Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'ProfD Fabrizia Grepioni' _publ_contact_author_address ; Dipartimento di Chimica G. Ciamician University of Bologna Via Selmi 2 Bologna 40126 ITALY ; _publ_contact_author_email FABRIZIA.GREPIONI@UNIBO.IT _publ_section_title ; Novel Organometallic Building Blocks For Molecular Crystal Engineering. 4. Synthesis and Characterization of Mono- and Bis-amido Derivatives of [CoIII(h5-C5H4-COOH)2]+ and Their Utilization as Ligands. ; loop_ _publ_author_name 'F. Grepioni' 'Dario Braga' 'Stefano Giaffreda' 'Marco Polito' data_7_2[Co(C5H4-COCl)2]+_[CoCl4]2- _database_code_depnum_ccdc_archive 'CCDC 269421' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 Cl8 Co3 O4' _chemical_formula_weight 828.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 13.8550(10) _cell_length_b 13.8550(10) _cell_length_c 29.570(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5676.3(18) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.940 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3272 _exptl_absorpt_coefficient_mu 2.519 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.899 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2702 _diffrn_reflns_av_R_equivalents 0.0825 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2482 _reflns_number_gt 2211 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0904P)^2^+13.1624P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0016(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2482 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1273 _refine_ls_wR_factor_gt 0.1229 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.003 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 0.19970(3) 0.50805(3) 0.098085(15) 0.0272(2) Uani 1 1 d . A . C1 C 0.21791(18) 0.36333(19) 0.09629(8) 0.0396(9) Uani 1 1 d G A . H1 H 0.2548 0.3268 0.1162 0.048 Uiso 1 1 calc R . . C2 C 0.11842(18) 0.3856(2) 0.10118(9) 0.0447(10) Uani 1 1 d G . . H2 H 0.0787 0.3662 0.1249 0.054 Uiso 1 1 calc R . . C3 C 0.09015(17) 0.4427(2) 0.06356(11) 0.0512(11) Uani 1 1 d G . . H3 H 0.0287 0.4672 0.0583 0.061 Uiso 1 1 calc R . . C4 C 0.1722(2) 0.4557(2) 0.03542(8) 0.0548(13) Uani 1 1 d G A . H4 H 0.1739 0.4903 0.0085 0.066 Uiso 1 1 calc R . . C5 C 0.25113(17) 0.4066(2) 0.05565(9) 0.0408(9) Uani 1 1 d G . . C6A C 0.3417(5) 0.4129(5) 0.0330(2) 0.0582(16) Uani 0.80 1 d P A 1 Cl1 Cl 0.42823(14) 0.34835(17) 0.06186(7) 0.0757(6) Uani 0.80 1 d P A 1 O1 O 0.3717(5) 0.4528(4) -0.00046(14) 0.0770(18) Uani 0.80 1 d P A 1 C6B C 0.3679(11) 0.3813(10) 0.0534(5) 0.010(3) Uiso 0.20 1 d P A 2 O1B O 0.379(3) 0.322(4) 0.0700(16) 0.169(18) Uiso 0.20 1 d P A 2 Cl1B Cl 0.4150(5) 0.4526(5) 0.0086(3) 0.0451(16) Uiso 0.20 1 d P A 2 C7 C 0.28440(19) 0.5626(2) 0.14743(8) 0.0415(9) Uani 1 1 d G . . H7 H 0.3335 0.5302 0.1625 0.050 Uiso 1 1 calc R A . C8 C 0.1860(2) 0.5667(2) 0.16078(8) 0.0539(12) Uani 1 1 d G A . H8 H 0.1594 0.5373 0.1862 0.065 Uiso 1 1 calc R . . C9 C 0.13546(14) 0.6234(2) 0.12856(10) 0.0501(11) Uani 1 1 d G A . H9 H 0.0699 0.6378 0.1291 0.060 Uiso 1 1 calc R . . C10 C 0.20257(18) 0.65444(18) 0.09531(8) 0.0390(9) Uani 1 1 d G A . H10 H 0.1887 0.6927 0.0703 0.047 Uiso 1 1 calc R . . C11 C 0.29462(15) 0.61688(19) 0.10697(8) 0.0327(8) Uani 1 1 d G A . C12 C 0.3848(3) 0.6309(3) 0.08359(15) 0.0447(10) Uani 1 1 d . . . O2 O 0.4600(3) 0.6012(3) 0.09473(15) 0.0763(12) Uani 1 1 d . A . Cl2 Cl 0.37487(12) 0.69945(13) 0.03411(6) 0.0871(5) Uani 1 1 d . A . Co2 Co 0.5000 0.2500 0.23600(2) 0.0271(2) Uani 1 2 d S . . Cl3 Cl 0.42654(7) 0.13611(7) 0.27876(3) 0.0401(3) Uani 1 1 d . . . Cl4 Cl 0.39088(6) 0.32722(7) 0.19131(3) 0.0381(3) 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 0.0341(3) 0.0261(3) 0.0215(3) -0.00068(17) -0.00434(17) -0.00213(18) C1 0.050(2) 0.0243(17) 0.044(2) 0.0025(15) -0.0018(18) 0.0009(15) C2 0.045(2) 0.032(2) 0.057(3) -0.0039(18) 0.0039(19) -0.0107(17) C3 0.048(2) 0.042(2) 0.064(3) -0.018(2) -0.023(2) -0.0016(19) C4 0.100(4) 0.039(2) 0.0254(19) -0.0070(16) -0.020(2) -0.007(2) C5 0.054(2) 0.036(2) 0.033(2) -0.0127(16) 0.0083(17) -0.0082(17) C6A 0.057(4) 0.061(4) 0.057(4) -0.024(3) 0.003(3) 0.003(3) Cl1 0.0556(10) 0.1048(15) 0.0667(11) 0.0042(10) -0.0059(8) 0.0300(10) O1 0.128(6) 0.086(4) 0.017(2) 0.021(2) 0.032(3) 0.005(4) C7 0.051(2) 0.043(2) 0.030(2) -0.0068(16) -0.0153(17) -0.0062(18) C8 0.070(3) 0.063(3) 0.029(2) -0.016(2) 0.005(2) -0.020(2) C9 0.042(2) 0.049(2) 0.060(3) -0.024(2) 0.006(2) -0.0008(19) C10 0.039(2) 0.0262(18) 0.052(2) -0.0049(16) -0.0101(17) -0.0009(15) C11 0.0364(19) 0.0277(17) 0.0340(19) -0.0030(14) -0.0106(15) -0.0012(14) C12 0.036(2) 0.044(2) 0.053(2) 0.0019(19) -0.0056(18) -0.0033(17) O2 0.0381(18) 0.108(3) 0.083(3) 0.012(2) -0.0064(17) 0.0107(19) Cl2 0.0745(9) 0.1015(12) 0.0852(10) 0.0480(9) 0.0083(8) -0.0166(8) Co2 0.0288(4) 0.0323(4) 0.0202(4) 0.000 0.000 -0.0022(2) Cl3 0.0422(5) 0.0422(5) 0.0358(5) 0.0104(4) 0.0038(4) -0.0056(4) Cl4 0.0351(5) 0.0470(5) 0.0321(5) 0.0076(4) -0.0063(3) -0.0009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C5 2.014(3) . ? Co1 C1 2.022(3) . ? Co1 C11 2.018(3) . ? Co1 C7 2.020(3) . ? Co1 C4 2.026(3) . ? Co1 C10 2.030(3) . ? Co1 C8 2.033(3) . ? Co1 C9 2.040(3) . ? Co1 C2 2.038(3) . ? Co1 C3 2.041(3) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C2 C3 1.4200 . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C5 C6A 1.426(7) . ? C5 C6B 1.657(16) . ? C6A O1 1.206(9) . ? C6A Cl1 1.722(8) . ? C6B O1B 0.97(5) . ? C6B Cl1B 1.777(17) . ? C7 C8 1.4200 . ? C7 C11 1.4200 . ? C8 C9 1.4200 . ? C9 C10 1.4200 . ? C10 C11 1.4200 . ? C11 C12 1.441(5) . ? C12 O2 1.168(6) . ? C12 Cl2 1.750(5) . ? Co2 Cl3 2.2638(10) . ? Co2 Cl3 2.2638(10) 6_554 ? Co2 Cl4 2.2752(10) . ? Co2 Cl4 2.2752(10) 6_554 ? 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 C5 Co1 C1 41.2 . . ? C5 Co1 C11 111.83(10) . . ? C1 Co1 C11 131.54(10) . . ? C5 Co1 C7 120.39(11) . . ? C1 Co1 C7 108.54(10) . . ? C11 Co1 C7 41.2 . . ? C5 Co1 C4 41.2 . . ? C1 Co1 C4 69.17(6) . . ? C11 Co1 C4 120.62(11) . . ? C7 Co1 C4 154.73(13) . . ? C5 Co1 C10 131.66(11) . . ? C1 Co1 C10 170.87(11) . . ? C11 Co1 C10 41.1 . . ? C7 Co1 C10 69.13(6) . . ? C4 Co1 C10 108.93(10) . . ? C5 Co1 C8 151.64(12) . . ? C1 Co1 C8 115.59(11) . . ? C11 Co1 C8 69.11(6) . . ? C7 Co1 C8 41.0 . . ? C4 Co1 C8 163.64(13) . . ? C10 Co1 C8 68.87(6) . . ? C5 Co1 C9 167.54(12) . . ? C1 Co1 C9 147.50(11) . . ? C11 Co1 C9 68.98(6) . . ? C7 Co1 C9 68.95(6) . . ? C4 Co1 C9 127.05(12) . . ? C10 Co1 C9 40.8 . . ? C8 Co1 C9 40.81(5) . . ? C5 Co1 C2 69.08(6) . . ? C1 Co1 C2 40.9 . . ? C11 Co1 C2 167.45(11) . . ? C7 Co1 C2 126.89(11) . . ? C4 Co1 C2 68.84(6) . . ? C10 Co1 C2 147.57(11) . . ? C8 Co1 C2 103.89(11) . . ? C9 Co1 C2 113.04(10) . . ? C5 Co1 C3 69.02(6) . . ? C1 Co1 C3 68.88(6) . . ? C11 Co1 C3 151.80(11) . . ? C7 Co1 C3 163.67(13) . . ? C4 Co1 C3 40.9 . . ? C10 Co1 C3 115.95(10) . . ? C8 Co1 C3 124.34(12) . . ? C9 Co1 C3 104.13(10) . . ? C2 Co1 C3 40.7 . . ? C2 C1 C5 108.0 . . ? C2 C1 Co1 70.16(10) . . ? C5 C1 Co1 69.12(10) . . ? C3 C2 C1 108.0 . . ? C3 C2 Co1 69.74(10) . . ? C1 C2 Co1 68.90(10) . . ? C2 C3 C4 108.0 . . ? C2 C3 Co1 69.52(10) . . ? C4 C3 Co1 69.00(10) . . ? C3 C4 C5 108.0 . . ? C3 C4 Co1 70.13(10) . . ? C5 C4 Co1 68.96(10) . . ? C4 C5 C1 108.0 . . ? C4 C5 C6A 116.8(4) . . ? C1 C5 C6A 135.2(4) . . ? C4 C5 C6B 146.8(6) . . ? C1 C5 C6B 105.1(6) . . ? C6A C5 C6B 30.1(5) . . ? C4 C5 Co1 69.88(10) . . ? C1 C5 Co1 69.68(10) . . ? C6A C5 Co1 124.2(3) . . ? C6B C5 Co1 121.2(5) . . ? O1 C6A C5 135.7(7) . . ? O1 C6A Cl1 113.9(6) . . ? C5 C6A Cl1 110.3(5) . . ? O1B C6B C5 108(3) . . ? O1B C6B Cl1B 142(3) . . ? C5 C6B Cl1B 105.6(10) . . ? C8 C7 C11 108.0 . . ? C8 C7 Co1 69.99(10) . . ? C11 C7 Co1 69.35(10) . . ? C9 C8 C7 108.0 . . ? C9 C8 Co1 69.84(10) . . ? C7 C8 Co1 68.98(10) . . ? C10 C9 C8 108.0 . . ? C10 C9 Co1 69.23(10) . . ? C8 C9 Co1 69.34(10) . . ? C11 C10 C9 108.0 . . ? C11 C10 Co1 69.00(10) . . ? C9 C10 Co1 69.93(10) . . ? C10 C11 C7 108.0 . . ? C10 C11 C12 127.8(2) . . ? C7 C11 C12 124.2(2) . . ? C10 C11 Co1 69.93(10) . . ? C7 C11 Co1 69.47(10) . . ? C12 C11 Co1 127.1(2) . . ? O2 C12 C11 126.2(4) . . ? O2 C12 Cl2 119.8(4) . . ? C11 C12 Cl2 114.0(3) . . ? Cl3 Co2 Cl3 112.09(6) . 6_554 ? Cl3 Co2 Cl4 110.70(3) . . ? Cl3 Co2 Cl4 107.18(4) 6_554 . ? Cl3 Co2 Cl4 107.18(3) . 6_554 ? Cl3 Co2 Cl4 110.70(3) 6_554 6_554 ? Cl4 Co2 Cl4 108.99(6) . 6_554 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.888 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.113 data_2_[Co(C5H4-CONHCH2C5H4N)2]+[PF6]- _database_code_depnum_ccdc_archive 'CCDC 269422' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H22 Co F6 N4 O2 P' _chemical_formula_weight 602.36 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 7.232(2) _cell_length_b 12.581(3) _cell_length_c 13.607(7) _cell_angle_alpha 88.91(3) _cell_angle_beta 79.74(3) _cell_angle_gamma 89.46(2) _cell_volume 1218.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.836 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5788 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.1876 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5567 _reflns_number_gt 2029 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+3.4986P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0007(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5567 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2283 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.2134 _refine_ls_wR_factor_gt 0.1443 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _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 0.09648(16) 0.92704(8) 0.23892(7) 0.0445(4) Uani 1 1 d . . . C1 C -0.1363(11) 0.9772(6) 0.1892(6) 0.050(2) Uani 1 1 d . . . H1 H -0.1436 1.0369 0.1487 0.060 Uiso 1 1 calc R . . C2 C -0.0908(11) 0.8732(6) 0.1567(6) 0.054(2) Uani 1 1 d . . . H2 H -0.0656 0.8519 0.0906 0.065 Uiso 1 1 calc R . . C3 C -0.0897(13) 0.8073(7) 0.2399(7) 0.070(3) Uani 1 1 d . . . H3 H -0.0628 0.7348 0.2389 0.085 Uiso 1 1 calc R . . C4 C -0.1364(12) 0.8693(6) 0.3262(7) 0.065(3) Uani 1 1 d . . . H4 H -0.1445 0.8456 0.3919 0.078 Uiso 1 1 calc R . . C5 C -0.1686(10) 0.9743(6) 0.2942(5) 0.0437(19) Uani 1 1 d . . . C6 C -0.2164(10) 1.0635(6) 0.3664(6) 0.0455(19) Uani 1 1 d . . . C7 C -0.2655(11) 1.2531(6) 0.3902(6) 0.052(2) Uani 1 1 d . . . H7A H -0.3705 1.2372 0.4434 0.062 Uiso 1 1 calc R . . H7B H -0.3031 1.3116 0.3506 0.062 Uiso 1 1 calc R . . C8 C -0.1059(11) 1.2869(5) 0.4348(5) 0.0433(19) Uani 1 1 d . . . C9 C -0.1334(13) 1.3418(6) 0.5241(6) 0.057(2) Uani 1 1 d . . . H9 H -0.2546 1.3522 0.5593 0.069 Uiso 1 1 calc R . . C10 C 0.0141(15) 1.3801(6) 0.5600(6) 0.061(2) Uani 1 1 d . . . H10 H -0.0051 1.4162 0.6200 0.073 Uiso 1 1 calc R . . C11 C 0.1910(14) 1.3657(7) 0.5084(7) 0.064(2) Uani 1 1 d . . . H11 H 0.2950 1.3936 0.5301 0.077 Uiso 1 1 calc R . . C12 C 0.2094(13) 1.3076(7) 0.4221(6) 0.063(2) Uani 1 1 d . . . H12 H 0.3303 1.2949 0.3875 0.075 Uiso 1 1 calc R . . C21 C 0.2672(10) 1.0236(6) 0.2973(5) 0.048(2) Uani 1 1 d . . . H21 H 0.2299 1.0762 0.3441 0.057 Uiso 1 1 calc R . . C22 C 0.3063(13) 0.9180(7) 0.3186(6) 0.064(3) Uani 1 1 d . . . H22 H 0.2977 0.8878 0.3821 0.077 Uiso 1 1 calc R . . C23 C 0.3611(13) 0.8644(7) 0.2281(6) 0.064(3) Uani 1 1 d . . . H23 H 0.3958 0.7932 0.2211 0.077 Uiso 1 1 calc R . . C24 C 0.3536(11) 0.9376(6) 0.1511(6) 0.051(2) Uani 1 1 d . . . H24 H 0.3831 0.9234 0.0833 0.061 Uiso 1 1 calc R . . C26 C 0.2940(10) 1.0372(6) 0.1925(5) 0.0409(18) Uani 1 1 d . . . C27 C 0.2629(9) 1.1313(6) 0.1303(5) 0.0374(17) Uani 1 1 d . . . C28 C 0.1606(11) 1.3157(6) 0.1262(6) 0.050(2) Uani 1 1 d . . . H28A H 0.2704 1.3341 0.0770 0.060 Uiso 1 1 calc R . . H28B H 0.1373 1.3733 0.1733 0.060 Uiso 1 1 calc R . . C29 C -0.0030(10) 1.3065(5) 0.0751(5) 0.0376(17) Uani 1 1 d . . . C30 C -0.0162(13) 1.3640(6) -0.0102(6) 0.053(2) Uani 1 1 d . . . H30 H 0.0843 1.4057 -0.0404 0.064 Uiso 1 1 calc R . . C31 C -0.1731(15) 1.3608(7) -0.0506(6) 0.063(3) Uani 1 1 d . . . H31 H -0.1834 1.4025 -0.1066 0.076 Uiso 1 1 calc R . . C32 C -0.3191(12) 1.2947(7) -0.0078(6) 0.055(2) Uani 1 1 d . . . H32 H -0.4297 1.2894 -0.0332 0.066 Uiso 1 1 calc R . . C33 C -0.2890(12) 1.2385(7) 0.0736(6) 0.056(2) Uani 1 1 d . . . H33 H -0.3844 1.1927 0.1025 0.067 Uiso 1 1 calc R . . N1 N -0.2266(9) 1.1602(5) 0.3271(5) 0.0455(17) Uani 1 1 d . . . N2 N 0.0692(9) 1.2691(5) 0.3855(4) 0.0466(16) Uani 1 1 d . . . N3 N 0.2012(8) 1.2193(5) 0.1794(5) 0.0408(15) Uani 1 1 d . . . N4 N -0.1411(9) 1.2412(5) 0.1162(4) 0.0444(15) Uani 1 1 d . . . O1 O -0.2410(9) 1.0453(5) 0.4558(4) 0.0690(18) Uani 1 1 d . . . O2 O 0.2926(7) 1.1261(4) 0.0393(4) 0.0520(14) Uani 1 1 d . . . P1 P -0.4378(3) 1.53689(19) 0.24621(17) 0.0588(7) Uani 1 1 d . . . F1 F -0.6566(7) 1.5563(5) 0.2567(4) 0.103(2) Uani 1 1 d . . . F2 F -0.4601(11) 1.4198(5) 0.2173(6) 0.139(3) Uani 1 1 d . . . F3 F -0.4648(8) 1.4964(4) 0.3583(4) 0.0873(17) Uani 1 1 d . . . F4 F -0.4225(10) 1.6510(5) 0.2895(7) 0.141(3) Uani 1 1 d . . . F5 F -0.4141(9) 1.5772(9) 0.1388(5) 0.199(5) Uani 1 1 d . . . F6 F -0.2210(7) 1.5227(6) 0.2372(5) 0.114(2) Uani 1 1 d . . . H100 H -0.197(10) 1.175(6) 0.270(5) 0.04(2) Uiso 1 1 d . . . H300 H 0.175(7) 1.225(4) 0.243(4) 0.008(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0639(8) 0.0342(6) 0.0331(6) -0.0010(4) -0.0023(5) -0.0006(5) C1 0.052(5) 0.045(5) 0.052(5) -0.009(4) -0.004(4) -0.014(4) C2 0.068(6) 0.048(5) 0.047(5) -0.007(4) -0.011(4) -0.014(4) C3 0.095(7) 0.035(5) 0.078(7) -0.001(5) -0.007(6) -0.024(5) C4 0.082(7) 0.046(5) 0.057(5) 0.003(4) 0.015(5) -0.012(4) C5 0.040(5) 0.053(5) 0.036(4) -0.002(4) 0.000(3) -0.014(4) C6 0.041(5) 0.042(5) 0.050(5) 0.004(4) -0.001(4) -0.003(4) C7 0.039(5) 0.058(5) 0.057(5) -0.008(4) -0.004(4) 0.008(4) C8 0.052(5) 0.037(4) 0.041(4) 0.000(3) -0.006(4) 0.006(4) C9 0.072(6) 0.043(5) 0.051(5) -0.007(4) 0.004(5) 0.017(4) C10 0.098(8) 0.041(5) 0.049(5) -0.009(4) -0.028(6) -0.002(5) C11 0.071(7) 0.056(5) 0.073(6) -0.008(5) -0.029(6) -0.007(5) C12 0.053(6) 0.078(6) 0.056(6) -0.007(5) -0.007(5) 0.000(5) C21 0.048(5) 0.062(5) 0.033(4) -0.001(4) -0.006(4) -0.002(4) C22 0.088(7) 0.058(6) 0.047(5) 0.003(4) -0.012(5) 0.028(5) C23 0.085(7) 0.062(6) 0.044(5) -0.012(4) -0.007(5) 0.030(5) C24 0.059(5) 0.055(5) 0.037(4) -0.007(4) -0.002(4) 0.010(4) C26 0.037(4) 0.050(5) 0.036(4) 0.001(3) -0.008(3) 0.008(3) C27 0.036(4) 0.044(4) 0.030(4) -0.005(3) -0.002(3) -0.008(3) C28 0.046(5) 0.034(4) 0.066(5) -0.006(4) -0.003(4) -0.005(4) C29 0.043(5) 0.025(4) 0.045(4) -0.010(3) -0.005(4) 0.002(3) C30 0.082(7) 0.032(4) 0.041(5) 0.004(3) 0.001(4) 0.002(4) C31 0.099(8) 0.051(5) 0.044(5) 0.000(4) -0.024(5) 0.019(5) C32 0.048(5) 0.062(5) 0.057(5) -0.011(4) -0.014(4) 0.015(5) C33 0.041(5) 0.071(6) 0.054(5) 0.009(4) -0.005(4) -0.002(4) N1 0.053(4) 0.043(4) 0.041(4) 0.002(3) -0.010(3) -0.008(3) N2 0.036(4) 0.060(4) 0.044(4) -0.012(3) -0.007(3) 0.009(3) N3 0.045(4) 0.042(4) 0.034(4) -0.005(3) -0.004(3) -0.005(3) N4 0.041(4) 0.050(4) 0.042(4) 0.004(3) -0.007(3) 0.000(3) O1 0.097(5) 0.069(4) 0.034(3) 0.007(3) 0.008(3) 0.007(3) O2 0.059(4) 0.056(3) 0.037(3) -0.003(2) 0.003(3) -0.005(3) P1 0.0542(15) 0.0651(16) 0.0556(14) 0.0044(12) -0.0063(11) 0.0099(12) F1 0.060(4) 0.166(6) 0.081(4) -0.012(4) -0.007(3) 0.023(4) F2 0.176(7) 0.107(5) 0.144(6) -0.078(5) -0.051(5) 0.013(5) F3 0.117(5) 0.086(4) 0.060(3) 0.006(3) -0.019(3) -0.004(3) F4 0.144(6) 0.053(4) 0.233(9) 0.016(4) -0.054(6) -0.011(4) F5 0.089(5) 0.413(15) 0.081(5) 0.124(7) 0.011(4) 0.060(7) F6 0.055(4) 0.172(6) 0.107(5) 0.029(4) -0.002(3) 0.035(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C4 2.013(8) . ? Co1 C26 2.011(7) . ? Co1 C21 2.012(8) . ? Co1 C22 2.017(9) . ? Co1 C5 2.019(7) . ? Co1 C1 2.014(8) . ? Co1 C3 2.028(8) . ? Co1 C24 2.027(8) . ? Co1 C2 2.032(8) . ? Co1 C23 2.044(9) . ? C1 C5 1.405(10) . ? C1 C2 1.406(10) . ? C1 H1 0.9300 . ? C2 C3 1.391(11) . ? C2 H2 0.9300 . ? C3 C4 1.411(11) . ? C3 H3 0.9300 . ? C4 C5 1.412(11) . ? C4 H4 0.9300 . ? C5 C6 1.503(10) . ? C6 O1 1.216(8) . ? C6 N1 1.325(9) . ? C7 N1 1.459(10) . ? C7 C8 1.467(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N2 1.343(9) . ? C8 C9 1.391(10) . ? C9 C10 1.346(11) . ? C9 H9 0.9300 . ? C10 C11 1.358(12) . ? C10 H10 0.9300 . ? C11 C12 1.380(12) . ? C11 H11 0.9300 . ? C12 N2 1.307(10) . ? C12 H12 0.9300 . ? C21 C22 1.391(10) . ? C21 C26 1.413(9) . ? C21 H21 0.9300 . ? C22 C23 1.407(11) . ? C22 H22 0.9300 . ? C23 C24 1.389(11) . ? C23 H23 0.9300 . ? C24 C26 1.416(10) . ? C24 H24 0.9300 . ? C26 C27 1.480(10) . ? C27 O2 1.222(8) . ? C27 N3 1.335(9) . ? C28 N3 1.455(9) . ? C28 C29 1.481(10) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N4 1.336(8) . ? C29 C30 1.373(10) . ? C30 C31 1.348(11) . ? C30 H30 0.9300 . ? C31 C32 1.387(11) . ? C31 H31 0.9300 . ? C32 C33 1.351(11) . ? C32 H32 0.9300 . ? C33 N4 1.305(9) . ? C33 H33 0.9300 . ? N1 H100 0.79(7) . ? N3 H300 0.86(5) . ? P1 F5 1.519(6) . ? P1 F2 1.549(6) . ? P1 F6 1.560(6) . ? P1 F4 1.574(7) . ? P1 F1 1.580(6) . ? P1 F3 1.577(5) . ? 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 C4 Co1 C26 154.8(3) . . ? C4 Co1 C21 119.7(3) . . ? C26 Co1 C21 41.1(3) . . ? C4 Co1 C22 107.4(4) . . ? C26 Co1 C22 68.6(3) . . ? C21 Co1 C22 40.4(3) . . ? C4 Co1 C5 41.0(3) . . ? C26 Co1 C5 119.3(3) . . ? C21 Co1 C5 106.3(3) . . ? C22 Co1 C5 124.5(3) . . ? C4 Co1 C1 69.1(3) . . ? C26 Co1 C1 106.1(3) . . ? C21 Co1 C1 123.8(3) . . ? C22 Co1 C1 161.0(3) . . ? C5 Co1 C1 40.8(3) . . ? C4 Co1 C3 40.9(3) . . ? C26 Co1 C3 162.3(3) . . ? C21 Co1 C3 155.9(3) . . ? C22 Co1 C3 122.0(4) . . ? C5 Co1 C3 68.4(3) . . ? C1 Co1 C3 68.4(4) . . ? C4 Co1 C24 162.4(3) . . ? C26 Co1 C24 41.0(3) . . ? C21 Co1 C24 68.3(3) . . ? C22 Co1 C24 67.7(3) . . ? C5 Co1 C24 155.7(3) . . ? C1 Co1 C24 121.1(3) . . ? C3 Co1 C24 126.1(3) . . ? C4 Co1 C2 68.3(4) . . ? C26 Co1 C2 125.0(3) . . ? C21 Co1 C2 161.7(3) . . ? C22 Co1 C2 157.0(3) . . ? C5 Co1 C2 68.0(3) . . ? C1 Co1 C2 40.7(3) . . ? C3 Co1 C2 40.1(3) . . ? C24 Co1 C2 109.2(3) . . ? C4 Co1 C23 125.6(4) . . ? C26 Co1 C23 68.6(3) . . ? C21 Co1 C23 68.2(3) . . ? C22 Co1 C23 40.5(3) . . ? C5 Co1 C23 162.2(3) . . ? C1 Co1 C23 156.4(3) . . ? C3 Co1 C23 109.2(4) . . ? C24 Co1 C23 39.9(3) . . ? C2 Co1 C23 122.3(3) . . ? C5 C1 C2 107.4(7) . . ? C5 C1 Co1 69.8(5) . . ? C2 C1 Co1 70.4(5) . . ? C5 C1 H1 126.3 . . ? C2 C1 H1 126.3 . . ? Co1 C1 H1 125.2 . . ? C3 C2 C1 108.7(7) . . ? C3 C2 Co1 69.8(5) . . ? C1 C2 Co1 69.0(5) . . ? C3 C2 H2 125.6 . . ? C1 C2 H2 125.6 . . ? Co1 C2 H2 127.2 . . ? C2 C3 C4 108.2(7) . . ? C2 C3 Co1 70.1(5) . . ? C4 C3 Co1 69.0(5) . . ? C2 C3 H3 125.9 . . ? C4 C3 H3 125.9 . . ? Co1 C3 H3 126.6 . . ? C3 C4 C5 107.3(7) . . ? C3 C4 Co1 70.2(5) . . ? C5 C4 Co1 69.7(4) . . ? C3 C4 H4 126.3 . . ? C5 C4 H4 126.3 . . ? Co1 C4 H4 125.4 . . ? C1 C5 C4 108.3(7) . . ? C1 C5 C6 129.4(7) . . ? C4 C5 C6 122.2(7) . . ? C1 C5 Co1 69.4(4) . . ? C4 C5 Co1 69.3(5) . . ? C6 C5 Co1 123.9(5) . . ? O1 C6 N1 123.4(7) . . ? O1 C6 C5 120.0(7) . . ? N1 C6 C5 116.6(7) . . ? N1 C7 C8 114.0(6) . . ? N1 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? N1 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? N2 C8 C9 119.9(8) . . ? N2 C8 C7 118.9(7) . . ? C9 C8 C7 121.1(7) . . ? C10 C9 C8 120.5(8) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 119.8(8) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 116.9(9) . . ? C10 C11 H11 121.6 . . ? C12 C11 H11 121.6 . . ? N2 C12 C11 124.7(8) . . ? N2 C12 H12 117.6 . . ? C11 C12 H12 117.6 . . ? C22 C21 C26 108.1(7) . . ? C22 C21 Co1 70.0(5) . . ? C26 C21 Co1 69.4(4) . . ? C22 C21 H21 125.9 . . ? C26 C21 H21 125.9 . . ? Co1 C21 H21 126.2 . . ? C21 C22 C23 108.8(7) . . ? C21 C22 Co1 69.6(5) . . ? C23 C22 Co1 70.8(5) . . ? C21 C22 H22 125.6 . . ? C23 C22 H22 125.6 . . ? Co1 C22 H22 125.6 . . ? C24 C23 C22 107.3(7) . . ? C24 C23 Co1 69.4(5) . . ? C22 C23 Co1 68.7(5) . . ? C24 C23 H23 126.4 . . ? C22 C23 H23 126.4 . . ? Co1 C23 H23 127.1 . . ? C23 C24 C26 109.1(7) . . ? C23 C24 Co1 70.7(5) . . ? C26 C24 Co1 68.9(4) . . ? C23 C24 H24 125.5 . . ? C26 C24 H24 125.5 . . ? Co1 C24 H24 126.6 . . ? C21 C26 C24 106.7(7) . . ? C21 C26 C27 130.6(7) . . ? C24 C26 C27 122.7(6) . . ? C21 C26 Co1 69.5(4) . . ? C24 C26 Co1 70.1(4) . . ? C27 C26 Co1 123.4(5) . . ? O2 C27 N3 123.3(7) . . ? O2 C27 C26 120.4(6) . . ? N3 C27 C26 116.3(6) . . ? N3 C28 C29 113.8(6) . . ? N3 C28 H28A 108.8 . . ? C29 C28 H28A 108.8 . . ? N3 C28 H28B 108.8 . . ? C29 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? N4 C29 C30 120.5(7) . . ? N4 C29 C28 117.5(6) . . ? C30 C29 C28 122.0(7) . . ? C31 C30 C29 120.8(8) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C32 119.2(8) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C33 C32 C31 115.2(8) . . ? C33 C32 H32 122.4 . . ? C31 C32 H32 122.4 . . ? N4 C33 C32 127.4(8) . . ? N4 C33 H33 116.3 . . ? C32 C33 H33 116.3 . . ? C6 N1 C7 121.2(7) . . ? C6 N1 H100 125(6) . . ? C7 N1 H100 113(6) . . ? C12 N2 C8 118.1(7) . . ? C27 N3 C28 121.2(6) . . ? C27 N3 H300 126(4) . . ? C28 N3 H300 113(3) . . ? C33 N4 C29 116.8(7) . . ? F5 P1 F2 93.3(6) . . ? F5 P1 F6 91.1(4) . . ? F2 P1 F6 91.5(4) . . ? F5 P1 F4 93.7(6) . . ? F2 P1 F4 172.9(5) . . ? F6 P1 F4 89.5(4) . . ? F5 P1 F1 88.9(3) . . ? F2 P1 F1 90.9(4) . . ? F6 P1 F1 177.6(4) . . ? F4 P1 F1 88.1(4) . . ? F5 P1 F3 179.1(5) . . ? F2 P1 F3 87.3(4) . . ? F6 P1 F3 89.6(3) . . ? F4 P1 F3 85.7(4) . . ? F1 P1 F3 90.4(3) . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.393 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.090 data_3_[Co(C5H4-CON(C5H4N)2)2]+[PF6]- _database_code_depnum_ccdc_archive 'CCDC 269423' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 Co F6 N6 O2 P' _chemical_formula_weight 728.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' Co Co 0.3490 0.9720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.186(3) _cell_length_b 12.622(3) _cell_length_c 13.089(4) _cell_angle_alpha 64.82(2) _cell_angle_beta 67.27(3) _cell_angle_gamma 80.85(2) _cell_volume 1542.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 0.686 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5668 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.1510 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 24.97 _reflns_number_total 5410 _reflns_number_gt 2372 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1161P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5410 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1955 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.2220 _refine_ls_wR_factor_gt 0.1650 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 C1 C 0.3123(7) 0.1634(6) 0.0044(8) 0.047(2) Uani 1 1 d . . . H1 H 0.3560 0.1671 -0.0736 0.057 Uiso 1 1 calc R . . C2 C 0.2865(8) 0.2578(7) 0.0370(9) 0.050(2) Uani 1 1 d . . . H2 H 0.3104 0.3351 -0.0150 0.060 Uiso 1 1 calc R . . C3 C 0.2188(8) 0.2174(7) 0.1608(9) 0.051(2) Uani 1 1 d . . . H3 H 0.1887 0.2635 0.2053 0.061 Uiso 1 1 calc R . . C4 C 0.2032(7) 0.0953(6) 0.2078(7) 0.0434(19) Uani 1 1 d . . . H4 H 0.1626 0.0460 0.2883 0.052 Uiso 1 1 calc R . . C5 C 0.2623(7) 0.0617(6) 0.1071(7) 0.0384(18) Uani 1 1 d . . . C6 C 0.2593(7) -0.0570(6) 0.1067(7) 0.0409(18) Uani 1 1 d . . . C7 C 0.3753(7) -0.1229(6) 0.2472(7) 0.0415(18) Uani 1 1 d . . . C8 C 0.3349(11) -0.1725(8) 0.3704(9) 0.078(3) Uani 1 1 d . . . H8 H 0.2613 -0.2199 0.4168 0.093 Uiso 1 1 calc R . . C9 C 0.5446(9) -0.0372(8) 0.2341(10) 0.069(3) Uani 1 1 d . . . H9 H 0.6169 0.0115 0.1859 0.083 Uiso 1 1 calc R . . C10 C 0.5157(13) -0.0823(10) 0.3533(12) 0.084(3) Uani 1 1 d . . . H10 H 0.5678 -0.0681 0.3869 0.101 Uiso 1 1 calc R . . C11 C 0.4077(14) -0.1496(11) 0.4234(11) 0.102(4) Uani 1 1 d . . . H11 H 0.3825 -0.1804 0.5071 0.122 Uiso 1 1 calc R . . C12 C 0.2906(7) -0.2649(6) 0.2102(7) 0.0395(17) Uani 1 1 d . . . C13 C 0.1798(8) -0.3073(7) 0.2236(7) 0.052(2) Uani 1 1 d . . . H13 H 0.1094 -0.2584 0.2161 0.062 Uiso 1 1 calc R . . C14 C 0.1721(9) -0.4241(8) 0.2485(8) 0.060(2) Uani 1 1 d . . . H14 H 0.0968 -0.4561 0.2588 0.072 Uiso 1 1 calc R . . C15 C 0.2811(9) -0.4927(7) 0.2578(8) 0.059(2) Uani 1 1 d . . . H15 H 0.2808 -0.5718 0.2736 0.071 Uiso 1 1 calc R . . C16 C 0.3865(9) -0.4419(7) 0.2434(8) 0.058(2) Uani 1 1 d . . . H16 H 0.4578 -0.4891 0.2520 0.069 Uiso 1 1 calc R . . C17 C 0.0265(8) 0.2945(6) -0.0261(8) 0.049(2) Uani 1 1 d . . . H17 H 0.0607 0.3641 -0.0916 0.059 Uiso 1 1 calc R . . C18 C 0.0326(9) 0.1826(8) -0.0297(9) 0.058(2) Uani 1 1 d . . . H18 H 0.0707 0.1660 -0.0981 0.070 Uiso 1 1 calc R . . C19 C -0.0289(8) 0.1024(7) 0.0881(9) 0.055(2) Uani 1 1 d . . . H19 H -0.0375 0.0224 0.1122 0.066 Uiso 1 1 calc R . . C20 C -0.0754(7) 0.1631(6) 0.1636(8) 0.0435(19) Uani 1 1 d . . . H20 H -0.1219 0.1303 0.2462 0.052 Uiso 1 1 calc R . . C21 C -0.0407(7) 0.2811(6) 0.0945(7) 0.0398(18) Uani 1 1 d . . . C22 C -0.0617(7) 0.3754(6) 0.1403(7) 0.0348(16) Uani 1 1 d . . . C23 C -0.2931(7) 0.3489(6) 0.1913(7) 0.0373(17) Uani 1 1 d . . . C24 C -0.2987(8) 0.3804(7) 0.0801(8) 0.052(2) Uani 1 1 d . . . H24 H -0.2382 0.4316 0.0106 0.063 Uiso 1 1 calc R . . C25 C -0.3971(9) 0.3335(10) 0.0752(10) 0.074(3) Uani 1 1 d . . . H25 H -0.4034 0.3504 0.0011 0.089 Uiso 1 1 calc R . . C26 C -0.4854(10) 0.2625(9) 0.1785(11) 0.073(3) Uani 1 1 d . . . H26 H -0.5526 0.2296 0.1764 0.087 Uiso 1 1 calc R . . C27 C -0.4739(8) 0.2403(8) 0.2851(9) 0.066(3) Uani 1 1 d . . . H27 H -0.5372 0.1945 0.3562 0.080 Uiso 1 1 calc R . . C28 C -0.2231(7) 0.4580(6) 0.2749(7) 0.0385(17) Uani 1 1 d . . . C29 C -0.1633(8) 0.4364(7) 0.3556(8) 0.053(2) Uani 1 1 d . . . H29 H -0.1008 0.3786 0.3650 0.064 Uiso 1 1 calc R . . C30 C -0.1996(10) 0.5042(9) 0.4226(9) 0.076(3) Uani 1 1 d . . . H30 H -0.1594 0.4958 0.4759 0.091 Uiso 1 1 calc R . . C31 C -0.2975(11) 0.5849(9) 0.4077(9) 0.076(3) Uani 1 1 d . . . H31 H -0.3257 0.6305 0.4527 0.091 Uiso 1 1 calc R . . C32 C -0.3518(9) 0.5968(8) 0.3271(9) 0.070(3) Uani 1 1 d . . . H32 H -0.4176 0.6513 0.3182 0.085 Uiso 1 1 calc R . . Co1 Co 0.11990(10) 0.18172(8) 0.08128(10) 0.0361(3) Uani 1 1 d . . . N1 N 0.4777(6) -0.0566(6) 0.1788(6) 0.0511(17) Uani 1 1 d . . . N2 N 0.3967(6) -0.3283(5) 0.2176(6) 0.0465(16) Uani 1 1 d . . . N3 N -0.3755(6) 0.2813(6) 0.2932(6) 0.0487(16) Uani 1 1 d . . . N4 N -0.3152(7) 0.5339(6) 0.2595(6) 0.0535(18) Uani 1 1 d . . . N5 N 0.3040(5) -0.1468(5) 0.1901(5) 0.0383(14) Uani 1 1 d . . . N6 N -0.1878(5) 0.3912(5) 0.2021(6) 0.0390(15) Uani 1 1 d . . . O1 O 0.2189(6) -0.0696(4) 0.0402(5) 0.0577(16) Uani 1 1 d . . . O2 O 0.0256(5) 0.4303(4) 0.1260(5) 0.0457(13) Uani 1 1 d . . . F1 F 0.9391(11) 0.7071(7) 0.4718(8) 0.188(4) Uani 1 1 d . . . F2 F 0.8467(15) 0.9536(7) 0.4405(10) 0.288(9) Uani 1 1 d . . . F3 F 0.918(3) 0.8102(14) 0.5604(14) 0.352(12) Uani 1 1 d . . . F4 F 0.8555(18) 0.8470(14) 0.3552(15) 0.308(9) Uani 1 1 d . . . F5 F 0.7623(10) 0.7809(11) 0.5363(16) 0.339(12) Uani 1 1 d . . . F6 F 1.0139(10) 0.8759(9) 0.3621(11) 0.218(6) Uani 1 1 d . . . P1 P 0.8879(3) 0.8322(2) 0.4580(3) 0.0767(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.040(4) 0.043(4) 0.059(6) -0.026(4) -0.015(4) 0.010(3) C2 0.046(5) 0.036(4) 0.074(7) -0.019(4) -0.031(5) 0.002(4) C3 0.049(5) 0.052(5) 0.082(7) -0.041(5) -0.041(5) 0.014(4) C4 0.044(4) 0.049(5) 0.042(5) -0.022(4) -0.019(4) 0.010(4) C5 0.041(4) 0.032(4) 0.049(5) -0.018(4) -0.025(4) 0.008(3) C6 0.045(4) 0.031(4) 0.049(5) -0.019(4) -0.018(4) 0.006(3) C7 0.048(5) 0.041(4) 0.044(5) -0.022(4) -0.025(4) 0.016(4) C8 0.106(8) 0.069(6) 0.057(7) -0.014(5) -0.036(6) -0.010(6) C9 0.072(6) 0.077(6) 0.091(8) -0.050(6) -0.044(6) 0.002(5) C10 0.116(10) 0.089(8) 0.095(9) -0.050(7) -0.074(8) 0.011(7) C11 0.150(12) 0.115(10) 0.062(8) -0.028(7) -0.063(8) -0.016(9) C12 0.043(4) 0.038(4) 0.038(5) -0.016(4) -0.015(4) 0.003(3) C13 0.050(5) 0.047(5) 0.063(6) -0.022(4) -0.027(5) 0.009(4) C14 0.058(6) 0.064(6) 0.067(6) -0.033(5) -0.020(5) -0.011(5) C15 0.075(6) 0.042(5) 0.073(7) -0.032(5) -0.033(5) 0.008(4) C16 0.073(6) 0.041(5) 0.074(7) -0.032(5) -0.038(5) 0.020(4) C17 0.063(5) 0.039(4) 0.064(6) -0.023(4) -0.046(5) 0.016(4) C18 0.071(6) 0.065(6) 0.072(7) -0.047(5) -0.045(6) 0.023(5) C19 0.061(5) 0.045(5) 0.085(7) -0.039(5) -0.043(5) 0.011(4) C20 0.040(4) 0.032(4) 0.056(5) -0.015(4) -0.015(4) -0.009(3) C21 0.041(4) 0.028(4) 0.058(6) -0.017(4) -0.029(4) 0.007(3) C22 0.032(4) 0.031(4) 0.044(5) -0.013(3) -0.019(4) -0.001(3) C23 0.045(4) 0.038(4) 0.041(5) -0.020(4) -0.025(4) 0.008(3) C24 0.050(5) 0.059(5) 0.048(5) -0.020(4) -0.023(4) 0.006(4) C25 0.059(6) 0.120(9) 0.071(7) -0.049(7) -0.042(6) 0.011(6) C26 0.067(7) 0.094(8) 0.093(8) -0.049(7) -0.049(7) -0.005(6) C27 0.039(5) 0.070(6) 0.083(7) -0.022(5) -0.019(5) -0.016(4) C28 0.036(4) 0.039(4) 0.041(5) -0.014(4) -0.014(4) -0.007(3) C29 0.047(5) 0.057(5) 0.059(6) -0.024(4) -0.023(4) 0.002(4) C30 0.091(8) 0.096(8) 0.060(7) -0.035(6) -0.038(6) -0.010(6) C31 0.096(8) 0.085(7) 0.070(7) -0.056(6) -0.025(6) 0.001(6) C32 0.066(6) 0.071(6) 0.095(8) -0.060(6) -0.025(6) 0.013(5) Co1 0.0412(6) 0.0287(5) 0.0461(7) -0.0181(5) -0.0229(5) 0.0078(4) N1 0.043(4) 0.062(4) 0.057(5) -0.032(4) -0.020(4) 0.009(3) N2 0.052(4) 0.042(4) 0.054(4) -0.024(3) -0.028(4) 0.014(3) N3 0.047(4) 0.059(4) 0.035(4) -0.013(3) -0.012(3) -0.011(3) N4 0.061(4) 0.057(4) 0.064(5) -0.040(4) -0.032(4) 0.017(3) N5 0.041(3) 0.031(3) 0.051(4) -0.021(3) -0.023(3) 0.008(3) N6 0.032(3) 0.039(3) 0.054(4) -0.023(3) -0.019(3) 0.002(3) O1 0.085(4) 0.046(3) 0.069(4) -0.029(3) -0.054(4) 0.014(3) O2 0.041(3) 0.036(3) 0.063(4) -0.022(3) -0.018(3) -0.002(2) F1 0.257(11) 0.091(6) 0.144(8) -0.034(5) -0.024(7) 0.029(6) F2 0.43(2) 0.083(6) 0.171(10) -0.042(7) 0.045(11) 0.056(9) F3 0.70(4) 0.284(17) 0.197(13) -0.126(13) -0.29(2) 0.09(2) F4 0.41(2) 0.302(18) 0.302(18) -0.041(15) -0.285(19) -0.047(17) F5 0.099(7) 0.218(12) 0.347(19) 0.080(13) 0.067(10) -0.015(8) F6 0.141(8) 0.175(9) 0.236(12) -0.090(8) 0.072(8) -0.071(7) P1 0.0706(19) 0.0689(18) 0.0639(19) -0.0113(15) -0.0088(16) -0.0135(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 C1 C2 1.384(10) . ? C1 C5 1.395(10) . ? C1 Co1 2.016(7) . ? C2 C3 1.389(11) . ? C2 Co1 1.998(8) . ? C3 C4 1.407(10) . ? C3 Co1 1.989(7) . ? C4 C5 1.437(10) . ? C4 Co1 2.033(7) . ? C5 C6 1.507(9) . ? C5 Co1 2.039(7) . ? C6 O1 1.196(8) . ? C6 N5 1.384(9) . ? C7 N1 1.300(9) . ? C7 C8 1.365(11) . ? C7 N5 1.418(9) . ? C8 C11 1.383(13) . ? C9 N1 1.331(10) . ? C9 C10 1.332(13) . ? C10 C11 1.352(15) . ? C12 N2 1.333(8) . ? C12 C13 1.348(10) . ? C12 N5 1.423(8) . ? C13 C14 1.376(11) . ? C14 C15 1.392(11) . ? C15 C16 1.342(11) . ? C16 N2 1.339(9) . ? C17 C21 1.407(11) . ? C17 C18 1.423(10) . ? C17 Co1 2.013(7) . ? C18 C19 1.396(12) . ? C18 Co1 2.035(8) . ? C19 C20 1.397(11) . ? C19 Co1 2.030(8) . ? C20 C21 1.398(9) . ? C20 Co1 2.029(7) . ? C21 C22 1.496(10) . ? C21 Co1 2.015(7) . ? C22 O2 1.197(7) . ? C22 N6 1.360(9) . ? C23 N3 1.299(9) . ? C23 C24 1.361(10) . ? C23 N6 1.445(8) . ? C24 C25 1.363(11) . ? C25 C26 1.350(13) . ? C26 C27 1.355(12) . ? C27 N3 1.344(9) . ? C28 N4 1.305(9) . ? C28 C29 1.371(10) . ? C28 N6 1.436(9) . ? C29 C30 1.385(12) . ? C30 C31 1.383(13) . ? C31 C32 1.356(12) . ? C32 N4 1.341(10) . ? F1 P1 1.550(8) . ? F2 P1 1.474(8) . ? F3 P1 1.408(11) . ? F4 P1 1.455(12) . ? F5 P1 1.434(9) . ? F6 P1 1.468(8) . ? 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 C2 C1 C5 109.2(8) . . ? C2 C1 Co1 69.1(4) . . ? C5 C1 Co1 70.8(4) . . ? C1 C2 C3 108.4(7) . . ? C1 C2 Co1 70.5(4) . . ? C3 C2 Co1 69.3(4) . . ? C2 C3 C4 108.8(7) . . ? C2 C3 Co1 69.9(5) . . ? C4 C3 Co1 71.2(4) . . ? C3 C4 C5 106.5(7) . . ? C3 C4 Co1 67.9(4) . . ? C5 C4 Co1 69.6(4) . . ? C1 C5 C4 107.1(6) . . ? C1 C5 C6 124.9(7) . . ? C4 C5 C6 127.6(7) . . ? C1 C5 Co1 69.0(4) . . ? C4 C5 Co1 69.1(4) . . ? C6 C5 Co1 121.9(5) . . ? O1 C6 N5 124.6(6) . . ? O1 C6 C5 121.2(6) . . ? N5 C6 C5 114.1(6) . . ? N1 C7 C8 123.4(8) . . ? N1 C7 N5 117.9(7) . . ? C8 C7 N5 118.7(8) . . ? C7 C8 C11 117.4(10) . . ? N1 C9 C10 125.0(10) . . ? C9 C10 C11 117.4(10) . . ? C10 C11 C8 119.9(11) . . ? N2 C12 C13 124.4(7) . . ? N2 C12 N5 113.1(6) . . ? C13 C12 N5 122.5(6) . . ? C12 C13 C14 119.1(7) . . ? C13 C14 C15 117.7(8) . . ? C16 C15 C14 118.4(8) . . ? N2 C16 C15 124.9(8) . . ? C21 C17 C18 107.7(8) . . ? C21 C17 Co1 69.6(4) . . ? C18 C17 Co1 70.2(4) . . ? C19 C18 C17 107.6(8) . . ? C19 C18 Co1 69.7(5) . . ? C17 C18 Co1 68.6(4) . . ? C18 C19 C20 108.2(7) . . ? C18 C19 Co1 70.1(5) . . ? C20 C19 Co1 69.9(4) . . ? C19 C20 C21 108.9(7) . . ? C19 C20 Co1 69.9(5) . . ? C21 C20 Co1 69.2(4) . . ? C20 C21 C17 107.6(7) . . ? C20 C21 C22 126.7(7) . . ? C17 C21 C22 125.5(7) . . ? C20 C21 Co1 70.3(4) . . ? C17 C21 Co1 69.5(4) . . ? C22 C21 Co1 122.2(5) . . ? O2 C22 N6 122.9(6) . . ? O2 C22 C21 122.7(6) . . ? N6 C22 C21 114.4(6) . . ? N3 C23 C24 125.7(7) . . ? N3 C23 N6 114.7(6) . . ? C24 C23 N6 119.6(7) . . ? C23 C24 C25 116.8(8) . . ? C26 C25 C24 119.8(9) . . ? C25 C26 C27 118.6(8) . . ? N3 C27 C26 123.2(9) . . ? N4 C28 C29 125.4(7) . . ? N4 C28 N6 114.9(6) . . ? C29 C28 N6 119.6(7) . . ? C28 C29 C30 117.4(8) . . ? C31 C30 C29 118.0(8) . . ? C32 C31 C30 119.4(9) . . ? N4 C32 C31 123.1(9) . . ? C3 Co1 C2 40.8(3) . . ? C3 Co1 C17 127.9(3) . . ? C2 Co1 C17 107.5(3) . . ? C3 Co1 C21 107.6(3) . . ? C2 Co1 C21 117.5(3) . . ? C17 Co1 C21 40.9(3) . . ? C3 Co1 C1 68.3(3) . . ? C2 Co1 C1 40.3(3) . . ? C17 Co1 C1 117.5(4) . . ? C21 Co1 C1 150.8(3) . . ? C3 Co1 C20 118.3(4) . . ? C2 Co1 C20 151.5(3) . . ? C17 Co1 C20 68.1(3) . . ? C21 Co1 C20 40.5(3) . . ? C1 Co1 C20 167.3(3) . . ? C3 Co1 C19 151.6(4) . . ? C2 Co1 C19 166.6(4) . . ? C17 Co1 C19 68.5(3) . . ? C21 Co1 C19 68.4(3) . . ? C1 Co1 C19 129.1(3) . . ? C20 Co1 C19 40.3(3) . . ? C3 Co1 C4 40.9(3) . . ? C2 Co1 C4 68.7(3) . . ? C17 Co1 C4 166.6(3) . . ? C21 Co1 C4 128.4(3) . . ? C1 Co1 C4 68.5(3) . . ? C20 Co1 C4 108.8(3) . . ? C19 Co1 C4 118.2(3) . . ? C3 Co1 C18 166.8(4) . . ? C2 Co1 C18 128.6(4) . . ? C17 Co1 C18 41.2(3) . . ? C21 Co1 C18 68.7(3) . . ? C1 Co1 C18 108.4(4) . . ? C20 Co1 C18 67.7(4) . . ? C19 Co1 C18 40.2(3) . . ? C4 Co1 C18 151.1(3) . . ? C3 Co1 C5 68.9(3) . . ? C2 Co1 C5 68.2(3) . . ? C17 Co1 C5 150.6(3) . . ? C21 Co1 C5 167.6(3) . . ? C1 Co1 C5 40.2(3) . . ? C20 Co1 C5 129.7(3) . . ? C19 Co1 C5 108.6(3) . . ? C4 Co1 C5 41.3(3) . . ? C18 Co1 C5 117.4(3) . . ? C7 N1 C9 116.9(8) . . ? C12 N2 C16 115.4(7) . . ? C23 N3 C27 115.7(7) . . ? C28 N4 C32 116.6(7) . . ? C6 N5 C7 121.1(6) . . ? C6 N5 C12 119.8(6) . . ? C7 N5 C12 118.8(6) . . ? C22 N6 C28 121.6(6) . . ? C22 N6 C23 121.8(6) . . ? C28 N6 C23 116.4(6) . . ? F3 P1 F5 89.2(11) . . ? F3 P1 F4 176.3(10) . . ? F5 P1 F4 88.8(12) . . ? F3 P1 F6 100.3(12) . . ? F5 P1 F6 168.9(11) . . ? F4 P1 F6 81.5(9) . . ? F3 P1 F2 94.2(9) . . ? F5 P1 F2 95.5(8) . . ? F4 P1 F2 89.0(9) . . ? F6 P1 F2 89.6(7) . . ? F3 P1 F1 85.8(8) . . ? F5 P1 F1 87.7(7) . . ? F4 P1 F1 91.1(8) . . ? F6 P1 F1 87.2(6) . . ? F2 P1 F1 176.8(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.676 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.093 data_4_[Co(C5H4-CON(C5H4N)2)(C5H4-COOH)]+[PF6]- _database_code_depnum_ccdc_archive 'CCDC 269424' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H17 Co F6 N3 O3 P' _chemical_formula_weight 575.29 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 10.034(2) _cell_length_b 24.647(5) _cell_length_c 9.579(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.70(3) _cell_angle_gamma 90.00 _cell_volume 2243.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 0.918 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.857 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4859 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 24.97 _reflns_number_total 2513 _reflns_number_gt 1969 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0964P)^2^+4.8679P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2513 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 0.725 _refine_ls_restrained_S_all 0.725 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.003 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 0.19361(5) 0.38700(3) 0.50360(5) 0.0364(3) Uani 1 1 d . . . C1 C 0.0021(3) 0.42169(14) 0.4062(3) 0.0396(15) Uani 1 1 d G . . H1 H -0.0176 0.4586 0.3937 0.047 Uiso 1 1 calc R . . C2 C 0.0387(3) 0.38725(17) 0.3053(2) 0.050(2) Uani 1 1 d G . . H2 H 0.0471 0.3976 0.2151 0.059 Uiso 1 1 calc R . . C3 C 0.0601(3) 0.33419(15) 0.3662(3) 0.0477(18) Uani 1 1 d G . . H3 H 0.0850 0.3037 0.3229 0.057 Uiso 1 1 calc R . . C4 C 0.0368(3) 0.33584(14) 0.5047(3) 0.0406(17) Uani 1 1 d G . . H4 H 0.0437 0.3066 0.5681 0.049 Uiso 1 1 calc R . . C5 C 0.0010(3) 0.38992(15) 0.5294(2) 0.0326(16) Uani 1 1 d G . . C6 C -0.0331(4) 0.4143(3) 0.6570(4) 0.0373(17) Uani 1 1 d . . . C7 C -0.2084(4) 0.3447(3) 0.6098(5) 0.035(2) Uani 1 1 d . . . C8 C -0.1903(5) 0.2923(3) 0.6568(6) 0.050(2) Uani 1 1 d . . . H8 H -0.1333 0.2842 0.7521 0.060 Uiso 1 1 calc R . . C10 C -0.2569(6) 0.2513(3) 0.5624(7) 0.068(2) Uani 1 1 d . . . H10 H -0.2456 0.2151 0.5907 0.081 Uiso 1 1 calc R . . C11 C -0.3419(6) 0.2669(4) 0.4223(7) 0.066(3) Uani 1 1 d . . . H11 H -0.3892 0.2406 0.3548 0.079 Uiso 1 1 calc R . . C12 C -0.3560(5) 0.3199(4) 0.3841(6) 0.054(3) Uani 1 1 d . . . H12 H -0.4137 0.3294 0.2902 0.065 Uiso 1 1 calc R . . C13 C -0.1830(4) 0.4055(2) 0.8178(4) 0.0387(16) Uani 1 1 d . . . C14 C -0.1371(5) 0.4512(3) 0.8981(6) 0.082(2) Uani 1 1 d . . . H14 H -0.0665 0.4726 0.8832 0.098 Uiso 1 1 calc R . . C15 C -0.1993(6) 0.4648(4) 1.0026(6) 0.095(3) Uani 1 1 d . . . H15 H -0.1711 0.4960 1.0591 0.114 Uiso 1 1 calc R . . C16 C -0.3010(5) 0.4330(3) 1.0231(5) 0.067(2) Uani 1 1 d . . . H16 H -0.3437 0.4418 1.0931 0.080 Uiso 1 1 calc R . . C17 C -0.3384(5) 0.3884(3) 0.9397(5) 0.057(2) Uani 1 1 d . . . H17 H -0.4081 0.3664 0.9541 0.069 Uiso 1 1 calc R . . C20 C 0.3386(3) 0.4173(2) 0.6873(3) 0.048(2) Uani 1 1 d G . . H20 H 0.3204 0.4337 0.7667 0.057 Uiso 1 1 calc R . . C21 C 0.3607(3) 0.36097(19) 0.6722(4) 0.060(2) Uani 1 1 d G . . H21 H 0.3594 0.3341 0.7399 0.072 Uiso 1 1 calc R . . C22 C 0.3849(3) 0.35293(16) 0.5355(4) 0.057(2) Uani 1 1 d G . . H22 H 0.4024 0.3199 0.4980 0.068 Uiso 1 1 calc R . . C23 C 0.3778(3) 0.40427(19) 0.4662(3) 0.0462(18) Uani 1 1 d G . . H23 H 0.3898 0.4107 0.3753 0.055 Uiso 1 1 calc R . . C24 C 0.3492(3) 0.44403(16) 0.5600(4) 0.042(2) Uani 1 1 d G . . C25 C 0.3347(4) 0.5044(3) 0.5135(5) 0.056(2) Uani 1 1 d . . . N1 N -0.1327(3) 0.38750(17) 0.7004(3) 0.0332(12) Uani 1 1 d . . . N2 N -0.2811(4) 0.37373(18) 0.8363(4) 0.0467(13) Uani 1 1 d . . . N3 N -0.2898(3) 0.3588(2) 0.4765(4) 0.0370(13) Uani 1 1 d . . . O1 O 0.0238(3) 0.45572(17) 0.7111(3) 0.0471(11) Uani 1 1 d . . . O2 O 0.3112(4) 0.53341(18) 0.6135(4) 0.0685(13) Uani 1 1 d . . . H200 H 0.3186 0.5890 0.5602 0.050 Uiso 1 1 d . . . O3 O 0.3503(3) 0.51797(18) 0.4033(4) 0.0674(13) Uani 1 1 d . . . P1 P 0.24048(14) 0.31959(9) 1.02587(13) 0.0548(7) Uani 1 1 d . . . F1 F 0.3857(4) 0.3324(3) 1.0187(4) 0.166(3) Uani 1 1 d . A . F2 F 0.0914(5) 0.3051(3) 1.0347(5) 0.154(2) Uani 1 1 d . A . F3A F 0.166(2) 0.3744(6) 1.052(3) 0.161(7) Uani 0.45 1 d P A 1 F4A F 0.295(3) 0.2675(8) 1.001(4) 0.209(10) Uani 0.45 1 d P A 1 F5A F 0.304(2) 0.319(2) 1.1932(18) 0.149(15) Uani 0.45 1 d P A 1 F6A F 0.1714(13) 0.3352(19) 0.8634(17) 0.183(16) Uani 0.45 1 d P A 1 F3B F 0.2078(17) 0.3711(6) 0.944(2) 0.178(8) Uani 0.55 1 d P A 2 F4B F 0.273(2) 0.2646(9) 1.110(3) 0.174(7) Uani 0.55 1 d P A 2 F5B F 0.285(2) 0.3468(11) 1.1740(17) 0.126(11) Uani 0.55 1 d P A 2 F6B F 0.1903(19) 0.2916(9) 0.8731(14) 0.137(9) Uani 0.55 1 d P A 2 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 0.0335(3) 0.0399(9) 0.0420(3) -0.0007(3) 0.0208(2) -0.0012(3) C1 0.0354(18) 0.041(5) 0.044(2) 0.004(2) 0.0152(16) 0.002(2) C2 0.044(2) 0.066(7) 0.042(2) -0.006(3) 0.0182(17) 0.000(3) C3 0.050(2) 0.039(6) 0.061(3) -0.024(3) 0.028(2) -0.007(3) C4 0.042(2) 0.033(6) 0.054(2) 0.000(3) 0.0262(18) -0.007(2) C5 0.0313(17) 0.027(6) 0.043(2) 0.001(2) 0.0171(15) -0.002(2) C6 0.0336(19) 0.038(6) 0.043(2) -0.005(2) 0.0173(17) -0.002(2) C7 0.038(2) 0.024(7) 0.052(3) -0.007(3) 0.0271(19) -0.009(3) C8 0.066(3) 0.027(8) 0.065(3) -0.007(4) 0.034(2) -0.013(3) C10 0.097(4) 0.030(7) 0.092(4) -0.013(4) 0.053(4) -0.019(4) C11 0.072(3) 0.055(10) 0.080(4) -0.034(4) 0.037(3) -0.025(4) C12 0.048(2) 0.059(9) 0.056(3) -0.021(4) 0.019(2) -0.012(3) C13 0.0347(18) 0.050(6) 0.0336(19) -0.002(2) 0.0146(15) 0.000(2) C14 0.077(3) 0.113(8) 0.074(3) -0.053(4) 0.050(3) -0.051(4) C15 0.091(4) 0.131(9) 0.081(4) -0.066(4) 0.051(3) -0.046(4) C16 0.057(3) 0.104(8) 0.047(3) -0.017(3) 0.029(2) -0.008(3) C17 0.052(2) 0.074(7) 0.058(3) 0.005(3) 0.034(2) -0.001(3) C20 0.040(2) 0.059(7) 0.044(2) -0.004(3) 0.0129(17) -0.002(3) C21 0.040(2) 0.075(8) 0.061(3) 0.023(3) 0.0128(19) 0.005(3) C22 0.038(2) 0.055(7) 0.085(4) 0.003(4) 0.030(2) 0.009(3) C23 0.040(2) 0.047(6) 0.061(3) -0.004(3) 0.0292(19) -0.003(2) C24 0.0311(19) 0.032(7) 0.063(3) 0.005(3) 0.0167(17) -0.002(2) C25 0.0315(19) 0.092(8) 0.048(3) -0.021(3) 0.0156(17) -0.009(3) N1 0.0366(15) 0.028(4) 0.0400(16) -0.0059(18) 0.0199(13) -0.0069(18) N2 0.054(2) 0.038(4) 0.061(2) 0.004(2) 0.0360(17) -0.001(2) N3 0.0361(16) 0.026(5) 0.051(2) -0.005(2) 0.0170(15) 0.0027(19) O1 0.0573(18) 0.039(4) 0.0542(17) -0.0094(19) 0.0306(15) -0.012(2) O2 0.069(2) 0.069(5) 0.071(2) -0.004(2) 0.0291(17) -0.008(2) O3 0.067(2) 0.072(4) 0.066(2) 0.007(2) 0.0258(17) 0.001(2) P1 0.0640(7) 0.063(3) 0.0418(6) -0.0020(8) 0.0236(5) -0.0042(8) F1 0.087(3) 0.330(9) 0.096(3) 0.007(4) 0.049(2) -0.054(4) F2 0.100(3) 0.254(8) 0.117(3) -0.012(4) 0.048(3) -0.051(4) F3A 0.237(17) 0.087(16) 0.222(17) 0.003(11) 0.162(16) 0.078(12) F4A 0.29(2) 0.067(19) 0.26(4) 0.03(2) 0.15(3) 0.099(17) F5A 0.098(9) 0.29(4) 0.048(6) 0.027(14) 0.007(5) -0.043(16) F6A 0.068(6) 0.42(5) 0.068(8) 0.104(17) 0.028(5) 0.038(14) F3B 0.29(2) 0.056(13) 0.159(12) 0.063(11) 0.031(12) 0.062(11) F4B 0.273(18) 0.072(17) 0.201(17) 0.094(13) 0.109(14) 0.007(12) F5B 0.145(12) 0.15(2) 0.097(13) -0.087(14) 0.058(11) -0.013(11) F6B 0.188(14) 0.17(2) 0.067(7) -0.063(10) 0.055(7) -0.091(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 C4 2.019(3) . ? Co1 C3 2.023(3) . ? Co1 C21 2.023(3) . ? Co1 C5 2.027(2) . ? Co1 C20 2.032(3) . ? Co1 C22 2.026(3) . ? Co1 C24 2.041(3) . ? Co1 C2 2.033(3) . ? Co1 C23 2.037(3) . ? Co1 C1 2.036(3) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C2 C3 1.4200 . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C5 C6 1.496(5) . ? C6 O1 1.203(6) . ? C6 N1 1.369(5) . ? C7 N3 1.322(6) . ? C7 C8 1.361(7) . ? C7 N1 1.421(7) . ? C8 C10 1.378(8) . ? C10 C11 1.393(9) . ? C11 C12 1.351(8) . ? C12 N3 1.330(7) . ? C13 N2 1.314(5) . ? C13 C14 1.359(7) . ? C13 N1 1.442(5) . ? C14 C15 1.380(6) . ? C15 C16 1.350(8) . ? C16 C17 1.340(8) . ? C17 N2 1.345(6) . ? C20 C21 1.4200 . ? C20 C24 1.4200 . ? C21 C22 1.4200 . ? C22 C23 1.4200 . ? C23 C24 1.4200 . ? C24 C25 1.547(8) . ? C25 O3 1.165(6) . ? C25 O2 1.276(6) . ? P1 F4A 1.443(15) . ? P1 F1 1.514(4) . ? P1 F3B 1.473(12) . ? P1 F5B 1.502(14) . ? P1 F2 1.566(4) . ? P1 F6A 1.536(13) . ? P1 F5A 1.524(17) . ? P1 F4B 1.557(14) . ? P1 F3A 1.599(12) . ? P1 F6B 1.550(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Co1 C3 41.14(6) . . ? C4 Co1 C21 104.21(13) . . ? C3 Co1 C21 121.45(17) . . ? C4 Co1 C5 41.1 . . ? C3 Co1 C5 69.13(7) . . ? C21 Co1 C5 119.49(12) . . ? C4 Co1 C20 124.58(13) . . ? C3 Co1 C20 160.20(17) . . ? C21 Co1 C20 41.00(6) . . ? C5 Co1 C20 109.10(10) . . ? C4 Co1 C22 116.27(15) . . ? C3 Co1 C22 103.25(14) . . ? C21 Co1 C22 41.05(6) . . ? C5 Co1 C22 152.92(16) . . ? C20 Co1 C22 68.96(7) . . ? C4 Co1 C24 163.76(13) . . ? C3 Co1 C24 155.03(13) . . ? C21 Co1 C24 68.86(7) . . ? C5 Co1 C24 128.44(14) . . ? C20 Co1 C24 40.81(6) . . ? C22 Co1 C24 68.79(7) . . ? C4 Co1 C2 69.09(7) . . ? C3 Co1 C2 40.99(5) . . ? C21 Co1 C2 159.48(18) . . ? C5 Co1 C2 68.93(6) . . ? C20 Co1 C2 158.28(18) . . ? C22 Co1 C2 123.08(13) . . ? C24 Co1 C2 122.44(14) . . ? C4 Co1 C23 152.12(16) . . ? C3 Co1 C23 117.97(13) . . ? C21 Co1 C23 68.92(7) . . ? C5 Co1 C23 165.56(17) . . ? C20 Co1 C23 68.75(7) . . ? C22 Co1 C23 40.9 . . ? C24 Co1 C23 40.76(6) . . ? C2 Co1 C23 107.47(10) . . ? C4 Co1 C1 69.03(6) . . ? C3 Co1 C1 68.96(6) . . ? C21 Co1 C1 156.61(13) . . ? C5 Co1 C1 40.9 . . ? C20 Co1 C1 123.46(15) . . ? C22 Co1 C1 162.24(13) . . ? C24 Co1 C1 111.20(14) . . ? C2 Co1 C1 40.9 . . ? C23 Co1 C1 127.43(14) . . ? C2 C1 C5 108.0 . . ? C2 C1 Co1 69.46(11) . . ? C5 C1 Co1 69.23(10) . . ? C1 C2 C3 108.0 . . ? C1 C2 Co1 69.68(11) . . ? C3 C2 Co1 69.12(12) . . ? C4 C3 C2 108.0 . . ? C4 C3 Co1 69.31(10) . . ? C2 C3 Co1 69.88(12) . . ? C5 C4 C3 108.0 . . ? C5 C4 Co1 69.76(11) . . ? C3 C4 Co1 69.56(10) . . ? C4 C5 C1 108.0 . . ? C4 C5 C6 130.5(3) . . ? C1 C5 C6 121.5(3) . . ? C4 C5 Co1 69.15(12) . . ? C1 C5 Co1 69.86(11) . . ? C6 C5 Co1 126.2(2) . . ? O1 C6 N1 124.7(4) . . ? O1 C6 C5 119.4(4) . . ? N1 C6 C5 115.8(5) . . ? N3 C7 C8 122.9(6) . . ? N3 C7 N1 116.1(6) . . ? C8 C7 N1 120.9(5) . . ? C10 C8 C7 119.6(7) . . ? C8 C10 C11 116.7(8) . . ? C12 C11 C10 120.4(7) . . ? N3 C12 C11 122.0(6) . . ? N2 C13 C14 123.4(4) . . ? N2 C13 N1 112.7(4) . . ? C14 C13 N1 123.9(4) . . ? C13 C14 C15 117.5(5) . . ? C16 C15 C14 120.2(6) . . ? C17 C16 C15 118.0(5) . . ? C16 C17 N2 123.8(5) . . ? C21 C20 C24 108.0 . . ? C21 C20 Co1 69.17(13) . . ? C24 C20 Co1 69.92(12) . . ? C20 C21 C22 108.0 . . ? C20 C21 Co1 69.84(13) . . ? C22 C21 Co1 69.60(11) . . ? C23 C22 C21 108.0 . . ? C23 C22 Co1 69.96(13) . . ? C21 C22 Co1 69.35(11) . . ? C22 C23 C24 108.0 . . ? C22 C23 Co1 69.14(13) . . ? C24 C23 Co1 69.75(12) . . ? C23 C24 C20 108.0 . . ? C23 C24 C25 120.1(3) . . ? C20 C24 C25 131.9(3) . . ? C23 C24 Co1 69.49(11) . . ? C20 C24 Co1 69.27(11) . . ? C25 C24 Co1 126.4(2) . . ? O3 C25 O2 129.1(7) . . ? O3 C25 C24 120.6(5) . . ? O2 C25 C24 110.2(5) . . ? C6 N1 C7 118.1(3) . . ? C6 N1 C13 124.1(4) . . ? C7 N1 C13 116.9(3) . . ? C13 N2 C17 117.1(5) . . ? C7 N3 C12 118.4(6) . . ? F4A P1 F1 76.1(10) . . ? F4A P1 F3B 135.2(14) . . ? F1 P1 F3B 81.3(8) . . ? F4A P1 F5B 122.6(15) . . ? F1 P1 F5B 87.1(8) . . ? F3B P1 F5B 93.9(12) . . ? F4A P1 F2 102.8(11) . . ? F1 P1 F2 178.7(5) . . ? F3B P1 F2 100.0(7) . . ? F5B P1 F2 93.0(8) . . ? F4A P1 F6A 97.4(16) . . ? F1 P1 F6A 91.7(6) . . ? F3B P1 F6A 45.0(13) . . ? F5B P1 F6A 138.3(19) . . ? F2 P1 F6A 89.0(6) . . ? F4A P1 F5A 96.0(18) . . ? F1 P1 F5A 88.0(9) . . ? F3B P1 F5A 121.5(18) . . ? F5B P1 F5A 28(2) . . ? F2 P1 F5A 91.5(9) . . ? F6A P1 F5A 166(2) . . ? F4A P1 F4B 44.3(10) . . ? F1 P1 F4B 99.4(7) . . ? F3B P1 F4B 178.8(12) . . ? F5B P1 F4B 87.1(12) . . ? F2 P1 F4B 79.4(7) . . ? F6A P1 F4B 133.9(17) . . ? F5A P1 F4B 59.6(14) . . ? F4A P1 F3A 174.4(13) . . ? F1 P1 F3A 109.5(8) . . ? F3B P1 F3A 47.1(7) . . ? F5B P1 F3A 59.4(10) . . ? F2 P1 F3A 71.6(7) . . ? F6A P1 F3A 82.1(14) . . ? F5A P1 F3A 84.9(15) . . ? F4B P1 F3A 133.2(9) . . ? F4A P1 F6B 58.2(11) . . ? F1 P1 F6B 94.4(6) . . ? F3B P1 F6B 86.0(10) . . ? F5B P1 F6B 178.5(10) . . ? F2 P1 F6B 85.6(6) . . ? F6A P1 F6B 41.4(14) . . ? F5A P1 F6B 152.4(19) . . ? F4B P1 F6B 92.9(11) . . ? F3A P1 F6B 119.7(12) . . ? _diffrn_measured_fraction_theta_max 0.638 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.638 _refine_diff_density_max 0.364 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.049 data_5_[Co(C5H4-CONHC2N3(C5H4N)2)(C5H4-COOH)]+[PF6]- _database_code_depnum_ccdc_archive 'CCDC 269425' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H20 Co F6 N6 O4 P' _chemical_formula_weight 660.36 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 7.7355(2) _cell_length_b 13.1359(4) _cell_length_c 13.5350(4) _cell_angle_alpha 105.7620(10) _cell_angle_beta 90.1450(10) _cell_angle_gamma 101.5180(10) _cell_volume 1294.61(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 0.813 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10464 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.04 _reflns_number_total 4557 _reflns_number_gt 3719 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0994P)^2^+0.3259P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4557 _refine_ls_number_parameters 366 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1454 _refine_ls_wR_factor_gt 0.1357 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.45384(6) 0.71323(3) 0.41430(3) 0.03302(18) Uani 1 1 d . . . C1 C 0.5454(2) 0.85366(19) 0.37820(17) 0.0425(8) Uani 1 1 d G . . H1 H 0.6588 0.8768 0.3593 0.051 Uiso 1 1 calc R . . C2 C 0.4880(3) 0.87518(19) 0.47998(14) 0.0520(10) Uani 1 1 d G . . H2 H 0.5572 0.9149 0.5394 0.062 Uiso 1 1 calc R . . C3 C 0.3063(3) 0.8254(2) 0.47504(14) 0.0508(10) Uani 1 1 d G . . H3 H 0.2356 0.8268 0.5307 0.061 Uiso 1 1 calc R . . C4 C 0.2514(2) 0.77312(19) 0.37021(16) 0.0396(8) Uani 1 1 d G . . H4 H 0.1384 0.7343 0.3452 0.048 Uiso 1 1 calc R . . C5 C 0.3991(3) 0.79059(19) 0.31036(12) 0.0330(7) Uani 1 1 d G . . C6 C 0.4134(4) 0.7471(2) 0.1975(2) 0.0310(7) Uani 1 1 d . . . C7 C 0.2589(4) 0.5379(2) 0.0116(2) 0.0315(7) Uani 1 1 d . . . C8 C 0.2990(4) 0.6820(3) -0.0442(2) 0.0322(7) Uani 1 1 d . . . C9 C 0.3044(4) 0.7916(3) -0.0527(2) 0.0345(7) Uani 1 1 d . . . C10 C 0.2311(5) 0.8667(3) 0.0154(3) 0.0450(8) Uani 1 1 d . . . H10 H 0.1800 0.8511 0.0731 0.054 Uiso 1 1 calc R . . C11 C 0.2335(6) 0.9661(3) -0.0024(3) 0.0535(10) Uani 1 1 d . . . H11 H 0.1824 1.0175 0.0424 0.064 Uiso 1 1 calc R . . C12 C 0.3133(6) 0.9872(3) -0.0877(3) 0.0556(10) Uani 1 1 d . . . H12 H 0.3203 1.0538 -0.1009 0.067 Uiso 1 1 calc R . . C13 C 0.3820(6) 0.9074(3) -0.1525(3) 0.0547(10) Uani 1 1 d . . . H13 H 0.4333 0.9211 -0.2109 0.066 Uiso 1 1 calc R . . C14 C 0.2114(4) 0.4631(2) 0.0759(2) 0.0312(7) Uani 1 1 d . . . C15 C 0.2626(5) 0.3653(3) 0.0526(3) 0.0438(8) Uani 1 1 d . . . H15 H 0.3312 0.3451 -0.0028 0.053 Uiso 1 1 calc R . . C16 C 0.2087(6) 0.2976(3) 0.1145(3) 0.0541(10) Uani 1 1 d . . . H16 H 0.2433 0.2316 0.1020 0.065 Uiso 1 1 calc R . . C17 C 0.1043(5) 0.3285(3) 0.1940(3) 0.0511(9) Uani 1 1 d . . . H17 H 0.0656 0.2839 0.2359 0.061 Uiso 1 1 calc R . . C18 C 0.0586(5) 0.4272(3) 0.2102(3) 0.0458(9) Uani 1 1 d . . . H18 H -0.0137 0.4475 0.2637 0.055 Uiso 1 1 calc R . . C19 C 0.6269(3) 0.6620(2) 0.49338(17) 0.0447(8) Uani 1 1 d G . . H19 H 0.7149 0.7058 0.5422 0.054 Uiso 1 1 calc R . . C20 C 0.6462(3) 0.6236(2) 0.38614(18) 0.0525(10) Uani 1 1 d G . . H20 H 0.7489 0.6378 0.3524 0.063 Uiso 1 1 calc R . . C21 C 0.4809(4) 0.5596(2) 0.33955(13) 0.0545(11) Uani 1 1 d G . . H21 H 0.4565 0.5246 0.2699 0.065 Uiso 1 1 calc R . . C22 C 0.3596(3) 0.55844(19) 0.41799(18) 0.0484(9) Uani 1 1 d G . . H22 H 0.2417 0.5225 0.4087 0.058 Uiso 1 1 calc R . . C23 C 0.4498(3) 0.6217(2) 0.51306(14) 0.0410(8) Uani 1 1 d G . . C24 C 0.3675(6) 0.6476(3) 0.6143(3) 0.0485(9) Uani 1 1 d . . . N1 N 0.2570(4) 0.7081(2) 0.14222(19) 0.0316(6) Uani 1 1 d . . . H100 H 0.165(4) 0.700(2) 0.166(2) 0.022(8) Uiso 1 1 d . . . N2 N 0.2586(3) 0.6460(2) 0.04122(18) 0.0307(6) Uani 1 1 d . . . N3 N 0.2956(4) 0.5095(2) -0.0851(2) 0.0368(6) Uani 1 1 d . . . N4 N 0.3214(4) 0.6006(2) -0.1205(2) 0.0374(6) Uani 1 1 d . . . N5 N 0.3799(4) 0.8111(2) -0.1371(2) 0.0431(7) Uani 1 1 d . . . N6 N 0.1111(4) 0.4957(2) 0.1543(2) 0.0408(7) Uani 1 1 d . . . O1 O 0.5548(3) 0.7493(2) 0.15912(18) 0.0477(6) Uani 1 1 d . . . O2 O 0.4864(4) 0.6973(2) 0.68939(19) 0.0598(7) Uani 1 1 d . . . H200 H 0.4468 0.7358 0.7629 0.050 Uiso 1 1 d . . . O3 O 0.2123(5) 0.6237(3) 0.6215(2) 0.0786(10) Uani 1 1 d . . . P1 P 0.05355(14) 0.01912(8) 0.30621(8) 0.0502(3) Uani 1 1 d . . . F1 F -0.0225(5) -0.0745(3) 0.2048(2) 0.1005(10) Uani 1 1 d . . . F2 F 0.0944(6) 0.0948(3) 0.2360(4) 0.1321(16) Uani 1 1 d . . . F3 F 0.0005(5) -0.0674(3) 0.3688(3) 0.1119(12) Uani 1 1 d . . . F4 F -0.1396(4) 0.0438(3) 0.3208(2) 0.0957(10) Uani 1 1 d . . . F5 F 0.1183(6) 0.1063(4) 0.4086(3) 0.1474(18) Uani 1 1 d . . . F6 F 0.2388(4) -0.0139(3) 0.2898(3) 0.1135(12) Uani 1 1 d . . . O100 O -0.0882(3) 0.69225(19) 0.2080(2) 0.0470(6) Uani 1 1 d . . . H101 H -0.1618 0.6352 0.1777 0.050 Uiso 1 1 d . . . H102 H -0.1351 0.7445 0.2034 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0477(3) 0.0309(3) 0.0232(3) 0.00741(18) 0.00635(18) 0.0147(2) C1 0.055(2) 0.0308(17) 0.0418(19) 0.0144(15) -0.0036(17) 0.0042(15) C2 0.091(3) 0.0303(18) 0.0313(18) -0.0024(15) -0.0112(19) 0.0203(19) C3 0.074(3) 0.058(2) 0.0294(18) 0.0092(17) 0.0127(18) 0.039(2) C4 0.0468(19) 0.0460(19) 0.0308(17) 0.0086(15) 0.0069(15) 0.0232(16) C5 0.0459(18) 0.0303(16) 0.0273(16) 0.0093(13) 0.0041(14) 0.0164(14) C6 0.0387(17) 0.0288(16) 0.0281(16) 0.0097(13) 0.0062(14) 0.0105(13) C7 0.0335(16) 0.0325(16) 0.0273(16) 0.0060(13) 0.0033(13) 0.0070(13) C8 0.0339(16) 0.0383(17) 0.0241(15) 0.0101(13) 0.0034(13) 0.0046(13) C9 0.0365(16) 0.0401(18) 0.0263(16) 0.0095(14) -0.0015(13) 0.0064(14) C10 0.055(2) 0.048(2) 0.0373(19) 0.0158(16) 0.0085(16) 0.0165(17) C11 0.066(2) 0.044(2) 0.054(2) 0.0112(18) 0.001(2) 0.0199(19) C12 0.071(3) 0.046(2) 0.056(2) 0.0234(19) -0.006(2) 0.013(2) C13 0.075(3) 0.055(2) 0.040(2) 0.0244(18) 0.0049(19) 0.010(2) C14 0.0317(15) 0.0303(16) 0.0309(16) 0.0072(13) 0.0010(13) 0.0068(13) C15 0.0464(19) 0.043(2) 0.044(2) 0.0113(16) 0.0070(16) 0.0170(16) C16 0.064(2) 0.038(2) 0.066(3) 0.0208(19) 0.002(2) 0.0154(18) C17 0.051(2) 0.049(2) 0.059(2) 0.0304(19) 0.0001(19) 0.0008(17) C18 0.0429(19) 0.052(2) 0.045(2) 0.0219(17) 0.0103(16) 0.0049(16) C19 0.056(2) 0.050(2) 0.0389(19) 0.0204(16) 0.0057(16) 0.0248(18) C20 0.068(3) 0.062(2) 0.044(2) 0.0229(19) 0.0198(19) 0.040(2) C21 0.101(3) 0.039(2) 0.0296(18) 0.0055(15) 0.009(2) 0.034(2) C22 0.074(3) 0.0311(18) 0.040(2) 0.0103(15) 0.0005(18) 0.0081(17) C23 0.063(2) 0.0344(18) 0.0306(17) 0.0126(14) 0.0081(16) 0.0168(16) C24 0.070(3) 0.048(2) 0.036(2) 0.0205(17) 0.0128(19) 0.0175(19) N1 0.0355(15) 0.0370(15) 0.0215(13) 0.0062(11) 0.0101(11) 0.0080(12) N2 0.0382(14) 0.0322(14) 0.0207(12) 0.0050(10) 0.0043(10) 0.0081(11) N3 0.0456(15) 0.0330(14) 0.0291(14) 0.0052(11) 0.0054(12) 0.0066(12) N4 0.0481(16) 0.0385(15) 0.0249(13) 0.0063(12) 0.0058(12) 0.0104(13) N5 0.0575(18) 0.0437(16) 0.0292(15) 0.0140(13) 0.0073(13) 0.0077(14) N6 0.0426(15) 0.0417(16) 0.0424(16) 0.0177(13) 0.0118(13) 0.0105(13) O1 0.0365(13) 0.0667(17) 0.0357(13) 0.0070(12) 0.0089(11) 0.0113(12) O2 0.0739(19) 0.0766(19) 0.0267(13) 0.0098(13) 0.0083(13) 0.0168(16) O3 0.072(2) 0.111(3) 0.0476(17) 0.0255(18) 0.0200(16) 0.0031(19) P1 0.0552(6) 0.0478(6) 0.0488(6) 0.0119(5) 0.0048(5) 0.0157(5) F1 0.113(2) 0.094(2) 0.075(2) -0.0128(17) 0.0013(18) 0.0256(19) F2 0.161(4) 0.109(3) 0.176(4) 0.105(3) 0.069(3) 0.052(3) F3 0.131(3) 0.124(3) 0.116(3) 0.075(2) 0.040(2) 0.050(2) F4 0.086(2) 0.124(3) 0.084(2) 0.0156(19) 0.0180(17) 0.0566(19) F5 0.125(3) 0.147(4) 0.106(3) -0.046(3) -0.022(3) -0.006(3) F6 0.0732(19) 0.159(3) 0.137(3) 0.068(3) 0.024(2) 0.056(2) O100 0.0407(13) 0.0397(13) 0.0539(15) 0.0012(12) 0.0053(11) 0.0095(11) _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 C23 2.023(2) . ? Co1 C1 2.028(2) . ? Co1 C2 2.033(2) . ? Co1 C19 2.034(2) . ? Co1 C5 2.034(2) . ? Co1 C22 2.033(2) . ? Co1 C3 2.042(2) . ? Co1 C4 2.042(2) . ? Co1 C20 2.050(2) . ? Co1 C21 2.050(2) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C1 H1 0.9300 . ? C2 C3 1.4200 . ? C2 H2 0.9300 . ? C3 C4 1.4200 . ? C3 H3 0.9300 . ? C4 C5 1.4200 . ? C4 H4 0.9300 . ? C5 C6 1.491(3) . ? C6 O1 1.210(4) . ? C6 N1 1.351(4) . ? C7 N3 1.307(4) . ? C7 N2 1.366(4) . ? C7 C14 1.477(4) . ? C8 N4 1.309(4) . ? C8 N2 1.378(4) . ? C8 C9 1.467(5) . ? C9 N5 1.346(4) . ? C9 C10 1.370(5) . ? C10 C11 1.387(5) . ? C10 H10 0.9300 . ? C11 C12 1.379(6) . ? C11 H11 0.9300 . ? C12 C13 1.370(6) . ? C12 H12 0.9300 . ? C13 N5 1.334(5) . ? C13 H13 0.9300 . ? C14 N6 1.343(4) . ? C14 C15 1.375(5) . ? C15 C16 1.386(5) . ? C15 H15 0.9300 . ? C16 C17 1.369(6) . ? C16 H16 0.9300 . ? C17 C18 1.372(5) . ? C17 H17 0.9300 . ? C18 N6 1.332(4) . ? C18 H18 0.9300 . ? C19 C20 1.4200 . ? C19 C23 1.4200 . ? C19 H19 0.9300 . ? C20 C21 1.4200 . ? C20 H20 0.9300 . ? C21 C22 1.4200 . ? C21 H21 0.9300 . ? C22 C23 1.4200 . ? C22 H22 0.9300 . ? C23 C24 1.495(4) . ? C24 O3 1.191(5) . ? C24 O2 1.304(5) . ? N1 N2 1.390(3) . ? N1 H100 0.78(3) . ? N3 N4 1.385(4) . ? O2 H200 1.0629 . ? P1 F2 1.542(3) . ? P1 F5 1.545(4) . ? P1 F6 1.577(3) . ? P1 F3 1.586(3) . ? P1 F1 1.591(3) . ? P1 F4 1.593(3) . ? O100 H101 0.8459 . ? O100 H102 0.8539 . ? 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 C23 Co1 C1 149.74(9) . . ? C23 Co1 C2 115.71(8) . . ? C1 Co1 C2 40.9 . . ? C23 Co1 C19 41.0 . . ? C1 Co1 C19 116.51(9) . . ? C2 Co1 C19 105.72(9) . . ? C23 Co1 C5 167.19(10) . . ? C1 Co1 C5 40.9 . . ? C2 Co1 C5 68.80(5) . . ? C19 Co1 C5 151.42(9) . . ? C23 Co1 C22 41.0 . . ? C1 Co1 C22 167.94(9) . . ? C2 Co1 C22 150.40(10) . . ? C19 Co1 C22 68.81(5) . . ? C5 Co1 C22 129.78(9) . . ? C23 Co1 C3 106.38(8) . . ? C1 Co1 C3 68.74(5) . . ? C2 Co1 C3 40.8 . . ? C19 Co1 C3 126.43(9) . . ? C5 Co1 C3 68.63(5) . . ? C22 Co1 C3 117.81(10) . . ? C23 Co1 C4 127.97(9) . . ? C1 Co1 C4 68.73(5) . . ? C2 Co1 C4 68.64(5) . . ? C19 Co1 C4 165.34(9) . . ? C5 Co1 C4 40.8 . . ? C22 Co1 C4 108.98(9) . . ? C3 Co1 C4 40.7 . . ? C23 Co1 C20 68.67(5) . . ? C1 Co1 C20 107.89(9) . . ? C2 Co1 C20 127.19(11) . . ? C19 Co1 C20 40.7 . . ? C5 Co1 C20 119.16(8) . . ? C22 Co1 C20 68.49(5) . . ? C3 Co1 C20 164.89(11) . . ? C4 Co1 C20 153.27(10) . . ? C23 Co1 C21 68.69(5) . . ? C1 Co1 C21 129.26(10) . . ? C2 Co1 C21 166.27(11) . . ? C19 Co1 C21 68.48(5) . . ? C5 Co1 C21 109.94(8) . . ? C22 Co1 C21 40.7 . . ? C3 Co1 C21 152.57(11) . . ? C4 Co1 C21 119.97(10) . . ? C20 Co1 C21 40.5 . . ? C2 C1 C5 108.0 . . ? C2 C1 Co1 69.71(9) . . ? C5 C1 Co1 69.76(9) . . ? C2 C1 H1 126.0 . . ? C5 C1 H1 126.0 . . ? Co1 C1 H1 126.1 . . ? C3 C2 C1 108.0 . . ? C3 C2 Co1 69.93(9) . . ? C1 C2 Co1 69.35(9) . . ? C3 C2 H2 126.0 . . ? C1 C2 H2 126.0 . . ? Co1 C2 H2 126.3 . . ? C2 C3 C4 108.0 . . ? C2 C3 Co1 69.27(9) . . ? C4 C3 Co1 69.68(8) . . ? C2 C3 H3 126.0 . . ? C4 C3 H3 126.0 . . ? Co1 C3 H3 126.6 . . ? C5 C4 C3 108.0 . . ? C5 C4 Co1 69.30(9) . . ? C3 C4 Co1 69.63(9) . . ? C5 C4 H4 126.0 . . ? C3 C4 H4 126.0 . . ? Co1 C4 H4 126.6 . . ? C4 C5 C1 108.0 . . ? C4 C5 C6 129.00(19) . . ? C1 C5 C6 122.87(19) . . ? C4 C5 Co1 69.93(9) . . ? C1 C5 Co1 69.32(9) . . ? C6 C5 Co1 123.04(17) . . ? O1 C6 N1 123.2(3) . . ? O1 C6 C5 122.1(3) . . ? N1 C6 C5 114.7(2) . . ? N3 C7 N2 109.3(3) . . ? N3 C7 C14 125.1(3) . . ? N2 C7 C14 125.4(3) . . ? N4 C8 N2 109.1(3) . . ? N4 C8 C9 124.4(3) . . ? N2 C8 C9 126.4(3) . . ? N5 C9 C10 122.0(3) . . ? N5 C9 C8 114.2(3) . . ? C10 C9 C8 123.7(3) . . ? C9 C10 C11 119.6(3) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 118.6(4) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C13 C12 C11 118.1(4) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? N5 C13 C12 124.1(4) . . ? N5 C13 H13 118.0 . . ? C12 C13 H13 118.0 . . ? N6 C14 C15 123.5(3) . . ? N6 C14 C7 115.4(3) . . ? C15 C14 C7 121.0(3) . . ? C14 C15 C16 117.9(3) . . ? C14 C15 H15 121.1 . . ? C16 C15 H15 121.1 . . ? C17 C16 C15 119.7(3) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 118.1(3) . . ? C16 C17 H17 121.0 . . ? C18 C17 H17 121.0 . . ? N6 C18 C17 124.2(4) . . ? N6 C18 H18 117.9 . . ? C17 C18 H18 117.9 . . ? C20 C19 C23 108.0 . . ? C20 C19 Co1 70.28(9) . . ? C23 C19 Co1 69.09(9) . . ? C20 C19 H19 126.0 . . ? C23 C19 H19 126.0 . . ? Co1 C19 H19 126.2 . . ? C19 C20 C21 108.0 . . ? C19 C20 Co1 69.03(9) . . ? C21 C20 Co1 69.71(9) . . ? C19 C20 H20 126.0 . . ? C21 C20 H20 126.0 . . ? Co1 C20 H20 126.8 . . ? C22 C21 C20 108.0 . . ? C22 C21 Co1 69.00(9) . . ? C20 C21 Co1 69.76(9) . . ? C22 C21 H21 126.0 . . ? C20 C21 H21 126.0 . . ? Co1 C21 H21 126.8 . . ? C21 C22 C23 108.0 . . ? C21 C22 Co1 70.29(9) . . ? C23 C22 Co1 69.13(9) . . ? C21 C22 H22 126.0 . . ? C23 C22 H22 126.0 . . ? Co1 C22 H22 126.2 . . ? C22 C23 C19 108.0 . . ? C22 C23 C24 125.4(2) . . ? C19 C23 C24 126.4(2) . . ? C22 C23 Co1 69.88(9) . . ? C19 C23 Co1 69.93(9) . . ? C24 C23 Co1 122.3(2) . . ? O3 C24 O2 126.5(4) . . ? O3 C24 C23 122.1(4) . . ? O2 C24 C23 111.4(3) . . ? C6 N1 N2 117.6(3) . . ? C6 N1 H100 124(2) . . ? N2 N1 H100 115(2) . . ? C7 N2 C8 105.8(2) . . ? C7 N2 N1 125.2(2) . . ? C8 N2 N1 127.6(3) . . ? C7 N3 N4 108.0(2) . . ? C8 N4 N3 107.7(2) . . ? C13 N5 C9 117.6(3) . . ? C18 N6 C14 116.7(3) . . ? C24 O2 H200 119.8 . . ? F2 P1 F5 96.5(3) . . ? F2 P1 F6 91.7(2) . . ? F5 P1 F6 93.4(2) . . ? F2 P1 F3 174.3(3) . . ? F5 P1 F3 89.1(3) . . ? F6 P1 F3 89.2(2) . . ? F2 P1 F1 86.7(2) . . ? F5 P1 F1 176.2(2) . . ? F6 P1 F1 88.5(2) . . ? F3 P1 F1 87.7(2) . . ? F2 P1 F4 90.8(2) . . ? F5 P1 F4 89.4(2) . . ? F6 P1 F4 176.0(2) . . ? F3 P1 F4 87.96(19) . . ? F1 P1 F4 88.60(18) . . ? H101 O100 H102 105.7 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.769 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.085 data_6 _database_code_depnum_ccdc_archive 'CCDC 269426' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Cd(NO3)2{Co(C5H4-CONHC2N3(C5H4N)(C5H4NH)(C5H4-COOH)}2]6+_2[PF6]-_2[CO3]2_.2H2O ; _chemical_name_common ;(Cd(NO3)2(Co(C5H4-CONHC2N3(C5H4N)(C5H4NH)(C5H4- COOH))2)6+_2(PF6)-_2(CO3)2_.2H2O ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H42 Cd Co2 F12 N14 O20 P2' _chemical_formula_weight 1679.18 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 8.715(3) _cell_length_b 12.051(6) _cell_length_c 15.228(6) _cell_angle_alpha 81.61(4) _cell_angle_beta 73.61(3) _cell_angle_gamma 88.83(4) _cell_volume 1517.5(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 1.065 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.840 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5543 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0830 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 24.98 _reflns_number_total 5326 _reflns_number_gt 2983 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5326 _refine_ls_number_parameters 447 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1222 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1386 _refine_ls_wR_factor_gt 0.1105 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.21330(9) 0.23043(7) 0.48155(5) 0.0367(2) Uani 1 1 d . . . C1 C 0.3945(5) 0.2678(3) 0.3627(3) 0.0432(15) Uani 1 1 d G . . H1 H 0.4098 0.3344 0.3215 0.052 Uiso 1 1 calc R . . C2 C 0.4562(5) 0.2441(4) 0.4402(3) 0.0548(18) Uani 1 1 d G . . H2 H 0.5190 0.2924 0.4587 0.066 Uiso 1 1 calc R . . C3 C 0.4052(6) 0.1337(4) 0.4846(3) 0.061(2) Uani 1 1 d G . . H3 H 0.4287 0.0970 0.5372 0.073 Uiso 1 1 calc R . . C4 C 0.3119(6) 0.0892(3) 0.4345(3) 0.0522(17) Uani 1 1 d G . . H4 H 0.2637 0.0182 0.4486 0.063 Uiso 1 1 calc R . . C5 C 0.3054(5) 0.1721(3) 0.3592(3) 0.0369(13) Uani 1 1 d G . . C6 C 0.2140(7) 0.1564(5) 0.2920(4) 0.0335(13) Uani 1 1 d . . . C7 C 0.1962(7) 0.1350(5) 0.0924(4) 0.0347(13) Uani 1 1 d . . . C8 C 0.1043(6) 0.3022(5) 0.1088(4) 0.0343(13) Uani 1 1 d . . . C9 C 0.0619(6) 0.4108(5) 0.1403(4) 0.0346(13) Uani 1 1 d . . . C10 C 0.1428(8) 0.4716(5) 0.1817(4) 0.0454(15) Uani 1 1 d . . . H10 H 0.2361 0.4447 0.1946 0.054 Uiso 1 1 calc R . . C11 C 0.0843(9) 0.5744(6) 0.2046(4) 0.0532(17) Uani 1 1 d . . . H11 H 0.1394 0.6168 0.2327 0.064 Uiso 1 1 calc R . . C12 C -0.0543(9) 0.6149(6) 0.1863(5) 0.0568(18) Uani 1 1 d . . . H12 H -0.0946 0.6833 0.2030 0.068 Uiso 1 1 calc R . . C13 C -0.1309(8) 0.5519(6) 0.1431(5) 0.0530(17) Uani 1 1 d . . . H13 H -0.2233 0.5776 0.1286 0.064 Uiso 1 1 calc R . . C14 C 0.2723(7) 0.0257(5) 0.0989(4) 0.0373(14) Uani 1 1 d . . . C15 C 0.4021(7) 0.0023(5) 0.1336(4) 0.0445(15) Uani 1 1 d . . . H15 H 0.4484 0.0575 0.1553 0.053 Uiso 1 1 calc R . . C16 C 0.4607(8) -0.1046(6) 0.1350(5) 0.0550(18) Uani 1 1 d . . . H16 H 0.5461 -0.1229 0.1593 0.066 Uiso 1 1 calc R . . C17 C 0.3950(8) -0.1828(5) 0.1012(5) 0.0537(17) Uani 1 1 d . . . H17 H 0.4335 -0.2553 0.1025 0.064 Uiso 1 1 calc R . . C18 C 0.2681(8) -0.1531(5) 0.0644(4) 0.0481(16) Uani 1 1 d . . . H18 H 0.2241 -0.2062 0.0394 0.058 Uiso 1 1 calc R . . C19 C -0.0235(5) 0.2621(4) 0.5050(3) 0.0469(16) Uani 1 1 d G . . C20 C 0.0022(5) 0.1891(3) 0.5813(3) 0.0542(18) Uani 1 1 d G . . H20 H -0.0425 0.1176 0.6039 0.065 Uiso 1 1 calc R . . C21 C 0.1083(6) 0.2446(4) 0.6172(3) 0.060(2) Uani 1 1 d G . . H21 H 0.1452 0.2157 0.6674 0.072 Uiso 1 1 calc R . . C22 C 0.1481(5) 0.3518(4) 0.5631(3) 0.061(2) Uani 1 1 d G . . H22 H 0.2157 0.4055 0.5715 0.073 Uiso 1 1 calc R . . C23 C 0.0667(6) 0.3626(3) 0.4937(3) 0.0500(17) Uani 1 1 d G . . H23 H 0.0716 0.4247 0.4487 0.060 Uiso 1 1 calc R . . C24 C -0.1214(8) 0.2338(6) 0.4454(5) 0.0538(18) Uani 1 1 d . . . Cd1 Cd 0.0000 0.0000 0.0000 0.0437(2) Uani 1 2 d S . . N1 N 0.2686(6) 0.2278(4) 0.2101(3) 0.0369(12) Uani 1 1 d . . . N2 N 0.1972(5) 0.2211(4) 0.1410(3) 0.0329(11) Uani 1 1 d . . . N3 N -0.0722(6) 0.4537(5) 0.1222(4) 0.0431(13) Uani 1 1 d . . . N4 N 0.0522(6) 0.2677(4) 0.0447(3) 0.0419(12) Uani 1 1 d . . . N5 N 0.1093(6) 0.1620(4) 0.0344(3) 0.0413(12) Uani 1 1 d . . . N6 N 0.2088(6) -0.0514(4) 0.0641(3) 0.0387(12) Uani 1 1 d . . . O1 O 0.1074(5) 0.0876(4) 0.3066(3) 0.0507(11) Uani 1 1 d . . . O2 O -0.2059(6) 0.1510(4) 0.4637(4) 0.0680(14) Uani 1 1 d . . . O3 O -0.1042(6) 0.3094(5) 0.3716(4) 0.0665(16) Uani 1 1 d . . . N7 N 0.2073(8) 0.0209(7) -0.1979(5) 0.0683(18) Uani 1 1 d . . . O4 O 0.2035(8) -0.0565(5) -0.1344(4) 0.0928(19) Uani 1 1 d . . . O5 O 0.2816(9) 0.0117(6) -0.2778(4) 0.107(2) Uani 1 1 d . . . O6 O 0.1361(8) 0.1053(6) -0.1750(5) 0.096(2) Uani 1 1 d . . . P1 P 0.4468(2) 0.61547(16) 0.33235(13) 0.0545(5) Uani 1 1 d . . . F1 F 0.3270(8) 0.5245(5) 0.3281(6) 0.150(3) Uani 1 1 d . . . F2 F 0.5243(9) 0.6314(7) 0.2287(4) 0.176(4) Uani 1 1 d . . . F3 F 0.3214(5) 0.7079(4) 0.3156(3) 0.0817(13) Uani 1 1 d . . . F4 F 0.5590(9) 0.7042(6) 0.3431(7) 0.182(4) Uani 1 1 d . . . F5 F 0.5702(6) 0.5203(4) 0.3466(4) 0.1079(18) Uani 1 1 d . . . F6 F 0.3664(9) 0.6013(7) 0.4396(4) 0.149(3) Uani 1 1 d . . . C100 C 0.5899(6) 0.3711(4) 1.0688(4) 0.0301(12) Uiso 1 1 d . . . O7 O 0.7257(5) 0.4032(5) 1.0229(3) 0.0691(15) Uani 1 1 d . . . O8 O 0.4801(6) 0.3649(5) 1.0333(3) 0.0700(14) Uani 1 1 d . . . O9 O 0.5609(6) 0.3421(5) 1.1534(3) 0.0696(15) Uani 1 1 d . . . O100 O -0.2322(6) 0.2382(5) 0.2547(3) 0.0735(15) Uani 1 1 d . . . H100 H 0.349(8) 0.264(5) 0.192(4) 0.04(2) Uiso 1 1 d . . . H200 H -0.105(7) 0.419(5) 0.087(4) 0.033(17) Uiso 1 1 d . . . H101 H -0.146(8) 0.294(5) 0.335(4) 0.04(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0346(5) 0.0438(5) 0.0351(5) -0.0053(4) -0.0157(4) 0.0055(4) C1 0.037(3) 0.061(4) 0.035(3) -0.014(3) -0.013(3) -0.001(3) C2 0.033(3) 0.091(6) 0.047(4) -0.019(4) -0.018(3) 0.007(3) C3 0.065(5) 0.084(6) 0.048(4) -0.019(4) -0.036(4) 0.039(4) C4 0.067(5) 0.048(4) 0.048(4) -0.011(3) -0.025(3) 0.022(3) C5 0.042(3) 0.038(3) 0.035(3) -0.010(3) -0.015(3) 0.010(3) C6 0.035(3) 0.035(3) 0.032(3) -0.009(3) -0.011(3) 0.005(3) C7 0.034(3) 0.036(3) 0.040(3) -0.007(3) -0.020(3) 0.002(2) C8 0.031(3) 0.037(3) 0.034(3) -0.001(3) -0.010(3) -0.003(2) C9 0.032(3) 0.039(3) 0.028(3) 0.004(3) -0.006(2) -0.001(3) C10 0.052(4) 0.041(4) 0.048(4) -0.013(3) -0.018(3) 0.001(3) C11 0.075(5) 0.045(4) 0.045(4) -0.010(3) -0.024(4) -0.003(4) C12 0.074(5) 0.044(4) 0.052(4) -0.009(3) -0.016(4) 0.015(4) C13 0.058(4) 0.044(4) 0.059(4) -0.008(3) -0.019(4) 0.017(3) C14 0.038(3) 0.041(3) 0.037(3) -0.008(3) -0.017(3) 0.002(3) C15 0.034(3) 0.054(4) 0.053(4) -0.014(3) -0.022(3) 0.004(3) C16 0.051(4) 0.062(5) 0.067(5) -0.015(4) -0.038(4) 0.018(3) C17 0.067(5) 0.042(4) 0.060(4) -0.008(3) -0.031(4) 0.022(3) C18 0.060(4) 0.040(4) 0.053(4) -0.012(3) -0.027(3) 0.003(3) C19 0.033(3) 0.057(4) 0.050(4) -0.003(3) -0.012(3) 0.005(3) C20 0.040(4) 0.072(5) 0.041(4) 0.006(3) -0.004(3) 0.001(3) C21 0.053(4) 0.097(6) 0.031(4) -0.013(4) -0.013(3) 0.009(4) C22 0.055(4) 0.071(5) 0.064(5) -0.036(4) -0.016(4) 0.011(4) C23 0.050(4) 0.045(4) 0.052(4) -0.010(3) -0.009(3) 0.008(3) C24 0.034(4) 0.067(5) 0.054(4) 0.012(4) -0.013(3) 0.001(3) Cd1 0.0454(4) 0.0447(5) 0.0559(5) -0.0159(3) -0.0342(4) 0.0050(3) N1 0.038(3) 0.044(3) 0.036(3) -0.004(2) -0.022(2) -0.009(3) N2 0.032(3) 0.034(3) 0.035(3) -0.004(2) -0.015(2) -0.004(2) N3 0.046(3) 0.043(3) 0.042(3) -0.004(3) -0.016(3) 0.004(3) N4 0.046(3) 0.045(3) 0.043(3) -0.011(2) -0.024(2) 0.011(2) N5 0.050(3) 0.038(3) 0.046(3) -0.012(2) -0.029(3) 0.010(2) N6 0.040(3) 0.040(3) 0.042(3) -0.004(2) -0.023(2) 0.000(2) O1 0.049(3) 0.057(3) 0.048(3) -0.003(2) -0.017(2) -0.014(2) O2 0.055(3) 0.073(4) 0.077(4) 0.017(3) -0.033(3) -0.016(3) O3 0.054(3) 0.082(4) 0.064(4) 0.016(3) -0.030(3) -0.011(3) N7 0.072(5) 0.082(5) 0.050(4) 0.003(4) -0.019(4) -0.025(4) O4 0.113(5) 0.095(5) 0.068(4) 0.018(3) -0.034(4) -0.022(4) O5 0.130(6) 0.120(6) 0.055(4) -0.012(4) -0.001(4) 0.006(4) O6 0.091(5) 0.092(5) 0.106(5) -0.027(4) -0.023(4) 0.013(4) P1 0.0517(11) 0.0585(12) 0.0578(12) -0.0015(9) -0.0255(9) -0.0061(9) F1 0.150(6) 0.075(4) 0.274(9) -0.008(4) -0.144(6) -0.019(4) F2 0.169(6) 0.258(9) 0.061(3) 0.013(4) 0.003(4) 0.163(6) F3 0.068(3) 0.070(3) 0.100(4) -0.007(3) -0.018(3) 0.019(2) F4 0.155(6) 0.109(5) 0.330(12) -0.012(6) -0.152(8) -0.038(5) F5 0.098(4) 0.097(4) 0.137(5) 0.022(3) -0.067(4) 0.017(3) F6 0.171(6) 0.198(7) 0.070(4) -0.003(4) -0.030(4) 0.040(6) O7 0.044(3) 0.101(4) 0.057(3) 0.003(3) -0.014(2) -0.008(3) O8 0.053(3) 0.105(4) 0.054(3) -0.007(3) -0.019(2) -0.009(3) O9 0.052(3) 0.104(4) 0.049(3) 0.010(3) -0.018(2) -0.016(3) O100 0.066(3) 0.098(4) 0.064(3) -0.018(3) -0.028(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C23 2.019(4) . ? Co1 C4 2.024(4) . ? Co1 C22 2.025(4) . ? Co1 C19 2.030(4) . ? Co1 C3 2.026(4) . ? Co1 C5 2.031(4) . ? Co1 C2 2.034(4) . ? Co1 C1 2.037(4) . ? Co1 C21 2.041(4) . ? Co1 C20 2.044(4) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C1 H1 0.9300 . ? C2 C3 1.4200 . ? C2 H2 0.9300 . ? C3 C4 1.4200 . ? C3 H3 0.9300 . ? C4 C5 1.4200 . ? C4 H4 0.9300 . ? C5 C6 1.496(6) . ? C6 O1 1.209(6) . ? C6 N1 1.375(7) . ? C7 N5 1.320(7) . ? C7 N2 1.361(7) . ? C7 C14 1.466(8) . ? C8 N4 1.306(7) . ? C8 N2 1.379(7) . ? C8 C9 1.464(8) . ? C9 N3 1.350(7) . ? C9 C10 1.356(8) . ? C10 C11 1.383(9) . ? C10 H10 0.9300 . ? C11 C12 1.379(9) . ? C11 H11 0.9300 . ? C12 C13 1.368(9) . ? C12 H12 0.9300 . ? C13 N3 1.325(8) . ? C13 H13 0.9300 . ? C14 N6 1.334(7) . ? C14 C15 1.385(8) . ? C15 C16 1.376(9) . ? C15 H15 0.9300 . ? C16 C17 1.345(9) . ? C16 H16 0.9300 . ? C17 C18 1.393(8) . ? C17 H17 0.9300 . ? C18 N6 1.320(7) . ? C18 H18 0.9300 . ? C19 C20 1.4200 . ? C19 C23 1.4200 . ? C19 C24 1.486(7) . ? C20 C21 1.4200 . ? C20 H20 0.9300 . ? C21 C22 1.4200 . ? C21 H21 0.9300 . ? C22 C23 1.4200 . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 O2 1.203(8) . ? C24 O3 1.315(8) . ? Cd1 N6 2.330(4) 2 ? Cd1 N6 2.330(4) . ? Cd1 N5 2.377(5) 2 ? Cd1 N5 2.377(5) . ? Cd1 O4 2.472(7) . ? Cd1 O4 2.472(7) 2 ? N1 N2 1.378(6) . ? N1 H100 0.79(6) . ? N3 H200 0.84(6) . ? N4 N5 1.373(7) . ? O3 H101 0.79(6) . ? N7 O6 1.223(9) . ? N7 O5 1.226(8) . ? N7 O4 1.235(8) . ? P1 F2 1.516(5) . ? P1 F4 1.520(6) . ? P1 F1 1.550(5) . ? P1 F6 1.570(6) . ? P1 F3 1.589(5) . ? P1 F5 1.590(5) . ? C100 O8 1.233(7) . ? C100 O7 1.229(7) . ? C100 O9 1.239(7) . ? 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 C23 Co1 C4 157.66(18) . . ? C23 Co1 C22 41.12(8) . . ? C4 Co1 C22 160.61(19) . . ? C23 Co1 C19 41.06(8) . . ? C4 Co1 C19 122.79(18) . . ? C22 Co1 C19 69.02(11) . . ? C23 Co1 C3 160.29(19) . . ? C4 Co1 C3 41.04(8) . . ? C22 Co1 C3 121.71(18) . . ? C19 Co1 C3 155.2(2) . . ? C23 Co1 C5 122.19(17) . . ? C4 Co1 C5 40.99(8) . . ? C22 Co1 C5 154.44(19) . . ? C19 Co1 C5 111.74(15) . . ? C3 Co1 C5 68.98(10) . . ? C23 Co1 C2 124.04(19) . . ? C4 Co1 C2 68.96(11) . . ? C22 Co1 C2 103.24(16) . . ? C19 Co1 C2 163.86(19) . . ? C3 Co1 C2 40.94(8) . . ? C5 Co1 C2 68.84(10) . . ? C23 Co1 C1 107.97(17) . . ? C4 Co1 C1 68.91(10) . . ? C22 Co1 C1 117.48(18) . . ? C19 Co1 C1 129.02(17) . . ? C3 Co1 C1 68.87(10) . . ? C5 Co1 C1 40.86(8) . . ? C2 Co1 C1 40.83(8) . . ? C23 Co1 C21 68.94(11) . . ? C4 Co1 C21 124.95(19) . . ? C22 Co1 C21 40.88(8) . . ? C19 Co1 C21 68.71(10) . . ? C3 Co1 C21 103.89(16) . . ? C5 Co1 C21 164.65(19) . . ? C2 Co1 C21 115.30(17) . . ? C1 Co1 C21 150.85(18) . . ? C23 Co1 C20 68.87(11) . . ? C4 Co1 C20 109.08(17) . . ? C22 Co1 C20 68.75(11) . . ? C19 Co1 C20 40.79(8) . . ? C3 Co1 C20 118.36(18) . . ? C5 Co1 C20 129.63(17) . . ? C2 Co1 C20 151.18(18) . . ? C1 Co1 C20 167.40(17) . . ? C21 Co1 C20 40.68(8) . . ? C2 C1 C5 108.0 . . ? C2 C1 Co1 69.47(16) . . ? C5 C1 Co1 69.35(16) . . ? C2 C1 H1 126.0 . . ? C5 C1 H1 126.0 . . ? Co1 C1 H1 126.7 . . ? C1 C2 C3 108.0 . . ? C1 C2 Co1 69.70(16) . . ? C3 C2 Co1 69.24(17) . . ? C1 C2 H2 126.0 . . ? C3 C2 H2 126.0 . . ? Co1 C2 H2 126.6 . . ? C4 C3 C2 108.0 . . ? C4 C3 Co1 69.41(16) . . ? C2 C3 Co1 69.82(16) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? Co1 C3 H3 126.3 . . ? C3 C4 C5 108.0 . . ? C3 C4 Co1 69.55(16) . . ? C5 C4 Co1 69.75(16) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Co1 C4 H4 126.3 . . ? C4 C5 C1 108.0 . . ? C4 C5 C6 123.5(3) . . ? C1 C5 C6 128.5(3) . . ? C4 C5 Co1 69.25(17) . . ? C1 C5 Co1 69.79(16) . . ? C6 C5 Co1 125.2(3) . . ? O1 C6 N1 123.7(5) . . ? O1 C6 C5 124.4(5) . . ? N1 C6 C5 111.9(5) . . ? N5 C7 N2 109.4(5) . . ? N5 C7 C14 121.3(5) . . ? N2 C7 C14 129.3(5) . . ? N4 C8 N2 109.9(5) . . ? N4 C8 C9 122.5(5) . . ? N2 C8 C9 127.6(5) . . ? N3 C9 C10 118.5(6) . . ? N3 C9 C8 113.7(5) . . ? C10 C9 C8 127.7(5) . . ? C9 C10 C11 118.9(6) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 121.1(6) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C13 C12 C11 118.2(6) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? N3 C13 C12 119.4(6) . . ? N3 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? N6 C14 C15 121.4(6) . . ? N6 C14 C7 113.6(5) . . ? C15 C14 C7 124.9(5) . . ? C16 C15 C14 118.2(6) . . ? C16 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? C17 C16 C15 120.2(6) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 118.8(6) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? N6 C18 C17 121.6(6) . . ? N6 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C20 C19 C23 108.0 . . ? C20 C19 C24 125.0(4) . . ? C23 C19 C24 126.9(4) . . ? C20 C19 Co1 70.13(17) . . ? C23 C19 Co1 69.02(17) . . ? C24 C19 Co1 124.1(4) . . ? C19 C20 C21 108.0 . . ? C19 C20 Co1 69.08(17) . . ? C21 C20 Co1 69.54(16) . . ? C19 C20 H20 126.0 . . ? C21 C20 H20 126.0 . . ? Co1 C20 H20 126.9 . . ? C22 C21 C20 108.0 . . ? C22 C21 Co1 68.96(17) . . ? C20 C21 Co1 69.78(16) . . ? C22 C21 H21 126.0 . . ? C20 C21 H21 126.0 . . ? Co1 C21 H21 126.8 . . ? C21 C22 C23 108.0 . . ? C21 C22 Co1 70.16(17) . . ? C23 C22 Co1 69.19(16) . . ? C21 C22 H22 126.0 . . ? C23 C22 H22 126.0 . . ? Co1 C22 H22 126.2 . . ? C19 C23 C22 108.0 . . ? C19 C23 Co1 69.92(17) . . ? C22 C23 Co1 69.69(17) . . ? C19 C23 H23 126.0 . . ? C22 C23 H23 126.0 . . ? Co1 C23 H23 126.0 . . ? O2 C24 O3 124.9(7) . . ? O2 C24 C19 123.1(6) . . ? O3 C24 C19 112.0(6) . . ? N6 Cd1 N6 180.0(3) 2 . ? N6 Cd1 N5 70.40(17) 2 2 ? N6 Cd1 N5 109.60(17) . 2 ? N6 Cd1 N5 109.60(17) 2 . ? N6 Cd1 N5 70.40(17) . . ? N5 Cd1 N5 180.0(2) 2 . ? N6 Cd1 O4 101.31(19) 2 . ? N6 Cd1 O4 78.69(19) . . ? N5 Cd1 O4 74.41(19) 2 . ? N5 Cd1 O4 105.59(19) . . ? N6 Cd1 O4 78.69(19) 2 2 ? N6 Cd1 O4 101.31(19) . 2 ? N5 Cd1 O4 105.59(19) 2 2 ? N5 Cd1 O4 74.41(19) . 2 ? O4 Cd1 O4 180.0(4) . 2 ? C6 N1 N2 118.3(5) . . ? C6 N1 H100 129(5) . . ? N2 N1 H100 112(5) . . ? C7 N2 C8 105.1(4) . . ? C7 N2 N1 129.1(5) . . ? C8 N2 N1 125.8(5) . . ? C13 N3 C9 123.9(6) . . ? C13 N3 H200 121(4) . . ? C9 N3 H200 114(4) . . ? C8 N4 N5 107.5(4) . . ? C7 N5 N4 108.1(4) . . ? C7 N5 Cd1 111.5(4) . . ? N4 N5 Cd1 132.7(3) . . ? C18 N6 C14 119.6(5) . . ? C18 N6 Cd1 121.8(4) . . ? C14 N6 Cd1 118.5(4) . . ? C24 O3 H101 115(5) . . ? O6 N7 O5 123.7(8) . . ? O6 N7 O4 115.8(7) . . ? O5 N7 O4 120.5(9) . . ? N7 O4 Cd1 104.2(6) . . ? F2 P1 F4 90.5(6) . . ? F2 P1 F1 93.2(5) . . ? F4 P1 F1 176.3(5) . . ? F2 P1 F6 179.0(4) . . ? F4 P1 F6 88.8(5) . . ? F1 P1 F6 87.5(5) . . ? F2 P1 F3 88.5(3) . . ? F4 P1 F3 91.3(3) . . ? F1 P1 F3 88.6(3) . . ? F6 P1 F3 90.8(3) . . ? F2 P1 F5 90.4(3) . . ? F4 P1 F5 90.5(4) . . ? F1 P1 F5 89.7(3) . . ? F6 P1 F5 90.4(4) . . ? F3 P1 F5 177.8(3) . . ? O8 C100 O7 122.2(6) . . ? O8 C100 O9 118.0(5) . . ? O7 C100 O9 119.8(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.694 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.095 data_1_[Co(C5H4-CONHC4H3N2)2]+[PF6]- _database_code_depnum_ccdc_archive 'CCDC 269427' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H16 Co F6 N6 O2 P' _chemical_formula_weight 576.29 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2145(2) _cell_length_b 10.0998(3) _cell_length_c 25.6180(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.3220(10) _cell_angle_gamma 90.00 _cell_volume 2103.01(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 0.980 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.757 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17330 _diffrn_reflns_av_R_equivalents 0.0925 _diffrn_reflns_av_sigmaI/netI 0.0916 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.99 _reflns_number_total 5058 _reflns_number_gt 2829 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5058 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1288 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1940 _refine_ls_wR_factor_gt 0.1548 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.28029(7) 0.69560(6) 0.10359(2) 0.0368(2) Uani 1 1 d . . . C1 C 0.1815(4) 0.7876(3) 0.16226(12) 0.0480(12) Uani 1 1 d G . . H1 H 0.2230 0.8625 0.1807 0.058 Uiso 1 1 calc R . . C2 C 0.0678(4) 0.7865(3) 0.11492(12) 0.0551(14) Uani 1 1 d G . . H2 H 0.0217 0.8606 0.0969 0.066 Uiso 1 1 calc R . . C3 C 0.0367(4) 0.6525(4) 0.09988(11) 0.0592(15) Uani 1 1 d G . . H3 H -0.0333 0.6234 0.0703 0.071 Uiso 1 1 calc R . . C4 C 0.1313(4) 0.5708(3) 0.13793(13) 0.0518(13) Uani 1 1 d G . . H4 H 0.1342 0.4787 0.1376 0.062 Uiso 1 1 calc R . . C5 C 0.2208(4) 0.6542(3) 0.17648(10) 0.0400(11) Uani 1 1 d G . . C6 C 0.3316(6) 0.5991(6) 0.22217(17) 0.0469(12) Uani 1 1 d . . . C7 C 0.5200(6) 0.6525(5) 0.30141(18) 0.0470(12) Uani 1 1 d . . . C8 C 0.7277(7) 0.6009(8) 0.3879(2) 0.0676(17) Uani 1 1 d . . . H8 H 0.7968 0.5854 0.4194 0.081 Uiso 1 1 calc R . . C9 C 0.5957(6) 0.5291(5) 0.3094(2) 0.0543(13) Uani 1 1 d . . . H9 H 0.5723 0.4639 0.2837 0.065 Uiso 1 1 calc R . . C10 C 0.6566(8) 0.7239(7) 0.3786(2) 0.0702(18) Uani 1 1 d . . . H10 H 0.6829 0.7904 0.4036 0.084 Uiso 1 1 calc R . . O1 O 0.3376(5) 0.4785(4) 0.22848(15) 0.0785(13) Uani 1 1 d . . . N1 N 0.4128(6) 0.6848(5) 0.25557(17) 0.0478(11) Uani 1 1 d . . . H100 H 0.398(6) 0.746(5) 0.2528(19) 0.026(16) Uiso 1 1 d . . . N2 N 0.5524(6) 0.7508(5) 0.33574(16) 0.0584(12) Uani 1 1 d . . . N3 N 0.6990(5) 0.5028(5) 0.35204(19) 0.0660(14) Uani 1 1 d . . . C11 C 0.4826(4) 0.7983(3) 0.08949(13) 0.0503(12) Uani 1 1 d G . . H11 H 0.5285 0.8709 0.1085 0.060 Uiso 1 1 calc R . . C12 C 0.3592(4) 0.8027(3) 0.04456(13) 0.0569(14) Uani 1 1 d G . . H12 H 0.3102 0.8788 0.0290 0.068 Uiso 1 1 calc R . . C13 C 0.3238(4) 0.6706(4) 0.02758(11) 0.0587(15) Uani 1 1 d G . . H13 H 0.2475 0.6450 -0.0011 0.070 Uiso 1 1 calc R . . C14 C 0.4253(4) 0.5846(3) 0.06202(13) 0.0509(12) Uani 1 1 d G . . H14 H 0.4271 0.4927 0.0599 0.061 Uiso 1 1 calc R . . C15 C 0.5234(4) 0.6634(3) 0.10029(11) 0.0423(11) Uani 1 1 d G . . C16 C 0.6409(6) 0.6029(6) 0.1428(2) 0.0517(13) Uani 1 1 d . . . C17 C 0.8338(6) 0.6459(5) 0.22308(18) 0.0448(11) Uani 1 1 d . . . C18 C 1.0472(7) 0.5907(6) 0.3079(2) 0.0634(15) Uani 1 1 d . . . H18 H 1.1207 0.5744 0.3383 0.076 Uiso 1 1 calc R . . C19 C 0.8938(7) 0.5180(6) 0.2333(2) 0.0614(15) Uani 1 1 d . . . H19 H 0.8570 0.4504 0.2099 0.074 Uiso 1 1 calc R . . C20 C 0.9896(7) 0.7166(6) 0.2979(2) 0.0610(15) Uani 1 1 d . . . H20 H 1.0261 0.7838 0.3215 0.073 Uiso 1 1 calc R . . O2 O 0.6605(6) 0.4842(4) 0.1429(2) 0.1062(19) Uani 1 1 d . . . N4 N 0.7229(5) 0.6828(5) 0.17878(18) 0.0520(11) Uani 1 1 d . . . H400 H 0.717(5) 0.754(5) 0.1813(16) 0.017(12) Uiso 1 1 d . . . N5 N 0.8830(6) 0.7456(5) 0.25543(17) 0.0566(11) Uani 1 1 d . . . N6 N 1.0007(6) 0.4905(5) 0.27491(19) 0.0662(13) Uani 1 1 d . . . P1 P 0.22466(17) 0.20490(16) 0.03660(5) 0.0549(4) Uani 1 1 d . . . F1 F 0.1802(5) 0.0909(4) 0.07451(15) 0.1070(14) Uani 1 1 d . A . F2 F 0.2705(6) 0.3178(5) -0.00138(16) 0.1062(15) Uani 1 1 d . A . F3 F 0.4047(10) 0.173(2) 0.0512(4) 0.180(8) Uani 0.70 1 d P A 1 F4 F 0.2155(19) 0.1153(10) -0.0130(3) 0.121(3) Uani 0.70 1 d P A 1 F5 F 0.0387(10) 0.2404(16) 0.0226(5) 0.136(5) Uani 0.70 1 d P A 1 F6 F 0.2337(18) 0.2933(11) 0.0858(4) 0.123(5) Uani 0.70 1 d P A 1 F3A F 0.344(5) 0.275(3) 0.0792(11) 0.166(16) Uani 0.30 1 d P A 2 F4A F 0.372(4) 0.114(2) 0.0250(16) 0.165(17) Uani 0.30 1 d P A 2 F5A F 0.092(5) 0.145(4) 0.0002(13) 0.20(2) Uani 0.30 1 d P A 2 F6A F 0.115(3) 0.328(2) 0.0468(13) 0.173(13) Uani 0.30 1 d P A 2 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 0.0344(3) 0.0418(4) 0.0333(3) -0.0020(3) 0.0015(2) 0.0006(3) C1 0.049(3) 0.054(3) 0.041(2) -0.003(2) 0.003(2) 0.007(2) C2 0.042(3) 0.073(4) 0.048(3) 0.000(3) 0.002(2) 0.016(3) C3 0.035(3) 0.092(5) 0.049(3) -0.005(3) -0.003(2) -0.007(3) C4 0.050(3) 0.055(4) 0.052(3) -0.006(2) 0.011(2) -0.012(2) C5 0.037(2) 0.048(3) 0.035(2) -0.003(2) 0.0089(18) 0.000(2) C6 0.052(3) 0.049(3) 0.040(2) -0.001(2) 0.008(2) 0.002(2) C7 0.049(3) 0.051(3) 0.041(2) 0.005(2) 0.005(2) -0.005(2) C8 0.052(3) 0.094(5) 0.055(3) 0.022(3) 0.001(2) -0.003(3) C9 0.050(3) 0.050(4) 0.060(3) 0.005(3) -0.002(2) -0.002(2) C10 0.077(4) 0.086(5) 0.044(3) -0.002(3) -0.002(3) -0.010(4) O1 0.103(3) 0.053(3) 0.067(2) -0.004(2) -0.026(2) 0.008(2) N1 0.060(3) 0.039(3) 0.042(2) 0.007(2) 0.0006(18) -0.001(2) N2 0.073(3) 0.061(3) 0.041(2) -0.008(2) 0.005(2) -0.003(2) N3 0.055(3) 0.074(4) 0.067(3) 0.022(3) -0.002(2) -0.002(2) C11 0.046(3) 0.045(3) 0.060(3) 0.001(2) 0.008(2) -0.005(2) C12 0.062(3) 0.060(4) 0.049(3) 0.017(3) 0.009(2) 0.002(3) C13 0.057(3) 0.084(5) 0.034(2) -0.003(3) 0.006(2) -0.004(3) C14 0.047(3) 0.051(3) 0.057(3) -0.015(3) 0.014(2) -0.004(2) C15 0.033(2) 0.044(3) 0.052(3) -0.001(2) 0.0116(19) -0.0010(19) C16 0.035(3) 0.046(3) 0.073(3) 0.004(3) 0.005(2) 0.000(2) C17 0.043(3) 0.042(3) 0.049(3) 0.000(2) 0.006(2) -0.002(2) C18 0.064(4) 0.066(4) 0.054(3) 0.004(3) -0.012(3) 0.003(3) C19 0.061(3) 0.051(4) 0.068(3) -0.002(3) -0.005(3) 0.007(3) C20 0.075(4) 0.053(4) 0.051(3) 0.000(3) -0.003(3) -0.014(3) O2 0.105(4) 0.047(3) 0.143(4) -0.008(3) -0.059(3) 0.012(3) N4 0.047(3) 0.046(3) 0.059(3) -0.004(2) -0.0070(19) 0.003(2) N5 0.064(3) 0.048(3) 0.056(3) -0.002(2) -0.001(2) 0.000(2) N6 0.072(3) 0.050(3) 0.072(3) 0.001(2) -0.007(2) 0.011(2) P1 0.0484(8) 0.0584(10) 0.0542(7) -0.0054(7) -0.0051(6) 0.0000(7) F1 0.136(4) 0.087(3) 0.093(3) 0.026(2) -0.001(2) -0.012(3) F2 0.113(3) 0.111(4) 0.096(3) 0.020(3) 0.020(2) -0.029(3) F3 0.059(4) 0.38(2) 0.092(6) -0.014(8) -0.007(4) 0.078(8) F4 0.176(10) 0.115(7) 0.069(4) -0.037(4) 0.005(6) 0.000(8) F5 0.044(4) 0.208(14) 0.160(10) 0.089(9) 0.026(5) 0.032(6) F6 0.197(13) 0.088(6) 0.095(6) -0.042(5) 0.061(9) -0.021(8) F3A 0.25(3) 0.096(19) 0.11(2) 0.038(15) -0.12(2) -0.09(2) F4A 0.21(3) 0.079(13) 0.25(3) 0.078(18) 0.18(3) 0.084(16) F5A 0.19(3) 0.23(4) 0.15(3) 0.09(2) -0.12(2) -0.18(3) F6A 0.115(16) 0.131(19) 0.25(3) -0.064(19) -0.051(18) 0.070(15) _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 C2 2.030(3) . ? Co1 C1 2.033(3) . ? Co1 C11 2.035(3) . ? Co1 C3 2.036(3) . ? Co1 C15 2.037(3) . ? Co1 C12 2.040(3) . ? Co1 C5 2.041(3) . ? Co1 C4 2.043(3) . ? Co1 C14 2.044(3) . ? Co1 C13 2.046(3) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C2 C3 1.4200 . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C5 C6 1.483(5) . ? C6 O1 1.229(6) . ? C6 N1 1.327(7) . ? C7 N2 1.327(7) . ? C7 C9 1.394(7) . ? C7 N1 1.400(6) . ? C8 N3 1.348(8) . ? C8 C10 1.379(9) . ? C9 N3 1.311(6) . ? C10 N2 1.320(7) . ? C11 C12 1.4200 . ? C11 C15 1.4200 . ? C12 C13 1.4200 . ? C13 C14 1.4200 . ? C14 C15 1.4200 . ? C15 C16 1.480(6) . ? C16 O2 1.209(6) . ? C16 N4 1.332(7) . ? C17 N5 1.330(6) . ? C17 C19 1.393(7) . ? C17 N4 1.399(6) . ? C18 N6 1.338(7) . ? C18 C20 1.368(8) . ? C19 N6 1.309(6) . ? C20 N5 1.326(7) . ? P1 F5A 1.460(15) . ? P1 F3 1.506(7) . ? P1 F6 1.537(8) . ? P1 F3A 1.533(17) . ? P1 F4 1.553(7) . ? P1 F5 1.559(7) . ? P1 F6A 1.582(18) . ? P1 F4A 1.582(17) . ? P1 F2 1.579(4) . ? P1 F1 1.583(4) . ? 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 C2 Co1 C1 40.91(6) . . ? C2 Co1 C11 122.42(14) . . ? C1 Co1 C11 108.78(12) . . ? C2 Co1 C3 40.88(6) . . ? C1 Co1 C3 68.75(8) . . ? C11 Co1 C3 157.32(15) . . ? C2 Co1 C15 161.17(15) . . ? C1 Co1 C15 127.02(12) . . ? C11 Co1 C15 40.82(6) . . ? C3 Co1 C15 157.90(15) . . ? C2 Co1 C12 103.78(13) . . ? C1 Co1 C12 120.62(14) . . ? C11 Co1 C12 40.79(6) . . ? C3 Co1 C12 119.61(13) . . ? C15 Co1 C12 68.60(8) . . ? C2 Co1 C5 68.72(7) . . ? C1 Co1 C5 40.80(5) . . ? C11 Co1 C5 125.21(12) . . ? C3 Co1 C5 68.61(7) . . ? C15 Co1 C5 111.80(11) . . ? C12 Co1 C5 158.56(14) . . ? C2 Co1 C4 68.68(8) . . ? C1 Co1 C4 68.63(7) . . ? C11 Co1 C4 161.17(14) . . ? C3 Co1 C4 40.75(6) . . ? C15 Co1 C4 124.85(13) . . ? C12 Co1 C4 157.07(14) . . ? C5 Co1 C4 40.70(6) . . ? C2 Co1 C14 154.24(13) . . ? C1 Co1 C14 163.93(13) . . ? C11 Co1 C14 68.58(7) . . ? C3 Co1 C14 120.08(13) . . ? C15 Co1 C14 40.72(6) . . ? C12 Co1 C14 68.47(8) . . ? C5 Co1 C14 126.81(13) . . ? C4 Co1 C14 108.44(12) . . ? C2 Co1 C13 117.65(12) . . ? C1 Co1 C13 154.62(14) . . ? C11 Co1 C13 68.54(8) . . ? C3 Co1 C13 103.59(11) . . ? C15 Co1 C13 68.49(7) . . ? C12 Co1 C13 40.68(6) . . ? C5 Co1 C13 160.70(15) . . ? C4 Co1 C13 122.14(13) . . ? C14 Co1 C13 40.64(6) . . ? C2 C1 C5 108.0 . . ? C2 C1 Co1 69.44(12) . . ? C5 C1 Co1 69.89(12) . . ? C3 C2 C1 108.0 . . ? C3 C2 Co1 69.79(12) . . ? C1 C2 Co1 69.65(11) . . ? C2 C3 C4 108.0 . . ? C2 C3 Co1 69.34(12) . . ? C4 C3 Co1 69.87(12) . . ? C3 C4 C5 108.0 . . ? C3 C4 Co1 69.38(12) . . ? C5 C4 Co1 69.57(11) . . ? C4 C5 C1 108.0 . . ? C4 C5 C6 121.5(3) . . ? C1 C5 C6 130.5(3) . . ? C4 C5 Co1 69.72(12) . . ? C1 C5 Co1 69.31(12) . . ? C6 C5 Co1 126.7(3) . . ? O1 C6 N1 123.7(5) . . ? O1 C6 C5 119.0(4) . . ? N1 C6 C5 117.2(5) . . ? N2 C7 C9 121.9(5) . . ? N2 C7 N1 115.0(5) . . ? C9 C7 N1 122.9(5) . . ? N3 C8 C10 121.2(5) . . ? N3 C9 C7 121.6(5) . . ? N2 C10 C8 122.4(6) . . ? C6 N1 C7 125.8(5) . . ? C10 N2 C7 116.2(5) . . ? C9 N3 C8 116.6(5) . . ? C12 C11 C15 108.0 . . ? C12 C11 Co1 69.80(12) . . ? C15 C11 Co1 69.68(12) . . ? C13 C12 C11 108.0 . . ? C13 C12 Co1 69.88(12) . . ? C11 C12 Co1 69.40(12) . . ? C12 C13 C14 108.0 . . ? C12 C13 Co1 69.44(13) . . ? C14 C13 Co1 69.62(12) . . ? C13 C14 C15 108.0 . . ? C13 C14 Co1 69.75(12) . . ? C15 C14 Co1 69.38(12) . . ? C14 C15 C11 108.0 . . ? C14 C15 C16 121.4(3) . . ? C11 C15 C16 130.6(3) . . ? C14 C15 Co1 69.90(12) . . ? C11 C15 Co1 69.50(13) . . ? C16 C15 Co1 125.1(3) . . ? O2 C16 N4 123.1(5) . . ? O2 C16 C15 118.9(5) . . ? N4 C16 C15 118.0(5) . . ? N5 C17 C19 121.2(5) . . ? N5 C17 N4 114.0(5) . . ? C19 C17 N4 124.8(5) . . ? N6 C18 C20 121.7(5) . . ? N6 C19 C17 121.8(5) . . ? N5 C20 C18 121.9(5) . . ? C16 N4 C17 127.1(5) . . ? C20 N5 C17 116.7(5) . . ? C19 N6 C18 116.7(5) . . ? F5A P1 F3 133(2) . . ? F5A P1 F6 135(2) . . ? F3 P1 F6 89.5(7) . . ? F5A P1 F3A 172(3) . . ? F3 P1 F3A 54.4(16) . . ? F6 P1 F3A 36.6(18) . . ? F5A P1 F4 45(2) . . ? F3 P1 F4 90.5(6) . . ? F6 P1 F4 179.8(6) . . ? F3A P1 F4 143(2) . . ? F5A P1 F5 48(2) . . ? F3 P1 F5 178.6(8) . . ? F6 P1 F5 89.1(7) . . ? F3A P1 F5 124.2(19) . . ? F4 P1 F5 90.9(6) . . ? F5A P1 F6A 92(2) . . ? F3 P1 F6A 133.6(12) . . ? F6 P1 F6A 50.8(10) . . ? F3A P1 F6A 80.8(17) . . ? F4 P1 F6A 129.3(11) . . ? F5 P1 F6A 45.0(8) . . ? F5A P1 F4A 99(2) . . ? F3 P1 F4A 34.2(15) . . ? F6 P1 F4A 122.9(18) . . ? F3A P1 F4A 89(2) . . ? F4 P1 F4A 57.0(15) . . ? F5 P1 F4A 147.3(16) . . ? F6A P1 F4A 163.6(15) . . ? F5A P1 F2 97.3(9) . . ? F3 P1 F2 89.6(7) . . ? F6 P1 F2 95.6(5) . . ? F3A P1 F2 85.3(10) . . ? F4 P1 F2 84.5(4) . . ? F5 P1 F2 90.3(4) . . ? F6A P1 F2 74.1(12) . . ? F4A P1 F2 92.7(7) . . ? F5A P1 F1 82.8(9) . . ? F3 P1 F1 89.9(7) . . ? F6 P1 F1 84.7(5) . . ? F3A P1 F1 94.7(10) . . ? F4 P1 F1 95.1(4) . . ? F5 P1 F1 90.2(4) . . ? F6A P1 F1 106.4(12) . . ? F4A P1 F1 86.7(7) . . ? F2 P1 F1 179.4(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.885 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.093