# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Wolfram Willy Seidel' 'Florian Hupka' 'Matthias J. Meel' 'Jan Weigand' _publ_contact_author_name 'Wolfram Willy Seidel' _publ_contact_author_email SEIDELWW@UNI-MUENSTER.DE _publ_section_title ; Acetylendithiolate as directional ligand in cobalt(I) alkyne platinum dithiolato bimetallic complexes ; # Attachment 'comp_2-PF6.cif' data_sad _database_code_depnum_ccdc_archive 'CCDC 740232' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C23 H47 Co P3 S2 Si, F6 P ' _chemical_formula_sum 'C23 H47 Co F6 P4 S2 Si' _chemical_formula_weight 712.63 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7241(7) _cell_length_b 23.9821(14) _cell_length_c 12.5138(8) _cell_angle_alpha 90.00 _cell_angle_beta 101.5140(10) _cell_angle_gamma 90.00 _cell_volume 3447.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description rod _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.885 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8861 _exptl_absorpt_correction_T_max 0.9739 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.784003 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18610 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.88 _reflns_number_total 8208 _reflns_number_gt 6253 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2(Bruker AXS, 2007)' _computing_cell_refinement 'APEX2(Bruker AXS, 2007)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2007 )' _computing_structure_solution ; SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_structure_refinement ; SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+0.3905P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8208 _refine_ls_number_parameters 346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.26170(2) 0.117892(11) 0.22310(2) 0.01921(8) Uani 1 1 d . . . P2 P 0.15422(5) 0.19477(2) 0.19851(5) 0.02451(13) Uani 1 1 d . . . S1 S 0.47279(5) 0.02900(2) 0.19737(5) 0.02934(14) Uani 1 1 d . . . P3 P 0.32919(5) 0.11305(2) 0.39543(5) 0.02759(14) Uani 1 1 d . . . P1 P 0.12723(5) 0.05599(2) 0.22486(5) 0.02777(14) Uani 1 1 d . . . Si1 Si 0.65790(5) 0.18509(3) -0.16692(5) 0.02644(14) Uani 1 1 d . . . S2 S 0.41022(5) 0.19039(2) 0.06270(5) 0.03173(14) Uani 1 1 d . . . C2 C 0.36828(18) 0.13776(9) 0.13764(18) 0.0229(4) Uani 1 1 d . . . C1 C 0.38665(18) 0.08676(9) 0.17711(18) 0.0233(5) Uani 1 1 d . . . C9 C 0.69037(18) -0.00147(9) 0.17943(18) 0.0247(5) Uani 1 1 d . . . C20 C 0.2356(2) 0.25821(9) 0.2435(2) 0.0367(6) Uani 1 1 d . . . H20A H 0.1869 0.2908 0.2195 0.055 Uiso 1 1 calc R . . H20B H 0.3057 0.2596 0.2120 0.055 Uiso 1 1 calc R . . H20C H 0.2581 0.2583 0.3233 0.055 Uiso 1 1 calc R . . C4 C 0.55874(19) 0.20942(9) -0.07525(19) 0.0270(5) Uani 1 1 d . . . H4A H 0.5968 0.2407 -0.0300 0.032 Uiso 1 1 calc R . . H4B H 0.4861 0.2239 -0.1211 0.032 Uiso 1 1 calc R . . C3 C 0.5275(2) 0.16428(9) -0.0001(2) 0.0303(5) Uani 1 1 d . . . H3A H 0.5964 0.1550 0.0570 0.036 Uiso 1 1 calc R . . H3B H 0.5021 0.1301 -0.0424 0.036 Uiso 1 1 calc R . . C14 C 0.7520(2) -0.00827(10) 0.2852(2) 0.0320(5) Uani 1 1 d . . . H14 H 0.7407 0.0171 0.3405 0.038 Uiso 1 1 calc R . . C19 C 0.0985(2) 0.20996(10) 0.0547(2) 0.0343(6) Uani 1 1 d . . . H19A H 0.0553 0.2452 0.0480 0.051 Uiso 1 1 calc R . . H19B H 0.0467 0.1798 0.0221 0.051 Uiso 1 1 calc R . . H19C H 0.1637 0.2131 0.0167 0.051 Uiso 1 1 calc R . . C8 C 0.6071(2) 0.04630(10) 0.1513(2) 0.0336(5) Uani 1 1 d . . . H8A H 0.5904 0.0527 0.0716 0.040 Uiso 1 1 calc R . . H8B H 0.6416 0.0808 0.1877 0.040 Uiso 1 1 calc R . . C13 C 0.8301(2) -0.05209(11) 0.3109(2) 0.0370(6) Uani 1 1 d . . . H13 H 0.8721 -0.0565 0.3836 0.044 Uiso 1 1 calc R . . C17 C 0.1758(2) -0.01546(9) 0.2150(2) 0.0406(6) Uani 1 1 d . . . H17A H 0.2339 -0.0248 0.2804 0.061 Uiso 1 1 calc R . . H17B H 0.2104 -0.0194 0.1504 0.061 Uiso 1 1 calc R . . H17C H 0.1092 -0.0408 0.2091 0.061 Uiso 1 1 calc R . . C22 C 0.4719(2) 0.14500(12) 0.4189(2) 0.0452(7) Uani 1 1 d . . . H22A H 0.5024 0.1479 0.4975 0.068 Uiso 1 1 calc R . . H22B H 0.4660 0.1823 0.3863 0.068 Uiso 1 1 calc R . . H22C H 0.5245 0.1221 0.3855 0.068 Uiso 1 1 calc R . . C21 C 0.2562(3) 0.15030(11) 0.4893(2) 0.0438(7) Uani 1 1 d . . . H21A H 0.2965 0.1430 0.5645 0.066 Uiso 1 1 calc R . . H21B H 0.1754 0.1375 0.4795 0.066 Uiso 1 1 calc R . . H21C H 0.2575 0.1904 0.4746 0.066 Uiso 1 1 calc R . . C6 C 0.7924(2) 0.15587(12) -0.0810(2) 0.0468(7) Uani 1 1 d . . . H6A H 0.7723 0.1235 -0.0406 0.070 Uiso 1 1 calc R . . H6B H 0.8296 0.1843 -0.0294 0.070 Uiso 1 1 calc R . . H6C H 0.8461 0.1444 -0.1276 0.070 Uiso 1 1 calc R . . F6 F 0.96952(19) 0.15599(8) 0.51670(19) 0.0870(7) Uani 1 1 d . . . C12 C 0.8470(2) -0.08911(10) 0.2318(2) 0.0402(7) Uani 1 1 d . . . H12 H 0.9008 -0.1189 0.2497 0.048 Uiso 1 1 calc R . . C18 C 0.0240(2) 0.20499(11) 0.2552(2) 0.0407(6) Uani 1 1 d . . . H18A H 0.0440 0.2012 0.3348 0.061 Uiso 1 1 calc R . . H18B H -0.0345 0.1769 0.2251 0.061 Uiso 1 1 calc R . . H18C H -0.0076 0.2423 0.2363 0.061 Uiso 1 1 calc R . . C5 C 0.5780(2) 0.13078(11) -0.2588(2) 0.0434(7) Uani 1 1 d . . . H5A H 0.6241 0.1198 -0.3126 0.065 Uiso 1 1 calc R . . H5B H 0.5029 0.1458 -0.2965 0.065 Uiso 1 1 calc R . . H5C H 0.5648 0.0982 -0.2157 0.065 Uiso 1 1 calc R . . C16 C 0.0466(2) 0.05340(11) 0.3341(3) 0.0462(7) Uani 1 1 d . . . H16A H -0.0151 0.0253 0.3170 0.069 Uiso 1 1 calc R . . H16B H 0.0118 0.0900 0.3418 0.069 Uiso 1 1 calc R . . H16C H 0.0993 0.0435 0.4025 0.069 Uiso 1 1 calc R . . C23 C 0.3606(2) 0.04553(10) 0.4600(2) 0.0413(6) Uani 1 1 d . . . H23A H 0.4083 0.0236 0.4194 0.062 Uiso 1 1 calc R . . H23B H 0.2875 0.0258 0.4603 0.062 Uiso 1 1 calc R . . H23C H 0.4030 0.0507 0.5351 0.062 Uiso 1 1 calc R . . C11 C 0.7855(2) -0.08280(11) 0.1263(2) 0.0439(7) Uani 1 1 d . . . H11 H 0.7970 -0.1083 0.0713 0.053 Uiso 1 1 calc R . . C15 C 0.0111(2) 0.06098(11) 0.1041(3) 0.0483(7) Uani 1 1 d . . . H15A H -0.0432 0.0299 0.1034 0.072 Uiso 1 1 calc R . . H15B H 0.0448 0.0594 0.0384 0.072 Uiso 1 1 calc R . . H15C H -0.0305 0.0963 0.1055 0.072 Uiso 1 1 calc R . . C10 C 0.7072(2) -0.03941(11) 0.1007(2) 0.0364(6) Uani 1 1 d . . . H10 H 0.6644 -0.0356 0.0282 0.044 Uiso 1 1 calc R . . C7 C 0.6931(2) 0.24572(11) -0.2474(2) 0.0446(7) Uani 1 1 d . . . H7A H 0.7356 0.2737 -0.1979 0.067 Uiso 1 1 calc R . . H7B H 0.6208 0.2621 -0.2883 0.067 Uiso 1 1 calc R . . H7C H 0.7414 0.2333 -0.2984 0.067 Uiso 1 1 calc R . . P4 P 0.84645(6) 0.13089(3) 0.52350(6) 0.03744(17) Uani 1 1 d . . . F2 F 0.90336(15) 0.07040(7) 0.53075(15) 0.0595(5) Uani 1 1 d . . . F1 F 0.87848(16) 0.13599(8) 0.65322(14) 0.0623(5) Uani 1 1 d . . . F3 F 0.81479(18) 0.12527(7) 0.39395(14) 0.0665(5) Uani 1 1 d . . . F4 F 0.7883(2) 0.18981(9) 0.51633(16) 0.1073(10) Uani 1 1 d . . . F5 F 0.72643(16) 0.10186(12) 0.53149(19) 0.0981(8) 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 0.01867(14) 0.01835(14) 0.02174(15) 0.00040(11) 0.00677(11) 0.00093(11) P2 0.0236(3) 0.0202(3) 0.0312(3) 0.0015(2) 0.0091(2) 0.0037(2) S1 0.0262(3) 0.0270(3) 0.0373(3) 0.0054(2) 0.0122(2) 0.0079(2) P3 0.0337(3) 0.0258(3) 0.0230(3) 0.0007(2) 0.0049(2) 0.0028(2) P1 0.0243(3) 0.0220(3) 0.0389(4) -0.0030(2) 0.0109(3) -0.0029(2) Si1 0.0239(3) 0.0307(3) 0.0257(3) 0.0030(3) 0.0073(3) 0.0017(3) S2 0.0313(3) 0.0285(3) 0.0406(4) 0.0090(3) 0.0194(3) 0.0045(2) C2 0.0198(10) 0.0278(11) 0.0222(11) 0.0011(9) 0.0067(9) -0.0004(9) C1 0.0207(10) 0.0258(11) 0.0241(11) -0.0022(9) 0.0067(9) 0.0028(8) C9 0.0191(10) 0.0247(11) 0.0310(12) 0.0048(9) 0.0067(9) 0.0020(8) C20 0.0436(15) 0.0230(12) 0.0444(15) -0.0036(11) 0.0107(12) -0.0011(10) C4 0.0270(11) 0.0276(12) 0.0291(12) 0.0072(9) 0.0118(10) 0.0050(9) C3 0.0296(12) 0.0307(12) 0.0351(13) 0.0066(10) 0.0172(10) 0.0052(10) C14 0.0342(13) 0.0343(13) 0.0284(12) -0.0010(10) 0.0086(10) -0.0020(10) C19 0.0297(13) 0.0350(13) 0.0373(14) 0.0075(11) 0.0045(11) 0.0054(10) C8 0.0288(12) 0.0327(13) 0.0424(14) 0.0106(11) 0.0148(11) 0.0086(10) C13 0.0282(12) 0.0417(15) 0.0379(15) 0.0159(12) -0.0015(11) -0.0028(11) C17 0.0438(15) 0.0224(12) 0.0585(18) -0.0068(12) 0.0171(13) -0.0033(11) C22 0.0387(15) 0.0520(17) 0.0382(15) -0.0022(13) -0.0083(12) -0.0078(13) C21 0.0617(18) 0.0414(15) 0.0305(14) -0.0048(12) 0.0149(13) 0.0109(13) C6 0.0311(14) 0.0605(19) 0.0458(16) -0.0063(14) 0.0005(12) 0.0139(13) F6 0.0908(15) 0.0800(14) 0.1077(18) -0.0231(13) 0.0618(13) -0.0440(12) C12 0.0258(12) 0.0243(12) 0.069(2) 0.0117(13) 0.0067(13) 0.0042(10) C18 0.0372(14) 0.0353(14) 0.0557(17) 0.0023(12) 0.0242(13) 0.0116(11) C5 0.0457(16) 0.0482(16) 0.0367(15) -0.0053(12) 0.0091(13) -0.0056(13) C16 0.0421(15) 0.0356(14) 0.070(2) 0.0000(13) 0.0333(14) -0.0073(12) C23 0.0525(16) 0.0392(14) 0.0326(14) 0.0091(11) 0.0097(12) 0.0120(13) C11 0.0383(15) 0.0338(14) 0.0595(19) -0.0150(13) 0.0092(13) 0.0091(11) C15 0.0364(15) 0.0410(16) 0.0609(19) -0.0089(14) -0.0059(14) -0.0088(12) C10 0.0312(13) 0.0429(15) 0.0329(14) -0.0092(11) 0.0009(11) 0.0060(11) C7 0.0526(17) 0.0469(16) 0.0412(16) 0.0042(13) 0.0259(13) -0.0045(13) P4 0.0382(4) 0.0420(4) 0.0363(4) 0.0089(3) 0.0173(3) 0.0139(3) F2 0.0649(12) 0.0437(9) 0.0672(12) 0.0088(8) 0.0071(9) 0.0169(8) F1 0.0680(12) 0.0832(13) 0.0361(9) 0.0045(9) 0.0114(8) 0.0226(10) F3 0.0975(15) 0.0652(12) 0.0379(10) 0.0058(8) 0.0161(10) 0.0327(10) F4 0.191(3) 0.0823(14) 0.0522(12) 0.0125(11) 0.0337(15) 0.0974(16) F5 0.0362(11) 0.172(2) 0.0902(17) 0.0132(16) 0.0222(11) -0.0050(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 C1 1.836(2) . ? Co1 C2 1.862(2) . ? Co1 P3 2.1468(7) . ? Co1 P1 2.1687(6) . ? Co1 P2 2.2196(6) . ? P2 C20 1.824(2) . ? P2 C19 1.824(2) . ? P2 C18 1.825(2) . ? S1 C1 1.703(2) . ? S1 C8 1.829(2) . ? P3 C22 1.810(3) . ? P3 C23 1.814(2) . ? P3 C21 1.820(3) . ? P1 C16 1.812(3) . ? P1 C17 1.817(2) . ? P1 C15 1.825(3) . ? Si1 C6 1.859(3) . ? Si1 C7 1.861(3) . ? Si1 C5 1.862(3) . ? Si1 C4 1.882(2) . ? S2 C2 1.702(2) . ? S2 C3 1.825(2) . ? C2 C1 1.320(3) . ? C9 C10 1.384(3) . ? C9 C14 1.385(3) . ? C9 C8 1.501(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C4 C3 1.526(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C14 C13 1.389(3) . ? C14 H14 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C13 C12 1.373(4) . ? C13 H13 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? F6 P4 1.5813(19) . ? C12 C11 1.381(4) . ? C12 H12 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C11 C10 1.382(3) . ? C11 H11 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C10 H10 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? P4 F4 1.5638(18) . ? P4 F5 1.591(2) . ? P4 F2 1.5917(17) . ? P4 F3 1.5949(18) . ? P4 F1 1.5961(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Co1 C2 41.84(9) . . ? C1 Co1 P3 97.80(7) . . ? C2 Co1 P3 115.84(7) . . ? C1 Co1 P1 110.61(7) . . ? C2 Co1 P1 138.91(7) . . ? P3 Co1 P1 94.34(3) . . ? C1 Co1 P2 139.52(7) . . ? C2 Co1 P2 97.78(7) . . ? P3 Co1 P2 105.63(2) . . ? P1 Co1 P2 100.15(2) . . ? C20 P2 C19 101.54(12) . . ? C20 P2 C18 101.24(12) . . ? C19 P2 C18 101.21(12) . . ? C20 P2 Co1 113.72(8) . . ? C19 P2 Co1 112.59(8) . . ? C18 P2 Co1 123.62(9) . . ? C1 S1 C8 106.91(10) . . ? C22 P3 C23 101.94(13) . . ? C22 P3 C21 103.05(14) . . ? C23 P3 C21 103.32(13) . . ? C22 P3 Co1 106.46(9) . . ? C23 P3 Co1 119.80(9) . . ? C21 P3 Co1 119.70(9) . . ? C16 P1 C17 103.67(13) . . ? C16 P1 C15 102.22(15) . . ? C17 P1 C15 101.39(13) . . ? C16 P1 Co1 121.42(9) . . ? C17 P1 Co1 113.99(9) . . ? C15 P1 Co1 111.73(10) . . ? C6 Si1 C7 110.71(14) . . ? C6 Si1 C5 110.96(13) . . ? C7 Si1 C5 110.55(13) . . ? C6 Si1 C4 108.65(12) . . ? C7 Si1 C4 108.55(11) . . ? C5 Si1 C4 107.31(12) . . ? C2 S2 C3 107.94(10) . . ? C1 C2 S2 148.13(18) . . ? C1 C2 Co1 68.05(13) . . ? S2 C2 Co1 143.80(13) . . ? C2 C1 S1 148.93(18) . . ? C2 C1 Co1 70.11(13) . . ? S1 C1 Co1 140.40(13) . . ? C10 C9 C14 118.8(2) . . ? C10 C9 C8 120.9(2) . . ? C14 C9 C8 120.3(2) . . ? P2 C20 H20A 109.5 . . ? P2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? P2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C3 C4 Si1 114.16(15) . . ? C3 C4 H4A 108.7 . . ? Si1 C4 H4A 108.7 . . ? C3 C4 H4B 108.7 . . ? Si1 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C4 C3 S2 108.42(15) . . ? C4 C3 H3A 110.0 . . ? S2 C3 H3A 110.0 . . ? C4 C3 H3B 110.0 . . ? S2 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? C9 C14 C13 120.2(2) . . ? C9 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? P2 C19 H19A 109.5 . . ? P2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? P2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C9 C8 S1 108.28(16) . . ? C9 C8 H8A 110.0 . . ? S1 C8 H8A 110.0 . . ? C9 C8 H8B 110.0 . . ? S1 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? C12 C13 C14 120.4(2) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? P1 C17 H17A 109.5 . . ? P1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P3 C22 H22A 109.5 . . ? P3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P3 C21 H21A 109.5 . . ? P3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C13 C12 C11 119.7(2) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? P2 C18 H18A 109.5 . . ? P2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P1 C16 H16A 109.5 . . ? P1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P3 C23 H23A 109.5 . . ? P3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C12 C11 C10 120.0(2) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? P1 C15 H15A 109.5 . . ? P1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C10 C9 120.8(2) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? F4 P4 F6 92.59(14) . . ? F4 P4 F5 91.03(15) . . ? F6 P4 F5 176.37(13) . . ? F4 P4 F2 178.94(14) . . ? F6 P4 F2 88.47(11) . . ? F5 P4 F2 87.91(12) . . ? F4 P4 F3 90.44(10) . . ? F6 P4 F3 90.41(12) . . ? F5 P4 F3 89.87(12) . . ? F2 P4 F3 89.47(9) . . ? F4 P4 F1 90.03(10) . . ? F6 P4 F1 89.63(12) . . ? F5 P4 F1 90.06(12) . . ? F2 P4 F1 90.05(10) . . ? F3 P4 F1 179.52(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Co1 P2 C20 -62.85(14) . . . . ? C2 Co1 P2 C20 -59.50(12) . . . . ? P3 Co1 P2 C20 60.17(10) . . . . ? P1 Co1 P2 C20 157.63(10) . . . . ? C1 Co1 P2 C19 51.96(14) . . . . ? C2 Co1 P2 C19 55.31(11) . . . . ? P3 Co1 P2 C19 174.98(9) . . . . ? P1 Co1 P2 C19 -87.56(9) . . . . ? C1 Co1 P2 C18 173.93(15) . . . . ? C2 Co1 P2 C18 177.28(13) . . . . ? P3 Co1 P2 C18 -63.05(12) . . . . ? P1 Co1 P2 C18 34.41(12) . . . . ? C1 Co1 P3 C22 52.01(12) . . . . ? C2 Co1 P3 C22 12.29(13) . . . . ? P1 Co1 P3 C22 163.51(10) . . . . ? P2 Co1 P3 C22 -94.67(10) . . . . ? C1 Co1 P3 C23 -62.69(13) . . . . ? C2 Co1 P3 C23 -102.41(13) . . . . ? P1 Co1 P3 C23 48.82(11) . . . . ? P2 Co1 P3 C23 150.63(11) . . . . ? C1 Co1 P3 C21 168.09(13) . . . . ? C2 Co1 P3 C21 128.37(13) . . . . ? P1 Co1 P3 C21 -80.40(11) . . . . ? P2 Co1 P3 C21 21.41(11) . . . . ? C1 Co1 P1 C16 139.61(14) . . . . ? C2 Co1 P1 C16 178.36(15) . . . . ? P3 Co1 P1 C16 39.59(12) . . . . ? P2 Co1 P1 C16 -67.15(12) . . . . ? C1 Co1 P1 C17 14.51(13) . . . . ? C2 Co1 P1 C17 53.26(15) . . . . ? P3 Co1 P1 C17 -85.50(11) . . . . ? P2 Co1 P1 C17 167.75(11) . . . . ? C1 Co1 P1 C15 -99.70(13) . . . . ? C2 Co1 P1 C15 -60.95(15) . . . . ? P3 Co1 P1 C15 160.28(11) . . . . ? P2 Co1 P1 C15 53.54(11) . . . . ? C3 S2 C2 C1 6.7(4) . . . . ? C3 S2 C2 Co1 -176.2(2) . . . . ? P3 Co1 C2 C1 71.65(13) . . . . ? P1 Co1 C2 C1 -61.44(16) . . . . ? P2 Co1 C2 C1 -176.74(12) . . . . ? C1 Co1 C2 S2 -178.3(3) . . . . ? P3 Co1 C2 S2 -106.7(2) . . . . ? P1 Co1 C2 S2 120.22(19) . . . . ? P2 Co1 C2 S2 4.9(2) . . . . ? S2 C2 C1 S1 7.2(6) . . . . ? Co1 C2 C1 S1 -170.9(4) . . . . ? S2 C2 C1 Co1 178.1(3) . . . . ? C8 S1 C1 C2 6.5(4) . . . . ? C8 S1 C1 Co1 -160.05(19) . . . . ? P3 Co1 C1 C2 -120.43(12) . . . . ? P1 Co1 C1 C2 141.92(12) . . . . ? P2 Co1 C1 C2 4.98(18) . . . . ? C2 Co1 C1 S1 172.7(3) . . . . ? P3 Co1 C1 S1 52.2(2) . . . . ? P1 Co1 C1 S1 -45.4(2) . . . . ? P2 Co1 C1 S1 177.64(12) . . . . ? C6 Si1 C4 C3 -56.7(2) . . . . ? C7 Si1 C4 C3 -177.13(18) . . . . ? C5 Si1 C4 C3 63.4(2) . . . . ? Si1 C4 C3 S2 -168.99(12) . . . . ? C2 S2 C3 C4 175.19(16) . . . . ? C10 C9 C14 C13 0.8(3) . . . . ? C8 C9 C14 C13 -179.2(2) . . . . ? C10 C9 C8 S1 101.9(2) . . . . ? C14 C9 C8 S1 -78.1(2) . . . . ? C1 S1 C8 C9 173.83(16) . . . . ? C9 C14 C13 C12 -0.1(4) . . . . ? C14 C13 C12 C11 -0.2(4) . . . . ? C13 C12 C11 C10 -0.1(4) . . . . ? C12 C11 C10 C9 0.8(4) . . . . ? C14 C9 C10 C11 -1.2(4) . . . . ? C8 C9 C10 C11 178.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.582 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.065 # Attachment 'comp_3-PF6.cif' data_sad2 _database_code_depnum_ccdc_archive 'CCDC 740233' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H67 Co F6 O2 P4 S2 Si' _chemical_formula_weight 1173.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.5606(14) _cell_length_b 15.0042(15) _cell_length_c 15.4084(15) _cell_angle_alpha 65.400(2) _cell_angle_beta 78.203(2) _cell_angle_gamma 67.958(2) _cell_volume 2832.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transparent plate' _exptl_crystal_colour grren/red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.572 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8472 _exptl_absorpt_correction_T_max 0.9831 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.852770 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20087 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 23.50 _reflns_number_total 8393 _reflns_number_gt 6310 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution ; SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_structure_refinement ; SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The data was collected up to theta_max 30 grad, however, the intensity was too low over 23.5 grad to be considered in the final refinement. ; _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^)+(0.0602P)^2^+9.4171P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8393 _refine_ls_number_parameters 666 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.1686 _refine_ls_wR_factor_gt 0.1551 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.24526(5) 0.26385(5) 0.32274(5) 0.0188(2) Uani 1 1 d . . . C1 C 0.2669(4) 0.1589(4) 0.4417(4) 0.0237(13) Uani 1 1 d . . . C2 C 0.1711(4) 0.1951(4) 0.4219(4) 0.0216(12) Uani 1 1 d . . . P1 P 0.39095(10) 0.24705(11) 0.24055(10) 0.0225(3) Uani 1 1 d . . . P2 P 0.24690(10) 0.41036(11) 0.31397(10) 0.0209(3) Uani 1 1 d . . . P3 P 0.16531(10) 0.33788(11) 0.18919(10) 0.0227(3) Uani 1 1 d . . . S1 S 0.34624(11) 0.06763(13) 0.52701(11) 0.0411(4) Uani 1 1 d . . . S2 S 0.07255(10) 0.16177(11) 0.49101(10) 0.0289(4) Uani 1 1 d . . . Si1 Si 0.15187(15) -0.01456(16) 0.79952(13) 0.0486(5) Uani 1 1 d . . . C3 C 0.3001(4) 0.4537(4) 0.1133(4) 0.0239(12) Uani 1 1 d . . . C4 C 0.3794(4) 0.3478(4) 0.1198(4) 0.0273(13) Uani 1 1 d . . . H4A H 0.4446 0.3583 0.0963 0.033 Uiso 1 1 calc R . . H4B H 0.3627 0.3228 0.0768 0.033 Uiso 1 1 calc R . . C5 C 0.2985(4) 0.4835(4) 0.1979(4) 0.0250(13) Uani 1 1 d . . . H5A H 0.2596 0.5580 0.1809 0.030 Uiso 1 1 calc R . . H5B H 0.3674 0.4749 0.2062 0.030 Uiso 1 1 calc R . . C6 C 0.1975(4) 0.4528(4) 0.1036(4) 0.0247(13) Uani 1 1 d . . . H6A H 0.1946 0.4578 0.0380 0.030 Uiso 1 1 calc R . . H6B H 0.1466 0.5153 0.1115 0.030 Uiso 1 1 calc R . . C7 C 0.3265(4) 0.5370(4) 0.0219(4) 0.0289(13) Uani 1 1 d . . . H7A H 0.2725 0.6033 0.0104 0.043 Uiso 1 1 calc R . . H7B H 0.3357 0.5162 -0.0325 0.043 Uiso 1 1 calc R . . H7C H 0.3879 0.5447 0.0296 0.043 Uiso 1 1 calc R . . C8 C 0.4501(4) 0.1253(4) 0.2208(4) 0.0282(13) Uani 1 1 d . . . C9 C 0.4621(4) 0.0320(4) 0.2991(5) 0.0374(15) Uani 1 1 d . . . H9 H 0.4396 0.0326 0.3613 0.045 Uiso 1 1 calc R . . C10 C 0.5063(5) -0.0608(5) 0.2865(5) 0.0473(18) Uani 1 1 d . . . H10 H 0.5161 -0.1238 0.3407 0.057 Uiso 1 1 calc R . . C11 C 0.5368(5) -0.0640(5) 0.1969(6) 0.0511(19) Uani 1 1 d . . . H11 H 0.5649 -0.1284 0.1887 0.061 Uiso 1 1 calc R . . C12 C 0.5256(6) 0.0284(5) 0.1189(5) 0.057(2) Uani 1 1 d . . . H12 H 0.5472 0.0272 0.0568 0.069 Uiso 1 1 calc R . . C13 C 0.4836(5) 0.1220(5) 0.1304(5) 0.0479(18) Uani 1 1 d . . . H13 H 0.4773 0.1848 0.0764 0.057 Uiso 1 1 calc R . . C14 C 0.4897(4) 0.2568(4) 0.2897(4) 0.0245(13) Uani 1 1 d . . . C15 C 0.5014(4) 0.2103(5) 0.3870(4) 0.0367(15) Uani 1 1 d . . . H15 H 0.4585 0.1728 0.4268 0.044 Uiso 1 1 calc R . . C16 C 0.5732(5) 0.2167(5) 0.4279(5) 0.0467(18) Uani 1 1 d . . . H16 H 0.5798 0.1828 0.4950 0.056 Uiso 1 1 calc R . . C17 C 0.6352(5) 0.2717(5) 0.3726(5) 0.0474(18) Uani 1 1 d . . . H17 H 0.6843 0.2769 0.4007 0.057 Uiso 1 1 calc R . . C18 C 0.6250(5) 0.3187(6) 0.2764(5) 0.053(2) Uani 1 1 d . . . H18 H 0.6674 0.3571 0.2373 0.064 Uiso 1 1 calc R . . C19 C 0.5534(5) 0.3112(5) 0.2350(5) 0.0446(17) Uani 1 1 d . . . H19 H 0.5481 0.3440 0.1677 0.054 Uiso 1 1 calc R . . C20 C 0.3150(4) 0.4040(4) 0.4049(4) 0.0268(13) Uani 1 1 d . . . C21 C 0.2970(4) 0.3437(4) 0.4992(4) 0.0289(13) Uani 1 1 d . . . H21 H 0.2553 0.3030 0.5132 0.035 Uiso 1 1 calc R . . C22 C 0.3383(5) 0.3419(5) 0.5727(4) 0.0408(16) Uani 1 1 d . . . H22 H 0.3243 0.3015 0.6371 0.049 Uiso 1 1 calc R . . C23 C 0.3998(6) 0.3990(6) 0.5520(5) 0.067(2) Uani 1 1 d . . . H23 H 0.4298 0.3973 0.6021 0.080 Uiso 1 1 calc R . . C24 C 0.4183(8) 0.4591(8) 0.4586(5) 0.090(4) Uani 1 1 d . . . H24 H 0.4606 0.4991 0.4449 0.108 Uiso 1 1 calc R . . C25 C 0.3764(6) 0.4617(6) 0.3849(5) 0.058(2) Uani 1 1 d . . . H25 H 0.3898 0.5031 0.3207 0.069 Uiso 1 1 calc R . . C26 C 0.1258(4) 0.5005(4) 0.3347(4) 0.0238(12) Uani 1 1 d . . . C27 C 0.0465(4) 0.4667(4) 0.3771(4) 0.0276(13) Uani 1 1 d . . . H27 H 0.0534 0.3959 0.3948 0.033 Uiso 1 1 calc R . . C28 C -0.0430(4) 0.5343(5) 0.3941(4) 0.0378(15) Uani 1 1 d . . . H28 H -0.0980 0.5103 0.4222 0.045 Uiso 1 1 calc R . . C29 C -0.0534(5) 0.6359(5) 0.3710(5) 0.0461(18) Uani 1 1 d . . . H29 H -0.1161 0.6834 0.3801 0.055 Uiso 1 1 calc R . . C30 C 0.0283(6) 0.6687(5) 0.3342(5) 0.057(2) Uani 1 1 d . . . H30 H 0.0225 0.7380 0.3221 0.069 Uiso 1 1 calc R . . C31 C 0.1175(5) 0.6030(5) 0.3149(5) 0.0431(17) Uani 1 1 d . . . H31 H 0.1729 0.6267 0.2884 0.052 Uiso 1 1 calc R . . C32 C 0.0300(4) 0.3852(4) 0.1833(4) 0.0254(13) Uani 1 1 d . . . C33 C -0.0269(4) 0.4804(4) 0.1919(4) 0.0309(14) Uani 1 1 d . . . H33 H 0.0051 0.5228 0.1967 0.037 Uiso 1 1 calc R . . C34 C -0.1294(5) 0.5129(5) 0.1934(4) 0.0398(16) Uani 1 1 d . . . H34 H -0.1672 0.5770 0.2003 0.048 Uiso 1 1 calc R . . C35 C -0.1773(5) 0.4538(6) 0.1851(5) 0.0498(19) Uani 1 1 d . . . H35 H -0.2477 0.4764 0.1868 0.060 Uiso 1 1 calc R . . C36 C -0.1228(5) 0.3625(6) 0.1745(5) 0.0458(18) Uani 1 1 d . . . H36 H -0.1556 0.3225 0.1667 0.055 Uiso 1 1 calc R . . C37 C -0.0202(4) 0.3271(5) 0.1749(4) 0.0328(14) Uani 1 1 d . . . H37 H 0.0163 0.2621 0.1694 0.039 Uiso 1 1 calc R . . C38 C 0.2033(4) 0.2436(4) 0.1307(4) 0.0294(14) Uani 1 1 d . . . C39 C 0.2158(5) 0.2702(5) 0.0334(4) 0.0421(17) Uani 1 1 d . . . H39 H 0.2034 0.3410 -0.0073 0.051 Uiso 1 1 calc R . . C40 C 0.2460(6) 0.1962(6) -0.0059(5) 0.055(2) Uani 1 1 d . . . H40 H 0.2558 0.2159 -0.0733 0.066 Uiso 1 1 calc R . . C41 C 0.2622(6) 0.0931(6) 0.0521(5) 0.055(2) Uani 1 1 d . . . H41 H 0.2824 0.0416 0.0252 0.067 Uiso 1 1 calc R . . C42 C 0.2487(6) 0.0666(6) 0.1490(5) 0.059(2) Uani 1 1 d . . . H42 H 0.2591 -0.0040 0.1896 0.070 Uiso 1 1 calc R . . C43 C 0.2203(5) 0.1405(5) 0.1881(5) 0.0413(16) Uani 1 1 d . . . H43 H 0.2122 0.1204 0.2556 0.050 Uiso 1 1 calc R . . C44 C 0.2726(4) 0.0027(4) 0.6273(4) 0.0344(15) Uani 1 1 d . . . H44A H 0.2235 -0.0097 0.6015 0.041 Uiso 1 1 calc R . . H44B H 0.3172 -0.0658 0.6659 0.041 Uiso 1 1 calc R . . C45 C 0.2181(5) 0.0605(5) 0.6922(4) 0.0391(16) Uani 1 1 d . . . H45A H 0.1690 0.1264 0.6553 0.047 Uiso 1 1 calc R . . H45B H 0.2660 0.0778 0.7144 0.047 Uiso 1 1 calc R . . C46 C 0.0963(7) 0.0623(7) 0.8767(6) 0.087(3) Uani 1 1 d . . . H46A H 0.0571 0.0270 0.9304 0.130 Uiso 1 1 calc R . . H46B H 0.0533 0.1313 0.8393 0.130 Uiso 1 1 calc R . . H46C H 0.1492 0.0692 0.9013 0.130 Uiso 1 1 calc R . . C47 C 0.2429(7) -0.1388(6) 0.8669(6) 0.083(3) Uani 1 1 d . . . H47A H 0.2118 -0.1729 0.9284 0.124 Uiso 1 1 calc R . . H47B H 0.2998 -0.1258 0.8779 0.124 Uiso 1 1 calc R . . H47C H 0.2655 -0.1837 0.8300 0.124 Uiso 1 1 calc R . . C48 C 0.0541(7) -0.0373(8) 0.7575(6) 0.083(3) Uani 1 1 d . . . H48A H 0.0856 -0.0843 0.7230 0.125 Uiso 1 1 calc R . . H48B H 0.0119 0.0288 0.7148 0.125 Uiso 1 1 calc R . . H48C H 0.0136 -0.0684 0.8127 0.125 Uiso 1 1 calc R . . C49 C -0.0331(4) 0.2276(5) 0.4167(4) 0.0334(15) Uani 1 1 d . . . H49A H -0.0432 0.3029 0.3856 0.040 Uiso 1 1 calc R . . H49B H -0.0230 0.1993 0.3665 0.040 Uiso 1 1 calc R . . C50 C -0.1207(4) 0.2082(5) 0.4831(4) 0.0280(13) Uani 1 1 d . . . C51 C -0.1816(5) 0.2792(6) 0.5231(5) 0.0512(19) Uani 1 1 d . . . H51 H -0.1697 0.3426 0.5063 0.061 Uiso 1 1 calc R . . C52 C -0.2600(5) 0.2587(7) 0.5877(6) 0.063(2) Uani 1 1 d . . . H52 H -0.3011 0.3078 0.6149 0.076 Uiso 1 1 calc R . . C53 C -0.2778(5) 0.1679(7) 0.6120(5) 0.052(2) Uani 1 1 d . . . H53 H -0.3319 0.1545 0.6556 0.063 Uiso 1 1 calc R . . C54 C -0.2189(5) 0.0967(6) 0.5743(5) 0.0465(19) Uani 1 1 d . . . H54 H -0.2315 0.0334 0.5923 0.056 Uiso 1 1 calc R . . C55 C -0.1395(4) 0.1158(5) 0.5089(4) 0.0362(15) Uani 1 1 d . . . H55 H -0.0988 0.0659 0.4823 0.043 Uiso 1 1 calc R . . P4 P 0.4880(2) 0.32771(17) 0.83180(15) 0.0677(7) Uani 1 1 d . . . F1 F 0.4026(4) 0.3530(5) 0.9088(4) 0.113(2) Uani 1 1 d . . . F2 F 0.4465(5) 0.4443(4) 0.7610(4) 0.114(2) Uani 1 1 d . . . F3 F 0.4040(5) 0.3072(5) 0.7922(4) 0.111(2) Uani 1 1 d . . . F4 F 0.5571(5) 0.3034(5) 0.7503(4) 0.138(3) Uani 1 1 d . . . F5 F 0.5267(6) 0.2118(4) 0.8974(3) 0.117(2) Uani 1 1 d . . . F6 F 0.5571(7) 0.3531(7) 0.8704(8) 0.198(4) Uani 1 1 d . . . C61 C 0.7993(9) 0.1547(8) 0.8563(8) 0.103(4) Uani 1 1 d . . . H61A H 0.8709 0.1184 0.8606 0.155 Uiso 1 1 calc R . . H61B H 0.7808 0.1746 0.7915 0.155 Uiso 1 1 calc R . . H61C H 0.7635 0.1088 0.9023 0.155 Uiso 1 1 calc R . . O61 O 0.7750(6) 0.2425(5) 0.8767(5) 0.093(2) Uani 1 1 d . . . H61 H 0.7185 0.2825 0.8574 0.139 Uiso 1 1 calc R . . C62 C 0.9831(11) 0.2595(11) 0.9728(10) 0.155(6) Uani 1 1 d . . . H62A H 0.9983 0.3095 0.9881 0.232 Uiso 1 1 calc R . . H62B H 1.0423 0.2224 0.9426 0.232 Uiso 1 1 calc R . . H62C H 0.9627 0.2098 1.0317 0.232 Uiso 1 1 calc R . . O62 O 0.9135(10) 0.3070(7) 0.9160(12) 0.225(7) Uani 1 1 d . . . H62 H 0.8924 0.2640 0.9119 0.337 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 0.0159(4) 0.0190(4) 0.0184(4) -0.0023(3) -0.0011(3) -0.0074(3) C1 0.019(3) 0.026(3) 0.021(3) -0.004(2) 0.002(2) -0.008(2) C2 0.022(3) 0.020(3) 0.023(3) -0.006(2) 0.002(2) -0.011(2) P1 0.0197(8) 0.0222(8) 0.0211(8) -0.0038(6) 0.0015(6) -0.0081(6) P2 0.0190(7) 0.0218(7) 0.0202(7) -0.0044(6) -0.0010(6) -0.0090(6) P3 0.0218(8) 0.0252(8) 0.0195(7) -0.0022(6) -0.0032(6) -0.0118(6) S1 0.0224(8) 0.0451(10) 0.0298(9) 0.0105(7) -0.0050(7) -0.0092(7) S2 0.0211(8) 0.0342(8) 0.0246(8) -0.0006(6) -0.0004(6) -0.0141(7) Si1 0.0481(12) 0.0501(12) 0.0308(10) -0.0031(9) 0.0067(9) -0.0163(10) C3 0.021(3) 0.025(3) 0.020(3) 0.000(2) -0.003(2) -0.008(2) C4 0.026(3) 0.029(3) 0.023(3) -0.004(3) 0.003(2) -0.012(3) C5 0.023(3) 0.023(3) 0.025(3) -0.003(2) -0.002(2) -0.010(2) C6 0.026(3) 0.025(3) 0.019(3) -0.001(2) -0.006(2) -0.010(3) C7 0.031(3) 0.028(3) 0.026(3) -0.003(3) -0.002(3) -0.016(3) C8 0.023(3) 0.023(3) 0.033(3) -0.009(3) -0.004(3) -0.003(3) C9 0.036(4) 0.028(3) 0.038(4) -0.008(3) 0.002(3) -0.007(3) C10 0.053(4) 0.018(3) 0.058(5) -0.005(3) -0.005(4) -0.006(3) C11 0.050(4) 0.035(4) 0.068(5) -0.029(4) -0.004(4) -0.003(3) C12 0.078(6) 0.042(4) 0.041(4) -0.022(4) 0.003(4) -0.003(4) C13 0.063(5) 0.034(4) 0.036(4) -0.014(3) 0.008(3) -0.011(3) C14 0.016(3) 0.015(3) 0.032(3) -0.003(2) -0.001(2) -0.002(2) C15 0.027(3) 0.039(4) 0.040(4) -0.002(3) -0.003(3) -0.019(3) C16 0.037(4) 0.057(4) 0.044(4) -0.002(3) -0.017(3) -0.025(4) C17 0.037(4) 0.046(4) 0.058(5) -0.004(4) -0.021(4) -0.019(3) C18 0.030(4) 0.060(5) 0.063(5) 0.000(4) -0.009(3) -0.030(4) C19 0.036(4) 0.049(4) 0.037(4) 0.005(3) -0.009(3) -0.021(3) C20 0.029(3) 0.024(3) 0.025(3) -0.005(3) -0.005(3) -0.010(3) C21 0.026(3) 0.027(3) 0.029(3) -0.007(3) -0.002(3) -0.008(3) C22 0.044(4) 0.049(4) 0.024(3) -0.006(3) -0.005(3) -0.017(3) C23 0.099(7) 0.088(6) 0.033(4) -0.003(4) -0.027(4) -0.060(5) C24 0.136(9) 0.125(8) 0.043(5) 0.007(5) -0.030(5) -0.108(7) C25 0.087(6) 0.076(5) 0.029(4) 0.001(4) -0.016(4) -0.064(5) C26 0.024(3) 0.023(3) 0.022(3) -0.008(2) -0.002(2) -0.005(2) C27 0.029(3) 0.024(3) 0.028(3) -0.009(3) -0.001(3) -0.008(3) C28 0.026(3) 0.042(4) 0.044(4) -0.020(3) 0.009(3) -0.011(3) C29 0.038(4) 0.033(4) 0.048(4) -0.012(3) 0.011(3) -0.002(3) C30 0.063(5) 0.025(4) 0.068(5) -0.017(4) 0.026(4) -0.013(4) C31 0.043(4) 0.029(4) 0.054(4) -0.016(3) 0.014(3) -0.016(3) C32 0.025(3) 0.032(3) 0.012(3) 0.003(2) -0.006(2) -0.012(3) C33 0.027(3) 0.034(3) 0.027(3) -0.002(3) -0.006(3) -0.013(3) C34 0.030(4) 0.044(4) 0.035(4) -0.006(3) -0.006(3) -0.009(3) C35 0.021(3) 0.072(5) 0.043(4) -0.006(4) -0.004(3) -0.019(4) C36 0.035(4) 0.058(5) 0.050(4) -0.011(4) -0.010(3) -0.028(4) C37 0.032(4) 0.039(4) 0.029(3) -0.006(3) -0.005(3) -0.020(3) C38 0.031(3) 0.032(3) 0.028(3) -0.010(3) -0.006(3) -0.013(3) C39 0.060(5) 0.038(4) 0.031(4) -0.012(3) 0.003(3) -0.022(3) C40 0.083(6) 0.063(5) 0.033(4) -0.022(4) 0.011(4) -0.040(5) C41 0.071(5) 0.051(5) 0.060(5) -0.037(4) 0.004(4) -0.023(4) C42 0.091(6) 0.039(4) 0.051(5) -0.016(4) -0.019(4) -0.020(4) C43 0.063(5) 0.035(4) 0.032(4) -0.010(3) -0.008(3) -0.023(3) C44 0.032(3) 0.029(3) 0.023(3) 0.007(3) 0.001(3) -0.009(3) C45 0.044(4) 0.037(4) 0.030(3) -0.003(3) -0.005(3) -0.015(3) C46 0.100(8) 0.092(7) 0.043(5) -0.024(5) 0.004(5) -0.009(6) C47 0.090(7) 0.054(5) 0.048(5) 0.010(4) 0.002(5) 0.001(5) C48 0.087(7) 0.103(7) 0.063(6) -0.015(5) 0.017(5) -0.065(6) C49 0.027(3) 0.044(4) 0.023(3) 0.000(3) -0.006(3) -0.018(3) C50 0.022(3) 0.040(4) 0.026(3) -0.009(3) -0.003(3) -0.017(3) C51 0.044(4) 0.062(5) 0.066(5) -0.032(4) 0.004(4) -0.032(4) C52 0.039(4) 0.103(7) 0.071(6) -0.061(5) 0.014(4) -0.024(5) C53 0.034(4) 0.087(6) 0.037(4) -0.013(4) 0.006(3) -0.036(4) C54 0.035(4) 0.053(4) 0.043(4) 0.008(4) -0.011(3) -0.029(4) C55 0.029(3) 0.032(3) 0.038(4) -0.002(3) -0.008(3) -0.010(3) P4 0.110(2) 0.0644(14) 0.0467(12) -0.0321(11) 0.0349(13) -0.0554(14) F1 0.106(4) 0.172(6) 0.061(3) -0.046(4) 0.025(3) -0.057(4) F2 0.121(5) 0.066(3) 0.133(5) -0.024(3) 0.044(4) -0.049(3) F3 0.144(6) 0.103(4) 0.107(4) -0.041(4) -0.033(4) -0.047(4) F4 0.140(6) 0.116(5) 0.063(3) -0.022(3) 0.040(4) 0.021(4) F5 0.217(7) 0.080(4) 0.055(3) 0.006(3) -0.027(4) -0.074(4) F6 0.182(8) 0.219(9) 0.292(11) -0.123(9) -0.073(8) -0.108(7) C61 0.146(10) 0.071(7) 0.100(8) -0.027(6) -0.035(7) -0.033(7) O61 0.131(6) 0.093(5) 0.084(5) -0.033(4) 0.008(5) -0.075(5) C62 0.176(15) 0.134(12) 0.140(12) -0.039(10) -0.087(11) -0.009(11) O62 0.213(12) 0.091(6) 0.388(18) -0.076(9) -0.204(13) 0.011(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C1 1.844(5) . ? Co1 C2 1.848(5) . ? Co1 P2 2.1546(16) . ? Co1 P3 2.2202(15) . ? Co1 P1 2.2211(16) . ? C1 C2 1.342(7) . ? C1 S1 1.695(5) . ? C2 S2 1.706(5) . ? P1 C8 1.830(6) . ? P1 C14 1.833(6) . ? P1 C4 1.836(5) . ? P2 C20 1.828(6) . ? P2 C26 1.839(5) . ? P2 C5 1.844(5) . ? P3 C32 1.834(5) . ? P3 C38 1.841(6) . ? P3 C6 1.842(5) . ? S1 C44 1.828(5) . ? S2 C49 1.815(6) . ? Si1 C47 1.846(8) . ? Si1 C46 1.857(8) . ? Si1 C48 1.868(9) . ? Si1 C45 1.882(6) . ? C3 C6 1.537(7) . ? C3 C5 1.538(7) . ? C3 C7 1.538(7) . ? C3 C4 1.552(8) . ? C8 C9 1.393(8) . ? C8 C13 1.393(8) . ? C9 C10 1.375(8) . ? C10 C11 1.377(10) . ? C11 C12 1.383(10) . ? C12 C13 1.378(9) . ? C14 C15 1.381(8) . ? C14 C19 1.382(8) . ? C15 C16 1.378(8) . ? C16 C17 1.372(9) . ? C17 C18 1.362(9) . ? C18 C19 1.388(9) . ? C20 C25 1.375(8) . ? C20 C21 1.388(8) . ? C21 C22 1.373(8) . ? C22 C23 1.367(9) . ? C23 C24 1.379(10) . ? C24 C25 1.375(9) . ? C26 C27 1.369(8) . ? C26 C31 1.399(8) . ? C27 C28 1.373(8) . ? C28 C29 1.368(9) . ? C29 C30 1.382(9) . ? C30 C31 1.368(9) . ? C32 C37 1.385(8) . ? C32 C33 1.404(8) . ? C33 C34 1.384(8) . ? C34 C35 1.371(9) . ? C35 C36 1.360(10) . ? C36 C37 1.386(9) . ? C38 C39 1.372(8) . ? C38 C43 1.379(8) . ? C39 C40 1.371(9) . ? C40 C41 1.381(10) . ? C41 C42 1.367(10) . ? C42 C43 1.369(9) . ? C44 C45 1.504(8) . ? C49 C50 1.502(8) . ? C50 C51 1.384(9) . ? C50 C55 1.392(8) . ? C51 C52 1.390(10) . ? C52 C53 1.365(11) . ? C53 C54 1.357(10) . ? C54 C55 1.401(9) . ? P4 F6 1.493(7) . ? P4 F4 1.521(5) . ? P4 F5 1.549(6) . ? P4 F2 1.582(6) . ? P4 F1 1.587(6) . ? P4 F3 1.646(6) . ? C61 O61 1.382(10) . ? C62 O62 1.266(13) . ? 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 C1 Co1 C2 42.6(2) . . ? C1 Co1 P2 115.18(18) . . ? C2 Co1 P2 118.61(17) . . ? C1 Co1 P3 147.20(17) . . ? C2 Co1 P3 109.24(17) . . ? P2 Co1 P3 92.18(6) . . ? C1 Co1 P1 106.86(17) . . ? C2 Co1 P1 144.94(17) . . ? P2 Co1 P1 87.53(6) . . ? P3 Co1 P1 91.27(6) . . ? C2 C1 S1 141.4(4) . . ? C2 C1 Co1 68.9(3) . . ? S1 C1 Co1 149.7(3) . . ? C1 C2 S2 129.8(4) . . ? C1 C2 Co1 68.5(3) . . ? S2 C2 Co1 161.5(3) . . ? C8 P1 C14 102.9(2) . . ? C8 P1 C4 104.3(3) . . ? C14 P1 C4 104.3(3) . . ? C8 P1 Co1 115.94(19) . . ? C14 P1 Co1 116.80(19) . . ? C4 P1 Co1 111.19(18) . . ? C20 P2 C26 99.1(3) . . ? C20 P2 C5 105.8(2) . . ? C26 P2 C5 105.8(2) . . ? C20 P2 Co1 115.70(18) . . ? C26 P2 Co1 115.61(18) . . ? C5 P2 Co1 113.33(18) . . ? C32 P3 C38 101.6(3) . . ? C32 P3 C6 101.3(2) . . ? C38 P3 C6 106.9(3) . . ? C32 P3 Co1 125.04(17) . . ? C38 P3 Co1 108.01(19) . . ? C6 P3 Co1 112.34(18) . . ? C1 S1 C44 107.2(3) . . ? C2 S2 C49 107.4(3) . . ? C47 Si1 C46 109.1(4) . . ? C47 Si1 C48 110.7(5) . . ? C46 Si1 C48 111.0(5) . . ? C47 Si1 C45 108.9(4) . . ? C46 Si1 C45 108.4(4) . . ? C48 Si1 C45 108.7(3) . . ? C6 C3 C5 111.0(4) . . ? C6 C3 C7 108.1(4) . . ? C5 C3 C7 107.4(4) . . ? C6 C3 C4 109.6(4) . . ? C5 C3 C4 113.1(4) . . ? C7 C3 C4 107.4(4) . . ? C3 C4 P1 114.4(4) . . ? C3 C5 P2 116.6(4) . . ? C3 C6 P3 115.3(4) . . ? C9 C8 C13 118.6(5) . . ? C9 C8 P1 118.8(4) . . ? C13 C8 P1 122.6(4) . . ? C10 C9 C8 120.1(6) . . ? C9 C10 C11 121.2(6) . . ? C10 C11 C12 118.8(6) . . ? C13 C12 C11 120.7(7) . . ? C12 C13 C8 120.4(6) . . ? C15 C14 C19 116.7(5) . . ? C15 C14 P1 119.5(4) . . ? C19 C14 P1 123.8(5) . . ? C16 C15 C14 122.0(6) . . ? C17 C16 C15 120.5(6) . . ? C18 C17 C16 118.7(6) . . ? C17 C18 C19 120.8(6) . . ? C14 C19 C18 121.4(6) . . ? C25 C20 C21 119.2(5) . . ? C25 C20 P2 123.1(4) . . ? C21 C20 P2 117.5(4) . . ? C22 C21 C20 121.2(6) . . ? C23 C22 C21 119.1(6) . . ? C22 C23 C24 120.3(6) . . ? C25 C24 C23 120.7(7) . . ? C24 C25 C20 119.5(6) . . ? C27 C26 C31 119.6(5) . . ? C27 C26 P2 121.0(4) . . ? C31 C26 P2 119.1(4) . . ? C26 C27 C28 120.5(5) . . ? C29 C28 C27 120.4(6) . . ? C28 C29 C30 119.2(6) . . ? C31 C30 C29 121.1(6) . . ? C30 C31 C26 119.0(6) . . ? C37 C32 C33 117.6(5) . . ? C37 C32 P3 121.9(5) . . ? C33 C32 P3 120.4(4) . . ? C34 C33 C32 120.3(6) . . ? C35 C34 C33 120.9(6) . . ? C36 C35 C34 119.3(6) . . ? C35 C36 C37 121.0(6) . . ? C32 C37 C36 120.9(6) . . ? C39 C38 C43 118.3(6) . . ? C39 C38 P3 123.7(5) . . ? C43 C38 P3 118.0(5) . . ? C40 C39 C38 121.0(6) . . ? C39 C40 C41 120.3(7) . . ? C42 C41 C40 118.8(7) . . ? C41 C42 C43 120.8(7) . . ? C42 C43 C38 120.8(6) . . ? C45 C44 S1 115.3(4) . . ? C44 C45 Si1 113.5(4) . . ? C50 C49 S2 105.6(4) . . ? C51 C50 C55 118.6(6) . . ? C51 C50 C49 121.0(5) . . ? C55 C50 C49 120.3(5) . . ? C50 C51 C52 120.7(7) . . ? C53 C52 C51 120.0(7) . . ? C54 C53 C52 120.5(6) . . ? C53 C54 C55 120.4(6) . . ? C50 C55 C54 119.7(6) . . ? F6 P4 F4 97.4(5) . . ? F6 P4 F5 91.6(5) . . ? F4 P4 F5 89.6(3) . . ? F6 P4 F2 91.3(5) . . ? F4 P4 F2 88.8(3) . . ? F5 P4 F2 176.8(4) . . ? F6 P4 F1 91.5(5) . . ? F4 P4 F1 170.9(4) . . ? F5 P4 F1 92.1(4) . . ? F2 P4 F1 89.0(3) . . ? F6 P4 F3 175.0(5) . . ? F4 P4 F3 86.8(4) . . ? F5 P4 F3 91.0(3) . . ? F2 P4 F3 86.1(3) . . ? F1 P4 F3 84.2(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.584 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.085 # Attachment 'comp_4.cif' data_sad3 _database_code_depnum_ccdc_archive 'CCDC 740234' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C212 H184 Co4 O3 P12 S8' _chemical_formula_weight 3643.43 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' 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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0667(18) _cell_length_b 15.000(2) _cell_length_c 25.050(3) _cell_angle_alpha 79.982(3) _cell_angle_beta 77.636(3) _cell_angle_gamma 63.855(2) _cell_volume 4615.6(10) _cell_formula_units_Z 1 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8396 _exptl_absorpt_correction_T_max 0.9590 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.853245 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46827 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 0.84 _diffrn_reflns_theta_max 27.88 _reflns_number_total 21998 _reflns_number_gt 15255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2(Bruker AXS, 2007)' _computing_cell_refinement 'APEX2(Bruker AXS, 2007)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2007 )' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The thf molecule on the symmetry position is disordered in two directions. The respective carbon atoms have been refined isotropically without hydrogen atoms attached. ; _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^)+(0.0866P)^2^+2.2814P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21998 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1689 _refine_ls_wR_factor_gt 0.1525 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 C222 C 0.7529(7) 0.3122(7) 0.7934(4) 0.122(3) Uiso 1 1 d . . . O333 O 0.9873(9) -0.0283(8) 0.0592(4) 0.111(3) Uiso 0.50 1 d P . . C98 C 0.9586(6) 0.0571(6) 0.0364(3) 0.0927(19) Uiso 1 1 d . . . Co1A Co 0.27889(3) 0.25482(3) 0.140660(17) 0.02105(10) Uani 1 1 d . . . Co2B Co 0.28446(3) 0.29391(3) 0.629388(18) 0.02374(11) Uani 1 1 d . . . P1A P 0.31815(7) 0.14981(6) 0.21346(3) 0.02271(17) Uani 1 1 d . . . P2B P 0.23610(7) 0.44907(6) 0.60082(4) 0.02548(18) Uani 1 1 d . . . P3A P 0.26392(6) 0.14609(6) 0.09860(3) 0.02295(17) Uani 1 1 d . . . S2A S 0.08282(7) 0.43730(6) 0.07596(4) 0.0344(2) Uani 1 1 d . . . P2A P 0.44806(7) 0.20465(6) 0.11111(3) 0.02369(18) Uani 1 1 d . . . S1A S 0.18872(8) 0.47011(7) 0.20266(4) 0.0354(2) Uani 1 1 d . . . S1B S 0.50310(8) 0.19171(8) 0.69511(4) 0.0421(2) Uani 1 1 d . . . P3B P 0.16647(7) 0.28274(6) 0.58913(4) 0.02787(19) Uani 1 1 d . . . S2B S 0.48715(8) 0.11883(8) 0.55318(4) 0.0443(3) Uani 1 1 d . . . P1B P 0.17023(7) 0.33464(6) 0.70480(3) 0.02717(19) Uani 1 1 d . . . C2A C 0.1755(2) 0.3730(2) 0.11792(14) 0.0255(7) Uani 1 1 d . . . C38A C 0.1550(3) 0.1124(2) 0.13487(13) 0.0253(7) Uani 1 1 d . . . C14A C 0.4019(3) 0.1596(2) 0.25700(13) 0.0250(7) Uani 1 1 d . . . C3A C 0.4566(3) 0.0055(2) 0.13738(13) 0.0253(7) Uani 1 1 d . . . C20A C 0.5228(3) 0.2563(3) 0.13786(13) 0.0276(7) Uani 1 1 d . . . C1A C 0.2101(3) 0.3860(2) 0.16083(14) 0.0262(7) Uani 1 1 d . . . C5B C 0.0390(3) 0.3955(3) 0.59004(15) 0.0344(8) Uani 1 1 d . . . H5B1 H 0.0380 0.4328 0.5533 0.041 Uiso 1 1 calc R . . H5B2 H -0.0207 0.3748 0.5970 0.041 Uiso 1 1 calc R . . C8B C 0.1873(3) 0.4006(3) 0.75429(14) 0.0302(7) Uani 1 1 d . . . C6A C 0.5230(3) 0.0681(2) 0.12432(14) 0.0284(7) Uani 1 1 d . . . H6A1 H 0.5777 0.0436 0.0917 0.034 Uiso 1 1 calc R . . H6A2 H 0.5617 0.0554 0.1555 0.034 Uiso 1 1 calc R . . C4A C 0.3888(3) 0.0201(2) 0.19519(13) 0.0272(7) Uani 1 1 d . . . H4A1 H 0.4364 -0.0199 0.2226 0.033 Uiso 1 1 calc R . . H4A2 H 0.3350 -0.0070 0.1979 0.033 Uiso 1 1 calc R . . C26A C 0.4814(3) 0.2386(3) 0.03764(14) 0.0295(7) Uani 1 1 d . . . C43A C 0.1644(3) 0.0160(3) 0.15217(16) 0.0364(8) Uani 1 1 d . . . H43A H 0.2311 -0.0392 0.1436 0.044 Uiso 1 1 calc R . . C32B C 0.2812(3) 0.4722(3) 0.52759(14) 0.0306(7) Uani 1 1 d . . . C5A C 0.3859(3) 0.0293(2) 0.09290(14) 0.0275(7) Uani 1 1 d . . . H5A1 H 0.3650 -0.0263 0.0948 0.033 Uiso 1 1 calc R . . H5A2 H 0.4292 0.0325 0.0564 0.033 Uiso 1 1 calc R . . C32A C 0.2356(3) 0.1705(2) 0.02841(13) 0.0260(7) Uani 1 1 d . . . C3B C 0.0188(3) 0.4664(2) 0.63356(14) 0.0278(7) Uani 1 1 d . . . C8A C 0.2039(3) 0.1479(2) 0.26439(13) 0.0257(7) Uani 1 1 d . . . C14B C 0.1566(3) 0.2315(3) 0.75097(13) 0.0291(7) Uani 1 1 d . . . C33B C 0.2157(3) 0.5211(3) 0.48810(16) 0.0399(9) Uani 1 1 d . . . H33B H 0.1401 0.5474 0.4983 0.048 Uiso 1 1 calc R . . C15B C 0.2357(3) 0.1356(3) 0.74562(15) 0.0371(8) Uani 1 1 d . . . H15B H 0.2958 0.1244 0.7175 0.045 Uiso 1 1 calc R . . C1B C 0.4201(3) 0.2211(3) 0.64980(15) 0.0313(7) Uani 1 1 d . . . C38B C 0.2852(3) 0.5222(3) 0.62992(15) 0.0319(8) Uani 1 1 d . . . C7B C -0.0985(3) 0.5428(3) 0.63673(16) 0.0344(8) Uani 1 1 d . . . H7B1 H -0.1118 0.5942 0.6603 0.052 Uiso 1 1 calc R . . H7B2 H -0.1456 0.5092 0.6521 0.052 Uiso 1 1 calc R . . H7B3 H -0.1130 0.5740 0.5998 0.052 Uiso 1 1 calc R . . C39A C 0.0563(3) 0.1914(3) 0.14708(16) 0.0361(8) Uani 1 1 d . . . H39A H 0.0484 0.2577 0.1353 0.043 Uiso 1 1 calc R . . C10A C 0.0190(3) 0.2330(3) 0.30471(16) 0.0373(8) Uani 1 1 d . . . H10A H -0.0476 0.2901 0.3052 0.045 Uiso 1 1 calc R . . C9B C 0.2773(3) 0.3512(3) 0.77948(15) 0.0386(9) Uani 1 1 d . . . H9B H 0.3263 0.2856 0.7708 0.046 Uiso 1 1 calc R . . C17A C 0.5226(3) 0.1867(3) 0.32272(16) 0.0403(9) Uani 1 1 d . . . H17A H 0.5640 0.1960 0.3449 0.048 Uiso 1 1 calc R . . C12A C 0.1255(3) 0.0676(3) 0.34118(15) 0.0396(9) Uani 1 1 d . . . H12A H 0.1316 0.0114 0.3669 0.048 Uiso 1 1 calc R . . C9A C 0.1069(3) 0.2316(3) 0.26621(15) 0.0318(8) Uani 1 1 d . . . H9A H 0.1005 0.2884 0.2410 0.038 Uiso 1 1 calc R . . C7A C 0.5354(3) -0.1048(3) 0.13642(16) 0.0355(8) Uani 1 1 d . . . H7A1 H 0.5877 -0.1202 0.1608 0.053 Uiso 1 1 calc R . . H7A2 H 0.5728 -0.1181 0.0989 0.053 Uiso 1 1 calc R . . H7A3 H 0.4959 -0.1465 0.1490 0.053 Uiso 1 1 calc R . . C13A C 0.2133(3) 0.0653(3) 0.30280(14) 0.0329(8) Uani 1 1 d . . . H13A H 0.2797 0.0081 0.3024 0.039 Uiso 1 1 calc R . . C43B C 0.3549(3) 0.4771(3) 0.66753(15) 0.0368(8) Uani 1 1 d . . . H43B H 0.3813 0.4072 0.6769 0.044 Uiso 1 1 calc R . . C4B C 0.0316(3) 0.4096(3) 0.69047(14) 0.0328(8) Uani 1 1 d . . . H4B1 H -0.0047 0.3645 0.6957 0.039 Uiso 1 1 calc R . . H4B2 H -0.0066 0.4585 0.7182 0.039 Uiso 1 1 calc R . . C26B C 0.1933(3) 0.2588(3) 0.51730(15) 0.0352(8) Uani 1 1 d . . . C16A C 0.4520(3) 0.2673(3) 0.29429(15) 0.0375(8) Uani 1 1 d . . . H16A H 0.4447 0.3325 0.2969 0.045 Uiso 1 1 calc R . . C19B C 0.0681(3) 0.2475(3) 0.79220(14) 0.0378(9) Uani 1 1 d . . . H19B H 0.0133 0.3128 0.7966 0.045 Uiso 1 1 calc R . . C2B C 0.4123(3) 0.1977(3) 0.60203(14) 0.0302(7) Uani 1 1 d . . . C15A C 0.3917(3) 0.2539(3) 0.26187(15) 0.0330(8) Uani 1 1 d . . . H15A H 0.3428 0.3101 0.2428 0.040 Uiso 1 1 calc R . . C31A C 0.4182(3) 0.3349(3) 0.01740(16) 0.0396(9) Uani 1 1 d . . . H31A H 0.3588 0.3774 0.0409 0.048 Uiso 1 1 calc R . . C20B C 0.1328(3) 0.1779(3) 0.62023(15) 0.0344(8) Uani 1 1 d . . . C37A C 0.2106(3) 0.1053(3) 0.00613(15) 0.0365(8) Uani 1 1 d . . . H37A H 0.2060 0.0486 0.0282 0.044 Uiso 1 1 calc R . . C11A C 0.0287(3) 0.1512(3) 0.34238(15) 0.0388(9) Uani 1 1 d . . . H11A H -0.0310 0.1524 0.3690 0.047 Uiso 1 1 calc R . . C33A C 0.2424(3) 0.2517(3) -0.00465(14) 0.0320(8) Uani 1 1 d . . . H33A H 0.2601 0.2962 0.0096 0.038 Uiso 1 1 calc R . . C35A C 0.1997(3) 0.2047(3) -0.07975(15) 0.0422(10) Uani 1 1 d . . . H35A H 0.1878 0.2164 -0.1168 0.051 Uiso 1 1 calc R . . C42B C 0.3866(3) 0.5341(3) 0.69168(18) 0.0458(10) Uani 1 1 d . . . H42B H 0.4336 0.5034 0.7181 0.055 Uiso 1 1 calc R . . C11B C 0.2255(4) 0.4899(3) 0.83100(16) 0.0508(12) Uani 1 1 d . . . H11B H 0.2368 0.5196 0.8582 0.061 Uiso 1 1 calc R . . C42A C 0.0767(3) -0.0002(3) 0.18202(18) 0.0439(10) Uani 1 1 d . . . H42A H 0.0840 -0.0663 0.1940 0.053 Uiso 1 1 calc R . . C16B C 0.2283(4) 0.0555(3) 0.78081(17) 0.0445(10) Uani 1 1 d . . . H16B H 0.2832 -0.0099 0.7770 0.053 Uiso 1 1 calc R . . C18B C 0.0610(4) 0.1663(4) 0.82703(16) 0.0459(10) Uani 1 1 d . . . H18B H 0.0006 0.1764 0.8549 0.055 Uiso 1 1 calc R . . C6B C 0.0887(3) 0.5239(3) 0.61479(16) 0.0337(8) Uani 1 1 d . . . H6B1 H 0.0737 0.5685 0.6433 0.040 Uiso 1 1 calc R . . H6B2 H 0.0659 0.5668 0.5809 0.040 Uiso 1 1 calc R . . C13B C 0.1171(3) 0.4970(3) 0.76690(17) 0.0433(9) Uani 1 1 d . . . H13B H 0.0555 0.5328 0.7494 0.052 Uiso 1 1 calc R . . C19A C 0.4723(3) 0.0791(3) 0.28644(15) 0.0359(8) Uani 1 1 d . . . H19A H 0.4789 0.0139 0.2844 0.043 Uiso 1 1 calc R . . C34A C 0.2237(3) 0.2697(3) -0.05876(15) 0.0377(9) Uani 1 1 d . . . H34A H 0.2276 0.3265 -0.0810 0.045 Uiso 1 1 calc R . . C45A C 0.1179(3) 0.6060(3) 0.04609(16) 0.0378(9) Uani 1 1 d . . . C41A C -0.0204(3) 0.0795(3) 0.19421(17) 0.0438(10) Uani 1 1 d . . . H41A H -0.0799 0.0686 0.2149 0.053 Uiso 1 1 calc R . . C21A C 0.4755(3) 0.3579(3) 0.14395(17) 0.0407(9) Uani 1 1 d . . . H21A H 0.4061 0.3983 0.1345 0.049 Uiso 1 1 calc R . . C36A C 0.1927(3) 0.1229(3) -0.04768(16) 0.0433(10) Uani 1 1 d . . . H36A H 0.1756 0.0786 -0.0625 0.052 Uiso 1 1 calc R . . C27A C 0.5677(4) 0.1788(3) 0.00259(16) 0.0441(10) Uani 1 1 d . . . H27A H 0.6123 0.1130 0.0155 0.053 Uiso 1 1 calc R . . C10B C 0.2971(4) 0.3961(3) 0.81740(16) 0.0474(10) Uani 1 1 d . . . H10B H 0.3602 0.3618 0.8339 0.057 Uiso 1 1 calc R . . C44A C 0.0442(3) 0.5680(3) 0.08486(18) 0.0402(9) Uani 1 1 d . . . H44A H -0.0304 0.6086 0.0779 0.048 Uiso 1 1 calc R . . H44B H 0.0472 0.5741 0.1231 0.048 Uiso 1 1 calc R . . C25A C 0.6243(3) 0.1999(3) 0.15196(17) 0.0421(9) Uani 1 1 d . . . H25A H 0.6587 0.1307 0.1473 0.050 Uiso 1 1 calc R . . C17B C 0.1406(4) 0.0724(3) 0.82111(17) 0.0472(11) Uani 1 1 d . . . H17B H 0.1351 0.0179 0.8453 0.057 Uiso 1 1 calc R . . C39B C 0.2515(3) 0.6233(3) 0.61409(18) 0.0423(9) Uani 1 1 d . . . H39B H 0.2065 0.6538 0.5867 0.051 Uiso 1 1 calc R . . C18A C 0.5325(3) 0.0919(3) 0.31849(17) 0.0428(9) Uani 1 1 d . . . H18A H 0.5810 0.0357 0.3378 0.051 Uiso 1 1 calc R . . C40A C -0.0309(3) 0.1750(3) 0.17630(18) 0.0432(10) Uani 1 1 d . . . H40A H -0.0982 0.2299 0.1840 0.052 Uiso 1 1 calc R . . C25B C 0.2165(4) 0.0835(3) 0.61470(18) 0.0453(10) Uani 1 1 d . . . H25B H 0.2851 0.0774 0.5960 0.054 Uiso 1 1 calc R . . C34B C 0.2599(4) 0.5321(3) 0.43354(17) 0.0478(10) Uani 1 1 d . . . H34B H 0.2137 0.5668 0.4070 0.057 Uiso 1 1 calc R . . C41B C 0.3496(4) 0.6355(4) 0.67720(19) 0.0523(11) Uani 1 1 d . . . H41B H 0.3704 0.6744 0.6944 0.063 Uiso 1 1 calc R . . C31B C 0.2825(3) 0.2621(3) 0.48328(16) 0.0432(10) Uani 1 1 d . . . H31B H 0.3302 0.2784 0.4971 0.052 Uiso 1 1 calc R . . C28A C 0.5898(4) 0.2145(3) -0.05158(17) 0.0550(13) Uani 1 1 d . . . H28A H 0.6501 0.1731 -0.0752 0.066 Uiso 1 1 calc R . . C40B C 0.2837(3) 0.6807(3) 0.6385(2) 0.0484(11) Uani 1 1 d . . . H40B H 0.2598 0.7503 0.6283 0.058 Uiso 1 1 calc R . . C29A C 0.5254(4) 0.3089(4) -0.07137(17) 0.0526(12) Uani 1 1 d . . . H29A H 0.5393 0.3317 -0.1088 0.063 Uiso 1 1 calc R . . C27B C 0.1237(4) 0.2359(3) 0.49596(18) 0.0500(11) Uani 1 1 d . . . H27B H 0.0612 0.2336 0.5186 0.060 Uiso 1 1 calc R . . C44B C 0.6190(3) 0.0509(3) 0.57498(19) 0.0452(10) Uani 1 1 d . . . H44C H 0.6103 0.0520 0.6152 0.054 Uiso 1 1 calc R . . H44D H 0.6480 -0.0195 0.5671 0.054 Uiso 1 1 calc R . . C36B C 0.4340(4) 0.4456(4) 0.45641(19) 0.0554(12) Uani 1 1 d . . . H36B H 0.5095 0.4201 0.4458 0.066 Uiso 1 1 calc R . . C23A C 0.6288(4) 0.3430(4) 0.17826(17) 0.0524(12) Uani 1 1 d . . . H23A H 0.6648 0.3727 0.1921 0.063 Uiso 1 1 calc R . . C35B C 0.3675(4) 0.4944(4) 0.41739(17) 0.0513(11) Uani 1 1 d . . . H35B H 0.3967 0.5014 0.3798 0.062 Uiso 1 1 calc R . . C37B C 0.3911(3) 0.4336(3) 0.51109(17) 0.0450(10) Uani 1 1 d . . . H37B H 0.4377 0.3985 0.5374 0.054 Uiso 1 1 calc R . . C12B C 0.1373(4) 0.5406(3) 0.80497(19) 0.0544(12) Uani 1 1 d . . . H12B H 0.0893 0.6067 0.8132 0.065 Uiso 1 1 calc R . . C45B C 0.6991(3) 0.0927(3) 0.54738(19) 0.0465(10) Uani 1 1 d . . . C24A C 0.6759(4) 0.2427(4) 0.17258(19) 0.0541(12) Uani 1 1 d . . . H24A H 0.7446 0.2025 0.1829 0.065 Uiso 1 1 calc R . . C30A C 0.4409(4) 0.3696(4) -0.03674(18) 0.0501(11) Uani 1 1 d . . . H30A H 0.3976 0.4358 -0.0498 0.060 Uiso 1 1 calc R . . C22A C 0.5294(4) 0.4000(4) 0.16377(18) 0.0516(12) Uani 1 1 d . . . H22A H 0.4969 0.4697 0.1674 0.062 Uiso 1 1 calc R . . C46A C 0.2104(4) 0.5978(3) 0.06079(19) 0.0498(11) Uani 1 1 d . . . H46A H 0.2255 0.5715 0.0969 0.060 Uiso 1 1 calc R . . C24B C 0.2014(4) -0.0019(3) 0.6361(2) 0.0589(13) Uani 1 1 d . . . H24B H 0.2584 -0.0661 0.6315 0.071 Uiso 1 1 calc R . . C23B C 0.1004(5) 0.0085(4) 0.6647(2) 0.0675(16) Uani 1 1 d . . . H23B H 0.0896 -0.0492 0.6808 0.081 Uiso 1 1 calc R . . C50A C 0.0977(4) 0.6460(3) -0.00736(19) 0.0531(11) Uani 1 1 d . . . H50A H 0.0342 0.6530 -0.0185 0.064 Uiso 1 1 calc R . . C21B C 0.0330(4) 0.1853(4) 0.6471(2) 0.0589(13) Uani 1 1 d . . . H21B H -0.0257 0.2489 0.6503 0.071 Uiso 1 1 calc R . . C28B C 0.1471(6) 0.2164(3) 0.4410(2) 0.0700(17) Uani 1 1 d . . . H28B H 0.0993 0.2018 0.4262 0.084 Uiso 1 1 calc R . . C29B C 0.2370(6) 0.2181(3) 0.4083(2) 0.0714(18) Uani 1 1 d . . . H29B H 0.2529 0.2028 0.3713 0.086 Uiso 1 1 calc R . . C46B C 0.7808(4) 0.0443(4) 0.5072(2) 0.0591(12) Uani 1 1 d . . . H46B H 0.7848 -0.0142 0.4952 0.071 Uiso 1 1 calc R . . C48A C 0.2625(5) 0.6650(4) -0.0284(2) 0.0664(14) Uani 1 1 d . . . H48A H 0.3123 0.6841 -0.0539 0.080 Uiso 1 1 calc R . . C22B C 0.0186(5) 0.0994(5) 0.6697(2) 0.0751(17) Uani 1 1 d . . . H22B H -0.0497 0.1052 0.6887 0.090 Uiso 1 1 calc R . . C30B C 0.3037(5) 0.2418(3) 0.42877(18) 0.0643(15) Uani 1 1 d . . . H30B H 0.3657 0.2445 0.4057 0.077 Uiso 1 1 calc R . . C47A C 0.2816(4) 0.6273(4) 0.0239(2) 0.0654(14) Uani 1 1 d . . . H47A H 0.3448 0.6213 0.0350 0.079 Uiso 1 1 calc R . . C49A C 0.1686(5) 0.6749(4) -0.0434(2) 0.0674(15) Uani 1 1 d . . . H49A H 0.1536 0.7021 -0.0794 0.081 Uiso 1 1 calc R . . C50B C 0.6957(5) 0.1768(4) 0.5649(2) 0.0780(17) Uani 1 1 d . . . H50B H 0.6414 0.2103 0.5936 0.094 Uiso 1 1 calc R . . C47B C 0.8579(4) 0.0799(5) 0.4840(2) 0.0759(16) Uani 1 1 d . . . H47B H 0.9137 0.0458 0.4561 0.091 Uiso 1 1 calc R . . C48B C 0.8543(5) 0.1629(5) 0.5006(3) 0.0851(19) Uani 1 1 d . . . H48B H 0.9074 0.1868 0.4851 0.102 Uiso 1 1 calc R . . C49B C 0.7723(6) 0.2112(5) 0.5403(3) 0.105(3) Uani 1 1 d . . . H49B H 0.7679 0.2705 0.5514 0.125 Uiso 1 1 calc R . . O1C O 0.7094(4) 0.2392(4) 0.8087(2) 0.1164(17) Uiso 1 1 d . . . C99 C 0.9375(6) 0.0812(6) -0.0222(3) 0.102(2) Uiso 1 1 d . . . C103 C 0.7012(7) 0.2975(7) 0.7119(4) 0.122(3) Uiso 1 1 d . . . C102 C 0.7383(9) 0.3587(8) 0.7368(5) 0.157(4) Uiso 1 1 d . . . C104 C 0.6793(6) 0.2295(5) 0.7585(3) 0.096(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1A 0.0186(2) 0.0196(2) 0.0239(2) -0.00232(16) -0.00309(16) -0.00711(17) Co2B 0.0230(2) 0.0213(2) 0.0239(2) -0.00173(17) -0.00340(17) -0.00680(17) P1A 0.0225(4) 0.0230(4) 0.0232(4) -0.0024(3) -0.0038(3) -0.0099(3) P2B 0.0235(4) 0.0239(4) 0.0293(4) -0.0006(3) -0.0055(3) -0.0102(3) P3A 0.0204(4) 0.0228(4) 0.0256(4) -0.0037(3) -0.0041(3) -0.0082(3) S2A 0.0282(4) 0.0267(4) 0.0488(6) -0.0014(4) -0.0168(4) -0.0078(4) P2A 0.0208(4) 0.0239(4) 0.0263(4) -0.0022(3) -0.0033(3) -0.0096(3) S1A 0.0396(5) 0.0285(4) 0.0340(5) -0.0119(4) -0.0038(4) -0.0080(4) S1B 0.0376(5) 0.0428(5) 0.0442(6) -0.0023(4) -0.0186(4) -0.0106(4) P3B 0.0267(4) 0.0251(4) 0.0327(5) -0.0058(4) -0.0051(4) -0.0103(4) S2B 0.0359(5) 0.0419(6) 0.0457(6) -0.0169(4) -0.0049(4) -0.0037(4) P1B 0.0270(4) 0.0257(4) 0.0235(4) -0.0006(3) -0.0026(3) -0.0074(4) C2A 0.0181(15) 0.0241(16) 0.0327(17) -0.0030(13) -0.0014(13) -0.0086(13) C38A 0.0274(17) 0.0302(17) 0.0253(16) -0.0008(13) -0.0058(13) -0.0184(14) C14A 0.0247(16) 0.0332(17) 0.0214(15) 0.0004(13) -0.0034(13) -0.0168(14) C3A 0.0220(16) 0.0211(15) 0.0300(17) -0.0035(13) -0.0062(13) -0.0052(13) C20A 0.0272(17) 0.0365(18) 0.0242(16) -0.0018(14) -0.0013(13) -0.0195(15) C1A 0.0212(16) 0.0240(16) 0.0308(17) -0.0059(13) 0.0018(13) -0.0086(13) C5B 0.0304(19) 0.0331(19) 0.040(2) -0.0046(15) -0.0127(16) -0.0099(15) C8B 0.040(2) 0.0283(17) 0.0241(16) -0.0020(13) 0.0011(14) -0.0185(15) C6A 0.0219(16) 0.0274(17) 0.0323(18) -0.0017(14) -0.0039(14) -0.0075(13) C4A 0.0305(18) 0.0221(16) 0.0281(17) -0.0011(13) -0.0077(14) -0.0093(14) C26A 0.0299(18) 0.0383(19) 0.0261(17) -0.0052(14) -0.0022(14) -0.0196(15) C43A 0.037(2) 0.0303(19) 0.044(2) 0.0002(16) -0.0097(17) -0.0158(16) C32B 0.0337(19) 0.0304(18) 0.0308(18) -0.0004(14) -0.0049(15) -0.0171(15) C5A 0.0238(16) 0.0255(16) 0.0315(18) -0.0078(13) -0.0032(14) -0.0074(13) C32A 0.0204(16) 0.0320(17) 0.0234(16) -0.0049(13) -0.0041(13) -0.0079(13) C3B 0.0249(17) 0.0247(16) 0.0279(17) -0.0026(13) -0.0026(13) -0.0057(13) C8A 0.0245(16) 0.0310(17) 0.0260(16) -0.0036(13) -0.0039(13) -0.0153(14) C14B 0.0361(19) 0.0371(19) 0.0208(16) 0.0032(14) -0.0081(14) -0.0218(16) C33B 0.038(2) 0.043(2) 0.041(2) -0.0004(17) -0.0084(17) -0.0184(18) C15B 0.040(2) 0.038(2) 0.036(2) 0.0075(16) -0.0109(17) -0.0202(17) C1B 0.0283(18) 0.0291(18) 0.0362(19) -0.0003(14) -0.0068(15) -0.0120(15) C38B 0.0294(18) 0.0325(18) 0.0366(19) -0.0098(15) 0.0032(15) -0.0167(15) C7B 0.0282(18) 0.0285(18) 0.041(2) -0.0028(15) -0.0063(15) -0.0061(15) C39A 0.0313(19) 0.036(2) 0.046(2) -0.0084(16) -0.0004(16) -0.0189(16) C10A 0.0292(19) 0.044(2) 0.039(2) -0.0106(17) 0.0027(16) -0.0168(17) C9B 0.055(2) 0.039(2) 0.0273(18) -0.0054(15) -0.0071(17) -0.0232(19) C17A 0.039(2) 0.055(2) 0.041(2) -0.0016(18) -0.0151(17) -0.0281(19) C12A 0.046(2) 0.049(2) 0.033(2) 0.0026(17) -0.0049(17) -0.031(2) C9A 0.0340(19) 0.0310(18) 0.0323(18) -0.0036(14) -0.0019(15) -0.0166(15) C7A 0.0294(19) 0.0247(17) 0.044(2) -0.0043(15) -0.0055(16) -0.0037(14) C13A 0.0319(19) 0.0358(19) 0.0327(19) 0.0014(15) -0.0061(15) -0.0169(16) C43B 0.036(2) 0.042(2) 0.037(2) -0.0046(16) -0.0028(16) -0.0215(17) C4B 0.0254(17) 0.0364(19) 0.0330(19) -0.0032(15) -0.0027(14) -0.0105(15) C26B 0.047(2) 0.0252(17) 0.0301(18) 0.0005(14) -0.0158(17) -0.0093(16) C16A 0.047(2) 0.041(2) 0.037(2) -0.0029(16) -0.0097(17) -0.0285(18) C19B 0.043(2) 0.052(2) 0.0261(18) -0.0037(16) -0.0062(16) -0.0266(19) C2B 0.0249(17) 0.0301(18) 0.0334(18) -0.0050(14) -0.0029(14) -0.0095(14) C15A 0.0352(19) 0.0346(19) 0.0320(19) 0.0002(15) -0.0085(15) -0.0170(16) C31A 0.033(2) 0.046(2) 0.036(2) 0.0051(17) -0.0044(16) -0.0172(18) C20B 0.043(2) 0.0358(19) 0.0339(19) -0.0034(15) -0.0077(16) -0.0238(17) C37A 0.035(2) 0.044(2) 0.034(2) -0.0066(16) -0.0063(16) -0.0187(17) C11A 0.039(2) 0.059(3) 0.0303(19) -0.0122(17) 0.0066(16) -0.033(2) C33A 0.0251(17) 0.0343(19) 0.0322(18) -0.0035(15) -0.0041(14) -0.0084(15) C35A 0.0282(19) 0.061(3) 0.0256(18) -0.0065(18) -0.0052(15) -0.0067(18) C42B 0.048(2) 0.055(3) 0.046(2) -0.0058(19) -0.0105(19) -0.030(2) C11B 0.086(4) 0.058(3) 0.031(2) -0.0123(19) 0.002(2) -0.052(3) C42A 0.045(2) 0.041(2) 0.053(3) 0.0083(18) -0.0107(19) -0.029(2) C16B 0.053(3) 0.040(2) 0.044(2) 0.0105(18) -0.018(2) -0.024(2) C18B 0.058(3) 0.070(3) 0.0284(19) 0.0012(19) -0.0038(18) -0.046(2) C6B 0.0293(18) 0.0243(17) 0.042(2) 0.0019(15) -0.0045(16) -0.0087(14) C13B 0.045(2) 0.037(2) 0.050(2) -0.0131(18) 0.0016(19) -0.0191(18) C19A 0.037(2) 0.036(2) 0.038(2) 0.0003(16) -0.0120(16) -0.0163(16) C34A 0.0252(18) 0.044(2) 0.0317(19) 0.0039(16) -0.0026(15) -0.0073(16) C45A 0.043(2) 0.0239(17) 0.045(2) -0.0033(15) -0.0126(18) -0.0101(16) C41A 0.043(2) 0.060(3) 0.043(2) 0.0002(19) -0.0039(18) -0.037(2) C21A 0.035(2) 0.044(2) 0.048(2) -0.0115(18) 0.0017(17) -0.0215(18) C36A 0.040(2) 0.058(3) 0.038(2) -0.0148(19) -0.0096(17) -0.021(2) C27A 0.057(3) 0.038(2) 0.037(2) -0.0141(17) 0.0072(19) -0.0226(19) C10B 0.060(3) 0.059(3) 0.034(2) 0.0007(19) -0.0106(19) -0.035(2) C44A 0.032(2) 0.0219(17) 0.059(3) -0.0033(16) -0.0114(18) -0.0029(15) C25A 0.038(2) 0.048(2) 0.047(2) 0.0107(18) -0.0163(18) -0.0266(19) C17B 0.073(3) 0.054(3) 0.035(2) 0.0110(19) -0.021(2) -0.044(2) C39B 0.033(2) 0.034(2) 0.059(3) -0.0077(18) -0.0056(18) -0.0125(17) C18A 0.038(2) 0.046(2) 0.047(2) 0.0051(18) -0.0223(18) -0.0164(18) C40A 0.0283(19) 0.045(2) 0.060(3) -0.0130(19) 0.0021(18) -0.0196(18) C25B 0.047(2) 0.040(2) 0.058(3) 0.0088(19) -0.024(2) -0.0246(19) C34B 0.053(3) 0.062(3) 0.035(2) 0.0043(19) -0.0141(19) -0.030(2) C41B 0.058(3) 0.060(3) 0.057(3) -0.020(2) -0.001(2) -0.039(2) C31B 0.045(2) 0.034(2) 0.036(2) -0.0024(16) -0.0048(18) -0.0047(17) C28A 0.085(4) 0.056(3) 0.034(2) -0.023(2) 0.016(2) -0.044(3) C40B 0.044(2) 0.037(2) 0.069(3) -0.013(2) 0.004(2) -0.0238(19) C29A 0.080(3) 0.070(3) 0.031(2) 0.001(2) -0.007(2) -0.055(3) C27B 0.071(3) 0.041(2) 0.046(2) 0.0041(19) -0.027(2) -0.025(2) C44B 0.031(2) 0.033(2) 0.058(3) -0.0041(18) -0.0066(18) -0.0007(16) C36B 0.040(2) 0.074(3) 0.047(3) -0.006(2) 0.005(2) -0.024(2) C23A 0.065(3) 0.082(3) 0.040(2) -0.006(2) -0.007(2) -0.058(3) C35B 0.059(3) 0.068(3) 0.031(2) -0.003(2) 0.001(2) -0.035(2) C37B 0.031(2) 0.056(3) 0.039(2) -0.0016(19) -0.0043(17) -0.0129(19) C12B 0.066(3) 0.048(3) 0.055(3) -0.023(2) 0.007(2) -0.030(2) C45B 0.037(2) 0.036(2) 0.055(3) -0.0015(19) -0.0039(19) -0.0081(18) C24A 0.056(3) 0.068(3) 0.060(3) 0.017(2) -0.030(2) -0.043(2) C30A 0.047(3) 0.060(3) 0.048(3) 0.016(2) -0.014(2) -0.031(2) C22A 0.063(3) 0.059(3) 0.050(3) -0.024(2) 0.012(2) -0.044(2) C46A 0.061(3) 0.045(2) 0.052(3) 0.009(2) -0.025(2) -0.028(2) C24B 0.070(3) 0.040(2) 0.084(4) 0.013(2) -0.043(3) -0.031(2) C23B 0.114(5) 0.072(4) 0.055(3) 0.015(3) -0.028(3) -0.075(4) C50A 0.060(3) 0.050(3) 0.056(3) 0.000(2) -0.025(2) -0.023(2) C21B 0.061(3) 0.058(3) 0.067(3) -0.022(2) 0.014(2) -0.039(3) C28B 0.128(5) 0.042(3) 0.051(3) 0.004(2) -0.053(3) -0.031(3) C29B 0.128(5) 0.034(2) 0.032(2) -0.0016(19) -0.023(3) -0.011(3) C46B 0.053(3) 0.048(3) 0.060(3) -0.006(2) 0.002(2) -0.010(2) C48A 0.081(4) 0.070(3) 0.058(3) 0.003(3) -0.001(3) -0.048(3) C22B 0.093(4) 0.089(4) 0.071(4) -0.025(3) 0.024(3) -0.073(4) C30B 0.083(4) 0.042(3) 0.035(2) -0.0064(19) -0.002(2) 0.001(2) C47A 0.069(3) 0.071(3) 0.077(4) 0.015(3) -0.025(3) -0.049(3) C49A 0.100(4) 0.067(3) 0.046(3) 0.010(2) -0.021(3) -0.046(3) C50B 0.086(4) 0.072(4) 0.083(4) -0.026(3) 0.018(3) -0.047(3) C47B 0.059(3) 0.082(4) 0.067(4) 0.001(3) 0.013(3) -0.025(3) C48B 0.080(4) 0.107(5) 0.086(4) -0.009(4) 0.010(3) -0.065(4) C49B 0.139(7) 0.105(5) 0.106(5) -0.035(4) 0.028(5) -0.095(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 C222 O1C 1.437(9) . ? C222 C102 1.480(13) . ? O333 C98 1.232(11) . ? O333 C99 1.305(11) 2_755 ? C98 C99 1.511(10) . ? C98 C99 1.982(10) 2_755 ? Co1A C2A 1.821(3) . ? Co1A C1A 1.876(3) . ? Co1A P2A 2.1537(10) . ? Co1A P1A 2.1857(10) . ? Co1A P3A 2.1932(9) . ? Co2B C2B 1.821(3) . ? Co2B C1B 1.865(4) . ? Co2B P2B 2.1507(10) . ? Co2B P1B 2.1819(10) . ? Co2B P3B 2.1956(10) . ? P1A C14A 1.832(3) . ? P1A C8A 1.834(3) . ? P1A C4A 1.843(3) . ? P2B C32B 1.834(4) . ? P2B C38B 1.837(4) . ? P2B C6B 1.859(4) . ? P3A C32A 1.825(3) . ? P3A C38A 1.832(3) . ? P3A C5A 1.835(3) . ? S2A C2A 1.691(3) . ? S2A C44A 1.830(4) . ? P2A C20A 1.831(3) . ? P2A C26A 1.839(3) . ? P2A C6A 1.851(3) . ? S1A C1A 1.665(3) . ? S1B C1B 1.669(4) . ? P3B C26B 1.823(4) . ? P3B C20B 1.837(4) . ? P3B C5B 1.844(4) . ? S2B C2B 1.691(3) . ? S2B C44B 1.831(4) . ? P1B C14B 1.819(3) . ? P1B C8B 1.827(4) . ? P1B C4B 1.850(4) . ? C2A C1A 1.346(5) . ? C38A C39A 1.385(5) . ? C38A C43A 1.391(5) . ? C14A C15A 1.382(5) . ? C14A C19A 1.390(5) . ? C3A C7A 1.534(4) . ? C3A C5A 1.543(4) . ? C3A C4A 1.546(5) . ? C3A C6A 1.548(5) . ? C20A C25A 1.388(5) . ? C20A C21A 1.390(5) . ? C5B C3B 1.551(5) . ? C8B C9B 1.379(5) . ? C8B C13B 1.390(5) . ? C26A C27A 1.381(5) . ? C26A C31A 1.393(5) . ? C43A C42A 1.395(5) . ? C32B C33B 1.381(5) . ? C32B C37B 1.385(5) . ? C32A C33A 1.378(5) . ? C32A C37A 1.403(5) . ? C3B C6B 1.530(5) . ? C3B C4B 1.531(5) . ? C3B C7B 1.533(5) . ? C8A C9A 1.386(5) . ? C8A C13A 1.405(5) . ? C14B C15B 1.385(5) . ? C14B C19B 1.395(5) . ? C33B C34B 1.389(6) . ? C15B C16B 1.390(5) . ? C1B C2B 1.343(5) . ? C38B C43B 1.377(5) . ? C38B C39B 1.385(5) . ? C39A C40A 1.386(5) . ? C10A C11A 1.386(6) . ? C10A C9A 1.390(5) . ? C9B C10B 1.391(5) . ? C17A C16A 1.379(5) . ? C17A C18A 1.387(6) . ? C12A C11A 1.384(6) . ? C12A C13A 1.385(5) . ? C43B C42B 1.387(5) . ? C26B C31B 1.374(6) . ? C26B C27B 1.395(6) . ? C16A C15A 1.387(5) . ? C19B C18B 1.398(6) . ? C31A C30A 1.388(5) . ? C20B C21B 1.386(6) . ? C20B C25B 1.394(6) . ? C37A C36A 1.383(5) . ? C33A C34A 1.394(5) . ? C35A C34A 1.372(6) . ? C35A C36A 1.375(6) . ? C42B C41B 1.382(6) . ? C11B C10B 1.372(6) . ? C11B C12B 1.373(7) . ? C42A C41A 1.377(6) . ? C16B C17B 1.374(6) . ? C18B C17B 1.368(6) . ? C13B C12B 1.383(6) . ? C19A C18A 1.374(5) . ? C45A C46A 1.375(6) . ? C45A C50A 1.402(6) . ? C45A C44A 1.497(6) . ? C41A C40A 1.376(6) . ? C21A C22A 1.384(5) . ? C27A C28A 1.392(6) . ? C25A C24A 1.375(6) . ? C39B C40B 1.402(6) . ? C25B C24B 1.388(6) . ? C34B C35B 1.356(6) . ? C41B C40B 1.364(6) . ? C31B C30B 1.392(6) . ? C28A C29A 1.374(7) . ? C29A C30A 1.369(6) . ? C27B C28B 1.397(6) . ? C44B C45B 1.509(6) . ? C36B C35B 1.380(6) . ? C36B C37B 1.389(6) . ? C23A C22A 1.369(7) . ? C23A C24A 1.371(7) . ? C45B C46B 1.373(6) . ? C45B C50B 1.384(7) . ? C46A C47A 1.380(6) . ? C24B C23B 1.401(8) . ? C23B C22B 1.348(8) . ? C50A C49A 1.363(7) . ? C21B C22B 1.395(7) . ? C28B C29B 1.359(8) . ? C29B C30B 1.354(8) . ? C46B C47B 1.390(7) . ? C48A C47A 1.365(7) . ? C48A C49A 1.389(7) . ? C50B C49B 1.379(8) . ? C47B C48B 1.357(8) . ? C48B C49B 1.366(9) . ? O1C C104 1.459(8) . ? C99 O333 1.305(11) 2_755 ? C99 C98 1.982(10) 2_755 ? C103 C104 1.485(11) . ? C103 C102 1.507(12) . ? 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 O1C C222 C102 111.7(8) . . ? C98 O333 C99 102.7(9) . 2_755 ? O333 C98 C99 122.1(8) . . ? O333 C98 C99 40.0(6) . 2_755 ? C99 C98 C99 91.6(5) . 2_755 ? C2A Co1A C1A 42.66(14) . . ? C2A Co1A P2A 124.95(11) . . ? C1A Co1A P2A 114.61(10) . . ? C2A Co1A P1A 141.42(11) . . ? C1A Co1A P1A 109.87(11) . . ? P2A Co1A P1A 88.53(3) . . ? C2A Co1A P3A 103.22(11) . . ? C1A Co1A P3A 144.08(11) . . ? P2A Co1A P3A 93.52(3) . . ? P1A Co1A P3A 91.85(4) . . ? C2B Co2B C1B 42.71(15) . . ? C2B Co2B P2B 122.24(12) . . ? C1B Co2B P2B 118.99(11) . . ? C2B Co2B P1B 142.31(12) . . ? C1B Co2B P1B 106.97(12) . . ? P2B Co2B P1B 90.10(4) . . ? C2B Co2B P3B 104.50(11) . . ? C1B Co2B P3B 142.70(11) . . ? P2B Co2B P3B 92.15(4) . . ? P1B Co2B P3B 91.86(4) . . ? C14A P1A C8A 101.18(14) . . ? C14A P1A C4A 104.14(15) . . ? C8A P1A C4A 103.00(15) . . ? C14A P1A Co1A 119.37(11) . . ? C8A P1A Co1A 116.00(11) . . ? C4A P1A Co1A 111.23(11) . . ? C32B P2B C38B 100.01(16) . . ? C32B P2B C6B 107.87(17) . . ? C38B P2B C6B 101.28(16) . . ? C32B P2B Co2B 114.24(12) . . ? C38B P2B Co2B 118.56(13) . . ? C6B P2B Co2B 113.25(11) . . ? C32A P3A C38A 100.67(15) . . ? C32A P3A C5A 100.25(15) . . ? C38A P3A C5A 106.51(16) . . ? C32A P3A Co1A 123.21(12) . . ? C38A P3A Co1A 111.59(11) . . ? C5A P3A Co1A 112.77(11) . . ? C2A S2A C44A 103.96(17) . . ? C20A P2A C26A 98.29(15) . . ? C20A P2A C6A 103.87(16) . . ? C26A P2A C6A 107.82(16) . . ? C20A P2A Co1A 118.37(11) . . ? C26A P2A Co1A 114.40(12) . . ? C6A P2A Co1A 112.58(11) . . ? C26B P3B C20B 98.83(17) . . ? C26B P3B C5B 100.22(17) . . ? C20B P3B C5B 106.82(18) . . ? C26B P3B Co2B 122.61(14) . . ? C20B P3B Co2B 112.25(12) . . ? C5B P3B Co2B 114.02(12) . . ? C2B S2B C44B 104.81(19) . . ? C14B P1B C8B 98.93(15) . . ? C14B P1B C4B 101.87(17) . . ? C8B P1B C4B 105.23(17) . . ? C14B P1B Co2B 115.85(12) . . ? C8B P1B Co2B 120.97(12) . . ? C4B P1B Co2B 111.62(12) . . ? C1A C2A S2A 140.1(3) . . ? C1A C2A Co1A 70.9(2) . . ? S2A C2A Co1A 148.9(2) . . ? C39A C38A C43A 118.5(3) . . ? C39A C38A P3A 115.8(3) . . ? C43A C38A P3A 125.7(3) . . ? C15A C14A C19A 118.2(3) . . ? C15A C14A P1A 117.4(3) . . ? C19A C14A P1A 124.4(3) . . ? C7A C3A C5A 107.3(3) . . ? C7A C3A C4A 107.7(3) . . ? C5A C3A C4A 111.3(3) . . ? C7A C3A C6A 107.8(3) . . ? C5A C3A C6A 110.9(3) . . ? C4A C3A C6A 111.7(3) . . ? C25A C20A C21A 118.2(3) . . ? C25A C20A P2A 123.8(3) . . ? C21A C20A P2A 118.1(3) . . ? C2A C1A S1A 142.7(3) . . ? C2A C1A Co1A 66.46(19) . . ? S1A C1A Co1A 150.7(2) . . ? C3B C5B P3B 114.5(2) . . ? C9B C8B C13B 118.8(3) . . ? C9B C8B P1B 117.0(3) . . ? C13B C8B P1B 124.2(3) . . ? C3A C6A P2A 116.7(2) . . ? C3A C4A P1A 115.5(2) . . ? C27A C26A C31A 118.3(3) . . ? C27A C26A P2A 125.0(3) . . ? C31A C26A P2A 116.5(3) . . ? C38A C43A C42A 120.5(4) . . ? C33B C32B C37B 118.2(4) . . ? C33B C32B P2B 125.9(3) . . ? C37B C32B P2B 115.9(3) . . ? C3A C5A P3A 114.7(2) . . ? C33A C32A C37A 118.4(3) . . ? C33A C32A P3A 120.5(3) . . ? C37A C32A P3A 121.1(3) . . ? C6B C3B C4B 114.3(3) . . ? C6B C3B C7B 107.4(3) . . ? C4B C3B C7B 106.8(3) . . ? C6B C3B C5B 110.0(3) . . ? C4B C3B C5B 110.8(3) . . ? C7B C3B C5B 107.1(3) . . ? C9A C8A C13A 119.3(3) . . ? C9A C8A P1A 119.0(3) . . ? C13A C8A P1A 121.6(3) . . ? C15B C14B C19B 119.2(3) . . ? C15B C14B P1B 119.7(3) . . ? C19B C14B P1B 121.1(3) . . ? C32B C33B C34B 120.4(4) . . ? C14B C15B C16B 121.0(4) . . ? C2B C1B S1B 143.1(3) . . ? C2B C1B Co2B 66.9(2) . . ? S1B C1B Co2B 149.9(2) . . ? C43B C38B C39B 119.9(3) . . ? C43B C38B P2B 120.3(3) . . ? C39B C38B P2B 119.8(3) . . ? C38A C39A C40A 120.9(4) . . ? C11A C10A C9A 119.9(4) . . ? C8B C9B C10B 120.8(4) . . ? C16A C17A C18A 119.1(3) . . ? C11A C12A C13A 120.4(4) . . ? C8A C9A C10A 120.5(3) . . ? C12A C13A C8A 119.8(3) . . ? C38B C43B C42B 119.9(4) . . ? C3B C4B P1B 116.8(2) . . ? C31B C26B C27B 118.7(4) . . ? C31B C26B P3B 120.8(3) . . ? C27B C26B P3B 120.5(3) . . ? C17A C16A C15A 120.5(3) . . ? C14B C19B C18B 119.3(4) . . ? C1B C2B S2B 140.0(3) . . ? C1B C2B Co2B 70.4(2) . . ? S2B C2B Co2B 149.6(2) . . ? C14A C15A C16A 120.7(3) . . ? C30A C31A C26A 120.8(4) . . ? C21B C20B C25B 118.7(4) . . ? C21B C20B P3B 125.9(3) . . ? C25B C20B P3B 115.4(3) . . ? C36A C37A C32A 120.5(4) . . ? C12A C11A C10A 120.0(3) . . ? C32A C33A C34A 121.0(4) . . ? C34A C35A C36A 120.6(4) . . ? C41B C42B C43B 119.9(4) . . ? C10B C11B C12B 119.5(4) . . ? C41A C42A C43A 120.1(4) . . ? C17B C16B C15B 119.1(4) . . ? C17B C18B C19B 120.3(4) . . ? C3B C6B P2B 117.1(2) . . ? C12B C13B C8B 119.8(4) . . ? C18A C19A C14A 121.3(4) . . ? C35A C34A C33A 119.6(4) . . ? C46A C45A C50A 118.0(4) . . ? C46A C45A C44A 121.0(4) . . ? C50A C45A C44A 120.9(4) . . ? C40A C41A C42A 119.8(4) . . ? C22A C21A C20A 120.0(4) . . ? C35A C36A C37A 119.9(4) . . ? C26A C27A C28A 120.3(4) . . ? C11B C10B C9B 119.9(4) . . ? C45A C44A S2A 110.3(3) . . ? C24A C25A C20A 121.1(4) . . ? C18B C17B C16B 121.1(4) . . ? C38B C39B C40B 120.0(4) . . ? C19A C18A C17A 120.2(4) . . ? C41A C40A C39A 120.3(4) . . ? C24B C25B C20B 121.1(4) . . ? C35B C34B C33B 121.4(4) . . ? C40B C41B C42B 120.9(4) . . ? C26B C31B C30B 120.6(5) . . ? C29A C28A C27A 120.8(4) . . ? C41B C40B C39B 119.2(4) . . ? C30A C29A C28A 119.4(4) . . ? C26B C27B C28B 119.2(5) . . ? C45B C44B S2B 113.9(3) . . ? C35B C36B C37B 120.4(4) . . ? C22A C23A C24A 119.4(4) . . ? C34B C35B C36B 118.9(4) . . ? C32B C37B C36B 120.7(4) . . ? C11B C12B C13B 121.0(4) . . ? C46B C45B C50B 118.8(5) . . ? C46B C45B C44B 120.7(4) . . ? C50B C45B C44B 120.3(4) . . ? C23A C24A C25A 120.3(4) . . ? C29A C30A C31A 120.3(4) . . ? C23A C22A C21A 121.1(4) . . ? C45A C46A C47A 121.0(4) . . ? C25B C24B C23B 118.7(5) . . ? C22B C23B C24B 120.6(4) . . ? C49A C50A C45A 120.5(4) . . ? C20B C21B C22B 120.1(5) . . ? C29B C28B C27B 121.1(5) . . ? C30B C29B C28B 119.7(5) . . ? C45B C46B C47B 120.6(5) . . ? C47A C48A C49A 118.5(5) . . ? C23B C22B C21B 120.7(5) . . ? C29B C30B C31B 120.7(5) . . ? C48A C47A C46A 121.0(5) . . ? C50A C49A C48A 121.0(5) . . ? C49B C50B C45B 119.1(5) . . ? C48B C47B C46B 120.8(5) . . ? C47B C48B C49B 118.3(5) . . ? C48B C49B C50B 122.3(6) . . ? C222 O1C C104 104.9(6) . . ? O333 C99 C98 117.2(8) 2_755 . ? O333 C99 C98 37.3(5) 2_755 2_755 ? C98 C99 C98 88.4(5) . 2_755 ? C104 C103 C102 104.5(8) . . ? C222 C102 C103 105.9(9) . . ? O1C C104 C103 112.0(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.493 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.089 # Attachment 'comp_6-BPh4.cif' data_sad4 _database_code_depnum_ccdc_archive 'CCDC 740235' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H67 B Co N2 P3 Pt S2' _chemical_formula_weight 1466.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -4.5932 6.9264 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1143(6) _cell_length_b 17.6581(12) _cell_length_c 18.2065(11) _cell_angle_alpha 64.204(4) _cell_angle_beta 89.668(4) _cell_angle_gamma 89.378(5) _cell_volume 3216.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 75 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 7.704 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2703 _exptl_absorpt_correction_T_max 0.8018 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.573548 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator goebel-mirror _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19176 _diffrn_reflns_av_R_equivalents 0.1120 _diffrn_reflns_av_sigmaI/netI 0.1307 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 72.59 _reflns_number_total 10952 _reflns_number_gt 8632 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution ; SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_structure_refinement ; SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10952 _refine_ls_number_parameters 803 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.1737 _refine_ls_wR_factor_gt 0.1600 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 Pt1 Pt 0.58858(3) 0.62995(2) 0.668653(18) 0.02783(12) Uani 1 1 d . . . Co1 Co 0.77115(10) 0.78778(7) 0.79100(6) 0.0209(2) Uani 1 1 d . . . P3 P 0.83055(15) 0.72791(11) 0.91752(10) 0.0214(4) Uani 1 1 d . . . P1 P 0.92768(16) 0.86729(11) 0.75305(10) 0.0241(4) Uani 1 1 d . . . P2 P 0.67233(15) 0.88514(11) 0.80787(11) 0.0237(4) Uani 1 1 d . . . S2 S 0.59741(16) 0.76965(11) 0.63889(11) 0.0299(4) Uani 1 1 d . . . S1 S 0.71887(17) 0.60120(12) 0.77301(12) 0.0329(4) Uani 1 1 d . . . N2 N 0.4621(5) 0.6443(4) 0.5811(4) 0.0261(13) Uani 1 1 d . . . N1 N 0.5770(6) 0.5061(4) 0.6868(4) 0.0322(15) Uani 1 1 d . . . C2 C 0.6893(6) 0.7680(4) 0.7148(4) 0.0223(14) Uani 1 1 d . . . C1 C 0.7406(6) 0.6970(5) 0.7705(4) 0.0258(15) Uani 1 1 d . . . C42 C 0.8822(6) 0.8956(4) 0.8946(4) 0.0231(14) Uani 1 1 d . . . C38 C 0.7448(6) 0.6243(5) 1.0743(4) 0.0292(16) Uani 1 1 d . . . H38 H 0.8163 0.6385 1.0936 0.035 Uiso 1 1 calc R . . C33 C 0.7238(6) 0.6568(4) 0.9912(4) 0.0224(14) Uani 1 1 d . . . C39 C 0.9785(6) 0.8979(4) 0.8327(4) 0.0229(14) Uani 1 1 d . . . H39A H 1.0456 0.8601 0.8629 0.028 Uiso 1 1 calc R . . H39B H 1.0107 0.9557 0.8056 0.028 Uiso 1 1 calc R . . C34 C 0.6186(6) 0.6358(5) 0.9636(4) 0.0269(15) Uani 1 1 d . . . H34 H 0.6035 0.6567 0.9068 0.032 Uiso 1 1 calc R . . C43 C 0.9316(7) 0.9431(4) 0.9397(4) 0.0292(16) Uani 1 1 d . . . H43A H 0.8789 0.9349 0.9859 0.044 Uiso 1 1 calc R . . H43B H 0.9354 1.0032 0.9026 0.044 Uiso 1 1 calc R . . H43C H 1.0125 0.9220 0.9599 0.044 Uiso 1 1 calc R . . C40 C 0.7664(6) 0.9415(4) 0.8496(4) 0.0272(15) Uani 1 1 d . . . H40A H 0.7899 0.9957 0.8043 0.033 Uiso 1 1 calc R . . H40B H 0.7169 0.9547 0.8880 0.033 Uiso 1 1 calc R . . C9 C 1.0637(6) 0.8260(5) 0.7275(4) 0.0305(17) Uani 1 1 d . . . C3 C 0.9076(6) 0.9634(5) 0.6587(4) 0.0279(16) Uani 1 1 d . . . C41 C 0.8552(6) 0.8061(4) 0.9576(4) 0.0207(14) Uani 1 1 d . . . H41A H 0.7827 0.8079 0.9886 0.025 Uiso 1 1 calc R . . H41B H 0.9231 0.7862 0.9966 0.025 Uiso 1 1 calc R . . C35 C 0.5362(7) 0.5841(5) 1.0199(5) 0.0343(18) Uani 1 1 d . . . H35 H 0.4628 0.5714 1.0014 0.041 Uiso 1 1 calc R . . C21 C 0.5449(6) 0.8428(5) 0.8776(4) 0.0275(15) Uani 1 1 d . . . C26 C 0.4565(7) 0.8041(5) 0.8525(5) 0.0334(17) Uani 1 1 d . . . H26 H 0.4685 0.7961 0.8046 0.040 Uiso 1 1 calc R . . C72 C -0.2661(7) 0.1720(5) 0.7462(5) 0.0386(19) Uani 1 1 d . . . H72 H -0.3239 0.1688 0.7095 0.046 Uiso 1 1 calc R . . C52 C 0.4346(7) 0.5706(6) 0.5801(5) 0.0369(19) Uani 1 1 d . . . C69 C -0.0953(7) 0.1807(5) 0.8506(5) 0.0342(18) Uani 1 1 d . . . H69 H -0.0364 0.1820 0.8876 0.041 Uiso 1 1 calc R . . C48 C 0.4945(7) 0.4973(5) 0.6351(5) 0.0365(19) Uani 1 1 d . . . C70 C -0.2057(7) 0.1438(5) 0.8811(5) 0.0387(19) Uani 1 1 d . . . H70 H -0.2215 0.1214 0.9380 0.046 Uiso 1 1 calc R . . C73 C -0.1554(7) 0.2089(5) 0.7174(5) 0.0336(17) Uani 1 1 d . . . H73 H -0.1394 0.2303 0.6606 0.040 Uiso 1 1 calc R . . C68 C -0.0677(6) 0.2160(5) 0.7669(4) 0.0291(16) Uani 1 1 d . . . C27 C 0.9684(6) 0.6640(4) 0.9389(4) 0.0249(15) Uani 1 1 d . . . C74 C 0.0817(6) 0.2885(5) 0.6376(5) 0.0324(17) Uani 1 1 d . . . C56 C 0.1670(6) 0.2037(5) 0.7900(4) 0.0317(17) Uani 1 1 d . . . C28 C 0.9830(7) 0.6123(5) 0.9015(5) 0.0328(17) Uani 1 1 d . . . H28 H 0.9229 0.6119 0.8647 0.039 Uiso 1 1 calc R . . C57 C 0.1662(7) 0.1175(5) 0.8149(5) 0.0354(18) Uani 1 1 d . . . H57 H 0.0998 0.0938 0.7999 0.042 Uiso 1 1 calc R . . C15 C 0.5905(6) 0.9692(5) 0.7252(4) 0.0281(16) Uani 1 1 d . . . C62 C 0.0517(6) 0.3546(5) 0.7432(4) 0.0286(16) Uani 1 1 d . . . C8 C 0.8712(7) 0.9518(6) 0.5918(5) 0.040(2) Uani 1 1 d . . . H8 H 0.8561 0.8965 0.5980 0.048 Uiso 1 1 calc R . . C20 C 0.5167(7) 1.0229(5) 0.7427(5) 0.0350(18) Uani 1 1 d . . . H20 H 0.5135 1.0173 0.7970 0.042 Uiso 1 1 calc R . . C37 C 0.6628(8) 0.5718(5) 1.1288(5) 0.0386(19) Uani 1 1 d . . . H37 H 0.6780 0.5495 1.1857 0.046 Uiso 1 1 calc R . . C16 C 0.5961(7) 0.9783(5) 0.6456(5) 0.0378(19) Uani 1 1 d . . . H16 H 0.6462 0.9423 0.6320 0.045 Uiso 1 1 calc R . . C47 C 0.4718(8) 0.4186(6) 0.6368(5) 0.040(2) Uani 1 1 d . . . C22 C 0.5268(7) 0.8521(6) 0.9482(5) 0.0380(19) Uani 1 1 d . . . H22 H 0.5859 0.8785 0.9663 0.046 Uiso 1 1 calc R . . C25 C 0.3516(7) 0.7774(5) 0.8966(5) 0.0384(19) Uani 1 1 d . . . H25 H 0.2907 0.7523 0.8784 0.046 Uiso 1 1 calc R . . C36 C 0.5587(8) 0.5513(5) 1.1014(5) 0.044(2) Uani 1 1 d . . . H36 H 0.5026 0.5142 1.1392 0.052 Uiso 1 1 calc R . . C24 C 0.3353(7) 0.7869(6) 0.9667(5) 0.045(2) Uani 1 1 d . . . H24 H 0.2632 0.7684 0.9974 0.054 Uiso 1 1 calc R . . C51 C 0.3492(7) 0.5660(6) 0.5253(6) 0.044(2) Uani 1 1 d . . . C75 C 0.0243(8) 0.3581(6) 0.5766(5) 0.041(2) Uani 1 1 d . . . H75 H -0.0278 0.3915 0.5924 0.050 Uiso 1 1 calc R . . C4 C 0.9310(7) 1.0424(5) 0.6497(5) 0.0366(18) Uani 1 1 d . . . H4 H 0.9563 1.0512 0.6951 0.044 Uiso 1 1 calc R . . C31 C 1.1575(7) 0.6116(5) 1.0071(5) 0.042(2) Uani 1 1 d . . . H31 H 1.2175 0.6113 1.0442 0.050 Uiso 1 1 calc R . . C23 C 0.4233(7) 0.8232(7) 0.9918(5) 0.050(2) Uani 1 1 d . . . H23 H 0.4125 0.8285 1.0412 0.060 Uiso 1 1 calc R . . B1 B 0.0584(7) 0.2650(5) 0.7351(5) 0.0281(18) Uani 1 1 d . . . C6 C 0.8795(8) 1.0996(6) 0.5078(5) 0.045(2) Uani 1 1 d . . . H6 H 0.8686 1.1466 0.4564 0.054 Uiso 1 1 calc R . . C32 C 1.0566(7) 0.6632(5) 0.9927(5) 0.0390(19) Uani 1 1 d . . . H32 H 1.0480 0.6982 1.0200 0.047 Uiso 1 1 calc R . . C53 C 0.2918(8) 0.6411(7) 0.4736(6) 0.053(3) Uani 1 1 d . . . H53 H 0.2324 0.6408 0.4364 0.064 Uiso 1 1 calc R . . C50 C 0.3308(8) 0.4849(7) 0.5267(6) 0.047(2) Uani 1 1 d . . . H50 H 0.2766 0.4807 0.4885 0.056 Uiso 1 1 calc R . . C5 C 0.9174(8) 1.1112(5) 0.5723(5) 0.044(2) Uani 1 1 d . . . H5 H 0.9352 1.1663 0.5657 0.053 Uiso 1 1 calc R . . C58 C 0.2576(8) 0.0641(6) 0.8607(5) 0.043(2) Uani 1 1 d . . . H58 H 0.2524 0.0053 0.8766 0.051 Uiso 1 1 calc R . . C61 C 0.2704(7) 0.2321(6) 0.8141(5) 0.040(2) Uani 1 1 d . . . H61 H 0.2772 0.2906 0.7990 0.049 Uiso 1 1 calc R . . C79 C 0.1558(7) 0.2426(6) 0.6109(5) 0.043(2) Uani 1 1 d . . . H79 H 0.1957 0.1939 0.6499 0.052 Uiso 1 1 calc R . . C71 C -0.2922(7) 0.1397(5) 0.8294(5) 0.0380(19) Uani 1 1 d . . . H71 H -0.3682 0.1153 0.8498 0.046 Uiso 1 1 calc R . . C67 C -0.0345(8) 0.3754(5) 0.7864(5) 0.041(2) Uani 1 1 d . . . H67 H -0.0917 0.3339 0.8170 0.049 Uiso 1 1 calc R . . C11 C 1.2738(8) 0.8461(6) 0.6903(5) 0.046(2) Uani 1 1 d . . . H11 H 1.3445 0.8792 0.6773 0.055 Uiso 1 1 calc R . . C30 C 1.1705(7) 0.5618(5) 0.9681(5) 0.039(2) Uani 1 1 d . . . H30 H 1.2405 0.5276 0.9770 0.047 Uiso 1 1 calc R . . C65 C 0.0366(8) 0.5161(5) 0.7416(5) 0.044(2) Uani 1 1 d . . . H65 H 0.0292 0.5708 0.7389 0.053 Uiso 1 1 calc R . . C29 C 1.0822(7) 0.5605(5) 0.9155(5) 0.040(2) Uani 1 1 d . . . H29 H 1.0898 0.5245 0.8893 0.047 Uiso 1 1 calc R . . C64 C 0.1249(8) 0.4975(6) 0.7002(5) 0.046(2) Uani 1 1 d . . . H64 H 0.1824 0.5390 0.6702 0.055 Uiso 1 1 calc R . . C55 C 0.4064(7) 0.7139(6) 0.5309(5) 0.0397(19) Uani 1 1 d . . . H55 H 0.4257 0.7656 0.5320 0.048 Uiso 1 1 calc R . . C10 C 1.1703(7) 0.8754(6) 0.7087(5) 0.0397(19) Uani 1 1 d . . . H10 H 1.1686 0.9290 0.7092 0.048 Uiso 1 1 calc R . . C19 C 0.4479(7) 1.0842(5) 0.6836(5) 0.040(2) Uani 1 1 d . . . H19 H 0.3973 1.1200 0.6969 0.048 Uiso 1 1 calc R . . C59 C 0.3555(7) 0.0957(7) 0.8831(5) 0.047(2) Uani 1 1 d . . . H59 H 0.4179 0.0595 0.9155 0.056 Uiso 1 1 calc R . . C14 C 1.0689(8) 0.7522(5) 0.7244(5) 0.046(2) Uani 1 1 d . . . H14 H 0.9981 0.7195 0.7347 0.055 Uiso 1 1 calc R . . C49 C 0.3860(9) 0.4159(7) 0.5788(6) 0.052(3) Uani 1 1 d . . . H49 H 0.3688 0.3636 0.5781 0.062 Uiso 1 1 calc R . . C46 C 0.5368(9) 0.3495(6) 0.6926(6) 0.049(2) Uani 1 1 d . . . H46 H 0.5236 0.2951 0.6956 0.058 Uiso 1 1 calc R . . C60 C 0.3608(7) 0.1805(7) 0.8575(5) 0.048(2) Uani 1 1 d . . . H60 H 0.4294 0.2038 0.8706 0.058 Uiso 1 1 calc R . . C66 C -0.0422(8) 0.4532(6) 0.7876(6) 0.047(2) Uani 1 1 d . . . H66 H -0.1017 0.4632 0.8201 0.056 Uiso 1 1 calc R . . C44 C 0.6357(8) 0.4398(6) 0.7385(6) 0.047(2) Uani 1 1 d . . . H44 H 0.6920 0.4461 0.7744 0.056 Uiso 1 1 calc R . . C63 C 0.1324(7) 0.4191(5) 0.7012(5) 0.0389(19) Uani 1 1 d . . . H63 H 0.1959 0.4084 0.6717 0.047 Uiso 1 1 calc R . . C45 C 0.6177(9) 0.3596(6) 0.7421(6) 0.052(2) Uani 1 1 d . . . H45 H 0.6627 0.3127 0.7793 0.062 Uiso 1 1 calc R . . C54 C 0.3199(8) 0.7131(7) 0.4763(6) 0.052(2) Uani 1 1 d . . . H54 H 0.2808 0.7640 0.4408 0.062 Uiso 1 1 calc R . . C12 C 1.2758(8) 0.7682(7) 0.6905(6) 0.052(3) Uani 1 1 d . . . H12 H 1.3490 0.7470 0.6792 0.063 Uiso 1 1 calc R . . C18 C 0.4533(8) 1.0928(5) 0.6044(5) 0.047(2) Uani 1 1 d . . . H18 H 0.4059 1.1346 0.5630 0.057 Uiso 1 1 calc R . . C78 C 0.1741(8) 0.2662(6) 0.5267(5) 0.050(2) Uani 1 1 d . . . H78 H 0.2261 0.2339 0.5096 0.060 Uiso 1 1 calc R . . C17 C 0.5267(9) 1.0412(6) 0.5856(5) 0.049(2) Uani 1 1 d . . . H17 H 0.5307 1.0481 0.5309 0.059 Uiso 1 1 calc R . . C76 C 0.0400(8) 0.3805(7) 0.4942(6) 0.053(2) Uani 1 1 d . . . H76 H -0.0027 0.4272 0.4546 0.063 Uiso 1 1 calc R . . C13 C 1.1760(9) 0.7217(6) 0.7063(6) 0.061(3) Uani 1 1 d . . . H13 H 1.1782 0.6683 0.7053 0.074 Uiso 1 1 calc R . . C77 C 0.1170(8) 0.3352(7) 0.4705(5) 0.053(3) Uani 1 1 d . . . H77 H 0.1310 0.3519 0.4141 0.064 Uiso 1 1 calc R . . C7 C 0.8565(8) 1.0189(6) 0.5163(5) 0.048(2) Uani 1 1 d . . . H7 H 0.8310 1.0102 0.4709 0.058 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 Pt1 0.02548(18) 0.03030(19) 0.03052(19) -0.01582(13) -0.00456(12) 0.00068(13) Co1 0.0196(5) 0.0191(6) 0.0233(6) -0.0087(4) -0.0043(4) 0.0012(5) P3 0.0205(8) 0.0191(8) 0.0236(9) -0.0083(6) -0.0021(7) 0.0000(7) P1 0.0235(9) 0.0227(9) 0.0228(9) -0.0070(7) -0.0015(7) -0.0003(7) P2 0.0210(9) 0.0221(9) 0.0281(9) -0.0112(7) -0.0048(7) 0.0036(7) S2 0.0320(9) 0.0263(9) 0.0320(10) -0.0132(7) -0.0122(7) 0.0049(8) S1 0.0378(10) 0.0230(9) 0.0410(11) -0.0168(8) -0.0167(8) 0.0061(8) N2 0.019(3) 0.038(4) 0.032(3) -0.024(3) -0.005(2) 0.000(3) N1 0.036(4) 0.036(4) 0.040(4) -0.031(3) -0.009(3) 0.001(3) C2 0.023(3) 0.024(3) 0.019(3) -0.008(3) -0.001(3) -0.002(3) C1 0.025(4) 0.026(4) 0.027(4) -0.012(3) 0.001(3) -0.003(3) C42 0.021(3) 0.020(3) 0.030(4) -0.012(3) -0.003(3) 0.000(3) C38 0.024(4) 0.027(4) 0.031(4) -0.008(3) 0.000(3) -0.001(3) C33 0.024(4) 0.019(3) 0.026(4) -0.011(3) -0.004(3) -0.001(3) C39 0.017(3) 0.019(3) 0.031(4) -0.009(3) -0.003(3) -0.003(3) C34 0.020(3) 0.027(4) 0.034(4) -0.013(3) -0.004(3) 0.000(3) C43 0.033(4) 0.019(3) 0.034(4) -0.010(3) -0.005(3) -0.001(3) C40 0.024(4) 0.026(4) 0.030(4) -0.011(3) -0.001(3) 0.003(3) C9 0.024(4) 0.038(4) 0.022(4) -0.007(3) 0.000(3) 0.004(3) C3 0.021(3) 0.029(4) 0.027(4) -0.007(3) -0.001(3) 0.004(3) C41 0.017(3) 0.023(3) 0.024(3) -0.012(3) 0.001(3) 0.000(3) C35 0.030(4) 0.029(4) 0.047(5) -0.019(3) 0.002(3) -0.010(3) C21 0.019(3) 0.025(4) 0.036(4) -0.012(3) 0.000(3) 0.002(3) C26 0.026(4) 0.041(5) 0.031(4) -0.014(3) -0.004(3) 0.000(3) C72 0.027(4) 0.032(4) 0.064(6) -0.026(4) -0.010(4) 0.000(4) C52 0.025(4) 0.052(5) 0.036(4) -0.021(4) 0.002(3) -0.002(4) C69 0.033(4) 0.024(4) 0.041(5) -0.010(3) 0.002(3) 0.005(3) C48 0.035(4) 0.043(5) 0.036(4) -0.022(4) 0.009(3) -0.008(4) C70 0.034(4) 0.029(4) 0.048(5) -0.013(4) 0.006(4) 0.005(4) C73 0.031(4) 0.030(4) 0.039(4) -0.015(3) 0.001(3) 0.000(3) C68 0.024(4) 0.028(4) 0.034(4) -0.013(3) -0.004(3) 0.007(3) C27 0.019(3) 0.020(3) 0.028(4) -0.004(3) 0.000(3) 0.002(3) C74 0.022(4) 0.041(5) 0.035(4) -0.017(3) 0.000(3) -0.007(3) C56 0.022(4) 0.048(5) 0.028(4) -0.018(3) 0.001(3) 0.003(4) C28 0.029(4) 0.034(4) 0.039(4) -0.020(3) -0.007(3) -0.002(3) C57 0.024(4) 0.045(5) 0.038(4) -0.018(4) -0.002(3) -0.003(4) C15 0.025(4) 0.025(4) 0.032(4) -0.009(3) -0.012(3) 0.001(3) C62 0.024(4) 0.031(4) 0.028(4) -0.010(3) -0.004(3) -0.002(3) C8 0.041(5) 0.042(5) 0.029(4) -0.008(3) 0.003(3) -0.004(4) C20 0.028(4) 0.040(5) 0.035(4) -0.015(3) -0.007(3) 0.006(4) C37 0.047(5) 0.040(5) 0.026(4) -0.012(3) 0.004(4) -0.004(4) C16 0.035(4) 0.031(4) 0.042(5) -0.011(3) -0.006(3) 0.005(4) C47 0.037(5) 0.049(5) 0.041(5) -0.026(4) 0.018(4) -0.019(4) C22 0.024(4) 0.062(6) 0.036(5) -0.029(4) -0.003(3) 0.001(4) C25 0.027(4) 0.045(5) 0.048(5) -0.025(4) -0.002(4) -0.005(4) C36 0.043(5) 0.036(5) 0.049(5) -0.017(4) 0.014(4) -0.014(4) C24 0.024(4) 0.060(6) 0.047(5) -0.018(4) 0.001(4) -0.007(4) C51 0.024(4) 0.068(6) 0.059(6) -0.045(5) 0.006(4) -0.005(4) C75 0.040(5) 0.044(5) 0.035(5) -0.012(4) -0.010(4) -0.002(4) C4 0.042(5) 0.033(4) 0.029(4) -0.008(3) 0.004(3) -0.001(4) C31 0.028(4) 0.036(5) 0.060(6) -0.021(4) -0.016(4) 0.008(4) C23 0.031(5) 0.084(7) 0.039(5) -0.031(5) 0.003(4) 0.001(5) B1 0.022(4) 0.028(4) 0.031(4) -0.010(3) 0.001(3) -0.001(4) C6 0.046(5) 0.043(5) 0.029(5) 0.000(4) 0.001(4) 0.004(4) C32 0.029(4) 0.042(5) 0.049(5) -0.022(4) -0.008(4) 0.005(4) C53 0.044(5) 0.079(8) 0.051(6) -0.042(5) -0.018(4) 0.005(5) C50 0.041(5) 0.067(7) 0.045(5) -0.035(5) 0.010(4) -0.026(5) C5 0.057(6) 0.021(4) 0.040(5) 0.001(3) 0.005(4) 0.002(4) C58 0.040(5) 0.038(5) 0.042(5) -0.011(4) 0.005(4) 0.011(4) C61 0.034(4) 0.052(5) 0.036(5) -0.019(4) -0.003(4) 0.001(4) C79 0.038(5) 0.055(6) 0.033(5) -0.016(4) -0.002(4) 0.001(4) C71 0.023(4) 0.025(4) 0.063(6) -0.017(4) 0.007(4) -0.003(3) C67 0.036(4) 0.039(5) 0.047(5) -0.019(4) 0.004(4) 0.002(4) C11 0.035(5) 0.065(6) 0.032(5) -0.017(4) -0.004(4) -0.002(4) C30 0.022(4) 0.029(4) 0.052(5) -0.004(4) 0.004(3) 0.007(3) C65 0.054(5) 0.026(4) 0.051(5) -0.016(4) -0.003(4) 0.002(4) C29 0.044(5) 0.030(4) 0.045(5) -0.018(4) -0.011(4) 0.014(4) C64 0.049(5) 0.039(5) 0.044(5) -0.014(4) -0.004(4) -0.011(4) C55 0.039(5) 0.043(5) 0.042(5) -0.023(4) -0.009(4) 0.006(4) C10 0.025(4) 0.052(5) 0.046(5) -0.025(4) -0.004(3) -0.007(4) C19 0.025(4) 0.034(5) 0.056(6) -0.015(4) -0.002(4) 0.011(4) C59 0.029(4) 0.074(7) 0.034(5) -0.019(4) -0.007(3) 0.011(5) C14 0.038(5) 0.031(5) 0.062(6) -0.014(4) 0.014(4) -0.005(4) C49 0.052(6) 0.071(7) 0.051(6) -0.043(5) 0.025(5) -0.028(5) C46 0.067(6) 0.034(5) 0.059(6) -0.034(4) 0.014(5) -0.012(5) C60 0.024(4) 0.073(7) 0.048(5) -0.028(5) -0.010(4) 0.001(4) C66 0.038(5) 0.045(5) 0.069(6) -0.036(5) 0.004(4) 0.003(4) C44 0.051(5) 0.044(5) 0.052(6) -0.027(4) -0.001(4) -0.006(4) C63 0.038(5) 0.042(5) 0.039(5) -0.019(4) 0.002(4) 0.004(4) C45 0.065(6) 0.029(5) 0.065(6) -0.023(4) -0.001(5) -0.004(5) C54 0.043(5) 0.070(7) 0.049(6) -0.032(5) -0.015(4) 0.009(5) C12 0.031(5) 0.067(7) 0.051(6) -0.018(5) 0.010(4) 0.007(5) C18 0.043(5) 0.033(5) 0.048(5) -0.002(4) -0.016(4) 0.014(4) C78 0.048(5) 0.070(7) 0.038(5) -0.031(5) 0.006(4) 0.008(5) C17 0.059(6) 0.049(6) 0.031(5) -0.010(4) -0.012(4) 0.008(5) C76 0.041(5) 0.061(6) 0.047(6) -0.014(5) -0.017(4) -0.002(5) C13 0.056(6) 0.039(5) 0.083(7) -0.022(5) 0.017(6) 0.018(5) C77 0.047(6) 0.081(8) 0.032(5) -0.024(5) -0.003(4) -0.003(5) C7 0.057(6) 0.055(6) 0.026(4) -0.011(4) -0.008(4) 0.003(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 Pt1 N2 2.062(6) . ? Pt1 N1 2.071(6) . ? Pt1 S1 2.2675(18) . ? Pt1 S2 2.2868(18) . ? Co1 C2 1.821(7) . ? Co1 C1 1.832(7) . ? Co1 P1 2.161(2) . ? Co1 P2 2.161(2) . ? Co1 P3 2.178(2) . ? P3 C33 1.825(7) . ? P3 C27 1.832(7) . ? P3 C41 1.843(7) . ? P1 C9 1.816(7) . ? P1 C3 1.828(7) . ? P1 C39 1.847(7) . ? P2 C15 1.827(7) . ? P2 C21 1.831(7) . ? P2 C40 1.831(7) . ? S2 C2 1.714(7) . ? S1 C1 1.693(7) . ? N2 C55 1.320(10) . ? N2 C52 1.347(10) . ? N1 C44 1.308(11) . ? N1 C48 1.376(10) . ? C2 C1 1.346(10) . ? C42 C43 1.516(9) . ? C42 C41 1.527(9) . ? C42 C39 1.538(9) . ? C42 C40 1.548(9) . ? C38 C37 1.372(10) . ? C38 C33 1.385(10) . ? C33 C34 1.390(9) . ? C34 C35 1.384(10) . ? C9 C14 1.329(11) . ? C9 C10 1.427(10) . ? C3 C4 1.359(11) . ? C3 C8 1.383(11) . ? C35 C36 1.361(11) . ? C21 C22 1.377(10) . ? C21 C26 1.390(10) . ? C26 C25 1.378(11) . ? C72 C73 1.388(11) . ? C72 C71 1.395(12) . ? C52 C48 1.408(12) . ? C52 C51 1.409(11) . ? C69 C70 1.390(11) . ? C69 C68 1.405(10) . ? C48 C47 1.403(12) . ? C70 C71 1.373(12) . ? C73 C68 1.374(10) . ? C68 B1 1.622(11) . ? C27 C28 1.365(10) . ? C27 C32 1.385(10) . ? C74 C79 1.378(11) . ? C74 C75 1.398(11) . ? C74 B1 1.657(11) . ? C56 C57 1.386(11) . ? C56 C61 1.406(11) . ? C56 B1 1.634(11) . ? C28 C29 1.376(11) . ? C57 C58 1.386(11) . ? C15 C20 1.384(10) . ? C15 C16 1.389(11) . ? C62 C67 1.380(10) . ? C62 C63 1.394(11) . ? C62 B1 1.652(11) . ? C8 C7 1.379(11) . ? C20 C19 1.376(11) . ? C37 C36 1.376(12) . ? C16 C17 1.399(11) . ? C47 C46 1.398(13) . ? C47 C49 1.443(13) . ? C22 C23 1.365(11) . ? C25 C24 1.368(11) . ? C24 C23 1.361(12) . ? C51 C53 1.397(14) . ? C51 C50 1.439(13) . ? C75 C76 1.387(12) . ? C4 C5 1.411(10) . ? C31 C30 1.356(12) . ? C31 C32 1.389(11) . ? C6 C5 1.348(12) . ? C6 C7 1.390(13) . ? C53 C54 1.335(14) . ? C50 C49 1.320(14) . ? C58 C59 1.370(12) . ? C61 C60 1.352(12) . ? C79 C78 1.417(11) . ? C67 C66 1.386(12) . ? C11 C10 1.356(12) . ? C11 C12 1.373(13) . ? C30 C29 1.383(11) . ? C65 C64 1.356(12) . ? C65 C66 1.381(12) . ? C64 C63 1.378(12) . ? C55 C54 1.391(11) . ? C19 C18 1.383(12) . ? C59 C60 1.363(14) . ? C14 C13 1.397(12) . ? C46 C45 1.344(13) . ? C44 C45 1.406(12) . ? C12 C13 1.341(13) . ? C18 C17 1.366(13) . ? C78 C77 1.356(13) . ? C76 C77 1.357(13) . ? 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 N2 Pt1 N1 80.8(2) . . ? N2 Pt1 S1 174.08(18) . . ? N1 Pt1 S1 94.40(18) . . ? N2 Pt1 S2 95.54(18) . . ? N1 Pt1 S2 175.83(18) . . ? S1 Pt1 S2 89.40(6) . . ? C2 Co1 C1 43.2(3) . . ? C2 Co1 P1 118.6(2) . . ? C1 Co1 P1 126.7(2) . . ? C2 Co1 P2 106.5(2) . . ? C1 Co1 P2 138.7(2) . . ? P1 Co1 P2 90.18(8) . . ? C2 Co1 P3 142.6(2) . . ? C1 Co1 P3 102.1(2) . . ? P1 Co1 P3 92.33(8) . . ? P2 Co1 P3 92.94(8) . . ? C33 P3 C27 102.9(3) . . ? C33 P3 C41 102.0(3) . . ? C27 P3 C41 106.3(3) . . ? C33 P3 Co1 116.1(2) . . ? C27 P3 Co1 116.6(2) . . ? C41 P3 Co1 111.4(2) . . ? C9 P1 C3 99.7(3) . . ? C9 P1 C39 103.3(3) . . ? C3 P1 C39 107.8(3) . . ? C9 P1 Co1 118.3(3) . . ? C3 P1 Co1 114.4(2) . . ? C39 P1 Co1 112.0(2) . . ? C15 P2 C21 97.4(3) . . ? C15 P2 C40 103.5(3) . . ? C21 P2 C40 107.0(3) . . ? C15 P2 Co1 122.7(3) . . ? C21 P2 Co1 112.0(2) . . ? C40 P2 Co1 112.3(2) . . ? C2 S2 Pt1 101.7(2) . . ? C1 S1 Pt1 102.7(3) . . ? C55 N2 C52 119.7(7) . . ? C55 N2 Pt1 128.1(5) . . ? C52 N2 Pt1 112.2(5) . . ? C44 N1 C48 119.4(7) . . ? C44 N1 Pt1 129.1(6) . . ? C48 N1 Pt1 111.4(5) . . ? C1 C2 S2 122.8(6) . . ? C1 C2 Co1 68.8(4) . . ? S2 C2 Co1 167.7(4) . . ? C2 C1 S1 123.3(6) . . ? C2 C1 Co1 67.9(4) . . ? S1 C1 Co1 167.8(5) . . ? C43 C42 C41 107.7(5) . . ? C43 C42 C39 107.2(6) . . ? C41 C42 C39 112.3(5) . . ? C43 C42 C40 107.9(6) . . ? C41 C42 C40 111.2(6) . . ? C39 C42 C40 110.2(6) . . ? C37 C38 C33 120.4(7) . . ? C38 C33 C34 119.3(7) . . ? C38 C33 P3 121.1(5) . . ? C34 C33 P3 119.6(5) . . ? C42 C39 P1 115.8(4) . . ? C35 C34 C33 119.2(7) . . ? C42 C40 P2 116.4(5) . . ? C14 C9 C10 118.1(7) . . ? C14 C9 P1 123.2(6) . . ? C10 C9 P1 118.7(6) . . ? C4 C3 C8 119.4(7) . . ? C4 C3 P1 125.0(6) . . ? C8 C3 P1 115.5(6) . . ? C42 C41 P3 116.3(4) . . ? C36 C35 C34 121.0(7) . . ? C22 C21 C26 118.8(7) . . ? C22 C21 P2 125.2(6) . . ? C26 C21 P2 115.8(6) . . ? C25 C26 C21 120.3(7) . . ? C73 C72 C71 119.8(8) . . ? N2 C52 C48 118.3(7) . . ? N2 C52 C51 121.6(8) . . ? C48 C52 C51 120.1(8) . . ? C70 C69 C68 122.3(8) . . ? N1 C48 C47 121.3(8) . . ? N1 C48 C52 117.3(7) . . ? C47 C48 C52 121.5(8) . . ? C71 C70 C69 120.3(8) . . ? C68 C73 C72 123.2(8) . . ? C73 C68 C69 115.6(7) . . ? C73 C68 B1 124.9(7) . . ? C69 C68 B1 119.4(7) . . ? C28 C27 C32 118.1(7) . . ? C28 C27 P3 117.9(6) . . ? C32 C27 P3 123.9(6) . . ? C79 C74 C75 115.8(8) . . ? C79 C74 B1 123.8(7) . . ? C75 C74 B1 120.4(7) . . ? C57 C56 C61 113.6(7) . . ? C57 C56 B1 122.0(7) . . ? C61 C56 B1 124.3(8) . . ? C27 C28 C29 121.9(7) . . ? C58 C57 C56 123.2(8) . . ? C20 C15 C16 119.0(7) . . ? C20 C15 P2 119.4(6) . . ? C16 C15 P2 121.6(6) . . ? C67 C62 C63 113.8(7) . . ? C67 C62 B1 125.2(7) . . ? C63 C62 B1 120.9(6) . . ? C7 C8 C3 121.3(8) . . ? C19 C20 C15 121.8(7) . . ? C38 C37 C36 120.2(8) . . ? C15 C16 C17 119.0(8) . . ? C46 C47 C48 117.5(8) . . ? C46 C47 C49 125.2(9) . . ? C48 C47 C49 117.3(9) . . ? C23 C22 C21 119.7(8) . . ? C24 C25 C26 120.0(8) . . ? C35 C36 C37 119.9(8) . . ? C23 C24 C25 119.3(8) . . ? C53 C51 C52 116.9(8) . . ? C53 C51 C50 126.1(8) . . ? C52 C51 C50 117.0(9) . . ? C76 C75 C74 122.8(9) . . ? C3 C4 C5 119.5(8) . . ? C30 C31 C32 120.0(8) . . ? C22 C23 C24 121.8(8) . . ? C68 B1 C56 108.1(6) . . ? C68 B1 C62 108.7(6) . . ? C56 B1 C62 112.1(6) . . ? C68 B1 C74 111.2(6) . . ? C56 B1 C74 109.4(6) . . ? C62 B1 C74 107.3(6) . . ? C5 C6 C7 120.1(8) . . ? C27 C32 C31 120.6(8) . . ? C54 C53 C51 120.3(8) . . ? C49 C50 C51 122.9(9) . . ? C6 C5 C4 120.8(8) . . ? C59 C58 C57 120.3(9) . . ? C60 C61 C56 123.3(9) . . ? C74 C79 C78 121.5(8) . . ? C70 C71 C72 118.7(7) . . ? C62 C67 C66 123.8(8) . . ? C10 C11 C12 119.5(9) . . ? C31 C30 C29 120.2(7) . . ? C64 C65 C66 118.1(8) . . ? C28 C29 C30 119.1(8) . . ? C65 C64 C63 120.9(8) . . ? N2 C55 C54 121.4(8) . . ? C11 C10 C9 120.3(8) . . ? C20 C19 C18 119.1(8) . . ? C60 C59 C58 118.0(8) . . ? C9 C14 C13 121.5(9) . . ? C50 C49 C47 121.1(9) . . ? C45 C46 C47 120.3(8) . . ? C61 C60 C59 121.5(9) . . ? C65 C66 C67 119.9(8) . . ? N1 C44 C45 121.7(9) . . ? C64 C63 C62 123.4(8) . . ? C46 C45 C44 119.8(9) . . ? C53 C54 C55 120.2(9) . . ? C13 C12 C11 121.1(8) . . ? C17 C18 C19 120.1(8) . . ? C77 C78 C79 119.8(8) . . ? C18 C17 C16 121.1(8) . . ? C77 C76 C75 119.4(9) . . ? C12 C13 C14 119.4(9) . . ? C78 C77 C76 120.6(8) . . ? C8 C7 C6 118.9(8) . . ? _diffrn_measured_fraction_theta_max 0.857 _diffrn_reflns_theta_full 72.59 _diffrn_measured_fraction_theta_full 0.857 _refine_diff_density_max 3.316 _refine_diff_density_min -2.008 _refine_diff_density_rms 0.173 # Attachment 'comp_7-BPh4.cif' data_sad5 _database_code_depnum_ccdc_archive 'CCDC 740236' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C95 H83 B Co O0.50 P5 Pt S2' _chemical_formula_weight 1716.41 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' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 12.3583(3) _cell_length_b 19.5334(5) _cell_length_c 34.3595(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.1190(10) _cell_angle_gamma 90.00 _cell_volume 8272.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3496 _exptl_absorpt_coefficient_mu 2.083 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6807 _exptl_absorpt_correction_T_max 0.8679 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.788688 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65527 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 24.85 _reflns_number_total 14303 _reflns_number_gt 11346 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2(Bruker AXS, 2007)' _computing_cell_refinement 'APEX2(Bruker AXS, 2007)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2007 )' _computing_structure_solution ; SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_structure_refinement ; SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One of the phenyl rings in the ancillary ligand (C47-C52) was restrained with the FLAT and DANG command. The solvent thf is disordered on two positions and is described with 50% occupancy per asymmetric unit, isotropically refined without hydrogen atoms attched. ; _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^)+(0.0619P)^2^+19.1407P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14303 _refine_ls_number_parameters 949 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1251 _refine_ls_wR_factor_gt 0.1155 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.7200(6) 0.0748(4) 0.3634(2) 0.0474(16) Uani 1 1 d . . . C1 C 0.2374(5) 0.0975(3) 0.12053(15) 0.0413(13) Uani 1 1 d . . . C2 C 0.1313(5) 0.1045(3) 0.11497(15) 0.0412(13) Uani 1 1 d . . . C3 C 0.2693(5) 0.2491(3) -0.04170(19) 0.0587(17) Uani 1 1 d . . . H3A H 0.2689 0.2975 -0.0331 0.070 Uiso 1 1 calc R . . H3B H 0.3108 0.2462 -0.0652 0.070 Uiso 1 1 calc R . . C4 C 0.1533(5) 0.2251(3) -0.05157(16) 0.0466(14) Uani 1 1 d . . . H4A H 0.1539 0.1818 -0.0665 0.056 Uiso 1 1 calc R . . H4B H 0.1136 0.2598 -0.0680 0.056 Uiso 1 1 calc R . . C5 C 0.3661(5) 0.1609(3) 0.22022(18) 0.0465(14) Uani 1 1 d . . . C6 C 0.4202(5) 0.1852(3) 0.1896(2) 0.0553(16) Uani 1 1 d . . . H6 H 0.4146 0.1618 0.1653 0.066 Uiso 1 1 calc R . . C7 C 0.4828(6) 0.2438(4) 0.1940(2) 0.076(2) Uani 1 1 d . . . H7 H 0.5178 0.2616 0.1724 0.091 Uiso 1 1 calc R . . C8 C 0.4943(7) 0.2763(4) 0.2296(3) 0.098(3) Uani 1 1 d . . . H8 H 0.5381 0.3161 0.2327 0.118 Uiso 1 1 calc R . . C9 C 0.4422(8) 0.2511(5) 0.2607(3) 0.109(4) Uani 1 1 d . . . H9 H 0.4511 0.2728 0.2855 0.131 Uiso 1 1 calc R . . C10 C 0.3775(7) 0.1944(4) 0.2556(2) 0.083(3) Uani 1 1 d . . . H10 H 0.3399 0.1778 0.2769 0.100 Uiso 1 1 calc R . . C11 C 0.4092(4) 0.0236(3) 0.21066(16) 0.0375(12) Uani 1 1 d . . . C12 C 0.4799(5) 0.0169(3) 0.24389(18) 0.0503(15) Uani 1 1 d . . . H12 H 0.4656 0.0405 0.2671 0.060 Uiso 1 1 calc R . . C13 C 0.5705(5) -0.0237(4) 0.2430(2) 0.066(2) Uani 1 1 d . . . H13 H 0.6187 -0.0280 0.2657 0.079 Uiso 1 1 calc R . . C14 C 0.5919(5) -0.0585(4) 0.2094(2) 0.066(2) Uani 1 1 d . . . H14 H 0.6540 -0.0870 0.2090 0.079 Uiso 1 1 calc R . . C15 C 0.5229(5) -0.0514(3) 0.1767(2) 0.0604(17) Uani 1 1 d . . . H15 H 0.5379 -0.0747 0.1534 0.073 Uiso 1 1 calc R . . C16 C 0.4318(4) -0.0107(3) 0.17726(17) 0.0455(14) Uani 1 1 d . . . H16 H 0.3844 -0.0063 0.1544 0.055 Uiso 1 1 calc R . . C17 C 0.1819(4) -0.0866(3) 0.18566(19) 0.0475(15) Uani 1 1 d . . . C18 C 0.2377(6) -0.1176(3) 0.2177(2) 0.072(2) Uani 1 1 d . . . H18 H 0.2310 -0.1007 0.2433 0.086 Uiso 1 1 calc R . . C19 C 0.3038(7) -0.1742(4) 0.2114(3) 0.091(3) Uani 1 1 d . . . H19 H 0.3443 -0.1942 0.2331 0.110 Uiso 1 1 calc R . . C20 C 0.3118(6) -0.2015(4) 0.1755(3) 0.076(2) Uani 1 1 d . . . H20 H 0.3546 -0.2412 0.1724 0.091 Uiso 1 1 calc R . . C21 C 0.2576(5) -0.1711(3) 0.1433(3) 0.068(2) Uani 1 1 d . . . H21 H 0.2639 -0.1892 0.1179 0.082 Uiso 1 1 calc R . . C22 C 0.1928(5) -0.1128(3) 0.1488(2) 0.0536(16) Uani 1 1 d . . . H22 H 0.1562 -0.0913 0.1268 0.064 Uiso 1 1 calc R . . C23 C -0.0304(4) -0.0449(3) 0.16469(16) 0.0410(13) Uani 1 1 d . . . C24 C -0.0754(4) -0.1030(3) 0.1795(2) 0.0506(15) Uani 1 1 d . . . H24 H -0.0420 -0.1244 0.2021 0.061 Uiso 1 1 calc R . . C25 C -0.1700(5) -0.1306(4) 0.1611(2) 0.0629(19) Uani 1 1 d . . . H25 H -0.2009 -0.1709 0.1711 0.076 Uiso 1 1 calc R . . C26 C -0.2177(5) -0.1000(4) 0.1291(2) 0.072(2) Uani 1 1 d . . . H26 H -0.2824 -0.1187 0.1168 0.086 Uiso 1 1 calc R . . C27 C -0.1732(5) -0.0418(4) 0.1142(2) 0.070(2) Uani 1 1 d . . . H27 H -0.2078 -0.0204 0.0918 0.084 Uiso 1 1 calc R . . C28 C -0.0783(5) -0.0141(3) 0.13153(18) 0.0521(16) Uani 1 1 d . . . H28 H -0.0466 0.0253 0.1208 0.063 Uiso 1 1 calc R . . C29 C -0.0894(5) 0.1357(3) 0.18053(17) 0.0464(14) Uani 1 1 d . . . C30 C -0.1651(5) 0.1062(4) 0.2028(2) 0.0635(18) Uani 1 1 d . . . H30 H -0.1427 0.0892 0.2280 0.076 Uiso 1 1 calc R . . C31 C -0.2726(6) 0.1008(4) 0.1894(3) 0.082(2) Uani 1 1 d . . . H31 H -0.3233 0.0809 0.2056 0.098 Uiso 1 1 calc R . . C32 C -0.3055(6) 0.1234(6) 0.1540(3) 0.101(3) Uani 1 1 d . . . H32 H -0.3796 0.1193 0.1448 0.121 Uiso 1 1 calc R . . C33 C -0.2330(7) 0.1521(6) 0.1311(3) 0.109(4) Uani 1 1 d . . . H33 H -0.2563 0.1676 0.1057 0.131 Uiso 1 1 calc R . . C34 C -0.1244(6) 0.1592(4) 0.1447(2) 0.076(2) Uani 1 1 d . . . H34 H -0.0747 0.1806 0.1287 0.091 Uiso 1 1 calc R . . C35 C 0.0784(5) 0.2334(3) 0.18848(17) 0.0455(14) Uani 1 1 d . . . C36 C 0.0053(7) 0.2809(4) 0.2016(2) 0.072(2) Uani 1 1 d . . . H36 H -0.0566 0.2656 0.2140 0.086 Uiso 1 1 calc R . . C37 C 0.0222(9) 0.3496(4) 0.1969(3) 0.097(3) Uani 1 1 d . . . H37 H -0.0296 0.3815 0.2051 0.116 Uiso 1 1 calc R . . C38 C 0.1124(8) 0.3728(4) 0.1805(3) 0.092(3) Uani 1 1 d . . . H38 H 0.1256 0.4206 0.1784 0.110 Uiso 1 1 calc R . . C39 C 0.1819(7) 0.3276(4) 0.1675(3) 0.104(4) Uani 1 1 d . . . H39 H 0.2445 0.3435 0.1557 0.125 Uiso 1 1 calc R . . C40 C 0.1651(5) 0.2577(3) 0.1706(2) 0.071(2) Uani 1 1 d . . . H40 H 0.2145 0.2266 0.1602 0.085 Uiso 1 1 calc R . . C41 C 0.3876(5) 0.1220(4) -0.02694(18) 0.0551(17) Uani 1 1 d . . . C42 C 0.4678(6) 0.1289(6) -0.0541(2) 0.084(3) Uani 1 1 d . . . H42 H 0.4950 0.1727 -0.0604 0.101 Uiso 1 1 calc R . . C43 C 0.5058(7) 0.0701(8) -0.0714(3) 0.114(5) Uani 1 1 d . . . H43 H 0.5618 0.0739 -0.0888 0.137 Uiso 1 1 calc R . . C44 C 0.4645(10) 0.0071(7) -0.0639(3) 0.121(5) Uani 1 1 d . . . H44 H 0.4893 -0.0320 -0.0770 0.145 Uiso 1 1 calc R . . C45 C 0.3882(8) 0.0003(5) -0.0378(2) 0.088(3) Uani 1 1 d . . . H45 H 0.3614 -0.0439 -0.0320 0.106 Uiso 1 1 calc R . . C46 C 0.3492(6) 0.0571(4) -0.01963(19) 0.0602(18) Uani 1 1 d . . . H46 H 0.2947 0.0516 -0.0017 0.072 Uiso 1 1 calc R . . C47 C 0.4612(5) 0.2422(4) 0.0116(2) 0.091(3) Uani 1 1 d D . . C48 C 0.4932(8) 0.3000(5) -0.0103(2) 0.158(6) Uani 1 1 d D . . H48 H 0.4475 0.3174 -0.0314 0.189 Uiso 1 1 calc R . . C49 C 0.5887(9) 0.3288(4) -0.0003(3) 0.182(7) Uani 1 1 d D . . H49 H 0.6104 0.3672 -0.0148 0.218 Uiso 1 1 calc R . . C50 C 0.6568(6) 0.3056(6) 0.0298(3) 0.157(6) Uani 1 1 d D . . H50 H 0.7246 0.3274 0.0360 0.189 Uiso 1 1 calc R . . C51 C 0.6257(7) 0.2497(7) 0.0511(3) 0.268(14) Uani 1 1 d D . . H51 H 0.6710 0.2327 0.0724 0.322 Uiso 1 1 calc R . . C52 C 0.5276(7) 0.2196(5) 0.0405(3) 0.136(5) Uani 1 1 d D . . H52 H 0.5066 0.1806 0.0548 0.163 Uiso 1 1 calc R . . C53 C -0.0305(5) 0.1580(3) -0.02013(16) 0.0442(14) Uani 1 1 d . . . C54 C -0.0126(6) 0.0921(3) -0.03241(19) 0.0582(17) Uani 1 1 d . . . H54 H 0.0598 0.0766 -0.0339 0.070 Uiso 1 1 calc R . . C55 C -0.0976(7) 0.0482(4) -0.0426(2) 0.074(2) Uani 1 1 d . . . H55 H -0.0837 0.0031 -0.0512 0.089 Uiso 1 1 calc R . . C56 C -0.2002(7) 0.0699(4) -0.0401(3) 0.083(2) Uani 1 1 d . . . H56 H -0.2588 0.0402 -0.0479 0.099 Uiso 1 1 calc R . . C57 C -0.2215(7) 0.1346(5) -0.0266(3) 0.097(3) Uani 1 1 d . . . H57 H -0.2940 0.1489 -0.0239 0.117 Uiso 1 1 calc R . . C58 C -0.1355(6) 0.1786(4) -0.0170(3) 0.073(2) Uani 1 1 d . . . H58 H -0.1496 0.2235 -0.0081 0.087 Uiso 1 1 calc R . . C59 C 0.0315(5) 0.2940(3) 0.00684(17) 0.0478(14) Uani 1 1 d . . . C60 C -0.0248(6) 0.3362(3) -0.0207(2) 0.0630(18) Uani 1 1 d . . . H60 H -0.0318 0.3233 -0.0474 0.076 Uiso 1 1 calc R . . C61 C -0.0706(7) 0.3974(4) -0.0086(3) 0.079(2) Uani 1 1 d . . . H61 H -0.1081 0.4264 -0.0273 0.095 Uiso 1 1 calc R . . C62 C -0.0617(7) 0.4158(4) 0.0298(3) 0.085(3) Uani 1 1 d . . . H62 H -0.0939 0.4571 0.0378 0.102 Uiso 1 1 calc R . . C63 C -0.0072(7) 0.3754(4) 0.0566(2) 0.076(2) Uani 1 1 d . . . H63 H -0.0002 0.3892 0.0832 0.092 Uiso 1 1 calc R . . C64 C 0.0388(6) 0.3138(3) 0.0456(2) 0.0588(17) Uani 1 1 d . . . H64 H 0.0752 0.2853 0.0647 0.071 Uiso 1 1 calc R . . C65 C 0.7598(6) 0.0664(3) 0.4100(2) 0.0577(17) Uani 1 1 d . . . C66 C 0.6967(6) 0.0789(3) 0.44047(18) 0.0566(17) Uani 1 1 d . . . H66 H 0.6254 0.0962 0.4348 0.068 Uiso 1 1 calc R . . C67 C 0.7326(7) 0.0672(3) 0.4796(2) 0.070(2) Uani 1 1 d . . . H67 H 0.6854 0.0758 0.4997 0.084 Uiso 1 1 calc R . . C68 C 0.8329(10) 0.0441(5) 0.4887(3) 0.113(4) Uani 1 1 d . . . H68 H 0.8587 0.0378 0.5152 0.136 Uiso 1 1 calc R . . C69 C 0.8965(10) 0.0299(7) 0.4599(3) 0.148(6) Uani 1 1 d . . . H69 H 0.9668 0.0115 0.4661 0.177 Uiso 1 1 calc R . . C70 C 0.8627(8) 0.0414(6) 0.4213(3) 0.117(4) Uani 1 1 d . . . H70 H 0.9113 0.0319 0.4018 0.140 Uiso 1 1 calc R . . C71 C 0.7441(5) -0.0003(3) 0.34386(17) 0.0446(14) Uani 1 1 d . . . C72 C 0.7156(6) -0.0603(4) 0.3628(2) 0.0676(19) Uani 1 1 d . . . H72 H 0.6833 -0.0567 0.3869 0.081 Uiso 1 1 calc R . . C73 C 0.7328(6) -0.1250(3) 0.3475(2) 0.071(2) Uani 1 1 d . . . H73 H 0.7098 -0.1644 0.3609 0.085 Uiso 1 1 calc R . . C74 C 0.7826(5) -0.1325(3) 0.3134(2) 0.0603(18) Uani 1 1 d . . . H74 H 0.7949 -0.1766 0.3030 0.072 Uiso 1 1 calc R . . C75 C 0.8141(4) -0.0749(3) 0.2948(2) 0.0525(16) Uani 1 1 d . . . H75 H 0.8498 -0.0791 0.2713 0.063 Uiso 1 1 calc R . . C76 C 0.7947(4) -0.0098(3) 0.30970(17) 0.0444(14) Uani 1 1 d . . . H76 H 0.8171 0.0293 0.2959 0.053 Uiso 1 1 calc R . . C77 C 0.7839(5) 0.1369(3) 0.3425(2) 0.0556(16) Uani 1 1 d . . . C78 C 0.8677(6) 0.1767(4) 0.3611(3) 0.081(3) Uani 1 1 d . . . H78 H 0.8920 0.1658 0.3872 0.097 Uiso 1 1 calc R . . C79 C 0.9156(8) 0.2301(5) 0.3433(4) 0.105(4) Uani 1 1 d . . . H79 H 0.9721 0.2551 0.3571 0.127 Uiso 1 1 calc R . . C80 C 0.8839(8) 0.2476(4) 0.3067(4) 0.097(3) Uani 1 1 d . . . H80 H 0.9174 0.2850 0.2947 0.116 Uiso 1 1 calc R . . C81 C 0.8026(7) 0.2114(4) 0.2865(3) 0.083(3) Uani 1 1 d . . . H81 H 0.7796 0.2235 0.2604 0.100 Uiso 1 1 calc R . . C82 C 0.7543(6) 0.1568(3) 0.3048(2) 0.0610(18) Uani 1 1 d . . . H82 H 0.6983 0.1321 0.2905 0.073 Uiso 1 1 calc R . . C83 C 0.5899(5) 0.0949(3) 0.36054(15) 0.0427(13) Uani 1 1 d . . . C84 C 0.5568(5) 0.1635(3) 0.36267(17) 0.0495(15) Uani 1 1 d . . . H84 H 0.6107 0.1982 0.3630 0.059 Uiso 1 1 calc R . . C85 C 0.4496(6) 0.1830(4) 0.36431(19) 0.0611(18) Uani 1 1 d . . . H85 H 0.4315 0.2300 0.3662 0.073 Uiso 1 1 calc R . . C86 C 0.3698(6) 0.1345(4) 0.3632(2) 0.0629(18) Uani 1 1 d . . . H86 H 0.2960 0.1476 0.3641 0.075 Uiso 1 1 calc R . . C87 C 0.3974(6) 0.0666(4) 0.3608(2) 0.0653(19) Uani 1 1 d . . . H87 H 0.3425 0.0325 0.3602 0.078 Uiso 1 1 calc R . . C88 C 0.5057(5) 0.0476(3) 0.35912(17) 0.0516(15) Uani 1 1 d . . . H88 H 0.5226 0.0004 0.3569 0.062 Uiso 1 1 calc R . . C93 C 0.2412(4) 0.0578(3) 0.26022(15) 0.0453(14) Uani 1 1 d . . . H93A H 0.2668 0.0112 0.2674 0.054 Uiso 1 1 calc R . . H93B H 0.2739 0.0897 0.2802 0.054 Uiso 1 1 calc R . . C94 C 0.0628(5) -0.0014(3) 0.24016(15) 0.0449(14) Uani 1 1 d . . . H94A H -0.0168 0.0031 0.2407 0.054 Uiso 1 1 calc R . . H94B H 0.0845 -0.0439 0.2544 0.054 Uiso 1 1 calc R . . C95 C 0.0692(5) 0.1294(3) 0.24775(16) 0.0468(14) Uani 1 1 d . . . H95A H 0.1161 0.1662 0.2594 0.056 Uiso 1 1 calc R . . H95B H -0.0033 0.1348 0.2579 0.056 Uiso 1 1 calc R . . C96 C 0.1166(4) 0.0598(3) 0.26213(15) 0.0456(14) Uani 1 1 d . . . C97 C 0.0934(5) 0.0524(4) 0.30563(16) 0.064(2) Uani 1 1 d . . . H97A H 0.0153 0.0462 0.3077 0.096 Uiso 1 1 calc R . . H97B H 0.1176 0.0938 0.3198 0.096 Uiso 1 1 calc R . . H97C H 0.1325 0.0127 0.3169 0.096 Uiso 1 1 calc R . . C101 C 0.2175(12) 0.9216(8) 0.4087(4) 0.067(4) Uiso 0.50 1 d P . . C102 C 0.1597(14) 0.8553(9) 0.4197(5) 0.079(4) Uiso 0.50 1 d P . . C103 C 0.0564(14) 0.9135(9) 0.3713(5) 0.086(5) Uiso 0.50 1 d P . . C104 C 0.0502(17) 0.8648(11) 0.4036(6) 0.107(6) Uiso 0.50 1 d P . . Co Co 0.16580(6) 0.07922(3) 0.165182(19) 0.03313(17) Uani 1 1 d . . . O101 O 0.1647(7) 0.9416(5) 0.3733(3) 0.059(2) Uiso 0.50 1 d P . . P1 P 0.29276(11) 0.08020(7) 0.21266(4) 0.0351(3) Uani 1 1 d . . . P2 P 0.09614(11) -0.01126(7) 0.18852(4) 0.0378(3) Uani 1 1 d . . . P3 P 0.05526(11) 0.14239(7) 0.19463(4) 0.0364(3) Uani 1 1 d . . . P4 P 0.33459(13) 0.19576(8) -0.00282(5) 0.0484(4) Uani 1 1 d . . . P5 P 0.08523(12) 0.21201(7) -0.00686(4) 0.0384(3) Uani 1 1 d . . . Pt1 Pt 0.206805(19) 0.167194(11) 0.037980(6) 0.04091(9) Uani 1 1 d . . . S1 S 0.32756(13) 0.12183(9) 0.08767(4) 0.0520(4) Uani 1 1 d . . . S2 S 0.06181(13) 0.13658(8) 0.07446(4) 0.0484(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.052(4) 0.043(4) 0.046(4) -0.009(3) -0.007(3) 0.003(3) C1 0.056(4) 0.036(3) 0.033(3) 0.004(2) 0.008(3) 0.016(3) C2 0.058(4) 0.036(3) 0.031(3) 0.004(2) 0.009(3) 0.011(3) C3 0.066(4) 0.051(4) 0.061(4) 0.026(3) 0.014(3) 0.010(3) C4 0.059(4) 0.045(3) 0.037(3) 0.013(3) 0.010(3) 0.014(3) C5 0.045(3) 0.034(3) 0.062(4) -0.006(3) 0.017(3) -0.009(3) C6 0.055(4) 0.054(4) 0.058(4) 0.001(3) 0.013(3) -0.013(3) C7 0.073(5) 0.066(5) 0.093(6) -0.001(4) 0.036(4) -0.030(4) C8 0.111(7) 0.072(5) 0.119(7) -0.042(5) 0.056(6) -0.052(5) C9 0.146(9) 0.087(6) 0.104(7) -0.045(5) 0.062(6) -0.066(6) C10 0.105(6) 0.071(5) 0.078(5) -0.027(4) 0.041(5) -0.055(5) C11 0.034(3) 0.036(3) 0.041(3) 0.006(2) -0.004(2) -0.007(2) C12 0.045(3) 0.057(4) 0.047(3) 0.002(3) -0.006(3) -0.006(3) C13 0.042(4) 0.075(5) 0.077(5) 0.016(4) -0.020(3) -0.007(3) C14 0.047(4) 0.053(4) 0.096(6) 0.008(4) -0.011(4) 0.007(3) C15 0.049(4) 0.058(4) 0.072(5) -0.009(3) -0.005(3) 0.012(3) C16 0.040(3) 0.044(3) 0.052(4) 0.000(3) -0.005(3) -0.001(3) C17 0.033(3) 0.036(3) 0.072(4) 0.011(3) -0.013(3) -0.004(2) C18 0.079(5) 0.040(4) 0.090(5) 0.015(4) -0.040(4) -0.001(3) C19 0.077(6) 0.054(5) 0.135(9) 0.018(5) -0.046(6) 0.013(4) C20 0.048(4) 0.041(4) 0.136(8) 0.006(5) -0.015(5) 0.007(3) C21 0.042(4) 0.049(4) 0.115(6) -0.007(4) 0.010(4) -0.004(3) C22 0.041(3) 0.045(4) 0.075(5) 0.006(3) 0.002(3) 0.004(3) C23 0.035(3) 0.040(3) 0.047(3) -0.010(3) -0.007(2) 0.002(2) C24 0.033(3) 0.041(3) 0.077(4) -0.003(3) -0.003(3) -0.003(3) C25 0.034(3) 0.057(4) 0.098(6) -0.022(4) 0.004(4) -0.005(3) C26 0.032(3) 0.092(6) 0.090(6) -0.048(5) -0.005(4) -0.007(4) C27 0.049(4) 0.095(6) 0.063(4) -0.028(4) -0.021(3) 0.025(4) C28 0.051(4) 0.054(4) 0.048(3) -0.008(3) -0.015(3) 0.006(3) C29 0.039(3) 0.058(4) 0.042(3) -0.013(3) 0.004(3) 0.003(3) C30 0.044(4) 0.063(4) 0.083(5) 0.003(4) 0.011(3) -0.004(3) C31 0.046(4) 0.085(6) 0.116(7) -0.011(5) 0.015(5) -0.013(4) C32 0.037(4) 0.143(9) 0.120(8) -0.038(7) -0.010(5) -0.004(5) C33 0.060(5) 0.192(12) 0.072(6) -0.009(6) -0.021(5) 0.020(6) C34 0.053(4) 0.122(7) 0.052(4) -0.003(4) 0.002(3) 0.017(4) C35 0.045(3) 0.039(3) 0.052(3) -0.003(3) -0.001(3) 0.006(3) C36 0.086(5) 0.056(4) 0.073(5) -0.010(4) 0.012(4) 0.010(4) C37 0.124(8) 0.046(5) 0.115(8) -0.017(5) -0.021(7) 0.027(5) C38 0.095(7) 0.038(4) 0.134(8) 0.009(5) -0.045(6) 0.004(5) C39 0.071(5) 0.058(5) 0.185(11) 0.041(6) 0.013(6) -0.008(4) C40 0.054(4) 0.035(3) 0.127(7) 0.020(4) 0.021(4) 0.003(3) C41 0.041(3) 0.079(5) 0.045(3) 0.006(3) 0.004(3) 0.021(3) C42 0.050(4) 0.154(9) 0.049(4) 0.003(5) 0.007(3) 0.006(5) C43 0.047(5) 0.233(14) 0.061(5) -0.046(8) 0.003(4) 0.058(7) C44 0.110(9) 0.177(12) 0.069(7) -0.056(8) -0.034(6) 0.092(9) C45 0.122(7) 0.088(6) 0.051(4) -0.017(4) -0.016(5) 0.064(5) C46 0.070(4) 0.061(4) 0.050(4) -0.001(3) -0.001(3) 0.034(4) C47 0.088(6) 0.070(5) 0.113(7) 0.023(5) -0.013(5) -0.005(5) C48 0.187(13) 0.149(11) 0.134(10) 0.017(9) -0.005(9) -0.105(10) C49 0.150(13) 0.168(14) 0.223(18) 0.008(12) -0.009(12) -0.090(11) C50 0.088(8) 0.199(16) 0.185(15) -0.041(12) 0.011(9) -0.041(10) C51 0.142(12) 0.38(3) 0.27(2) 0.23(2) -0.110(13) -0.167(16) C52 0.095(7) 0.145(10) 0.160(10) 0.084(9) -0.050(7) -0.047(7) C53 0.057(4) 0.038(3) 0.039(3) 0.009(2) 0.011(3) 0.010(3) C54 0.070(4) 0.050(4) 0.054(4) -0.004(3) 0.000(3) 0.006(3) C55 0.100(6) 0.049(4) 0.072(5) -0.004(4) -0.006(4) -0.002(4) C56 0.080(6) 0.060(5) 0.106(7) 0.024(5) -0.005(5) -0.014(4) C57 0.063(5) 0.072(6) 0.158(9) 0.016(6) 0.021(5) -0.006(4) C58 0.059(4) 0.048(4) 0.112(7) 0.010(4) 0.019(4) 0.009(3) C59 0.063(4) 0.037(3) 0.045(3) 0.002(3) 0.009(3) 0.015(3) C60 0.083(5) 0.041(4) 0.065(4) 0.008(3) 0.005(4) 0.016(3) C61 0.090(6) 0.043(4) 0.105(7) 0.019(4) 0.011(5) 0.029(4) C62 0.110(7) 0.045(4) 0.101(7) -0.016(4) 0.020(5) 0.028(4) C63 0.100(6) 0.057(5) 0.074(5) -0.017(4) 0.020(4) 0.026(4) C64 0.080(5) 0.042(4) 0.056(4) -0.004(3) 0.014(3) 0.017(3) C65 0.067(4) 0.043(4) 0.059(4) -0.011(3) -0.021(3) 0.007(3) C66 0.087(5) 0.032(3) 0.048(4) -0.001(3) -0.017(3) -0.003(3) C67 0.120(7) 0.036(4) 0.049(4) -0.004(3) -0.019(4) -0.001(4) C68 0.172(10) 0.089(6) 0.067(6) -0.019(5) -0.067(7) 0.055(7) C69 0.148(10) 0.197(13) 0.087(7) -0.036(8) -0.059(7) 0.105(10) C70 0.098(7) 0.160(10) 0.085(6) -0.036(6) -0.039(5) 0.060(7) C71 0.043(3) 0.039(3) 0.050(3) -0.003(3) -0.010(3) -0.001(3) C72 0.076(5) 0.056(4) 0.072(5) -0.001(4) 0.013(4) 0.005(4) C73 0.070(5) 0.037(4) 0.105(6) 0.001(4) 0.006(4) 0.004(3) C74 0.038(3) 0.048(4) 0.095(5) -0.018(4) 0.000(3) 0.005(3) C75 0.031(3) 0.059(4) 0.068(4) -0.014(3) 0.004(3) 0.008(3) C76 0.028(3) 0.047(3) 0.056(4) -0.005(3) -0.005(3) 0.004(2) C77 0.053(4) 0.042(3) 0.072(5) -0.014(3) 0.007(3) 0.000(3) C78 0.063(5) 0.079(6) 0.102(6) -0.045(5) 0.025(4) -0.020(4) C79 0.094(7) 0.076(6) 0.155(10) -0.060(7) 0.067(7) -0.045(5) C80 0.109(7) 0.043(4) 0.149(9) -0.022(6) 0.081(7) -0.013(5) C81 0.094(6) 0.049(5) 0.112(7) 0.005(4) 0.053(5) 0.016(4) C82 0.066(4) 0.041(4) 0.078(5) -0.001(3) 0.022(4) 0.002(3) C83 0.054(3) 0.045(3) 0.028(3) -0.008(2) -0.005(2) -0.001(3) C84 0.056(4) 0.048(4) 0.042(3) -0.006(3) -0.006(3) 0.000(3) C85 0.070(5) 0.054(4) 0.057(4) -0.003(3) -0.015(3) 0.019(4) C86 0.052(4) 0.074(5) 0.060(4) -0.010(4) -0.014(3) 0.015(4) C87 0.057(4) 0.081(5) 0.057(4) -0.014(4) -0.008(3) -0.013(4) C88 0.055(4) 0.049(4) 0.050(4) -0.010(3) -0.003(3) -0.001(3) C93 0.043(3) 0.059(4) 0.033(3) 0.005(3) 0.002(2) -0.016(3) C94 0.042(3) 0.053(4) 0.039(3) 0.017(3) -0.001(2) -0.015(3) C95 0.047(3) 0.054(4) 0.041(3) -0.009(3) 0.009(3) -0.012(3) C96 0.040(3) 0.067(4) 0.029(3) 0.005(3) 0.000(2) -0.010(3) C97 0.047(4) 0.115(6) 0.030(3) 0.012(3) 0.003(3) -0.022(4) Co 0.0392(4) 0.0332(4) 0.0273(3) 0.0048(3) 0.0040(3) 0.0044(3) P1 0.0366(7) 0.0347(7) 0.0341(7) 0.0030(6) 0.0044(6) -0.0055(6) P2 0.0381(8) 0.0341(7) 0.0395(8) 0.0069(6) -0.0082(6) -0.0036(6) P3 0.0365(7) 0.0383(8) 0.0349(7) -0.0008(6) 0.0065(6) -0.0012(6) P4 0.0547(9) 0.0417(9) 0.0490(9) 0.0116(7) 0.0041(7) 0.0042(7) P5 0.0545(9) 0.0312(7) 0.0303(7) 0.0053(6) 0.0084(6) 0.0126(6) Pt1 0.05752(15) 0.03485(13) 0.03114(12) 0.00629(9) 0.00850(9) 0.01503(10) S1 0.0501(9) 0.0688(11) 0.0387(8) 0.0135(7) 0.0141(7) 0.0229(8) S2 0.0552(9) 0.0584(9) 0.0317(7) 0.0114(7) 0.0040(6) 0.0146(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 C77 1.639(10) . ? B1 C71 1.648(9) . ? B1 C65 1.649(9) . ? B1 C83 1.651(9) . ? C1 C2 1.319(8) . ? C1 S1 1.709(6) . ? C1 Co 1.860(5) . ? C2 S2 1.702(5) . ? C2 Co 1.815(5) . ? C3 C4 1.522(9) . ? C3 P4 1.835(6) . ? C4 P5 1.822(5) . ? C5 C6 1.372(8) . ? C5 C10 1.380(9) . ? C5 P1 1.827(5) . ? C6 C7 1.384(9) . ? C7 C8 1.377(11) . ? C8 C9 1.378(11) . ? C9 C10 1.369(10) . ? C11 C16 1.374(8) . ? C11 C12 1.393(8) . ? C11 P1 1.820(6) . ? C12 C13 1.374(9) . ? C13 C14 1.382(10) . ? C14 C15 1.366(9) . ? C15 C16 1.380(8) . ? C17 C22 1.382(9) . ? C17 C18 1.393(8) . ? C17 P2 1.821(6) . ? C18 C19 1.400(11) . ? C19 C20 1.354(12) . ? C20 C21 1.384(11) . ? C21 C22 1.412(9) . ? C23 C24 1.378(8) . ? C23 C28 1.382(8) . ? C23 P2 1.834(5) . ? C24 C25 1.397(8) . ? C25 C26 1.349(11) . ? C26 C27 1.379(11) . ? C27 C28 1.386(9) . ? C29 C34 1.355(9) . ? C29 C30 1.377(9) . ? C29 P3 1.823(6) . ? C30 C31 1.377(10) . ? C31 C32 1.330(13) . ? C32 C33 1.356(14) . ? C33 C34 1.396(11) . ? C35 C40 1.357(9) . ? C35 C36 1.393(9) . ? C35 P3 1.816(6) . ? C36 C37 1.369(11) . ? C37 C38 1.363(13) . ? C38 C39 1.333(13) . ? C39 C40 1.386(10) . ? C41 C46 1.382(10) . ? C41 C42 1.416(9) . ? C41 P4 1.809(7) . ? C42 C43 1.388(14) . ? C43 C44 1.364(16) . ? C44 C45 1.354(15) . ? C45 C46 1.377(9) . ? C47 C52 1.318(10) . ? C47 C48 1.430(10) . ? C47 P4 1.845(6) . ? C48 C49 1.330(11) . ? C49 C50 1.363(14) . ? C50 C51 1.384(13) . ? C51 C52 1.372(10) . ? C53 C58 1.369(9) . ? C53 C54 1.377(8) . ? C53 P5 1.809(6) . ? C54 C55 1.381(10) . ? C55 C56 1.345(11) . ? C56 C57 1.379(12) . ? C57 C58 1.388(11) . ? C59 C64 1.382(8) . ? C59 C60 1.401(8) . ? C59 P5 1.809(6) . ? C60 C61 1.398(9) . ? C61 C62 1.366(11) . ? C62 C63 1.354(11) . ? C63 C64 1.395(9) . ? C65 C66 1.372(10) . ? C65 C70 1.392(10) . ? C66 C67 1.405(9) . ? C67 C68 1.336(12) . ? C68 C69 1.337(15) . ? C69 C70 1.381(13) . ? C71 C76 1.382(8) . ? C71 C72 1.397(9) . ? C72 C73 1.390(10) . ? C73 C74 1.371(10) . ? C74 C75 1.364(9) . ? C75 C76 1.399(8) . ? C77 C82 1.379(10) . ? C77 C78 1.410(9) . ? C78 C79 1.366(12) . ? C79 C80 1.333(14) . ? C80 C81 1.375(13) . ? C81 C82 1.392(10) . ? C83 C88 1.391(8) . ? C83 C84 1.403(8) . ? C84 C85 1.384(9) . ? C85 C86 1.365(10) . ? C86 C87 1.374(10) . ? C87 C88 1.394(9) . ? C93 C96 1.547(8) . ? C93 P1 1.849(5) . ? C94 C96 1.539(8) . ? C94 P2 1.860(6) . ? C95 C96 1.548(9) . ? C95 P3 1.839(6) . ? C96 C97 1.548(7) . ? C101 O101 1.396(16) . ? C101 C102 1.54(2) . ? C102 C104 1.44(2) . ? C103 O101 1.443(19) . ? C103 C104 1.47(3) . ? Co P2 2.1464(15) . ? Co P3 2.1473(15) . ? Co P1 2.1807(15) . ? P4 Pt1 2.2557(16) . ? P5 Pt1 2.2506(14) . ? Pt1 S2 2.3371(15) . ? Pt1 S1 2.3583(15) . ? 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 C77 B1 C71 112.0(5) . . ? C77 B1 C65 112.2(5) . . ? C71 B1 C65 104.9(5) . . ? C77 B1 C83 107.2(5) . . ? C71 B1 C83 113.1(5) . . ? C65 B1 C83 107.6(5) . . ? C2 C1 S1 124.4(4) . . ? C2 C1 Co 67.2(3) . . ? S1 C1 Co 165.8(4) . . ? C1 C2 S2 126.5(4) . . ? C1 C2 Co 70.8(3) . . ? S2 C2 Co 161.4(4) . . ? C4 C3 P4 110.2(4) . . ? C3 C4 P5 109.9(4) . . ? C6 C5 C10 119.2(6) . . ? C6 C5 P1 117.0(5) . . ? C10 C5 P1 123.6(5) . . ? C5 C6 C7 120.2(7) . . ? C8 C7 C6 119.9(7) . . ? C9 C8 C7 120.1(7) . . ? C10 C9 C8 119.3(8) . . ? C9 C10 C5 121.2(7) . . ? C16 C11 C12 119.1(5) . . ? C16 C11 P1 122.4(4) . . ? C12 C11 P1 118.5(4) . . ? C13 C12 C11 120.0(6) . . ? C12 C13 C14 120.5(6) . . ? C15 C14 C13 119.5(6) . . ? C14 C15 C16 120.5(7) . . ? C11 C16 C15 120.5(6) . . ? C22 C17 C18 119.2(6) . . ? C22 C17 P2 116.4(4) . . ? C18 C17 P2 124.4(6) . . ? C17 C18 C19 118.9(8) . . ? C20 C19 C18 122.1(8) . . ? C19 C20 C21 119.7(7) . . ? C20 C21 C22 119.1(8) . . ? C17 C22 C21 120.9(7) . . ? C24 C23 C28 120.1(5) . . ? C24 C23 P2 119.0(4) . . ? C28 C23 P2 120.9(5) . . ? C23 C24 C25 119.9(6) . . ? C26 C25 C24 120.0(7) . . ? C25 C26 C27 120.4(6) . . ? C26 C27 C28 120.6(7) . . ? C23 C28 C27 119.0(7) . . ? C34 C29 C30 117.4(6) . . ? C34 C29 P3 117.4(5) . . ? C30 C29 P3 125.1(5) . . ? C29 C30 C31 121.6(8) . . ? C32 C31 C30 120.3(8) . . ? C31 C32 C33 119.7(8) . . ? C32 C33 C34 120.5(9) . . ? C29 C34 C33 120.4(8) . . ? C40 C35 C36 117.7(6) . . ? C40 C35 P3 122.0(5) . . ? C36 C35 P3 120.2(5) . . ? C37 C36 C35 120.4(8) . . ? C38 C37 C36 120.7(9) . . ? C39 C38 C37 119.0(8) . . ? C38 C39 C40 121.5(9) . . ? C35 C40 C39 120.5(7) . . ? C46 C41 C42 118.2(7) . . ? C46 C41 P4 120.4(5) . . ? C42 C41 P4 121.3(7) . . ? C43 C42 C41 118.5(10) . . ? C44 C43 C42 121.5(10) . . ? C45 C44 C43 120.1(10) . . ? C44 C45 C46 120.2(10) . . ? C45 C46 C41 121.4(8) . . ? C52 C47 C48 118.7(6) . . ? C52 C47 P4 120.6(6) . . ? C48 C47 P4 120.5(6) . . ? C49 C48 C47 118.2(7) . . ? C48 C49 C50 122.9(7) . . ? C49 C50 C51 118.9(6) . . ? C52 C51 C50 118.2(7) . . ? C47 C52 C51 123.1(7) . . ? C58 C53 C54 118.2(6) . . ? C58 C53 P5 123.1(5) . . ? C54 C53 P5 118.7(5) . . ? C53 C54 C55 121.4(7) . . ? C56 C55 C54 119.5(7) . . ? C55 C56 C57 120.8(8) . . ? C56 C57 C58 119.1(8) . . ? C53 C58 C57 120.9(7) . . ? C64 C59 C60 118.7(6) . . ? C64 C59 P5 119.9(4) . . ? C60 C59 P5 121.3(5) . . ? C61 C60 C59 119.7(7) . . ? C62 C61 C60 120.3(7) . . ? C63 C62 C61 120.4(7) . . ? C62 C63 C64 120.7(7) . . ? C59 C64 C63 120.2(6) . . ? C66 C65 C70 114.0(7) . . ? C66 C65 B1 125.3(6) . . ? C70 C65 B1 120.6(7) . . ? C65 C66 C67 123.0(7) . . ? C68 C67 C66 120.2(8) . . ? C69 C68 C67 118.8(8) . . ? C68 C69 C70 121.7(9) . . ? C69 C70 C65 122.2(10) . . ? C76 C71 C72 115.3(6) . . ? C76 C71 B1 124.8(5) . . ? C72 C71 B1 119.9(6) . . ? C73 C72 C71 122.5(7) . . ? C74 C73 C72 120.5(7) . . ? C75 C74 C73 118.3(6) . . ? C74 C75 C76 121.0(6) . . ? C71 C76 C75 122.2(6) . . ? C82 C77 C78 113.9(7) . . ? C82 C77 B1 121.1(6) . . ? C78 C77 B1 124.9(7) . . ? C79 C78 C77 123.2(10) . . ? C80 C79 C78 120.6(9) . . ? C79 C80 C81 120.0(9) . . ? C80 C81 C82 119.1(9) . . ? C77 C82 C81 123.2(8) . . ? C88 C83 C84 114.6(6) . . ? C88 C83 B1 124.5(5) . . ? C84 C83 B1 120.7(5) . . ? C85 C84 C83 123.3(6) . . ? C86 C85 C84 120.0(6) . . ? C85 C86 C87 119.3(7) . . ? C86 C87 C88 120.2(7) . . ? C83 C88 C87 122.7(6) . . ? C96 C93 P1 116.1(4) . . ? C96 C94 P2 115.5(4) . . ? C96 C95 P3 116.4(4) . . ? C94 C96 C95 112.7(4) . . ? C94 C96 C97 107.4(5) . . ? C95 C96 C97 107.3(5) . . ? C94 C96 C93 110.8(5) . . ? C95 C96 C93 111.3(5) . . ? C97 C96 C93 107.0(4) . . ? O101 C101 C102 104.7(12) . . ? C104 C102 C101 103.8(15) . . ? O101 C103 C104 108.0(15) . . ? C102 C104 C103 106.0(17) . . ? C2 Co C1 42.0(2) . . ? C2 Co P2 120.38(19) . . ? C1 Co P2 133.94(18) . . ? C2 Co P3 100.22(18) . . ? C1 Co P3 129.38(17) . . ? P2 Co P3 90.65(6) . . ? C2 Co P1 144.7(2) . . ? C1 Co P1 104.82(19) . . ? P2 Co P1 90.81(6) . . ? P3 Co P1 95.19(6) . . ? C101 O101 C103 108.0(11) . . ? C11 P1 C5 98.3(3) . . ? C11 P1 C93 102.3(3) . . ? C5 P1 C93 106.1(3) . . ? C11 P1 Co 119.65(18) . . ? C5 P1 Co 115.9(2) . . ? C93 P1 Co 112.58(18) . . ? C17 P2 C23 99.7(3) . . ? C17 P2 C94 107.7(3) . . ? C23 P2 C94 102.9(3) . . ? C17 P2 Co 113.3(2) . . ? C23 P2 Co 118.7(2) . . ? C94 P2 Co 113.19(19) . . ? C35 P3 C29 101.5(3) . . ? C35 P3 C95 104.3(3) . . ? C29 P3 C95 105.9(3) . . ? C35 P3 Co 113.4(2) . . ? C29 P3 Co 118.61(19) . . ? C95 P3 Co 111.8(2) . . ? C41 P4 C3 105.9(3) . . ? C41 P4 C47 100.8(3) . . ? C3 P4 C47 103.7(3) . . ? C41 P4 Pt1 112.4(2) . . ? C3 P4 Pt1 107.6(2) . . ? C47 P4 Pt1 124.9(3) . . ? C59 P5 C53 106.5(3) . . ? C59 P5 C4 107.2(3) . . ? C53 P5 C4 105.9(3) . . ? C59 P5 Pt1 113.9(2) . . ? C53 P5 Pt1 115.01(18) . . ? C4 P5 Pt1 107.80(19) . . ? P5 Pt1 P4 86.62(5) . . ? P5 Pt1 S2 88.10(5) . . ? P4 Pt1 S2 174.00(6) . . ? P5 Pt1 S1 176.79(5) . . ? P4 Pt1 S1 96.20(5) . . ? S2 Pt1 S1 89.16(5) . . ? C1 S1 Pt1 100.02(19) . . ? C2 S2 Pt1 99.9(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.85 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.359 _refine_diff_density_min -1.338 _refine_diff_density_rms 0.101