Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Takagi, Hideo D.' 'Funahashi, Shigenobu' 'Hasegawa, Atsushi' 'Kashiwabara, Kazuo' 'Suzuki, Takayoshi' 'Twatsuki, Satoshi' _publ_contact_author_name 'Prof Hideo D Takagi' _publ_contact_author_address ; Department of Chemistry Nagoya University Nagoya 464-8602 JAPAN ; _publ_contact_author_email 'HTAKAGI@CHEM4.CHEM.NAGOYA-U.AC.JP' _publ_section_title ; Preparation, crystal structures and isomerization kinetics fo the cis-and trans-[Co(dtc)2(PHPh2)2]+ (dtc-=N,N-Dimethyldithiocarbamate) complexes: thermodynamically and kinetically stable Cobalt(III)-P bonds through interplay of sigma-donicity, pi-acidity, and steric bulkiness ; data_cisPHPh2 _database_code_CSD 172897 _audit_creation_date 'Fri Feb 18 2000' _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis-Bis(diphenylphosphine)bis(N,N-dimethyldithiocarbamato)cobalt(III) Tetrafluoroborate Acetonitrile and Hemi(diethyl ether) Solvate ; _chemical_name_common 'cis-[Co(dtc)~2~(PHPh~2~)~2~]BF~4~.CH~3~CN.0.5Et~2~O' _chemical_melting_point ? _chemical_formula_moiety 'Co (C12 H11 P)2 (C3 H6 N S2)2 1+, B F4 1-, C2 H3 N, 0.5(C4 H10 O)' _chemical_formula_sum 'C34 H42 B Co F4 N3 O0.5 P2 S4' _chemical_formula_weight 836.63 _ccdc_compound_id ? _ccdc_biological_activity ? _ccdc_polymorph ? _ccdc_chemdiag_type ? loop_ _ccdc_chemdiag_records ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_colour 'dark red' _diffrn_radiation_type 'Mo K\a' _diffrn_measurement_device 'Rigaku RAXIS-RAPID Imaging Plate' _ccdc_temp_data_collection 293(2) _ccdc_ls_R_squared ? _refine_ls_abs_structure_details centrosymmetric _ccdc_disorder none _ccdc_comments none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' 0.3494 0.9721 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 '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 'P 1 2/n 1' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y, -z-1/2' _cell_length_a 19.3594(11) _cell_length_b 11.1101(7) _cell_length_c 20.6423(10) _cell_angle_alpha 90.00 _cell_angle_beta 115.830(2) _cell_angle_gamma 90.00 _cell_volume 3996.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28021 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description 'block' _exptl_crystal_colour 'dark-red' _exptl_crystal_size_max 0.480 _exptl_crystal_size_mid 0.420 _exptl_crystal_size_min 0.300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1732 _exptl_absorpt_coefficient_mu 0.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.562 _exptl_absorpt_correction_T_max 0.794 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details none _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean '100 x 100' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35921 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9084 _reflns_number_gt 6901 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 and teXsan Ver. 1.10' _computing_molecular_graphics 'ORTEP in teXsan' _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. Hydrogen atoms bound directly to P, H1 and H2, were refined isotropically, and the other H atoms were treated by means of a riding model. ; _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^)+(0.0500P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9084 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1169 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.265 _refine_ls_restrained_S_all 1.265 _refine_ls_shift/su_max 0.010 _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 Co Co 0.251022(16) 0.39820(3) 0.952388(14) 0.03515(9) Uani 1 1 d . . . S1 S 0.37187(4) 0.32195(6) 1.00051(3) 0.04974(16) Uani 1 1 d . . . S2 S 0.27199(3) 0.35888(6) 0.85458(3) 0.04265(14) Uani 1 1 d . . . S3 S 0.29813(4) 0.59123(5) 0.97183(3) 0.04749(15) Uani 1 1 d . . . S4 S 0.25716(4) 0.44506(5) 1.06120(3) 0.04582(15) Uani 1 1 d . . . P1 P 0.13328(3) 0.47541(5) 0.89394(3) 0.03871(14) Uani 1 1 d . . . P2 P 0.20174(3) 0.21534(5) 0.94673(3) 0.03829(14) Uani 1 1 d . . . F1 F 0.5051(2) 0.1677(3) 0.73835(18) 0.1567(13) Uani 1 1 d . . . F2 F 0.5373(2) 0.2540(3) 0.6644(2) 0.1641(14) Uani 1 1 d . . . F3 F 0.50086(16) 0.0680(3) 0.64395(16) 0.1472(12) Uani 1 1 d . . . F4 F 0.61057(16) 0.1094(3) 0.73293(15) 0.1475(12) Uani 1 1 d . . . O1 O 0.2500 0.4304(4) 1.2500 0.0885(10) Uani 1 2 d S . . N1 N 0.40840(13) 0.2485(2) 0.89527(12) 0.0572(6) Uani 1 1 d . . . N2 N 0.29621(15) 0.6772(2) 1.09325(12) 0.0610(6) Uani 1 1 d . . . N3 N 0.4954(4) 1.0725(5) 1.1254(3) 0.162(2) Uani 1 1 d . . . C1 C 0.35917(14) 0.3020(2) 0.91400(13) 0.0442(5) Uani 1 1 d . . . C2 C 0.48222(19) 0.2049(4) 0.94925(19) 0.0871(11) Uani 1 1 d . . . H2A H 0.5203 0.2665 0.9592 0.131 Uiso 1 1 calc R . . H2B H 0.4970 0.1345 0.9314 0.131 Uiso 1 1 calc R . . H2C H 0.4779 0.1852 0.9926 0.131 Uiso 1 1 calc R . . C3 C 0.3889(2) 0.2247(3) 0.81916(17) 0.0757(9) Uani 1 1 d . . . H3A H 0.3582 0.1531 0.8039 0.114 Uiso 1 1 calc R . . H3B H 0.4352 0.2139 0.8135 0.114 Uiso 1 1 calc R . . H3C H 0.3605 0.2915 0.7904 0.114 Uiso 1 1 calc R . . C6 C 0.28625(14) 0.5862(2) 1.04935(13) 0.0462(5) Uani 1 1 d . . . C7 C 0.3192(2) 0.7962(3) 1.0793(2) 0.0830(11) Uani 1 1 d . . . H7A H 0.3368 0.7899 1.0425 0.125 Uiso 1 1 calc R . . H7B H 0.3598 0.8269 1.1226 0.125 Uiso 1 1 calc R . . H7C H 0.2760 0.8498 1.0635 0.125 Uiso 1 1 calc R . . C8 C 0.2806(2) 0.6664(3) 1.15652(18) 0.0837(11) Uani 1 1 d . . . H8A H 0.2695 0.5840 1.1624 0.126 Uiso 1 1 calc R . . H8B H 0.2374 0.7158 1.1500 0.126 Uiso 1 1 calc R . . H8C H 0.3248 0.6924 1.1986 0.126 Uiso 1 1 calc R . . C11 C 0.10197(14) 0.5120(2) 0.79962(13) 0.0441(5) Uani 1 1 d . . . C12 C 0.03048(17) 0.4745(3) 0.74907(16) 0.0643(7) Uani 1 1 d . . . H12 H -0.0016 0.4311 0.7633 0.077 Uiso 1 1 calc R . . C13 C 0.0070(2) 0.5023(4) 0.67662(18) 0.0867(11) Uani 1 1 d . . . H13 H -0.0415 0.4790 0.6428 0.104 Uiso 1 1 calc R . . C14 C 0.0540(2) 0.5629(4) 0.65494(18) 0.0865(11) Uani 1 1 d . . . H14 H 0.0380 0.5794 0.6064 0.104 Uiso 1 1 calc R . . C15 C 0.1244(2) 0.5996(3) 0.70403(18) 0.0748(9) Uani 1 1 d . . . H15 H 0.1563 0.6416 0.6888 0.090 Uiso 1 1 calc R . . C16 C 0.14930(16) 0.5749(2) 0.77679(15) 0.0551(6) Uani 1 1 d . . . H16 H 0.1975 0.6005 0.8101 0.066 Uiso 1 1 calc R . . C17 C 0.10784(14) 0.6035(2) 0.93392(14) 0.0456(5) Uani 1 1 d . . . C18 C 0.11837(18) 0.7215(2) 0.91806(17) 0.0602(7) Uani 1 1 d . . . H18 H 0.1365 0.7374 0.8839 0.072 Uiso 1 1 calc R . . C19 C 0.1019(2) 0.8152(3) 0.9530(2) 0.0812(10) Uani 1 1 d . . . H19 H 0.1085 0.8942 0.9419 0.097 Uiso 1 1 calc R . . C20 C 0.0761(2) 0.7925(3) 1.0037(2) 0.0834(11) Uani 1 1 d . . . H20 H 0.0658 0.8561 1.0275 0.100 Uiso 1 1 calc R . . C21 C 0.0653(2) 0.6767(3) 1.01956(19) 0.0763(9) Uani 1 1 d . . . H21 H 0.0471 0.6618 1.0537 0.092 Uiso 1 1 calc R . . C22 C 0.08109(17) 0.5815(3) 0.98512(16) 0.0595(7) Uani 1 1 d . . . H22 H 0.0738 0.5028 0.9962 0.071 Uiso 1 1 calc R . . C31 C 0.19922(15) 0.1587(2) 1.02784(12) 0.0428(5) Uani 1 1 d . . . C32 C 0.12854(18) 0.1401(3) 1.02892(16) 0.0603(7) Uani 1 1 d . . . H32 H 0.0833 0.1616 0.9895 0.072 Uiso 1 1 calc R . . C33 C 0.1264(2) 0.0893(3) 1.0891(2) 0.0808(11) Uani 1 1 d . . . H33 H 0.0794 0.0782 1.0903 0.097 Uiso 1 1 calc R . . C34 C 0.1922(3) 0.0553(3) 1.14684(18) 0.0788(10) Uani 1 1 d . . . H34 H 0.1898 0.0188 1.1864 0.095 Uiso 1 1 calc R . . C35 C 0.2616(2) 0.0752(3) 1.14633(16) 0.0720(9) Uani 1 1 d . . . H35 H 0.3065 0.0524 1.1857 0.086 Uiso 1 1 calc R . . C36 C 0.26558(18) 0.1289(3) 1.08754(14) 0.0578(7) Uani 1 1 d . . . H36 H 0.3131 0.1450 1.0883 0.069 Uiso 1 1 calc R . . C37 C 0.23341(15) 0.0877(2) 0.91061(13) 0.0449(5) Uani 1 1 d . . . C38 C 0.30461(18) 0.0355(3) 0.94561(15) 0.0617(7) Uani 1 1 d . . . H38 H 0.3392 0.0644 0.9903 0.074 Uiso 1 1 calc R . . C39 C 0.3248(2) -0.0603(3) 0.9142(2) 0.0780(10) Uani 1 1 d . . . H39 H 0.3734 -0.0943 0.9370 0.094 Uiso 1 1 calc R . . C40 C 0.2724(3) -0.1047(3) 0.8492(2) 0.0839(11) Uani 1 1 d . . . H40 H 0.2855 -0.1700 0.8287 0.101 Uiso 1 1 calc R . . C41 C 0.2023(2) -0.0548(3) 0.8147(2) 0.0836(10) Uani 1 1 d . . . H41 H 0.1675 -0.0853 0.7706 0.100 Uiso 1 1 calc R . . C42 C 0.18204(18) 0.0420(3) 0.84500(15) 0.0605(7) Uani 1 1 d . . . H42 H 0.1336 0.0764 0.8211 0.073 Uiso 1 1 calc R . . C46 C 0.4903(3) 1.1149(4) 1.1715(3) 0.1040(14) Uani 1 1 d . . . C47 C 0.4810(3) 1.1727(5) 1.2288(3) 0.1236(17) Uani 1 1 d . . . H47A H 0.5042 1.2511 1.2368 0.185 Uiso 1 1 calc R . . H47B H 0.5053 1.1255 1.2719 0.185 Uiso 1 1 calc R . . H47C H 0.4273 1.1806 1.2164 0.185 Uiso 1 1 calc R . . C48 C 0.3146(3) 0.3624(5) 1.2818(3) 0.141(2) Uani 1 1 d . . . H48A H 0.3070 0.3063 1.3141 0.170 Uiso 1 1 calc R . . H48B H 0.3196 0.3152 1.2445 0.170 Uiso 1 1 calc R . . C49 C 0.3815(3) 0.4193(6) 1.3191(4) 0.166(3) Uani 1 1 d . . . H49A H 0.4083 0.4272 1.2896 0.249 Uiso 1 1 calc R . . H49B H 0.4122 0.3736 1.3614 0.249 Uiso 1 1 calc R . . H49C H 0.3719 0.4977 1.3329 0.249 Uiso 1 1 calc R . . B1 B 0.5399(2) 0.1475(3) 0.69587(19) 0.0625(8) Uani 1 1 d . . . H1 H 0.0768(15) 0.397(2) 0.8904(13) 0.048(7) Uiso 1 1 d . . . H2 H 0.1254(14) 0.210(2) 0.9013(12) 0.042(6) 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 Co 0.03729(17) 0.03360(15) 0.03377(16) 0.00133(11) 0.01475(13) 0.00176(12) S1 0.0409(3) 0.0615(4) 0.0391(3) -0.0012(3) 0.0103(2) 0.0105(3) S2 0.0430(3) 0.0494(3) 0.0362(3) 0.0043(2) 0.0178(2) 0.0050(3) S3 0.0508(4) 0.0414(3) 0.0530(3) -0.0021(3) 0.0251(3) -0.0074(3) S4 0.0586(4) 0.0405(3) 0.0396(3) -0.0021(2) 0.0224(3) -0.0021(3) P1 0.0387(3) 0.0342(3) 0.0445(3) 0.0042(2) 0.0193(2) 0.0025(2) P2 0.0427(3) 0.0329(3) 0.0367(3) 0.0018(2) 0.0150(2) 0.0026(2) F1 0.194(3) 0.174(3) 0.166(3) -0.033(2) 0.139(3) -0.008(3) F2 0.223(4) 0.123(2) 0.187(3) 0.065(2) 0.127(3) 0.049(2) F3 0.103(2) 0.161(3) 0.137(2) -0.077(2) 0.0139(17) -0.0061(18) F4 0.0912(17) 0.163(3) 0.124(2) -0.0395(18) -0.0127(15) 0.0577(18) O1 0.078(2) 0.099(3) 0.088(2) 0.000 0.036(2) 0.000 N1 0.0511(13) 0.0711(15) 0.0545(12) 0.0018(11) 0.0277(10) 0.0154(11) N2 0.0780(17) 0.0472(12) 0.0585(13) -0.0157(10) 0.0303(12) -0.0120(12) N3 0.208(6) 0.155(4) 0.117(4) 0.013(3) 0.064(4) 0.077(4) C1 0.0408(12) 0.0471(13) 0.0451(12) -0.0001(10) 0.0192(10) 0.0025(11) C2 0.0550(19) 0.117(3) 0.087(2) 0.002(2) 0.0285(17) 0.035(2) C3 0.084(2) 0.092(2) 0.0664(18) -0.0033(17) 0.0467(18) 0.0166(19) C6 0.0449(13) 0.0415(13) 0.0479(13) -0.0043(10) 0.0161(11) -0.0028(10) C7 0.119(3) 0.0444(15) 0.094(2) -0.0181(16) 0.053(2) -0.0237(18) C8 0.123(3) 0.071(2) 0.0646(18) -0.0247(16) 0.048(2) -0.018(2) C11 0.0431(13) 0.0415(12) 0.0441(12) 0.0058(10) 0.0158(10) 0.0094(10) C12 0.0528(16) 0.0721(19) 0.0581(16) -0.0011(14) 0.0151(13) 0.0006(15) C13 0.070(2) 0.104(3) 0.0535(18) 0.0023(18) -0.0032(16) 0.004(2) C14 0.094(3) 0.106(3) 0.0486(17) 0.0182(18) 0.0209(18) 0.025(2) C15 0.083(2) 0.079(2) 0.069(2) 0.0301(17) 0.0401(19) 0.0191(18) C16 0.0523(15) 0.0575(16) 0.0528(14) 0.0134(12) 0.0204(12) 0.0073(13) C17 0.0408(13) 0.0438(12) 0.0538(14) 0.0011(10) 0.0221(11) 0.0056(10) C18 0.0690(19) 0.0423(14) 0.0751(18) 0.0051(13) 0.0368(16) 0.0089(13) C19 0.088(2) 0.0438(16) 0.117(3) -0.0083(17) 0.050(2) 0.0064(16) C20 0.081(2) 0.073(2) 0.107(3) -0.029(2) 0.052(2) 0.0072(19) C21 0.076(2) 0.086(2) 0.084(2) -0.0161(19) 0.0518(19) 0.0066(19) C22 0.0599(17) 0.0593(16) 0.0717(18) -0.0033(14) 0.0402(15) 0.0019(14) C31 0.0543(14) 0.0342(11) 0.0451(12) -0.0013(9) 0.0265(11) 0.0000(10) C32 0.0613(17) 0.0692(18) 0.0577(16) -0.0091(14) 0.0327(14) -0.0127(15) C33 0.094(3) 0.092(2) 0.080(2) -0.0219(19) 0.060(2) -0.037(2) C34 0.124(3) 0.070(2) 0.0599(19) -0.0036(16) 0.057(2) -0.023(2) C35 0.099(3) 0.071(2) 0.0466(15) 0.0103(14) 0.0326(16) 0.0089(19) C36 0.0658(17) 0.0635(17) 0.0458(14) 0.0083(12) 0.0258(13) 0.0047(14) C37 0.0615(16) 0.0342(11) 0.0458(13) 0.0043(9) 0.0296(12) 0.0025(11) C38 0.0735(19) 0.0507(15) 0.0570(16) 0.0064(13) 0.0248(14) 0.0190(14) C39 0.099(3) 0.0586(18) 0.088(2) 0.0170(17) 0.051(2) 0.0369(18) C40 0.133(4) 0.0545(18) 0.090(3) -0.0086(17) 0.072(3) 0.011(2) C41 0.107(3) 0.073(2) 0.077(2) -0.0312(19) 0.045(2) -0.007(2) C42 0.0704(19) 0.0583(16) 0.0558(15) -0.0122(13) 0.0302(14) -0.0030(14) C46 0.105(3) 0.095(3) 0.095(3) 0.009(3) 0.027(3) 0.023(3) C47 0.127(4) 0.119(4) 0.129(4) -0.034(3) 0.059(3) -0.035(3) C48 0.102(4) 0.111(4) 0.173(6) 0.015(4) 0.025(4) 0.024(3) C49 0.089(4) 0.180(6) 0.198(7) 0.019(5) 0.034(4) -0.001(4) B1 0.060(2) 0.063(2) 0.0593(19) -0.0002(16) 0.0213(16) 0.0120(17) _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 Co P2 2.2258(7) . ? Co P1 2.2340(6) . ? Co S4 2.2577(6) . ? Co S2 2.2684(6) . ? Co S1 2.2699(7) . ? Co S3 2.2963(7) . ? S1 C1 1.708(2) . ? S2 C1 1.717(2) . ? S3 C6 1.714(3) . ? S4 C6 1.719(3) . ? P1 C11 1.815(2) . ? P1 C17 1.818(2) . ? P1 H1 1.37(3) . ? P2 C31 1.809(2) . ? P2 C37 1.828(2) . ? P2 H2 1.36(2) . ? F1 B1 1.337(4) . ? F2 B1 1.341(5) . ? F3 B1 1.339(4) . ? F4 B1 1.313(4) . ? O1 C48 1.360(5) 4_658 ? O1 C48 1.360(5) . ? N1 C1 1.316(3) . ? N1 C2 1.460(4) . ? N1 C3 1.471(4) . ? N2 C6 1.314(3) . ? N2 C7 1.463(4) . ? N2 C8 1.468(4) . ? N3 C46 1.105(6) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C11 C12 1.385(4) . ? C11 C16 1.388(4) . ? C12 C13 1.395(5) . ? C12 H12 0.9300 . ? C13 C14 1.354(5) . ? C13 H13 0.9300 . ? C14 C15 1.360(5) . ? C14 H14 0.9300 . ? C15 C16 1.390(4) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.386(4) . ? C17 C18 1.387(4) . ? C18 C19 1.380(4) . ? C18 H18 0.9300 . ? C19 C20 1.368(5) . ? C19 H19 0.9300 . ? C20 C21 1.366(5) . ? C20 H20 0.9300 . ? C21 C22 1.381(4) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C31 C36 1.378(4) . ? C31 C32 1.394(4) . ? C32 C33 1.381(4) . ? C32 H32 0.9300 . ? C33 C34 1.365(5) . ? C33 H33 0.9300 . ? C34 C35 1.367(5) . ? C34 H34 0.9300 . ? C35 C36 1.384(4) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.375(4) . ? C37 C42 1.381(4) . ? C38 C39 1.389(4) . ? C38 H38 0.9300 . ? C39 C40 1.373(5) . ? C39 H39 0.9300 . ? C40 C41 1.347(5) . ? C40 H40 0.9300 . ? C41 C42 1.383(4) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C46 C47 1.425(7) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 C49 1.342(7) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? 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 P2 Co P1 90.51(2) . . ? P2 Co S4 95.64(2) . . ? P1 Co S4 92.74(2) . . ? P2 Co S2 90.94(2) . . ? P1 Co S2 97.43(2) . . ? S4 Co S2 167.83(3) . . ? P2 Co S1 91.08(3) . . ? P1 Co S1 173.81(3) . . ? S4 Co S1 93.05(2) . . ? S2 Co S1 76.57(2) . . ? P2 Co S3 171.94(3) . . ? P1 Co S3 88.27(3) . . ? S4 Co S3 76.47(2) . . ? S2 Co S3 97.12(3) . . ? S1 Co S3 90.97(3) . . ? C1 S1 Co 86.53(8) . . ? C1 S2 Co 86.36(8) . . ? C6 S3 Co 85.88(8) . . ? C6 S4 Co 86.98(8) . . ? C11 P1 C17 106.37(11) . . ? C11 P1 Co 116.78(8) . . ? C17 P1 Co 118.03(8) . . ? C11 P1 H1 101.4(10) . . ? C17 P1 H1 98.7(10) . . ? Co P1 H1 112.9(10) . . ? C31 P2 C37 104.86(10) . . ? C31 P2 Co 116.93(8) . . ? C37 P2 Co 121.15(8) . . ? C31 P2 H2 99.5(10) . . ? C37 P2 H2 98.3(10) . . ? Co P2 H2 112.6(10) . . ? C48 O1 C48 112.6(6) 4_658 . ? C1 N1 C2 121.3(2) . . ? C1 N1 C3 120.9(2) . . ? C2 N1 C3 117.8(2) . . ? C6 N2 C7 121.6(2) . . ? C6 N2 C8 121.7(2) . . ? C7 N2 C8 116.6(2) . . ? N1 C1 S1 124.97(19) . . ? N1 C1 S2 124.66(18) . . ? S1 C1 S2 110.36(13) . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C6 S3 125.4(2) . . ? N2 C6 S4 124.2(2) . . ? S3 C6 S4 110.37(13) . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C12 C11 C16 119.1(2) . . ? C12 C11 P1 119.9(2) . . ? C16 C11 P1 121.03(19) . . ? C11 C12 C13 119.5(3) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 120.8(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.2(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 120.6(3) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C11 C16 C15 119.8(3) . . ? C11 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C22 C17 C18 119.3(2) . . ? C22 C17 P1 118.2(2) . . ? C18 C17 P1 122.4(2) . . ? C19 C18 C17 119.9(3) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 120.4(3) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 120.1(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.4(3) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C17 119.8(3) . . ? C21 C22 H22 120.1 . . ? C17 C22 H22 120.1 . . ? C36 C31 C32 119.3(2) . . ? C36 C31 P2 121.4(2) . . ? C32 C31 P2 119.3(2) . . ? C33 C32 C31 119.3(3) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C34 C33 C32 121.1(3) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C33 C34 C35 119.7(3) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C35 C36 120.4(3) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C31 C36 C35 120.1(3) . . ? C31 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C42 119.3(2) . . ? C38 C37 P2 123.4(2) . . ? C42 C37 P2 117.3(2) . . ? C37 C38 C39 119.9(3) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 119.6(3) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C41 C40 C39 120.9(3) . . ? C41 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C40 C41 C42 120.0(3) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C37 C42 C41 120.3(3) . . ? C37 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? N3 C46 C47 177.5(6) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 O1 118.1(5) . . ? C49 C48 H48A 107.8 . . ? O1 C48 H48A 107.8 . . ? C49 C48 H48B 107.8 . . ? O1 C48 H48B 107.8 . . ? H48A C48 H48B 107.1 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? F4 B1 F1 111.5(3) . . ? F4 B1 F3 109.6(3) . . ? F1 B1 F3 111.5(4) . . ? F4 B1 F2 112.1(4) . . ? F1 B1 F2 104.3(3) . . ? F3 B1 F2 107.8(3) . . ? 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 P2 Co S1 C1 87.97(9) . . . . ? P1 Co S1 C1 -16.9(3) . . . . ? S4 Co S1 C1 -176.33(9) . . . . ? S2 Co S1 C1 -2.74(9) . . . . ? S3 Co S1 C1 -99.83(9) . . . . ? P2 Co S2 C1 -88.16(9) . . . . ? P1 Co S2 C1 -178.80(9) . . . . ? S4 Co S2 C1 34.68(16) . . . . ? S1 Co S2 C1 2.73(9) . . . . ? S3 Co S2 C1 92.02(9) . . . . ? P2 Co S3 C6 8.3(2) . . . . ? P1 Co S3 C6 89.67(9) . . . . ? S4 Co S3 C6 -3.57(9) . . . . ? S2 Co S3 C6 -173.05(9) . . . . ? S1 Co S3 C6 -96.47(9) . . . . ? P2 Co S4 C6 -174.79(9) . . . . ? P1 Co S4 C6 -84.01(9) . . . . ? S2 Co S4 C6 62.79(15) . . . . ? S1 Co S4 C6 93.82(9) . . . . ? S3 Co S4 C6 3.55(9) . . . . ? P2 Co P1 C11 -103.53(9) . . . . ? S4 Co P1 C11 160.80(9) . . . . ? S2 Co P1 C11 -12.52(9) . . . . ? S1 Co P1 C11 1.4(3) . . . . ? S3 Co P1 C11 84.44(9) . . . . ? P2 Co P1 C17 127.69(10) . . . . ? S4 Co P1 C17 32.02(10) . . . . ? S2 Co P1 C17 -141.30(10) . . . . ? S1 Co P1 C17 -127.4(3) . . . . ? S3 Co P1 C17 -44.34(10) . . . . ? P1 Co P2 C31 -102.75(9) . . . . ? S4 Co P2 C31 -9.95(10) . . . . ? S2 Co P2 C31 159.80(9) . . . . ? S1 Co P2 C31 83.22(9) . . . . ? S3 Co P2 C31 -21.5(2) . . . . ? P1 Co P2 C37 127.22(10) . . . . ? S4 Co P2 C37 -139.98(10) . . . . ? S2 Co P2 C37 29.78(10) . . . . ? S1 Co P2 C37 -46.81(10) . . . . ? S3 Co P2 C37 -151.53(19) . . . . ? C2 N1 C1 S1 -2.8(4) . . . . ? C3 N1 C1 S1 173.7(2) . . . . ? C2 N1 C1 S2 178.6(3) . . . . ? C3 N1 C1 S2 -4.9(4) . . . . ? Co S1 C1 N1 -175.0(2) . . . . ? Co S1 C1 S2 3.76(12) . . . . ? Co S2 C1 N1 175.0(2) . . . . ? Co S2 C1 S1 -3.76(12) . . . . ? C7 N2 C6 S3 0.1(4) . . . . ? C8 N2 C6 S3 176.6(3) . . . . ? C7 N2 C6 S4 -178.4(3) . . . . ? C8 N2 C6 S4 -1.9(4) . . . . ? Co S3 C6 N2 -173.8(2) . . . . ? Co S3 C6 S4 4.86(12) . . . . ? Co S4 C6 N2 173.8(2) . . . . ? Co S4 C6 S3 -4.94(12) . . . . ? C17 P1 C11 C12 -94.0(2) . . . . ? Co P1 C11 C12 131.8(2) . . . . ? C17 P1 C11 C16 87.5(2) . . . . ? Co P1 C11 C16 -46.7(2) . . . . ? C16 C11 C12 C13 -1.0(4) . . . . ? P1 C11 C12 C13 -179.6(3) . . . . ? C11 C12 C13 C14 1.6(6) . . . . ? C12 C13 C14 C15 -1.3(6) . . . . ? C13 C14 C15 C16 0.4(6) . . . . ? C12 C11 C16 C15 0.2(4) . . . . ? P1 C11 C16 C15 178.7(2) . . . . ? C14 C15 C16 C11 0.2(5) . . . . ? C11 P1 C17 C22 141.6(2) . . . . ? Co P1 C17 C22 -84.9(2) . . . . ? C11 P1 C17 C18 -42.1(3) . . . . ? Co P1 C17 C18 91.4(2) . . . . ? C22 C17 C18 C19 -0.2(5) . . . . ? P1 C17 C18 C19 -176.5(3) . . . . ? C17 C18 C19 C20 0.7(5) . . . . ? C18 C19 C20 C21 -0.9(6) . . . . ? C19 C20 C21 C22 0.7(6) . . . . ? C20 C21 C22 C17 -0.3(5) . . . . ? C18 C17 C22 C21 0.0(4) . . . . ? P1 C17 C22 C21 176.4(2) . . . . ? C37 P2 C31 C36 68.5(2) . . . . ? Co P2 C31 C36 -68.8(2) . . . . ? C37 P2 C31 C32 -108.8(2) . . . . ? Co P2 C31 C32 113.9(2) . . . . ? C36 C31 C32 C33 -1.6(4) . . . . ? P2 C31 C32 C33 175.7(2) . . . . ? C31 C32 C33 C34 -1.2(5) . . . . ? C32 C33 C34 C35 2.2(5) . . . . ? C33 C34 C35 C36 -0.3(5) . . . . ? C32 C31 C36 C35 3.4(4) . . . . ? P2 C31 C36 C35 -173.9(2) . . . . ? C34 C35 C36 C31 -2.5(5) . . . . ? C31 P2 C37 C38 -64.4(2) . . . . ? Co P2 C37 C38 70.7(2) . . . . ? C31 P2 C37 C42 115.1(2) . . . . ? Co P2 C37 C42 -109.9(2) . . . . ? C42 C37 C38 C39 1.4(4) . . . . ? P2 C37 C38 C39 -179.2(2) . . . . ? C37 C38 C39 C40 -2.0(5) . . . . ? C38 C39 C40 C41 1.5(6) . . . . ? C39 C40 C41 C42 -0.4(6) . . . . ? C38 C37 C42 C41 -0.4(4) . . . . ? P2 C37 C42 C41 -179.9(3) . . . . ? C40 C41 C42 C37 -0.1(5) . . . . ? C48 O1 C48 C49 -175.6(8) 4_658 . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.650 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.138 #===END data_transPHPh2 _database_code_CSD 172898 _audit_creation_date 'Fri Feb 18 2000' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-Bis(diphenylphosphine)bis(N,N-dimethyldithiocarbamato)cobalt(III) Tetrafluoroborate ; _chemical_name_common 'trans-[Co(dtc)~2~(PHPh~2~)~2~]BF~4~' _chemical_melting_point ? _chemical_formula_moiety 'Co (C12 H11 P)2 (C3 H6 N S2)2 1+, B F4 1-' _chemical_formula_sum 'C30 H34 B Co F4 N2 P2 S4' _chemical_formula_weight 758.51 _ccdc_compound_id ? _ccdc_biological_activity ? _ccdc_polymorph ? _ccdc_chemdiag_type ? loop_ _ccdc_chemdiag_records ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_colour 'dark red' _diffrn_radiation_type 'Mo K\a' _diffrn_measurement_device 'Rigaku AFC5R' _ccdc_temp_data_collection 296(2) _ccdc_ls_R_squared ? _refine_ls_abs_structure_details centrosymmetric _ccdc_disorder ; F atoms of the BF~4~^-^ anion showed positional disorder over four possible tetrahedral arrangements, and refined isotropically. ; _ccdc_comments none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' 0.3494 0.9721 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.507(4) _cell_length_b 14.529(5) _cell_length_c 14.445(3) _cell_angle_alpha 90.00 _cell_angle_beta 122.200(10) _cell_angle_gamma 90.00 _cell_volume 3464.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.5 _cell_measurement_theta_max 15.0 _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'dark-red' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.875 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details none _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.62 _diffrn_reflns_number 5203 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0751 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 30.03 _reflns_number_total 5070 _reflns_number_gt 2841 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 and teXsan Ver. 1.10' _computing_molecular_graphics 'ORTEP in teXsan Ver. 1.10' _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. F atoms of the BF~4~^-^ anion showed positional disorder over four possible tetrahedral arrangements, and refined isotropically. Hydrogen atom bound directly to P, H1, were refined isotropically, and the other H atoms were treated by means of a riding model. ; _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^)+(0.0607P)^2^+3.0353P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5070 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1309 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1468 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.5000 0.5000 0.5000 0.03533(17) Uani 1 2 d S . . S1 S 0.56554(5) 0.44187(7) 0.67223(7) 0.0464(2) Uani 1 1 d . . . S2 S 0.62196(5) 0.45804(7) 0.52886(8) 0.0479(2) Uani 1 1 d . . . P P 0.44706(5) 0.36036(7) 0.42404(7) 0.0407(2) Uani 1 1 d . . . F1 F 0.0328(5) 0.4250(5) 0.7030(7) 0.0738(17) Uiso 0.50 1 d P . . F2 F -0.0512(6) 0.3135(7) 0.6703(8) 0.138(3) Uiso 0.50 1 d P . . F3 F 0.0000 0.2812(9) 0.7500 0.133(4) Uiso 0.50 2 d SP . . F4 F 0.0630(8) 0.4246(9) 0.7606(12) 0.075(3) Uiso 0.25 1 d P . . F5 F -0.0043(10) 0.4019(10) 0.6577(12) 0.094(4) Uiso 0.25 1 d P . . F6 F 0.0776(9) 0.3860(11) 0.8442(12) 0.104(4) Uiso 0.25 1 d P . . N N 0.72155(19) 0.4096(2) 0.7403(3) 0.0586(9) Uani 1 1 d . . . C1 C 0.6478(2) 0.4319(2) 0.6599(3) 0.0456(8) Uani 1 1 d . . . C2 C 0.7403(3) 0.3954(4) 0.8514(4) 0.0772(15) Uani 1 1 d . . . H2A H 0.6920 0.4034 0.8529 0.116 Uiso 1 1 calc R . . H2B H 0.7803 0.4393 0.8996 0.116 Uiso 1 1 calc R . . H2C H 0.7608 0.3342 0.8750 0.116 Uiso 1 1 calc R . . C3 C 0.7887(2) 0.4040(4) 0.7240(4) 0.0754(14) Uani 1 1 d . . . H3A H 0.8031 0.3406 0.7250 0.113 Uiso 1 1 calc R . . H3B H 0.8343 0.4368 0.7814 0.113 Uiso 1 1 calc R . . H3C H 0.7730 0.4308 0.6546 0.113 Uiso 1 1 calc R . . C11 C 0.3482(2) 0.3534(3) 0.2973(3) 0.0456(8) Uani 1 1 d . . . C12 C 0.3439(3) 0.3494(3) 0.1975(3) 0.0589(11) Uani 1 1 d . . . H12 H 0.3910 0.3501 0.1962 0.071 Uiso 1 1 calc R . . C13 C 0.2695(3) 0.3443(4) 0.1012(3) 0.0779(15) Uani 1 1 d . . . H13 H 0.2670 0.3416 0.0352 0.093 Uiso 1 1 calc R . . C14 C 0.1993(3) 0.3431(4) 0.1006(4) 0.0813(16) Uani 1 1 d . . . H14 H 0.1496 0.3398 0.0347 0.098 Uiso 1 1 calc R . . C15 C 0.2022(3) 0.3467(4) 0.1978(4) 0.0743(14) Uani 1 1 d . . . H15 H 0.1546 0.3454 0.1978 0.089 Uiso 1 1 calc R . . C16 C 0.2764(2) 0.3524(3) 0.2958(3) 0.0567(10) Uani 1 1 d . . . H16 H 0.2781 0.3556 0.3613 0.068 Uiso 1 1 calc R . . C17 C 0.4414(2) 0.2711(3) 0.5072(3) 0.0463(8) Uani 1 1 d . . . C18 C 0.4096(3) 0.2886(3) 0.5712(3) 0.0582(10) Uani 1 1 d . . . H18 H 0.3943 0.3482 0.5761 0.070 Uiso 1 1 calc R . . C19 C 0.4004(3) 0.2180(4) 0.6278(4) 0.0759(14) Uani 1 1 d . . . H19 H 0.3783 0.2299 0.6699 0.091 Uiso 1 1 calc R . . C20 C 0.4240(3) 0.1300(3) 0.6221(4) 0.0778(16) Uani 1 1 d . . . H20 H 0.4178 0.0825 0.6602 0.093 Uiso 1 1 calc R . . C21 C 0.4563(3) 0.1123(3) 0.5608(4) 0.0728(14) Uani 1 1 d . . . H21 H 0.4726 0.0528 0.5577 0.087 Uiso 1 1 calc R . . C22 C 0.4653(2) 0.1814(3) 0.5034(3) 0.0592(11) Uani 1 1 d . . . H22 H 0.4875 0.1684 0.4617 0.071 Uiso 1 1 calc R . . B B 0.0000 0.3744(5) 0.7500 0.0516(15) Uani 1 2 d S . . H1 H 0.488(2) 0.321(2) 0.397(3) 0.044(10) 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 Co 0.0271(3) 0.0426(4) 0.0331(3) 0.0007(3) 0.0138(2) 0.0014(3) S1 0.0372(4) 0.0561(6) 0.0381(4) 0.0051(4) 0.0148(4) -0.0032(4) S2 0.0329(4) 0.0616(6) 0.0475(5) -0.0028(4) 0.0202(4) 0.0052(4) P 0.0350(4) 0.0453(5) 0.0411(5) -0.0046(4) 0.0198(4) -0.0011(4) N 0.0401(17) 0.060(2) 0.058(2) 0.0114(17) 0.0137(15) 0.0110(16) C1 0.0385(18) 0.0385(19) 0.048(2) 0.0017(15) 0.0154(16) 0.0037(15) C2 0.057(3) 0.084(3) 0.056(3) 0.019(2) 0.007(2) 0.013(3) C3 0.038(2) 0.081(3) 0.084(3) 0.002(3) 0.017(2) 0.018(2) C11 0.045(2) 0.044(2) 0.0416(19) -0.0043(16) 0.0191(16) -0.0089(16) C12 0.065(3) 0.066(3) 0.046(2) -0.0118(19) 0.030(2) -0.022(2) C13 0.089(4) 0.090(4) 0.037(2) -0.008(2) 0.022(2) -0.029(3) C14 0.062(3) 0.095(4) 0.049(3) 0.001(2) 0.004(2) -0.030(3) C15 0.047(2) 0.096(4) 0.064(3) 0.006(3) 0.018(2) -0.017(2) C16 0.046(2) 0.070(3) 0.047(2) 0.0033(19) 0.0198(18) -0.010(2) C17 0.0413(19) 0.040(2) 0.0423(19) 0.0002(15) 0.0122(16) -0.0015(16) C18 0.073(3) 0.049(2) 0.056(2) 0.0040(19) 0.037(2) 0.000(2) C19 0.095(4) 0.071(3) 0.058(3) 0.015(2) 0.039(3) -0.006(3) C20 0.081(3) 0.059(3) 0.055(3) 0.019(2) 0.011(3) -0.016(3) C21 0.073(3) 0.043(2) 0.061(3) 0.006(2) 0.008(2) 0.004(2) C22 0.048(2) 0.052(2) 0.055(2) -0.0073(19) 0.0119(19) 0.0014(19) B 0.058(4) 0.046(4) 0.058(4) 0.000 0.036(3) 0.000 _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 Co S1 2.2688(10) . ? Co S2 2.2690(10) . ? Co P 2.2757(11) . ? S1 C1 1.713(4) . ? S2 C1 1.722(4) . ? P C17 1.810(4) . ? P C11 1.821(4) . ? P H1 1.21(3) . ? N C1 1.319(4) . ? N C3 1.451(5) . ? N C2 1.459(5) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C11 C16 1.389(5) . ? C11 C12 1.399(5) . ? C12 C13 1.376(6) . ? C12 H12 0.9300 . ? C13 C14 1.365(7) . ? C13 H13 0.9300 . ? C14 C15 1.375(7) . ? C14 H14 0.9300 . ? C15 C16 1.387(6) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.383(5) . ? C17 C22 1.395(5) . ? C18 C19 1.382(6) . ? C18 H18 0.9300 . ? C19 C20 1.376(7) . ? C19 H19 0.9300 . ? C20 C21 1.357(7) . ? C20 H20 0.9300 . ? C21 C22 1.370(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? F1 B 1.369(7) . ? F2 B 1.371(10) . ? F3 B 1.354(14) . ? F4 B 1.366(12) . ? F5 B 1.352(14) . ? F6 B 1.406(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 S1 Co S1 180.0 5_666 . ? S1 Co S2 102.97(4) 5_666 . ? S1 Co S2 77.03(4) . . ? S2 Co S2 180.0 . 5_666 ? S1 Co P 92.44(4) . . ? S2 Co P 90.63(4) . . ? S2 Co P 89.37(4) 5_666 . ? S1 Co P 87.56(4) . 5_666 ? P Co P 180.0 5_666 . ? C1 S1 Co 85.95(13) . . ? C1 S2 Co 85.73(13) . . ? C17 P C11 102.77(17) . . ? C17 P Co 119.40(12) . . ? C11 P Co 119.96(13) . . ? C17 P H1 99.3(16) . . ? C11 P H1 100.3(16) . . ? Co P H1 111.6(16) . . ? C1 N C3 121.7(4) . . ? C1 N C2 121.3(4) . . ? C3 N C2 116.9(3) . . ? N C1 S1 124.9(3) . . ? N C1 S2 124.4(3) . . ? S1 C1 S2 110.70(19) . . ? N C2 H2A 109.5 . . ? N C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N C3 H3A 109.5 . . ? N C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C16 C11 C12 118.4(4) . . ? C16 C11 P 122.3(3) . . ? C12 C11 P 119.3(3) . . ? C13 C12 C11 119.7(4) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C14 C13 C12 121.4(4) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 119.8(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 119.9(5) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C11 120.8(4) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? C18 C17 C22 118.4(4) . . ? C18 C17 P 121.3(3) . . ? C22 C17 P 120.2(3) . . ? C19 C18 C17 120.3(4) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C18 120.1(5) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 120.1(4) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.6(4) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C17 120.5(5) . . ? C21 C22 H22 119.7 . . ? C17 C22 H22 119.7 . . ? F1 B F1 114.9(7) . 2_556 ? F1 B F2 104.7(5) . . ? F1 B F2 116.1(5) . 2_556 ? F2 B F2 99.6(10) 2_556 . ? F3 B F4 122.3(6) . . ? F5 B F3 107.3(7) . . ? F3 B F6 96.9(7) . . ? F5 B F4 98.7(9) . 2_556 ? F4 B F6 119.0(9) . 2_556 ? F5 B F6 112.8(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 Co S1 C1 -159(11) 5_666 . . . ? S2 Co S1 C1 4.94(13) . . . . ? P Co S1 C1 95.03(13) . . . . ? S1 Co S2 C1 -4.92(13) . . . . ? S2 Co S2 C1 -145(13) 5_666 . . . ? P Co S2 C1 -97.28(13) . . . . ? S1 Co P C17 20.15(15) . . . . ? S2 Co P C17 97.19(15) . . . . ? P Co P C17 142(33) 5_666 . . . ? S1 Co P C11 148.30(15) . . . . ? S2 Co P C11 -134.66(15) . . . . ? P Co P C11 -90(33) 5_666 . . . ? C3 N C1 S1 -179.0(3) . . . . ? C2 N C1 S1 -3.1(6) . . . . ? C3 N C1 S2 -0.8(6) . . . . ? C2 N C1 S2 175.1(3) . . . . ? Co S1 C1 N 171.6(3) . . . . ? Co S1 C1 S2 -6.79(17) . . . . ? Co S2 C1 N -171.6(3) . . . . ? Co S2 C1 S1 6.79(17) . . . . ? C17 P C11 C16 49.7(4) . . . . ? Co P C11 C16 -85.6(3) . . . . ? C17 P C11 C12 -130.6(3) . . . . ? Co P C11 C12 94.0(3) . . . . ? C16 C11 C12 C13 -0.2(6) . . . . ? P C11 C12 C13 -179.9(4) . . . . ? C11 C12 C13 C14 0.0(8) . . . . ? C12 C13 C14 C15 -0.2(8) . . . . ? C13 C14 C15 C16 0.6(8) . . . . ? C14 C15 C16 C11 -0.8(8) . . . . ? C12 C11 C16 C15 0.6(7) . . . . ? P C11 C16 C15 -179.8(4) . . . . ? C11 P C17 C18 -86.9(3) . . . . ? Co P C17 C18 48.7(4) . . . . ? C11 P C17 C22 89.6(3) . . . . ? Co P C17 C22 -134.7(3) . . . . ? C22 C17 C18 C19 -1.3(6) . . . . ? P C17 C18 C19 175.3(3) . . . . ? C17 C18 C19 C20 0.9(7) . . . . ? C18 C19 C20 C21 0.0(8) . . . . ? C19 C20 C21 C22 -0.5(7) . . . . ? C20 C21 C22 C17 0.1(7) . . . . ? C18 C17 C22 C21 0.8(6) . . . . ? P C17 C22 C21 -175.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.500 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.075 #===END