Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Hideo D. Takagi' 'Shigenobu Funahashi' 'Satoshi Iwatsuki' 'Shinsaku Kashiwamura' 'Kazuo Kashuwabara' 'Takayoshi Suzuki' _publ_contact_author_name 'Dr Hideo D. Takagi' _publ_contact_author_address ; Department of Chemistry and Physics Nagoya University Furocho, Chikusa Nagoya City Aichi Prefecture 464-8602 JAPAN ; _publ_contact_author_email HTAKAGI@CHEM.NAGOYA-U.AC.JP _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Syntheses, Crystal Structures and Isomerization Kinetics of a Series of [Co(dtc)2{P(OMe)3|nPhn}2]+ (n = 0-2) Complexes (dtc-|= N,N-dimethyldithiocarbamate): Role of o-Donicity, n-Acidity, and Cone Angle of P-Ligands in the Trans Influence and Trans Effect ; data_cisPOMe3 _database_code_CSD 206913 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis-Bis(N,N-dimethyldithiocarbamato)bis(trimethylphosphite)cobalt(III) Tetrafluoroborate ; _chemical_name_common cis-[Co(dtc)~2~(P(OMe)~3~)~2~]BF~4~ _chemical_melting_point ? _chemical_formula_moiety 'C12 H30 Co N2 O6 P2 S4 1+, B F4 1-' _chemical_formula_sum 'C12 H30 B Co F4 N2 O6 P2 S4' _chemical_formula_weight 634.30 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 7.323(4) _cell_length_b 13.349(3) _cell_length_c 26.733(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.56(2) _cell_angle_gamma 90.00 _cell_volume 2600.9(15) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 _exptl_crystal_description column _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 1.163 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.718 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_process_details 'Coppens numerical' _exptl_special_details none _diffrn_ambient_temperature 296(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 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.98 _diffrn_reflns_number 8124 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.1276 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 30.00 _reflns_number_total 7587 _reflns_number_gt 3441 _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. 11' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP in teXsan' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0500P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7587 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1679 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1343 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.002 _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 0.81356(7) 0.78859(4) 0.894933(17) 0.03091(12) Uani 1 1 d . . . S1 S 1.10445(13) 0.73120(8) 0.91398(4) 0.0388(2) Uani 1 1 d . . . S2 S 0.80571(13) 0.71023(8) 0.97105(4) 0.0401(2) Uani 1 1 d . . . S3 S 0.53427(14) 0.85887(8) 0.90006(4) 0.0406(2) Uani 1 1 d . . . S4 S 0.87823(14) 0.93889(8) 0.93455(4) 0.0422(2) Uani 1 1 d . . . P1 P 0.69743(14) 0.65223(7) 0.85816(4) 0.0355(2) Uani 1 1 d . . . P2 P 0.87978(14) 0.86628(7) 0.82638(4) 0.0361(2) Uani 1 1 d . . . F1 F 1.1630(7) 0.7942(3) 0.60898(13) 0.1291(18) Uani 1 1 d . . . F2 F 1.2799(5) 0.8472(2) 0.68389(12) 0.0944(11) Uani 1 1 d . . . F3 F 1.1770(7) 0.6919(3) 0.67505(15) 0.1223(15) Uani 1 1 d . . . F4 F 1.4233(6) 0.7298(4) 0.64174(18) 0.1375(17) Uani 1 1 d . . . O1 O 0.5985(4) 0.6553(2) 0.80277(10) 0.0502(7) Uani 1 1 d . . . O2 O 0.5513(4) 0.6052(2) 0.89069(11) 0.0519(8) Uani 1 1 d . . . O3 O 0.8299(4) 0.5596(2) 0.85284(12) 0.0547(8) Uani 1 1 d . . . O4 O 0.8709(5) 0.7965(2) 0.77855(10) 0.0545(8) Uani 1 1 d . . . O5 O 1.0813(4) 0.9091(2) 0.83472(11) 0.0509(7) Uani 1 1 d . . . O6 O 0.7530(4) 0.9555(2) 0.80458(11) 0.0496(7) Uani 1 1 d . . . N1 N 1.1387(5) 0.6401(3) 1.00467(12) 0.0466(8) Uani 1 1 d . . . N2 N 0.5639(5) 1.0419(3) 0.94170(13) 0.0496(9) Uani 1 1 d . . . C1 C 1.0327(5) 0.6865(3) 0.96889(14) 0.0367(8) Uani 1 1 d . . . C2 C 1.3303(6) 0.6162(4) 0.99897(18) 0.0592(12) Uani 1 1 d . . . H2A H 1.4053 0.6349 1.0290 0.073 Uiso 1 1 calc R . . H2B H 1.3694 0.6524 0.9709 0.073 Uiso 1 1 calc R . . H2C H 1.3422 0.5456 0.9933 0.073 Uiso 1 1 calc R . . C3 C 1.0671(7) 0.6078(4) 1.05119(16) 0.0666(14) Uani 1 1 d . . . H3A H 0.9610 0.6471 1.0567 0.080 Uiso 1 1 calc R . . H3B H 1.1595 0.6169 1.0788 0.080 Uiso 1 1 calc R . . H3C H 1.0336 0.5384 1.0486 0.080 Uiso 1 1 calc R . . C4 C 0.6467(5) 0.9599(3) 0.92839(14) 0.0384(9) Uani 1 1 d . . . C5 C 0.3637(7) 1.0523(4) 0.93378(18) 0.0611(13) Uani 1 1 d . . . H5A H 0.3233 1.0990 0.9577 0.074 Uiso 1 1 calc R . . H5B H 0.3075 0.9883 0.9381 0.074 Uiso 1 1 calc R . . H5C H 0.3295 1.0763 0.9003 0.074 Uiso 1 1 calc R . . C6 C 0.6690(8) 1.1279(3) 0.9619(2) 0.0712(15) Uani 1 1 d . . . H6A H 0.7670 1.1054 0.9857 0.086 Uiso 1 1 calc R . . H6B H 0.5901 1.1720 0.9783 0.086 Uiso 1 1 calc R . . H6C H 0.7191 1.1630 0.9350 0.086 Uiso 1 1 calc R . . C11 C 0.9637(7) 0.5571(4) 0.8166(2) 0.0716(15) Uani 1 1 d . . . H11A H 1.0217 0.4926 0.8173 0.085 Uiso 1 1 calc R . . H11B H 1.0546 0.6079 0.8247 0.085 Uiso 1 1 calc R . . H11C H 0.9037 0.5693 0.7836 0.085 Uiso 1 1 calc R . . C17 C 0.4535(7) 0.5135(3) 0.87421(19) 0.0649(14) Uani 1 1 d . . . H17A H 0.3606 0.4995 0.8962 0.078 Uiso 1 1 calc R . . H17B H 0.5385 0.4587 0.8751 0.078 Uiso 1 1 calc R . . H17C H 0.3973 0.5223 0.8405 0.078 Uiso 1 1 calc R . . C23 C 0.4463(6) 0.7214(4) 0.78947(18) 0.0611(13) Uani 1 1 d . . . H23A H 0.4908 0.7883 0.7858 0.074 Uiso 1 1 calc R . . H23B H 0.3644 0.7201 0.8154 0.074 Uiso 1 1 calc R . . H23C H 0.3820 0.6998 0.7583 0.074 Uiso 1 1 calc R . . C31 C 0.7679(8) 1.0587(3) 0.81938(19) 0.0693(15) Uani 1 1 d . . . H31A H 0.8944 1.0750 0.8285 0.085 Uiso 1 1 calc R . . H31B H 0.6989 1.0698 0.8476 0.085 Uiso 1 1 calc R . . H31C H 0.7203 1.1004 0.7919 0.085 Uiso 1 1 calc R . . C37 C 1.1749(6) 0.9560(4) 0.79571(18) 0.0623(13) Uani 1 1 d . . . H37A H 1.2987 0.9713 0.8085 0.077 Uiso 1 1 calc R . . H37B H 1.1122 1.0166 0.7851 0.077 Uiso 1 1 calc R . . H37C H 1.1757 0.9112 0.7677 0.077 Uiso 1 1 calc R . . C43 C 0.8330(8) 0.8247(4) 0.72672(17) 0.0693(15) Uani 1 1 d . . . H43A H 0.8610 0.8944 0.7229 0.086 Uiso 1 1 calc R . . H43B H 0.7056 0.8134 0.7162 0.086 Uiso 1 1 calc R . . H43C H 0.9070 0.7853 0.7065 0.086 Uiso 1 1 calc R . . B1 B 1.2602(9) 0.7672(4) 0.6510(2) 0.0619(15) 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 Co 0.0312(2) 0.0278(2) 0.0333(2) 0.0001(2) 0.00139(18) -0.0013(2) S1 0.0324(5) 0.0437(5) 0.0400(5) 0.0030(4) 0.0020(4) 0.0000(4) S2 0.0379(5) 0.0442(5) 0.0383(5) 0.0052(4) 0.0046(4) -0.0012(5) S3 0.0339(5) 0.0370(5) 0.0503(6) -0.0062(4) 0.0006(4) 0.0010(4) S4 0.0430(5) 0.0364(5) 0.0462(5) -0.0068(4) -0.0008(4) -0.0073(4) P1 0.0376(5) 0.0288(5) 0.0395(5) -0.0018(4) 0.0005(4) -0.0012(4) P2 0.0411(5) 0.0284(5) 0.0384(5) 0.0028(4) 0.0023(4) -0.0017(4) F1 0.204(5) 0.083(2) 0.086(2) -0.012(2) -0.057(3) 0.051(3) F2 0.133(3) 0.0500(18) 0.094(2) -0.0150(16) -0.018(2) -0.0024(19) F3 0.182(5) 0.066(2) 0.124(3) 0.002(2) 0.041(3) -0.032(3) F4 0.108(3) 0.132(4) 0.175(4) 0.003(3) 0.030(3) 0.049(3) O1 0.0562(19) 0.0472(18) 0.0446(16) -0.0038(13) -0.0082(14) 0.0009(14) O2 0.0597(19) 0.0455(17) 0.0512(17) -0.0068(14) 0.0094(14) -0.0211(15) O3 0.0553(18) 0.0348(15) 0.073(2) -0.0072(14) 0.0029(16) 0.0099(14) O4 0.087(2) 0.0368(15) 0.0410(15) -0.0016(12) 0.0152(15) -0.0038(16) O5 0.0424(16) 0.0563(18) 0.0539(17) 0.0167(15) 0.0032(13) -0.0108(14) O6 0.0549(18) 0.0339(15) 0.0581(18) 0.0095(13) -0.0032(14) 0.0066(14) N1 0.050(2) 0.045(2) 0.0432(19) 0.0043(16) -0.0034(15) 0.0087(17) N2 0.069(3) 0.0359(18) 0.0442(19) -0.0058(15) 0.0065(18) 0.0104(18) C1 0.039(2) 0.0327(19) 0.037(2) -0.0010(15) -0.0031(16) 0.0000(16) C2 0.053(3) 0.058(3) 0.064(3) -0.004(2) -0.007(2) 0.019(2) C3 0.077(4) 0.074(3) 0.047(3) 0.019(2) 0.000(2) 0.005(3) C4 0.048(2) 0.0315(19) 0.0351(19) -0.0007(15) 0.0014(17) 0.0004(17) C5 0.070(3) 0.053(3) 0.062(3) 0.005(2) 0.012(2) 0.030(3) C6 0.105(5) 0.034(2) 0.074(3) -0.014(2) 0.007(3) -0.001(3) C11 0.063(3) 0.068(3) 0.082(4) -0.028(3) 0.002(3) 0.020(3) C17 0.066(3) 0.049(3) 0.077(3) -0.003(2) -0.003(3) -0.028(3) C23 0.059(3) 0.058(3) 0.062(3) -0.002(2) -0.019(2) 0.006(3) C31 0.112(5) 0.033(2) 0.063(3) 0.005(2) 0.011(3) 0.021(3) C37 0.052(3) 0.069(3) 0.068(3) 0.021(3) 0.011(2) -0.013(3) C43 0.101(4) 0.064(3) 0.044(3) -0.004(2) 0.011(3) -0.015(3) B1 0.076(4) 0.043(3) 0.066(4) -0.001(3) 0.000(3) 0.010(3) _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 2.2003(11) . ? Co P1 2.2003(11) . ? Co S3 2.2663(15) . ? Co S1 2.2745(15) . ? Co S2 2.2937(11) . ? Co S4 2.2965(11) . ? S1 C1 1.714(4) . ? S2 C1 1.699(4) . ? S3 C4 1.717(4) . ? S4 C4 1.711(4) . ? P1 O2 1.574(3) . ? P1 O1 1.585(3) . ? P1 O3 1.587(3) . ? P2 O4 1.578(3) . ? P2 O5 1.578(3) . ? P2 O6 1.586(3) . ? F1 B1 1.322(7) . ? F2 B1 1.381(6) . ? F3 B1 1.368(7) . ? F4 B1 1.340(7) . ? O1 C23 1.439(5) . ? O2 C17 1.464(5) . ? O3 C11 1.444(5) . ? O4 C43 1.437(5) . ? O5 C37 1.445(5) . ? O6 C31 1.435(5) . ? N1 C1 1.325(5) . ? N1 C3 1.461(5) . ? N1 C2 1.461(5) . ? N2 C4 1.317(5) . ? N2 C6 1.456(6) . ? N2 C5 1.467(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 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 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 97.16(4) . . ? P2 Co S3 97.37(5) . . ? P1 Co S3 93.30(5) . . ? P2 Co S1 93.90(5) . . ? P1 Co S1 97.73(5) . . ? S3 Co S1 163.13(4) . . ? P2 Co S2 168.63(4) . . ? P1 Co S2 88.70(4) . . ? S3 Co S2 91.99(5) . . ? S1 Co S2 75.59(4) . . ? P2 Co S4 85.42(4) . . ? P1 Co S4 169.21(5) . . ? S3 Co S4 75.96(4) . . ? S1 Co S4 92.53(4) . . ? S2 Co S4 90.63(4) . . ? C1 S1 Co 87.19(14) . . ? C1 S2 Co 86.92(13) . . ? C4 S3 Co 87.41(14) . . ? C4 S4 Co 86.60(13) . . ? O2 P1 O1 104.64(17) . . ? O2 P1 O3 101.11(17) . . ? O1 P1 O3 99.48(17) . . ? O2 P1 Co 109.72(11) . . ? O1 P1 Co 121.20(12) . . ? O3 P1 Co 118.15(13) . . ? O4 P2 O5 107.00(18) . . ? O4 P2 O6 99.71(16) . . ? O5 P2 O6 106.64(17) . . ? O4 P2 Co 113.68(12) . . ? O5 P2 Co 109.36(11) . . ? O6 P2 Co 119.44(13) . . ? C23 O1 P1 121.3(3) . . ? C17 O2 P1 120.4(3) . . ? C11 O3 P1 122.5(3) . . ? C43 O4 P2 128.0(3) . . ? C37 O5 P2 123.9(3) . . ? C31 O6 P2 126.4(3) . . ? C1 N1 C3 121.2(4) . . ? C1 N1 C2 121.9(4) . . ? C3 N1 C2 116.9(4) . . ? C4 N2 C6 121.0(4) . . ? C4 N2 C5 121.3(4) . . ? C6 N2 C5 117.7(4) . . ? N1 C1 S2 124.7(3) . . ? N1 C1 S1 125.0(3) . . ? S2 C1 S1 110.3(2) . . ? 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 C4 S4 126.0(3) . . ? N2 C4 S3 123.9(3) . . ? S4 C4 S3 110.0(2) . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C11 H11A 109.5 . . ? O3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O2 C17 H17A 109.5 . . ? O2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O1 C23 H23A 109.5 . . ? O1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O6 C31 H31A 109.5 . . ? O6 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O6 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O5 C37 H37A 109.5 . . ? O5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O4 C43 H43A 109.5 . . ? O4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? F1 B1 F4 111.1(6) . . ? F1 B1 F3 111.9(6) . . ? F4 B1 F3 105.0(5) . . ? F1 B1 F2 110.1(4) . . ? F4 B1 F2 111.5(6) . . ? F3 B1 F2 107.1(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Co S1 C1 174.32(13) . . . . ? P1 Co S1 C1 -87.91(13) . . . . ? S3 Co S1 C1 42.4(2) . . . . ? S2 Co S1 C1 -1.26(13) . . . . ? S4 Co S1 C1 88.74(13) . . . . ? P2 Co S2 C1 -21.7(3) . . . . ? P1 Co S2 C1 99.59(13) . . . . ? S3 Co S2 C1 -167.16(13) . . . . ? S1 Co S2 C1 1.27(13) . . . . ? S4 Co S2 C1 -91.18(13) . . . . ? P2 Co S3 C4 -82.35(13) . . . . ? P1 Co S3 C4 179.99(13) . . . . ? S1 Co S3 C4 49.2(2) . . . . ? S2 Co S3 C4 91.18(13) . . . . ? S4 Co S3 C4 1.02(13) . . . . ? P2 Co S4 C4 97.76(13) . . . . ? P1 Co S4 C4 -6.5(3) . . . . ? S3 Co S4 C4 -1.03(13) . . . . ? S1 Co S4 C4 -168.53(13) . . . . ? S2 Co S4 C4 -92.92(13) . . . . ? P2 Co P1 O2 -151.76(14) . . . . ? S3 Co P1 O2 -53.90(14) . . . . ? S1 Co P1 O2 113.29(14) . . . . ? S2 Co P1 O2 38.02(14) . . . . ? S4 Co P1 O2 -48.6(3) . . . . ? P2 Co P1 O1 -29.70(15) . . . . ? S3 Co P1 O1 68.16(15) . . . . ? S1 Co P1 O1 -124.64(15) . . . . ? S2 Co P1 O1 160.08(15) . . . . ? S4 Co P1 O1 73.5(3) . . . . ? P2 Co P1 O3 93.16(15) . . . . ? S3 Co P1 O3 -168.98(15) . . . . ? S1 Co P1 O3 -1.79(15) . . . . ? S2 Co P1 O3 -77.06(15) . . . . ? S4 Co P1 O3 -163.6(2) . . . . ? P1 Co P2 O4 -13.36(15) . . . . ? S3 Co P2 O4 -107.65(15) . . . . ? S1 Co P2 O4 84.94(15) . . . . ? S2 Co P2 O4 107.2(3) . . . . ? S4 Co P2 O4 177.17(15) . . . . ? P1 Co P2 O5 -132.87(13) . . . . ? S3 Co P2 O5 132.84(13) . . . . ? S1 Co P2 O5 -34.57(14) . . . . ? S2 Co P2 O5 -12.3(3) . . . . ? S4 Co P2 O5 57.66(13) . . . . ? P1 Co P2 O6 103.97(14) . . . . ? S3 Co P2 O6 9.69(14) . . . . ? S1 Co P2 O6 -157.73(14) . . . . ? S2 Co P2 O6 -135.5(2) . . . . ? S4 Co P2 O6 -65.49(14) . . . . ? O2 P1 O1 C23 68.5(4) . . . . ? O3 P1 O1 C23 172.8(3) . . . . ? Co P1 O1 C23 -55.9(4) . . . . ? O1 P1 O2 C17 48.4(4) . . . . ? O3 P1 O2 C17 -54.6(4) . . . . ? Co P1 O2 C17 179.9(3) . . . . ? O2 P1 O3 C11 165.4(3) . . . . ? O1 P1 O3 C11 58.3(4) . . . . ? Co P1 O3 C11 -74.9(4) . . . . ? O5 P2 O4 C43 -86.4(4) . . . . ? O6 P2 O4 C43 24.5(4) . . . . ? Co P2 O4 C43 152.8(4) . . . . ? O4 P2 O5 C37 50.3(4) . . . . ? O6 P2 O5 C37 -55.7(4) . . . . ? Co P2 O5 C37 173.9(3) . . . . ? O4 P2 O6 C31 -149.9(4) . . . . ? O5 P2 O6 C31 -38.7(4) . . . . ? Co P2 O6 C31 85.8(4) . . . . ? C3 N1 C1 S2 -2.3(6) . . . . ? C2 N1 C1 S2 175.9(3) . . . . ? C3 N1 C1 S1 177.6(3) . . . . ? C2 N1 C1 S1 -4.2(6) . . . . ? Co S2 C1 N1 178.2(3) . . . . ? Co S2 C1 S1 -1.74(18) . . . . ? Co S1 C1 N1 -178.1(3) . . . . ? Co S1 C1 S2 1.76(18) . . . . ? C6 N2 C4 S4 2.8(6) . . . . ? C5 N2 C4 S4 178.9(3) . . . . ? C6 N2 C4 S3 -175.0(3) . . . . ? C5 N2 C4 S3 1.1(6) . . . . ? Co S4 C4 N2 -176.7(4) . . . . ? Co S4 C4 S3 1.40(18) . . . . ? Co S3 C4 N2 176.7(3) . . . . ? Co S3 C4 S4 -1.42(18) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.550 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.098 #===END data_cisPPhOMe2 _database_code_CSD 206914 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis-Bis(dimethyldithiocarbamato)bis(dimethyl phenylphosphonito)cobalt(III) Hexafluorophosphate ; _chemical_name_common cis-[Co(dtc)~2~{P(OMe)~2~Ph}~2~]PF~6~ _chemical_melting_point ? _chemical_formula_moiety 'C22 H34 Co N2 O4 P2 S4 1+, F6 P 1-' _chemical_formula_sum 'C22 H34 Co F6 N2 O4 P3 S4' _chemical_formula_weight 784.59 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 11.732(3) _cell_length_b 19.827(5) _cell_length_c 14.553(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.91(2) _cell_angle_gamma 90.00 _cell_volume 3372.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.9 _cell_measurement_theta_max 14.7 _exptl_crystal_description prism _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.963 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.964 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details none _diffrn_ambient_temperature 296(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_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.51 _diffrn_reflns_number 8092 _diffrn_reflns_av_R_equivalents 0.1070 _diffrn_reflns_av_sigmaI/netI 0.5270 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7728 _reflns_number_gt 1687 _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. 1.11' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP in teXsan' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7728 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3883 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1318 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.012 _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 0.78059(9) 0.11973(6) 0.10945(7) 0.0447(3) Uani 1 1 d . . . S1 S 0.64138(17) 0.07894(11) 0.00755(15) 0.0502(6) Uani 1 1 d . . . S2 S 0.87820(18) 0.05461(11) 0.01309(15) 0.0486(6) Uani 1 1 d . . . S3 S 0.94138(19) 0.16452(12) 0.18233(15) 0.0576(7) Uani 1 1 d . . . S4 S 0.8189(2) 0.21045(12) 0.01937(15) 0.0550(7) Uani 1 1 d . . . P1 P 0.7654(2) 0.02960(13) 0.19834(17) 0.0557(7) Uani 1 1 d . . . P2 P 0.6714(2) 0.18414(12) 0.19008(15) 0.0508(7) Uani 1 1 d . . . P3 P 0.3018(3) 0.1132(2) 0.4381(3) 0.1036(11) Uani 1 1 d . . . F1 F 0.2709(8) 0.1416(4) 0.5279(5) 0.204(4) Uani 1 1 d . . . F2 F 0.3734(8) 0.1768(4) 0.4266(8) 0.238(5) Uani 1 1 d . . . F3 F 0.1994(8) 0.1495(5) 0.3854(6) 0.219(5) Uani 1 1 d . . . F4 F 0.4067(7) 0.0752(5) 0.4791(6) 0.237(5) Uani 1 1 d . . . F5 F 0.2256(8) 0.0541(4) 0.4529(7) 0.228(5) Uani 1 1 d . . . F6 F 0.3409(9) 0.0880(4) 0.3462(5) 0.209(4) Uani 1 1 d . . . O1 O 0.6481(5) 0.0295(3) 0.2463(4) 0.0615(17) Uani 1 1 d . . . O2 O 0.8675(5) 0.0201(4) 0.2749(4) 0.088(2) Uani 1 1 d . . . O4 O 0.6905(5) 0.1656(3) 0.2966(4) 0.0722(19) Uani 1 1 d . . . O5 O 0.5419(4) 0.1740(3) 0.1542(4) 0.0640(17) Uani 1 1 d . . . N1 N 0.7305(6) -0.0094(3) -0.1089(5) 0.0489(19) Uani 1 1 d . . . N2 N 1.0024(7) 0.2760(4) 0.0945(5) 0.071(2) Uani 1 1 d . . . C1 C 0.7467(6) 0.0341(4) -0.0419(5) 0.041(2) Uani 1 1 d . . . C2 C 0.6170(7) -0.0240(4) -0.1518(6) 0.073(3) Uani 1 1 d . . . H2A H 0.5768 0.0175 -0.1652 0.087 Uiso 1 1 calc R . . H2B H 0.5759 -0.0506 -0.1105 0.087 Uiso 1 1 calc R . . H2C H 0.6233 -0.0485 -0.2080 0.087 Uiso 1 1 calc R . . C3 C 0.8233(6) -0.0507(4) -0.1415(5) 0.056(2) Uani 1 1 d . . . H3A H 0.8337 -0.0903 -0.1038 0.071 Uiso 1 1 calc R . . H3B H 0.8928 -0.0250 -0.1375 0.071 Uiso 1 1 calc R . . H3C H 0.8037 -0.0637 -0.2044 0.071 Uiso 1 1 calc R . . C4 C 0.9324(7) 0.2243(4) 0.0976(6) 0.055(2) Uani 1 1 d . . . C5 C 1.1004(8) 0.2838(5) 0.1657(6) 0.110(4) Uani 1 1 d . . . H5A H 1.1577 0.2507 0.1557 0.134 Uiso 1 1 calc R . . H5B H 1.0743 0.2777 0.2259 0.134 Uiso 1 1 calc R . . H5C H 1.1324 0.3282 0.1614 0.134 Uiso 1 1 calc R . . C6 C 0.9832(9) 0.3280(5) 0.0239(7) 0.118(5) Uani 1 1 d . . . H6A H 1.0216 0.3687 0.0446 0.127 Uiso 1 1 calc R . . H6B H 0.9026 0.3366 0.0128 0.127 Uiso 1 1 calc R . . H6C H 1.0127 0.3130 -0.0321 0.127 Uiso 1 1 calc R . . C11 C 0.7710(9) -0.0536(5) 0.1462(6) 0.062(3) Uani 1 1 d . . . C12 C 0.6672(9) -0.0846(5) 0.1123(7) 0.076(3) Uani 1 1 d . . . H12 H 0.5974 -0.0632 0.1168 0.085 Uiso 1 1 calc R . . C13 C 0.6726(11) -0.1491(5) 0.0714(7) 0.098(4) Uani 1 1 d . . . H13 H 0.6048 -0.1702 0.0496 0.115 Uiso 1 1 calc R . . C14 C 0.7725(12) -0.1809(5) 0.0628(8) 0.100(4) Uani 1 1 d . . . H14 H 0.7731 -0.2229 0.0346 0.118 Uiso 1 1 calc R . . C15 C 0.8734(11) -0.1509(6) 0.0957(7) 0.093(4) Uani 1 1 d . . . H15 H 0.9427 -0.1728 0.0905 0.114 Uiso 1 1 calc R . . C16 C 0.8712(8) -0.0884(6) 0.1365(7) 0.075(3) Uani 1 1 d . . . H16 H 0.9401 -0.0687 0.1585 0.090 Uiso 1 1 calc R . . C17 C 0.8981(9) 0.0486(6) 0.3515(7) 0.153(6) Uani 1 1 d . . . H17A H 0.9058 0.0152 0.3994 0.163 Uiso 1 1 calc R . . H17B H 0.8414 0.0810 0.3654 0.163 Uiso 1 1 calc R . . H17C H 0.9701 0.0709 0.3474 0.163 Uiso 1 1 calc R . . C23 C 0.6245(8) -0.0168(5) 0.3202(6) 0.107(4) Uani 1 1 d . . . H23A H 0.5502 -0.0073 0.3400 0.136 Uiso 1 1 calc R . . H23B H 0.6813 -0.0112 0.3711 0.136 Uiso 1 1 calc R . . H23C H 0.6264 -0.0624 0.2980 0.136 Uiso 1 1 calc R . . C31 C 0.6938(7) 0.2749(4) 0.1892(6) 0.048(2) Uani 1 1 d . . . C32 C 0.6362(8) 0.3161(5) 0.1232(6) 0.069(3) Uani 1 1 d . . . H32 H 0.5805 0.2979 0.0810 0.085 Uiso 1 1 calc R . . C33 C 0.6621(9) 0.3845(6) 0.1203(7) 0.083(3) Uani 1 1 d . . . H33 H 0.6251 0.4121 0.0754 0.096 Uiso 1 1 calc R . . C34 C 0.7422(10) 0.4109(5) 0.1839(8) 0.082(3) Uani 1 1 d . . . H34 H 0.7592 0.4567 0.1818 0.095 Uiso 1 1 calc R . . C35 C 0.7978(9) 0.3719(6) 0.2501(7) 0.084(3) Uani 1 1 d . . . H35 H 0.8529 0.3909 0.2920 0.105 Uiso 1 1 calc R . . C36 C 0.7720(7) 0.3022(4) 0.2556(6) 0.060(3) Uani 1 1 d . . . H36 H 0.8068 0.2755 0.3025 0.082 Uiso 1 1 calc R . . C37 C 0.4431(7) 0.2112(4) 0.1813(6) 0.082(3) Uani 1 1 d . . . H37A H 0.4679 0.2533 0.2089 0.097 Uiso 1 1 calc R . . H37B H 0.4050 0.1851 0.2251 0.097 Uiso 1 1 calc R . . H37C H 0.3913 0.2197 0.1279 0.097 Uiso 1 1 calc R . . C43 C 0.6212(8) 0.1841(5) 0.3668(6) 0.103(4) Uani 1 1 d . . . H43A H 0.6046 0.2315 0.3623 0.119 Uiso 1 1 calc R . . H43B H 0.6607 0.1746 0.4259 0.119 Uiso 1 1 calc R . . H43C H 0.5510 0.1590 0.3600 0.119 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 Co 0.0430(7) 0.0454(7) 0.0456(7) -0.0002(6) 0.0025(5) 0.0003(6) S1 0.0361(13) 0.0588(17) 0.0555(15) -0.0088(12) 0.0030(11) 0.0064(12) S2 0.0391(13) 0.0497(16) 0.0566(15) -0.0025(12) 0.0024(11) 0.0019(12) S3 0.0522(16) 0.0613(17) 0.0582(16) -0.0030(13) -0.0009(12) -0.0061(13) S4 0.0679(17) 0.0458(15) 0.0527(15) 0.0041(12) 0.0131(13) 0.0014(13) P1 0.0539(16) 0.0568(18) 0.0558(17) 0.0060(14) 0.0012(13) -0.0040(14) P2 0.0520(16) 0.0542(17) 0.0462(16) -0.0068(13) 0.0045(12) -0.0028(13) P3 0.109(3) 0.099(3) 0.107(3) 0.005(3) 0.035(2) 0.016(3) F1 0.247(10) 0.222(11) 0.152(8) -0.070(7) 0.074(7) 0.025(8) F2 0.202(10) 0.104(7) 0.431(16) -0.003(9) 0.147(10) -0.010(7) F3 0.166(9) 0.226(10) 0.250(10) 0.077(9) -0.064(8) 0.031(8) F4 0.168(8) 0.301(13) 0.249(10) 0.125(9) 0.057(7) 0.133(9) F5 0.192(9) 0.136(8) 0.372(15) -0.008(9) 0.119(9) -0.081(7) F6 0.332(12) 0.203(10) 0.102(6) -0.055(6) 0.079(7) 0.015(9) O1 0.073(4) 0.062(4) 0.051(4) 0.010(3) 0.014(3) 0.002(4) O2 0.082(5) 0.125(7) 0.052(5) 0.001(4) -0.021(4) -0.016(5) O4 0.111(5) 0.065(5) 0.043(4) -0.005(3) 0.020(4) -0.002(4) O5 0.045(4) 0.062(4) 0.087(5) -0.026(4) 0.015(3) -0.008(3) N1 0.044(4) 0.058(5) 0.044(4) -0.016(4) 0.006(4) -0.003(4) N2 0.078(6) 0.058(6) 0.080(6) -0.012(5) 0.020(5) -0.019(5) C1 0.053(5) 0.047(6) 0.024(5) 0.008(4) 0.006(4) 0.003(5) C2 0.050(6) 0.090(9) 0.082(7) -0.022(6) 0.016(6) 0.003(6) C3 0.049(6) 0.050(6) 0.071(7) -0.008(5) 0.024(5) 0.002(5) C4 0.048(6) 0.045(6) 0.074(7) -0.006(5) 0.024(5) 0.000(5) C5 0.105(10) 0.116(11) 0.110(10) -0.034(8) 0.011(8) -0.058(8) C6 0.122(10) 0.074(9) 0.166(12) 0.025(9) 0.062(9) -0.037(8) C11 0.060(7) 0.066(7) 0.063(7) 0.017(5) 0.014(5) -0.005(6) C12 0.076(8) 0.046(7) 0.107(9) 0.011(6) 0.005(7) 0.001(6) C13 0.112(10) 0.035(7) 0.148(11) -0.026(7) 0.017(9) -0.014(7) C14 0.128(12) 0.026(7) 0.150(12) -0.003(7) 0.035(10) 0.003(8) C15 0.105(11) 0.065(9) 0.114(10) 0.001(7) 0.036(8) 0.038(8) C16 0.052(7) 0.091(9) 0.083(8) 0.038(7) 0.002(6) 0.014(7) C17 0.120(11) 0.240(18) 0.093(10) -0.014(11) -0.034(9) -0.007(11) C23 0.105(9) 0.124(11) 0.094(9) 0.042(8) 0.022(7) -0.039(8) C31 0.046(5) 0.047(6) 0.051(6) -0.013(5) 0.008(5) -0.004(5) C32 0.072(7) 0.081(9) 0.055(7) 0.014(6) 0.010(5) 0.038(7) C33 0.119(10) 0.064(8) 0.068(8) 0.018(7) 0.026(7) 0.026(8) C34 0.115(10) 0.049(7) 0.086(9) -0.006(7) 0.029(7) -0.001(7) C35 0.096(9) 0.066(8) 0.087(8) -0.017(7) -0.006(7) 0.002(7) C36 0.066(7) 0.044(7) 0.072(7) -0.017(5) 0.012(5) 0.001(5) C37 0.067(7) 0.071(8) 0.112(9) -0.012(7) 0.021(6) 0.005(6) C43 0.116(10) 0.130(11) 0.068(8) -0.010(7) 0.033(7) -0.041(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co P2 2.214(3) . ? Co P1 2.222(3) . ? Co S1 2.260(2) . ? Co S3 2.265(2) . ? Co S2 2.285(2) . ? Co S4 2.293(3) . ? S1 C1 1.728(7) . ? S2 C1 1.725(7) . ? S3 C4 1.707(8) . ? S4 C4 1.699(8) . ? P1 O2 1.576(6) . ? P1 O1 1.596(6) . ? P1 C11 1.819(9) . ? P2 O5 1.577(5) . ? P2 O4 1.591(6) . ? P2 C31 1.818(8) . ? P3 F1 1.495(7) . ? P3 F5 1.500(7) . ? P3 F4 1.521(8) . ? P3 F2 1.533(8) . ? P3 F6 1.534(7) . ? P3 F3 1.546(8) . ? O1 C23 1.457(9) . ? O2 C17 1.273(10) . ? O4 C43 1.408(9) . ? O5 C37 1.457(8) . ? N1 C1 1.304(8) . ? N1 C2 1.450(9) . ? N1 C3 1.472(8) . ? N2 C4 1.316(9) . ? N2 C6 1.460(10) . ? N2 C5 1.488(10) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C11 C16 1.380(11) . ? C11 C12 1.415(11) . ? C12 C13 1.414(11) . ? C12 H12 0.9300 . ? C13 C14 1.345(13) . ? C13 H13 0.9300 . ? C14 C15 1.374(13) . ? C14 H14 0.9300 . ? C15 C16 1.377(12) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C31 C36 1.383(10) . ? C31 C32 1.392(10) . ? C32 C33 1.393(12) . ? C32 H32 0.9300 . ? C33 C34 1.366(12) . ? C33 H33 0.9300 . ? C34 C35 1.358(12) . ? C34 H34 0.9300 . ? C35 C36 1.419(11) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 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 94.39(10) . . ? P2 Co S1 97.81(9) . . ? P1 Co S1 90.28(10) . . ? P2 Co S3 91.26(9) . . ? P1 Co S3 98.49(10) . . ? S1 Co S3 166.88(10) . . ? P2 Co S2 173.72(10) . . ? P1 Co S2 88.41(10) . . ? S1 Co S2 76.53(8) . . ? S3 Co S2 93.89(9) . . ? P2 Co S4 90.06(10) . . ? P1 Co S4 173.29(10) . . ? S1 Co S4 94.10(9) . . ? S3 Co S4 76.35(9) . . ? S2 Co S4 87.67(9) . . ? C1 S1 Co 87.4(3) . . ? C1 S2 Co 86.7(3) . . ? C4 S3 Co 86.4(3) . . ? C4 S4 Co 85.7(3) . . ? O2 P1 O1 108.8(3) . . ? O2 P1 C11 97.7(4) . . ? O1 P1 C11 104.1(4) . . ? O2 P1 Co 114.4(3) . . ? O1 P1 Co 111.8(2) . . ? C11 P1 Co 118.6(3) . . ? O5 P2 O4 110.2(3) . . ? O5 P2 C31 105.0(4) . . ? O4 P2 C31 103.1(4) . . ? O5 P2 Co 109.6(2) . . ? O4 P2 Co 110.1(3) . . ? C31 P2 Co 118.5(3) . . ? F1 P3 F5 88.6(5) . . ? F1 P3 F4 95.3(6) . . ? F5 P3 F4 91.7(5) . . ? F1 P3 F2 87.8(6) . . ? F5 P3 F2 175.7(6) . . ? F4 P3 F2 91.0(6) . . ? F1 P3 F6 175.6(6) . . ? F5 P3 F6 95.6(6) . . ? F4 P3 F6 83.5(5) . . ? F2 P3 F6 88.0(5) . . ? F1 P3 F3 91.2(5) . . ? F5 P3 F3 89.2(6) . . ? F4 P3 F3 173.4(6) . . ? F2 P3 F3 88.5(5) . . ? F6 P3 F3 89.8(5) . . ? C23 O1 P1 123.3(6) . . ? C17 O2 P1 134.9(8) . . ? C43 O4 P2 127.2(6) . . ? C37 O5 P2 127.8(5) . . ? C1 N1 C2 121.6(7) . . ? C1 N1 C3 123.0(7) . . ? C2 N1 C3 115.3(6) . . ? C4 N2 C6 121.0(9) . . ? C4 N2 C5 120.3(9) . . ? C6 N2 C5 118.6(8) . . ? N1 C1 S2 124.7(6) . . ? N1 C1 S1 126.0(6) . . ? S2 C1 S1 109.2(4) . . ? 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 C4 S4 123.9(7) . . ? N2 C4 S3 124.4(7) . . ? S4 C4 S3 111.6(5) . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C16 C11 C12 117.5(9) . . ? C16 C11 P1 123.9(9) . . ? C12 C11 P1 118.6(8) . . ? C13 C12 C11 118.2(10) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? C14 C13 C12 122.2(11) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C13 C14 C15 119.8(11) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 119.4(11) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C11 122.9(11) . . ? C15 C16 H16 118.6 . . ? C11 C16 H16 118.6 . . ? O2 C17 H17A 109.5 . . ? O2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O1 C23 H23A 109.5 . . ? O1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C36 C31 C32 120.5(8) . . ? C36 C31 P2 118.0(7) . . ? C32 C31 P2 121.5(8) . . ? C31 C32 C33 119.9(10) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 119.5(10) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C35 C34 C33 121.6(10) . . ? C35 C34 H34 119.2 . . ? C33 C34 H34 119.2 . . ? C34 C35 C36 120.2(10) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C31 C36 C35 118.3(9) . . ? C31 C36 H36 120.9 . . ? C35 C36 H36 120.9 . . ? O5 C37 H37A 109.5 . . ? O5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O4 C43 H43A 109.5 . . ? O4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Co S1 C1 179.8(3) . . . . ? P1 Co S1 C1 -85.7(3) . . . . ? S3 Co S1 C1 46.5(5) . . . . ? S2 Co S1 C1 2.6(3) . . . . ? S4 Co S1 C1 89.2(3) . . . . ? P2 Co S2 C1 -28.5(10) . . . . ? P1 Co S2 C1 88.0(3) . . . . ? S1 Co S2 C1 -2.6(3) . . . . ? S3 Co S2 C1 -173.5(3) . . . . ? S4 Co S2 C1 -97.4(3) . . . . ? P2 Co S3 C4 -88.9(3) . . . . ? P1 Co S3 C4 176.5(3) . . . . ? S1 Co S3 C4 45.0(5) . . . . ? S2 Co S3 C4 87.5(3) . . . . ? S4 Co S3 C4 0.9(3) . . . . ? P2 Co S4 C4 90.4(3) . . . . ? P1 Co S4 C4 -41.2(10) . . . . ? S1 Co S4 C4 -171.7(3) . . . . ? S3 Co S4 C4 -0.9(3) . . . . ? S2 Co S4 C4 -95.4(3) . . . . ? P2 Co P1 O2 -96.4(3) . . . . ? S1 Co P1 O2 165.7(3) . . . . ? S3 Co P1 O2 -4.5(3) . . . . ? S2 Co P1 O2 89.2(3) . . . . ? S4 Co P1 O2 35.0(10) . . . . ? P2 Co P1 O1 27.8(3) . . . . ? S1 Co P1 O1 -70.0(3) . . . . ? S3 Co P1 O1 119.8(3) . . . . ? S2 Co P1 O1 -146.5(3) . . . . ? S4 Co P1 O1 159.3(9) . . . . ? P2 Co P1 C11 149.0(4) . . . . ? S1 Co P1 C11 51.1(4) . . . . ? S3 Co P1 C11 -119.1(4) . . . . ? S2 Co P1 C11 -25.4(4) . . . . ? S4 Co P1 C11 -79.6(10) . . . . ? P1 Co P2 O5 -86.4(3) . . . . ? S1 Co P2 O5 4.4(3) . . . . ? S3 Co P2 O5 174.9(3) . . . . ? S2 Co P2 O5 29.8(10) . . . . ? S4 Co P2 O5 98.6(3) . . . . ? P1 Co P2 O4 34.9(3) . . . . ? S1 Co P2 O4 125.8(3) . . . . ? S3 Co P2 O4 -63.7(3) . . . . ? S2 Co P2 O4 151.2(9) . . . . ? S4 Co P2 O4 -140.1(3) . . . . ? P1 Co P2 C31 153.1(4) . . . . ? S1 Co P2 C31 -116.0(3) . . . . ? S3 Co P2 C31 54.5(4) . . . . ? S2 Co P2 C31 -90.6(10) . . . . ? S4 Co P2 C31 -21.8(4) . . . . ? O2 P1 O1 C23 -41.5(8) . . . . ? C11 P1 O1 C23 62.0(7) . . . . ? Co P1 O1 C23 -168.8(6) . . . . ? O1 P1 O2 C17 -51.0(12) . . . . ? C11 P1 O2 C17 -158.9(12) . . . . ? Co P1 O2 C17 74.8(12) . . . . ? O5 P2 O4 C43 -44.3(8) . . . . ? C31 P2 O4 C43 67.4(8) . . . . ? Co P2 O4 C43 -165.3(7) . . . . ? O4 P2 O5 C37 65.4(8) . . . . ? C31 P2 O5 C37 -45.1(8) . . . . ? Co P2 O5 C37 -173.3(6) . . . . ? C2 N1 C1 S2 180.0(6) . . . . ? C3 N1 C1 S2 4.8(11) . . . . ? C2 N1 C1 S1 1.4(12) . . . . ? C3 N1 C1 S1 -173.7(6) . . . . ? Co S2 C1 N1 -175.3(7) . . . . ? Co S2 C1 S1 3.5(3) . . . . ? Co S1 C1 N1 175.2(7) . . . . ? Co S1 C1 S2 -3.6(3) . . . . ? C6 N2 C4 S4 3.0(12) . . . . ? C5 N2 C4 S4 -179.5(7) . . . . ? C6 N2 C4 S3 -174.8(7) . . . . ? C5 N2 C4 S3 2.7(12) . . . . ? Co S4 C4 N2 -176.9(7) . . . . ? Co S4 C4 S3 1.2(4) . . . . ? Co S3 C4 N2 176.8(7) . . . . ? Co S3 C4 S4 -1.2(4) . . . . ? O2 P1 C11 C16 -36.1(8) . . . . ? O1 P1 C11 C16 -147.8(7) . . . . ? Co P1 C11 C16 87.2(8) . . . . ? O2 P1 C11 C12 144.7(7) . . . . ? O1 P1 C11 C12 32.9(8) . . . . ? Co P1 C11 C12 -92.0(7) . . . . ? C16 C11 C12 C13 0.3(13) . . . . ? P1 C11 C12 C13 179.6(7) . . . . ? C11 C12 C13 C14 -0.9(16) . . . . ? C12 C13 C14 C15 1.0(19) . . . . ? C13 C14 C15 C16 -0.6(18) . . . . ? C14 C15 C16 C11 0.0(17) . . . . ? C12 C11 C16 C15 0.1(15) . . . . ? P1 C11 C16 C15 -179.2(8) . . . . ? O5 P2 C31 C36 147.8(7) . . . . ? O4 P2 C31 C36 32.4(7) . . . . ? Co P2 C31 C36 -89.4(7) . . . . ? O5 P2 C31 C32 -33.4(8) . . . . ? O4 P2 C31 C32 -148.8(7) . . . . ? Co P2 C31 C32 89.4(7) . . . . ? C36 C31 C32 C33 3.8(13) . . . . ? P2 C31 C32 C33 -175.0(7) . . . . ? C31 C32 C33 C34 -1.5(14) . . . . ? C32 C33 C34 C35 0.1(16) . . . . ? C33 C34 C35 C36 -1.0(16) . . . . ? C32 C31 C36 C35 -4.6(13) . . . . ? P2 C31 C36 C35 174.2(7) . . . . ? C34 C35 C36 C31 3.3(14) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.485 _refine_diff_density_min -0.624 _refine_diff_density_rms 0.096 #===END data_cisPPh2OMe _database_code_CSD 206915 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis-Bis(N,N-dimethyldithiocarbamato)bis(methyl diphenylphosphinite)cobalt(III) Hexafluorophosphate ; _chemical_name_common cis-[Co(dtc)~2~(P(OMe)Ph~2~)~2~]PF~6~ _chemical_melting_point ? _chemical_formula_moiety 'C32 H38 Co N2 O2 P2 S4 1+, F6 P 1-' _chemical_formula_sum 'C32 H38 Co F6 N2 O2 P3 S4' _chemical_formula_weight 876.72 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' O O 0.0106 0.0060 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 18.893(6) _cell_length_b 25.288(3) _cell_length_c 16.688(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7973(3) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3600 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.906 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details none _diffrn_ambient_temperature 296(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 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.99 _diffrn_reflns_number 13392 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.1470 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 30.02 _reflns_number_total 11635 _reflns_number_gt 4255 _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. 1.11' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP in teXsan' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11635 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2147 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1606 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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 Co Co 0.19322(2) 0.441718(19) 0.35750(3) 0.03895(13) Uani 1 1 d . . . S1 S 0.09902(5) 0.38785(4) 0.33580(6) 0.0465(2) Uani 1 1 d . . . S2 S 0.19551(5) 0.42707(4) 0.22225(5) 0.0461(2) Uani 1 1 d . . . S3 S 0.27000(5) 0.51068(4) 0.35061(7) 0.0548(3) Uani 1 1 d . . . S4 S 0.12241(6) 0.51382(4) 0.33332(7) 0.0557(3) Uani 1 1 d . . . P1 P 0.27492(5) 0.37754(4) 0.36548(6) 0.0413(2) Uani 1 1 d . . . P2 P 0.19046(5) 0.45272(4) 0.49099(6) 0.0444(2) Uani 1 1 d . . . P3 P 0.00892(9) 0.29844(6) 0.90055(9) 0.0828(4) Uani 1 1 d . . . F1 F -0.0644(2) 0.32409(19) 0.8808(3) 0.1669(17) Uani 1 1 d . . . F2 F -0.0296(3) 0.2463(2) 0.9113(3) 0.219(3) Uani 1 1 d . . . F3 F 0.0211(4) 0.2884(3) 0.8150(3) 0.273(4) Uani 1 1 d . . . F4 F -0.0035(2) 0.3077(3) 0.9889(3) 0.201(3) Uani 1 1 d . . . F5 F 0.0462(3) 0.3500(2) 0.8939(5) 0.267(4) Uani 1 1 d . . . F6 F 0.0806(2) 0.2741(2) 0.9266(3) 0.196(2) Uani 1 1 d . . . O1 O 0.27551(14) 0.34814(10) 0.45035(14) 0.0530(7) Uani 1 1 d . . . O4 O 0.27055(13) 0.45092(11) 0.52348(15) 0.0545(7) Uani 1 1 d . . . N1 N 0.09387(17) 0.35828(13) 0.18113(19) 0.0510(8) Uani 1 1 d . . . N2 N 0.2017(2) 0.60265(15) 0.3301(3) 0.0778(12) Uani 1 1 d . . . C1 C 0.12416(18) 0.38669(14) 0.2369(2) 0.0424(8) Uani 1 1 d . . . C2 C 0.0334(2) 0.32443(18) 0.1983(3) 0.0688(12) Uani 1 1 d . . . H2A H -0.0007 0.3438 0.2292 0.083 Uiso 1 1 calc R . . H2B H 0.0489 0.2941 0.2282 0.083 Uiso 1 1 calc R . . H2C H 0.0122 0.3131 0.1490 0.083 Uiso 1 1 calc R . . C3 C 0.1223(3) 0.3574(2) 0.0995(3) 0.0790(15) Uani 1 1 d . . . H3A H 0.1518 0.3268 0.0928 0.099 Uiso 1 1 calc R . . H3B H 0.1496 0.3888 0.0903 0.099 Uiso 1 1 calc R . . H3C H 0.0839 0.3559 0.0618 0.099 Uiso 1 1 calc R . . C4 C 0.1983(2) 0.55052(15) 0.3366(2) 0.0554(11) Uani 1 1 d . . . C5 C 0.2687(4) 0.6298(2) 0.3401(4) 0.111(2) Uani 1 1 d . . . H5A H 0.2904 0.6187 0.3893 0.129 Uiso 1 1 calc R . . H5B H 0.2607 0.6672 0.3415 0.129 Uiso 1 1 calc R . . H5C H 0.2993 0.6213 0.2960 0.129 Uiso 1 1 calc R . . C6 C 0.1373(4) 0.6340(2) 0.3180(4) 0.115(2) Uani 1 1 d . . . H6A H 0.1466 0.6702 0.3316 0.137 Uiso 1 1 calc R . . H6B H 0.1002 0.6205 0.3516 0.137 Uiso 1 1 calc R . . H6C H 0.1231 0.6318 0.2629 0.137 Uiso 1 1 calc R . . C11 C 0.2691(2) 0.32243(14) 0.2958(2) 0.0451(9) Uani 1 1 d . . . C12 C 0.2103(2) 0.28902(15) 0.3016(3) 0.0568(11) Uani 1 1 d . . . H12 H 0.1775 0.2943 0.3424 0.070 Uiso 1 1 calc R . . C13 C 0.2003(2) 0.24819(17) 0.2475(3) 0.0672(12) Uani 1 1 d . . . H13 H 0.1607 0.2265 0.2519 0.082 Uiso 1 1 calc R . . C14 C 0.2480(3) 0.23967(19) 0.1881(3) 0.0775(15) Uani 1 1 d . . . H14 H 0.2399 0.2134 0.1502 0.092 Uiso 1 1 calc R . . C15 C 0.3082(3) 0.26993(19) 0.1840(3) 0.0771(14) Uani 1 1 d . . . H15 H 0.3424 0.2623 0.1457 0.095 Uiso 1 1 calc R . . C16 C 0.3185(2) 0.31136(17) 0.2360(3) 0.0612(12) Uani 1 1 d . . . H16 H 0.3588 0.3322 0.2313 0.075 Uiso 1 1 calc R . . C17 C 0.36213(19) 0.40667(15) 0.3536(2) 0.0470(9) Uani 1 1 d . . . C18 C 0.3836(2) 0.42935(15) 0.2808(3) 0.0553(10) Uani 1 1 d . . . H18 H 0.3552 0.4259 0.2356 0.069 Uiso 1 1 calc R . . C19 C 0.4466(2) 0.45680(18) 0.2759(3) 0.0669(13) Uani 1 1 d . . . H19 H 0.4611 0.4712 0.2273 0.081 Uiso 1 1 calc R . . C20 C 0.4876(2) 0.4628(2) 0.3428(4) 0.0811(16) Uani 1 1 d . . . H20 H 0.5297 0.4817 0.3393 0.096 Uiso 1 1 calc R . . C21 C 0.4681(2) 0.4419(2) 0.4142(4) 0.0782(15) Uani 1 1 d . . . H21 H 0.4967 0.4465 0.4590 0.095 Uiso 1 1 calc R . . C22 C 0.4052(2) 0.41332(18) 0.4204(3) 0.0625(12) Uani 1 1 d . . . H22 H 0.3920 0.3987 0.4694 0.077 Uiso 1 1 calc R . . C23 C 0.3162(3) 0.30033(19) 0.4654(3) 0.0804(15) Uani 1 1 d . . . H23A H 0.3271 0.2979 0.5214 0.100 Uiso 1 1 calc R . . H23B H 0.3594 0.3015 0.4351 0.100 Uiso 1 1 calc R . . H23C H 0.2890 0.2700 0.4495 0.100 Uiso 1 1 calc R . . C31 C 0.1586(2) 0.51725(16) 0.5219(2) 0.0497(10) Uani 1 1 d . . . C32 C 0.0865(2) 0.5271(2) 0.5272(3) 0.0736(14) Uani 1 1 d . . . H32 H 0.0544 0.4995 0.5202 0.089 Uiso 1 1 calc R . . C33 C 0.0618(3) 0.5776(2) 0.5430(3) 0.0873(17) Uani 1 1 d . . . H33 H 0.0133 0.5838 0.5462 0.101 Uiso 1 1 calc R . . C34 C 0.1079(3) 0.6181(2) 0.5537(3) 0.0810(16) Uani 1 1 d . . . H34 H 0.0910 0.6520 0.5639 0.094 Uiso 1 1 calc R . . C35 C 0.1793(3) 0.6091(2) 0.5495(3) 0.0799(15) Uani 1 1 d . . . H35 H 0.2108 0.6369 0.5576 0.099 Uiso 1 1 calc R . . C36 C 0.2050(2) 0.55922(16) 0.5334(3) 0.0592(11) Uani 1 1 d . . . H36 H 0.2535 0.5536 0.5302 0.069 Uiso 1 1 calc R . . C37 C 0.1384(2) 0.40823(17) 0.5535(2) 0.0542(10) Uani 1 1 d . . . C38 C 0.1211(2) 0.35777(18) 0.5272(2) 0.0569(11) Uani 1 1 d . . . H38 H 0.1372 0.3462 0.4775 0.070 Uiso 1 1 calc R . . C39 C 0.0802(2) 0.32447(19) 0.5737(3) 0.0684(12) Uani 1 1 d . . . H39 H 0.0685 0.2910 0.5549 0.083 Uiso 1 1 calc R . . C40 C 0.0568(3) 0.3408(2) 0.6476(3) 0.0838(16) Uani 1 1 d . . . H40 H 0.0278 0.3188 0.6780 0.103 Uiso 1 1 calc R . . C41 C 0.0762(3) 0.3894(3) 0.6766(3) 0.0911(17) Uani 1 1 d . . . H41 H 0.0630 0.3994 0.7282 0.112 Uiso 1 1 calc R . . C42 C 0.1150(3) 0.4236(2) 0.6300(3) 0.0783(14) Uani 1 1 d . . . H42 H 0.1259 0.4571 0.6492 0.097 Uiso 1 1 calc R . . C43 C 0.2907(3) 0.4416(2) 0.6052(3) 0.0796(15) Uani 1 1 d . . . H43A H 0.2807 0.4056 0.6191 0.102 Uiso 1 1 calc R . . H43B H 0.2645 0.4648 0.6397 0.102 Uiso 1 1 calc R . . H43C H 0.3404 0.4483 0.6114 0.102 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 Co 0.0353(2) 0.0436(3) 0.0380(3) -0.0003(2) 0.0001(2) 0.0043(2) S1 0.0381(5) 0.0570(6) 0.0444(5) 0.0008(5) 0.0018(4) 0.0002(5) S2 0.0463(5) 0.0550(6) 0.0371(5) 0.0037(4) 0.0019(4) 0.0012(5) S3 0.0482(6) 0.0485(6) 0.0677(7) 0.0034(5) 0.0038(5) -0.0017(5) S4 0.0517(6) 0.0561(6) 0.0594(6) -0.0003(5) -0.0073(5) 0.0153(5) P1 0.0374(5) 0.0474(6) 0.0390(5) 0.0021(4) 0.0023(4) 0.0064(4) P2 0.0390(5) 0.0538(6) 0.0405(5) -0.0077(4) -0.0013(4) 0.0036(5) P3 0.0930(11) 0.0922(11) 0.0633(9) -0.0077(7) 0.0119(8) -0.0066(9) F1 0.151(4) 0.173(4) 0.176(4) 0.026(3) -0.052(3) 0.022(3) F2 0.265(6) 0.140(4) 0.253(6) 0.067(4) -0.111(5) -0.098(4) F3 0.472(10) 0.276(7) 0.072(3) -0.012(3) 0.095(5) 0.051(7) F4 0.131(3) 0.373(8) 0.099(3) -0.086(4) 0.006(2) 0.013(4) F5 0.234(6) 0.146(5) 0.420(11) 0.084(6) -0.052(6) -0.096(5) F6 0.117(3) 0.261(6) 0.209(5) 0.049(4) 0.043(3) 0.066(4) O1 0.0572(16) 0.0593(17) 0.0426(15) 0.0086(13) 0.0034(13) 0.0146(14) O4 0.0434(15) 0.0701(19) 0.0500(16) -0.0065(13) -0.0121(13) 0.0122(14) N1 0.0474(19) 0.057(2) 0.0483(19) -0.0047(16) -0.0111(16) 0.0004(17) N2 0.089(3) 0.051(2) 0.093(3) 0.015(2) 0.007(2) 0.011(2) C1 0.0406(19) 0.048(2) 0.0386(19) 0.0026(17) -0.0023(16) 0.0083(17) C2 0.059(3) 0.064(3) 0.083(3) -0.008(3) -0.015(2) -0.009(2) C3 0.078(3) 0.108(4) 0.051(3) -0.026(3) -0.001(2) -0.002(3) C4 0.067(3) 0.045(2) 0.054(2) 0.0034(18) 0.001(2) 0.010(2) C5 0.122(5) 0.056(3) 0.155(6) 0.019(3) 0.018(4) -0.023(4) C6 0.138(6) 0.064(3) 0.142(6) 0.030(3) 0.007(5) 0.038(4) C11 0.048(2) 0.042(2) 0.045(2) 0.0060(17) -0.0006(18) 0.0103(18) C12 0.059(3) 0.047(2) 0.065(3) 0.002(2) 0.002(2) 0.011(2) C13 0.074(3) 0.046(2) 0.082(3) -0.004(2) -0.011(3) 0.000(2) C14 0.112(4) 0.056(3) 0.065(3) -0.012(2) -0.001(3) 0.004(3) C15 0.099(4) 0.063(3) 0.069(3) -0.012(2) 0.025(3) 0.011(3) C16 0.064(3) 0.060(3) 0.060(3) -0.003(2) 0.020(2) 0.005(2) C17 0.0368(19) 0.051(2) 0.053(2) -0.0065(19) 0.0059(18) 0.0093(18) C18 0.045(2) 0.056(2) 0.066(3) 0.003(2) 0.008(2) 0.006(2) C19 0.049(3) 0.065(3) 0.087(4) 0.007(3) 0.019(3) 0.007(2) C20 0.043(2) 0.077(3) 0.123(5) -0.014(3) 0.014(3) -0.007(2) C21 0.046(3) 0.090(4) 0.099(4) -0.029(3) -0.002(3) -0.004(3) C22 0.043(2) 0.078(3) 0.067(3) -0.009(2) 0.001(2) 0.008(2) C23 0.097(4) 0.076(3) 0.068(3) 0.024(3) -0.007(3) 0.027(3) C31 0.047(2) 0.058(2) 0.044(2) -0.0147(19) -0.0037(18) 0.013(2) C32 0.049(3) 0.080(3) 0.091(4) -0.037(3) -0.001(3) 0.007(2) C33 0.061(3) 0.104(4) 0.097(4) -0.040(3) -0.005(3) 0.033(3) C34 0.091(4) 0.077(4) 0.075(3) -0.025(3) -0.015(3) 0.034(3) C35 0.082(4) 0.069(3) 0.090(4) -0.022(3) -0.025(3) 0.001(3) C36 0.055(3) 0.057(3) 0.066(3) -0.012(2) -0.009(2) 0.009(2) C37 0.051(2) 0.069(3) 0.043(2) 0.001(2) 0.0017(19) 0.004(2) C38 0.056(2) 0.069(3) 0.045(2) 0.011(2) 0.003(2) 0.006(2) C39 0.078(3) 0.061(3) 0.066(3) 0.015(2) 0.005(3) 0.000(3) C40 0.091(4) 0.090(4) 0.070(4) 0.018(3) 0.024(3) 0.002(3) C41 0.114(5) 0.112(5) 0.047(3) 0.004(3) 0.032(3) 0.014(4) C42 0.096(4) 0.082(3) 0.056(3) -0.009(3) 0.019(3) -0.003(3) C43 0.081(3) 0.097(4) 0.061(3) -0.006(3) -0.032(3) 0.011(3) 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 P1 2.2437(11) . ? Co P2 2.2456(11) . ? Co S1 2.2703(12) . ? Co S3 2.2712(12) . ? Co S2 2.2877(11) . ? Co S4 2.2972(11) . ? S1 C1 1.718(4) . ? S2 C1 1.709(4) . ? S3 C4 1.704(4) . ? S4 C4 1.709(4) . ? P1 O1 1.600(3) . ? P1 C17 1.816(4) . ? P1 C11 1.818(4) . ? P2 O4 1.608(3) . ? P2 C31 1.814(4) . ? P2 C37 1.822(4) . ? P3 F3 1.468(4) . ? P3 F5 1.487(5) . ? P3 F4 1.512(4) . ? P3 F2 1.517(4) . ? P3 F6 1.549(4) . ? P3 F1 1.564(4) . ? O1 C23 1.454(5) . ? O4 C43 1.435(5) . ? N1 C1 1.308(4) . ? N1 C2 1.456(5) . ? N1 C3 1.464(5) . ? N2 C4 1.324(5) . ? N2 C5 1.450(7) . ? N2 C6 1.465(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 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C11 C16 1.394(5) . ? C11 C12 1.399(5) . ? C12 C13 1.385(6) . ? C12 H12 0.9300 . ? C13 C14 1.357(6) . ? C13 H13 0.9300 . ? C14 C15 1.372(7) . ? C14 H14 0.9300 . ? C15 C16 1.374(6) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.390(5) . ? C17 C18 1.403(5) . ? C18 C19 1.379(6) . ? C18 H18 0.9300 . ? C19 C20 1.368(7) . ? C19 H19 0.9300 . ? C20 C21 1.354(7) . ? C20 H20 0.9300 . ? C21 C22 1.394(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C31 C32 1.389(5) . ? C31 C36 1.389(5) . ? C32 C33 1.386(6) . ? C32 H32 0.9300 . ? C33 C34 1.356(7) . ? C33 H33 0.9300 . ? C34 C35 1.371(6) . ? C34 H34 0.9300 . ? C35 C36 1.378(6) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.389(6) . ? C37 C42 1.406(6) . ? C38 C39 1.380(6) . ? C38 H38 0.9300 . ? C39 C40 1.374(6) . ? C39 H39 0.9300 . ? C40 C41 1.373(7) . ? C40 H40 0.9300 . ? C41 C42 1.373(7) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 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 P1 Co P2 92.68(4) . . ? P1 Co S1 96.59(4) . . ? P2 Co S1 102.38(4) . . ? P1 Co S3 96.83(4) . . ? P2 Co S3 88.28(4) . . ? S1 Co S3 162.42(4) . . ? P1 Co S2 85.89(4) . . ? P2 Co S2 177.78(4) . . ? S1 Co S2 76.13(4) . . ? S3 Co S2 93.57(4) . . ? P1 Co S4 170.12(4) . . ? P2 Co S4 93.58(4) . . ? S1 Co S4 89.52(4) . . ? S3 Co S4 75.73(4) . . ? S2 Co S4 88.07(4) . . ? C1 S1 Co 86.95(13) . . ? C1 S2 Co 86.60(12) . . ? C4 S3 Co 87.33(15) . . ? C4 S4 Co 86.36(13) . . ? O1 P1 C17 106.19(17) . . ? O1 P1 C11 102.14(16) . . ? C17 P1 C11 107.20(17) . . ? O1 P1 Co 113.17(10) . . ? C17 P1 Co 108.93(12) . . ? C11 P1 Co 118.37(12) . . ? O4 P2 C31 103.99(16) . . ? O4 P2 C37 107.29(16) . . ? C31 P2 C37 102.36(19) . . ? O4 P2 Co 108.01(10) . . ? C31 P2 Co 113.63(13) . . ? C37 P2 Co 120.25(14) . . ? F3 P3 F5 90.3(4) . . ? F3 P3 F4 178.9(4) . . ? F5 P3 F4 90.6(4) . . ? F3 P3 F2 92.3(4) . . ? F5 P3 F2 177.4(5) . . ? F4 P3 F2 86.8(3) . . ? F3 P3 F6 93.9(4) . . ? F5 P3 F6 87.5(4) . . ? F4 P3 F6 85.6(3) . . ? F2 P3 F6 92.3(3) . . ? F3 P3 F1 90.3(4) . . ? F5 P3 F1 92.3(3) . . ? F4 P3 F1 90.2(3) . . ? F2 P3 F1 87.8(3) . . ? F6 P3 F1 175.8(3) . . ? C23 O1 P1 122.9(3) . . ? C43 O4 P2 125.1(3) . . ? C1 N1 C2 121.7(3) . . ? C1 N1 C3 120.7(3) . . ? C2 N1 C3 117.5(3) . . ? C4 N2 C5 120.2(4) . . ? C4 N2 C6 120.7(4) . . ? C5 N2 C6 119.0(4) . . ? N1 C1 S2 124.9(3) . . ? N1 C1 S1 124.9(3) . . ? S2 C1 S1 110.2(2) . . ? 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 C4 S3 124.2(4) . . ? N2 C4 S4 125.3(3) . . ? S3 C4 S4 110.5(2) . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C16 C11 C12 117.4(4) . . ? C16 C11 P1 124.9(3) . . ? C12 C11 P1 117.8(3) . . ? C13 C12 C11 120.9(4) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 C12 120.3(5) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 119.8(5) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 120.7(4) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C11 120.7(4) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? C22 C17 C18 118.4(4) . . ? C22 C17 P1 119.5(3) . . ? C18 C17 P1 121.5(3) . . ? C19 C18 C17 120.5(4) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C18 119.7(5) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C21 C20 C19 121.3(5) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 120.0(5) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C17 C22 C21 120.1(4) . . ? C17 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? O1 C23 H23A 109.5 . . ? O1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C32 C31 C36 118.3(4) . . ? C32 C31 P2 120.3(3) . . ? C36 C31 P2 121.2(3) . . ? C33 C32 C31 120.5(5) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 120.4(5) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 120.0(5) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C36 120.5(5) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C35 C36 C31 120.3(4) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? C38 C37 C42 117.8(4) . . ? C38 C37 P2 121.0(3) . . ? C42 C37 P2 121.3(4) . . ? C39 C38 C37 121.0(4) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C40 C39 C38 120.1(5) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C41 C40 C39 119.9(5) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 120.4(5) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C37 120.6(5) . . ? C41 C42 H42 119.7 . . ? C37 C42 H42 119.7 . . ? O4 C43 H43A 109.5 . . ? O4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Co S1 C1 -81.91(12) . . . . ? P2 Co S1 C1 -176.13(12) . . . . ? S3 Co S1 C1 57.66(19) . . . . ? S2 Co S1 C1 2.19(12) . . . . ? S4 Co S1 C1 90.32(12) . . . . ? P1 Co S2 C1 95.63(12) . . . . ? P2 Co S2 C1 45.7(11) . . . . ? S1 Co S2 C1 -2.20(12) . . . . ? S3 Co S2 C1 -167.76(12) . . . . ? S4 Co S2 C1 -92.19(12) . . . . ? P1 Co S3 C4 175.03(15) . . . . ? P2 Co S3 C4 -92.47(15) . . . . ? S1 Co S3 C4 35.5(2) . . . . ? S2 Co S3 C4 88.75(15) . . . . ? S4 Co S3 C4 1.66(14) . . . . ? P1 Co S4 C4 -43.6(3) . . . . ? P2 Co S4 C4 85.65(15) . . . . ? S1 Co S4 C4 -171.97(14) . . . . ? S3 Co S4 C4 -1.66(14) . . . . ? S2 Co S4 C4 -95.84(14) . . . . ? P2 Co P1 O1 23.98(12) . . . . ? S1 Co P1 O1 -78.81(12) . . . . ? S3 Co P1 O1 112.57(12) . . . . ? S2 Co P1 O1 -154.32(12) . . . . ? S4 Co P1 O1 153.3(3) . . . . ? P2 Co P1 C17 -93.88(14) . . . . ? S1 Co P1 C17 163.33(13) . . . . ? S3 Co P1 C17 -5.29(14) . . . . ? S2 Co P1 C17 87.82(14) . . . . ? S4 Co P1 C17 35.4(3) . . . . ? P2 Co P1 C11 143.41(15) . . . . ? S1 Co P1 C11 40.61(15) . . . . ? S3 Co P1 C11 -128.01(15) . . . . ? S2 Co P1 C11 -34.89(15) . . . . ? S4 Co P1 C11 -87.3(3) . . . . ? P1 Co P2 O4 42.33(11) . . . . ? S1 Co P2 O4 139.68(11) . . . . ? S3 Co P2 O4 -54.43(11) . . . . ? S2 Co P2 O4 92.2(11) . . . . ? S4 Co P2 O4 -130.02(11) . . . . ? P1 Co P2 C31 157.15(15) . . . . ? S1 Co P2 C31 -105.50(15) . . . . ? S3 Co P2 C31 60.38(15) . . . . ? S2 Co P2 C31 -153.0(11) . . . . ? S4 Co P2 C31 -15.20(15) . . . . ? P1 Co P2 C37 -81.13(16) . . . . ? S1 Co P2 C37 16.22(16) . . . . ? S3 Co P2 C37 -177.90(16) . . . . ? S2 Co P2 C37 -31.3(11) . . . . ? S4 Co P2 C37 106.51(16) . . . . ? C17 P1 O1 C23 -70.1(3) . . . . ? C11 P1 O1 C23 42.1(4) . . . . ? Co P1 O1 C23 170.5(3) . . . . ? C31 P2 O4 C43 77.4(3) . . . . ? C37 P2 O4 C43 -30.6(4) . . . . ? Co P2 O4 C43 -161.6(3) . . . . ? C2 N1 C1 S2 179.5(3) . . . . ? C3 N1 C1 S2 2.8(5) . . . . ? C2 N1 C1 S1 0.8(5) . . . . ? C3 N1 C1 S1 -175.9(3) . . . . ? Co S2 C1 N1 -175.9(3) . . . . ? Co S2 C1 S1 3.01(16) . . . . ? Co S1 C1 N1 175.9(3) . . . . ? Co S1 C1 S2 -3.03(16) . . . . ? C5 N2 C4 S3 -4.1(7) . . . . ? C6 N2 C4 S3 179.9(4) . . . . ? C5 N2 C4 S4 175.2(4) . . . . ? C6 N2 C4 S4 -0.9(7) . . . . ? Co S3 C4 N2 177.0(4) . . . . ? Co S3 C4 S4 -2.3(2) . . . . ? Co S4 C4 N2 -177.0(4) . . . . ? Co S4 C4 S3 2.3(2) . . . . ? O1 P1 C11 C16 -121.2(3) . . . . ? C17 P1 C11 C16 -9.8(4) . . . . ? Co P1 C11 C16 113.8(3) . . . . ? O1 P1 C11 C12 59.8(3) . . . . ? C17 P1 C11 C12 171.3(3) . . . . ? Co P1 C11 C12 -65.2(3) . . . . ? C16 C11 C12 C13 -3.0(6) . . . . ? P1 C11 C12 C13 176.1(3) . . . . ? C11 C12 C13 C14 0.6(7) . . . . ? C12 C13 C14 C15 3.3(7) . . . . ? C13 C14 C15 C16 -4.7(7) . . . . ? C14 C15 C16 C11 2.2(7) . . . . ? C12 C11 C16 C15 1.6(6) . . . . ? P1 C11 C16 C15 -177.4(3) . . . . ? O1 P1 C17 C22 -17.9(3) . . . . ? C11 P1 C17 C22 -126.6(3) . . . . ? Co P1 C17 C22 104.2(3) . . . . ? O1 P1 C17 C18 171.0(3) . . . . ? C11 P1 C17 C18 62.4(3) . . . . ? Co P1 C17 C18 -66.8(3) . . . . ? C22 C17 C18 C19 1.0(6) . . . . ? P1 C17 C18 C19 172.2(3) . . . . ? C17 C18 C19 C20 -1.3(6) . . . . ? C18 C19 C20 C21 0.7(7) . . . . ? C19 C20 C21 C22 0.2(8) . . . . ? C18 C17 C22 C21 -0.2(6) . . . . ? P1 C17 C22 C21 -171.5(3) . . . . ? C20 C21 C22 C17 -0.5(7) . . . . ? O4 P2 C31 C32 -159.6(3) . . . . ? C37 P2 C31 C32 -48.0(4) . . . . ? Co P2 C31 C32 83.2(4) . . . . ? O4 P2 C31 C36 26.5(4) . . . . ? C37 P2 C31 C36 138.1(3) . . . . ? Co P2 C31 C36 -90.7(3) . . . . ? C36 C31 C32 C33 0.6(7) . . . . ? P2 C31 C32 C33 -173.6(4) . . . . ? C31 C32 C33 C34 -0.3(8) . . . . ? C32 C33 C34 C35 -0.4(8) . . . . ? C33 C34 C35 C36 0.8(8) . . . . ? C34 C35 C36 C31 -0.6(7) . . . . ? C32 C31 C36 C35 -0.1(6) . . . . ? P2 C31 C36 C35 173.9(4) . . . . ? O4 P2 C37 C38 -100.6(3) . . . . ? C31 P2 C37 C38 150.3(3) . . . . ? Co P2 C37 C38 23.3(4) . . . . ? O4 P2 C37 C42 78.9(4) . . . . ? C31 P2 C37 C42 -30.2(4) . . . . ? Co P2 C37 C42 -157.3(3) . . . . ? C42 C37 C38 C39 2.1(6) . . . . ? P2 C37 C38 C39 -178.4(3) . . . . ? C37 C38 C39 C40 -0.9(7) . . . . ? C38 C39 C40 C41 -2.4(8) . . . . ? C39 C40 C41 C42 4.4(9) . . . . ? C40 C41 C42 C37 -3.2(8) . . . . ? C38 C37 C42 C41 -0.1(7) . . . . ? P2 C37 C42 C41 -179.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.586 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.077 #===END data_trPOMe3 _database_code_CSD 206916 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-Bis(dimethyldithiocarbamato)bis(trimethylphosphite)cobalt(III) Tetrafluoroborate ; _chemical_name_common trans-[Co(dtc)~2~{P(OMe)~3~}~2~]BF~4~ _chemical_melting_point ? _chemical_formula_moiety 'C12 H30 Co N2 O6 P2 S4 1+, B F4 1-' _chemical_formula_sum 'C12 H30 B Co F4 N2 O6 P2 S4' _chemical_formula_weight 634.30 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' 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' _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 11.170(2) _cell_length_b 12.212(2) _cell_length_c 12.319(2) _cell_angle_alpha 109.669(16) _cell_angle_beta 109.066(14) _cell_angle_gamma 107.363(16) _cell_volume 1328.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 _exptl_crystal_description red _exptl_crystal_colour prism _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 1.138 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.898 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 AFC-5R' _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_% 6.31 _diffrn_reflns_number 8122 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0873 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 30.01 _reflns_number_total 7753 _reflns_number_gt 3622 _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. 1.11' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP in teXsan' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1102P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7753 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1599 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1994 _refine_ls_wR_factor_gt 0.1591 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 0.5000 0.5000 0.0404(2) Uani 1 2 d S . . Co2 Co 0.5000 1.0000 1.0000 0.0442(2) Uani 1 2 d S . . S1 S 0.44637(14) 0.36499(11) 0.29292(11) 0.0534(3) Uani 1 1 d . . . S2 S 0.38713(13) 0.57735(12) 0.37797(11) 0.0530(3) Uani 1 1 d . . . S3 S 0.30940(13) 1.01075(12) 1.02143(13) 0.0576(3) Uani 1 1 d . . . S4 S 0.34678(13) 0.78650(11) 0.91940(11) 0.0554(3) Uani 1 1 d . . . P1 P 0.70481(13) 0.63124(13) 0.52110(12) 0.0568(3) Uani 1 1 d . . . P2 P 0.59468(13) 1.00377(12) 1.19303(11) 0.0526(3) Uani 1 1 d . . . F1 F 0.0375(9) 0.6594(6) 0.3159(8) 0.186(3) Uani 1 1 d . . . F2 F -0.0336(8) 0.7528(10) 0.2045(8) 0.222(4) Uani 1 1 d . . . F3 F 0.1475(14) 0.8524(7) 0.3816(8) 0.334(8) Uani 1 1 d . . . F4 F 0.1392(13) 0.7242(14) 0.2170(14) 0.331(7) Uani 1 1 d . . . O1 O 0.8201(4) 0.5804(6) 0.5512(6) 0.1088(17) Uani 1 1 d . . . O2 O 0.7932(5) 0.7747(5) 0.6387(5) 0.1052(16) Uani 1 1 d . . . O3 O 0.6957(5) 0.6560(5) 0.4028(4) 0.0951(14) Uani 1 1 d . . . O4 O 0.7192(3) 1.1360(3) 1.3170(3) 0.0601(8) Uani 1 1 d . . . O5 O 0.6722(5) 0.9132(4) 1.1946(4) 0.0822(12) Uani 1 1 d . . . O6 O 0.4814(4) 0.9515(5) 1.2346(4) 0.0902(14) Uani 1 1 d . . . N1 N 0.3401(4) 0.4524(4) 0.1309(4) 0.0588(10) Uani 1 1 d . . . N2 N 0.1068(4) 0.7692(4) 0.9349(4) 0.0659(11) Uani 1 1 d . . . C1 C 0.3831(4) 0.4628(4) 0.2480(4) 0.0477(9) Uani 1 1 d . . . C2 C 0.3467(7) 0.3533(7) 0.0273(5) 0.0832(17) Uani 1 1 d . . . H2A H 0.2692 0.2690 -0.0076 0.100 Uiso 1 1 calc R . . H2B H 0.4355 0.3508 0.0635 0.100 Uiso 1 1 calc R . . H2C H 0.3399 0.3755 -0.0414 0.100 Uiso 1 1 calc R . . C3 C 0.2947(7) 0.5438(6) 0.0988(6) 0.0813(17) Uani 1 1 d . . . H3A H 0.3686 0.6034 0.0936 0.101 Uiso 1 1 calc R . . H3B H 0.2767 0.5922 0.1658 0.101 Uiso 1 1 calc R . . H3C H 0.2093 0.4956 0.0161 0.101 Uiso 1 1 calc R . . C4 C 0.2350(5) 0.8449(4) 0.9560(4) 0.0511(10) Uani 1 1 d . . . C5 C 0.0155(6) 0.8269(7) 0.9645(7) 0.0878(19) Uani 1 1 d . . . H5A H 0.0417 0.8590 1.0557 0.108 Uiso 1 1 calc R . . H5B H -0.0824 0.7614 0.9123 0.108 Uiso 1 1 calc R . . H5C H 0.0278 0.8979 0.9448 0.108 Uiso 1 1 calc R . . C6 C 0.0510(6) 0.6282(6) 0.8822(7) 0.090(2) Uani 1 1 d . . . H6A H -0.0456 0.5853 0.8136 0.109 Uiso 1 1 calc R . . H6B H 0.0536 0.6064 0.9506 0.109 Uiso 1 1 calc R . . H6C H 0.1082 0.5998 0.8475 0.109 Uiso 1 1 calc R . . C11 C 0.7394(14) 0.634(2) 0.3210(14) 0.361(15) Uani 1 1 d . . . H11A H 0.7472 0.5542 0.3025 0.295 Uiso 1 1 calc R . . H11B H 0.8312 0.7050 0.3555 0.295 Uiso 1 1 calc R . . H11C H 0.6735 0.6255 0.2419 0.295 Uiso 1 1 calc R . . C17 C 0.7444(11) 0.8687(7) 0.6467(9) 0.131(3) Uani 1 1 d . . . H17A H 0.8231 0.9545 0.7068 0.158 Uiso 1 1 calc R . . H17B H 0.6751 0.8544 0.6771 0.158 Uiso 1 1 calc R . . H17C H 0.7014 0.8617 0.5616 0.158 Uiso 1 1 calc R . . C23 C 0.9647(7) 0.6483(11) 0.5804(9) 0.142(4) Uani 1 1 d . . . H23A H 1.0174 0.6053 0.6093 0.167 Uiso 1 1 calc R . . H23B H 1.0068 0.7368 0.6484 0.167 Uiso 1 1 calc R . . H23C H 0.9671 0.6483 0.5032 0.167 Uiso 1 1 calc R . . C31 C 0.5119(8) 0.9319(8) 1.3474(6) 0.110(3) Uani 1 1 d . . . H31A H 0.4490 0.9465 1.3818 0.135 Uiso 1 1 calc R . . H31B H 0.6089 0.9923 1.4132 0.135 Uiso 1 1 calc R . . H31C H 0.4982 0.8439 1.3226 0.135 Uiso 1 1 calc R . . C37 C 0.8179(10) 0.9578(9) 1.2827(8) 0.173(6) Uani 1 1 d . . . H37A H 0.8369 0.8841 1.2708 0.184 Uiso 1 1 calc R . . H37B H 0.8360 1.0034 1.3712 0.184 Uiso 1 1 calc R . . H37C H 0.8788 1.0157 1.2651 0.184 Uiso 1 1 calc R . . C43 C 0.6901(7) 1.2400(6) 1.3831(6) 0.0817(17) Uani 1 1 d . . . H43A H 0.7544 1.2849 1.4754 0.102 Uiso 1 1 calc R . . H43B H 0.5937 1.2034 1.3680 0.102 Uiso 1 1 calc R . . H43C H 0.7032 1.3006 1.3494 0.102 Uiso 1 1 calc R . . B1 B 0.0745(7) 0.7493(7) 0.2780(7) 0.0721(17) 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 0.0426(4) 0.0434(4) 0.0385(4) 0.0214(3) 0.0183(3) 0.0226(3) Co2 0.0441(4) 0.0410(4) 0.0367(4) 0.0150(3) 0.0155(3) 0.0152(3) S1 0.0700(7) 0.0529(6) 0.0439(5) 0.0232(5) 0.0267(5) 0.0364(5) S2 0.0658(7) 0.0594(6) 0.0482(6) 0.0299(5) 0.0270(5) 0.0413(6) S3 0.0564(6) 0.0531(6) 0.0615(7) 0.0251(5) 0.0295(5) 0.0243(5) S4 0.0554(6) 0.0437(6) 0.0520(6) 0.0189(5) 0.0185(5) 0.0173(5) P1 0.0483(6) 0.0627(7) 0.0516(6) 0.0291(6) 0.0213(5) 0.0171(5) P2 0.0522(6) 0.0557(7) 0.0381(5) 0.0186(5) 0.0171(5) 0.0204(5) F1 0.222(7) 0.138(5) 0.251(8) 0.117(6) 0.141(6) 0.089(5) F2 0.160(6) 0.402(13) 0.197(7) 0.193(8) 0.090(5) 0.179(8) F3 0.451(16) 0.115(5) 0.130(6) 0.032(4) -0.034(8) -0.009(7) F4 0.367(13) 0.507(19) 0.501(18) 0.356(17) 0.377(15) 0.332(15) O1 0.057(2) 0.141(4) 0.160(5) 0.104(4) 0.052(3) 0.046(3) O2 0.092(3) 0.078(3) 0.086(3) 0.018(2) 0.040(3) -0.003(2) O3 0.085(3) 0.125(4) 0.079(3) 0.066(3) 0.041(2) 0.031(3) O4 0.0556(18) 0.0602(19) 0.0461(16) 0.0132(14) 0.0150(14) 0.0290(16) O5 0.116(3) 0.071(2) 0.060(2) 0.0310(19) 0.033(2) 0.054(2) O6 0.062(2) 0.127(4) 0.059(2) 0.051(2) 0.0223(18) 0.017(2) N1 0.068(2) 0.068(2) 0.043(2) 0.0293(19) 0.0237(18) 0.036(2) N2 0.047(2) 0.069(3) 0.068(3) 0.036(2) 0.0194(19) 0.017(2) C1 0.047(2) 0.050(2) 0.043(2) 0.0238(19) 0.0169(18) 0.0223(19) C2 0.107(5) 0.099(5) 0.045(3) 0.033(3) 0.034(3) 0.053(4) C3 0.101(4) 0.098(4) 0.068(3) 0.057(3) 0.035(3) 0.059(4) C4 0.046(2) 0.055(2) 0.042(2) 0.0234(19) 0.0154(18) 0.0176(19) C5 0.058(3) 0.110(5) 0.098(5) 0.055(4) 0.039(3) 0.033(3) C6 0.064(3) 0.072(4) 0.101(5) 0.047(4) 0.016(3) 0.014(3) C11 0.177(12) 0.84(5) 0.304(19) 0.46(3) 0.176(13) 0.25(2) C17 0.179(9) 0.064(4) 0.140(8) 0.039(5) 0.085(7) 0.044(5) C23 0.056(4) 0.232(11) 0.145(8) 0.100(8) 0.050(5) 0.062(6) C31 0.112(5) 0.129(6) 0.070(4) 0.062(4) 0.037(4) 0.025(5) C37 0.182(9) 0.173(9) 0.095(6) 0.008(6) -0.007(6) 0.146(8) C43 0.097(4) 0.078(4) 0.065(3) 0.020(3) 0.032(3) 0.056(3) B1 0.057(3) 0.074(4) 0.068(4) 0.033(3) 0.023(3) 0.021(3) _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 P1 2.2389(14) 2_666 ? Co1 P1 2.2389(14) . ? Co1 S1 2.2727(13) . ? Co1 S1 2.2727(13) 2_666 ? Co1 S2 2.2737(11) 2_666 ? Co1 S2 2.2737(11) . ? Co2 P2 2.2425(13) 2_677 ? Co2 P2 2.2425(13) . ? Co2 S3 2.2650(13) 2_677 ? Co2 S3 2.2650(13) . ? Co2 S4 2.2796(14) . ? Co2 S4 2.2796(14) 2_677 ? S1 C1 1.710(4) . ? S2 C1 1.711(4) . ? S3 C4 1.703(5) . ? S4 C4 1.719(5) . ? P1 O3 1.563(4) . ? P1 O2 1.570(5) . ? P1 O1 1.582(5) . ? P2 O6 1.560(4) . ? P2 O4 1.576(3) . ? P2 O5 1.597(4) . ? F1 B1 1.339(9) . ? F2 B1 1.273(9) . ? F3 B1 1.226(10) . ? F4 B1 1.230(10) . ? O1 C23 1.430(8) . ? O2 C17 1.400(9) . ? O3 C11 1.241(13) . ? O4 C43 1.451(6) . ? O5 C37 1.429(9) . ? O6 C31 1.437(6) . ? N1 C1 1.311(5) . ? N1 C3 1.470(7) . ? N1 C2 1.475(7) . ? N2 C4 1.333(6) . ? N2 C6 1.456(7) . ? N2 C5 1.472(8) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 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 P1 Co1 P1 180.0 2_666 . ? P1 Co1 S1 92.41(5) 2_666 . ? P1 Co1 S1 87.59(5) . . ? P1 Co1 S1 87.59(5) 2_666 2_666 ? P1 Co1 S1 92.41(5) . 2_666 ? S1 Co1 S1 180.00(4) . 2_666 ? P1 Co1 S2 88.25(5) 2_666 2_666 ? P1 Co1 S2 91.75(5) . 2_666 ? S1 Co1 S2 103.58(4) . 2_666 ? S1 Co1 S2 76.42(4) 2_666 2_666 ? P1 Co1 S2 91.75(5) 2_666 . ? P1 Co1 S2 88.25(5) . . ? S1 Co1 S2 76.42(4) . . ? S1 Co1 S2 103.58(4) 2_666 . ? S2 Co1 S2 180.0 2_666 . ? P2 Co2 P2 180.00(7) 2_677 . ? P2 Co2 S3 91.99(5) 2_677 2_677 ? P2 Co2 S3 88.01(5) . 2_677 ? P2 Co2 S3 88.00(5) 2_677 . ? P2 Co2 S3 91.99(5) . . ? S3 Co2 S3 180.000(1) 2_677 . ? P2 Co2 S4 93.70(5) 2_677 . ? P2 Co2 S4 86.30(5) . . ? S3 Co2 S4 103.24(5) 2_677 . ? S3 Co2 S4 76.76(5) . . ? P2 Co2 S4 86.30(5) 2_677 2_677 ? P2 Co2 S4 93.70(5) . 2_677 ? S3 Co2 S4 76.76(5) 2_677 2_677 ? S3 Co2 S4 103.24(5) . 2_677 ? S4 Co2 S4 180.0 . 2_677 ? C1 S1 Co1 86.34(15) . . ? C1 S2 Co1 86.28(14) . . ? C4 S3 Co2 86.49(17) . . ? C4 S4 Co2 85.66(16) . . ? O3 P1 O2 101.5(3) . . ? O3 P1 O1 106.7(3) . . ? O2 P1 O1 99.6(3) . . ? O3 P1 Co1 116.72(18) . . ? O2 P1 Co1 118.44(19) . . ? O1 P1 Co1 111.94(18) . . ? O6 P2 O4 106.2(2) . . ? O6 P2 O5 103.3(3) . . ? O4 P2 O5 99.0(2) . . ? O6 P2 Co2 113.22(15) . . ? O4 P2 Co2 119.18(15) . . ? O5 P2 Co2 113.94(15) . . ? C23 O1 P1 125.2(6) . . ? C17 O2 P1 122.2(6) . . ? C11 O3 P1 138.6(9) . . ? C43 O4 P2 120.7(3) . . ? C37 O5 P2 125.0(4) . . ? C31 O6 P2 124.3(4) . . ? C1 N1 C3 122.6(4) . . ? C1 N1 C2 120.5(4) . . ? C3 N1 C2 116.8(4) . . ? C4 N2 C6 122.3(5) . . ? C4 N2 C5 120.4(5) . . ? C6 N2 C5 117.3(5) . . ? N1 C1 S1 124.4(4) . . ? N1 C1 S2 125.0(3) . . ? S1 C1 S2 110.6(2) . . ? 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 C4 S3 125.0(4) . . ? N2 C4 S4 123.9(4) . . ? S3 C4 S4 111.1(3) . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C11 H11A 109.5 . . ? O3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O2 C17 H17A 109.5 . . ? O2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O1 C23 H23A 109.5 . . ? O1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O6 C31 H31A 109.5 . . ? O6 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O6 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O5 C37 H37A 109.5 . . ? O5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O4 C43 H43A 109.5 . . ? O4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? F3 B1 F4 113.6(10) . . ? F3 B1 F2 110.0(9) . . ? F4 B1 F2 108.2(9) . . ? F3 B1 F1 103.4(8) . . ? F4 B1 F1 109.7(9) . . ? F2 B1 F1 112.0(7) . . ? 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 P1 Co1 S1 C1 95.31(16) 2_666 . . . ? P1 Co1 S1 C1 -84.69(16) . . . . ? S1 Co1 S1 C1 -168(44) 2_666 . . . ? S2 Co1 S1 C1 -175.91(15) 2_666 . . . ? S2 Co1 S1 C1 4.09(15) . . . . ? P1 Co1 S2 C1 -96.14(16) 2_666 . . . ? P1 Co1 S2 C1 83.86(16) . . . . ? S1 Co1 S2 C1 -4.09(15) . . . . ? S1 Co1 S2 C1 175.91(15) 2_666 . . . ? S2 Co1 S2 C1 155(34) 2_666 . . . ? P2 Co2 S3 C4 94.66(15) 2_677 . . . ? P2 Co2 S3 C4 -85.34(15) . . . . ? S3 Co2 S3 C4 106(35) 2_677 . . . ? S4 Co2 S3 C4 0.39(15) . . . . ? S4 Co2 S3 C4 -179.61(15) 2_677 . . . ? P2 Co2 S4 C4 -87.46(15) 2_677 . . . ? P2 Co2 S4 C4 92.54(15) . . . . ? S3 Co2 S4 C4 179.61(15) 2_677 . . . ? S3 Co2 S4 C4 -0.39(15) . . . . ? S4 Co2 S4 C4 -53(9) 2_677 . . . ? P1 Co1 P1 O3 -48(4) 2_666 . . . ? S1 Co1 P1 O3 43.5(2) . . . . ? S1 Co1 P1 O3 -136.5(2) 2_666 . . . ? S2 Co1 P1 O3 147.0(2) 2_666 . . . ? S2 Co1 P1 O3 -33.0(2) . . . . ? P1 Co1 P1 O2 73(4) 2_666 . . . ? S1 Co1 P1 O2 165.2(3) . . . . ? S1 Co1 P1 O2 -14.8(3) 2_666 . . . ? S2 Co1 P1 O2 -91.2(3) 2_666 . . . ? S2 Co1 P1 O2 88.8(3) . . . . ? P1 Co1 P1 O1 -172(4) 2_666 . . . ? S1 Co1 P1 O1 -79.8(2) . . . . ? S1 Co1 P1 O1 100.2(2) 2_666 . . . ? S2 Co1 P1 O1 23.8(2) 2_666 . . . ? S2 Co1 P1 O1 -156.2(2) . . . . ? P2 Co2 P2 O6 59(23) 2_677 . . . ? S3 Co2 P2 O6 -154.8(2) 2_677 . . . ? S3 Co2 P2 O6 25.2(2) . . . . ? S4 Co2 P2 O6 -51.4(2) . . . . ? S4 Co2 P2 O6 128.6(2) 2_677 . . . ? P2 Co2 P2 O4 -67(22) 2_677 . . . ? S3 Co2 P2 O4 79.19(16) 2_677 . . . ? S3 Co2 P2 O4 -100.81(16) . . . . ? S4 Co2 P2 O4 -177.40(16) . . . . ? S4 Co2 P2 O4 2.60(16) 2_677 . . . ? P2 Co2 P2 O5 176(23) 2_677 . . . ? S3 Co2 P2 O5 -37.1(2) 2_677 . . . ? S3 Co2 P2 O5 142.9(2) . . . . ? S4 Co2 P2 O5 66.3(2) . . . . ? S4 Co2 P2 O5 -113.7(2) 2_677 . . . ? O3 P1 O1 C23 56.6(7) . . . . ? O2 P1 O1 C23 -48.5(7) . . . . ? Co1 P1 O1 C23 -174.6(6) . . . . ? O3 P1 O2 C17 61.3(6) . . . . ? O1 P1 O2 C17 170.7(6) . . . . ? Co1 P1 O2 C17 -67.8(6) . . . . ? O2 P1 O3 C11 114.0(15) . . . . ? O1 P1 O3 C11 10.2(15) . . . . ? Co1 P1 O3 C11 -115.8(15) . . . . ? O6 P2 O4 C43 -53.8(5) . . . . ? O5 P2 O4 C43 -160.6(4) . . . . ? Co2 P2 O4 C43 75.4(4) . . . . ? O6 P2 O5 C37 -114.1(7) . . . . ? O4 P2 O5 C37 -4.9(8) . . . . ? Co2 P2 O5 C37 122.7(7) . . . . ? O4 P2 O6 C31 -53.5(6) . . . . ? O5 P2 O6 C31 50.1(6) . . . . ? Co2 P2 O6 C31 173.9(5) . . . . ? C3 N1 C1 S1 -176.1(4) . . . . ? C2 N1 C1 S1 -1.3(7) . . . . ? C3 N1 C1 S2 2.6(7) . . . . ? C2 N1 C1 S2 177.4(4) . . . . ? Co1 S1 C1 N1 173.2(4) . . . . ? Co1 S1 C1 S2 -5.6(2) . . . . ? Co1 S2 C1 N1 -173.2(4) . . . . ? Co1 S2 C1 S1 5.6(2) . . . . ? C6 N2 C4 S3 -178.1(4) . . . . ? C5 N2 C4 S3 2.1(7) . . . . ? C6 N2 C4 S4 2.1(7) . . . . ? C5 N2 C4 S4 -177.7(4) . . . . ? Co2 S3 C4 N2 179.7(4) . . . . ? Co2 S3 C4 S4 -0.5(2) . . . . ? Co2 S4 C4 N2 -179.7(4) . . . . ? Co2 S4 C4 S3 0.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.858 _refine_diff_density_min -0.766 _refine_diff_density_rms 0.094 #===END data_trPOMe2Ph _database_code_CSD 206917 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-Bis(dimethyldithiocarbamato)bis(dimethyl phenylphosphonito)cobalt(III) Tetrafluoroborate Acetone solvate ; _chemical_name_common trans-[Co(dtc)~2~{P(OMe)~2~Ph}~2~]BF~4~.(CH~3~)~2~CO _chemical_melting_point ? _chemical_formula_moiety 'C22 H34 Co N2 O4 P2 S4 1+, B F4 1-, C3 H6 O' _chemical_formula_sum 'C25 H40 B Co F4 N2 O5 P2 S4' _chemical_formula_weight 784.51 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' H H 0.0000 0.0000 '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 'P 1 21/a 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 11.025(2) _cell_length_b 12.5943(17) _cell_length_c 25.5808(18) _cell_angle_alpha 90.00 _cell_angle_beta 94.410(10) _cell_angle_gamma 90.00 _cell_volume 3541.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.868 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.948 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; A linear decay correction was applied ; _diffrn_ambient_temperature 296(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 AFC-5R' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.90 _diffrn_reflns_number 10839 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0747 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 30.01 _reflns_number_total 10336 _reflns_number_gt 3559 _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. 1.11' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP in teXsan' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0850P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0025(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10336 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1789 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1880 _refine_ls_wR_factor_gt 0.1427 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.0000 0.5000 0.0354(3) Uani 1 2 d S . . Co2 Co 0.0000 0.5000 0.0000 0.0347(3) Uani 1 2 d S . . S1 S 0.01380(12) 0.08231(11) 0.57868(5) 0.0434(4) Uani 1 1 d . . . S2 S 0.02602(12) -0.13656(10) 0.55754(5) 0.0461(4) Uani 1 1 d . . . S3 S 0.01686(11) 0.58135(11) 0.07934(5) 0.0426(4) Uani 1 1 d . . . S4 S 0.02616(12) 0.36235(10) 0.05672(5) 0.0447(4) Uani 1 1 d . . . P1 P 0.20490(13) -0.00427(12) 0.49839(5) 0.0410(4) Uani 1 1 d . . . P2 P 0.20516(12) 0.49501(11) -0.00255(5) 0.0387(4) Uani 1 1 d . . . F1 F 0.8071(5) 0.3129(6) 0.2195(2) 0.178(3) Uani 1 1 d . . . F2 F 0.6626(6) 0.4175(5) 0.2209(2) 0.207(3) Uani 1 1 d . . . F3 F 0.7041(5) 0.3117(5) 0.2843(2) 0.190(3) Uani 1 1 d . . . F4 F 0.8342(6) 0.4337(5) 0.2748(3) 0.252(4) Uani 1 1 d . . . O1 O 0.2723(3) 0.0818(3) 0.46491(15) 0.0628(11) Uani 1 1 d . . . O2 O 0.2474(3) -0.1179(3) 0.47892(13) 0.0539(10) Uani 1 1 d . . . O4 O 0.2700(3) 0.5820(3) -0.03685(13) 0.0536(10) Uani 1 1 d . . . O5 O 0.2440(3) 0.3814(3) -0.02344(13) 0.0519(10) Uani 1 1 d . . . O51 O 0.9179(4) 0.7322(4) 0.2447(2) 0.1097(16) Uani 1 1 d . . . N1 N 0.0547(4) -0.0625(4) 0.65646(17) 0.0619(14) Uani 1 1 d . . . N2 N 0.0607(4) 0.4373(4) 0.15488(16) 0.0580(14) Uani 1 1 d . . . C1 C 0.0362(4) -0.0414(4) 0.6061(2) 0.0473(16) Uani 1 1 d . . . C2 C 0.0664(6) 0.0246(5) 0.69459(19) 0.087(2) Uani 1 1 d . . . H2A H 0.0636 -0.0035 0.7294 0.107 Uiso 1 1 calc R . . H2B H 0.0007 0.0739 0.6876 0.107 Uiso 1 1 calc R . . H2C H 0.1425 0.0604 0.6918 0.107 Uiso 1 1 calc R . . C3 C 0.0732(6) -0.1722(5) 0.6755(2) 0.092(2) Uani 1 1 d . . . H3A H 0.0040 -0.2147 0.6638 0.109 Uiso 1 1 calc R . . H3B H 0.0824 -0.1723 0.7131 0.109 Uiso 1 1 calc R . . H3C H 0.1450 -0.2011 0.6620 0.109 Uiso 1 1 calc R . . C4 C 0.0375(4) 0.4559(4) 0.10500(17) 0.0421(15) Uani 1 1 d . . . C5 C 0.0746(6) 0.5218(5) 0.1942(2) 0.091(2) Uani 1 1 d . . . H5A H 0.1016 0.4917 0.2276 0.111 Uiso 1 1 calc R . . H5B H -0.0022 0.5566 0.1969 0.111 Uiso 1 1 calc R . . H5C H 0.1334 0.5725 0.1841 0.111 Uiso 1 1 calc R . . C6 C 0.0798(6) 0.3275(5) 0.1750(2) 0.083(2) Uani 1 1 d . . . H6A H 0.0160 0.2824 0.1601 0.108 Uiso 1 1 calc R . . H6B H 0.0788 0.3276 0.2125 0.108 Uiso 1 1 calc R . . H6C H 0.1569 0.3016 0.1654 0.108 Uiso 1 1 calc R . . C11 C 0.2956(4) 0.0158(4) 0.5590(2) 0.0474(15) Uani 1 1 d . . . C12 C 0.3278(5) -0.0653(4) 0.5942(2) 0.0623(18) Uani 1 1 d . . . H12 H 0.3026 -0.1341 0.5858 0.072 Uiso 1 1 calc R . . C13 C 0.3962(5) -0.0480(5) 0.6418(2) 0.0684(19) Uani 1 1 d . . . H13 H 0.4157 -0.1038 0.6647 0.084 Uiso 1 1 calc R . . C14 C 0.4343(5) 0.0544(5) 0.6537(2) 0.0715(19) Uani 1 1 d . . . H14 H 0.4803 0.0672 0.6851 0.094 Uiso 1 1 calc R . . C15 C 0.4051(5) 0.1390(4) 0.6197(2) 0.0583(16) Uani 1 1 d . . . H15 H 0.4309 0.2077 0.6279 0.077 Uiso 1 1 calc R . . C16 C 0.3362(4) 0.1172(5) 0.57310(19) 0.0526(16) Uani 1 1 d . . . H16 H 0.3162 0.1731 0.5503 0.066 Uiso 1 1 calc R . . C17 C 0.3732(5) -0.1410(4) 0.4719(2) 0.076(2) Uani 1 1 d . . . H17A H 0.3796 -0.2112 0.4577 0.096 Uiso 1 1 calc R . . H17B H 0.4198 -0.1370 0.5051 0.096 Uiso 1 1 calc R . . H17C H 0.4038 -0.0903 0.4481 0.096 Uiso 1 1 calc R . . C23 C 0.2676(5) 0.0843(5) 0.4095(2) 0.0712(18) Uani 1 1 d . . . H23A H 0.3449 0.1071 0.3986 0.084 Uiso 1 1 calc R . . H23B H 0.2055 0.1329 0.3964 0.084 Uiso 1 1 calc R . . H23C H 0.2495 0.0145 0.3959 0.084 Uiso 1 1 calc R . . C31 C 0.2986(4) 0.5170(5) 0.0590(2) 0.0494(16) Uani 1 1 d . . . C32 C 0.3255(4) 0.4297(5) 0.0906(2) 0.0608(18) Uani 1 1 d . . . H32 H 0.3000 0.3620 0.0802 0.078 Uiso 1 1 calc R . . C33 C 0.3916(6) 0.4462(6) 0.1383(3) 0.079(2) Uani 1 1 d . . . H33 H 0.4092 0.3884 0.1601 0.097 Uiso 1 1 calc R . . C34 C 0.4316(6) 0.5437(8) 0.1541(2) 0.093(3) Uani 1 1 d . . . H34 H 0.4763 0.5528 0.1861 0.099 Uiso 1 1 calc R . . C35 C 0.4044(5) 0.6287(6) 0.1217(2) 0.079(2) Uani 1 1 d . . . H35 H 0.4312 0.6958 0.1326 0.086 Uiso 1 1 calc R . . C36 C 0.3396(5) 0.6191(4) 0.0742(2) 0.0586(17) Uani 1 1 d . . . H36 H 0.3232 0.6778 0.0527 0.068 Uiso 1 1 calc R . . C37 C 0.3705(4) 0.3578(5) -0.0315(2) 0.0738(19) Uani 1 1 d . . . H37A H 0.3750 0.2919 -0.0501 0.086 Uiso 1 1 calc R . . H37B H 0.4163 0.3522 0.0019 0.086 Uiso 1 1 calc R . . H37C H 0.4036 0.4137 -0.0516 0.086 Uiso 1 1 calc R . . C43 C 0.2669(5) 0.5846(4) -0.09279(18) 0.0707(19) Uani 1 1 d . . . H43A H 0.3424 0.6125 -0.1033 0.089 Uiso 1 1 calc R . . H43B H 0.2011 0.6291 -0.1063 0.089 Uiso 1 1 calc R . . H43C H 0.2552 0.5140 -0.1064 0.089 Uiso 1 1 calc R . . C51 C 0.8151(7) 0.7085(5) 0.2460(3) 0.093(2) Uani 1 1 d . . . C52 C 0.7371(6) 0.6816(6) 0.1973(3) 0.140(3) Uani 1 1 d . . . H52A H 0.6552 0.6691 0.2061 0.168 Uiso 1 1 calc R . . H52B H 0.7680 0.6188 0.1817 0.168 Uiso 1 1 calc R . . H52C H 0.7381 0.7395 0.1730 0.168 Uiso 1 1 calc R . . C53 C 0.7554(7) 0.6999(7) 0.2942(3) 0.163(4) Uani 1 1 d . . . H53A H 0.7279 0.7687 0.3042 0.174 Uiso 1 1 calc R . . H53B H 0.8117 0.6723 0.3214 0.174 Uiso 1 1 calc R . . H53C H 0.6871 0.6528 0.2891 0.174 Uiso 1 1 calc R . . B B 0.7451(13) 0.3838(6) 0.2534(5) 0.084(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0381(7) 0.0336(6) 0.0348(6) -0.0008(5) 0.0054(5) 0.0046(6) Co2 0.0377(7) 0.0320(6) 0.0347(6) -0.0007(5) 0.0046(5) 0.0022(6) S1 0.0491(10) 0.0384(9) 0.0429(8) -0.0023(8) 0.0054(7) 0.0037(8) S2 0.0543(10) 0.0386(9) 0.0457(9) 0.0043(7) 0.0056(8) 0.0048(8) S3 0.0463(9) 0.0442(10) 0.0377(8) -0.0084(8) 0.0051(7) 0.0041(8) S4 0.0538(10) 0.0356(9) 0.0450(9) 0.0025(7) 0.0063(8) 0.0047(7) P1 0.0387(10) 0.0430(11) 0.0417(9) -0.0003(9) 0.0055(8) 0.0026(10) P2 0.0367(9) 0.0375(10) 0.0428(9) -0.0004(9) 0.0092(8) 0.0030(9) F1 0.134(4) 0.254(7) 0.151(5) -0.053(5) 0.029(4) -0.017(4) F2 0.215(7) 0.194(6) 0.197(6) 0.068(5) -0.086(5) 0.018(5) F3 0.165(5) 0.268(7) 0.143(5) 0.091(5) 0.047(4) 0.062(5) F4 0.211(7) 0.237(7) 0.290(8) -0.097(6) -0.086(6) -0.098(6) O1 0.058(3) 0.066(3) 0.066(3) 0.012(2) 0.012(2) -0.008(2) O2 0.045(3) 0.049(3) 0.068(3) -0.012(2) 0.007(2) 0.009(2) O4 0.060(3) 0.060(2) 0.044(2) 0.003(2) 0.0175(19) -0.011(2) O5 0.042(2) 0.050(3) 0.064(2) -0.011(2) 0.010(2) 0.010(2) O51 0.070(3) 0.125(4) 0.135(4) -0.001(3) 0.014(3) -0.025(3) N1 0.069(4) 0.077(4) 0.041(3) 0.001(3) 0.009(3) 0.011(3) N2 0.068(3) 0.069(4) 0.037(3) 0.014(3) 0.003(2) 0.015(3) C1 0.045(4) 0.044(4) 0.054(4) -0.009(3) 0.010(3) -0.001(3) C2 0.112(6) 0.104(5) 0.042(3) -0.010(4) -0.007(3) 0.013(4) C3 0.121(6) 0.086(5) 0.070(5) 0.045(4) 0.007(4) 0.029(4) C4 0.045(4) 0.056(4) 0.026(3) 0.008(3) 0.005(2) 0.006(3) C5 0.113(6) 0.120(6) 0.041(3) -0.021(4) 0.008(4) 0.021(4) C6 0.108(6) 0.088(5) 0.053(4) 0.019(4) 0.018(4) 0.011(4) C11 0.040(4) 0.047(4) 0.056(4) -0.008(3) 0.010(3) -0.005(3) C12 0.068(5) 0.046(3) 0.071(4) 0.015(3) -0.007(4) 0.011(3) C13 0.059(4) 0.080(5) 0.065(4) 0.018(4) -0.003(3) 0.013(4) C14 0.062(4) 0.092(5) 0.061(4) -0.022(4) 0.009(3) -0.015(4) C15 0.054(4) 0.059(3) 0.063(4) -0.002(3) 0.016(3) -0.014(3) C16 0.033(3) 0.079(5) 0.045(3) -0.009(3) 0.000(2) 0.000(3) C17 0.066(5) 0.074(4) 0.093(5) -0.014(3) 0.026(4) 0.028(4) C23 0.047(4) 0.091(5) 0.076(4) 0.010(4) 0.012(3) -0.013(4) C31 0.035(3) 0.068(4) 0.044(3) 0.002(3) -0.004(3) 0.016(3) C32 0.045(4) 0.087(5) 0.050(3) -0.003(4) 0.004(3) 0.003(3) C33 0.064(5) 0.113(7) 0.058(4) 0.011(4) -0.007(3) 0.013(5) C34 0.053(4) 0.182(9) 0.043(4) -0.001(5) -0.008(3) -0.003(5) C35 0.051(4) 0.125(6) 0.059(4) -0.043(4) 0.001(3) -0.014(4) C36 0.054(4) 0.043(3) 0.082(5) -0.006(3) 0.022(3) -0.005(3) C37 0.046(4) 0.085(5) 0.091(5) -0.016(4) 0.010(4) 0.016(4) C43 0.083(5) 0.090(5) 0.042(3) 0.018(3) 0.027(3) 0.001(4) C51 0.081(4) 0.059(4) 0.140(7) -0.007(4) 0.014(4) 0.012(3) C52 0.098(6) 0.123(7) 0.193(9) 0.042(6) -0.031(6) -0.036(5) C53 0.153(8) 0.156(8) 0.193(10) -0.068(8) 0.101(7) -0.025(7) B 0.093(5) 0.078(4) 0.076(5) 0.024(6) -0.020(4) -0.023(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 S1 2.2587(12) . ? Co1 S1 2.2588(12) 3_556 ? Co1 P1 2.2632(15) 3_556 ? Co1 P1 2.2632(15) . ? Co1 S2 2.2675(12) 3_556 ? Co1 S2 2.2675(12) . ? Co2 S4 2.2647(12) . ? Co2 S4 2.2648(12) 3_565 ? Co2 S3 2.2684(12) . ? Co2 S3 2.2684(12) 3_565 ? Co2 P2 2.2688(14) 3_565 ? Co2 P2 2.2688(14) . ? S1 C1 1.719(6) . ? S2 C1 1.724(5) . ? S3 C4 1.719(5) . ? S4 C4 1.705(5) . ? P1 O2 1.597(3) . ? P1 O1 1.600(4) . ? P1 C11 1.796(5) . ? P2 O5 1.598(3) . ? P2 O4 1.605(3) . ? P2 C31 1.835(5) . ? F1 B 1.451(11) . ? F2 B 1.258(11) . ? F3 B 1.307(9) . ? F4 B 1.255(11) . ? O1 C23 1.414(5) . ? O2 C17 1.442(5) . ? O4 C43 1.429(5) . ? O5 C37 1.456(5) . ? O51 C51 1.175(8) . ? N1 C1 1.315(6) . ? N1 C2 1.466(6) . ? N1 C3 1.474(6) . ? N2 C4 1.303(5) . ? N2 C5 1.465(6) . ? N2 C6 1.485(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 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C11 C12 1.391(6) . ? C11 C16 1.391(6) . ? C12 C13 1.398(7) . ? C12 H12 0.9300 . ? C13 C14 1.383(7) . ? C13 H13 0.9300 . ? C14 C15 1.398(7) . ? C14 H14 0.9300 . ? C15 C16 1.391(6) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C31 C32 1.384(6) . ? C31 C36 1.408(6) . ? C32 C33 1.387(7) . ? C32 H32 0.9300 . ? C33 C34 1.356(9) . ? C33 H33 0.9300 . ? C34 C35 1.372(9) . ? C34 H34 0.9300 . ? C35 C36 1.367(7) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C51 C53 1.446(9) . ? C51 C52 1.497(9) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 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 S1 Co1 S1 180.0 . 3_556 ? S1 Co1 P1 88.39(5) . 3_556 ? S1 Co1 P1 91.61(5) 3_556 3_556 ? S1 Co1 P1 91.61(5) . . ? S1 Co1 P1 88.39(5) 3_556 . ? P1 Co1 P1 180.0 3_556 . ? S1 Co1 S2 103.11(5) . 3_556 ? S1 Co1 S2 76.89(5) 3_556 3_556 ? P1 Co1 S2 85.24(5) 3_556 3_556 ? P1 Co1 S2 94.75(5) . 3_556 ? S1 Co1 S2 76.89(5) . . ? S1 Co1 S2 103.11(5) 3_556 . ? P1 Co1 S2 94.75(5) 3_556 . ? P1 Co1 S2 85.25(5) . . ? S2 Co1 S2 180.0 3_556 . ? S4 Co2 S4 180.0 . 3_565 ? S4 Co2 S3 76.99(5) . . ? S4 Co2 S3 103.01(5) 3_565 . ? S4 Co2 S3 103.01(5) . 3_565 ? S4 Co2 S3 76.99(5) 3_565 3_565 ? S3 Co2 S3 180.0 . 3_565 ? S4 Co2 P2 94.64(5) . 3_565 ? S4 Co2 P2 85.36(5) 3_565 3_565 ? S3 Co2 P2 88.57(5) . 3_565 ? S3 Co2 P2 91.43(5) 3_565 3_565 ? S4 Co2 P2 85.36(5) . . ? S4 Co2 P2 94.64(5) 3_565 . ? S3 Co2 P2 91.43(5) . . ? S3 Co2 P2 88.57(5) 3_565 . ? P2 Co2 P2 180.0 3_565 . ? C1 S1 Co1 86.89(18) . . ? C1 S2 Co1 86.5(2) . . ? C4 S3 Co2 85.76(16) . . ? C4 S4 Co2 86.19(16) . . ? O2 P1 O1 106.32(19) . . ? O2 P1 C11 103.8(2) . . ? O1 P1 C11 96.6(2) . . ? O2 P1 Co1 110.12(15) . . ? O1 P1 Co1 119.92(15) . . ? C11 P1 Co1 118.13(18) . . ? O5 P2 O4 106.66(18) . . ? O5 P2 C31 106.0(2) . . ? O4 P2 C31 97.0(2) . . ? O5 P2 Co2 109.13(14) . . ? O4 P2 Co2 118.92(14) . . ? C31 P2 Co2 117.81(18) . . ? C23 O1 P1 124.7(4) . . ? C17 O2 P1 121.9(3) . . ? C43 O4 P2 125.9(3) . . ? C37 O5 P2 120.9(3) . . ? C1 N1 C2 120.0(5) . . ? C1 N1 C3 121.3(5) . . ? C2 N1 C3 118.6(5) . . ? C4 N2 C5 123.0(5) . . ? C4 N2 C6 121.2(5) . . ? C5 N2 C6 115.7(4) . . ? N1 C1 S1 126.1(4) . . ? N1 C1 S2 124.2(5) . . ? S1 C1 S2 109.6(3) . . ? 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 C4 S4 125.7(4) . . ? N2 C4 S3 123.3(4) . . ? S4 C4 S3 111.0(2) . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C11 C16 116.4(5) . . ? C12 C11 P1 123.6(4) . . ? C16 C11 P1 120.0(4) . . ? C11 C12 C13 122.9(5) . . ? C11 C12 H12 118.5 . . ? C13 C12 H12 118.5 . . ? C14 C13 C12 118.2(6) . . ? C14 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? C13 C14 C15 121.4(6) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C16 C15 C14 117.9(5) . . ? C16 C15 H15 121.0 . . ? C14 C15 H15 121.0 . . ? C15 C16 C11 123.2(5) . . ? C15 C16 H16 118.4 . . ? C11 C16 H16 118.4 . . ? O2 C17 H17A 109.5 . . ? O2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O1 C23 H23A 109.5 . . ? O1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C32 C31 C36 121.0(5) . . ? C32 C31 P2 117.5(5) . . ? C36 C31 P2 121.5(5) . . ? C31 C32 C33 118.0(6) . . ? C31 C32 H32 121.0 . . ? C33 C32 H32 121.0 . . ? C34 C33 C32 122.4(7) . . ? C34 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? C33 C34 C35 118.4(6) . . ? C33 C34 H34 120.8 . . ? C35 C34 H34 120.8 . . ? C36 C35 C34 122.8(6) . . ? C36 C35 H35 118.6 . . ? C34 C35 H35 118.6 . . ? C35 C36 C31 117.5(6) . . ? C35 C36 H36 121.3 . . ? C31 C36 H36 121.3 . . ? O5 C37 H37A 109.5 . . ? O5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O4 C43 H43A 109.5 . . ? O4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O51 C51 C53 123.1(8) . . ? O51 C51 C52 121.9(8) . . ? C53 C51 C52 115.0(7) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? F4 B F2 128.4(8) . . ? F4 B F3 112.3(10) . . ? F2 B F3 111.5(11) . . ? F4 B F1 100.4(12) . . ? F2 B F1 99.4(9) . . ? F3 B F1 97.8(6) . . ? 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 Co1 S1 C1 -88(100) 3_556 . . . ? P1 Co1 S1 C1 97.17(17) 3_556 . . . ? P1 Co1 S1 C1 -82.83(17) . . . . ? S2 Co1 S1 C1 -178.09(17) 3_556 . . . ? S2 Co1 S1 C1 1.91(17) . . . . ? S1 Co1 S2 C1 -1.91(17) . . . . ? S1 Co1 S2 C1 178.09(17) 3_556 . . . ? P1 Co1 S2 C1 -89.14(17) 3_556 . . . ? P1 Co1 S2 C1 90.86(17) . . . . ? S2 Co1 S2 C1 -88(26) 3_556 . . . ? S4 Co2 S3 C4 1.55(16) . . . . ? S4 Co2 S3 C4 -178.45(16) 3_565 . . . ? S3 Co2 S3 C4 7.1(3) 3_565 . . . ? P2 Co2 S3 C4 96.64(16) 3_565 . . . ? P2 Co2 S3 C4 -83.36(16) . . . . ? S4 Co2 S4 C4 159.1(9) 3_565 . . . ? S3 Co2 S4 C4 -1.56(16) . . . . ? S3 Co2 S4 C4 178.44(16) 3_565 . . . ? P2 Co2 S4 C4 -89.01(16) 3_565 . . . ? P2 Co2 S4 C4 90.99(16) . . . . ? S1 Co1 P1 O2 136.27(15) . . . . ? S1 Co1 P1 O2 -43.73(15) 3_556 . . . ? P1 Co1 P1 O2 -47(4) 3_556 . . . ? S2 Co1 P1 O2 -120.43(15) 3_556 . . . ? S2 Co1 P1 O2 59.57(15) . . . . ? S1 Co1 P1 O1 -99.95(19) . . . . ? S1 Co1 P1 O1 80.05(19) 3_556 . . . ? P1 Co1 P1 O1 77(4) 3_556 . . . ? S2 Co1 P1 O1 3.35(19) 3_556 . . . ? S2 Co1 P1 O1 -176.65(19) . . . . ? S1 Co1 P1 C11 17.4(2) . . . . ? S1 Co1 P1 C11 -162.6(2) 3_556 . . . ? P1 Co1 P1 C11 -166(4) 3_556 . . . ? S2 Co1 P1 C11 120.7(2) 3_556 . . . ? S2 Co1 P1 C11 -59.3(2) . . . . ? S4 Co2 P2 O5 60.11(14) . . . . ? S4 Co2 P2 O5 -119.89(14) 3_565 . . . ? S3 Co2 P2 O5 136.93(15) . . . . ? S3 Co2 P2 O5 -43.07(15) 3_565 . . . ? P2 Co2 P2 O5 47.9(3) 3_565 . . . ? S4 Co2 P2 O4 -177.32(16) . . . . ? S4 Co2 P2 O4 2.68(16) 3_565 . . . ? S3 Co2 P2 O4 -100.50(16) . . . . ? S3 Co2 P2 O4 79.50(16) 3_565 . . . ? P2 Co2 P2 O4 170.5(3) 3_565 . . . ? S4 Co2 P2 C31 -60.7(2) . . . . ? S4 Co2 P2 C31 119.3(2) 3_565 . . . ? S3 Co2 P2 C31 16.1(2) . . . . ? S3 Co2 P2 C31 -163.9(2) 3_565 . . . ? P2 Co2 P2 C31 -72.9(4) 3_565 . . . ? O2 P1 O1 C23 54.0(4) . . . . ? C11 P1 O1 C23 160.5(4) . . . . ? Co1 P1 O1 C23 -71.6(4) . . . . ? O1 P1 O2 C17 45.7(4) . . . . ? C11 P1 O2 C17 -55.6(4) . . . . ? Co1 P1 O2 C17 177.1(3) . . . . ? O5 P2 O4 C43 50.3(4) . . . . ? C31 P2 O4 C43 159.3(4) . . . . ? Co2 P2 O4 C43 -73.5(4) . . . . ? O4 P2 O5 C37 47.3(4) . . . . ? C31 P2 O5 C37 -55.3(4) . . . . ? Co2 P2 O5 C37 177.0(3) . . . . ? C2 N1 C1 S1 -4.4(8) . . . . ? C3 N1 C1 S1 -179.8(4) . . . . ? C2 N1 C1 S2 177.8(4) . . . . ? C3 N1 C1 S2 2.3(8) . . . . ? Co1 S1 C1 N1 179.3(5) . . . . ? Co1 S1 C1 S2 -2.6(2) . . . . ? Co1 S2 C1 N1 -179.2(5) . . . . ? Co1 S2 C1 S1 2.6(2) . . . . ? C5 N2 C4 S4 177.2(4) . . . . ? C6 N2 C4 S4 -0.3(7) . . . . ? C5 N2 C4 S3 -1.5(7) . . . . ? C6 N2 C4 S3 -179.0(4) . . . . ? Co2 S4 C4 N2 -176.7(5) . . . . ? Co2 S4 C4 S3 2.2(2) . . . . ? Co2 S3 C4 N2 176.7(4) . . . . ? Co2 S3 C4 S4 -2.1(2) . . . . ? O2 P1 C11 C12 -36.1(5) . . . . ? O1 P1 C11 C12 -144.7(5) . . . . ? Co1 P1 C11 C12 86.1(5) . . . . ? O2 P1 C11 C16 144.9(4) . . . . ? O1 P1 C11 C16 36.3(5) . . . . ? Co1 P1 C11 C16 -92.9(4) . . . . ? C16 C11 C12 C13 0.5(9) . . . . ? P1 C11 C12 C13 -178.6(5) . . . . ? C11 C12 C13 C14 -0.6(9) . . . . ? C12 C13 C14 C15 0.4(9) . . . . ? C13 C14 C15 C16 0.0(8) . . . . ? C14 C15 C16 C11 -0.1(8) . . . . ? C12 C11 C16 C15 -0.1(8) . . . . ? P1 C11 C16 C15 179.0(4) . . . . ? O5 P2 C31 C32 -35.4(5) . . . . ? O4 P2 C31 C32 -145.0(4) . . . . ? Co2 P2 C31 C32 87.0(4) . . . . ? O5 P2 C31 C36 145.9(4) . . . . ? O4 P2 C31 C36 36.3(5) . . . . ? Co2 P2 C31 C36 -91.7(5) . . . . ? C36 C31 C32 C33 1.5(8) . . . . ? P2 C31 C32 C33 -177.2(4) . . . . ? C31 C32 C33 C34 -1.0(10) . . . . ? C32 C33 C34 C35 0.5(11) . . . . ? C33 C34 C35 C36 -0.4(10) . . . . ? C34 C35 C36 C31 0.8(9) . . . . ? C32 C31 C36 C35 -1.4(8) . . . . ? P2 C31 C36 C35 177.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.877 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.073 #===END data_trPPh2OMe _database_code_CSD 206918 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-Bis(N,N-dimethyldithiocarbamato)bis(methyl diphenylphosphinito) cobalt(III) tetrafluoroborate hemimethanol solvate ; _chemical_name_common trans-[Co(dtc)~2~(PPh~2~(OMe))~2~]BF~4~.0.5MeOH _chemical_melting_point ? _chemical_formula_moiety '2(C32 H38 Co N2 O2 P2 S4 1+), 2(B F4 1-), (C H4 O)' _chemical_formula_sum 'C65 H80 B2 Co2 F8 N4 O5 P4 S8' _chemical_formula_weight 1669.17 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6508(5) _cell_length_b 10.9697(8) _cell_length_c 37.114(3) _cell_angle_alpha 88.261(8) _cell_angle_beta 84.228(7) _cell_angle_gamma 85.066(8) _cell_volume 3893.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5443 _cell_measurement_theta_min 4.2104 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 0.790 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.641 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_radiation_detector CCD _diffrn_measurement_device 'Mercury CCD (2x2 bin mode)' _diffrn_source_power 9.0000 _diffrn_source_voltage 50.0000 _diffrn_source_current 180.0000 _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19442 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 4.21 _diffrn_reflns_theta_max 27.44 _reflns_number_total 12588 _reflns_number_gt 10170 _reflns_threshold_expression 'I > 2\s(I)' _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_measurement_details ; scan: Number of images: 900 Slice: -80.0000 - 100.0000 Image width: 0.2000 Exp time: 15.0000 Rotation axis: Phi Omega: 0.0000 Chi: 0.0000 Phi: 0.0000 XTD: 85.5886 2theta: 29.9219 scan: Number of images: 260 Slice: -10.0000 - 42.0000 Image width: 0.2000 Exp time: 15.0000 Rotation axis: Omega Omega: 0.0000 Chi: 90.0000 Phi: 0.0000 XTD: 85.5886 2theta: 29.9219 scan: Number of images: 260 Slice: -10.0000 - 42.0000 Image width: 0.2000 Exp time: 15.0000 Rotation axis: Omega Omega: 0.0000 Chi: 90.0000 Phi: 90.0000 XTD: 85.5886 2theta: 29.9219 scan: Number of images: 260 Slice: -10.0000 - 42.0000 Image width: 0.2000 Exp time: 15.0000 Rotation axis: Omega Omega: 0.0000 Chi: 90.0000 Phi: 180.0000 XTD: 85.5886 2theta: 29.9219 scan: Number of images: 260 Slice: -10.0000 - 42.0000 Image width: 0.2000 Exp time: 15.0000 Rotation axis: Omega Omega: 0.0000 Chi: 90.0000 Phi: 270.0000 XTD: 85.5886 2theta: 29.9219 ; _diffrn_measurement_device_details ; AFC7: Eulerian 3-circle ; _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+14.1476P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12588 _refine_ls_number_parameters 897 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1202 _refine_ls_R_factor_gt 0.0929 _refine_ls_wR_factor_ref 0.1879 _refine_ls_wR_factor_gt 0.1756 _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_restrained_S_all 1.215 _refine_ls_shift/su_max 0.005 _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 0.47987(8) 0.83730(8) 0.27384(2) 0.0366(2) Uani 1 1 d . . . Co51 Co 0.5000 0.5000 0.0000 0.0355(3) Uani 1 2 d S . . Co52 Co 0.5000 1.0000 0.5000 0.0343(3) Uani 1 2 d S . . S1 S 0.24298(17) 0.86867(16) 0.27500(5) 0.0452(4) Uani 1 1 d . . . S2 S 0.44095(16) 0.83755(15) 0.21425(5) 0.0413(4) Uani 1 1 d . . . S3 S 0.71565(16) 0.81163(16) 0.27652(5) 0.0417(4) Uani 1 1 d . . . S4 S 0.50207(18) 0.82613(18) 0.33432(5) 0.0493(4) Uani 1 1 d . . . S51 S 0.26653(16) 0.49869(15) -0.00560(5) 0.0421(4) Uani 1 1 d . . . S52 S 0.43266(17) 0.69793(16) -0.01486(5) 0.0448(4) Uani 1 1 d . . . S53 S 0.53001(17) 0.98715(15) 0.55992(5) 0.0408(4) Uani 1 1 d . . . S54 S 0.73417(17) 0.95561(15) 0.50015(5) 0.0432(4) Uani 1 1 d . . . P1 P 0.48698(17) 0.63259(15) 0.26579(5) 0.0387(4) Uani 1 1 d . . . P2 P 0.48258(18) 1.04732(16) 0.27546(5) 0.0420(4) Uani 1 1 d . . . P51 P 0.46459(17) 0.56300(16) 0.05857(5) 0.0406(4) Uani 1 1 d . . . P52 P 0.48253(17) 0.79341(15) 0.49516(5) 0.0367(4) Uani 1 1 d . . . F1 F -0.0078(9) 0.0470(7) 0.1116(2) 0.160(3) Uani 1 1 d . . . F2 F 0.0368(16) 0.2206(13) 0.1258(5) 0.284(7) Uani 1 1 d . . . F3 F -0.0755(13) 0.1307(12) 0.1647(3) 0.237(6) Uani 1 1 d . . . F4 F -0.1648(11) 0.2009(10) 0.1163(3) 0.221(6) Uani 1 1 d . . . F5 F 0.9361(9) 0.4429(11) 0.4190(2) 0.189(4) Uani 1 1 d . . . F6 F 0.8606(8) 0.4612(10) 0.3629(3) 0.193(4) Uani 1 1 d . . . F7 F 1.0546(12) 0.3556(13) 0.3707(3) 0.222(6) Uani 1 1 d . . . F8A F 1.0504(14) 0.5246(11) 0.3774(3) 0.148(5) Uani 0.67 1 d P . . F8B F 0.906(3) 0.318(2) 0.3959(7) 0.152(10) Uani 0.33 1 d P . . O1 O 0.5162(5) 0.5434(4) 0.29998(13) 0.0526(12) Uani 1 1 d . . . O4 O 0.3633(5) 1.1060(4) 0.30487(13) 0.0517(12) Uani 1 1 d . . . O51 O 0.4981(6) 0.4608(5) 0.08937(14) 0.0635(14) Uani 1 1 d . . . O54 O 0.5989(5) 0.7383(4) 0.46411(12) 0.0463(11) Uani 1 1 d . . . O98 O 0.2047(13) 0.0549(12) 0.0486(3) 0.196(5) Uani 1 1 d . . . H98 H 0.1481 0.0743 0.0658 0.196 Uiso 1 1 calc R . . N1 N 0.1672(6) 0.8730(6) 0.20665(17) 0.0531(15) Uani 1 1 d . . . N2 N 0.7761(6) 0.8061(6) 0.34571(16) 0.0566(16) Uani 1 1 d . . . N51 N 0.1543(6) 0.7259(5) -0.01979(16) 0.0498(15) Uani 1 1 d . . . N52 N 0.8025(6) 0.9371(5) 0.56909(17) 0.0520(15) Uani 1 1 d . . . C1 C 0.2664(7) 0.8631(6) 0.22860(19) 0.0424(16) Uani 1 1 d . . . C2 C 0.0179(8) 0.8839(10) 0.2211(3) 0.083(3) Uani 1 1 d . . . H2A H 0.0052 0.9370 0.2415 0.083 Uiso 1 1 calc R . . H2B H -0.0103 0.8045 0.2286 0.083 Uiso 1 1 calc R . . H2C H -0.0379 0.9173 0.2026 0.083 Uiso 1 1 calc R . . C3 C 0.1990(9) 0.8665(9) 0.1672(2) 0.076(3) Uani 1 1 d . . . H3A H 0.2216 0.7827 0.1606 0.076 Uiso 1 1 calc R . . H3B H 0.2771 0.9131 0.1597 0.076 Uiso 1 1 calc R . . H3C H 0.1191 0.8995 0.1556 0.076 Uiso 1 1 calc R . . C4 C 0.6808(7) 0.8135(6) 0.32288(18) 0.0438(16) Uani 1 1 d . . . C5 C 0.9253(7) 0.7981(9) 0.3330(2) 0.073(3) Uani 1 1 d . . . H5A H 0.9528 0.8783 0.3262 0.073 Uiso 1 1 calc R . . H5B H 0.9423 0.7462 0.3123 0.073 Uiso 1 1 calc R . . H5C H 0.9784 0.7644 0.3520 0.073 Uiso 1 1 calc R . . C6 C 0.7400(9) 0.8085(10) 0.3849(2) 0.082(3) Uani 1 1 d . . . H6A H 0.8137 0.7649 0.3969 0.082 Uiso 1 1 calc R . . H6B H 0.6546 0.7705 0.3910 0.082 Uiso 1 1 calc R . . H6C H 0.7282 0.8918 0.3927 0.082 Uiso 1 1 calc R . . C11 C 0.3227(7) 0.5749(6) 0.25669(19) 0.0432(16) Uani 1 1 d . . . C12 C 0.2872(8) 0.5605(7) 0.2219(2) 0.0563(19) Uani 1 1 d . . . H12 H 0.3506 0.5768 0.2022 0.068 Uiso 1 1 calc R . . C13 C 0.1570(9) 0.5217(8) 0.2162(3) 0.071(2) Uani 1 1 d . . . H13 H 0.1342 0.5120 0.1927 0.087 Uiso 1 1 calc R . . C14 C 0.0626(9) 0.4977(8) 0.2455(3) 0.074(3) Uani 1 1 d . . . H14 H -0.0247 0.4734 0.2417 0.089 Uiso 1 1 calc R . . C15 C 0.0966(8) 0.5096(7) 0.2803(3) 0.066(2) Uani 1 1 d . . . H15 H 0.0336 0.4911 0.3000 0.082 Uiso 1 1 calc R . . C16 C 0.2253(7) 0.5493(6) 0.2861(2) 0.0522(18) Uani 1 1 d . . . H16 H 0.2472 0.5590 0.3096 0.067 Uiso 1 1 calc R . . C17 C 0.6135(7) 0.5700(6) 0.22975(18) 0.0405(15) Uani 1 1 d . . . C18 C 0.7043(6) 0.6396(6) 0.20796(17) 0.0407(15) Uani 1 1 d . . . H18 H 0.6981 0.7240 0.2106 0.050 Uiso 1 1 calc R . . C19 C 0.8044(7) 0.5855(7) 0.18229(18) 0.0487(17) Uani 1 1 d . . . H19 H 0.8636 0.6339 0.1680 0.060 Uiso 1 1 calc R . . C20 C 0.8160(8) 0.4607(7) 0.1780(2) 0.0545(19) Uani 1 1 d . . . H20 H 0.8838 0.4249 0.1611 0.067 Uiso 1 1 calc R . . C21 C 0.7274(9) 0.3889(7) 0.1989(2) 0.063(2) Uani 1 1 d . . . H21 H 0.7340 0.3048 0.1958 0.077 Uiso 1 1 calc R . . C22 C 0.6264(8) 0.4437(6) 0.2250(2) 0.0533(18) Uani 1 1 d . . . H22 H 0.5675 0.3948 0.2392 0.063 Uiso 1 1 calc R . . C23 C 0.6506(8) 0.5119(7) 0.3125(2) 0.063(2) Uani 1 1 d . . . H23A H 0.6549 0.5495 0.3353 0.063 Uiso 1 1 calc R . . H23B H 0.7218 0.5406 0.2951 0.063 Uiso 1 1 calc R . . H23C H 0.6653 0.4247 0.3153 0.063 Uiso 1 1 calc R . . C31 C 0.6417(8) 1.1050(6) 0.2888(2) 0.0507(18) Uani 1 1 d . . . C32 C 0.6539(9) 1.1115(8) 0.3256(3) 0.070(2) Uani 1 1 d . . . H32 H 0.5804 1.0908 0.3422 0.086 Uiso 1 1 calc R . . C33 C 0.7760(12) 1.1490(9) 0.3381(3) 0.089(3) Uani 1 1 d . . . H33 H 0.7838 1.1523 0.3628 0.112 Uiso 1 1 calc R . . C34 C 0.8827(12) 1.1804(10) 0.3137(4) 0.101(4) Uani 1 1 d . . . H34 H 0.9627 1.2065 0.3220 0.118 Uiso 1 1 calc R . . C35 C 0.8750(10) 1.1745(9) 0.2773(4) 0.096(3) Uani 1 1 d . . . H35 H 0.9495 1.1951 0.2611 0.110 Uiso 1 1 calc R . . C36 C 0.7530(9) 1.1367(8) 0.2646(3) 0.072(2) Uani 1 1 d . . . H36 H 0.7470 1.1329 0.2398 0.091 Uiso 1 1 calc R . . C37 C 0.4424(8) 1.1208(6) 0.2323(2) 0.0524(18) Uani 1 1 d . . . C38 C 0.5363(11) 1.1145(8) 0.2014(2) 0.074(3) Uani 1 1 d . . . H38 H 0.6272 1.0801 0.2028 0.091 Uiso 1 1 calc R . . C39 C 0.4946(17) 1.1596(10) 0.1682(3) 0.104(4) Uani 1 1 d . . . H39 H 0.5584 1.1572 0.1476 0.126 Uiso 1 1 calc R . . C40 C 0.358(2) 1.2080(11) 0.1659(4) 0.130(6) Uani 1 1 d . . . H40 H 0.3293 1.2378 0.1439 0.151 Uiso 1 1 calc R . . C41 C 0.2670(15) 1.2111(10) 0.1963(4) 0.110(4) Uani 1 1 d . . . H41 H 0.1751 1.2422 0.1946 0.135 Uiso 1 1 calc R . . C42 C 0.3063(10) 1.1697(8) 0.2294(3) 0.074(3) Uani 1 1 d . . . H42 H 0.2419 1.1745 0.2498 0.093 Uiso 1 1 calc R . . C43 C 0.3474(9) 1.2381(7) 0.3114(2) 0.071(2) Uani 1 1 d . . . H43A H 0.3819 1.2815 0.2900 0.071 Uiso 1 1 calc R . . H43B H 0.3994 1.2553 0.3311 0.071 Uiso 1 1 calc R . . H43C H 0.2503 1.2637 0.3174 0.071 Uiso 1 1 calc R . . C51 C 0.2668(6) 0.6528(6) -0.01423(18) 0.0406(15) Uani 1 1 d . . . C52 C 0.0162(7) 0.6806(8) -0.0177(3) 0.069(2) Uani 1 1 d . . . H52A H -0.0430 0.7336 -0.0318 0.069 Uiso 1 1 calc R . . H52B H -0.0234 0.6791 0.0070 0.069 Uiso 1 1 calc R . . H52C H 0.0239 0.5994 -0.0271 0.069 Uiso 1 1 calc R . . C53 C 0.1644(9) 0.8574(7) -0.0258(2) 0.067(2) Uani 1 1 d . . . H53A H 0.0855 0.8919 -0.0376 0.067 Uiso 1 1 calc R . . H53B H 0.2489 0.8708 -0.0408 0.067 Uiso 1 1 calc R . . H53C H 0.1654 0.8959 -0.0029 0.067 Uiso 1 1 calc R . . C54 C 0.7049(7) 0.9562(6) 0.54658(18) 0.0412(15) Uani 1 1 d . . . C55 C 0.7690(9) 0.9350(9) 0.6084(2) 0.079(3) Uani 1 1 d . . . H55A H 0.8508 0.9060 0.6199 0.079 Uiso 1 1 calc R . . H55B H 0.6964 0.8815 0.6148 0.079 Uiso 1 1 calc R . . H55C H 0.7379 1.0161 0.6164 0.079 Uiso 1 1 calc R . . C56 C 0.9510(8) 0.9178(9) 0.5560(3) 0.082(3) Uani 1 1 d . . . H56A H 0.9984 0.8649 0.5727 0.082 Uiso 1 1 calc R . . H56B H 0.9913 0.9950 0.5540 0.082 Uiso 1 1 calc R . . H56C H 0.9606 0.8808 0.5327 0.082 Uiso 1 1 calc R . . C61 C 0.2817(7) 0.6023(7) 0.07433(18) 0.0454(16) Uani 1 1 d . . . C62 C 0.2192(8) 0.7213(7) 0.0717(2) 0.0568(19) Uani 1 1 d . . . H62 H 0.2737 0.7846 0.0638 0.071 Uiso 1 1 calc R . . C63 C 0.0760(9) 0.7465(9) 0.0809(2) 0.071(2) Uani 1 1 d . . . H63 H 0.0356 0.8264 0.0796 0.085 Uiso 1 1 calc R . . C64 C -0.0052(9) 0.6517(11) 0.0918(2) 0.082(3) Uani 1 1 d . . . H64 H -0.1013 0.6677 0.0969 0.100 Uiso 1 1 calc R . . C65 C 0.0536(9) 0.5354(11) 0.0953(2) 0.079(3) Uani 1 1 d . . . H65 H -0.0018 0.4731 0.1036 0.095 Uiso 1 1 calc R . . C66 C 0.1977(8) 0.5088(8) 0.0863(2) 0.063(2) Uani 1 1 d . . . H66 H 0.2373 0.4288 0.0884 0.078 Uiso 1 1 calc R . . C67 C 0.5536(6) 0.6949(6) 0.07062(18) 0.0406(15) Uani 1 1 d . . . C68 C 0.6384(7) 0.7603(6) 0.0464(2) 0.0470(17) Uani 1 1 d . . . H68 H 0.6512 0.7382 0.0223 0.058 Uiso 1 1 calc R . . C69 C 0.7047(8) 0.8579(7) 0.0573(2) 0.0562(19) Uani 1 1 d . . . H69 H 0.7616 0.9003 0.0404 0.068 Uiso 1 1 calc R . . C70 C 0.6866(9) 0.8924(8) 0.0929(3) 0.069(2) Uani 1 1 d . . . H70 H 0.7307 0.9583 0.1002 0.083 Uiso 1 1 calc R . . C71 C 0.6030(10) 0.8291(9) 0.1175(2) 0.077(3) Uani 1 1 d . . . H71 H 0.5912 0.8517 0.1416 0.090 Uiso 1 1 calc R . . C72 C 0.5361(8) 0.7319(7) 0.1067(2) 0.060(2) Uani 1 1 d . . . H72 H 0.4786 0.6905 0.1236 0.074 Uiso 1 1 calc R . . C73 C 0.6258(9) 0.4247(9) 0.1021(3) 0.089(3) Uani 1 1 d . . . H73A H 0.6689 0.3550 0.0889 0.089 Uiso 1 1 calc R . . H73B H 0.6117 0.4033 0.1274 0.089 Uiso 1 1 calc R . . H73C H 0.6854 0.4907 0.0988 0.089 Uiso 1 1 calc R . . C81 C 0.5226(7) 0.7066(6) 0.53587(18) 0.0423(16) Uani 1 1 d . . . C82 C 0.6592(8) 0.6538(6) 0.5375(2) 0.0546(19) Uani 1 1 d . . . H82 H 0.7241 0.6564 0.5173 0.069 Uiso 1 1 calc R . . C83 C 0.6975(10) 0.5977(8) 0.5694(3) 0.075(3) Uani 1 1 d . . . H83 H 0.7886 0.5630 0.5700 0.090 Uiso 1 1 calc R . . C84 C 0.6069(13) 0.5915(8) 0.5996(3) 0.079(3) Uani 1 1 d . . . H84 H 0.6349 0.5529 0.6206 0.096 Uiso 1 1 calc R . . C85 C 0.4723(11) 0.6439(8) 0.5984(2) 0.073(3) Uani 1 1 d . . . H85 H 0.4084 0.6393 0.6188 0.089 Uiso 1 1 calc R . . C86 C 0.4304(9) 0.7042(7) 0.5668(2) 0.0563(19) Uani 1 1 d . . . H86 H 0.3406 0.7423 0.5667 0.069 Uiso 1 1 calc R . . C87 C 0.3190(7) 0.7429(6) 0.4813(2) 0.0461(17) Uani 1 1 d . . . C88 C 0.2994(9) 0.7522(7) 0.4447(2) 0.065(2) Uani 1 1 d . . . H88 H 0.3698 0.7799 0.4283 0.080 Uiso 1 1 calc R . . C89 C 0.1767(13) 0.7209(9) 0.4320(3) 0.090(3) Uani 1 1 d . . . H89 H 0.1659 0.7272 0.4074 0.108 Uiso 1 1 calc R . . C90 C 0.0715(11) 0.6807(10) 0.4560(4) 0.098(4) Uani 1 1 d . . . H90 H -0.0117 0.6617 0.4477 0.120 Uiso 1 1 calc R . . C91 C 0.0897(9) 0.6687(9) 0.4922(3) 0.091(3) Uani 1 1 d . . . H91 H 0.0192 0.6402 0.5084 0.110 Uiso 1 1 calc R . . C92 C 0.2127(7) 0.6987(8) 0.5046(2) 0.066(2) Uani 1 1 d . . . H92 H 0.2242 0.6890 0.5292 0.083 Uiso 1 1 calc R . . C93 C 0.6074(9) 0.6091(6) 0.4545(2) 0.067(2) Uani 1 1 d . . . H93A H 0.5466 0.5990 0.4361 0.067 Uiso 1 1 calc R . . H93B H 0.5795 0.5608 0.4756 0.067 Uiso 1 1 calc R . . H93C H 0.7018 0.5829 0.4456 0.067 Uiso 1 1 calc R . . C99 C 0.3367(17) 0.0704(18) 0.0571(5) 0.199(9) Uani 1 1 d . . . H99A H 0.3559 0.0211 0.0781 0.199 Uiso 1 1 calc R . . H99B H 0.3436 0.1550 0.0620 0.199 Uiso 1 1 calc R . . H99C H 0.4033 0.0460 0.0371 0.199 Uiso 1 1 calc R . . B1 B -0.0607(14) 0.1435(15) 0.1299(4) 0.096(5) Uani 1 1 d . . . B2 B 0.9562(11) 0.4351(14) 0.3843(3) 0.084(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 Co1 0.0315(4) 0.0387(5) 0.0381(5) 0.0021(4) 0.0007(4) -0.0005(4) Co51 0.0278(6) 0.0342(7) 0.0444(8) 0.0023(5) -0.0020(5) -0.0050(5) Co52 0.0356(6) 0.0278(6) 0.0384(7) -0.0035(5) 0.0019(5) -0.0023(5) S1 0.0321(8) 0.0502(11) 0.0511(11) -0.0007(8) 0.0025(8) 0.0010(7) S2 0.0366(9) 0.0451(10) 0.0407(10) 0.0016(7) -0.0004(7) -0.0007(7) S3 0.0340(8) 0.0488(10) 0.0409(10) -0.0009(7) 0.0008(7) -0.0009(7) S4 0.0398(9) 0.0656(13) 0.0395(10) 0.0011(8) 0.0041(8) 0.0027(8) S51 0.0301(8) 0.0381(10) 0.0583(11) 0.0026(7) -0.0034(7) -0.0062(7) S52 0.0376(9) 0.0391(10) 0.0588(12) 0.0060(8) -0.0068(8) -0.0092(7) S53 0.0421(9) 0.0374(9) 0.0417(10) -0.0034(7) 0.0024(7) -0.0027(7) S54 0.0380(9) 0.0399(10) 0.0503(11) -0.0040(7) 0.0021(8) -0.0022(7) P1 0.0343(9) 0.0383(10) 0.0415(10) 0.0045(7) 0.0024(7) -0.0009(7) P2 0.0395(9) 0.0379(10) 0.0475(11) -0.0015(7) -0.0006(8) -0.0010(7) P51 0.0371(9) 0.0414(10) 0.0430(10) 0.0036(7) -0.0014(8) -0.0067(7) P52 0.0387(9) 0.0283(9) 0.0426(10) -0.0024(7) -0.0016(7) -0.0021(7) F1 0.193(8) 0.106(6) 0.179(8) -0.056(5) -0.047(6) 0.055(5) F2 0.265(15) 0.261(15) 0.36(2) -0.025(13) -0.080(13) -0.136(13) F3 0.281(13) 0.270(13) 0.120(8) 0.036(8) 0.014(8) 0.149(11) F4 0.202(9) 0.252(11) 0.202(9) -0.072(8) -0.106(8) 0.150(9) F5 0.146(7) 0.306(13) 0.115(7) -0.046(7) 0.008(5) -0.028(7) F6 0.102(5) 0.276(12) 0.210(9) 0.061(8) -0.086(6) -0.014(6) F7 0.187(10) 0.300(15) 0.167(9) -0.085(9) -0.057(8) 0.119(10) F8A 0.184(11) 0.154(10) 0.130(9) 0.044(8) -0.077(8) -0.098(9) F8B 0.22(3) 0.092(16) 0.15(2) -0.021(14) 0.012(19) -0.064(17) O1 0.046(3) 0.054(3) 0.055(3) 0.021(2) -0.001(2) 0.001(2) O4 0.049(3) 0.042(3) 0.060(3) -0.009(2) 0.008(2) 0.007(2) O51 0.073(4) 0.057(3) 0.062(4) 0.021(3) -0.019(3) -0.005(3) O54 0.053(3) 0.032(3) 0.051(3) -0.012(2) 0.011(2) -0.003(2) O98 0.166(11) 0.239(14) 0.172(11) -0.035(9) -0.020(9) 0.051(10) N1 0.045(3) 0.059(4) 0.054(4) 0.001(3) -0.005(3) 0.001(3) N2 0.044(3) 0.082(5) 0.042(4) 0.000(3) -0.002(3) 0.004(3) N51 0.041(3) 0.045(4) 0.064(4) 0.005(3) -0.011(3) -0.001(3) N52 0.049(4) 0.051(4) 0.056(4) 0.001(3) -0.010(3) 0.001(3) C1 0.039(4) 0.035(4) 0.053(4) 0.004(3) -0.007(3) -0.001(3) C2 0.042(5) 0.115(8) 0.092(7) -0.005(6) -0.014(5) 0.009(5) C3 0.057(5) 0.105(8) 0.063(6) 0.004(5) -0.015(4) 0.014(5) C4 0.040(4) 0.047(4) 0.043(4) 0.004(3) -0.004(3) 0.004(3) C5 0.042(4) 0.111(8) 0.066(6) -0.002(5) -0.012(4) 0.006(4) C6 0.072(6) 0.134(9) 0.036(5) 0.000(5) -0.009(4) 0.013(6) C11 0.037(4) 0.037(4) 0.054(5) 0.000(3) -0.001(3) 0.000(3) C12 0.050(4) 0.053(5) 0.066(5) 0.000(4) -0.001(4) -0.004(4) C13 0.064(6) 0.073(6) 0.080(6) 0.001(5) -0.020(5) -0.016(5) C14 0.048(5) 0.077(6) 0.099(8) 0.013(5) -0.011(5) -0.020(4) C15 0.042(4) 0.058(5) 0.096(7) 0.017(5) 0.008(4) -0.008(4) C16 0.044(4) 0.047(4) 0.063(5) 0.007(3) 0.004(4) -0.003(3) C17 0.039(4) 0.037(4) 0.044(4) -0.001(3) -0.001(3) 0.003(3) C18 0.037(4) 0.041(4) 0.043(4) 0.000(3) -0.004(3) 0.002(3) C19 0.043(4) 0.060(5) 0.042(4) -0.002(3) 0.002(3) -0.001(3) C20 0.060(5) 0.058(5) 0.044(5) -0.013(3) 0.002(4) -0.001(4) C21 0.082(6) 0.039(5) 0.065(6) -0.011(4) 0.000(5) 0.014(4) C22 0.056(4) 0.041(4) 0.060(5) 0.001(3) 0.005(4) -0.003(3) C23 0.058(5) 0.057(5) 0.071(6) 0.026(4) -0.008(4) 0.002(4) C31 0.057(5) 0.033(4) 0.064(5) -0.003(3) -0.015(4) -0.003(3) C32 0.061(5) 0.063(6) 0.088(7) -0.018(5) -0.017(5) -0.004(4) C33 0.091(8) 0.077(7) 0.105(8) -0.031(6) -0.037(7) 0.001(6) C34 0.076(7) 0.077(8) 0.157(12) -0.024(8) -0.043(8) 0.000(6) C35 0.053(6) 0.084(8) 0.153(12) 0.007(7) -0.014(6) -0.022(5) C36 0.064(6) 0.059(6) 0.096(7) 0.005(5) -0.016(5) -0.012(4) C37 0.072(5) 0.029(4) 0.058(5) 0.007(3) -0.011(4) -0.011(3) C38 0.106(7) 0.063(6) 0.055(6) -0.001(4) -0.002(5) -0.031(5) C39 0.188(14) 0.081(8) 0.053(6) 0.014(5) -0.023(8) -0.068(9) C40 0.25(2) 0.075(8) 0.086(10) 0.029(7) -0.086(12) -0.041(10) C41 0.154(12) 0.076(8) 0.108(10) 0.006(7) -0.072(9) 0.019(7) C42 0.086(6) 0.058(6) 0.079(7) 0.007(4) -0.034(5) 0.012(5) C43 0.070(5) 0.054(5) 0.088(7) -0.016(4) -0.003(5) 0.009(4) C51 0.034(3) 0.040(4) 0.049(4) -0.001(3) -0.006(3) -0.003(3) C52 0.034(4) 0.064(6) 0.111(7) -0.004(5) -0.017(4) -0.001(4) C53 0.065(5) 0.046(5) 0.091(7) 0.002(4) -0.020(5) 0.007(4) C54 0.043(4) 0.029(4) 0.050(4) 0.003(3) -0.005(3) 0.000(3) C55 0.075(6) 0.102(8) 0.061(6) 0.007(5) -0.019(5) 0.007(5) C56 0.047(5) 0.109(8) 0.088(7) -0.008(6) -0.012(5) 0.008(5) C61 0.042(4) 0.055(5) 0.040(4) -0.002(3) 0.001(3) -0.012(3) C62 0.050(4) 0.062(5) 0.057(5) -0.002(4) -0.003(4) 0.000(4) C63 0.056(5) 0.080(7) 0.073(6) -0.009(5) -0.006(4) 0.012(5) C64 0.049(5) 0.122(9) 0.070(7) -0.004(6) 0.007(4) 0.003(6) C65 0.049(5) 0.125(9) 0.062(6) 0.005(5) 0.019(4) -0.023(5) C66 0.064(5) 0.064(5) 0.058(5) 0.003(4) 0.009(4) -0.015(4) C67 0.034(3) 0.042(4) 0.047(4) -0.005(3) -0.002(3) -0.008(3) C68 0.044(4) 0.042(4) 0.056(5) -0.006(3) -0.005(3) -0.008(3) C69 0.053(4) 0.049(5) 0.066(5) -0.007(4) 0.001(4) -0.015(4) C70 0.069(6) 0.056(6) 0.087(7) -0.025(5) -0.007(5) -0.019(4) C71 0.083(6) 0.092(7) 0.057(6) -0.031(5) -0.002(5) -0.020(5) C72 0.058(5) 0.071(6) 0.053(5) -0.006(4) 0.000(4) -0.016(4) C73 0.074(6) 0.097(8) 0.098(8) 0.035(6) -0.030(6) 0.000(5) C81 0.050(4) 0.027(4) 0.051(4) -0.007(3) -0.006(3) -0.008(3) C82 0.055(5) 0.044(4) 0.065(5) 0.003(4) -0.014(4) 0.002(3) C83 0.085(7) 0.054(6) 0.090(8) 0.003(5) -0.042(6) 0.004(5) C84 0.130(9) 0.046(5) 0.067(7) 0.005(4) -0.043(7) 0.002(5) C85 0.120(8) 0.052(5) 0.048(5) 0.010(4) -0.014(5) -0.017(5) C86 0.070(5) 0.053(5) 0.045(5) 0.003(3) 0.004(4) -0.008(4) C87 0.047(4) 0.029(4) 0.063(5) -0.005(3) -0.011(4) 0.001(3) C88 0.086(6) 0.050(5) 0.065(6) 0.005(4) -0.028(5) -0.014(4) C89 0.112(9) 0.071(7) 0.098(8) -0.002(6) -0.060(7) -0.010(6) C90 0.075(7) 0.070(7) 0.158(12) -0.035(7) -0.054(8) 0.004(5) C91 0.051(5) 0.096(8) 0.128(10) -0.035(7) 0.001(6) -0.023(5) C92 0.036(4) 0.084(6) 0.079(6) -0.020(5) -0.001(4) -0.010(4) C93 0.077(6) 0.039(5) 0.082(6) -0.020(4) 0.016(5) -0.006(4) C99 0.140(14) 0.27(2) 0.206(18) 0.056(16) -0.036(13) -0.135(15) B1 0.075(8) 0.115(11) 0.098(11) -0.048(9) -0.032(7) 0.037(7) B2 0.055(6) 0.133(12) 0.066(8) -0.030(7) -0.022(6) 0.003(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 P1 2.2686(19) . ? Co1 S4 2.275(2) . ? Co1 S1 2.2788(18) . ? Co1 S2 2.2801(19) . ? Co1 S3 2.2805(18) . ? Co1 P2 2.3090(19) . ? Co51 S52 2.2797(17) 2_665 ? Co51 S52 2.2798(17) . ? Co51 S51 2.2848(15) 2_665 ? Co51 S51 2.2848(15) . ? Co51 P51 2.2848(18) . ? Co51 P51 2.2850(18) 2_665 ? Co52 S53 2.2700(17) . ? Co52 S53 2.2701(17) 2_676 ? Co52 S54 2.2710(16) . ? Co52 S54 2.2710(16) 2_676 ? Co52 P52 2.3007(16) . ? Co52 P52 2.3007(16) 2_676 ? S1 C1 1.716(7) . ? S2 C1 1.717(7) . ? S3 C4 1.720(7) . ? S4 C4 1.729(7) . ? S51 C51 1.712(7) . ? S52 C51 1.714(6) . ? S53 C54 1.718(7) . ? S54 C54 1.718(7) . ? P1 O1 1.611(5) . ? P1 C11 1.822(7) . ? P1 C17 1.826(6) . ? P2 O4 1.611(5) . ? P2 C31 1.829(7) . ? P2 C37 1.831(8) . ? P51 O51 1.613(5) . ? P51 C61 1.822(7) . ? P51 C67 1.833(6) . ? P52 O54 1.619(4) . ? P52 C81 1.818(7) . ? P52 C87 1.843(7) . ? F1 B1 1.314(12) . ? F2 B1 1.314(18) . ? F3 B1 1.289(16) . ? F4 B1 1.279(13) . ? F5 B2 1.287(13) . ? F5 F8B 1.70(2) . ? F6 B2 1.285(12) . ? F7 B2 1.306(13) . ? F7 F8B 1.71(3) . ? F8A B2 1.395(16) . ? F8B B2 1.45(2) . ? O1 C23 1.431(8) . ? O4 C43 1.469(8) . ? O51 C73 1.386(9) . ? O54 C93 1.465(8) . ? O98 C99 1.368(15) . ? O98 H98 0.8200 . ? N1 C1 1.314(8) . ? N1 C3 1.468(10) . ? N1 C2 1.481(9) . ? N2 C4 1.308(8) . ? N2 C6 1.463(9) . ? N2 C5 1.466(9) . ? N51 C51 1.322(8) . ? N51 C52 1.456(9) . ? N51 C53 1.463(9) . ? N52 C54 1.320(8) . ? N52 C55 1.463(10) . ? N52 C56 1.466(9) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C11 C12 1.384(10) . ? C11 C16 1.405(9) . ? C12 C13 1.399(10) . ? C12 H12 0.9300 . ? C13 C14 1.382(12) . ? C13 H13 0.9300 . ? C14 C15 1.378(12) . ? C14 H14 0.9300 . ? C15 C16 1.389(10) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.394(9) . ? C17 C22 1.395(9) . ? C18 C19 1.394(9) . ? C18 H18 0.9300 . ? C19 C20 1.377(10) . ? C19 H19 0.9300 . ? C20 C21 1.377(11) . ? C20 H20 0.9300 . ? C21 C22 1.412(10) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C31 C32 1.385(11) . ? C31 C36 1.391(11) . ? C32 C33 1.407(12) . ? C32 H32 0.9300 . ? C33 C34 1.363(15) . ? C33 H33 0.9300 . ? C34 C35 1.362(15) . ? C34 H34 0.9300 . ? C35 C36 1.411(12) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C42 1.389(11) . ? C37 C38 1.389(11) . ? C38 C39 1.398(13) . ? C38 H38 0.9300 . ? C39 C40 1.388(18) . ? C39 H39 0.9300 . ? C40 C41 1.358(18) . ? C40 H40 0.9300 . ? C41 C42 1.377(14) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C61 C62 1.394(10) . ? C61 C66 1.396(10) . ? C62 C63 1.395(10) . ? C62 H62 0.9300 . ? C63 C64 1.383(13) . ? C63 H63 0.9300 . ? C64 C65 1.359(13) . ? C64 H64 0.9300 . ? C65 C66 1.405(11) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 C68 1.380(9) . ? C67 C72 1.401(10) . ? C68 C69 1.384(9) . ? C68 H68 0.9300 . ? C69 C70 1.376(11) . ? C69 H69 0.9300 . ? C70 C71 1.370(12) . ? C70 H70 0.9300 . ? C71 C72 1.382(11) . ? C71 H71 0.9300 . ? C72 H72 0.9300 . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? C81 C86 1.380(10) . ? C81 C82 1.400(9) . ? C82 C83 1.385(11) . ? C82 H82 0.9300 . ? C83 C84 1.354(13) . ? C83 H83 0.9300 . ? C84 C85 1.379(13) . ? C84 H84 0.9300 . ? C85 C86 1.407(11) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? C87 C92 1.386(10) . ? C87 C88 1.389(10) . ? C88 C89 1.389(12) . ? C88 H88 0.9300 . ? C89 C90 1.374(15) . ? C89 H89 0.9300 . ? C90 C91 1.372(15) . ? C90 H90 0.9300 . ? C91 C92 1.385(11) . ? C91 H91 0.9300 . ? C92 H92 0.9300 . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? C99 H99A 0.9600 . ? C99 H99B 0.9600 . ? C99 H99C 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 P1 Co1 S4 96.29(7) . . ? P1 Co1 S1 94.84(7) . . ? S4 Co1 S1 99.96(7) . . ? P1 Co1 S2 80.57(7) . . ? S4 Co1 S2 174.75(8) . . ? S1 Co1 S2 76.23(7) . . ? P1 Co1 S3 87.28(7) . . ? S4 Co1 S3 76.48(7) . . ? S1 Co1 S3 176.07(8) . . ? S2 Co1 S3 107.42(7) . . ? P1 Co1 P2 173.71(7) . . ? S4 Co1 P2 89.30(7) . . ? S1 Co1 P2 87.02(7) . . ? S2 Co1 P2 94.07(7) . . ? S3 Co1 P2 91.22(7) . . ? S52 Co51 S52 180.00(7) 2_665 . ? S52 Co51 S51 76.08(6) 2_665 2_665 ? S52 Co51 S51 103.92(6) . 2_665 ? S52 Co51 S51 103.92(6) 2_665 . ? S52 Co51 S51 76.08(6) . . ? S51 Co51 S51 180.0 2_665 . ? S52 Co51 P51 94.73(6) 2_665 . ? S52 Co51 P51 85.27(6) . . ? S51 Co51 P51 86.53(6) 2_665 . ? S51 Co51 P51 93.47(6) . . ? S52 Co51 P51 85.27(6) 2_665 2_665 ? S52 Co51 P51 94.73(6) . 2_665 ? S51 Co51 P51 93.47(6) 2_665 2_665 ? S51 Co51 P51 86.53(6) . 2_665 ? P51 Co51 P51 180.0 . 2_665 ? S53 Co52 S53 180.0 . 2_676 ? S53 Co52 S54 76.90(6) . . ? S53 Co52 S54 103.10(6) 2_676 . ? S53 Co52 S54 103.10(6) . 2_676 ? S53 Co52 S54 76.90(6) 2_676 2_676 ? S54 Co52 S54 180.0 . 2_676 ? S53 Co52 P52 94.15(6) . . ? S53 Co52 P52 85.85(6) 2_676 . ? S54 Co52 P52 87.26(6) . . ? S54 Co52 P52 92.74(6) 2_676 . ? S53 Co52 P52 85.85(6) . 2_676 ? S53 Co52 P52 94.15(6) 2_676 2_676 ? S54 Co52 P52 92.74(6) . 2_676 ? S54 Co52 P52 87.26(6) 2_676 2_676 ? P52 Co52 P52 179.997(1) . 2_676 ? C1 S1 Co1 86.9(2) . . ? C1 S2 Co1 86.8(2) . . ? C4 S3 Co1 86.9(2) . . ? C4 S4 Co1 86.9(2) . . ? C51 S51 Co51 86.7(2) . . ? C51 S52 Co51 86.8(2) . . ? C54 S53 Co52 86.3(2) . . ? C54 S54 Co52 86.3(2) . . ? O1 P1 C11 97.1(3) . . ? O1 P1 C17 103.1(3) . . ? C11 P1 C17 104.2(3) . . ? O1 P1 Co1 117.7(2) . . ? C11 P1 Co1 115.7(2) . . ? C17 P1 Co1 116.3(2) . . ? O4 P2 C31 102.9(3) . . ? O4 P2 C37 104.6(3) . . ? C31 P2 C37 108.8(4) . . ? O4 P2 Co1 111.55(19) . . ? C31 P2 Co1 116.4(2) . . ? C37 P2 Co1 111.6(2) . . ? O51 P51 C61 97.7(3) . . ? O51 P51 C67 104.2(3) . . ? C61 P51 C67 104.1(3) . . ? O51 P51 Co51 116.3(2) . . ? C61 P51 Co51 113.9(2) . . ? C67 P51 Co51 118.0(2) . . ? O54 P52 C81 104.0(3) . . ? O54 P52 C87 102.8(3) . . ? C81 P52 C87 107.8(3) . . ? O54 P52 Co52 109.76(17) . . ? C81 P52 Co52 112.9(2) . . ? C87 P52 Co52 118.2(2) . . ? B2 F5 F8B 56.2(11) . . ? B2 F7 F8B 55.7(11) . . ? B2 F8B F5 47.4(8) . . ? B2 F8B F7 47.9(9) . . ? F5 F8B F7 81.4(11) . . ? C23 O1 P1 125.1(4) . . ? C43 O4 P2 121.4(5) . . ? C73 O51 P51 128.1(6) . . ? C93 O54 P52 121.1(4) . . ? C99 O98 H98 109.5 . . ? C1 N1 C3 121.7(6) . . ? C1 N1 C2 120.8(6) . . ? C3 N1 C2 117.4(6) . . ? C4 N2 C6 122.2(6) . . ? C4 N2 C5 121.1(6) . . ? C6 N2 C5 116.7(6) . . ? C51 N51 C52 121.7(6) . . ? C51 N51 C53 120.3(6) . . ? C52 N51 C53 117.9(6) . . ? C54 N52 C55 122.1(6) . . ? C54 N52 C56 121.7(7) . . ? C55 N52 C56 116.2(6) . . ? N1 C1 S1 126.2(5) . . ? N1 C1 S2 123.7(5) . . ? S1 C1 S2 110.1(4) . . ? 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 C4 S3 124.6(5) . . ? N2 C4 S4 125.7(5) . . ? S3 C4 S4 109.7(4) . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C11 C16 118.5(6) . . ? C12 C11 P1 122.7(5) . . ? C16 C11 P1 118.7(5) . . ? C11 C12 C13 120.8(7) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C14 C13 C12 119.6(8) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 120.5(8) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.9(8) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C11 120.6(8) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? C18 C17 C22 117.5(6) . . ? C18 C17 P1 124.1(5) . . ? C22 C17 P1 118.4(5) . . ? C17 C18 C19 121.4(6) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C20 C19 C18 120.3(7) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 120.0(7) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C22 119.7(7) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C17 C22 C21 121.1(7) . . ? C17 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? O1 C23 H23A 109.5 . . ? O1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C32 C31 C36 118.5(7) . . ? C32 C31 P2 117.3(6) . . ? C36 C31 P2 124.1(6) . . ? C31 C32 C33 120.8(9) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 C32 119.3(10) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C35 C34 C33 121.6(10) . . ? C35 C34 H34 119.2 . . ? C33 C34 H34 119.2 . . ? C34 C35 C36 119.5(11) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C31 C36 C35 120.4(10) . . ? C31 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C42 C37 C38 118.8(8) . . ? C42 C37 P2 118.0(6) . . ? C38 C37 P2 122.6(7) . . ? C37 C38 C39 120.2(10) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C40 C39 C38 120.0(12) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C41 C40 C39 119.0(12) . . ? C41 C40 H40 120.5 . . ? C39 C40 H40 120.5 . . ? C40 C41 C42 122.2(13) . . ? C40 C41 H41 118.9 . . ? C42 C41 H41 118.9 . . ? C41 C42 C37 119.8(10) . . ? C41 C42 H42 120.1 . . ? C37 C42 H42 120.1 . . ? O4 C43 H43A 109.5 . . ? O4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N51 C51 S51 124.4(5) . . ? N51 C51 S52 125.2(5) . . ? S51 C51 S52 110.4(3) . . ? N51 C52 H52A 109.5 . . ? N51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N51 C53 H53A 109.5 . . ? N51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N52 C54 S54 125.2(5) . . ? N52 C54 S53 124.3(5) . . ? S54 C54 S53 110.5(4) . . ? N52 C55 H55A 109.5 . . ? N52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N52 C56 H56A 109.5 . . ? N52 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N52 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C62 C61 C66 118.5(7) . . ? C62 C61 P51 122.2(5) . . ? C66 C61 P51 119.0(6) . . ? C61 C62 C63 120.8(8) . . ? C61 C62 H62 119.6 . . ? C63 C62 H62 119.6 . . ? C64 C63 C62 119.4(9) . . ? C64 C63 H63 120.3 . . ? C62 C63 H63 120.3 . . ? C65 C64 C63 120.8(8) . . ? C65 C64 H64 119.6 . . ? C63 C64 H64 119.6 . . ? C64 C65 C66 120.3(9) . . ? C64 C65 H65 119.9 . . ? C66 C65 H65 119.9 . . ? C61 C66 C65 120.1(8) . . ? C61 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C68 C67 C72 117.3(6) . . ? C68 C67 P51 124.2(5) . . ? C72 C67 P51 118.4(5) . . ? C67 C68 C69 121.7(7) . . ? C67 C68 H68 119.2 . . ? C69 C68 H68 119.2 . . ? C70 C69 C68 120.1(8) . . ? C70 C69 H69 120.0 . . ? C68 C69 H69 120.0 . . ? C71 C70 C69 119.5(7) . . ? C71 C70 H70 120.2 . . ? C69 C70 H70 120.2 . . ? C70 C71 C72 120.5(8) . . ? C70 C71 H71 119.8 . . ? C72 C71 H71 119.8 . . ? C71 C72 C67 120.9(8) . . ? C71 C72 H72 119.5 . . ? C67 C72 H72 119.5 . . ? O51 C73 H73A 109.5 . . ? O51 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? O51 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C86 C81 C82 118.4(7) . . ? C86 C81 P52 122.9(6) . . ? C82 C81 P52 118.2(5) . . ? C83 C82 C81 119.9(8) . . ? C83 C82 H82 120.1 . . ? C81 C82 H82 120.1 . . ? C84 C83 C82 122.3(9) . . ? C84 C83 H83 118.8 . . ? C82 C83 H83 118.8 . . ? C83 C84 C85 118.4(9) . . ? C83 C84 H84 120.8 . . ? C85 C84 H84 120.8 . . ? C84 C85 C86 120.9(9) . . ? C84 C85 H85 119.5 . . ? C86 C85 H85 119.5 . . ? C81 C86 C85 120.0(8) . . ? C81 C86 H86 120.0 . . ? C85 C86 H86 120.0 . . ? C92 C87 C88 117.5(7) . . ? C92 C87 P52 125.0(6) . . ? C88 C87 P52 117.6(6) . . ? C87 C88 C89 121.4(9) . . ? C87 C88 H88 119.3 . . ? C89 C88 H88 119.3 . . ? C90 C89 C88 119.9(10) . . ? C90 C89 H89 120.1 . . ? C88 C89 H89 120.1 . . ? C91 C90 C89 119.7(9) . . ? C91 C90 H90 120.1 . . ? C89 C90 H90 120.1 . . ? C90 C91 C92 120.3(10) . . ? C90 C91 H91 119.9 . . ? C92 C91 H91 119.9 . . ? C91 C92 C87 121.3(9) . . ? C91 C92 H92 119.4 . . ? C87 C92 H92 119.4 . . ? O54 C93 H93A 109.5 . . ? O54 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? O54 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? O98 C99 H99A 109.5 . . ? O98 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? O98 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? F4 B1 F3 114.8(12) . . ? F4 B1 F2 104.0(16) . . ? F3 B1 F2 100.7(12) . . ? F4 B1 F1 113.5(11) . . ? F3 B1 F1 116.7(15) . . ? F2 B1 F1 104.8(14) . . ? F6 B2 F5 124.1(11) . . ? F6 B2 F7 112.6(11) . . ? F5 B2 F7 118.0(12) . . ? F6 B2 F8A 105.8(13) . . ? F5 B2 F8A 98.6(10) . . ? F7 B2 F8A 87.8(12) . . ? F6 B2 F8B 94.3(14) . . ? F5 B2 F8B 76.4(13) . . ? F7 B2 F8B 76.4(14) . . ? F8A B2 F8B 158.2(16) . . ? 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 P1 Co1 S1 C1 -79.5(2) . . . . ? S4 Co1 S1 C1 -176.8(2) . . . . ? S2 Co1 S1 C1 -0.5(2) . . . . ? S3 Co1 S1 C1 158.0(11) . . . . ? P2 Co1 S1 C1 94.5(2) . . . . ? P1 Co1 S2 C1 97.9(2) . . . . ? S4 Co1 S2 C1 44.4(9) . . . . ? S1 Co1 S2 C1 0.5(2) . . . . ? S3 Co1 S2 C1 -178.0(2) . . . . ? P2 Co1 S2 C1 -85.5(2) . . . . ? P1 Co1 S3 C4 -98.9(2) . . . . ? S4 Co1 S3 C4 -1.8(2) . . . . ? S1 Co1 S3 C4 23.7(12) . . . . ? S2 Co1 S3 C4 -178.1(2) . . . . ? P2 Co1 S3 C4 87.2(2) . . . . ? P1 Co1 S4 C4 87.4(2) . . . . ? S1 Co1 S4 C4 -176.5(2) . . . . ? S2 Co1 S4 C4 140.4(8) . . . . ? S3 Co1 S4 C4 1.8(2) . . . . ? P2 Co1 S4 C4 -89.7(2) . . . . ? S52 Co51 S51 C51 178.0(2) 2_665 . . . ? S52 Co51 S51 C51 -2.0(2) . . . . ? S51 Co51 S51 C51 -104(3) 2_665 . . . ? P51 Co51 S51 C51 82.3(2) . . . . ? P51 Co51 S51 C51 -97.7(2) 2_665 . . . ? S52 Co51 S52 C51 84(6) 2_665 . . . ? S51 Co51 S52 C51 -178.0(2) 2_665 . . . ? S51 Co51 S52 C51 2.0(2) . . . . ? P51 Co51 S52 C51 -92.8(2) . . . . ? P51 Co51 S52 C51 87.2(2) 2_665 . . . ? S53 Co52 S53 C54 -45(33) 2_676 . . . ? S54 Co52 S53 C54 0.2(2) . . . . ? S54 Co52 S53 C54 -179.8(2) 2_676 . . . ? P52 Co52 S53 C54 86.4(2) . . . . ? P52 Co52 S53 C54 -93.6(2) 2_676 . . . ? S53 Co52 S54 C54 -0.2(2) . . . . ? S53 Co52 S54 C54 179.8(2) 2_676 . . . ? S54 Co52 S54 C54 161(13) 2_676 . . . ? P52 Co52 S54 C54 -95.1(2) . . . . ? P52 Co52 S54 C54 84.9(2) 2_676 . . . ? S4 Co1 P1 O1 -4.8(2) . . . . ? S1 Co1 P1 O1 -105.4(2) . . . . ? S2 Co1 P1 O1 179.4(2) . . . . ? S3 Co1 P1 O1 71.3(2) . . . . ? P2 Co1 P1 O1 147.6(6) . . . . ? S4 Co1 P1 C11 109.3(3) . . . . ? S1 Co1 P1 C11 8.7(3) . . . . ? S2 Co1 P1 C11 -66.5(3) . . . . ? S3 Co1 P1 C11 -174.7(3) . . . . ? P2 Co1 P1 C11 -98.3(7) . . . . ? S4 Co1 P1 C17 -127.9(2) . . . . ? S1 Co1 P1 C17 131.4(2) . . . . ? S2 Co1 P1 C17 56.3(2) . . . . ? S3 Co1 P1 C17 -51.9(2) . . . . ? P2 Co1 P1 C17 24.5(8) . . . . ? P1 Co1 P2 O4 152.0(6) . . . . ? S4 Co1 P2 O4 -55.4(2) . . . . ? S1 Co1 P2 O4 44.6(2) . . . . ? S2 Co1 P2 O4 120.6(2) . . . . ? S3 Co1 P2 O4 -131.9(2) . . . . ? P1 Co1 P2 C31 -90.4(7) . . . . ? S4 Co1 P2 C31 62.2(3) . . . . ? S1 Co1 P2 C31 162.2(3) . . . . ? S2 Co1 P2 C31 -121.8(3) . . . . ? S3 Co1 P2 C31 -14.3(3) . . . . ? P1 Co1 P2 C37 35.4(8) . . . . ? S4 Co1 P2 C37 -172.0(3) . . . . ? S1 Co1 P2 C37 -72.0(3) . . . . ? S2 Co1 P2 C37 3.9(3) . . . . ? S3 Co1 P2 C37 111.5(3) . . . . ? S52 Co51 P51 O51 1.5(2) 2_665 . . . ? S52 Co51 P51 O51 -178.5(2) . . . . ? S51 Co51 P51 O51 -74.3(2) 2_665 . . . ? S51 Co51 P51 O51 105.7(2) . . . . ? P51 Co51 P51 O51 -177(21) 2_665 . . . ? S52 Co51 P51 C61 -111.0(3) 2_665 . . . ? S52 Co51 P51 C61 69.0(3) . . . . ? S51 Co51 P51 C61 173.2(3) 2_665 . . . ? S51 Co51 P51 C61 -6.8(3) . . . . ? P51 Co51 P51 C61 71(21) 2_665 . . . ? S52 Co51 P51 C67 126.4(2) 2_665 . . . ? S52 Co51 P51 C67 -53.6(2) . . . . ? S51 Co51 P51 C67 50.7(2) 2_665 . . . ? S51 Co51 P51 C67 -129.3(2) . . . . ? P51 Co51 P51 C67 -52(21) 2_665 . . . ? S53 Co52 P52 O54 -123.6(2) . . . . ? S53 Co52 P52 O54 56.4(2) 2_676 . . . ? S54 Co52 P52 O54 -47.0(2) . . . . ? S54 Co52 P52 O54 133.0(2) 2_676 . . . ? P52 Co52 P52 O54 47(10) 2_676 . . . ? S53 Co52 P52 C81 -8.1(2) . . . . ? S53 Co52 P52 C81 171.9(3) 2_676 . . . ? S54 Co52 P52 C81 68.6(2) . . . . ? S54 Co52 P52 C81 -111.4(2) 2_676 . . . ? P52 Co52 P52 C81 162(10) 2_676 . . . ? S53 Co52 P52 C87 119.0(3) . . . . ? S53 Co52 P52 C87 -61.0(3) 2_676 . . . ? S54 Co52 P52 C87 -164.4(3) . . . . ? S54 Co52 P52 C87 15.6(3) 2_676 . . . ? P52 Co52 P52 C87 -71(10) 2_676 . . . ? B2 F5 F8B F7 38.6(8) . . . . ? B2 F7 F8B F5 -38.3(8) . . . . ? C11 P1 O1 C23 157.3(6) . . . . ? C17 P1 O1 C23 50.8(6) . . . . ? Co1 P1 O1 C23 -78.7(6) . . . . ? C31 P2 O4 C43 52.8(6) . . . . ? C37 P2 O4 C43 -60.9(6) . . . . ? Co1 P2 O4 C43 178.3(5) . . . . ? C61 P51 O51 C73 -153.9(8) . . . . ? C67 P51 O51 C73 -47.2(8) . . . . ? Co51 P51 O51 C73 84.5(8) . . . . ? C81 P52 O54 C93 61.2(6) . . . . ? C87 P52 O54 C93 -51.1(6) . . . . ? Co52 P52 O54 C93 -177.8(5) . . . . ? C3 N1 C1 S1 -179.8(6) . . . . ? C2 N1 C1 S1 -3.4(10) . . . . ? C3 N1 C1 S2 -1.9(10) . . . . ? C2 N1 C1 S2 174.5(6) . . . . ? Co1 S1 C1 N1 178.8(6) . . . . ? Co1 S1 C1 S2 0.6(3) . . . . ? Co1 S2 C1 N1 -178.8(6) . . . . ? Co1 S2 C1 S1 -0.6(3) . . . . ? C6 N2 C4 S3 179.8(6) . . . . ? C5 N2 C4 S3 1.4(11) . . . . ? C6 N2 C4 S4 -0.4(11) . . . . ? C5 N2 C4 S4 -178.8(6) . . . . ? Co1 S3 C4 N2 -177.8(6) . . . . ? Co1 S3 C4 S4 2.4(3) . . . . ? Co1 S4 C4 N2 177.8(7) . . . . ? Co1 S4 C4 S3 -2.4(3) . . . . ? O1 P1 C11 C12 -141.2(6) . . . . ? C17 P1 C11 C12 -35.7(6) . . . . ? Co1 P1 C11 C12 93.3(6) . . . . ? O1 P1 C11 C16 41.8(6) . . . . ? C17 P1 C11 C16 147.4(5) . . . . ? Co1 P1 C11 C16 -83.7(6) . . . . ? C16 C11 C12 C13 0.2(11) . . . . ? P1 C11 C12 C13 -176.8(6) . . . . ? C11 C12 C13 C14 0.2(12) . . . . ? C12 C13 C14 C15 -1.2(14) . . . . ? C13 C14 C15 C16 1.8(13) . . . . ? C14 C15 C16 C11 -1.5(12) . . . . ? C12 C11 C16 C15 0.4(10) . . . . ? P1 C11 C16 C15 177.6(6) . . . . ? O1 P1 C17 C18 -129.5(6) . . . . ? C11 P1 C17 C18 129.5(6) . . . . ? Co1 P1 C17 C18 0.9(7) . . . . ? O1 P1 C17 C22 46.5(6) . . . . ? C11 P1 C17 C22 -54.5(6) . . . . ? Co1 P1 C17 C22 176.9(5) . . . . ? C22 C17 C18 C19 0.0(10) . . . . ? P1 C17 C18 C19 176.1(5) . . . . ? C17 C18 C19 C20 -0.3(10) . . . . ? C18 C19 C20 C21 0.9(11) . . . . ? C19 C20 C21 C22 -1.1(12) . . . . ? C18 C17 C22 C21 -0.3(11) . . . . ? P1 C17 C22 C21 -176.6(6) . . . . ? C20 C21 C22 C17 0.8(12) . . . . ? O4 P2 C31 C32 38.6(6) . . . . ? C37 P2 C31 C32 149.2(6) . . . . ? Co1 P2 C31 C32 -83.7(6) . . . . ? O4 P2 C31 C36 -144.7(6) . . . . ? C37 P2 C31 C36 -34.1(8) . . . . ? Co1 P2 C31 C36 93.0(7) . . . . ? C36 C31 C32 C33 -0.1(12) . . . . ? P2 C31 C32 C33 176.8(7) . . . . ? C31 C32 C33 C34 0.7(14) . . . . ? C32 C33 C34 C35 -1.1(16) . . . . ? C33 C34 C35 C36 1.0(16) . . . . ? C32 C31 C36 C35 -0.1(12) . . . . ? P2 C31 C36 C35 -176.7(7) . . . . ? C34 C35 C36 C31 -0.4(15) . . . . ? O4 P2 C37 C42 -22.7(7) . . . . ? C31 P2 C37 C42 -132.1(6) . . . . ? Co1 P2 C37 C42 98.0(6) . . . . ? O4 P2 C37 C38 166.4(6) . . . . ? C31 P2 C37 C38 57.0(7) . . . . ? Co1 P2 C37 C38 -72.9(6) . . . . ? C42 C37 C38 C39 1.6(11) . . . . ? P2 C37 C38 C39 172.4(6) . . . . ? C37 C38 C39 C40 -1.7(14) . . . . ? C38 C39 C40 C41 0.3(17) . . . . ? C39 C40 C41 C42 1.1(18) . . . . ? C40 C41 C42 C37 -1.2(16) . . . . ? C38 C37 C42 C41 -0.2(12) . . . . ? P2 C37 C42 C41 -171.4(7) . . . . ? C52 N51 C51 S51 2.2(10) . . . . ? C53 N51 C51 S51 178.0(6) . . . . ? C52 N51 C51 S52 -178.2(6) . . . . ? C53 N51 C51 S52 -2.4(10) . . . . ? Co51 S51 C51 N51 -177.6(6) . . . . ? Co51 S51 C51 S52 2.7(3) . . . . ? Co51 S52 C51 N51 177.6(6) . . . . ? Co51 S52 C51 S51 -2.7(3) . . . . ? C55 N52 C54 S54 -177.9(6) . . . . ? C56 N52 C54 S54 2.6(10) . . . . ? C55 N52 C54 S53 2.9(10) . . . . ? C56 N52 C54 S53 -176.6(6) . . . . ? Co52 S54 C54 N52 -179.0(6) . . . . ? Co52 S54 C54 S53 0.3(3) . . . . ? Co52 S53 C54 N52 179.0(6) . . . . ? Co52 S53 C54 S54 -0.3(3) . . . . ? O51 P51 C61 C62 144.6(6) . . . . ? C67 P51 C61 C62 37.8(7) . . . . ? Co51 P51 C61 C62 -92.1(6) . . . . ? O51 P51 C61 C66 -41.5(6) . . . . ? C67 P51 C61 C66 -148.3(6) . . . . ? Co51 P51 C61 C66 81.8(6) . . . . ? C66 C61 C62 C63 0.0(11) . . . . ? P51 C61 C62 C63 173.9(6) . . . . ? C61 C62 C63 C64 -1.5(12) . . . . ? C62 C63 C64 C65 2.8(14) . . . . ? C63 C64 C65 C66 -2.6(14) . . . . ? C62 C61 C66 C65 0.3(11) . . . . ? P51 C61 C66 C65 -173.8(6) . . . . ? C64 C65 C66 C61 1.0(13) . . . . ? O51 P51 C67 C68 132.1(6) . . . . ? C61 P51 C67 C68 -126.0(6) . . . . ? Co51 P51 C67 C68 1.4(7) . . . . ? O51 P51 C67 C72 -47.4(6) . . . . ? C61 P51 C67 C72 54.5(6) . . . . ? Co51 P51 C67 C72 -178.1(5) . . . . ? C72 C67 C68 C69 0.6(10) . . . . ? P51 C67 C68 C69 -178.9(5) . . . . ? C67 C68 C69 C70 -0.3(11) . . . . ? C68 C69 C70 C71 0.3(13) . . . . ? C69 C70 C71 C72 -0.6(14) . . . . ? C70 C71 C72 C67 0.9(14) . . . . ? C68 C67 C72 C71 -0.9(11) . . . . ? P51 C67 C72 C71 178.6(7) . . . . ? O54 P52 C81 C86 -164.6(6) . . . . ? C87 P52 C81 C86 -55.9(6) . . . . ? Co52 P52 C81 C86 76.5(6) . . . . ? O54 P52 C81 C82 24.2(6) . . . . ? C87 P52 C81 C82 132.9(5) . . . . ? Co52 P52 C81 C82 -94.7(5) . . . . ? C86 C81 C82 C83 1.9(10) . . . . ? P52 C81 C82 C83 173.5(6) . . . . ? C81 C82 C83 C84 0.0(12) . . . . ? C82 C83 C84 C85 -0.4(13) . . . . ? C83 C84 C85 C86 -1.1(13) . . . . ? C82 C81 C86 C85 -3.3(10) . . . . ? P52 C81 C86 C85 -174.5(6) . . . . ? C84 C85 C86 C81 3.0(12) . . . . ? O54 P52 C87 C92 138.8(6) . . . . ? C81 P52 C87 C92 29.3(7) . . . . ? Co52 P52 C87 C92 -100.2(6) . . . . ? O54 P52 C87 C88 -42.6(6) . . . . ? C81 P52 C87 C88 -152.1(5) . . . . ? Co52 P52 C87 C88 78.5(6) . . . . ? C92 C87 C88 C89 1.4(11) . . . . ? P52 C87 C88 C89 -177.4(7) . . . . ? C87 C88 C89 C90 0.5(14) . . . . ? C88 C89 C90 C91 -1.7(16) . . . . ? C89 C90 C91 C92 1.0(15) . . . . ? C90 C91 C92 C87 0.9(14) . . . . ? C88 C87 C92 C91 -2.1(12) . . . . ? P52 C87 C92 C91 176.6(7) . . . . ? F8B F5 B2 F6 86.0(19) . . . . ? F8B F5 B2 F7 -66.2(18) . . . . ? F8B F5 B2 F8A -158.3(17) . . . . ? F8B F7 B2 F6 -89.0(16) . . . . ? F8B F7 B2 F5 66.2(17) . . . . ? F8B F7 B2 F8A 164.8(14) . . . . ? F5 F8B B2 F6 -124.0(11) . . . . ? F7 F8B B2 F6 112.3(11) . . . . ? F7 F8B B2 F5 -123.7(10) . . . . ? F5 F8B B2 F7 123.7(10) . . . . ? F5 F8B B2 F8A 79(4) . . . . ? F7 F8B B2 F8A -45(4) . . . . ? _diffrn_measured_fraction_theta_max 0.707 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.707 _refine_diff_density_max 0.536 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.073 #===END