# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'NEELS, Antonia' _publ_contact_author_email Antonia.NEELS@csem.ch loop_ _publ_author_name 'Ying-Fen Ran.' 'Shi-Xia Liu.' 'Olha Sereda' 'Antonia Neels' 'Silvio Decurtins' data_Complex1 _database_code_depnum_ccdc_archive 'CCDC 806935' #TrackingRef 'Complex1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H28 Co F12 N4 O5 S6' _chemical_formula_weight 1111.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5303(8) _cell_length_b 15.1120(11) _cell_length_c 15.8877(13) _cell_angle_alpha 83.671(6) _cell_angle_beta 77.538(7) _cell_angle_gamma 81.979(6) _cell_volume 2204.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15871 _cell_measurement_theta_min 1.32 _cell_measurement_theta_max 25.56 _exptl_crystal_description plate _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1122 _exptl_absorpt_coefficient_mu 0.773 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.809 _exptl_absorpt_correction_T_max 0.882 _exptl_absorpt_process_details 'MULscanABS, (PLATON03, Speck, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20132 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.14 _reflns_number_total 7833 _reflns_number_gt 5496 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1216P)^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 7833 _refine_ls_number_parameters 566 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0865 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1881 _refine_ls_wR_factor_gt 0.1792 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.3007(6) 0.3209(4) 0.0983(3) 0.0357(12) Uani 1 1 d . . . C2 C 1.3660(7) 0.2785(4) 0.0161(4) 0.0460(14) Uani 1 1 d . . . C3 C 1.3094(6) 0.4113(4) 0.1018(4) 0.0441(13) Uani 1 1 d . . . H3A H 1.3504 0.4452 0.0506 0.053 Uiso 1 1 calc R . . C4 C 1.2600(6) 0.4536(4) 0.1778(4) 0.0429(13) Uani 1 1 d . . . C5 C 1.2793(7) 0.5491(5) 0.1765(5) 0.0611(19) Uani 1 1 d . . . C6 C 0.8639(6) 0.4204(3) 0.1975(4) 0.0396(13) Uani 1 1 d . . . C7 C 0.8079(7) 0.4582(4) 0.1175(5) 0.0506(15) Uani 1 1 d . . . C8 C 0.7940(7) 0.4508(4) 0.2771(4) 0.0510(16) Uani 1 1 d . A . H8A H 0.7175 0.4985 0.2792 0.061 Uiso 1 1 calc R . . C9 C 0.8336(7) 0.4130(4) 0.3533(4) 0.0508(16) Uani 1 1 d . . . C10 C 0.738(2) 0.4440(12) 0.4361(15) 0.1084(19) Uani 0.50 1 d PD A 1 C10A C 0.749(2) 0.4488(13) 0.4381(15) 0.1084(19) Uani 0.50 1 d PD A 2 C11 C 1.1146(5) 0.1166(3) 0.3409(3) 0.0256(10) Uani 1 1 d . . . C12 C 1.1923(5) 0.1588(3) 0.3918(3) 0.0274(10) Uani 1 1 d . . . C13 C 1.2789(6) 0.2891(4) 0.4116(4) 0.0388(12) Uani 1 1 d . . . H13A H 1.2896 0.3506 0.3954 0.047 Uiso 1 1 calc R . . C14 C 1.3382(6) 0.2450(4) 0.4807(3) 0.0423(14) Uani 1 1 d . . . H14A H 1.3882 0.2767 0.5111 0.051 Uiso 1 1 calc R . . C15 C 1.3237(6) 0.1558(4) 0.5044(3) 0.0376(12) Uani 1 1 d . . . H15A H 1.3642 0.1258 0.5509 0.045 Uiso 1 1 calc R . . C16 C 1.2492(5) 0.1094(4) 0.4597(3) 0.0320(11) Uani 1 1 d . . . C17 C 1.2296(5) 0.0151(3) 0.4796(3) 0.0293(11) Uani 1 1 d . . . C18 C 1.1531(5) -0.0271(3) 0.4313(3) 0.0288(11) Uani 1 1 d . . . C19 C 1.1799(6) -0.1618(4) 0.5103(3) 0.0363(12) Uani 1 1 d . . . H19A H 1.1626 -0.2228 0.5219 0.044 Uiso 1 1 calc R . . C20 C 1.2596(6) -0.1278(4) 0.5602(3) 0.0404(13) Uani 1 1 d . . . H20A H 1.2971 -0.1654 0.6042 0.048 Uiso 1 1 calc R . . C21 C 1.2833(6) -0.0406(4) 0.5456(3) 0.0397(13) Uani 1 1 d . . . H21A H 1.3365 -0.0168 0.5801 0.048 Uiso 1 1 calc R . . C22 C 1.0975(5) 0.0251(3) 0.3595(3) 0.0271(10) Uani 1 1 d . . . C23 C 0.9847(5) 0.0309(3) 0.2451(3) 0.0255(10) Uani 1 1 d . . . C24 C 1.0043(5) 0.1231(3) 0.2252(3) 0.0231(9) Uani 1 1 d . . . C25 C 0.9626(5) 0.1695(3) 0.1499(3) 0.0250(10) Uani 1 1 d . . . H25A H 0.9761 0.2309 0.1353 0.030 Uiso 1 1 calc R . . C26 C 0.9032(5) 0.1249(3) 0.0989(3) 0.0247(10) Uani 1 1 d . . . C27 C 0.7826(5) 0.0834(3) -0.0216(3) 0.0267(10) Uani 1 1 d . . . C28 C 0.8778(5) 0.0333(3) 0.1208(3) 0.0250(10) Uani 1 1 d . . . C29 C 0.9185(5) -0.0132(3) 0.1918(3) 0.0261(10) Uani 1 1 d . . . H29A H 0.9029 -0.0743 0.2056 0.031 Uiso 1 1 calc R . . C30 C 0.7263(5) 0.0868(3) -0.0923(3) 0.0252(10) Uani 1 1 d . . . C31 C 0.5966(5) 0.0528(3) -0.2104(3) 0.0262(10) Uani 1 1 d . . . C32 C 0.4973(5) -0.1125(3) -0.2121(3) 0.0297(10) Uani 1 1 d . . . H32A H 0.5959 -0.1417 -0.2091 0.036 Uiso 1 1 calc R . . H32B H 0.4405 -0.1076 -0.1524 0.036 Uiso 1 1 calc R . . C33 C 0.4250(5) -0.1665(3) -0.2617(3) 0.0333(11) Uani 1 1 d . . . H33A H 0.4792 -0.1666 -0.3224 0.040 Uiso 1 1 calc R . . H33B H 0.3256 -0.1371 -0.2624 0.040 Uiso 1 1 calc R . . C34 C 0.4175(6) -0.2628(4) -0.2233(4) 0.0460(14) Uani 1 1 d . . . H34A H 0.5158 -0.2940 -0.2278 0.069 Uiso 1 1 calc R . . H34B H 0.3634 -0.2932 -0.2551 0.069 Uiso 1 1 calc R . . H34C H 0.3686 -0.2632 -0.1624 0.069 Uiso 1 1 calc R . . C35 C 0.6228(5) 0.1384(3) -0.2311(3) 0.0265(10) Uani 1 1 d . . . C36 C 0.4170(6) 0.2765(3) -0.2662(3) 0.0352(11) Uani 1 1 d . . . H36A H 0.4434 0.3058 -0.2200 0.042 Uiso 1 1 calc R . . H36B H 0.3878 0.3244 -0.3090 0.042 Uiso 1 1 calc R . . C37 C 0.2885(6) 0.2258(4) -0.2269(4) 0.0450(14) Uani 1 1 d . . . H37A H 0.2660 0.1927 -0.2718 0.054 Uiso 1 1 calc R . . H37B H 0.3142 0.1813 -0.1804 0.054 Uiso 1 1 calc R . . C38 C 0.1556(7) 0.2879(4) -0.1900(5) 0.0557(17) Uani 1 1 d . . . H38A H 0.1754 0.3178 -0.1429 0.084 Uiso 1 1 calc R . . H38B H 0.0741 0.2530 -0.1678 0.084 Uiso 1 1 calc R . . H38C H 0.1314 0.3330 -0.2355 0.084 Uiso 1 1 calc R . . C39 C -0.0048(8) 0.2833(5) 0.6156(5) 0.0638(19) Uani 1 1 d . . . H39A H -0.1087 0.2924 0.6404 0.096 Uiso 1 1 calc R . . H39B H 0.0100 0.2821 0.5528 0.096 Uiso 1 1 calc R . . H39C H 0.0417 0.3324 0.6290 0.096 Uiso 1 1 calc R . . Co1 Co 1.10206(7) 0.30454(4) 0.26753(4) 0.0303(2) Uani 1 1 d . . . F1 F 1.3981(6) 0.3326(3) -0.0529(3) 0.0852(8) Uani 1 1 d . . . F2 F 1.4817(6) 0.2207(3) 0.0242(3) 0.0852(8) Uani 1 1 d . . . F3 F 1.2739(6) 0.2269(3) -0.0035(3) 0.0852(8) Uani 1 1 d . . . F4 F 1.3620(6) 0.5620(3) 0.2313(5) 0.1148(12) Uani 1 1 d . . . F5 F 1.3502(7) 0.5854(3) 0.1019(5) 0.1148(12) Uani 1 1 d . . . F6 F 1.1593(6) 0.6014(3) 0.1982(5) 0.1148(12) Uani 1 1 d . . . F7 F 0.8163(5) 0.3980(3) 0.0631(3) 0.0868(8) Uani 1 1 d . . . F8 F 0.8826(6) 0.5226(3) 0.0734(3) 0.0868(8) Uani 1 1 d . . . F9 F 0.6703(6) 0.4955(3) 0.1353(3) 0.0868(8) Uani 1 1 d . . . F10 F 0.6821(15) 0.5291(9) 0.4275(10) 0.1084(19) Uani 0.50 1 d PD A 1 F11 F 0.8095(13) 0.4389(7) 0.5020(6) 0.1084(19) Uani 0.50 1 d PD A 1 F12 F 0.6395(13) 0.3891(7) 0.4663(7) 0.1084(19) Uani 0.50 1 d PD A 1 F10A F 0.6972(14) 0.3867(7) 0.4971(7) 0.1084(19) Uani 0.50 1 d PD A 2 F11A F 0.8399(12) 0.4824(7) 0.4800(7) 0.1084(19) Uani 0.50 1 d PD A 2 F12A F 0.6430(14) 0.5137(9) 0.4331(10) 0.1084(19) Uani 0.50 1 d PD A 2 N1 N 1.0644(4) 0.1660(3) 0.2762(2) 0.0247(8) Uani 1 1 d . A . N2 N 1.2078(4) 0.2458(3) 0.3682(3) 0.0301(9) Uani 1 1 d . A . N3 N 1.1266(4) -0.1127(3) 0.4468(3) 0.0310(9) Uani 1 1 d . . . N4 N 1.0297(4) -0.0177(3) 0.3136(2) 0.0259(8) Uani 1 1 d . . . O1 O 1.2476(4) 0.2671(2) 0.1588(2) 0.0348(8) Uani 1 1 d . A . O2 O 1.1984(4) 0.4207(3) 0.2505(3) 0.0434(9) Uani 1 1 d . A . O3 O 0.9727(4) 0.3636(2) 0.1827(2) 0.0366(8) Uani 1 1 d . A . O4 O 0.9342(4) 0.3517(3) 0.3636(2) 0.0453(10) Uani 1 1 d . A . O5 O 0.0564(5) 0.2013(3) 0.6512(3) 0.0595(12) Uani 1 1 d . . . H5 H 0.0091 0.1601 0.6458 0.089 Uiso 1 1 calc R . . S1 S 0.85244(14) 0.17555(8) 0.00433(8) 0.0312(3) Uani 1 1 d . . . S2 S 0.79755(13) -0.01400(8) 0.05019(8) 0.0291(3) Uani 1 1 d . . . S3 S 0.65822(13) -0.00541(8) -0.12092(8) 0.0295(3) Uani 1 1 d . . . S4 S 0.50515(14) -0.00274(9) -0.26974(8) 0.0336(3) Uani 1 1 d . . . S5 S 0.72035(14) 0.18180(8) -0.16617(8) 0.0310(3) Uani 1 1 d . . . S6 S 0.57549(14) 0.20665(9) -0.31906(8) 0.0335(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(3) 0.034(3) 0.037(3) 0.005(2) -0.008(2) 0.001(2) C2 0.056(4) 0.042(3) 0.037(3) 0.002(3) -0.010(3) 0.005(3) C3 0.041(3) 0.040(3) 0.047(3) 0.005(3) -0.005(3) -0.004(2) C4 0.031(3) 0.036(3) 0.061(4) -0.003(3) -0.009(3) -0.003(2) C5 0.039(3) 0.047(4) 0.096(6) -0.015(4) 0.000(4) -0.017(3) C6 0.038(3) 0.025(3) 0.056(4) -0.003(2) -0.011(3) -0.005(2) C7 0.047(4) 0.036(3) 0.067(4) 0.001(3) -0.014(3) 0.003(3) C8 0.044(3) 0.034(3) 0.064(4) 0.002(3) 0.001(3) 0.009(3) C9 0.050(4) 0.035(3) 0.057(4) -0.004(3) 0.007(3) 0.006(3) C10 0.136(5) 0.079(3) 0.069(2) 0.007(2) 0.034(2) 0.035(3) C10A 0.136(5) 0.079(3) 0.069(2) 0.007(2) 0.034(2) 0.035(3) C11 0.019(2) 0.034(3) 0.025(2) -0.012(2) -0.0037(18) -0.0012(19) C12 0.024(2) 0.038(3) 0.022(2) -0.009(2) -0.0057(19) -0.001(2) C13 0.035(3) 0.046(3) 0.038(3) -0.013(2) -0.009(2) -0.004(2) C14 0.039(3) 0.061(4) 0.034(3) -0.021(3) -0.012(2) -0.010(3) C15 0.034(3) 0.055(4) 0.027(3) -0.010(2) -0.013(2) -0.002(2) C16 0.023(2) 0.051(3) 0.023(2) -0.011(2) -0.0049(19) -0.001(2) C17 0.024(2) 0.040(3) 0.022(2) -0.005(2) -0.0036(19) 0.001(2) C18 0.023(2) 0.044(3) 0.018(2) -0.004(2) -0.0043(19) 0.002(2) C19 0.039(3) 0.039(3) 0.027(3) 0.002(2) -0.008(2) 0.003(2) C20 0.038(3) 0.052(4) 0.028(3) 0.007(2) -0.012(2) 0.006(2) C21 0.034(3) 0.058(4) 0.030(3) -0.006(2) -0.016(2) 0.000(3) C22 0.025(2) 0.033(3) 0.022(2) -0.0039(19) -0.0043(19) -0.0004(19) C23 0.021(2) 0.031(3) 0.024(2) -0.0022(19) -0.0044(18) -0.0019(19) C24 0.019(2) 0.027(2) 0.024(2) -0.0057(19) -0.0052(18) 0.0003(18) C25 0.027(2) 0.025(2) 0.024(2) -0.0021(18) -0.0078(19) -0.0036(18) C26 0.022(2) 0.030(3) 0.022(2) -0.0019(19) -0.0068(18) 0.0006(18) C27 0.031(2) 0.027(2) 0.024(2) -0.0053(19) -0.009(2) -0.0024(19) C28 0.026(2) 0.025(2) 0.026(2) -0.0064(19) -0.0067(19) -0.0025(18) C29 0.029(2) 0.022(2) 0.029(2) -0.0019(19) -0.009(2) -0.0034(19) C30 0.024(2) 0.028(2) 0.024(2) -0.0040(19) -0.0054(19) -0.0002(18) C31 0.025(2) 0.033(3) 0.022(2) -0.0063(19) -0.0096(19) -0.0008(19) C32 0.031(3) 0.031(3) 0.030(3) -0.004(2) -0.010(2) -0.003(2) C33 0.030(3) 0.040(3) 0.034(3) -0.010(2) -0.010(2) -0.004(2) C34 0.044(3) 0.044(3) 0.054(4) -0.012(3) -0.012(3) -0.008(3) C35 0.027(2) 0.031(3) 0.023(2) -0.0049(19) -0.0081(19) -0.0021(19) C36 0.038(3) 0.032(3) 0.036(3) -0.002(2) -0.016(2) 0.004(2) C37 0.037(3) 0.045(3) 0.053(4) -0.009(3) -0.012(3) 0.001(2) C38 0.041(3) 0.059(4) 0.066(4) -0.018(3) -0.010(3) 0.006(3) C39 0.064(4) 0.077(5) 0.055(4) -0.007(4) -0.009(3) -0.025(4) Co1 0.0292(4) 0.0318(4) 0.0312(4) -0.0081(3) -0.0067(3) -0.0026(3) F1 0.111(2) 0.0875(19) 0.0449(13) -0.0065(13) 0.0009(14) 0.0043(16) F2 0.111(2) 0.0875(19) 0.0449(13) -0.0065(13) 0.0009(14) 0.0043(16) F3 0.111(2) 0.0875(19) 0.0449(13) -0.0065(13) 0.0009(14) 0.0043(16) F4 0.108(2) 0.0535(16) 0.181(3) -0.0193(19) -0.011(2) -0.0254(16) F5 0.108(2) 0.0535(16) 0.181(3) -0.0193(19) -0.011(2) -0.0254(16) F6 0.108(2) 0.0535(16) 0.181(3) -0.0193(19) -0.011(2) -0.0254(16) F7 0.092(2) 0.0808(18) 0.0869(19) 0.0119(15) -0.0353(16) 0.0049(15) F8 0.092(2) 0.0808(18) 0.0869(19) 0.0119(15) -0.0353(16) 0.0049(15) F9 0.092(2) 0.0808(18) 0.0869(19) 0.0119(15) -0.0353(16) 0.0049(15) F10 0.136(5) 0.079(3) 0.069(2) 0.007(2) 0.034(2) 0.035(3) F11 0.136(5) 0.079(3) 0.069(2) 0.007(2) 0.034(2) 0.035(3) F12 0.136(5) 0.079(3) 0.069(2) 0.007(2) 0.034(2) 0.035(3) F10A 0.136(5) 0.079(3) 0.069(2) 0.007(2) 0.034(2) 0.035(3) F11A 0.136(5) 0.079(3) 0.069(2) 0.007(2) 0.034(2) 0.035(3) F12A 0.136(5) 0.079(3) 0.069(2) 0.007(2) 0.034(2) 0.035(3) N1 0.0217(19) 0.031(2) 0.0225(19) -0.0038(16) -0.0079(16) 0.0002(16) N2 0.030(2) 0.034(2) 0.029(2) -0.0100(18) -0.0078(17) -0.0052(17) N3 0.032(2) 0.033(2) 0.026(2) 0.0026(17) -0.0079(18) 0.0000(18) N4 0.026(2) 0.033(2) 0.0204(19) -0.0012(16) -0.0088(16) -0.0038(16) O1 0.0342(19) 0.0331(19) 0.0353(19) -0.0049(16) -0.0052(15) 0.0006(15) O2 0.045(2) 0.040(2) 0.049(2) -0.0116(18) -0.0113(19) -0.0078(18) O3 0.0335(19) 0.0308(19) 0.047(2) -0.0076(16) -0.0110(16) 0.0001(15) O4 0.045(2) 0.044(2) 0.042(2) -0.0064(18) 0.0008(18) 0.0022(18) O5 0.067(3) 0.069(3) 0.053(3) -0.003(2) -0.022(2) -0.028(2) S1 0.0425(7) 0.0284(6) 0.0281(6) 0.0008(5) -0.0187(5) -0.0071(5) S2 0.0366(7) 0.0271(6) 0.0284(6) -0.0031(5) -0.0159(5) -0.0047(5) S3 0.0363(7) 0.0290(6) 0.0276(6) -0.0016(5) -0.0160(5) -0.0052(5) S4 0.0421(7) 0.0362(7) 0.0281(6) -0.0031(5) -0.0184(6) -0.0057(6) S5 0.0392(7) 0.0297(6) 0.0274(6) -0.0007(5) -0.0138(5) -0.0058(5) S6 0.0390(7) 0.0372(7) 0.0234(6) 0.0019(5) -0.0093(5) -0.0011(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 C1 O1 1.254(6) . ? C1 C3 1.388(8) . ? C1 C2 1.492(8) . ? C2 F1 1.301(7) . ? C2 F2 1.328(7) . ? C2 F3 1.356(8) . ? C3 C4 1.390(8) . ? C3 H3A 0.9500 . ? C4 O2 1.260(7) . ? C4 C5 1.478(8) . ? C5 F6 1.300(8) . ? C5 F5 1.332(9) . ? C5 F4 1.339(10) . ? C6 O3 1.248(6) . ? C6 C8 1.390(8) . ? C6 C7 1.508(9) . ? C7 F7 1.306(8) . ? C7 F8 1.331(8) . ? C7 F9 1.337(8) . ? C8 C9 1.386(9) . ? C8 H8A 0.9500 . ? C9 O4 1.261(7) . ? C9 C10 1.51(3) . ? C9 C10A 1.53(3) . ? C10 F12 1.319(17) . ? C10 F10 1.325(16) . ? C10 F11 1.355(17) . ? C10A F12A 1.314(17) . ? C10A F10A 1.317(17) . ? C10A F11A 1.379(18) . ? C11 N1 1.336(6) . ? C11 C22 1.406(7) . ? C11 C12 1.453(6) . ? C12 N2 1.347(6) . ? C12 C16 1.406(7) . ? C13 N2 1.336(6) . ? C13 C14 1.404(8) . ? C13 H13A 0.9500 . ? C14 C15 1.376(8) . ? C14 H14A 0.9500 . ? C15 C16 1.402(7) . ? C15 H15A 0.9500 . ? C16 C17 1.455(8) . ? C17 C21 1.409(7) . ? C17 C18 1.416(7) . ? C18 N3 1.339(7) . ? C18 C22 1.467(7) . ? C19 N3 1.333(6) . ? C19 C20 1.388(8) . ? C19 H19A 0.9500 . ? C20 C21 1.355(8) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 N4 1.339(6) . ? C23 N4 1.358(6) . ? C23 C24 1.424(7) . ? C23 C29 1.425(6) . ? C24 N1 1.351(6) . ? C24 C25 1.423(6) . ? C25 C26 1.363(6) . ? C25 H25A 0.9500 . ? C26 C28 1.431(7) . ? C26 S1 1.741(5) . ? C27 C30 1.339(7) . ? C27 S1 1.748(5) . ? C27 S2 1.769(5) . ? C28 C29 1.361(7) . ? C28 S2 1.748(4) . ? C29 H29A 0.9500 . ? C30 S5 1.754(5) . ? C30 S3 1.757(5) . ? C31 C35 1.344(7) . ? C31 S3 1.755(5) . ? C31 S4 1.756(4) . ? C32 C33 1.515(6) . ? C32 S4 1.808(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.519(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 S6 1.744(5) . ? C35 S5 1.759(5) . ? C36 C37 1.518(8) . ? C36 S6 1.818(5) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.516(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 O5 1.407(9) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? Co1 O1 2.048(3) . ? Co1 O2 2.058(4) . ? Co1 O4 2.065(4) . ? Co1 O3 2.069(4) . ? Co1 N2 2.120(4) . ? Co1 N1 2.157(4) . ? O5 H5 0.8400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C3 127.3(5) . . ? O1 C1 C2 113.7(5) . . ? C3 C1 C2 118.9(5) . . ? F1 C2 F2 109.1(5) . . ? F1 C2 F3 104.6(5) . . ? F2 C2 F3 103.6(5) . . ? F1 C2 C1 116.6(5) . . ? F2 C2 C1 111.5(5) . . ? F3 C2 C1 110.6(5) . . ? C1 C3 C4 121.9(5) . . ? C1 C3 H3A 119.0 . . ? C4 C3 H3A 119.0 . . ? O2 C4 C3 128.0(5) . . ? O2 C4 C5 113.7(6) . . ? C3 C4 C5 118.3(6) . . ? F6 C5 F5 106.7(7) . . ? F6 C5 F4 105.5(6) . . ? F5 C5 F4 101.7(6) . . ? F6 C5 C4 114.1(5) . . ? F5 C5 C4 115.6(6) . . ? F4 C5 C4 112.0(7) . . ? O3 C6 C8 127.3(6) . . ? O3 C6 C7 113.5(5) . . ? C8 C6 C7 119.2(5) . . ? F7 C7 F8 105.7(6) . . ? F7 C7 F9 107.4(6) . . ? F8 C7 F9 105.6(5) . . ? F7 C7 C6 112.7(5) . . ? F8 C7 C6 112.2(5) . . ? F9 C7 C6 112.8(6) . . ? C9 C8 C6 121.5(5) . . ? C9 C8 H8A 119.3 . . ? C6 C8 H8A 119.3 . . ? O4 C9 C8 128.7(6) . . ? O4 C9 C10 114.8(9) . . ? C8 C9 C10 116.4(8) . . ? O4 C9 C10A 113.2(9) . . ? C8 C9 C10A 118.1(8) . . ? C10 C9 C10A 5.4(12) . . ? F12 C10 F10 113.1(17) . . ? F12 C10 F11 102.4(15) . . ? F10 C10 F11 105.2(16) . . ? F12 C10 C9 110.0(15) . . ? F10 C10 C9 112.5(15) . . ? F11 C10 C9 113.2(16) . . ? F12A C10A F10A 107.5(16) . . ? F12A C10A F11A 105.2(17) . . ? F10A C10A F11A 100.8(15) . . ? F12A C10A C9 117.1(16) . . ? F10A C10A C9 114.4(15) . . ? F11A C10A C9 110.3(15) . . ? N1 C11 C22 122.0(4) . . ? N1 C11 C12 118.5(4) . . ? C22 C11 C12 119.4(4) . . ? N2 C12 C16 123.4(4) . . ? N2 C12 C11 115.8(4) . . ? C16 C12 C11 120.8(5) . . ? N2 C13 C14 121.0(5) . . ? N2 C13 H13A 119.5 . . ? C14 C13 H13A 119.5 . . ? C15 C14 C13 119.8(5) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C14 C15 C16 120.0(5) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C15 C16 C12 116.5(5) . . ? C15 C16 C17 123.8(5) . . ? C12 C16 C17 119.7(4) . . ? C21 C17 C18 115.3(5) . . ? C21 C17 C16 124.3(5) . . ? C18 C17 C16 120.4(4) . . ? N3 C18 C17 124.3(4) . . ? N3 C18 C22 116.7(4) . . ? C17 C18 C22 119.0(5) . . ? N3 C19 C20 122.9(5) . . ? N3 C19 H19A 118.5 . . ? C20 C19 H19A 118.5 . . ? C21 C20 C19 119.4(5) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.3 . . ? C20 C21 C17 120.5(5) . . ? C20 C21 H21A 119.7 . . ? C17 C21 H21A 119.7 . . ? N4 C22 C11 122.1(4) . . ? N4 C22 C18 117.3(4) . . ? C11 C22 C18 120.7(4) . . ? N4 C23 C24 121.7(4) . . ? N4 C23 C29 118.3(4) . . ? C24 C23 C29 120.0(4) . . ? N1 C24 C25 120.0(4) . . ? N1 C24 C23 120.6(4) . . ? C25 C24 C23 119.4(4) . . ? C26 C25 C24 119.2(4) . . ? C26 C25 H25A 120.4 . . ? C24 C25 H25A 120.4 . . ? C25 C26 C28 121.4(4) . . ? C25 C26 S1 122.4(4) . . ? C28 C26 S1 116.2(3) . . ? C30 C27 S1 121.6(4) . . ? C30 C27 S2 123.3(4) . . ? S1 C27 S2 115.1(3) . . ? C29 C28 C26 120.6(4) . . ? C29 C28 S2 123.3(4) . . ? C26 C28 S2 116.1(3) . . ? C28 C29 C23 119.3(4) . . ? C28 C29 H29A 120.4 . . ? C23 C29 H29A 120.4 . . ? C27 C30 S5 123.0(4) . . ? C27 C30 S3 122.6(4) . . ? S5 C30 S3 114.4(3) . . ? C35 C31 S3 118.2(3) . . ? C35 C31 S4 122.6(4) . . ? S3 C31 S4 119.2(3) . . ? C33 C32 S4 106.7(3) . . ? C33 C32 H32A 110.4 . . ? S4 C32 H32A 110.4 . . ? C33 C32 H32B 110.4 . . ? S4 C32 H32B 110.4 . . ? H32A C32 H32B 108.6 . . ? C32 C33 C34 112.9(4) . . ? C32 C33 H33A 109.0 . . ? C34 C33 H33A 109.0 . . ? C32 C33 H33B 109.0 . . ? C34 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 S6 125.3(4) . . ? C31 C35 S5 116.2(4) . . ? S6 C35 S5 118.4(3) . . ? C37 C36 S6 114.0(4) . . ? C37 C36 H36A 108.8 . . ? S6 C36 H36A 108.8 . . ? C37 C36 H36B 108.8 . . ? S6 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C38 C37 C36 112.0(5) . . ? C38 C37 H37A 109.2 . . ? C36 C37 H37A 109.2 . . ? C38 C37 H37B 109.2 . . ? C36 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O5 C39 H39A 109.5 . . ? O5 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O5 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O1 Co1 O2 86.30(15) . . ? O1 Co1 O4 170.72(16) . . ? O2 Co1 O4 93.51(16) . . ? O1 Co1 O3 85.19(14) . . ? O2 Co1 O3 88.27(15) . . ? O4 Co1 O3 85.53(15) . . ? O1 Co1 N2 102.55(15) . . ? O2 Co1 N2 94.43(16) . . ? O4 Co1 N2 86.72(16) . . ? O3 Co1 N2 171.94(15) . . ? O1 Co1 N1 81.71(14) . . ? O2 Co1 N1 163.64(15) . . ? O4 Co1 N1 100.12(15) . . ? O3 Co1 N1 101.69(14) . . ? N2 Co1 N1 77.49(15) . . ? C11 N1 C24 117.1(4) . . ? C11 N1 Co1 112.8(3) . . ? C24 N1 Co1 130.0(3) . . ? C13 N2 C12 119.3(5) . . ? C13 N2 Co1 125.5(4) . . ? C12 N2 Co1 115.1(3) . . ? C19 N3 C18 117.5(4) . . ? C22 N4 C23 116.3(4) . . ? C1 O1 Co1 124.3(3) . . ? C4 O2 Co1 123.5(4) . . ? C6 O3 Co1 127.9(4) . . ? C9 O4 Co1 125.9(4) . . ? C39 O5 H5 109.5 . . ? C26 S1 C27 96.6(2) . . ? C28 S2 C27 96.0(2) . . ? C31 S3 C30 95.0(2) . . ? C31 S4 C32 103.4(2) . . ? C30 S5 C35 95.8(2) . . ? C35 S6 C36 101.3(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 O1 C1 C2 F1 167.5(5) . . . . ? C3 C1 C2 F1 -15.2(8) . . . . ? O1 C1 C2 F2 -66.4(7) . . . . ? C3 C1 C2 F2 111.0(6) . . . . ? O1 C1 C2 F3 48.2(7) . . . . ? C3 C1 C2 F3 -134.4(6) . . . . ? O1 C1 C3 C4 1.5(9) . . . . ? C2 C1 C3 C4 -175.4(5) . . . . ? C1 C3 C4 O2 -2.8(10) . . . . ? C1 C3 C4 C5 177.4(6) . . . . ? O2 C4 C5 F6 -58.6(9) . . . . ? C3 C4 C5 F6 121.2(7) . . . . ? O2 C4 C5 F5 177.0(6) . . . . ? C3 C4 C5 F5 -3.2(9) . . . . ? O2 C4 C5 F4 61.1(7) . . . . ? C3 C4 C5 F4 -119.1(7) . . . . ? O3 C6 C7 F7 38.2(7) . . . . ? C8 C6 C7 F7 -142.3(6) . . . . ? O3 C6 C7 F8 -81.0(6) . . . . ? C8 C6 C7 F8 98.5(7) . . . . ? O3 C6 C7 F9 160.0(5) . . . . ? C8 C6 C7 F9 -20.5(8) . . . . ? O3 C6 C8 C9 -6.0(10) . . . . ? C7 C6 C8 C9 174.6(6) . . . . ? C6 C8 C9 O4 2.5(11) . . . . ? C6 C8 C9 C10 -172.8(9) . . . . ? C6 C8 C9 C10A -178.5(10) . . . . ? O4 C9 C10 F12 -82.0(14) . . . . ? C8 C9 C10 F12 93.9(13) . . . . ? C10A C9 C10 F12 -156(14) . . . . ? O4 C9 C10 F10 150.9(13) . . . . ? C8 C9 C10 F10 -33.1(18) . . . . ? C10A C9 C10 F10 77(13) . . . . ? O4 C9 C10 F11 31.9(16) . . . . ? C8 C9 C10 F11 -152.1(11) . . . . ? C10A C9 C10 F11 -42(12) . . . . ? O4 C9 C10A F12A 179.2(13) . . . . ? C8 C9 C10A F12A 0.0(19) . . . . ? C10 C9 C10A F12A -72(13) . . . . ? O4 C9 C10A F10A -53.8(17) . . . . ? C8 C9 C10A F10A 127.1(13) . . . . ? C10 C9 C10A F10A 55(12) . . . . ? O4 C9 C10A F11A 58.9(14) . . . . ? C8 C9 C10A F11A -120.2(11) . . . . ? C10 C9 C10A F11A 167(14) . . . . ? N1 C11 C12 N2 -0.4(6) . . . . ? C22 C11 C12 N2 178.0(4) . . . . ? N1 C11 C12 C16 -179.1(4) . . . . ? C22 C11 C12 C16 -0.6(7) . . . . ? N2 C13 C14 C15 0.2(8) . . . . ? C13 C14 C15 C16 -0.4(8) . . . . ? C14 C15 C16 C12 -0.1(7) . . . . ? C14 C15 C16 C17 179.4(5) . . . . ? N2 C12 C16 C15 0.8(7) . . . . ? C11 C12 C16 C15 179.3(4) . . . . ? N2 C12 C16 C17 -178.8(4) . . . . ? C11 C12 C16 C17 -0.3(7) . . . . ? C15 C16 C17 C21 -0.2(8) . . . . ? C12 C16 C17 C21 179.4(5) . . . . ? C15 C16 C17 C18 -179.9(5) . . . . ? C12 C16 C17 C18 -0.3(7) . . . . ? C21 C17 C18 N3 2.3(7) . . . . ? C16 C17 C18 N3 -178.0(4) . . . . ? C21 C17 C18 C22 -178.0(4) . . . . ? C16 C17 C18 C22 1.7(7) . . . . ? N3 C19 C20 C21 1.1(8) . . . . ? C19 C20 C21 C17 -0.9(8) . . . . ? C18 C17 C21 C20 -0.7(7) . . . . ? C16 C17 C21 C20 179.7(5) . . . . ? N1 C11 C22 N4 -0.1(7) . . . . ? C12 C11 C22 N4 -178.5(4) . . . . ? N1 C11 C22 C18 -179.6(4) . . . . ? C12 C11 C22 C18 2.0(7) . . . . ? N3 C18 C22 N4 -2.3(6) . . . . ? C17 C18 C22 N4 178.0(4) . . . . ? N3 C18 C22 C11 177.2(4) . . . . ? C17 C18 C22 C11 -2.5(7) . . . . ? N4 C23 C24 N1 -2.3(7) . . . . ? C29 C23 C24 N1 178.7(4) . . . . ? N4 C23 C24 C25 176.4(4) . . . . ? C29 C23 C24 C25 -2.5(6) . . . . ? N1 C24 C25 C26 179.5(4) . . . . ? C23 C24 C25 C26 0.8(6) . . . . ? C24 C25 C26 C28 1.9(7) . . . . ? C24 C25 C26 S1 -178.7(3) . . . . ? C25 C26 C28 C29 -2.9(7) . . . . ? S1 C26 C28 C29 177.6(4) . . . . ? C25 C26 C28 S2 178.7(4) . . . . ? S1 C26 C28 S2 -0.7(5) . . . . ? C26 C28 C29 C23 1.1(7) . . . . ? S2 C28 C29 C23 179.3(3) . . . . ? N4 C23 C29 C28 -177.4(4) . . . . ? C24 C23 C29 C28 1.6(7) . . . . ? S1 C27 C30 S5 1.3(6) . . . . ? S2 C27 C30 S5 -176.6(3) . . . . ? S1 C27 C30 S3 178.9(2) . . . . ? S2 C27 C30 S3 0.9(6) . . . . ? S4 C32 C33 C34 177.0(4) . . . . ? S3 C31 C35 S6 178.1(3) . . . . ? S4 C31 C35 S6 -1.4(6) . . . . ? S3 C31 C35 S5 1.2(5) . . . . ? S4 C31 C35 S5 -178.2(2) . . . . ? S6 C36 C37 C38 -175.4(4) . . . . ? C22 C11 N1 C24 -4.3(6) . . . . ? C12 C11 N1 C24 174.2(4) . . . . ? C22 C11 N1 Co1 178.1(3) . . . . ? C12 C11 N1 Co1 -3.4(5) . . . . ? C25 C24 N1 C11 -173.3(4) . . . . ? C23 C24 N1 C11 5.4(6) . . . . ? C25 C24 N1 Co1 3.8(6) . . . . ? C23 C24 N1 Co1 -177.5(3) . . . . ? O1 Co1 N1 C11 109.1(3) . . . . ? O2 Co1 N1 C11 65.9(6) . . . . ? O4 Co1 N1 C11 -80.1(3) . . . . ? O3 Co1 N1 C11 -167.6(3) . . . . ? N2 Co1 N1 C11 4.2(3) . . . . ? O1 Co1 N1 C24 -68.1(4) . . . . ? O2 Co1 N1 C24 -111.4(6) . . . . ? O4 Co1 N1 C24 102.7(4) . . . . ? O3 Co1 N1 C24 15.2(4) . . . . ? N2 Co1 N1 C24 -173.0(4) . . . . ? C14 C13 N2 C12 0.4(7) . . . . ? C14 C13 N2 Co1 176.2(4) . . . . ? C16 C12 N2 C13 -0.9(7) . . . . ? C11 C12 N2 C13 -179.5(4) . . . . ? C16 C12 N2 Co1 -177.2(4) . . . . ? C11 C12 N2 Co1 4.2(5) . . . . ? O1 Co1 N2 C13 101.1(4) . . . . ? O2 Co1 N2 C13 13.9(4) . . . . ? O4 Co1 N2 C13 -79.4(4) . . . . ? O3 Co1 N2 C13 -95.5(11) . . . . ? N1 Co1 N2 C13 179.5(4) . . . . ? O1 Co1 N2 C12 -83.0(3) . . . . ? O2 Co1 N2 C12 -170.2(3) . . . . ? O4 Co1 N2 C12 96.6(3) . . . . ? O3 Co1 N2 C12 80.5(11) . . . . ? N1 Co1 N2 C12 -4.6(3) . . . . ? C20 C19 N3 C18 0.4(7) . . . . ? C17 C18 N3 C19 -2.2(7) . . . . ? C22 C18 N3 C19 178.2(4) . . . . ? C11 C22 N4 C23 3.2(7) . . . . ? C18 C22 N4 C23 -177.3(4) . . . . ? C24 C23 N4 C22 -2.0(6) . . . . ? C29 C23 N4 C22 176.9(4) . . . . ? C3 C1 O1 Co1 20.9(8) . . . . ? C2 C1 O1 Co1 -162.0(4) . . . . ? O2 Co1 O1 C1 -29.3(4) . . . . ? O4 Co1 O1 C1 59.8(11) . . . . ? O3 Co1 O1 C1 59.3(4) . . . . ? N2 Co1 O1 C1 -123.0(4) . . . . ? N1 Co1 O1 C1 161.9(4) . . . . ? C3 C4 O2 Co1 -18.3(8) . . . . ? C5 C4 O2 Co1 161.5(4) . . . . ? O1 Co1 O2 C4 27.8(4) . . . . ? O4 Co1 O2 C4 -142.9(4) . . . . ? O3 Co1 O2 C4 -57.5(4) . . . . ? N2 Co1 O2 C4 130.1(4) . . . . ? N1 Co1 O2 C4 70.6(7) . . . . ? C8 C6 O3 Co1 -7.4(8) . . . . ? C7 C6 O3 Co1 172.0(4) . . . . ? O1 Co1 O3 C6 -164.3(4) . . . . ? O2 Co1 O3 C6 -77.9(4) . . . . ? O4 Co1 O3 C6 15.8(4) . . . . ? N2 Co1 O3 C6 31.9(12) . . . . ? N1 Co1 O3 C6 115.2(4) . . . . ? C8 C9 O4 Co1 13.6(10) . . . . ? C10 C9 O4 Co1 -171.0(8) . . . . ? C10A C9 O4 Co1 -165.4(8) . . . . ? O1 Co1 O4 C9 -18.9(12) . . . . ? O2 Co1 O4 C9 69.6(5) . . . . ? O3 Co1 O4 C9 -18.4(5) . . . . ? N2 Co1 O4 C9 163.9(5) . . . . ? N1 Co1 O4 C9 -119.5(5) . . . . ? C25 C26 S1 C27 -177.9(4) . . . . ? C28 C26 S1 C27 1.6(4) . . . . ? C30 C27 S1 C26 179.9(4) . . . . ? S2 C27 S1 C26 -1.9(3) . . . . ? C29 C28 S2 C27 -178.8(4) . . . . ? C26 C28 S2 C27 -0.5(4) . . . . ? C30 C27 S2 C28 179.7(4) . . . . ? S1 C27 S2 C28 1.6(3) . . . . ? C35 C31 S3 C30 3.1(4) . . . . ? S4 C31 S3 C30 -177.5(3) . . . . ? C27 C30 S3 C31 176.0(4) . . . . ? S5 C30 S3 C31 -6.2(3) . . . . ? C35 C31 S4 C32 -178.6(4) . . . . ? S3 C31 S4 C32 2.0(3) . . . . ? C33 C32 S4 C31 -177.6(3) . . . . ? C27 C30 S5 C35 -175.5(4) . . . . ? S3 C30 S5 C35 6.8(3) . . . . ? C31 C35 S5 C30 -4.8(4) . . . . ? S6 C35 S5 C30 178.1(3) . . . . ? C31 C35 S6 C36 102.8(5) . . . . ? S5 C35 S6 C36 -80.3(3) . . . . ? C37 C36 S6 C35 -66.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.14 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.110 _refine_diff_density_min -1.192 _refine_diff_density_rms 0.106 # Attachment 'Complex2-mod.CIF' data_complex2 _database_code_depnum_ccdc_archive 'CCDC 806936' #TrackingRef 'Complex2-mod.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52.50 H34 Cl1.50 Co F24 N4.50 Ni O9 S6' _chemical_formula_weight 1691.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.3332(14) _cell_length_b 17.2210(17) _cell_length_c 25.434(2) _cell_angle_alpha 70.737(7) _cell_angle_beta 78.157(7) _cell_angle_gamma 70.913(7) _cell_volume 6344.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 21563 _cell_measurement_theta_min 1.30 _cell_measurement_theta_max 25.09 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3380 _exptl_absorpt_coefficient_mu 0.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.72162 _exptl_absorpt_correction_T_max 0.78061 _exptl_absorpt_process_details 'MULSCANABS in PLATON (Spek, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-2' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 47711 _diffrn_reflns_av_R_equivalents 0.0939 _diffrn_reflns_av_sigmaI/netI 0.2286 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.20 _reflns_number_total 21793 _reflns_number_gt 8273 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area V1.26 (STOE, 2005)' _computing_cell_refinement 'X-Area V1.26' _computing_data_reduction 'X-RED32 V1.26 (STOE, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material SHELXL-97 _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0745P)^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 21793 _refine_ls_number_parameters 1583 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1685 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.1852 _refine_ls_wR_factor_gt 0.1628 _refine_ls_goodness_of_fit_ref 0.831 _refine_ls_restrained_S_all 0.836 _refine_ls_shift/su_max 0.018 _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 Co1 Co 0.60308(7) 0.08365(7) 0.67571(5) 0.032 Uani 0.50 1 d P . . Ni1 Ni 0.60308(7) 0.08365(7) 0.67571(5) 0.032 Uani 0.50 1 d P . . Co2 Co 0.21091(7) 0.24944(7) 0.55926(5) 0.029 Uani 0.50 1 d P . . Ni2 Ni 0.21091(7) 0.24944(7) 0.55926(5) 0.029 Uani 0.50 1 d P . . S1 S 0.66582(14) 0.04953(16) 0.44695(10) 0.043 Uani 1 1 d . . . S2 S 0.49882(15) 0.10792(16) 0.39757(9) 0.040 Uani 1 1 d . . . S3 S 0.77264(16) 0.01891(16) 0.33173(10) 0.047 Uani 1 1 d . . . S4 S 0.88523(19) 0.03401(17) 0.22172(12) 0.063 Uani 1 1 d . . . S5 S 0.60911(17) 0.07427(16) 0.28049(10) 0.047 Uani 1 1 d . . . S6 S 0.7046(2) 0.08497(19) 0.16376(11) 0.067 Uani 1 1 d . . . F8 F 0.7780(4) -0.2418(4) 0.6997(3) 0.093 Uani 1 1 d . . . F9 F 0.6407(4) -0.2142(4) 0.7051(3) 0.076 Uani 1 1 d . . . F10 F 0.7112(4) -0.1665(4) 0.6268(3) 0.072 Uani 1 1 d . . . F11 F 0.8674(4) 0.0172(5) 0.7482(3) 0.101 Uani 1 1 d . . . F12 F 0.7771(5) 0.0038(5) 0.8221(3) 0.098 Uani 1 1 d . . . F13 F 0.8631(4) -0.1075(4) 0.8005(3) 0.089 Uani 1 1 d . . . F5 F 0.5401(4) 0.3903(4) 0.6131(3) 0.091 Uani 1 1 d . . . F6 F 0.5697(4) 0.3490(4) 0.6967(3) 0.091 Uani 1 1 d . . . F7 F 0.6663(4) 0.3844(4) 0.6305(3) 0.091 Uani 1 1 d . . . F1 F 0.8163(10) 0.1183(10) 0.5224(6) 0.105 Uiso 0.50 1 d PD A 1 F2 F 0.8831(10) 0.0362(9) 0.5984(7) 0.105 Uiso 0.50 1 d PD A 1 F3 F 0.8834(10) 0.1726(10) 0.5599(8) 0.105 Uiso 0.50 1 d PD A 1 F1A F 0.8508(10) 0.0762(9) 0.5364(7) 0.105 Uiso 0.50 1 d PD A 2 F2A F 0.8387(10) 0.2036(8) 0.5248(6) 0.105 Uiso 0.50 1 d PD A 2 F3A F 0.8995(10) 0.1247(10) 0.5977(7) 0.105 Uiso 0.50 1 d PD A 2 F14 F 0.2417(6) 0.4714(4) 0.3609(3) 0.105 Uani 1 1 d . . . F15 F 0.1845(6) 0.3731(5) 0.3733(3) 0.117 Uani 1 1 d . . . F16 F 0.3200(6) 0.3435(5) 0.3626(3) 0.116 Uani 1 1 d . . . F17 F 0.3185(4) 0.5313(4) 0.5047(2) 0.072 Uani 1 1 d . . . F18 F 0.3653(4) 0.4275(4) 0.5758(3) 0.066 Uani 1 1 d . . . F19 F 0.2351(4) 0.5054(4) 0.5805(3) 0.064 Uani 1 1 d . . . F20 F -0.0440(4) 0.4380(4) 0.4664(3) 0.100 Uani 1 1 d . . . F21 F -0.0674(4) 0.4372(4) 0.5500(3) 0.098 Uani 1 1 d . . . F22 F -0.1200(4) 0.3624(4) 0.5226(4) 0.100 Uani 1 1 d . . . F23 F 0.1797(4) 0.0722(4) 0.4689(3) 0.067 Uani 1 1 d . . . F24 F 0.0394(4) 0.1051(4) 0.4814(3) 0.073 Uani 1 1 d . . . F25 F 0.1144(4) 0.0244(4) 0.5477(3) 0.070 Uani 1 1 d . . . O3 O 0.6298(4) -0.0412(4) 0.6772(3) 0.047 Uani 1 1 d . . . O4 O 0.6916(4) 0.0480(4) 0.7322(3) 0.046 Uani 1 1 d . . . O2 O 0.5805(4) 0.2117(4) 0.6649(3) 0.053 Uani 1 1 d . . . O1 O 0.7066(4) 0.0897(4) 0.6150(3) 0.053 Uani 1 1 d . . . O5 O 0.2364(4) 0.2950(3) 0.4742(2) 0.037 Uani 1 1 d . . . O6 O 0.2510(3) 0.3465(3) 0.5680(2) 0.033 Uani 1 1 d . . . O7 O 0.0860(3) 0.3269(3) 0.5514(2) 0.035 Uani 1 1 d . . . O8 O 0.1791(3) 0.1565(3) 0.5437(2) 0.035 Uani 1 1 d . . . N1 N 0.4973(4) 0.1100(4) 0.6284(3) 0.024 Uani 1 1 d . . . N2 N 0.4985(4) 0.0882(4) 0.7375(3) 0.032 Uani 1 1 d . . . N3 N 0.1867(4) 0.2072(4) 0.6455(3) 0.029 Uani 1 1 d . . . N4 N 0.3382(4) 0.1687(4) 0.5817(3) 0.026 Uani 1 1 d . . . C6 C 0.6956(5) -0.0998(6) 0.6963(4) 0.044 Uani 1 1 d . . . C7 C 0.7089(7) -0.1816(6) 0.6822(5) 0.062 Uani 1 1 d . . . C8 C 0.7546(6) -0.0960(6) 0.7281(4) 0.047 Uani 1 1 d . . . H8 H 0.8018 -0.1455 0.7394 0.070 Uiso 1 1 calc R . . C9 C 0.7479(5) -0.0247(6) 0.7436(4) 0.039 Uani 1 1 d . . . C10 C 0.8134(7) -0.0279(7) 0.7793(5) 0.067 Uani 1 1 d . . . C4 C 0.6356(6) 0.2515(7) 0.6413(4) 0.053 Uani 1 1 d . . . C5 C 0.6044(7) 0.3438(8) 0.6437(6) 0.074 Uani 1 1 d . . . C3 C 0.7156(6) 0.2244(6) 0.6147(4) 0.053 Uani 1 1 d . . . H3 H 0.7535 0.2600 0.6046 0.080 Uiso 1 1 calc R . . C1 C 0.7451(6) 0.1470(7) 0.6014(4) 0.053 Uani 1 1 d . A . C2 C 0.8442(6) 0.1153(6) 0.5690(4) 0.053 Uani 1 1 d D . . C11 C 0.4207(5) 0.1281(5) 0.6596(3) 0.026 Uani 1 1 d . . . C12 C 0.4196(5) 0.1133(5) 0.7189(3) 0.029 Uani 1 1 d . . . C13 C 0.5009(6) 0.0726(6) 0.7923(4) 0.045 Uani 1 1 d . . . H13 H 0.5562 0.0544 0.8057 0.067 Uiso 1 1 calc R . . C14 C 0.4277(6) 0.0813(5) 0.8303(4) 0.038 Uani 1 1 d . . . H14 H 0.4328 0.0714 0.8687 0.057 Uiso 1 1 calc R . . C15 C 0.3468(6) 0.1043(5) 0.8123(4) 0.037 Uani 1 1 d . . . H15 H 0.2956 0.1072 0.8382 0.055 Uiso 1 1 calc R . . C16 C 0.3415(5) 0.1237(5) 0.7541(3) 0.027 Uani 1 1 d . . . C17 C 0.2592(5) 0.1515(5) 0.7305(3) 0.026 Uani 1 1 d . . . C18 C 0.2598(5) 0.1739(5) 0.6724(4) 0.029 Uani 1 1 d . . . C19 C 0.2504(5) 0.3666(6) 0.4491(4) 0.040 Uani 1 1 d . . . C20 C 0.2473(8) 0.3900(7) 0.3865(4) 0.067 Uani 1 1 d . . . C21 C 0.2666(5) 0.4228(6) 0.4712(4) 0.038 Uani 1 1 d . . . H21 H 0.2759 0.4751 0.4466 0.057 Uiso 1 1 calc R . . C22 C 0.2699(5) 0.4057(5) 0.5274(3) 0.031 Uani 1 1 d . . . C23 C 0.2966(6) 0.4690(6) 0.5464(4) 0.043 Uani 1 1 d . . . C24 C 0.0320(5) 0.3127(6) 0.5298(4) 0.038 Uani 1 1 d . . . C25 C -0.0514(6) 0.3864(6) 0.5187(4) 0.048 Uani 1 1 d . . . C26 C 0.0388(6) 0.2422(6) 0.5140(4) 0.039 Uani 1 1 d . . . H26 H -0.0077 0.2425 0.4967 0.058 Uiso 1 1 calc R . . C27 C 0.1115(5) 0.1684(5) 0.5223(4) 0.037 Uani 1 1 d . . . C28 C 0.1107(6) 0.0934(6) 0.5044(4) 0.050 Uani 1 1 d . . . C29 C 0.3408(5) 0.1584(5) 0.6357(4) 0.026 Uani 1 1 d . . . C30 C 0.4144(5) 0.1423(5) 0.5515(3) 0.028 Uani 1 1 d . . . C31 C 0.4967(5) 0.1134(5) 0.5744(3) 0.027 Uani 1 1 d . . . C32 C 0.5747(5) 0.0849(5) 0.5426(3) 0.031 Uani 1 1 d . . . H32 H 0.6284 0.0653 0.5582 0.047 Uiso 1 1 calc R . . C33 C 0.5735(5) 0.0852(5) 0.4892(4) 0.034 Uani 1 1 d . . . C34 C 0.6124(5) 0.0700(5) 0.3889(4) 0.035 Uani 1 1 d . . . C35 C 0.4908(5) 0.1151(5) 0.4660(3) 0.028 Uani 1 1 d . . . C36 C 0.4143(5) 0.1428(5) 0.4955(3) 0.034 Uani 1 1 d . . . H36 H 0.3612 0.1624 0.4792 0.050 Uiso 1 1 calc R . . C37 C 0.6574(6) 0.0578(5) 0.3407(4) 0.039 Uani 1 1 d . . . C38 C 0.7814(7) 0.0480(6) 0.2576(4) 0.052 Uani 1 1 d . . . C39 C 0.9172(7) 0.1157(7) 0.2359(5) 0.071 Uani 1 1 d . . . H39A H 0.9251 0.0978 0.2761 0.107 Uiso 1 1 calc R . . H39B H 0.9743 0.1189 0.2142 0.107 Uiso 1 1 calc R . . C40 C 0.8529(7) 0.2056(7) 0.2217(5) 0.071 Uani 1 1 d . . . H40A H 0.7955 0.2036 0.2435 0.107 Uiso 1 1 calc R . . H40B H 0.8743 0.2451 0.2325 0.107 Uiso 1 1 calc R . . C41 C 0.8425(7) 0.2385(7) 0.1604(5) 0.071 Uani 1 1 d . . . H41A H 0.8218 0.1991 0.1496 0.107 Uiso 1 1 calc R . . H41B H 0.8988 0.2427 0.1389 0.107 Uiso 1 1 calc R . . H41C H 0.8002 0.2953 0.1525 0.107 Uiso 1 1 calc R . . C42 C 0.7064(6) 0.0710(6) 0.2352(4) 0.044 Uani 1 1 d . . . C43 C 0.6013(10) 0.1627(9) 0.1482(7) 0.111 Uani 1 1 d . . . H43A H 0.5891 0.1667 0.1107 0.167 Uiso 1 1 calc R . . H43B H 0.5544 0.1441 0.1761 0.167 Uiso 1 1 calc R . . C44 C 0.6020(10) 0.2524(9) 0.1494(7) 0.111 Uani 1 1 d . . . H44A H 0.6051 0.2514 0.1881 0.167 Uiso 1 1 calc R . . H44B H 0.6532 0.2684 0.1253 0.167 Uiso 1 1 calc R . . C45 C 0.5287(10) 0.3086(9) 0.1307(6) 0.111 Uani 1 1 d . . . H45A H 0.4786 0.2915 0.1544 0.167 Uiso 1 1 calc R . . H45B H 0.5270 0.3102 0.0920 0.167 Uiso 1 1 calc R . . H45C H 0.5267 0.3656 0.1318 0.167 Uiso 1 1 calc R . . C46 C 0.1094(5) 0.2155(5) 0.6770(4) 0.034 Uani 1 1 d . . . H46 H 0.0577 0.2384 0.6589 0.051 Uiso 1 1 calc R . . C47 C 0.1021(6) 0.1917(6) 0.7350(4) 0.041 Uani 1 1 d . . . H47 H 0.0464 0.1963 0.7561 0.062 Uiso 1 1 calc R . . C48 C 0.1763(5) 0.1612(5) 0.7620(4) 0.038 Uani 1 1 d . . . H48 H 0.1716 0.1468 0.8017 0.057 Uiso 1 1 calc R . . Co3 Co 1.11953(7) 0.59879(7) 0.16288(5) 0.032 Uani 0.50 1 d P . . Ni3 Ni 1.11953(7) 0.59879(7) 0.16288(5) 0.032 Uani 0.50 1 d P . . Co4 Co 0.69796(7) 0.72558(7) 0.09013(5) 0.031 Uani 0.50 1 d P . . Ni4 Ni 0.69796(7) 0.72558(7) 0.09013(5) 0.031 Uani 0.50 1 d P . . S7 S 1.12997(14) 0.56027(14) -0.06205(9) 0.036 Uani 1 1 d . . . S8 S 0.95082(15) 0.62668(16) -0.09620(10) 0.041 Uani 1 1 d . . . S9 S 1.20689(15) 0.53906(15) -0.18589(10) 0.041 Uani 1 1 d . . . S10 S 1.29181(17) 0.56019(18) -0.30508(11) 0.055 Uani 1 1 d . . . S11 S 1.02951(16) 0.60310(15) -0.21991(10) 0.042 Uani 1 1 d . . . S12 S 1.09342(19) 0.62689(18) -0.34203(11) 0.058 Uani 1 1 d . . . F26 F 1.4205(7) 0.4518(9) 0.2493(6) 0.088 Uani 0.50 1 d PD B 3 F27 F 1.3374(7) 0.5631(11) 0.2651(6) 0.088 Uani 0.50 1 d PD B 3 F28 F 1.4108(8) 0.5712(11) 0.1819(5) 0.088 Uani 0.50 1 d PD B 3 F26A F 1.4480(7) 0.4873(9) 0.2002(6) 0.088 Uani 0.50 1 d PD B 4 F27A F 1.3756(8) 0.6143(8) 0.1927(6) 0.088 Uani 0.50 1 d PD B 4 F28A F 1.3645(8) 0.5360(11) 0.2690(6) 0.088 Uani 0.50 1 d PD B 4 F29 F 1.3288(4) 0.2860(4) 0.1740(3) 0.093 Uani 1 1 d . . . F30 F 1.2580(4) 0.3593(4) 0.1017(3) 0.077 Uani 1 1 d . . . F31 F 1.1932(4) 0.3046(3) 0.1808(3) 0.074 Uani 1 1 d . . . F32 F 0.9717(5) 0.8902(4) 0.1295(4) 0.113 Uani 1 1 d . . . F33 F 1.0705(5) 0.8846(4) 0.1687(4) 0.113 Uani 1 1 d . . . F34 F 1.0712(5) 0.9356(4) 0.0784(4) 0.113 Uani 1 1 d . . . F35 F 1.2506(4) 0.6692(4) -0.0245(2) 0.077 Uani 1 1 d . . . F36 F 1.2942(4) 0.7681(4) -0.0154(3) 0.084 Uani 1 1 d . . . F37 F 1.3536(4) 0.6372(5) 0.0244(3) 0.090 Uani 1 1 d . . . F38 F 0.6386(5) 0.4692(4) 0.1028(3) 0.100 Uani 1 1 d . . . F39 F 0.5321(4) 0.5335(4) 0.0550(4) 0.100 Uani 1 1 d . . . F40 F 0.6643(5) 0.5292(5) 0.0171(4) 0.108 Uani 1 1 d . . . F41 F 0.3976(4) 0.8352(4) 0.1375(4) 0.093 Uani 1 1 d . . . F42 F 0.4168(4) 0.8938(5) 0.0571(3) 0.093 Uani 1 1 d . . . F43 F 0.3602(4) 0.7944(4) 0.0797(3) 0.093 Uani 1 1 d . . . F44 F 0.6159(6) 0.9374(4) -0.1054(3) 0.131 Uani 1 1 d . . . F45 F 0.7149(6) 0.8273(5) -0.1176(3) 0.099 Uani 1 1 d . . . F46 F 0.5916(5) 0.8165(5) -0.0769(3) 0.106 Uani 1 1 d . . . F47 F 0.8057(4) 0.9508(4) 0.0778(2) 0.062 Uani 1 1 d . . . F48 F 0.6791(4) 1.0287(3) 0.0571(2) 0.061 Uani 1 1 d . . . F49 F 0.7835(4) 1.0174(4) -0.0084(2) 0.071 Uani 1 1 d . . . O9 O 1.2244(4) 0.5808(4) 0.2019(3) 0.043 Uani 1 1 d . . . O10 O 1.1616(4) 0.4743(3) 0.1637(2) 0.040 Uani 1 1 d . . . O11 O 1.0762(3) 0.7276(3) 0.1553(2) 0.036 Uani 1 1 d . . . O12 O 1.1980(3) 0.6251(4) 0.0892(2) 0.039 Uani 1 1 d . . . O13 O 0.6732(5) 0.6187(5) 0.0876(4) 0.093 Uani 1 1 d . . . O14 O 0.5680(5) 0.7849(5) 0.0969(4) 0.093 Uani 1 1 d . . . O15 O 0.6901(3) 0.7640(3) 0.0049(2) 0.037 Uani 1 1 d . . . O16 O 0.7311(3) 0.8362(3) 0.0796(2) 0.034 Uani 1 1 d . . . N5 N 1.0038(4) 0.6113(4) 0.1295(3) 0.029 Uani 1 1 d . . . N6 N 1.0329(4) 0.5867(4) 0.2344(3) 0.033 Uani 1 1 d . . . N7 N 0.6961(4) 0.6914(4) 0.1766(3) 0.032 Uani 1 1 d . . . N8 N 0.8339(4) 0.6632(4) 0.0995(3) 0.029 Uani 1 1 d . . . C49 C 1.2913(6) 0.5176(6) 0.2032(4) 0.043 Uani 1 1 d . B . C51 C 1.3006(7) 0.4451(6) 0.1900(5) 0.060 Uani 1 1 d . . . H51 H 1.3552 0.4026 0.1938 0.090 Uiso 1 1 calc R . . C52 C 1.2358(6) 0.4284(6) 0.1712(4) 0.047 Uani 1 1 d . . . C53 C 1.2562(7) 0.3424(7) 0.1569(5) 0.063 Uani 1 1 d . . . C54 C 1.1050(6) 0.7846(5) 0.1173(4) 0.044 Uani 1 1 d . . . C55 C 1.0592(7) 0.8703(7) 0.1205(5) 0.059 Uani 1 1 d . . . C56 C 1.1712(6) 0.7737(6) 0.0748(4) 0.048 Uani 1 1 d . . . H56 H 1.1904 0.8222 0.0526 0.072 Uiso 1 1 calc R . . C57 C 1.2113(5) 0.6972(6) 0.0623(4) 0.036 Uani 1 1 d . . . C58 C 1.2788(7) 0.6931(7) 0.0120(4) 0.059 Uani 1 1 d . . . C59 C 0.9344(5) 0.6252(5) 0.1668(3) 0.027 Uani 1 1 d . . . C60 C 0.9486(5) 0.6086(5) 0.2251(3) 0.027 Uani 1 1 d . . . C61 C 1.0496(6) 0.5693(5) 0.2869(4) 0.037 Uani 1 1 d . . . H61 H 1.1083 0.5548 0.2941 0.056 Uiso 1 1 calc R . . C62 C 0.9840(6) 0.5718(6) 0.3313(4) 0.043 Uani 1 1 d . . . H62 H 0.9982 0.5585 0.3683 0.064 Uiso 1 1 calc R . . C63 C 0.8990(6) 0.5934(6) 0.3217(4) 0.042 Uani 1 1 d . . . H63 H 0.8542 0.5939 0.3521 0.063 Uiso 1 1 calc R . . C64 C 0.8778(5) 0.6150(5) 0.2669(4) 0.033 Uani 1 1 d . . . C65 C 0.7886(5) 0.6429(5) 0.2522(3) 0.031 Uani 1 1 d . . . C66 C 0.7758(5) 0.6635(5) 0.1950(3) 0.029 Uani 1 1 d . . . C67 C 0.6022(7) 0.6182(8) 0.0751(7) 0.093 Uani 1 1 d . . . C68 C 0.6080(7) 0.5393(6) 0.0604(5) 0.060 Uani 1 1 d . . . C69 C 0.5234(7) 0.6843(8) 0.0754(6) 0.093 Uani 1 1 d . . . H69 H 0.4735 0.6756 0.0670 0.139 Uiso 1 1 calc R . . C70 C 0.5126(7) 0.7573(9) 0.0864(7) 0.093 Uani 1 1 d . . . C71 C 0.4240(7) 0.8140(9) 0.0871(7) 0.093 Uani 1 1 d . . . C72 C 0.6840(6) 0.8386(6) -0.0253(4) 0.043 Uani 1 1 d . . . C73 C 0.6490(8) 0.8557(7) -0.0807(5) 0.069 Uani 1 1 d . . . C74 C 0.7011(6) 0.9051(6) -0.0151(4) 0.045 Uani 1 1 d . . . H74 H 0.6949 0.9581 -0.0436 0.067 Uiso 1 1 calc R . . C75 C 0.7268(5) 0.8973(5) 0.0347(4) 0.034 Uani 1 1 d . . . C76 C 0.7512(7) 0.9732(6) 0.0406(4) 0.047 Uani 1 1 d . . . C77 C 0.8501(5) 0.6502(5) 0.1524(3) 0.025 Uani 1 1 d . . . C78 C 0.9027(5) 0.6435(5) 0.0629(3) 0.027 Uani 1 1 d . . . C79 C 0.9903(5) 0.6155(5) 0.0781(3) 0.026 Uani 1 1 d . . . C80 C 1.0605(5) 0.5928(5) 0.0387(4) 0.032 Uani 1 1 d . . . H80 H 1.1185 0.5760 0.0478 0.048 Uiso 1 1 calc R . . C81 C 1.0460(5) 0.5947(5) -0.0130(3) 0.031 Uani 1 1 d . . . C82 C 1.0627(5) 0.5879(5) -0.1154(3) 0.033 Uani 1 1 d . . . C83 C 0.9604(5) 0.6259(5) -0.0288(3) 0.029 Uani 1 1 d . . . C84 C 0.8897(5) 0.6495(5) 0.0077(3) 0.031 Uani 1 1 d . . . H84 H 0.8326 0.6697 -0.0034 0.047 Uiso 1 1 calc R . . C85 C 1.0943(5) 0.5792(5) -0.1661(3) 0.033 Uani 1 1 d . . . C86 C 1.1977(5) 0.5761(5) -0.2590(4) 0.036 Uani 1 1 d . . . C87 C 1.3747(9) 0.5579(8) -0.2682(7) 0.103 Uani 1 1 d . . . H87A H 1.3744 0.5133 -0.2317 0.155 Uiso 1 1 calc R . . H87B H 1.4320 0.5409 -0.2898 0.155 Uiso 1 1 calc R . . C88 C 1.3652(9) 0.6407(8) -0.2578(6) 0.103 Uani 1 1 d . . . H88A H 1.4063 0.6316 -0.2312 0.155 Uiso 1 1 calc R . . H88B H 1.3053 0.6623 -0.2407 0.155 Uiso 1 1 calc R . . C89 C 1.3833(9) 0.7055(8) -0.3113(6) 0.103 Uani 1 1 d . . . H89A H 1.3418 0.7154 -0.3373 0.155 Uiso 1 1 calc R . . H89B H 1.4428 0.6843 -0.3281 0.155 Uiso 1 1 calc R . . H89C H 1.3771 0.7594 -0.3036 0.155 Uiso 1 1 calc R . . C90 C 1.1175(6) 0.6054(6) -0.2741(4) 0.040 Uani 1 1 d . . . C91 C 1.0064(10) 0.7247(8) -0.3504(6) 0.104 Uani 1 1 d . . . H91A H 0.9887 0.7420 -0.3885 0.156 Uiso 1 1 calc R . . H91B H 0.9558 0.7128 -0.3234 0.156 Uiso 1 1 calc R . . C92 C 1.0253(10) 0.7984(9) -0.3424(6) 0.104 Uani 1 1 d . . . H92A H 0.9746 0.8495 -0.3512 0.156 Uiso 1 1 calc R . . H92B H 1.0333 0.7856 -0.3026 0.156 Uiso 1 1 calc R . . C93 C 1.1005(10) 0.8174(9) -0.3764(6) 0.104 Uani 1 1 d . . . H93A H 1.0921 0.8325 -0.4160 0.156 Uiso 1 1 calc R . . H93B H 1.1511 0.7671 -0.3678 0.156 Uiso 1 1 calc R . . H93C H 1.1105 0.8657 -0.3689 0.156 Uiso 1 1 calc R . . C94 C 0.6264(6) 0.7002(6) 0.2151(4) 0.045 Uani 1 1 d . . . H94 H 0.5700 0.7206 0.2029 0.067 Uiso 1 1 calc R . . C95 C 0.6329(6) 0.6807(5) 0.2723(4) 0.043 Uani 1 1 d . . . H95 H 0.5823 0.6859 0.2986 0.064 Uiso 1 1 calc R . . C96 C 0.7149(5) 0.6539(5) 0.2891(4) 0.038 Uani 1 1 d . . . H96 H 0.7205 0.6426 0.3275 0.057 Uiso 1 1 calc R . . C50 C 1.3688(7) 0.5286(7) 0.2206(5) 0.076 Uani 1 1 d D . . N9 N 0.1042(8) 0.7257(10) 0.3242(8) 0.148 Uani 1 1 d . . . C99 C 0.1564(11) 0.7445(10) 0.2878(8) 0.109 Uani 1 1 d . . . C100 C 0.2269(9) 0.7647(10) 0.2430(7) 0.126 Uani 1 1 d . . . H10A H 0.2662 0.7833 0.2575 0.189 Uiso 1 1 calc R . . H10B H 0.2014 0.8105 0.2111 0.189 Uiso 1 1 calc R . . H10C H 0.2597 0.7134 0.2311 0.189 Uiso 1 1 calc R . . C101 C 1.0198(12) 1.1518(9) 0.0264(8) 0.130 Uani 1 1 d . . . C102 C 0.9343(10) 1.1182(12) 0.0502(8) 0.155 Uani 1 1 d . . . H112 H 0.8968 1.1498 0.0761 0.233 Uiso 1 1 calc R . . H122 H 0.9519 1.0569 0.0699 0.233 Uiso 1 1 calc R . . H132 H 0.9024 1.1275 0.0190 0.233 Uiso 1 1 calc R . . C105 C 1.0658(14) 1.1383(13) 0.0788(8) 0.179 Uani 1 1 d . . . H115 H 1.0838 1.0770 0.0987 0.269 Uiso 1 1 calc R . . H125 H 1.0251 1.1695 0.1039 0.269 Uiso 1 1 calc R . . H135 H 1.1172 1.1599 0.0662 0.269 Uiso 1 1 calc R . . C103 C 1.4497(19) 0.6725(14) -0.4709(13) 0.237 Uani 1 1 d . . . C104 C 1.3533(12) 0.7160(12) -0.4722(8) 0.165 Uani 1 1 d . . . H114 H 1.3396 0.7383 -0.5111 0.248 Uiso 1 1 calc R . . H124 H 1.3369 0.7635 -0.4555 0.248 Uiso 1 1 calc R . . H134 H 1.3207 0.6746 -0.4510 0.248 Uiso 1 1 calc R . . O17 O 1.0424(9) 1.1822(8) -0.0183(5) 0.154 Uani 1 1 d . . . C106 C 1.4778(11) 0.5893(12) -0.4385(8) 0.174 Uani 1 1 d . . . H116 H 1.5403 0.5662 -0.4486 0.261 Uiso 1 1 calc R . . H126 H 1.4458 0.5545 -0.4448 0.261 Uiso 1 1 calc R . . H136 H 1.4673 0.5877 -0.3988 0.261 Uiso 1 1 calc R . . O18 O 1.5043(11) 0.7012(8) -0.5081(8) 0.237 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 Co1 0.029 0.040 0.029 -0.010 -0.005 -0.011 Ni1 0.029 0.040 0.029 -0.010 -0.005 -0.011 Co2 0.028 0.034 0.024 -0.003 -0.005 -0.011 Ni2 0.028 0.034 0.024 -0.003 -0.005 -0.011 S1 0.032 0.062 0.030 -0.017 0.006 -0.010 S2 0.041 0.059 0.023 -0.014 0.001 -0.019 S3 0.054 0.047 0.033 -0.010 0.012 -0.016 S4 0.076 0.045 0.056 -0.022 0.037 -0.022 S5 0.066 0.052 0.031 -0.014 0.005 -0.032 S6 0.118 0.073 0.030 -0.022 0.014 -0.060 F8 0.084 0.068 0.125 -0.051 -0.043 0.025 F9 0.094 0.059 0.082 -0.008 -0.011 -0.040 F10 0.094 0.065 0.060 -0.032 0.000 -0.018 F11 0.082 0.106 0.124 0.010 -0.051 -0.056 F12 0.109 0.132 0.078 -0.047 -0.053 -0.024 F13 0.072 0.083 0.109 0.001 -0.057 -0.016 F5 0.098 0.069 0.123 -0.037 -0.006 -0.042 F6 0.098 0.069 0.123 -0.037 -0.006 -0.042 F7 0.098 0.069 0.123 -0.037 -0.006 -0.042 F14 0.210 0.066 0.042 0.015 -0.038 -0.056 F15 0.192 0.119 0.064 0.021 -0.076 -0.083 F16 0.180 0.114 0.033 -0.031 0.024 -0.025 F17 0.121 0.072 0.040 -0.003 -0.008 -0.063 F18 0.063 0.069 0.075 -0.007 -0.020 -0.036 F19 0.077 0.063 0.066 -0.040 0.006 -0.025 F20 0.091 0.079 0.084 0.020 -0.031 0.005 F21 0.061 0.093 0.150 -0.073 -0.051 0.032 F22 0.037 0.069 0.184 -0.022 -0.032 -0.004 F23 0.075 0.081 0.061 -0.038 0.002 -0.030 F24 0.070 0.068 0.099 -0.029 -0.043 -0.018 F25 0.096 0.049 0.068 0.003 -0.019 -0.038 O3 0.047 0.048 0.054 -0.018 -0.019 -0.013 O4 0.036 0.053 0.048 -0.010 -0.010 -0.015 O2 0.051 0.061 0.061 -0.027 0.004 -0.031 O1 0.051 0.061 0.061 -0.027 0.004 -0.031 O5 0.042 0.036 0.028 -0.003 -0.005 -0.012 O6 0.040 0.038 0.019 -0.002 0.002 -0.017 O7 0.030 0.040 0.035 -0.005 -0.006 -0.012 O8 0.030 0.039 0.041 -0.006 -0.014 -0.013 N1 0.025 0.027 0.019 -0.007 -0.001 -0.007 N2 0.034 0.033 0.031 -0.007 -0.005 -0.013 N3 0.020 0.036 0.029 -0.003 -0.003 -0.010 N4 0.024 0.036 0.017 -0.005 0.000 -0.008 C6 0.033 0.038 0.065 -0.014 -0.008 -0.012 C7 0.057 0.044 0.091 -0.033 -0.024 0.000 C8 0.051 0.045 0.051 -0.013 -0.013 -0.019 C9 0.026 0.062 0.034 -0.011 -0.010 -0.017 C10 0.056 0.065 0.082 -0.002 -0.035 -0.021 C4 0.051 0.061 0.061 -0.027 0.004 -0.031 C5 0.062 0.076 0.099 -0.019 -0.039 -0.026 C3 0.051 0.061 0.061 -0.027 0.004 -0.031 C1 0.051 0.061 0.061 -0.027 0.004 -0.031 C2 0.051 0.061 0.061 -0.027 0.004 -0.031 C11 0.022 0.025 0.030 -0.006 -0.008 -0.005 C12 0.032 0.034 0.021 -0.008 0.000 -0.013 C13 0.049 0.053 0.033 -0.005 -0.015 -0.015 C14 0.049 0.040 0.021 -0.005 -0.005 -0.012 C15 0.042 0.038 0.030 -0.009 0.006 -0.016 C16 0.039 0.026 0.013 0.003 0.000 -0.015 C17 0.024 0.025 0.025 -0.006 0.007 -0.009 C18 0.026 0.028 0.035 -0.013 0.002 -0.012 C19 0.040 0.045 0.028 -0.010 -0.007 -0.003 C20 0.127 0.051 0.032 0.006 -0.018 -0.050 C21 0.045 0.041 0.025 -0.003 0.007 -0.022 C22 0.031 0.035 0.024 -0.005 -0.002 -0.010 C23 0.042 0.049 0.033 0.004 -0.007 -0.020 C24 0.030 0.041 0.033 0.002 -0.002 -0.012 C25 0.043 0.052 0.049 -0.015 -0.008 -0.010 C26 0.045 0.046 0.033 -0.008 -0.006 -0.026 C27 0.036 0.036 0.040 -0.007 -0.001 -0.016 C28 0.049 0.059 0.052 -0.017 -0.014 -0.020 C29 0.018 0.018 0.040 -0.004 -0.005 -0.004 C30 0.029 0.033 0.018 -0.003 0.001 -0.010 C31 0.033 0.033 0.018 -0.001 0.000 -0.020 C32 0.031 0.040 0.021 -0.003 -0.002 -0.015 C33 0.028 0.034 0.034 -0.005 0.003 -0.010 C34 0.043 0.043 0.025 -0.015 0.003 -0.017 C35 0.038 0.030 0.019 -0.005 -0.008 -0.013 C36 0.036 0.040 0.026 -0.006 -0.005 -0.017 C37 0.051 0.037 0.028 0.000 -0.005 -0.020 C38 0.070 0.052 0.040 -0.022 0.018 -0.030 C39 0.074 0.056 0.083 -0.013 0.002 -0.030 C40 0.074 0.056 0.083 -0.013 0.002 -0.030 C41 0.074 0.056 0.083 -0.013 0.002 -0.030 C42 0.068 0.038 0.031 -0.009 0.016 -0.033 C43 0.132 0.084 0.115 -0.014 -0.011 -0.043 C44 0.132 0.084 0.115 -0.014 -0.011 -0.043 C45 0.132 0.084 0.115 -0.014 -0.011 -0.043 C46 0.029 0.028 0.035 -0.004 0.001 -0.002 C47 0.035 0.045 0.035 0.002 0.005 -0.016 C48 0.043 0.034 0.031 -0.002 0.002 -0.013 Co3 0.030 0.036 0.029 -0.008 -0.006 -0.010 Ni3 0.030 0.036 0.029 -0.008 -0.006 -0.010 Co4 0.029 0.030 0.034 -0.005 -0.007 -0.010 Ni4 0.029 0.030 0.034 -0.005 -0.007 -0.010 S7 0.036 0.042 0.029 -0.009 -0.002 -0.009 S8 0.041 0.056 0.030 -0.012 -0.007 -0.015 S9 0.047 0.040 0.035 -0.011 -0.004 -0.010 S10 0.061 0.061 0.043 -0.024 0.008 -0.017 S11 0.053 0.048 0.029 -0.010 -0.006 -0.019 S12 0.077 0.067 0.033 -0.023 -0.007 -0.017 F26 0.040 0.133 0.105 -0.049 -0.018 -0.021 F27 0.040 0.133 0.105 -0.049 -0.018 -0.021 F28 0.040 0.133 0.105 -0.049 -0.018 -0.021 F26A 0.040 0.133 0.105 -0.049 -0.018 -0.021 F27A 0.040 0.133 0.105 -0.049 -0.018 -0.021 F28A 0.040 0.133 0.105 -0.049 -0.018 -0.021 F29 0.083 0.065 0.134 -0.049 -0.057 0.021 F30 0.092 0.067 0.076 -0.039 -0.008 -0.009 F31 0.096 0.044 0.088 -0.007 -0.043 -0.020 F32 0.115 0.059 0.148 -0.043 0.023 -0.012 F33 0.115 0.059 0.148 -0.043 0.023 -0.012 F34 0.115 0.059 0.148 -0.043 0.023 -0.012 F35 0.091 0.118 0.045 -0.044 0.022 -0.055 F36 0.099 0.082 0.072 -0.031 0.052 -0.057 F37 0.041 0.131 0.080 -0.029 0.007 -0.008 F38 0.121 0.034 0.152 -0.004 -0.059 -0.029 F39 0.069 0.071 0.194 -0.059 -0.062 -0.014 F40 0.125 0.089 0.134 -0.069 -0.021 -0.021 F41 0.045 0.088 0.149 -0.055 -0.020 0.002 F42 0.045 0.088 0.149 -0.055 -0.020 0.002 F43 0.045 0.088 0.149 -0.055 -0.020 0.002 F44 0.240 0.051 0.101 0.002 -0.122 -0.001 F45 0.161 0.104 0.047 -0.036 -0.009 -0.045 F46 0.139 0.125 0.081 0.001 -0.069 -0.069 F47 0.070 0.064 0.067 -0.012 -0.023 -0.035 F48 0.088 0.051 0.049 -0.024 0.003 -0.024 F49 0.112 0.072 0.040 -0.012 0.020 -0.063 O9 0.038 0.049 0.041 -0.011 -0.007 -0.012 O10 0.038 0.036 0.044 -0.011 -0.014 -0.003 O11 0.038 0.035 0.036 -0.012 0.005 -0.014 O12 0.036 0.046 0.037 -0.013 0.002 -0.016 O13 0.045 0.088 0.149 -0.055 -0.020 0.002 O14 0.045 0.088 0.149 -0.055 -0.020 0.002 O15 0.044 0.035 0.033 -0.009 -0.010 -0.007 O16 0.040 0.035 0.029 -0.007 -0.005 -0.015 N5 0.033 0.031 0.025 -0.004 -0.005 -0.013 N6 0.041 0.033 0.026 -0.003 -0.008 -0.017 N7 0.026 0.033 0.038 -0.004 -0.006 -0.012 N8 0.036 0.021 0.034 -0.009 -0.003 -0.014 C49 0.045 0.049 0.048 -0.026 -0.011 -0.012 C51 0.055 0.047 0.083 -0.034 -0.035 0.010 C52 0.048 0.042 0.054 -0.018 -0.020 -0.005 C53 0.049 0.064 0.072 -0.031 -0.032 0.015 C54 0.051 0.030 0.056 -0.013 0.001 -0.019 C55 0.070 0.061 0.045 -0.018 0.027 -0.033 C56 0.047 0.047 0.056 -0.022 0.019 -0.028 C57 0.035 0.046 0.031 -0.016 0.000 -0.015 C58 0.070 0.061 0.045 -0.018 0.027 -0.033 C59 0.034 0.028 0.028 -0.011 0.001 -0.018 C60 0.036 0.020 0.021 0.000 -0.006 -0.008 C61 0.050 0.040 0.025 -0.011 -0.012 -0.011 C62 0.043 0.056 0.031 -0.003 -0.005 -0.024 C63 0.060 0.046 0.016 0.001 -0.002 -0.023 C64 0.040 0.031 0.029 -0.008 0.004 -0.015 C65 0.037 0.025 0.029 -0.001 -0.002 -0.015 C66 0.029 0.016 0.034 -0.002 0.004 -0.008 C67 0.045 0.088 0.149 -0.055 -0.020 0.002 C68 0.075 0.043 0.077 -0.020 -0.027 -0.021 C69 0.045 0.088 0.149 -0.055 -0.020 0.002 C70 0.045 0.088 0.149 -0.055 -0.020 0.002 C71 0.045 0.088 0.149 -0.055 -0.020 0.002 C72 0.058 0.039 0.030 -0.007 -0.020 -0.006 C73 0.117 0.044 0.051 -0.004 -0.040 -0.017 C74 0.075 0.037 0.026 -0.008 -0.014 -0.017 C75 0.042 0.026 0.026 -0.005 0.003 -0.006 C76 0.074 0.040 0.037 -0.007 -0.004 -0.031 C77 0.031 0.026 0.019 -0.005 -0.001 -0.015 C78 0.030 0.030 0.021 -0.002 -0.001 -0.013 C79 0.027 0.028 0.024 -0.005 0.002 -0.014 C80 0.028 0.027 0.038 -0.004 -0.005 -0.008 C81 0.038 0.028 0.030 -0.007 -0.003 -0.015 C82 0.044 0.040 0.022 -0.013 -0.007 -0.015 C83 0.032 0.040 0.016 0.000 -0.002 -0.018 C84 0.038 0.030 0.030 -0.005 -0.010 -0.014 C85 0.042 0.032 0.024 -0.002 -0.008 -0.012 C86 0.036 0.041 0.029 -0.009 -0.002 -0.009 C87 0.109 0.072 0.128 -0.030 0.008 -0.035 C88 0.109 0.072 0.128 -0.030 0.008 -0.035 C89 0.109 0.072 0.128 -0.030 0.008 -0.035 C90 0.064 0.042 0.017 -0.011 0.005 -0.023 C91 0.141 0.090 0.081 -0.011 -0.038 -0.029 C92 0.141 0.090 0.081 -0.011 -0.038 -0.029 C93 0.141 0.090 0.081 -0.011 -0.038 -0.029 C94 0.031 0.041 0.057 -0.001 -0.001 -0.017 C95 0.046 0.030 0.042 -0.001 0.010 -0.014 C96 0.041 0.042 0.027 -0.005 0.000 -0.012 C50 0.048 0.090 0.108 -0.058 -0.007 -0.012 N9 0.069 0.147 0.220 -0.055 -0.040 -0.004 C99 0.104 0.099 0.136 -0.038 -0.060 -0.012 C100 0.096 0.123 0.163 -0.052 -0.055 0.001 C101 0.182 0.053 0.103 -0.015 0.029 0.000 C102 0.090 0.200 0.139 -0.019 -0.010 -0.023 C105 0.213 0.190 0.120 -0.041 -0.054 -0.018 C103 0.245 0.089 0.291 0.023 0.039 -0.052 C104 0.178 0.146 0.176 -0.053 -0.069 -0.014 O17 0.240 0.131 0.100 -0.003 -0.013 -0.099 C106 0.130 0.145 0.164 0.057 -0.018 -0.032 O18 0.245 0.089 0.291 0.023 0.039 -0.052 _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 Co1 O3 2.038(6) . ? Co1 O2 2.046(7) . ? Co1 O1 2.047(7) . ? Co1 O4 2.055(6) . ? Co1 N2 2.070(7) . ? Co1 N1 2.150(6) . ? Co2 O8 2.009(6) . ? Co2 O7 2.047(5) . ? Co2 O5 2.047(6) . ? Co2 N3 2.067(7) . ? Co2 O6 2.071(6) . ? Co2 N4 2.158(6) . ? S1 C33 1.723(9) . ? S1 C34 1.746(8) . ? S2 C34 1.747(9) . ? S2 C35 1.759(8) . ? S3 C38 1.773(10) . ? S3 C37 1.773(9) . ? S4 C38 1.735(10) . ? S4 C39 1.809(11) . ? S5 C42 1.758(10) . ? S5 C37 1.765(9) . ? S6 C42 1.757(10) . ? S6 C43 1.801(14) . ? F8 C7 1.298(10) . ? F9 C7 1.351(12) . ? F10 C7 1.340(12) . ? F11 C10 1.327(12) . ? F12 C10 1.323(14) . ? F13 C10 1.340(11) . ? F5 C5 1.314(11) . ? F6 C5 1.370(14) . ? F7 C5 1.338(12) . ? F1 C2 1.333(13) . ? F2 C2 1.333(13) . ? F3 C2 1.281(13) . ? F1A C2 1.197(13) . ? F2A C2 1.552(13) . ? F3A C2 1.349(13) . ? F14 C20 1.317(11) . ? F15 C20 1.287(12) . ? F16 C20 1.349(14) . ? F17 C23 1.323(9) . ? F18 C23 1.340(9) . ? F19 C23 1.320(11) . ? F20 C25 1.340(11) . ? F21 C25 1.302(11) . ? F22 C25 1.291(10) . ? F23 C28 1.324(11) . ? F24 C28 1.338(9) . ? F25 C28 1.321(10) . ? O3 C6 1.262(9) . ? O4 C9 1.271(10) . ? O2 C4 1.244(10) . ? O1 C1 1.256(10) . ? O5 C19 1.259(10) . ? O6 C22 1.258(9) . ? O7 C24 1.254(9) . ? O8 C27 1.258(9) . ? N1 C11 1.339(10) . ? N1 C31 1.356(10) . ? N2 C13 1.335(10) . ? N2 C12 1.349(9) . ? N3 C46 1.342(10) . ? N3 C18 1.361(9) . ? N4 C29 1.333(10) . ? N4 C30 1.347(10) . ? C6 C8 1.408(12) . ? C6 C7 1.504(13) . ? C8 C9 1.375(13) . ? C8 H8 0.9500 . ? C9 C10 1.515(12) . ? C4 C3 1.352(13) . ? C4 C5 1.521(15) . ? C3 C1 1.392(13) . ? C3 H3 0.9500 . ? C1 C2 1.664(14) . ? C11 C29 1.421(10) . ? C11 C12 1.442(11) . ? C12 C16 1.396(11) . ? C13 C14 1.376(12) . ? C13 H13 0.9500 . ? C14 C15 1.379(11) . ? C14 H14 0.9500 . ? C15 C16 1.418(11) . ? C15 H15 0.9500 . ? C16 C17 1.456(10) . ? C17 C18 1.398(11) . ? C17 C48 1.414(11) . ? C18 C29 1.455(11) . ? C19 C21 1.383(12) . ? C19 C20 1.515(13) . ? C21 C22 1.369(11) . ? C21 H21 0.9500 . ? C22 C23 1.533(12) . ? C24 C26 1.365(12) . ? C24 C25 1.528(12) . ? C26 C27 1.418(12) . ? C26 H26 0.9500 . ? C27 C28 1.508(13) . ? C30 C36 1.421(11) . ? C30 C31 1.444(10) . ? C31 C32 1.396(11) . ? C32 C33 1.359(11) . ? C32 H32 0.9500 . ? C33 C35 1.454(10) . ? C34 C37 1.336(12) . ? C35 C36 1.347(11) . ? C36 H36 0.9500 . ? C38 C42 1.341(13) . ? C39 C40 1.534(14) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.498(15) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C43 C44 1.558(18) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.329(17) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.387(12) . ? C46 H46 0.9500 . ? C47 C48 1.379(11) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? Co3 O10 2.020(6) . ? Co3 O9 2.040(5) . ? Co3 O12 2.048(6) . ? Co3 O11 2.051(6) . ? Co3 N6 2.060(7) . ? Co3 N5 2.147(6) . ? Co4 O14 2.032(7) . ? Co4 O13 2.033(8) . ? Co4 O15 2.065(6) . ? Co4 O16 2.067(5) . ? Co4 N7 2.077(7) . ? Co4 N8 2.151(6) . ? S7 C81 1.745(9) . ? S7 C82 1.765(8) . ? S8 C83 1.748(8) . ? S8 C82 1.754(9) . ? S9 C85 1.769(9) . ? S9 C86 1.778(9) . ? S10 C86 1.734(9) . ? S10 C87 1.782(14) . ? S11 C85 1.762(8) . ? S11 C90 1.777(9) . ? S12 C90 1.742(9) . ? S12 C91 1.797(14) . ? F26 C50 1.372(13) . ? F27 C50 1.379(14) . ? F28 C50 1.247(13) . ? F26A C50 1.349(13) . ? F27A C50 1.441(14) . ? F28A C50 1.263(14) . ? F29 C53 1.311(10) . ? F30 C53 1.333(12) . ? F31 C53 1.332(12) . ? F32 C55 1.344(11) . ? F33 C55 1.385(13) . ? F34 C55 1.310(11) . ? F35 C58 1.341(12) . ? F36 C58 1.329(11) . ? F37 C58 1.306(11) . ? F38 C68 1.356(11) . ? F39 C68 1.314(11) . ? F40 C68 1.302(13) . ? F41 C71 1.393(15) . ? F42 C71 1.312(14) . ? F43 C71 1.260(13) . ? F44 C73 1.313(11) . ? F45 C73 1.351(14) . ? F46 C73 1.296(12) . ? F47 C76 1.309(10) . ? F48 C76 1.343(11) . ? F49 C76 1.332(10) . ? O9 C49 1.261(10) . ? O10 C52 1.224(9) . ? O11 C54 1.269(10) . ? O12 C57 1.270(9) . ? O13 C67 1.266(12) . ? O14 C70 1.257(13) . ? O15 C72 1.244(9) . ? O16 C75 1.269(9) . ? N5 C59 1.332(10) . ? N5 C79 1.346(10) . ? N6 C61 1.332(10) . ? N6 C60 1.352(9) . ? N7 C94 1.344(11) . ? N7 C66 1.355(9) . ? N8 C78 1.333(10) . ? N8 C77 1.356(9) . ? C49 C51 1.352(13) . ? C49 C50 1.509(13) . ? C51 C52 1.389(12) . ? C51 H51 0.9500 . ? C52 C53 1.554(14) . ? C54 C56 1.376(13) . ? C54 C55 1.441(13) . ? C56 C57 1.375(12) . ? C56 H56 0.9500 . ? C57 C58 1.511(13) . ? C59 C77 1.391(10) . ? C59 C60 1.466(11) . ? C60 C64 1.404(11) . ? C61 C62 1.390(12) . ? C61 H61 0.9500 . ? C62 C63 1.367(11) . ? C62 H62 0.9500 . ? C63 C64 1.404(11) . ? C63 H63 0.9500 . ? C64 C65 1.463(11) . ? C65 C96 1.367(11) . ? C65 C66 1.424(11) . ? C66 C77 1.462(11) . ? C67 C69 1.413(15) . ? C67 C68 1.493(16) . ? C69 C70 1.325(17) . ? C69 H69 0.9500 . ? C70 C71 1.458(15) . ? C72 C74 1.374(12) . ? C72 C73 1.533(13) . ? C74 C75 1.366(11) . ? C74 H74 0.9500 . ? C75 C76 1.546(12) . ? C78 C84 1.427(11) . ? C78 C79 1.442(10) . ? C79 C80 1.403(11) . ? C80 C81 1.370(11) . ? C80 H80 0.9500 . ? C81 C83 1.416(10) . ? C82 C85 1.325(11) . ? C83 C84 1.365(11) . ? C84 H84 0.9500 . ? C86 C90 1.327(11) . ? C87 C88 1.487(17) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 C89 1.495(17) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C91 C92 1.482(18) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 C93 1.415(18) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 C95 1.399(13) . ? C94 H94 0.9500 . ? C95 C96 1.375(11) . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? N9 C99 1.16(2) . ? C99 C100 1.48(2) . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? C101 O17 1.125(17) . ? C101 C105 1.58(2) . ? C101 C102 1.61(2) . ? C102 H112 0.9800 . ? C102 H122 0.9800 . ? C102 H132 0.9800 . ? C105 H115 0.9800 . ? C105 H125 0.9800 . ? C105 H135 0.9800 . ? C103 O18 1.25(2) . ? C103 C106 1.37(2) . ? C103 C104 1.51(3) . ? C104 H114 0.9800 . ? C104 H124 0.9800 . ? C104 H134 0.9800 . ? C106 H116 0.9800 . ? C106 H126 0.9800 . ? C106 H136 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 O2 173.7(3) . . ? O3 Co1 O1 86.5(3) . . ? O2 Co1 O1 88.3(3) . . ? O3 Co1 O4 89.8(2) . . ? O2 Co1 O4 93.5(3) . . ? O1 Co1 O4 86.2(3) . . ? O3 Co1 N2 98.6(3) . . ? O2 Co1 N2 86.7(3) . . ? O1 Co1 N2 174.8(3) . . ? O4 Co1 N2 92.7(3) . . ? O3 Co1 N1 86.8(2) . . ? O2 Co1 N1 90.8(2) . . ? O1 Co1 N1 102.7(2) . . ? O4 Co1 N1 170.2(2) . . ? N2 Co1 N1 78.8(2) . . ? O3 Co1 Co2 99.40(15) . . ? O2 Co1 Co2 79.13(17) . . ? O1 Co1 Co2 111.28(18) . . ? O4 Co1 Co2 160.52(19) . . ? N2 Co1 Co2 69.10(17) . . ? N1 Co1 Co2 14.95(17) . . ? O8 Co2 O7 90.5(2) . . ? O8 Co2 O5 86.3(2) . . ? O7 Co2 O5 87.7(2) . . ? O8 Co2 N3 96.0(2) . . ? O7 Co2 N3 92.4(2) . . ? O5 Co2 N3 177.7(3) . . ? O8 Co2 O6 174.5(2) . . ? O7 Co2 O6 91.5(2) . . ? O5 Co2 O6 88.7(2) . . ? N3 Co2 O6 89.0(2) . . ? O8 Co2 N4 93.7(2) . . ? O7 Co2 N4 170.5(2) . . ? O5 Co2 N4 101.1(2) . . ? N3 Co2 N4 78.7(2) . . ? O6 Co2 N4 85.0(2) . . ? O8 Co2 Co1 110.23(14) . . ? O7 Co2 Co1 154.02(17) . . ? O5 Co2 Co1 108.48(15) . . ? N3 Co2 Co1 70.66(16) . . ? O6 Co2 Co1 69.31(14) . . ? N4 Co2 Co1 18.04(18) . . ? C33 S1 C34 96.0(4) . . ? C34 S2 C35 96.0(4) . . ? C38 S3 C37 95.2(4) . . ? C38 S4 C39 99.8(5) . . ? C42 S5 C37 94.9(5) . . ? C42 S6 C43 103.6(6) . . ? C6 O3 Co1 124.4(5) . . ? C9 O4 Co1 123.6(6) . . ? C4 O2 Co1 123.5(7) . . ? C1 O1 Co1 123.9(7) . . ? C19 O5 Co2 124.8(6) . . ? C22 O6 Co2 123.8(5) . . ? C24 O7 Co2 123.2(6) . . ? C27 O8 Co2 124.0(5) . . ? C11 N1 C31 118.3(6) . . ? C11 N1 Co1 110.4(5) . . ? C31 N1 Co1 131.3(5) . . ? C13 N2 C12 117.7(7) . . ? C13 N2 Co1 127.3(6) . . ? C12 N2 Co1 115.0(5) . . ? C46 N3 C18 117.7(7) . . ? C46 N3 Co2 128.1(5) . . ? C18 N3 Co2 113.9(5) . . ? C29 N4 C30 117.1(6) . . ? C29 N4 Co2 108.3(5) . . ? C30 N4 Co2 133.2(5) . . ? O3 C6 C8 127.6(9) . . ? O3 C6 C7 113.3(8) . . ? C8 C6 C7 119.1(8) . . ? F8 C7 F10 109.2(9) . . ? F8 C7 F9 106.4(9) . . ? F10 C7 F9 105.2(8) . . ? F8 C7 C6 114.4(8) . . ? F10 C7 C6 110.5(9) . . ? F9 C7 C6 110.6(9) . . ? C9 C8 C6 123.7(9) . . ? C9 C8 H8 118.1 . . ? C6 C8 H8 118.1 . . ? O4 C9 C8 128.4(7) . . ? O4 C9 C10 111.8(8) . . ? C8 C9 C10 119.8(8) . . ? F12 C10 F11 107.4(10) . . ? F12 C10 F13 106.8(9) . . ? F11 C10 F13 106.4(9) . . ? F12 C10 C9 113.5(9) . . ? F11 C10 C9 109.6(9) . . ? F13 C10 C9 112.8(9) . . ? O2 C4 C3 129.6(10) . . ? O2 C4 C5 112.4(9) . . ? C3 C4 C5 118.1(9) . . ? F5 C5 F7 109.0(10) . . ? F5 C5 F6 103.8(10) . . ? F7 C5 F6 103.9(9) . . ? F5 C5 C4 112.3(9) . . ? F7 C5 C4 115.4(10) . . ? F6 C5 C4 111.5(10) . . ? C4 C3 C1 123.1(9) . . ? C4 C3 H3 118.4 . . ? C1 C3 H3 118.4 . . ? O1 C1 C3 126.9(10) . . ? O1 C1 C2 111.0(8) . . ? C3 C1 C2 121.9(8) . . ? F1A C2 F3 123.4(14) . . ? F1A C2 F2 79.4(12) . . ? F3 C2 F2 117.0(12) . . ? F1A C2 F1 35.6(9) . . ? F3 C2 F1 111.6(11) . . ? F2 C2 F1 113.6(12) . . ? F1A C2 F3A 135.5(14) . . ? F3 C2 F3A 47.2(8) . . ? F2 C2 F3A 74.6(10) . . ? F1 C2 F3A 153.9(13) . . ? F1A C2 F2A 96.4(10) . . ? F3 C2 F2A 46.6(8) . . ? F2 C2 F2A 156.3(12) . . ? F1 C2 F2A 69.2(9) . . ? F3A C2 F2A 93.5(9) . . ? F1A C2 C1 116.4(11) . . ? F3 C2 C1 108.8(11) . . ? F2 C2 C1 108.3(10) . . ? F1 C2 C1 95.2(10) . . ? F3A C2 C1 105.8(11) . . ? F2A C2 C1 94.5(9) . . ? N1 C11 C29 121.1(7) . . ? N1 C11 C12 119.2(6) . . ? C29 C11 C12 119.6(7) . . ? N2 C12 C16 123.1(7) . . ? N2 C12 C11 115.5(7) . . ? C16 C12 C11 121.4(7) . . ? N2 C13 C14 123.6(8) . . ? N2 C13 H13 118.2 . . ? C14 C13 H13 118.2 . . ? C13 C14 C15 119.3(8) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C14 C15 C16 118.6(8) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? C12 C16 C15 117.6(7) . . ? C12 C16 C17 119.5(7) . . ? C15 C16 C17 122.9(7) . . ? C18 C17 C48 116.2(7) . . ? C18 C17 C16 119.0(7) . . ? C48 C17 C16 124.7(7) . . ? N3 C18 C17 124.1(7) . . ? N3 C18 C29 114.3(7) . . ? C17 C18 C29 121.6(7) . . ? O5 C19 C21 128.7(8) . . ? O5 C19 C20 111.9(8) . . ? C21 C19 C20 119.4(8) . . ? F15 C20 F14 107.3(9) . . ? F15 C20 F16 104.4(10) . . ? F14 C20 F16 107.1(9) . . ? F15 C20 C19 113.8(9) . . ? F14 C20 C19 113.2(9) . . ? F16 C20 C19 110.4(9) . . ? C22 C21 C19 122.3(8) . . ? C22 C21 H21 118.9 . . ? C19 C21 H21 118.9 . . ? O6 C22 C21 130.1(8) . . ? O6 C22 C23 112.4(7) . . ? C21 C22 C23 117.5(7) . . ? F19 C23 F17 107.2(8) . . ? F19 C23 F18 105.2(8) . . ? F17 C23 F18 107.1(7) . . ? F19 C23 C22 112.8(7) . . ? F17 C23 C22 114.0(8) . . ? F18 C23 C22 110.0(7) . . ? O7 C24 C26 128.8(8) . . ? O7 C24 C25 114.3(8) . . ? C26 C24 C25 116.8(8) . . ? F22 C25 F21 108.9(9) . . ? F22 C25 F20 105.4(8) . . ? F21 C25 F20 103.8(9) . . ? F22 C25 C24 114.2(8) . . ? F21 C25 C24 113.3(8) . . ? F20 C25 C24 110.5(8) . . ? C24 C26 C27 123.4(8) . . ? C24 C26 H26 118.3 . . ? C27 C26 H26 118.3 . . ? O8 C27 C26 127.5(8) . . ? O8 C27 C28 113.9(7) . . ? C26 C27 C28 118.6(7) . . ? F25 C28 F23 105.7(8) . . ? F25 C28 F24 105.2(7) . . ? F23 C28 F24 108.1(8) . . ? F25 C28 C27 111.0(8) . . ? F23 C28 C27 111.5(8) . . ? F24 C28 C27 114.7(8) . . ? N4 C29 C11 121.9(7) . . ? N4 C29 C18 119.7(6) . . ? C11 C29 C18 118.3(7) . . ? N4 C30 C36 119.4(7) . . ? N4 C30 C31 121.8(7) . . ? C36 C30 C31 118.8(7) . . ? N1 C31 C32 119.9(7) . . ? N1 C31 C30 119.3(7) . . ? C32 C31 C30 120.7(7) . . ? C33 C32 C31 119.8(7) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C35 119.5(8) . . ? C32 C33 S1 123.5(6) . . ? C35 C33 S1 117.1(6) . . ? C37 C34 S2 122.9(6) . . ? C37 C34 S1 120.8(7) . . ? S2 C34 S1 116.3(5) . . ? C36 C35 C33 122.3(8) . . ? C36 C35 S2 123.2(6) . . ? C33 C35 S2 114.5(6) . . ? C35 C36 C30 118.9(7) . . ? C35 C36 H36 120.6 . . ? C30 C36 H36 120.6 . . ? C34 C37 S5 124.0(7) . . ? C34 C37 S3 123.1(7) . . ? S5 C37 S3 112.8(5) . . ? C42 C38 S4 126.4(8) . . ? C42 C38 S3 115.8(7) . . ? S4 C38 S3 117.6(6) . . ? C40 C39 S4 115.2(8) . . ? C40 C39 H39A 108.5 . . ? S4 C39 H39A 108.5 . . ? C40 C39 H39B 108.5 . . ? S4 C39 H39B 108.5 . . ? H39A C39 H39B 107.5 . . ? C41 C40 C39 110.9(10) . . ? C41 C40 H40A 109.4 . . ? C39 C40 H40A 109.4 . . ? C41 C40 H40B 109.4 . . ? C39 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C38 C42 S6 121.8(8) . . ? C38 C42 S5 118.3(7) . . ? S6 C42 S5 119.4(6) . . ? C44 C43 S6 110.7(10) . . ? C44 C43 H43A 109.5 . . ? S6 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? S6 C43 H43B 109.5 . . ? H43A C43 H43B 108.1 . . ? C45 C44 C43 107.6(13) . . ? C45 C44 H44A 110.2 . . ? C43 C44 H44A 110.2 . . ? C45 C44 H44B 110.2 . . ? C43 C44 H44B 110.2 . . ? H44A C44 H44B 108.5 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N3 C46 C47 122.4(8) . . ? N3 C46 H46 118.8 . . ? C47 C46 H46 118.8 . . ? C48 C47 C46 119.6(8) . . ? C48 C47 H47 120.2 . . ? C46 C47 H47 120.2 . . ? C47 C48 C17 119.8(8) . . ? C47 C48 H48 120.1 . . ? C17 C48 H48 120.1 . . ? O10 Co3 O9 89.5(2) . . ? O10 Co3 O12 88.0(2) . . ? O9 Co3 O12 86.4(2) . . ? O10 Co3 O11 175.5(2) . . ? O9 Co3 O11 93.3(2) . . ? O12 Co3 O11 88.6(2) . . ? O10 Co3 N6 98.0(3) . . ? O9 Co3 N6 95.9(2) . . ? O12 Co3 N6 173.6(3) . . ? O11 Co3 N6 85.3(2) . . ? O10 Co3 N5 89.1(2) . . ? O9 Co3 N5 174.5(2) . . ? O12 Co3 N5 98.9(2) . . ? O11 Co3 N5 88.5(2) . . ? N6 Co3 N5 79.0(3) . . ? O10 Co3 Co4 102.77(15) . . ? O9 Co3 Co4 162.63(19) . . ? O12 Co3 Co4 106.04(15) . . ? O11 Co3 Co4 75.31(15) . . ? N6 Co3 Co4 70.49(17) . . ? N5 Co3 Co4 15.37(19) . . ? O14 Co4 O13 90.0(3) . . ? O14 Co4 O15 85.6(3) . . ? O13 Co4 O15 83.9(3) . . ? O14 Co4 O16 93.2(3) . . ? O13 Co4 O16 170.9(3) . . ? O15 Co4 O16 87.9(2) . . ? O14 Co4 N7 90.1(3) . . ? O13 Co4 N7 96.2(3) . . ? O15 Co4 N7 175.8(2) . . ? O16 Co4 N7 92.3(2) . . ? O14 Co4 N8 168.8(3) . . ? O13 Co4 N8 93.9(3) . . ? O15 Co4 N8 105.2(2) . . ? O16 Co4 N8 84.4(2) . . ? N7 Co4 N8 79.1(3) . . ? O14 Co4 Co3 154.7(3) . . ? O13 Co4 Co3 106.7(2) . . ? O15 Co4 Co3 114.29(16) . . ? O16 Co4 Co3 73.18(14) . . ? N7 Co4 Co3 69.77(17) . . ? N8 Co4 Co3 15.38(17) . . ? C81 S7 C82 95.6(4) . . ? C83 S8 C82 96.2(4) . . ? C85 S9 C86 94.9(4) . . ? C86 S10 C87 104.1(6) . . ? C85 S11 C90 94.6(4) . . ? C90 S12 C91 102.9(6) . . ? C49 O9 Co3 122.9(6) . . ? C52 O10 Co3 124.5(6) . . ? C54 O11 Co3 125.1(6) . . ? C57 O12 Co3 126.3(6) . . ? C67 O13 Co4 124.0(8) . . ? C70 O14 Co4 122.8(8) . . ? C72 O15 Co4 123.8(6) . . ? C75 O16 Co4 124.4(5) . . ? C59 N5 C79 117.8(6) . . ? C59 N5 Co3 110.3(5) . . ? C79 N5 Co3 131.5(5) . . ? C61 N6 C60 117.7(7) . . ? C61 N6 Co3 127.4(6) . . ? C60 N6 Co3 114.5(5) . . ? C94 N7 C66 117.3(7) . . ? C94 N7 Co4 128.0(6) . . ? C66 N7 Co4 114.5(5) . . ? C78 N8 C77 116.7(6) . . ? C78 N8 Co4 132.4(5) . . ? C77 N8 Co4 110.6(5) . . ? O9 C49 C51 127.8(8) . . ? O9 C49 C50 113.5(8) . . ? C51 C49 C50 118.7(9) . . ? C49 C51 C52 124.6(9) . . ? C49 C51 H51 117.7 . . ? C52 C51 H51 117.7 . . ? O10 C52 C51 127.6(9) . . ? O10 C52 C53 113.5(8) . . ? C51 C52 C53 118.9(8) . . ? F29 C53 F31 106.0(9) . . ? F29 C53 F30 110.2(9) . . ? F31 C53 F30 106.9(8) . . ? F29 C53 C52 114.3(8) . . ? F31 C53 C52 110.5(9) . . ? F30 C53 C52 108.6(9) . . ? O11 C54 C56 128.1(9) . . ? O11 C54 C55 113.1(9) . . ? C56 C54 C55 118.8(8) . . ? F34 C55 F32 101.7(9) . . ? F34 C55 F33 107.3(9) . . ? F32 C55 F33 95.8(9) . . ? F34 C55 C54 119.2(10) . . ? F32 C55 C54 117.1(9) . . ? F33 C55 C54 112.7(9) . . ? C54 C56 C57 124.4(8) . . ? C54 C56 H56 117.8 . . ? C57 C56 H56 117.8 . . ? O12 C57 C56 126.7(9) . . ? O12 C57 C58 113.0(8) . . ? C56 C57 C58 120.4(8) . . ? F37 C58 F36 107.4(9) . . ? F37 C58 F35 106.2(9) . . ? F36 C58 F35 106.7(9) . . ? F37 C58 C57 113.5(8) . . ? F36 C58 C57 113.0(9) . . ? F35 C58 C57 109.6(8) . . ? N5 C59 C77 121.7(7) . . ? N5 C59 C60 118.3(7) . . ? C77 C59 C60 119.9(7) . . ? N6 C60 C64 124.2(7) . . ? N6 C60 C59 115.2(7) . . ? C64 C60 C59 120.5(7) . . ? N6 C61 C62 122.3(8) . . ? N6 C61 H61 118.8 . . ? C62 C61 H61 118.8 . . ? C63 C62 C61 119.7(8) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C62 C63 C64 120.2(9) . . ? C62 C63 H63 119.9 . . ? C64 C63 H63 119.9 . . ? C63 C64 C60 115.8(8) . . ? C63 C64 C65 124.1(8) . . ? C60 C64 C65 120.1(7) . . ? C96 C65 C66 116.2(7) . . ? C96 C65 C64 125.1(8) . . ? C66 C65 C64 118.6(7) . . ? N7 C66 C65 123.4(7) . . ? N7 C66 C77 115.7(7) . . ? C65 C66 C77 120.7(7) . . ? O13 C67 C69 124.6(12) . . ? O13 C67 C68 113.7(10) . . ? C69 C67 C68 121.7(11) . . ? F40 C68 F39 111.7(9) . . ? F40 C68 F38 104.5(10) . . ? F39 C68 F38 104.4(8) . . ? F40 C68 C67 112.5(10) . . ? F39 C68 C67 113.6(10) . . ? F38 C68 C67 109.4(10) . . ? C70 C69 C67 125.9(12) . . ? C70 C69 H69 117.0 . . ? C67 C69 H69 117.0 . . ? O14 C70 C69 129.3(11) . . ? O14 C70 C71 114.6(12) . . ? C69 C70 C71 116.1(12) . . ? F43 C71 F42 107.1(10) . . ? F43 C71 F41 103.7(11) . . ? F42 C71 F41 93.4(10) . . ? F43 C71 C70 122.6(12) . . ? F42 C71 C70 114.6(12) . . ? F41 C71 C70 111.0(11) . . ? O15 C72 C74 129.9(8) . . ? O15 C72 C73 112.0(8) . . ? C74 C72 C73 118.1(8) . . ? F46 C73 F44 107.9(10) . . ? F46 C73 F45 105.2(10) . . ? F44 C73 F45 105.3(10) . . ? F46 C73 C72 114.5(9) . . ? F44 C73 C72 113.7(9) . . ? F45 C73 C72 109.6(9) . . ? C75 C74 C72 122.1(8) . . ? C75 C74 H74 119.0 . . ? C72 C74 H74 119.0 . . ? O16 C75 C74 129.3(8) . . ? O16 C75 C76 112.4(8) . . ? C74 C75 C76 118.3(7) . . ? F47 C76 F49 109.4(8) . . ? F47 C76 F48 106.5(8) . . ? F49 C76 F48 105.8(7) . . ? F47 C76 C75 113.7(7) . . ? F49 C76 C75 111.6(8) . . ? F48 C76 C75 109.4(7) . . ? N8 C77 C59 122.0(7) . . ? N8 C77 C66 118.2(7) . . ? C59 C77 C66 119.8(7) . . ? N8 C78 C84 119.5(7) . . ? N8 C78 C79 121.3(7) . . ? C84 C78 C79 119.3(7) . . ? N5 C79 C80 120.8(7) . . ? N5 C79 C78 120.1(7) . . ? C80 C79 C78 119.1(7) . . ? C81 C80 C79 120.4(7) . . ? C81 C80 H80 119.8 . . ? C79 C80 H80 119.8 . . ? C80 C81 C83 120.4(8) . . ? C80 C81 S7 122.6(6) . . ? C83 C81 S7 116.9(6) . . ? C85 C82 S8 122.3(6) . . ? C85 C82 S7 122.5(7) . . ? S8 C82 S7 115.2(5) . . ? C84 C83 C81 121.4(7) . . ? C84 C83 S8 122.6(6) . . ? C81 C83 S8 115.9(6) . . ? C83 C84 C78 119.2(7) . . ? C83 C84 H84 120.4 . . ? C78 C84 H84 120.4 . . ? C82 C85 S11 124.1(6) . . ? C82 C85 S9 122.9(6) . . ? S11 C85 S9 113.0(5) . . ? C90 C86 S10 124.3(7) . . ? C90 C86 S9 116.6(7) . . ? S10 C86 S9 118.6(5) . . ? C88 C87 S10 114.4(10) . . ? C88 C87 H87A 108.7 . . ? S10 C87 H87A 108.7 . . ? C88 C87 H87B 108.7 . . ? S10 C87 H87B 108.7 . . ? H87A C87 H87B 107.6 . . ? C87 C88 C89 110.7(13) . . ? C87 C88 H88A 109.5 . . ? C89 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? C89 C88 H88B 109.5 . . ? H88A C88 H88B 108.1 . . ? C88 C89 H89A 109.5 . . ? C88 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C88 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C86 C90 S12 124.3(7) . . ? C86 C90 S11 117.5(6) . . ? S12 C90 S11 117.1(5) . . ? C92 C91 S12 116.4(10) . . ? C92 C91 H91A 108.2 . . ? S12 C91 H91A 108.2 . . ? C92 C91 H91B 108.2 . . ? S12 C91 H91B 108.2 . . ? H91A C91 H91B 107.3 . . ? C93 C92 C91 113.0(15) . . ? C93 C92 H92A 109.0 . . ? C91 C92 H92A 109.0 . . ? C93 C92 H92B 109.0 . . ? C91 C92 H92B 109.0 . . ? H92A C92 H92B 107.8 . . ? C92 C93 H93A 109.5 . . ? C92 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C92 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? N7 C94 C95 123.2(8) . . ? N7 C94 H94 118.4 . . ? C95 C94 H94 118.4 . . ? C96 C95 C94 117.8(8) . . ? C96 C95 H95 121.1 . . ? C94 C95 H95 121.1 . . ? C65 C96 C95 122.1(8) . . ? C65 C96 H96 119.0 . . ? C95 C96 H96 119.0 . . ? F28 C50 F28A 116.8(14) . . ? F28 C50 F26A 61.5(9) . . ? F28A C50 F26A 115.2(12) . . ? F28 C50 F26 112.8(12) . . ? F28A C50 F26 75.6(11) . . ? F26A C50 F26 55.1(8) . . ? F28 C50 F27 113.2(12) . . ? F28A C50 F27 22.4(9) . . ? F26A C50 F27 135.0(12) . . ? F26 C50 F27 97.3(12) . . ? F28 C50 F27A 36.7(8) . . ? F28A C50 F27A 93.6(13) . . ? F26A C50 F27A 96.6(10) . . ? F26 C50 F27A 137.5(11) . . ? F27 C50 F27A 81.2(11) . . ? F28 C50 C49 114.1(11) . . ? F28A C50 C49 119.5(11) . . ? F26A C50 C49 116.4(10) . . ? F26 C50 C49 111.7(10) . . ? F27 C50 C49 106.4(9) . . ? F27A C50 C49 109.3(9) . . ? N9 C99 C100 176.8(17) . . ? C99 C100 H10A 109.5 . . ? C99 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C99 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? O17 C101 C105 125(2) . . ? O17 C101 C102 128(2) . . ? C105 C101 C102 106.7(15) . . ? C101 C102 H112 109.5 . . ? C101 C102 H122 109.5 . . ? H112 C102 H122 109.5 . . ? C101 C102 H132 109.5 . . ? H112 C102 H132 109.5 . . ? H122 C102 H132 109.5 . . ? C101 C105 H115 109.5 . . ? C101 C105 H125 109.5 . . ? H115 C105 H125 109.5 . . ? C101 C105 H135 109.5 . . ? H115 C105 H135 109.5 . . ? H125 C105 H135 109.5 . . ? O18 C103 C106 117(2) . . ? O18 C103 C104 121(2) . . ? C106 C103 C104 120(2) . . ? C103 C104 H114 109.5 . . ? C103 C104 H124 109.5 . . ? H114 C104 H124 109.5 . . ? C103 C104 H134 109.5 . . ? H114 C104 H134 109.5 . . ? H124 C104 H134 109.5 . . ? C103 C106 H116 109.5 . . ? C103 C106 H126 109.5 . . ? H116 C106 H126 109.5 . . ? C103 C106 H136 109.5 . . ? H116 C106 H136 109.5 . . ? H126 C106 H136 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Co1 Co2 O8 -0.1(3) . . . . ? O2 Co1 Co2 O8 173.7(3) . . . . ? O1 Co1 Co2 O8 89.9(3) . . . . ? O4 Co1 Co2 O8 -117.3(5) . . . . ? N2 Co1 Co2 O8 -95.7(3) . . . . ? N1 Co1 Co2 O8 32.9(7) . . . . ? O3 Co1 Co2 O7 141.0(4) . . . . ? O2 Co1 Co2 O7 -45.2(4) . . . . ? O1 Co1 Co2 O7 -129.0(4) . . . . ? O4 Co1 Co2 O7 23.8(6) . . . . ? N2 Co1 Co2 O7 45.4(4) . . . . ? N1 Co1 Co2 O7 174.0(7) . . . . ? O3 Co1 Co2 O5 -92.9(3) . . . . ? O2 Co1 Co2 O5 80.8(3) . . . . ? O1 Co1 Co2 O5 -3.0(3) . . . . ? O4 Co1 Co2 O5 149.8(5) . . . . ? N2 Co1 Co2 O5 171.4(3) . . . . ? N1 Co1 Co2 O5 -60.0(7) . . . . ? O3 Co1 Co2 N3 89.3(3) . . . . ? O2 Co1 Co2 N3 -97.0(3) . . . . ? O1 Co1 Co2 N3 179.2(3) . . . . ? O4 Co1 Co2 N3 -28.0(5) . . . . ? N2 Co1 Co2 N3 -6.4(3) . . . . ? N1 Co1 Co2 N3 122.2(7) . . . . ? O3 Co1 Co2 O6 -174.2(3) . . . . ? O2 Co1 Co2 O6 -0.5(3) . . . . ? O1 Co1 Co2 O6 -84.3(3) . . . . ? O4 Co1 Co2 O6 68.5(5) . . . . ? N2 Co1 Co2 O6 90.1(3) . . . . ? N1 Co1 Co2 O6 -141.3(6) . . . . ? O3 Co1 Co2 N4 -24.8(6) . . . . ? O2 Co1 Co2 N4 148.9(6) . . . . ? O1 Co1 Co2 N4 65.2(6) . . . . ? O4 Co1 Co2 N4 -142.1(7) . . . . ? N2 Co1 Co2 N4 -120.4(6) . . . . ? N1 Co1 Co2 N4 8.2(8) . . . . ? O2 Co1 O3 C6 105(2) . . . . ? O1 Co1 O3 C6 70.5(7) . . . . ? O4 Co1 O3 C6 -15.8(8) . . . . ? N2 Co1 O3 C6 -108.4(7) . . . . ? N1 Co1 O3 C6 173.4(8) . . . . ? Co2 Co1 O3 C6 -178.5(7) . . . . ? O3 Co1 O4 C9 14.8(7) . . . . ? O2 Co1 O4 C9 -159.8(7) . . . . ? O1 Co1 O4 C9 -71.8(7) . . . . ? N2 Co1 O4 C9 113.4(7) . . . . ? N1 Co1 O4 C9 84.5(17) . . . . ? Co2 Co1 O4 C9 133.5(6) . . . . ? O3 Co1 O2 C4 -53(2) . . . . ? O1 Co1 O2 C4 -17.7(8) . . . . ? O4 Co1 O2 C4 68.4(8) . . . . ? N2 Co1 O2 C4 160.9(8) . . . . ? N1 Co1 O2 C4 -120.4(8) . . . . ? Co2 Co1 O2 C4 -129.8(8) . . . . ? O3 Co1 O1 C1 -161.8(8) . . . . ? O2 Co1 O1 C1 21.8(8) . . . . ? O4 Co1 O1 C1 -71.8(8) . . . . ? N2 Co1 O1 C1 6(3) . . . . ? N1 Co1 O1 C1 112.2(8) . . . . ? Co2 Co1 O1 C1 99.4(7) . . . . ? O8 Co2 O5 C19 169.2(6) . . . . ? O7 Co2 O5 C19 78.5(6) . . . . ? N3 Co2 O5 C19 -14(6) . . . . ? O6 Co2 O5 C19 -13.1(6) . . . . ? N4 Co2 O5 C19 -97.8(6) . . . . ? Co1 Co2 O5 C19 -80.7(6) . . . . ? O8 Co2 O6 C22 30(2) . . . . ? O7 Co2 O6 C22 -81.2(6) . . . . ? O5 Co2 O6 C22 6.4(6) . . . . ? N3 Co2 O6 C22 -173.6(6) . . . . ? N4 Co2 O6 C22 107.6(6) . . . . ? Co1 Co2 O6 C22 116.7(6) . . . . ? O8 Co2 O7 C24 -15.1(6) . . . . ? O5 Co2 O7 C24 71.2(6) . . . . ? N3 Co2 O7 C24 -111.1(6) . . . . ? O6 Co2 O7 C24 159.8(6) . . . . ? N4 Co2 O7 C24 -131.6(14) . . . . ? Co1 Co2 O7 C24 -158.9(5) . . . . ? O7 Co2 O8 C27 16.4(7) . . . . ? O5 Co2 O8 C27 -71.2(7) . . . . ? N3 Co2 O8 C27 108.9(7) . . . . ? O6 Co2 O8 C27 -95(2) . . . . ? N4 Co2 O8 C27 -172.1(7) . . . . ? Co1 Co2 O8 C27 -179.6(6) . . . . ? O3 Co1 N1 C11 108.6(5) . . . . ? O2 Co1 N1 C11 -77.3(5) . . . . ? O1 Co1 N1 C11 -165.7(5) . . . . ? O4 Co1 N1 C11 38.7(17) . . . . ? N2 Co1 N1 C11 9.2(5) . . . . ? Co2 Co1 N1 C11 -38.9(5) . . . . ? O3 Co1 N1 C31 -73.7(7) . . . . ? O2 Co1 N1 C31 100.5(7) . . . . ? O1 Co1 N1 C31 12.1(7) . . . . ? O4 Co1 N1 C31 -143.6(14) . . . . ? N2 Co1 N1 C31 -173.1(7) . . . . ? Co2 Co1 N1 C31 138.8(11) . . . . ? O3 Co1 N2 C13 91.0(7) . . . . ? O2 Co1 N2 C13 -92.5(7) . . . . ? O1 Co1 N2 C13 -77(3) . . . . ? O4 Co1 N2 C13 0.8(7) . . . . ? N1 Co1 N2 C13 176.0(8) . . . . ? Co2 Co1 N2 C13 -172.2(8) . . . . ? O3 Co1 N2 C12 -91.8(6) . . . . ? O2 Co1 N2 C12 84.6(6) . . . . ? O1 Co1 N2 C12 100(3) . . . . ? O4 Co1 N2 C12 178.0(6) . . . . ? N1 Co1 N2 C12 -6.8(5) . . . . ? Co2 Co1 N2 C12 5.0(5) . . . . ? O8 Co2 N3 C46 -76.4(7) . . . . ? O7 Co2 N3 C46 14.4(7) . . . . ? O5 Co2 N3 C46 106(6) . . . . ? O6 Co2 N3 C46 105.9(7) . . . . ? N4 Co2 N3 C46 -169.0(7) . . . . ? Co1 Co2 N3 C46 174.3(7) . . . . ? O8 Co2 N3 C18 109.7(5) . . . . ? O7 Co2 N3 C18 -159.5(5) . . . . ? O5 Co2 N3 C18 -67(6) . . . . ? O6 Co2 N3 C18 -68.0(5) . . . . ? N4 Co2 N3 C18 17.1(5) . . . . ? Co1 Co2 N3 C18 0.4(5) . . . . ? O8 Co2 N4 C29 -115.0(5) . . . . ? O7 Co2 N4 C29 1.3(17) . . . . ? O5 Co2 N4 C29 158.1(5) . . . . ? N3 Co2 N4 C29 -19.6(5) . . . . ? O6 Co2 N4 C29 70.4(5) . . . . ? Co1 Co2 N4 C29 41.9(5) . . . . ? O8 Co2 N4 C30 79.0(7) . . . . ? O7 Co2 N4 C30 -164.8(12) . . . . ? O5 Co2 N4 C30 -8.0(8) . . . . ? N3 Co2 N4 C30 174.3(8) . . . . ? O6 Co2 N4 C30 -95.7(7) . . . . ? Co1 Co2 N4 C30 -124.2(10) . . . . ? Co1 O3 C6 C8 11.4(14) . . . . ? Co1 O3 C6 C7 -168.6(7) . . . . ? O3 C6 C7 F8 177.6(9) . . . . ? C8 C6 C7 F8 -2.4(15) . . . . ? O3 C6 C7 F10 53.8(12) . . . . ? C8 C6 C7 F10 -126.3(10) . . . . ? O3 C6 C7 F9 -62.3(12) . . . . ? C8 C6 C7 F9 117.7(10) . . . . ? O3 C6 C8 C9 0.5(17) . . . . ? C7 C6 C8 C9 -179.5(10) . . . . ? Co1 O4 C9 C8 -9.5(13) . . . . ? Co1 O4 C9 C10 170.8(6) . . . . ? C6 C8 C9 O4 -1.5(17) . . . . ? C6 C8 C9 C10 178.3(10) . . . . ? O4 C9 C10 F12 46.8(12) . . . . ? C8 C9 C10 F12 -133.0(10) . . . . ? O4 C9 C10 F11 -73.3(12) . . . . ? C8 C9 C10 F11 106.9(11) . . . . ? O4 C9 C10 F13 168.4(9) . . . . ? C8 C9 C10 F13 -11.4(15) . . . . ? Co1 O2 C4 C3 5.9(16) . . . . ? Co1 O2 C4 C5 -174.9(6) . . . . ? O2 C4 C5 F5 -68.4(14) . . . . ? C3 C4 C5 F5 111.0(12) . . . . ? O2 C4 C5 F7 165.8(9) . . . . ? C3 C4 C5 F7 -14.8(16) . . . . ? O2 C4 C5 F6 47.6(12) . . . . ? C3 C4 C5 F6 -133.0(10) . . . . ? O2 C4 C3 C1 10.7(19) . . . . ? C5 C4 C3 C1 -168.5(10) . . . . ? Co1 O1 C1 C3 -14.7(15) . . . . ? Co1 O1 C1 C2 159.8(6) . . . . ? C4 C3 C1 O1 -5.6(18) . . . . ? C4 C3 C1 C2 -179.5(9) . . . . ? O1 C1 C2 F1A 40.3(14) . . . . ? C3 C1 C2 F1A -144.9(13) . . . . ? O1 C1 C2 F3 -174.8(11) . . . . ? C3 C1 C2 F3 0.0(15) . . . . ? O1 C1 C2 F2 -46.7(13) . . . . ? C3 C1 C2 F2 128.1(12) . . . . ? O1 C1 C2 F1 70.3(11) . . . . ? C3 C1 C2 F1 -114.9(12) . . . . ? O1 C1 C2 F3A -125.3(11) . . . . ? C3 C1 C2 F3A 49.5(14) . . . . ? O1 C1 C2 F2A 139.7(9) . . . . ? C3 C1 C2 F2A -45.5(12) . . . . ? C31 N1 C11 C29 -6.2(11) . . . . ? Co1 N1 C11 C29 171.8(6) . . . . ? C31 N1 C11 C12 171.3(7) . . . . ? Co1 N1 C11 C12 -10.6(9) . . . . ? C13 N2 C12 C16 0.4(12) . . . . ? Co1 N2 C12 C16 -177.1(6) . . . . ? C13 N2 C12 C11 -179.1(8) . . . . ? Co1 N2 C12 C11 3.4(9) . . . . ? N1 C11 C12 N2 5.3(11) . . . . ? C29 C11 C12 N2 -177.1(7) . . . . ? N1 C11 C12 C16 -174.2(7) . . . . ? C29 C11 C12 C16 3.4(12) . . . . ? C12 N2 C13 C14 -0.6(13) . . . . ? Co1 N2 C13 C14 176.6(7) . . . . ? N2 C13 C14 C15 2.5(14) . . . . ? C13 C14 C15 C16 -4.0(13) . . . . ? N2 C12 C16 C15 -2.0(12) . . . . ? C11 C12 C16 C15 177.4(7) . . . . ? N2 C12 C16 C17 179.6(7) . . . . ? C11 C12 C16 C17 -1.0(12) . . . . ? C14 C15 C16 C12 3.8(12) . . . . ? C14 C15 C16 C17 -177.9(8) . . . . ? C12 C16 C17 C18 -5.2(11) . . . . ? C15 C16 C17 C18 176.5(8) . . . . ? C12 C16 C17 C48 177.4(8) . . . . ? C15 C16 C17 C48 -0.9(12) . . . . ? C46 N3 C18 C17 -3.1(12) . . . . ? Co2 N3 C18 C17 171.4(6) . . . . ? C46 N3 C18 C29 173.7(7) . . . . ? Co2 N3 C18 C29 -11.8(8) . . . . ? C48 C17 C18 N3 3.2(12) . . . . ? C16 C17 C18 N3 -174.4(7) . . . . ? C48 C17 C18 C29 -173.4(7) . . . . ? C16 C17 C18 C29 9.0(11) . . . . ? Co2 O5 C19 C21 12.3(13) . . . . ? Co2 O5 C19 C20 -167.4(6) . . . . ? O5 C19 C20 F15 42.5(13) . . . . ? C21 C19 C20 F15 -137.2(10) . . . . ? O5 C19 C20 F14 165.4(9) . . . . ? C21 C19 C20 F14 -14.3(15) . . . . ? O5 C19 C20 F16 -74.5(11) . . . . ? C21 C19 C20 F16 105.7(10) . . . . ? O5 C19 C21 C22 0.1(15) . . . . ? C20 C19 C21 C22 179.8(9) . . . . ? Co2 O6 C22 C21 2.4(12) . . . . ? Co2 O6 C22 C23 179.4(5) . . . . ? C19 C21 C22 O6 -8.5(15) . . . . ? C19 C21 C22 C23 174.6(8) . . . . ? O6 C22 C23 F19 -58.7(9) . . . . ? C21 C22 C23 F19 118.8(9) . . . . ? O6 C22 C23 F17 178.8(7) . . . . ? C21 C22 C23 F17 -3.7(12) . . . . ? O6 C22 C23 F18 58.5(10) . . . . ? C21 C22 C23 F18 -124.1(8) . . . . ? Co2 O7 C24 C26 8.9(13) . . . . ? Co2 O7 C24 C25 -169.6(5) . . . . ? O7 C24 C25 F22 -148.4(9) . . . . ? C26 C24 C25 F22 32.9(12) . . . . ? O7 C24 C25 F21 -23.0(12) . . . . ? C26 C24 C25 F21 158.3(9) . . . . ? O7 C24 C25 F20 93.0(10) . . . . ? C26 C24 C25 F20 -85.7(10) . . . . ? O7 C24 C26 C27 2.4(15) . . . . ? C25 C24 C26 C27 -179.1(8) . . . . ? Co2 O8 C27 C26 -11.8(12) . . . . ? Co2 O8 C27 C28 168.7(6) . . . . ? C24 C26 C27 O8 -0.9(15) . . . . ? C24 C26 C27 C28 178.5(9) . . . . ? O8 C27 C28 F25 61.1(11) . . . . ? C26 C27 C28 F25 -118.4(9) . . . . ? O8 C27 C28 F23 -56.5(11) . . . . ? C26 C27 C28 F23 124.0(9) . . . . ? O8 C27 C28 F24 -179.8(8) . . . . ? C26 C27 C28 F24 0.7(13) . . . . ? C30 N4 C29 C11 5.4(11) . . . . ? Co2 N4 C29 C11 -163.2(6) . . . . ? C30 N4 C29 C18 -171.1(7) . . . . ? Co2 N4 C29 C18 20.3(8) . . . . ? N1 C11 C29 N4 1.2(11) . . . . ? C12 C11 C29 N4 -176.3(7) . . . . ? N1 C11 C29 C18 177.8(7) . . . . ? C12 C11 C29 C18 0.2(11) . . . . ? N3 C18 C29 N4 -6.8(10) . . . . ? C17 C18 C29 N4 170.1(7) . . . . ? N3 C18 C29 C11 176.6(7) . . . . ? C17 C18 C29 C11 -6.5(11) . . . . ? C29 N4 C30 C36 173.0(7) . . . . ? Co2 N4 C30 C36 -21.9(11) . . . . ? C29 N4 C30 C31 -7.0(11) . . . . ? Co2 N4 C30 C31 158.1(6) . . . . ? C11 N1 C31 C32 -172.2(7) . . . . ? Co1 N1 C31 C32 10.2(11) . . . . ? C11 N1 C31 C30 4.6(10) . . . . ? Co1 N1 C31 C30 -173.0(5) . . . . ? N4 C30 C31 N1 2.1(11) . . . . ? C36 C30 C31 N1 -177.9(7) . . . . ? N4 C30 C31 C32 178.8(7) . . . . ? C36 C30 C31 C32 -1.1(11) . . . . ? N1 C31 C32 C33 177.4(7) . . . . ? C30 C31 C32 C33 0.7(12) . . . . ? C31 C32 C33 C35 -0.2(12) . . . . ? C31 C32 C33 S1 -178.8(6) . . . . ? C34 S1 C33 C32 180.0(7) . . . . ? C34 S1 C33 C35 1.4(7) . . . . ? C35 S2 C34 C37 -175.2(8) . . . . ? C35 S2 C34 S1 3.9(6) . . . . ? C33 S1 C34 C37 175.7(7) . . . . ? C33 S1 C34 S2 -3.4(6) . . . . ? C32 C33 C35 C36 0.1(12) . . . . ? S1 C33 C35 C36 178.7(6) . . . . ? C32 C33 C35 S2 -177.6(6) . . . . ? S1 C33 C35 S2 1.0(8) . . . . ? C34 S2 C35 C36 179.5(7) . . . . ? C34 S2 C35 C33 -2.9(7) . . . . ? C33 C35 C36 C30 -0.5(12) . . . . ? S2 C35 C36 C30 177.0(6) . . . . ? N4 C30 C36 C35 -179.0(7) . . . . ? C31 C30 C36 C35 1.0(11) . . . . ? S2 C34 C37 S5 -2.5(11) . . . . ? S1 C34 C37 S5 178.4(5) . . . . ? S2 C34 C37 S3 -179.7(5) . . . . ? S1 C34 C37 S3 1.2(11) . . . . ? C42 S5 C37 C34 166.6(8) . . . . ? C42 S5 C37 S3 -15.9(5) . . . . ? C38 S3 C37 C34 -165.4(8) . . . . ? C38 S3 C37 S5 17.1(5) . . . . ? C39 S4 C38 C42 118.1(9) . . . . ? C39 S4 C38 S3 -68.9(7) . . . . ? C37 S3 C38 C42 -12.0(8) . . . . ? C37 S3 C38 S4 174.3(6) . . . . ? C38 S4 C39 C40 -52.5(10) . . . . ? S4 C39 C40 C41 -61.9(11) . . . . ? S4 C38 C42 S6 3.6(13) . . . . ? S3 C38 C42 S6 -169.5(5) . . . . ? S4 C38 C42 S5 175.7(5) . . . . ? S3 C38 C42 S5 2.6(11) . . . . ? C43 S6 C42 C38 -152.0(9) . . . . ? C43 S6 C42 S5 36.0(7) . . . . ? C37 S5 C42 C38 8.3(8) . . . . ? C37 S5 C42 S6 -179.4(6) . . . . ? C42 S6 C43 C44 70.0(11) . . . . ? S6 C43 C44 C45 172.1(12) . . . . ? C18 N3 C46 C47 0.2(12) . . . . ? Co2 N3 C46 C47 -173.5(6) . . . . ? N3 C46 C47 C48 2.4(13) . . . . ? C46 C47 C48 C17 -2.3(13) . . . . ? C18 C17 C48 C47 -0.3(12) . . . . ? C16 C17 C48 C47 177.1(8) . . . . ? O10 Co3 Co4 O14 135.0(6) . . . . ? O9 Co3 Co4 O14 1.1(8) . . . . ? O12 Co3 Co4 O14 -133.4(6) . . . . ? O11 Co3 Co4 O14 -49.2(6) . . . . ? N6 Co3 Co4 O14 40.9(7) . . . . ? N5 Co3 Co4 O14 162.7(9) . . . . ? O10 Co3 Co4 O13 5.3(3) . . . . ? O9 Co3 Co4 O13 -128.5(6) . . . . ? O12 Co3 Co4 O13 96.9(3) . . . . ? O11 Co3 Co4 O13 -178.9(3) . . . . ? N6 Co3 Co4 O13 -88.8(4) . . . . ? N5 Co3 Co4 O13 33.0(7) . . . . ? O10 Co3 Co4 O15 -85.4(2) . . . . ? O9 Co3 Co4 O15 140.7(6) . . . . ? O12 Co3 Co4 O15 6.2(2) . . . . ? O11 Co3 Co4 O15 90.3(2) . . . . ? N6 Co3 Co4 O15 -179.5(3) . . . . ? N5 Co3 Co4 O15 -57.7(7) . . . . ? O10 Co3 Co4 O16 -165.2(2) . . . . ? O9 Co3 Co4 O16 60.9(6) . . . . ? O12 Co3 Co4 O16 -73.6(2) . . . . ? O11 Co3 Co4 O16 10.6(2) . . . . ? N6 Co3 Co4 O16 100.7(3) . . . . ? N5 Co3 Co4 O16 -137.5(7) . . . . ? O10 Co3 Co4 N7 95.9(3) . . . . ? O9 Co3 Co4 N7 -38.0(6) . . . . ? O12 Co3 Co4 N7 -172.5(3) . . . . ? O11 Co3 Co4 N7 -88.4(3) . . . . ? N6 Co3 Co4 N7 1.8(3) . . . . ? N5 Co3 Co4 N7 123.6(7) . . . . ? O10 Co3 Co4 N8 -29.4(7) . . . . ? O9 Co3 Co4 N8 -163.3(8) . . . . ? O12 Co3 Co4 N8 62.2(7) . . . . ? O11 Co3 Co4 N8 146.3(7) . . . . ? N6 Co3 Co4 N8 -123.5(7) . . . . ? N5 Co3 Co4 N8 -1.7(9) . . . . ? O10 Co3 O9 C49 17.7(7) . . . . ? O12 Co3 O9 C49 -70.3(7) . . . . ? O11 Co3 O9 C49 -158.7(7) . . . . ? N6 Co3 O9 C49 115.7(7) . . . . ? N5 Co3 O9 C49 93(3) . . . . ? Co4 Co3 O9 C49 153.1(6) . . . . ? O9 Co3 O10 C52 -17.4(8) . . . . ? O12 Co3 O10 C52 69.1(7) . . . . ? O11 Co3 O10 C52 111(3) . . . . ? N6 Co3 O10 C52 -113.2(7) . . . . ? N5 Co3 O10 C52 168.0(7) . . . . ? Co4 Co3 O10 C52 175.1(7) . . . . ? O10 Co3 O11 C54 -46(3) . . . . ? O9 Co3 O11 C54 81.7(7) . . . . ? O12 Co3 O11 C54 -4.6(7) . . . . ? N6 Co3 O11 C54 177.3(7) . . . . ? N5 Co3 O11 C54 -103.6(7) . . . . ? Co4 Co3 O11 C54 -111.6(7) . . . . ? O10 Co3 O12 C57 -175.0(6) . . . . ? O9 Co3 O12 C57 -85.4(6) . . . . ? O11 Co3 O12 C57 8.1(6) . . . . ? N6 Co3 O12 C57 26(2) . . . . ? N5 Co3 O12 C57 96.3(6) . . . . ? Co4 Co3 O12 C57 82.3(6) . . . . ? O14 Co4 O13 C67 19.8(11) . . . . ? O15 Co4 O13 C67 -65.8(11) . . . . ? O16 Co4 O13 C67 -91.4(19) . . . . ? N7 Co4 O13 C67 109.9(11) . . . . ? N8 Co4 O13 C67 -170.6(11) . . . . ? Co3 Co4 O13 C67 -179.4(11) . . . . ? O13 Co4 O14 C70 -15.2(12) . . . . ? O15 Co4 O14 C70 68.7(11) . . . . ? O16 Co4 O14 C70 156.3(11) . . . . ? N7 Co4 O14 C70 -111.4(11) . . . . ? N8 Co4 O14 C70 -126.2(16) . . . . ? Co3 Co4 O14 C70 -147.7(9) . . . . ? O14 Co4 O15 C72 76.1(7) . . . . ? O13 Co4 O15 C72 166.6(7) . . . . ? O16 Co4 O15 C72 -17.3(7) . . . . ? N7 Co4 O15 C72 75(3) . . . . ? N8 Co4 O15 C72 -101.0(7) . . . . ? Co3 Co4 O15 C72 -87.8(7) . . . . ? O14 Co4 O16 C75 -75.7(7) . . . . ? O13 Co4 O16 C75 35.3(19) . . . . ? O15 Co4 O16 C75 9.8(7) . . . . ? N7 Co4 O16 C75 -165.9(7) . . . . ? N8 Co4 O16 C75 115.3(7) . . . . ? Co3 Co4 O16 C75 126.0(7) . . . . ? O10 Co3 N5 C59 112.9(5) . . . . ? O9 Co3 N5 C59 38(3) . . . . ? O12 Co3 N5 C59 -159.3(5) . . . . ? O11 Co3 N5 C59 -71.0(5) . . . . ? N6 Co3 N5 C59 14.5(5) . . . . ? Co4 Co3 N5 C59 -40.2(6) . . . . ? O10 Co3 N5 C79 -74.4(7) . . . . ? O9 Co3 N5 C79 -149(2) . . . . ? O12 Co3 N5 C79 13.4(7) . . . . ? O11 Co3 N5 C79 101.8(7) . . . . ? N6 Co3 N5 C79 -172.7(7) . . . . ? Co4 Co3 N5 C79 132.6(11) . . . . ? O10 Co3 N6 C61 88.1(7) . . . . ? O9 Co3 N6 C61 -2.2(7) . . . . ? O12 Co3 N6 C61 -113(2) . . . . ? O11 Co3 N6 C61 -95.1(7) . . . . ? N5 Co3 N6 C61 175.6(7) . . . . ? Co4 Co3 N6 C61 -171.1(7) . . . . ? O10 Co3 N6 C60 -99.8(5) . . . . ? O9 Co3 N6 C60 169.9(5) . . . . ? O12 Co3 N6 C60 59(2) . . . . ? O11 Co3 N6 C60 77.0(5) . . . . ? N5 Co3 N6 C60 -12.3(5) . . . . ? Co4 Co3 N6 C60 1.0(5) . . . . ? O14 Co4 N7 C94 8.2(7) . . . . ? O13 Co4 N7 C94 -81.9(7) . . . . ? O15 Co4 N7 C94 9(4) . . . . ? O16 Co4 N7 C94 101.4(7) . . . . ? N8 Co4 N7 C94 -174.7(7) . . . . ? Co3 Co4 N7 C94 172.5(7) . . . . ? O14 Co4 N7 C66 -166.1(6) . . . . ? O13 Co4 N7 C66 103.8(6) . . . . ? O15 Co4 N7 C66 -165(3) . . . . ? O16 Co4 N7 C66 -72.9(5) . . . . ? N8 Co4 N7 C66 11.0(5) . . . . ? Co3 Co4 N7 C66 -1.7(5) . . . . ? O14 Co4 N8 C78 -169.6(14) . . . . ? O13 Co4 N8 C78 79.7(7) . . . . ? O15 Co4 N8 C78 -5.0(7) . . . . ? O16 Co4 N8 C78 -91.3(7) . . . . ? N7 Co4 N8 C78 175.3(7) . . . . ? Co3 Co4 N8 C78 -133.4(11) . . . . ? O14 Co4 N8 C77 3.1(18) . . . . ? O13 Co4 N8 C77 -107.5(5) . . . . ? O15 Co4 N8 C77 167.8(5) . . . . ? O16 Co4 N8 C77 81.5(5) . . . . ? N7 Co4 N8 C77 -11.9(5) . . . . ? Co3 Co4 N8 C77 39.3(6) . . . . ? Co3 O9 C49 C51 -13.5(15) . . . . ? Co3 O9 C49 C50 165.1(6) . . . . ? O9 C49 C51 C52 1.2(19) . . . . ? C50 C49 C51 C52 -177.4(10) . . . . ? Co3 O10 C52 C51 12.3(15) . . . . ? Co3 O10 C52 C53 -167.2(7) . . . . ? C49 C51 C52 O10 -0.3(19) . . . . ? C49 C51 C52 C53 179.2(11) . . . . ? O10 C52 C53 F29 -168.2(9) . . . . ? C51 C52 C53 F29 12.2(16) . . . . ? O10 C52 C53 F31 -48.7(12) . . . . ? C51 C52 C53 F31 131.7(10) . . . . ? O10 C52 C53 F30 68.3(12) . . . . ? C51 C52 C53 F30 -111.3(10) . . . . ? Co3 O11 C54 C56 -2.0(14) . . . . ? Co3 O11 C54 C55 176.7(6) . . . . ? O11 C54 C55 F34 -167.7(9) . . . . ? C56 C54 C55 F34 11.2(16) . . . . ? O11 C54 C55 F32 -44.5(14) . . . . ? C56 C54 C55 F32 134.4(10) . . . . ? O11 C54 C55 F33 65.2(11) . . . . ? C56 C54 C55 F33 -115.9(10) . . . . ? O11 C54 C56 C57 8.4(17) . . . . ? C55 C54 C56 C57 -170.3(10) . . . . ? Co3 O12 C57 C56 -5.2(12) . . . . ? Co3 O12 C57 C58 175.1(6) . . . . ? C54 C56 C57 O12 -4.3(16) . . . . ? C54 C56 C57 C58 175.4(9) . . . . ? O12 C57 C58 F37 -55.9(11) . . . . ? C56 C57 C58 F37 124.3(10) . . . . ? O12 C57 C58 F36 -178.6(8) . . . . ? C56 C57 C58 F36 1.7(14) . . . . ? O12 C57 C58 F35 62.6(10) . . . . ? C56 C57 C58 F35 -117.2(10) . . . . ? C79 N5 C59 C77 -5.1(11) . . . . ? Co3 N5 C59 C77 168.7(6) . . . . ? C79 N5 C59 C60 171.2(7) . . . . ? Co3 N5 C59 C60 -15.0(8) . . . . ? C61 N6 C60 C64 0.7(12) . . . . ? Co3 N6 C60 C64 -172.2(6) . . . . ? C61 N6 C60 C59 -178.8(7) . . . . ? Co3 N6 C60 C59 8.3(8) . . . . ? N5 C59 C60 N6 5.2(10) . . . . ? C77 C59 C60 N6 -178.5(7) . . . . ? N5 C59 C60 C64 -174.4(7) . . . . ? C77 C59 C60 C64 2.0(11) . . . . ? C60 N6 C61 C62 1.0(12) . . . . ? Co3 N6 C61 C62 172.9(6) . . . . ? N6 C61 C62 C63 -0.6(14) . . . . ? C61 C62 C63 C64 -1.5(13) . . . . ? C62 C63 C64 C60 2.9(12) . . . . ? C62 C63 C64 C65 -176.9(8) . . . . ? N6 C60 C64 C63 -2.6(12) . . . . ? C59 C60 C64 C63 176.9(7) . . . . ? N6 C60 C64 C65 177.2(7) . . . . ? C59 C60 C64 C65 -3.3(11) . . . . ? C63 C64 C65 C96 1.8(13) . . . . ? C60 C64 C65 C96 -178.0(8) . . . . ? C63 C64 C65 C66 179.6(8) . . . . ? C60 C64 C65 C66 -0.2(11) . . . . ? C94 N7 C66 C65 0.4(11) . . . . ? Co4 N7 C66 C65 175.3(6) . . . . ? C94 N7 C66 C77 176.8(7) . . . . ? Co4 N7 C66 C77 -8.3(8) . . . . ? C96 C65 C66 N7 -0.8(12) . . . . ? C64 C65 C66 N7 -178.7(7) . . . . ? C96 C65 C66 C77 -177.0(7) . . . . ? C64 C65 C66 C77 5.0(11) . . . . ? Co4 O13 C67 C69 -17(2) . . . . ? Co4 O13 C67 C68 163.7(9) . . . . ? O13 C67 C68 F40 -60.6(16) . . . . ? C69 C67 C68 F40 120.2(14) . . . . ? O13 C67 C68 F39 171.2(11) . . . . ? C69 C67 C68 F39 -8(2) . . . . ? O13 C67 C68 F38 55.0(16) . . . . ? C69 C67 C68 F38 -124.2(14) . . . . ? O13 C67 C69 C70 3(3) . . . . ? C68 C67 C69 C70 -178.0(16) . . . . ? Co4 O14 C70 C69 8(2) . . . . ? Co4 O14 C70 C71 -173.0(10) . . . . ? C67 C69 C70 O14 2(3) . . . . ? C67 C69 C70 C71 -176.8(15) . . . . ? O14 C70 C71 F43 -177.0(14) . . . . ? C69 C70 C71 F43 2(2) . . . . ? O14 C70 C71 F42 50.4(19) . . . . ? C69 C70 C71 F42 -130.3(15) . . . . ? O14 C70 C71 F41 -53.8(18) . . . . ? C69 C70 C71 F41 125.4(15) . . . . ? Co4 O15 C72 C74 17.0(15) . . . . ? Co4 O15 C72 C73 -160.7(7) . . . . ? O15 C72 C73 F46 35.0(14) . . . . ? C74 C72 C73 F46 -143.0(10) . . . . ? O15 C72 C73 F44 159.7(10) . . . . ? C74 C72 C73 F44 -18.4(16) . . . . ? O15 C72 C73 F45 -82.9(11) . . . . ? C74 C72 C73 F45 99.1(11) . . . . ? O15 C72 C74 C75 -2.2(18) . . . . ? C73 C72 C74 C75 175.4(10) . . . . ? Co4 O16 C75 C74 -0.3(13) . . . . ? Co4 O16 C75 C76 177.0(5) . . . . ? C72 C74 C75 O16 -7.4(16) . . . . ? C72 C74 C75 C76 175.4(9) . . . . ? O16 C75 C76 F47 28.2(12) . . . . ? C74 C75 C76 F47 -154.2(9) . . . . ? O16 C75 C76 F49 152.5(8) . . . . ? C74 C75 C76 F49 -29.9(12) . . . . ? O16 C75 C76 F48 -90.8(9) . . . . ? C74 C75 C76 F48 86.8(10) . . . . ? C78 N8 C77 C59 5.8(10) . . . . ? Co4 N8 C77 C59 -168.2(6) . . . . ? C78 N8 C77 C66 -174.5(7) . . . . ? Co4 N8 C77 C66 11.5(8) . . . . ? N5 C59 C77 N8 -1.2(11) . . . . ? C60 C59 C77 N8 -177.5(7) . . . . ? N5 C59 C77 C66 179.0(7) . . . . ? C60 C59 C77 C66 2.8(11) . . . . ? N7 C66 C77 N8 -2.6(10) . . . . ? C65 C66 C77 N8 173.9(7) . . . . ? N7 C66 C77 C59 177.1(7) . . . . ? C65 C66 C77 C59 -6.4(11) . . . . ? C77 N8 C78 C84 175.3(7) . . . . ? Co4 N8 C78 C84 -12.3(11) . . . . ? C77 N8 C78 C79 -4.1(10) . . . . ? Co4 N8 C78 C79 168.3(5) . . . . ? C59 N5 C79 C80 -173.3(7) . . . . ? Co3 N5 C79 C80 14.4(11) . . . . ? C59 N5 C79 C78 6.7(10) . . . . ? Co3 N5 C79 C78 -165.6(5) . . . . ? N8 C78 C79 N5 -2.1(11) . . . . ? C84 C78 C79 N5 178.5(7) . . . . ? N8 C78 C79 C80 177.9(7) . . . . ? C84 C78 C79 C80 -1.5(11) . . . . ? N5 C79 C80 C81 177.9(7) . . . . ? C78 C79 C80 C81 -2.0(11) . . . . ? C79 C80 C81 C83 4.9(11) . . . . ? C79 C80 C81 S7 -175.5(6) . . . . ? C82 S7 C81 C80 -176.7(7) . . . . ? C82 S7 C81 C83 2.9(7) . . . . ? C83 S8 C82 C85 -176.8(7) . . . . ? C83 S8 C82 S7 3.9(5) . . . . ? C81 S7 C82 C85 176.6(7) . . . . ? C81 S7 C82 S8 -4.2(5) . . . . ? C80 C81 C83 C84 -4.3(12) . . . . ? S7 C81 C83 C84 176.0(6) . . . . ? C80 C81 C83 S8 178.9(6) . . . . ? S7 C81 C83 S8 -0.7(8) . . . . ? C82 S8 C83 C84 -178.6(7) . . . . ? C82 S8 C83 C81 -1.9(7) . . . . ? C81 C83 C84 C78 0.7(12) . . . . ? S8 C83 C84 C78 177.3(6) . . . . ? N8 C78 C84 C83 -177.3(7) . . . . ? C79 C78 C84 C83 2.1(11) . . . . ? S8 C82 C85 S11 -1.1(11) . . . . ? S7 C82 C85 S11 178.1(5) . . . . ? S8 C82 C85 S9 -179.2(5) . . . . ? S7 C82 C85 S9 0.0(11) . . . . ? C90 S11 C85 C82 164.0(8) . . . . ? C90 S11 C85 S9 -17.7(5) . . . . ? C86 S9 C85 C82 -164.2(8) . . . . ? C86 S9 C85 S11 17.5(5) . . . . ? C87 S10 C86 C90 160.3(9) . . . . ? C87 S10 C86 S9 -27.8(7) . . . . ? C85 S9 C86 C90 -10.3(8) . . . . ? C85 S9 C86 S10 177.2(5) . . . . ? C86 S10 C87 C88 -66.2(12) . . . . ? S10 C87 C88 C89 -69.9(14) . . . . ? S10 C86 C90 S12 3.9(12) . . . . ? S9 C86 C90 S12 -168.2(5) . . . . ? S10 C86 C90 S11 171.4(5) . . . . ? S9 C86 C90 S11 -0.7(10) . . . . ? C91 S12 C90 C86 -139.4(9) . . . . ? C91 S12 C90 S11 53.1(7) . . . . ? C85 S11 C90 C86 11.4(8) . . . . ? C85 S11 C90 S12 179.7(5) . . . . ? C90 S12 C91 C92 57.6(13) . . . . ? S12 C91 C92 C93 53.9(16) . . . . ? C66 N7 C94 C95 -1.0(12) . . . . ? Co4 N7 C94 C95 -175.1(6) . . . . ? N7 C94 C95 C96 2.0(13) . . . . ? C66 C65 C96 C95 1.9(12) . . . . ? C64 C65 C96 C95 179.7(8) . . . . ? C94 C95 C96 C65 -2.5(13) . . . . ? O9 C49 C50 F28 -82.5(14) . . . . ? C51 C49 C50 F28 96.3(14) . . . . ? O9 C49 C50 F28A 62.8(16) . . . . ? C51 C49 C50 F28A -118.5(14) . . . . ? O9 C49 C50 F26A -151.3(11) . . . . ? C51 C49 C50 F26A 27.4(16) . . . . ? O9 C49 C50 F26 148.1(11) . . . . ? C51 C49 C50 F26 -33.2(15) . . . . ? O9 C49 C50 F27 43.0(14) . . . . ? C51 C49 C50 F27 -138.2(12) . . . . ? O9 C49 C50 F27A -43.2(13) . . . . ? C51 C49 C50 F27A 135.5(12) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.714 _refine_diff_density_min -1.574 _refine_diff_density_rms 0.103 # Attachment 'TTF-PPB.CIF' data_TTF-PPB _database_code_depnum_ccdc_archive 'CCDC 806937' #TrackingRef 'TTF-PPB.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H24 Cl2 N4 S6' _chemical_formula_weight 691.78 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' Cl Cl 0.1484 0.1585 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4996(10) _cell_length_b 9.8334(10) _cell_length_c 16.7952(19) _cell_angle_alpha 78.014(9) _cell_angle_beta 75.026(9) _cell_angle_gamma 89.230(9) _cell_volume 1481.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12374 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 29.50 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.672 _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 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28698 _diffrn_reflns_av_R_equivalents 0.1260 _diffrn_reflns_av_sigmaI/netI 0.1124 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 29.25 _reflns_number_total 8000 _reflns_number_gt 4706 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^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 8000 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0926 _refine_ls_wR_factor_gt 0.0852 _refine_ls_goodness_of_fit_ref 0.798 _refine_ls_restrained_S_all 0.798 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6239(3) 0.2747(3) 0.38665(16) 0.0335(6) Uani 1 1 d . . . H1A H 0.5587 0.1946 0.4215 0.040 Uiso 1 1 calc R . . H1B H 0.7246 0.2539 0.3903 0.040 Uiso 1 1 calc R . . C2 C 0.1606(2) 0.3766(2) 0.20801(13) 0.0200(4) Uani 1 1 d . . . C3 C 0.2970(3) 0.2119(2) 0.11354(14) 0.0227(5) Uani 1 1 d . . . C4 C 0.5890(3) 0.1415(3) 0.09234(18) 0.0395(7) Uani 1 1 d . . . H4A H 0.5713 0.1524 0.1514 0.047 Uiso 1 1 calc R . . H4B H 0.6573 0.0654 0.0850 0.047 Uiso 1 1 calc R . . C5 C 0.6622(3) 0.2738(3) 0.0351(2) 0.0533(9) Uani 1 1 d . . . H5A H 0.7480 0.2974 0.0536 0.064 Uiso 1 1 calc R . . H5B H 0.5937 0.3500 0.0411 0.064 Uiso 1 1 calc R . . C6 C 0.7115(4) 0.2662(4) -0.0570(2) 0.0660(10) Uani 1 1 d . . . H6A H 0.7798 0.1912 -0.0637 0.099 Uiso 1 1 calc R . . H6B H 0.7601 0.3549 -0.0901 0.099 Uiso 1 1 calc R . . H6C H 0.6267 0.2475 -0.0767 0.099 Uiso 1 1 calc R . . C7 C 0.1712(3) 0.2352(2) 0.09179(14) 0.0232(5) Uani 1 1 d . . . C8 C 0.1041(3) 0.3140(3) -0.05880(15) 0.0336(6) Uani 1 1 d . . . H8A H 0.0645 0.2867 -0.1025 0.040 Uiso 1 1 calc R . . H8B H 0.0350 0.3776 -0.0318 0.040 Uiso 1 1 calc R . . C9 C 0.2480(3) 0.3919(3) -0.10106(17) 0.0384(6) Uani 1 1 d . . . H9A H 0.2927 0.4113 -0.0573 0.046 Uiso 1 1 calc R . . H9B H 0.2307 0.4823 -0.1353 0.046 Uiso 1 1 calc R . . C10 C 0.3542(4) 0.3126(4) -0.1577(2) 0.0661(10) Uani 1 1 d . . . H10A H 0.3769 0.2257 -0.1236 0.099 Uiso 1 1 calc R . . H10B H 0.4441 0.3698 -0.1853 0.099 Uiso 1 1 calc R . . H10C H 0.3099 0.2914 -0.2005 0.099 Uiso 1 1 calc R . . C11 C 0.1202(2) 0.4562(2) 0.26547(13) 0.0197(4) Uani 1 1 d . . . C12 C -0.0328(2) 0.6036(2) 0.36632(13) 0.0179(4) Uani 1 1 d . . . C13 C 0.1034(2) 0.5876(2) 0.38748(13) 0.0171(4) Uani 1 1 d . . . C14 C 0.1301(2) 0.6452(2) 0.44983(13) 0.0178(4) Uani 1 1 d . . . H14A H 0.2200 0.6316 0.4646 0.021 Uiso 1 1 calc R . . C15 C 0.0223(2) 0.7254(2) 0.49221(12) 0.0168(4) Uani 1 1 d . . . C16 C -0.0522(2) 0.8646(2) 0.58721(13) 0.0175(4) Uani 1 1 d . . . C17 C -0.1855(2) 0.8847(2) 0.56318(13) 0.0176(4) Uani 1 1 d . . . C18 C -0.1132(2) 0.7420(2) 0.47016(13) 0.0172(4) Uani 1 1 d . . . C19 C -0.1398(2) 0.6773(2) 0.40765(13) 0.0189(4) Uani 1 1 d . . . H19A H -0.2313 0.6850 0.3944 0.023 Uiso 1 1 calc R . . C20 C -0.2928(2) 0.9785(2) 0.59974(13) 0.0190(4) Uani 1 1 d . . . C21 C -0.5084(3) 1.0850(3) 0.60010(15) 0.0276(5) Uani 1 1 d . . . H21A H -0.5917 1.1009 0.5785 0.033 Uiso 1 1 calc R . . C22 C -0.4945(3) 1.1522(3) 0.66324(15) 0.0287(5) Uani 1 1 d . . . H22A H -0.5671 1.2127 0.6840 0.034 Uiso 1 1 calc R . . C23 C -0.3754(3) 1.1300(3) 0.69491(14) 0.0265(5) Uani 1 1 d . . . H23A H -0.3656 1.1741 0.7385 0.032 Uiso 1 1 calc R . . C24 C -0.2674(2) 1.0418(2) 0.66285(13) 0.0191(4) Uani 1 1 d . . . C25 C -0.1331(2) 1.0188(2) 0.68965(13) 0.0199(4) Uani 1 1 d . . . C26 C -0.0261(2) 0.9335(2) 0.65204(13) 0.0186(4) Uani 1 1 d . . . C27 C 0.1264(3) 0.9729(3) 0.73100(15) 0.0276(5) Uani 1 1 d . . . H27A H 0.2168 0.9585 0.7452 0.033 Uiso 1 1 calc R . . C28 C 0.0269(3) 1.0572(3) 0.77299(15) 0.0275(5) Uani 1 1 d . . . H28A H 0.0484 1.0974 0.8155 0.033 Uiso 1 1 calc R . . C29 C -0.1022(3) 1.0804(2) 0.75152(14) 0.0245(5) Uani 1 1 d . . . H29A H -0.1709 1.1384 0.7786 0.029 Uiso 1 1 calc R . . Cl1 Cl 0.61615(8) 0.29782(8) 0.28057(4) 0.04426(18) Uani 1 1 d . . . Cl2 Cl 0.57044(8) 0.42531(8) 0.42589(5) 0.0479(2) Uani 1 1 d . . . N1 N 0.05084(19) 0.78561(19) 0.55193(11) 0.0186(4) Uani 1 1 d . . . N2 N -0.21647(19) 0.82254(19) 0.50637(11) 0.0182(4) Uani 1 1 d . . . N3 N -0.4098(2) 0.9999(2) 0.56906(12) 0.0233(4) Uani 1 1 d . . . N4 N 0.1012(2) 0.9119(2) 0.67222(12) 0.0244(4) Uani 1 1 d . . . S1 S 0.05035(7) 0.34564(7) 0.14401(4) 0.02660(14) Uani 1 1 d . . . S2 S 0.32843(6) 0.29492(6) 0.19091(4) 0.02481(13) Uani 1 1 d . . . S3 S 0.41854(7) 0.08923(7) 0.07664(4) 0.02926(15) Uani 1 1 d . . . S4 S 0.11233(7) 0.15863(7) 0.02058(4) 0.03021(15) Uani 1 1 d . . . S5 S -0.05192(6) 0.52911(7) 0.28376(4) 0.02550(14) Uani 1 1 d . . . S6 S 0.23218(6) 0.49364(6) 0.32736(3) 0.02210(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0378(15) 0.0332(15) 0.0376(14) -0.0133(12) -0.0195(12) 0.0067(12) C2 0.0212(11) 0.0196(11) 0.0198(10) -0.0064(9) -0.0046(8) 0.0039(9) C3 0.0289(12) 0.0179(12) 0.0215(11) -0.0089(9) -0.0032(9) 0.0032(9) C4 0.0302(14) 0.0463(18) 0.0502(16) -0.0253(14) -0.0135(12) 0.0157(12) C5 0.0327(16) 0.0471(19) 0.085(2) -0.0380(18) -0.0054(16) -0.0017(14) C6 0.063(2) 0.054(2) 0.067(2) -0.0055(19) 0.0055(19) -0.0177(18) C7 0.0294(12) 0.0196(12) 0.0208(11) -0.0066(9) -0.0053(9) 0.0026(9) C8 0.0397(15) 0.0404(16) 0.0267(12) -0.0130(11) -0.0152(11) 0.0120(12) C9 0.0496(17) 0.0340(15) 0.0302(13) -0.0044(11) -0.0101(12) 0.0076(13) C10 0.061(2) 0.070(3) 0.053(2) -0.0119(19) 0.0067(17) 0.0207(19) C11 0.0206(11) 0.0209(11) 0.0183(10) -0.0045(9) -0.0063(8) 0.0043(9) C12 0.0207(11) 0.0165(11) 0.0178(10) -0.0051(8) -0.0062(8) 0.0043(8) C13 0.0183(10) 0.0156(11) 0.0167(9) -0.0029(8) -0.0039(8) 0.0042(8) C14 0.0165(10) 0.0186(11) 0.0199(10) -0.0049(9) -0.0069(8) 0.0027(8) C15 0.0191(10) 0.0153(11) 0.0151(9) -0.0028(8) -0.0033(8) 0.0017(8) C16 0.0202(11) 0.0146(11) 0.0178(10) -0.0043(8) -0.0045(8) 0.0014(8) C17 0.0203(11) 0.0151(11) 0.0170(9) -0.0038(8) -0.0040(8) 0.0031(8) C18 0.0187(10) 0.0151(11) 0.0172(9) -0.0037(8) -0.0035(8) 0.0041(8) C19 0.0195(11) 0.0203(11) 0.0199(10) -0.0079(9) -0.0077(8) 0.0055(9) C20 0.0199(11) 0.0173(11) 0.0187(10) -0.0041(9) -0.0031(8) 0.0035(9) C21 0.0224(12) 0.0321(14) 0.0297(12) -0.0104(10) -0.0063(10) 0.0102(10) C22 0.0256(12) 0.0304(14) 0.0314(12) -0.0134(11) -0.0047(10) 0.0117(10) C23 0.0308(13) 0.0261(13) 0.0251(11) -0.0123(10) -0.0063(10) 0.0050(10) C24 0.0210(11) 0.0154(11) 0.0187(10) -0.0034(8) -0.0016(8) 0.0007(8) C25 0.0236(11) 0.0163(11) 0.0189(10) -0.0041(8) -0.0036(8) -0.0011(9) C26 0.0206(11) 0.0170(11) 0.0186(10) -0.0031(8) -0.0065(8) 0.0015(9) C27 0.0291(13) 0.0294(13) 0.0298(12) -0.0095(10) -0.0150(10) 0.0024(10) C28 0.0354(14) 0.0253(13) 0.0263(12) -0.0110(10) -0.0119(10) -0.0003(10) C29 0.0292(12) 0.0224(12) 0.0234(11) -0.0103(10) -0.0052(9) 0.0018(10) Cl1 0.0498(4) 0.0523(5) 0.0378(4) -0.0119(3) -0.0226(3) 0.0111(3) Cl2 0.0449(4) 0.0449(4) 0.0655(5) -0.0324(4) -0.0191(4) 0.0118(3) N1 0.0189(9) 0.0191(10) 0.0181(8) -0.0054(7) -0.0047(7) 0.0032(7) N2 0.0185(9) 0.0184(10) 0.0190(8) -0.0065(7) -0.0054(7) 0.0050(7) N3 0.0209(10) 0.0237(11) 0.0266(10) -0.0089(8) -0.0056(8) 0.0072(8) N4 0.0264(10) 0.0250(11) 0.0273(10) -0.0103(8) -0.0132(8) 0.0045(8) S1 0.0278(3) 0.0313(3) 0.0267(3) -0.0144(3) -0.0116(2) 0.0101(3) S2 0.0232(3) 0.0282(3) 0.0277(3) -0.0147(2) -0.0082(2) 0.0079(2) S3 0.0291(3) 0.0238(3) 0.0359(3) -0.0155(3) -0.0033(3) 0.0067(3) S4 0.0408(4) 0.0269(3) 0.0291(3) -0.0132(3) -0.0143(3) 0.0025(3) S5 0.0254(3) 0.0333(3) 0.0264(3) -0.0177(3) -0.0134(2) 0.0127(2) S6 0.0194(3) 0.0267(3) 0.0235(3) -0.0125(2) -0.0062(2) 0.0077(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 Cl2 1.760(3) . ? C1 Cl1 1.769(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C11 1.344(3) . ? C2 S1 1.753(2) . ? C2 S2 1.759(2) . ? C3 C7 1.341(3) . ? C3 S3 1.754(2) . ? C3 S2 1.758(2) . ? C4 C5 1.503(4) . ? C4 S3 1.804(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.513(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 S4 1.744(2) . ? C7 S1 1.763(2) . ? C8 C9 1.503(4) . ? C8 S4 1.823(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.524(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 S5 1.756(2) . ? C11 S6 1.757(2) . ? C12 C19 1.366(3) . ? C12 C13 1.426(3) . ? C12 S5 1.746(2) . ? C13 C14 1.367(3) . ? C13 S6 1.758(2) . ? C14 C15 1.418(3) . ? C14 H14A 0.9500 . ? C15 N1 1.350(3) . ? C15 C18 1.428(3) . ? C16 N1 1.335(3) . ? C16 C17 1.425(3) . ? C16 C26 1.469(3) . ? C17 N2 1.328(3) . ? C17 C20 1.467(3) . ? C18 N2 1.353(3) . ? C18 C19 1.410(3) . ? C19 H19A 0.9500 . ? C20 N3 1.338(3) . ? C20 C24 1.407(3) . ? C21 N3 1.326(3) . ? C21 C22 1.394(3) . ? C21 H21A 0.9500 . ? C22 C23 1.366(3) . ? C22 H22A 0.9500 . ? C23 C24 1.407(3) . ? C23 H23A 0.9500 . ? C24 C25 1.459(3) . ? C25 C29 1.399(3) . ? C25 C26 1.414(3) . ? C26 N4 1.341(3) . ? C27 N4 1.328(3) . ? C27 C28 1.399(3) . ? C27 H27A 0.9500 . ? C28 C29 1.368(3) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 C1 Cl1 110.65(15) . . ? Cl2 C1 H1A 109.5 . . ? Cl1 C1 H1A 109.5 . . ? Cl2 C1 H1B 109.5 . . ? Cl1 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? C11 C2 S1 122.74(17) . . ? C11 C2 S2 122.75(17) . . ? S1 C2 S2 114.51(12) . . ? C7 C3 S3 122.48(17) . . ? C7 C3 S2 117.42(16) . . ? S3 C3 S2 119.72(14) . . ? C5 C4 S3 116.0(2) . . ? C5 C4 H4A 108.3 . . ? S3 C4 H4A 108.3 . . ? C5 C4 H4B 108.3 . . ? S3 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? C4 C5 C6 114.0(3) . . ? C4 C5 H5A 108.7 . . ? C6 C5 H5A 108.7 . . ? C4 C5 H5B 108.7 . . ? C6 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 S4 125.73(17) . . ? C3 C7 S1 117.10(17) . . ? S4 C7 S1 117.07(13) . . ? C9 C8 S4 114.65(18) . . ? C9 C8 H8A 108.6 . . ? S4 C8 H8A 108.6 . . ? C9 C8 H8B 108.6 . . ? S4 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C8 C9 C10 113.0(3) . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 S5 121.13(17) . . ? C2 C11 S6 123.32(17) . . ? S5 C11 S6 115.55(12) . . ? C19 C12 C13 120.83(19) . . ? C19 C12 S5 122.56(16) . . ? C13 C12 S5 116.58(15) . . ? C14 C13 C12 120.91(18) . . ? C14 C13 S6 123.30(16) . . ? C12 C13 S6 115.78(15) . . ? C13 C14 C15 119.41(19) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? N1 C15 C14 119.24(19) . . ? N1 C15 C18 121.41(18) . . ? C14 C15 C18 119.35(18) . . ? N1 C16 C17 121.91(19) . . ? N1 C16 C26 118.81(19) . . ? C17 C16 C26 119.28(18) . . ? N2 C17 C16 121.93(18) . . ? N2 C17 C20 117.57(19) . . ? C16 C17 C20 120.49(18) . . ? N2 C18 C19 118.68(19) . . ? N2 C18 C15 121.26(18) . . ? C19 C18 C15 120.03(18) . . ? C12 C19 C18 119.41(19) . . ? C12 C19 H19A 120.3 . . ? C18 C19 H19A 120.3 . . ? N3 C20 C24 123.90(19) . . ? N3 C20 C17 116.67(19) . . ? C24 C20 C17 119.43(19) . . ? N3 C21 C22 122.4(2) . . ? N3 C21 H21A 118.8 . . ? C22 C21 H21A 118.8 . . ? C23 C22 C21 119.3(2) . . ? C23 C22 H22A 120.3 . . ? C21 C22 H22A 120.3 . . ? C22 C23 C24 119.9(2) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C20 C24 C23 116.1(2) . . ? C20 C24 C25 120.46(19) . . ? C23 C24 C25 123.4(2) . . ? C29 C25 C26 116.9(2) . . ? C29 C25 C24 122.6(2) . . ? C26 C25 C24 120.46(18) . . ? N4 C26 C25 123.17(19) . . ? N4 C26 C16 117.07(18) . . ? C25 C26 C16 119.76(19) . . ? N4 C27 C28 123.4(2) . . ? N4 C27 H27A 118.3 . . ? C28 C27 H27A 118.3 . . ? C29 C28 C27 118.5(2) . . ? C29 C28 H28A 120.7 . . ? C27 C28 H28A 120.7 . . ? C28 C29 C25 120.1(2) . . ? C28 C29 H29A 120.0 . . ? C25 C29 H29A 120.0 . . ? C16 N1 C15 116.61(18) . . ? C17 N2 C18 116.82(18) . . ? C21 N3 C20 118.31(19) . . ? C27 N4 C26 117.96(19) . . ? C2 S1 C7 95.53(10) . . ? C3 S2 C2 95.41(10) . . ? C3 S3 C4 103.79(12) . . ? C7 S4 C8 99.46(11) . . ? C12 S5 C11 96.02(10) . . ? C11 S6 C13 95.97(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 S3 C4 C5 C6 -64.7(3) . . . . ? S3 C3 C7 S4 -4.0(3) . . . . ? S2 C3 C7 S4 -176.85(14) . . . . ? S3 C3 C7 S1 172.35(13) . . . . ? S2 C3 C7 S1 -0.5(3) . . . . ? S4 C8 C9 C10 68.6(3) . . . . ? S1 C2 C11 S5 3.0(3) . . . . ? S2 C2 C11 S5 -177.01(13) . . . . ? S1 C2 C11 S6 -177.54(13) . . . . ? S2 C2 C11 S6 2.5(3) . . . . ? C19 C12 C13 C14 0.3(3) . . . . ? S5 C12 C13 C14 178.40(17) . . . . ? C19 C12 C13 S6 -178.56(17) . . . . ? S5 C12 C13 S6 -0.4(2) . . . . ? C12 C13 C14 C15 -1.9(3) . . . . ? S6 C13 C14 C15 176.81(16) . . . . ? C13 C14 C15 N1 -178.0(2) . . . . ? C13 C14 C15 C18 1.3(3) . . . . ? N1 C16 C17 N2 2.2(3) . . . . ? C26 C16 C17 N2 -178.4(2) . . . . ? N1 C16 C17 C20 -176.5(2) . . . . ? C26 C16 C17 C20 2.9(3) . . . . ? N1 C15 C18 N2 2.2(3) . . . . ? C14 C15 C18 N2 -177.06(19) . . . . ? N1 C15 C18 C19 -179.8(2) . . . . ? C14 C15 C18 C19 0.9(3) . . . . ? C13 C12 C19 C18 2.0(3) . . . . ? S5 C12 C19 C18 -176.03(17) . . . . ? N2 C18 C19 C12 175.5(2) . . . . ? C15 C18 C19 C12 -2.5(3) . . . . ? N2 C17 C20 N3 -3.7(3) . . . . ? C16 C17 C20 N3 175.0(2) . . . . ? N2 C17 C20 C24 177.21(19) . . . . ? C16 C17 C20 C24 -4.0(3) . . . . ? N3 C21 C22 C23 -0.1(4) . . . . ? C21 C22 C23 C24 0.9(4) . . . . ? N3 C20 C24 C23 1.2(3) . . . . ? C17 C20 C24 C23 -179.9(2) . . . . ? N3 C20 C24 C25 -176.7(2) . . . . ? C17 C20 C24 C25 2.3(3) . . . . ? C22 C23 C24 C20 -1.4(3) . . . . ? C22 C23 C24 C25 176.4(2) . . . . ? C20 C24 C25 C29 179.3(2) . . . . ? C23 C24 C25 C29 1.7(4) . . . . ? C20 C24 C25 C26 0.5(3) . . . . ? C23 C24 C25 C26 -177.1(2) . . . . ? C29 C25 C26 N4 -0.9(3) . . . . ? C24 C25 C26 N4 177.9(2) . . . . ? C29 C25 C26 C16 179.4(2) . . . . ? C24 C25 C26 C16 -1.7(3) . . . . ? N1 C16 C26 N4 -0.3(3) . . . . ? C17 C16 C26 N4 -179.7(2) . . . . ? N1 C16 C26 C25 179.4(2) . . . . ? C17 C16 C26 C25 0.0(3) . . . . ? N4 C27 C28 C29 -1.3(4) . . . . ? C27 C28 C29 C25 0.9(4) . . . . ? C26 C25 C29 C28 0.1(3) . . . . ? C24 C25 C29 C28 -178.7(2) . . . . ? C17 C16 N1 C15 -0.1(3) . . . . ? C26 C16 N1 C15 -179.48(19) . . . . ? C14 C15 N1 C16 177.29(19) . . . . ? C18 C15 N1 C16 -2.0(3) . . . . ? C16 C17 N2 C18 -2.0(3) . . . . ? C20 C17 N2 C18 176.76(19) . . . . ? C19 C18 N2 C17 -178.1(2) . . . . ? C15 C18 N2 C17 -0.1(3) . . . . ? C22 C21 N3 C20 -0.2(4) . . . . ? C24 C20 N3 C21 -0.4(3) . . . . ? C17 C20 N3 C21 -179.4(2) . . . . ? C28 C27 N4 C26 0.5(4) . . . . ? C25 C26 N4 C27 0.7(3) . . . . ? C16 C26 N4 C27 -179.7(2) . . . . ? C11 C2 S1 C7 -178.5(2) . . . . ? S2 C2 S1 C7 1.45(15) . . . . ? C3 C7 S1 C2 -0.6(2) . . . . ? S4 C7 S1 C2 176.07(14) . . . . ? C7 C3 S2 C2 1.3(2) . . . . ? S3 C3 S2 C2 -171.75(14) . . . . ? C11 C2 S2 C3 178.3(2) . . . . ? S1 C2 S2 C3 -1.67(15) . . . . ? C7 C3 S3 C4 160.5(2) . . . . ? S2 C3 S3 C4 -26.82(18) . . . . ? C5 C4 S3 C3 -70.7(2) . . . . ? C3 C7 S4 C8 -117.8(2) . . . . ? S1 C7 S4 C8 65.93(16) . . . . ? C9 C8 S4 C7 62.3(2) . . . . ? C19 C12 S5 C11 -179.7(2) . . . . ? C13 C12 S5 C11 2.19(19) . . . . ? C2 C11 S5 C12 176.27(19) . . . . ? S6 C11 S5 C12 -3.26(15) . . . . ? C2 C11 S6 C13 -176.44(19) . . . . ? S5 C11 S6 C13 3.08(14) . . . . ? C14 C13 S6 C11 179.63(19) . . . . ? C12 C13 S6 C11 -1.58(18) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.25 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.264 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.082