data_i-4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H40 Co F12 N8 O12 P2' _chemical_formula_weight 1173.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 23.169(3) _cell_length_b 23.169(3) _cell_length_c 8.2203(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4412.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2388 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type 'SORTAV' _exptl_absorpt_correction_T_min 0.462 _exptl_absorpt_correction_T_max 0.782 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(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 'Nonius Kappa CCD' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 0.72 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2824 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 28.13 _reflns_number_total 2824 _reflns_number_gt 2009 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Kappa CCD' _computing_cell_refinement 'Scalepack' _computing_data_reduction 'Maxus' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Simens SHEXLTL-90' _computing_publication_material 'Simens SHELXL-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1236P)^2^+1.0547P] 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 0.0047(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 2824 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1110 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.1955 _refine_ls_wR_factor_gt 0.1739 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 P1 P -0.16976(9) 0.73301(10) -0.4927(3) 0.0512(6) Uani 1 1 d . . . Co1 Co 1.0000 0.5000 0.7500 0.0304(5) Uani 1 4 d S . . Co2 Co 0.5000 0.5000 0.5000 0.0308(5) Uani 1 4 d S . . F1 F -0.1258(3) 0.6875(4) -0.543(2) 0.179(7) Uani 1 1 d . . . F2 F -0.2114(4) 0.7063(7) -0.6144(17) 0.192(7) Uani 1 1 d . . . F3 F -0.1258(4) 0.7565(6) -0.3652(18) 0.165(5) Uani 1 1 d . . . F4 F -0.2117(3) 0.7785(3) -0.4352(19) 0.152(5) Uani 1 1 d . . . F5 F -0.1992(7) 0.6926(5) -0.379(2) 0.222(8) Uani 1 1 d . . . F6 F -0.1406(7) 0.7750(6) -0.606(3) 0.246(10) Uani 1 1 d . . . O1 O 1.0200(2) 0.4135(2) 0.7455(7) 0.0461(13) Uani 1 1 d . . . O2 O 0.9404(3) 0.0827(2) 1.4250(7) 0.0519(15) Uani 1 1 d . . . O3 O 1.0000 0.5000 1.0095(8) 0.0399(15) Uani 1 2 d S . . O4 O 0.4507(2) 0.5758(2) 0.4979(7) 0.0416(12) Uani 1 1 d . . . O5 O 0.4358(3) 0.9183(2) -0.1730(8) 0.0511(15) Uani 1 1 d . . . O6 O 0.5000 0.5000 0.2401(9) 0.0394(15) Uani 1 2 d S . . O7 O 0.2305(4) 0.8360(4) -0.0028(16) 0.113(4) Uani 1 1 d . . . N1 N 1.0084(3) 0.3721(2) 0.8531(7) 0.0349(14) Uani 1 1 d . . . N2 N 0.9516(3) 0.1304(2) 1.3443(7) 0.0363(14) Uani 1 1 d . . . N3 N 0.4498(3) 0.6177(3) 0.3885(8) 0.0361(14) Uani 1 1 d . . . N4 N 0.4389(3) 0.8687(3) -0.0953(7) 0.0373(14) Uani 1 1 d . . . C1 C 1.0486(3) 0.3312(3) 0.8763(10) 0.0372(16) Uani 1 1 d . . . H1A H 1.0838 0.3335 0.8222 0.045 Uiso 1 1 calc R . . C2 C 1.0380(3) 0.2862(3) 0.9790(10) 0.0379(16) Uani 1 1 d . . . H2A H 1.0667 0.2588 0.9967 0.045 Uiso 1 1 calc R . . C3 C 0.9858(3) 0.2802(3) 1.0572(9) 0.0326(15) Uani 1 1 d . . . C4 C 0.9457(3) 0.3222(3) 1.0314(9) 0.0380(17) Uani 1 1 d . . . H4A H 0.9100 0.3200 1.0825 0.046 Uiso 1 1 calc R . . C5 C 0.9580(3) 0.3681(3) 0.9297(9) 0.0369(16) Uani 1 1 d . . . H5A H 0.9304 0.3968 0.9146 0.044 Uiso 1 1 calc R . . C6 C 0.9734(3) 0.2289(3) 1.1612(8) 0.0322(15) Uani 1 1 d . . . C7 C 1.0168(3) 0.1946(3) 1.2271(11) 0.0393(18) Uani 1 1 d . . . H7A H 1.0551 0.2050 1.2091 0.047 Uiso 1 1 calc R . . C8 C 1.0056(4) 0.1463(3) 1.3173(10) 0.0419(19) Uani 1 1 d . . . H8A H 1.0359 0.1247 1.3596 0.050 Uiso 1 1 calc R . . C9 C 0.9077(4) 0.1623(3) 1.2879(9) 0.0416(18) Uani 1 1 d . . . H9A H 0.8698 0.1515 1.3101 0.050 Uiso 1 1 calc R . . C10 C 0.9184(3) 0.2109(3) 1.1974(9) 0.0346(16) Uani 1 1 d . . . H10A H 0.8873 0.2324 1.1593 0.042 Uiso 1 1 calc R . . C11 C 0.4988(3) 0.6362(3) 0.3141(10) 0.0384(17) Uani 1 1 d . . . H11A H 0.5336 0.6173 0.3327 0.046 Uiso 1 1 calc R . . C12 C 0.4969(3) 0.6836(3) 0.2101(9) 0.0372(17) Uani 1 1 d . . . H12A H 0.5305 0.6953 0.1578 0.045 Uiso 1 1 calc R . . C13 C 0.4465(3) 0.7136(3) 0.1825(9) 0.0328(16) Uani 1 1 d . . . C14 C 0.3973(3) 0.6897(3) 0.2574(10) 0.0383(16) Uani 1 1 d . . . H14A H 0.3614 0.7063 0.2369 0.046 Uiso 1 1 calc R . . C15 C 0.4001(3) 0.6437(3) 0.3578(10) 0.0400(17) Uani 1 1 d . . . H15A H 0.3666 0.6300 0.4063 0.048 Uiso 1 1 calc R . . C16 C 0.4438(3) 0.7661(3) 0.0821(9) 0.0359(16) Uani 1 1 d . . . C17 C 0.4920(3) 0.7945(3) 0.0277(9) 0.0362(16) Uani 1 1 d . . . H17A H 0.5279 0.7785 0.0507 0.043 Uiso 1 1 calc R . . C18 C 0.4903(4) 0.8454(3) -0.0592(11) 0.0422(19) Uani 1 1 d . . . H18A H 0.5243 0.8633 -0.0922 0.051 Uiso 1 1 calc R . . C19 C 0.3904(4) 0.8408(3) -0.0545(11) 0.0435(19) Uani 1 1 d . . . H19A H 0.3549 0.8555 -0.0878 0.052 Uiso 1 1 calc R . . C20 C 0.3919(3) 0.7912(3) 0.0349(9) 0.0370(17) Uani 1 1 d . . . H20A H 0.3573 0.7737 0.0650 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0386(11) 0.0437(11) 0.0714(15) 0.0025(12) -0.0046(12) -0.0026(9) Co1 0.0310(7) 0.0310(7) 0.0292(9) 0.000 0.000 0.000 Co2 0.0305(6) 0.0305(6) 0.0314(10) 0.000 0.000 0.000 F1 0.061(4) 0.104(6) 0.37(2) -0.107(10) -0.007(8) 0.009(4) F2 0.086(6) 0.302(16) 0.188(12) -0.119(12) -0.069(7) 0.019(8) F3 0.077(5) 0.194(10) 0.225(13) -0.094(10) -0.067(7) 0.028(6) F4 0.061(4) 0.082(5) 0.312(16) -0.052(7) 0.011(7) 0.024(4) F5 0.283(17) 0.086(6) 0.296(19) 0.063(9) 0.154(15) -0.004(8) F6 0.226(14) 0.149(10) 0.36(3) 0.126(13) 0.165(17) 0.006(10) O1 0.055(3) 0.035(3) 0.048(3) 0.005(3) 0.014(3) 0.002(2) O2 0.068(4) 0.035(3) 0.052(3) 0.010(3) 0.015(3) -0.003(3) O3 0.039(4) 0.049(4) 0.031(3) 0.000 0.000 0.010(4) O4 0.047(3) 0.034(3) 0.044(3) 0.011(3) 0.008(3) 0.004(2) O5 0.068(4) 0.035(3) 0.051(3) 0.004(3) -0.015(3) 0.001(3) O6 0.041(4) 0.049(4) 0.028(3) 0.000 0.000 -0.009(4) O7 0.109(7) 0.061(5) 0.169(11) 0.002(6) -0.040(7) -0.010(5) N1 0.040(3) 0.031(3) 0.033(3) -0.002(3) 0.003(3) -0.003(3) N2 0.046(4) 0.024(3) 0.038(3) -0.001(3) 0.003(3) -0.001(3) N3 0.040(3) 0.035(3) 0.034(3) -0.005(3) 0.005(3) 0.002(3) N4 0.051(4) 0.025(3) 0.036(3) 0.002(3) -0.006(3) 0.000(3) C1 0.034(4) 0.034(4) 0.044(4) -0.003(3) 0.008(3) -0.003(3) C2 0.036(4) 0.029(3) 0.048(4) 0.000(3) -0.004(3) 0.003(3) C3 0.037(4) 0.030(4) 0.031(3) -0.006(3) -0.001(3) 0.001(3) C4 0.029(3) 0.042(4) 0.043(4) 0.003(3) 0.007(3) 0.005(3) C5 0.036(4) 0.034(4) 0.040(4) 0.000(3) 0.005(3) 0.006(3) C6 0.034(4) 0.034(4) 0.029(4) 0.002(3) -0.002(3) -0.001(3) C7 0.033(4) 0.034(4) 0.050(5) -0.001(4) -0.001(4) 0.001(3) C8 0.044(5) 0.040(4) 0.042(4) 0.004(3) 0.000(4) 0.009(4) C9 0.041(4) 0.041(4) 0.043(4) 0.003(3) 0.005(3) 0.005(3) C10 0.035(4) 0.029(4) 0.040(4) 0.001(3) -0.001(3) 0.004(3) C11 0.034(4) 0.037(4) 0.044(4) -0.004(3) 0.002(3) 0.002(3) C12 0.032(4) 0.038(4) 0.041(4) -0.003(3) 0.006(3) -0.005(3) C13 0.038(4) 0.028(3) 0.032(3) 0.000(3) 0.000(3) 0.003(3) C14 0.035(4) 0.037(4) 0.043(4) -0.005(4) 0.000(4) 0.000(3) C15 0.026(4) 0.046(4) 0.048(4) -0.002(4) -0.001(3) 0.002(3) C16 0.041(4) 0.031(4) 0.036(4) -0.005(3) -0.007(3) 0.002(3) C17 0.040(4) 0.031(4) 0.038(4) 0.000(3) -0.006(3) 0.001(3) C18 0.047(5) 0.035(4) 0.044(4) 0.003(3) -0.006(4) -0.006(3) C19 0.043(5) 0.040(4) 0.047(4) 0.003(4) -0.011(4) 0.006(3) C20 0.036(4) 0.037(4) 0.038(4) 0.003(3) 0.002(3) 0.001(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 P1 F5 1.488(11) . ? P1 F6 1.505(11) . ? P1 F4 1.509(7) . ? P1 F2 1.522(9) . ? P1 F1 1.524(8) . ? P1 F3 1.559(10) . ? Co1 O1 2.057(5) 8_646 ? Co1 O1 2.057(5) 2_765 ? Co1 O1 2.057(5) . ? Co1 O1 2.057(5) 7_566 ? Co1 O3 2.133(7) 7_566 ? Co1 O3 2.133(7) . ? Co2 O4 2.095(5) 3_566 ? Co2 O4 2.095(5) . ? Co2 O4 2.095(5) 2_665 ? Co2 O4 2.095(5) 4_656 ? Co2 O6 2.137(7) 3_566 ? Co2 O6 2.137(7) . ? O1 N1 1.331(8) . ? O2 N2 1.316(8) . ? O4 N3 1.324(8) . ? O5 N4 1.316(8) . ? N1 C5 1.331(9) . ? N1 C1 1.343(9) . ? N2 C8 1.324(10) . ? N2 C9 1.341(10) . ? N3 C15 1.323(9) . ? N3 C11 1.358(10) . ? N4 C19 1.340(10) . ? N4 C18 1.341(10) . ? C1 C2 1.365(11) . ? C2 C3 1.377(10) . ? C3 C4 1.362(10) . ? C3 C6 1.491(10) . ? C4 C5 1.382(11) . ? C6 C10 1.375(10) . ? C6 C7 1.391(10) . ? C7 C8 1.366(11) . ? C9 C10 1.372(11) . ? C11 C12 1.391(11) . ? C12 C13 1.377(11) . ? C13 C14 1.409(11) . ? C13 C16 1.472(10) . ? C14 C15 1.350(11) . ? C16 C17 1.372(11) . ? C16 C20 1.391(10) . ? C17 C18 1.380(11) . ? C19 C20 1.365(11) . ? 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 F5 P1 F6 178.7(9) . . ? F5 P1 F4 87.0(7) . . ? F6 P1 F4 91.8(7) . . ? F5 P1 F2 82.4(10) . . ? F6 P1 F2 98.1(12) . . ? F4 P1 F2 94.7(7) . . ? F5 P1 F1 92.4(8) . . ? F6 P1 F1 88.8(7) . . ? F4 P1 F1 177.3(8) . . ? F2 P1 F1 87.8(6) . . ? F5 P1 F3 95.5(11) . . ? F6 P1 F3 84.1(10) . . ? F4 P1 F3 88.1(6) . . ? F2 P1 F3 176.4(8) . . ? F1 P1 F3 89.4(6) . . ? O1 Co1 O1 90.018(8) 8_646 2_765 ? O1 Co1 O1 90.018(7) 8_646 . ? O1 Co1 O1 178.0(3) 2_765 . ? O1 Co1 O1 178.0(3) 8_646 7_566 ? O1 Co1 O1 90.018(9) 2_765 7_566 ? O1 Co1 O1 90.018(9) . 7_566 ? O1 Co1 O3 91.02(17) 8_646 7_566 ? O1 Co1 O3 88.98(17) 2_765 7_566 ? O1 Co1 O3 88.98(17) . 7_566 ? O1 Co1 O3 91.02(17) 7_566 7_566 ? O1 Co1 O3 88.98(17) 8_646 . ? O1 Co1 O3 91.02(17) 2_765 . ? O1 Co1 O3 91.02(17) . . ? O1 Co1 O3 88.98(17) 7_566 . ? O3 Co1 O3 180.000(2) 7_566 . ? O4 Co2 O4 90.004(4) 3_566 . ? O4 Co2 O4 90.004(4) 3_566 2_665 ? O4 Co2 O4 179.1(3) . 2_665 ? O4 Co2 O4 179.1(3) 3_566 4_656 ? O4 Co2 O4 90.004(5) . 4_656 ? O4 Co2 O4 90.004(4) 2_665 4_656 ? O4 Co2 O6 89.53(16) 3_566 3_566 ? O4 Co2 O6 90.47(16) . 3_566 ? O4 Co2 O6 90.47(16) 2_665 3_566 ? O4 Co2 O6 89.53(16) 4_656 3_566 ? O4 Co2 O6 90.47(16) 3_566 . ? O4 Co2 O6 89.53(16) . . ? O4 Co2 O6 89.53(16) 2_665 . ? O4 Co2 O6 90.47(16) 4_656 . ? O6 Co2 O6 180.000(1) 3_566 . ? N1 O1 Co1 130.1(4) . . ? N3 O4 Co2 129.0(4) . . ? O1 N1 C5 122.8(6) . . ? O1 N1 C1 117.6(6) . . ? C5 N1 C1 119.5(6) . . ? O2 N2 C8 120.4(6) . . ? O2 N2 C9 119.2(7) . . ? C8 N2 C9 120.4(7) . . ? C15 N3 O4 118.5(6) . . ? C15 N3 C11 119.8(7) . . ? O4 N3 C11 121.7(6) . . ? O5 N4 C19 119.8(6) . . ? O5 N4 C18 120.4(7) . . ? C19 N4 C18 119.8(6) . . ? N1 C1 C2 120.2(7) . . ? C1 C2 C3 121.6(7) . . ? C4 C3 C2 117.0(7) . . ? C4 C3 C6 122.0(6) . . ? C2 C3 C6 121.1(6) . . ? C3 C4 C5 120.3(7) . . ? N1 C5 C4 121.4(7) . . ? C10 C6 C7 114.4(6) . . ? C10 C6 C3 122.9(6) . . ? C7 C6 C3 122.7(6) . . ? C8 C7 C6 122.8(7) . . ? N2 C8 C7 119.9(7) . . ? N2 C9 C10 120.2(8) . . ? C9 C10 C6 122.3(7) . . ? N3 C11 C12 119.9(7) . . ? C13 C12 C11 121.7(7) . . ? C12 C13 C14 114.7(7) . . ? C12 C13 C16 123.1(7) . . ? C14 C13 C16 122.3(6) . . ? C15 C14 C13 122.4(7) . . ? N3 C15 C14 121.3(7) . . ? C17 C16 C20 114.4(7) . . ? C17 C16 C13 123.0(7) . . ? C20 C16 C13 122.7(7) . . ? C16 C17 C18 123.7(7) . . ? N4 C18 C17 118.9(8) . . ? N4 C19 C20 121.3(7) . . ? C19 C20 C16 121.6(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 28.13 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.781 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.132