data_compound_6 _publ_contact_author_name 'Peter Edwards' _publ_contact_author_address ;School of Chemistry Cardiff University Cardiff, CF10 3AT ; _publ_contact_author_email edwardspg@Cardiff.ac.uk _publ_contact_author_phone '+44 (0)29 20874083' _publ_contact_author_fax '+44 (0)29 20874030' loop_ _publ_author_name _publ_author_address 'Edwards, Peter G.' ;School of Chemistry Cardiff University Cardiff, CF10 3AT ; 'Newman, Paul D.' ;School of Chemistry Cardiff University Cardiff, CF10 3AT ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H42 F6 Fe P4 Si' _chemical_formula_weight 616.37 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' 'Fe' 'Fe' 0.3463 0.8444 '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 10.9946(5) _cell_length_b 16.3024(7) _cell_length_c 16.0530(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.311(2) _cell_angle_gamma 90.00 _cell_volume 2811.1(2) _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 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.856 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8144 _exptl_absorpt_correction_T_max 0.8752 _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 17383 _diffrn_reflns_av_R_equivalents 0.1584 _diffrn_reflns_av_sigmaI/netI 0.1123 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.45 _reflns_number_total 5143 _reflns_number_gt 3932 _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^)+(0.0418P)^2^+1.7505P] 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 5143 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1290 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 Fe1 Fe 0.24183(4) 0.24817(3) 0.03900(3) 0.03308(16) Uani 1 1 d . . . P1 P 0.36013(8) 0.18663(6) 0.14710(6) 0.0383(2) Uani 1 1 d . . . P2 P 0.41328(9) 0.29389(6) 0.00838(6) 0.0426(2) Uani 1 1 d . . . P3 P 0.24546(8) 0.36008(6) 0.11520(6) 0.0397(2) Uani 1 1 d . . . P4 P 0.71416(11) -0.02836(7) 0.29524(8) 0.0602(3) Uani 1 1 d . . . Si1 Si -0.04016(9) 0.14484(6) 0.09001(7) 0.0452(3) Uani 1 1 d . . . F1 F 0.7185(4) -0.0590(3) 0.3883(2) 0.1304(15) Uani 1 1 d . . . F2 F 0.6448(4) 0.0524(2) 0.3120(3) 0.1332(16) Uani 1 1 d . . . F3 F 0.5848(3) -0.0711(2) 0.2639(3) 0.1203(14) Uani 1 1 d . . . F4 F 0.7112(4) 0.0025(3) 0.2025(2) 0.1334(16) Uani 1 1 d . . . F5 F 0.7843(4) -0.1092(2) 0.2798(3) 0.1213(14) Uani 1 1 d . . . F6 F 0.8438(3) 0.0150(2) 0.3281(2) 0.1055(11) Uani 1 1 d . . . C1 C 0.0657(3) 0.1859(2) 0.0233(2) 0.0388(8) Uani 1 1 d . . . C2 C 0.0538(3) 0.2638(2) -0.0189(3) 0.0466(9) Uani 1 1 d . . . H2 H 0.0043 0.3066 -0.0069 0.056 Uiso 1 1 calc R . . C3 C 0.1259(4) 0.2669(3) -0.0802(3) 0.0582(12) Uani 1 1 d . . . H3 H 0.1331 0.3112 -0.1153 0.070 Uiso 1 1 calc R . . C4 C 0.1860(4) 0.1901(3) -0.0792(2) 0.0583(11) Uani 1 1 d . . . H4 H 0.2399 0.1748 -0.1140 0.070 Uiso 1 1 calc R . . C5 C 0.1505(3) 0.1413(2) -0.0169(2) 0.0447(9) Uani 1 1 d . . . H5 H 0.1777 0.0880 -0.0034 0.054 Uiso 1 1 calc R . . C6 C -0.0870(5) 0.2261(3) 0.1579(3) 0.0728(13) Uani 1 1 d . . . H6A H -0.0153 0.2447 0.1986 0.109 Uiso 1 1 calc R . . H6B H -0.1473 0.2044 0.1874 0.109 Uiso 1 1 calc R . . H6C H -0.1228 0.2713 0.1227 0.109 Uiso 1 1 calc R . . C7 C -0.1827(4) 0.1086(3) 0.0141(3) 0.0635(12) Uani 1 1 d . . . H7A H -0.2290 0.1550 -0.0126 0.095 Uiso 1 1 calc R . . H7B H -0.2333 0.0774 0.0444 0.095 Uiso 1 1 calc R . . H7C H -0.1591 0.0747 -0.0288 0.095 Uiso 1 1 calc R . . C8 C 0.0271(4) 0.0553(3) 0.1558(3) 0.0699(13) Uani 1 1 d . . . H8A H 0.0462 0.0127 0.1193 0.105 Uiso 1 1 calc R . . H8B H -0.0321 0.0352 0.1871 0.105 Uiso 1 1 calc R . . H8C H 0.1018 0.0718 0.1950 0.105 Uiso 1 1 calc R . . C9 C 0.5245(3) 0.2177(3) 0.1596(3) 0.0517(10) Uani 1 1 d . . . H9A H 0.5423 0.2634 0.1990 0.062 Uiso 1 1 calc R . . H9B H 0.5785 0.1725 0.1827 0.062 Uiso 1 1 calc R . . C10 C 0.5499(3) 0.2429(3) 0.0729(3) 0.0541(10) Uani 1 1 d . . . H10A H 0.5701 0.1947 0.0432 0.065 Uiso 1 1 calc R . . H10B H 0.6207 0.2798 0.0814 0.065 Uiso 1 1 calc R . . C11 C 0.4346(4) 0.4029(2) 0.0376(3) 0.0558(10) Uani 1 1 d . . . H11A H 0.5213 0.4183 0.0439 0.067 Uiso 1 1 calc R . . H11B H 0.3849 0.4369 -0.0064 0.067 Uiso 1 1 calc R . . C12 C 0.3941(4) 0.4148(2) 0.1206(3) 0.0518(10) Uani 1 1 d . . . H12A H 0.3834 0.4727 0.1306 0.062 Uiso 1 1 calc R . . H12B H 0.4570 0.3933 0.1673 0.062 Uiso 1 1 calc R . . C13 C 0.2344(4) 0.3509(2) 0.2276(2) 0.0504(9) Uani 1 1 d . . . H13A H 0.2421 0.4052 0.2529 0.060 Uiso 1 1 calc R . . H13B H 0.1524 0.3302 0.2296 0.060 Uiso 1 1 calc R . . C14 C 0.3316(4) 0.2952(3) 0.2815(2) 0.0558(10) Uani 1 1 d . . . H14A H 0.3201 0.2966 0.3398 0.067 Uiso 1 1 calc R . . H14B H 0.4134 0.3176 0.2817 0.067 Uiso 1 1 calc R . . C15 C 0.3297(4) 0.2054(2) 0.2530(2) 0.0510(10) Uani 1 1 d . . . H15A H 0.2488 0.1825 0.2546 0.061 Uiso 1 1 calc R . . H15B H 0.3912 0.1755 0.2942 0.061 Uiso 1 1 calc R . . C16 C 0.3724(4) 0.0750(2) 0.1470(3) 0.0516(10) Uani 1 1 d . . . H16A H 0.4204 0.0574 0.2020 0.062 Uiso 1 1 calc R . . H16B H 0.2895 0.0519 0.1403 0.062 Uiso 1 1 calc R . . C17 C 0.4329(4) 0.0400(3) 0.0773(3) 0.0627(12) Uani 1 1 d . . . H17A H 0.3872 0.0578 0.0225 0.094 Uiso 1 1 calc R . . H17B H 0.4322 -0.0188 0.0798 0.094 Uiso 1 1 calc R . . H17C H 0.5173 0.0590 0.0858 0.094 Uiso 1 1 calc R . . C18 C 0.4420(4) 0.2896(3) -0.0992(3) 0.0658(12) Uani 1 1 d . . . H18A H 0.4393 0.2328 -0.1173 0.079 Uiso 1 1 calc R . . H18B H 0.3754 0.3184 -0.1373 0.079 Uiso 1 1 calc R . . C19 C 0.5670(5) 0.3268(4) -0.1083(4) 0.0895(17) Uani 1 1 d . . . H19A H 0.5712 0.3830 -0.0901 0.134 Uiso 1 1 calc R . . H19B H 0.5739 0.3240 -0.1669 0.134 Uiso 1 1 calc R . . H19C H 0.6341 0.2966 -0.0736 0.134 Uiso 1 1 calc R . . C20 C 0.1276(4) 0.4381(2) 0.0738(3) 0.0573(11) Uani 1 1 d . . . H20A H 0.1227 0.4433 0.0130 0.069 Uiso 1 1 calc R . . H20B H 0.0476 0.4179 0.0812 0.069 Uiso 1 1 calc R . . C21 C 0.1470(5) 0.5231(3) 0.1130(3) 0.0709(13) Uani 1 1 d . . . H21A H 0.1643 0.5187 0.1740 0.106 Uiso 1 1 calc R . . H21B H 0.0731 0.5553 0.0941 0.106 Uiso 1 1 calc R . . H21C H 0.2158 0.5492 0.0955 0.106 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 Fe1 0.0292(2) 0.0370(3) 0.0333(3) -0.0002(2) 0.00710(19) -0.0040(2) P1 0.0341(5) 0.0422(5) 0.0386(5) 0.0029(4) 0.0081(4) -0.0013(4) P2 0.0357(5) 0.0497(6) 0.0447(5) 0.0034(4) 0.0140(4) -0.0082(4) P3 0.0349(5) 0.0397(5) 0.0430(5) -0.0048(4) 0.0054(4) -0.0014(4) P4 0.0516(6) 0.0595(7) 0.0674(7) 0.0045(6) 0.0077(6) 0.0097(5) Si1 0.0355(5) 0.0495(6) 0.0536(6) -0.0029(5) 0.0164(5) -0.0040(5) F1 0.137(3) 0.176(4) 0.080(2) 0.032(2) 0.026(2) 0.005(3) F2 0.105(3) 0.086(2) 0.208(4) -0.019(3) 0.033(3) 0.040(2) F3 0.074(2) 0.104(2) 0.168(4) 0.015(2) -0.009(2) -0.0246(19) F4 0.109(3) 0.200(4) 0.085(2) 0.053(3) 0.007(2) -0.004(3) F5 0.114(3) 0.104(2) 0.139(3) -0.024(2) 0.012(3) 0.046(2) F6 0.0707(19) 0.108(2) 0.125(3) 0.004(2) -0.0087(19) -0.0121(18) C1 0.0288(16) 0.0410(18) 0.0456(19) -0.0033(16) 0.0058(15) -0.0062(15) C2 0.0363(19) 0.0407(19) 0.056(2) 0.0032(17) -0.0065(18) -0.0043(16) C3 0.051(2) 0.075(3) 0.041(2) 0.012(2) -0.0062(19) -0.022(2) C4 0.051(2) 0.087(3) 0.040(2) -0.020(2) 0.0157(18) -0.030(2) C5 0.0394(19) 0.0414(19) 0.052(2) -0.0128(17) 0.0073(17) -0.0076(17) C6 0.057(3) 0.088(3) 0.080(3) -0.024(3) 0.029(2) -0.002(3) C7 0.046(2) 0.071(3) 0.076(3) -0.008(2) 0.019(2) -0.020(2) C8 0.061(3) 0.073(3) 0.083(3) 0.023(3) 0.030(3) 0.001(2) C9 0.0335(18) 0.055(2) 0.062(2) 0.0074(19) 0.0011(18) 0.0011(18) C10 0.0330(18) 0.065(3) 0.066(3) 0.006(2) 0.0157(18) -0.0020(19) C11 0.050(2) 0.052(2) 0.064(2) 0.007(2) 0.009(2) -0.0160(19) C12 0.048(2) 0.043(2) 0.062(2) -0.0065(18) 0.006(2) -0.0102(18) C13 0.055(2) 0.053(2) 0.044(2) -0.0117(18) 0.0140(19) -0.0002(19) C14 0.063(3) 0.065(3) 0.040(2) -0.0058(19) 0.0137(19) -0.001(2) C15 0.057(2) 0.058(2) 0.0353(19) 0.0066(17) 0.0054(18) -0.001(2) C16 0.048(2) 0.048(2) 0.060(2) 0.0076(18) 0.0146(19) 0.0029(18) C17 0.053(2) 0.057(2) 0.080(3) -0.012(2) 0.017(2) 0.008(2) C18 0.062(3) 0.088(3) 0.055(2) 0.004(2) 0.029(2) -0.014(3) C19 0.074(3) 0.122(5) 0.086(4) 0.012(3) 0.048(3) -0.019(3) C20 0.049(2) 0.053(2) 0.065(3) -0.008(2) 0.000(2) 0.005(2) C21 0.066(3) 0.052(2) 0.089(3) -0.010(2) 0.005(3) 0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C3 2.083(4) . ? Fe1 C4 2.092(4) . ? Fe1 C2 2.094(3) . ? Fe1 C5 2.112(3) . ? Fe1 C1 2.153(3) . ? Fe1 P2 2.1784(10) . ? Fe1 P1 2.1788(10) . ? Fe1 P3 2.1921(10) . ? P1 C16 1.826(4) . ? P1 C15 1.827(4) . ? P1 C9 1.847(4) . ? P2 C18 1.822(4) . ? P2 C10 1.833(4) . ? P2 C11 1.840(4) . ? P3 C20 1.836(4) . ? P3 C13 1.840(4) . ? P3 C12 1.847(4) . ? P4 F4 1.566(4) . ? P4 F1 1.566(4) . ? P4 F3 1.568(3) . ? P4 F5 1.573(3) . ? P4 F2 1.573(3) . ? P4 F6 1.578(3) . ? Si1 C6 1.857(5) . ? Si1 C8 1.860(4) . ? Si1 C7 1.865(4) . ? Si1 C1 1.866(4) . ? C1 C2 1.431(5) . ? C1 C5 1.440(5) . ? C2 C3 1.390(6) . ? C3 C4 1.414(6) . ? C4 C5 1.398(6) . ? C9 C10 1.531(6) . ? C11 C12 1.505(6) . ? C13 C14 1.524(6) . ? C14 C15 1.533(6) . ? C16 C17 1.529(6) . ? C18 C19 1.537(6) . ? C20 C21 1.519(6) . ? 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 C3 Fe1 C4 39.59(18) . . ? C3 Fe1 C2 38.87(18) . . ? C4 Fe1 C2 65.26(17) . . ? C3 Fe1 C5 65.69(16) . . ? C4 Fe1 C5 38.82(16) . . ? C2 Fe1 C5 64.97(14) . . ? C3 Fe1 C1 66.59(15) . . ? C4 Fe1 C1 66.33(15) . . ? C2 Fe1 C1 39.37(14) . . ? C5 Fe1 C1 39.44(14) . . ? C3 Fe1 P2 97.59(13) . . ? C4 Fe1 P2 92.89(12) . . ? C2 Fe1 P2 132.71(12) . . ? C5 Fe1 P2 122.81(11) . . ? C1 Fe1 P2 159.22(10) . . ? C3 Fe1 P1 160.66(14) . . ? C4 Fe1 P1 121.60(14) . . ? C2 Fe1 P1 140.79(11) . . ? C5 Fe1 P1 96.17(11) . . ? C1 Fe1 P1 104.20(10) . . ? P2 Fe1 P1 86.50(4) . . ? C3 Fe1 P3 108.99(14) . . ? C4 Fe1 P3 148.16(14) . . ? C2 Fe1 P3 92.60(11) . . ? C5 Fe1 P3 150.89(11) . . ? C1 Fe1 P3 111.49(10) . . ? P2 Fe1 P3 85.85(4) . . ? P1 Fe1 P3 90.12(4) . . ? C16 P1 C15 101.27(19) . . ? C16 P1 C9 101.73(19) . . ? C15 P1 C9 102.9(2) . . ? C16 P1 Fe1 119.36(13) . . ? C15 P1 Fe1 117.88(14) . . ? C9 P1 Fe1 111.35(13) . . ? C18 P2 C10 103.4(2) . . ? C18 P2 C11 103.9(2) . . ? C10 P2 C11 104.44(19) . . ? C18 P2 Fe1 122.29(15) . . ? C10 P2 Fe1 111.21(14) . . ? C11 P2 Fe1 110.00(15) . . ? C20 P3 C13 102.9(2) . . ? C20 P3 C12 103.40(19) . . ? C13 P3 C12 103.64(19) . . ? C20 P3 Fe1 116.55(13) . . ? C13 P3 Fe1 118.82(13) . . ? C12 P3 Fe1 109.79(14) . . ? F4 P4 F1 179.4(3) . . ? F4 P4 F3 90.3(2) . . ? F1 P4 F3 90.3(3) . . ? F4 P4 F5 91.8(3) . . ? F1 P4 F5 88.1(2) . . ? F3 P4 F5 91.1(2) . . ? F4 P4 F2 88.9(3) . . ? F1 P4 F2 91.2(3) . . ? F3 P4 F2 89.3(2) . . ? F5 P4 F2 179.2(2) . . ? F4 P4 F6 90.4(2) . . ? F1 P4 F6 89.0(2) . . ? F3 P4 F6 179.1(3) . . ? F5 P4 F6 89.4(2) . . ? F2 P4 F6 90.3(2) . . ? C6 Si1 C8 110.7(2) . . ? C6 Si1 C7 108.1(2) . . ? C8 Si1 C7 107.4(2) . . ? C6 Si1 C1 111.4(2) . . ? C8 Si1 C1 112.74(19) . . ? C7 Si1 C1 106.20(19) . . ? C2 C1 C5 103.8(3) . . ? C2 C1 Si1 125.8(3) . . ? C5 C1 Si1 128.2(3) . . ? C2 C1 Fe1 68.1(2) . . ? C5 C1 Fe1 68.78(19) . . ? Si1 C1 Fe1 139.29(18) . . ? C3 C2 C1 111.1(4) . . ? C3 C2 Fe1 70.2(2) . . ? C1 C2 Fe1 72.54(19) . . ? C2 C3 C4 107.2(4) . . ? C2 C3 Fe1 71.0(2) . . ? C4 C3 Fe1 70.5(2) . . ? C5 C4 C3 108.1(4) . . ? C5 C4 Fe1 71.4(2) . . ? C3 C4 Fe1 69.9(2) . . ? C4 C5 C1 109.9(4) . . ? C4 C5 Fe1 69.8(2) . . ? C1 C5 Fe1 71.78(19) . . ? C10 C9 P1 109.8(3) . . ? C9 C10 P2 110.4(3) . . ? C12 C11 P2 107.7(3) . . ? C11 C12 P3 108.8(3) . . ? C14 C13 P3 114.9(3) . . ? C13 C14 C15 115.8(3) . . ? C14 C15 P1 116.4(3) . . ? C17 C16 P1 114.6(3) . . ? C19 C18 P2 114.5(3) . . ? C21 C20 P3 117.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Fe1 P1 C16 -7.4(4) . . . . ? C4 Fe1 P1 C16 -19.2(2) . . . . ? C2 Fe1 P1 C16 69.5(2) . . . . ? C5 Fe1 P1 C16 12.2(2) . . . . ? C1 Fe1 P1 C16 51.5(2) . . . . ? P2 Fe1 P1 C16 -110.41(17) . . . . ? P3 Fe1 P1 C16 163.76(16) . . . . ? C3 Fe1 P1 C15 -130.8(4) . . . . ? C4 Fe1 P1 C15 -142.6(2) . . . . ? C2 Fe1 P1 C15 -54.0(2) . . . . ? C5 Fe1 P1 C15 -111.22(19) . . . . ? C1 Fe1 P1 C15 -71.93(19) . . . . ? P2 Fe1 P1 C15 126.13(16) . . . . ? P3 Fe1 P1 C15 40.30(16) . . . . ? C3 Fe1 P1 C9 110.7(4) . . . . ? C4 Fe1 P1 C9 98.9(2) . . . . ? C2 Fe1 P1 C9 -172.4(2) . . . . ? C5 Fe1 P1 C9 130.29(19) . . . . ? C1 Fe1 P1 C9 169.58(18) . . . . ? P2 Fe1 P1 C9 7.64(16) . . . . ? P3 Fe1 P1 C9 -78.19(16) . . . . ? C3 Fe1 P2 C18 -28.0(3) . . . . ? C4 Fe1 P2 C18 11.5(3) . . . . ? C2 Fe1 P2 C18 -47.0(3) . . . . ? C5 Fe1 P2 C18 37.9(3) . . . . ? C1 Fe1 P2 C18 10.9(4) . . . . ? P1 Fe1 P2 C18 133.0(2) . . . . ? P3 Fe1 P2 C18 -136.7(2) . . . . ? C3 Fe1 P2 C10 -150.7(2) . . . . ? C4 Fe1 P2 C10 -111.2(2) . . . . ? C2 Fe1 P2 C10 -169.6(2) . . . . ? C5 Fe1 P2 C10 -84.7(2) . . . . ? C1 Fe1 P2 C10 -111.8(3) . . . . ? P1 Fe1 P2 C10 10.35(16) . . . . ? P3 Fe1 P2 C10 100.72(16) . . . . ? C3 Fe1 P2 C11 94.1(2) . . . . ? C4 Fe1 P2 C11 133.6(2) . . . . ? C2 Fe1 P2 C11 75.2(2) . . . . ? C5 Fe1 P2 C11 160.06(19) . . . . ? C1 Fe1 P2 C11 133.0(3) . . . . ? P1 Fe1 P2 C11 -104.85(14) . . . . ? P3 Fe1 P2 C11 -14.48(14) . . . . ? C3 Fe1 P3 C20 12.5(2) . . . . ? C4 Fe1 P3 C20 20.3(3) . . . . ? C2 Fe1 P3 C20 -23.6(2) . . . . ? C5 Fe1 P3 C20 -61.5(3) . . . . ? C1 Fe1 P3 C20 -59.1(2) . . . . ? P2 Fe1 P3 C20 109.07(18) . . . . ? P1 Fe1 P3 C20 -164.45(18) . . . . ? C3 Fe1 P3 C13 136.4(2) . . . . ? C4 Fe1 P3 C13 144.3(3) . . . . ? C2 Fe1 P3 C13 100.40(19) . . . . ? C5 Fe1 P3 C13 62.5(3) . . . . ? C1 Fe1 P3 C13 64.86(18) . . . . ? P2 Fe1 P3 C13 -126.95(16) . . . . ? P1 Fe1 P3 C13 -40.47(16) . . . . ? C3 Fe1 P3 C12 -104.61(19) . . . . ? C4 Fe1 P3 C12 -96.8(3) . . . . ? C2 Fe1 P3 C12 -140.65(18) . . . . ? C5 Fe1 P3 C12 -178.5(3) . . . . ? C1 Fe1 P3 C12 -176.19(17) . . . . ? P2 Fe1 P3 C12 -8.00(14) . . . . ? P1 Fe1 P3 C12 78.48(14) . . . . ? C6 Si1 C1 C2 -40.1(4) . . . . ? C8 Si1 C1 C2 -165.3(3) . . . . ? C7 Si1 C1 C2 77.3(3) . . . . ? C6 Si1 C1 C5 159.5(3) . . . . ? C8 Si1 C1 C5 34.4(4) . . . . ? C7 Si1 C1 C5 -83.0(3) . . . . ? C6 Si1 C1 Fe1 57.5(3) . . . . ? C8 Si1 C1 Fe1 -67.7(3) . . . . ? C7 Si1 C1 Fe1 174.9(3) . . . . ? C3 Fe1 C1 C2 -35.9(3) . . . . ? C4 Fe1 C1 C2 -79.3(3) . . . . ? C5 Fe1 C1 C2 -115.6(3) . . . . ? P2 Fe1 C1 C2 -78.6(4) . . . . ? P1 Fe1 C1 C2 162.1(2) . . . . ? P3 Fe1 C1 C2 66.2(2) . . . . ? C3 Fe1 C1 C5 79.6(3) . . . . ? C4 Fe1 C1 C5 36.3(2) . . . . ? C2 Fe1 C1 C5 115.6(3) . . . . ? P2 Fe1 C1 C5 36.9(4) . . . . ? P1 Fe1 C1 C5 -82.4(2) . . . . ? P3 Fe1 C1 C5 -178.20(19) . . . . ? C3 Fe1 C1 Si1 -155.8(3) . . . . ? C4 Fe1 C1 Si1 160.8(3) . . . . ? C2 Fe1 C1 Si1 -119.9(4) . . . . ? C5 Fe1 C1 Si1 124.5(4) . . . . ? P2 Fe1 C1 Si1 161.46(14) . . . . ? P1 Fe1 C1 Si1 42.2(3) . . . . ? P3 Fe1 C1 Si1 -53.7(3) . . . . ? C5 C1 C2 C3 -0.1(4) . . . . ? Si1 C1 C2 C3 -164.3(3) . . . . ? Fe1 C1 C2 C3 59.8(3) . . . . ? C5 C1 C2 Fe1 -60.0(2) . . . . ? Si1 C1 C2 Fe1 135.8(3) . . . . ? C4 Fe1 C2 C3 -38.7(3) . . . . ? C5 Fe1 C2 C3 -81.7(3) . . . . ? C1 Fe1 C2 C3 -120.9(3) . . . . ? P2 Fe1 C2 C3 30.8(3) . . . . ? P1 Fe1 C2 C3 -149.1(2) . . . . ? P3 Fe1 C2 C3 117.6(2) . . . . ? C3 Fe1 C2 C1 120.9(3) . . . . ? C4 Fe1 C2 C1 82.2(2) . . . . ? C5 Fe1 C2 C1 39.2(2) . . . . ? P2 Fe1 C2 C1 151.74(17) . . . . ? P1 Fe1 C2 C1 -28.1(3) . . . . ? P3 Fe1 C2 C1 -121.5(2) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? Fe1 C2 C3 C4 61.6(2) . . . . ? C1 C2 C3 Fe1 -61.3(3) . . . . ? C4 Fe1 C3 C2 117.0(3) . . . . ? C5 Fe1 C3 C2 79.7(2) . . . . ? C1 Fe1 C3 C2 36.4(2) . . . . ? P2 Fe1 C3 C2 -157.7(2) . . . . ? P1 Fe1 C3 C2 101.1(5) . . . . ? P3 Fe1 C3 C2 -69.5(2) . . . . ? C2 Fe1 C3 C4 -117.0(3) . . . . ? C5 Fe1 C3 C4 -37.3(2) . . . . ? C1 Fe1 C3 C4 -80.6(2) . . . . ? P2 Fe1 C3 C4 85.3(2) . . . . ? P1 Fe1 C3 C4 -15.8(5) . . . . ? P3 Fe1 C3 C4 173.5(2) . . . . ? C2 C3 C4 C5 -0.4(4) . . . . ? Fe1 C3 C4 C5 61.5(3) . . . . ? C2 C3 C4 Fe1 -61.9(3) . . . . ? C3 Fe1 C4 C5 -118.2(4) . . . . ? C2 Fe1 C4 C5 -80.2(3) . . . . ? C1 Fe1 C4 C5 -36.8(2) . . . . ? P2 Fe1 C4 C5 143.4(2) . . . . ? P1 Fe1 C4 C5 55.7(3) . . . . ? P3 Fe1 C4 C5 -129.8(2) . . . . ? C2 Fe1 C4 C3 38.0(2) . . . . ? C5 Fe1 C4 C3 118.2(4) . . . . ? C1 Fe1 C4 C3 81.3(3) . . . . ? P2 Fe1 C4 C3 -98.4(2) . . . . ? P1 Fe1 C4 C3 173.9(2) . . . . ? P3 Fe1 C4 C3 -11.6(4) . . . . ? C3 C4 C5 C1 0.3(4) . . . . ? Fe1 C4 C5 C1 60.8(2) . . . . ? C3 C4 C5 Fe1 -60.5(3) . . . . ? C2 C1 C5 C4 -0.1(4) . . . . ? Si1 C1 C5 C4 163.5(3) . . . . ? Fe1 C1 C5 C4 -59.6(2) . . . . ? C2 C1 C5 Fe1 59.5(2) . . . . ? Si1 C1 C5 Fe1 -136.8(3) . . . . ? C3 Fe1 C5 C4 38.1(3) . . . . ? C2 Fe1 C5 C4 81.0(3) . . . . ? C1 Fe1 C5 C4 120.2(3) . . . . ? P2 Fe1 C5 C4 -45.1(3) . . . . ? P1 Fe1 C5 C4 -134.9(2) . . . . ? P3 Fe1 C5 C4 123.6(3) . . . . ? C3 Fe1 C5 C1 -82.1(2) . . . . ? C4 Fe1 C5 C1 -120.2(3) . . . . ? C2 Fe1 C5 C1 -39.2(2) . . . . ? P2 Fe1 C5 C1 -165.30(17) . . . . ? P1 Fe1 C5 C1 104.9(2) . . . . ? P3 Fe1 C5 C1 3.4(4) . . . . ? C16 P1 C9 C10 100.6(3) . . . . ? C15 P1 C9 C10 -154.8(3) . . . . ? Fe1 P1 C9 C10 -27.6(3) . . . . ? P1 C9 C10 P2 35.2(4) . . . . ? C18 P2 C10 C9 -163.0(3) . . . . ? C11 P2 C10 C9 88.6(3) . . . . ? Fe1 P2 C10 C9 -30.0(3) . . . . ? C18 P2 C11 C12 171.7(3) . . . . ? C10 P2 C11 C12 -80.2(3) . . . . ? Fe1 P2 C11 C12 39.2(3) . . . . ? P2 C11 C12 P3 -44.8(3) . . . . ? C20 P3 C12 C11 -90.8(3) . . . . ? C13 P3 C12 C11 162.1(3) . . . . ? Fe1 P3 C12 C11 34.2(3) . . . . ? C20 P3 C13 C14 -174.4(3) . . . . ? C12 P3 C13 C14 -67.0(3) . . . . ? Fe1 P3 C13 C14 55.1(3) . . . . ? P3 C13 C14 C15 -60.7(5) . . . . ? C13 C14 C15 P1 62.0(5) . . . . ? C16 P1 C15 C14 171.8(3) . . . . ? C9 P1 C15 C14 66.8(3) . . . . ? Fe1 P1 C15 C14 -56.1(3) . . . . ? C15 P1 C16 C17 -163.9(3) . . . . ? C9 P1 C16 C17 -58.0(3) . . . . ? Fe1 P1 C16 C17 64.9(3) . . . . ? C10 P2 C18 C19 -55.2(5) . . . . ? C11 P2 C18 C19 53.6(5) . . . . ? Fe1 P2 C18 C19 178.6(3) . . . . ? C13 P3 C20 C21 62.5(4) . . . . ? C12 P3 C20 C21 -45.1(4) . . . . ? Fe1 P3 C20 C21 -165.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.45 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.754 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.100 #===END data_compound_10a _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H38 F6 Fe P4' _chemical_formula_weight 620.27 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' F F 0.0171 0.0103 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'R -3' _symmetry_int_tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 42.467(6) _cell_length_b 42.467(6) _cell_length_c 9.690(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 15134(4) _cell_formula_units_Z 18 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour red _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5796 _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_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 28355 _diffrn_reflns_av_R_equivalents 0.0939 _diffrn_reflns_av_sigmaI/netI 0.0826 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -54 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7692 _reflns_number_gt 5363 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXs-97 (Sheldrick, 1997)' _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^)+(0.1282P)^2^+29.3775P] 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 0.00025(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7692 _refine_ls_number_parameters 363 _refine_ls_number_restraints 71 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0771 _refine_ls_wR_factor_ref 0.2286 _refine_ls_wR_factor_gt 0.2155 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.650 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.05586(2) 0.80972(2) 0.49982(8) 0.0277(3) Uani 1 1 d . . . P1 P 0.08334(4) 0.81074(4) 0.69300(16) 0.0356(4) Uani 1 1 d . . . P2 P 0.10264(5) 0.85993(5) 0.43751(19) 0.0468(5) Uani 1 1 d D . . H2 H 0.1006 0.8613 0.3372 0.056 Uiso 1 1 calc RD . . P3 P 0.03862(5) 0.84339(5) 0.60691(19) 0.0441(5) Uani 1 1 d D . . H3 H 0.0123 0.8328 0.5949 0.053 Uiso 1 1 calc RD . . P4 P 0.16434(5) 0.92992(5) 0.0666(2) 0.0550(6) Uani 1 1 d D . . F1 F 0.20570(14) 0.9576(2) 0.0475(9) 0.130(3) Uani 1 1 d DU A . F2 F 0.12272(12) 0.90297(17) 0.0855(6) 0.098(2) Uani 1 1 d DU A . F3 F 0.1546(5) 0.9577(5) 0.005(2) 0.113(7) Uani 0.64(3) 1 d PDU A 1 F3' F 0.1488(8) 0.9317(11) -0.076(2) 0.152(15) Uani 0.36(3) 1 d PDU A 2 F4 F 0.1641(4) 0.9453(4) 0.2134(9) 0.104(6) Uani 0.72(2) 1 d PDU A 1 F4' F 0.1641(11) 0.9681(8) 0.054(4) 0.099(12) Uani 0.28(2) 1 d PU A 2 F5 F 0.1750(3) 0.9036(3) 0.1343(10) 0.117(4) Uani 0.83(2) 1 d PDU A 1 F5' F 0.1663(12) 0.9348(10) 0.2250(9) 0.065(11) Uani 0.17(2) 1 d PDU A 2 F6 F 0.1656(2) 0.9154(3) -0.0799(7) 0.095(5) Uani 0.78(2) 1 d PDU A 1 F6' F 0.1599(12) 0.8935(7) 0.016(6) 0.137(19) Uani 0.22(2) 1 d PDU A 2 C1 C 0.0428(2) 0.75712(18) 0.4355(7) 0.0465(17) Uani 1 1 d . . . C2 C 0.01059(17) 0.75720(17) 0.4797(6) 0.0413(15) Uani 1 1 d . . . C3 C 0.00591(16) 0.78139(18) 0.3925(6) 0.0392(14) Uani 1 1 d . . . C4 C 0.03501(17) 0.79644(19) 0.2970(6) 0.0408(15) Uani 1 1 d . . . C5 C 0.05807(17) 0.7817(2) 0.3246(7) 0.0441(16) Uani 1 1 d . . . C6 C 0.0554(3) 0.7319(2) 0.4872(10) 0.079(3) Uani 1 1 d . . . H6A H 0.0458 0.7108 0.4290 0.119 Uiso 1 1 calc R . . H6B H 0.0470 0.7246 0.5800 0.119 Uiso 1 1 calc R . . H6C H 0.0815 0.7441 0.4856 0.119 Uiso 1 1 calc R . . C7 C -0.0165(2) 0.7328(2) 0.5842(7) 0.064(2) Uani 1 1 d . . . H7A H -0.0052 0.7238 0.6460 0.095 Uiso 1 1 calc R . . H7B H -0.0366 0.7128 0.5381 0.095 Uiso 1 1 calc R . . H7C H -0.0253 0.7463 0.6356 0.095 Uiso 1 1 calc R . . C8 C -0.0266(2) 0.7865(3) 0.3906(9) 0.068(2) Uani 1 1 d . . . H8A H -0.0399 0.7766 0.3066 0.102 Uiso 1 1 calc R . . H8B H -0.0187 0.8119 0.3957 0.102 Uiso 1 1 calc R . . H8C H -0.0419 0.7741 0.4681 0.102 Uiso 1 1 calc R . . C9 C 0.0381(2) 0.8207(3) 0.1796(7) 0.066(2) Uani 1 1 d . . . H9A H 0.0322 0.8385 0.2112 0.099 Uiso 1 1 calc R . . H9B H 0.0215 0.8064 0.1077 0.099 Uiso 1 1 calc R . . H9C H 0.0625 0.8326 0.1445 0.099 Uiso 1 1 calc R . . C10 C 0.0899(2) 0.7879(3) 0.2356(9) 0.070(3) Uani 1 1 d . . . H10A H 0.1024 0.8125 0.2032 0.105 Uiso 1 1 calc R . . H10B H 0.0813 0.7716 0.1582 0.105 Uiso 1 1 calc R . . H10C H 0.1064 0.7834 0.2890 0.105 Uiso 1 1 calc R . . C11 C 0.06689(19) 0.77009(17) 0.8010(6) 0.0395(14) Uani 1 1 d . . . C12 C 0.0861(2) 0.7515(2) 0.8147(8) 0.0550(19) Uani 1 1 d . . . H12 H 0.1081 0.7597 0.7693 0.066 Uiso 1 1 calc R . . C13 C 0.0715(3) 0.7202(2) 0.8981(10) 0.075(3) Uani 1 1 d . . . H13 H 0.0842 0.7077 0.9074 0.090 Uiso 1 1 calc R . . C14 C 0.0397(3) 0.7080(2) 0.9647(10) 0.080(3) Uani 1 1 d . . . H14 H 0.0305 0.6870 1.0177 0.097 Uiso 1 1 calc R . . C15 C 0.0209(2) 0.7262(2) 0.9551(8) 0.066(2) Uani 1 1 d . . . H15 H -0.0006 0.7183 1.0044 0.079 Uiso 1 1 calc R . . C16 C 0.0340(2) 0.7568(2) 0.8711(7) 0.0499(17) Uani 1 1 d . . . H16 H 0.0206 0.7685 0.8615 0.060 Uiso 1 1 calc R . . C17 C 0.13263(18) 0.8268(2) 0.6798(8) 0.0497(17) Uani 1 1 d . . . H17A H 0.1416 0.8261 0.7712 0.060 Uiso 1 1 calc R . . H17B H 0.1357 0.8098 0.6227 0.060 Uiso 1 1 calc R . . C18 C 0.15633(19) 0.8650(2) 0.6205(8) 0.057(2) Uani 1 1 d . . . H18A H 0.1528 0.8820 0.6758 0.069 Uiso 1 1 calc R . . H18B H 0.1816 0.8716 0.6293 0.069 Uiso 1 1 calc R . . C19 C 0.14880(18) 0.8694(2) 0.4694(7) 0.0547(19) Uani 1 1 d . . . H19A H 0.1533 0.8532 0.4132 0.066 Uiso 1 1 calc R . . H19B H 0.1657 0.8941 0.4403 0.066 Uiso 1 1 calc R . . C20 C 0.1014(2) 0.89978(19) 0.5090(9) 0.060(2) Uani 1 1 d . . . H20A H 0.1150 0.9074 0.5946 0.072 Uiso 1 1 calc R . . H20B H 0.1124 0.9199 0.4443 0.072 Uiso 1 1 calc R . . C21 C 0.0616(2) 0.8890(2) 0.5353(9) 0.062(2) Uani 1 1 d . . . H21A H 0.0501 0.8896 0.4496 0.074 Uiso 1 1 calc R . . H21B H 0.0604 0.9059 0.5995 0.074 Uiso 1 1 calc R . . C22 C 0.08256(19) 0.84367(18) 0.8147(7) 0.0436(15) Uani 1 1 d . . . H22A H 0.0831 0.8359 0.9085 0.052 Uiso 1 1 calc R . . H22B H 0.1041 0.8673 0.8010 0.052 Uiso 1 1 calc R . . C23 C 0.0491(2) 0.8470(2) 0.7951(8) 0.058(2) Uani 1 1 d . . . H23 H 0.0290 0.8256 0.8390 0.069 Uiso 1 1 calc R . . C24 C 0.0514(3) 0.8799(3) 0.8643(10) 0.076(3) Uani 1 1 d . . . H24A H 0.0288 0.8796 0.8521 0.114 Uiso 1 1 calc R . . H24B H 0.0708 0.9016 0.8237 0.114 Uiso 1 1 calc R . . H24C H 0.0560 0.8795 0.9610 0.114 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 Fe1 0.0236(4) 0.0301(5) 0.0250(4) -0.0021(3) -0.0017(3) 0.0101(3) P1 0.0386(9) 0.0344(8) 0.0303(8) -0.0028(6) -0.0075(6) 0.0155(7) P2 0.0359(9) 0.0479(11) 0.0392(9) 0.0041(8) 0.0018(7) 0.0079(8) P3 0.0411(10) 0.0466(10) 0.0487(10) -0.0054(8) -0.0043(8) 0.0249(8) P4 0.0485(11) 0.0490(11) 0.0522(11) 0.0019(9) 0.0014(9) 0.0128(9) F1 0.063(4) 0.114(5) 0.158(6) -0.011(5) 0.013(4) 0.005(4) F2 0.057(3) 0.100(4) 0.076(3) 0.016(3) 0.007(3) -0.006(3) F3 0.126(11) 0.094(12) 0.130(13) 0.043(9) 0.020(8) 0.064(9) F3' 0.138(18) 0.15(2) 0.142(18) 0.015(13) 0.000(12) 0.057(13) F4 0.113(8) 0.111(9) 0.091(8) -0.047(6) -0.009(6) 0.060(7) F4' 0.117(17) 0.056(13) 0.104(16) -0.012(10) 0.006(11) 0.027(10) F5 0.160(8) 0.139(7) 0.106(7) 0.036(5) 0.024(5) 0.115(7) F5' 0.065(15) 0.066(16) 0.027(12) 0.027(10) -0.014(9) 0.005(11) F6 0.078(5) 0.113(7) 0.046(4) -0.022(4) 0.014(3) 0.011(4) F6' 0.14(2) 0.12(2) 0.17(3) 0.004(13) -0.022(14) 0.078(16) C1 0.059(4) 0.038(3) 0.048(4) -0.023(3) -0.025(3) 0.029(3) C2 0.038(3) 0.034(3) 0.033(3) -0.007(3) -0.006(3) 0.004(3) C3 0.030(3) 0.046(4) 0.035(3) -0.011(3) -0.007(2) 0.014(3) C4 0.033(3) 0.057(4) 0.029(3) -0.014(3) -0.009(2) 0.019(3) C5 0.034(3) 0.057(4) 0.038(3) -0.019(3) -0.004(3) 0.019(3) C6 0.112(8) 0.061(5) 0.090(7) -0.040(5) -0.052(6) 0.062(6) C7 0.059(5) 0.044(4) 0.046(4) -0.004(3) 0.000(3) -0.006(4) C8 0.043(4) 0.103(7) 0.065(5) -0.025(5) -0.010(4) 0.042(5) C9 0.074(6) 0.076(6) 0.036(4) 0.001(4) -0.011(4) 0.029(5) C10 0.042(4) 0.102(7) 0.065(5) -0.037(5) -0.001(4) 0.035(5) C11 0.051(4) 0.032(3) 0.033(3) -0.002(2) -0.011(3) 0.019(3) C12 0.062(5) 0.058(5) 0.052(4) -0.006(4) -0.019(4) 0.036(4) C13 0.109(8) 0.052(5) 0.075(6) -0.011(4) -0.043(6) 0.049(6) C14 0.097(8) 0.044(5) 0.076(6) 0.013(4) -0.036(6) 0.017(5) C15 0.065(5) 0.048(4) 0.056(5) 0.016(4) -0.010(4) 0.007(4) C16 0.059(4) 0.048(4) 0.039(3) 0.002(3) -0.014(3) 0.024(4) C17 0.034(3) 0.062(5) 0.055(4) -0.005(3) -0.010(3) 0.025(3) C18 0.032(4) 0.077(5) 0.052(4) -0.006(4) -0.003(3) 0.019(4) C19 0.032(3) 0.066(5) 0.048(4) -0.006(4) 0.004(3) 0.011(3) C20 0.060(5) 0.031(4) 0.076(5) 0.012(4) 0.001(4) 0.013(3) C21 0.061(5) 0.050(4) 0.077(6) 0.003(4) -0.002(4) 0.030(4) C22 0.048(4) 0.038(3) 0.038(3) -0.005(3) -0.007(3) 0.017(3) C23 0.064(5) 0.075(5) 0.042(4) -0.012(4) -0.003(3) 0.040(4) C24 0.101(7) 0.081(6) 0.070(6) -0.020(5) -0.004(5) 0.063(6) _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 Fe1 C2 2.102(6) . ? Fe1 C5 2.103(6) . ? Fe1 C1 2.109(6) . ? Fe1 C4 2.113(6) . ? Fe1 C3 2.116(6) . ? Fe1 P2 2.1498(19) . ? Fe1 P3 2.169(2) . ? Fe1 P1 2.1949(17) . ? P1 C11 1.833(6) . ? P1 C22 1.842(7) . ? P1 C17 1.854(7) . ? P2 C19 1.820(7) . ? P2 C20 1.854(8) . ? P3 C21 1.817(8) . ? P3 C23 1.866(8) . ? P4 F6' 1.541(8) . ? P4 F5' 1.546(8) . ? P4 F5 1.546(6) . ? P4 F3' 1.552(8) . ? P4 F3 1.553(7) . ? P4 F6 1.558(5) . ? P4 F1 1.561(5) . ? P4 F2 1.564(4) . ? P4 F4 1.569(6) . ? P4 F4' 1.63(3) . ? C1 C5 1.409(10) . ? C1 C2 1.436(10) . ? C1 C6 1.505(10) . ? C2 C3 1.419(9) . ? C2 C7 1.493(9) . ? C3 C4 1.415(9) . ? C3 C8 1.498(10) . ? C4 C5 1.427(9) . ? C4 C9 1.496(10) . ? C5 C10 1.512(10) . ? C11 C16 1.392(10) . ? C11 C12 1.394(10) . ? C12 C13 1.407(12) . ? C13 C14 1.344(15) . ? C14 C15 1.366(14) . ? C15 C16 1.391(10) . ? C17 C18 1.532(11) . ? C18 C19 1.530(10) . ? C20 C21 1.535(12) . ? C22 C23 1.506(10) . ? C23 C24 1.511(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 C2 Fe1 C5 66.5(3) . . ? C2 Fe1 C1 39.9(3) . . ? C5 Fe1 C1 39.1(3) . . ? C2 Fe1 C4 65.9(3) . . ? C5 Fe1 C4 39.6(3) . . ? C1 Fe1 C4 65.7(3) . . ? C2 Fe1 C3 39.3(3) . . ? C5 Fe1 C3 66.2(2) . . ? C1 Fe1 C3 66.1(3) . . ? C4 Fe1 C3 39.1(2) . . ? C2 Fe1 P2 158.05(18) . . ? C5 Fe1 P2 93.1(2) . . ? C1 Fe1 P2 126.2(2) . . ? C4 Fe1 P2 93.4(2) . . ? C3 Fe1 P2 126.34(19) . . ? C2 Fe1 P3 108.2(2) . . ? C5 Fe1 P3 152.3(2) . . ? C1 Fe1 P3 147.5(2) . . ? C4 Fe1 P3 112.74(19) . . ? C3 Fe1 P3 92.12(18) . . ? P2 Fe1 P3 85.97(8) . . ? C2 Fe1 P1 107.16(19) . . ? C5 Fe1 P1 121.7(2) . . ? C1 Fe1 P1 97.39(19) . . ? C4 Fe1 P1 161.1(2) . . ? C3 Fe1 P1 143.36(19) . . ? P2 Fe1 P1 90.07(7) . . ? P3 Fe1 P1 86.00(7) . . ? C11 P1 C22 101.9(3) . . ? C11 P1 C17 102.3(3) . . ? C22 P1 C17 102.2(3) . . ? C11 P1 Fe1 121.3(2) . . ? C22 P1 Fe1 110.5(2) . . ? C17 P1 Fe1 116.1(2) . . ? C19 P2 C20 104.7(4) . . ? C19 P2 Fe1 122.1(3) . . ? C20 P2 Fe1 111.5(3) . . ? C21 P3 C23 107.9(4) . . ? C21 P3 Fe1 110.0(3) . . ? C23 P3 Fe1 112.0(3) . . ? F6' P4 F5' 115(3) . . ? F6' P4 F5 49.0(18) . . ? F5' P4 F5 70.1(17) . . ? F6' P4 F3' 85(3) . . ? F5' P4 F3' 151(2) . . ? F5 P4 F3' 134.3(19) . . ? F6' P4 F3 134(2) . . ? F5' P4 F3 107.4(18) . . ? F5 P4 F3 177.1(10) . . ? F3' P4 F3 48.5(16) . . ? F6' P4 F6 48(2) . . ? F5' P4 F6 161.4(17) . . ? F5 P4 F6 91.2(6) . . ? F3' P4 F6 46.0(17) . . ? F3 P4 F6 91.3(9) . . ? F6' P4 F1 104.3(18) . . ? F5' P4 F1 93.0(16) . . ? F5 P4 F1 88.2(5) . . ? F3' P4 F1 101.8(12) . . ? F3 P4 F1 90.4(8) . . ? F6 P4 F1 86.7(4) . . ? F6' P4 F2 77.0(17) . . ? F5' P4 F2 86.9(16) . . ? F5 P4 F2 93.1(5) . . ? F3' P4 F2 77.7(11) . . ? F3 P4 F2 88.2(7) . . ? F6 P4 F2 93.8(4) . . ? F1 P4 F2 178.6(5) . . ? F6' P4 F4 133(2) . . ? F5' P4 F4 19.0(17) . . ? F5 P4 F4 89.0(6) . . ? F3' P4 F4 134.2(19) . . ? F3 P4 F4 88.5(9) . . ? F6 P4 F4 178.6(7) . . ? F1 P4 F4 91.9(6) . . ? F2 P4 F4 87.6(6) . . ? F6' P4 F4' 156(2) . . ? F5' P4 F4' 88.1(19) . . ? F5 P4 F4' 154.1(13) . . ? F3' P4 F4' 71(2) . . ? F3 P4 F4' 22.9(13) . . ? F6 P4 F4' 110.0(13) . . ? F1 P4 F4' 78.9(14) . . ? F2 P4 F4' 99.7(14) . . ? F4 P4 F4' 69.4(13) . . ? C5 C1 C2 108.2(6) . . ? C5 C1 C6 125.9(8) . . ? C2 C1 C6 125.6(8) . . ? C5 C1 Fe1 70.2(4) . . ? C2 C1 Fe1 69.8(3) . . ? C6 C1 Fe1 131.2(5) . . ? C3 C2 C1 107.6(6) . . ? C3 C2 C7 124.5(7) . . ? C1 C2 C7 127.4(7) . . ? C3 C2 Fe1 70.8(3) . . ? C1 C2 Fe1 70.3(4) . . ? C7 C2 Fe1 130.7(4) . . ? C4 C3 C2 108.0(6) . . ? C4 C3 C8 125.8(7) . . ? C2 C3 C8 125.7(7) . . ? C4 C3 Fe1 70.3(3) . . ? C2 C3 Fe1 69.8(3) . . ? C8 C3 Fe1 131.1(5) . . ? C3 C4 C5 108.4(6) . . ? C3 C4 C9 124.3(6) . . ? C5 C4 C9 127.0(6) . . ? C3 C4 Fe1 70.6(3) . . ? C5 C4 Fe1 69.8(3) . . ? C9 C4 Fe1 130.0(5) . . ? C1 C5 C4 107.8(6) . . ? C1 C5 C10 127.1(7) . . ? C4 C5 C10 124.6(7) . . ? C1 C5 Fe1 70.7(4) . . ? C4 C5 Fe1 70.6(3) . . ? C10 C5 Fe1 130.6(5) . . ? C16 C11 C12 118.3(6) . . ? C16 C11 P1 119.5(5) . . ? C12 C11 P1 122.1(6) . . ? C11 C12 C13 119.0(8) . . ? C14 C13 C12 121.4(9) . . ? C13 C14 C15 120.6(8) . . ? C14 C15 C16 119.5(9) . . ? C15 C16 C11 121.2(8) . . ? C18 C17 P1 116.0(5) . . ? C19 C18 C17 114.9(6) . . ? C18 C19 P2 113.8(5) . . ? C21 C20 P2 108.7(5) . . ? C20 C21 P3 107.7(5) . . ? C23 C22 P1 111.4(5) . . ? C22 C23 C24 113.8(7) . . ? C22 C23 P3 108.3(5) . . ? C24 C23 P3 114.2(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.404 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.110 #===END data_compound_14 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H36 F6 Fe P4' _chemical_formula_weight 630.27 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' '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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.0310(2) _cell_length_b 15.2330(3) _cell_length_c 19.7330(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2714.65(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 27972 _diffrn_reflns_av_R_equivalents 0.0826 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6202 _reflns_number_gt 5061 _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^)+(0.0428P)^2^+0.3324P] 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 0.0035(6) _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 -0.011(17) _refine_ls_number_reflns 6202 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 Fe1 Fe 0.20611(5) -0.01087(3) 0.12409(2) 0.01968(12) Uani 1 1 d . . . F1 F 0.4000(4) 0.26643(17) 0.31317(17) 0.0696(9) Uani 1 1 d . . . F2 F 0.6179(4) 0.2000(2) 0.30356(16) 0.0733(9) Uani 1 1 d . . . F3 F 0.5309(4) 0.08223(17) 0.35879(16) 0.0727(10) Uani 1 1 d . . . F4 F 0.3121(4) 0.1477(3) 0.37024(19) 0.0931(12) Uani 1 1 d . . . F5 F 0.4074(4) 0.13191(16) 0.26732(14) 0.0651(9) Uani 1 1 d . . . F6 F 0.5209(3) 0.21489(16) 0.40575(12) 0.0508(7) Uani 1 1 d . . . P1 P 0.03044(10) 0.08831(5) 0.13052(4) 0.02314(19) Uani 1 1 d . . . P2 P 0.18308(10) -0.05833(5) 0.22900(4) 0.02166(19) Uani 1 1 d . . . P3 P 0.05346(10) -0.11750(6) 0.09723(4) 0.02202(19) Uani 1 1 d . . . P4 P 0.46373(12) 0.17398(6) 0.33633(5) 0.0316(2) Uani 1 1 d . . . C1 C 0.3793(4) 0.0798(2) 0.10827(18) 0.0270(8) Uani 1 1 d . . . H1 H 0.3870 0.1357 0.1293 0.032 Uiso 1 1 calc R . . C2 C 0.4382(4) 0.0005(2) 0.13275(18) 0.0278(7) Uani 1 1 d . . . H2 H 0.4938 -0.0062 0.1733 0.033 Uiso 1 1 calc R . . C3 C 0.4010(4) -0.0678(2) 0.0870(2) 0.0290(8) Uani 1 1 d . . . H3 H 0.4255 -0.1281 0.0919 0.035 Uiso 1 1 calc R . . C4 C 0.3206(4) -0.0296(2) 0.03258(17) 0.0278(8) Uani 1 1 d . . . H4 H 0.2835 -0.0597 -0.0060 0.033 Uiso 1 1 calc R . . C5 C 0.3057(4) 0.0607(2) 0.04593(17) 0.0272(7) Uani 1 1 d . . . H5 H 0.2552 0.1020 0.0182 0.033 Uiso 1 1 calc R . . C6 C -0.0745(5) 0.1061(2) 0.21026(19) 0.0329(9) Uani 1 1 d . . . H6A H -0.0294 0.1567 0.2341 0.040 Uiso 1 1 calc R . . H6B H -0.1767 0.1233 0.1979 0.040 Uiso 1 1 calc R . . C7 C -0.0845(4) 0.0302(2) 0.26043(18) 0.0293(8) Uani 1 1 d . . . H7A H -0.1304 -0.0209 0.2376 0.035 Uiso 1 1 calc R . . H7B H -0.1495 0.0475 0.2986 0.035 Uiso 1 1 calc R . . C8 C 0.0663(4) 0.0032(2) 0.28839(17) 0.0288(7) Uani 1 1 d . . . H8A H 0.0507 -0.0331 0.3294 0.035 Uiso 1 1 calc R . . H8B H 0.1202 0.0568 0.3025 0.035 Uiso 1 1 calc R . . C9 C 0.0931(4) -0.1670(2) 0.22840(18) 0.0255(7) Uani 1 1 d . . . H9A H 0.1683 -0.2131 0.2203 0.031 Uiso 1 1 calc R . . H9B H 0.0467 -0.1783 0.2730 0.031 Uiso 1 1 calc R . . C10 C -0.0241(4) -0.1705(2) 0.17319(17) 0.0263(7) Uani 1 1 d . . . H10A H -0.1145 -0.1392 0.1881 0.032 Uiso 1 1 calc R . . H10B H -0.0505 -0.2322 0.1631 0.032 Uiso 1 1 calc R . . C11 C -0.1094(4) -0.0920(2) 0.04542(19) 0.0298(8) Uani 1 1 d . . . H11A H -0.0766 -0.0793 -0.0014 0.036 Uiso 1 1 calc R . . H11B H -0.1743 -0.1443 0.0438 0.036 Uiso 1 1 calc R . . C12 C -0.1998(4) -0.0138(2) 0.07154(19) 0.0315(8) Uani 1 1 d . . . H12A H -0.2277 -0.0249 0.1193 0.038 Uiso 1 1 calc R . . H12B H -0.2924 -0.0095 0.0448 0.038 Uiso 1 1 calc R . . C13 C -0.1173(4) 0.0752(2) 0.06753(19) 0.0301(8) Uani 1 1 d . . . H13A H -0.1901 0.1232 0.0736 0.036 Uiso 1 1 calc R . . H13B H -0.0739 0.0814 0.0217 0.036 Uiso 1 1 calc R . . C14 C 0.0890(4) 0.2029(2) 0.11530(18) 0.0248(7) Uani 1 1 d . . . C15 C 0.1837(4) 0.2419(2) 0.16307(18) 0.0292(8) Uani 1 1 d . . . H15 H 0.2116 0.2103 0.2026 0.035 Uiso 1 1 calc R . . C16 C 0.2370(4) 0.3268(2) 0.1528(2) 0.0338(9) Uani 1 1 d . . . H16 H 0.3020 0.3521 0.1852 0.041 Uiso 1 1 calc R . . C17 C 0.1973(5) 0.3739(2) 0.0971(2) 0.0359(9) Uani 1 1 d . . . H17 H 0.2343 0.4317 0.0906 0.043 Uiso 1 1 calc R . . C18 C 0.1025(5) 0.3370(2) 0.0499(2) 0.0358(9) Uani 1 1 d . . . H18 H 0.0736 0.3699 0.0113 0.043 Uiso 1 1 calc R . . C19 C 0.0488(4) 0.2514(2) 0.05870(18) 0.0298(8) Uani 1 1 d . . . H19 H -0.0154 0.2265 0.0258 0.036 Uiso 1 1 calc R . . C20 C 0.3506(4) -0.0812(2) 0.27939(17) 0.0275(8) Uani 1 1 d . . . H20A H 0.4139 -0.1225 0.2536 0.033 Uiso 1 1 calc R . . H20B H 0.4067 -0.0259 0.2848 0.033 Uiso 1 1 calc R . . C21 C 0.3229(5) -0.1193(3) 0.3483(2) 0.0379(9) Uani 1 1 d . . . H21 H 0.2841 -0.0812 0.3820 0.045 Uiso 1 1 calc R . . C22 C 0.3482(5) -0.2009(3) 0.3654(2) 0.0455(11) Uani 1 1 d . . . H22A H 0.3869 -0.2410 0.3331 0.055 Uiso 1 1 calc R . . H22B H 0.3277 -0.2201 0.4103 0.055 Uiso 1 1 calc R . . C23 C 0.1366(4) -0.2110(2) 0.05127(18) 0.0249(7) Uani 1 1 d . . . H23A H 0.1556 -0.1925 0.0040 0.030 Uiso 1 1 calc R . . H23B H 0.2336 -0.2244 0.0722 0.030 Uiso 1 1 calc R . . C24 C 0.0468(4) -0.2938(2) 0.04973(17) 0.0259(7) Uani 1 1 d . . . H24 H -0.0495 -0.2911 0.0304 0.031 Uiso 1 1 calc R . . C25 C 0.0925(5) -0.3694(2) 0.07327(18) 0.0319(8) Uani 1 1 d . . . H25A H 0.1882 -0.3742 0.0929 0.038 Uiso 1 1 calc R . . H25B H 0.0300 -0.4194 0.0707 0.038 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 Fe1 0.0169(2) 0.0216(2) 0.0205(2) -0.00019(18) 0.0021(2) 0.00033(19) F1 0.074(2) 0.0421(15) 0.092(2) -0.0089(14) -0.0327(18) 0.0125(15) F2 0.055(2) 0.104(2) 0.061(2) 0.0103(17) 0.0163(15) -0.0163(18) F3 0.102(3) 0.0399(13) 0.076(2) 0.0042(13) -0.0500(19) 0.0015(15) F4 0.057(2) 0.135(3) 0.088(2) -0.011(2) 0.018(2) -0.052(2) F5 0.107(3) 0.0472(14) 0.0410(14) -0.0053(12) -0.0366(16) -0.0015(15) F6 0.0646(18) 0.0515(14) 0.0361(13) -0.0080(10) -0.0076(13) -0.0166(13) P1 0.0203(4) 0.0247(4) 0.0243(4) 0.0005(3) 0.0017(4) 0.0030(3) P2 0.0222(5) 0.0217(4) 0.0211(4) -0.0009(3) 0.0016(4) -0.0017(4) P3 0.0186(4) 0.0249(4) 0.0227(4) -0.0025(3) 0.0002(4) -0.0007(3) P4 0.0336(6) 0.0321(5) 0.0292(5) -0.0012(4) -0.0053(4) -0.0075(4) C1 0.0223(18) 0.0215(16) 0.037(2) -0.0023(14) 0.0096(15) -0.0048(14) C2 0.0184(15) 0.0363(19) 0.0287(18) 0.0037(15) 0.0040(14) 0.0004(15) C3 0.0226(19) 0.0244(17) 0.040(2) -0.0016(15) 0.0098(16) 0.0016(14) C4 0.0231(19) 0.0370(19) 0.0233(17) -0.0062(13) 0.0082(14) -0.0029(15) C5 0.0231(18) 0.0279(16) 0.0307(18) 0.0056(13) 0.0077(16) 0.0012(16) C6 0.032(2) 0.0314(19) 0.035(2) 0.0013(15) 0.0139(16) 0.0069(16) C7 0.028(2) 0.0334(19) 0.0264(18) -0.0011(14) 0.0083(15) 0.0019(15) C8 0.0321(19) 0.0278(18) 0.0264(17) -0.0031(14) 0.0048(14) -0.0029(16) C9 0.0282(19) 0.0241(17) 0.0242(17) 0.0012(14) 0.0028(15) -0.0040(15) C10 0.0231(18) 0.0260(17) 0.0297(18) -0.0006(13) 0.0030(15) -0.0057(15) C11 0.0232(19) 0.0358(19) 0.0304(19) -0.0003(15) -0.0077(15) 0.0013(16) C12 0.0219(18) 0.0361(18) 0.037(2) -0.0035(15) -0.0039(16) 0.0005(18) C13 0.0220(19) 0.0346(19) 0.034(2) -0.0029(15) -0.0040(15) 0.0061(16) C14 0.0235(18) 0.0239(16) 0.0269(18) 0.0010(13) 0.0034(14) 0.0055(13) C15 0.030(2) 0.0272(17) 0.0304(19) -0.0013(14) 0.0033(16) 0.0064(16) C16 0.029(2) 0.0319(18) 0.041(2) -0.0085(17) 0.0055(16) 0.0041(16) C17 0.031(2) 0.0273(17) 0.049(2) 0.0030(16) 0.006(2) -0.0012(17) C18 0.033(2) 0.033(2) 0.042(2) 0.0115(16) 0.0044(18) 0.0044(17) C19 0.029(2) 0.0299(18) 0.0308(19) 0.0029(15) 0.0047(16) 0.0029(16) C20 0.030(2) 0.0281(17) 0.0246(18) -0.0009(14) -0.0054(15) -0.0018(15) C21 0.036(2) 0.049(2) 0.0281(19) 0.0038(17) -0.0047(17) 0.0018(19) C22 0.048(3) 0.053(3) 0.036(2) 0.0143(19) -0.008(2) -0.006(2) C23 0.0265(19) 0.0241(16) 0.0241(17) -0.0038(13) 0.0017(15) 0.0010(14) C24 0.0244(19) 0.0292(17) 0.0241(17) -0.0032(13) -0.0016(15) -0.0049(15) C25 0.035(2) 0.0323(19) 0.0281(19) -0.0018(15) -0.0017(16) -0.0049(16) _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 Fe1 C5 2.092(3) . ? Fe1 C3 2.094(4) . ? Fe1 C4 2.100(3) . ? Fe1 C1 2.109(3) . ? Fe1 C2 2.110(3) . ? Fe1 P1 2.1943(9) . ? Fe1 P3 2.1954(10) . ? Fe1 P2 2.2026(9) . ? F1 P4 1.589(3) . ? F2 P4 1.585(3) . ? F3 P4 1.587(3) . ? F4 P4 1.576(3) . ? F5 P4 1.589(3) . ? F6 P4 1.591(2) . ? P1 C13 1.835(4) . ? P1 C14 1.849(3) . ? P1 C6 1.857(4) . ? P2 C8 1.834(3) . ? P2 C9 1.844(3) . ? P2 C20 1.844(4) . ? P3 C11 1.833(4) . ? P3 C10 1.840(3) . ? P3 C23 1.848(3) . ? C1 C2 1.405(5) . ? C1 C5 1.428(5) . ? C2 C3 1.418(5) . ? C3 C4 1.422(5) . ? C4 C5 1.407(5) . ? C6 C7 1.526(5) . ? C7 C8 1.526(5) . ? C9 C10 1.520(5) . ? C11 C12 1.534(5) . ? C12 C13 1.548(5) . ? C14 C19 1.388(5) . ? C14 C15 1.404(5) . ? C15 C16 1.395(5) . ? C16 C17 1.361(6) . ? C17 C18 1.384(6) . ? C18 C19 1.401(5) . ? C20 C21 1.498(5) . ? C21 C22 1.309(5) . ? C23 C24 1.499(5) . ? C24 C25 1.309(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 C5 Fe1 C3 66.24(14) . . ? C5 Fe1 C4 39.23(13) . . ? C3 Fe1 C4 39.62(14) . . ? C5 Fe1 C1 39.74(14) . . ? C3 Fe1 C1 66.18(14) . . ? C4 Fe1 C1 66.21(14) . . ? C5 Fe1 C2 65.79(14) . . ? C3 Fe1 C2 39.41(14) . . ? C4 Fe1 C2 65.91(14) . . ? C1 Fe1 C2 38.89(13) . . ? C5 Fe1 P1 89.67(10) . . ? C3 Fe1 P1 155.91(11) . . ? C4 Fe1 P1 119.94(10) . . ? C1 Fe1 P1 95.39(10) . . ? C2 Fe1 P1 131.05(10) . . ? C5 Fe1 P3 118.53(10) . . ? C3 Fe1 P3 97.89(10) . . ? C4 Fe1 P3 90.06(10) . . ? C1 Fe1 P3 156.08(10) . . ? C2 Fe1 P3 134.77(10) . . ? P1 Fe1 P3 93.98(4) . . ? C5 Fe1 P2 154.77(11) . . ? C3 Fe1 P2 105.77(11) . . ? C4 Fe1 P2 144.10(10) . . ? C1 Fe1 P2 115.08(10) . . ? C2 Fe1 P2 92.57(10) . . ? P1 Fe1 P2 95.93(4) . . ? P3 Fe1 P2 85.68(3) . . ? C13 P1 C14 101.59(17) . . ? C13 P1 C6 102.63(19) . . ? C14 P1 C6 98.38(16) . . ? C13 P1 Fe1 114.31(12) . . ? C14 P1 Fe1 115.71(11) . . ? C6 P1 Fe1 121.25(13) . . ? C8 P2 C9 102.10(16) . . ? C8 P2 C20 102.93(17) . . ? C9 P2 C20 101.25(16) . . ? C8 P2 Fe1 119.15(12) . . ? C9 P2 Fe1 109.28(12) . . ? C20 P2 Fe1 119.44(12) . . ? C11 P3 C10 104.01(17) . . ? C11 P3 C23 102.46(17) . . ? C10 P3 C23 102.50(16) . . ? C11 P3 Fe1 118.79(12) . . ? C10 P3 Fe1 111.50(12) . . ? C23 P3 Fe1 115.69(12) . . ? F4 P4 F2 178.9(2) . . ? F4 P4 F3 89.4(2) . . ? F2 P4 F3 89.9(2) . . ? F4 P4 F1 91.9(2) . . ? F2 P4 F1 88.82(19) . . ? F3 P4 F1 178.7(2) . . ? F4 P4 F5 89.05(19) . . ? F2 P4 F5 91.84(19) . . ? F3 P4 F5 90.37(14) . . ? F1 P4 F5 89.71(15) . . ? F4 P4 F6 90.91(17) . . ? F2 P4 F6 88.19(16) . . ? F3 P4 F6 88.88(15) . . ? F1 P4 F6 91.03(15) . . ? F5 P4 F6 179.26(16) . . ? C2 C1 C5 107.3(3) . . ? C2 C1 Fe1 70.58(19) . . ? C5 C1 Fe1 69.48(19) . . ? C1 C2 C3 108.8(3) . . ? C1 C2 Fe1 70.5(2) . . ? C3 C2 Fe1 69.7(2) . . ? C2 C3 C4 107.5(3) . . ? C2 C3 Fe1 70.89(19) . . ? C4 C3 Fe1 70.4(2) . . ? C5 C4 C3 107.9(3) . . ? C5 C4 Fe1 70.07(19) . . ? C3 C4 Fe1 70.0(2) . . ? C4 C5 C1 108.4(3) . . ? C4 C5 Fe1 70.70(19) . . ? C1 C5 Fe1 70.78(19) . . ? C7 C6 P1 118.0(2) . . ? C6 C7 C8 112.7(3) . . ? C7 C8 P2 114.8(2) . . ? C10 C9 P2 110.0(2) . . ? C9 C10 P3 107.7(2) . . ? C12 C11 P3 113.9(2) . . ? C11 C12 C13 114.0(3) . . ? C12 C13 P1 114.3(2) . . ? C19 C14 C15 118.3(3) . . ? C19 C14 P1 124.0(3) . . ? C15 C14 P1 117.7(3) . . ? C16 C15 C14 120.3(3) . . ? C17 C16 C15 121.1(4) . . ? C16 C17 C18 119.4(3) . . ? C17 C18 C19 120.6(4) . . ? C14 C19 C18 120.3(4) . . ? C21 C20 P2 115.2(3) . . ? C22 C21 C20 125.0(4) . . ? C24 C23 P3 116.0(3) . . ? C25 C24 C23 124.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 Fe1 P1 C13 81.94(17) . . . . ? C3 Fe1 P1 C13 82.9(3) . . . . ? C4 Fe1 P1 C13 55.73(19) . . . . ? C1 Fe1 P1 C13 121.33(17) . . . . ? C2 Fe1 P1 C13 138.66(19) . . . . ? P3 Fe1 P1 C13 -36.64(14) . . . . ? P2 Fe1 P1 C13 -122.70(14) . . . . ? C5 Fe1 P1 C14 -35.59(17) . . . . ? C3 Fe1 P1 C14 -34.7(3) . . . . ? C4 Fe1 P1 C14 -61.80(17) . . . . ? C1 Fe1 P1 C14 3.79(16) . . . . ? C2 Fe1 P1 C14 21.13(19) . . . . ? P3 Fe1 P1 C14 -154.17(13) . . . . ? P2 Fe1 P1 C14 119.76(13) . . . . ? C5 Fe1 P1 C6 -154.37(19) . . . . ? C3 Fe1 P1 C6 -153.4(3) . . . . ? C4 Fe1 P1 C6 179.42(19) . . . . ? C1 Fe1 P1 C6 -114.98(19) . . . . ? C2 Fe1 P1 C6 -97.6(2) . . . . ? P3 Fe1 P1 C6 87.06(16) . . . . ? P2 Fe1 P1 C6 0.99(16) . . . . ? C5 Fe1 P2 C8 91.7(3) . . . . ? C3 Fe1 P2 C8 159.19(17) . . . . ? C4 Fe1 P2 C8 172.1(2) . . . . ? C1 Fe1 P2 C8 88.53(17) . . . . ? C2 Fe1 P2 C8 121.46(16) . . . . ? P1 Fe1 P2 C8 -10.26(14) . . . . ? P3 Fe1 P2 C8 -103.82(14) . . . . ? C5 Fe1 P2 C9 -151.6(3) . . . . ? C3 Fe1 P2 C9 -84.10(16) . . . . ? C4 Fe1 P2 C9 -71.2(2) . . . . ? C1 Fe1 P2 C9 -154.76(16) . . . . ? C2 Fe1 P2 C9 -121.83(16) . . . . ? P1 Fe1 P2 C9 106.45(13) . . . . ? P3 Fe1 P2 C9 12.89(13) . . . . ? C5 Fe1 P2 C20 -35.8(3) . . . . ? C3 Fe1 P2 C20 31.67(17) . . . . ? C4 Fe1 P2 C20 44.5(2) . . . . ? C1 Fe1 P2 C20 -38.99(18) . . . . ? C2 Fe1 P2 C20 -6.06(16) . . . . ? P1 Fe1 P2 C20 -137.79(13) . . . . ? P3 Fe1 P2 C20 128.65(13) . . . . ? C5 Fe1 P3 C11 -58.09(19) . . . . ? C3 Fe1 P3 C11 -125.28(18) . . . . ? C4 Fe1 P3 C11 -86.32(18) . . . . ? C1 Fe1 P3 C11 -79.2(3) . . . . ? C2 Fe1 P3 C11 -141.30(19) . . . . ? P1 Fe1 P3 C11 33.71(15) . . . . ? P2 Fe1 P3 C11 129.37(15) . . . . ? C5 Fe1 P3 C10 -178.97(17) . . . . ? C3 Fe1 P3 C10 113.83(17) . . . . ? C4 Fe1 P3 C10 152.80(16) . . . . ? C1 Fe1 P3 C10 159.9(3) . . . . ? C2 Fe1 P3 C10 97.82(19) . . . . ? P1 Fe1 P3 C10 -87.18(13) . . . . ? P2 Fe1 P3 C10 8.49(13) . . . . ? C5 Fe1 P3 C23 64.43(17) . . . . ? C3 Fe1 P3 C23 -2.76(17) . . . . ? C4 Fe1 P3 C23 36.20(16) . . . . ? C1 Fe1 P3 C23 43.3(3) . . . . ? C2 Fe1 P3 C23 -18.8(2) . . . . ? P1 Fe1 P3 C23 156.23(13) . . . . ? P2 Fe1 P3 C23 -108.11(13) . . . . ? C5 Fe1 C1 C2 -118.0(3) . . . . ? C3 Fe1 C1 C2 -37.1(2) . . . . ? C4 Fe1 C1 C2 -80.6(2) . . . . ? P1 Fe1 C1 C2 159.03(19) . . . . ? P3 Fe1 C1 C2 -88.4(3) . . . . ? P2 Fe1 C1 C2 59.9(2) . . . . ? C3 Fe1 C1 C5 80.9(2) . . . . ? C4 Fe1 C1 C5 37.4(2) . . . . ? C2 Fe1 C1 C5 118.0(3) . . . . ? P1 Fe1 C1 C5 -82.97(19) . . . . ? P3 Fe1 C1 C5 29.6(4) . . . . ? P2 Fe1 C1 C5 177.89(17) . . . . ? C5 C1 C2 C3 -0.6(4) . . . . ? Fe1 C1 C2 C3 59.4(2) . . . . ? C5 C1 C2 Fe1 -60.0(2) . . . . ? C5 Fe1 C2 C1 38.2(2) . . . . ? C3 Fe1 C2 C1 119.7(3) . . . . ? C4 Fe1 C2 C1 81.4(2) . . . . ? P1 Fe1 C2 C1 -28.2(3) . . . . ? P3 Fe1 C2 C1 145.19(17) . . . . ? P2 Fe1 C2 C1 -128.3(2) . . . . ? C5 Fe1 C2 C3 -81.5(2) . . . . ? C4 Fe1 C2 C3 -38.3(2) . . . . ? C1 Fe1 C2 C3 -119.7(3) . . . . ? P1 Fe1 C2 C3 -147.89(18) . . . . ? P3 Fe1 C2 C3 25.5(3) . . . . ? P2 Fe1 C2 C3 112.0(2) . . . . ? C1 C2 C3 C4 1.3(4) . . . . ? Fe1 C2 C3 C4 61.2(2) . . . . ? C1 C2 C3 Fe1 -59.9(2) . . . . ? C5 Fe1 C3 C2 80.2(2) . . . . ? C4 Fe1 C3 C2 117.5(3) . . . . ? C1 Fe1 C3 C2 36.6(2) . . . . ? P1 Fe1 C3 C2 79.2(3) . . . . ? P3 Fe1 C3 C2 -162.03(19) . . . . ? P2 Fe1 C3 C2 -74.3(2) . . . . ? C5 Fe1 C3 C4 -37.3(2) . . . . ? C1 Fe1 C3 C4 -80.9(2) . . . . ? C2 Fe1 C3 C4 -117.5(3) . . . . ? P1 Fe1 C3 C4 -38.3(4) . . . . ? P3 Fe1 C3 C4 80.47(19) . . . . ? P2 Fe1 C3 C4 168.18(17) . . . . ? C2 C3 C4 C5 -1.5(4) . . . . ? Fe1 C3 C4 C5 60.0(3) . . . . ? C2 C3 C4 Fe1 -61.5(2) . . . . ? C3 Fe1 C4 C5 -118.7(3) . . . . ? C1 Fe1 C4 C5 -37.9(2) . . . . ? C2 Fe1 C4 C5 -80.6(2) . . . . ? P1 Fe1 C4 C5 44.3(2) . . . . ? P3 Fe1 C4 C5 138.9(2) . . . . ? P2 Fe1 C4 C5 -138.4(2) . . . . ? C5 Fe1 C4 C3 118.7(3) . . . . ? C1 Fe1 C4 C3 80.8(2) . . . . ? C2 Fe1 C4 C3 38.1(2) . . . . ? P1 Fe1 C4 C3 163.02(17) . . . . ? P3 Fe1 C4 C3 -102.35(19) . . . . ? P2 Fe1 C4 C3 -19.6(3) . . . . ? C3 C4 C5 C1 1.1(4) . . . . ? Fe1 C4 C5 C1 61.1(2) . . . . ? C3 C4 C5 Fe1 -60.0(3) . . . . ? C2 C1 C5 C4 -0.3(4) . . . . ? Fe1 C1 C5 C4 -61.0(2) . . . . ? C2 C1 C5 Fe1 60.7(2) . . . . ? C3 Fe1 C5 C4 37.7(2) . . . . ? C1 Fe1 C5 C4 118.4(3) . . . . ? C2 Fe1 C5 C4 81.0(2) . . . . ? P1 Fe1 C5 C4 -142.8(2) . . . . ? P3 Fe1 C5 C4 -48.4(2) . . . . ? P2 Fe1 C5 C4 113.9(3) . . . . ? C3 Fe1 C5 C1 -80.7(2) . . . . ? C4 Fe1 C5 C1 -118.4(3) . . . . ? C2 Fe1 C5 C1 -37.4(2) . . . . ? P1 Fe1 C5 C1 98.84(19) . . . . ? P3 Fe1 C5 C1 -166.81(17) . . . . ? P2 Fe1 C5 C1 -4.5(4) . . . . ? C13 P1 C6 C7 104.2(3) . . . . ? C14 P1 C6 C7 -151.8(3) . . . . ? Fe1 P1 C6 C7 -24.8(4) . . . . ? P1 C6 C7 C8 63.0(4) . . . . ? C6 C7 C8 P2 -74.5(3) . . . . ? C9 P2 C8 C7 -74.2(3) . . . . ? C20 P2 C8 C7 -178.9(3) . . . . ? Fe1 P2 C8 C7 46.2(3) . . . . ? C8 P2 C9 C10 90.2(3) . . . . ? C20 P2 C9 C10 -163.8(3) . . . . ? Fe1 P2 C9 C10 -36.8(3) . . . . ? P2 C9 C10 P3 42.5(3) . . . . ? C11 P3 C10 C9 -161.7(2) . . . . ? C23 P3 C10 C9 91.8(3) . . . . ? Fe1 P3 C10 C9 -32.5(3) . . . . ? C10 P3 C11 C12 74.7(3) . . . . ? C23 P3 C11 C12 -178.8(3) . . . . ? Fe1 P3 C11 C12 -49.9(3) . . . . ? P3 C11 C12 C13 66.3(4) . . . . ? C11 C12 C13 P1 -73.1(4) . . . . ? C14 P1 C13 C12 -175.1(3) . . . . ? C6 P1 C13 C12 -73.6(3) . . . . ? Fe1 P1 C13 C12 59.6(3) . . . . ? C13 P1 C14 C19 -13.5(3) . . . . ? C6 P1 C14 C19 -118.3(3) . . . . ? Fe1 P1 C14 C19 110.9(3) . . . . ? C13 P1 C14 C15 168.6(3) . . . . ? C6 P1 C14 C15 63.8(3) . . . . ? Fe1 P1 C14 C15 -67.0(3) . . . . ? C19 C14 C15 C16 -0.9(5) . . . . ? P1 C14 C15 C16 177.1(3) . . . . ? C14 C15 C16 C17 0.8(6) . . . . ? C15 C16 C17 C18 0.0(6) . . . . ? C16 C17 C18 C19 -0.8(6) . . . . ? C15 C14 C19 C18 0.2(5) . . . . ? P1 C14 C19 C18 -177.7(3) . . . . ? C17 C18 C19 C14 0.7(6) . . . . ? C8 P2 C20 C21 49.5(3) . . . . ? C9 P2 C20 C21 -55.9(3) . . . . ? Fe1 P2 C20 C21 -175.8(2) . . . . ? P2 C20 C21 C22 107.1(4) . . . . ? C11 P3 C23 C24 -65.7(3) . . . . ? C10 P3 C23 C24 42.0(3) . . . . ? Fe1 P3 C23 C24 163.5(2) . . . . ? P3 C23 C24 C25 -121.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.427 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.085