) . . ? F6 C14 C13 108.2(3) . . ? C15 C14 C13 102.3(3) . . ? C16 C15 C11 121.4(3) . . ? C16 C15 C14 129.3(3) . . ? C11 C15 C14 109.3(3) . . ? C15 C16 N3 127.2(3) . . ? C15 C16 C2B 115.4(4) . . ? N3 C16 C2B 113.5(5) . . ? C15 C16 C2A 116.5(3) . . ? N3 C16 C2A 115.8(3) . . ? N3 C17 C18 121.6(3) . . ? N3 C17 S2B 118.7(7) . . ? C18 C17 S2B 118.8(7) . . ? N3 C17 S2A 118.2(4) . . ? C18 C17 S2A 120.3(4) . . ? N4 C18 C19 122.7(3) . . ? N4 C18 C17 115.7(3) . . ? C19 C18 C17 121.6(3) . . ? C20 C19 C18 118.7(4) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? C21 C20 C19 118.9(4) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? C20 C21 C22 119.4(4) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? N4 C22 C21 122.3(4) . . ? N4 C22 H22 118.8 . . ? C21 C22 H22 118.8 . . ? F8 C23 F9 108.6(5) . . ? F8 C23 F7 107.3(5) . . ? F9 C23 F7 106.8(4) . . ? F8 C23 C24 111.9(4) . . ? F9 C23 C24 113.0(5) . . ? F7 C23 C24 109.1(5) . . ? O1 C24 C25 128.2(4) . . ? O1 C24 C23 115.2(4) . . ? C25 C24 C23 116.6(4) . . ? C26 C25 C24 122.6(4) . . ? C26 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? O2 C26 C25 130.6(4) . . ? O2 C26 C27 112.4(4) . . ? C25 C26 C27 117.0(4) . . ? F10 C27 F12 111.2(6) . . ? F10 C27 F11 106.0(5) . . ? F12 C27 F11 103.6(5) . . ? F10 C27 C26 111.9(4) . . ? F12 C27 C26 114.1(4) . . ? F11 C27 C26 109.4(5) . . ? F15 C28 F13 114.1(7) . . ? F15 C28 F14 106.2(8) . . ? F13 C28 F14 100.3(5) . . ? F15 C28 C29 112.4(4) . . ? F13 C28 C29 111.9(4) . . ? F14 C28 C29 111.1(5) . . ? O3 C29 C30 129.1(4) . . ? O3 C29 C28 115.4(4) . . ? C30 C29 C28 115.5(4) . . ? C29 C30 C31 120.0(4) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? O4 C31 C30 129.2(4) . . ? O4 C31 C32 112.6(3) . . ? C30 C31 C32 118.2(4) . . ? F18 C32 F17 107.4(3) . . ? F18 C32 F16 108.0(3) . . ? F17 C32 F16 106.4(3) . . ? F18 C32 C31 111.5(3) . . ? F17 C32 C31 113.3(3) . . ? F16 C32 C31 110.0(3) . . ? F19 C33 F21 106.9(3) . . ? F19 C33 F20 106.7(4) . . ? F21 C33 F20 106.7(4) . . ? F19 C33 C34 109.9(3) . . ? F21 C33 C34 111.4(3) . . ? F20 C33 C34 114.8(4) . . ? O5 C34 C35 129.2(4) . . ? O5 C34 C33 118.6(4) . . ? C35 C34 C33 111.1(4) . . ? C36 C35 C34 123.1(4) . . ? C36 C35 H35 118.5 . . ? C34 C35 H35 118.5 . . ? O6 C36 C35 129.7(4) . . ? O6 C36 C37 111.6(4) . . ? C35 C36 C37 118.6(4) . . ? F24 C37 F23 108.4(5) . . ? F24 C37 F22 106.3(5) . . ? F23 C37 F22 107.7(5) . . ? F24 C37 C36 111.8(4) . . ? F23 C37 C36 109.6(4) . . ? F22 C37 C36 112.8(5) . . ? F25 C38 F27 107.7(4) . . ? F25 C38 F26 108.1(4) . . ? F27 C38 F26 106.6(3) . . ? F25 C38 C39 110.9(3) . . ? F27 C38 C39 110.5(4) . . ? F26 C38 C39 112.7(3) . . ? O7 C39 C40 128.8(4) . . ? O7 C39 C38 113.2(3) . . ? C40 C39 C38 118.0(4) . . ? C39 C40 C41 120.5(4) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? O8 C41 C40 128.7(4) . . ? O8 C41 C42 114.7(3) . . ? C40 C41 C42 116.6(4) . . ? F28 C42 F30 109.3(4) . . ? F28 C42 F29 109.3(5) . . ? F30 C42 F29 103.6(4) . . ? F28 C42 C41 111.5(4) . . ? F30 C42 C41 112.5(4) . . ? F29 C42 C41 110.4(3) . . ? C5 N1 C4 110.2(3) . . ? C10 N2 C6 118.6(3) . . ? C10 N2 Cu1 119.9(3) . . ? C6 N2 Cu1 121.5(2) . . ? C17 N3 C16 110.6(3) . . ? C22 N4 C18 118.0(3) . . ? C22 N4 Cu2 119.1(3) . . ? C18 N4 Cu2 122.9(2) . . ? C24 O1 Cu1 119.5(3) . . ? C26 O2 Cu1 124.6(3) . . ? C29 O3 Cu1 124.5(2) . . ? C31 O4 Cu1 124.8(2) . . ? C34 O5 Cu2 118.5(3) . . ? C36 O6 Cu2 127.4(3) . . ? C39 O7 Cu2 124.6(2) . . ? C41 O8 Cu2 125.6(2) . . ? O4 Cu1 O2 177.79(13) . . ? O4 Cu1 O3 92.12(12) . . ? O2 Cu1 O3 87.79(13) . . ? O4 Cu1 N2 87.45(13) . . ? O2 Cu1 N2 92.57(14) . . ? O3 Cu1 N2 178.21(14) . . ? O4 Cu1 O1 94.79(12) . . ? O2 Cu1 O1 87.42(12) . . ? O3 Cu1 O1 89.08(13) . . ? N2 Cu1 O1 92.68(13) . . ? O8 Cu2 O6 176.56(12) . . ? O8 Cu2 O7 91.57(12) . . ? O6 Cu2 O7 89.18(12) . . ? O8 Cu2 N4 87.69(13) . . ? O6 Cu2 N4 91.77(13) . . ? O7 Cu2 N4 176.54(12) . . ? O8 Cu2 O5 97.08(11) . . ? O6 Cu2 O5 86.34(12) . . ? O7 Cu2 O5 83.47(13) . . ? N4 Cu2 O5 93.26(13) . . ? 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 C4 C1A C2A C43A -64.5(5) . . . . ? C3A C1A C2A C43A 172.6(5) . . . . ? S1A C1A C2A C43A 51.7(6) . . . . ? C4 C1A C2A C16 58.5(5) . . . . ? C3A C1A C2A C16 -64.3(6) . . . . ? S1A C1A C2A C16 174.7(4) . . . . ? C4 C1A C2A S2A 171.0(4) . . . . ? C3A C1A C2A S2A 48.1(6) . . . . ? S1A C1A C2A S2A -72.8(6) . . . . ? C2A C1A S1A C5 -137.2(5) . . . . ? C4 C1A S1A C5 -17.8(4) . . . . ? C3A C1A S1A C5 97.3(4) . . . . ? C1A C2A S2A C17 -124.3(5) . . . . ? C43A C2A S2A C17 108.4(4) . . . . ? C16 C2A S2A C17 -9.5(4) . . . . ? C43B C1B C2B C16 59.7(10) . . . . ? C4 C1B C2B C16 -66.4(8) . . . . ? S1B C1B C2B C16 -177.0(8) . . . . ? C43B C1B C2B C3B -176.5(8) . . . . ? C4 C1B C2B C3B 57.4(10) . . . . ? S1B C1B C2B C3B -53.2(12) . . . . ? C43B C1B C2B S2B -60.5(13) . . . . ? C4 C1B C2B S2B 173.4(9) . . . . ? S1B C1B C2B S2B 62.7(14) . . . . ? C1B C2B S2B C17 135.5(9) . . . . ? C16 C2B S2B C17 13.4(6) . . . . ? C3B C2B S2B C17 -101.9(7) . . . . ? C2B C1B S1B C5 121.0(9) . . . . ? C43B C1B S1B C5 -111.5(7) . . . . ? C4 C1B S1B C5 7.8(5) . . . . ? C2A C1A C4 C11 -41.7(6) . . . . ? C3A C1A C4 C11 83.0(5) . . . . ? S1A C1A C4 C11 -166.0(4) . . . . ? C2A C1A C4 N1 149.0(4) . . . . ? C3A C1A C4 N1 -86.4(5) . . . . ? S1A C1A C4 N1 24.6(5) . . . . ? C2A C1A C4 C1B 45.6(8) . . . . ? C3A C1A C4 C1B 170.3(9) . . . . ? S1A C1A C4 C1B -78.7(8) . . . . ? C2B C1B C4 C11 57.7(8) . . . . ? C43B C1B C4 C11 -66.4(9) . . . . ? S1B C1B C4 C11 -175.8(4) . . . . ? C2B C1B C4 N1 -141.3(6) . . . . ? C43B C1B C4 N1 94.6(8) . . . . ? S1B C1B C4 N1 -14.8(6) . . . . ? C2B C1B C4 C1A -49.7(7) . . . . ? C43B C1B C4 C1A -173.8(13) . . . . ? S1B C1B C4 C1A 76.8(8) . . . . ? C1B S1B C5 N1 -0.4(6) . . . . ? C1B S1B C5 C6 173.3(4) . . . . ? C1B S1B C5 S1A -100(5) . . . . ? C1A S1A C5 N1 10.5(4) . . . . ? C1A S1A C5 C6 -164.5(3) . . . . ? C1A S1A C5 S1B 96(5) . . . . ? N1 C5 C6 N2 -20.1(5) . . . . ? S1B C5 C6 N2 166.5(4) . . . . ? S1A C5 C6 N2 154.7(3) . . . . ? N1 C5 C6 C7 159.7(4) . . . . ? S1B C5 C6 C7 -13.7(6) . . . . ? S1A C5 C6 C7 -25.5(5) . . . . ? N2 C6 C7 C8 1.1(6) . . . . ? C5 C6 C7 C8 -178.7(4) . . . . ? C6 C7 C8 C9 0.4(6) . . . . ? C7 C8 C9 C10 -1.2(7) . . . . ? C8 C9 C10 N2 0.5(7) . . . . ? N1 C4 C11 C15 175.0(4) . . . . ? C1A C4 C11 C15 7.4(6) . . . . ? C1B C4 C11 C15 -26.5(6) . . . . ? N1 C4 C11 C12 0.3(7) . . . . ? C1A C4 C11 C12 -167.3(4) . . . . ? C1B C4 C11 C12 158.7(5) . . . . ? C4 C11 C12 F2 -44.8(5) . . . . ? C15 C11 C12 F2 140.0(3) . . . . ? C4 C11 C12 F1 77.6(5) . . . . ? C15 C11 C12 F1 -97.6(3) . . . . ? C4 C11 C12 C13 -166.0(4) . . . . ? C15 C11 C12 C13 18.8(4) . . . . ? F2 C12 C13 F3 80.4(4) . . . . ? F1 C12 C13 F3 -37.0(5) . . . . ? C11 C12 C13 F3 -155.8(3) . . . . ? F2 C12 C13 F4 -40.4(4) . . . . ? F1 C12 C13 F4 -157.8(3) . . . . ? C11 C12 C13 F4 83.3(3) . . . . ? F2 C12 C13 C14 -156.5(3) . . . . ? F1 C12 C13 C14 86.2(3) . . . . ? C11 C12 C13 C14 -32.7(4) . . . . ? F3 C13 C14 F5 -79.0(4) . . . . ? F4 C13 C14 F5 41.6(4) . . . . ? C12 C13 C14 F5 157.9(3) . . . . ? F3 C13 C14 F6 39.2(4) . . . . ? F4 C13 C14 F6 159.9(3) . . . . ? C12 C13 C14 F6 -83.8(3) . . . . ? F3 C13 C14 C15 157.5(3) . . . . ? F4 C13 C14 C15 -81.9(3) . . . . ? C12 C13 C14 C15 34.4(4) . . . . ? C4 C11 C15 C16 5.6(5) . . . . ? C12 C11 C15 C16 -178.7(3) . . . . ? C4 C11 C15 C14 -172.5(3) . . . . ? C12 C11 C15 C14 3.2(4) . . . . ? F5 C14 C15 C16 37.3(5) . . . . ? F6 C14 C15 C16 -85.8(5) . . . . ? C13 C14 C15 C16 158.6(4) . . . . ? F5 C14 C15 C11 -144.8(3) . . . . ? F6 C14 C15 C11 92.0(3) . . . . ? C13 C14 C15 C11 -23.6(4) . . . . ? C11 C15 C16 N3 -171.6(4) . . . . ? C14 C15 C16 N3 6.0(7) . . . . ? C11 C15 C16 C2B -15.5(7) . . . . ? C14 C15 C16 C2B 162.1(5) . . . . ? C11 C15 C16 C2A 16.7(6) . . . . ? C14 C15 C16 C2A -165.7(4) . . . . ? C1B C2B C16 C15 48.9(9) . . . . ? C3B C2B C16 C15 -74.8(8) . . . . ? S2B C2B C16 C15 -179.6(5) . . . . ? C1B C2B C16 N3 -151.7(6) . . . . ? C3B C2B C16 N3 84.6(8) . . . . ? S2B C2B C16 N3 -20.2(7) . . . . ? C1B C2B C16 C2A -50.4(8) . . . . ? C3B C2B C16 C2A -174.0(13) . . . . ? S2B C2B C16 C2A 81.1(9) . . . . ? C1A C2A C16 C15 -49.2(6) . . . . ? C43A C2A C16 C15 74.1(6) . . . . ? S2A C2A C16 C15 -171.8(4) . . . . ? C1A C2A C16 N3 138.1(4) . . . . ? C43A C2A C16 N3 -98.6(5) . . . . ? S2A C2A C16 N3 15.5(5) . . . . ? C1A C2A C16 C2B 45.9(8) . . . . ? C43A C2A C16 C2B 169.2(10) . . . . ? S2A C2A C16 C2B -76.7(8) . . . . ? C2B S2B C17 N3 -5.5(6) . . . . ? C2B S2B C17 C18 163.3(5) . . . . ? C2B S2B C17 S2A -96(5) . . . . ? C2A S2A C17 N3 3.2(4) . . . . ? C2A S2A C17 C18 -176.4(4) . . . . ? C2A S2A C17 S2B 99(5) . . . . ? N3 C17 C18 N4 12.1(6) . . . . ? S2B C17 C18 N4 -156.4(5) . . . . ? S2A C17 C18 N4 -168.3(3) . . . . ? N3 C17 C18 C19 -167.9(4) . . . . ? S2B C17 C18 C19 23.6(7) . . . . ? S2A C17 C18 C19 11.7(6) . . . . ? N4 C18 C19 C20 0.3(7) . . . . ? C17 C18 C19 C20 -179.7(5) . . . . ? C18 C19 C20 C21 -0.5(8) . . . . ? C19 C20 C21 C22 0.7(8) . . . . ? C20 C21 C22 N4 -0.7(8) . . . . ? F8 C23 C24 O1 28.9(8) . . . . ? F9 C23 C24 O1 151.8(5) . . . . ? F7 C23 C24 O1 -89.6(6) . . . . ? F8 C23 C24 C25 -152.2(5) . . . . ? F9 C23 C24 C25 -29.3(7) . . . . ? F7 C23 C24 C25 89.3(6) . . . . ? O1 C24 C25 C26 -1.9(9) . . . . ? C23 C24 C25 C26 179.4(5) . . . . ? C24 C25 C26 O2 -1.3(9) . . . . ? C24 C25 C26 C27 -179.2(5) . . . . ? O2 C26 C27 F10 -64.2(7) . . . . ? C25 C26 C27 F10 114.1(6) . . . . ? O2 C26 C27 F12 168.4(5) . . . . ? C25 C26 C27 F12 -13.3(8) . . . . ? O2 C26 C27 F11 52.9(6) . . . . ? C25 C26 C27 F11 -128.8(5) . . . . ? F15 C28 C29 O3 -113.3(9) . . . . ? F13 C28 C29 O3 16.7(7) . . . . ? F14 C28 C29 O3 127.9(5) . . . . ? F15 C28 C29 C30 67.0(10) . . . . ? F13 C28 C29 C30 -163.1(5) . . . . ? F14 C28 C29 C30 -51.8(6) . . . . ? O3 C29 C30 C31 3.2(7) . . . . ? C28 C29 C30 C31 -177.1(4) . . . . ? C29 C30 C31 O4 -1.3(7) . . . . ? C29 C30 C31 C32 177.2(4) . . . . ? O4 C31 C32 F18 -44.2(5) . . . . ? C30 C31 C32 F18 137.0(4) . . . . ? O4 C31 C32 F17 -165.5(3) . . . . ? C30 C31 C32 F17 15.7(5) . . . . ? O4 C31 C32 F16 75.5(4) . . . . ? C30 C31 C32 F16 -103.3(4) . . . . ? F19 C33 C34 O5 -16.1(6) . . . . ? F21 C33 C34 O5 -134.5(5) . . . . ? F20 C33 C34 O5 104.1(5) . . . . ? F19 C33 C34 C35 174.4(4) . . . . ? F21 C33 C34 C35 56.0(5) . . . . ? F20 C33 C34 C35 -65.4(5) . . . . ? O5 C34 C35 C36 0.7(10) . . . . ? C33 C34 C35 C36 168.8(5) . . . . ? C34 C35 C36 O6 -4.5(9) . . . . ? C34 C35 C36 C37 172.1(5) . . . . ? O6 C36 C37 F24 -47.4(6) . . . . ? C35 C36 C37 F24 135.4(5) . . . . ? O6 C36 C37 F23 72.9(6) . . . . ? C35 C36 C37 F23 -104.3(6) . . . . ? O6 C36 C37 F22 -167.1(5) . . . . ? C35 C36 C37 F22 15.7(7) . . . . ? F25 C38 C39 O7 -76.3(5) . . . . ? F27 C38 C39 O7 43.2(5) . . . . ? F26 C38 C39 O7 162.4(4) . . . . ? F25 C38 C39 C40 103.5(4) . . . . ? F27 C38 C39 C40 -137.1(4) . . . . ? F26 C38 C39 C40 -17.9(5) . . . . ? O7 C39 C40 C41 -0.3(6) . . . . ? C38 C39 C40 C41 -179.9(3) . . . . ? C39 C40 C41 O8 -1.5(6) . . . . ? C39 C40 C41 C42 179.0(3) . . . . ? O8 C41 C42 F28 103.6(5) . . . . ? C40 C41 C42 F28 -76.8(5) . . . . ? O8 C41 C42 F30 -19.6(5) . . . . ? C40 C41 C42 F30 160.0(4) . . . . ? O8 C41 C42 F29 -134.7(4) . . . . ? C40 C41 C42 F29 44.8(5) . . . . ? C6 C5 N1 C4 177.8(3) . . . . ? S1B C5 N1 C4 -8.7(5) . . . . ? S1A C5 N1 C4 3.0(5) . . . . ? C11 C4 N1 C5 173.4(4) . . . . ? C1A C4 N1 C5 -18.5(5) . . . . ? C1B C4 N1 C5 15.8(6) . . . . ? C9 C10 N2 C6 1.0(7) . . . . ? C9 C10 N2 Cu1 -178.1(4) . . . . ? C7 C6 N2 C10 -1.8(6) . . . . ? C5 C6 N2 C10 178.0(4) . . . . ? C7 C6 N2 Cu1 177.2(3) . . . . ? C5 C6 N2 Cu1 -3.0(5) . . . . ? C18 C17 N3 C16 -174.5(4) . . . . ? S2B C17 N3 C16 -6.0(6) . . . . ? S2A C17 N3 C16 5.9(5) . . . . ? C15 C16 N3 C17 173.9(4) . . . . ? C2B C16 N3 C17 17.4(6) . . . . ? C2A C16 N3 C17 -14.4(5) . . . . ? C21 C22 N4 C18 0.4(6) . . . . ? C21 C22 N4 Cu2 178.8(4) . . . . ? C19 C18 N4 C22 -0.2(6) . . . . ? C17 C18 N4 C22 179.8(4) . . . . ? C19 C18 N4 Cu2 -178.5(3) . . . . ? C17 C18 N4 Cu2 1.5(5) . . . . ? C25 C24 O1 Cu1 -13.7(7) . . . . ? C23 C24 O1 Cu1 165.1(4) . . . . ? C25 C26 O2 Cu1 23.0(8) . . . . ? C27 C26 O2 Cu1 -159.0(3) . . . . ? C30 C29 O3 Cu1 -0.6(7) . . . . ? C28 C29 O3 Cu1 179.8(3) . . . . ? C30 C31 O4 Cu1 -2.8(6) . . . . ? C32 C31 O4 Cu1 178.5(2) . . . . ? C35 C34 O5 Cu2 16.6(8) . . . . ? C33 C34 O5 Cu2 -150.7(3) . . . . ? C35 C36 O6 Cu2 -14.5(7) . . . . ? C37 C36 O6 Cu2 168.7(3) . . . . ? C40 C39 O7 Cu2 4.8(6) . . . . ? C38 C39 O7 Cu2 -175.6(2) . . . . ? C40 C41 O8 Cu2 -1.8(5) . . . . ? C42 C41 O8 Cu2 177.8(2) . . . . ? C31 O4 Cu1 O3 4.0(3) . . . . ? C31 O4 Cu1 N2 -174.2(3) . . . . ? C31 O4 Cu1 O1 93.3(3) . . . . ? C26 O2 Cu1 O3 61.9(4) . . . . ? C26 O2 Cu1 N2 -119.9(4) . . . . ? C26 O2 Cu1 O1 -27.3(4) . . . . ? C29 O3 Cu1 O4 -2.5(3) . . . . ? C29 O3 Cu1 O2 175.3(3) . . . . ? C29 O3 Cu1 O1 -97.3(3) . . . . ? C10 N2 Cu1 O4 -71.5(3) . . . . ? C6 N2 Cu1 O4 109.5(3) . . . . ? C10 N2 Cu1 O2 110.8(3) . . . . ? C6 N2 Cu1 O2 -68.2(3) . . . . ? C10 N2 Cu1 O1 23.2(3) . . . . ? C6 N2 Cu1 O1 -155.8(3) . . . . ? C24 O1 Cu1 O4 -156.4(4) . . . . ? C24 O1 Cu1 O2 23.5(4) . . . . ? C24 O1 Cu1 O3 -64.3(4) . . . . ? C24 O1 Cu1 N2 115.9(4) . . . . ? C41 O8 Cu2 O7 4.4(3) . . . . ? C41 O8 Cu2 N4 -172.2(3) . . . . ? C41 O8 Cu2 O5 -79.2(3) . . . . ? C36 O6 Cu2 O7 -60.8(4) . . . . ? C36 O6 Cu2 N4 115.9(4) . . . . ? C36 O6 Cu2 O5 22.7(4) . . . . ? C39 O7 Cu2 O8 -5.7(3) . . . . ? C39 O7 Cu2 O6 177.6(3) . . . . ? C39 O7 Cu2 O5 91.2(3) . . . . ? C22 N4 Cu2 O8 74.5(3) . . . . ? C18 N4 Cu2 O8 -107.2(3) . . . . ? C22 N4 Cu2 O6 -108.9(3) . . . . ? C18 N4 Cu2 O6 69.4(3) . . . . ? C22 N4 Cu2 O5 -22.4(3) . . . . ? C18 N4 Cu2 O5 155.8(3) . . . . ? C34 O5 Cu2 O8 157.0(4) . . . . ? C34 O5 Cu2 O6 -23.3(4) . . . . ? C34 O5 Cu2 O7 66.2(4) . . . . ? C34 O5 Cu2 N4 -114.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.788 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.857 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.121 data_(hfac)2Cu-2 _database_code_depnum_ccdc_archive 'CCDC 715797' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H9 Cu F19 N2 O4 S' _chemical_formula_sum 'C24 H9 Cu F19 N2 O4 S ' _chemical_formula_weight 845.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1250 0.1230 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.4416(4) _cell_length_b 15.5291(4) _cell_length_c 15.5304(3) _cell_angle_alpha 107.0200(10) _cell_angle_beta 100.3160(10) _cell_angle_gamma 104.6300(10) _cell_volume 3099.57(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9029 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.813 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 0.922 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.905 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21991 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14111 _reflns_number_gt 8320 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1210P)^2^+1.9391P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14111 _refine_ls_number_parameters 921 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1213 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.2292 _refine_ls_wR_factor_gt 0.1910 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.084 _refine_ls_shift/su_mean 0.011 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 C10 C 0.2177(4) 0.3965(4) 0.1599(4) 0.0764(13) Uani 1 1 d . . . C11 C 0.1598(5) 0.3437(6) 0.0742(5) 0.108(2) Uani 1 1 d . . . C12 C 0.0752(7) 0.3742(8) 0.0434(7) 0.147(3) Uani 1 1 d . . . C13 C 0.0924(7) 0.4665(7) 0.1206(7) 0.133(3) Uani 1 1 d . . . C14 C 0.1786(5) 0.4741(5) 0.2011(6) 0.1015(19) Uani 1 1 d . . . C20 C 0.0213(6) 0.1892(7) 0.5416(6) 0.116(2) Uani 1 1 d . . . C24 C 0.1687(9) 0.5283(7) 0.5792(13) 0.182(6) Uani 1 1 d . . . F1 F 0.1700(4) 0.2668(4) 0.0195(3) 0.1488(17) Uani 1 1 d . . . F2 F 0.0746(6) 0.3873(6) -0.0392(4) 0.231(3) Uani 1 1 d . . . F3 F -0.0104(4) 0.3110(5) 0.0285(6) 0.228(4) Uani 1 1 d . . . F4 F 0.1234(6) 0.5403(5) 0.0916(5) 0.212(3) Uani 1 1 d . . . F5 F 0.0156(5) 0.4746(6) 0.1454(5) 0.230(4) Uani 1 1 d . . . F6 F 0.1449(4) 0.4666(4) 0.2744(4) 0.1488(17) Uani 1 1 d . . . F7 F 0.2465(3) 0.5596(3) 0.2355(4) 0.1458(17) Uani 1 1 d . . . F8 F -0.1263(4) 0.1640(4) 0.1521(5) 0.203(3) Uani 1 1 d . . . F9 F -0.0791(4) 0.3080(4) 0.2338(4) 0.173(2) Uani 1 1 d . . . F10 F -0.1131(4) 0.2037(8) 0.2922(7) 0.249(4) Uani 1 1 d . . . F11 F 0.1221(4) 0.0377(4) 0.0640(3) 0.168(2) Uani 1 1 d . . . F12 F 0.2671(3) 0.0812(4) 0.1539(3) 0.1418(17) Uani 1 1 d . . . F13 F 0.1534(4) -0.0112(3) 0.1780(3) 0.1378(15) Uani 1 1 d . . . F14 F -0.0620(4) 0.1653(6) 0.4825(6) 0.244(4) Uani 1 1 d . . . F15 F 0.0424(5) 0.1136(4) 0.5409(5) 0.182(2) Uani 1 1 d . . . F16 F 0.0091(5) 0.2243(5) 0.6237(5) 0.190(3) Uani 1 1 d . . . F17 F 0.2511(6) 0.5807(5) 0.6384(7) 0.254(5) Uani 1 1 d . . . F18 F 0.0977(6) 0.5382(4) 0.6130(8) 0.311(7) Uani 1 1 d . . . F19 F 0.1647(9) 0.5715(6) 0.5149(9) 0.275(6) Uani 1 1 d . . . F21 F 0.5938(5) 1.3318(5) 1.0352(4) 0.181(2) Uani 1 1 d . . . F22 F 0.7394(8) 1.4121(6) 1.0442(5) 0.300(6) Uani 1 1 d . . . F23 F 0.7979(8) 1.2894(12) 1.0494(5) 0.386(10) Uani 1 1 d . . . F24 F 0.6583(12) 1.2014(9) 1.0471(8) 0.349(8) Uani 1 1 d . . . F25 F 0.7808(4) 1.1747(5) 0.8984(4) 0.174(2) Uani 1 1 d . . . F26 F 0.6331(5) 1.0972(4) 0.8806(5) 0.192(3) Uani 1 1 d . . . F27 F 0.3526(9) 1.0338(4) 1.0026(5) 0.275(5) Uani 1 1 d . . . F28 F 0.3178(10) 1.1388(8) 0.9825(5) 0.287(6) Uani 1 1 d . . . F29 F 0.4444(8) 1.1499(11) 1.0269(4) 0.329(8) Uani 1 1 d . . . F30 F 0.3422(4) 0.7819(2) 0.7483(3) 0.1372(17) Uani 1 1 d . . . F31 F 0.3262(7) 0.7910(3) 0.6156(3) 0.222(4) Uani 1 1 d . . . F32 F 0.4671(6) 0.8308(4) 0.7026(6) 0.201(3) Uani 1 1 d . . . F33 F 0.3576(6) 1.4125(3) 0.7448(4) 0.200(3) Uani 1 1 d . . . F34 F 0.2613(6) 1.4069(3) 0.8263(6) 0.223(4) Uani 1 1 d . . . F35 F 0.4016(6) 1.4131(3) 0.8766(4) 0.187(3) Uani 1 1 d . . . F36 F 0.0283(4) 1.1314(5) 0.7815(6) 0.219(3) Uani 1 1 d . . . F37 F 0.0226(4) 1.0013(5) 0.6965(4) 0.204(3) Uani 1 1 d . . . F38 F 0.0970(4) 1.0512(5) 0.8347(4) 0.183(3) Uani 1 1 d . . . C1 C 0.3948(4) 0.3255(4) 0.5386(3) 0.0763(13) Uani 1 1 d . . . H1 H 0.3451 0.3031 0.5649 0.092 Uiso 1 1 calc R . . C2 C 0.4938(5) 0.3512(4) 0.5872(4) 0.0870(15) Uani 1 1 d . . . H2 H 0.5104 0.3472 0.6462 0.104 Uiso 1 1 calc R . . C3 C 0.5667(4) 0.3822(4) 0.5483(4) 0.0851(15) Uani 1 1 d . . . H3 H 0.6332 0.3979 0.5800 0.102 Uiso 1 1 calc R . . C4 C 0.5419(4) 0.3905(4) 0.4619(4) 0.0780(13) Uani 1 1 d . . . H4 H 0.5910 0.4126 0.4348 0.094 Uiso 1 1 calc R . . C5 C 0.4420(3) 0.3650(3) 0.4160(3) 0.0624(10) Uani 1 1 d . . . C6 C 0.4090(3) 0.3746(3) 0.3248(3) 0.0628(10) Uani 1 1 d . . . C7 C 0.3886(4) 0.3868(4) 0.1708(4) 0.0758(13) Uani 1 1 d . . . C8 C 0.3100(4) 0.3874(3) 0.2087(3) 0.0683(11) Uani 1 1 d . . . C9 C 0.4006(5) 0.3949(5) 0.0810(4) 0.0968(17) Uani 1 1 d . . . H9A H 0.3702 0.3336 0.0321 0.145 Uiso 1 1 calc R . . H9B H 0.4701 0.4177 0.0851 0.145 Uiso 1 1 calc R . . H9C H 0.3692 0.4387 0.0671 0.145 Uiso 1 1 calc R . . C15 C -0.0723(5) 0.2263(6) 0.2303(8) 0.124(3) Uani 1 1 d . . . C16 C 0.0363(4) 0.2274(4) 0.2518(5) 0.0855(15) Uani 1 1 d . . . C17 C 0.0640(4) 0.1601(4) 0.1927(4) 0.0805(13) Uani 1 1 d . . . H17 H 0.0205 0.1224 0.1339 0.097 Uiso 1 1 calc R . . C18 C 0.1530(4) 0.1466(3) 0.2171(3) 0.0676(11) Uani 1 1 d . . . C19 C 0.1746(5) 0.0644(5) 0.1508(4) 0.0972(18) Uani 1 1 d . . . C21 C 0.1007(4) 0.2621(5) 0.5191(4) 0.0916(16) Uani 1 1 d . . . C22 C 0.1023(5) 0.3553(5) 0.5485(5) 0.115(2) Uani 1 1 d . . . H22 H 0.0574 0.3706 0.5815 0.138 Uiso 1 1 calc R . . C23 C 0.1673(5) 0.4288(4) 0.5317(6) 0.114(2) Uani 1 1 d . . . Cu1 Cu 0.22571(4) 0.30685(4) 0.38930(4) 0.06794(19) Uani 1 1 d . . . N1 N 0.3700(3) 0.3325(2) 0.4536(3) 0.0633(9) Uani 1 1 d . . . N2 N 0.3212(3) 0.3807(3) 0.2958(3) 0.0637(9) Uani 1 1 d . . . O1 O 0.0894(3) 0.2905(3) 0.3276(3) 0.0902(10) Uani 1 1 d . . . O2 O 0.2222(2) 0.1912(2) 0.2908(2) 0.0673(7) Uani 1 1 d . . . O3 O 0.1561(3) 0.2279(3) 0.4787(3) 0.0911(10) Uani 1 1 d . . . O4 O 0.2292(3) 0.4230(2) 0.4851(3) 0.0953(12) Uani 1 1 d . . . S1 S 0.48112(10) 0.37591(10) 0.24887(11) 0.0801(4) Uani 1 1 d . . . C25 C 0.2655(4) 1.0563(4) 0.5079(4) 0.0794(13) Uani 1 1 d . . . H25 H 0.2104 1.0462 0.5313 0.095 Uiso 1 1 calc R . . C26 C 0.2507(5) 1.0397(5) 0.4129(4) 0.0980(18) Uani 1 1 d . . . H26 H 0.1867 1.0186 0.3733 0.118 Uiso 1 1 calc R . . C27 C 0.3318(6) 1.0551(5) 0.3786(4) 0.106(2) Uani 1 1 d . . . H27 H 0.3238 1.0457 0.3154 0.128 Uiso 1 1 calc R . . C28 C 0.4246(5) 1.0843(4) 0.4383(4) 0.0890(16) Uani 1 1 d . . . H28 H 0.4803 1.0931 0.4155 0.107 Uiso 1 1 calc R . . C29 C 0.4358(4) 1.1010(3) 0.5324(3) 0.0680(11) Uani 1 1 d . . . C30 C 0.5314(3) 1.1388(3) 0.6011(3) 0.0650(11) Uani 1 1 d . . . C31 C 0.7060(4) 1.2033(4) 0.6928(4) 0.0871(15) Uani 1 1 d . . . C32 C 0.6370(3) 1.1996(3) 0.7427(3) 0.0670(11) Uani 1 1 d . . . C33 C 0.8184(4) 1.2383(6) 0.7254(6) 0.123(2) Uani 1 1 d . . . H33A H 0.8404 1.2874 0.7861 0.184 Uiso 1 1 calc R . . H33B H 0.8446 1.2634 0.6819 0.184 Uiso 1 1 calc R . . H33C H 0.8417 1.1864 0.7288 0.184 Uiso 1 1 calc R . . C34 C 0.6580(4) 1.2338(4) 0.8451(4) 0.0752(12) Uani 1 1 d . . . C35 C 0.6410(5) 1.3101(4) 0.8961(4) 0.0956(17) Uani 1 1 d . . . C36 C 0.6664(7) 1.3289(7) 0.9987(6) 0.138(3) Uani 1 1 d . . . C37 C 0.7036(7) 1.2485(9) 1.0048(5) 0.146(4) Uani 1 1 d . . . C38 C 0.6928(5) 1.1871(6) 0.9056(5) 0.1025(19) Uani 1 1 d . . . C39 C 0.3692(6) 1.0927(5) 0.9682(4) 0.0949(18) Uani 1 1 d . . . C40 C 0.3837(4) 1.0662(3) 0.8722(3) 0.0665(11) Uani 1 1 d . . . C41 C 0.3708(4) 0.9704(3) 0.8275(3) 0.0732(12) Uani 1 1 d . . . H41 H 0.3562 0.9286 0.8592 0.088 Uiso 1 1 calc R . . C42 C 0.3789(4) 0.9359(3) 0.7378(3) 0.0691(12) Uani 1 1 d . . . C43 C 0.3740(7) 0.8334(4) 0.7015(5) 0.112(2) Uani 1 1 d . . . C44 C 0.0804(6) 1.0724(6) 0.7611(6) 0.110(2) Uani 1 1 d . . . C45 C 0.1781(4) 1.1172(4) 0.7412(4) 0.0780(13) Uani 1 1 d . . . C46 C 0.2153(4) 1.2173(4) 0.7750(4) 0.0801(13) Uani 1 1 d . . . H46 H 0.1792 1.2510 0.8066 0.096 Uiso 1 1 calc R . . C47 C 0.3019(4) 1.2673(3) 0.7637(3) 0.0685(11) Uani 1 1 d . . . C48 C 0.3290(5) 1.3747(4) 0.7994(5) 0.0929(17) Uani 1 1 d . . . Cu2 Cu 0.37938(4) 1.10984(4) 0.70590(3) 0.05870(17) Uani 1 1 d . . . F20 F 0.6062(5) 1.3670(4) 0.8662(4) 0.167(2) Uani 1 1 d . . . N3 N 0.3557(3) 1.0860(3) 0.5667(2) 0.0639(9) Uani 1 1 d . . . N4 N 0.5389(3) 1.1630(3) 0.6909(3) 0.0615(8) Uani 1 1 d . . . O5 O 0.4013(3) 1.1321(2) 0.8402(2) 0.0716(8) Uani 1 1 d . . . O6 O 0.3904(3) 0.9788(2) 0.6821(2) 0.0712(8) Uani 1 1 d . . . O7 O 0.2147(3) 1.0612(3) 0.6989(3) 0.0834(9) Uani 1 1 d . . . O8 O 0.3655(2) 1.2391(2) 0.7291(2) 0.0703(8) Uani 1 1 d . . . S2 S 0.64456(11) 1.16060(12) 0.57565(11) 0.0898(4) 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 C10 0.069(3) 0.070(3) 0.090(3) 0.037(3) 0.011(3) 0.020(2) C11 0.086(4) 0.116(5) 0.108(5) 0.036(4) 0.004(4) 0.026(4) C12 0.102(6) 0.169(9) 0.139(7) 0.064(7) -0.030(5) 0.029(6) C13 0.108(6) 0.145(7) 0.159(7) 0.072(7) 0.005(5) 0.063(5) C14 0.080(4) 0.098(5) 0.143(6) 0.063(4) 0.022(4) 0.039(3) C20 0.086(5) 0.139(7) 0.121(5) 0.045(5) 0.045(4) 0.022(4) C24 0.116(7) 0.081(6) 0.308(16) -0.006(8) 0.097(9) 0.023(6) F1 0.139(4) 0.132(4) 0.118(3) -0.003(3) -0.010(3) 0.036(3) F2 0.243(8) 0.324(10) 0.148(5) 0.114(6) -0.008(5) 0.134(7) F3 0.095(4) 0.211(7) 0.278(9) 0.022(6) -0.041(4) 0.022(4) F4 0.236(7) 0.197(6) 0.236(7) 0.144(6) -0.001(5) 0.094(5) F5 0.122(4) 0.305(10) 0.240(7) 0.044(6) 0.002(4) 0.125(6) F6 0.162(4) 0.195(5) 0.162(4) 0.092(4) 0.073(3) 0.125(4) F7 0.125(3) 0.089(3) 0.199(5) 0.045(3) -0.009(3) 0.039(3) F8 0.082(3) 0.170(5) 0.260(7) -0.014(5) -0.050(4) 0.050(3) F9 0.115(3) 0.141(4) 0.225(6) 0.016(4) -0.014(3) 0.077(3) F10 0.083(3) 0.436(13) 0.306(10) 0.212(10) 0.077(5) 0.101(5) F11 0.174(4) 0.231(6) 0.071(2) -0.003(3) 0.006(2) 0.103(4) F12 0.107(3) 0.208(5) 0.101(3) 0.015(3) 0.051(2) 0.067(3) F13 0.175(4) 0.101(3) 0.140(3) 0.021(3) 0.059(3) 0.063(3) F14 0.103(4) 0.319(9) 0.279(8) 0.204(8) -0.014(4) -0.050(5) F15 0.194(6) 0.148(4) 0.263(7) 0.110(5) 0.134(5) 0.059(4) F16 0.202(6) 0.225(6) 0.188(5) 0.088(5) 0.131(5) 0.070(5) F17 0.180(6) 0.105(4) 0.340(11) -0.077(6) 0.070(7) 0.002(4) F18 0.199(7) 0.133(5) 0.525(16) -0.055(7) 0.214(9) 0.048(4) F19 0.344(14) 0.115(5) 0.393(15) 0.057(8) 0.138(12) 0.134(7) F21 0.201(5) 0.250(7) 0.146(4) 0.061(4) 0.105(4) 0.135(5) F22 0.291(10) 0.233(8) 0.156(5) -0.078(6) 0.046(6) -0.095(8) F23 0.248(10) 0.66(2) 0.142(5) -0.051(9) -0.069(6) 0.269(13) F24 0.65(2) 0.441(15) 0.311(11) 0.299(12) 0.363(15) 0.414(17) F25 0.159(4) 0.253(6) 0.163(4) 0.072(4) 0.050(3) 0.156(5) F26 0.202(6) 0.153(5) 0.229(6) 0.126(5) 0.009(5) 0.036(4) F27 0.630(17) 0.144(4) 0.188(5) 0.104(4) 0.295(9) 0.171(7) F28 0.543(18) 0.387(12) 0.177(6) 0.168(8) 0.248(10) 0.378(14) F29 0.241(9) 0.533(19) 0.072(3) 0.020(6) 0.037(4) -0.004(11) F30 0.245(5) 0.073(2) 0.132(3) 0.058(2) 0.108(3) 0.052(3) F31 0.483(13) 0.068(2) 0.091(3) 0.016(2) 0.073(5) 0.065(4) F32 0.285(8) 0.149(4) 0.305(9) 0.125(5) 0.213(8) 0.151(5) F33 0.392(10) 0.081(3) 0.176(4) 0.067(3) 0.164(6) 0.077(4) F34 0.225(7) 0.091(3) 0.376(10) 0.037(4) 0.169(7) 0.079(4) F35 0.262(7) 0.090(3) 0.137(4) 0.004(3) 0.007(4) 0.014(4) F36 0.134(4) 0.214(6) 0.388(11) 0.149(7) 0.169(6) 0.072(4) F37 0.099(3) 0.251(7) 0.156(4) 0.007(4) 0.044(3) -0.052(4) F38 0.137(4) 0.248(6) 0.166(4) 0.129(5) 0.053(3) -0.007(4) C1 0.087(4) 0.076(3) 0.063(3) 0.019(2) 0.015(2) 0.032(3) C2 0.101(4) 0.082(3) 0.070(3) 0.021(3) 0.005(3) 0.035(3) C3 0.067(3) 0.076(3) 0.093(4) 0.017(3) -0.009(3) 0.028(3) C4 0.058(3) 0.074(3) 0.097(4) 0.026(3) 0.013(3) 0.025(2) C5 0.058(3) 0.051(2) 0.073(3) 0.015(2) 0.013(2) 0.0211(19) C6 0.055(2) 0.053(2) 0.082(3) 0.028(2) 0.019(2) 0.0162(19) C7 0.071(3) 0.071(3) 0.093(3) 0.037(3) 0.027(3) 0.024(2) C8 0.069(3) 0.054(2) 0.083(3) 0.029(2) 0.016(2) 0.019(2) C9 0.107(5) 0.100(4) 0.104(4) 0.051(3) 0.044(4) 0.042(4) C15 0.068(4) 0.109(5) 0.181(8) 0.043(5) 0.005(5) 0.033(4) C16 0.050(3) 0.083(4) 0.123(5) 0.045(4) 0.012(3) 0.018(3) C17 0.068(3) 0.082(3) 0.084(3) 0.028(3) 0.010(3) 0.022(3) C18 0.063(3) 0.076(3) 0.063(3) 0.030(2) 0.018(2) 0.015(2) C19 0.097(5) 0.121(5) 0.072(3) 0.023(3) 0.031(3) 0.041(4) C21 0.075(3) 0.098(4) 0.088(4) 0.017(3) 0.031(3) 0.020(3) C22 0.079(4) 0.103(5) 0.138(5) -0.001(4) 0.055(4) 0.022(4) C23 0.080(4) 0.072(4) 0.156(6) -0.007(4) 0.038(4) 0.020(3) Cu1 0.0542(3) 0.0605(3) 0.0864(4) 0.0202(3) 0.0196(3) 0.0207(2) N1 0.058(2) 0.058(2) 0.072(2) 0.0197(17) 0.0151(17) 0.0210(17) N2 0.051(2) 0.063(2) 0.080(2) 0.0293(18) 0.0156(17) 0.0194(16) O1 0.059(2) 0.083(2) 0.123(3) 0.027(2) 0.015(2) 0.0297(19) O2 0.0624(18) 0.0689(19) 0.0738(19) 0.0254(16) 0.0213(16) 0.0248(15) O3 0.089(3) 0.084(2) 0.107(3) 0.031(2) 0.045(2) 0.030(2) O4 0.071(2) 0.062(2) 0.134(3) 0.007(2) 0.035(2) 0.0180(17) S1 0.0687(8) 0.0907(9) 0.1014(9) 0.0472(8) 0.0365(7) 0.0356(7) C25 0.073(3) 0.093(4) 0.078(3) 0.027(3) 0.018(3) 0.042(3) C26 0.096(4) 0.124(5) 0.081(3) 0.036(3) 0.011(3) 0.057(4) C27 0.133(6) 0.147(6) 0.072(3) 0.052(4) 0.038(4) 0.078(5) C28 0.108(4) 0.111(4) 0.079(3) 0.049(3) 0.045(3) 0.056(4) C29 0.091(3) 0.071(3) 0.065(3) 0.035(2) 0.037(2) 0.040(3) C30 0.073(3) 0.072(3) 0.075(3) 0.038(2) 0.041(2) 0.037(2) C31 0.071(3) 0.083(3) 0.105(4) 0.022(3) 0.037(3) 0.027(3) C32 0.062(3) 0.058(2) 0.085(3) 0.023(2) 0.029(2) 0.022(2) C33 0.060(3) 0.140(6) 0.155(6) 0.032(5) 0.041(4) 0.025(4) C34 0.059(3) 0.077(3) 0.083(3) 0.021(3) 0.017(2) 0.022(2) C35 0.104(4) 0.077(4) 0.101(4) 0.016(3) 0.032(3) 0.036(3) C36 0.114(6) 0.158(8) 0.105(5) 0.003(5) 0.031(5) 0.037(6) C37 0.114(6) 0.261(12) 0.087(4) 0.065(6) 0.023(4) 0.100(7) C38 0.101(5) 0.119(5) 0.108(5) 0.049(4) 0.027(4) 0.060(4) C39 0.145(6) 0.090(4) 0.062(3) 0.027(3) 0.040(4) 0.053(4) C40 0.071(3) 0.069(3) 0.067(3) 0.028(2) 0.027(2) 0.025(2) C41 0.099(4) 0.067(3) 0.070(3) 0.035(2) 0.039(3) 0.031(3) C42 0.085(3) 0.060(2) 0.078(3) 0.033(2) 0.040(2) 0.026(2) C43 0.191(8) 0.079(4) 0.117(5) 0.052(4) 0.100(5) 0.067(5) C44 0.091(5) 0.112(5) 0.135(6) 0.055(5) 0.045(4) 0.020(4) C45 0.070(3) 0.087(4) 0.083(3) 0.039(3) 0.027(3) 0.021(3) C46 0.077(3) 0.086(4) 0.090(3) 0.032(3) 0.038(3) 0.038(3) C47 0.085(3) 0.066(3) 0.064(2) 0.027(2) 0.028(2) 0.031(2) C48 0.118(5) 0.071(3) 0.091(4) 0.019(3) 0.045(4) 0.033(3) Cu2 0.0657(3) 0.0569(3) 0.0605(3) 0.0237(2) 0.0258(2) 0.0222(2) F20 0.247(6) 0.119(3) 0.180(4) 0.048(3) 0.087(4) 0.119(4) N3 0.069(2) 0.066(2) 0.066(2) 0.0261(17) 0.0260(18) 0.0301(18) N4 0.065(2) 0.062(2) 0.070(2) 0.0304(17) 0.0286(18) 0.0262(17) O5 0.094(2) 0.0602(17) 0.0640(17) 0.0228(15) 0.0280(16) 0.0247(16) O6 0.091(2) 0.0623(17) 0.0731(18) 0.0306(15) 0.0397(17) 0.0264(16) O7 0.087(2) 0.071(2) 0.095(2) 0.0297(19) 0.037(2) 0.0229(19) O8 0.074(2) 0.0668(18) 0.0804(19) 0.0294(15) 0.0357(17) 0.0261(16) S2 0.0856(9) 0.1061(10) 0.0983(9) 0.0415(8) 0.0563(8) 0.0374(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C10 C11 1.327(8) . ? C10 C8 1.472(7) . ? C10 C14 1.485(9) . ? C11 F1 1.307(8) . ? C11 C12 1.470(11) . ? C12 F3 1.303(11) . ? C12 F2 1.355(11) . ? C12 C13 1.504(13) . ? C13 F5 1.260(11) . ? C13 F4 1.353(10) . ? C13 C14 1.553(9) . ? C14 F7 1.322(7) . ? C14 F6 1.339(8) . ? C20 F14 1.268(9) . ? C20 F15 1.282(10) . ? C20 F16 1.295(9) . ? C20 C21 1.561(9) . ? C24 F18 1.255(11) . ? C24 F17 1.267(15) . ? C24 F19 1.357(19) . ? C24 C23 1.498(10) . ? F8 C15 1.269(10) . ? F9 C15 1.284(9) . ? F10 C15 1.301(11) . ? F11 C19 1.309(7) . ? F12 C19 1.284(7) . ? F13 C19 1.344(8) . ? F21 C36 1.282(9) . ? F22 C36 1.338(11) . ? F23 C37 1.306(13) . ? F24 C37 1.259(13) . ? F25 C38 1.352(8) . ? F26 C38 1.340(9) . ? F27 C39 1.183(7) . ? F28 C39 1.162(8) . ? F29 C39 1.218(10) . ? F30 C43 1.286(6) . ? F31 C43 1.271(9) . ? F32 C43 1.354(10) . ? F33 C48 1.236(7) . ? F34 C48 1.285(8) . ? F35 C48 1.307(8) . ? F36 C44 1.331(9) . ? F37 C44 1.228(9) . ? F38 C44 1.278(9) . ? C1 N1 1.350(6) . ? C1 C2 1.387(8) . ? C1 H1 0.9300 . ? C2 C3 1.358(9) . ? C2 H2 0.9300 . ? C3 C4 1.378(8) . ? C3 H3 0.9300 . ? C4 C5 1.387(6) . ? C4 H4 0.9300 . ? C5 N1 1.342(6) . ? C5 C6 1.475(6) . ? C6 N2 1.305(6) . ? C6 S1 1.708(5) . ? C7 C8 1.370(7) . ? C7 C9 1.474(7) . ? C7 S1 1.714(5) . ? C8 N2 1.370(6) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C15 C16 1.538(9) . ? C16 O1 1.247(7) . ? C16 C17 1.371(8) . ? C17 C18 1.359(7) . ? C17 H17 0.9300 . ? C18 O2 1.252(5) . ? C18 C19 1.527(8) . ? C21 O3 1.231(7) . ? C21 C22 1.377(9) . ? C22 C23 1.404(10) . ? C22 H22 0.9300 . ? C23 O4 1.252(7) . ? Cu1 O1 1.946(4) . ? Cu1 O4 1.955(4) . ? Cu1 O2 1.971(3) . ? Cu1 N1 2.024(4) . ? Cu1 O3 2.305(4) . ? C25 N3 1.329(6) . ? C25 C26 1.388(8) . ? C25 H25 0.9300 . ? C26 C27 1.367(9) . ? C26 H26 0.9300 . ? C27 C28 1.365(9) . ? C27 H27 0.9300 . ? C28 C29 1.380(7) . ? C28 H28 0.9300 . ? C29 N3 1.353(6) . ? C29 C30 1.444(7) . ? C30 N4 1.310(6) . ? C30 S2 1.724(4) . ? C31 C32 1.367(7) . ? C31 C33 1.512(8) . ? C31 S2 1.720(6) . ? C32 N4 1.376(6) . ? C32 C34 1.468(7) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.327(7) . ? C34 C38 1.441(8) . ? C35 F20 1.276(8) . ? C35 C36 1.492(10) . ? C36 C37 1.499(13) . ? C37 C38 1.512(11) . ? C39 C40 1.494(7) . ? C40 O5 1.253(5) . ? C40 C41 1.392(6) . ? C41 C42 1.376(6) . ? C41 H41 0.9300 . ? C42 O6 1.247(5) . ? C42 C43 1.503(7) . ? C44 C45 1.535(8) . ? C45 O7 1.220(6) . ? C45 C46 1.408(8) . ? C46 C47 1.366(7) . ? C46 H46 0.9300 . ? C47 O8 1.251(5) . ? C47 C48 1.516(7) . ? Cu2 O5 1.964(3) . ? Cu2 O8 2.001(3) . ? Cu2 O6 2.012(3) . ? Cu2 N3 2.032(4) . ? Cu2 O7 2.278(4) . ? Cu2 N4 2.321(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 C11 C10 C8 128.1(6) . . ? C11 C10 C14 109.1(5) . . ? C8 C10 C14 122.7(5) . . ? F1 C11 C10 125.3(6) . . ? F1 C11 C12 119.6(7) . . ? C10 C11 C12 115.0(8) . . ? F3 C12 F2 105.4(8) . . ? F3 C12 C11 112.7(9) . . ? F2 C12 C11 110.9(9) . . ? F3 C12 C13 112.9(10) . . ? F2 C12 C13 111.1(9) . . ? C11 C12 C13 104.0(7) . . ? F5 C13 F4 105.5(8) . . ? F5 C13 C12 114.2(9) . . ? F4 C13 C12 109.8(9) . . ? F5 C13 C14 113.7(9) . . ? F4 C13 C14 107.9(7) . . ? C12 C13 C14 105.6(6) . . ? F7 C14 F6 103.4(7) . . ? F7 C14 C10 113.5(6) . . ? F6 C14 C10 113.2(5) . . ? F7 C14 C13 111.6(6) . . ? F6 C14 C13 110.1(6) . . ? C10 C14 C13 105.2(7) . . ? F14 C20 F15 108.5(8) . . ? F14 C20 F16 107.0(8) . . ? F15 C20 F16 105.1(8) . . ? F14 C20 C21 109.1(7) . . ? F15 C20 C21 114.2(6) . . ? F16 C20 C21 112.6(7) . . ? F18 C24 F17 110.6(13) . . ? F18 C24 F19 104.4(14) . . ? F17 C24 F19 101.8(10) . . ? F18 C24 C23 117.4(8) . . ? F17 C24 C23 112.9(11) . . ? F19 C24 C23 108.2(12) . . ? N1 C1 C2 120.5(5) . . ? N1 C1 H1 119.7 . . ? C2 C1 H1 119.7 . . ? C3 C2 C1 120.0(5) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 119.8(5) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 118.5(5) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 121.7(4) . . ? N1 C5 C6 116.3(4) . . ? C4 C5 C6 122.0(4) . . ? N2 C6 C5 121.8(4) . . ? N2 C6 S1 115.4(3) . . ? C5 C6 S1 122.8(3) . . ? C8 C7 C9 130.1(5) . . ? C8 C7 S1 108.0(4) . . ? C9 C7 S1 121.9(4) . . ? C7 C8 N2 117.0(4) . . ? C7 C8 C10 122.3(5) . . ? N2 C8 C10 120.7(4) . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? F8 C15 F9 109.3(8) . . ? F8 C15 F10 105.0(8) . . ? F9 C15 F10 106.8(9) . . ? F8 C15 C16 113.3(8) . . ? F9 C15 C16 112.4(6) . . ? F10 C15 C16 109.7(7) . . ? O1 C16 C17 127.0(5) . . ? O1 C16 C15 112.8(6) . . ? C17 C16 C15 120.0(6) . . ? C18 C17 C16 122.1(5) . . ? C18 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? O2 C18 C17 128.7(5) . . ? O2 C18 C19 112.3(4) . . ? C17 C18 C19 118.9(5) . . ? F12 C19 F11 109.3(5) . . ? F12 C19 F13 103.2(6) . . ? F11 C19 F13 107.7(6) . . ? F12 C19 C18 113.7(6) . . ? F11 C19 C18 112.9(6) . . ? F13 C19 C18 109.5(5) . . ? O3 C21 C22 128.3(6) . . ? O3 C21 C20 114.4(6) . . ? C22 C21 C20 117.3(6) . . ? C21 C22 C23 124.2(6) . . ? C21 C22 H22 117.9 . . ? C23 C22 H22 117.9 . . ? O4 C23 C22 128.2(6) . . ? O4 C23 C24 114.4(7) . . ? C22 C23 C24 117.4(7) . . ? O1 Cu1 O4 89.01(17) . . ? O1 Cu1 O2 90.60(15) . . ? O4 Cu1 O2 178.80(16) . . ? O1 Cu1 N1 176.34(15) . . ? O4 Cu1 N1 88.67(16) . . ? O2 Cu1 N1 91.66(14) . . ? O1 Cu1 O3 85.35(16) . . ? O4 Cu1 O3 85.74(16) . . ? O2 Cu1 O3 95.36(13) . . ? N1 Cu1 O3 97.30(15) . . ? C5 N1 C1 119.5(4) . . ? C5 N1 Cu1 120.2(3) . . ? C1 N1 Cu1 120.0(3) . . ? C6 N2 C8 109.4(4) . . ? C16 O1 Cu1 126.5(4) . . ? C18 O2 Cu1 124.2(3) . . ? C21 O3 Cu1 115.8(4) . . ? C23 O4 Cu1 125.2(4) . . ? C6 S1 C7 90.3(2) . . ? N3 C25 C26 122.4(5) . . ? N3 C25 H25 118.8 . . ? C26 C25 H25 118.8 . . ? C27 C26 C25 118.8(6) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C28 C27 C26 119.1(5) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C27 C28 C29 120.0(5) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? N3 C29 C28 121.1(5) . . ? N3 C29 C30 115.6(4) . . ? C28 C29 C30 123.3(5) . . ? N4 C30 C29 121.5(4) . . ? N4 C30 S2 113.7(4) . . ? C29 C30 S2 124.8(3) . . ? C32 C31 C33 130.7(6) . . ? C32 C31 S2 108.5(4) . . ? C33 C31 S2 120.8(5) . . ? C31 C32 N4 116.1(5) . . ? C31 C32 C34 126.1(5) . . ? N4 C32 C34 117.8(4) . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C38 108.9(5) . . ? C35 C34 C32 124.7(5) . . ? C38 C34 C32 126.2(5) . . ? F20 C35 C34 126.8(6) . . ? F20 C35 C36 118.5(6) . . ? C34 C35 C36 114.6(7) . . ? F21 C36 F22 107.5(8) . . ? F21 C36 C35 114.7(8) . . ? F22 C36 C35 110.0(8) . . ? F21 C36 C37 112.3(9) . . ? F22 C36 C37 110.0(10) . . ? C35 C36 C37 102.2(6) . . ? F24 C37 F23 111.3(10) . . ? F24 C37 C36 112.6(8) . . ? F23 C37 C36 104.6(12) . . ? F24 C37 C38 111.8(11) . . ? F23 C37 C38 109.4(8) . . ? C36 C37 C38 106.8(6) . . ? F26 C38 F25 101.8(6) . . ? F26 C38 C34 111.8(6) . . ? F25 C38 C34 112.8(6) . . ? F26 C38 C37 113.7(8) . . ? F25 C38 C37 109.6(6) . . ? C34 C38 C37 107.2(6) . . ? F28 C39 F27 109.6(8) . . ? F28 C39 F29 96.8(9) . . ? F27 C39 F29 99.6(9) . . ? F28 C39 C40 116.1(6) . . ? F27 C39 C40 119.3(6) . . ? F29 C39 C40 111.9(7) . . ? O5 C40 C41 128.0(4) . . ? O5 C40 C39 115.9(4) . . ? C41 C40 C39 115.9(4) . . ? C42 C41 C40 122.0(4) . . ? C42 C41 H41 119.0 . . ? C40 C41 H41 119.0 . . ? O6 C42 C41 128.4(4) . . ? O6 C42 C43 115.0(4) . . ? C41 C42 C43 116.6(4) . . ? F31 C43 F30 109.0(7) . . ? F31 C43 F32 103.3(6) . . ? F30 C43 F32 105.6(7) . . ? F31 C43 C42 112.9(6) . . ? F30 C43 C42 116.6(5) . . ? F32 C43 C42 108.3(6) . . ? F37 C44 F38 108.6(7) . . ? F37 C44 F36 105.4(8) . . ? F38 C44 F36 102.7(8) . . ? F37 C44 C45 114.5(7) . . ? F38 C44 C45 111.1(7) . . ? F36 C44 C45 113.6(6) . . ? O7 C45 C46 127.9(5) . . ? O7 C45 C44 115.7(5) . . ? C46 C45 C44 116.4(6) . . ? C47 C46 C45 123.0(5) . . ? C47 C46 H46 118.5 . . ? C45 C46 H46 118.5 . . ? O8 C47 C46 130.6(5) . . ? O8 C47 C48 112.7(5) . . ? C46 C47 C48 116.7(5) . . ? F33 C48 F34 108.3(7) . . ? F33 C48 F35 105.8(7) . . ? F34 C48 F35 101.3(6) . . ? F33 C48 C47 114.5(5) . . ? F34 C48 C47 115.2(6) . . ? F35 C48 C47 110.7(6) . . ? O5 Cu2 O8 89.56(13) . . ? O5 Cu2 O6 90.48(13) . . ? O8 Cu2 O6 178.87(13) . . ? O5 Cu2 N3 179.56(15) . . ? O8 Cu2 N3 90.64(14) . . ? O6 Cu2 N3 89.31(13) . . ? O5 Cu2 O7 84.97(14) . . ? O8 Cu2 O7 85.18(13) . . ? O6 Cu2 O7 93.70(13) . . ? N3 Cu2 O7 94.67(14) . . ? O5 Cu2 N4 103.53(14) . . ? O8 Cu2 N4 91.51(12) . . ? O6 Cu2 N4 89.58(13) . . ? N3 Cu2 N4 76.85(14) . . ? O7 Cu2 N4 170.88(13) . . ? C25 N3 C29 118.6(4) . . ? C25 N3 Cu2 123.1(3) . . ? C29 N3 Cu2 118.3(3) . . ? C30 N4 C32 111.1(4) . . ? C30 N4 Cu2 107.0(3) . . ? C32 N4 Cu2 141.2(3) . . ? C40 O5 Cu2 123.2(3) . . ? C42 O6 Cu2 122.8(3) . . ? C45 O7 Cu2 120.1(3) . . ? C47 O8 Cu2 125.7(3) . . ? C31 S2 C30 90.6(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 C10 C11 F1 6.7(12) . . . . ? C14 C10 C11 F1 -176.8(7) . . . . ? C8 C10 C11 C12 -176.7(6) . . . . ? C14 C10 C11 C12 -0.1(9) . . . . ? F1 C11 C12 F3 60.8(12) . . . . ? C10 C11 C12 F3 -116.0(10) . . . . ? F1 C11 C12 F2 -57.1(12) . . . . ? C10 C11 C12 F2 126.1(9) . . . . ? F1 C11 C12 C13 -176.5(8) . . . . ? C10 C11 C12 C13 6.6(11) . . . . ? F3 C12 C13 F5 -13.1(11) . . . . ? F2 C12 C13 F5 105.2(10) . . . . ? C11 C12 C13 F5 -135.5(9) . . . . ? F3 C12 C13 F4 -131.2(8) . . . . ? F2 C12 C13 F4 -13.0(10) . . . . ? C11 C12 C13 F4 106.3(8) . . . . ? F3 C12 C13 C14 112.7(8) . . . . ? F2 C12 C13 C14 -129.1(8) . . . . ? C11 C12 C13 C14 -9.8(10) . . . . ? C11 C10 C14 F7 -128.6(6) . . . . ? C8 C10 C14 F7 48.2(8) . . . . ? C11 C10 C14 F6 114.0(7) . . . . ? C8 C10 C14 F6 -69.3(7) . . . . ? C11 C10 C14 C13 -6.3(8) . . . . ? C8 C10 C14 C13 170.5(6) . . . . ? F5 C13 C14 F7 -100.5(10) . . . . ? F4 C13 C14 F7 16.1(11) . . . . ? C12 C13 C14 F7 133.5(8) . . . . ? F5 C13 C14 F6 13.7(11) . . . . ? F4 C13 C14 F6 130.3(8) . . . . ? C12 C13 C14 F6 -112.3(8) . . . . ? F5 C13 C14 C10 136.0(9) . . . . ? F4 C13 C14 C10 -107.4(8) . . . . ? C12 C13 C14 C10 10.0(9) . . . . ? N1 C1 C2 C3 -1.2(8) . . . . ? C1 C2 C3 C4 1.8(8) . . . . ? C2 C3 C4 C5 -1.0(8) . . . . ? C3 C4 C5 N1 -0.3(7) . . . . ? C3 C4 C5 C6 178.0(4) . . . . ? N1 C5 C6 N2 20.9(6) . . . . ? C4 C5 C6 N2 -157.6(4) . . . . ? N1 C5 C6 S1 -157.7(3) . . . . ? C4 C5 C6 S1 23.8(6) . . . . ? C9 C7 C8 N2 -178.5(5) . . . . ? S1 C7 C8 N2 0.7(5) . . . . ? C9 C7 C8 C10 0.5(8) . . . . ? S1 C7 C8 C10 179.6(4) . . . . ? C11 C10 C8 C7 54.0(8) . . . . ? C14 C10 C8 C7 -122.1(6) . . . . ? C11 C10 C8 N2 -127.1(7) . . . . ? C14 C10 C8 N2 56.8(7) . . . . ? F8 C15 C16 O1 178.2(7) . . . . ? F9 C15 C16 O1 53.8(10) . . . . ? F10 C15 C16 O1 -64.8(9) . . . . ? F8 C15 C16 C17 -5.2(11) . . . . ? F9 C15 C16 C17 -129.6(8) . . . . ? F10 C15 C16 C17 111.8(9) . . . . ? O1 C16 C17 C18 8.9(9) . . . . ? C15 C16 C17 C18 -167.1(6) . . . . ? C16 C17 C18 O2 -2.3(9) . . . . ? C16 C17 C18 C19 174.7(5) . . . . ? O2 C18 C19 F12 -33.5(7) . . . . ? C17 C18 C19 F12 149.1(5) . . . . ? O2 C18 C19 F11 -158.7(6) . . . . ? C17 C18 C19 F11 23.8(8) . . . . ? O2 C18 C19 F13 81.3(6) . . . . ? C17 C18 C19 F13 -96.1(6) . . . . ? F14 C20 C21 O3 -102.0(9) . . . . ? F15 C20 C21 O3 19.6(10) . . . . ? F16 C20 C21 O3 139.4(7) . . . . ? F14 C20 C21 C22 79.8(10) . . . . ? F15 C20 C21 C22 -158.7(8) . . . . ? F16 C20 C21 C22 -38.9(10) . . . . ? O3 C21 C22 C23 3.7(13) . . . . ? C20 C21 C22 C23 -178.4(7) . . . . ? C21 C22 C23 O4 4.0(14) . . . . ? C21 C22 C23 C24 -172.0(10) . . . . ? F18 C24 C23 O4 167.7(14) . . . . ? F17 C24 C23 O4 -61.9(18) . . . . ? F19 C24 C23 O4 50.0(14) . . . . ? F18 C24 C23 C22 -16(2) . . . . ? F17 C24 C23 C22 114.7(12) . . . . ? F19 C24 C23 C22 -133.4(10) . . . . ? C4 C5 N1 C1 0.9(6) . . . . ? C6 C5 N1 C1 -177.5(4) . . . . ? C4 C5 N1 Cu1 174.8(3) . . . . ? C6 C5 N1 Cu1 -3.6(5) . . . . ? C2 C1 N1 C5 -0.2(7) . . . . ? C2 C1 N1 Cu1 -174.1(4) . . . . ? O4 Cu1 N1 C5 -105.3(3) . . . . ? O2 Cu1 N1 C5 73.5(3) . . . . ? O3 Cu1 N1 C5 169.1(3) . . . . ? O4 Cu1 N1 C1 68.6(4) . . . . ? O2 Cu1 N1 C1 -112.6(3) . . . . ? O3 Cu1 N1 C1 -17.0(4) . . . . ? C5 C6 N2 C8 -179.0(4) . . . . ? S1 C6 N2 C8 -0.3(5) . . . . ? C7 C8 N2 C6 -0.2(6) . . . . ? C10 C8 N2 C6 -179.2(4) . . . . ? C17 C16 O1 Cu1 -4.6(9) . . . . ? C15 C16 O1 Cu1 171.7(5) . . . . ? O4 Cu1 O1 C16 175.9(5) . . . . ? O2 Cu1 O1 C16 -3.0(5) . . . . ? O3 Cu1 O1 C16 -98.3(5) . . . . ? C17 C18 O2 Cu1 -7.2(7) . . . . ? C19 C18 O2 Cu1 175.6(4) . . . . ? O1 Cu1 O2 C18 8.4(4) . . . . ? N1 Cu1 O2 C18 -168.7(3) . . . . ? O3 Cu1 O2 C18 93.8(3) . . . . ? C22 C21 O3 Cu1 -27.2(9) . . . . ? C20 C21 O3 Cu1 154.8(5) . . . . ? O1 Cu1 O3 C21 -54.6(4) . . . . ? O4 Cu1 O3 C21 34.8(4) . . . . ? O2 Cu1 O3 C21 -144.7(4) . . . . ? N1 Cu1 O3 C21 122.9(4) . . . . ? C22 C23 O4 Cu1 20.8(12) . . . . ? C24 C23 O4 Cu1 -163.0(9) . . . . ? O1 Cu1 O4 C23 53.3(6) . . . . ? N1 Cu1 O4 C23 -129.5(6) . . . . ? O3 Cu1 O4 C23 -32.1(6) . . . . ? N2 C6 S1 C7 0.6(4) . . . . ? C5 C6 S1 C7 179.3(4) . . . . ? C8 C7 S1 C6 -0.7(4) . . . . ? C9 C7 S1 C6 178.5(5) . . . . ? N3 C25 C26 C27 -0.4(9) . . . . ? C25 C26 C27 C28 1.3(10) . . . . ? C26 C27 C28 C29 -2.1(10) . . . . ? C27 C28 C29 N3 2.0(8) . . . . ? C27 C28 C29 C30 -175.2(5) . . . . ? N3 C29 C30 N4 -4.6(6) . . . . ? C28 C29 C30 N4 172.7(5) . . . . ? N3 C29 C30 S2 177.8(3) . . . . ? C28 C29 C30 S2 -4.9(7) . . . . ? C33 C31 C32 N4 -179.9(6) . . . . ? S2 C31 C32 N4 1.0(6) . . . . ? C33 C31 C32 C34 2.3(10) . . . . ? S2 C31 C32 C34 -176.7(4) . . . . ? C31 C32 C34 C35 109.2(7) . . . . ? N4 C32 C34 C35 -68.5(7) . . . . ? C31 C32 C34 C38 -75.9(8) . . . . ? N4 C32 C34 C38 106.4(6) . . . . ? C38 C34 C35 F20 -177.2(7) . . . . ? C32 C34 C35 F20 -1.6(11) . . . . ? C38 C34 C35 C36 2.9(8) . . . . ? C32 C34 C35 C36 178.6(6) . . . . ? F20 C35 C36 F21 58.1(11) . . . . ? C34 C35 C36 F21 -122.1(9) . . . . ? F20 C35 C36 F22 -63.3(11) . . . . ? C34 C35 C36 F22 116.6(10) . . . . ? F20 C35 C36 C37 179.9(8) . . . . ? C34 C35 C36 C37 -0.2(9) . . . . ? F21 C36 C37 F24 -2.0(14) . . . . ? F22 C36 C37 F24 117.7(12) . . . . ? C35 C36 C37 F24 -125.5(11) . . . . ? F21 C36 C37 F23 -123.0(9) . . . . ? F22 C36 C37 F23 -3.4(11) . . . . ? C35 C36 C37 F23 113.5(8) . . . . ? F21 C36 C37 C38 121.1(8) . . . . ? F22 C36 C37 C38 -119.3(8) . . . . ? C35 C36 C37 C38 -2.4(10) . . . . ? C35 C34 C38 F26 120.9(7) . . . . ? C32 C34 C38 F26 -54.7(9) . . . . ? C35 C34 C38 F25 -125.1(7) . . . . ? C32 C34 C38 F25 59.3(9) . . . . ? C35 C34 C38 C37 -4.3(8) . . . . ? C32 C34 C38 C37 -179.9(6) . . . . ? F24 C37 C38 F26 3.7(11) . . . . ? F23 C37 C38 F26 127.5(12) . . . . ? C36 C37 C38 F26 -119.9(8) . . . . ? F24 C37 C38 F25 -109.5(10) . . . . ? F23 C37 C38 F25 14.3(14) . . . . ? C36 C37 C38 F25 126.9(8) . . . . ? F24 C37 C38 C34 127.8(9) . . . . ? F23 C37 C38 C34 -108.5(12) . . . . ? C36 C37 C38 C34 4.2(10) . . . . ? F28 C39 C40 O5 45.6(12) . . . . ? F27 C39 C40 O5 -179.8(9) . . . . ? F29 C39 C40 O5 -64.2(12) . . . . ? F28 C39 C40 C41 -131.1(10) . . . . ? F27 C39 C40 C41 3.5(12) . . . . ? F29 C39 C40 C41 119.1(11) . . . . ? O5 C40 C41 C42 1.7(9) . . . . ? C39 C40 C41 C42 177.9(6) . . . . ? C40 C41 C42 O6 -5.8(9) . . . . ? C40 C41 C42 C43 173.7(6) . . . . ? O6 C42 C43 F31 -38.8(9) . . . . ? C41 C42 C43 F31 141.6(7) . . . . ? O6 C42 C43 F30 -166.3(7) . . . . ? C41 C42 C43 F30 14.1(10) . . . . ? O6 C42 C43 F32 75.0(8) . . . . ? C41 C42 C43 F32 -104.6(6) . . . . ? F37 C44 C45 O7 -40.1(10) . . . . ? F38 C44 C45 O7 83.5(8) . . . . ? F36 C44 C45 O7 -161.3(7) . . . . ? F37 C44 C45 C46 140.9(8) . . . . ? F38 C44 C45 C46 -95.5(8) . . . . ? F36 C44 C45 C46 19.7(10) . . . . ? O7 C45 C46 C47 0.3(9) . . . . ? C44 C45 C46 C47 179.2(6) . . . . ? C45 C46 C47 O8 -4.4(9) . . . . ? C45 C46 C47 C48 176.7(5) . . . . ? O8 C47 C48 F33 46.2(8) . . . . ? C46 C47 C48 F33 -134.7(7) . . . . ? O8 C47 C48 F34 172.7(7) . . . . ? C46 C47 C48 F34 -8.2(9) . . . . ? O8 C47 C48 F35 -73.1(7) . . . . ? C46 C47 C48 F35 105.9(7) . . . . ? C26 C25 N3 C29 0.3(7) . . . . ? C26 C25 N3 Cu2 -179.6(4) . . . . ? C28 C29 N3 C25 -1.1(7) . . . . ? C30 C29 N3 C25 176.3(4) . . . . ? C28 C29 N3 Cu2 178.8(4) . . . . ? C30 C29 N3 Cu2 -3.8(5) . . . . ? O8 Cu2 N3 C25 -82.4(4) . . . . ? O6 Cu2 N3 C25 96.5(4) . . . . ? O7 Cu2 N3 C25 2.8(4) . . . . ? N4 Cu2 N3 C25 -173.8(4) . . . . ? O8 Cu2 N3 C29 97.8(3) . . . . ? O6 Cu2 N3 C29 -83.3(3) . . . . ? O7 Cu2 N3 C29 -177.0(3) . . . . ? N4 Cu2 N3 C29 6.4(3) . . . . ? C29 C30 N4 C32 -178.3(4) . . . . ? S2 C30 N4 C32 -0.5(5) . . . . ? C29 C30 N4 Cu2 9.1(5) . . . . ? S2 C30 N4 Cu2 -173.1(2) . . . . ? C31 C32 N4 C30 -0.4(6) . . . . ? C34 C32 N4 C30 177.6(4) . . . . ? C31 C32 N4 Cu2 168.3(4) . . . . ? C34 C32 N4 Cu2 -13.7(7) . . . . ? O5 Cu2 N4 C30 171.8(3) . . . . ? O8 Cu2 N4 C30 -98.3(3) . . . . ? O6 Cu2 N4 C30 81.4(3) . . . . ? N3 Cu2 N4 C30 -8.0(3) . . . . ? O5 Cu2 N4 C32 2.8(5) . . . . ? O8 Cu2 N4 C32 92.7(5) . . . . ? O6 Cu2 N4 C32 -87.6(5) . . . . ? N3 Cu2 N4 C32 -177.0(5) . . . . ? C41 C40 O5 Cu2 17.4(7) . . . . ? C39 C40 O5 Cu2 -158.9(4) . . . . ? O8 Cu2 O5 C40 155.4(4) . . . . ? O6 Cu2 O5 C40 -23.5(4) . . . . ? O7 Cu2 O5 C40 70.2(4) . . . . ? N4 Cu2 O5 C40 -113.2(4) . . . . ? C41 C42 O6 Cu2 -9.6(8) . . . . ? C43 C42 O6 Cu2 170.8(5) . . . . ? O5 Cu2 O6 C42 20.0(4) . . . . ? N3 Cu2 O6 C42 -159.6(4) . . . . ? O7 Cu2 O6 C42 -65.0(4) . . . . ? N4 Cu2 O6 C42 123.5(4) . . . . ? C46 C45 O7 Cu2 19.6(8) . . . . ? C44 C45 O7 Cu2 -159.2(4) . . . . ? O5 Cu2 O7 C45 63.0(4) . . . . ? O8 Cu2 O7 C45 -27.0(4) . . . . ? O6 Cu2 O7 C45 153.2(4) . . . . ? N3 Cu2 O7 C45 -117.2(4) . . . . ? C46 C47 O8 Cu2 -16.4(7) . . . . ? C48 C47 O8 Cu2 162.5(4) . . . . ? O5 Cu2 O8 C47 -59.7(4) . . . . ? N3 Cu2 O8 C47 119.9(4) . . . . ? O7 Cu2 O8 C47 25.3(4) . . . . ? N4 Cu2 O8 C47 -163.2(4) . . . . ? C32 C31 S2 C30 -1.1(4) . . . . ? C33 C31 S2 C30 179.8(5) . . . . ? N4 C30 S2 C31 0.9(4) . . . . ? C29 C30 S2 C31 178.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.933 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.069 data_(hfac)2Zn-1o-Zn(hfac)2 _database_code_depnum_ccdc_archive 'CCDC 715798' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H18 F30 N4 O8 S2 Zn2 ' _chemical_formula_sum 'C43 H18 F30 N4 O8 S2 Zn2 ' _chemical_formula_weight 1483.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0031 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 0.0109 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0176 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1250 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2863 1.4353 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n' _symmetry_int_tables_number 86 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 17.681(5) _cell_length_b 17.681(5) _cell_length_c 17.726(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 5542(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 7388 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 29.51 _exptl_crystal_description cube _exptl_crystal_colour none _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2920 _exptl_absorpt_coefficient_mu 1.095 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.849 _exptl_absorpt_correction_T_max 0.849 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_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 55891 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 30.76 _reflns_number_total 7680 _reflns_number_gt 5718 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0962P)^2^+12.2457P] 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_number_reflns 7680 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1767 _refine_ls_wR_factor_gt 0.1553 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.011 _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 C1 C 0.86062(19) 0.23844(18) 0.55955(19) 0.0227(6) Uani 1 1 d . . . C3 C 0.8573(2) 0.32190(19) 0.5732(2) 0.0342(9) Uani 1 1 d . . . H3A H 0.8464 0.3475 0.5267 0.051 Uiso 1 1 calc R . . H3B H 0.9050 0.3390 0.5925 0.051 Uiso 1 1 calc R . . H3C H 0.8182 0.3328 0.6092 0.051 Uiso 1 1 calc R . . C4 C 0.82397(17) 0.19524(16) 0.50730(16) 0.0171(5) Uani 1 1 d . . . C5 C 0.89092(17) 0.10415(16) 0.56134(17) 0.0171(5) Uani 1 1 d . . . C6 C 0.92130(17) 0.02766(16) 0.57173(17) 0.0177(6) Uani 1 1 d . . . C7 C 0.98692(18) 0.01263(18) 0.61159(17) 0.0201(6) Uani 1 1 d . . . H7 H 1.0129 0.0512 0.6361 0.024 Uiso 1 1 calc R . . C8 C 1.01304(18) -0.06149(18) 0.61413(19) 0.0221(6) Uani 1 1 d . . . H8 H 1.0571 -0.0733 0.6403 0.027 Uiso 1 1 calc R . . C9 C 0.97297(19) -0.11740(18) 0.5774(2) 0.0238(7) Uani 1 1 d . . . H9 H 0.9895 -0.1673 0.5785 0.029 Uiso 1 1 calc R . . C10 C 0.90779(19) -0.09793(17) 0.53879(19) 0.0223(6) Uani 1 1 d . . . H10 H 0.8808 -0.1356 0.5140 0.027 Uiso 1 1 calc R . . C11 C 0.77888(17) 0.22555(16) 0.44426(16) 0.0164(5) Uani 1 1 d . . . C12 C 0.80486(18) 0.20922(17) 0.36519(18) 0.0205(6) Uani 1 1 d . . . C13 C 0.7647(4) 0.2610(3) 0.31409(16) 0.0225(17) Uani 0.50 1 d P . . C14 C 0.5777(2) 0.0531(2) 0.3616(2) 0.0328(8) Uani 1 1 d . . . C15 C 0.66139(18) 0.03403(18) 0.37483(19) 0.0226(6) Uani 1 1 d . . . C16 C 0.69866(19) -0.00644(18) 0.31842(19) 0.0235(6) Uani 1 1 d . . . H16 H 0.6721 -0.0203 0.2753 0.028 Uiso 1 1 calc R . . C17 C 0.77417(18) -0.02670(17) 0.32466(18) 0.0211(6) Uani 1 1 d . . . C18 C 0.8113(2) -0.0641(2) 0.2560(2) 0.0341(8) Uani 1 1 d . . . C19 C 0.6301(4) -0.1854(3) 0.4976(4) 0.0638(17) Uani 1 1 d . . . C20 C 0.6777(2) -0.1180(2) 0.5272(2) 0.0328(8) Uani 1 1 d . . . C21 C 0.6592(3) -0.0897(2) 0.5972(2) 0.0431(10) Uani 1 1 d . . . H21 H 0.6231 -0.1147 0.6262 0.052 Uiso 1 1 calc R . . C22 C 0.6931(2) -0.0246(2) 0.6257(2) 0.0330(8) Uani 1 1 d . . . C23 C 0.6745(3) -0.0037(3) 0.7078(2) 0.0524(13) Uani 1 1 d . . . N1 N 0.88227(15) -0.02659(14) 0.53596(15) 0.0195(5) Uani 1 1 d . . . N2 N 0.84104(15) 0.11899(14) 0.50909(14) 0.0167(5) Uani 1 1 d . . . O1 O 0.68686(12) 0.05656(13) 0.43697(13) 0.0222(5) Uani 1 1 d . . . O2 O 0.81876(12) -0.01784(12) 0.37870(13) 0.0212(4) Uani 1 1 d . . . O3 O 0.72630(14) -0.09558(13) 0.48226(14) 0.0258(5) Uani 1 1 d . . . O4 O 0.73689(14) 0.02107(13) 0.59403(13) 0.0241(5) Uani 1 1 d . . . F1 F 0.80766(14) 0.13629(11) 0.34732(11) 0.0338(5) Uani 1 1 d . . . F2 F 0.87496(18) 0.2352(2) 0.35486(17) 0.0740(12) Uani 1 1 d . . . F3 F 0.7413(3) 0.22687(19) 0.2515(2) 0.0354(12) Uani 0.50 1 d P . . F4 F 0.8069(2) 0.31865(18) 0.2906(2) 0.0317(10) Uani 0.50 1 d P . . F5 F 0.55884(13) 0.11811(14) 0.39246(17) 0.0471(7) Uani 1 1 d . . . F6 F 0.53427(14) 0.00051(17) 0.3920(2) 0.0641(9) Uani 1 1 d . . . F7 F 0.55951(17) 0.0566(2) 0.28930(17) 0.0695(10) Uani 1 1 d . . . F8 F 0.76665(18) -0.0740(2) 0.19851(17) 0.0723(10) Uani 1 1 d . . . F9 F 0.8691(3) -0.0261(3) 0.2336(2) 0.136(3) Uani 1 1 d . . . F10 F 0.8364(3) -0.1306(3) 0.2720(2) 0.127(2) Uani 1 1 d . . . F11 F 0.66571(18) -0.23007(16) 0.4551(2) 0.0640(9) Uani 1 1 d . . . F12 F 0.5740(3) -0.1562(3) 0.4475(4) 0.1140(18) Uani 1 1 d . . . F13 F 0.5871(2) -0.2159(2) 0.5461(2) 0.0881(14) Uani 1 1 d . . . F14 F 0.7338(3) -0.0091(3) 0.74973(19) 0.1070(18) Uani 1 1 d . . . F15 F 0.6243(4) -0.0500(3) 0.7392(2) 0.125(2) Uani 1 1 d . . . F16 F 0.6502(2) 0.06481(18) 0.71542(16) 0.0741(11) Uani 1 1 d . . . S S 0.91911(5) 0.18126(4) 0.61243(5) 0.02541(19) Uani 1 1 d . . . Zn Zn 0.78103(2) 0.009384(19) 0.48524(2) 0.01744(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0267(16) 0.0180(14) 0.0232(15) 0.0007(12) -0.0064(12) 0.0036(12) C3 0.049(2) 0.0155(15) 0.038(2) -0.0041(14) -0.0195(17) 0.0053(14) C4 0.0193(14) 0.0146(13) 0.0173(13) 0.0019(10) 0.0018(11) 0.0029(10) C5 0.0180(13) 0.0153(13) 0.0180(13) 0.0009(10) 0.0003(11) 0.0014(10) C6 0.0210(14) 0.0152(13) 0.0171(13) 0.0032(10) 0.0008(11) 0.0015(11) C7 0.0208(14) 0.0206(14) 0.0190(13) 0.0031(11) -0.0013(11) 0.0015(11) C8 0.0195(14) 0.0220(15) 0.0249(15) 0.0082(12) -0.0008(12) 0.0042(12) C9 0.0249(15) 0.0156(14) 0.0310(17) 0.0060(12) 0.0036(13) 0.0047(11) C10 0.0259(16) 0.0151(14) 0.0259(15) 0.0027(12) 0.0023(13) 0.0010(12) C11 0.0212(14) 0.0132(12) 0.0148(12) 0.0007(10) 0.0010(11) 0.0020(10) C12 0.0269(15) 0.0158(14) 0.0188(13) 0.0000(11) 0.0043(12) 0.0025(11) C13 0.021(5) 0.029(5) 0.017(2) 0.000(3) 0.001(2) 0.009(3) C14 0.0253(17) 0.0335(19) 0.039(2) -0.0066(16) -0.0082(15) 0.0038(14) C15 0.0202(14) 0.0214(15) 0.0263(15) -0.0025(12) -0.0037(12) 0.0007(12) C16 0.0254(15) 0.0223(15) 0.0227(14) -0.0045(12) -0.0044(12) -0.0006(12) C17 0.0269(16) 0.0172(14) 0.0190(14) -0.0017(11) 0.0033(12) -0.0014(11) C18 0.0331(19) 0.043(2) 0.0264(17) -0.0128(15) 0.0052(14) 0.0022(16) C19 0.078(4) 0.040(3) 0.074(4) -0.020(3) 0.033(3) -0.030(3) C20 0.041(2) 0.0199(16) 0.0375(19) -0.0035(14) 0.0098(16) -0.0080(14) C21 0.058(3) 0.034(2) 0.038(2) -0.0027(17) 0.023(2) -0.0127(18) C22 0.048(2) 0.0286(18) 0.0222(16) 0.0005(14) 0.0106(15) 0.0036(16) C23 0.091(4) 0.041(2) 0.0252(19) -0.0005(17) 0.019(2) -0.001(2) N1 0.0211(13) 0.0165(12) 0.0209(12) 0.0033(10) 0.0002(10) 0.0024(10) N2 0.0185(12) 0.0136(11) 0.0179(11) 0.0017(9) -0.0005(9) 0.0014(9) O1 0.0210(11) 0.0226(11) 0.0229(11) -0.0042(9) -0.0023(9) 0.0045(8) O2 0.0220(11) 0.0199(10) 0.0217(11) -0.0008(8) 0.0013(8) 0.0011(8) O3 0.0329(13) 0.0175(11) 0.0271(12) -0.0019(9) 0.0068(10) -0.0028(9) O4 0.0279(12) 0.0240(11) 0.0205(11) -0.0027(9) 0.0012(9) 0.0013(9) F1 0.0641(15) 0.0151(9) 0.0220(10) -0.0023(7) 0.0049(10) 0.0070(9) F2 0.0624(18) 0.115(3) 0.0449(16) -0.0350(17) 0.0355(14) -0.0615(19) F3 0.052(3) 0.037(3) 0.0175(17) -0.0118(14) -0.0107(19) 0.018(3) F4 0.038(2) 0.024(2) 0.033(2) 0.0154(17) 0.0167(18) 0.0136(17) F5 0.0297(12) 0.0422(14) 0.0695(18) -0.0188(13) -0.0105(12) 0.0156(10) F6 0.0260(12) 0.0516(16) 0.115(3) 0.0072(17) -0.0005(15) -0.0078(11) F7 0.0464(16) 0.117(3) 0.0452(16) -0.0183(17) -0.0226(13) 0.0333(17) F8 0.0606(19) 0.115(3) 0.0417(16) -0.0448(17) -0.0058(14) 0.0221(18) F9 0.116(3) 0.201(5) 0.090(3) -0.096(3) 0.084(3) -0.108(4) F10 0.212(5) 0.108(3) 0.059(2) -0.008(2) 0.030(3) 0.118(4) F11 0.0592(18) 0.0428(15) 0.090(2) -0.0349(16) 0.0124(17) -0.0125(13) F12 0.092(3) 0.085(3) 0.165(5) -0.030(3) -0.061(3) -0.010(2) F13 0.097(3) 0.063(2) 0.105(3) -0.028(2) 0.047(2) -0.051(2) F14 0.160(4) 0.130(4) 0.0311(16) -0.0278(19) -0.030(2) 0.073(3) F15 0.220(6) 0.098(3) 0.056(2) -0.027(2) 0.083(3) -0.070(3) F16 0.132(3) 0.0562(18) 0.0342(14) -0.0037(13) 0.0291(17) 0.0352(19) S 0.0328(4) 0.0169(4) 0.0265(4) -0.0013(3) -0.0131(3) 0.0028(3) Zn 0.01833(19) 0.01580(19) 0.01818(19) -0.00058(12) -0.00051(13) 0.00137(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C4 1.364(4) . ? C1 C3 1.497(4) . ? C1 S 1.724(3) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 N2 1.382(4) . ? C4 C11 1.474(4) . ? C5 N2 1.306(4) . ? C5 C6 1.467(4) . ? C5 S 1.711(3) . ? C6 N1 1.341(4) . ? C6 C7 1.384(4) . ? C7 C8 1.390(4) . ? C7 H7 0.9300 . ? C8 C9 1.380(5) . ? C8 H8 0.9300 . ? C9 C10 1.383(5) . ? C9 H9 0.9300 . ? C10 N1 1.340(4) . ? C10 H10 0.9300 . ? C11 C12 1.503(4) . ? C12 F1 1.329(4) . ? C12 F2 1.335(4) . ? C12 C13 1.470(8) . ? C13 F3 1.3298(11) . ? C13 F4 1.3298(11) . ? C14 F5 1.316(4) . ? C14 F6 1.321(5) . ? C14 F7 1.323(5) . ? C14 C15 1.535(5) . ? C15 O1 1.255(4) . ? C15 C16 1.395(5) . ? C16 C17 1.387(5) . ? C16 H16 0.9300 . ? C17 O2 1.251(4) . ? C17 C18 1.532(5) . ? C18 F9 1.286(5) . ? C18 F10 1.287(6) . ? C18 F8 1.301(5) . ? C19 F11 1.260(6) . ? C19 F13 1.268(6) . ? C19 F12 1.429(9) . ? C19 C20 1.551(6) . ? C20 O3 1.237(4) . ? C20 C21 1.378(6) . ? C21 C22 1.392(6) . ? C21 H21 0.9300 . ? C22 O4 1.252(5) . ? C22 C23 1.537(5) . ? C23 F14 1.289(7) . ? C23 F16 1.292(6) . ? C23 F15 1.331(6) . ? N1 Zn 2.102(3) . ? N2 Zn 2.250(3) . ? O1 Zn 2.049(2) . ? O2 Zn 2.060(2) . ? O3 Zn 2.094(2) . ? O4 Zn 2.090(2) . ? 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 C4 C1 C3 130.0(3) . . ? C4 C1 S 109.0(2) . . ? C3 C1 S 120.9(2) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 N2 115.3(3) . . ? C1 C4 C11 124.6(3) . . ? N2 C4 C11 119.4(3) . . ? N2 C5 C6 121.4(3) . . ? N2 C5 S 114.3(2) . . ? C6 C5 S 124.2(2) . . ? N1 C6 C7 122.4(3) . . ? N1 C6 C5 114.3(3) . . ? C7 C6 C5 123.2(3) . . ? C6 C7 C8 118.4(3) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C9 C8 C7 119.3(3) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 118.9(3) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N1 C10 C9 122.2(3) . . ? N1 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C4 C11 C12 118.2(3) . . ? F1 C12 F2 105.5(3) . . ? F1 C12 C13 118.4(3) . . ? F2 C12 C13 98.6(3) . . ? F1 C12 C11 114.8(3) . . ? F2 C12 C11 110.2(3) . . ? C13 C12 C11 107.9(3) . . ? F3 C13 F4 105.10(11) . . ? F3 C13 C12 112.4(5) . . ? F4 C13 C12 113.6(5) . . ? F5 C14 F6 107.3(3) . . ? F5 C14 F7 107.5(3) . . ? F6 C14 F7 106.7(4) . . ? F5 C14 C15 111.9(3) . . ? F6 C14 C15 110.1(3) . . ? F7 C14 C15 113.1(3) . . ? O1 C15 C16 128.5(3) . . ? O1 C15 C14 114.2(3) . . ? C16 C15 C14 117.3(3) . . ? C17 C16 C15 122.0(3) . . ? C17 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? O2 C17 C16 129.5(3) . . ? O2 C17 C18 113.1(3) . . ? C16 C17 C18 117.4(3) . . ? F9 C18 F10 105.7(5) . . ? F9 C18 F8 108.1(4) . . ? F10 C18 F8 105.0(4) . . ? F9 C18 C17 111.1(3) . . ? F10 C18 C17 111.5(3) . . ? F8 C18 C17 114.9(3) . . ? F11 C19 F13 116.0(5) . . ? F11 C19 F12 101.7(5) . . ? F13 C19 F12 99.1(5) . . ? F11 C19 C20 114.4(4) . . ? F13 C19 C20 115.0(5) . . ? F12 C19 C20 108.0(4) . . ? O3 C20 C21 129.0(4) . . ? O3 C20 C19 113.9(4) . . ? C21 C20 C19 117.0(4) . . ? C20 C21 C22 121.6(4) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? O4 C22 C21 129.6(3) . . ? O4 C22 C23 113.6(4) . . ? C21 C22 C23 116.8(4) . . ? F14 C23 F16 106.3(5) . . ? F14 C23 F15 104.8(5) . . ? F16 C23 F15 108.1(5) . . ? F14 C23 C22 110.7(4) . . ? F16 C23 C22 113.4(4) . . ? F15 C23 C22 113.0(4) . . ? C10 N1 C6 118.8(3) . . ? C10 N1 Zn 126.0(2) . . ? C6 N1 Zn 115.1(2) . . ? C5 N2 C4 111.1(3) . . ? C5 N2 Zn 106.19(19) . . ? C4 N2 Zn 137.1(2) . . ? C15 O1 Zn 121.9(2) . . ? C17 O2 Zn 121.8(2) . . ? C20 O3 Zn 126.0(2) . . ? C22 O4 Zn 125.5(2) . . ? C5 S C1 90.28(15) . . ? O1 Zn O2 88.59(9) . . ? O1 Zn O4 92.39(9) . . ? O2 Zn O4 171.76(9) . . ? O1 Zn O3 88.56(10) . . ? O2 Zn O3 85.38(9) . . ? O4 Zn O3 86.46(9) . . ? O1 Zn N1 173.58(10) . . ? O2 Zn N1 92.61(10) . . ? O4 Zn N1 87.32(10) . . ? O3 Zn N1 97.82(10) . . ? O1 Zn N2 96.37(9) . . ? O2 Zn N2 102.76(9) . . ? O4 Zn N2 85.27(9) . . ? O3 Zn N2 170.54(9) . . ? N1 Zn N2 77.21(9) . . ? 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 C3 C1 C4 N2 178.9(4) . . . . ? S C1 C4 N2 0.4(4) . . . . ? C3 C1 C4 C11 8.8(6) . . . . ? S C1 C4 C11 -169.6(2) . . . . ? N2 C5 C6 N1 -14.1(4) . . . . ? S C5 C6 N1 168.5(2) . . . . ? N2 C5 C6 C7 162.6(3) . . . . ? S C5 C6 C7 -14.8(4) . . . . ? N1 C6 C7 C8 0.2(5) . . . . ? C5 C6 C7 C8 -176.2(3) . . . . ? C6 C7 C8 C9 -0.2(5) . . . . ? C7 C8 C9 C10 0.1(5) . . . . ? C8 C9 C10 N1 0.0(5) . . . . ? C1 C4 C11 C11 -54.1(6) . . . 2_655 ? N2 C4 C11 C11 136.2(4) . . . 2_655 ? C1 C4 C11 C12 116.8(3) . . . . ? N2 C4 C11 C12 -52.8(4) . . . . ? C11 C11 C12 F1 -126.6(4) 2_655 . . . ? C4 C11 C12 F1 60.8(4) . . . . ? C11 C11 C12 F2 114.5(4) 2_655 . . . ? C4 C11 C12 F2 -58.1(4) . . . . ? C11 C11 C12 C13 7.8(4) 2_655 . . . ? C4 C11 C12 C13 -164.8(3) . . . . ? C11 C11 C12 C13 -16.3(4) 2_655 . . 2_655 ? C4 C11 C12 C13 171.1(3) . . . 2_655 ? F1 C12 C13 C13 50.7(11) . . . 2_655 ? F2 C12 C13 C13 163.5(9) . . . 2_655 ? C11 C12 C13 C13 -81.9(9) . . . 2_655 ? F1 C12 C13 F3 -43.6(8) . . . 2_655 ? F2 C12 C13 F3 69.3(7) . . . 2_655 ? C11 C12 C13 F3 -176.1(6) . . . 2_655 ? C13 C12 C13 F3 -94.3(10) 2_655 . . 2_655 ? F1 C12 C13 F3 -5.4(5) . . . . ? F2 C12 C13 F3 107.4(4) . . . . ? C11 C12 C13 F3 -138.0(4) . . . . ? C13 C12 C13 F3 -56.1(7) 2_655 . . . ? F1 C12 C13 F4 -124.6(4) . . . . ? F2 C12 C13 F4 -11.8(5) . . . . ? C11 C12 C13 F4 102.8(4) . . . . ? C13 C12 C13 F4 -175.3(13) 2_655 . . . ? F1 C12 C13 C12 115.7(4) . . . 2_655 ? F2 C12 C13 C12 -131.5(3) . . . 2_655 ? C11 C12 C13 C12 -16.9(2) . . . 2_655 ? C13 C12 C13 C12 65.0(9) 2_655 . . 2_655 ? F5 C14 C15 O1 33.7(5) . . . . ? F6 C14 C15 O1 -85.5(4) . . . . ? F7 C14 C15 O1 155.3(3) . . . . ? F5 C14 C15 C16 -147.4(3) . . . . ? F6 C14 C15 C16 93.4(4) . . . . ? F7 C14 C15 C16 -25.8(5) . . . . ? O1 C15 C16 C17 -1.2(6) . . . . ? C14 C15 C16 C17 -179.9(3) . . . . ? C15 C16 C17 O2 4.5(6) . . . . ? C15 C16 C17 C18 -174.1(3) . . . . ? O2 C17 C18 F9 -56.7(5) . . . . ? C16 C17 C18 F9 122.1(5) . . . . ? O2 C17 C18 F10 61.0(5) . . . . ? C16 C17 C18 F10 -120.3(5) . . . . ? O2 C17 C18 F8 -179.7(4) . . . . ? C16 C17 C18 F8 -1.0(5) . . . . ? F11 C19 C20 O3 32.9(7) . . . . ? F13 C19 C20 O3 170.9(5) . . . . ? F12 C19 C20 O3 -79.5(5) . . . . ? F11 C19 C20 C21 -149.2(5) . . . . ? F13 C19 C20 C21 -11.2(8) . . . . ? F12 C19 C20 C21 98.4(6) . . . . ? O3 C20 C21 C22 4.1(8) . . . . ? C19 C20 C21 C22 -173.4(5) . . . . ? C20 C21 C22 O4 7.5(8) . . . . ? C20 C21 C22 C23 -173.4(5) . . . . ? O4 C22 C23 F14 -66.8(5) . . . . ? C21 C22 C23 F14 113.9(5) . . . . ? O4 C22 C23 F16 52.6(6) . . . . ? C21 C22 C23 F16 -126.7(5) . . . . ? O4 C22 C23 F15 176.0(5) . . . . ? C21 C22 C23 F15 -3.3(7) . . . . ? C9 C10 N1 C6 0.0(5) . . . . ? C9 C10 N1 Zn -176.0(2) . . . . ? C7 C6 N1 C10 -0.1(5) . . . . ? C5 C6 N1 C10 176.6(3) . . . . ? C7 C6 N1 Zn 176.3(2) . . . . ? C5 C6 N1 Zn -6.9(3) . . . . ? C6 C5 N2 C4 -176.7(3) . . . . ? S C5 N2 C4 1.0(3) . . . . ? C6 C5 N2 Zn 24.8(3) . . . . ? S C5 N2 Zn -157.52(15) . . . . ? C1 C4 N2 C5 -0.9(4) . . . . ? C11 C4 N2 C5 169.7(3) . . . . ? C1 C4 N2 Zn 147.9(3) . . . . ? C11 C4 N2 Zn -41.5(4) . . . . ? C16 C15 O1 Zn -20.5(5) . . . . ? C14 C15 O1 Zn 158.3(2) . . . . ? C16 C17 O2 Zn 14.7(5) . . . . ? C18 C17 O2 Zn -166.7(2) . . . . ? C21 C20 O3 Zn -15.7(7) . . . . ? C19 C20 O3 Zn 161.9(4) . . . . ? C21 C22 O4 Zn -4.8(6) . . . . ? C23 C22 O4 Zn 176.0(3) . . . . ? C13 C13 F3 F3 141.3(18) 2_655 . . 2_655 ? F4 C13 F3 F3 -18.3(8) . . . 2_655 ? C12 C13 F3 F3 -142.3(8) . . . 2_655 ? C12 C13 F3 F3 102.1(7) 2_655 . . 2_655 ? F3 C13 F3 C13 -141.3(18) 2_655 . . 2_655 ? F4 C13 F3 C13 -160(2) . . . 2_655 ? C12 C13 F3 C13 76.5(13) . . . 2_655 ? C12 C13 F3 C13 -39.1(12) 2_655 . . 2_655 ? C13 C13 F3 F4 -11.7(15) 2_655 . . 2_655 ? F3 C13 F3 F4 -152.9(8) 2_655 . . 2_655 ? F4 C13 F3 F4 -171.2(5) . . . 2_655 ? C12 C13 F3 F4 64.8(4) . . . 2_655 ? C12 C13 F3 F4 -50.8(4) 2_655 . . 2_655 ? C13 C13 F4 F3 -33(3) 2_655 . . 2_655 ? F3 C13 F4 F3 12.8(5) . . . 2_655 ? C12 C13 F4 F3 136.1(7) . . . 2_655 ? C12 C13 F4 F3 -108.6(6) 2_655 . . 2_655 ? N2 C5 S C1 -0.6(3) . . . . ? C6 C5 S C1 176.9(3) . . . . ? C4 C1 S C5 0.1(3) . . . . ? C3 C1 S C5 -178.5(3) . . . . ? C15 O1 Zn O2 27.9(3) . . . . ? C15 O1 Zn O4 -143.9(3) . . . . ? C15 O1 Zn O3 -57.5(3) . . . . ? C15 O1 Zn N2 130.6(3) . . . . ? C17 O2 Zn O1 -25.3(2) . . . . ? C17 O2 Zn O3 63.4(2) . . . . ? C17 O2 Zn N1 161.0(2) . . . . ? C17 O2 Zn N2 -121.5(2) . . . . ? C22 O4 Zn O1 84.6(3) . . . . ? C22 O4 Zn O3 -3.8(3) . . . . ? C22 O4 Zn N1 -101.8(3) . . . . ? C22 O4 Zn N2 -179.2(3) . . . . ? C20 O3 Zn O1 -79.3(3) . . . . ? C20 O3 Zn O2 -168.0(3) . . . . ? C20 O3 Zn O4 13.2(3) . . . . ? C20 O3 Zn N1 100.0(3) . . . . ? C10 N1 Zn O2 -66.6(3) . . . . ? C6 N1 Zn O2 117.3(2) . . . . ? C10 N1 Zn O4 105.2(3) . . . . ? C6 N1 Zn O4 -71.0(2) . . . . ? C10 N1 Zn O3 19.1(3) . . . . ? C6 N1 Zn O3 -157.0(2) . . . . ? C10 N1 Zn N2 -169.1(3) . . . . ? C6 N1 Zn N2 14.8(2) . . . . ? C5 N2 Zn O1 159.8(2) . . . . ? C4 N2 Zn O1 10.0(3) . . . . ? C5 N2 Zn O2 -110.2(2) . . . . ? C4 N2 Zn O2 100.0(3) . . . . ? C5 N2 Zn O4 67.9(2) . . . . ? C4 N2 Zn O4 -81.8(3) . . . . ? C5 N2 Zn N1 -20.38(19) . . . . ? C4 N2 Zn N1 -170.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.002 _refine_diff_density_min -1.027 _refine_diff_density_rms 0.127 data_(hfac)2Ni-1o-Ni(hfac)2 _database_code_depnum_ccdc_archive 'CCDC 715799' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H18 F30 N4 Ni2 O8 S2' _chemical_formula_sum 'C43 H18 F30 N4 Ni2 O8 S2' _chemical_formula_weight 1470.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0031 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 0.0109 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0176 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1250 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3421 1.1165 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n' _symmetry_int_tables_number 86 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 17.8094(3) _cell_length_b 17.8094(3) _cell_length_c 18.0024(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5709.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 6348 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.75 _exptl_crystal_description plate _exptl_crystal_colour 'bleue green' _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.250 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2904 _exptl_absorpt_coefficient_mu 0.882 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 0.801 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_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 35272 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.90 _reflns_number_total 6790 _reflns_number_gt 4689 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1533P)^2^+11.9883P] 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_number_reflns 6790 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1101 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.2661 _refine_ls_wR_factor_gt 0.2257 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8622(3) 0.2365(2) 0.5552(3) 0.0507(12) Uani 1 1 d . . . C3 C 0.8621(4) 0.3194(3) 0.5667(4) 0.081(2) Uani 1 1 d . . . H3A H 0.9091 0.3346 0.5881 0.121 Uiso 1 1 calc R . . H3B H 0.8219 0.3329 0.5996 0.121 Uiso 1 1 calc R . . H3C H 0.8553 0.3442 0.5198 0.121 Uiso 1 1 calc R . . C4 C 0.8232(2) 0.1939(2) 0.5055(3) 0.0384(9) Uani 1 1 d . . . C5 C 0.8890(2) 0.1034(2) 0.5580(3) 0.0390(9) Uani 1 1 d . . . C6 C 0.9176(2) 0.0272(2) 0.5691(3) 0.0393(9) Uani 1 1 d . . . C7 C 0.9825(3) 0.0105(3) 0.6077(3) 0.0473(11) Uani 1 1 d . . . H7 H 1.0097 0.0481 0.6313 0.057 Uiso 1 1 calc R . . C8 C 1.0064(3) -0.0636(3) 0.6107(3) 0.0540(12) Uani 1 1 d . . . H8 H 1.0503 -0.0762 0.6357 0.065 Uiso 1 1 calc R . . C9 C 0.9647(3) -0.1178(3) 0.5764(3) 0.0586(14) Uani 1 1 d . . . H9 H 0.9794 -0.1679 0.5782 0.070 Uiso 1 1 calc R . . C10 C 0.9002(3) -0.0970(3) 0.5391(3) 0.0532(12) Uani 1 1 d . . . H10 H 0.8721 -0.1340 0.5156 0.064 Uiso 1 1 calc R . . C11 C 0.7783(2) 0.2254(2) 0.4446(2) 0.0377(9) Uani 1 1 d . . . C12 C 0.8042(3) 0.2094(3) 0.3659(3) 0.0468(11) Uani 1 1 d . . . C13 C 0.7624(13) 0.2600(14) 0.3155(6) 0.051(5) Uani 0.50 1 d P . . C14 C 0.5806(4) 0.0501(4) 0.3626(5) 0.079(2) Uani 1 1 d . . . C15 C 0.6629(3) 0.0325(3) 0.3780(3) 0.0533(12) Uani 1 1 d . . . C16 C 0.7020(3) -0.0063(3) 0.3233(3) 0.0570(13) Uani 1 1 d . . . H16 H 0.6770 -0.0210 0.2804 0.068 Uiso 1 1 calc R . . C17 C 0.7771(3) -0.0235(3) 0.3313(3) 0.0511(11) Uani 1 1 d . . . C18 C 0.8135(4) -0.0590(5) 0.2645(5) 0.084(2) Uani 1 1 d . . . C19 C 0.6355(6) -0.1790(5) 0.4990(8) 0.117(4) Uani 1 1 d . . . C20 C 0.6786(3) -0.1099(3) 0.5266(4) 0.0626(15) Uani 1 1 d . . . C21 C 0.6586(5) -0.0796(4) 0.5939(4) 0.086(2) Uani 1 1 d . . . H21 H 0.6214 -0.1030 0.6218 0.104 Uiso 1 1 calc R . . C22 C 0.6919(4) -0.0156(3) 0.6216(4) 0.0670(16) Uani 1 1 d . . . C23 C 0.6734(7) 0.0079(6) 0.7005(5) 0.111(3) Uani 1 1 d . . . N1 N 0.8765(2) -0.0259(2) 0.5353(2) 0.0433(9) Uani 1 1 d . . . N2 N 0.8388(2) 0.11796(19) 0.5077(2) 0.0359(8) Uani 1 1 d . . . O1 O 0.68676(19) 0.05530(19) 0.4398(2) 0.0511(8) Uani 1 1 d . . . O2 O 0.82012(18) -0.01322(18) 0.38484(19) 0.0470(8) Uani 1 1 d . . . O3 O 0.7275(2) -0.08894(19) 0.4827(2) 0.0549(9) Uani 1 1 d . . . O4 O 0.7373(2) 0.02783(19) 0.5903(2) 0.0532(8) Uani 1 1 d . . . F1 F 0.8095(2) 0.13798(18) 0.34877(19) 0.0749(11) Uani 1 1 d . . . F2 F 0.8743(2) 0.2359(3) 0.3571(2) 0.1079(17) Uani 1 1 d . . . F3 F 0.7362(8) 0.2240(6) 0.2564(5) 0.102(5) Uani 0.50 1 d P . . F4 F 0.8043(6) 0.3188(5) 0.2937(6) 0.085(3) Uani 0.50 1 d P . . F5 F 0.5592(3) 0.1125(3) 0.3913(4) 0.129(2) Uani 1 1 d . . . F6 F 0.5385(3) 0.0000(4) 0.3922(6) 0.176(4) Uani 1 1 d . . . F7 F 0.5626(3) 0.0508(6) 0.2942(4) 0.182(4) Uani 1 1 d . . . F8 F 0.7764(4) -0.0830(7) 0.2156(4) 0.232(6) Uani 1 1 d . . . F9 F 0.8559(8) -0.0161(7) 0.2329(7) 0.288(9) Uani 1 1 d . . . F10 F 0.8607(8) -0.1053(8) 0.2788(5) 0.274(8) Uani 1 1 d . . . F11 F 0.6691(5) -0.2244(4) 0.4685(9) 0.277(8) Uani 1 1 d . . . F12 F 0.5839(8) -0.1588(6) 0.4530(10) 0.296(8) Uani 1 1 d . . . F13 F 0.5947(8) -0.2089(6) 0.5465(6) 0.251(7) Uani 1 1 d . . . F14 F 0.7240(8) -0.0072(8) 0.7451(4) 0.246(6) Uani 1 1 d . . . F15 F 0.6242(8) -0.0360(7) 0.7312(5) 0.243(6) Uani 1 1 d . . . F16 F 0.6557(8) 0.0701(5) 0.7104(4) 0.267(7) Uani 1 1 d . . . S S 0.92020(9) 0.17952(7) 0.60660(9) 0.0599(4) Uani 1 1 d . . . Ni Ni 0.77995(3) 0.01256(3) 0.48668(4) 0.0395(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.064(3) 0.034(2) 0.054(3) 0.000(2) -0.018(2) 0.0058(19) C3 0.114(5) 0.030(2) 0.099(5) -0.010(3) -0.051(4) 0.005(3) C4 0.040(2) 0.034(2) 0.042(2) 0.0008(17) -0.0014(17) 0.0043(16) C5 0.044(2) 0.0316(19) 0.041(2) -0.0016(17) -0.0059(18) 0.0009(16) C6 0.044(2) 0.0325(19) 0.042(2) 0.0055(17) -0.0012(18) 0.0027(16) C7 0.049(2) 0.042(2) 0.050(3) 0.004(2) -0.010(2) 0.0018(19) C8 0.053(3) 0.053(3) 0.056(3) 0.015(2) -0.006(2) 0.012(2) C9 0.063(3) 0.037(2) 0.076(4) 0.012(2) -0.001(3) 0.010(2) C10 0.062(3) 0.032(2) 0.066(3) 0.001(2) -0.001(3) 0.000(2) C11 0.043(2) 0.0337(19) 0.036(2) -0.0019(16) -0.0002(18) 0.0043(16) C12 0.057(3) 0.042(2) 0.042(3) 0.0011(19) 0.006(2) 0.012(2) C13 0.066(15) 0.050(13) 0.037(5) -0.003(5) 0.008(5) 0.016(8) C14 0.053(3) 0.094(5) 0.089(5) -0.021(4) -0.018(3) 0.011(3) C15 0.045(2) 0.052(3) 0.063(3) -0.013(2) -0.007(2) 0.002(2) C16 0.059(3) 0.063(3) 0.049(3) -0.018(2) -0.013(2) 0.000(2) C17 0.052(3) 0.050(3) 0.051(3) -0.010(2) -0.001(2) 0.002(2) C18 0.065(4) 0.111(6) 0.076(5) -0.042(4) 0.010(3) 0.006(4) C19 0.091(6) 0.062(5) 0.197(11) -0.025(6) 0.019(7) -0.043(4) C20 0.064(3) 0.046(3) 0.078(4) -0.007(3) 0.004(3) -0.009(2) C21 0.096(5) 0.075(4) 0.088(5) -0.008(4) 0.035(4) -0.030(4) C22 0.092(4) 0.057(3) 0.052(3) 0.001(3) 0.018(3) -0.001(3) C23 0.158(9) 0.116(7) 0.061(5) 0.012(5) 0.036(6) 0.013(7) N1 0.049(2) 0.0334(17) 0.048(2) 0.0022(16) -0.0075(17) 0.0032(15) N2 0.0364(17) 0.0297(16) 0.041(2) 0.0001(14) -0.0020(14) 0.0010(13) O1 0.0474(18) 0.0514(18) 0.054(2) -0.0153(16) -0.0068(15) 0.0090(14) O2 0.0466(17) 0.0449(17) 0.050(2) -0.0114(14) -0.0012(15) 0.0033(13) O3 0.059(2) 0.0392(17) 0.067(2) -0.0098(16) 0.0026(18) -0.0078(15) O4 0.062(2) 0.0493(19) 0.048(2) -0.0056(15) 0.0022(17) -0.0020(16) F1 0.128(3) 0.0469(16) 0.0497(19) -0.0092(14) 0.0057(19) 0.0284(18) F2 0.082(3) 0.167(5) 0.075(3) -0.021(3) 0.036(2) -0.039(3) F3 0.142(12) 0.118(11) 0.047(4) -0.034(5) -0.034(6) 0.070(11) F4 0.105(7) 0.072(5) 0.078(6) 0.033(4) 0.035(5) 0.025(4) F5 0.072(3) 0.136(4) 0.178(6) -0.055(4) -0.034(3) 0.051(3) F6 0.060(3) 0.170(6) 0.300(11) 0.054(7) -0.007(4) -0.019(3) F7 0.105(4) 0.310(11) 0.130(5) -0.054(6) -0.067(4) 0.085(5) F8 0.115(5) 0.417(15) 0.164(7) -0.217(9) 0.004(5) 0.007(7) F9 0.344(16) 0.286(13) 0.234(11) -0.124(10) 0.227(13) -0.125(12) F10 0.362(15) 0.346(14) 0.116(6) -0.081(7) -0.002(7) 0.266(14) F11 0.144(6) 0.113(5) 0.57(2) -0.192(9) 0.111(9) -0.066(5) F12 0.277(14) 0.172(9) 0.44(2) -0.043(12) -0.193(15) -0.093(10) F13 0.365(15) 0.172(7) 0.216(9) -0.057(7) 0.106(10) -0.194(10) F14 0.291(13) 0.379(16) 0.070(4) -0.050(6) -0.037(7) 0.127(13) F15 0.338(15) 0.273(12) 0.117(6) -0.051(7) 0.120(8) -0.127(11) F16 0.57(2) 0.141(6) 0.089(5) 0.003(4) 0.116(8) 0.157(10) S 0.0788(9) 0.0365(6) 0.0643(9) -0.0042(5) -0.0349(7) 0.0032(5) Ni 0.0413(3) 0.0344(3) 0.0429(4) -0.0059(2) -0.0026(2) 0.0015(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C4 1.363(7) . ? C1 C3 1.492(6) . ? C1 S 1.717(5) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 N2 1.382(5) . ? C4 C11 1.469(6) . ? C5 N2 1.299(6) . ? C5 C6 1.463(6) . ? C5 S 1.707(4) . ? C6 N1 1.342(6) . ? C6 C7 1.382(6) . ? C7 C8 1.387(7) . ? C7 H7 0.9300 . ? C8 C9 1.365(8) . ? C8 H8 0.9300 . ? C9 C10 1.381(8) . ? C9 H9 0.9300 . ? C10 N1 1.337(6) . ? C10 H10 0.9300 . ? C11 C12 1.517(7) . ? C12 F1 1.313(6) . ? C12 F2 1.342(6) . ? C12 C13 1.48(3) . ? C13 F3 1.326(14) . ? C13 F4 1.344(18) . ? C14 F7 1.272(9) . ? C14 F6 1.282(10) . ? C14 F5 1.284(8) . ? C14 C15 1.525(8) . ? C15 O1 1.259(6) . ? C15 C16 1.389(8) . ? C16 C17 1.380(7) . ? C16 H16 0.9300 . ? C17 O2 1.244(6) . ? C17 C18 1.505(8) . ? C18 F8 1.180(9) . ? C18 F10 1.206(11) . ? C18 F9 1.215(13) . ? C19 F11 1.145(12) . ? C19 F13 1.242(13) . ? C19 F12 1.288(16) . ? C19 C20 1.532(9) . ? C20 O3 1.233(7) . ? C20 C21 1.374(10) . ? C21 C22 1.378(10) . ? C21 H21 0.9300 . ? C22 O4 1.254(7) . ? C22 C23 1.516(11) . ? C23 F16 1.165(11) . ? C23 F14 1.238(14) . ? C23 F15 1.298(13) . ? N1 Ni 2.047(4) . ? N2 Ni 2.183(3) . ? O1 Ni 2.011(3) . ? O2 Ni 2.021(3) . ? O3 Ni 2.036(3) . ? O4 Ni 2.032(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 C4 C1 C3 129.8(5) . . ? C4 C1 S 109.4(3) . . ? C3 C1 S 120.7(4) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 N2 115.0(4) . . ? C1 C4 C11 123.8(4) . . ? N2 C4 C11 120.3(4) . . ? N2 C5 C6 121.4(4) . . ? N2 C5 S 115.0(3) . . ? C6 C5 S 123.6(3) . . ? N1 C6 C7 122.2(4) . . ? N1 C6 C5 113.6(4) . . ? C7 C6 C5 124.1(4) . . ? C6 C7 C8 118.7(5) . . ? C6 C7 H7 120.6 . . ? C8 C7 H7 120.6 . . ? C9 C8 C7 119.2(5) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 118.9(4) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N1 C10 C9 122.8(5) . . ? N1 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? C4 C11 C12 117.4(4) . . ? F1 C12 F2 104.2(5) . . ? F1 C12 C13 118.9(8) . . ? F2 C12 C13 100.5(7) . . ? F1 C12 C11 115.0(4) . . ? F2 C12 C11 109.1(4) . . ? C13 C12 C11 107.8(8) . . ? F3 C13 F4 109.7(12) . . ? F3 C13 C12 112.0(19) . . ? F4 C13 C12 112.0(15) . . ? F7 C14 F6 105.2(8) . . ? F7 C14 F5 107.9(7) . . ? F6 C14 F5 105.2(8) . . ? F7 C14 C15 114.9(7) . . ? F6 C14 C15 110.0(7) . . ? F5 C14 C15 113.0(6) . . ? O1 C15 C16 128.2(5) . . ? O1 C15 C14 114.8(5) . . ? C16 C15 C14 117.1(5) . . ? C17 C16 C15 121.5(5) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? O2 C17 C16 130.1(5) . . ? O2 C17 C18 114.6(5) . . ? C16 C17 C18 115.2(5) . . ? F8 C18 F10 107.5(10) . . ? F8 C18 F9 103.1(11) . . ? F10 C18 F9 95.5(10) . . ? F8 C18 C17 120.5(6) . . ? F10 C18 C17 114.6(8) . . ? F9 C18 C17 112.2(8) . . ? F11 C19 F13 109.4(11) . . ? F11 C19 F12 105.1(15) . . ? F13 C19 F12 98.4(12) . . ? F11 C19 C20 117.4(8) . . ? F13 C19 C20 114.5(10) . . ? F12 C19 C20 110.0(9) . . ? O3 C20 C21 128.9(5) . . ? O3 C20 C19 112.9(6) . . ? C21 C20 C19 118.2(7) . . ? C20 C21 C22 122.2(6) . . ? C20 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? O4 C22 C21 128.7(6) . . ? O4 C22 C23 113.1(7) . . ? C21 C22 C23 118.3(7) . . ? F16 C23 F14 107.7(13) . . ? F16 C23 F15 108.9(12) . . ? F14 C23 F15 94.8(11) . . ? F16 C23 C22 117.7(8) . . ? F14 C23 C22 112.9(10) . . ? F15 C23 C22 112.3(10) . . ? C10 N1 C6 118.1(4) . . ? C10 N1 Ni 127.2(3) . . ? C6 N1 Ni 114.6(3) . . ? C5 N2 C4 110.8(4) . . ? C5 N2 Ni 106.2(3) . . ? C4 N2 Ni 137.8(3) . . ? C15 O1 Ni 121.8(3) . . ? C17 O2 Ni 121.2(3) . . ? C20 O3 Ni 124.8(4) . . ? C22 O4 Ni 124.9(4) . . ? C5 S C1 89.9(2) . . ? O1 Ni O2 89.86(14) . . ? O1 Ni O4 91.50(15) . . ? O2 Ni O4 174.51(14) . . ? O1 Ni O3 86.70(15) . . ? O2 Ni O3 85.93(15) . . ? O4 Ni O3 88.83(15) . . ? O1 Ni N1 177.30(14) . . ? O2 Ni N1 90.83(15) . . ? O4 Ni N1 88.06(16) . . ? O3 Ni N1 95.94(15) . . ? O1 Ni N2 98.25(14) . . ? O2 Ni N2 100.52(14) . . ? O4 Ni N2 84.55(14) . . ? O3 Ni N2 171.82(15) . . ? N1 Ni N2 79.06(14) . . ? 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 C3 C1 C4 N2 177.5(6) . . . . ? S C1 C4 N2 -0.2(6) . . . . ? C3 C1 C4 C11 8.4(10) . . . . ? S C1 C4 C11 -169.3(4) . . . . ? N2 C5 C6 N1 -13.5(7) . . . . ? S C5 C6 N1 168.6(4) . . . . ? N2 C5 C6 C7 163.6(5) . . . . ? S C5 C6 C7 -14.3(7) . . . . ? N1 C6 C7 C8 0.9(8) . . . . ? C5 C6 C7 C8 -176.0(5) . . . . ? C6 C7 C8 C9 -1.0(8) . . . . ? C7 C8 C9 C10 0.7(9) . . . . ? C8 C9 C10 N1 -0.4(9) . . . . ? C1 C4 C11 C11 -56.2(9) . . . 2_655 ? N2 C4 C11 C11 135.3(6) . . . 2_655 ? C1 C4 C11 C12 114.5(5) . . . . ? N2 C4 C11 C12 -54.0(6) . . . . ? C11 C11 C12 F1 -129.6(5) 2_655 . . . ? C4 C11 C12 F1 57.8(6) . . . . ? C11 C11 C12 F2 113.8(6) 2_655 . . . ? C4 C11 C12 F2 -58.8(6) . . . . ? C11 C11 C12 C13 5.5(8) 2_655 . . . ? C4 C11 C12 C13 -167.1(7) . . . . ? C11 C11 C12 C13 -15.9(9) 2_655 . . 2_655 ? C4 C11 C12 C13 171.5(7) . . . 2_655 ? F1 C12 C13 C13 51(4) . . . 2_655 ? F2 C12 C13 C13 163(4) . . . 2_655 ? C11 C12 C13 C13 -83(4) . . . 2_655 ? F1 C12 C13 F3 -56(2) . . . 2_655 ? F2 C12 C13 F3 57(2) . . . 2_655 ? C11 C12 C13 F3 171.3(19) . . . 2_655 ? C13 C12 C13 F3 -106(5) 2_655 . . 2_655 ? F1 C12 C13 F3 -1.3(16) . . . . ? F2 C12 C13 F3 111.5(12) . . . . ? C11 C12 C13 F3 -134.4(12) . . . . ? C13 C12 C13 F3 -52(3) 2_655 . . . ? F1 C12 C13 F4 -125.1(11) . . . . ? F2 C12 C13 F4 -12.3(14) . . . . ? C11 C12 C13 F4 101.8(13) . . . . ? C13 C12 C13 F4 -176(5) 2_655 . . . ? F1 C12 C13 C12 118.5(9) . . . 2_655 ? F2 C12 C13 C12 -128.7(7) . . . 2_655 ? C11 C12 C13 C12 -14.6(9) . . . 2_655 ? C13 C12 C13 C12 68(4) 2_655 . . 2_655 ? F1 C12 C13 F4 34.4(10) . . . 2_655 ? F2 C12 C13 F4 147.1(6) . . . 2_655 ? C11 C12 C13 F4 -98.8(7) . . . 2_655 ? C13 C12 C13 F4 -16(3) 2_655 . . 2_655 ? F7 C14 C15 O1 157.6(8) . . . . ? F6 C14 C15 O1 -84.0(8) . . . . ? F5 C14 C15 O1 33.2(10) . . . . ? F7 C14 C15 C16 -22.6(11) . . . . ? F6 C14 C15 C16 95.9(9) . . . . ? F5 C14 C15 C16 -146.9(7) . . . . ? O1 C15 C16 C17 -1.6(10) . . . . ? C14 C15 C16 C17 178.6(6) . . . . ? C15 C16 C17 O2 4.4(10) . . . . ? C15 C16 C17 C18 -174.4(6) . . . . ? O2 C17 C18 F8 167.0(10) . . . . ? C16 C17 C18 F8 -14.1(14) . . . . ? O2 C17 C18 F10 36.2(14) . . . . ? C16 C17 C18 F10 -144.9(12) . . . . ? O2 C17 C18 F9 -71.3(13) . . . . ? C16 C17 C18 F9 107.6(12) . . . . ? F11 C19 C20 O3 38.5(18) . . . . ? F13 C19 C20 O3 168.7(12) . . . . ? F12 C19 C20 O3 -81.7(14) . . . . ? F11 C19 C20 C21 -142.1(14) . . . . ? F13 C19 C20 C21 -11.8(17) . . . . ? F12 C19 C20 C21 97.8(15) . . . . ? O3 C20 C21 C22 2.3(14) . . . . ? C19 C20 C21 C22 -177.0(9) . . . . ? C20 C21 C22 O4 7.3(14) . . . . ? C20 C21 C22 C23 -172.3(8) . . . . ? O4 C22 C23 F16 49.9(16) . . . . ? C21 C22 C23 F16 -130.4(14) . . . . ? O4 C22 C23 F14 -76.6(13) . . . . ? C21 C22 C23 F14 103.1(14) . . . . ? O4 C22 C23 F15 177.6(11) . . . . ? C21 C22 C23 F15 -2.7(15) . . . . ? C9 C10 N1 C6 0.3(8) . . . . ? C9 C10 N1 Ni -176.7(4) . . . . ? C7 C6 N1 C10 -0.5(7) . . . . ? C5 C6 N1 C10 176.7(5) . . . . ? C7 C6 N1 Ni 176.9(4) . . . . ? C5 C6 N1 Ni -5.9(5) . . . . ? C6 C5 N2 C4 -177.4(4) . . . . ? S C5 N2 C4 0.6(5) . . . . ? C6 C5 N2 Ni 23.4(5) . . . . ? S C5 N2 Ni -158.6(2) . . . . ? C1 C4 N2 C5 -0.3(6) . . . . ? C11 C4 N2 C5 169.2(4) . . . . ? C1 C4 N2 Ni 149.3(4) . . . . ? C11 C4 N2 Ni -41.3(7) . . . . ? C16 C15 O1 Ni -19.5(8) . . . . ? C14 C15 O1 Ni 160.4(5) . . . . ? C16 C17 O2 Ni 14.5(8) . . . . ? C18 C17 O2 Ni -166.8(5) . . . . ? C21 C20 O3 Ni -14.1(10) . . . . ? C19 C20 O3 Ni 165.3(6) . . . . ? C21 C22 O4 Ni -2.9(11) . . . . ? C23 C22 O4 Ni 176.7(6) . . . . ? C13 C13 F3 F3 151(8) 2_655 . . 2_655 ? F4 C13 F3 F3 -9.3(17) . . . 2_655 ? C12 C13 F3 F3 -134(2) . . . 2_655 ? C12 C13 F3 F3 110(2) 2_655 . . 2_655 ? F4 C13 F3 F3 163.8(19) 2_655 . . 2_655 ? F3 C13 F3 C13 -151(8) 2_655 . . 2_655 ? F4 C13 F3 C13 -161(8) . . . 2_655 ? C12 C13 F3 C13 74(6) . . . 2_655 ? C12 C13 F3 C13 -41(5) 2_655 . . 2_655 ? F4 C13 F3 C13 13(7) 2_655 . . 2_655 ? C13 C13 F3 F4 -13(7) 2_655 . . 2_655 ? F3 C13 F3 F4 -163.8(19) 2_655 . . 2_655 ? F4 C13 F3 F4 -173.2(18) . . . 2_655 ? C12 C13 F3 F4 61.7(13) . . . 2_655 ? C12 C13 F3 F4 -53.5(15) 2_655 . . 2_655 ? C13 C13 F4 F3 -36(13) 2_655 . . 2_655 ? F3 C13 F4 F3 8.2(14) . . . 2_655 ? C12 C13 F4 F3 133(2) . . . 2_655 ? C12 C13 F4 F3 -113(2) 2_655 . . 2_655 ? F4 C13 F4 F3 -1(3) 2_655 . . 2_655 ? F3 C13 F4 C13 36(13) 2_655 . . 2_655 ? F3 C13 F4 C13 44(12) . . . 2_655 ? C12 C13 F4 C13 169(15) . . . 2_655 ? C12 C13 F4 C13 -78(15) 2_655 . . 2_655 ? F4 C13 F4 C13 35(10) 2_655 . . 2_655 ? N2 C5 S C1 -0.6(4) . . . . ? C6 C5 S C1 177.3(4) . . . . ? C4 C1 S C5 0.4(4) . . . . ? C3 C1 S C5 -177.5(6) . . . . ? C15 O1 Ni O2 27.4(4) . . . . ? C15 O1 Ni O4 -147.3(4) . . . . ? C15 O1 Ni O3 -58.6(4) . . . . ? C15 O1 Ni N2 128.0(4) . . . . ? C17 O2 Ni O1 -24.9(4) . . . . ? C17 O2 Ni O3 61.8(4) . . . . ? C17 O2 Ni N1 157.7(4) . . . . ? C17 O2 Ni N2 -123.3(4) . . . . ? C22 O4 Ni O1 81.2(5) . . . . ? C22 O4 Ni O3 -5.5(5) . . . . ? C22 O4 Ni N1 -101.5(5) . . . . ? C22 O4 Ni N2 179.3(5) . . . . ? C20 O3 Ni O1 -78.3(5) . . . . ? C20 O3 Ni O2 -168.4(5) . . . . ? C20 O3 Ni O4 13.3(5) . . . . ? C20 O3 Ni N1 101.2(5) . . . . ? C10 N1 Ni O2 -68.7(5) . . . . ? C6 N1 Ni O2 114.2(3) . . . . ? C10 N1 Ni O4 105.9(5) . . . . ? C6 N1 Ni O4 -71.2(3) . . . . ? C10 N1 Ni O3 17.3(5) . . . . ? C6 N1 Ni O3 -159.8(3) . . . . ? C10 N1 Ni N2 -169.3(5) . . . . ? C6 N1 Ni N2 13.7(3) . . . . ? C5 N2 Ni O1 160.6(3) . . . . ? C4 N2 Ni O1 10.2(5) . . . . ? C5 N2 Ni O2 -108.0(3) . . . . ? C4 N2 Ni O2 101.6(4) . . . . ? C5 N2 Ni O4 69.9(3) . . . . ? C4 N2 Ni O4 -80.6(5) . . . . ? C5 N2 Ni N1 -19.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.166 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.160 data_(hfac)2Co-1o-Co(hfac)2 _database_code_depnum_ccdc_archive 'CCDC 715800' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H18 Co2 F30 N4 O8 S2 ' _chemical_formula_sum 'C43 H18 Co2 F30 N4 O8 S2 ' _chemical_formula_weight 1470.61 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n' _symmetry_int_tables_number 86 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 17.718(5) _cell_length_b 17.718(5) _cell_length_c 17.836(5) _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_volume 5599(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3855 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 23.65 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.080 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.827 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_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 18745 _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 24.06 _reflns_number_total 4380 _reflns_number_gt 2956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1181P)^2^+24.7095P] 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 4380 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1176 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.2268 _refine_ls_wR_factor_gt 0.1856 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.008 _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 C1 C 0.8626(4) 0.2377(4) 0.5583(4) 0.0300(17) Uani 1 1 d . . . C3 C 0.8602(5) 0.3214(4) 0.5709(5) 0.044(2) Uani 1 1 d . . . H3A H 0.9072 0.3377 0.5922 0.066 Uiso 1 1 calc R . . H3B H 0.8198 0.3333 0.6046 0.066 Uiso 1 1 calc R . . H3C H 0.8522 0.3466 0.5239 0.066 Uiso 1 1 calc R . . C4 C 0.8241(4) 0.1950(3) 0.5079(4) 0.0204(15) Uani 1 1 d . . . C5 C 0.8910(4) 0.1041(4) 0.5608(4) 0.0229(15) Uani 1 1 d . . . C6 C 0.9207(4) 0.0274(4) 0.5712(4) 0.0205(15) Uani 1 1 d . . . C7 C 0.9859(4) 0.0119(4) 0.6102(4) 0.0255(16) Uani 1 1 d . . . H7 H 1.0126 0.0499 0.6344 0.031 Uiso 1 1 calc R . . C8 C 1.0105(4) -0.0627(4) 0.6122(4) 0.0287(17) Uani 1 1 d . . . H8 H 1.0544 -0.0752 0.6381 0.034 Uiso 1 1 calc R . . C9 C 0.9700(4) -0.1178(4) 0.5760(4) 0.0292(17) Uani 1 1 d . . . H9 H 0.9858 -0.1678 0.5771 0.035 Uiso 1 1 calc R . . C10 C 0.9051(4) -0.0974(4) 0.5376(4) 0.0312(18) Uani 1 1 d . . . H10 H 0.8778 -0.1346 0.5128 0.037 Uiso 1 1 calc R . . C11 C 0.7790(4) 0.2254(4) 0.4455(4) 0.0218(15) Uani 1 1 d . . . C12 C 0.8049(4) 0.2095(4) 0.3665(4) 0.0274(17) Uani 1 1 d . . . C13 C 0.7648(13) 0.2590(11) 0.3161(4) 0.024(5) Uani 0.50 1 d P . . C14 C 0.5789(5) 0.0514(5) 0.3604(5) 0.044(2) Uani 1 1 d . . . C15 C 0.6615(4) 0.0328(4) 0.3746(4) 0.0290(17) Uani 1 1 d . . . C16 C 0.7009(4) -0.0071(4) 0.3204(4) 0.0304(18) Uani 1 1 d . . . H16 H 0.6757 -0.0212 0.2769 0.037 Uiso 1 1 calc R . . C17 C 0.7751(4) -0.0266(4) 0.3279(4) 0.0271(17) Uani 1 1 d . . . C18 C 0.8130(5) -0.0625(5) 0.2608(5) 0.046(2) Uani 1 1 d . . . C19 C 0.6340(7) -0.1833(6) 0.5007(7) 0.071(3) Uani 1 1 d . . . C20 C 0.6766(5) -0.1138(4) 0.5266(5) 0.041(2) Uani 1 1 d . . . C21 C 0.6574(6) -0.0837(5) 0.5961(6) 0.061(3) Uani 1 1 d . . . H21 H 0.6201 -0.1075 0.6243 0.073 Uiso 1 1 calc R . . C22 C 0.6918(5) -0.0198(5) 0.6248(5) 0.044(2) Uani 1 1 d . . . C23 C 0.6759(8) 0.0029(7) 0.7052(6) 0.072(3) Uani 1 1 d . . . N1 N 0.8804(3) -0.0260(3) 0.5349(3) 0.0256(14) Uani 1 1 d . . . N2 N 0.8395(3) 0.1188(3) 0.5101(3) 0.0208(13) Uani 1 1 d . . . O1 O 0.6858(3) 0.0557(3) 0.4375(3) 0.0286(12) Uani 1 1 d . . . O2 O 0.8193(3) -0.0161(3) 0.3819(3) 0.0273(11) Uani 1 1 d . . . O3 O 0.7249(3) -0.0909(3) 0.4824(3) 0.0308(12) Uani 1 1 d . . . O4 O 0.7377(3) 0.0243(3) 0.5929(3) 0.0324(13) Uani 1 1 d . . . F1 F 0.8082(3) 0.1374(2) 0.3494(2) 0.0423(12) Uani 1 1 d . . . F2 F 0.8751(3) 0.2356(4) 0.3568(3) 0.076(2) Uani 1 1 d . . . F3 F 0.7403(7) 0.2254(4) 0.2540(5) 0.056(4) Uani 0.50 1 d P . . F4 F 0.8050(5) 0.3177(4) 0.2923(5) 0.046(3) Uani 0.50 1 d P . . F5 F 0.5582(3) 0.1156(3) 0.3894(3) 0.0673(17) Uani 1 1 d . . . F6 F 0.5352(3) -0.0005(4) 0.3893(5) 0.090(2) Uani 1 1 d . . . F7 F 0.5619(3) 0.0538(5) 0.2884(4) 0.096(2) Uani 1 1 d . . . F8 F 0.7730(4) -0.0793(6) 0.2062(4) 0.129(4) Uani 1 1 d . . . F9 F 0.8662(6) -0.0223(7) 0.2356(6) 0.195(7) Uani 1 1 d . . . F10 F 0.8467(8) -0.1216(6) 0.2765(5) 0.192(6) Uani 1 1 d . . . F11 F 0.6664(4) -0.2260(4) 0.4585(6) 0.128(4) Uani 1 1 d . . . F12 F 0.5769(6) -0.1588(6) 0.4516(8) 0.182(5) Uani 1 1 d . . . F13 F 0.5893(6) -0.2124(5) 0.5479(5) 0.152(4) Uani 1 1 d . . . F14 F 0.7327(7) -0.0087(6) 0.7479(4) 0.154(5) Uani 1 1 d . . . F15 F 0.6244(7) -0.0432(6) 0.7362(5) 0.170(5) Uani 1 1 d . . . F16 F 0.6553(7) 0.0682(4) 0.7145(4) 0.144(4) Uani 1 1 d . . . S S 0.92110(12) 0.18069(10) 0.60993(11) 0.0342(5) Uani 1 1 d . . . Co Co 0.77992(5) 0.01221(5) 0.48605(5) 0.0230(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(4) 0.023(4) 0.034(4) -0.001(3) -0.005(4) 0.000(3) C3 0.060(6) 0.016(4) 0.056(6) -0.007(4) -0.029(5) 0.007(4) C4 0.023(4) 0.011(3) 0.027(4) 0.001(3) 0.002(3) 0.005(3) C5 0.025(4) 0.022(4) 0.022(4) -0.003(3) 0.000(3) -0.001(3) C6 0.022(4) 0.019(4) 0.021(4) 0.002(3) 0.001(3) 0.001(3) C7 0.024(4) 0.025(4) 0.028(4) 0.003(3) -0.001(3) 0.001(3) C8 0.023(4) 0.033(4) 0.030(4) 0.008(3) -0.002(3) 0.003(3) C9 0.028(4) 0.022(4) 0.038(4) 0.008(3) 0.003(3) 0.011(3) C10 0.037(5) 0.014(4) 0.042(5) 0.003(3) 0.006(4) -0.004(3) C11 0.025(4) 0.013(3) 0.027(4) 0.000(3) 0.001(3) -0.001(3) C12 0.037(5) 0.017(4) 0.028(4) -0.001(3) 0.004(3) 0.007(3) C13 0.023(19) 0.030(12) 0.020(7) -0.007(8) 0.003(6) 0.003(9) C14 0.034(5) 0.050(6) 0.049(6) -0.011(4) -0.004(4) 0.010(5) C15 0.023(4) 0.027(4) 0.036(5) -0.002(3) -0.004(3) -0.003(3) C16 0.034(4) 0.030(4) 0.027(4) -0.003(3) -0.006(3) -0.003(4) C17 0.032(4) 0.018(4) 0.032(4) -0.005(3) 0.001(3) 0.000(3) C18 0.040(5) 0.055(6) 0.043(6) -0.018(5) 0.006(4) -0.001(5) C19 0.063(7) 0.058(7) 0.093(9) -0.024(6) 0.031(7) -0.037(6) C20 0.048(5) 0.030(4) 0.044(5) -0.007(4) 0.008(4) -0.008(4) C21 0.073(7) 0.052(6) 0.059(7) -0.008(5) 0.030(5) -0.024(5) C22 0.065(6) 0.038(5) 0.028(5) -0.001(4) 0.015(4) -0.006(5) C23 0.105(9) 0.068(7) 0.043(7) 0.001(6) 0.036(7) -0.019(7) N1 0.026(3) 0.023(3) 0.028(3) 0.002(3) 0.000(3) 0.002(3) N2 0.018(3) 0.020(3) 0.025(3) 0.001(2) 0.002(3) 0.000(2) O1 0.031(3) 0.025(3) 0.030(3) -0.008(2) -0.003(2) 0.005(2) O2 0.022(3) 0.027(3) 0.033(3) -0.004(2) 0.001(2) 0.005(2) O3 0.036(3) 0.020(3) 0.037(3) -0.002(2) 0.005(3) -0.006(2) O4 0.038(3) 0.029(3) 0.030(3) -0.005(2) -0.001(2) -0.001(3) F1 0.074(3) 0.022(2) 0.031(2) -0.0020(19) 0.003(2) 0.010(2) F2 0.058(3) 0.115(5) 0.055(4) -0.028(3) 0.031(3) -0.049(3) F3 0.074(10) 0.059(10) 0.034(5) -0.016(4) -0.019(6) 0.041(11) F4 0.051(6) 0.041(6) 0.047(6) 0.024(5) 0.026(5) 0.019(5) F5 0.044(3) 0.062(4) 0.096(5) -0.026(3) -0.016(3) 0.024(3) F6 0.034(3) 0.079(4) 0.157(7) 0.014(4) -0.002(4) -0.011(3) F7 0.056(4) 0.165(7) 0.068(5) -0.024(4) -0.029(3) 0.045(4) F8 0.069(4) 0.240(10) 0.078(5) -0.107(6) -0.004(4) 0.021(5) F9 0.185(9) 0.256(13) 0.144(9) -0.132(9) 0.137(8) -0.134(10) F10 0.316(16) 0.174(9) 0.085(6) -0.021(6) 0.044(8) 0.181(11) F11 0.095(5) 0.069(4) 0.219(10) -0.089(6) 0.059(6) -0.042(4) F12 0.145(9) 0.116(8) 0.285(16) -0.059(9) -0.081(10) -0.038(7) F13 0.217(10) 0.108(6) 0.130(7) -0.041(6) 0.077(7) -0.120(7) F14 0.213(11) 0.209(11) 0.040(4) -0.035(5) -0.040(6) 0.093(9) F15 0.257(13) 0.177(9) 0.076(6) -0.042(6) 0.089(7) -0.105(9) F16 0.290(13) 0.092(6) 0.051(4) 0.000(4) 0.063(6) 0.086(7) S 0.0449(12) 0.0196(10) 0.0381(11) -0.0024(8) -0.0190(9) 0.0043(9) Co 0.0246(6) 0.0190(5) 0.0254(5) -0.0025(4) -0.0012(4) 0.0020(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C4 1.359(10) . ? C1 C3 1.500(10) . ? C1 S 1.715(7) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 N2 1.377(8) . ? C4 C11 1.473(9) . ? C5 N2 1.311(9) . ? C5 C6 1.470(9) . ? C5 S 1.701(7) . ? C6 N1 1.351(9) . ? C6 C7 1.376(10) . ? C7 C8 1.392(10) . ? C7 H7 0.9300 . ? C8 C9 1.373(10) . ? C8 H8 0.9300 . ? C9 C10 1.386(10) . ? C9 H9 0.9300 . ? C10 N1 1.339(9) . ? C10 H10 0.9300 . ? C11 C11 1.347(13) 2_655 ? C11 C12 1.509(10) . ? C12 F1 1.314(8) . ? C12 F2 1.338(9) . ? C12 C13 1.44(2) . ? C12 C13 1.63(3) 2_655 ? C13 C13 0.61(2) 2_655 ? C13 F3 1.144(9) 2_655 ? C13 F3 1.3300(11) . ? C13 F4 1.3300(11) . ? C13 C12 1.63(3) 2_655 ? C13 F4 1.887(13) 2_655 ? C14 F5 1.303(10) . ? C14 F6 1.309(10) . ? C14 F7 1.319(10) . ? C14 C15 1.522(11) . ? C15 O1 1.269(9) . ? C15 C16 1.386(10) . ? C16 C17 1.365(10) . ? C16 H16 0.9300 . ? C17 O2 1.256(8) . ? C17 C18 1.512(11) . ? C18 F10 1.236(12) . ? C18 F8 1.242(11) . ? C18 F9 1.265(12) . ? C19 F11 1.212(12) . ? C19 F13 1.266(12) . ? C19 F12 1.407(16) . ? C19 C20 1.516(12) . ? C20 O3 1.233(9) . ? C20 C21 1.391(12) . ? C21 C22 1.385(12) . ? C21 H21 0.9300 . ? C22 O4 1.264(9) . ? C22 C23 1.516(13) . ? C23 F16 1.225(13) . ? C23 F14 1.277(15) . ? C23 F15 1.343(13) . ? N1 Co 2.094(6) . ? N2 Co 2.205(5) . ? O1 Co 2.031(5) . ? O2 Co 2.046(5) . ? O3 Co 2.071(5) . ? O4 Co 2.058(5) . ? F3 F3 0.937(14) 2_655 ? F3 C13 1.144(9) 2_655 ? F3 F4 1.301(16) 2_655 ? F4 F3 1.301(16) 2_655 ? F4 C13 1.887(13) 2_655 ? 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 C4 C1 C3 129.4(7) . . ? C4 C1 S 109.3(5) . . ? C3 C1 S 121.2(5) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 N2 115.3(6) . . ? C1 C4 C11 124.7(6) . . ? N2 C4 C11 119.2(6) . . ? N2 C5 C6 121.3(6) . . ? N2 C5 S 114.5(5) . . ? C6 C5 S 124.1(5) . . ? N1 C6 C7 123.2(6) . . ? N1 C6 C5 113.4(6) . . ? C7 C6 C5 123.3(6) . . ? C6 C7 C8 117.7(7) . . ? C6 C7 H7 121.1 . . ? C8 C7 H7 121.1 . . ? C9 C8 C7 119.9(7) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 118.7(6) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N1 C10 C9 122.4(7) . . ? N1 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C11 C11 C4 130.6(4) 2_655 . ? C11 C11 C12 110.7(4) 2_655 . ? C4 C11 C12 118.2(6) . . ? F1 C12 F2 105.4(6) . . ? F1 C12 C13 118.0(7) . . ? F2 C12 C13 99.6(7) . . ? F1 C12 C11 114.3(6) . . ? F2 C12 C11 109.8(6) . . ? C13 C12 C11 108.5(9) . . ? F3 C13 F4 104.99(11) . . ? F3 C13 C12 114.0(16) . . ? F4 C13 C12 114.3(14) . . ? F5 C14 F6 106.9(7) . . ? F5 C14 F7 107.2(8) . . ? F6 C14 F7 105.8(8) . . ? F5 C14 C15 113.1(7) . . ? F6 C14 C15 110.6(7) . . ? F7 C14 C15 112.8(7) . . ? O1 C15 C16 127.5(7) . . ? O1 C15 C14 113.9(7) . . ? C16 C15 C14 118.6(7) . . ? C17 C16 C15 123.0(7) . . ? C17 C16 H16 118.5 . . ? C15 C16 H16 118.5 . . ? O2 C17 C16 129.7(7) . . ? O2 C17 C18 113.1(7) . . ? C16 C17 C18 117.1(7) . . ? F10 C18 F8 104.5(10) . . ? F10 C18 F9 101.4(11) . . ? F8 C18 F9 106.3(10) . . ? F10 C18 C17 113.0(8) . . ? F8 C18 C17 118.0(8) . . ? F9 C18 C17 112.0(8) . . ? F11 C19 F13 117.1(10) . . ? F11 C19 F12 98.4(12) . . ? F13 C19 F12 95.1(11) . . ? F11 C19 C20 117.4(9) . . ? F13 C19 C20 116.1(10) . . ? F12 C19 C20 107.3(10) . . ? O3 C20 C21 127.9(8) . . ? O3 C20 C19 114.7(8) . . ? C21 C20 C19 117.4(8) . . ? C22 C21 C20 122.4(8) . . ? C22 C21 H21 118.8 . . ? C20 C21 H21 118.8 . . ? O4 C22 C21 128.5(8) . . ? O4 C22 C23 112.5(8) . . ? C21 C22 C23 119.0(8) . . ? F16 C23 F14 107.9(12) . . ? F16 C23 F15 108.4(11) . . ? F14 C23 F15 101.1(11) . . ? F16 C23 C22 115.6(10) . . ? F14 C23 C22 112.0(10) . . ? F15 C23 C22 110.7(9) . . ? C10 N1 C6 118.1(6) . . ? C10 N1 Co 126.8(5) . . ? C6 N1 Co 115.0(4) . . ? C5 N2 C4 110.6(6) . . ? C5 N2 Co 107.3(4) . . ? C4 N2 Co 137.6(4) . . ? C15 O1 Co 122.3(4) . . ? C17 O2 Co 121.3(4) . . ? C20 O3 Co 126.7(5) . . ? C22 O4 Co 126.0(5) . . ? C5 S C1 90.2(3) . . ? O1 Co O2 89.21(19) . . ? O1 Co O4 93.3(2) . . ? O2 Co O4 171.75(19) . . ? O1 Co O3 86.28(19) . . ? O2 Co O3 85.2(2) . . ? O4 Co O3 87.1(2) . . ? O1 Co N1 176.3(2) . . ? O2 Co N1 90.5(2) . . ? O4 Co N1 87.6(2) . . ? O3 Co N1 97.4(2) . . ? O1 Co N2 98.65(19) . . ? O2 Co N2 102.9(2) . . ? O4 Co N2 84.5(2) . . ? O3 Co N2 170.5(2) . . ? N1 Co N2 77.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C1 C4 N2 179.5(8) . . . . ? S C1 C4 N2 0.7(8) . . . . ? C3 C1 C4 C11 10.0(13) . . . . ? S C1 C4 C11 -168.8(6) . . . . ? N2 C5 C6 N1 -11.8(9) . . . . ? S C5 C6 N1 170.1(5) . . . . ? N2 C5 C6 C7 164.3(7) . . . . ? S C5 C6 C7 -13.7(10) . . . . ? N1 C6 C7 C8 -0.4(10) . . . . ? C5 C6 C7 C8 -176.2(6) . . . . ? C6 C7 C8 C9 0.0(10) . . . . ? C7 C8 C9 C10 0.3(11) . . . . ? C8 C9 C10 N1 -0.3(11) . . . . ? C1 C4 C11 C12 114.5(8) . . . . ? N2 C4 C11 C12 -54.5(8) . . . . ? C4 C11 C12 F1 60.2(8) . . . . ? C4 C11 C12 F2 -57.9(8) . . . . ? C4 C11 C12 C13 -165.8(6) . . . . ? F1 C12 C13 F3 -4.9(16) . . . . ? F2 C12 C13 F3 108.3(12) . . . . ? C11 C12 C13 F3 -136.9(12) . . . . ? F1 C12 C13 F4 -125.7(11) . . . . ? F2 C12 C13 F4 -12.4(14) . . . . ? C11 C12 C13 F4 102.3(13) . . . . ? F5 C14 C15 O1 34.3(11) . . . . ? F6 C14 C15 O1 -85.6(9) . . . . ? F7 C14 C15 O1 156.1(8) . . . . ? F5 C14 C15 C16 -146.9(8) . . . . ? F6 C14 C15 C16 93.3(9) . . . . ? F7 C14 C15 C16 -25.0(11) . . . . ? O1 C15 C16 C17 -1.2(12) . . . . ? C14 C15 C16 C17 -179.9(7) . . . . ? C15 C16 C17 O2 2.6(13) . . . . ? C15 C16 C17 C18 -173.5(7) . . . . ? O2 C17 C18 F10 53.5(12) . . . . ? C16 C17 C18 F10 -129.7(11) . . . . ? O2 C17 C18 F8 175.9(9) . . . . ? C16 C17 C18 F8 -7.4(13) . . . . ? O2 C17 C18 F9 -60.2(12) . . . . ? C16 C17 C18 F9 116.5(11) . . . . ? F11 C19 C20 O3 27.7(17) . . . . ? F13 C19 C20 O3 173.4(11) . . . . ? F12 C19 C20 O3 -81.7(12) . . . . ? F11 C19 C20 C21 -152.1(12) . . . . ? F13 C19 C20 C21 -6.4(17) . . . . ? F12 C19 C20 C21 98.5(12) . . . . ? O3 C20 C21 C22 1.2(17) . . . . ? C19 C20 C21 C22 -179.1(10) . . . . ? C20 C21 C22 O4 7.5(17) . . . . ? C20 C21 C22 C23 -171.3(11) . . . . ? O4 C22 C23 F16 53.4(16) . . . . ? C21 C22 C23 F16 -127.6(12) . . . . ? O4 C22 C23 F14 -70.8(13) . . . . ? C21 C22 C23 F14 108.2(13) . . . . ? O4 C22 C23 F15 177.2(11) . . . . ? C21 C22 C23 F15 -3.8(16) . . . . ? C9 C10 N1 C6 -0.1(10) . . . . ? C9 C10 N1 Co -175.3(5) . . . . ? C7 C6 N1 C10 0.4(10) . . . . ? C5 C6 N1 C10 176.6(6) . . . . ? C7 C6 N1 Co 176.2(5) . . . . ? C5 C6 N1 Co -7.6(7) . . . . ? C6 C5 N2 C4 -176.3(6) . . . . ? S C5 N2 C4 1.9(7) . . . . ? C6 C5 N2 Co 23.0(7) . . . . ? S C5 N2 Co -158.8(3) . . . . ? C1 C4 N2 C5 -1.7(8) . . . . ? C11 C4 N2 C5 168.4(6) . . . . ? C1 C4 N2 Co 150.4(6) . . . . ? C11 C4 N2 Co -39.5(10) . . . . ? C16 C15 O1 Co -18.7(10) . . . . ? C14 C15 O1 Co 160.1(5) . . . . ? C16 C17 O2 Co 15.8(11) . . . . ? C18 C17 O2 Co -168.0(5) . . . . ? C21 C20 O3 Co -13.1(14) . . . . ? C19 C20 O3 Co 167.1(7) . . . . ? C21 C22 O4 Co -2.4(14) . . . . ? C23 C22 O4 Co 176.4(7) . . . . ? N2 C5 S C1 -1.3(6) . . . . ? C6 C5 S C1 176.8(6) . . . . ? C4 C1 S C5 0.3(6) . . . . ? C3 C1 S C5 -178.6(7) . . . . ? C15 O1 Co O2 26.3(5) . . . . ? C15 O1 Co O4 -145.8(5) . . . . ? C15 O1 Co O3 -58.9(5) . . . . ? C15 O1 Co N2 129.2(5) . . . . ? C17 O2 Co O1 -24.8(5) . . . . ? C17 O2 Co O3 61.6(5) . . . . ? C17 O2 Co N1 158.9(5) . . . . ? C17 O2 Co N2 -123.5(5) . . . . ? C22 O4 Co O1 80.4(7) . . . . ? C22 O4 Co O3 -5.7(7) . . . . ? C22 O4 Co N1 -103.2(7) . . . . ? C22 O4 Co N2 178.8(7) . . . . ? C20 O3 Co O1 -80.4(7) . . . . ? C20 O3 Co O2 -169.9(7) . . . . ? C20 O3 Co O4 13.1(7) . . . . ? C20 O3 Co N1 100.3(7) . . . . ? C10 N1 Co O2 -66.8(6) . . . . ? C6 N1 Co O2 117.8(5) . . . . ? C10 N1 Co O4 105.2(6) . . . . ? C6 N1 Co O4 -70.2(5) . . . . ? C10 N1 Co O3 18.4(6) . . . . ? C6 N1 Co O3 -157.0(5) . . . . ? C10 N1 Co N2 -169.9(6) . . . . ? C6 N1 Co N2 14.7(5) . . . . ? C5 N2 Co O1 161.7(4) . . . . ? C4 N2 Co O1 9.0(7) . . . . ? C5 N2 Co O2 -107.1(4) . . . . ? C4 N2 Co O2 100.2(7) . . . . ? C5 N2 Co O4 69.3(4) . . . . ? C4 N2 Co O4 -83.5(7) . . . . ? C5 N2 Co N1 -19.4(4) . . . . ? C4 N2 Co N1 -172.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 24.06 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.821 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.147