Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Shie-Ming Peng' _publ_contact_author_address ; Department of Chemistry National Taiwan University No.1, Sec. 4, Roosevelt Road Taipei 106 TAIWAN ; _publ_contact_author_email SMPENG@NTU.EDU.TW _publ_section_title ; Novel linear hexanuclear cobalt string complexes (Co612+) and one-electron reduction products (Co611+) supported by four bpyany2- ligands ; loop_ _publ_author_name 'Shie-Ming Peng.' 'Jung-Che Chang.' 'Chih-Hsien Chien.' 'Jim-Min Fang.' ; Gene-Hsiang Lee ; 'Chen-Yu Yeh.' # Attachment 'Co6-revised-2006-0112.cif' data_ic11346(compd_1) _database_code_depnum_ccdc_archive 'CCDC 283614' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co6(bpyany)(NCS)2)(PF6) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H62 Cl12 Co6 F6 N26 O P S2' _chemical_formula_weight 2391.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 27.3324(4) _cell_length_b 12.9324(2) _cell_length_c 25.6423(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9063.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4796 _exptl_absorpt_coefficient_mu 1.566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.510 _exptl_absorpt_correction_T_max 0.836 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60692 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.50 _reflns_number_total 18376 _reflns_number_gt 14475 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1404P)^2^+13.8102P] 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 SHELXL _refine_ls_extinction_coef 0.00157(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.283(19) _refine_ls_number_reflns 18376 _refine_ls_number_parameters 1188 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.2117 _refine_ls_wR_factor_gt 0.1943 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.027 _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 0.60663(3) -0.05729(8) 0.61193(4) 0.0255(2) Uani 1 1 d . . . Co2 Co 0.61009(3) 0.06387(8) 0.67823(4) 0.0216(2) Uani 1 1 d . . . Co3 Co 0.61386(3) 0.18519(8) 0.74227(4) 0.0189(2) Uani 1 1 d . . . Co4 Co 0.61763(3) 0.30561(8) 0.80577(4) 0.0194(2) Uani 1 1 d . . . Co5 Co 0.62132(3) 0.42674(8) 0.86986(4) 0.0226(2) Uani 1 1 d . . . Co6 Co 0.62702(3) 0.54995(8) 0.93496(4) 0.0269(2) Uani 1 1 d . . . S1 S 0.61967(18) -0.2745(4) 0.4587(2) 0.0772(12) Uiso 0.70 1 d P A 1 S1' S 0.6280(5) -0.3198(10) 0.4833(6) 0.082(3) Uiso 0.30 1 d P A 2 S2 S 0.66377(10) 0.83672(19) 1.04645(12) 0.0572(6) Uani 1 1 d . . . N1 N 0.5539(2) 0.0283(5) 0.5816(2) 0.0272(13) Uani 1 1 d . . . N2 N 0.5798(2) 0.1633(4) 0.6335(2) 0.0243(12) Uani 1 1 d . . . N3 N 0.6028(2) 0.2904(4) 0.6905(2) 0.0219(12) Uani 1 1 d . . . N4 N 0.62422(19) 0.4125(4) 0.7534(2) 0.0198(11) Uani 1 1 d . . . N5 N 0.6466(2) 0.5210(4) 0.8194(2) 0.0254(12) Uani 1 1 d . . . N6 N 0.6762(2) 0.6188(4) 0.8882(2) 0.0240(12) Uani 1 1 d . . . N7 N 0.6557(2) 0.0310(5) 0.5756(2) 0.0255(12) Uani 1 1 d . . . N8 N 0.67283(19) 0.1079(4) 0.6545(2) 0.0233(12) Uani 1 1 d . . . N9 N 0.68355(19) 0.1985(4) 0.7315(2) 0.0223(12) Uani 1 1 d . . . N10 N 0.68859(19) 0.2920(4) 0.8082(2) 0.0232(11) Uani 1 1 d . . . N11 N 0.6876(2) 0.3820(5) 0.8851(2) 0.0263(12) Uani 1 1 d . . . N12 N 0.6793(2) 0.4655(5) 0.9643(2) 0.0306(14) Uani 1 1 d . . . N13 N 0.6591(2) -0.1299(5) 0.6509(3) 0.0291(13) Uani 1 1 d . . . N14 N 0.6414(2) -0.0316(4) 0.7255(2) 0.0253(12) Uani 1 1 d . . . N15 N 0.62652(19) 0.0791(5) 0.7929(2) 0.0221(12) Uani 1 1 d . . . N16 N 0.6124(2) 0.1992(5) 0.8584(2) 0.0239(13) Uani 1 1 d . . . N17 N 0.5973(2) 0.3273(5) 0.9188(2) 0.0248(12) Uani 1 1 d . . . N18 N 0.5792(2) 0.4643(5) 0.9734(3) 0.0351(15) Uani 1 1 d . . . N19 N 0.5573(2) -0.1284(5) 0.6556(3) 0.0297(13) Uani 1 1 d . . . N20 N 0.5471(2) 0.0229(4) 0.7031(2) 0.0259(12) Uani 1 1 d . . . N21 N 0.54420(19) 0.1722(4) 0.7525(2) 0.0209(12) Uani 1 1 d . . . N22 N 0.54733(19) 0.3193(4) 0.8047(2) 0.0230(12) Uani 1 1 d . . . N23 N 0.5560(2) 0.4683(5) 0.8530(2) 0.0271(13) Uani 1 1 d . . . N24 N 0.5722(2) 0.6193(5) 0.8987(2) 0.0278(13) Uani 1 1 d . . . N25 N 0.6055(2) -0.1654(5) 0.5522(3) 0.0356(15) Uani 1 1 d . A . N26 N 0.6333(3) 0.6623(5) 0.9919(3) 0.0401(16) Uani 1 1 d . . . C1 C 0.5219(3) -0.0128(6) 0.5457(3) 0.0379(18) Uani 1 1 d . . . H1A H 0.5265 -0.0822 0.5346 0.045 Uiso 1 1 calc R . . C2 C 0.4841(3) 0.0418(7) 0.5256(4) 0.044(2) Uani 1 1 d . . . H2A H 0.4626 0.0105 0.5011 0.052 Uiso 1 1 calc R . . C3 C 0.4768(3) 0.1425(7) 0.5407(4) 0.042(2) Uani 1 1 d . . . H3A H 0.4508 0.1820 0.5264 0.050 Uiso 1 1 calc R . . C4 C 0.5077(3) 0.1847(7) 0.5766(3) 0.0369(18) Uani 1 1 d . . . H4A H 0.5021 0.2530 0.5888 0.044 Uiso 1 1 calc R . . C5 C 0.5481(2) 0.1282(5) 0.5957(3) 0.0252(14) Uani 1 1 d . . . C6 C 0.5891(2) 0.2657(5) 0.6418(3) 0.0258(14) Uani 1 1 d . . . C7 C 0.5898(3) 0.3402(6) 0.6003(3) 0.0279(15) Uani 1 1 d . . . H7A H 0.5811 0.3209 0.5658 0.034 Uiso 1 1 calc R . . C8 C 0.6033(3) 0.4406(5) 0.6119(3) 0.0284(15) Uani 1 1 d . . . H8A H 0.6050 0.4904 0.5847 0.034 Uiso 1 1 calc R . . C9 C 0.6143(2) 0.4694(5) 0.6626(3) 0.0244(15) Uani 1 1 d . . . C10 C 0.6136(2) 0.3912(6) 0.7019(3) 0.0240(15) Uani 1 1 d . . . C11 C 0.6286(3) 0.5682(5) 0.6787(3) 0.0273(15) Uani 1 1 d . . . H11A H 0.6306 0.6221 0.6536 0.033 Uiso 1 1 calc R . . C12 C 0.6401(2) 0.5898(5) 0.7300(3) 0.0275(15) Uani 1 1 d . . . H12A H 0.6488 0.6580 0.7402 0.033 Uiso 1 1 calc R . . C13 C 0.6385(2) 0.5092(5) 0.7673(3) 0.0250(14) Uani 1 1 d . . . C14 C 0.6818(2) 0.5918(5) 0.8372(3) 0.0237(14) Uani 1 1 d . . . C15 C 0.7221(3) 0.6238(6) 0.8087(3) 0.0341(17) Uani 1 1 d . . . H15A H 0.7260 0.6005 0.7738 0.041 Uiso 1 1 calc R . . C16 C 0.7561(3) 0.6876(6) 0.8295(4) 0.0401(19) Uani 1 1 d . . . H16A H 0.7837 0.7093 0.8099 0.048 Uiso 1 1 calc R . . C17 C 0.7493(3) 0.7210(7) 0.8816(3) 0.0390(19) Uani 1 1 d . . . H17A H 0.7714 0.7683 0.8974 0.047 Uiso 1 1 calc R . . C18 C 0.7097(3) 0.6832(5) 0.9090(3) 0.0317(16) Uani 1 1 d . . . H18A H 0.7059 0.7036 0.9443 0.038 Uiso 1 1 calc R . . C19 C 0.6595(3) 0.0277(6) 0.5231(3) 0.0358(17) Uani 1 1 d . . . H19A H 0.6402 -0.0210 0.5044 0.043 Uiso 1 1 calc R . . C20 C 0.6900(3) 0.0919(6) 0.4958(3) 0.0401(19) Uani 1 1 d . . . H20A H 0.6936 0.0849 0.4591 0.048 Uiso 1 1 calc R . . C21 C 0.7152(3) 0.1661(7) 0.5225(3) 0.0414(19) Uani 1 1 d . . . H21A H 0.7350 0.2139 0.5039 0.050 Uiso 1 1 calc R . . C22 C 0.7123(3) 0.1728(6) 0.5751(3) 0.0345(17) Uani 1 1 d . . . H22A H 0.7303 0.2241 0.5934 0.041 Uiso 1 1 calc R . . C23 C 0.6820(2) 0.1017(5) 0.6023(3) 0.0270(15) Uani 1 1 d . . . C24 C 0.7043(2) 0.1526(5) 0.6899(3) 0.0261(14) Uani 1 1 d . . . C25 C 0.7561(3) 0.1479(7) 0.6844(3) 0.0359(18) Uani 1 1 d . . . H25A H 0.7704 0.1153 0.6549 0.043 Uiso 1 1 calc R . . C26 C 0.7848(3) 0.1909(7) 0.7221(4) 0.040(2) Uani 1 1 d . . . H26A H 0.8194 0.1848 0.7195 0.048 Uiso 1 1 calc R . . C27 C 0.7643(3) 0.2441(7) 0.7649(3) 0.0334(17) Uani 1 1 d . . . C28 C 0.7123(2) 0.2449(5) 0.7684(3) 0.0222(13) Uani 1 1 d . . . C29 C 0.7897(2) 0.2928(7) 0.8044(3) 0.0398(19) Uani 1 1 d . . . H29A H 0.8244 0.2941 0.8035 0.048 Uiso 1 1 calc R . . C30 C 0.7655(3) 0.3393(6) 0.8449(3) 0.0341(17) Uani 1 1 d . . . H30A H 0.7834 0.3739 0.8714 0.041 Uiso 1 1 calc R . . C31 C 0.7141(2) 0.3357(5) 0.8473(3) 0.0261(14) Uani 1 1 d . . . C32 C 0.7033(2) 0.3921(6) 0.9354(3) 0.0307(16) Uani 1 1 d . . . C33 C 0.7378(3) 0.3268(6) 0.9585(3) 0.0359(18) Uani 1 1 d . . . H33A H 0.7535 0.2747 0.9384 0.043 Uiso 1 1 calc R . . C34 C 0.7489(3) 0.3379(7) 1.0099(3) 0.043(2) Uani 1 1 d . . . H34A H 0.7727 0.2941 1.0256 0.052 Uiso 1 1 calc R . . C35 C 0.7258(3) 0.4126(7) 1.0393(3) 0.042(2) Uani 1 1 d . . . H35A H 0.7341 0.4224 1.0750 0.051 Uiso 1 1 calc R . . C36 C 0.6915(3) 0.4710(6) 1.0167(3) 0.0364(18) Uani 1 1 d . . . H36A H 0.6744 0.5193 1.0378 0.044 Uiso 1 1 calc R . . C37 C 0.6876(3) -0.2024(5) 0.6276(3) 0.0290(15) Uani 1 1 d . . . H37A H 0.6786 -0.2243 0.5936 0.035 Uiso 1 1 calc R . . C38 C 0.7278(3) -0.2457(6) 0.6492(3) 0.0362(18) Uani 1 1 d . . . H38A H 0.7459 -0.2968 0.6308 0.043 Uiso 1 1 calc R . . C39 C 0.7419(3) -0.2144(7) 0.6978(4) 0.041(2) Uani 1 1 d . . . H39A H 0.7706 -0.2426 0.7131 0.050 Uiso 1 1 calc R . . C40 C 0.7146(3) -0.1419(5) 0.7247(3) 0.0312(16) Uani 1 1 d . . . H40A H 0.7248 -0.1184 0.7581 0.037 Uiso 1 1 calc R . . C41 C 0.6711(2) -0.1034(6) 0.7017(3) 0.0266(14) Uani 1 1 d . . . C42 C 0.6387(3) -0.0167(5) 0.7766(3) 0.0265(14) Uani 1 1 d . . . C43 C 0.6454(3) -0.0983(6) 0.8153(3) 0.0315(16) Uani 1 1 d . . . H43A H 0.6547 -0.1657 0.8044 0.038 Uiso 1 1 calc R . . C44 C 0.6388(3) -0.0793(6) 0.8652(3) 0.0353(18) Uani 1 1 d . . . H44A H 0.6414 -0.1344 0.8895 0.042 Uiso 1 1 calc R . . C45 C 0.6278(3) 0.0212(6) 0.8834(3) 0.0300(16) Uani 1 1 d . . . C46 C 0.6217(2) 0.0985(6) 0.8463(3) 0.0234(14) Uani 1 1 d . . . C47 C 0.6235(3) 0.0508(7) 0.9371(4) 0.0376(18) Uani 1 1 d . . . H47A H 0.6295 0.0019 0.9640 0.045 Uiso 1 1 calc R . . C48 C 0.6108(3) 0.1494(6) 0.9489(3) 0.0350(17) Uani 1 1 d . . . H48A H 0.6057 0.1682 0.9843 0.042 Uiso 1 1 calc R . . C49 C 0.6050(2) 0.2256(6) 0.9088(3) 0.0254(14) Uani 1 1 d . . . C50 C 0.5710(3) 0.3627(6) 0.9599(3) 0.0351(17) Uani 1 1 d . . . C51 C 0.5332(3) 0.3105(7) 0.9850(4) 0.049(2) Uani 1 1 d . . . H51A H 0.5247 0.2435 0.9728 0.059 Uiso 1 1 calc R . . C52 C 0.5076(4) 0.3503(9) 1.0262(4) 0.066(3) Uani 1 1 d . . . H52A H 0.4833 0.3116 1.0442 0.079 Uiso 1 1 calc R . . C53 C 0.5198(4) 0.4534(9) 1.0404(5) 0.075(4) Uani 1 1 d . . . H53A H 0.5039 0.4853 1.0691 0.091 Uiso 1 1 calc R . . C54 C 0.5537(4) 0.5060(8) 1.0132(4) 0.055(3) Uani 1 1 d . . . H54A H 0.5600 0.5758 1.0225 0.066 Uiso 1 1 calc R . . C55 C 0.5469(3) -0.2269(6) 0.6483(3) 0.0330(17) Uani 1 1 d . . . H55A H 0.5632 -0.2615 0.6207 0.040 Uiso 1 1 calc R . . C56 C 0.5148(3) -0.2827(6) 0.6770(4) 0.0374(18) Uani 1 1 d . . . H56A H 0.5091 -0.3536 0.6695 0.045 Uiso 1 1 calc R . . C57 C 0.4905(3) -0.2346(6) 0.7172(3) 0.0373(18) Uani 1 1 d . . . H57A H 0.4679 -0.2716 0.7382 0.045 Uiso 1 1 calc R . . C58 C 0.4999(3) -0.1314(6) 0.7265(3) 0.0332(17) Uani 1 1 d . . . H58A H 0.4838 -0.0964 0.7541 0.040 Uiso 1 1 calc R . . C59 C 0.5335(3) -0.0780(6) 0.6947(3) 0.0314(16) Uani 1 1 d . . . C60 C 0.5190(2) 0.0926(5) 0.7297(3) 0.0238(14) Uani 1 1 d . . . C61 C 0.4675(2) 0.0925(5) 0.7305(3) 0.0261(14) Uani 1 1 d . . . H61A H 0.4501 0.0394 0.7128 0.031 Uiso 1 1 calc R . . C62 C 0.4419(3) 0.1683(6) 0.7566(3) 0.0332(17) Uani 1 1 d . . . H62A H 0.4072 0.1680 0.7568 0.040 Uiso 1 1 calc R . . C63 C 0.4678(2) 0.2455(6) 0.7828(3) 0.0279(15) Uani 1 1 d . . . C64 C 0.5185(2) 0.2449(5) 0.7810(3) 0.0201(13) Uani 1 1 d . . . C65 C 0.4456(2) 0.3229(6) 0.8140(3) 0.0336(17) Uani 1 1 d . . . H65A H 0.4112 0.3223 0.8190 0.040 Uiso 1 1 calc R . . C66 C 0.4735(3) 0.3990(6) 0.8371(3) 0.0329(16) Uani 1 1 d . . . H66A H 0.4582 0.4516 0.8572 0.039 Uiso 1 1 calc R . . C67 C 0.5250(2) 0.3986(6) 0.8307(3) 0.0261(14) Uani 1 1 d . . . C68 C 0.5435(3) 0.5668(5) 0.8637(3) 0.0281(15) Uani 1 1 d . . . C69 C 0.5054(3) 0.6221(7) 0.8372(3) 0.0374(18) Uani 1 1 d . . . H69A H 0.4865 0.5881 0.8112 0.045 Uiso 1 1 calc R . . C70 C 0.4958(3) 0.7238(6) 0.8492(4) 0.0398(19) Uani 1 1 d . . . H70A H 0.4698 0.7598 0.8325 0.048 Uiso 1 1 calc R . . C71 C 0.5250(3) 0.7729(7) 0.8862(4) 0.046(2) Uani 1 1 d . . . H71A H 0.5185 0.8422 0.8963 0.056 Uiso 1 1 calc R . . C72 C 0.5636(3) 0.7194(6) 0.9082(3) 0.0397(19) Uani 1 1 d . . . H72A H 0.5850 0.7553 0.9311 0.048 Uiso 1 1 calc R . . C73 C 0.6111(4) -0.2175(8) 0.5158(4) 0.053(2) Uiso 1 1 d . . . C74 C 0.6463(3) 0.7346(6) 1.0156(3) 0.0361(17) Uani 1 1 d . . . P1 P 0.86062(11) 0.9020(2) 0.77537(14) 0.0653(8) Uani 1 1 d D . . F1 F 0.8577(5) 0.7856(9) 0.7560(6) 0.098(3) Uiso 0.70 1 d PD B 1 F2 F 0.8354(5) 0.9337(12) 0.7184(6) 0.114(4) Uiso 0.70 1 d PD B 1 F3 F 0.8616(5) 1.0218(10) 0.7878(6) 0.108(4) Uiso 0.70 1 d PD B 1 F4 F 0.8786(9) 0.8372(18) 0.8234(9) 0.186(9) Uiso 0.70 1 d PD B 1 F1' F 0.8765(8) 0.7751(14) 0.7842(9) 0.065(6) Uiso 0.30 1 d PD B 2 F2' F 0.8494(14) 0.856(3) 0.7174(11) 0.129(11) Uiso 0.30 1 d PD B 2 F3' F 0.8501(10) 1.0102(18) 0.7549(11) 0.091(8) Uiso 0.30 1 d PD B 2 F4' F 0.8802(4) 0.8982(16) 0.8333(4) 0.049(4) Uiso 0.30 1 d PD B 2 F5 F 0.9151(3) 0.9124(7) 0.7539(4) 0.095(2) Uani 1 1 d . B . F6 F 0.8063(2) 0.8917(7) 0.7984(4) 0.101(3) Uani 1 1 d D B . O1 O 0.7540(2) 0.5708(6) 0.3684(4) 0.070(2) Uani 1 1 d . . . H1B H 0.7451 0.5155 0.3461 0.105 Uiso 1 1 d . . . H1C H 0.7412 0.5474 0.4022 0.105 Uiso 1 1 d . . . C75 C 0.8066(3) 0.4472(10) 0.6699(5) 0.078(4) Uani 1 1 d D . . H75A H 0.8190 0.3753 0.6715 0.094 Uiso 1 1 calc R . . H75B H 0.8182 0.4781 0.6367 0.094 Uiso 1 1 calc R . . Cl1 Cl 0.83065(12) 0.5171(3) 0.72183(13) 0.0789(8) Uani 1 1 d D . . Cl2 Cl 0.74235(11) 0.4453(3) 0.66996(16) 0.0823(10) Uani 1 1 d D . . C76 C 0.4228(3) 0.4264(9) 0.6764(5) 0.069(3) Uani 1 1 d D . . H76A H 0.4127 0.4954 0.6635 0.083 Uiso 1 1 calc R . . H76B H 0.4096 0.4180 0.7121 0.083 Uiso 1 1 calc R . . Cl3 Cl 0.48711(8) 0.4199(2) 0.67854(11) 0.0581(6) Uani 1 1 d D . . Cl4 Cl 0.39767(12) 0.3300(3) 0.63549(12) 0.0839(10) Uani 1 1 d D . . C77 C 0.5657(3) -0.0475(15) 0.4029(5) 0.142(8) Uani 1 1 d D . . H77A H 0.5657 -0.0071 0.4357 0.171 Uiso 1 1 calc R . . H77B H 0.5791 -0.1168 0.4108 0.171 Uiso 1 1 calc R . . Cl5 Cl 0.50510(10) -0.0614(2) 0.38141(13) 0.0706(8) Uani 1 1 d D . . Cl6 Cl 0.6040(2) 0.0139(7) 0.3578(3) 0.179(3) Uani 1 1 d D . . C78 C 0.6121(6) 1.2050(8) 1.1395(4) 0.111(6) Uani 1 1 d D . . H78A H 0.5878 1.2375 1.1629 0.133 Uiso 1 1 calc R . . H78B H 0.6399 1.1812 1.1611 0.133 Uiso 1 1 calc R . . Cl7 Cl 0.58538(18) 1.0985(4) 1.10802(17) 0.1111(13) Uani 1 1 d D . . Cl8 Cl 0.6324(4) 1.2946(6) 1.0949(2) 0.240(6) Uani 1 1 d D . . C79 C 0.7224(9) 0.499(3) 0.5160(7) 0.227(15) Uiso 1 1 d D . . H79A H 0.7203 0.4333 0.5359 0.272 Uiso 1 1 calc R . . H79B H 0.6908 0.5356 0.5188 0.272 Uiso 1 1 calc R . . Cl9 Cl 0.7713(6) 0.5775(7) 0.5399(4) 0.339(9) Uani 1 1 d D . . Cl10 Cl 0.7372(4) 0.4745(8) 0.4499(6) 0.302(8) Uani 1 1 d D . . C80 C 0.6119(9) 0.3412(13) 0.4389(16) 0.250(18) Uiso 1 1 d D . . H80A H 0.6141 0.3419 0.4004 0.300 Uiso 1 1 calc R . . H80B H 0.6449 0.3541 0.4537 0.300 Uiso 1 1 calc R . . Cl11 Cl 0.5882(6) 0.2258(9) 0.4612(3) 0.369(10) Uani 1 1 d D . . Cl12 Cl 0.5683(4) 0.4359(4) 0.4621(3) 0.230(5) Uani 1 1 d 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 0.0278(5) 0.0249(5) 0.0239(5) -0.0037(4) 0.0006(4) -0.0001(4) Co2 0.0222(4) 0.0220(5) 0.0205(5) -0.0006(4) 0.0002(3) 0.0001(3) Co3 0.0191(4) 0.0204(5) 0.0173(5) 0.0009(4) 0.0002(3) -0.0002(3) Co4 0.0193(4) 0.0213(4) 0.0177(5) 0.0001(4) 0.0003(3) -0.0015(3) Co5 0.0228(4) 0.0251(5) 0.0197(5) -0.0024(4) -0.0001(3) -0.0022(3) Co6 0.0292(5) 0.0296(5) 0.0220(5) -0.0050(4) -0.0007(4) -0.0032(4) S2 0.0606(14) 0.0472(13) 0.0638(17) -0.0218(13) -0.0042(12) -0.0075(11) N1 0.026(3) 0.032(3) 0.023(3) -0.004(3) -0.003(2) 0.000(2) N2 0.025(3) 0.027(3) 0.021(3) -0.006(2) -0.006(2) 0.004(2) N3 0.021(3) 0.021(3) 0.024(3) 0.003(2) -0.001(2) 0.003(2) N4 0.025(3) 0.015(3) 0.019(3) 0.001(2) 0.002(2) -0.004(2) N5 0.026(3) 0.023(3) 0.027(3) -0.001(2) -0.003(2) -0.005(2) N6 0.026(3) 0.024(3) 0.022(3) -0.002(2) -0.002(2) -0.001(2) N7 0.028(3) 0.028(3) 0.021(3) -0.003(3) 0.005(2) 0.008(2) N8 0.024(3) 0.023(3) 0.023(3) 0.000(2) -0.003(2) 0.001(2) N9 0.020(3) 0.019(3) 0.027(3) 0.001(2) 0.002(2) 0.004(2) N10 0.020(2) 0.027(3) 0.022(3) -0.001(2) -0.001(2) -0.003(2) N11 0.024(3) 0.032(3) 0.023(3) -0.004(3) -0.004(2) -0.007(2) N12 0.042(3) 0.030(3) 0.019(3) -0.003(3) -0.003(3) -0.007(3) N13 0.026(3) 0.026(3) 0.035(4) 0.000(3) -0.003(2) -0.006(2) N14 0.026(3) 0.028(3) 0.022(3) 0.002(3) 0.003(2) 0.004(2) N15 0.021(3) 0.028(3) 0.017(3) 0.002(2) 0.002(2) 0.004(2) N16 0.026(3) 0.029(3) 0.016(3) 0.003(2) -0.002(2) -0.004(2) N17 0.024(3) 0.031(3) 0.019(3) 0.002(2) 0.000(2) -0.004(2) N18 0.039(3) 0.038(4) 0.028(4) -0.005(3) 0.002(3) -0.015(3) N19 0.027(3) 0.029(3) 0.033(3) -0.004(3) 0.001(2) -0.003(2) N20 0.030(3) 0.028(3) 0.020(3) -0.003(2) 0.003(2) -0.001(2) N21 0.018(2) 0.024(3) 0.021(3) -0.002(2) -0.003(2) -0.003(2) N22 0.018(2) 0.027(3) 0.024(3) -0.001(2) 0.001(2) 0.002(2) N23 0.023(3) 0.032(3) 0.027(3) 0.000(3) -0.001(2) 0.004(2) N24 0.028(3) 0.030(3) 0.025(3) -0.006(3) 0.001(2) 0.005(2) N25 0.039(3) 0.033(3) 0.035(4) -0.021(3) -0.006(3) 0.002(3) N26 0.048(4) 0.037(4) 0.036(4) -0.006(3) -0.008(3) -0.002(3) C1 0.053(5) 0.026(4) 0.035(4) -0.007(4) -0.015(4) -0.008(3) C2 0.038(4) 0.049(5) 0.044(5) -0.005(4) -0.021(4) -0.006(4) C3 0.032(4) 0.048(5) 0.046(5) -0.005(4) -0.018(4) 0.003(3) C4 0.032(4) 0.042(5) 0.037(5) -0.012(4) -0.007(3) 0.006(3) C5 0.030(3) 0.022(3) 0.024(4) -0.002(3) -0.002(3) -0.002(3) C6 0.028(3) 0.030(4) 0.020(3) 0.002(3) 0.003(3) 0.004(3) C7 0.034(4) 0.037(4) 0.013(3) -0.001(3) -0.003(3) 0.001(3) C8 0.036(4) 0.024(4) 0.026(4) 0.010(3) 0.006(3) 0.003(3) C9 0.024(3) 0.017(3) 0.032(4) 0.004(3) 0.001(3) -0.002(2) C10 0.014(3) 0.033(4) 0.024(4) -0.002(3) 0.000(2) 0.002(2) C11 0.034(4) 0.022(3) 0.026(4) 0.007(3) 0.001(3) -0.001(3) C12 0.030(3) 0.022(3) 0.030(4) 0.002(3) -0.002(3) -0.003(3) C13 0.021(3) 0.030(4) 0.024(4) 0.001(3) -0.003(3) 0.003(3) C14 0.032(3) 0.017(3) 0.022(4) 0.001(3) 0.000(3) 0.000(3) C15 0.037(4) 0.040(4) 0.025(4) 0.011(3) -0.003(3) 0.000(3) C16 0.041(4) 0.039(5) 0.040(5) 0.008(4) -0.008(3) -0.009(3) C17 0.045(4) 0.044(5) 0.029(4) 0.002(4) -0.006(3) -0.014(4) C18 0.042(4) 0.024(4) 0.029(4) -0.005(3) -0.010(3) -0.004(3) C19 0.041(4) 0.033(4) 0.033(4) -0.004(3) -0.001(3) 0.006(3) C20 0.058(5) 0.037(4) 0.026(4) -0.003(4) 0.009(4) -0.001(4) C21 0.046(5) 0.046(5) 0.032(4) 0.001(4) 0.007(3) 0.005(4) C22 0.034(4) 0.041(4) 0.028(4) -0.005(3) 0.012(3) -0.003(3) C23 0.031(3) 0.026(3) 0.024(4) 0.000(3) 0.008(3) 0.011(3) C24 0.024(3) 0.023(3) 0.032(4) -0.005(3) -0.003(3) -0.004(3) C25 0.026(3) 0.057(5) 0.024(4) -0.012(4) -0.002(3) 0.008(3) C26 0.014(3) 0.055(5) 0.051(5) -0.005(4) -0.002(3) 0.001(3) C27 0.021(4) 0.047(4) 0.032(4) -0.005(4) -0.001(3) -0.002(3) C28 0.018(3) 0.024(3) 0.025(4) 0.002(3) 0.002(2) 0.003(2) C29 0.016(3) 0.065(5) 0.038(4) -0.012(4) -0.001(3) -0.001(3) C30 0.025(3) 0.052(5) 0.026(4) -0.013(4) -0.005(3) -0.006(3) C31 0.024(3) 0.028(4) 0.027(4) -0.001(3) -0.007(3) -0.001(3) C32 0.029(3) 0.036(4) 0.027(4) -0.003(3) -0.005(3) -0.009(3) C33 0.047(4) 0.030(4) 0.031(4) 0.002(3) -0.014(3) -0.003(3) C34 0.055(5) 0.049(5) 0.025(4) -0.003(4) -0.019(4) 0.013(4) C35 0.056(5) 0.042(5) 0.029(4) -0.002(4) -0.016(4) -0.012(4) C36 0.060(5) 0.030(4) 0.019(4) -0.002(3) -0.014(3) -0.011(4) C37 0.033(4) 0.021(3) 0.033(4) -0.005(3) 0.005(3) -0.004(3) C38 0.042(4) 0.034(4) 0.032(4) 0.007(4) 0.011(3) 0.014(3) C39 0.031(4) 0.045(5) 0.048(5) 0.013(4) 0.008(4) 0.010(3) C40 0.042(4) 0.025(4) 0.026(4) 0.003(3) 0.000(3) 0.007(3) C41 0.028(3) 0.029(4) 0.023(4) 0.001(3) 0.000(3) 0.003(3) C42 0.028(3) 0.023(3) 0.029(4) 0.004(3) -0.005(3) 0.003(3) C43 0.040(4) 0.021(3) 0.033(4) 0.007(3) -0.001(3) 0.000(3) C44 0.046(4) 0.029(4) 0.032(4) 0.006(3) 0.010(3) -0.005(3) C45 0.036(4) 0.030(4) 0.023(4) -0.001(3) 0.002(3) 0.002(3) C46 0.023(3) 0.030(4) 0.017(3) 0.003(3) 0.000(2) 0.004(3) C47 0.051(5) 0.038(4) 0.023(4) 0.012(4) 0.000(3) -0.002(3) C48 0.044(4) 0.039(4) 0.023(4) 0.012(3) 0.003(3) -0.008(3) C49 0.026(3) 0.036(4) 0.014(3) -0.003(3) 0.001(2) -0.008(3) C50 0.039(4) 0.042(4) 0.024(4) -0.010(3) 0.002(3) -0.008(3) C51 0.051(5) 0.054(5) 0.042(5) -0.019(4) 0.024(4) -0.018(4) C52 0.072(7) 0.071(7) 0.054(7) -0.019(5) 0.048(5) -0.025(5) C53 0.081(8) 0.079(7) 0.066(7) -0.053(6) 0.050(6) -0.041(6) C54 0.057(6) 0.061(6) 0.046(6) -0.022(5) 0.023(4) -0.014(5) C55 0.035(4) 0.024(4) 0.040(5) -0.009(3) -0.001(3) -0.006(3) C56 0.034(4) 0.031(4) 0.047(5) 0.010(4) -0.003(3) -0.007(3) C57 0.034(4) 0.032(4) 0.046(5) 0.004(4) 0.003(3) -0.013(3) C58 0.037(4) 0.032(4) 0.031(4) 0.001(3) 0.003(3) -0.005(3) C59 0.032(4) 0.030(4) 0.032(4) 0.002(3) -0.004(3) 0.000(3) C60 0.024(3) 0.026(3) 0.021(3) 0.000(3) -0.002(3) 0.002(3) C61 0.023(3) 0.029(4) 0.026(4) -0.001(3) -0.007(3) -0.005(3) C62 0.027(3) 0.035(4) 0.037(5) -0.007(3) -0.005(3) -0.001(3) C63 0.021(3) 0.027(3) 0.036(4) 0.002(3) 0.001(3) -0.003(3) C64 0.020(3) 0.024(3) 0.016(3) 0.000(3) 0.000(2) 0.005(2) C65 0.019(3) 0.048(5) 0.034(4) 0.002(4) 0.001(3) 0.002(3) C66 0.031(4) 0.035(4) 0.033(4) -0.006(3) 0.004(3) 0.004(3) C67 0.025(3) 0.032(4) 0.021(3) 0.000(3) 0.001(3) 0.001(3) C68 0.028(3) 0.029(4) 0.027(4) -0.010(3) 0.006(3) -0.004(3) C69 0.032(4) 0.049(5) 0.031(4) -0.009(4) -0.006(3) 0.000(3) C70 0.043(4) 0.033(4) 0.043(5) -0.006(4) -0.001(4) 0.011(3) C71 0.049(5) 0.035(5) 0.055(6) -0.026(4) -0.005(4) 0.007(4) C72 0.048(5) 0.035(4) 0.036(5) -0.009(4) -0.009(4) -0.009(4) C74 0.040(4) 0.039(4) 0.030(4) -0.009(4) -0.002(3) 0.001(3) P1 0.0567(16) 0.0654(17) 0.074(2) 0.0064(16) -0.0026(14) -0.0095(13) F5 0.059(4) 0.110(6) 0.116(7) 0.026(5) 0.011(4) 0.013(4) F6 0.064(4) 0.106(6) 0.132(7) -0.016(5) 0.030(4) -0.017(4) O1 0.038(3) 0.059(4) 0.113(7) 0.022(4) 0.003(4) -0.008(3) C75 0.056(6) 0.080(8) 0.098(10) -0.034(7) 0.018(6) -0.002(6) Cl1 0.0798(19) 0.097(2) 0.0599(18) -0.0051(16) 0.0138(15) 0.0039(16) Cl2 0.0615(16) 0.077(2) 0.108(3) 0.0061(18) 0.0129(17) 0.0114(14) C76 0.034(4) 0.105(9) 0.068(7) -0.014(7) 0.004(5) -0.003(5) Cl3 0.0455(12) 0.0673(16) 0.0616(16) 0.0193(13) 0.0002(11) -0.0030(11) Cl4 0.0626(16) 0.139(3) 0.0497(17) -0.0039(18) 0.0030(13) -0.0239(18) C77 0.069(9) 0.23(2) 0.131(17) -0.046(16) -0.029(10) 0.038(12) Cl5 0.0542(14) 0.0730(18) 0.085(2) -0.0335(16) 0.0021(13) 0.0057(12) Cl6 0.122(4) 0.281(8) 0.134(5) -0.093(5) 0.041(3) -0.085(5) C78 0.114(13) 0.094(11) 0.124(15) -0.053(11) 0.033(10) -0.027(9) Cl7 0.134(3) 0.122(3) 0.077(3) 0.001(2) -0.014(2) -0.037(3) Cl8 0.426(14) 0.215(7) 0.080(4) 0.036(4) -0.047(5) -0.220(9) Cl9 0.67(3) 0.171(7) 0.175(8) 0.006(7) 0.092(13) 0.168(12) Cl10 0.199(9) 0.285(11) 0.421(18) -0.229(13) 0.096(10) -0.062(8) Cl11 0.64(2) 0.374(13) 0.089(4) -0.070(6) -0.120(8) 0.402(15) Cl12 0.485(15) 0.092(3) 0.114(4) 0.013(3) -0.144(7) 0.020(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 Co1 N1 1.978(6) . ? Co1 N19 1.979(6) . ? Co1 N13 1.984(6) . ? Co1 N7 1.992(6) . ? Co1 N25 2.073(6) . ? Co1 Co2 2.3139(13) . ? Co2 N8 1.906(6) . ? Co2 N20 1.911(6) . ? Co2 N2 1.912(6) . ? Co2 N14 1.930(6) . ? Co2 Co3 2.2735(13) . ? Co3 N15 1.921(6) . ? Co3 N3 1.924(6) . ? Co3 N21 1.929(5) . ? Co3 N9 1.933(5) . ? Co3 Co4 2.2555(12) . ? Co4 N22 1.930(5) . ? Co4 N16 1.932(6) . ? Co4 N4 1.936(6) . ? Co4 N10 1.949(5) . ? Co4 Co5 2.2727(13) . ? Co5 N5 1.908(6) . ? Co5 N17 1.915(6) . ? Co5 N23 1.915(6) . ? Co5 N11 1.941(6) . ? Co5 Co6 2.3129(13) . ? Co6 N12 1.949(7) . ? Co6 N18 1.975(6) . ? Co6 N24 1.979(6) . ? Co6 N6 2.010(6) . ? Co6 N26 2.067(7) . ? S1 C73 1.657(12) . ? S1' C73 1.630(17) . ? S2 C74 1.612(8) . ? N1 C5 1.350(9) . ? N1 C1 1.376(9) . ? N2 C6 1.365(9) . ? N2 C5 1.376(9) . ? N3 C6 1.344(9) . ? N3 C10 1.368(9) . ? N4 C13 1.358(9) . ? N4 C10 1.381(9) . ? N5 C13 1.363(9) . ? N5 C14 1.404(9) . ? N6 C18 1.347(9) . ? N6 C14 1.362(9) . ? N7 C23 1.349(10) . ? N7 C19 1.352(10) . ? N8 C23 1.364(9) . ? N8 C24 1.377(9) . ? N9 C24 1.345(9) . ? N9 C28 1.369(9) . ? N10 C31 1.346(9) . ? N10 C28 1.353(9) . ? N11 C31 1.351(9) . ? N11 C32 1.366(9) . ? N12 C32 1.372(10) . ? N12 C36 1.385(9) . ? N13 C37 1.358(9) . ? N13 C41 1.385(9) . ? N14 C42 1.326(10) . ? N14 C41 1.378(9) . ? N15 C42 1.349(9) . ? N15 C46 1.398(9) . ? N16 C49 1.354(9) . ? N16 C46 1.362(10) . ? N17 C50 1.355(9) . ? N17 C49 1.356(9) . ? N18 C54 1.349(11) . ? N18 C50 1.377(10) . ? N19 C55 1.318(9) . ? N19 C59 1.361(10) . ? N20 C60 1.368(9) . ? N20 C59 1.374(9) . ? N21 C60 1.369(9) . ? N21 C64 1.382(9) . ? N22 C67 1.366(9) . ? N22 C64 1.384(9) . ? N23 C68 1.345(9) . ? N23 C67 1.362(9) . ? N24 C72 1.338(10) . ? N24 C68 1.371(9) . ? N25 C73 1.162(13) . ? N26 C74 1.171(10) . ? C1 C2 1.354(11) . ? C2 C3 1.373(12) . ? C3 C4 1.363(11) . ? C4 C5 1.411(10) . ? C6 C7 1.434(10) . ? C7 C8 1.382(10) . ? C8 C9 1.386(11) . ? C9 C11 1.399(10) . ? C9 C10 1.428(11) . ? C11 C12 1.381(11) . ? C12 C13 1.415(10) . ? C14 C15 1.386(10) . ? C15 C16 1.352(11) . ? C16 C17 1.417(12) . ? C17 C18 1.378(11) . ? C19 C20 1.370(12) . ? C20 C21 1.365(12) . ? C21 C22 1.352(11) . ? C22 C23 1.422(10) . ? C24 C25 1.423(9) . ? C25 C26 1.365(11) . ? C26 C27 1.411(11) . ? C27 C29 1.380(11) . ? C27 C28 1.425(9) . ? C29 C30 1.372(11) . ? C30 C31 1.405(10) . ? C32 C33 1.397(11) . ? C33 C34 1.359(11) . ? C34 C35 1.380(13) . ? C35 C36 1.337(12) . ? C37 C38 1.351(11) . ? C38 C39 1.366(13) . ? C39 C40 1.384(11) . ? C40 C41 1.418(10) . ? C42 C43 1.460(10) . ? C43 C44 1.314(11) . ? C44 C45 1.414(11) . ? C45 C46 1.390(11) . ? C45 C47 1.434(12) . ? C47 C48 1.356(12) . ? C48 C49 1.433(11) . ? C50 C51 1.392(11) . ? C51 C52 1.367(12) . ? C52 C53 1.422(14) . ? C53 C54 1.344(13) . ? C55 C56 1.354(11) . ? C56 C57 1.374(12) . ? C57 C58 1.380(11) . ? C58 C59 1.407(11) . ? C60 C61 1.408(9) . ? C61 C62 1.377(10) . ? C62 C63 1.396(10) . ? C63 C64 1.388(9) . ? C63 C65 1.417(11) . ? C65 C66 1.378(11) . ? C66 C67 1.419(10) . ? C68 C69 1.436(11) . ? C69 C70 1.375(12) . ? C70 C71 1.395(12) . ? C71 C72 1.382(12) . ? P1 F3' 1.52(2) . ? P1 F4 1.57(2) . ? P1 F4' 1.580(8) . ? P1 F3 1.583(13) . ? P1 F1 1.586(12) . ? P1 F5 1.594(8) . ? P1 F6 1.602(7) . ? P1 F2' 1.63(3) . ? P1 F2 1.666(14) . ? P1 F1' 1.713(19) . ? C75 Cl1 1.739(8) . ? C75 Cl2 1.758(8) . ? C76 Cl3 1.762(7) . ? C76 Cl4 1.768(8) . ? C77 Cl6 1.751(9) . ? C77 Cl5 1.754(8) . ? C78 Cl8 1.720(9) . ? C78 Cl7 1.755(8) . ? C79 Cl10 1.770(10) . ? C79 Cl9 1.787(10) . ? C80 Cl11 1.724(10) . ? C80 Cl12 1.811(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N19 89.2(3) . . ? N1 Co1 N13 171.9(3) . . ? N19 Co1 N13 89.2(3) . . ? N1 Co1 N7 89.2(2) . . ? N19 Co1 N7 171.6(3) . . ? N13 Co1 N7 91.2(2) . . ? N1 Co1 N25 94.4(3) . . ? N19 Co1 N25 95.4(3) . . ? N13 Co1 N25 93.6(3) . . ? N7 Co1 N25 93.0(3) . . ? N1 Co1 Co2 86.52(18) . . ? N19 Co1 Co2 85.80(19) . . ? N13 Co1 Co2 85.46(19) . . ? N7 Co1 Co2 85.85(17) . . ? N25 Co1 Co2 178.48(19) . . ? N8 Co2 N20 178.5(3) . . ? N8 Co2 N2 89.9(2) . . ? N20 Co2 N2 89.8(3) . . ? N8 Co2 N14 89.6(2) . . ? N20 Co2 N14 90.7(3) . . ? N2 Co2 N14 177.5(3) . . ? N8 Co2 Co3 89.04(18) . . ? N20 Co2 Co3 89.47(18) . . ? N2 Co2 Co3 89.40(17) . . ? N14 Co2 Co3 88.13(18) . . ? N8 Co2 Co1 90.29(18) . . ? N20 Co2 Co1 91.20(18) . . ? N2 Co2 Co1 89.79(17) . . ? N14 Co2 Co1 92.68(18) . . ? Co3 Co2 Co1 178.94(6) . . ? N15 Co3 N3 178.4(2) . . ? N15 Co3 N21 91.4(2) . . ? N3 Co3 N21 90.0(2) . . ? N15 Co3 N9 89.0(2) . . ? N3 Co3 N9 89.6(2) . . ? N21 Co3 N9 179.5(3) . . ? N15 Co3 Co4 89.82(18) . . ? N3 Co3 Co4 90.97(18) . . ? N21 Co3 Co4 90.42(17) . . ? N9 Co3 Co4 89.81(18) . . ? N15 Co3 Co2 90.20(18) . . ? N3 Co3 Co2 89.01(18) . . ? N21 Co3 Co2 89.61(17) . . ? N9 Co3 Co2 90.16(18) . . ? Co4 Co3 Co2 179.96(7) . . ? N22 Co4 N16 90.1(2) . . ? N22 Co4 N4 91.0(2) . . ? N16 Co4 N4 178.9(2) . . ? N22 Co4 N10 179.0(3) . . ? N16 Co4 N10 89.2(2) . . ? N4 Co4 N10 89.7(2) . . ? N22 Co4 Co3 90.44(18) . . ? N16 Co4 Co3 90.50(19) . . ? N4 Co4 Co3 89.80(17) . . ? N10 Co4 Co3 90.36(18) . . ? N22 Co4 Co5 89.49(18) . . ? N16 Co4 Co5 89.40(19) . . ? N4 Co4 Co5 90.30(17) . . ? N10 Co4 Co5 89.71(18) . . ? Co3 Co4 Co5 179.88(6) . . ? N5 Co5 N17 177.5(3) . . ? N5 Co5 N23 90.3(3) . . ? N17 Co5 N23 91.0(3) . . ? N5 Co5 N11 89.4(2) . . ? N17 Co5 N11 89.3(3) . . ? N23 Co5 N11 178.3(3) . . ? N5 Co5 Co4 88.06(18) . . ? N17 Co5 Co4 89.77(19) . . ? N23 Co5 Co4 89.36(19) . . ? N11 Co5 Co4 88.94(18) . . ? N5 Co5 Co6 91.42(18) . . ? N17 Co5 Co6 90.72(19) . . ? N23 Co5 Co6 91.86(19) . . ? N11 Co5 Co6 89.84(18) . . ? Co4 Co5 Co6 178.68(5) . . ? N12 Co6 N18 88.7(3) . . ? N12 Co6 N24 172.0(3) . . ? N18 Co6 N24 89.3(3) . . ? N12 Co6 N6 89.3(2) . . ? N18 Co6 N6 171.2(3) . . ? N24 Co6 N6 91.5(2) . . ? N12 Co6 N26 93.5(3) . . ? N18 Co6 N26 95.6(3) . . ? N24 Co6 N26 94.4(3) . . ? N6 Co6 N26 93.1(3) . . ? N12 Co6 Co5 86.67(18) . . ? N18 Co6 Co5 85.92(19) . . ? N24 Co6 Co5 85.51(17) . . ? N6 Co6 Co5 85.40(17) . . ? N26 Co6 Co5 178.5(2) . . ? C5 N1 C1 118.3(6) . . ? C5 N1 Co1 121.0(5) . . ? C1 N1 Co1 120.6(5) . . ? C6 N2 C5 123.2(6) . . ? C6 N2 Co2 118.5(4) . . ? C5 N2 Co2 118.3(5) . . ? C6 N3 C10 119.0(6) . . ? C6 N3 Co3 121.2(5) . . ? C10 N3 Co3 119.6(5) . . ? C13 N4 C10 119.8(6) . . ? C13 N4 Co4 120.1(5) . . ? C10 N4 Co4 120.1(5) . . ? C13 N5 C14 120.2(6) . . ? C13 N5 Co5 122.3(5) . . ? C14 N5 Co5 116.4(5) . . ? C18 N6 C14 117.5(6) . . ? C18 N6 Co6 119.5(5) . . ? C14 N6 Co6 122.3(4) . . ? C23 N7 C19 119.1(6) . . ? C23 N7 Co1 120.6(5) . . ? C19 N7 Co1 119.9(5) . . ? C23 N8 C24 123.8(6) . . ? C23 N8 Co2 117.4(5) . . ? C24 N8 Co2 118.5(5) . . ? C24 N9 C28 120.0(5) . . ? C24 N9 Co3 119.3(4) . . ? C28 N9 Co3 120.4(4) . . ? C31 N10 C28 120.2(6) . . ? C31 N10 Co4 120.1(5) . . ? C28 N10 Co4 119.5(5) . . ? C31 N11 C32 123.4(6) . . ? C31 N11 Co5 119.3(5) . . ? C32 N11 Co5 117.1(5) . . ? C32 N12 C36 116.3(7) . . ? C32 N12 Co6 122.0(5) . . ? C36 N12 Co6 121.5(5) . . ? C37 N13 C41 116.6(6) . . ? C37 N13 Co1 121.3(5) . . ? C41 N13 Co1 121.9(5) . . ? C42 N14 C41 124.7(6) . . ? C42 N14 Co2 120.2(5) . . ? C41 N14 Co2 114.5(5) . . ? C42 N15 C46 119.5(6) . . ? C42 N15 Co3 119.4(5) . . ? C46 N15 Co3 121.1(5) . . ? C49 N16 C46 119.1(6) . . ? C49 N16 Co4 119.9(5) . . ? C46 N16 Co4 120.5(5) . . ? C50 N17 C49 123.9(6) . . ? C50 N17 Co5 117.7(5) . . ? C49 N17 Co5 118.3(5) . . ? C54 N18 C50 119.1(7) . . ? C54 N18 Co6 119.7(6) . . ? C50 N18 Co6 121.3(5) . . ? C55 N19 C59 117.6(7) . . ? C55 N19 Co1 121.1(5) . . ? C59 N19 Co1 121.3(5) . . ? C60 N20 C59 123.5(6) . . ? C60 N20 Co2 119.3(5) . . ? C59 N20 Co2 117.1(5) . . ? C60 N21 C64 118.8(5) . . ? C60 N21 Co3 120.3(4) . . ? C64 N21 Co3 120.9(4) . . ? C67 N22 C64 118.9(5) . . ? C67 N22 Co4 120.4(5) . . ? C64 N22 Co4 120.6(4) . . ? C68 N23 C67 123.8(6) . . ? C68 N23 Co5 117.1(5) . . ? C67 N23 Co5 119.2(5) . . ? C72 N24 C68 119.9(6) . . ? C72 N24 Co6 119.0(5) . . ? C68 N24 Co6 121.1(5) . . ? C73 N25 Co1 169.3(7) . . ? C74 N26 Co6 162.5(7) . . ? C2 C1 N1 122.6(7) . . ? C1 C2 C3 119.8(7) . . ? C4 C3 C2 118.8(7) . . ? C3 C4 C5 120.8(7) . . ? N1 C5 N2 115.5(6) . . ? N1 C5 C4 119.6(6) . . ? N2 C5 C4 124.5(6) . . ? N3 C6 N2 115.3(6) . . ? N3 C6 C7 121.7(6) . . ? N2 C6 C7 122.6(6) . . ? C8 C7 C6 118.5(6) . . ? C7 C8 C9 120.8(7) . . ? C8 C9 C11 125.7(7) . . ? C8 C9 C10 117.9(6) . . ? C11 C9 C10 116.3(7) . . ? N3 C10 N4 116.1(6) . . ? N3 C10 C9 121.9(7) . . ? N4 C10 C9 122.0(6) . . ? C12 C11 C9 121.9(7) . . ? C11 C12 C13 119.2(6) . . ? N4 C13 N5 114.1(6) . . ? N4 C13 C12 120.6(6) . . ? N5 C13 C12 125.1(6) . . ? N6 C14 C15 121.2(7) . . ? N6 C14 N5 113.8(6) . . ? C15 C14 N5 124.6(7) . . ? C16 C15 C14 121.4(8) . . ? C15 C16 C17 117.9(8) . . ? C18 C17 C16 118.4(7) . . ? N6 C18 C17 123.5(7) . . ? N7 C19 C20 122.5(8) . . ? C21 C20 C19 118.4(8) . . ? C22 C21 C20 121.1(8) . . ? C21 C22 C23 118.9(8) . . ? N7 C23 N8 116.1(6) . . ? N7 C23 C22 119.9(6) . . ? N8 C23 C22 123.5(7) . . ? N9 C24 N8 116.3(6) . . ? N9 C24 C25 121.1(6) . . ? N8 C24 C25 122.5(6) . . ? C26 C25 C24 119.0(7) . . ? C25 C26 C27 121.4(7) . . ? C29 C27 C26 126.4(7) . . ? C29 C27 C28 116.8(7) . . ? C26 C27 C28 116.7(7) . . ? N10 C28 N9 116.4(5) . . ? N10 C28 C27 122.0(6) . . ? N9 C28 C27 121.7(6) . . ? C30 C29 C27 121.0(6) . . ? C29 C30 C31 120.0(7) . . ? N10 C31 N11 116.2(6) . . ? N10 C31 C30 119.9(7) . . ? N11 C31 C30 123.6(6) . . ? N11 C32 N12 115.2(6) . . ? N11 C32 C33 123.8(7) . . ? N12 C32 C33 120.8(7) . . ? C34 C33 C32 119.9(8) . . ? C33 C34 C35 120.1(8) . . ? C36 C35 C34 118.6(8) . . ? C35 C36 N12 124.2(8) . . ? C38 C37 N13 125.0(7) . . ? C37 C38 C39 118.7(7) . . ? C38 C39 C40 120.3(8) . . ? C39 C40 C41 118.8(8) . . ? N14 C41 N13 116.3(6) . . ? N14 C41 C40 123.1(7) . . ? N13 C41 C40 120.3(6) . . ? N14 C42 N15 116.9(6) . . ? N14 C42 C43 124.0(6) . . ? N15 C42 C43 118.9(7) . . ? C44 C43 C42 120.6(7) . . ? C43 C44 C45 121.5(7) . . ? C46 C45 C44 117.4(7) . . ? C46 C45 C47 117.1(7) . . ? C44 C45 C47 125.4(7) . . ? N16 C46 C45 123.7(7) . . ? N16 C46 N15 114.4(6) . . ? C45 C46 N15 121.9(7) . . ? C48 C47 C45 119.1(8) . . ? C47 C48 C49 121.0(8) . . ? N16 C49 N17 116.7(6) . . ? N16 C49 C48 119.7(7) . . ? N17 C49 C48 123.3(6) . . ? N17 C50 N18 115.5(7) . . ? N17 C50 C51 126.1(7) . . ? N18 C50 C51 118.0(7) . . ? C52 C51 C50 123.6(9) . . ? C51 C52 C53 115.5(8) . . ? C54 C53 C52 120.2(8) . . ? C53 C54 N18 123.2(9) . . ? N19 C55 C56 125.3(8) . . ? C55 C56 C57 118.7(7) . . ? C56 C57 C58 118.5(7) . . ? C57 C58 C59 119.7(7) . . ? N19 C59 N20 116.2(6) . . ? N19 C59 C58 120.2(7) . . ? N20 C59 C58 123.4(7) . . ? N20 C60 N21 115.2(6) . . ? N20 C60 C61 124.6(6) . . ? N21 C60 C61 119.9(6) . . ? C62 C61 C60 120.9(6) . . ? C61 C62 C63 119.1(7) . . ? C64 C63 C62 119.1(7) . . ? C64 C63 C65 116.8(7) . . ? C62 C63 C65 124.0(6) . . ? N21 C64 N22 114.7(5) . . ? N21 C64 C63 121.9(6) . . ? N22 C64 C63 123.3(6) . . ? C66 C65 C63 120.7(6) . . ? C65 C66 C67 119.8(7) . . ? N23 C67 N22 115.1(6) . . ? N23 C67 C66 124.5(6) . . ? N22 C67 C66 120.1(6) . . ? N23 C68 N24 117.2(6) . . ? N23 C68 C69 124.0(7) . . ? N24 C68 C69 118.5(6) . . ? C70 C69 C68 120.7(7) . . ? C69 C70 C71 118.5(8) . . ? C72 C71 C70 119.2(7) . . ? N24 C72 C71 122.9(7) . . ? N25 C73 S1' 156.8(11) . . ? N25 C73 S1 171.0(10) . . ? S1' C73 S1 31.5(5) . . ? N26 C74 S2 177.9(8) . . ? F3' P1 F4 145.1(15) . . ? F3' P1 F4' 114.6(14) . . ? F4 P1 F4' 30.5(8) . . ? F3' P1 F3 34.1(10) . . ? F4 P1 F3 111.1(11) . . ? F4' P1 F3 80.5(10) . . ? F3' P1 F1 139.0(13) . . ? F4 P1 F1 75.8(10) . . ? F4' P1 F1 106.4(9) . . ? F3 P1 F1 173.1(8) . . ? F3' P1 F5 88.9(11) . . ? F4 P1 F5 91.3(9) . . ? F4' P1 F5 90.6(6) . . ? F3 P1 F5 88.4(6) . . ? F1 P1 F5 91.1(6) . . ? F3' P1 F6 91.6(11) . . ? F4 P1 F6 87.5(10) . . ? F4' P1 F6 88.0(5) . . ? F3 P1 F6 91.3(6) . . ? F1 P1 F6 89.5(6) . . ? F5 P1 F6 178.6(5) . . ? F3' P1 F2' 89.1(15) . . ? F4 P1 F2' 125.5(15) . . ? F4' P1 F2' 155.6(15) . . ? F3 P1 F2' 122.9(13) . . ? F1 P1 F2' 50.2(12) . . ? F5 P1 F2' 83.8(14) . . ? F6 P1 F2' 97.6(14) . . ? F3' P1 F2 52.7(12) . . ? F4 P1 F2 161.7(11) . . ? F4' P1 F2 166.4(9) . . ? F3 P1 F2 86.7(7) . . ? F1 P1 F2 86.4(8) . . ? F5 P1 F2 93.6(6) . . ? F6 P1 F2 87.8(6) . . ? F2' P1 F2 38.0(11) . . ? F3' P1 F1' 167.1(13) . . ? F4 P1 F1' 45.9(11) . . ? F4' P1 F1' 76.1(10) . . ? F3 P1 F1' 155.1(10) . . ? F1 P1 F1' 31.3(7) . . ? F5 P1 F1' 83.7(8) . . ? F6 P1 F1' 96.1(8) . . ? F2' P1 F1' 79.7(13) . . ? F2 P1 F1' 117.2(10) . . ? Cl1 C75 Cl2 112.6(5) . . ? Cl3 C76 Cl4 111.8(5) . . ? Cl6 C77 Cl5 113.8(7) . . ? Cl8 C78 Cl7 111.0(7) . . ? Cl10 C79 Cl9 105.0(11) . . ? Cl11 C80 Cl12 103.2(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.185 _refine_diff_density_min -1.282 _refine_diff_density_rms 0.211 #===END data_ic11047(compd_2) _database_code_depnum_ccdc_archive 'CCDC 283615' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co6(bpyany)4(NCS)2)(PF6)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H56 Cl8 Co6 F12 N26 P2 S2' _chemical_formula_weight 2348.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 17.3930(2) _cell_length_b 17.3930(2) _cell_length_c 28.0060(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8472.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour dark-purple _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.841 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4696 _exptl_absorpt_coefficient_mu 1.578 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.686 _exptl_absorpt_correction_T_max 0.855 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONISU KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46542 _diffrn_reflns_av_R_equivalents 0.0761 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7470 _reflns_number_gt 5693 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+8.7700P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 7470 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1369 _refine_ls_wR_factor_gt 0.1229 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.60049(5) 0.25757(5) 1.13636(3) 0.0348(2) Uani 1 1 d . . . Co2 Co 0.53344(5) 0.32996(5) 1.08100(3) 0.0319(2) Uani 1 1 d . . . Co3 Co 0.46484(5) 0.39730(5) 1.02695(3) 0.0301(2) Uani 1 1 d . . . S1 S 0.73146(13) 0.09890(12) 1.25088(7) 0.0599(6) Uani 1 1 d . . . N1 N 0.5164(3) 0.1823(3) 1.13303(19) 0.0363(13) Uani 1 1 d . . . N2 N 0.4759(3) 0.2398(3) 1.06302(17) 0.0331(12) Uani 1 1 d . . . N3 N 0.4336(3) 0.3028(3) 0.99625(18) 0.0309(11) Uani 1 1 d . . . N4 N 0.3912(3) 0.3762(3) 0.93232(17) 0.0305(12) Uani 1 1 d . . . N5 N 0.3537(3) 0.4576(3) 0.87224(17) 0.0331(12) Uani 1 1 d . . . N6 N 0.3140(3) 0.5419(3) 0.81389(17) 0.0383(13) Uani 1 1 d . . . N7 N 0.6489(3) 0.2080(3) 1.08007(18) 0.0359(12) Uani 1 1 d . . . N8 N 0.6081(3) 0.3084(3) 1.03295(17) 0.0337(12) Uani 1 1 d . . . N9 N 0.5554(3) 0.4038(3) 0.98664(16) 0.0294(11) Uani 1 1 d . . . N10 N 0.4928(3) 0.4972(3) 0.94286(16) 0.0314(12) Uani 1 1 d . . . N11 N 0.4208(3) 0.5890(3) 0.90347(17) 0.0314(12) Uani 1 1 d . . . N12 N 0.3410(3) 0.6794(3) 0.86830(17) 0.0313(12) Uani 1 1 d . . . N13 N 0.6623(3) 0.1955(3) 1.18446(19) 0.0428(14) Uani 1 1 d . . . C1 C 0.5065(4) 0.1295(4) 1.1683(2) 0.0427(17) Uani 1 1 d . . . H1A H 0.5423 0.1286 1.1940 0.051 Uiso 1 1 calc R . . C2 C 0.4474(4) 0.0777(4) 1.1685(2) 0.0473(18) Uani 1 1 d . . . H2A H 0.4431 0.0411 1.1936 0.057 Uiso 1 1 calc R . . C3 C 0.3939(4) 0.0789(4) 1.1319(2) 0.0451(17) Uani 1 1 d . . . H3A H 0.3533 0.0423 1.1310 0.054 Uiso 1 1 calc R . . C4 C 0.4004(4) 0.1342(4) 1.0967(2) 0.0388(16) Uani 1 1 d . . . H4A H 0.3619 0.1391 1.0729 0.047 Uiso 1 1 calc R . . C5 C 0.4643(4) 0.1829(4) 1.0965(2) 0.0363(15) Uani 1 1 d . . . C6 C 0.4456(4) 0.2339(3) 1.0181(2) 0.0333(15) Uani 1 1 d . . . C7 C 0.4323(4) 0.1649(4) 0.9936(2) 0.0362(15) Uani 1 1 d . . . H7A H 0.4412 0.1171 1.0091 0.043 Uiso 1 1 calc R . . C8 C 0.4069(4) 0.1658(4) 0.9478(2) 0.0383(16) Uani 1 1 d . . . H8A H 0.3984 0.1187 0.9314 0.046 Uiso 1 1 calc R . . C9 C 0.3929(4) 0.2369(3) 0.9241(2) 0.0343(14) Uani 1 1 d . . . C10 C 0.4070(3) 0.3045(4) 0.9507(2) 0.0312(14) Uani 1 1 d . . . C11 C 0.3654(4) 0.2452(4) 0.8776(2) 0.0429(17) Uani 1 1 d . . . H11A H 0.3547 0.2006 0.8591 0.051 Uiso 1 1 calc R . . C12 C 0.3534(4) 0.3166(4) 0.8580(2) 0.0421(17) Uani 1 1 d . . . H12A H 0.3359 0.3216 0.8260 0.051 Uiso 1 1 calc R . . C13 C 0.3675(3) 0.3828(3) 0.8862(2) 0.0315(14) Uani 1 1 d . . . C14 C 0.3559(4) 0.4787(4) 0.8250(2) 0.0368(15) Uani 1 1 d . . . C15 C 0.4007(4) 0.4416(4) 0.7902(2) 0.0398(16) Uani 1 1 d . . . H15A H 0.4338 0.4005 0.7990 0.048 Uiso 1 1 calc R . . C16 C 0.3969(4) 0.4644(4) 0.7440(2) 0.0483(17) Uani 1 1 d . . . H16A H 0.4251 0.4380 0.7201 0.058 Uiso 1 1 calc R . . C17 C 0.3508(5) 0.5272(4) 0.7321(2) 0.053(2) Uani 1 1 d . . . H17A H 0.3467 0.5431 0.6997 0.064 Uiso 1 1 calc R . . C18 C 0.3115(4) 0.5660(4) 0.7671(2) 0.0484(18) Uani 1 1 d . . . H18A H 0.2822 0.6101 0.7590 0.058 Uiso 1 1 calc R . . C19 C 0.6819(4) 0.1384(4) 1.0850(2) 0.0395(16) Uani 1 1 d . . . H19A H 0.6826 0.1157 1.1158 0.047 Uiso 1 1 calc R . . C20 C 0.7141(4) 0.0992(4) 1.0485(3) 0.0493(18) Uani 1 1 d . . . H20A H 0.7378 0.0507 1.0538 0.059 Uiso 1 1 calc R . . C21 C 0.7120(4) 0.1315(4) 1.0027(3) 0.0473(18) Uani 1 1 d . . . H21A H 0.7336 0.1049 0.9763 0.057 Uiso 1 1 calc R . . C22 C 0.6789(4) 0.2005(4) 0.9966(2) 0.0414(16) Uani 1 1 d . . . H22A H 0.6765 0.2227 0.9656 0.050 Uiso 1 1 calc R . . C23 C 0.6473(3) 0.2406(4) 1.0362(2) 0.0344(15) Uani 1 1 d . . . C24 C 0.6177(4) 0.3612(3) 0.9961(2) 0.0324(14) Uani 1 1 d . . . C25 C 0.6890(3) 0.3759(4) 0.9740(2) 0.0359(15) Uani 1 1 d . . . H25A H 0.7330 0.3458 0.9814 0.043 Uiso 1 1 calc R . . C26 C 0.6932(4) 0.4349(4) 0.9414(2) 0.0399(16) Uani 1 1 d . . . H26A H 0.7410 0.4462 0.9266 0.048 Uiso 1 1 calc R . . C27 C 0.6280(3) 0.4787(4) 0.9296(2) 0.0335(14) Uani 1 1 d . . . C28 C 0.5594(3) 0.4612(4) 0.9528(2) 0.0299(14) Uani 1 1 d . . . C29 C 0.6274(4) 0.5421(4) 0.8970(2) 0.0364(15) Uani 1 1 d . . . H29A H 0.6732 0.5569 0.8810 0.044 Uiso 1 1 calc R . . C30 C 0.5616(4) 0.5808(4) 0.8892(2) 0.0346(14) Uani 1 1 d . . . H30A H 0.5618 0.6241 0.8685 0.042 Uiso 1 1 calc R . . C31 C 0.4916(4) 0.5579(3) 0.9114(2) 0.0325(14) Uani 1 1 d . . . C32 C 0.4097(4) 0.6645(3) 0.8901(2) 0.0326(14) Uani 1 1 d . . . C33 C 0.4599(4) 0.7254(4) 0.9009(2) 0.0379(15) Uani 1 1 d . . . H33A H 0.5073 0.7151 0.9164 0.046 Uiso 1 1 calc R . . C34 C 0.4414(4) 0.7982(4) 0.8892(3) 0.0447(17) Uani 1 1 d . . . H34A H 0.4742 0.8394 0.8982 0.054 Uiso 1 1 calc R . . C35 C 0.3753(4) 0.8128(4) 0.8646(3) 0.0469(18) Uani 1 1 d . . . H35A H 0.3634 0.8631 0.8537 0.056 Uiso 1 1 calc R . . C36 C 0.3264(4) 0.7520(4) 0.8559(2) 0.0398(16) Uani 1 1 d . . . H36A H 0.2792 0.7624 0.8400 0.048 Uiso 1 1 calc R . . C37 C 0.6903(4) 0.1567(4) 1.2117(2) 0.0429(17) Uani 1 1 d . . . C38 C 0.4803(5) -0.0660(5) 1.0449(3) 0.061(2) Uani 1 1 d . . . H38A H 0.4306 -0.0407 1.0377 0.073 Uiso 1 1 calc R . . H38B H 0.4901 -0.1049 1.0198 0.073 Uiso 1 1 calc R . . Cl1 Cl 0.55412(12) 0.00290(12) 1.04418(7) 0.0607(5) Uani 1 1 d . . . Cl2 Cl 0.47474(12) -0.11112(11) 1.10023(7) 0.0577(5) Uani 1 1 d . . . C39 C 0.6199(5) 0.3433(6) 0.8192(3) 0.079(3) Uani 1 1 d . . . H39A H 0.5938 0.3317 0.7886 0.094 Uiso 1 1 calc R . . H39B H 0.6313 0.3991 0.8196 0.094 Uiso 1 1 calc R . . Cl3 Cl 0.55857(16) 0.32267(16) 0.86500(9) 0.0877(8) Uani 1 1 d . . . Cl4 Cl 0.7034(2) 0.2941(2) 0.8214(3) 0.206(3) Uani 1 1 d . . . P1 P 0.45847(15) 0.22195(13) 0.72411(8) 0.0616(6) Uani 1 1 d . . . F1 F 0.3950(3) 0.2556(4) 0.69005(19) 0.0965(18) Uani 1 1 d . . . F2 F 0.3992(4) 0.2157(5) 0.7653(2) 0.129(3) Uani 1 1 d . . . F3 F 0.5218(4) 0.2303(3) 0.6821(2) 0.102(2) Uani 1 1 d . . . F4 F 0.4804(4) 0.3067(3) 0.7397(2) 0.106(2) Uani 1 1 d . . . F5 F 0.4404(5) 0.1367(3) 0.7080(2) 0.121(3) Uani 1 1 d . . . F6 F 0.5230(4) 0.1882(3) 0.7589(2) 0.104(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0352(5) 0.0409(5) 0.0284(4) 0.0028(4) -0.0017(4) -0.0002(4) Co2 0.0322(5) 0.0372(5) 0.0263(4) 0.0027(4) -0.0003(4) -0.0029(4) Co3 0.0319(4) 0.0330(5) 0.0253(4) 0.0003(3) 0.0005(3) -0.0021(4) S1 0.0803(15) 0.0556(12) 0.0438(11) 0.0094(9) -0.0090(10) 0.0219(11) N1 0.040(3) 0.034(3) 0.035(3) 0.001(2) 0.003(3) -0.003(2) N2 0.040(3) 0.036(3) 0.023(3) 0.006(2) 0.003(2) -0.005(2) N3 0.032(3) 0.027(3) 0.033(3) -0.001(2) -0.003(2) -0.003(2) N4 0.036(3) 0.028(3) 0.028(3) -0.002(2) -0.006(2) -0.002(2) N5 0.036(3) 0.037(3) 0.026(3) -0.005(2) -0.004(2) 0.003(2) N6 0.056(4) 0.036(3) 0.024(3) -0.002(2) -0.002(2) 0.000(3) N7 0.035(3) 0.041(3) 0.032(3) -0.001(3) 0.001(2) -0.005(2) N8 0.030(3) 0.044(3) 0.028(3) 0.002(2) 0.005(2) 0.003(2) N9 0.028(3) 0.036(3) 0.024(3) 0.001(2) 0.002(2) -0.003(2) N10 0.038(3) 0.034(3) 0.022(3) 0.004(2) 0.002(2) -0.009(2) N11 0.037(3) 0.032(3) 0.026(3) 0.000(2) -0.001(2) -0.009(2) N12 0.033(3) 0.036(3) 0.025(3) 0.005(2) 0.002(2) 0.000(2) N13 0.046(4) 0.054(4) 0.028(3) 0.006(3) -0.004(3) 0.006(3) C1 0.061(5) 0.042(4) 0.025(3) 0.012(3) 0.002(3) 0.005(4) C2 0.067(5) 0.039(4) 0.035(4) 0.009(3) 0.000(4) -0.010(4) C3 0.043(4) 0.042(4) 0.051(4) 0.005(3) -0.001(4) -0.011(3) C4 0.037(4) 0.047(4) 0.032(4) 0.009(3) -0.006(3) -0.006(3) C5 0.040(4) 0.039(4) 0.030(3) -0.001(3) 0.003(3) 0.001(3) C6 0.034(4) 0.029(3) 0.037(4) 0.002(3) 0.000(3) -0.003(3) C7 0.042(4) 0.030(3) 0.037(4) 0.005(3) 0.001(3) 0.003(3) C8 0.042(4) 0.034(4) 0.039(4) -0.002(3) -0.002(3) -0.007(3) C9 0.037(4) 0.034(4) 0.032(3) -0.002(3) -0.003(3) -0.005(3) C10 0.025(3) 0.038(4) 0.030(3) 0.000(3) -0.001(3) -0.001(3) C11 0.049(4) 0.041(4) 0.039(4) -0.013(3) -0.009(3) 0.001(3) C12 0.052(4) 0.043(4) 0.032(4) -0.002(3) -0.011(3) -0.006(3) C13 0.036(3) 0.031(3) 0.028(3) -0.003(3) 0.001(3) 0.000(3) C14 0.038(4) 0.038(4) 0.035(4) -0.005(3) -0.006(3) 0.000(3) C15 0.054(4) 0.033(4) 0.032(3) -0.003(3) -0.003(3) 0.006(3) C16 0.066(5) 0.050(4) 0.028(3) -0.003(3) 0.004(3) 0.000(4) C17 0.080(6) 0.052(5) 0.027(4) 0.008(3) 0.003(4) 0.002(4) C18 0.066(5) 0.052(4) 0.027(4) 0.005(3) -0.004(3) -0.001(4) C19 0.051(4) 0.035(4) 0.032(4) 0.001(3) 0.003(3) 0.004(3) C20 0.050(4) 0.045(4) 0.053(4) 0.007(4) -0.004(4) 0.009(4) C21 0.057(5) 0.034(4) 0.051(4) -0.013(3) 0.010(4) -0.001(3) C22 0.045(4) 0.049(4) 0.031(3) 0.004(3) 0.003(3) 0.000(3) C23 0.024(3) 0.041(4) 0.038(4) -0.004(3) 0.000(3) -0.001(3) C24 0.041(4) 0.038(3) 0.019(3) -0.004(3) 0.001(3) -0.001(3) C25 0.029(3) 0.038(4) 0.041(4) -0.003(3) 0.000(3) -0.003(3) C26 0.035(4) 0.040(4) 0.044(4) -0.005(3) 0.006(3) -0.012(3) C27 0.029(3) 0.039(4) 0.032(3) 0.003(3) -0.001(3) -0.004(3) C28 0.028(3) 0.037(4) 0.025(3) -0.004(3) -0.001(3) 0.001(3) C29 0.034(4) 0.040(4) 0.035(4) -0.005(3) 0.006(3) -0.002(3) C30 0.045(4) 0.035(4) 0.023(3) -0.002(3) 0.008(3) -0.015(3) C31 0.043(4) 0.031(3) 0.024(3) -0.003(3) -0.004(3) -0.003(3) C32 0.042(4) 0.036(4) 0.020(3) -0.002(3) 0.003(3) -0.004(3) C33 0.039(4) 0.039(4) 0.035(4) 0.002(3) 0.006(3) 0.001(3) C34 0.051(4) 0.033(4) 0.050(4) -0.006(3) 0.013(4) -0.006(3) C35 0.049(4) 0.035(4) 0.056(5) 0.009(3) 0.007(4) 0.002(3) C36 0.038(4) 0.044(4) 0.038(4) 0.004(3) 0.006(3) 0.000(3) C37 0.047(4) 0.050(4) 0.032(4) -0.006(3) 0.004(3) 0.000(3) C38 0.066(5) 0.064(5) 0.053(5) -0.003(4) -0.008(4) -0.003(4) Cl1 0.0606(12) 0.0623(12) 0.0594(12) 0.0159(10) 0.0032(10) 0.0017(10) Cl2 0.0598(12) 0.0579(12) 0.0554(11) -0.0012(9) 0.0139(9) -0.0015(9) C39 0.063(6) 0.090(7) 0.082(7) -0.001(6) -0.002(5) 0.004(5) Cl3 0.0969(18) 0.0979(18) 0.0683(15) -0.0175(13) 0.0063(13) -0.0301(15) Cl4 0.068(2) 0.098(3) 0.453(10) 0.042(4) 0.052(3) 0.0054(17) P1 0.0837(16) 0.0597(13) 0.0414(11) -0.0033(10) -0.0006(11) 0.0116(12) F1 0.085(4) 0.124(5) 0.080(4) 0.035(3) -0.036(3) -0.014(4) F2 0.134(6) 0.183(7) 0.070(4) 0.032(4) 0.042(4) 0.044(5) F3 0.132(5) 0.088(4) 0.085(4) 0.000(3) 0.039(4) 0.013(4) F4 0.161(6) 0.064(3) 0.093(4) -0.021(3) -0.033(4) 0.023(4) F5 0.228(8) 0.070(4) 0.064(4) 0.002(3) -0.007(4) -0.033(4) F6 0.112(5) 0.095(4) 0.106(5) 0.015(3) -0.030(4) 0.035(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.965(5) . ? Co1 N6 1.986(5) 7_557 ? Co1 N7 1.985(5) . ? Co1 N12 2.001(5) 7_557 ? Co1 N13 2.034(6) . ? Co1 Co2 2.3130(12) . ? Co2 N11 1.902(5) 7_557 ? Co2 N5 1.904(5) 7_557 ? Co2 N8 1.907(5) . ? Co2 N2 1.928(5) . ? Co2 Co3 2.2553(11) . ? Co3 N4 1.921(5) 7_557 ? Co3 N3 1.934(5) . ? Co3 N9 1.941(5) . ? Co3 N10 1.947(5) 7_557 ? Co3 Co3 2.2448(16) 7_557 ? S1 C37 1.652(8) . ? N1 C1 1.360(8) . ? N1 C5 1.367(8) . ? N2 C6 1.367(8) . ? N2 C5 1.377(8) . ? N3 C10 1.358(8) . ? N3 C6 1.361(8) . ? N4 C13 1.360(8) . ? N4 C10 1.377(8) . ? N4 Co3 1.921(5) 7_557 ? N5 C14 1.375(8) . ? N5 C13 1.379(8) . ? N5 Co2 1.904(5) 7_557 ? N6 C14 1.355(8) . ? N6 C18 1.375(8) . ? N6 Co1 1.986(5) 7_557 ? N7 C19 1.345(8) . ? N7 C23 1.353(8) . ? N8 C23 1.366(8) . ? N8 C24 1.392(8) . ? N9 C24 1.338(8) . ? N9 C28 1.377(8) . ? N10 C28 1.347(8) . ? N10 C31 1.374(8) . ? N10 Co3 1.947(5) 7_557 ? N11 C31 1.363(8) . ? N11 C32 1.379(8) . ? N11 Co2 1.902(5) 7_557 ? N12 C36 1.334(8) . ? N12 C32 1.367(8) . ? N12 Co1 2.001(5) 7_557 ? N13 C37 1.128(8) . ? C1 C2 1.367(10) . ? C2 C3 1.386(10) . ? C3 C4 1.382(9) . ? C4 C5 1.397(9) . ? C6 C7 1.403(9) . ? C7 C8 1.356(9) . ? C8 C9 1.424(9) . ? C9 C11 1.395(9) . ? C9 C10 1.413(9) . ? C11 C12 1.374(10) . ? C12 C13 1.419(9) . ? C14 C15 1.405(9) . ? C15 C16 1.354(9) . ? C16 C17 1.394(10) . ? C17 C18 1.374(10) . ? C19 C20 1.350(10) . ? C20 C21 1.403(10) . ? C21 C22 1.342(10) . ? C22 C23 1.422(9) . ? C24 C25 1.409(9) . ? C25 C26 1.375(9) . ? C26 C27 1.405(9) . ? C27 C28 1.394(9) . ? C27 C29 1.431(9) . ? C29 C30 1.345(9) . ? C30 C31 1.424(9) . ? C32 C33 1.405(9) . ? C33 C34 1.348(9) . ? C34 C35 1.365(10) . ? C35 C36 1.379(9) . ? C38 Cl2 1.740(8) . ? C38 Cl1 1.756(8) . ? C39 Cl4 1.688(10) . ? C39 Cl3 1.707(10) . ? P1 F2 1.550(6) . ? P1 F1 1.571(5) . ? P1 F5 1.581(6) . ? P1 F4 1.583(6) . ? P1 F6 1.597(6) . ? P1 F3 1.618(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N6 88.9(2) . 7_557 ? N1 Co1 N7 89.4(2) . . ? N6 Co1 N7 171.9(2) 7_557 . ? N1 Co1 N12 172.0(2) . 7_557 ? N6 Co1 N12 92.3(2) 7_557 7_557 ? N7 Co1 N12 88.4(2) . 7_557 ? N1 Co1 N13 94.1(2) . . ? N6 Co1 N13 93.9(2) 7_557 . ? N7 Co1 N13 94.1(2) . . ? N12 Co1 N13 93.8(2) 7_557 . ? N1 Co1 Co2 87.44(16) . . ? N6 Co1 Co2 86.71(15) 7_557 . ? N7 Co1 Co2 85.31(15) . . ? N12 Co1 Co2 84.70(14) 7_557 . ? N13 Co1 Co2 178.36(18) . . ? N11 Co2 N5 90.8(2) 7_557 7_557 ? N11 Co2 N8 88.8(2) 7_557 . ? N5 Co2 N8 178.3(2) 7_557 . ? N11 Co2 N2 177.8(2) 7_557 . ? N5 Co2 N2 89.8(2) 7_557 . ? N8 Co2 N2 90.5(2) . . ? N11 Co2 Co3 89.48(15) 7_557 . ? N5 Co2 Co3 88.99(15) 7_557 . ? N8 Co2 Co3 89.34(15) . . ? N2 Co2 Co3 88.43(15) . . ? N11 Co2 Co1 92.44(15) 7_557 . ? N5 Co2 Co1 90.37(15) 7_557 . ? N8 Co2 Co1 91.31(15) . . ? N2 Co2 Co1 89.66(15) . . ? Co3 Co2 Co1 177.98(5) . . ? N4 Co3 N3 89.5(2) 7_557 . ? N4 Co3 N9 179.1(2) 7_557 . ? N3 Co3 N9 91.1(2) . . ? N4 Co3 N10 91.3(2) 7_557 7_557 ? N3 Co3 N10 179.2(2) . 7_557 ? N9 Co3 N10 88.2(2) . 7_557 ? N4 Co3 Co3 90.48(15) 7_557 7_557 ? N3 Co3 Co3 89.93(15) . 7_557 ? N9 Co3 Co3 90.18(14) . 7_557 ? N10 Co3 Co3 89.83(15) 7_557 7_557 ? N4 Co3 Co2 89.84(14) 7_557 . ? N3 Co3 Co2 90.32(15) . . ? N9 Co3 Co2 89.50(14) . . ? N10 Co3 Co2 89.91(15) 7_557 . ? Co3 Co3 Co2 179.60(4) 7_557 . ? C1 N1 C5 117.8(6) . . ? C1 N1 Co1 120.6(5) . . ? C5 N1 Co1 121.6(4) . . ? C6 N2 C5 121.1(5) . . ? C6 N2 Co2 120.0(4) . . ? C5 N2 Co2 118.9(4) . . ? C10 N3 C6 119.6(5) . . ? C10 N3 Co3 119.7(4) . . ? C6 N3 Co3 120.3(4) . . ? C13 N4 C10 119.5(5) . . ? C13 N4 Co3 120.8(4) . 7_557 ? C10 N4 Co3 119.6(4) . 7_557 ? C14 N5 C13 121.4(5) . . ? C14 N5 Co2 118.9(4) . 7_557 ? C13 N5 Co2 119.7(4) . 7_557 ? C14 N6 C18 118.8(6) . . ? C14 N6 Co1 121.5(4) . 7_557 ? C18 N6 Co1 119.7(5) . 7_557 ? C19 N7 C23 118.6(6) . . ? C19 N7 Co1 119.3(4) . . ? C23 N7 Co1 122.0(4) . . ? C23 N8 C24 124.0(5) . . ? C23 N8 Co2 117.6(4) . . ? C24 N8 Co2 118.4(4) . . ? C24 N9 C28 119.7(5) . . ? C24 N9 Co3 120.6(4) . . ? C28 N9 Co3 118.9(4) . . ? C28 N10 C31 120.2(5) . . ? C28 N10 Co3 120.6(4) . 7_557 ? C31 N10 Co3 119.2(4) . 7_557 ? C31 N11 C32 123.3(5) . . ? C31 N11 Co2 120.7(4) . 7_557 ? C32 N11 Co2 115.4(4) . 7_557 ? C36 N12 C32 117.6(5) . . ? C36 N12 Co1 119.6(4) . 7_557 ? C32 N12 Co1 122.2(4) . 7_557 ? C37 N13 Co1 173.2(6) . . ? N1 C1 C2 122.9(7) . . ? C1 C2 C3 119.5(6) . . ? C4 C3 C2 118.8(6) . . ? C3 C4 C5 119.5(6) . . ? N1 C5 N2 114.7(6) . . ? N1 C5 C4 121.2(6) . . ? N2 C5 C4 123.8(6) . . ? N3 C6 N2 114.1(5) . . ? N3 C6 C7 120.5(6) . . ? N2 C6 C7 125.3(6) . . ? C8 C7 C6 120.4(6) . . ? C7 C8 C9 120.4(6) . . ? C11 C9 C10 117.7(6) . . ? C11 C9 C8 125.7(6) . . ? C10 C9 C8 116.6(5) . . ? N3 C10 N4 116.0(5) . . ? N3 C10 C9 122.4(5) . . ? N4 C10 C9 121.5(5) . . ? C12 C11 C9 121.2(6) . . ? C11 C12 C13 119.0(6) . . ? N4 C13 N5 113.7(5) . . ? N4 C13 C12 120.8(5) . . ? N5 C13 C12 125.3(6) . . ? N6 C14 N5 115.0(6) . . ? N6 C14 C15 120.8(6) . . ? N5 C14 C15 124.1(6) . . ? C16 C15 C14 120.0(6) . . ? C15 C16 C17 119.2(7) . . ? C18 C17 C16 119.9(6) . . ? N6 C18 C17 121.0(7) . . ? N7 C19 C20 123.6(6) . . ? C19 C20 C21 118.6(7) . . ? C22 C21 C20 119.1(7) . . ? C21 C22 C23 120.4(6) . . ? N7 C23 N8 115.7(5) . . ? N7 C23 C22 119.6(6) . . ? N8 C23 C22 124.4(6) . . ? N9 C24 N8 114.5(5) . . ? N9 C24 C25 121.7(6) . . ? N8 C24 C25 123.4(6) . . ? C26 C25 C24 118.3(6) . . ? C25 C26 C27 121.2(6) . . ? C28 C27 C26 117.5(6) . . ? C28 C27 C29 117.4(6) . . ? C26 C27 C29 125.1(6) . . ? N10 C28 N9 115.9(5) . . ? N10 C28 C27 122.5(5) . . ? N9 C28 C27 121.5(5) . . ? C30 C29 C27 119.7(6) . . ? C29 C30 C31 121.1(6) . . ? N11 C31 N10 115.1(5) . . ? N11 C31 C30 126.2(5) . . ? N10 C31 C30 118.8(6) . . ? N12 C32 N11 115.1(5) . . ? N12 C32 C33 119.8(6) . . ? N11 C32 C33 124.9(6) . . ? C34 C33 C32 120.5(7) . . ? C33 C34 C35 119.9(7) . . ? C34 C35 C36 117.9(7) . . ? N12 C36 C35 124.2(6) . . ? N13 C37 S1 179.1(7) . . ? Cl2 C38 Cl1 111.0(4) . . ? Cl4 C39 Cl3 113.8(6) . . ? F2 P1 F1 90.6(4) . . ? F2 P1 F5 90.8(4) . . ? F1 P1 F5 92.1(4) . . ? F2 P1 F4 91.2(4) . . ? F1 P1 F4 89.4(3) . . ? F5 P1 F4 177.5(5) . . ? F2 P1 F6 89.3(4) . . ? F1 P1 F6 179.7(4) . . ? F5 P1 F6 88.2(4) . . ? F4 P1 F6 90.3(3) . . ? F2 P1 F3 178.3(4) . . ? F1 P1 F3 90.2(3) . . ? F5 P1 F3 90.7(4) . . ? F4 P1 F3 87.3(4) . . ? F6 P1 F3 89.9(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.537 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.110 #===END data_ic10799(compd_3) _database_code_depnum_ccdc_archive 'CCDC 283616' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co6(bpyany)4(OTf)2)(OTf)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H60 Cl12 Co6 F12 N24 O12 S4' _chemical_formula_weight 2708.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 48.8644(4) _cell_length_b 16.91220(10) _cell_length_c 24.1983(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.5410(4) _cell_angle_gamma 90.00 _cell_volume 19867.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.811 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10832 _exptl_absorpt_coefficient_mu 1.481 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_T_max 0.744 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 91642 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -62 _diffrn_reflns_limit_h_max 63 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 27.50 _reflns_number_total 22806 _reflns_number_gt 15502 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0878P)^2^+66.6377P] 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 22806 _refine_ls_number_parameters 1369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0896 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1731 _refine_ls_wR_factor_gt 0.1552 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.023 _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 0.657151(11) 0.55307(3) 0.47337(2) 0.02024(13) Uani 1 1 d . . . Co2 Co 0.644570(10) 0.43597(3) 0.43178(2) 0.01932(12) Uani 1 1 d . . . Co3 Co 0.631847(10) 0.31924(3) 0.39315(2) 0.01724(12) Uani 1 1 d . . . Co4 Co 0.619040(10) 0.20140(3) 0.35373(2) 0.01724(12) Uani 1 1 d . . . Co5 Co 0.606261(10) 0.08554(3) 0.31355(2) 0.01954(12) Uani 1 1 d . . . Co6 Co 0.592352(11) -0.03300(3) 0.27398(2) 0.02084(13) Uani 1 1 d . . . N1 N 0.69489(7) 0.52601(19) 0.46018(13) 0.0224(7) Uani 1 1 d . . . N2 N 0.67672(6) 0.43610(19) 0.39383(13) 0.0206(7) Uani 1 1 d . . . N3 N 0.65749(6) 0.33561(18) 0.33876(13) 0.0194(7) Uani 1 1 d . . . N4 N 0.63671(6) 0.22996(19) 0.28889(12) 0.0190(7) Uani 1 1 d . . . N5 N 0.61352(6) 0.12672(19) 0.24345(13) 0.0212(7) Uani 1 1 d . . . N6 N 0.58606(7) 0.02597(19) 0.20288(13) 0.0230(7) Uani 1 1 d . . . N7 N 0.66240(7) 0.49463(19) 0.54384(13) 0.0217(7) Uani 1 1 d . . . N8 N 0.66454(7) 0.37997(19) 0.49260(13) 0.0217(7) Uani 1 1 d . . . N9 N 0.66075(6) 0.26627(18) 0.44037(12) 0.0188(7) Uani 1 1 d . . . N10 N 0.65333(6) 0.15404(18) 0.38541(13) 0.0196(7) Uani 1 1 d . . . N11 N 0.64360(6) 0.04942(19) 0.32587(13) 0.0215(7) Uani 1 1 d . . . N12 N 0.63121(7) -0.05072(19) 0.26246(14) 0.0234(7) Uani 1 1 d . . . N13 N 0.61828(7) 0.56852(19) 0.48425(14) 0.0229(7) Uani 1 1 d . . . N14 N 0.61217(7) 0.43428(19) 0.46942(13) 0.0222(7) Uani 1 1 d . . . N15 N 0.60677(6) 0.30242(18) 0.44797(13) 0.0189(7) Uani 1 1 d . . . N16 N 0.60188(6) 0.17265(18) 0.41887(13) 0.0192(7) Uani 1 1 d . . . N17 N 0.59940(7) 0.04545(19) 0.38514(13) 0.0218(7) Uani 1 1 d . . . N18 N 0.60042(7) -0.07999(19) 0.34798(14) 0.0234(7) Uani 1 1 d . . . N19 N 0.65118(7) 0.59940(19) 0.39737(13) 0.0211(7) Uani 1 1 d . . . N20 N 0.62459(6) 0.49019(19) 0.37106(13) 0.0216(7) Uani 1 1 d . . . N21 N 0.60324(6) 0.37260(19) 0.34510(13) 0.0198(7) Uani 1 1 d . . . N22 N 0.58509(6) 0.24959(19) 0.32058(13) 0.0196(7) Uani 1 1 d . . . N23 N 0.56958(6) 0.12339(19) 0.30136(14) 0.0220(7) Uani 1 1 d . . . N24 N 0.55519(7) -0.0067(2) 0.29254(13) 0.0228(7) Uani 1 1 d . . . C1 C 0.71649(8) 0.5590(2) 0.49189(17) 0.0256(9) Uani 1 1 d . . . H1 H 0.7129 0.5946 0.5206 0.031 Uiso 1 1 calc R . . C2 C 0.74318(9) 0.5434(3) 0.48438(18) 0.0300(10) Uani 1 1 d . . . H2 H 0.7578 0.5690 0.5066 0.036 Uiso 1 1 calc R . . C3 C 0.74858(8) 0.4895(3) 0.44363(18) 0.0300(9) Uani 1 1 d . . . H3 H 0.7670 0.4777 0.4377 0.036 Uiso 1 1 calc R . . C4 C 0.72693(8) 0.4534(2) 0.41202(17) 0.0258(9) Uani 1 1 d . . . H4 H 0.7303 0.4157 0.3846 0.031 Uiso 1 1 calc R . . C5 C 0.69986(8) 0.4726(2) 0.42046(16) 0.0216(8) Uani 1 1 d . . . C6 C 0.67642(8) 0.3952(2) 0.34564(16) 0.0212(8) Uani 1 1 d . . . C7 C 0.69277(8) 0.4131(2) 0.30216(16) 0.0243(8) Uani 1 1 d . . . H7 H 0.7051 0.4567 0.3057 0.029 Uiso 1 1 calc R . . C8 C 0.69077(8) 0.3682(2) 0.25616(17) 0.0259(9) Uani 1 1 d . . . H8 H 0.7020 0.3799 0.2277 0.031 Uiso 1 1 calc R . . C9 C 0.67222(8) 0.3037(2) 0.24928(16) 0.0227(8) Uani 1 1 d . . . C10 C 0.65563(7) 0.2900(2) 0.29215(16) 0.0197(8) Uani 1 1 d . . . C11 C 0.66884(9) 0.2532(3) 0.20277(17) 0.0283(9) Uani 1 1 d . . . H11 H 0.6803 0.2595 0.1739 0.034 Uiso 1 1 calc R . . C12 C 0.64927(9) 0.1954(3) 0.19882(17) 0.0275(9) Uani 1 1 d . . . H12 H 0.6468 0.1626 0.1668 0.033 Uiso 1 1 calc R . . C13 C 0.63279(8) 0.1843(2) 0.24220(16) 0.0218(8) Uani 1 1 d . . . C14 C 0.59796(8) 0.0984(2) 0.19676(16) 0.0225(8) Uani 1 1 d . . . C15 C 0.59206(9) 0.1416(3) 0.14776(18) 0.0300(9) Uani 1 1 d . . . H15 H 0.6001 0.1921 0.1442 0.036 Uiso 1 1 calc R . . C16 C 0.57450(10) 0.1109(3) 0.10446(18) 0.0350(10) Uani 1 1 d . . . H16 H 0.5705 0.1399 0.0709 0.042 Uiso 1 1 calc R . . C17 C 0.56268(9) 0.0369(3) 0.11070(18) 0.0302(10) Uani 1 1 d . . . H17 H 0.5508 0.0141 0.0812 0.036 Uiso 1 1 calc R . . C18 C 0.56855(8) -0.0021(3) 0.15973(17) 0.0259(9) Uani 1 1 d . . . H18 H 0.5599 -0.0517 0.1641 0.031 Uiso 1 1 calc R . . C19 C 0.66073(9) 0.5313(3) 0.59292(17) 0.0280(9) Uani 1 1 d . . . H19 H 0.6563 0.5860 0.5924 0.034 Uiso 1 1 calc R . . C20 C 0.66501(9) 0.4942(3) 0.64315(17) 0.0320(10) Uani 1 1 d . . . H20 H 0.6639 0.5224 0.6767 0.038 Uiso 1 1 calc R . . C21 C 0.67113(10) 0.4137(3) 0.64384(18) 0.0343(10) Uani 1 1 d . . . H21 H 0.6750 0.3866 0.6782 0.041 Uiso 1 1 calc R . . C22 C 0.67153(9) 0.3737(3) 0.59453(17) 0.0301(9) Uani 1 1 d . . . H22 H 0.6749 0.3184 0.5945 0.036 Uiso 1 1 calc R . . C23 C 0.66689(8) 0.4153(2) 0.54421(16) 0.0232(8) Uani 1 1 d . . . C24 C 0.67475(8) 0.3070(2) 0.48298(16) 0.0219(8) Uani 1 1 d . . . C25 C 0.69930(8) 0.2747(2) 0.51152(17) 0.0259(9) Uani 1 1 d . . . H25 H 0.7095 0.3039 0.5405 0.031 Uiso 1 1 calc R . . C26 C 0.70821(8) 0.2021(3) 0.49744(17) 0.0271(9) Uani 1 1 d . . . H26 H 0.7247 0.1810 0.5163 0.032 Uiso 1 1 calc R . . C27 C 0.69310(8) 0.1578(2) 0.45494(16) 0.0229(8) Uani 1 1 d . . . C28 C 0.66923(8) 0.1926(2) 0.42727(15) 0.0196(8) Uani 1 1 d . . . C29 C 0.70024(9) 0.0816(2) 0.43785(17) 0.0275(9) Uani 1 1 d . . . H29 H 0.7161 0.0561 0.4560 0.033 Uiso 1 1 calc R . . C30 C 0.68450(8) 0.0437(2) 0.39533(17) 0.0262(9) Uani 1 1 d . . . H30 H 0.6894 -0.0078 0.3842 0.031 Uiso 1 1 calc R . . C31 C 0.66073(8) 0.0821(2) 0.36800(16) 0.0221(8) Uani 1 1 d . . . C32 C 0.65180(8) -0.0072(2) 0.28963(16) 0.0241(8) Uani 1 1 d . . . C33 C 0.67908(9) -0.0156(3) 0.27735(18) 0.0305(10) Uani 1 1 d . . . H33 H 0.6931 0.0189 0.2936 0.037 Uiso 1 1 calc R . . C34 C 0.68524(9) -0.0746(3) 0.24133(19) 0.0351(11) Uani 1 1 d . . . H34 H 0.7037 -0.0824 0.2336 0.042 Uiso 1 1 calc R . . C35 C 0.66431(9) -0.1224(3) 0.21648(19) 0.0353(10) Uani 1 1 d . . . H35 H 0.6683 -0.1651 0.1932 0.042 Uiso 1 1 calc R . . C36 C 0.63778(9) -0.1069(2) 0.22616(17) 0.0276(9) Uani 1 1 d . . . H36 H 0.6233 -0.1367 0.2066 0.033 Uiso 1 1 calc R . . C37 C 0.60821(9) 0.6406(2) 0.49436(17) 0.0264(9) Uani 1 1 d . . . H37 H 0.6205 0.6844 0.4963 0.032 Uiso 1 1 calc R . . C38 C 0.58108(9) 0.6542(3) 0.50200(18) 0.0316(10) Uani 1 1 d . . . H38 H 0.5749 0.7059 0.5097 0.038 Uiso 1 1 calc R . . C39 C 0.56306(9) 0.5909(3) 0.49823(19) 0.0318(10) Uani 1 1 d . . . H39 H 0.5442 0.5986 0.5032 0.038 Uiso 1 1 calc R . . C40 C 0.57270(8) 0.5162(3) 0.48713(18) 0.0287(9) Uani 1 1 d . . . H40 H 0.5604 0.4725 0.4831 0.034 Uiso 1 1 calc R . . C41 C 0.60082(8) 0.5057(2) 0.48182(16) 0.0233(8) Uani 1 1 d . . . C42 C 0.60123(8) 0.3629(2) 0.48172(16) 0.0214(8) Uani 1 1 d . . . C43 C 0.58660(9) 0.3489(2) 0.52843(17) 0.0255(9) Uani 1 1 d . . . H43 H 0.5832 0.3911 0.5527 0.031 Uiso 1 1 calc R . . C44 C 0.57748(9) 0.2747(2) 0.53819(17) 0.0288(9) Uani 1 1 d . . . H44 H 0.5681 0.2650 0.5698 0.035 Uiso 1 1 calc R . . C45 C 0.58185(8) 0.2123(2) 0.50189(17) 0.0256(9) Uani 1 1 d . . . C46 C 0.59664(7) 0.2291(2) 0.45665(15) 0.0196(8) Uani 1 1 d . . . C47 C 0.57228(9) 0.1342(2) 0.50657(18) 0.0282(9) Uani 1 1 d . . . H47 H 0.5619 0.1209 0.5362 0.034 Uiso 1 1 calc R . . C48 C 0.57761(9) 0.0779(2) 0.46953(17) 0.0275(9) Uani 1 1 d . . . H48 H 0.5709 0.0256 0.4731 0.033 Uiso 1 1 calc R . . C49 C 0.59320(8) 0.0970(2) 0.42520(16) 0.0223(8) Uani 1 1 d . . . C50 C 0.60282(8) -0.0343(2) 0.39459(16) 0.0228(8) Uani 1 1 d . . . C51 C 0.61074(9) -0.0686(2) 0.44699(17) 0.0282(9) Uani 1 1 d . . . H51 H 0.6132 -0.0362 0.4793 0.034 Uiso 1 1 calc R . . C52 C 0.61491(10) -0.1482(3) 0.45151(19) 0.0333(10) Uani 1 1 d . . . H52 H 0.6197 -0.1716 0.4870 0.040 Uiso 1 1 calc R . . C53 C 0.61217(10) -0.1944(3) 0.40418(18) 0.0320(10) Uani 1 1 d . . . H53 H 0.6149 -0.2500 0.4066 0.038 Uiso 1 1 calc R . . C54 C 0.60537(9) -0.1585(3) 0.35351(18) 0.0293(9) Uani 1 1 d . . . H54 H 0.6041 -0.1902 0.3209 0.035 Uiso 1 1 calc R . . C55 C 0.66446(9) 0.6657(2) 0.38416(17) 0.0268(9) Uani 1 1 d . . . H55 H 0.6768 0.6901 0.4122 0.032 Uiso 1 1 calc R . . C56 C 0.66098(9) 0.6997(3) 0.33229(18) 0.0320(10) Uani 1 1 d . . . H56 H 0.6703 0.7471 0.3249 0.038 Uiso 1 1 calc R . . C57 C 0.64349(9) 0.6631(3) 0.29103(18) 0.0318(10) Uani 1 1 d . . . H57 H 0.6404 0.6857 0.2549 0.038 Uiso 1 1 calc R . . C58 C 0.63068(9) 0.5945(3) 0.30251(18) 0.0303(10) Uani 1 1 d . . . H58 H 0.6191 0.5683 0.2740 0.036 Uiso 1 1 calc R . . C59 C 0.63445(8) 0.5626(2) 0.35616(17) 0.0237(8) Uani 1 1 d . . . C60 C 0.60275(8) 0.4525(2) 0.34189(16) 0.0234(8) Uani 1 1 d . . . C61 C 0.57974(8) 0.4920(2) 0.31265(18) 0.0273(9) Uani 1 1 d . . . H61 H 0.5791 0.5481 0.3117 0.033 Uiso 1 1 calc R . . C62 C 0.55892(9) 0.4493(3) 0.28628(18) 0.0291(9) Uani 1 1 d . . . H62 H 0.5436 0.4758 0.2670 0.035 Uiso 1 1 calc R . . C63 C 0.55955(8) 0.3655(2) 0.28681(17) 0.0242(8) Uani 1 1 d . . . C64 C 0.58240(8) 0.3296(2) 0.31741(15) 0.0204(8) Uani 1 1 d . . . C65 C 0.53938(8) 0.3163(3) 0.25928(19) 0.0303(10) Uani 1 1 d . . . H65 H 0.5241 0.3388 0.2371 0.036 Uiso 1 1 calc R . . C66 C 0.54158(8) 0.2360(3) 0.26411(18) 0.0283(9) Uani 1 1 d . . . H66 H 0.5276 0.2028 0.2462 0.034 Uiso 1 1 calc R . . C67 C 0.56481(8) 0.2027(2) 0.29601(16) 0.0219(8) Uani 1 1 d . . . C68 C 0.54835(8) 0.0692(2) 0.30354(16) 0.0226(8) Uani 1 1 d . . . C69 C 0.52317(8) 0.0876(3) 0.32168(18) 0.0300(9) Uani 1 1 d . . . H69 H 0.5189 0.1409 0.3297 0.036 Uiso 1 1 calc R . . C70 C 0.50457(9) 0.0288(3) 0.3280(2) 0.0342(10) Uani 1 1 d . . . H70 H 0.4872 0.0409 0.3400 0.041 Uiso 1 1 calc R . . C71 C 0.51131(9) -0.0492(3) 0.31655(19) 0.0338(10) Uani 1 1 d . . . H71 H 0.4986 -0.0909 0.3201 0.041 Uiso 1 1 calc R . . C72 C 0.53660(9) -0.0641(2) 0.30010(17) 0.0270(9) Uani 1 1 d . . . H72 H 0.5414 -0.1175 0.2936 0.032 Uiso 1 1 calc R . . C73 C 0.69483(11) 0.8037(3) 0.5134(2) 0.0413(12) Uani 1 1 d . . . C74 C 0.55205(11) -0.2817(3) 0.2404(2) 0.0460(13) Uani 1 1 d . . . C75 C 0.75791(10) 0.7217(3) 0.1497(2) 0.0393(11) Uani 1 1 d . . . C76 C 0.48383(16) 0.3006(6) 0.0752(3) 0.087(3) Uani 1 1 d . . . S1 S 0.67678(2) 0.72842(6) 0.54944(4) 0.0256(2) Uani 1 1 d . . . S2 S 0.56996(2) -0.21381(7) 0.19790(5) 0.0337(3) Uani 1 1 d . . . S3 S 0.73152(2) 0.78508(7) 0.17358(5) 0.0328(3) Uani 1 1 d . . . S4 S 0.51779(3) 0.28763(9) 0.10541(6) 0.0527(4) Uani 1 1 d . . . F1 F 0.67939(7) 0.83106(18) 0.46910(13) 0.0532(8) Uani 1 1 d . . . F2 F 0.70166(8) 0.86448(19) 0.54644(15) 0.0690(10) Uani 1 1 d . . . F3 F 0.71742(6) 0.7739(2) 0.49653(14) 0.0565(8) Uani 1 1 d . . . F4 F 0.56836(8) -0.3004(2) 0.28694(15) 0.0686(10) Uani 1 1 d . . . F5 F 0.54575(8) -0.34863(18) 0.21371(17) 0.0705(10) Uani 1 1 d . . . F6 F 0.52946(6) -0.25086(19) 0.25471(15) 0.0608(9) Uani 1 1 d . . . F7 F 0.77056(9) 0.6783(3) 0.18970(16) 0.0931(14) Uani 1 1 d . . . F8 F 0.74795(7) 0.6724(2) 0.10996(16) 0.0691(11) Uani 1 1 d . . . F9 F 0.77791(8) 0.7621(2) 0.13049(18) 0.0810(12) Uani 1 1 d . . . F10 F 0.47616(11) 0.2372(4) 0.0422(3) 0.145(2) Uani 1 1 d . . . F11 F 0.48080(12) 0.3618(4) 0.0406(3) 0.143(2) Uani 1 1 d . . . F12 F 0.46487(10) 0.3082(6) 0.1052(2) 0.195(4) Uani 1 1 d . . . O1 O 0.66961(6) 0.67039(16) 0.50597(11) 0.0260(6) Uani 1 1 d . . . O2 O 0.65360(6) 0.76866(18) 0.56748(12) 0.0320(7) Uani 1 1 d . . . O3 O 0.69738(6) 0.70141(19) 0.59241(12) 0.0354(7) Uani 1 1 d . . . O4 O 0.57712(6) -0.14859(17) 0.23620(12) 0.0295(7) Uani 1 1 d . . . O5 O 0.54948(8) -0.1938(2) 0.15266(15) 0.0484(9) Uani 1 1 d . . . O6 O 0.59316(8) -0.2578(2) 0.18408(16) 0.0533(10) Uani 1 1 d . . . O7 O 0.71185(10) 0.7324(3) 0.1890(3) 0.100(2) Uani 1 1 d . . . O8 O 0.74621(8) 0.8272(3) 0.2170(2) 0.0925(19) Uani 1 1 d . . . O9 O 0.72299(12) 0.8311(3) 0.12643(18) 0.0858(17) Uani 1 1 d . . . O10 O 0.53344(9) 0.2741(3) 0.0611(2) 0.0922(18) Uani 1 1 d . . . O11 O 0.51563(10) 0.2224(3) 0.14208(17) 0.0768(14) Uani 1 1 d . . . O12 O 0.52361(17) 0.3617(3) 0.1332(3) 0.135(3) Uani 1 1 d . . . C77 C 0.66484(12) 0.0629(3) 0.5750(3) 0.0531(14) Uani 1 1 d . . . H77A H 0.6797 0.0752 0.6050 0.064 Uiso 1 1 calc R . . H77B H 0.6735 0.0481 0.5413 0.064 Uiso 1 1 calc R . . C78 C 0.7426(2) 0.8437(6) 0.6775(5) 0.138(5) Uani 1 1 d . . . H78A H 0.7422 0.8106 0.7111 0.166 Uiso 1 1 calc R . . H78B H 0.7361 0.8101 0.6450 0.166 Uiso 1 1 calc R . . C79 C 0.58674(16) 0.4321(4) 0.1454(3) 0.074(2) Uani 1 1 d . . . H79A H 0.5906 0.4235 0.1065 0.089 Uiso 1 1 calc R . . H79B H 0.5677 0.4140 0.1484 0.089 Uiso 1 1 calc R . . C80 C 0.75010(13) 0.8822(5) 0.3416(2) 0.076(2) Uani 1 1 d . . . H80A H 0.7672 0.8551 0.3571 0.092 Uiso 1 1 calc R . . H80B H 0.7460 0.8664 0.3022 0.092 Uiso 1 1 calc R . . C81 C 0.4986(4) 0.5326(7) 0.3732(5) 0.188(7) Uani 1 1 d . . . H81A H 0.5104 0.4863 0.3843 0.226 Uiso 1 1 calc R . . H81B H 0.4840 0.5161 0.3437 0.226 Uiso 1 1 calc R . . C82 C 0.51220(18) 0.8194(7) 0.4425(4) 0.123(4) Uani 1 1 d . . . H82A H 0.5110 0.7806 0.4727 0.148 Uiso 1 1 calc R . . H82B H 0.4986 0.8043 0.4107 0.148 Uiso 1 1 calc R . . Cl1 Cl 0.64422(3) 0.14660(10) 0.56082(7) 0.0633(4) Uani 1 1 d . . . Cl2 Cl 0.64532(4) -0.01702(10) 0.59537(7) 0.0760(5) Uani 1 1 d . . . Cl3 Cl 0.71970(6) 0.91730(18) 0.68060(11) 0.1241(10) Uani 1 1 d . . . Cl4 Cl 0.77512(5) 0.86886(17) 0.67252(17) 0.1530(14) Uani 1 1 d . . . Cl5 Cl 0.58897(4) 0.53275(9) 0.16018(6) 0.0625(4) Uani 1 1 d . . . Cl6 Cl 0.60964(3) 0.37559(10) 0.18982(8) 0.0687(5) Uani 1 1 d . . . Cl7 Cl 0.72265(4) 0.85161(10) 0.37885(7) 0.0673(4) Uani 1 1 d . . . Cl8 Cl 0.75505(4) 0.98204(15) 0.34535(11) 0.1037(7) Uani 1 1 d . . . Cl9 Cl 0.48438(7) 0.5700(3) 0.42952(15) 0.1775(16) Uani 1 1 d . . . Cl10 Cl 0.51792(9) 0.6075(3) 0.3497(2) 0.253(3) Uani 1 1 d . . . Cl11 Cl 0.50419(6) 0.9146(2) 0.46600(13) 0.1460(12) Uani 1 1 d . . . Cl12 Cl 0.54430(5) 0.8172(3) 0.42246(16) 0.202(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0220(3) 0.0211(3) 0.0177(3) -0.0005(2) 0.0026(2) -0.0011(2) Co2 0.0207(3) 0.0207(3) 0.0164(3) -0.0003(2) 0.0014(2) -0.0008(2) Co3 0.0174(2) 0.0206(3) 0.0138(2) 0.0002(2) 0.00157(19) 0.0007(2) Co4 0.0169(2) 0.0209(3) 0.0140(3) -0.0007(2) 0.00163(19) 0.0014(2) Co5 0.0195(3) 0.0220(3) 0.0168(3) -0.0027(2) 0.0010(2) 0.0017(2) Co6 0.0214(3) 0.0223(3) 0.0186(3) -0.0028(2) 0.0012(2) 0.0025(2) N1 0.0222(16) 0.0226(17) 0.0214(17) 0.0017(13) -0.0013(13) -0.0006(14) N2 0.0208(16) 0.0235(17) 0.0172(16) -0.0014(13) 0.0002(13) -0.0032(13) N3 0.0212(16) 0.0224(17) 0.0146(16) 0.0008(13) 0.0025(13) 0.0021(13) N4 0.0195(15) 0.0229(17) 0.0145(15) -0.0008(13) 0.0019(12) 0.0018(13) N5 0.0212(16) 0.0243(17) 0.0176(16) -0.0012(13) 0.0003(13) 0.0011(14) N6 0.0229(16) 0.0271(18) 0.0185(17) -0.0056(14) 0.0002(13) 0.0027(14) N7 0.0238(16) 0.0240(17) 0.0177(16) -0.0013(13) 0.0038(13) -0.0022(14) N8 0.0256(17) 0.0223(17) 0.0168(16) 0.0000(13) 0.0003(13) -0.0017(14) N9 0.0190(15) 0.0226(17) 0.0144(16) 0.0009(13) -0.0001(12) 0.0005(13) N10 0.0196(15) 0.0215(17) 0.0174(16) 0.0014(13) 0.0002(12) 0.0021(13) N11 0.0207(16) 0.0258(17) 0.0171(16) -0.0018(13) -0.0011(13) 0.0047(14) N12 0.0272(17) 0.0225(17) 0.0202(17) -0.0018(13) 0.0018(14) 0.0051(14) N13 0.0250(17) 0.0223(17) 0.0211(17) -0.0006(13) 0.0022(14) 0.0009(14) N14 0.0258(17) 0.0216(17) 0.0196(17) -0.0030(13) 0.0045(14) -0.0019(14) N15 0.0211(16) 0.0200(16) 0.0157(16) 0.0003(13) 0.0028(13) 0.0012(13) N16 0.0206(16) 0.0215(17) 0.0150(16) -0.0013(13) -0.0001(12) -0.0017(13) N17 0.0273(17) 0.0223(17) 0.0160(16) -0.0009(13) 0.0031(13) 0.0004(14) N18 0.0265(17) 0.0233(17) 0.0210(17) -0.0014(14) 0.0049(14) 0.0013(14) N19 0.0222(16) 0.0217(17) 0.0198(17) 0.0017(13) 0.0041(13) 0.0006(14) N20 0.0243(17) 0.0208(17) 0.0193(17) -0.0004(13) 0.0008(13) 0.0004(14) N21 0.0215(16) 0.0213(17) 0.0166(16) -0.0015(13) 0.0015(13) 0.0008(13) N22 0.0188(15) 0.0233(17) 0.0166(16) -0.0007(13) 0.0014(12) 0.0027(13) N23 0.0181(15) 0.0236(17) 0.0238(18) -0.0043(14) 0.0005(13) 0.0008(13) N24 0.0224(16) 0.0270(18) 0.0186(17) -0.0046(14) -0.0001(13) -0.0012(14) C1 0.028(2) 0.026(2) 0.023(2) -0.0018(17) 0.0001(17) -0.0026(17) C2 0.025(2) 0.030(2) 0.033(2) -0.0010(18) -0.0039(18) -0.0071(18) C3 0.021(2) 0.035(2) 0.034(2) 0.0005(19) -0.0007(17) -0.0001(18) C4 0.025(2) 0.025(2) 0.026(2) -0.0016(17) -0.0008(17) 0.0005(17) C5 0.0222(19) 0.023(2) 0.020(2) 0.0014(16) 0.0013(15) 0.0003(16) C6 0.0187(18) 0.024(2) 0.021(2) 0.0049(16) 0.0022(15) 0.0031(16) C7 0.024(2) 0.026(2) 0.023(2) 0.0034(17) 0.0035(16) -0.0023(17) C8 0.0217(19) 0.035(2) 0.022(2) 0.0066(17) 0.0049(16) 0.0014(17) C9 0.0225(19) 0.029(2) 0.0169(19) 0.0045(16) 0.0018(15) 0.0039(17) C10 0.0170(18) 0.024(2) 0.0184(19) 0.0012(15) 0.0013(14) 0.0040(16) C11 0.029(2) 0.038(2) 0.019(2) 0.0007(18) 0.0087(17) 0.0014(19) C12 0.030(2) 0.034(2) 0.019(2) -0.0035(17) 0.0030(17) 0.0009(18) C13 0.0216(19) 0.026(2) 0.0173(19) 0.0003(16) -0.0002(15) 0.0056(16) C14 0.0216(19) 0.026(2) 0.019(2) -0.0047(16) -0.0001(15) 0.0071(16) C15 0.034(2) 0.028(2) 0.026(2) -0.0013(18) -0.0020(18) -0.0011(19) C16 0.043(3) 0.040(3) 0.020(2) 0.0019(19) -0.0047(19) 0.002(2) C17 0.030(2) 0.032(2) 0.026(2) -0.0074(18) -0.0048(18) 0.0028(19) C18 0.023(2) 0.028(2) 0.025(2) -0.0091(17) -0.0004(16) 0.0037(17) C19 0.032(2) 0.027(2) 0.025(2) -0.0062(17) 0.0067(18) -0.0056(18) C20 0.041(2) 0.038(3) 0.017(2) -0.0048(18) 0.0058(18) -0.006(2) C21 0.050(3) 0.035(2) 0.018(2) 0.0032(18) 0.0006(19) -0.004(2) C22 0.041(2) 0.025(2) 0.023(2) 0.0027(17) 0.0039(19) -0.0007(19) C23 0.0234(19) 0.027(2) 0.019(2) 0.0021(16) 0.0013(16) -0.0036(17) C24 0.0240(19) 0.023(2) 0.0178(19) 0.0021(15) -0.0001(15) -0.0033(16) C25 0.025(2) 0.031(2) 0.020(2) -0.0012(17) -0.0068(16) -0.0003(17) C26 0.021(2) 0.034(2) 0.024(2) 0.0021(18) -0.0060(16) 0.0027(17) C27 0.0208(19) 0.028(2) 0.0186(19) 0.0029(16) -0.0010(15) -0.0002(16) C28 0.0191(18) 0.024(2) 0.0158(19) 0.0040(15) 0.0017(15) -0.0004(15) C29 0.025(2) 0.030(2) 0.027(2) 0.0020(18) -0.0013(17) 0.0087(18) C30 0.026(2) 0.026(2) 0.025(2) -0.0023(17) -0.0022(17) 0.0060(17) C31 0.0200(19) 0.025(2) 0.021(2) 0.0004(16) 0.0015(15) 0.0039(16) C32 0.0239(19) 0.028(2) 0.020(2) -0.0012(16) -0.0009(16) 0.0049(17) C33 0.024(2) 0.039(2) 0.028(2) -0.0071(19) 0.0012(17) 0.0047(19) C34 0.026(2) 0.044(3) 0.035(3) -0.008(2) 0.0066(19) 0.009(2) C35 0.038(2) 0.036(3) 0.032(2) -0.011(2) 0.005(2) 0.010(2) C36 0.032(2) 0.027(2) 0.024(2) -0.0067(17) 0.0038(17) 0.0059(18) C37 0.029(2) 0.024(2) 0.026(2) 0.0019(17) 0.0026(17) -0.0004(17) C38 0.033(2) 0.029(2) 0.033(2) -0.0008(19) 0.0037(19) 0.0043(19) C39 0.027(2) 0.033(2) 0.036(3) -0.0019(19) 0.0066(19) 0.0050(19) C40 0.023(2) 0.032(2) 0.032(2) -0.0024(18) 0.0045(17) -0.0028(18) C41 0.026(2) 0.027(2) 0.0167(19) -0.0006(16) 0.0005(16) 0.0003(17) C42 0.0216(19) 0.024(2) 0.0177(19) -0.0029(15) 0.0005(15) 0.0002(16) C43 0.033(2) 0.023(2) 0.022(2) -0.0045(16) 0.0089(17) -0.0015(17) C44 0.035(2) 0.030(2) 0.023(2) -0.0015(17) 0.0132(18) -0.0031(19) C45 0.029(2) 0.028(2) 0.021(2) 0.0002(17) 0.0062(17) -0.0013(18) C46 0.0181(18) 0.024(2) 0.0170(19) -0.0004(15) 0.0022(14) 0.0017(15) C47 0.034(2) 0.027(2) 0.026(2) 0.0043(17) 0.0135(18) -0.0018(18) C48 0.033(2) 0.023(2) 0.028(2) 0.0012(17) 0.0084(18) -0.0058(18) C49 0.0214(19) 0.027(2) 0.0185(19) -0.0001(16) 0.0004(15) 0.0013(16) C50 0.0206(19) 0.026(2) 0.022(2) -0.0008(16) 0.0031(16) 0.0009(16) C51 0.034(2) 0.029(2) 0.021(2) -0.0017(17) 0.0044(18) 0.0019(18) C52 0.040(3) 0.031(2) 0.028(2) 0.0078(19) 0.0021(19) 0.007(2) C53 0.043(3) 0.023(2) 0.030(2) 0.0022(18) 0.006(2) 0.0069(19) C54 0.036(2) 0.028(2) 0.024(2) -0.0029(17) 0.0041(18) 0.0049(19) C55 0.031(2) 0.025(2) 0.025(2) -0.0023(17) 0.0032(17) -0.0012(18) C56 0.040(2) 0.028(2) 0.029(2) 0.0016(18) 0.0056(19) -0.010(2) C57 0.041(2) 0.032(2) 0.023(2) 0.0061(18) 0.0035(19) 0.001(2) C58 0.032(2) 0.033(2) 0.025(2) 0.0014(18) -0.0014(18) -0.0020(19) C59 0.026(2) 0.023(2) 0.022(2) 0.0011(16) 0.0022(16) 0.0022(17) C60 0.024(2) 0.027(2) 0.019(2) 0.0015(16) 0.0037(16) 0.0041(17) C61 0.028(2) 0.023(2) 0.030(2) 0.0018(17) 0.0003(17) 0.0028(17) C62 0.026(2) 0.030(2) 0.030(2) 0.0034(18) -0.0052(17) 0.0090(18) C63 0.0211(19) 0.027(2) 0.025(2) -0.0001(17) 0.0011(16) 0.0035(16) C64 0.0209(18) 0.025(2) 0.0154(19) -0.0005(15) 0.0033(15) 0.0011(16) C65 0.020(2) 0.034(2) 0.034(2) 0.0021(19) -0.0060(17) 0.0070(18) C66 0.023(2) 0.030(2) 0.031(2) -0.0051(18) -0.0010(17) 0.0002(17) C67 0.0207(19) 0.025(2) 0.020(2) -0.0037(16) 0.0030(15) 0.0022(16) C68 0.0215(19) 0.027(2) 0.019(2) -0.0045(16) -0.0013(15) -0.0009(16) C69 0.025(2) 0.032(2) 0.033(2) -0.0048(19) 0.0015(18) 0.0020(18) C70 0.023(2) 0.042(3) 0.038(3) -0.005(2) 0.0045(19) -0.0011(19) C71 0.031(2) 0.037(3) 0.033(3) -0.003(2) 0.0053(19) -0.007(2) C72 0.030(2) 0.026(2) 0.024(2) -0.0012(17) -0.0005(17) -0.0020(18) C73 0.044(3) 0.040(3) 0.043(3) -0.006(2) 0.014(2) -0.013(2) C74 0.045(3) 0.034(3) 0.058(3) -0.008(2) 0.005(3) -0.004(2) C75 0.034(3) 0.042(3) 0.041(3) -0.004(2) -0.001(2) 0.000(2) C76 0.065(5) 0.130(7) 0.069(5) 0.026(5) 0.012(4) 0.022(5) S1 0.0274(5) 0.0281(5) 0.0213(5) -0.0024(4) 0.0036(4) -0.0021(4) S2 0.0358(6) 0.0326(6) 0.0322(6) -0.0098(5) 0.0016(5) 0.0002(5) S3 0.0268(5) 0.0432(7) 0.0281(6) -0.0053(5) 0.0010(4) -0.0012(5) S4 0.0502(8) 0.0621(9) 0.0447(8) 0.0072(7) 0.0012(6) -0.0190(7) F1 0.063(2) 0.0469(17) 0.0508(19) 0.0185(14) 0.0119(16) -0.0056(15) F2 0.087(3) 0.0488(19) 0.074(2) -0.0184(17) 0.021(2) -0.0382(18) F3 0.0415(17) 0.068(2) 0.064(2) 0.0068(17) 0.0236(15) -0.0083(15) F4 0.083(3) 0.052(2) 0.067(2) 0.0219(17) -0.007(2) -0.0094(18) F5 0.079(2) 0.0374(18) 0.097(3) -0.0246(18) 0.017(2) -0.0179(17) F6 0.0489(18) 0.0476(18) 0.091(3) -0.0097(17) 0.0286(18) -0.0085(15) F7 0.093(3) 0.119(4) 0.062(2) 0.009(2) -0.014(2) 0.063(3) F8 0.0490(19) 0.058(2) 0.093(3) -0.0423(19) -0.0214(18) 0.0164(16) F9 0.069(2) 0.069(2) 0.116(3) -0.036(2) 0.055(2) -0.0104(19) F10 0.086(3) 0.174(6) 0.160(5) -0.052(5) -0.044(4) -0.029(4) F11 0.112(4) 0.171(6) 0.136(5) 0.051(4) -0.034(4) 0.035(4) F12 0.063(3) 0.429(13) 0.099(4) -0.031(6) 0.034(3) 0.054(5) O1 0.0325(15) 0.0234(14) 0.0220(15) -0.0046(11) 0.0021(12) -0.0046(12) O2 0.0326(16) 0.0362(17) 0.0274(16) -0.0038(13) 0.0046(13) 0.0037(14) O3 0.0318(16) 0.0472(19) 0.0259(16) -0.0037(14) -0.0028(13) 0.0068(14) O4 0.0347(16) 0.0282(16) 0.0248(15) -0.0069(12) 0.0002(13) -0.0022(13) O5 0.052(2) 0.051(2) 0.039(2) -0.0081(16) -0.0124(17) -0.0051(17) O6 0.048(2) 0.049(2) 0.065(3) -0.0237(19) 0.0140(19) 0.0050(18) O7 0.065(3) 0.071(3) 0.178(6) 0.010(3) 0.069(4) -0.010(3) O8 0.030(2) 0.151(5) 0.095(4) -0.092(4) 0.001(2) 0.004(2) O9 0.129(4) 0.082(3) 0.048(3) 0.008(2) 0.016(3) 0.062(3) O10 0.054(3) 0.136(5) 0.091(4) 0.053(3) 0.027(3) 0.007(3) O11 0.091(3) 0.087(3) 0.050(3) 0.021(2) -0.001(2) -0.049(3) O12 0.212(8) 0.074(4) 0.097(4) 0.014(3) -0.081(5) -0.046(4) C77 0.046(3) 0.062(4) 0.051(3) 0.012(3) 0.007(3) 0.002(3) C78 0.102(7) 0.121(8) 0.203(12) 0.090(8) 0.068(8) 0.036(6) C79 0.099(5) 0.061(4) 0.056(4) 0.004(3) -0.022(4) 0.017(4) C80 0.055(4) 0.140(7) 0.035(3) 0.013(4) 0.010(3) 0.056(4) C81 0.34(2) 0.118(9) 0.099(9) 0.013(7) -0.020(11) -0.060(11) C82 0.084(6) 0.179(10) 0.115(8) 0.072(7) 0.045(6) 0.057(6) Cl1 0.0510(8) 0.0653(9) 0.0711(10) 0.0297(8) -0.0042(7) 0.0010(7) Cl2 0.1089(14) 0.0556(9) 0.0611(10) 0.0118(8) -0.0003(10) -0.0183(9) Cl3 0.122(2) 0.158(2) 0.0993(17) 0.0218(16) 0.0436(15) 0.0644(18) Cl4 0.0972(17) 0.1143(19) 0.260(4) 0.094(2) 0.074(2) 0.0337(15) Cl5 0.0895(11) 0.0556(9) 0.0422(8) 0.0128(6) 0.0072(7) 0.0239(8) Cl6 0.0633(9) 0.0632(10) 0.0821(11) 0.0328(8) 0.0193(8) 0.0242(8) Cl7 0.0937(12) 0.0607(9) 0.0497(9) 0.0030(7) 0.0176(8) 0.0074(9) Cl8 0.0556(10) 0.1260(18) 0.1304(19) 0.0415(15) 0.0150(11) -0.0107(11) Cl9 0.125(2) 0.291(5) 0.122(3) -0.012(3) 0.039(2) -0.035(3) Cl10 0.168(3) 0.298(6) 0.324(6) 0.193(5) 0.156(4) 0.107(4) Cl11 0.114(2) 0.199(3) 0.124(2) 0.051(2) 0.0122(18) 0.008(2) Cl12 0.0714(14) 0.311(5) 0.234(4) 0.218(4) 0.0596(19) 0.069(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 Co1 N1 1.961(3) . ? Co1 N7 1.962(3) . ? Co1 N13 1.965(3) . ? Co1 N19 1.990(3) . ? Co1 O1 2.196(3) . ? Co1 Co2 2.2742(7) . ? Co2 N20 1.904(3) . ? Co2 N2 1.908(3) . ? Co2 N14 1.915(3) . ? Co2 N8 1.920(3) . ? Co2 Co3 2.2417(7) . ? Co3 N15 1.927(3) . ? Co3 N9 1.933(3) . ? Co3 N21 1.937(3) . ? Co3 N3 1.938(3) . ? Co3 Co4 2.2665(7) . ? Co4 N16 1.930(3) . ? Co4 N10 1.935(3) . ? Co4 N4 1.936(3) . ? Co4 N22 1.938(3) . ? Co4 Co5 2.2442(7) . ? Co5 N23 1.894(3) . ? Co5 N5 1.904(3) . ? Co5 N11 1.915(3) . ? Co5 N17 1.925(3) . ? Co5 Co6 2.2912(7) . ? Co6 N18 1.958(3) . ? Co6 N24 1.970(3) . ? Co6 N12 1.973(3) . ? Co6 N6 1.982(3) . ? Co6 O4 2.249(3) . ? N1 C1 1.353(5) . ? N1 C5 1.361(5) . ? N2 C6 1.355(5) . ? N2 C5 1.382(5) . ? N3 C10 1.362(5) . ? N3 C6 1.365(5) . ? N4 C13 1.363(5) . ? N4 C10 1.369(5) . ? N5 C13 1.358(5) . ? N5 C14 1.374(5) . ? N6 C18 1.358(5) . ? N6 C14 1.371(5) . ? N7 C19 1.350(5) . ? N7 C23 1.360(5) . ? N8 C24 1.361(5) . ? N8 C23 1.377(5) . ? N9 C24 1.358(5) . ? N9 C28 1.362(5) . ? N10 C31 1.350(5) . ? N10 C28 1.370(5) . ? N11 C31 1.361(5) . ? N11 C32 1.388(5) . ? N12 C32 1.355(5) . ? N12 C36 1.356(5) . ? N13 C37 1.347(5) . ? N13 C41 1.359(5) . ? N14 C42 1.367(5) . ? N14 C41 1.377(5) . ? N15 C42 1.355(5) . ? N15 C46 1.360(5) . ? N16 C49 1.363(5) . ? N16 C46 1.366(5) . ? N17 C49 1.363(5) . ? N17 C50 1.375(5) . ? N18 C54 1.353(5) . ? N18 C50 1.361(5) . ? N19 C55 1.352(5) . ? N19 C59 1.366(5) . ? N20 C60 1.368(5) . ? N20 C59 1.378(5) . ? N21 C60 1.354(5) . ? N21 C64 1.363(5) . ? N22 C67 1.353(5) . ? N22 C64 1.361(5) . ? N23 C67 1.365(5) . ? N23 C68 1.390(5) . ? N24 C72 1.356(5) . ? N24 C68 1.360(5) . ? C1 C2 1.363(6) . ? C2 C3 1.390(6) . ? C3 C4 1.375(6) . ? C4 C5 1.399(6) . ? C6 C7 1.424(5) . ? C7 C8 1.341(6) . ? C8 C9 1.415(6) . ? C9 C10 1.407(5) . ? C9 C11 1.408(6) . ? C11 C12 1.363(6) . ? C12 C13 1.406(5) . ? C14 C15 1.395(6) . ? C15 C16 1.377(6) . ? C16 C17 1.395(6) . ? C17 C18 1.359(6) . ? C19 C20 1.363(6) . ? C20 C21 1.393(6) . ? C21 C22 1.374(6) . ? C22 C23 1.402(6) . ? C24 C25 1.424(5) . ? C25 C26 1.359(6) . ? C26 C27 1.411(6) . ? C27 C28 1.406(5) . ? C27 C29 1.410(6) . ? C29 C30 1.371(6) . ? C30 C31 1.426(5) . ? C32 C33 1.405(6) . ? C33 C34 1.381(6) . ? C34 C35 1.386(7) . ? C35 C36 1.369(6) . ? C37 C38 1.379(6) . ? C38 C39 1.382(6) . ? C39 C40 1.385(6) . ? C40 C41 1.406(6) . ? C42 C43 1.424(5) . ? C43 C44 1.361(6) . ? C44 C45 1.404(6) . ? C45 C46 1.408(5) . ? C45 C47 1.410(6) . ? C47 C48 1.353(6) . ? C48 C49 1.422(6) . ? C50 C51 1.408(6) . ? C51 C52 1.364(6) . ? C52 C53 1.381(6) . ? C53 C54 1.375(6) . ? C55 C56 1.373(6) . ? C56 C57 1.384(6) . ? C57 C58 1.362(6) . ? C58 C59 1.399(6) . ? C60 C61 1.424(6) . ? C61 C62 1.347(6) . ? C62 C63 1.418(6) . ? C63 C65 1.399(6) . ? C63 C64 1.405(5) . ? C65 C66 1.365(6) . ? C66 C67 1.415(6) . ? C68 C69 1.389(6) . ? C69 C70 1.368(6) . ? C70 C71 1.394(6) . ? C71 C72 1.365(6) . ? C73 F3 1.320(6) . ? C73 F2 1.322(6) . ? C73 F1 1.322(6) . ? C73 S1 1.826(5) . ? C74 F6 1.303(6) . ? C74 F5 1.322(6) . ? C74 F4 1.340(6) . ? C74 S2 1.830(6) . ? C75 F7 1.312(6) . ? C75 F9 1.320(6) . ? C75 F8 1.324(6) . ? C75 S3 1.820(5) . ? C76 F12 1.247(8) . ? C76 F11 1.329(9) . ? C76 F10 1.363(11) . ? C76 S4 1.750(8) . ? S1 O2 1.431(3) . ? S1 O3 1.437(3) . ? S1 O1 1.452(3) . ? S2 O6 1.427(4) . ? S2 O5 1.437(4) . ? S2 O4 1.457(3) . ? S3 O7 1.392(4) . ? S3 O8 1.398(4) . ? S3 O9 1.404(4) . ? S4 O10 1.405(5) . ? S4 O11 1.427(4) . ? S4 O12 1.435(6) . ? C77 Cl1 1.749(6) . ? C77 Cl2 1.757(6) . ? C78 Cl4 1.665(10) . ? C78 Cl3 1.680(9) . ? C79 Cl5 1.740(7) . ? C79 Cl6 1.746(6) . ? C80 Cl8 1.707(8) . ? C80 Cl7 1.775(7) . ? C81 Cl10 1.714(13) . ? C81 Cl9 1.721(15) . ? C82 Cl12 1.694(8) . ? C82 Cl11 1.765(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N7 89.52(13) . . ? N1 Co1 N13 173.88(14) . . ? N7 Co1 N13 89.04(13) . . ? N1 Co1 N19 89.03(13) . . ? N7 Co1 N19 172.94(14) . . ? N13 Co1 N19 91.68(13) . . ? N1 Co1 O1 92.41(12) . . ? N7 Co1 O1 98.02(12) . . ? N13 Co1 O1 93.69(12) . . ? N19 Co1 O1 88.95(12) . . ? N1 Co1 Co2 86.37(10) . . ? N7 Co1 Co2 87.01(10) . . ? N13 Co1 Co2 87.61(10) . . ? N19 Co1 Co2 86.00(10) . . ? O1 Co1 Co2 174.82(8) . . ? N20 Co2 N2 90.33(14) . . ? N20 Co2 N14 89.73(14) . . ? N2 Co2 N14 179.14(14) . . ? N20 Co2 N8 179.24(15) . . ? N2 Co2 N8 89.72(14) . . ? N14 Co2 N8 90.20(14) . . ? N20 Co2 Co3 90.51(10) . . ? N2 Co2 Co3 90.28(10) . . ? N14 Co2 Co3 88.87(10) . . ? N8 Co2 Co3 88.73(10) . . ? N20 Co2 Co1 90.63(10) . . ? N2 Co2 Co1 90.92(10) . . ? N14 Co2 Co1 89.94(10) . . ? N8 Co2 Co1 90.13(10) . . ? Co3 Co2 Co1 178.34(3) . . ? N15 Co3 N9 90.22(13) . . ? N15 Co3 N21 90.57(13) . . ? N9 Co3 N21 179.22(13) . . ? N15 Co3 N3 179.19(14) . . ? N9 Co3 N3 88.99(13) . . ? N21 Co3 N3 90.23(13) . . ? N15 Co3 Co2 90.62(10) . . ? N9 Co3 Co2 90.71(10) . . ? N21 Co3 Co2 89.25(10) . . ? N3 Co3 Co2 89.27(10) . . ? N15 Co3 Co4 89.61(10) . . ? N9 Co3 Co4 89.40(10) . . ? N21 Co3 Co4 90.64(10) . . ? N3 Co3 Co4 90.50(10) . . ? Co2 Co3 Co4 179.74(3) . . ? N16 Co4 N10 90.53(13) . . ? N16 Co4 N4 179.27(14) . . ? N10 Co4 N4 88.76(13) . . ? N16 Co4 N22 90.73(13) . . ? N10 Co4 N22 178.73(13) . . ? N4 Co4 N22 89.97(13) . . ? N16 Co4 Co5 90.49(9) . . ? N10 Co4 Co5 89.76(10) . . ? N4 Co4 Co5 89.69(10) . . ? N22 Co4 Co5 90.29(10) . . ? N16 Co4 Co3 90.15(9) . . ? N10 Co4 Co3 90.70(10) . . ? N4 Co4 Co3 89.68(10) . . ? N22 Co4 Co3 89.24(10) . . ? Co5 Co4 Co3 179.21(3) . . ? N23 Co5 N5 90.38(14) . . ? N23 Co5 N11 178.86(14) . . ? N5 Co5 N11 89.11(14) . . ? N23 Co5 N17 90.03(14) . . ? N5 Co5 N17 178.88(15) . . ? N11 Co5 N17 90.46(14) . . ? N23 Co5 Co4 89.09(10) . . ? N5 Co5 Co4 89.76(10) . . ? N11 Co5 Co4 89.89(10) . . ? N17 Co5 Co4 89.20(10) . . ? N23 Co5 Co6 90.01(10) . . ? N5 Co5 Co6 91.38(10) . . ? N11 Co5 Co6 91.02(10) . . ? N17 Co5 Co6 89.66(10) . . ? Co4 Co5 Co6 178.55(3) . . ? N18 Co6 N24 88.73(14) . . ? N18 Co6 N12 88.32(14) . . ? N24 Co6 N12 173.27(14) . . ? N18 Co6 N6 173.39(14) . . ? N24 Co6 N6 91.65(14) . . ? N12 Co6 N6 90.59(14) . . ? N18 Co6 O4 92.40(12) . . ? N24 Co6 O4 91.01(12) . . ? N12 Co6 O4 95.15(12) . . ? N6 Co6 O4 94.19(12) . . ? N18 Co6 Co5 87.35(10) . . ? N24 Co6 Co5 86.83(10) . . ? N12 Co6 Co5 87.00(10) . . ? N6 Co6 Co5 86.09(10) . . ? O4 Co6 Co5 177.83(8) . . ? C1 N1 C5 119.0(3) . . ? C1 N1 Co1 119.9(3) . . ? C5 N1 Co1 121.1(3) . . ? C6 N2 C5 123.9(3) . . ? C6 N2 Co2 119.0(3) . . ? C5 N2 Co2 116.8(2) . . ? C10 N3 C6 120.0(3) . . ? C10 N3 Co3 119.6(3) . . ? C6 N3 Co3 120.3(2) . . ? C13 N4 C10 119.8(3) . . ? C13 N4 Co4 119.8(3) . . ? C10 N4 Co4 119.9(2) . . ? C13 N5 C14 123.5(3) . . ? C13 N5 Co5 118.8(3) . . ? C14 N5 Co5 117.6(3) . . ? C18 N6 C14 117.9(3) . . ? C18 N6 Co6 120.9(3) . . ? C14 N6 Co6 121.2(3) . . ? C19 N7 C23 118.2(3) . . ? C19 N7 Co1 121.2(3) . . ? C23 N7 Co1 120.5(3) . . ? C24 N8 C23 123.6(3) . . ? C24 N8 Co2 118.7(3) . . ? C23 N8 Co2 117.6(3) . . ? C24 N9 C28 120.1(3) . . ? C24 N9 Co3 119.0(3) . . ? C28 N9 Co3 120.5(2) . . ? C31 N10 C28 120.7(3) . . ? C31 N10 Co4 120.0(3) . . ? C28 N10 Co4 119.2(3) . . ? C31 N11 C32 123.8(3) . . ? C31 N11 Co5 118.7(3) . . ? C32 N11 Co5 117.4(3) . . ? C32 N12 C36 118.5(3) . . ? C32 N12 Co6 121.5(3) . . ? C36 N12 Co6 120.0(3) . . ? C37 N13 C41 118.3(3) . . ? C37 N13 Co1 121.5(3) . . ? C41 N13 Co1 120.1(3) . . ? C42 N14 C41 123.4(3) . . ? C42 N14 Co2 118.8(3) . . ? C41 N14 Co2 117.8(3) . . ? C42 N15 C46 119.6(3) . . ? C42 N15 Co3 119.3(3) . . ? C46 N15 Co3 120.8(2) . . ? C49 N16 C46 119.8(3) . . ? C49 N16 Co4 119.9(3) . . ? C46 N16 Co4 120.2(2) . . ? C49 N17 C50 122.8(3) . . ? C49 N17 Co5 119.4(3) . . ? C50 N17 Co5 117.7(3) . . ? C54 N18 C50 118.5(4) . . ? C54 N18 Co6 120.2(3) . . ? C50 N18 Co6 121.1(3) . . ? C55 N19 C59 118.0(3) . . ? C55 N19 Co1 121.4(3) . . ? C59 N19 Co1 120.5(3) . . ? C60 N20 C59 123.6(3) . . ? C60 N20 Co2 118.4(3) . . ? C59 N20 Co2 117.8(3) . . ? C60 N21 C64 119.8(3) . . ? C60 N21 Co3 120.4(3) . . ? C64 N21 Co3 119.6(3) . . ? C67 N22 C64 119.8(3) . . ? C67 N22 Co4 119.0(3) . . ? C64 N22 Co4 120.9(3) . . ? C67 N23 C68 122.1(3) . . ? C67 N23 Co5 119.7(3) . . ? C68 N23 Co5 117.9(3) . . ? C72 N24 C68 117.8(3) . . ? C72 N24 Co6 121.2(3) . . ? C68 N24 Co6 120.7(3) . . ? N1 C1 C2 122.7(4) . . ? C1 C2 C3 118.9(4) . . ? C4 C3 C2 119.3(4) . . ? C3 C4 C5 119.7(4) . . ? N1 C5 N2 115.1(3) . . ? N1 C5 C4 120.3(4) . . ? N2 C5 C4 124.4(4) . . ? N2 C6 N3 115.0(3) . . ? N2 C6 C7 125.1(4) . . ? N3 C6 C7 119.8(4) . . ? C8 C7 C6 119.9(4) . . ? C7 C8 C9 121.2(4) . . ? C10 C9 C11 117.6(4) . . ? C10 C9 C8 117.1(4) . . ? C11 C9 C8 125.2(4) . . ? N3 C10 N4 116.7(3) . . ? N3 C10 C9 121.8(3) . . ? N4 C10 C9 121.5(3) . . ? C12 C11 C9 120.6(4) . . ? C11 C12 C13 120.0(4) . . ? N5 C13 N4 114.8(3) . . ? N5 C13 C12 124.7(4) . . ? N4 C13 C12 120.3(4) . . ? N6 C14 N5 115.1(3) . . ? N6 C14 C15 120.7(4) . . ? N5 C14 C15 123.9(4) . . ? C16 C15 C14 120.0(4) . . ? C15 C16 C17 119.0(4) . . ? C18 C17 C16 118.8(4) . . ? N6 C18 C17 123.6(4) . . ? N7 C19 C20 123.7(4) . . ? C19 C20 C21 118.1(4) . . ? C22 C21 C20 119.7(4) . . ? C21 C22 C23 119.4(4) . . ? N7 C23 N8 115.2(3) . . ? N7 C23 C22 120.7(4) . . ? N8 C23 C22 124.0(4) . . ? N9 C24 N8 115.3(3) . . ? N9 C24 C25 119.8(4) . . ? N8 C24 C25 124.8(4) . . ? C26 C25 C24 120.1(4) . . ? C25 C26 C27 120.4(4) . . ? C28 C27 C29 117.6(4) . . ? C28 C27 C26 117.5(4) . . ? C29 C27 C26 124.9(4) . . ? N9 C28 N10 116.5(3) . . ? N9 C28 C27 122.0(3) . . ? N10 C28 C27 121.5(4) . . ? C30 C29 C27 120.7(4) . . ? C29 C30 C31 119.5(4) . . ? N10 C31 N11 115.9(3) . . ? N10 C31 C30 119.9(4) . . ? N11 C31 C30 124.1(4) . . ? N12 C32 N11 115.4(3) . . ? N12 C32 C33 120.8(4) . . ? N11 C32 C33 123.5(4) . . ? C34 C33 C32 119.1(4) . . ? C33 C34 C35 119.5(4) . . ? C36 C35 C34 118.7(4) . . ? N12 C36 C35 122.9(4) . . ? N13 C37 C38 123.5(4) . . ? C37 C38 C39 118.5(4) . . ? C38 C39 C40 119.4(4) . . ? C39 C40 C41 119.4(4) . . ? N13 C41 N14 115.4(3) . . ? N13 C41 C40 120.8(4) . . ? N14 C41 C40 123.6(4) . . ? N15 C42 N14 115.2(3) . . ? N15 C42 C43 120.4(4) . . ? N14 C42 C43 124.3(3) . . ? C44 C43 C42 119.7(4) . . ? C43 C44 C45 120.5(4) . . ? C44 C45 C46 117.6(4) . . ? C44 C45 C47 125.3(4) . . ? C46 C45 C47 117.1(4) . . ? N15 C46 N16 115.7(3) . . ? N15 C46 C45 122.1(3) . . ? N16 C46 C45 122.1(4) . . ? C48 C47 C45 121.0(4) . . ? C47 C48 C49 120.0(4) . . ? N16 C49 N17 115.0(3) . . ? N16 C49 C48 119.9(4) . . ? N17 C49 C48 125.0(4) . . ? N18 C50 N17 114.9(3) . . ? N18 C50 C51 120.1(4) . . ? N17 C50 C51 124.7(4) . . ? C52 C51 C50 120.1(4) . . ? C51 C52 C53 119.5(4) . . ? C54 C53 C52 118.7(4) . . ? N18 C54 C53 123.0(4) . . ? N19 C55 C56 123.4(4) . . ? C55 C56 C57 118.3(4) . . ? C58 C57 C56 119.6(4) . . ? C57 C58 C59 120.2(4) . . ? N19 C59 N20 114.3(3) . . ? N19 C59 C58 120.4(4) . . ? N20 C59 C58 125.0(4) . . ? N21 C60 N20 115.3(3) . . ? N21 C60 C61 120.3(4) . . ? N20 C60 C61 124.3(4) . . ? C62 C61 C60 119.7(4) . . ? C61 C62 C63 121.1(4) . . ? C65 C63 C64 117.9(4) . . ? C65 C63 C62 125.2(4) . . ? C64 C63 C62 116.9(4) . . ? N22 C64 N21 116.2(3) . . ? N22 C64 C63 121.7(4) . . ? N21 C64 C63 122.2(4) . . ? C66 C65 C63 120.4(4) . . ? C65 C66 C67 119.6(4) . . ? N22 C67 N23 115.2(3) . . ? N22 C67 C66 120.5(4) . . ? N23 C67 C66 124.1(4) . . ? N24 C68 C69 121.4(4) . . ? N24 C68 N23 114.5(3) . . ? C69 C68 N23 123.8(4) . . ? C70 C69 C68 119.7(4) . . ? C69 C70 C71 119.4(4) . . ? C72 C71 C70 118.4(4) . . ? N24 C72 C71 123.4(4) . . ? F3 C73 F2 108.8(4) . . ? F3 C73 F1 107.7(4) . . ? F2 C73 F1 107.4(4) . . ? F3 C73 S1 110.4(4) . . ? F2 C73 S1 110.8(3) . . ? F1 C73 S1 111.7(3) . . ? F6 C74 F5 108.4(4) . . ? F6 C74 F4 108.2(5) . . ? F5 C74 F4 107.0(4) . . ? F6 C74 S2 111.8(4) . . ? F5 C74 S2 111.2(4) . . ? F4 C74 S2 110.1(4) . . ? F7 C75 F9 104.1(4) . . ? F7 C75 F8 106.6(4) . . ? F9 C75 F8 107.2(4) . . ? F7 C75 S3 112.8(4) . . ? F9 C75 S3 112.8(4) . . ? F8 C75 S3 112.7(3) . . ? F12 C76 F11 104.5(8) . . ? F12 C76 F10 104.4(8) . . ? F11 C76 F10 104.0(7) . . ? F12 C76 S4 120.1(6) . . ? F11 C76 S4 113.1(6) . . ? F10 C76 S4 109.3(6) . . ? O2 S1 O3 116.36(18) . . ? O2 S1 O1 114.10(18) . . ? O3 S1 O1 113.63(18) . . ? O2 S1 C73 104.8(2) . . ? O3 S1 C73 103.3(2) . . ? O1 S1 C73 102.4(2) . . ? O6 S2 O5 116.5(2) . . ? O6 S2 O4 113.8(2) . . ? O5 S2 O4 113.7(2) . . ? O6 S2 C74 104.4(2) . . ? O5 S2 C74 103.9(2) . . ? O4 S2 C74 102.3(2) . . ? O7 S3 O8 115.8(4) . . ? O7 S3 O9 115.0(4) . . ? O8 S3 O9 114.1(4) . . ? O7 S3 C75 104.1(3) . . ? O8 S3 C75 102.5(2) . . ? O9 S3 C75 102.9(2) . . ? O10 S4 O11 115.7(3) . . ? O10 S4 O12 113.8(4) . . ? O11 S4 O12 114.1(3) . . ? O10 S4 C76 105.9(3) . . ? O11 S4 C76 102.9(4) . . ? O12 S4 C76 102.4(5) . . ? S1 O1 Co1 154.85(18) . . ? S2 O4 Co6 163.9(2) . . ? Cl1 C77 Cl2 111.0(3) . . ? Cl4 C78 Cl3 117.3(6) . . ? Cl5 C79 Cl6 112.8(4) . . ? Cl8 C80 Cl7 111.9(3) . . ? Cl10 C81 Cl9 106.2(7) . . ? Cl12 C82 Cl11 111.0(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.512 _refine_diff_density_min -1.528 _refine_diff_density_rms 0.162 #===END data_ic11104(compd_4) _database_code_depnum_ccdc_archive 'CCDC 283617' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co6(bpyany)4(OTf)2)(OTf) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H69.50 Cl10 Co6 F9 N24 O10.75 S3' _chemical_formula_weight 2562.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9988(2) _cell_length_b 28.3349(5) _cell_length_c 26.0264(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.2970(8) _cell_angle_gamma 90.00 _cell_volume 9570.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5154 _exptl_absorpt_coefficient_mu 1.452 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.654 _exptl_absorpt_correction_T_max 0.843 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 100270 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16872 _reflns_number_gt 12036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1661P)^2^+78.4081P] 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 16872 _refine_ls_number_parameters 1284 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1200 _refine_ls_R_factor_gt 0.0891 _refine_ls_wR_factor_ref 0.2924 _refine_ls_wR_factor_gt 0.2599 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.33237(8) 0.09773(4) 0.10200(4) 0.0254(3) Uani 1 1 d . . . Co2 Co 0.45622(7) 0.10743(3) 0.16748(4) 0.0239(3) Uani 1 1 d . . . Co3 Co 0.58122(7) 0.11553(3) 0.23036(4) 0.0237(3) Uani 1 1 d . . . Co4 Co 0.70579(7) 0.12381(3) 0.29343(4) 0.0238(3) Uani 1 1 d . . . Co5 Co 0.83018(7) 0.13202(4) 0.35640(4) 0.0243(3) Uani 1 1 d . . . Co6 Co 0.95347(7) 0.13941(4) 0.42160(4) 0.0260(3) Uani 1 1 d . . . N1 N 0.4141(5) 0.0432(2) 0.0798(2) 0.0283(14) Uani 1 1 d . . . N2 N 0.5529(5) 0.0739(2) 0.1282(2) 0.0258(13) Uani 1 1 d . . . N3 N 0.6856(4) 0.1000(2) 0.1832(2) 0.0217(13) Uani 1 1 d . . . N4 N 0.8100(5) 0.1260(2) 0.2434(2) 0.0265(14) Uani 1 1 d . . . N5 N 0.9235(5) 0.1533(2) 0.3077(2) 0.0260(14) Uani 1 1 d . . . N6 N 1.0211(5) 0.1838(2) 0.3762(3) 0.0293(14) Uani 1 1 d . . . N7 N 0.2630(5) 0.0543(2) 0.1472(2) 0.0267(14) Uani 1 1 d . . . N8 N 0.4145(5) 0.0499(2) 0.1980(2) 0.0261(14) Uani 1 1 d . . . N9 N 0.5667(5) 0.0495(2) 0.2484(2) 0.0238(13) Uani 1 1 d . . . N10 N 0.7191(5) 0.0563(2) 0.2982(2) 0.0248(13) Uani 1 1 d . . . N11 N 0.8711(5) 0.0680(2) 0.3458(2) 0.0270(14) Uani 1 1 d . . . N12 N 1.0245(5) 0.0869(2) 0.3896(2) 0.0272(14) Uani 1 1 d . . . N13 N 0.2616(5) 0.1521(2) 0.1325(2) 0.0255(13) Uani 1 1 d . . . N14 N 0.3629(5) 0.1416(2) 0.2078(2) 0.0266(14) Uani 1 1 d . . . N15 N 0.4767(4) 0.1320(2) 0.2774(2) 0.0227(13) Uani 1 1 d . . . N16 N 0.6022(5) 0.1225(2) 0.3438(2) 0.0246(13) Uani 1 1 d . . . N17 N 0.7343(5) 0.1112(2) 0.4048(2) 0.0262(14) Uani 1 1 d . . . N18 N 0.8743(5) 0.0933(2) 0.4596(2) 0.0269(14) Uani 1 1 d . . . N19 N 0.4145(5) 0.1415(2) 0.0615(2) 0.0267(14) Uani 1 1 d . . . N20 N 0.4999(5) 0.1652(2) 0.1376(2) 0.0247(13) Uani 1 1 d . . . N21 N 0.5943(4) 0.1817(2) 0.2123(2) 0.0246(13) Uani 1 1 d . . . N22 N 0.6925(4) 0.1917(2) 0.2890(2) 0.0230(13) Uani 1 1 d . . . N23 N 0.7870(5) 0.1957(2) 0.3664(2) 0.0275(14) Uani 1 1 d . . . N24 N 0.8667(4) 0.1904(2) 0.4476(2) 0.0263(14) Uani 1 1 d . . . C1 C 0.3675(6) 0.0069(3) 0.0538(3) 0.0323(18) Uani 1 1 d . . . H1A H 0.2973 0.0103 0.0421 0.039 Uiso 1 1 calc R . . C2 C 0.4165(7) -0.0342(3) 0.0437(3) 0.039(2) Uani 1 1 d . . . H2A H 0.3814 -0.0587 0.0249 0.047 Uiso 1 1 calc R . . C3 C 0.5197(7) -0.0398(3) 0.0614(3) 0.039(2) Uani 1 1 d . . . H3A H 0.5558 -0.0681 0.0548 0.047 Uiso 1 1 calc R . . C4 C 0.5673(7) -0.0038(3) 0.0885(3) 0.0326(18) Uani 1 1 d . . . H4A H 0.6369 -0.0071 0.1013 0.039 Uiso 1 1 calc R . . C5 C 0.5133(6) 0.0379(3) 0.0973(3) 0.0287(17) Uani 1 1 d . . . C6 C 0.6547(6) 0.0818(3) 0.1364(3) 0.0260(16) Uani 1 1 d . . . C7 C 0.7290(6) 0.0761(3) 0.0981(3) 0.0311(17) Uani 1 1 d . . . H7A H 0.7085 0.0631 0.0655 0.037 Uiso 1 1 calc R . . C8 C 0.8289(6) 0.0893(3) 0.1086(3) 0.0326(18) Uani 1 1 d . . . H8A H 0.8770 0.0869 0.0826 0.039 Uiso 1 1 calc R . . C9 C 0.8611(6) 0.1063(3) 0.1577(3) 0.0309(17) Uani 1 1 d . . . C10 C 0.7869(5) 0.1108(2) 0.1942(3) 0.0219(15) Uani 1 1 d . . . C11 C 0.9641(6) 0.1197(3) 0.1733(3) 0.0310(17) Uani 1 1 d . . . H11A H 1.0171 0.1172 0.1498 0.037 Uiso 1 1 calc R . . C12 C 0.9862(6) 0.1360(3) 0.2215(3) 0.0296(17) Uani 1 1 d . . . H12A H 1.0548 0.1450 0.2316 0.036 Uiso 1 1 calc R . . C13 C 0.9087(6) 0.1399(3) 0.2572(3) 0.0268(16) Uani 1 1 d . . . C14 C 0.9981(5) 0.1849(3) 0.3246(3) 0.0276(17) Uani 1 1 d . . . C15 C 1.0427(6) 0.2195(3) 0.2937(3) 0.0354(19) Uani 1 1 d . . . H15A H 1.0242 0.2208 0.2579 0.042 Uiso 1 1 calc R . . C16 C 1.1119(7) 0.2509(3) 0.3149(3) 0.041(2) Uani 1 1 d . . . H16A H 1.1429 0.2736 0.2938 0.049 Uiso 1 1 calc R . . C17 C 1.1367(7) 0.2497(3) 0.3668(4) 0.043(2) Uani 1 1 d . . . H17A H 1.1850 0.2713 0.3822 0.051 Uiso 1 1 calc R . . C18 C 1.0897(6) 0.2164(3) 0.3959(3) 0.0317(18) Uani 1 1 d . . . H18A H 1.1060 0.2161 0.4320 0.038 Uiso 1 1 calc R . . C19 C 0.1626(6) 0.0426(3) 0.1372(3) 0.0313(18) Uani 1 1 d . . . H19A H 0.1271 0.0564 0.1080 0.038 Uiso 1 1 calc R . . C20 C 0.1102(6) 0.0126(3) 0.1663(3) 0.0357(19) Uani 1 1 d . . . H20A H 0.0405 0.0048 0.1569 0.043 Uiso 1 1 calc R . . C21 C 0.1599(6) -0.0067(3) 0.2102(3) 0.0344(18) Uani 1 1 d . . . H21A H 0.1249 -0.0281 0.2312 0.041 Uiso 1 1 calc R . . C22 C 0.2611(6) 0.0058(3) 0.2227(3) 0.0324(18) Uani 1 1 d . . . H22A H 0.2950 -0.0057 0.2536 0.039 Uiso 1 1 calc R . . C23 C 0.3133(6) 0.0352(3) 0.1899(3) 0.0271(16) Uani 1 1 d . . . C24 C 0.4846(6) 0.0244(3) 0.2279(3) 0.0287(17) Uani 1 1 d . . . C25 C 0.4823(6) -0.0256(3) 0.2350(3) 0.0326(18) Uani 1 1 d . . . H25A H 0.4277 -0.0436 0.2190 0.039 Uiso 1 1 calc R . . C26 C 0.5572(6) -0.0474(3) 0.2642(3) 0.0343(19) Uani 1 1 d . . . H26A H 0.5537 -0.0805 0.2697 0.041 Uiso 1 1 calc R . . C27 C 0.6411(6) -0.0213(3) 0.2867(3) 0.0297(17) Uani 1 1 d . . . C28 C 0.6420(6) 0.0273(3) 0.2777(3) 0.0273(16) Uani 1 1 d . . . C29 C 0.7232(6) -0.0405(3) 0.3178(3) 0.0350(19) Uani 1 1 d . . . H29A H 0.7237 -0.0733 0.3254 0.042 Uiso 1 1 calc R . . C30 C 0.8014(6) -0.0127(3) 0.3370(3) 0.0318(18) Uani 1 1 d . . . H30A H 0.8568 -0.0261 0.3575 0.038 Uiso 1 1 calc R . . C31 C 0.7997(6) 0.0363(3) 0.3264(3) 0.0250(16) Uani 1 1 d . . . C32 C 0.9730(6) 0.0565(3) 0.3564(3) 0.0259(16) Uani 1 1 d . . . C33 C 1.0261(6) 0.0193(3) 0.3339(3) 0.0308(17) Uani 1 1 d . . . H33A H 0.9897 -0.0020 0.3113 0.037 Uiso 1 1 calc R . . C34 C 1.1295(6) 0.0135(3) 0.3443(3) 0.0344(19) Uani 1 1 d . . . H34A H 1.1651 -0.0121 0.3298 0.041 Uiso 1 1 calc R . . C35 C 1.1821(6) 0.0459(3) 0.3768(3) 0.0324(18) Uani 1 1 d . . . H35A H 1.2543 0.0431 0.3840 0.039 Uiso 1 1 calc R . . C36 C 1.1278(6) 0.0816(3) 0.3979(3) 0.0297(17) Uani 1 1 d . . . H36A H 1.1643 0.1038 0.4194 0.036 Uiso 1 1 calc R . . C37 C 0.1925(6) 0.1773(3) 0.1035(3) 0.0316(18) Uani 1 1 d . . . H37A H 0.1769 0.1673 0.0690 0.038 Uiso 1 1 calc R . . C38 C 0.1434(6) 0.2164(3) 0.1207(3) 0.0349(19) Uani 1 1 d . . . H38A H 0.0921 0.2320 0.0995 0.042 Uiso 1 1 calc R . . C39 C 0.1706(6) 0.2331(3) 0.1706(3) 0.0333(18) Uani 1 1 d . . . H39A H 0.1394 0.2607 0.1835 0.040 Uiso 1 1 calc R . . C40 C 0.2431(6) 0.2087(3) 0.2002(3) 0.0304(17) Uani 1 1 d . . . H40A H 0.2638 0.2199 0.2336 0.036 Uiso 1 1 calc R . . C41 C 0.2874(6) 0.1670(3) 0.1813(3) 0.0278(17) Uani 1 1 d . . . C42 C 0.3792(5) 0.1423(2) 0.2599(3) 0.0229(15) Uani 1 1 d . . . C43 C 0.3018(6) 0.1496(3) 0.2954(3) 0.0289(17) Uani 1 1 d . . . H43A H 0.2329 0.1556 0.2829 0.035 Uiso 1 1 calc R . . C44 C 0.3248(6) 0.1480(3) 0.3466(3) 0.0290(17) Uani 1 1 d . . . H44A H 0.2724 0.1536 0.3699 0.035 Uiso 1 1 calc R . . C45 C 0.4266(6) 0.1383(3) 0.3658(3) 0.0265(16) Uani 1 1 d . . . C46 C 0.5004(5) 0.1313(2) 0.3294(3) 0.0227(15) Uani 1 1 d . . . C47 C 0.4586(6) 0.1353(3) 0.4181(3) 0.0312(18) Uani 1 1 d . . . H47A H 0.4105 0.1403 0.4437 0.037 Uiso 1 1 calc R . . C48 C 0.5600(6) 0.1252(3) 0.4324(3) 0.0295(17) Uani 1 1 d . . . H48A H 0.5815 0.1226 0.4678 0.035 Uiso 1 1 calc R . . C49 C 0.6319(6) 0.1185(3) 0.3943(3) 0.0254(16) Uani 1 1 d . . . C50 C 0.7739(6) 0.0856(3) 0.4470(3) 0.0272(16) Uani 1 1 d . . . C51 C 0.7181(6) 0.0511(3) 0.4717(3) 0.0332(18) Uani 1 1 d . . . H51A H 0.6474 0.0460 0.4621 0.040 Uiso 1 1 calc R . . C52 C 0.7670(7) 0.0245(3) 0.5103(3) 0.0367(19) Uani 1 1 d . . . H52A H 0.7298 0.0014 0.5281 0.044 Uiso 1 1 calc R . . C53 C 0.8712(7) 0.0317(3) 0.5228(3) 0.0374(19) Uani 1 1 d . . . H53A H 0.9064 0.0136 0.5490 0.045 Uiso 1 1 calc R . . C54 C 0.9222(6) 0.0656(3) 0.4965(3) 0.0334(18) Uani 1 1 d . . . H54A H 0.9938 0.0700 0.5043 0.040 Uiso 1 1 calc R . . C55 C 0.4032(6) 0.1422(3) 0.0100(3) 0.0318(18) Uani 1 1 d . . . H55A H 0.3503 0.1233 -0.0061 0.038 Uiso 1 1 calc R . . C56 C 0.4625(7) 0.1685(3) -0.0210(3) 0.038(2) Uani 1 1 d . . . H56A H 0.4495 0.1687 -0.0573 0.046 Uiso 1 1 calc R . . C57 C 0.5430(7) 0.1949(3) 0.0025(3) 0.040(2) Uani 1 1 d . . . H57A H 0.5883 0.2122 -0.0178 0.048 Uiso 1 1 calc R . . C58 C 0.5558(7) 0.1956(3) 0.0551(3) 0.0362(19) Uani 1 1 d . . . H58A H 0.6095 0.2138 0.0716 0.043 Uiso 1 1 calc R . . C59 C 0.4887(6) 0.1691(3) 0.0847(3) 0.0274(16) Uani 1 1 d . . . C60 C 0.5497(5) 0.1980(3) 0.1684(3) 0.0246(16) Uani 1 1 d . . . C61 C 0.5480(6) 0.2479(3) 0.1581(3) 0.0321(18) Uani 1 1 d . . . H61A H 0.5155 0.2596 0.1270 0.039 Uiso 1 1 calc R . . C62 C 0.5930(7) 0.2784(3) 0.1929(3) 0.0352(19) Uani 1 1 d . . . H62A H 0.5885 0.3114 0.1869 0.042 Uiso 1 1 calc R . . C63 C 0.6467(6) 0.2613(3) 0.2380(3) 0.0299(17) Uani 1 1 d . . . C64 C 0.6446(5) 0.2121(3) 0.2464(3) 0.0245(16) Uani 1 1 d . . . C65 C 0.6971(6) 0.2893(3) 0.2761(3) 0.0339(18) Uani 1 1 d . . . H65A H 0.6989 0.3226 0.2719 0.041 Uiso 1 1 calc R . . C66 C 0.7434(6) 0.2694(3) 0.3191(3) 0.0336(18) Uani 1 1 d . . . H66A H 0.7785 0.2886 0.3443 0.040 Uiso 1 1 calc R . . C67 C 0.7392(5) 0.2194(3) 0.3262(3) 0.0252(16) Uani 1 1 d . . . C68 C 0.7962(6) 0.2135(3) 0.4153(3) 0.0301(17) Uani 1 1 d . . . C69 C 0.7315(6) 0.2477(3) 0.4345(3) 0.0328(18) Uani 1 1 d . . . H69A H 0.6828 0.2635 0.4120 0.039 Uiso 1 1 calc R . . C70 C 0.7384(7) 0.2584(3) 0.4862(3) 0.039(2) Uani 1 1 d . . . H70A H 0.6951 0.2820 0.4993 0.047 Uiso 1 1 calc R . . C71 C 0.8087(6) 0.2349(3) 0.5191(3) 0.0362(19) Uani 1 1 d . . . H71A H 0.8142 0.2418 0.5548 0.043 Uiso 1 1 calc R . . C72 C 0.8698(6) 0.2013(3) 0.4984(3) 0.0324(18) Uani 1 1 d . . . H72A H 0.9171 0.1846 0.5209 0.039 Uiso 1 1 calc R . . S1 S 0.11944(19) 0.09413(9) 0.00515(9) 0.0448(6) Uani 1 1 d . . . O1 O 0.2157(4) 0.0863(2) 0.0357(2) 0.0359(13) Uani 1 1 d . . . O2 O 0.0277(5) 0.0873(3) 0.0323(3) 0.072(2) Uani 1 1 d . . . O3 O 0.1205(7) 0.1348(3) -0.0259(3) 0.068(2) Uani 1 1 d . . . C73 C 0.1184(10) 0.0447(5) -0.0386(5) 0.074(4) Uani 1 1 d . . . F1 F 0.0364(6) 0.0454(3) -0.0712(3) 0.090(3) Uani 1 1 d . . . F2 F 0.2039(7) 0.0474(5) -0.0668(3) 0.137(5) Uani 1 1 d . . . F3 F 0.1243(7) 0.0045(3) -0.0161(4) 0.103(3) Uani 1 1 d . . . S2 S 1.1384(3) 0.15969(10) 0.52917(16) 0.0866(13) Uani 1 1 d . . . O4 O 1.0743(4) 0.1457(2) 0.4858(2) 0.0347(13) Uani 1 1 d . . . O5 O 1.0663(10) 0.1502(5) 0.5823(5) 0.116(4) Uiso 1 1 d . . . O6 O 1.1766(8) 0.2028(3) 0.5353(4) 0.087(3) Uani 1 1 d . . . C74 C 1.2230(12) 0.1139(4) 0.5444(5) 0.079(4) Uani 1 1 d . . . F4 F 1.2821(6) 0.1162(5) 0.5026(3) 0.126(4) Uani 1 1 d . . . F5 F 1.1805(6) 0.0723(2) 0.5470(3) 0.082(2) Uani 1 1 d . . . F6 F 1.2804(6) 0.1207(3) 0.5877(3) 0.083(2) Uani 1 1 d . . . S3 S 0.2552(2) 0.37719(10) 0.20467(11) 0.0568(7) Uani 1 1 d . . . O7 O 0.2247(8) 0.3365(3) 0.2315(3) 0.080(3) Uani 1 1 d . . . O8 O 0.3591(8) 0.3920(3) 0.2200(3) 0.080(3) Uani 1 1 d . . . O9 O 0.1891(8) 0.4158(3) 0.1967(4) 0.093(3) Uani 1 1 d . . . C75 C 0.2713(10) 0.3557(4) 0.1391(5) 0.061(3) Uani 1 1 d . . . F7 F 0.1831(6) 0.3404(3) 0.1181(3) 0.077(2) Uani 1 1 d . . . F8 F 0.3383(5) 0.3206(3) 0.1391(3) 0.079(2) Uani 1 1 d . . . F9 F 0.3063(8) 0.3895(3) 0.1096(3) 0.099(3) Uani 1 1 d . . . C76 C 0.4370(10) 0.3159(4) 0.3095(5) 0.071(3) Uani 1 1 d . . . H76A H 0.3681 0.3309 0.3073 0.085 Uiso 1 1 calc R . . H76B H 0.4711 0.3227 0.2773 0.085 Uiso 1 1 calc R . . Cl1 Cl 0.5137(3) 0.33941(11) 0.36440(14) 0.0759(9) Uani 1 1 d . . . Cl2 Cl 0.4245(3) 0.25543(11) 0.31726(16) 0.0858(10) Uani 1 1 d . . . C77 C 0.4656(13) -0.0467(4) 0.3932(5) 0.082(4) Uani 1 1 d . . . H77A H 0.3944 -0.0591 0.3889 0.098 Uiso 1 1 calc R . . H77B H 0.5080 -0.0636 0.3686 0.098 Uiso 1 1 calc R . . Cl3 Cl 0.4649(2) 0.01340(10) 0.37878(14) 0.0694(8) Uani 1 1 d . . . Cl4 Cl 0.5129(4) -0.0577(2) 0.45362(19) 0.1315(19) Uani 1 1 d . . . C78 C 0.8445(10) 0.2869(5) 0.1391(6) 0.083(4) Uani 1 1 d . . . H78A H 0.8622 0.2920 0.1030 0.100 Uiso 1 1 calc R . . H78B H 0.7739 0.2990 0.1427 0.100 Uiso 1 1 calc R . . Cl5 Cl 0.8474(3) 0.22675(12) 0.15250(19) 0.1014(13) Uani 1 1 d . . . Cl6 Cl 0.9302(4) 0.31819(18) 0.1799(3) 0.144(2) Uani 1 1 d . . . C79 C 1.4238(17) 0.2588(6) 0.5021(5) 0.143(8) Uiso 1 1 d D . . H79A H 1.3597 0.2645 0.5199 0.171 Uiso 1 1 calc R . . H79B H 1.4692 0.2865 0.5086 0.171 Uiso 1 1 calc R . . Cl7 Cl 1.4811(6) 0.2123(3) 0.5275(3) 0.166(2) Uiso 1 1 d D . . Cl8 Cl 1.3951(7) 0.2553(3) 0.4410(3) 0.200 Uiso 1 1 d D . . C80 C 0.6595(10) 0.4306(4) 0.3008(5) 0.069(3) Uani 1 1 d . . . H80A H 0.6436 0.4204 0.2648 0.083 Uiso 0.75 1 calc PR A 1 H80B H 0.6035 0.4192 0.3219 0.083 Uiso 0.75 1 calc PR A 1 H80C H 0.7273 0.4181 0.2919 0.083 Uiso 0.25 1 d PR A 2 H80D H 0.6442 0.4181 0.3350 0.083 Uiso 0.25 1 d PR A 2 Cl9 Cl 0.7771(3) 0.40528(13) 0.32374(18) 0.0708(11) Uani 0.75 1 d P B 1 O10 O 0.5516(8) 0.3961(4) 0.1783(6) 0.083(4) Uani 0.75 1 d P C 1 H10 H 0.6194 0.3949 0.1800 0.124 Uiso 0.75 1 d P D 1 H10' H 0.5155 0.3710 0.1881 0.124 Uiso 0.75 1 d P E 1 Cl9' Cl 0.5707(9) 0.4131(4) 0.2581(5) 0.064(3) Uiso 0.25 1 d P B 2 Cl10 Cl 0.6644(2) 0.49206(10) 0.30325(12) 0.0675(8) Uani 1 1 d . B . C81 C 1.2653(9) 0.3604(4) 0.4798(4) 0.059(3) Uiso 1 1 d D . . H81A H 1.2752 0.3785 0.5118 0.088 Uiso 1 1 calc R . . H81B H 1.3033 0.3306 0.4833 0.088 Uiso 1 1 calc R . . H81C H 1.1918 0.3538 0.4730 0.088 Uiso 1 1 calc R . . C82 C 1.305(2) 0.3886(10) 0.4356(6) 0.220(14) Uiso 1 1 d D . . H82A H 1.3012 0.4227 0.4436 0.263 Uiso 1 1 calc R . . H82B H 1.3781 0.3805 0.4314 0.263 Uiso 1 1 calc R . . O11 O 1.2431(9) 0.3787(5) 0.3860(4) 0.139(5) Uiso 1 1 d D . . C83 C 1.1755(13) 0.3931(9) 0.3433(8) 0.172(10) Uiso 1 1 d D . . H83A H 1.2038 0.3829 0.3106 0.207 Uiso 1 1 calc R . . H83B H 1.1689 0.4279 0.3427 0.207 Uiso 1 1 calc R . . C84 C 1.0725(10) 0.3710(6) 0.3490(7) 0.111(6) Uiso 1 1 d D . . H84A H 1.0492 0.3559 0.3165 0.167 Uiso 1 1 calc R . . H84B H 1.0229 0.3954 0.3577 0.167 Uiso 1 1 calc R . . H84C H 1.0779 0.3473 0.3764 0.167 Uiso 1 1 calc R . . 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 0.0248(5) 0.0246(5) 0.0266(5) 0.0003(4) -0.0016(4) 0.0004(4) Co2 0.0211(5) 0.0233(5) 0.0271(6) 0.0002(4) -0.0007(4) 0.0006(4) Co3 0.0214(5) 0.0225(5) 0.0271(6) 0.0003(4) 0.0007(4) 0.0012(4) Co4 0.0206(5) 0.0237(5) 0.0270(6) 0.0003(4) 0.0003(4) 0.0010(4) Co5 0.0199(5) 0.0255(5) 0.0272(6) 0.0003(4) -0.0009(4) 0.0017(4) Co6 0.0214(5) 0.0279(6) 0.0283(6) -0.0011(4) -0.0013(4) 0.0018(4) N1 0.034(4) 0.022(3) 0.028(3) -0.001(3) -0.001(3) 0.000(3) N2 0.024(3) 0.023(3) 0.031(3) 0.000(3) 0.000(3) 0.003(3) N3 0.020(3) 0.017(3) 0.027(3) -0.001(2) 0.001(2) 0.003(2) N4 0.025(3) 0.020(3) 0.034(4) 0.001(3) 0.003(3) 0.001(3) N5 0.021(3) 0.028(3) 0.029(3) -0.003(3) 0.003(3) -0.001(3) N6 0.020(3) 0.031(4) 0.036(4) -0.002(3) 0.002(3) 0.005(3) N7 0.026(3) 0.024(3) 0.029(3) 0.000(3) -0.005(3) -0.004(3) N8 0.024(3) 0.023(3) 0.030(3) 0.000(3) -0.003(3) -0.001(3) N9 0.024(3) 0.023(3) 0.024(3) 0.001(3) 0.002(2) 0.001(3) N10 0.024(3) 0.028(3) 0.023(3) 0.002(3) 0.002(2) 0.003(3) N11 0.026(3) 0.028(3) 0.026(3) 0.003(3) -0.001(3) 0.002(3) N12 0.026(3) 0.030(3) 0.026(3) 0.001(3) 0.002(3) 0.004(3) N13 0.022(3) 0.028(3) 0.027(3) -0.002(3) 0.001(3) -0.001(3) N14 0.022(3) 0.031(3) 0.026(3) 0.000(3) -0.002(3) 0.005(3) N15 0.020(3) 0.019(3) 0.029(3) 0.002(2) -0.001(2) 0.001(2) N16 0.024(3) 0.020(3) 0.029(3) -0.002(3) -0.003(3) -0.001(2) N17 0.024(3) 0.028(3) 0.026(3) -0.001(3) -0.005(3) 0.000(3) N18 0.026(3) 0.032(4) 0.023(3) -0.001(3) 0.001(3) 0.003(3) N19 0.030(3) 0.021(3) 0.029(3) -0.001(3) -0.002(3) 0.002(3) N20 0.023(3) 0.024(3) 0.027(3) 0.003(3) -0.002(3) 0.001(3) N21 0.021(3) 0.023(3) 0.030(3) 0.000(3) -0.001(3) 0.001(2) N22 0.017(3) 0.024(3) 0.028(3) 0.003(3) -0.002(2) 0.000(2) N23 0.024(3) 0.029(3) 0.029(3) -0.001(3) -0.001(3) 0.001(3) N24 0.019(3) 0.028(3) 0.032(3) -0.001(3) -0.002(3) 0.001(3) C1 0.031(4) 0.031(4) 0.036(4) -0.005(3) 0.001(3) -0.005(3) C2 0.052(5) 0.027(4) 0.038(5) -0.005(4) -0.004(4) -0.005(4) C3 0.048(5) 0.028(4) 0.042(5) -0.007(4) 0.002(4) 0.001(4) C4 0.037(4) 0.024(4) 0.037(5) -0.002(3) 0.004(4) 0.001(3) C5 0.026(4) 0.029(4) 0.032(4) 0.002(3) 0.001(3) 0.000(3) C6 0.026(4) 0.023(4) 0.029(4) 0.004(3) -0.001(3) 0.001(3) C7 0.033(4) 0.035(4) 0.026(4) -0.004(3) 0.004(3) -0.002(3) C8 0.035(4) 0.029(4) 0.035(4) -0.001(3) 0.009(3) 0.002(3) C9 0.024(4) 0.027(4) 0.042(5) 0.000(3) 0.002(3) 0.000(3) C10 0.022(4) 0.019(3) 0.025(4) 0.002(3) 0.002(3) 0.003(3) C11 0.028(4) 0.030(4) 0.035(4) 0.001(3) 0.009(3) -0.001(3) C12 0.022(4) 0.030(4) 0.037(5) 0.000(3) 0.003(3) -0.002(3) C13 0.026(4) 0.022(4) 0.032(4) 0.003(3) 0.000(3) 0.000(3) C14 0.019(4) 0.030(4) 0.034(4) -0.006(3) 0.005(3) -0.001(3) C15 0.038(5) 0.036(5) 0.033(4) 0.000(4) 0.005(4) 0.003(4) C16 0.038(5) 0.043(5) 0.041(5) -0.003(4) 0.011(4) -0.010(4) C17 0.037(5) 0.048(5) 0.044(5) -0.013(4) 0.010(4) -0.012(4) C18 0.025(4) 0.033(4) 0.037(4) -0.007(4) -0.003(3) -0.004(3) C19 0.028(4) 0.034(4) 0.031(4) -0.001(3) -0.003(3) -0.002(3) C20 0.025(4) 0.040(5) 0.042(5) 0.001(4) 0.000(4) -0.006(4) C21 0.029(4) 0.036(5) 0.039(5) 0.003(4) 0.004(3) -0.006(4) C22 0.028(4) 0.035(4) 0.033(4) 0.002(4) -0.004(3) -0.004(3) C23 0.025(4) 0.025(4) 0.031(4) -0.005(3) 0.001(3) -0.001(3) C24 0.030(4) 0.028(4) 0.028(4) 0.000(3) 0.001(3) -0.001(3) C25 0.024(4) 0.029(4) 0.044(5) 0.000(4) -0.003(3) 0.001(3) C26 0.035(4) 0.019(4) 0.048(5) 0.004(3) -0.003(4) -0.003(3) C27 0.029(4) 0.026(4) 0.033(4) 0.007(3) -0.001(3) 0.001(3) C28 0.026(4) 0.023(4) 0.032(4) 0.002(3) 0.000(3) 0.001(3) C29 0.033(4) 0.026(4) 0.046(5) 0.007(4) -0.003(4) 0.004(3) C30 0.032(4) 0.027(4) 0.035(4) 0.008(3) -0.003(3) 0.006(3) C31 0.027(4) 0.027(4) 0.021(4) -0.001(3) 0.000(3) 0.002(3) C32 0.025(4) 0.029(4) 0.024(4) 0.004(3) 0.001(3) 0.003(3) C33 0.028(4) 0.032(4) 0.032(4) -0.002(3) -0.005(3) 0.004(3) C34 0.035(4) 0.039(5) 0.030(4) 0.003(4) 0.004(3) 0.010(4) C35 0.019(4) 0.044(5) 0.035(4) 0.004(4) 0.001(3) 0.003(3) C36 0.022(4) 0.033(4) 0.034(4) 0.003(3) -0.003(3) 0.002(3) C37 0.029(4) 0.037(4) 0.028(4) 0.006(3) -0.004(3) -0.001(3) C38 0.032(4) 0.032(4) 0.040(5) 0.010(4) -0.003(4) 0.008(4) C39 0.027(4) 0.030(4) 0.043(5) 0.004(4) 0.003(3) 0.006(3) C40 0.032(4) 0.026(4) 0.033(4) -0.002(3) -0.001(3) -0.002(3) C41 0.023(4) 0.023(4) 0.037(4) 0.003(3) -0.002(3) 0.003(3) C42 0.023(4) 0.015(3) 0.030(4) 0.000(3) 0.004(3) -0.002(3) C43 0.018(4) 0.033(4) 0.035(4) -0.001(3) -0.001(3) 0.003(3) C44 0.022(4) 0.032(4) 0.033(4) -0.001(3) 0.003(3) 0.001(3) C45 0.026(4) 0.025(4) 0.028(4) -0.004(3) 0.001(3) 0.000(3) C46 0.018(3) 0.021(4) 0.029(4) -0.002(3) 0.005(3) -0.002(3) C47 0.027(4) 0.038(5) 0.029(4) 0.000(3) 0.008(3) 0.000(3) C48 0.031(4) 0.030(4) 0.028(4) -0.001(3) 0.002(3) 0.004(3) C49 0.029(4) 0.020(4) 0.027(4) 0.000(3) 0.000(3) -0.001(3) C50 0.026(4) 0.027(4) 0.029(4) 0.000(3) 0.002(3) 0.003(3) C51 0.025(4) 0.039(5) 0.035(4) 0.000(4) 0.000(3) 0.002(3) C52 0.037(5) 0.037(5) 0.037(5) 0.011(4) 0.004(4) -0.001(4) C53 0.037(5) 0.039(5) 0.036(5) 0.008(4) -0.002(4) 0.006(4) C54 0.030(4) 0.036(5) 0.033(4) 0.004(4) -0.006(3) 0.003(4) C55 0.038(5) 0.027(4) 0.029(4) -0.002(3) -0.005(3) 0.000(3) C56 0.057(6) 0.029(4) 0.029(4) 0.000(3) 0.005(4) -0.001(4) C57 0.053(5) 0.037(5) 0.031(5) 0.003(4) 0.011(4) -0.002(4) C58 0.038(5) 0.025(4) 0.046(5) 0.006(4) 0.003(4) -0.004(4) C59 0.024(4) 0.023(4) 0.035(4) 0.001(3) 0.002(3) 0.003(3) C60 0.020(4) 0.027(4) 0.027(4) 0.002(3) 0.004(3) -0.001(3) C61 0.032(4) 0.028(4) 0.036(4) 0.004(3) -0.003(3) 0.004(3) C62 0.046(5) 0.019(4) 0.039(5) 0.006(3) -0.001(4) -0.001(4) C63 0.031(4) 0.026(4) 0.032(4) 0.004(3) 0.002(3) 0.002(3) C64 0.021(4) 0.022(4) 0.031(4) -0.001(3) 0.002(3) 0.004(3) C65 0.045(5) 0.018(4) 0.039(5) 0.003(3) -0.001(4) 0.001(3) C66 0.033(4) 0.027(4) 0.041(5) -0.007(4) -0.001(4) -0.006(3) C67 0.021(4) 0.024(4) 0.031(4) -0.005(3) 0.001(3) 0.002(3) C68 0.027(4) 0.030(4) 0.033(4) -0.004(3) 0.000(3) -0.008(3) C69 0.031(4) 0.033(4) 0.033(4) -0.006(4) -0.005(3) 0.006(3) C70 0.045(5) 0.035(5) 0.037(5) -0.004(4) 0.002(4) 0.006(4) C71 0.036(4) 0.041(5) 0.033(4) -0.006(4) 0.003(4) 0.004(4) C72 0.030(4) 0.034(4) 0.032(4) -0.004(4) -0.003(3) 0.003(3) S1 0.0449(13) 0.0424(13) 0.0458(13) -0.0020(10) -0.0080(10) -0.0011(10) O1 0.030(3) 0.040(3) 0.037(3) -0.002(3) -0.007(2) -0.005(3) O2 0.043(4) 0.114(7) 0.059(5) 0.011(5) 0.010(3) 0.012(4) O3 0.081(5) 0.052(4) 0.068(5) 0.014(4) -0.027(4) -0.008(4) C73 0.069(8) 0.067(8) 0.082(9) -0.022(7) -0.028(7) 0.007(6) F1 0.077(5) 0.097(6) 0.090(5) -0.040(4) -0.049(4) 0.012(4) F2 0.079(6) 0.249(14) 0.082(6) -0.063(7) 0.007(5) 0.044(7) F3 0.105(6) 0.050(4) 0.146(8) -0.028(5) -0.060(6) 0.014(4) S2 0.088(2) 0.0414(15) 0.121(3) 0.0022(17) -0.076(2) -0.0012(15) O4 0.028(3) 0.045(3) 0.030(3) 0.000(3) -0.004(2) 0.004(3) O6 0.119(7) 0.033(4) 0.103(7) -0.008(4) -0.048(6) 0.010(4) C74 0.102(10) 0.054(7) 0.075(9) -0.001(6) -0.044(8) 0.009(7) F4 0.073(5) 0.238(13) 0.070(5) -0.027(7) 0.024(4) -0.023(7) F5 0.100(5) 0.036(3) 0.103(5) 0.007(3) -0.043(4) -0.008(3) F6 0.107(6) 0.066(4) 0.071(4) 0.001(3) -0.050(4) 0.004(4) S3 0.0755(19) 0.0444(14) 0.0506(15) -0.0080(12) 0.0044(13) 0.0068(13) O7 0.110(7) 0.075(6) 0.057(5) 0.000(4) 0.021(5) -0.024(5) O8 0.102(7) 0.067(5) 0.072(6) -0.010(4) -0.004(5) -0.008(5) O9 0.110(7) 0.077(6) 0.091(7) -0.033(5) -0.011(6) 0.045(6) C75 0.082(8) 0.041(6) 0.061(7) 0.006(5) 0.011(6) 0.007(6) F7 0.087(5) 0.077(5) 0.064(4) -0.011(4) -0.015(4) -0.001(4) F8 0.079(5) 0.075(5) 0.082(5) -0.026(4) 0.010(4) 0.027(4) F9 0.148(8) 0.083(5) 0.069(5) 0.017(4) 0.026(5) -0.019(5) C76 0.076(8) 0.048(6) 0.087(9) -0.012(6) -0.011(7) 0.003(6) Cl1 0.074(2) 0.0587(18) 0.093(2) -0.0139(16) -0.0051(17) -0.0192(15) Cl2 0.080(2) 0.0487(17) 0.128(3) -0.0067(18) 0.003(2) -0.0194(15) C77 0.121(12) 0.049(7) 0.074(8) -0.008(6) -0.010(8) 0.005(7) Cl3 0.0483(15) 0.0514(16) 0.109(2) -0.0078(16) 0.0080(15) 0.0012(12) Cl4 0.115(3) 0.176(5) 0.102(3) 0.070(3) -0.005(3) -0.009(3) C78 0.074(8) 0.061(8) 0.114(11) 0.041(8) -0.001(8) 0.000(6) Cl5 0.091(2) 0.058(2) 0.158(4) 0.039(2) 0.032(2) 0.0236(18) Cl6 0.133(4) 0.093(3) 0.198(6) -0.030(3) -0.066(4) 0.026(3) C80 0.073(8) 0.052(7) 0.084(8) -0.006(6) 0.020(6) -0.011(6) Cl9 0.077(3) 0.046(2) 0.090(3) -0.0122(19) 0.010(2) -0.0078(18) O10 0.058(6) 0.039(6) 0.147(11) 0.011(6) -0.024(7) -0.014(5) Cl10 0.0784(19) 0.0445(14) 0.083(2) -0.0122(14) 0.0350(16) -0.0094(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N7 1.959(6) . ? Co1 N19 1.979(6) . ? Co1 N1 1.980(6) . ? Co1 N13 1.983(6) . ? Co1 O1 2.254(5) . ? Co1 Co2 2.2926(13) . ? Co2 N8 1.905(6) . ? Co2 N20 1.912(6) . ? Co2 N14 1.912(6) . ? Co2 N2 1.916(6) . ? Co2 Co3 2.2506(13) . ? Co3 N3 1.933(6) . ? Co3 N15 1.937(6) . ? Co3 N9 1.941(6) . ? Co3 N21 1.943(6) . ? Co3 Co4 2.2507(13) . ? Co4 N10 1.926(6) . ? Co4 N16 1.933(6) . ? Co4 N22 1.934(6) . ? Co4 N4 1.934(6) . ? Co4 Co5 2.2471(13) . ? Co5 N5 1.903(6) . ? Co5 N23 1.912(6) . ? Co5 N17 1.915(7) . ? Co5 N11 1.916(6) . ? Co5 Co6 2.2757(13) . ? Co6 N12 1.963(6) . ? Co6 N18 1.966(7) . ? Co6 N6 1.968(7) . ? Co6 N24 1.977(6) . ? Co6 O4 2.234(5) . ? N1 C5 1.352(10) . ? N1 C1 1.355(10) . ? N2 C6 1.347(10) . ? N2 C5 1.381(10) . ? N3 C6 1.360(10) . ? N3 C10 1.367(9) . ? N4 C10 1.367(10) . ? N4 C13 1.371(10) . ? N5 C13 1.369(10) . ? N5 C14 1.373(10) . ? N6 C14 1.359(10) . ? N6 C18 1.362(10) . ? N7 C19 1.357(10) . ? N7 C23 1.369(10) . ? N8 C24 1.370(10) . ? N8 C23 1.385(10) . ? N9 C28 1.360(9) . ? N9 C24 1.363(10) . ? N10 C31 1.367(9) . ? N10 C28 1.379(10) . ? N11 C31 1.366(10) . ? N11 C32 1.377(9) . ? N12 C36 1.356(10) . ? N12 C32 1.366(10) . ? N13 C37 1.345(10) . ? N13 C41 1.362(10) . ? N14 C42 1.361(10) . ? N14 C41 1.371(9) . ? N15 C42 1.354(9) . ? N15 C46 1.373(10) . ? N16 C49 1.353(10) . ? N16 C46 1.377(9) . ? N17 C49 1.359(10) . ? N17 C50 1.390(10) . ? N18 C50 1.344(10) . ? N18 C54 1.361(10) . ? N19 C55 1.343(10) . ? N19 C59 1.356(10) . ? N20 C60 1.367(10) . ? N20 C59 1.379(10) . ? N21 C60 1.335(10) . ? N21 C64 1.373(9) . ? N22 C67 1.361(9) . ? N22 C64 1.370(9) . ? N23 C67 1.364(10) . ? N23 C68 1.368(10) . ? N24 C72 1.356(10) . ? N24 C68 1.372(10) . ? C1 C2 1.360(12) . ? C2 C3 1.402(13) . ? C3 C4 1.368(12) . ? C4 C5 1.400(11) . ? C6 C7 1.437(11) . ? C7 C8 1.363(11) . ? C8 C9 1.407(12) . ? C9 C10 1.397(11) . ? C9 C11 1.428(11) . ? C11 C12 1.354(11) . ? C12 C13 1.413(11) . ? C14 C15 1.414(12) . ? C15 C16 1.359(12) . ? C16 C17 1.371(13) . ? C17 C18 1.375(12) . ? C19 C20 1.348(12) . ? C20 C21 1.392(12) . ? C21 C22 1.383(11) . ? C22 C23 1.397(11) . ? C24 C25 1.431(11) . ? C25 C26 1.349(11) . ? C26 C27 1.416(11) . ? C27 C28 1.397(11) . ? C27 C29 1.412(11) . ? C29 C30 1.359(12) . ? C30 C31 1.417(11) . ? C32 C33 1.407(11) . ? C33 C34 1.366(11) . ? C34 C35 1.398(12) . ? C35 C36 1.368(12) . ? C37 C38 1.369(12) . ? C38 C39 1.408(12) . ? C39 C40 1.368(11) . ? C40 C41 1.416(11) . ? C42 C43 1.419(11) . ? C43 C44 1.350(11) . ? C44 C45 1.415(11) . ? C45 C46 1.400(10) . ? C45 C47 1.404(11) . ? C47 C48 1.379(11) . ? C48 C49 1.414(11) . ? C50 C51 1.396(11) . ? C51 C52 1.382(12) . ? C52 C53 1.390(12) . ? C53 C54 1.373(12) . ? C55 C56 1.367(12) . ? C56 C57 1.398(13) . ? C57 C58 1.370(12) . ? C58 C59 1.412(11) . ? C60 C61 1.439(11) . ? C61 C62 1.358(12) . ? C62 C63 1.416(11) . ? C63 C65 1.405(11) . ? C63 C64 1.411(11) . ? C65 C66 1.362(12) . ? C66 C67 1.429(11) . ? C68 C69 1.394(11) . ? C69 C70 1.376(12) . ? C70 C71 1.387(12) . ? C71 C72 1.370(12) . ? S1 O3 1.408(8) . ? S1 O2 1.434(8) . ? S1 O1 1.460(6) . ? S1 C73 1.804(13) . ? C73 F3 1.282(16) . ? C73 F1 1.325(13) . ? C73 F2 1.370(17) . ? S2 O6 1.326(9) . ? S2 O4 1.420(6) . ? S2 C74 1.731(13) . ? S2 O5 1.735(13) . ? C74 F5 1.306(15) . ? C74 F6 1.329(13) . ? C74 F4 1.368(17) . ? S3 O9 1.399(9) . ? S3 O7 1.417(9) . ? S3 O8 1.448(10) . ? S3 C75 1.835(12) . ? C75 F7 1.316(14) . ? C75 F8 1.321(13) . ? C75 F9 1.324(13) . ? C76 Cl2 1.732(12) . ? C76 Cl1 1.820(12) . ? C77 Cl4 1.685(14) . ? C77 Cl3 1.744(13) . ? C78 Cl6 1.737(15) . ? C78 Cl5 1.740(12) . ? C79 Cl8 1.616(9) . ? C79 Cl7 1.635(9) . ? C80 Cl9' 1.633(17) . ? C80 Cl10 1.744(12) . ? C80 Cl9 1.762(14) . ? C81 C82 1.518(10) . ? C82 O11 1.506(10) . ? O11 C83 1.436(10) . ? C83 C84 1.492(10) . ? 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 N7 Co1 N19 174.1(3) . . ? N7 Co1 N1 87.6(3) . . ? N19 Co1 N1 91.1(3) . . ? N7 Co1 N13 90.4(3) . . ? N19 Co1 N13 90.2(3) . . ? N1 Co1 N13 172.7(3) . . ? N7 Co1 O1 93.3(2) . . ? N19 Co1 O1 92.4(2) . . ? N1 Co1 O1 90.7(2) . . ? N13 Co1 O1 96.4(2) . . ? N7 Co1 Co2 87.51(18) . . ? N19 Co1 Co2 86.72(18) . . ? N1 Co1 Co2 86.86(18) . . ? N13 Co1 Co2 86.07(18) . . ? O1 Co1 Co2 177.43(16) . . ? N8 Co2 N20 179.1(3) . . ? N8 Co2 N14 89.9(3) . . ? N20 Co2 N14 90.2(3) . . ? N8 Co2 N2 90.5(3) . . ? N20 Co2 N2 89.3(3) . . ? N14 Co2 N2 178.4(3) . . ? N8 Co2 Co3 89.70(18) . . ? N20 Co2 Co3 89.43(18) . . ? N14 Co2 Co3 90.22(18) . . ? N2 Co2 Co3 88.28(18) . . ? N8 Co2 Co1 90.18(18) . . ? N20 Co2 Co1 90.69(18) . . ? N14 Co2 Co1 91.60(18) . . ? N2 Co2 Co1 89.91(18) . . ? Co3 Co2 Co1 178.18(6) . . ? N3 Co3 N15 179.2(3) . . ? N3 Co3 N9 90.9(2) . . ? N15 Co3 N9 89.9(2) . . ? N3 Co3 N21 89.6(3) . . ? N15 Co3 N21 89.7(3) . . ? N9 Co3 N21 179.4(3) . . ? N3 Co3 Co2 91.06(18) . . ? N15 Co3 Co2 88.88(18) . . ? N9 Co3 Co2 90.04(18) . . ? N21 Co3 Co2 89.58(18) . . ? N3 Co3 Co4 89.15(18) . . ? N15 Co3 Co4 90.91(18) . . ? N9 Co3 Co4 90.03(18) . . ? N21 Co3 Co4 90.35(18) . . ? Co2 Co3 Co4 179.77(7) . . ? N10 Co4 N16 90.1(3) . . ? N10 Co4 N22 179.7(3) . . ? N16 Co4 N22 89.7(3) . . ? N10 Co4 N4 90.6(3) . . ? N16 Co4 N4 179.2(3) . . ? N22 Co4 N4 89.6(3) . . ? N10 Co4 Co5 89.87(18) . . ? N16 Co4 Co5 90.40(18) . . ? N22 Co4 Co5 89.91(17) . . ? N4 Co4 Co5 89.18(19) . . ? N10 Co4 Co3 90.09(18) . . ? N16 Co4 Co3 89.60(18) . . ? N22 Co4 Co3 90.13(17) . . ? N4 Co4 Co3 90.82(19) . . ? Co5 Co4 Co3 179.96(8) . . ? N5 Co5 N23 89.7(3) . . ? N5 Co5 N17 179.0(3) . . ? N23 Co5 N17 89.6(3) . . ? N5 Co5 N11 90.6(3) . . ? N23 Co5 N11 179.0(3) . . ? N17 Co5 N11 90.0(3) . . ? N5 Co5 Co4 90.35(19) . . ? N23 Co5 Co4 89.56(19) . . ? N17 Co5 Co4 88.83(18) . . ? N11 Co5 Co4 89.49(19) . . ? N5 Co5 Co6 91.10(19) . . ? N23 Co5 Co6 90.65(19) . . ? N17 Co5 Co6 89.72(18) . . ? N11 Co5 Co6 90.29(19) . . ? Co4 Co5 Co6 178.53(6) . . ? N12 Co6 N18 89.0(3) . . ? N12 Co6 N6 89.6(3) . . ? N18 Co6 N6 172.9(3) . . ? N12 Co6 N24 172.6(3) . . ? N18 Co6 N24 89.3(3) . . ? N6 Co6 N24 91.2(3) . . ? N12 Co6 O4 92.9(2) . . ? N18 Co6 O4 92.5(2) . . ? N6 Co6 O4 94.5(2) . . ? N24 Co6 O4 94.3(2) . . ? N12 Co6 Co5 86.68(18) . . ? N18 Co6 Co5 86.95(18) . . ? N6 Co6 Co5 86.06(19) . . ? N24 Co6 Co5 86.06(18) . . ? O4 Co6 Co5 179.28(16) . . ? C5 N1 C1 118.3(7) . . ? C5 N1 Co1 120.4(5) . . ? C1 N1 Co1 120.4(5) . . ? C6 N2 C5 123.0(6) . . ? C6 N2 Co2 120.1(5) . . ? C5 N2 Co2 116.3(5) . . ? C6 N3 C10 120.3(6) . . ? C6 N3 Co3 118.2(5) . . ? C10 N3 Co3 121.3(5) . . ? C10 N4 C13 119.3(6) . . ? C10 N4 Co4 119.8(5) . . ? C13 N4 Co4 120.8(5) . . ? C13 N5 C14 123.2(6) . . ? C13 N5 Co5 119.4(5) . . ? C14 N5 Co5 117.2(5) . . ? C14 N6 C18 117.3(7) . . ? C14 N6 Co6 121.8(5) . . ? C18 N6 Co6 120.8(6) . . ? C19 N7 C23 117.9(7) . . ? C19 N7 Co1 120.6(5) . . ? C23 N7 Co1 121.5(5) . . ? C24 N8 C23 121.4(6) . . ? C24 N8 Co2 119.5(5) . . ? C23 N8 Co2 119.1(5) . . ? C28 N9 C24 120.0(6) . . ? C28 N9 Co3 120.2(5) . . ? C24 N9 Co3 119.5(5) . . ? C31 N10 C28 118.7(6) . . ? C31 N10 Co4 120.5(5) . . ? C28 N10 Co4 120.4(5) . . ? C31 N11 C32 123.1(6) . . ? C31 N11 Co5 119.1(5) . . ? C32 N11 Co5 117.8(5) . . ? C36 N12 C32 118.5(6) . . ? C36 N12 Co6 120.1(5) . . ? C32 N12 Co6 121.4(5) . . ? C37 N13 C41 118.7(7) . . ? C37 N13 Co1 119.8(5) . . ? C41 N13 Co1 121.3(5) . . ? C42 N14 C41 124.0(6) . . ? C42 N14 Co2 119.2(5) . . ? C41 N14 Co2 116.7(5) . . ? C42 N15 C46 119.2(6) . . ? C42 N15 Co3 121.2(5) . . ? C46 N15 Co3 119.6(5) . . ? C49 N16 C46 119.7(6) . . ? C49 N16 Co4 119.3(5) . . ? C46 N16 Co4 120.5(5) . . ? C49 N17 C50 123.5(6) . . ? C49 N17 Co5 119.2(5) . . ? C50 N17 Co5 117.1(5) . . ? C50 N18 C54 118.5(7) . . ? C50 N18 Co6 121.0(5) . . ? C54 N18 Co6 120.4(5) . . ? C55 N19 C59 118.1(7) . . ? C55 N19 Co1 120.6(5) . . ? C59 N19 Co1 121.1(5) . . ? C60 N20 C59 123.3(6) . . ? C60 N20 Co2 119.0(5) . . ? C59 N20 Co2 117.3(5) . . ? C60 N21 C64 120.2(6) . . ? C60 N21 Co3 120.0(5) . . ? C64 N21 Co3 119.6(5) . . ? C67 N22 C64 119.7(6) . . ? C67 N22 Co4 119.9(5) . . ? C64 N22 Co4 120.2(5) . . ? C67 N23 C68 123.0(7) . . ? C67 N23 Co5 119.0(5) . . ? C68 N23 Co5 117.6(5) . . ? C72 N24 C68 118.1(7) . . ? C72 N24 Co6 120.9(5) . . ? C68 N24 Co6 120.8(5) . . ? N1 C1 C2 123.1(8) . . ? C1 C2 C3 118.9(8) . . ? C4 C3 C2 118.7(8) . . ? C3 C4 C5 119.8(8) . . ? N1 C5 N2 115.5(7) . . ? N1 C5 C4 121.1(7) . . ? N2 C5 C4 123.1(7) . . ? N2 C6 N3 116.2(7) . . ? N2 C6 C7 124.4(7) . . ? N3 C6 C7 119.2(7) . . ? C8 C7 C6 120.1(7) . . ? C7 C8 C9 120.4(7) . . ? C10 C9 C8 117.9(7) . . ? C10 C9 C11 117.1(7) . . ? C8 C9 C11 125.0(8) . . ? N3 C10 N4 115.1(6) . . ? N3 C10 C9 122.1(7) . . ? N4 C10 C9 122.8(7) . . ? C12 C11 C9 120.0(7) . . ? C11 C12 C13 121.0(7) . . ? N5 C13 N4 114.2(7) . . ? N5 C13 C12 125.8(7) . . ? N4 C13 C12 119.8(7) . . ? N6 C14 N5 114.5(7) . . ? N6 C14 C15 120.2(7) . . ? N5 C14 C15 125.0(7) . . ? C16 C15 C14 120.5(8) . . ? C15 C16 C17 119.7(8) . . ? C16 C17 C18 118.3(8) . . ? N6 C18 C17 124.0(8) . . ? C20 C19 N7 123.9(7) . . ? C19 C20 C21 118.8(7) . . ? C22 C21 C20 118.9(8) . . ? C21 C22 C23 119.8(7) . . ? N7 C23 N8 114.1(7) . . ? N7 C23 C22 120.4(7) . . ? N8 C23 C22 125.3(7) . . ? N9 C24 N8 115.3(7) . . ? N9 C24 C25 119.2(7) . . ? N8 C24 C25 125.3(7) . . ? C26 C25 C24 120.4(7) . . ? C25 C26 C27 120.5(7) . . ? C28 C27 C29 117.6(7) . . ? C28 C27 C26 117.3(7) . . ? C29 C27 C26 125.0(7) . . ? N9 C28 N10 115.2(6) . . ? N9 C28 C27 122.4(7) . . ? N10 C28 C27 122.3(7) . . ? C30 C29 C27 120.8(7) . . ? C29 C30 C31 119.7(7) . . ? N11 C31 N10 114.3(6) . . ? N11 C31 C30 124.7(7) . . ? N10 C31 C30 120.8(7) . . ? N12 C32 N11 114.2(6) . . ? N12 C32 C33 120.1(7) . . ? N11 C32 C33 125.6(7) . . ? C34 C33 C32 120.5(7) . . ? C33 C34 C35 118.9(8) . . ? C36 C35 C34 118.9(7) . . ? N12 C36 C35 123.0(7) . . ? N13 C37 C38 123.7(7) . . ? C37 C38 C39 118.5(7) . . ? C40 C39 C38 118.6(8) . . ? C39 C40 C41 120.5(7) . . ? N13 C41 N14 115.9(7) . . ? N13 C41 C40 120.0(7) . . ? N14 C41 C40 124.0(7) . . ? N15 C42 N14 114.9(6) . . ? N15 C42 C43 119.8(7) . . ? N14 C42 C43 125.1(7) . . ? C44 C43 C42 120.9(7) . . ? C43 C44 C45 120.3(7) . . ? C46 C45 C47 118.1(7) . . ? C46 C45 C44 117.0(7) . . ? C47 C45 C44 125.0(7) . . ? N15 C46 N16 115.4(6) . . ? N15 C46 C45 122.7(6) . . ? N16 C46 C45 121.8(7) . . ? C48 C47 C45 120.0(7) . . ? C47 C48 C49 119.9(7) . . ? N16 C49 N17 115.4(7) . . ? N16 C49 C48 120.5(7) . . ? N17 C49 C48 124.0(7) . . ? N18 C50 N17 114.7(7) . . ? N18 C50 C51 121.6(7) . . ? N17 C50 C51 123.4(7) . . ? C52 C51 C50 119.2(7) . . ? C51 C52 C53 119.4(8) . . ? C54 C53 C52 118.6(8) . . ? N18 C54 C53 122.7(7) . . ? N19 C55 C56 124.3(8) . . ? C55 C56 C57 117.9(8) . . ? C58 C57 C56 119.3(8) . . ? C57 C58 C59 119.7(8) . . ? N19 C59 N20 115.3(7) . . ? N19 C59 C58 120.6(7) . . ? N20 C59 C58 123.7(7) . . ? N21 C60 N20 115.8(6) . . ? N21 C60 C61 120.0(7) . . ? N20 C60 C61 124.0(7) . . ? C62 C61 C60 119.9(7) . . ? C61 C62 C63 120.5(7) . . ? C65 C63 C64 117.5(7) . . ? C65 C63 C62 125.4(7) . . ? C64 C63 C62 116.9(7) . . ? N22 C64 N21 115.8(6) . . ? N22 C64 C63 122.0(7) . . ? N21 C64 C63 122.1(7) . . ? C66 C65 C63 120.7(7) . . ? C65 C66 C67 119.9(7) . . ? N22 C67 N23 115.2(6) . . ? N22 C67 C66 120.0(7) . . ? N23 C67 C66 124.6(7) . . ? N23 C68 N24 114.5(7) . . ? N23 C68 C69 124.5(7) . . ? N24 C68 C69 120.5(7) . . ? C70 C69 C68 119.8(8) . . ? C69 C70 C71 120.1(8) . . ? C72 C71 C70 117.9(8) . . ? N24 C72 C71 123.7(7) . . ? O3 S1 O2 115.4(5) . . ? O3 S1 O1 113.6(4) . . ? O2 S1 O1 115.0(4) . . ? O3 S1 C73 105.9(6) . . ? O2 S1 C73 103.3(6) . . ? O1 S1 C73 101.6(5) . . ? S1 O1 Co1 155.8(4) . . ? F3 C73 F1 109.3(11) . . ? F3 C73 F2 105.3(12) . . ? F1 C73 F2 107.6(11) . . ? F3 C73 S1 113.9(10) . . ? F1 C73 S1 111.7(9) . . ? F2 C73 S1 108.6(9) . . ? O6 S2 O4 123.5(5) . . ? O6 S2 C74 115.7(6) . . ? O4 S2 C74 108.0(5) . . ? O6 S2 O5 105.3(7) . . ? O4 S2 O5 105.7(5) . . ? C74 S2 O5 93.8(7) . . ? S2 O4 Co6 166.4(4) . . ? F5 C74 F6 107.8(10) . . ? F5 C74 F4 110.0(12) . . ? F6 C74 F4 110.7(12) . . ? F5 C74 S2 115.0(10) . . ? F6 C74 S2 113.8(9) . . ? F4 C74 S2 99.3(9) . . ? O9 S3 O7 121.5(7) . . ? O9 S3 O8 111.6(6) . . ? O7 S3 O8 112.5(6) . . ? O9 S3 C75 102.9(6) . . ? O7 S3 C75 103.9(5) . . ? O8 S3 C75 101.4(6) . . ? F7 C75 F8 108.0(9) . . ? F7 C75 F9 108.6(10) . . ? F8 C75 F9 107.3(10) . . ? F7 C75 S3 110.6(8) . . ? F8 C75 S3 111.1(8) . . ? F9 C75 S3 111.1(8) . . ? Cl2 C76 Cl1 108.8(7) . . ? Cl4 C77 Cl3 112.2(7) . . ? Cl6 C78 Cl5 111.8(7) . . ? Cl8 C79 Cl7 115.0(10) . . ? Cl9' C80 Cl10 110.6(9) . . ? Cl9' C80 Cl9 132.2(9) . . ? Cl10 C80 Cl9 111.4(7) . . ? O11 C82 C81 111.3(10) . . ? C83 O11 C82 152(2) . . ? O11 C83 C84 108.5(10) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.719 _refine_diff_density_min -2.155 _refine_diff_density_rms 0.230 #===END