Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Takayoshi Suzuki' _publ_contact_author_address ; Osaka University Graduate School of Science Toyonaka Osaka 560-0043 JAPAN ; _publ_contact_author_email SUZUKI@CHEM.SCI.OSAKA-U.AC.JP _publ_section_title ; Preparation and characterization of mixed-ligand cobalt(III) complexes containing (3-aminopropyl)dimethylphosphine (pdmp). Conformation of the six-membered pdmp chelate ring ; loop_ _publ_author_name 'Takayoshi Suzuki' 'Katsuhiro Fujiiwara' 'Kazuo Kashiwabara' H.D.Takagi # Attachment 'B612025C_CIF_rev1.cif' data_pdmpCl2C _database_code_depnum_ccdc_archive 'CCDC 618530' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans(Cl,Cl)cis(P,P)-dichlorobis((3-aminopropyl)dimethylphosphine)cobalt(III) hexafluorophosphate acetonitrile solvate ; _chemical_name_common ; trans(Cl,Cl)cis(P,P)-dichlorobis((3- aminopropyl)dimethylphosphine)cobalt(iii) hexafluorophosphate acetonitrile solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C10 H28 Cl2 Co N2 P2 1+, F6 P 1-, C2 H3 N' _chemical_formula_sum 'C12 H31 Cl2 Co F6 N3 P3' _chemical_formula_weight 554.14 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'C 1 2/m 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 16.771(9) _cell_length_b 17.947(8) _cell_length_c 7.952(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.58(2) _cell_angle_gamma 90.00 _cell_volume 2316(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8517 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 1.230 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7485 _exptl_absorpt_correction_T_max 0.7910 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11386 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2738 _reflns_number_gt 2362 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'CrystalStructure 3.7.0' _computing_structure_solution SIR92 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ORTEP3 for win' _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^)+(0.0667P)^2^+11.8368P] 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 2738 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1660 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 1.0000 0.22206(4) 1.0000 0.0340(2) Uani 1 2 d S . . Cl1 Cl 1.09068(7) 0.21842(8) 0.83557(15) 0.0559(3) Uani 1 1 d . . . P1 P 0.93058(7) 0.30759(7) 0.81650(15) 0.0467(3) Uani 1 1 d . . . P2 P 0.70303(12) 0.0000 0.7034(3) 0.0551(5) Uani 1 2 d S . . F1 F 0.7029(5) -0.0862(3) 0.7087(13) 0.193(4) Uani 1 1 d . . . F2 F 0.6109(4) 0.0000 0.5968(9) 0.147(3) Uani 1 2 d S . . F3 F 0.6692(4) 0.0000 0.8726(7) 0.0925(17) Uani 1 2 d S . . F4 F 0.7343(5) 0.0000 0.5355(9) 0.160(4) Uani 1 2 d S . . F5 F 0.7949(4) 0.0000 0.8051(10) 0.132(3) Uani 1 2 d S . . N1 N 0.9308(3) 0.1387(2) 0.8520(5) 0.0522(9) Uani 1 1 d . . . H1A H 0.9576 0.0959 0.8887 0.063 Uiso 1 1 calc R . . H1B H 0.8834 0.1368 0.8855 0.063 Uiso 1 1 calc R . . N2 N 0.9587(9) 0.0000 1.1623(18) 0.123(4) Uani 1 2 d S . . C1 C 0.8386(4) 0.3447(4) 0.8613(8) 0.0793(19) Uani 1 1 d . . . H1C H 0.8056 0.3046 0.8868 0.095 Uiso 1 1 calc R . . H1D H 0.8078 0.3716 0.7617 0.095 Uiso 1 1 calc R . . H1E H 0.8532 0.3776 0.9593 0.095 Uiso 1 1 calc R . . C2 C 0.9866(5) 0.3891(3) 0.7682(9) 0.084(2) Uani 1 1 d . . . H2A H 1.0369 0.3733 0.7424 0.101 Uiso 1 1 calc R . . H2B H 0.9991 0.4217 0.8670 0.101 Uiso 1 1 calc R . . H2C H 0.9532 0.4150 0.6698 0.101 Uiso 1 1 calc R . . C3 C 0.8928(3) 0.2714(3) 0.5988(6) 0.0543(12) Uani 1 1 d . . . H3A H 0.8553 0.3078 0.5311 0.065 Uiso 1 1 calc R . . H3B H 0.9391 0.2669 0.5470 0.065 Uiso 1 1 calc R . . C4 C 0.8488(3) 0.1968(3) 0.5818(6) 0.0612(13) Uani 1 1 d . . . H4A H 0.8251 0.1861 0.4598 0.073 Uiso 1 1 calc R . . H4B H 0.8041 0.1995 0.6388 0.073 Uiso 1 1 calc R . . C5 C 0.9067(3) 0.1338(3) 0.6618(6) 0.0577(12) Uani 1 1 d . . . H5A H 0.8798 0.0864 0.6274 0.069 Uiso 1 1 calc R . . H5B H 0.9557 0.1359 0.6180 0.069 Uiso 1 1 calc R . . C6 C 0.9034(7) 0.0000 1.201(2) 0.100(4) Uani 1 2 d S . . C7 C 0.8274(11) 0.0000 1.231(2) 0.156(7) Uani 1 2 d S . . H7A H 0.8002 0.0461 1.1913 0.188 Uiso 0.50 1 calc PR . . H7B H 0.8323 -0.0054 1.3534 0.188 Uiso 0.50 1 calc PR . . H7C H 0.7959 -0.0407 1.1698 0.188 Uiso 0.50 1 calc PR . . 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 0.0391(4) 0.0330(4) 0.0286(4) 0.000 0.0059(3) 0.000 Cl1 0.0503(6) 0.0764(8) 0.0445(6) 0.0071(5) 0.0181(5) 0.0005(5) P1 0.0494(6) 0.0413(6) 0.0412(6) 0.0044(5) -0.0039(5) 0.0021(5) P2 0.0552(10) 0.0572(11) 0.0526(10) 0.000 0.0133(8) 0.000 F1 0.233(8) 0.065(3) 0.337(11) -0.045(5) 0.180(8) -0.015(4) F2 0.071(4) 0.270(11) 0.088(4) 0.000 -0.003(3) 0.000 F3 0.112(4) 0.103(4) 0.070(3) 0.000 0.038(3) 0.000 F4 0.130(6) 0.297(12) 0.071(4) 0.000 0.060(4) 0.000 F5 0.072(4) 0.200(9) 0.107(5) 0.000 -0.012(3) 0.000 N1 0.070(3) 0.044(2) 0.0410(19) -0.0053(16) 0.0102(17) -0.0149(18) N2 0.170(12) 0.061(5) 0.171(11) 0.000 0.104(10) 0.000 C1 0.078(4) 0.087(4) 0.064(3) -0.007(3) -0.001(3) 0.039(3) C2 0.103(5) 0.050(3) 0.081(4) 0.026(3) -0.014(4) -0.018(3) C3 0.055(3) 0.064(3) 0.039(2) 0.010(2) 0.003(2) -0.002(2) C4 0.059(3) 0.078(4) 0.041(2) -0.008(2) 0.001(2) -0.019(3) C5 0.073(3) 0.059(3) 0.039(2) -0.014(2) 0.009(2) -0.014(2) C6 0.061(5) 0.053(5) 0.176(13) 0.000 0.009(7) 0.000 C7 0.154(15) 0.23(2) 0.100(10) 0.000 0.059(10) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.070(4) . ? Co1 N1 2.070(4) 2_757 ? Co1 P1 2.2328(14) . ? Co1 P1 2.2328(14) 2_757 ? Co1 Cl1 2.2422(14) 2_757 ? Co1 Cl1 2.2423(14) . ? P1 C1 1.796(6) . ? P1 C3 1.808(5) . ? P1 C2 1.831(6) . ? P2 F1 1.548(5) . ? P2 F1 1.548(5) 6 ? P2 F5 1.550(6) . ? P2 F4 1.553(6) . ? P2 F2 1.564(7) . ? P2 F3 1.586(6) . ? N1 C5 1.466(6) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C6 1.050(14) . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.519(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.521(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.353(18) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 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 N1 Co1 N1 87.4(2) . 2_757 ? N1 Co1 P1 89.99(13) . . ? N1 Co1 P1 173.81(11) 2_757 . ? N1 Co1 P1 173.81(11) . 2_757 ? N1 Co1 P1 89.98(13) 2_757 2_757 ? P1 Co1 P1 93.14(7) . 2_757 ? N1 Co1 Cl1 86.85(13) . 2_757 ? N1 Co1 Cl1 90.75(13) 2_757 2_757 ? P1 Co1 Cl1 94.73(6) . 2_757 ? P1 Co1 Cl1 87.57(6) 2_757 2_757 ? N1 Co1 Cl1 90.74(13) . . ? N1 Co1 Cl1 86.84(13) 2_757 . ? P1 Co1 Cl1 87.57(6) . . ? P1 Co1 Cl1 94.73(6) 2_757 . ? Cl1 Co1 Cl1 176.67(8) 2_757 . ? C1 P1 C3 102.2(3) . . ? C1 P1 C2 104.9(4) . . ? C3 P1 C2 99.2(3) . . ? C1 P1 Co1 117.2(2) . . ? C3 P1 Co1 112.24(18) . . ? C2 P1 Co1 118.4(2) . . ? F1 P2 F1 176.9(7) . 6 ? F1 P2 F5 89.6(4) . . ? F1 P2 F5 89.6(4) 6 . ? F1 P2 F4 91.5(3) . . ? F1 P2 F4 91.5(3) 6 . ? F5 P2 F4 86.7(5) . . ? F1 P2 F2 90.4(4) . . ? F1 P2 F2 90.4(4) 6 . ? F5 P2 F2 178.7(4) . . ? F4 P2 F2 92.0(4) . . ? F1 P2 F3 88.5(3) . . ? F1 P2 F3 88.5(3) 6 . ? F5 P2 F3 94.5(4) . . ? F4 P2 F3 178.8(4) . . ? F2 P2 F3 86.8(4) . . ? C5 N1 Co1 126.8(3) . . ? C5 N1 H1A 105.6 . . ? Co1 N1 H1A 105.6 . . ? C5 N1 H1B 105.6 . . ? Co1 N1 H1B 105.6 . . ? H1A N1 H1B 106.1 . . ? P1 C1 H1C 109.5 . . ? P1 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? P1 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 116.5(3) . . ? C4 C3 H3A 108.2 . . ? P1 C3 H3A 108.2 . . ? C4 C3 H3B 108.2 . . ? P1 C3 H3B 108.2 . . ? H3A C3 H3B 107.3 . . ? C3 C4 C5 111.9(4) . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N1 C5 C4 111.6(4) . . ? N1 C5 H5A 109.3 . . ? C4 C5 H5A 109.3 . . ? N1 C5 H5B 109.3 . . ? C4 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? N2 C6 C7 173(2) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 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 N1 Co1 P1 C1 89.6(3) . . . . ? P1 Co1 P1 C1 -85.0(3) 2_757 . . . ? Cl1 Co1 P1 C1 2.8(3) 2_757 . . . ? Cl1 Co1 P1 C1 -179.6(3) . . . . ? N1 Co1 P1 C3 -28.3(2) . . . . ? P1 Co1 P1 C3 157.1(2) 2_757 . . . ? Cl1 Co1 P1 C3 -115.1(2) 2_757 . . . ? Cl1 Co1 P1 C3 62.49(19) . . . . ? N1 Co1 P1 C2 -143.0(3) . . . . ? P1 Co1 P1 C2 42.4(3) 2_757 . . . ? Cl1 Co1 P1 C2 130.2(3) 2_757 . . . ? Cl1 Co1 P1 C2 -52.2(3) . . . . ? N1 Co1 N1 C5 -132.4(5) 2_757 . . . ? P1 Co1 N1 C5 41.9(4) . . . . ? Cl1 Co1 N1 C5 136.7(4) 2_757 . . . ? Cl1 Co1 N1 C5 -45.6(4) . . . . ? C1 P1 C3 C4 -78.6(5) . . . . ? C2 P1 C3 C4 173.8(4) . . . . ? Co1 P1 C3 C4 47.8(5) . . . . ? P1 C3 C4 C5 -66.3(5) . . . . ? Co1 N1 C5 C4 -65.3(6) . . . . ? C3 C4 C5 N1 70.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.890 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.096 #==END #============================================================================== data_pdmpCl2P _database_code_depnum_ccdc_archive 'CCDC 618531' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans(Cl,Cl)cis(P,P)-dichlorobis((3-aminopropyl)dimethylphosphine)cobalt(III) hexafluorophosphate ; _chemical_name_common ; trans(Cl,Cl)cis(P,P)-dichlorobis((3- aminopropyl)dimethylphosphine)cobalt(iii) hexafluorophosphate ; _chemical_melting_point ? _chemical_formula_moiety 'C10 H28 Cl2 Co N2 P2 1+, F6 P 1-' _chemical_formula_sum 'C10 H28 Cl2 Co F6 N2 P3' _chemical_formula_weight 513.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 8.178(11) _cell_length_b 10.073(13) _cell_length_c 12.811(16) _cell_angle_alpha 105.659(12) _cell_angle_beta 94.09(2) _cell_angle_gamma 98.15(2) _cell_volume 999(2) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 3077 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 1.416 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7648 _exptl_absorpt_correction_T_max 0.9325 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ? _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7883 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4364 _reflns_number_gt 3617 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction 'CrystalStructure 3.7.0' _computing_structure_solution SIR92 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ORTEP3 for win' _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^)+(0.0430P)^2^+0.3128P] 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 4364 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.0985 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co -0.01482(4) 0.83736(4) 0.74476(3) 0.01582(11) Uani 1 1 d . . . Cl1 Cl 0.14064(9) 0.73548(8) 0.61793(6) 0.02578(17) Uani 1 1 d . . . Cl2 Cl -0.17103(9) 0.94521(7) 0.86758(5) 0.02531(17) Uani 1 1 d . . . P1 P -0.25405(9) 0.74350(7) 0.63949(6) 0.01928(16) Uani 1 1 d . . . P2 P -0.00244(9) 0.65719(8) 0.81232(6) 0.02312(17) Uani 1 1 d . . . P3 P 0.44222(10) 0.27158(8) 0.77718(7) 0.02595(18) Uani 1 1 d . . . F1 F 0.2634(3) 0.2904(3) 0.7299(2) 0.0575(6) Uani 1 1 d . . . F2 F 0.3920(3) 0.1073(2) 0.71727(18) 0.0480(5) Uani 1 1 d . . . F3 F 0.5173(3) 0.2916(2) 0.66967(17) 0.0471(5) Uani 1 1 d . . . F4 F 0.3642(3) 0.2474(2) 0.88247(17) 0.0493(6) Uani 1 1 d . . . F5 F 0.4862(3) 0.4341(2) 0.83434(19) 0.0538(6) Uani 1 1 d . . . F6 F 0.6173(3) 0.2495(3) 0.82239(19) 0.0575(6) Uani 1 1 d . . . N1 N 0.0086(3) 0.9987(3) 0.6744(2) 0.0270(6) Uani 1 1 d . . . H1A H 0.0922 1.0656 0.7182 0.032 Uiso 1 1 calc R . . H1B H 0.0504 0.9645 0.6095 0.032 Uiso 1 1 calc R . . N2 N 0.1865(3) 0.9453(2) 0.85406(18) 0.0216(5) Uani 1 1 d . . . H2A H 0.2146 1.0290 0.8384 0.026 Uiso 1 1 calc R . . H2B H 0.1485 0.9665 0.9215 0.026 Uiso 1 1 calc R . . C1 C -0.4123(4) 0.6491(3) 0.6956(3) 0.0320(7) Uani 1 1 d . . . H1C H -0.4260 0.7056 0.7687 0.038 Uiso 1 1 calc R . . H1D H -0.3791 0.5608 0.7001 0.038 Uiso 1 1 calc R . . H1E H -0.5177 0.6294 0.6484 0.038 Uiso 1 1 calc R . . C2 C -0.2426(4) 0.6273(3) 0.5063(2) 0.0331(7) Uani 1 1 d . . . H2C H -0.1584 0.6715 0.4699 0.040 Uiso 1 1 calc R . . H2D H -0.3510 0.6078 0.4624 0.040 Uiso 1 1 calc R . . H2E H -0.2124 0.5395 0.5143 0.040 Uiso 1 1 calc R . . C3 C -0.3625(4) 0.8772(3) 0.6101(3) 0.0269(6) Uani 1 1 d . . . H3A H -0.4608 0.8304 0.5564 0.032 Uiso 1 1 calc R . . H3B H -0.4037 0.9279 0.6779 0.032 Uiso 1 1 calc R . . C4 C -0.2604(4) 0.9832(3) 0.5661(3) 0.0330(7) Uani 1 1 d . . . H4A H -0.2122 0.9332 0.5011 0.040 Uiso 1 1 calc R . . H4B H -0.3344 1.0422 0.5427 0.040 Uiso 1 1 calc R . . C5 C -0.1218(4) 1.0761(3) 0.6488(3) 0.0293(7) Uani 1 1 d . . . H5A H -0.0715 1.1524 0.6201 0.035 Uiso 1 1 calc R . . H5B H -0.1685 1.1190 0.7167 0.035 Uiso 1 1 calc R . . C6 C -0.0747(4) 0.4815(3) 0.7231(3) 0.0384(8) Uani 1 1 d . . . H6A H -0.0252 0.4706 0.6544 0.046 Uiso 1 1 calc R . . H6B H -0.1961 0.4659 0.7080 0.046 Uiso 1 1 calc R . . H6C H -0.0417 0.4131 0.7588 0.046 Uiso 1 1 calc R . . C7 C -0.1012(5) 0.6642(4) 0.9357(3) 0.0426(9) Uani 1 1 d . . . H7A H -0.0672 0.7572 0.9876 0.051 Uiso 1 1 calc R . . H7B H -0.0674 0.5934 0.9684 0.051 Uiso 1 1 calc R . . H7C H -0.2223 0.6459 0.9177 0.051 Uiso 1 1 calc R . . C8 C 0.2125(4) 0.6439(3) 0.8513(3) 0.0299(7) Uani 1 1 d . . . H8A H 0.2111 0.5714 0.8904 0.036 Uiso 1 1 calc R . . H8B H 0.2649 0.6108 0.7838 0.036 Uiso 1 1 calc R . . C9 C 0.3227(4) 0.7777(4) 0.9229(3) 0.0342(7) Uani 1 1 d . . . H9A H 0.2730 0.8107 0.9915 0.041 Uiso 1 1 calc R . . H9B H 0.4333 0.7560 0.9421 0.041 Uiso 1 1 calc R . . C10 C 0.3444(4) 0.8929(3) 0.8685(3) 0.0280(7) Uani 1 1 d . . . H10A H 0.4301 0.9707 0.9135 0.034 Uiso 1 1 calc R . . H10B H 0.3836 0.8575 0.7964 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0170(2) 0.01512(19) 0.01634(18) 0.00464(14) 0.00302(13) 0.00519(14) Cl1 0.0235(4) 0.0301(4) 0.0234(3) 0.0038(3) 0.0080(3) 0.0081(3) Cl2 0.0278(4) 0.0279(4) 0.0211(3) 0.0029(3) 0.0058(3) 0.0137(3) P1 0.0177(4) 0.0166(3) 0.0226(4) 0.0040(3) 0.0011(3) 0.0036(3) P2 0.0245(4) 0.0213(4) 0.0305(4) 0.0138(3) 0.0101(3) 0.0108(3) P3 0.0243(4) 0.0242(4) 0.0329(4) 0.0134(3) 0.0039(3) 0.0053(3) F1 0.0371(12) 0.0638(16) 0.0758(17) 0.0241(13) -0.0063(11) 0.0198(11) F2 0.0593(14) 0.0259(11) 0.0565(14) 0.0078(10) 0.0178(11) 0.0021(10) F3 0.0538(13) 0.0536(14) 0.0391(11) 0.0243(10) 0.0122(10) 0.0008(11) F4 0.0624(14) 0.0488(13) 0.0441(12) 0.0206(10) 0.0254(11) 0.0100(11) F5 0.0632(14) 0.0277(11) 0.0645(15) 0.0074(10) 0.0096(12) -0.0023(10) F6 0.0388(12) 0.0876(18) 0.0572(14) 0.0323(13) -0.0003(10) 0.0273(12) N1 0.0254(13) 0.0260(13) 0.0327(14) 0.0155(11) -0.0003(11) 0.0025(11) N2 0.0238(12) 0.0207(12) 0.0197(11) 0.0047(9) -0.0015(9) 0.0055(10) C1 0.0239(16) 0.0267(16) 0.0465(19) 0.0142(14) 0.0044(14) 0.0004(13) C2 0.0348(18) 0.0319(18) 0.0264(16) -0.0022(13) -0.0035(13) 0.0087(14) C3 0.0222(15) 0.0258(15) 0.0330(16) 0.0097(13) -0.0032(12) 0.0056(12) C4 0.0337(17) 0.0355(18) 0.0357(18) 0.0207(15) -0.0030(14) 0.0083(14) C5 0.0319(17) 0.0219(15) 0.0395(18) 0.0160(13) 0.0037(14) 0.0081(13) C6 0.0347(19) 0.0226(16) 0.063(2) 0.0178(16) 0.0089(17) 0.0087(14) C7 0.050(2) 0.050(2) 0.048(2) 0.0335(18) 0.0264(18) 0.0267(18) C8 0.0311(17) 0.0320(17) 0.0357(17) 0.0178(14) 0.0081(13) 0.0172(14) C9 0.0335(17) 0.045(2) 0.0285(16) 0.0127(15) -0.0014(13) 0.0186(15) C10 0.0201(15) 0.0324(17) 0.0294(16) 0.0059(13) -0.0043(12) 0.0066(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 2.049(3) . ? Co1 N1 2.053(3) . ? Co1 P2 2.223(2) . ? Co1 P1 2.225(2) . ? Co1 Cl2 2.246(2) . ? Co1 Cl1 2.252(2) . ? P1 C1 1.802(3) . ? P1 C2 1.808(3) . ? P1 C3 1.819(3) . ? P2 C7 1.815(4) . ? P2 C6 1.818(4) . ? P2 C8 1.826(4) . ? P3 F6 1.573(3) . ? P3 F5 1.579(3) . ? P3 F4 1.594(3) . ? P3 F3 1.597(3) . ? P3 F1 1.598(3) . ? P3 F2 1.604(3) . ? N1 C5 1.476(4) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C10 1.481(4) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C1 H1E 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C2 H2E 0.9800 . ? C3 C4 1.515(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.508(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.529(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.503(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N1 87.95(12) . . ? N2 Co1 P2 88.33(10) . . ? N1 Co1 P2 171.18(8) . . ? N2 Co1 P1 171.57(7) . . ? N1 Co1 P1 89.58(9) . . ? P2 Co1 P1 95.20(7) . . ? N2 Co1 Cl2 86.32(12) . . ? N1 Co1 Cl2 92.01(11) . . ? P2 Co1 Cl2 95.74(8) . . ? P1 Co1 Cl2 85.71(10) . . ? N2 Co1 Cl1 94.05(12) . . ? N1 Co1 Cl1 85.77(11) . . ? P2 Co1 Cl1 86.52(8) . . ? P1 Co1 Cl1 93.80(10) . . ? Cl2 Co1 Cl1 177.73(3) . . ? C1 P1 C2 104.37(18) . . ? C1 P1 C3 100.98(17) . . ? C2 P1 C3 103.83(17) . . ? C1 P1 Co1 117.27(14) . . ? C2 P1 Co1 116.96(12) . . ? C3 P1 Co1 111.46(13) . . ? C7 P2 C6 105.36(19) . . ? C7 P2 C8 103.86(17) . . ? C6 P2 C8 100.09(16) . . ? C7 P2 Co1 115.63(12) . . ? C6 P2 Co1 118.62(15) . . ? C8 P2 Co1 111.25(11) . . ? F6 P3 F5 91.08(15) . . ? F6 P3 F4 90.95(14) . . ? F5 P3 F4 90.65(14) . . ? F6 P3 F3 89.65(14) . . ? F5 P3 F3 90.88(13) . . ? F4 P3 F3 178.35(13) . . ? F6 P3 F1 178.74(15) . . ? F5 P3 F1 90.17(14) . . ? F4 P3 F1 89.09(15) . . ? F3 P3 F1 90.28(15) . . ? F6 P3 F2 90.78(14) . . ? F5 P3 F2 178.13(14) . . ? F4 P3 F2 89.51(13) . . ? F3 P3 F2 88.94(13) . . ? F1 P3 F2 87.97(14) . . ? C5 N1 Co1 127.7(2) . . ? C5 N1 H1A 105.4 . . ? Co1 N1 H1A 105.4 . . ? C5 N1 H1B 105.4 . . ? Co1 N1 H1B 105.4 . . ? H1A N1 H1B 106.0 . . ? C10 N2 Co1 124.76(19) . . ? C10 N2 H2A 106.1 . . ? Co1 N2 H2A 106.1 . . ? C10 N2 H2B 106.1 . . ? Co1 N2 H2B 106.1 . . ? H2A N2 H2B 106.3 . . ? P1 C1 H1C 109.5 . . ? P1 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? P1 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? P1 C2 H2C 109.5 . . ? P1 C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? P1 C2 H2E 109.5 . . ? H2C C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? C4 C3 P1 115.5(2) . . ? C4 C3 H3A 108.4 . . ? P1 C3 H3A 108.4 . . ? C4 C3 H3B 108.4 . . ? P1 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? C5 C4 C3 112.8(3) . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? N1 C5 C4 112.3(3) . . ? N1 C5 H5A 109.1 . . ? C4 C5 H5A 109.1 . . ? N1 C5 H5B 109.1 . . ? C4 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P2 C7 H7A 109.5 . . ? P2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 P2 116.5(2) . . ? C9 C8 H8A 108.2 . . ? P2 C8 H8A 108.2 . . ? C9 C8 H8B 108.2 . . ? P2 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? C10 C9 C8 113.1(3) . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9B 109.0 . . ? C8 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? N2 C10 C9 111.3(3) . . ? N2 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? N2 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? 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 N1 Co1 P1 C1 -147.36(14) . . . . ? P2 Co1 P1 C1 40.07(13) . . . . ? Cl2 Co1 P1 C1 -55.31(15) . . . . ? Cl1 Co1 P1 C1 126.91(14) . . . . ? N1 Co1 P1 C2 87.51(17) . . . . ? P2 Co1 P1 C2 -85.06(15) . . . . ? Cl2 Co1 P1 C2 179.56(13) . . . . ? Cl1 Co1 P1 C2 1.78(13) . . . . ? N1 Co1 P1 C3 -31.70(14) . . . . ? P2 Co1 P1 C3 155.72(12) . . . . ? Cl2 Co1 P1 C3 60.34(12) . . . . ? Cl1 Co1 P1 C3 -117.43(12) . . . . ? N2 Co1 P2 C7 82.69(19) . . . . ? P1 Co1 P2 C7 -89.64(17) . . . . ? Cl2 Co1 P2 C7 -3.44(15) . . . . ? Cl1 Co1 P2 C7 176.85(15) . . . . ? N2 Co1 P2 C6 -150.69(15) . . . . ? P1 Co1 P2 C6 36.98(13) . . . . ? Cl2 Co1 P2 C6 123.18(15) . . . . ? Cl1 Co1 P2 C6 -56.53(15) . . . . ? N2 Co1 P2 C8 -35.45(14) . . . . ? P1 Co1 P2 C8 152.22(12) . . . . ? Cl2 Co1 P2 C8 -121.59(13) . . . . ? Cl1 Co1 P2 C8 58.71(13) . . . . ? N2 Co1 N1 C5 -129.0(3) . . . . ? P1 Co1 N1 C5 42.9(3) . . . . ? Cl2 Co1 N1 C5 -42.8(3) . . . . ? Cl1 Co1 N1 C5 136.8(3) . . . . ? N1 Co1 N2 C10 -120.1(2) . . . . ? P2 Co1 N2 C10 51.9(2) . . . . ? Cl2 Co1 N2 C10 147.7(2) . . . . ? Cl1 Co1 N2 C10 -34.5(2) . . . . ? C1 P1 C3 C4 176.9(2) . . . . ? C2 P1 C3 C4 -75.2(3) . . . . ? Co1 P1 C3 C4 51.6(3) . . . . ? P1 C3 C4 C5 -67.0(3) . . . . ? Co1 N1 C5 C4 -62.8(4) . . . . ? C3 C4 C5 N1 68.0(4) . . . . ? C7 P2 C8 C9 -75.1(3) . . . . ? C6 P2 C8 C9 176.1(2) . . . . ? Co1 P2 C8 C9 49.9(3) . . . . ? P2 C8 C9 C10 -62.1(3) . . . . ? Co1 N2 C10 C9 -71.5(3) . . . . ? C8 C9 C10 N2 67.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.406 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.078 #==END #============================================================================== data_dmppCl2 _database_code_depnum_ccdc_archive 'CCDC 618532' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-Dichlorobis(1,3-bis(dimethylphosphino)propane)cobalt(III) Perchlorate ; _chemical_name_common ;trans-Dichlorobis(1,3- bis(dimethylphosphino)propane)cobalt(iii) Perchlorate ; _chemical_melting_point ? _chemical_formula_moiety 'C14 H36 Cl2 Co P4 1+, Cl O4 1-' _chemical_formula_sum 'C14 H36 Cl3 Co O4 P4' _chemical_formula_weight 557.59 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' Cl Cl 0.1484 0.1585 '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' 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 tetragonal _symmetry_space_group_name_H-M 'P 42/n b c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x, z+1/2' '-x+1/2, -y+1/2, z' 'y, -x+1/2, z+1/2' '-x, y+1/2, z' 'y+1/2, x+1/2, z+1/2' 'x+1/2, -y, z' '-y, -x, z+1/2' '-x, -y, -z' 'y-1/2, -x, -z-1/2' 'x-1/2, y-1/2, -z' '-y, x-1/2, -z-1/2' 'x, -y-1/2, -z' '-y-1/2, -x-1/2, -z-1/2' '-x-1/2, y, -z' 'y, x, -z-1/2' _cell_length_a 11.4228(15) _cell_length_b 11.4228(15) _cell_length_c 18.262(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2382.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.3 _cell_measurement_theta_max 17.4 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.343 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.5896 _exptl_absorpt_correction_T_max 0.7050 _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 AFC7R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 1815 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 29.98 _reflns_number_total 1746 _reflns_number_gt 1262 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection WinAFC _computing_cell_refinement WinAFC _computing_data_reduction 'CrystalStructure 3.7.0' _computing_structure_solution SIR92 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ORTEP3 for win' _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^)+(0.0681P)^2^+1.7271P] 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 1746 _refine_ls_number_parameters 63 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1354 _refine_ls_wR_factor_gt 0.1220 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.7500 0.2500 0.5000 0.02722(18) Uani 1 4 d S . . Cl1 Cl 0.94746(7) 0.2500 0.5000 0.0381(2) Uani 1 2 d S . . Cl2 Cl 0.2500 0.2500 0.2500 0.0735(6) Uani 1 4 d S . . P1 P 0.76355(5) 0.10723(6) 0.41267(4) 0.03371(19) Uani 1 1 d . . . O1 O 0.1566(7) 0.2452(7) 0.2917(5) 0.280(6) Uani 1 1 d . . . C1 C 0.8621(3) 0.1351(3) 0.33638(17) 0.0453(7) Uani 1 1 d . . . H1A H 0.9360 0.1625 0.3547 0.054 Uiso 1 1 calc R . . H1B H 0.8286 0.1935 0.3049 0.054 Uiso 1 1 calc R . . H1C H 0.8738 0.0641 0.3092 0.054 Uiso 1 1 calc R . . C2 C 0.6304(3) 0.0570(3) 0.36794(18) 0.0482(7) Uani 1 1 d . . . H2A H 0.5898 0.1227 0.3473 0.058 Uiso 1 1 calc R . . H2B H 0.5810 0.0189 0.4032 0.058 Uiso 1 1 calc R . . H2C H 0.6502 0.0027 0.3297 0.058 Uiso 1 1 calc R . . C3 C 0.8280(3) -0.0273(2) 0.44813(17) 0.0428(6) Uani 1 1 d . . . H3A H 0.8494 -0.0765 0.4069 0.051 Uiso 1 1 calc R . . H3B H 0.8995 -0.0074 0.4739 0.051 Uiso 1 1 calc R . . C4 C 0.7500 -0.0991(3) 0.5000 0.0467(9) Uani 1 2 d S . . H4A H 0.7001 -0.1494 0.4707 0.056 Uiso 0.50 1 calc PR . . H4B H 0.7999 -0.1494 0.5293 0.056 Uiso 0.50 1 calc PR . . 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 0.0207(3) 0.0259(3) 0.0351(3) 0.000 0.000 0.000 Cl1 0.0221(4) 0.0421(5) 0.0501(5) 0.0064(4) 0.000 0.000 Cl2 0.0770(9) 0.0770(9) 0.0664(11) 0.000 0.000 -0.0279(11) P1 0.0282(3) 0.0326(3) 0.0404(4) -0.0040(3) 0.0040(2) 0.0016(2) O1 0.247(10) 0.250(12) 0.343(14) -0.039(8) 0.197(10) -0.058(8) C1 0.0420(14) 0.0513(16) 0.0426(15) -0.0009(13) 0.0103(12) 0.0061(12) C2 0.0384(14) 0.0493(17) 0.0570(18) -0.0134(14) -0.0031(13) -0.0036(13) C3 0.0393(14) 0.0314(13) 0.0577(18) -0.0022(12) 0.0090(12) 0.0079(10) C4 0.053(2) 0.0255(17) 0.062(3) 0.000 0.007(2) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 Cl1 2.2555(9) . ? Co1 Cl1 2.2556(9) 3_655 ? Co1 P1 2.2862(7) 15_756 ? Co1 P1 2.2862(7) 13_566 ? Co1 P1 2.2862(7) 3_655 ? Co1 P1 2.2863(7) . ? Cl2 O1 1.312(6) 16_556 ? Cl2 O1 1.312(6) 3 ? Cl2 O1 1.312(6) . ? Cl2 O1 1.312(6) 14_666 ? P1 C2 1.819(3) . ? P1 C1 1.819(3) . ? P1 C3 1.823(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.537(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C3 1.537(4) 15_756 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? 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 Cl1 Co1 Cl1 180.0 . 3_655 ? Cl1 Co1 P1 93.883(16) . 15_756 ? Cl1 Co1 P1 86.117(16) 3_655 15_756 ? Cl1 Co1 P1 86.118(16) . 13_566 ? Cl1 Co1 P1 93.882(16) 3_655 13_566 ? P1 Co1 P1 91.54(4) 15_756 13_566 ? Cl1 Co1 P1 93.883(16) . 3_655 ? Cl1 Co1 P1 86.116(16) 3_655 3_655 ? P1 Co1 P1 172.23(3) 15_756 3_655 ? P1 Co1 P1 88.99(4) 13_566 3_655 ? Cl1 Co1 P1 86.118(16) . . ? Cl1 Co1 P1 93.883(16) 3_655 . ? P1 Co1 P1 88.99(4) 15_756 . ? P1 Co1 P1 172.24(3) 13_566 . ? P1 Co1 P1 91.54(4) 3_655 . ? O1 Cl2 O1 113.9(8) 16_556 3 ? O1 Cl2 O1 105.6(7) 16_556 . ? O1 Cl2 O1 109.0(9) 3 . ? O1 Cl2 O1 109.0(9) 16_556 14_666 ? O1 Cl2 O1 105.6(7) 3 14_666 ? O1 Cl2 O1 113.9(8) . 14_666 ? C2 P1 C1 103.23(15) . . ? C2 P1 C3 103.34(15) . . ? C1 P1 C3 99.78(14) . . ? C2 P1 Co1 118.80(10) . . ? C1 P1 Co1 116.82(11) . . ? C3 P1 Co1 112.40(10) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 115.78(19) . . ? C4 C3 H3A 108.3 . . ? P1 C3 H3A 108.3 . . ? C4 C3 H3B 108.3 . . ? P1 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? C3 C4 C3 115.5(3) 15_756 . ? C3 C4 H4A 108.4 15_756 . ? C3 C4 H4A 108.4 . . ? C3 C4 H4B 108.4 15_756 . ? C3 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? 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 Cl1 Co1 P1 C2 -173.43(13) . . . . ? Cl1 Co1 P1 C2 6.57(13) 3_655 . . . ? P1 Co1 P1 C2 92.61(13) 15_756 . . . ? P1 Co1 P1 C2 -79.64(13) 3_655 . . . ? Cl1 Co1 P1 C1 -48.64(12) . . . . ? Cl1 Co1 P1 C1 131.36(12) 3_655 . . . ? P1 Co1 P1 C1 -142.61(13) 15_756 . . . ? P1 Co1 P1 C1 45.15(12) 3_655 . . . ? Cl1 Co1 P1 C3 65.82(10) . . . . ? Cl1 Co1 P1 C3 -114.18(10) 3_655 . . . ? P1 Co1 P1 C3 -28.14(10) 15_756 . . . ? P1 Co1 P1 C3 159.61(11) 3_655 . . . ? C2 P1 C3 C4 -57.1(2) . . . . ? C1 P1 C3 C4 -163.3(2) . . . . ? Co1 P1 C3 C4 72.2(2) . . . . ? P1 C3 C4 C3 -36.64(12) . . . 15_756 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.711 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.104 #==END #============================================================================== data_pdmpen2 _database_code_depnum_ccdc_archive 'CCDC 618533' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(1,2-diaminoethane)((3-aminopropyl)dimethylphosphine)cobalt(III) Dichloride Hexafluorophosphate ; _chemical_name_common ; Bis(1,2-diaminoethane)((3- aminopropyl)dimethylphosphine)cobalt(iii) Dichloride Hexafluorophosphate ; _chemical_melting_point ? _chemical_formula_moiety 'C9 H30 Co N5 P 3+, 2(Cl 1-), F6 P 1-' _chemical_formula_sum 'C9 H30 Cl2 Co F6 N5 P2' _chemical_formula_weight 514.15 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.6831(13) _cell_length_b 12.793(3) _cell_length_c 7.807(2) _cell_angle_alpha 107.309(19) _cell_angle_beta 96.862(17) _cell_angle_gamma 88.801(16) _cell_volume 1011.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.7 _cell_measurement_theta_max 15.0 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 1.328 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6914 _exptl_absorpt_correction_T_max 0.8787 _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 AFC5R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 6151 _diffrn_reflns_av_R_equivalents 0.0145 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 30.00 _reflns_number_total 5862 _reflns_number_gt 4603 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'CrystalStructure 3.7.0' _computing_structure_solution SIR92 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ORTEP3 for win' _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^)+(0.0727P)^2^+1.2083P] 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 5862 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1350 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.27423(3) 0.15610(3) 0.28980(4) 0.01941(10) Uani 1 1 d . . . Cl1 Cl -0.09137(7) 0.01596(7) 0.26757(10) 0.03707(17) Uani 1 1 d . . . Cl2 Cl 0.42492(6) 0.09971(6) 0.77887(9) 0.03172(15) Uani 1 1 d . . . P1 P 0.21276(7) 0.29489(6) 0.51491(9) 0.02782(15) Uani 1 1 d . . . P2 P 0.27375(11) 0.59033(8) 0.18908(14) 0.0476(2) Uani 1 1 d . . . F1 F 0.3584(4) 0.6971(3) 0.2831(5) 0.0948(11) Uani 1 1 d . . . F2 F 0.2186(6) 0.6317(5) 0.0350(9) 0.192(3) Uani 1 1 d . . . F3 F 0.1731(5) 0.6301(6) 0.3043(10) 0.215(4) Uani 1 1 d . . . F4 F 0.3866(5) 0.5496(5) 0.0766(7) 0.174(3) Uani 1 1 d . . . F5 F 0.3424(5) 0.5418(4) 0.3401(7) 0.147(2) Uani 1 1 d . . . F6 F 0.2035(5) 0.4780(3) 0.0969(6) 0.1318(18) Uani 1 1 d . . . N1 N 0.1067(2) 0.15484(18) 0.1467(3) 0.0246(4) Uani 1 1 d . . . H1A H 0.1132 0.1093 0.0354 0.029 Uiso 1 1 calc R . . H1B H 0.0524 0.1225 0.1956 0.029 Uiso 1 1 calc R . . N2 N 0.3125(2) 0.01717(18) 0.0952(3) 0.0244(4) Uani 1 1 d . . . H2A H 0.2896 0.0251 -0.0149 0.029 Uiso 1 1 calc R . . H2B H 0.3958 0.0041 0.1059 0.029 Uiso 1 1 calc R . . N3 N 0.2158(2) 0.05202(19) 0.4073(3) 0.0251(4) Uani 1 1 d . . . H3A H 0.2501 0.0711 0.5235 0.030 Uiso 1 1 calc R . . H3B H 0.1315 0.0559 0.4055 0.030 Uiso 1 1 calc R . . N4 N 0.4505(2) 0.1541(2) 0.4045(3) 0.0276(4) Uani 1 1 d . . . H4A H 0.4576 0.1975 0.5196 0.033 Uiso 1 1 calc R . . H4B H 0.4704 0.0856 0.4054 0.033 Uiso 1 1 calc R . . N5 N 0.3468(2) 0.25304(19) 0.1674(3) 0.0281(5) Uani 1 1 d . . . H5A H 0.3458 0.2172 0.0490 0.034 Uiso 1 1 calc R . . H5B H 0.2988 0.3128 0.1777 0.034 Uiso 1 1 calc R . . C1 C 0.1219(4) 0.2539(3) 0.6656(5) 0.0510(9) Uani 1 1 d . . . H1C H 0.1703 0.2047 0.7182 0.061 Uiso 1 1 calc R . . H1D H 0.0454 0.2178 0.5992 0.061 Uiso 1 1 calc R . . H1E H 0.1017 0.3174 0.7596 0.061 Uiso 1 1 calc R . . C2 C 0.3337(4) 0.3850(4) 0.6658(6) 0.0603(12) Uani 1 1 d . . . H2C H 0.3943 0.3425 0.7164 0.072 Uiso 1 1 calc R . . H2D H 0.2959 0.4365 0.7613 0.072 Uiso 1 1 calc R . . H2E H 0.3751 0.4237 0.5998 0.072 Uiso 1 1 calc R . . C3 C 0.1068(4) 0.3851(3) 0.4315(5) 0.0452(8) Uani 1 1 d . . . H3C H 0.0718 0.4355 0.5331 0.054 Uiso 1 1 calc R . . H3D H 0.1549 0.4281 0.3780 0.054 Uiso 1 1 calc R . . C4 C -0.0018(4) 0.3271(3) 0.2916(5) 0.0483(9) Uani 1 1 d . . . H4C H -0.0497 0.2832 0.3437 0.058 Uiso 1 1 calc R . . H4D H -0.0577 0.3816 0.2622 0.058 Uiso 1 1 calc R . . C5 C 0.0432(3) 0.2544(2) 0.1204(4) 0.0343(6) Uani 1 1 d . . . H5C H -0.0283 0.2324 0.0278 0.041 Uiso 1 1 calc R . . H5D H 0.1016 0.2956 0.0782 0.041 Uiso 1 1 calc R . . C6 C 0.2415(3) -0.0756(2) 0.1165(4) 0.0297(5) Uani 1 1 d . . . H6A H 0.2777 -0.1447 0.0541 0.036 Uiso 1 1 calc R . . H6B H 0.1541 -0.0748 0.0663 0.036 Uiso 1 1 calc R . . C7 C 0.2503(3) -0.0621(2) 0.3162(4) 0.0292(5) Uani 1 1 d . . . H7A H 0.1932 -0.1132 0.3386 0.035 Uiso 1 1 calc R . . H7B H 0.3355 -0.0763 0.3617 0.035 Uiso 1 1 calc R . . C8 C 0.5389(3) 0.1935(3) 0.3021(4) 0.0342(6) Uani 1 1 d . . . H8A H 0.5558 0.1348 0.1962 0.041 Uiso 1 1 calc R . . H8B H 0.6181 0.2175 0.3775 0.041 Uiso 1 1 calc R . . C9 C 0.4779(3) 0.2874(3) 0.2466(5) 0.0365(6) Uani 1 1 d . . . H9A H 0.4781 0.3518 0.3507 0.044 Uiso 1 1 calc R . . H9B H 0.5237 0.3049 0.1584 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02078(16) 0.02091(16) 0.01649(15) 0.00533(11) 0.00264(11) 0.00016(11) Cl1 0.0331(3) 0.0515(4) 0.0285(3) 0.0152(3) 0.0008(3) -0.0109(3) Cl2 0.0297(3) 0.0417(4) 0.0262(3) 0.0133(3) 0.0055(2) 0.0044(3) P1 0.0316(3) 0.0274(3) 0.0219(3) 0.0030(2) 0.0050(2) 0.0038(3) P2 0.0612(6) 0.0318(4) 0.0475(5) 0.0116(4) -0.0028(4) -0.0035(4) F1 0.106(3) 0.0619(18) 0.099(2) 0.0088(17) -0.020(2) -0.0281(18) F2 0.197(5) 0.196(5) 0.219(6) 0.171(5) -0.130(5) -0.093(4) F3 0.106(4) 0.230(7) 0.239(7) -0.066(6) 0.100(5) 0.010(4) F4 0.129(4) 0.200(6) 0.132(4) -0.061(4) 0.057(3) -0.038(4) F5 0.171(5) 0.130(4) 0.158(4) 0.100(4) -0.064(4) -0.040(3) F6 0.187(5) 0.093(3) 0.103(3) 0.023(2) -0.033(3) -0.091(3) N1 0.0243(10) 0.0253(10) 0.0236(10) 0.0077(8) 0.0000(8) 0.0005(8) N2 0.0277(10) 0.0252(10) 0.0204(9) 0.0064(8) 0.0050(8) 0.0023(8) N3 0.0252(10) 0.0301(11) 0.0228(10) 0.0115(8) 0.0048(8) 0.0009(8) N4 0.0243(10) 0.0326(12) 0.0256(10) 0.0091(9) 0.0006(8) -0.0004(9) N5 0.0335(12) 0.0265(11) 0.0269(11) 0.0106(9) 0.0064(9) -0.0009(9) C1 0.067(2) 0.049(2) 0.0462(19) 0.0191(16) 0.0338(18) 0.0195(18) C2 0.050(2) 0.060(2) 0.045(2) -0.0208(18) 0.0010(17) -0.0060(18) C3 0.065(2) 0.0280(14) 0.0378(16) 0.0062(12) -0.0004(15) 0.0143(14) C4 0.0468(19) 0.0440(18) 0.0482(19) 0.0088(15) -0.0005(15) 0.0226(15) C5 0.0366(15) 0.0304(14) 0.0353(14) 0.0128(11) -0.0060(12) 0.0031(11) C6 0.0345(14) 0.0241(12) 0.0299(13) 0.0065(10) 0.0048(10) -0.0019(10) C7 0.0333(13) 0.0257(12) 0.0332(13) 0.0146(10) 0.0072(11) 0.0018(10) C8 0.0234(12) 0.0424(16) 0.0373(15) 0.0118(12) 0.0054(11) -0.0050(11) C9 0.0352(15) 0.0354(15) 0.0405(16) 0.0125(12) 0.0054(12) -0.0099(12) _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 N3 1.975(2) . ? Co1 N4 1.989(2) . ? Co1 N1 1.992(2) . ? Co1 N5 1.994(2) . ? Co1 N2 2.036(2) . ? Co1 P1 2.2456(10) . ? P1 C3 1.804(3) . ? P1 C1 1.807(4) . ? P1 C2 1.810(4) . ? P2 F3 1.470(4) . ? P2 F2 1.507(4) . ? P2 F6 1.565(3) . ? P2 F4 1.566(5) . ? P2 F1 1.587(3) . ? P2 F5 1.589(4) . ? N1 C5 1.486(3) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C6 1.483(3) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C7 1.482(3) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C8 1.491(4) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N5 C9 1.482(4) . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C2 H2C 0.9600 . ? C2 H2D 0.9600 . ? C2 H2E 0.9600 . ? C3 C4 1.530(5) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 C5 1.510(5) . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C5 H5C 0.9700 . ? C5 H5D 0.9700 . ? C6 C7 1.508(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.504(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? 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 N3 Co1 N4 92.20(10) . . ? N3 Co1 N1 92.36(9) . . ? N4 Co1 N1 173.01(9) . . ? N3 Co1 N5 174.91(10) . . ? N4 Co1 N5 83.98(10) . . ? N1 Co1 N5 91.15(10) . . ? N3 Co1 N2 83.52(9) . . ? N4 Co1 N2 87.95(10) . . ? N1 Co1 N2 87.29(9) . . ? N5 Co1 N2 92.97(9) . . ? N3 Co1 P1 89.13(7) . . ? N4 Co1 P1 95.42(8) . . ? N1 Co1 P1 89.95(7) . . ? N5 Co1 P1 94.57(8) . . ? N2 Co1 P1 172.03(7) . . ? C3 P1 C1 102.52(19) . . ? C3 P1 C2 104.5(2) . . ? C1 P1 C2 103.7(2) . . ? C3 P1 Co1 112.01(12) . . ? C1 P1 Co1 114.68(13) . . ? C2 P1 Co1 117.82(14) . . ? F3 P2 F2 96.4(5) . . ? F3 P2 F6 91.6(3) . . ? F2 P2 F6 90.1(3) . . ? F3 P2 F4 176.6(4) . . ? F2 P2 F4 86.3(4) . . ? F6 P2 F4 90.3(3) . . ? F3 P2 F1 92.9(3) . . ? F2 P2 F1 93.5(2) . . ? F6 P2 F1 173.9(3) . . ? F4 P2 F1 85.0(2) . . ? F3 P2 F5 89.1(4) . . ? F2 P2 F5 174.5(4) . . ? F6 P2 F5 89.5(2) . . ? F4 P2 F5 88.2(4) . . ? F1 P2 F5 86.5(2) . . ? C5 N1 Co1 124.17(18) . . ? C5 N1 H1A 106.3 . . ? Co1 N1 H1A 106.3 . . ? C5 N1 H1B 106.3 . . ? Co1 N1 H1B 106.3 . . ? H1A N1 H1B 106.4 . . ? C6 N2 Co1 108.74(16) . . ? C6 N2 H2A 109.9 . . ? Co1 N2 H2A 109.9 . . ? C6 N2 H2B 109.9 . . ? Co1 N2 H2B 109.9 . . ? H2A N2 H2B 108.3 . . ? C7 N3 Co1 111.92(16) . . ? C7 N3 H3A 109.2 . . ? Co1 N3 H3A 109.2 . . ? C7 N3 H3B 109.2 . . ? Co1 N3 H3B 109.2 . . ? H3A N3 H3B 107.9 . . ? C8 N4 Co1 109.86(17) . . ? C8 N4 H4A 109.7 . . ? Co1 N4 H4A 109.7 . . ? C8 N4 H4B 109.7 . . ? Co1 N4 H4B 109.7 . . ? H4A N4 H4B 108.2 . . ? C9 N5 Co1 111.48(18) . . ? C9 N5 H5A 109.3 . . ? Co1 N5 H5A 109.3 . . ? C9 N5 H5B 109.3 . . ? Co1 N5 H5B 109.3 . . ? H5A N5 H5B 108.0 . . ? P1 C1 H1C 109.5 . . ? P1 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? P1 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? P1 C2 H2C 109.5 . . ? P1 C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? P1 C2 H2E 109.5 . . ? H2C C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? C4 C3 P1 114.6(2) . . ? C4 C3 H3C 108.6 . . ? P1 C3 H3C 108.6 . . ? C4 C3 H3D 108.6 . . ? P1 C3 H3D 108.6 . . ? H3C C3 H3D 107.6 . . ? C5 C4 C3 112.6(3) . . ? C5 C4 H4C 109.1 . . ? C3 C4 H4C 109.1 . . ? C5 C4 H4D 109.1 . . ? C3 C4 H4D 109.1 . . ? H4C C4 H4D 107.8 . . ? N1 C5 C4 112.4(3) . . ? N1 C5 H5C 109.1 . . ? C4 C5 H5C 109.1 . . ? N1 C5 H5D 109.1 . . ? C4 C5 H5D 109.1 . . ? H5C C5 H5D 107.8 . . ? N2 C6 C7 107.1(2) . . ? N2 C6 H6A 110.3 . . ? C7 C6 H6A 110.3 . . ? N2 C6 H6B 110.3 . . ? C7 C6 H6B 110.3 . . ? H6A C6 H6B 108.5 . . ? N3 C7 C6 107.6(2) . . ? N3 C7 H7A 110.2 . . ? C6 C7 H7A 110.2 . . ? N3 C7 H7B 110.2 . . ? C6 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? N4 C8 C9 107.9(2) . . ? N4 C8 H8A 110.1 . . ? C9 C8 H8A 110.1 . . ? N4 C8 H8B 110.1 . . ? C9 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? N5 C9 C8 107.4(2) . . ? N5 C9 H9A 110.2 . . ? C8 C9 H9A 110.2 . . ? N5 C9 H9B 110.2 . . ? C8 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? 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 N3 Co1 P1 C3 -125.74(17) . . . . ? N4 Co1 P1 C3 142.14(17) . . . . ? N1 Co1 P1 C3 -33.38(17) . . . . ? N5 Co1 P1 C3 57.76(17) . . . . ? N3 Co1 P1 C1 -9.44(18) . . . . ? N4 Co1 P1 C1 -101.57(18) . . . . ? N1 Co1 P1 C1 82.92(18) . . . . ? N5 Co1 P1 C1 174.06(18) . . . . ? N3 Co1 P1 C2 113.1(2) . . . . ? N4 Co1 P1 C2 20.9(2) . . . . ? N1 Co1 P1 C2 -154.6(2) . . . . ? N5 Co1 P1 C2 -63.4(2) . . . . ? N3 Co1 N1 C5 136.5(2) . . . . ? N5 Co1 N1 C5 -47.2(2) . . . . ? N2 Co1 N1 C5 -140.1(2) . . . . ? P1 Co1 N1 C5 47.4(2) . . . . ? N3 Co1 N2 C6 17.88(18) . . . . ? N4 Co1 N2 C6 110.32(18) . . . . ? N1 Co1 N2 C6 -74.81(18) . . . . ? N5 Co1 N2 C6 -165.81(18) . . . . ? N4 Co1 N3 C7 -77.68(19) . . . . ? N1 Co1 N3 C7 97.01(19) . . . . ? N2 Co1 N3 C7 10.00(18) . . . . ? P1 Co1 N3 C7 -173.08(18) . . . . ? N3 Co1 N4 C8 160.20(19) . . . . ? N5 Co1 N4 C8 -16.44(19) . . . . ? N2 Co1 N4 C8 76.8(2) . . . . ? P1 Co1 N4 C8 -110.48(19) . . . . ? N4 Co1 N5 C9 -10.3(2) . . . . ? N1 Co1 N5 C9 174.7(2) . . . . ? N2 Co1 N5 C9 -98.0(2) . . . . ? P1 Co1 N5 C9 84.6(2) . . . . ? C1 P1 C3 C4 -75.0(3) . . . . ? C2 P1 C3 C4 177.0(3) . . . . ? Co1 P1 C3 C4 48.4(3) . . . . ? P1 C3 C4 C5 -63.6(4) . . . . ? Co1 N1 C5 C4 -69.9(3) . . . . ? C3 C4 C5 N1 71.0(4) . . . . ? Co1 N2 C6 C7 -41.3(3) . . . . ? Co1 N3 C7 C6 -35.4(3) . . . . ? N2 C6 C7 N3 49.7(3) . . . . ? Co1 N4 C8 C9 39.5(3) . . . . ? Co1 N5 C9 C8 34.4(3) . . . . ? N4 C8 C9 N5 -47.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.186 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.098 #==END #============================================================================== data_pdmpdtc2 _database_code_depnum_ccdc_archive 'CCDC 618534' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(N,N-dimethyldithiocarbamato)((3-aminopropyl)dimethylphosphine)cobalt(III) Hexafluorophosphate ; _chemical_name_common ; Bis(N,N-dimethyldithiocarbamato)((3- aminopropyl)dimethylphosphine)cobalt(iii) Hexafluorophosphate ; _chemical_melting_point ? _chemical_formula_moiety 'C11 H26 Co N3 P S4 1+, F6 P 1-' _chemical_formula_sum 'C11 H26 Co F6 N3 P2 S4' _chemical_formula_weight 563.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/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 10.924(5) _cell_length_b 15.016(5) _cell_length_c 13.904(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.129(17) _cell_angle_gamma 90.00 _cell_volume 2280.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 17485 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour 'dark red-purple' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 1.310 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6947 _exptl_absorpt_correction_T_max 0.8278 _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21752 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0150 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5195 _reflns_number_gt 4646 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'CrystalStructure 3.7.0' _computing_structure_solution SIR92 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ORTEP3 for win' _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^)+(0.0717P)^2^+1.1985P] 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 5195 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.1148 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.18496(3) 0.064624(18) 0.75431(2) 0.02708(10) Uani 1 1 d . . . S1 S 0.06971(6) -0.00337(4) 0.87231(4) 0.03873(15) Uani 1 1 d . . . S2 S -0.01200(5) 0.09058(4) 0.70812(4) 0.03889(15) Uani 1 1 d . . . S3 S 0.20293(6) 0.19247(4) 0.83932(5) 0.04050(16) Uani 1 1 d . . . S4 S 0.36139(6) 0.04539(4) 0.84067(4) 0.03739(15) Uani 1 1 d . . . P1 P 0.26760(5) 0.12953(4) 0.62678(4) 0.03261(14) Uani 1 1 d . . . P2 P 0.48374(8) -0.20988(6) 0.69891(6) 0.0567(2) Uani 1 1 d . . . F1 F 0.3805(4) -0.2155(3) 0.6226(3) 0.1431(14) Uani 1 1 d . . . F2 F 0.5878(4) -0.2186(2) 0.6231(3) 0.1405(16) Uani 1 1 d . . . F3 F 0.4835(4) -0.3113(2) 0.7174(3) 0.159(2) Uani 1 1 d . . . F4 F 0.4836(3) -0.10602(17) 0.6816(3) 0.1341(13) Uani 1 1 d . . . F5 F 0.3803(3) -0.1981(2) 0.7772(2) 0.1130(10) Uani 1 1 d . . . F6 F 0.5826(4) -0.1991(5) 0.7788(3) 0.203(3) Uani 1 1 d . . . N1 N 0.1950(2) -0.05492(12) 0.68860(14) 0.0354(4) Uani 1 1 d . . . H1A H 0.2736 -0.0725 0.6933 0.042 Uiso 1 1 calc R . . H1B H 0.1511 -0.0929 0.7248 0.042 Uiso 1 1 calc R . . N2 N -0.1672(2) -0.00444(17) 0.81905(16) 0.0473(5) Uani 1 1 d . . . N3 N 0.4039(2) 0.18851(15) 0.95302(16) 0.0448(5) Uani 1 1 d . . . C1 C 0.2280(4) 0.2438(2) 0.6038(3) 0.0734(11) Uani 1 1 d . . . H1C H 0.1406 0.2503 0.6047 0.088 Uiso 1 1 calc R . . H1D H 0.2586 0.2610 0.5418 0.088 Uiso 1 1 calc R . . H1E H 0.2637 0.2810 0.6524 0.088 Uiso 1 1 calc R . . C2 C 0.4329(3) 0.1289(3) 0.6224(3) 0.0783(12) Uani 1 1 d . . . H2A H 0.4623 0.0696 0.6337 0.094 Uiso 1 1 calc R . . H2B H 0.4647 0.1681 0.6710 0.094 Uiso 1 1 calc R . . H2C H 0.4595 0.1488 0.5602 0.094 Uiso 1 1 calc R . . C3 C 0.2224(4) 0.0762(2) 0.5154(2) 0.0602(9) Uani 1 1 d . . . H3A H 0.1371 0.0897 0.5027 0.072 Uiso 1 1 calc R . . H3B H 0.2704 0.1010 0.4632 0.072 Uiso 1 1 calc R . . C4 C 0.2390(4) -0.0251(2) 0.5162(2) 0.0721(11) Uani 1 1 d . . . H4A H 0.2218 -0.0482 0.4525 0.087 Uiso 1 1 calc R . . H4B H 0.3236 -0.0388 0.5314 0.087 Uiso 1 1 calc R . . C5 C 0.1577(3) -0.07096(18) 0.5874(2) 0.0505(7) Uani 1 1 d . . . H5A H 0.0744 -0.0503 0.5784 0.061 Uiso 1 1 calc R . . H5B H 0.1589 -0.1345 0.5749 0.061 Uiso 1 1 calc R . . C6 C -0.0540(2) 0.02385(17) 0.80315(16) 0.0357(5) Uani 1 1 d . . . C7 C -0.1933(3) -0.0699(3) 0.8942(2) 0.0682(10) Uani 1 1 d . . . H7A H -0.2624 -0.0504 0.9312 0.082 Uiso 1 1 calc R . . H7B H -0.1233 -0.0759 0.9355 0.082 Uiso 1 1 calc R . . H7C H -0.2116 -0.1264 0.8651 0.082 Uiso 1 1 calc R . . C8 C -0.2685(3) 0.0223(3) 0.7567(3) 0.0693(10) Uani 1 1 d . . . H8A H -0.3387 0.0363 0.7953 0.083 Uiso 1 1 calc R . . H8B H -0.2883 -0.0256 0.7136 0.083 Uiso 1 1 calc R . . H8C H -0.2451 0.0738 0.7201 0.083 Uiso 1 1 calc R . . C9 C 0.3338(2) 0.14899(16) 0.88796(17) 0.0353(5) Uani 1 1 d . . . C10 C 0.3771(4) 0.2782(2) 0.9873(3) 0.0658(9) Uani 1 1 d . . . H10A H 0.4483 0.3150 0.9801 0.079 Uiso 1 1 calc R . . H10B H 0.3545 0.2758 1.0540 0.079 Uiso 1 1 calc R . . H10C H 0.3107 0.3028 0.9505 0.079 Uiso 1 1 calc R . . C11 C 0.5125(3) 0.1447(2) 0.9911(2) 0.0578(8) Uani 1 1 d . . . H11A H 0.5577 0.1859 1.0303 0.069 Uiso 1 1 calc R . . H11B H 0.5630 0.1249 0.9389 0.069 Uiso 1 1 calc R . . H11C H 0.4885 0.0945 1.0294 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02833(17) 0.02735(17) 0.02557(16) 0.00060(10) -0.00100(11) -0.00025(10) S1 0.0404(3) 0.0493(3) 0.0266(3) 0.0061(2) 0.0002(2) -0.0051(2) S2 0.0310(3) 0.0482(3) 0.0374(3) 0.0106(2) -0.0016(2) 0.0000(2) S3 0.0437(3) 0.0350(3) 0.0427(3) -0.0090(2) -0.0054(3) 0.0047(2) S4 0.0365(3) 0.0394(3) 0.0362(3) -0.0021(2) -0.0073(2) 0.0040(2) P1 0.0340(3) 0.0317(3) 0.0322(3) 0.0046(2) 0.0009(2) -0.0048(2) P2 0.0585(5) 0.0547(4) 0.0568(5) -0.0004(3) 0.0000(4) 0.0207(4) F1 0.160(3) 0.159(3) 0.109(2) -0.016(2) -0.069(2) -0.013(3) F2 0.170(3) 0.0922(19) 0.160(3) 0.039(2) 0.113(3) 0.048(2) F3 0.170(3) 0.0806(18) 0.228(4) 0.071(2) 0.115(3) 0.060(2) F4 0.105(2) 0.0571(14) 0.240(4) -0.016(2) 0.014(2) 0.0099(14) F5 0.0939(19) 0.149(3) 0.096(2) -0.0086(18) 0.0313(16) 0.0362(19) F6 0.097(3) 0.375(8) 0.137(3) 0.039(4) -0.055(2) 0.005(4) N1 0.0452(11) 0.0293(9) 0.0315(10) -0.0012(7) 0.0017(8) -0.0005(8) N2 0.0391(11) 0.0685(15) 0.0343(11) 0.0033(10) 0.0021(9) -0.0152(10) N3 0.0488(12) 0.0492(12) 0.0364(11) -0.0045(9) -0.0069(9) -0.0100(10) C1 0.116(3) 0.0377(15) 0.067(2) 0.0170(14) 0.014(2) 0.0077(17) C2 0.0396(16) 0.130(4) 0.066(2) 0.035(2) 0.0049(14) -0.0153(19) C3 0.093(3) 0.0589(17) 0.0291(13) 0.0061(12) -0.0051(14) -0.0223(17) C4 0.128(3) 0.0559(18) 0.0324(14) -0.0106(13) 0.0175(17) -0.022(2) C5 0.075(2) 0.0391(13) 0.0379(13) -0.0077(10) -0.0055(13) -0.0140(13) C6 0.0356(11) 0.0435(12) 0.0281(10) -0.0027(9) 0.0028(9) -0.0047(9) C7 0.063(2) 0.099(3) 0.0426(16) 0.0159(16) 0.0037(14) -0.0348(18) C8 0.0359(15) 0.117(3) 0.0555(18) 0.0153(19) -0.0029(13) -0.0165(17) C9 0.0370(12) 0.0382(11) 0.0307(11) -0.0008(9) -0.0005(9) -0.0056(9) C10 0.081(2) 0.0544(18) 0.0620(19) -0.0196(15) -0.0172(17) -0.0095(16) C11 0.0500(16) 0.075(2) 0.0487(16) 0.0015(14) -0.0180(13) -0.0130(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.017(2) . ? Co1 P1 2.2171(9) . ? Co1 S3 2.2628(9) . ? Co1 S2 2.2776(12) . ? Co1 S4 2.2868(11) . ? Co1 S1 2.3085(9) . ? S1 C6 1.706(3) . ? S2 C6 1.721(2) . ? S3 C9 1.709(3) . ? S4 C9 1.716(3) . ? P1 C1 1.798(3) . ? P1 C2 1.807(3) . ? P1 C3 1.812(3) . ? P2 F3 1.545(3) . ? P2 F1 1.549(3) . ? P2 F6 1.556(4) . ? P2 F2 1.558(3) . ? P2 F4 1.578(3) . ? P2 F5 1.581(3) . ? N1 C5 1.484(3) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C6 1.326(3) . ? N2 C8 1.461(4) . ? N2 C7 1.463(4) . ? N3 C9 1.325(3) . ? N3 C11 1.455(4) . ? N3 C10 1.459(4) . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.532(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.498(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 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 N1 Co1 P1 90.36(6) . . ? N1 Co1 S3 170.67(7) . . ? P1 Co1 S3 90.56(4) . . ? N1 Co1 S2 94.42(7) . . ? P1 Co1 S2 94.90(3) . . ? S3 Co1 S2 94.75(3) . . ? N1 Co1 S4 94.51(7) . . ? P1 Co1 S4 97.54(4) . . ? S3 Co1 S4 76.16(3) . . ? S2 Co1 S4 164.62(3) . . ? N1 Co1 S1 87.63(7) . . ? P1 Co1 S1 170.58(3) . . ? S3 Co1 S1 92.91(3) . . ? S2 Co1 S1 76.10(3) . . ? S4 Co1 S1 91.79(4) . . ? C6 S1 Co1 85.76(9) . . ? C6 S2 Co1 86.40(9) . . ? C9 S3 Co1 87.37(9) . . ? C9 S4 Co1 86.44(8) . . ? C1 P1 C2 103.8(2) . . ? C1 P1 C3 101.82(18) . . ? C2 P1 C3 103.8(2) . . ? C1 P1 Co1 117.63(13) . . ? C2 P1 Co1 115.68(12) . . ? C3 P1 Co1 112.26(11) . . ? F3 P2 F1 93.4(3) . . ? F3 P2 F6 89.2(3) . . ? F1 P2 F6 176.2(3) . . ? F3 P2 F2 91.81(16) . . ? F1 P2 F2 93.6(2) . . ? F6 P2 F2 89.2(3) . . ? F3 P2 F4 179.1(2) . . ? F1 P2 F4 87.1(2) . . ? F6 P2 F4 90.3(3) . . ? F2 P2 F4 88.89(18) . . ? F3 P2 F5 89.69(18) . . ? F1 P2 F5 87.5(2) . . ? F6 P2 F5 89.6(2) . . ? F2 P2 F5 178.0(2) . . ? F4 P2 F5 89.60(19) . . ? C5 N1 Co1 123.97(16) . . ? C5 N1 H1A 106.3 . . ? Co1 N1 H1A 106.3 . . ? C5 N1 H1B 106.3 . . ? Co1 N1 H1B 106.3 . . ? H1A N1 H1B 106.4 . . ? C6 N2 C8 121.2(2) . . ? C6 N2 C7 121.2(3) . . ? C8 N2 C7 117.4(2) . . ? C9 N3 C11 121.1(2) . . ? C9 N3 C10 121.4(3) . . ? C11 N3 C10 117.5(2) . . ? P1 C1 H1C 109.5 . . ? P1 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? P1 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 113.6(2) . . ? C4 C3 H3A 108.8 . . ? P1 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? P1 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 113.0(3) . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? N1 C5 C4 112.9(2) . . ? N1 C5 H5A 109.0 . . ? C4 C5 H5A 109.0 . . ? N1 C5 H5B 109.0 . . ? C4 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N2 C6 S1 124.52(19) . . ? N2 C6 S2 124.4(2) . . ? S1 C6 S2 111.09(14) . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 S3 125.5(2) . . ? N3 C9 S4 124.5(2) . . ? S3 C9 S4 110.02(13) . . ? N3 C10 H10A 109.5 . . ? N3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 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 N1 Co1 S1 C6 -89.93(11) . . . . ? S3 Co1 S1 C6 99.39(9) . . . . ? S2 Co1 S1 C6 5.21(8) . . . . ? S4 Co1 S1 C6 175.62(9) . . . . ? N1 Co1 S2 C6 81.29(10) . . . . ? P1 Co1 S2 C6 172.03(8) . . . . ? S3 Co1 S2 C6 -96.99(9) . . . . ? S4 Co1 S2 C6 -44.04(14) . . . . ? S1 Co1 S2 C6 -5.16(8) . . . . ? P1 Co1 S3 C9 -98.24(9) . . . . ? S2 Co1 S3 C9 166.79(8) . . . . ? S4 Co1 S3 C9 -0.61(8) . . . . ? S1 Co1 S3 C9 90.52(9) . . . . ? N1 Co1 S4 C9 -179.71(10) . . . . ? P1 Co1 S4 C9 89.33(9) . . . . ? S3 Co1 S4 C9 0.61(8) . . . . ? S2 Co1 S4 C9 -54.39(13) . . . . ? S1 Co1 S4 C9 -91.95(9) . . . . ? N1 Co1 P1 C1 151.55(18) . . . . ? S3 Co1 P1 C1 -37.74(17) . . . . ? S2 Co1 P1 C1 57.08(17) . . . . ? S4 Co1 P1 C1 -113.85(17) . . . . ? N1 Co1 P1 C2 -85.0(2) . . . . ? S3 Co1 P1 C2 85.69(19) . . . . ? S2 Co1 P1 C2 -179.49(19) . . . . ? S4 Co1 P1 C2 9.57(19) . . . . ? N1 Co1 P1 C3 33.90(16) . . . . ? S3 Co1 P1 C3 -155.38(15) . . . . ? S2 Co1 P1 C3 -60.56(15) . . . . ? S4 Co1 P1 C3 128.50(15) . . . . ? P1 Co1 N1 C5 -45.7(2) . . . . ? S2 Co1 N1 C5 49.2(2) . . . . ? S4 Co1 N1 C5 -143.3(2) . . . . ? S1 Co1 N1 C5 125.1(2) . . . . ? C1 P1 C3 C4 -176.6(3) . . . . ? C2 P1 C3 C4 75.8(3) . . . . ? Co1 P1 C3 C4 -49.9(3) . . . . ? P1 C3 C4 C5 64.9(4) . . . . ? Co1 N1 C5 C4 67.3(4) . . . . ? C3 C4 C5 N1 -71.2(4) . . . . ? C8 N2 C6 S1 179.7(3) . . . . ? C7 N2 C6 S1 -6.0(4) . . . . ? C8 N2 C6 S2 -2.1(4) . . . . ? C7 N2 C6 S2 172.2(2) . . . . ? Co1 S1 C6 N2 171.3(2) . . . . ? Co1 S1 C6 S2 -7.19(12) . . . . ? Co1 S2 C6 N2 -171.2(2) . . . . ? Co1 S2 C6 S1 7.28(12) . . . . ? C11 N3 C9 S3 178.8(2) . . . . ? C10 N3 C9 S3 -2.7(4) . . . . ? C11 N3 C9 S4 -0.8(4) . . . . ? C10 N3 C9 S4 177.7(2) . . . . ? Co1 S3 C9 N3 -178.8(2) . . . . ? Co1 S3 C9 S4 0.84(11) . . . . ? Co1 S4 C9 N3 178.8(2) . . . . ? Co1 S4 C9 S3 -0.84(11) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.714 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.100 #==END #============================================================================== data_pdmp2dtc _database_code_depnum_ccdc_archive 'CCDC 618535' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans(P,N)-(N,N-Dimethyldithiocarbamato)bis((3-aminopropyl)dimethylphosphine) cobalt(III) Bis(tetraphenylborate) ; _chemical_name_common ; trans(P,N)-(N,N-Dimethyldithiocarbamato)bis((3- aminopropyl)dimethylphosphine) cobalt(iii) Bis(tetraphenylborate) ; _chemical_melting_point ? _chemical_formula_moiety 'C13 H34 Co N3 P2 S2 2+, 2(C24 H20 B 1-)' _chemical_formula_sum 'C61 H74 B2 Co N3 P2 S2' _chemical_formula_weight 1055.84 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' 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/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 17.854(4) _cell_length_b 14.294(4) _cell_length_c 22.041(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.825(9) _cell_angle_gamma 90.00 _cell_volume 5612(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 36079 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 0.479 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8466 _exptl_absorpt_correction_T_max 0.8938 _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53694 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12687 _reflns_number_gt 10114 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'CrystalStructure 3.7.0' _computing_structure_solution SIR92 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ORTEP3 for win' _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^)+(0.0659P)^2^+1.4751P] 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 12687 _refine_ls_number_parameters 643 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1205 _refine_ls_wR_factor_gt 0.1126 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.248457(14) 0.212315(17) 0.360968(10) 0.03473(8) Uani 1 1 d . . . S1 S 0.25439(3) 0.35336(4) 0.30999(2) 0.05335(14) Uani 1 1 d . . . S2 S 0.17631(3) 0.30878(4) 0.41299(2) 0.05040(13) Uani 1 1 d . . . P1 P 0.21645(3) 0.10007(3) 0.42522(2) 0.03829(11) Uani 1 1 d . . . P2 P 0.35441(3) 0.25507(4) 0.41315(2) 0.04417(12) Uani 1 1 d . . . N1 N 0.15705(10) 0.17719(12) 0.30342(7) 0.0457(4) Uani 1 1 d . . . H1A H 0.1170 0.2077 0.3164 0.055 Uiso 1 1 calc R . . H1B H 0.1652 0.2003 0.2664 0.055 Uiso 1 1 calc R . . N2 N 0.31211(11) 0.13679(13) 0.30553(8) 0.0530(4) Uani 1 1 d . . . H2A H 0.3316 0.0888 0.3278 0.064 Uiso 1 1 calc R . . H2B H 0.2804 0.1117 0.2765 0.064 Uiso 1 1 calc R . . N3 N 0.17156(13) 0.48127(13) 0.36598(10) 0.0692(6) Uani 1 1 d . . . C1 C 0.26120(15) -0.01318(16) 0.42325(12) 0.0645(6) Uani 1 1 d . . . H1C H 0.2607 -0.0347 0.3820 0.077 Uiso 1 1 calc R . . H1D H 0.2345 -0.0569 0.4469 0.077 Uiso 1 1 calc R . . H1E H 0.3121 -0.0082 0.4399 0.077 Uiso 1 1 calc R . . C2 C 0.22128(13) 0.13196(18) 0.50491(9) 0.0545(5) Uani 1 1 d . . . H2C H 0.1984 0.1921 0.5094 0.065 Uiso 1 1 calc R . . H2D H 0.2729 0.1345 0.5202 0.065 Uiso 1 1 calc R . . H2E H 0.1951 0.0861 0.5273 0.065 Uiso 1 1 calc R . . C3 C 0.11694(12) 0.07615(18) 0.41012(10) 0.0554(5) Uani 1 1 d . . . H3A H 0.1019 0.0310 0.4398 0.066 Uiso 1 1 calc R . . H3B H 0.0894 0.1335 0.4165 0.066 Uiso 1 1 calc R . . C4 C 0.09294(15) 0.03907(19) 0.34681(11) 0.0647(6) Uani 1 1 d . . . H4A H 0.0983 -0.0285 0.3473 0.078 Uiso 1 1 calc R . . H4B H 0.0401 0.0529 0.3384 0.078 Uiso 1 1 calc R . . C5 C 0.13536(14) 0.07716(16) 0.29521(10) 0.0562(5) Uani 1 1 d . . . H5A H 0.1803 0.0401 0.2916 0.067 Uiso 1 1 calc R . . H5B H 0.1044 0.0707 0.2576 0.067 Uiso 1 1 calc R . . C6 C 0.35257(17) 0.3589(2) 0.46028(14) 0.0803(8) Uani 1 1 d . . . H6A H 0.3154 0.3515 0.4895 0.096 Uiso 1 1 calc R . . H6B H 0.3403 0.4123 0.4352 0.096 Uiso 1 1 calc R . . H6C H 0.4010 0.3678 0.4811 0.096 Uiso 1 1 calc R . . C7 C 0.40256(13) 0.1699(2) 0.46289(11) 0.0628(6) Uani 1 1 d . . . H7A H 0.3697 0.1497 0.4931 0.075 Uiso 1 1 calc R . . H7B H 0.4467 0.1979 0.4825 0.075 Uiso 1 1 calc R . . H7C H 0.4167 0.1170 0.4394 0.075 Uiso 1 1 calc R . . C8 C 0.42692(14) 0.2812(2) 0.36144(12) 0.0659(7) Uani 1 1 d . . . H8A H 0.4126 0.3373 0.3388 0.079 Uiso 1 1 calc R . . H8B H 0.4733 0.2946 0.3853 0.079 Uiso 1 1 calc R . . C9 C 0.44135(15) 0.2039(2) 0.31678(13) 0.0775(8) Uani 1 1 d . . . H9A H 0.4828 0.2225 0.2931 0.093 Uiso 1 1 calc R . . H9B H 0.4568 0.1482 0.3395 0.093 Uiso 1 1 calc R . . C10 C 0.37533(15) 0.1793(2) 0.27378(11) 0.0668(7) Uani 1 1 d . . . H10A H 0.3575 0.2355 0.2527 0.080 Uiso 1 1 calc R . . H10B H 0.3914 0.1357 0.2436 0.080 Uiso 1 1 calc R . . C11 C 0.19640(13) 0.39478(14) 0.36259(10) 0.0511(5) Uani 1 1 d . . . C12 C 0.1929(2) 0.55109(19) 0.32174(16) 0.1008(12) Uani 1 1 d . . . H12A H 0.1813 0.6125 0.3361 0.121 Uiso 1 1 calc R . . H12B H 0.1656 0.5399 0.2834 0.121 Uiso 1 1 calc R . . H12C H 0.2458 0.5467 0.3167 0.121 Uiso 1 1 calc R . . C13 C 0.1239(2) 0.5095(2) 0.41436(16) 0.1006(12) Uani 1 1 d . . . H13A H 0.1018 0.5694 0.4047 0.121 Uiso 1 1 calc R . . H13B H 0.1537 0.5137 0.4522 0.121 Uiso 1 1 calc R . . H13C H 0.0848 0.4641 0.4179 0.121 Uiso 1 1 calc R . . C14 C 0.12679(11) 0.20235(13) 0.13395(8) 0.0379(4) Uani 1 1 d . . . C15 C 0.10721(13) 0.10778(16) 0.12692(10) 0.0542(5) Uani 1 1 d . . . H15 H 0.0566 0.0920 0.1247 0.065 Uiso 1 1 calc R . . C16 C 0.15938(16) 0.03645(17) 0.12305(12) 0.0646(6) Uani 1 1 d . . . H16 H 0.1432 -0.0251 0.1183 0.077 Uiso 1 1 calc R . . C17 C 0.23437(15) 0.05613(18) 0.12613(10) 0.0606(6) Uani 1 1 d . . . H17 H 0.2696 0.0086 0.1235 0.073 Uiso 1 1 calc R . . C18 C 0.25646(13) 0.14733(19) 0.13320(11) 0.0626(6) Uani 1 1 d . . . H18 H 0.3073 0.1621 0.1354 0.075 Uiso 1 1 calc R . . C19 C 0.20343(12) 0.21826(16) 0.13711(10) 0.0506(5) Uani 1 1 d . . . H19 H 0.2204 0.2795 0.1421 0.061 Uiso 1 1 calc R . . C20 C 0.09380(10) 0.39005(13) 0.12310(8) 0.0370(4) Uani 1 1 d . . . C21 C 0.15353(12) 0.42868(14) 0.15962(9) 0.0448(4) Uani 1 1 d . . . H21 H 0.1741 0.3935 0.1921 0.054 Uiso 1 1 calc R . . C22 C 0.18348(13) 0.51652(16) 0.14985(10) 0.0514(5) Uani 1 1 d . . . H22 H 0.2242 0.5380 0.1745 0.062 Uiso 1 1 calc R . . C23 C 0.15253(13) 0.57211(15) 0.10331(10) 0.0528(5) Uani 1 1 d . . . H23 H 0.1723 0.6310 0.0962 0.063 Uiso 1 1 calc R . . C24 C 0.09230(13) 0.53918(15) 0.06781(10) 0.0506(5) Uani 1 1 d . . . H24 H 0.0701 0.5768 0.0372 0.061 Uiso 1 1 calc R . . C25 C 0.06405(11) 0.45011(14) 0.07713(8) 0.0418(4) Uani 1 1 d . . . H25 H 0.0237 0.4293 0.0518 0.050 Uiso 1 1 calc R . . C26 C -0.00383(11) 0.25847(13) 0.08001(8) 0.0386(4) Uani 1 1 d . . . C27 C 0.01544(13) 0.21801(18) 0.02549(9) 0.0549(6) Uani 1 1 d . . . H27 H 0.0658 0.2061 0.0202 0.066 Uiso 1 1 calc R . . C28 C -0.03724(15) 0.1949(2) -0.02111(10) 0.0636(6) Uani 1 1 d . . . H28 H -0.0217 0.1669 -0.0562 0.076 Uiso 1 1 calc R . . C29 C -0.11207(14) 0.21294(16) -0.01606(10) 0.0540(5) Uani 1 1 d . . . H29 H -0.1475 0.1970 -0.0472 0.065 Uiso 1 1 calc R . . C30 C -0.13352(12) 0.25515(15) 0.03623(10) 0.0487(5) Uani 1 1 d . . . H30 H -0.1838 0.2690 0.0403 0.058 Uiso 1 1 calc R . . C31 C -0.08007(11) 0.27711(13) 0.08294(9) 0.0422(4) Uani 1 1 d . . . H31 H -0.0960 0.3056 0.1178 0.051 Uiso 1 1 calc R . . C32 C 0.02183(10) 0.28122(14) 0.20101(8) 0.0399(4) Uani 1 1 d . . . C33 C -0.01415(12) 0.20044(17) 0.21971(9) 0.0505(5) Uani 1 1 d . . . H33 H -0.0154 0.1484 0.1943 0.061 Uiso 1 1 calc R . . C34 C -0.04829(13) 0.1940(2) 0.27462(10) 0.0605(6) Uani 1 1 d . . . H34 H -0.0714 0.1386 0.2852 0.073 Uiso 1 1 calc R . . C35 C -0.04785(14) 0.2693(2) 0.31291(10) 0.0705(8) Uani 1 1 d . . . H35 H -0.0707 0.2657 0.3495 0.085 Uiso 1 1 calc R . . C36 C -0.01331(16) 0.3498(2) 0.29651(11) 0.0713(7) Uani 1 1 d . . . H36 H -0.0124 0.4012 0.3224 0.086 Uiso 1 1 calc R . . C37 C 0.02084(13) 0.35599(17) 0.24115(9) 0.0532(5) Uani 1 1 d . . . H37 H 0.0435 0.4119 0.2310 0.064 Uiso 1 1 calc R . . C38 C 0.35445(11) 0.80401(15) 0.33834(8) 0.0430(4) Uani 1 1 d . . . C39 C 0.37040(13) 0.86817(19) 0.29294(10) 0.0603(6) Uani 1 1 d . . . H39 H 0.4193 0.8900 0.2916 0.072 Uiso 1 1 calc R . . C40 C 0.31641(15) 0.9007(2) 0.24979(11) 0.0693(7) Uani 1 1 d . . . H40 H 0.3296 0.9436 0.2206 0.083 Uiso 1 1 calc R . . C41 C 0.24391(14) 0.86971(19) 0.25001(11) 0.0626(6) Uani 1 1 d . . . H41 H 0.2080 0.8893 0.2202 0.075 Uiso 1 1 calc R . . C42 C 0.22484(12) 0.80903(18) 0.29504(11) 0.0571(6) Uani 1 1 d . . . H42 H 0.1755 0.7886 0.2964 0.068 Uiso 1 1 calc R . . C43 C 0.27940(12) 0.77837(15) 0.33851(9) 0.0480(5) Uani 1 1 d . . . H43 H 0.2650 0.7388 0.3691 0.058 Uiso 1 1 calc R . . C44 C 0.38760(11) 0.73122(14) 0.45008(9) 0.0430(4) Uani 1 1 d . . . C45 C 0.35107(18) 0.64582(18) 0.45940(11) 0.0721(7) Uani 1 1 d . . . H45 H 0.3480 0.6026 0.4278 0.087 Uiso 1 1 calc R . . C46 C 0.3193(2) 0.6224(2) 0.51336(13) 0.0848(9) Uani 1 1 d . . . H46 H 0.2944 0.5656 0.5167 0.102 Uiso 1 1 calc R . . C47 C 0.32459(17) 0.6834(2) 0.56168(11) 0.0724(7) Uani 1 1 d . . . H47 H 0.3065 0.6669 0.5988 0.087 Uiso 1 1 calc R . . C48 C 0.35672(17) 0.7679(2) 0.55394(11) 0.0689(7) Uani 1 1 d . . . H48 H 0.3585 0.8112 0.5855 0.083 Uiso 1 1 calc R . . C49 C 0.38717(15) 0.79098(17) 0.49924(11) 0.0592(6) Uani 1 1 d . . . H49 H 0.4084 0.8500 0.4957 0.071 Uiso 1 1 calc R . . C50 C 0.49214(10) 0.83037(14) 0.38884(8) 0.0403(4) Uani 1 1 d . . . C51 C 0.48573(12) 0.92165(15) 0.41128(10) 0.0482(5) Uani 1 1 d . . . H51 H 0.4400 0.9398 0.4254 0.058 Uiso 1 1 calc R . . C52 C 0.54338(12) 0.98609(16) 0.41360(10) 0.0523(5) Uani 1 1 d . . . H52 H 0.5361 1.0452 0.4298 0.063 Uiso 1 1 calc R . . C53 C 0.61188(12) 0.96300(17) 0.39188(10) 0.0546(5) Uani 1 1 d . . . H53 H 0.6512 1.0058 0.3935 0.066 Uiso 1 1 calc R . . C54 C 0.62016(13) 0.87585(18) 0.36808(12) 0.0612(6) Uani 1 1 d . . . H54 H 0.6655 0.8594 0.3525 0.073 Uiso 1 1 calc R . . C55 C 0.56183(12) 0.81111(17) 0.36671(10) 0.0530(5) Uani 1 1 d . . . H55 H 0.5697 0.7523 0.3503 0.064 Uiso 1 1 calc R . . C56 C 0.44811(13) 0.65792(16) 0.35397(11) 0.0563(5) Uani 1 1 d . . . C57 C 0.50024(18) 0.6008(2) 0.38677(19) 0.0921(10) Uani 1 1 d . . . H57 H 0.5180 0.6198 0.4255 0.110 Uiso 1 1 calc R . . C58 C 0.5266(2) 0.5174(3) 0.3642(3) 0.1301(19) Uani 1 1 d . . . H58 H 0.5618 0.4822 0.3873 0.156 Uiso 1 1 calc R . . C59 C 0.5008(3) 0.4873(3) 0.3084(3) 0.138(2) Uani 1 1 d . . . H59 H 0.5177 0.4309 0.2934 0.166 Uiso 1 1 calc R . . C60 C 0.4505(3) 0.5396(3) 0.2747(2) 0.1213(18) Uani 1 1 d . . . H60 H 0.4333 0.5190 0.2363 0.146 Uiso 1 1 calc R . . C61 C 0.42404(19) 0.6247(2) 0.29722(13) 0.0801(9) Uani 1 1 d . . . H61 H 0.3894 0.6595 0.2732 0.096 Uiso 1 1 calc R . . B1 B 0.06057(12) 0.28462(15) 0.13471(9) 0.0361(4) Uani 1 1 d . . . B2 B 0.42083(13) 0.75667(16) 0.38375(10) 0.0419(5) 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 0.03932(14) 0.03374(13) 0.03143(13) 0.00444(9) 0.00461(9) 0.00473(10) S1 0.0623(3) 0.0455(3) 0.0518(3) 0.0179(2) 0.0004(2) 0.0011(2) S2 0.0561(3) 0.0435(3) 0.0524(3) -0.0008(2) 0.0100(2) 0.0144(2) P1 0.0408(3) 0.0394(3) 0.0349(2) 0.00647(18) 0.00433(18) 0.00083(19) P2 0.0424(3) 0.0453(3) 0.0445(3) 0.0033(2) 0.0004(2) 0.0002(2) N1 0.0510(10) 0.0479(9) 0.0374(8) 0.0060(7) -0.0036(7) 0.0008(8) N2 0.0576(11) 0.0550(11) 0.0483(9) -0.0025(8) 0.0176(8) 0.0072(8) N3 0.0867(15) 0.0363(10) 0.0809(14) -0.0044(9) -0.0211(11) 0.0118(10) C1 0.0718(16) 0.0428(12) 0.0790(16) 0.0121(11) 0.0051(12) 0.0083(11) C2 0.0540(12) 0.0749(16) 0.0352(10) 0.0076(9) 0.0067(8) -0.0049(11) C3 0.0472(12) 0.0662(15) 0.0526(12) 0.0110(10) 0.0028(9) -0.0104(10) C4 0.0700(15) 0.0610(15) 0.0609(14) 0.0109(11) -0.0135(11) -0.0223(12) C5 0.0687(14) 0.0511(13) 0.0466(11) -0.0024(9) -0.0123(10) -0.0049(11) C6 0.0754(18) 0.0732(19) 0.089(2) -0.0268(15) -0.0167(15) -0.0036(14) C7 0.0470(12) 0.0834(18) 0.0574(13) 0.0201(12) -0.0019(10) 0.0067(11) C8 0.0479(13) 0.0793(18) 0.0710(15) 0.0207(13) 0.0083(11) -0.0132(12) C9 0.0516(15) 0.111(2) 0.0730(17) 0.0147(15) 0.0254(12) 0.0039(14) C10 0.0674(16) 0.0859(18) 0.0502(12) 0.0067(12) 0.0272(11) 0.0107(13) C11 0.0576(12) 0.0360(10) 0.0572(12) -0.0012(9) -0.0140(10) 0.0058(9) C12 0.151(3) 0.0368(14) 0.110(2) 0.0146(14) -0.031(2) 0.0066(17) C13 0.128(3) 0.0608(18) 0.110(2) -0.0295(17) -0.015(2) 0.0434(19) C14 0.0429(10) 0.0413(10) 0.0298(8) 0.0047(7) 0.0047(7) 0.0032(8) C15 0.0508(12) 0.0459(12) 0.0666(13) 0.0034(10) 0.0089(10) 0.0000(9) C16 0.0800(18) 0.0391(12) 0.0753(16) 0.0008(10) 0.0097(13) 0.0075(11) C17 0.0671(15) 0.0576(14) 0.0573(13) 0.0018(10) 0.0054(11) 0.0266(12) C18 0.0433(12) 0.0715(17) 0.0725(15) -0.0025(12) -0.0001(10) 0.0153(11) C19 0.0413(11) 0.0482(12) 0.0621(13) -0.0024(9) 0.0031(9) 0.0033(9) C20 0.0377(9) 0.0409(10) 0.0335(8) 0.0026(7) 0.0091(7) 0.0053(7) C21 0.0506(11) 0.0440(11) 0.0394(10) 0.0018(8) 0.0006(8) 0.0031(9) C22 0.0535(12) 0.0483(12) 0.0527(12) -0.0078(9) 0.0049(9) -0.0031(9) C23 0.0643(14) 0.0360(10) 0.0595(12) 0.0003(9) 0.0152(10) -0.0008(9) C24 0.0596(13) 0.0435(11) 0.0496(11) 0.0095(9) 0.0094(9) 0.0091(9) C25 0.0405(10) 0.0441(11) 0.0411(9) 0.0041(8) 0.0054(7) 0.0059(8) C26 0.0421(10) 0.0407(10) 0.0334(9) 0.0048(7) 0.0050(7) -0.0011(8) C27 0.0470(12) 0.0830(17) 0.0351(10) -0.0007(9) 0.0065(8) 0.0076(11) C28 0.0752(16) 0.0822(18) 0.0331(10) -0.0063(10) 0.0008(10) 0.0085(13) C29 0.0643(14) 0.0524(13) 0.0431(11) 0.0042(9) -0.0128(9) -0.0073(10) C30 0.0409(11) 0.0462(11) 0.0583(12) 0.0081(9) -0.0013(9) -0.0020(9) C31 0.0435(10) 0.0404(10) 0.0431(10) -0.0001(8) 0.0049(8) 0.0013(8) C32 0.0362(9) 0.0528(11) 0.0307(8) 0.0061(7) 0.0029(7) 0.0050(8) C33 0.0485(12) 0.0631(14) 0.0405(10) 0.0061(9) 0.0086(8) -0.0063(10) C34 0.0520(13) 0.0889(18) 0.0411(11) 0.0140(11) 0.0066(9) -0.0164(12) C35 0.0571(14) 0.121(2) 0.0350(11) 0.0029(13) 0.0146(10) -0.0105(14) C36 0.0788(18) 0.094(2) 0.0429(12) -0.0163(12) 0.0175(11) -0.0035(15) C37 0.0580(13) 0.0613(14) 0.0415(10) -0.0039(9) 0.0113(9) 0.0030(10) C38 0.0393(10) 0.0514(11) 0.0384(9) -0.0008(8) 0.0031(7) -0.0011(8) C39 0.0416(11) 0.0879(18) 0.0509(12) 0.0176(11) 0.0004(9) -0.0125(11) C40 0.0643(15) 0.0869(19) 0.0553(13) 0.0249(13) -0.0056(11) -0.0116(13) C41 0.0537(13) 0.0746(17) 0.0573(13) 0.0111(11) -0.0126(10) -0.0025(11) C42 0.0390(11) 0.0703(15) 0.0610(13) 0.0029(11) -0.0036(9) -0.0072(10) C43 0.0455(11) 0.0518(12) 0.0466(11) 0.0050(9) 0.0014(8) -0.0078(9) C44 0.0456(11) 0.0423(10) 0.0402(10) 0.0019(8) -0.0033(8) 0.0033(8) C45 0.113(2) 0.0503(14) 0.0534(13) 0.0007(10) 0.0105(14) -0.0090(14) C46 0.126(3) 0.0644(17) 0.0656(16) 0.0157(13) 0.0137(16) -0.0146(17) C47 0.096(2) 0.0729(17) 0.0499(13) 0.0131(12) 0.0151(13) 0.0037(15) C48 0.0837(18) 0.0722(17) 0.0529(13) -0.0099(12) 0.0192(12) -0.0046(14) C49 0.0679(15) 0.0527(13) 0.0586(13) -0.0078(10) 0.0160(11) -0.0086(11) C50 0.0388(10) 0.0431(10) 0.0384(9) -0.0026(7) -0.0019(7) 0.0055(8) C51 0.0425(11) 0.0456(11) 0.0567(12) -0.0039(9) 0.0061(9) 0.0065(9) C52 0.0534(12) 0.0430(11) 0.0601(13) -0.0031(9) 0.0005(10) 0.0024(9) C53 0.0420(11) 0.0555(13) 0.0653(13) 0.0039(10) -0.0041(9) -0.0043(9) C54 0.0383(11) 0.0680(16) 0.0781(16) -0.0086(12) 0.0103(10) 0.0033(10) C55 0.0433(11) 0.0533(13) 0.0627(13) -0.0146(10) 0.0064(9) 0.0054(9) C56 0.0512(12) 0.0481(12) 0.0711(14) -0.0170(10) 0.0157(10) -0.0076(10) C57 0.0741(19) 0.0503(16) 0.151(3) -0.0196(17) -0.0015(19) 0.0168(14) C58 0.090(3) 0.0528(19) 0.255(6) -0.014(3) 0.065(3) 0.0130(17) C59 0.155(4) 0.056(2) 0.221(6) -0.045(3) 0.141(4) -0.032(2) C60 0.178(5) 0.086(3) 0.111(3) -0.051(2) 0.088(3) -0.054(3) C61 0.102(2) 0.0726(18) 0.0706(16) -0.0309(14) 0.0385(15) -0.0320(16) B1 0.0364(10) 0.0412(11) 0.0313(9) 0.0025(7) 0.0054(7) 0.0026(8) B2 0.0402(11) 0.0417(12) 0.0437(11) -0.0048(9) 0.0021(8) 0.0022(9) _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 N2 2.0336(17) . ? Co1 N1 2.0611(17) . ? Co1 P2 2.2327(7) . ? Co1 P1 2.2392(6) . ? Co1 S2 2.2521(7) . ? Co1 S1 2.3139(8) . ? S1 C11 1.711(2) . ? S2 C11 1.711(2) . ? P1 C1 1.807(2) . ? P1 C2 1.811(2) . ? P1 C3 1.818(2) . ? P2 C6 1.813(3) . ? P2 C7 1.816(2) . ? P2 C8 1.820(2) . ? N1 C5 1.489(3) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C10 1.496(3) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C11 1.317(3) . ? N3 C12 1.463(4) . ? N3 C13 1.465(4) . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C2 H2C 0.9600 . ? C2 H2D 0.9600 . ? C2 H2E 0.9600 . ? C3 C4 1.527(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.509(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.514(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.504(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C19 1.384(3) . ? C14 C15 1.402(3) . ? C14 B1 1.668(3) . ? C15 C16 1.387(3) . ? C15 H15 0.9300 . ? C16 C17 1.365(4) . ? C16 H16 0.9300 . ? C17 C18 1.368(4) . ? C17 H17 0.9300 . ? C18 C19 1.394(3) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C25 1.405(3) . ? C20 C21 1.406(3) . ? C20 B1 1.646(3) . ? C21 C22 1.387(3) . ? C21 H21 0.9300 . ? C22 C23 1.383(3) . ? C22 H22 0.9300 . ? C23 C24 1.370(3) . ? C23 H23 0.9300 . ? C24 C25 1.390(3) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C31 1.393(3) . ? C26 C27 1.397(3) . ? C26 B1 1.652(3) . ? C27 C28 1.385(3) . ? C27 H27 0.9300 . ? C28 C29 1.372(4) . ? C28 H28 0.9300 . ? C29 C30 1.378(3) . ? C29 H29 0.9300 . ? C30 C31 1.392(3) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C37 1.388(3) . ? C32 C33 1.397(3) . ? C32 B1 1.659(3) . ? C33 C34 1.394(3) . ? C33 H33 0.9300 . ? C34 C35 1.367(4) . ? C34 H34 0.9300 . ? C35 C36 1.366(4) . ? C35 H35 0.9300 . ? C36 C37 1.403(3) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C43 1.390(3) . ? C38 C39 1.401(3) . ? C38 B2 1.645(3) . ? C39 C40 1.388(3) . ? C39 H39 0.9300 . ? C40 C41 1.368(3) . ? C40 H40 0.9300 . ? C41 C42 1.378(3) . ? C41 H41 0.9300 . ? C42 C43 1.391(3) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 C49 1.380(3) . ? C44 C45 1.406(3) . ? C44 B2 1.654(3) . ? C45 C46 1.393(4) . ? C45 H45 0.9300 . ? C46 C47 1.374(4) . ? C46 H46 0.9300 . ? C47 C48 1.353(4) . ? C47 H47 0.9300 . ? C48 C49 1.395(3) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C50 C55 1.394(3) . ? C50 C51 1.403(3) . ? C50 B2 1.650(3) . ? C51 C52 1.379(3) . ? C51 H51 0.9300 . ? C52 C53 1.383(3) . ? C52 H52 0.9300 . ? C53 C54 1.364(3) . ? C53 H53 0.9300 . ? C54 C55 1.392(3) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C56 C61 1.380(4) . ? C56 C57 1.402(4) . ? C56 B2 1.644(3) . ? C57 C58 1.387(5) . ? C57 H57 0.9300 . ? C58 C59 1.353(7) . ? C58 H58 0.9300 . ? C59 C60 1.352(7) . ? C59 H59 0.9300 . ? C60 C61 1.408(5) . ? C60 H60 0.9300 . ? C61 H61 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N1 87.26(8) . . ? N2 Co1 P2 88.08(6) . . ? N1 Co1 P2 173.03(5) . . ? N2 Co1 P1 100.14(6) . . ? N1 Co1 P1 89.40(5) . . ? P2 Co1 P1 96.52(2) . . ? N2 Co1 S2 172.96(6) . . ? N1 Co1 S2 90.36(6) . . ? P2 Co1 S2 93.66(3) . . ? P1 Co1 S2 86.44(3) . . ? N2 Co1 S1 97.19(6) . . ? N1 Co1 S1 88.48(5) . . ? P2 Co1 S1 86.96(2) . . ? P1 Co1 S1 162.42(2) . . ? S2 Co1 S1 76.12(3) . . ? C11 S1 Co1 85.59(7) . . ? C11 S2 Co1 87.57(8) . . ? C1 P1 C2 104.84(12) . . ? C1 P1 C3 104.80(12) . . ? C2 P1 C3 101.98(10) . . ? C1 P1 Co1 119.66(9) . . ? C2 P1 Co1 115.80(8) . . ? C3 P1 Co1 107.85(8) . . ? C6 P2 C7 103.24(14) . . ? C6 P2 C8 103.39(15) . . ? C7 P2 C8 100.84(12) . . ? C6 P2 Co1 118.17(10) . . ? C7 P2 Co1 118.56(9) . . ? C8 P2 Co1 110.32(9) . . ? C5 N1 Co1 119.83(13) . . ? C5 N1 H1A 107.4 . . ? Co1 N1 H1A 107.4 . . ? C5 N1 H1B 107.4 . . ? Co1 N1 H1B 107.4 . . ? H1A N1 H1B 106.9 . . ? C10 N2 Co1 122.31(16) . . ? C10 N2 H2A 106.8 . . ? Co1 N2 H2A 106.8 . . ? C10 N2 H2B 106.8 . . ? Co1 N2 H2B 106.8 . . ? H2A N2 H2B 106.6 . . ? C11 N3 C12 119.9(3) . . ? C11 N3 C13 121.0(2) . . ? C12 N3 C13 119.1(2) . . ? P1 C1 H1C 109.5 . . ? P1 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? P1 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? P1 C2 H2C 109.5 . . ? P1 C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? P1 C2 H2E 109.5 . . ? H2C C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? C4 C3 P1 116.34(17) . . ? C4 C3 H3A 108.2 . . ? P1 C3 H3A 108.2 . . ? C4 C3 H3B 108.2 . . ? P1 C3 H3B 108.2 . . ? H3A C3 H3B 107.4 . . ? C5 C4 C3 116.03(19) . . ? C5 C4 H4A 108.3 . . ? C3 C4 H4A 108.3 . . ? C5 C4 H4B 108.3 . . ? C3 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? N1 C5 C4 113.23(19) . . ? N1 C5 H5A 108.9 . . ? C4 C5 H5A 108.9 . . ? N1 C5 H5B 108.9 . . ? C4 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P2 C7 H7A 109.5 . . ? P2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 P2 114.59(18) . . ? C9 C8 H8A 108.6 . . ? P2 C8 H8A 108.6 . . ? C9 C8 H8B 108.6 . . ? P2 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C8 114.8(2) . . ? C10 C9 H9A 108.6 . . ? C8 C9 H9A 108.6 . . ? C10 C9 H9B 108.6 . . ? C8 C9 H9B 108.6 . . ? H9A C9 H9B 107.5 . . ? N2 C10 C9 112.58(19) . . ? N2 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? N2 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? N3 C11 S2 123.5(2) . . ? N3 C11 S1 125.8(2) . . ? S2 C11 S1 110.73(12) . . ? N3 C12 H12A 109.5 . . ? N3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 113.72(18) . . ? C19 C14 B1 125.63(18) . . ? C15 C14 B1 120.59(17) . . ? C16 C15 C14 123.5(2) . . ? C16 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? C17 C16 C15 120.4(2) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 118.4(2) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? C17 C18 C19 120.6(2) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C14 C19 C18 123.4(2) . . ? C14 C19 H19 118.3 . . ? C18 C19 H19 118.3 . . ? C25 C20 C21 114.13(18) . . ? C25 C20 B1 123.28(17) . . ? C21 C20 B1 122.57(16) . . ? C22 C21 C20 123.53(18) . . ? C22 C21 H21 118.2 . . ? C20 C21 H21 118.2 . . ? C23 C22 C21 119.7(2) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 119.1(2) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C23 C24 C25 120.60(19) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C24 C25 C20 122.88(19) . . ? C24 C25 H25 118.6 . . ? C20 C25 H25 118.6 . . ? C31 C26 C27 114.62(18) . . ? C31 C26 B1 123.89(16) . . ? C27 C26 B1 121.46(17) . . ? C28 C27 C26 122.8(2) . . ? C28 C27 H27 118.6 . . ? C26 C27 H27 118.6 . . ? C29 C28 C27 120.8(2) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 118.5(2) . . ? C28 C29 H29 120.8 . . ? C30 C29 H29 120.8 . . ? C29 C30 C31 120.2(2) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C30 C31 C26 123.12(19) . . ? C30 C31 H31 118.4 . . ? C26 C31 H31 118.4 . . ? C37 C32 C33 114.99(18) . . ? C37 C32 B1 124.25(18) . . ? C33 C32 B1 120.75(17) . . ? C34 C33 C32 123.2(2) . . ? C34 C33 H33 118.4 . . ? C32 C33 H33 118.4 . . ? C35 C34 C33 120.0(2) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C36 C35 C34 118.9(2) . . ? C36 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? C35 C36 C37 120.9(2) . . ? C35 C36 H36 119.5 . . ? C37 C36 H36 119.5 . . ? C32 C37 C36 122.0(2) . . ? C32 C37 H37 119.0 . . ? C36 C37 H37 119.0 . . ? C43 C38 C39 114.63(18) . . ? C43 C38 B2 123.07(18) . . ? C39 C38 B2 122.11(18) . . ? C40 C39 C38 122.9(2) . . ? C40 C39 H39 118.5 . . ? C38 C39 H39 118.5 . . ? C41 C40 C39 120.2(2) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 119.0(2) . . ? C40 C41 H41 120.5 . . ? C42 C41 H41 120.5 . . ? C41 C42 C43 120.0(2) . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C38 C43 C42 123.1(2) . . ? C38 C43 H43 118.4 . . ? C42 C43 H43 118.4 . . ? C49 C44 C45 113.3(2) . . ? C49 C44 B2 125.36(19) . . ? C45 C44 B2 121.15(19) . . ? C46 C45 C44 123.6(2) . . ? C46 C45 H45 118.2 . . ? C44 C45 H45 118.2 . . ? C47 C46 C45 119.9(3) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C48 C47 C46 118.4(2) . . ? C48 C47 H47 120.8 . . ? C46 C47 H47 120.8 . . ? C47 C48 C49 120.9(2) . . ? C47 C48 H48 119.6 . . ? C49 C48 H48 119.6 . . ? C44 C49 C48 123.7(2) . . ? C44 C49 H49 118.1 . . ? C48 C49 H49 118.1 . . ? C55 C50 C51 113.75(19) . . ? C55 C50 B2 123.56(18) . . ? C51 C50 B2 122.48(17) . . ? C52 C51 C50 123.77(19) . . ? C52 C51 H51 118.1 . . ? C50 C51 H51 118.1 . . ? C51 C52 C53 120.2(2) . . ? C51 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? C54 C53 C52 118.2(2) . . ? C54 C53 H53 120.9 . . ? C52 C53 H53 120.9 . . ? C53 C54 C55 121.0(2) . . ? C53 C54 H54 119.5 . . ? C55 C54 H54 119.5 . . ? C54 C55 C50 123.0(2) . . ? C54 C55 H55 118.5 . . ? C50 C55 H55 118.5 . . ? C61 C56 C57 115.0(3) . . ? C61 C56 B2 125.1(2) . . ? C57 C56 B2 119.9(2) . . ? C58 C57 C56 123.0(4) . . ? C58 C57 H57 118.5 . . ? C56 C57 H57 118.5 . . ? C59 C58 C57 119.8(5) . . ? C59 C58 H58 120.1 . . ? C57 C58 H58 120.1 . . ? C60 C59 C58 119.8(4) . . ? C60 C59 H59 120.1 . . ? C58 C59 H59 120.1 . . ? C59 C60 C61 120.7(4) . . ? C59 C60 H60 119.7 . . ? C61 C60 H60 119.7 . . ? C56 C61 C60 121.7(4) . . ? C56 C61 H61 119.2 . . ? C60 C61 H61 119.2 . . ? C20 B1 C26 109.53(14) . . ? C20 B1 C32 109.85(15) . . ? C26 B1 C32 108.99(15) . . ? C20 B1 C14 112.38(15) . . ? C26 B1 C14 107.00(15) . . ? C32 B1 C14 109.01(14) . . ? C56 B2 C38 109.32(17) . . ? C56 B2 C50 109.11(16) . . ? C38 B2 C50 107.45(17) . . ? C56 B2 C44 107.29(17) . . ? C38 B2 C44 109.99(16) . . ? C50 B2 C44 113.63(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 N2 Co1 S1 C11 177.58(9) . . . . ? N1 Co1 S1 C11 90.53(9) . . . . ? P2 Co1 S1 C11 -94.74(7) . . . . ? P1 Co1 S1 C11 7.32(11) . . . . ? S2 Co1 S1 C11 -0.21(7) . . . . ? N1 Co1 S2 C11 -88.13(8) . . . . ? P2 Co1 S2 C11 86.17(7) . . . . ? P1 Co1 S2 C11 -177.51(7) . . . . ? S1 Co1 S2 C11 0.21(7) . . . . ? N2 Co1 P1 C1 9.86(12) . . . . ? N1 Co1 P1 C1 96.97(12) . . . . ? P2 Co1 P1 C1 -79.35(11) . . . . ? S2 Co1 P1 C1 -172.64(11) . . . . ? S1 Co1 P1 C1 -179.97(12) . . . . ? N2 Co1 P1 C2 136.92(10) . . . . ? N1 Co1 P1 C2 -135.97(10) . . . . ? P2 Co1 P1 C2 47.71(9) . . . . ? S2 Co1 P1 C2 -45.58(9) . . . . ? S1 Co1 P1 C2 -52.91(12) . . . . ? N2 Co1 P1 C3 -109.63(11) . . . . ? N1 Co1 P1 C3 -22.52(10) . . . . ? P2 Co1 P1 C3 161.16(9) . . . . ? S2 Co1 P1 C3 67.87(9) . . . . ? S1 Co1 P1 C3 60.55(12) . . . . ? N2 Co1 P2 C6 159.79(14) . . . . ? P1 Co1 P2 C6 -100.22(13) . . . . ? S2 Co1 P2 C6 -13.39(13) . . . . ? S1 Co1 P2 C6 62.48(13) . . . . ? N2 Co1 P2 C7 -74.25(11) . . . . ? P1 Co1 P2 C7 25.74(10) . . . . ? S2 Co1 P2 C7 112.58(10) . . . . ? S1 Co1 P2 C7 -171.55(10) . . . . ? N2 Co1 P2 C8 41.21(11) . . . . ? P1 Co1 P2 C8 141.20(10) . . . . ? S2 Co1 P2 C8 -131.96(10) . . . . ? S1 Co1 P2 C8 -56.09(10) . . . . ? N2 Co1 N1 C5 61.94(17) . . . . ? P1 Co1 N1 C5 -38.25(16) . . . . ? S2 Co1 N1 C5 -124.68(16) . . . . ? S1 Co1 N1 C5 159.21(16) . . . . ? N1 Co1 N2 C10 120.45(18) . . . . ? P2 Co1 N2 C10 -54.36(17) . . . . ? P1 Co1 N2 C10 -150.65(17) . . . . ? S1 Co1 N2 C10 32.33(18) . . . . ? C1 P1 C3 C4 -66.3(2) . . . . ? C2 P1 C3 C4 -175.35(19) . . . . ? Co1 P1 C3 C4 62.2(2) . . . . ? P1 C3 C4 C5 -35.2(3) . . . . ? Co1 N1 C5 C4 78.8(2) . . . . ? C3 C4 C5 N1 -35.5(3) . . . . ? C6 P2 C8 C9 179.0(2) . . . . ? C7 P2 C8 C9 72.4(2) . . . . ? Co1 P2 C8 C9 -53.7(2) . . . . ? P2 C8 C9 C10 61.9(3) . . . . ? Co1 N2 C10 C9 70.4(3) . . . . ? C8 C9 C10 N2 -66.4(3) . . . . ? C12 N3 C11 S2 178.6(2) . . . . ? C13 N3 C11 S2 -0.1(3) . . . . ? C12 N3 C11 S1 0.6(3) . . . . ? C13 N3 C11 S1 -178.0(2) . . . . ? Co1 S2 C11 N3 -178.51(19) . . . . ? Co1 S2 C11 S1 -0.30(10) . . . . ? Co1 S1 C11 N3 178.4(2) . . . . ? Co1 S1 C11 S2 0.29(10) . . . . ? C19 C14 C15 C16 -0.4(3) . . . . ? B1 C14 C15 C16 176.9(2) . . . . ? C14 C15 C16 C17 0.1(4) . . . . ? C15 C16 C17 C18 0.1(4) . . . . ? C16 C17 C18 C19 0.0(4) . . . . ? C15 C14 C19 C18 0.5(3) . . . . ? B1 C14 C19 C18 -176.6(2) . . . . ? C17 C18 C19 C14 -0.3(4) . . . . ? C25 C20 C21 C22 -3.0(3) . . . . ? B1 C20 C21 C22 178.54(18) . . . . ? C20 C21 C22 C23 2.3(3) . . . . ? C21 C22 C23 C24 0.3(3) . . . . ? C22 C23 C24 C25 -2.0(3) . . . . ? C23 C24 C25 C20 1.1(3) . . . . ? C21 C20 C25 C24 1.3(3) . . . . ? B1 C20 C25 C24 179.75(18) . . . . ? C31 C26 C27 C28 -2.3(3) . . . . ? B1 C26 C27 C28 179.7(2) . . . . ? C26 C27 C28 C29 1.4(4) . . . . ? C27 C28 C29 C30 0.5(4) . . . . ? C28 C29 C30 C31 -1.1(3) . . . . ? C29 C30 C31 C26 0.0(3) . . . . ? C27 C26 C31 C30 1.7(3) . . . . ? B1 C26 C31 C30 179.55(18) . . . . ? C37 C32 C33 C34 -0.4(3) . . . . ? B1 C32 C33 C34 -179.32(19) . . . . ? C32 C33 C34 C35 0.3(4) . . . . ? C33 C34 C35 C36 -0.3(4) . . . . ? C34 C35 C36 C37 0.5(4) . . . . ? C33 C32 C37 C36 0.6(3) . . . . ? B1 C32 C37 C36 179.4(2) . . . . ? C35 C36 C37 C32 -0.6(4) . . . . ? C43 C38 C39 C40 -2.7(4) . . . . ? B2 C38 C39 C40 172.4(2) . . . . ? C38 C39 C40 C41 -0.4(4) . . . . ? C39 C40 C41 C42 2.6(4) . . . . ? C40 C41 C42 C43 -1.6(4) . . . . ? C39 C38 C43 C42 3.8(3) . . . . ? B2 C38 C43 C42 -171.2(2) . . . . ? C41 C42 C43 C38 -1.8(4) . . . . ? C49 C44 C45 C46 -1.6(4) . . . . ? B2 C44 C45 C46 -177.2(3) . . . . ? C44 C45 C46 C47 -1.9(5) . . . . ? C45 C46 C47 C48 4.3(5) . . . . ? C46 C47 C48 C49 -3.2(5) . . . . ? C45 C44 C49 C48 2.8(4) . . . . ? B2 C44 C49 C48 178.1(2) . . . . ? C47 C48 C49 C44 -0.5(5) . . . . ? C55 C50 C51 C52 -2.3(3) . . . . ? B2 C50 C51 C52 -177.07(19) . . . . ? C50 C51 C52 C53 1.4(3) . . . . ? C51 C52 C53 C54 0.4(3) . . . . ? C52 C53 C54 C55 -1.2(4) . . . . ? C53 C54 C55 C50 0.3(4) . . . . ? C51 C50 C55 C54 1.4(3) . . . . ? B2 C50 C55 C54 176.2(2) . . . . ? C61 C56 C57 C58 0.5(5) . . . . ? B2 C56 C57 C58 -179.0(3) . . . . ? C56 C57 C58 C59 -1.1(6) . . . . ? C57 C58 C59 C60 1.1(6) . . . . ? C58 C59 C60 C61 -0.6(6) . . . . ? C57 C56 C61 C60 0.0(4) . . . . ? B2 C56 C61 C60 179.5(2) . . . . ? C59 C60 C61 C56 0.0(5) . . . . ? C25 C20 B1 C26 6.7(2) . . . . ? C21 C20 B1 C26 -174.98(16) . . . . ? C25 C20 B1 C32 -112.99(18) . . . . ? C21 C20 B1 C32 65.3(2) . . . . ? C25 C20 B1 C14 125.46(18) . . . . ? C21 C20 B1 C14 -56.2(2) . . . . ? C31 C26 B1 C20 -90.7(2) . . . . ? C27 C26 B1 C20 87.1(2) . . . . ? C31 C26 B1 C32 29.5(2) . . . . ? C27 C26 B1 C32 -152.73(19) . . . . ? C31 C26 B1 C14 147.26(18) . . . . ? C27 C26 B1 C14 -35.0(2) . . . . ? C37 C32 B1 C20 -2.3(3) . . . . ? C33 C32 B1 C20 176.44(17) . . . . ? C37 C32 B1 C26 -122.3(2) . . . . ? C33 C32 B1 C26 56.4(2) . . . . ? C37 C32 B1 C14 121.2(2) . . . . ? C33 C32 B1 C14 -60.0(2) . . . . ? C19 C14 B1 C20 13.9(3) . . . . ? C15 C14 B1 C20 -163.09(17) . . . . ? C19 C14 B1 C26 134.11(19) . . . . ? C15 C14 B1 C26 -42.8(2) . . . . ? C19 C14 B1 C32 -108.2(2) . . . . ? C15 C14 B1 C32 74.9(2) . . . . ? C61 C56 B2 C38 5.6(3) . . . . ? C57 C56 B2 C38 -174.9(2) . . . . ? C61 C56 B2 C50 -111.6(2) . . . . ? C57 C56 B2 C50 67.8(3) . . . . ? C61 C56 B2 C44 124.8(2) . . . . ? C57 C56 B2 C44 -55.7(3) . . . . ? C43 C38 B2 C56 83.1(2) . . . . ? C39 C38 B2 C56 -91.5(2) . . . . ? C43 C38 B2 C50 -158.58(19) . . . . ? C39 C38 B2 C50 26.8(3) . . . . ? C43 C38 B2 C44 -34.4(3) . . . . ? C39 C38 B2 C44 150.9(2) . . . . ? C55 C50 B2 C56 4.2(3) . . . . ? C51 C50 B2 C56 178.49(19) . . . . ? C55 C50 B2 C38 -114.2(2) . . . . ? C51 C50 B2 C38 60.1(2) . . . . ? C55 C50 B2 C44 123.9(2) . . . . ? C51 C50 B2 C44 -61.8(2) . . . . ? C49 C44 B2 C56 152.4(2) . . . . ? C45 C44 B2 C56 -32.6(3) . . . . ? C49 C44 B2 C38 -88.8(3) . . . . ? C45 C44 B2 C38 86.2(3) . . . . ? C49 C44 B2 C50 31.7(3) . . . . ? C45 C44 B2 C50 -153.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.532 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.053 #==END #============================================================================== data_transPN _database_code_depnum_ccdc_archive 'CCDC 618536' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans(P,N)-(pentane-2,4-dionato)bis((3-aminopropyl) dimethylphosphine)cobalt(III) Bis(hexafluorophospate) Hemi(diethyl ether) Solvate ; _chemical_name_common ; trans(P,N)-(pentane-2,4-dionato)bis((3-aminopropyl) dimethylphosphine)cobalt(iii) Bis(hexafluorophospate) Hemi(diethyl ether) Solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C15 H35 Co N2 O2 P2 2+, 2(F6 P 1-), 0.5(C4 H10 O)' _chemical_formula_sum 'C17 H40 Co F12 N2 O2.50 P4' _chemical_formula_weight 723.32 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' 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 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 16.765(5) _cell_length_b 11.701(3) _cell_length_c 31.311(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.258(12) _cell_angle_gamma 90.00 _cell_volume 6125(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26557 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.4 _exptl_crystal_description orange _exptl_crystal_colour octahedron _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2968 _exptl_absorpt_coefficient_mu 0.863 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8131 _exptl_absorpt_correction_T_max 0.8463 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53373 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.46 _reflns_number_total 13967 _reflns_number_gt 9602 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'CrystalStructure 3.7.0' _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ORTEP-3 for Win' _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^)+(0.0871P)^2^+4.6916P] 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 13967 _refine_ls_number_parameters 754 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1751 _refine_ls_wR_factor_gt 0.1589 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Co1 Co 0.07413(3) 0.24709(4) 0.626297(14) 0.03855(13) Uani 1 1 d . . . Co2 Co 0.42047(3) 0.26296(4) 0.377622(13) 0.03650(12) Uani 1 1 d . . . P1 P 0.03593(6) 0.42825(8) 0.61809(3) 0.0522(2) Uani 1 1 d . . . P2 P 0.09141(6) 0.21676(9) 0.55700(3) 0.0518(2) Uani 1 1 d . . . P3 P 0.46635(6) 0.44071(7) 0.37830(3) 0.0424(2) Uani 1 1 d . . . P4 P 0.43082(6) 0.24030(8) 0.44870(3) 0.0445(2) Uani 1 1 d . . . P5 P 0.41556(6) 0.16190(8) 0.60644(3) 0.0521(2) Uani 1 1 d . . . P6 P 0.21183(7) 0.00181(12) 0.75289(4) 0.0688(3) Uani 1 1 d . . . P7 P 0.75086(7) 0.34850(11) 0.49283(4) 0.0621(3) Uani 1 1 d . . . P8 P 0.08150(6) 0.17470(9) 0.39226(4) 0.0541(3) Uani 1 1 d . . . F1 F 0.46447(18) 0.0713(3) 0.63449(10) 0.0956(9) Uani 1 1 d . . . F2 F 0.4867(2) 0.1812(4) 0.57764(13) 0.1434(16) Uani 1 1 d . . . F3 F 0.4464(2) 0.2615(2) 0.63652(11) 0.1052(11) Uani 1 1 d . . . F4 F 0.3831(3) 0.0644(3) 0.57537(12) 0.1322(14) Uani 1 1 d . . . F5 F 0.34217(17) 0.1445(3) 0.63400(11) 0.1015(10) Uani 1 1 d . . . F6 F 0.3638(2) 0.2516(2) 0.57721(10) 0.0965(10) Uani 1 1 d . . . F7 F 0.2139(3) 0.1003(3) 0.78675(11) 0.1372(14) Uani 1 1 d . . . F8 F 0.1963(2) -0.0860(3) 0.78949(10) 0.1081(10) Uani 1 1 d . . . F9 F 0.11905(18) 0.0173(3) 0.74222(11) 0.1094(11) Uani 1 1 d . . . F10 F 0.30415(18) -0.0136(4) 0.76259(13) 0.1358(15) Uani 1 1 d . . . F11 F 0.2262(2) 0.0930(4) 0.71628(10) 0.1236(13) Uani 1 1 d . . . F12 F 0.2094(2) -0.0974(4) 0.71896(11) 0.1284(13) Uani 1 1 d . . . F13 F 0.84123(18) 0.3465(4) 0.48222(12) 0.1335(15) Uani 1 1 d . . . F18 F 0.66011(18) 0.3634(3) 0.50262(11) 0.1149(12) Uani 1 1 d . . . F222 F 0.1485(9) 0.1405(14) 0.4268(5) 0.190(6) Uiso 0.50 1 d P . . F141 F 0.7213(7) 0.2472(10) 0.4634(5) 0.159(5) Uani 0.50 1 d P . . F142 F 0.7261(8) 0.3052(11) 0.4481(4) 0.138(4) Uiso 0.50 1 d P . . F151 F 0.7636(7) 0.2798(11) 0.5339(3) 0.165(4) Uani 0.50 1 d P . . F152 F 0.7618(7) 0.2211(11) 0.5074(4) 0.151(4) Uiso 0.50 1 d P . . F161 F 0.7369(4) 0.4306(10) 0.4513(2) 0.116(3) Uani 0.50 1 d P . . F162 F 0.7417(6) 0.4695(9) 0.4750(4) 0.130(4) Uiso 0.50 1 d P . . F171 F 0.7718(5) 0.4593(8) 0.5222(3) 0.117(3) Uani 0.50 1 d P . . F172 F 0.7760(6) 0.3851(10) 0.5383(3) 0.120(3) Uiso 0.50 1 d P . . F191 F 0.0003(5) 0.1823(13) 0.3655(4) 0.146(5) Uani 0.50 1 d P . . F192 F 0.1115(6) 0.2676(9) 0.3628(4) 0.127(5) Uani 0.50 1 d P . . F201 F 0.0226(6) 0.2293(10) 0.4200(4) 0.139(4) Uani 0.50 1 d P . . F202 F 0.0436(10) 0.0857(14) 0.3656(5) 0.192(7) Uani 0.50 1 d P . . F211 F 0.0659(19) 0.2631(13) 0.3613(5) 0.304(14) Uani 0.50 1 d P . . F212 F 0.1570(6) 0.1449(10) 0.3706(4) 0.134(3) Uiso 0.50 1 d P . . F221 F 0.0536(8) 0.0687(12) 0.4192(5) 0.143(5) Uiso 0.50 1 d P . . F231 F 0.1112(13) 0.0821(9) 0.3614(3) 0.181(6) Uani 0.50 1 d P . . F232 F 0.0831(11) 0.2773(7) 0.4208(3) 0.190(6) Uani 0.50 1 d P . . F241 F 0.1594(5) 0.2006(14) 0.4204(3) 0.163(6) Uani 0.50 1 d P . . F242 F 0.0611(15) 0.0881(14) 0.4243(6) 0.289(14) Uani 0.50 1 d P . . O1 O 0.06477(16) 0.2596(2) 0.68746(8) 0.0506(6) Uani 1 1 d . . . O2 O -0.03579(15) 0.2106(2) 0.61434(8) 0.0532(6) Uani 1 1 d . . . O3 O 0.40276(15) 0.2646(2) 0.31607(7) 0.0495(6) Uani 1 1 d . . . O4 O 0.52892(14) 0.2160(2) 0.37649(8) 0.0493(6) Uani 1 1 d . . . O5 O 0.6756(3) 0.4853(4) 0.20993(14) 0.1299(17) Uani 1 1 d . . . N1 N 0.18739(17) 0.2820(3) 0.64304(10) 0.0531(7) Uani 1 1 d . . . H1A H 0.1925 0.2763 0.6718 0.064 Uiso 1 1 calc R . . H1B H 0.2155 0.2234 0.6331 0.064 Uiso 1 1 calc R . . N2 N 0.09405(18) 0.0760(2) 0.63807(10) 0.0504(7) Uani 1 1 d . . . H2A H 0.1014 0.0700 0.6667 0.060 Uiso 1 1 calc R . . H2B H 0.0471 0.0415 0.6306 0.060 Uiso 1 1 calc R . . N3 N 0.30753(16) 0.3134(2) 0.37397(9) 0.0462(7) Uani 1 1 d . . . H3A H 0.2929 0.3192 0.3458 0.055 Uiso 1 1 calc R . . H3B H 0.2797 0.2542 0.3836 0.055 Uiso 1 1 calc R . . N4 N 0.39129(18) 0.0918(2) 0.37308(10) 0.0488(7) Uani 1 1 d . . . H4A H 0.3767 0.0799 0.3452 0.059 Uiso 1 1 calc R . . H4B H 0.4378 0.0543 0.3784 0.059 Uiso 1 1 calc R . . C1 C -0.0370(4) 0.4577(4) 0.57394(19) 0.1009(19) Uani 1 1 d . . . H1C H -0.0173 0.4307 0.5478 0.121 Uiso 1 1 calc R . . H1D H -0.0463 0.5385 0.5720 0.121 Uiso 1 1 calc R . . H1E H -0.0863 0.4194 0.5787 0.121 Uiso 1 1 calc R . . C2 C -0.0085(3) 0.4833(4) 0.66461(17) 0.0834(15) Uani 1 1 d . . . H2C H 0.0271 0.4702 0.6896 0.100 Uiso 1 1 calc R . . H2D H -0.0584 0.4451 0.6678 0.100 Uiso 1 1 calc R . . H2E H -0.0177 0.5638 0.6612 0.100 Uiso 1 1 calc R . . C3 C 0.1183(3) 0.5255(4) 0.61160(15) 0.0702(12) Uani 1 1 d . . . H3C H 0.1332 0.5218 0.5823 0.084 Uiso 1 1 calc R . . H3D H 0.1011 0.6030 0.6170 0.084 Uiso 1 1 calc R . . C4 C 0.1914(3) 0.4972(4) 0.64204(18) 0.0798(14) Uani 1 1 d . . . H4C H 0.2300 0.5586 0.6407 0.096 Uiso 1 1 calc R . . H4D H 0.1749 0.4945 0.6711 0.096 Uiso 1 1 calc R . . C5 C 0.2319(3) 0.3864(4) 0.63272(16) 0.0699(12) Uani 1 1 d . . . H5A H 0.2413 0.3847 0.6025 0.084 Uiso 1 1 calc R . . H5B H 0.2837 0.3848 0.6488 0.084 Uiso 1 1 calc R . . C6 C 0.0018(3) 0.1660(4) 0.52763(14) 0.0722(12) Uani 1 1 d . . . H6A H -0.0220 0.1068 0.5437 0.087 Uiso 1 1 calc R . . H6B H 0.0151 0.1360 0.5005 0.087 Uiso 1 1 calc R . . H6C H -0.0353 0.2280 0.5230 0.087 Uiso 1 1 calc R . . C7 C 0.1309(4) 0.3274(4) 0.52384(14) 0.0981(19) Uani 1 1 d . . . H7A H 0.1793 0.3577 0.5378 0.118 Uiso 1 1 calc R . . H7B H 0.0922 0.3876 0.5195 0.118 Uiso 1 1 calc R . . H7C H 0.1421 0.2955 0.4967 0.118 Uiso 1 1 calc R . . C8 C 0.1641(3) 0.1045(4) 0.55055(14) 0.0742(13) Uani 1 1 d . . . H8A H 0.1657 0.0892 0.5202 0.089 Uiso 1 1 calc R . . H8B H 0.2163 0.1330 0.5609 0.089 Uiso 1 1 calc R . . C9 C 0.1496(3) -0.0080(4) 0.57318(14) 0.0724(13) Uani 1 1 d . . . H9A H 0.0966 -0.0355 0.5639 0.087 Uiso 1 1 calc R . . H9B H 0.1879 -0.0640 0.5645 0.087 Uiso 1 1 calc R . . C10 C 0.1565(2) 0.0002(3) 0.62095(13) 0.0594(10) Uani 1 1 d . . . H10A H 0.2091 0.0295 0.6303 0.071 Uiso 1 1 calc R . . H10B H 0.1519 -0.0758 0.6329 0.071 Uiso 1 1 calc R . . C11 C 0.5625(2) 0.4611(3) 0.40722(15) 0.0647(11) Uani 1 1 d . . . H11A H 0.6000 0.4068 0.3974 0.078 Uiso 1 1 calc R . . H11B H 0.5574 0.4501 0.4373 0.078 Uiso 1 1 calc R . . H11C H 0.5812 0.5372 0.4024 0.078 Uiso 1 1 calc R . . C12 C 0.4818(3) 0.4898(3) 0.32488(13) 0.0612(10) Uani 1 1 d . . . H12A H 0.4329 0.4820 0.3071 0.073 Uiso 1 1 calc R . . H12B H 0.5229 0.4450 0.3133 0.073 Uiso 1 1 calc R . . H12C H 0.4976 0.5687 0.3259 0.073 Uiso 1 1 calc R . . C13 C 0.3990(2) 0.5451(3) 0.39850(12) 0.0536(9) Uani 1 1 d . . . H13A H 0.4018 0.5405 0.4295 0.064 Uiso 1 1 calc R . . H13B H 0.4162 0.6211 0.3908 0.064 Uiso 1 1 calc R . . C14 C 0.3125(2) 0.5275(3) 0.38093(14) 0.0596(10) Uani 1 1 d . . . H14A H 0.2808 0.5909 0.3902 0.072 Uiso 1 1 calc R . . H14B H 0.3107 0.5298 0.3499 0.072 Uiso 1 1 calc R . . C15 C 0.2746(2) 0.4179(3) 0.39418(13) 0.0576(10) Uani 1 1 d . . . H15A H 0.2824 0.4106 0.4251 0.069 Uiso 1 1 calc R . . H15B H 0.2175 0.4218 0.3866 0.069 Uiso 1 1 calc R . . C16 C 0.4271(3) 0.3587(3) 0.48632(12) 0.0726(13) Uani 1 1 d . . . H16A H 0.3801 0.4037 0.4792 0.087 Uiso 1 1 calc R . . H16B H 0.4738 0.4056 0.4847 0.087 Uiso 1 1 calc R . . H16C H 0.4255 0.3293 0.5149 0.087 Uiso 1 1 calc R . . C17 C 0.5216(2) 0.1663(4) 0.46684(13) 0.0631(11) Uani 1 1 d . . . H17A H 0.5670 0.2100 0.4594 0.076 Uiso 1 1 calc R . . H17B H 0.5225 0.0926 0.4534 0.076 Uiso 1 1 calc R . . H17C H 0.5236 0.1569 0.4974 0.076 Uiso 1 1 calc R . . C18 C 0.3507(3) 0.1482(4) 0.46454(13) 0.0613(10) Uani 1 1 d . . . H18A H 0.3554 0.1402 0.4955 0.074 Uiso 1 1 calc R . . H18B H 0.2998 0.1849 0.4566 0.074 Uiso 1 1 calc R . . C19 C 0.3502(3) 0.0293(4) 0.44449(14) 0.0670(11) Uani 1 1 d . . . H19A H 0.4021 -0.0056 0.4511 0.080 Uiso 1 1 calc R . . H19B H 0.3108 -0.0171 0.4576 0.080 Uiso 1 1 calc R . . C20 C 0.3319(2) 0.0277(3) 0.39682(13) 0.0580(10) Uani 1 1 d . . . H20A H 0.3304 -0.0510 0.3871 0.070 Uiso 1 1 calc R . . H20B H 0.2793 0.0605 0.3901 0.070 Uiso 1 1 calc R . . C21 C 0.0088(4) 0.2498(4) 0.75486(14) 0.0871(16) Uani 1 1 d . . . H21A H 0.0633 0.2379 0.7656 0.105 Uiso 1 1 calc R . . H21B H -0.0250 0.1952 0.7676 0.105 Uiso 1 1 calc R . . H21C H -0.0075 0.3257 0.7619 0.105 Uiso 1 1 calc R . . C22 C 0.0019(3) 0.2350(3) 0.70690(14) 0.0599(10) Uani 1 1 d . . . C23 C -0.0702(3) 0.1999(4) 0.68616(16) 0.0705(12) Uani 1 1 d . . . H23 H -0.1109 0.1789 0.7032 0.085 Uiso 1 1 calc R . . C24 C -0.0864(2) 0.1939(3) 0.64222(16) 0.0603(10) Uani 1 1 d . . . C25 C -0.1692(2) 0.1681(4) 0.62402(19) 0.0859(16) Uani 1 1 d . . . H25A H -0.1787 0.2058 0.5969 0.103 Uiso 1 1 calc R . . H25B H -0.2070 0.1947 0.6433 0.103 Uiso 1 1 calc R . . H25C H -0.1752 0.0870 0.6201 0.103 Uiso 1 1 calc R . . C26 C 0.4212(3) 0.2378(5) 0.24335(13) 0.0872(16) Uani 1 1 d . . . H26A H 0.3944 0.3096 0.2383 0.105 Uiso 1 1 calc R . . H26B H 0.3843 0.1764 0.2369 0.105 Uiso 1 1 calc R . . H26C H 0.4650 0.2320 0.2253 0.105 Uiso 1 1 calc R . . C27 C 0.4525(3) 0.2306(3) 0.28944(13) 0.0614(11) Uani 1 1 d . . . C28 C 0.5287(3) 0.1919(4) 0.30131(14) 0.0677(12) Uani 1 1 d . . . H28 H 0.5587 0.1640 0.2798 0.081 Uiso 1 1 calc R . . C29 C 0.5641(2) 0.1910(3) 0.34270(14) 0.0574(10) Uani 1 1 d . . . C30 C 0.6508(3) 0.1593(4) 0.35136(18) 0.0808(15) Uani 1 1 d . . . H30A H 0.6605 0.1365 0.3807 0.097 Uiso 1 1 calc R . . H30B H 0.6837 0.2240 0.3458 0.097 Uiso 1 1 calc R . . H30C H 0.6636 0.0971 0.3330 0.097 Uiso 1 1 calc R . . C31 C 0.6380(5) 0.2896(6) 0.1963(3) 0.146(3) Uani 1 1 d . . . H31A H 0.6028 0.2308 0.2051 0.175 Uiso 1 1 calc R . . H31B H 0.6925 0.2647 0.2013 0.175 Uiso 1 1 calc R . . H31C H 0.6266 0.3052 0.1664 0.175 Uiso 1 1 calc R . . C32 C 0.6270(8) 0.3857(8) 0.2192(3) 0.235(7) Uani 1 1 d . . . H32A H 0.6371 0.3674 0.2493 0.282 Uiso 1 1 calc R . . H32B H 0.5711 0.4074 0.2147 0.282 Uiso 1 1 calc R . . C33 C 0.7384(6) 0.4987(9) 0.2382(3) 0.164(4) Uani 1 1 d . . . H33A H 0.7700 0.4292 0.2390 0.197 Uiso 1 1 calc R . . H33B H 0.7193 0.5097 0.2664 0.197 Uiso 1 1 calc R . . C34 C 0.7887(6) 0.5935(9) 0.2287(3) 0.190(5) Uani 1 1 d . . . H34A H 0.8314 0.6004 0.2507 0.228 Uiso 1 1 calc R . . H34B H 0.7577 0.6626 0.2274 0.228 Uiso 1 1 calc R . . H34C H 0.8107 0.5810 0.2016 0.228 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0372(2) 0.0410(2) 0.0370(2) 0.00113(18) -0.00032(18) 0.00124(18) Co2 0.0386(2) 0.0368(2) 0.0339(2) -0.00235(17) 0.00211(17) -0.00009(18) P1 0.0577(6) 0.0420(5) 0.0558(6) 0.0043(4) -0.0027(5) 0.0037(4) P2 0.0599(6) 0.0576(6) 0.0375(5) -0.0030(4) 0.0001(4) -0.0085(5) P3 0.0466(5) 0.0373(4) 0.0428(5) 0.0009(4) 0.0002(4) -0.0028(4) P4 0.0534(5) 0.0440(5) 0.0356(4) 0.0010(4) 0.0003(4) -0.0028(4) P5 0.0541(6) 0.0469(5) 0.0561(6) -0.0003(4) 0.0090(4) 0.0013(4) P6 0.0606(7) 0.0920(9) 0.0522(6) 0.0058(6) -0.0062(5) -0.0037(6) P7 0.0566(6) 0.0740(7) 0.0549(6) -0.0044(5) -0.0019(5) 0.0008(5) P8 0.0536(6) 0.0464(5) 0.0630(6) -0.0010(5) 0.0085(5) -0.0024(4) F1 0.082(2) 0.0873(19) 0.114(2) 0.0217(17) -0.0095(17) 0.0284(16) F2 0.111(3) 0.194(4) 0.134(3) 0.035(3) 0.072(2) 0.015(3) F3 0.147(3) 0.0734(19) 0.091(2) -0.0129(15) -0.021(2) -0.0300(18) F4 0.189(4) 0.084(2) 0.116(3) -0.040(2) -0.041(3) 0.005(2) F5 0.0705(18) 0.111(2) 0.127(3) 0.036(2) 0.0358(17) 0.0099(17) F6 0.122(3) 0.087(2) 0.0781(19) 0.0166(15) -0.0084(18) 0.0238(17) F7 0.206(4) 0.116(3) 0.085(2) -0.024(2) -0.018(2) -0.014(3) F8 0.110(2) 0.120(3) 0.092(2) 0.0363(19) -0.0003(18) -0.022(2) F9 0.0698(19) 0.136(3) 0.120(3) 0.009(2) -0.0065(17) 0.0098(19) F10 0.0608(19) 0.209(4) 0.135(3) 0.047(3) -0.0122(19) -0.002(2) F11 0.120(3) 0.164(3) 0.083(2) 0.053(2) -0.0214(19) -0.032(2) F12 0.139(3) 0.144(3) 0.101(3) -0.039(2) 0.007(2) 0.016(3) F13 0.0639(19) 0.223(5) 0.115(3) 0.019(3) 0.0154(18) 0.032(2) F18 0.0684(19) 0.160(3) 0.119(3) -0.018(2) 0.0260(18) -0.017(2) F141 0.152(9) 0.144(9) 0.181(11) -0.119(9) 0.021(8) -0.040(7) F151 0.227(11) 0.161(9) 0.107(6) 0.097(7) 0.004(7) 0.046(8) F161 0.071(4) 0.200(9) 0.077(5) 0.073(6) 0.001(3) 0.006(5) F171 0.115(6) 0.113(6) 0.124(6) -0.067(5) 0.014(5) -0.037(5) F191 0.085(5) 0.168(10) 0.174(10) 0.065(9) -0.072(6) -0.033(6) F192 0.111(6) 0.136(9) 0.133(8) 0.076(6) 0.001(5) -0.070(7) F201 0.109(6) 0.170(11) 0.144(8) -0.020(7) 0.063(7) 0.060(6) F202 0.187(13) 0.199(13) 0.196(12) -0.112(11) 0.062(10) -0.150(11) F211 0.64(4) 0.140(12) 0.122(10) 0.028(9) -0.053(19) 0.219(19) F231 0.335(18) 0.087(6) 0.134(7) -0.031(5) 0.102(11) 0.060(9) F232 0.39(2) 0.069(5) 0.101(7) -0.055(5) -0.050(11) 0.052(9) F241 0.073(5) 0.274(14) 0.133(7) 0.112(9) -0.056(5) -0.078(7) F242 0.51(3) 0.170(12) 0.192(14) 0.112(11) 0.088(14) -0.150(15) O1 0.0547(15) 0.0554(15) 0.0420(13) 0.0019(11) 0.0064(11) 0.0039(12) O2 0.0411(13) 0.0567(15) 0.0608(16) -0.0002(13) -0.0030(11) -0.0022(12) O3 0.0570(15) 0.0574(15) 0.0343(12) -0.0045(11) 0.0035(11) 0.0012(12) O4 0.0447(13) 0.0482(13) 0.0552(15) -0.0006(11) 0.0059(11) 0.0044(11) O5 0.178(5) 0.119(3) 0.086(3) 0.020(2) -0.030(3) -0.046(3) N1 0.0434(16) 0.0633(19) 0.0519(18) -0.0078(15) -0.0012(13) -0.0033(15) N2 0.0475(17) 0.0501(17) 0.0526(17) 0.0012(14) -0.0020(14) 0.0041(14) N3 0.0406(15) 0.0499(16) 0.0477(16) -0.0036(13) 0.0014(12) 0.0009(13) N4 0.0474(17) 0.0426(15) 0.0561(18) -0.0064(13) 0.0007(14) -0.0022(13) C1 0.109(4) 0.068(3) 0.116(5) 0.008(3) -0.053(4) 0.018(3) C2 0.100(4) 0.055(2) 0.100(4) 0.008(2) 0.039(3) 0.021(3) C3 0.085(3) 0.049(2) 0.077(3) 0.001(2) 0.010(2) -0.011(2) C4 0.073(3) 0.061(3) 0.104(4) -0.017(3) 0.000(3) -0.019(2) C5 0.053(2) 0.069(3) 0.088(3) -0.003(2) 0.006(2) -0.012(2) C6 0.076(3) 0.082(3) 0.055(2) -0.013(2) -0.017(2) -0.002(2) C7 0.164(6) 0.085(3) 0.048(3) -0.003(2) 0.028(3) -0.040(4) C8 0.067(3) 0.101(4) 0.056(2) -0.015(2) 0.011(2) 0.005(3) C9 0.078(3) 0.068(3) 0.071(3) -0.022(2) 0.001(2) 0.023(2) C10 0.051(2) 0.053(2) 0.074(3) -0.0037(19) -0.0013(19) 0.0142(18) C11 0.058(2) 0.052(2) 0.081(3) 0.004(2) -0.013(2) -0.0150(19) C12 0.081(3) 0.048(2) 0.056(2) 0.0070(18) 0.015(2) -0.008(2) C13 0.073(3) 0.0391(18) 0.049(2) -0.0029(15) 0.0055(18) 0.0026(17) C14 0.060(2) 0.053(2) 0.066(2) 0.0011(19) 0.007(2) 0.0187(19) C15 0.051(2) 0.055(2) 0.068(2) -0.0070(19) 0.0105(19) 0.0071(18) C16 0.124(4) 0.056(2) 0.0364(19) -0.0036(18) 0.002(2) -0.005(3) C17 0.060(2) 0.072(3) 0.055(2) 0.013(2) -0.0117(19) 0.003(2) C18 0.066(3) 0.070(3) 0.048(2) 0.0055(19) 0.0090(19) -0.014(2) C19 0.072(3) 0.059(2) 0.070(3) 0.014(2) 0.004(2) -0.020(2) C20 0.054(2) 0.047(2) 0.073(3) -0.0024(18) 0.0040(19) -0.0137(18) C21 0.112(4) 0.098(4) 0.055(3) 0.004(2) 0.024(3) 0.009(3) C22 0.067(3) 0.055(2) 0.060(2) 0.0073(18) 0.020(2) 0.011(2) C23 0.063(3) 0.071(3) 0.080(3) 0.004(2) 0.026(2) -0.008(2) C24 0.041(2) 0.048(2) 0.093(3) 0.007(2) 0.011(2) 0.0018(17) C25 0.043(2) 0.076(3) 0.138(5) 0.004(3) 0.003(3) 0.000(2) C26 0.118(4) 0.106(4) 0.039(2) -0.009(2) 0.014(3) 0.006(3) C27 0.085(3) 0.056(2) 0.046(2) -0.0040(18) 0.016(2) -0.001(2) C28 0.079(3) 0.069(3) 0.058(3) -0.003(2) 0.027(2) 0.016(2) C29 0.055(2) 0.045(2) 0.074(3) 0.0069(19) 0.021(2) 0.0041(17) C30 0.054(3) 0.079(3) 0.113(4) 0.011(3) 0.032(3) 0.012(2) C31 0.173(8) 0.104(5) 0.168(8) -0.003(5) 0.059(6) -0.034(5) C32 0.45(2) 0.133(7) 0.128(7) -0.024(6) 0.096(9) -0.158(10) C33 0.144(8) 0.222(11) 0.120(7) -0.006(7) -0.027(6) 0.018(7) C34 0.200(10) 0.249(11) 0.123(6) -0.021(7) 0.014(6) -0.148(9) _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 O2 1.902(3) . ? Co1 O1 1.939(2) . ? Co1 N1 1.975(3) . ? Co1 N2 2.059(3) . ? Co1 P1 2.2236(12) . ? Co1 P2 2.2385(12) . ? Co2 O4 1.902(2) . ? Co2 O3 1.928(2) . ? Co2 N3 1.978(3) . ? Co2 N4 2.063(3) . ? Co2 P3 2.2170(11) . ? Co2 P4 2.2353(12) . ? P1 C2 1.803(5) . ? P1 C1 1.810(5) . ? P1 C3 1.812(4) . ? P2 C6 1.803(4) . ? P2 C8 1.812(5) . ? P2 C7 1.815(4) . ? P3 C11 1.805(4) . ? P3 C12 1.805(4) . ? P3 C13 1.809(4) . ? P4 C17 1.806(4) . ? P4 C18 1.820(4) . ? P4 C16 1.823(4) . ? P5 F3 1.562(3) . ? P5 F2 1.564(3) . ? P5 F5 1.568(3) . ? P5 F1 1.569(3) . ? P5 F4 1.570(3) . ? P5 F6 1.604(3) . ? P6 F7 1.564(4) . ? P6 F10 1.565(3) . ? P6 F12 1.572(4) . ? P6 F8 1.575(3) . ? P6 F9 1.577(3) . ? P6 F11 1.597(3) . ? P7 F172 1.515(9) . ? P7 F142 1.517(13) . ? P7 F151 1.519(6) . ? P7 F162 1.526(11) . ? P7 F141 1.560(7) . ? P7 F152 1.565(12) . ? P7 F13 1.575(3) . ? P7 F18 1.584(3) . ? P7 F171 1.613(6) . ? P7 F161 1.620(6) . ? P8 F211 1.429(12) . ? P8 F202 1.451(8) . ? P8 F242 1.483(9) . ? P8 F232 1.496(7) . ? P8 F201 1.505(7) . ? P8 F212 1.521(10) . ? P8 F192 1.535(7) . ? P8 F191 1.548(7) . ? P8 F241 1.550(7) . ? P8 F222 1.553(15) . ? P8 F231 1.558(7) . ? P8 F221 1.588(13) . ? O1 C22 1.288(5) . ? O2 C24 1.276(5) . ? O3 C27 1.285(5) . ? O4 C29 1.283(4) . ? O5 C33 1.332(9) . ? O5 C32 1.464(8) . ? N1 C5 1.480(5) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C10 1.501(4) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C15 1.501(4) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C20 1.488(5) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C2 H2C 0.9600 . ? C2 H2D 0.9600 . ? C2 H2E 0.9600 . ? C3 C4 1.532(7) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 C5 1.502(6) . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.523(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.495(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.525(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.503(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.526(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.501(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.508(6) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.391(6) . ? C23 C24 1.384(6) . ? C23 H23 0.9300 . ? C24 C25 1.493(6) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.501(6) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.379(6) . ? C28 C29 1.385(6) . ? C28 H28 0.9300 . ? C29 C30 1.506(6) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.353(10) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.439(11) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 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 O2 Co1 O1 93.63(11) . . ? O2 Co1 N1 175.89(12) . . ? O1 Co1 N1 82.46(12) . . ? O2 Co1 N2 87.64(12) . . ? O1 Co1 N2 85.45(11) . . ? N1 Co1 N2 90.78(13) . . ? O2 Co1 P1 85.69(9) . . ? O1 Co1 P1 89.90(8) . . ? N1 Co1 P1 95.54(10) . . ? N2 Co1 P1 171.61(9) . . ? O2 Co1 P2 88.10(9) . . ? O1 Co1 P2 174.43(8) . . ? N1 Co1 P2 95.68(10) . . ? N2 Co1 P2 89.33(9) . . ? P1 Co1 P2 95.51(4) . . ? O4 Co2 O3 93.48(11) . . ? O4 Co2 N3 175.59(11) . . ? O3 Co2 N3 82.16(11) . . ? O4 Co2 N4 86.59(11) . . ? O3 Co2 N4 85.55(11) . . ? N3 Co2 N4 93.70(12) . . ? O4 Co2 P3 86.54(8) . . ? O3 Co2 P3 91.61(8) . . ? N3 Co2 P3 92.90(9) . . ? N4 Co2 P3 172.39(9) . . ? O4 Co2 P4 88.89(8) . . ? O3 Co2 P4 172.38(8) . . ? N3 Co2 P4 95.52(9) . . ? N4 Co2 P4 87.37(9) . . ? P3 Co2 P4 95.77(4) . . ? C2 P1 C1 104.6(3) . . ? C2 P1 C3 103.3(2) . . ? C1 P1 C3 105.8(3) . . ? C2 P1 Co1 112.31(16) . . ? C1 P1 Co1 116.24(17) . . ? C3 P1 Co1 113.36(16) . . ? C6 P2 C8 104.2(2) . . ? C6 P2 C7 105.6(3) . . ? C8 P2 C7 100.1(3) . . ? C6 P2 Co1 112.58(16) . . ? C8 P2 Co1 111.06(15) . . ? C7 P2 Co1 121.35(16) . . ? C11 P3 C12 103.8(2) . . ? C11 P3 C13 107.0(2) . . ? C12 P3 C13 104.17(18) . . ? C11 P3 Co2 115.15(14) . . ? C12 P3 Co2 111.30(14) . . ? C13 P3 Co2 114.31(13) . . ? C17 P4 C18 104.6(2) . . ? C17 P4 C16 103.3(2) . . ? C18 P4 C16 102.3(2) . . ? C17 P4 Co2 111.79(14) . . ? C18 P4 Co2 109.71(14) . . ? C16 P4 Co2 123.33(14) . . ? F3 P5 F2 90.4(2) . . ? F3 P5 F5 90.1(2) . . ? F2 P5 F5 177.9(2) . . ? F3 P5 F1 91.79(19) . . ? F2 P5 F1 91.8(2) . . ? F5 P5 F1 90.18(17) . . ? F3 P5 F4 178.3(2) . . ? F2 P5 F4 89.5(3) . . ? F5 P5 F4 89.8(2) . . ? F1 P5 F4 89.9(2) . . ? F3 P5 F6 89.80(18) . . ? F2 P5 F6 88.9(2) . . ? F5 P5 F6 89.17(18) . . ? F1 P5 F6 178.29(19) . . ? F4 P5 F6 88.50(19) . . ? F7 P6 F10 88.9(2) . . ? F7 P6 F12 179.7(3) . . ? F10 P6 F12 91.2(2) . . ? F7 P6 F8 89.1(2) . . ? F10 P6 F8 89.9(2) . . ? F12 P6 F8 90.7(2) . . ? F7 P6 F9 91.8(2) . . ? F10 P6 F9 179.0(2) . . ? F12 P6 F9 88.1(2) . . ? F8 P6 F9 90.87(19) . . ? F7 P6 F11 89.9(2) . . ? F10 P6 F11 90.9(2) . . ? F12 P6 F11 90.3(2) . . ? F8 P6 F11 178.6(2) . . ? F9 P6 F11 88.28(19) . . ? F172 P7 F142 176.9(7) . . ? F172 P7 F162 95.5(6) . . ? F142 P7 F162 87.6(6) . . ? F151 P7 F141 96.8(8) . . ? F172 P7 F152 88.7(6) . . ? F142 P7 F152 88.2(6) . . ? F162 P7 F152 175.3(6) . . ? F172 P7 F13 89.8(4) . . ? F142 P7 F13 90.1(5) . . ? F151 P7 F13 95.4(4) . . ? F162 P7 F13 90.5(4) . . ? F141 P7 F13 97.6(4) . . ? F152 P7 F13 87.4(4) . . ? F172 P7 F18 89.5(4) . . ? F142 P7 F18 90.8(5) . . ? F151 P7 F18 88.3(4) . . ? F162 P7 F18 84.1(4) . . ? F141 P7 F18 86.0(4) . . ? F152 P7 F18 98.2(4) . . ? F13 P7 F18 174.4(3) . . ? F151 P7 F171 86.0(6) . . ? F141 P7 F171 173.7(6) . . ? F13 P7 F171 87.7(3) . . ? F18 P7 F171 88.4(3) . . ? F151 P7 F161 175.5(7) . . ? F141 P7 F161 87.4(7) . . ? F13 P7 F161 85.6(3) . . ? F18 P7 F161 90.3(3) . . ? F171 P7 F161 89.7(6) . . ? F211 P8 F202 94.6(10) . . ? F211 P8 F242 156.0(17) . . ? F202 P8 F242 77.6(11) . . ? F211 P8 F232 79.6(8) . . ? F202 P8 F232 155.1(10) . . ? F242 P8 F232 98.0(10) . . ? F211 P8 F201 89.4(10) . . ? F202 P8 F201 110.9(8) . . ? F242 P8 F201 72.9(10) . . ? F232 P8 F201 45.4(6) . . ? F211 P8 F212 88.8(11) . . ? F202 P8 F212 85.6(6) . . ? F242 P8 F212 112.8(11) . . ? F232 P8 F212 118.1(9) . . ? F201 P8 F212 163.4(6) . . ? F202 P8 F192 108.2(8) . . ? F242 P8 F192 173.1(11) . . ? F232 P8 F192 78.4(8) . . ? F201 P8 F192 107.7(7) . . ? F212 P8 F192 64.7(6) . . ? F211 P8 F191 58.8(12) . . ? F202 P8 F191 53.1(7) . . ? F242 P8 F191 99.7(11) . . ? F232 P8 F191 104.7(9) . . ? F201 P8 F191 72.5(7) . . ? F212 P8 F191 120.0(7) . . ? F192 P8 F191 87.0(5) . . ? F211 P8 F241 110.4(14) . . ? F202 P8 F241 141.4(11) . . ? F242 P8 F241 88.6(10) . . ? F232 P8 F241 61.7(7) . . ? F201 P8 F241 98.7(7) . . ? F212 P8 F241 66.7(6) . . ? F192 P8 F241 84.4(5) . . ? F191 P8 F241 165.2(9) . . ? F211 P8 F222 138.2(15) . . ? F202 P8 F222 118.6(11) . . ? F242 P8 F222 62.9(10) . . ? F232 P8 F222 79.1(7) . . ? F201 P8 F222 100.4(8) . . ? F212 P8 F222 70.7(7) . . ? F192 P8 F222 110.4(8) . . ? F191 P8 F222 162.5(8) . . ? F211 P8 F231 97.6(8) . . ? F242 P8 F231 92.6(10) . . ? F232 P8 F231 159.4(11) . . ? F201 P8 F231 155.1(9) . . ? F192 P8 F231 89.1(7) . . ? F191 P8 F231 90.7(8) . . ? F241 P8 F231 101.2(10) . . ? F222 P8 F231 90.3(9) . . ? F211 P8 F221 151.5(15) . . ? F202 P8 F221 67.1(9) . . ? F232 P8 F221 107.6(8) . . ? F201 P8 F221 78.2(7) . . ? F212 P8 F221 110.2(7) . . ? F192 P8 F221 173.8(8) . . ? F191 P8 F221 92.9(7) . . ? F241 P8 F221 96.9(7) . . ? F222 P8 F221 69.8(9) . . ? F231 P8 F221 84.6(7) . . ? C22 O1 Co1 125.4(3) . . ? C24 O2 Co1 125.7(3) . . ? C27 O3 Co2 125.9(3) . . ? C29 O4 Co2 125.4(3) . . ? C33 O5 C32 112.7(7) . . ? C5 N1 Co1 127.1(3) . . ? C5 N1 H1A 105.5 . . ? Co1 N1 H1A 105.5 . . ? C5 N1 H1B 105.5 . . ? Co1 N1 H1B 105.5 . . ? H1A N1 H1B 106.1 . . ? C10 N2 Co1 128.2(2) . . ? C10 N2 H2A 105.2 . . ? Co1 N2 H2A 105.2 . . ? C10 N2 H2B 105.2 . . ? Co1 N2 H2B 105.2 . . ? H2A N2 H2B 106.0 . . ? C15 N3 Co2 126.8(2) . . ? C15 N3 H3A 105.6 . . ? Co2 N3 H3A 105.6 . . ? C15 N3 H3B 105.6 . . ? Co2 N3 H3B 105.6 . . ? H3A N3 H3B 106.1 . . ? C20 N4 Co2 128.2(2) . . ? C20 N4 H4A 105.2 . . ? Co2 N4 H4A 105.2 . . ? C20 N4 H4B 105.2 . . ? Co2 N4 H4B 105.2 . . ? H4A N4 H4B 106.0 . . ? P1 C1 H1C 109.5 . . ? P1 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? P1 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? P1 C2 H2C 109.5 . . ? P1 C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? P1 C2 H2E 109.5 . . ? H2C C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? C4 C3 P1 112.0(3) . . ? C4 C3 H3C 109.2 . . ? P1 C3 H3C 109.2 . . ? C4 C3 H3D 109.2 . . ? P1 C3 H3D 109.2 . . ? H3C C3 H3D 107.9 . . ? C5 C4 C3 114.7(4) . . ? C5 C4 H4C 108.6 . . ? C3 C4 H4C 108.6 . . ? C5 C4 H4D 108.6 . . ? C3 C4 H4D 108.6 . . ? H4C C4 H4D 107.6 . . ? N1 C5 C4 115.3(4) . . ? N1 C5 H5A 108.5 . . ? C4 C5 H5A 108.5 . . ? N1 C5 H5B 108.5 . . ? C4 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P2 C7 H7A 109.5 . . ? P2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 P2 116.3(3) . . ? C9 C8 H8A 108.2 . . ? P2 C8 H8A 108.2 . . ? C9 C8 H8B 108.2 . . ? P2 C8 H8B 108.2 . . ? H8A C8 H8B 107.4 . . ? C10 C9 C8 114.0(4) . . ? C10 C9 H9A 108.7 . . ? C8 C9 H9A 108.7 . . ? C10 C9 H9B 108.7 . . ? C8 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C9 C10 N2 113.0(3) . . ? C9 C10 H10A 109.0 . . ? N2 C10 H10A 109.0 . . ? C9 C10 H10B 109.0 . . ? N2 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? P3 C11 H11A 109.5 . . ? P3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P3 C12 H12A 109.5 . . ? P3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 P3 112.6(3) . . ? C14 C13 H13A 109.1 . . ? P3 C13 H13A 109.1 . . ? C14 C13 H13B 109.1 . . ? P3 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C15 C14 C13 115.2(3) . . ? C15 C14 H14A 108.5 . . ? C13 C14 H14A 108.5 . . ? C15 C14 H14B 108.5 . . ? C13 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? N3 C15 C14 113.7(3) . . ? N3 C15 H15A 108.8 . . ? C14 C15 H15A 108.8 . . ? N3 C15 H15B 108.8 . . ? C14 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? P4 C16 H16A 109.5 . . ? P4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P4 C17 H17A 109.5 . . ? P4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 P4 114.2(3) . . ? C19 C18 H18A 108.7 . . ? P4 C18 H18A 108.7 . . ? C19 C18 H18B 108.7 . . ? P4 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C20 C19 C18 114.5(3) . . ? C20 C19 H19A 108.6 . . ? C18 C19 H19A 108.6 . . ? C20 C19 H19B 108.6 . . ? C18 C19 H19B 108.6 . . ? H19A C19 H19B 107.6 . . ? N4 C20 C19 113.3(3) . . ? N4 C20 H20A 108.9 . . ? C19 C20 H20A 108.9 . . ? N4 C20 H20B 108.9 . . ? C19 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O1 C22 C23 124.0(4) . . ? O1 C22 C21 116.1(4) . . ? C23 C22 C21 119.9(4) . . ? C24 C23 C22 125.3(4) . . ? C24 C23 H23 117.3 . . ? C22 C23 H23 117.3 . . ? O2 C24 C23 125.5(4) . . ? O2 C24 C25 114.6(4) . . ? C23 C24 C25 119.9(4) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C27 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O3 C27 C28 124.0(4) . . ? O3 C27 C26 114.1(4) . . ? C28 C27 C26 121.9(4) . . ? C27 C28 C29 125.3(4) . . ? C27 C28 H28 117.3 . . ? C29 C28 H28 117.3 . . ? O4 C29 C28 125.4(4) . . ? O4 C29 C30 113.9(4) . . ? C28 C29 C30 120.8(4) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C31 C32 O5 117.2(8) . . ? C31 C32 H32A 108.0 . . ? O5 C32 H32A 108.0 . . ? C31 C32 H32B 108.0 . . ? O5 C32 H32B 108.0 . . ? H32A C32 H32B 107.3 . . ? O5 C33 C34 113.6(8) . . ? O5 C33 H33A 108.8 . . ? C34 C33 H33A 108.8 . . ? O5 C33 H33B 108.8 . . ? C34 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? 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 O2 Co1 P1 C2 78.5(2) . . . . ? O1 Co1 P1 C2 -15.2(2) . . . . ? N1 Co1 P1 C2 -97.6(2) . . . . ? P2 Co1 P1 C2 166.1(2) . . . . ? O2 Co1 P1 C1 -42.0(3) . . . . ? O1 Co1 P1 C1 -135.6(3) . . . . ? N1 Co1 P1 C1 141.9(3) . . . . ? P2 Co1 P1 C1 45.7(3) . . . . ? O2 Co1 P1 C3 -164.92(19) . . . . ? O1 Co1 P1 C3 101.44(19) . . . . ? N1 Co1 P1 C3 19.02(19) . . . . ? P2 Co1 P1 C3 -77.25(17) . . . . ? O2 Co1 P2 C6 -4.30(19) . . . . ? N1 Co1 P2 C6 174.1(2) . . . . ? N2 Co1 P2 C6 83.36(19) . . . . ? P1 Co1 P2 C6 -89.78(18) . . . . ? O2 Co1 P2 C8 -120.7(2) . . . . ? N1 Co1 P2 C8 57.6(2) . . . . ? N2 Co1 P2 C8 -33.1(2) . . . . ? P1 Co1 P2 C8 153.78(18) . . . . ? O2 Co1 P2 C7 122.2(3) . . . . ? N1 Co1 P2 C7 -59.5(3) . . . . ? N2 Co1 P2 C7 -150.2(3) . . . . ? P1 Co1 P2 C7 36.7(3) . . . . ? O4 Co2 P3 C11 -34.33(19) . . . . ? O3 Co2 P3 C11 -127.72(19) . . . . ? N3 Co2 P3 C11 150.04(19) . . . . ? P4 Co2 P3 C11 54.20(18) . . . . ? O4 Co2 P3 C12 83.45(18) . . . . ? O3 Co2 P3 C12 -9.94(18) . . . . ? N3 Co2 P3 C12 -92.18(18) . . . . ? P4 Co2 P3 C12 171.98(16) . . . . ? O4 Co2 P3 C13 -158.88(16) . . . . ? O3 Co2 P3 C13 107.73(16) . . . . ? N3 Co2 P3 C13 25.49(17) . . . . ? P4 Co2 P3 C13 -70.35(14) . . . . ? O4 Co2 P4 C17 -11.41(17) . . . . ? N3 Co2 P4 C17 168.69(18) . . . . ? N4 Co2 P4 C17 75.23(18) . . . . ? P3 Co2 P4 C17 -97.82(16) . . . . ? O4 Co2 P4 C18 -127.02(17) . . . . ? N3 Co2 P4 C18 53.08(18) . . . . ? N4 Co2 P4 C18 -40.38(18) . . . . ? P3 Co2 P4 C18 146.57(16) . . . . ? O4 Co2 P4 C16 112.6(2) . . . . ? N3 Co2 P4 C16 -67.3(2) . . . . ? N4 Co2 P4 C16 -160.8(2) . . . . ? P3 Co2 P4 C16 26.1(2) . . . . ? O2 Co1 O1 C22 6.5(3) . . . . ? N1 Co1 O1 C22 -172.3(3) . . . . ? N2 Co1 O1 C22 -80.9(3) . . . . ? P1 Co1 O1 C22 92.2(3) . . . . ? O1 Co1 O2 C24 -5.2(3) . . . . ? N2 Co1 O2 C24 80.1(3) . . . . ? P1 Co1 O2 C24 -94.8(3) . . . . ? P2 Co1 O2 C24 169.5(3) . . . . ? O4 Co2 O3 C27 6.0(3) . . . . ? N3 Co2 O3 C27 -174.6(3) . . . . ? N4 Co2 O3 C27 -80.3(3) . . . . ? P3 Co2 O3 C27 92.7(3) . . . . ? O3 Co2 O4 C29 -4.0(3) . . . . ? N4 Co2 O4 C29 81.3(3) . . . . ? P3 Co2 O4 C29 -95.4(3) . . . . ? P4 Co2 O4 C29 168.7(3) . . . . ? O1 Co1 N1 C5 -113.2(3) . . . . ? N2 Co1 N1 C5 161.5(3) . . . . ? P1 Co1 N1 C5 -24.0(3) . . . . ? P2 Co1 N1 C5 72.1(3) . . . . ? O2 Co1 N2 C10 130.9(3) . . . . ? O1 Co1 N2 C10 -135.3(3) . . . . ? N1 Co1 N2 C10 -52.9(3) . . . . ? P2 Co1 N2 C10 42.8(3) . . . . ? O3 Co2 N3 C15 -125.5(3) . . . . ? N4 Co2 N3 C15 149.5(3) . . . . ? P3 Co2 N3 C15 -34.3(3) . . . . ? P4 Co2 N3 C15 61.8(3) . . . . ? O4 Co2 N4 C20 137.2(3) . . . . ? O3 Co2 N4 C20 -129.0(3) . . . . ? N3 Co2 N4 C20 -47.2(3) . . . . ? P4 Co2 N4 C20 48.2(3) . . . . ? C2 P1 C3 C4 80.3(4) . . . . ? C1 P1 C3 C4 -170.0(4) . . . . ? Co1 P1 C3 C4 -41.5(4) . . . . ? P1 C3 C4 C5 67.8(5) . . . . ? Co1 N1 C5 C4 49.6(5) . . . . ? C3 C4 C5 N1 -71.7(6) . . . . ? C6 P2 C8 C9 -69.0(4) . . . . ? C7 P2 C8 C9 -178.1(4) . . . . ? Co1 P2 C8 C9 52.5(4) . . . . ? P2 C8 C9 C10 -65.8(5) . . . . ? C8 C9 C10 N2 64.3(5) . . . . ? Co1 N2 C10 C9 -60.3(5) . . . . ? C11 P3 C13 C14 -172.5(3) . . . . ? C12 P3 C13 C14 77.9(3) . . . . ? Co2 P3 C13 C14 -43.8(3) . . . . ? P3 C13 C14 C15 64.9(4) . . . . ? Co2 N3 C15 C14 57.6(4) . . . . ? C13 C14 C15 N3 -70.4(5) . . . . ? C17 P4 C18 C19 -60.7(4) . . . . ? C16 P4 C18 C19 -168.1(3) . . . . ? Co2 P4 C18 C19 59.4(3) . . . . ? P4 C18 C19 C20 -66.3(5) . . . . ? Co2 N4 C20 C19 -60.5(5) . . . . ? C18 C19 C20 N4 61.3(5) . . . . ? Co1 O1 C22 C23 -2.9(6) . . . . ? Co1 O1 C22 C21 179.2(3) . . . . ? O1 C22 C23 C24 -4.5(7) . . . . ? C21 C22 C23 C24 173.4(4) . . . . ? Co1 O2 C24 C23 0.3(6) . . . . ? Co1 O2 C24 C25 179.2(3) . . . . ? C22 C23 C24 O2 6.0(7) . . . . ? C22 C23 C24 C25 -172.8(4) . . . . ? Co2 O3 C27 C28 -2.9(6) . . . . ? Co2 O3 C27 C26 177.8(3) . . . . ? O3 C27 C28 C29 -4.5(7) . . . . ? C26 C27 C28 C29 174.7(4) . . . . ? Co2 O4 C29 C28 -1.2(6) . . . . ? Co2 O4 C29 C30 178.6(3) . . . . ? C27 C28 C29 O4 6.9(7) . . . . ? C27 C28 C29 C30 -173.0(4) . . . . ? C33 O5 C32 C31 -99.8(11) . . . . ? C32 O5 C33 C34 177.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.623 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.072 #==END #============================================================================== data_transNN _database_code_depnum_ccdc_archive 'CCDC 618537' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans(N,N)-(pentane-2,4-dionato)bis((3-aminopropyl) dimethylphosphine)cobalt(III) Bis(hexafluorophospate) ; _chemical_name_common ; trans(N,N)-(pentane-2,4-dionato)bis((3-aminopropyl) dimethylphosphine)cobalt(iii) Bis(hexafluorophospate) ; _chemical_melting_point ? _chemical_formula_moiety 'C15 H35 Co N2 O2 P2 2+, 2(F6 P 1-)' _chemical_formula_sum 'C15 H35 Co F12 N2 O2 P4' _chemical_formula_weight 686.26 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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I b c a' 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+1/2, y+1/2, z+1/2' '-x+1, y+1, z+1/2' 'x+1/2, -y+1, z+1' '-x+1, -y+1/2, z+1' '-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+1/2, -y+1/2, -z+1/2' 'x, -y, -z+1/2' '-x+1/2, y, -z' 'x, y+1/2, -z' _cell_length_a 15.177(3) _cell_length_b 16.827(2) _cell_length_c 21.443(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5476.1(16) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17911 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _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 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2800 _exptl_absorpt_coefficient_mu 0.959 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8167 _exptl_absorpt_correction_T_max 0.8774 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25892 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0143 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3140 _reflns_number_gt 2759 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'CrystalStructure 3.7.0' _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Win' _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0732P)^2^+8.4006P] 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 3140 _refine_ls_number_parameters 185 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.1244 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.2500 0.14876(2) 0.03067(16) Uani 1 2 d S . . P1 P 0.06003(4) 0.15890(4) 0.08471(3) 0.03670(18) Uani 1 1 d . . . P2 P 0.2500 -0.07748(6) 0.0000 0.0477(3) Uani 1 2 d S . . P3 P 0.31948(7) 0.0000 0.2500 0.0505(3) Uani 1 2 d S . . F1 F 0.2712(4) -0.0795(2) -0.06965(14) 0.1650(18) Uani 1 1 d . . . F2 F 0.1792(2) -0.14467(15) -0.01323(18) 0.1154(11) Uani 1 1 d . . . F3 F 0.1807(2) -0.01072(16) -0.01280(19) 0.1200(13) Uani 1 1 d . . . F4 F 0.3204(4) 0.09011(17) 0.23468(17) 0.161(2) Uani 1 1 d . . . F5 F 0.2282(4) 0.0238(7) 0.2707(6) 0.174(4) Uani 0.50 1 d P . . F6 F 0.2828(10) -0.0171(4) 0.1848(4) 0.130(3) Uani 0.50 1 d P . . F7 F 0.3554(8) -0.0102(5) 0.1822(4) 0.124(3) Uani 0.50 1 d P . . F8 F 0.4117(4) -0.0331(4) 0.2284(4) 0.116(2) Uani 0.50 1 d P . . O1 O 0.03840(13) 0.17385(11) 0.21135(9) 0.0427(4) Uani 1 1 d . . . N1 N 0.11540(14) 0.30605(13) 0.15041(10) 0.0385(5) Uani 1 1 d . . . H1A H 0.1244 0.3254 0.1118 0.046 Uiso 1 1 calc R . . H1B H 0.1089 0.3483 0.1757 0.046 Uiso 1 1 calc R . . C1 C 0.0062(2) 0.06344(17) 0.08785(18) 0.0542(7) Uani 1 1 d . . . H1C H -0.0535 0.0688 0.0738 0.065 Uiso 1 1 calc R . . H1D H 0.0067 0.0441 0.1300 0.065 Uiso 1 1 calc R . . H1E H 0.0369 0.0266 0.0614 0.065 Uiso 1 1 calc R . . C2 C 0.0737(3) 0.1770(2) 0.00194(15) 0.0602(8) Uani 1 1 d . . . H2A H 0.1023 0.2273 -0.0042 0.072 Uiso 1 1 calc R . . H2B H 0.0170 0.1777 -0.0179 0.072 Uiso 1 1 calc R . . H2C H 0.1091 0.1355 -0.0160 0.072 Uiso 1 1 calc R . . C3 C 0.17016(19) 0.13610(18) 0.11256(16) 0.0511(7) Uani 1 1 d . . . H3A H 0.1652 0.1085 0.1521 0.061 Uiso 1 1 calc R . . H3B H 0.1978 0.1000 0.0832 0.061 Uiso 1 1 calc R . . C4 C 0.23037(18) 0.20787(19) 0.12134(17) 0.0547(7) Uani 1 1 d . . . H4A H 0.2885 0.1893 0.1332 0.066 Uiso 1 1 calc R . . H4B H 0.2360 0.2354 0.0818 0.066 Uiso 1 1 calc R . . C5 C 0.19837(18) 0.26549(18) 0.16945(15) 0.0485(6) Uani 1 1 d . . . H5A H 0.1884 0.2374 0.2083 0.058 Uiso 1 1 calc R . . H5B H 0.2436 0.3051 0.1768 0.058 Uiso 1 1 calc R . . C6 C 0.0634(3) 0.1135(2) 0.30823(17) 0.0689(10) Uani 1 1 d . . . H6A H 0.1152 0.0911 0.2895 0.083 Uiso 1 1 calc R . . H6B H 0.0178 0.0740 0.3100 0.083 Uiso 1 1 calc R . . H6C H 0.0770 0.1312 0.3497 0.083 Uiso 1 1 calc R . . C7 C 0.03245(19) 0.18269(18) 0.26998(13) 0.0483(7) Uani 1 1 d . . . C8 C 0.0000 0.2500 0.2993(2) 0.0615(12) Uani 1 2 d S . . H8 H 0.0000 0.2500 0.3426 0.074 Uiso 1 2 calc SR . . 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 0.0316(3) 0.0285(3) 0.0319(3) 0.000 0.000 0.00048(15) P1 0.0382(3) 0.0316(3) 0.0402(3) -0.0024(2) 0.0012(3) 0.0035(2) P2 0.0550(6) 0.0430(5) 0.0452(5) 0.000 -0.0091(4) 0.000 P3 0.0420(5) 0.0508(6) 0.0586(6) -0.0188(5) 0.000 0.000 F1 0.278(5) 0.155(3) 0.0619(18) 0.0144(18) 0.040(3) 0.057(3) F2 0.102(2) 0.0732(16) 0.171(3) -0.0258(18) -0.044(2) -0.0185(14) F3 0.0907(19) 0.0746(16) 0.195(3) -0.036(2) -0.052(2) 0.0318(14) F4 0.323(7) 0.0563(16) 0.105(2) -0.0064(15) -0.014(3) -0.016(3) F5 0.058(3) 0.217(12) 0.248(14) -0.093(9) 0.023(5) 0.031(5) F6 0.208(10) 0.101(5) 0.081(5) -0.007(4) -0.071(6) -0.009(7) F7 0.179(8) 0.115(5) 0.078(4) -0.038(4) 0.054(5) -0.001(6) F8 0.067(3) 0.137(6) 0.144(6) -0.007(4) 0.032(4) 0.034(3) O1 0.0441(10) 0.0426(10) 0.0414(10) 0.0075(7) -0.0021(8) 0.0011(8) N1 0.0358(11) 0.0353(10) 0.0442(12) -0.0030(8) -0.0012(8) -0.0012(8) C1 0.0560(17) 0.0331(14) 0.074(2) -0.0080(13) 0.0035(14) -0.0008(11) C2 0.078(2) 0.0595(18) 0.0430(15) -0.0025(14) 0.0121(15) 0.0142(16) C3 0.0421(15) 0.0435(15) 0.0679(18) -0.0042(13) -0.0033(13) 0.0120(11) C4 0.0347(14) 0.0566(18) 0.073(2) -0.0040(15) -0.0006(13) 0.0061(12) C5 0.0351(13) 0.0503(16) 0.0601(17) -0.0019(13) -0.0090(12) -0.0018(11) C6 0.074(2) 0.073(2) 0.059(2) 0.0266(17) -0.0175(17) -0.0059(18) C7 0.0457(15) 0.0578(17) 0.0414(14) 0.0110(12) -0.0073(11) -0.0119(13) C8 0.086(4) 0.065(3) 0.034(2) 0.000 0.000 -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.9449(18) 8_454 ? Co1 O1 1.9450(18) . ? Co1 N1 1.990(2) . ? Co1 N1 1.990(2) 8_454 ? Co1 P1 2.2508(7) . ? Co1 P1 2.2509(7) 8_454 ? P1 C1 1.803(3) . ? P1 C2 1.813(3) . ? P1 C3 1.816(3) . ? P2 F1 1.528(3) 15 ? P2 F1 1.528(3) . ? P2 F3 1.564(3) 15 ? P2 F3 1.564(3) . ? P2 F2 1.585(3) . ? P2 F2 1.585(3) 15 ? P3 F5 1.509(6) . ? P3 F5 1.509(6) 14 ? P3 F6 1.532(6) 14 ? P3 F6 1.532(6) . ? P3 F4 1.551(3) . ? P3 F4 1.552(3) 14 ? P3 F7 1.562(6) 14 ? P3 F7 1.562(6) . ? P3 F8 1.576(5) 14 ? P3 F8 1.576(5) . ? O1 C7 1.269(3) . ? N1 C5 1.489(3) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.526(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.497(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.499(4) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.385(4) . ? C8 C7 1.385(4) 8_454 ? C8 H8 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O1 92.73(12) 8_454 . ? O1 Co1 N1 86.51(8) 8_454 . ? O1 Co1 N1 92.08(9) . . ? O1 Co1 N1 92.08(9) 8_454 8_454 ? O1 Co1 N1 86.51(8) . 8_454 ? N1 Co1 N1 177.96(12) . 8_454 ? O1 Co1 P1 172.32(6) 8_454 . ? O1 Co1 P1 81.44(6) . . ? N1 Co1 P1 88.70(6) . . ? N1 Co1 P1 92.54(7) 8_454 . ? O1 Co1 P1 81.44(6) 8_454 8_454 ? O1 Co1 P1 172.32(6) . 8_454 ? N1 Co1 P1 92.54(7) . 8_454 ? N1 Co1 P1 88.70(6) 8_454 8_454 ? P1 Co1 P1 104.80(4) . 8_454 ? C1 P1 C2 103.77(17) . . ? C1 P1 C3 102.49(15) . . ? C2 P1 C3 104.59(17) . . ? C1 P1 Co1 113.62(11) . . ? C2 P1 Co1 121.98(11) . . ? C3 P1 Co1 108.41(11) . . ? F1 P2 F1 177.4(3) 15 . ? F1 P2 F3 89.2(2) 15 15 ? F1 P2 F3 92.6(3) . 15 ? F1 P2 F3 92.6(3) 15 . ? F1 P2 F3 89.2(2) . . ? F3 P2 F3 88.1(2) 15 . ? F1 P2 F2 90.9(2) 15 . ? F1 P2 F2 87.2(3) . . ? F3 P2 F2 179.55(18) 15 . ? F3 P2 F2 91.42(15) . . ? F1 P2 F2 87.3(3) 15 15 ? F1 P2 F2 90.9(2) . 15 ? F3 P2 F2 91.41(15) 15 15 ? F3 P2 F2 179.55(17) . 15 ? F2 P2 F2 89.0(2) . 15 ? F5 P3 F6 89.1(9) 14 14 ? F5 P3 F6 89.1(9) . . ? F6 P3 F6 137.4(12) 14 . ? F5 P3 F4 79.2(6) . . ? F5 P3 F4 101.8(6) 14 . ? F6 P3 F4 90.7(3) 14 . ? F6 P3 F4 89.7(3) . . ? F5 P3 F4 101.8(6) . 14 ? F5 P3 F4 79.2(6) 14 14 ? F6 P3 F4 89.7(3) 14 14 ? F6 P3 F4 90.7(3) . 14 ? F4 P3 F4 178.9(4) . 14 ? F5 P3 F7 91.0(6) . 14 ? F5 P3 F7 128.6(8) 14 14 ? F6 P3 F7 175.3(5) . 14 ? F4 P3 F7 95.0(3) . 14 ? F4 P3 F7 84.7(3) 14 14 ? F5 P3 F7 128.6(8) . . ? F5 P3 F7 91.0(6) 14 . ? F6 P3 F7 175.3(5) 14 . ? F4 P3 F7 84.7(3) . . ? F4 P3 F7 95.0(3) 14 . ? F7 P3 F7 139.1(10) 14 . ? F5 P3 F8 129.5(4) . 14 ? F5 P3 F8 174.6(5) 14 14 ? F6 P3 F8 89.3(6) 14 14 ? F6 P3 F8 131.1(7) . 14 ? F4 P3 F8 73.1(3) . 14 ? F4 P3 F8 105.9(4) 14 14 ? F7 P3 F8 51.5(4) 14 14 ? F7 P3 F8 90.1(6) . 14 ? F5 P3 F8 174.6(5) . . ? F5 P3 F8 129.5(4) 14 . ? F6 P3 F8 131.1(7) 14 . ? F6 P3 F8 89.3(6) . . ? F4 P3 F8 105.9(4) . . ? F4 P3 F8 73.1(3) 14 . ? F7 P3 F8 90.1(6) 14 . ? F7 P3 F8 51.5(4) . . ? F8 P3 F8 54.7(6) 14 . ? F5 F5 F6 120.0(13) 14 14 ? F5 F5 P3 66.7(4) 14 . ? F6 F5 P3 66.3(4) 14 . ? F7 F6 F5 134.1(8) . 14 ? F7 F6 P3 70.4(5) . . ? F5 F6 P3 64.4(5) 14 . ? F6 F7 F8 123.8(8) . . ? F6 F7 P3 67.5(5) . . ? F8 F7 P3 64.8(4) . . ? F7 F8 F8 104.3(7) . 14 ? F7 F8 P3 63.7(3) . . ? F8 F8 P3 62.6(3) 14 . ? C7 O1 Co1 125.81(19) . . ? C5 N1 Co1 122.13(17) . . ? C5 N1 H1A 106.8 . . ? Co1 N1 H1A 106.8 . . ? C5 N1 H1B 106.8 . . ? Co1 N1 H1B 106.8 . . ? H1A N1 H1B 106.6 . . ? P1 C1 H1C 109.5 . . ? P1 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? P1 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 115.1(2) . . ? C4 C3 H3A 108.5 . . ? P1 C3 H3A 108.5 . . ? C4 C3 H3B 108.5 . . ? P1 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C5 C4 C3 113.8(3) . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? N1 C5 C4 112.5(2) . . ? N1 C5 H5A 109.1 . . ? C4 C5 H5A 109.1 . . ? N1 C5 H5B 109.1 . . ? C4 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 C7 C8 124.7(3) . . ? O1 C7 C6 115.4(3) . . ? C8 C7 C6 119.9(3) . . ? C7 C8 C7 126.1(4) . 8_454 ? C7 C8 H8 116.9 . . ? C7 C8 H8 116.9 8_454 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co1 P1 C1 62.57(14) . . . . ? N1 Co1 P1 C1 154.87(14) . . . . ? N1 Co1 P1 C1 -23.51(14) 8_454 . . . ? P1 Co1 P1 C1 -112.84(13) 8_454 . . . ? O1 Co1 P1 C2 -172.03(16) . . . . ? N1 Co1 P1 C2 -79.74(16) . . . . ? N1 Co1 P1 C2 101.88(16) 8_454 . . . ? P1 Co1 P1 C2 12.55(15) 8_454 . . . ? O1 Co1 P1 C3 -50.65(13) . . . . ? N1 Co1 P1 C3 41.65(13) . . . . ? N1 Co1 P1 C3 -136.73(13) 8_454 . . . ? P1 Co1 P1 C3 133.94(12) 8_454 . . . ? O1 Co1 O1 C7 1.14(18) 8_454 . . . ? N1 Co1 O1 C7 87.7(2) . . . . ? N1 Co1 O1 C7 -90.8(2) 8_454 . . . ? P1 Co1 O1 C7 176.1(2) . . . . ? O1 Co1 N1 C5 118.1(2) 8_454 . . . ? O1 Co1 N1 C5 25.5(2) . . . . ? P1 Co1 N1 C5 -55.9(2) . . . . ? P1 Co1 N1 C5 -160.6(2) 8_454 . . . ? C1 P1 C3 C4 -174.3(3) . . . . ? C2 P1 C3 C4 77.6(3) . . . . ? Co1 P1 C3 C4 -53.9(3) . . . . ? P1 C3 C4 C5 62.7(4) . . . . ? Co1 N1 C5 C4 72.4(3) . . . . ? C3 C4 C5 N1 -66.9(3) . . . . ? Co1 O1 C7 C8 -2.3(4) . . . . ? Co1 O1 C7 C6 177.5(2) . . . . ? O1 C7 C8 C7 1.3(2) . . . 8_454 ? C6 C7 C8 C7 -178.5(3) . . . 8_454 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.678 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.107 #==END #==============================================================================