data_publication_text _publ_requested_journal J.Am.Chem.Soc. _publ_contact_author_name 'Masaaki Okazaki' _publ_contact_author_address 'Institute for Chemical Research, Kyoto University' _publ_contact_author_email mokazaki@scl.kyoto-u.ac.jp _publ_contact_author_phone 81-774-38-3029 _publ_contact_author_fax 81-774-38-3039 loop_ _publ_author_name _publ_author_address 'Masaaki Okazaki' 'Institute for Chemical Research, Kyoto University' data_okazaki _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H48 F12 Fe4 P2 Si2' _chemical_properties_physical air-sensitive _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour brown _diffrn_ambient_temperature 173(2) _chemical_formula_weight 1074.28 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' Fe Fe 0.3463 0.8444 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 31 2 1' _symmetry_int_tables_number 152 _chemical_absolute_configuration unk loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' 'y, x, -z' _cell_length_a 11.366(10) _cell_length_b 11.366(10) _cell_length_c 29.309(27) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3279(5) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9067 _cell_measurement_theta_min 3.4647 _cell_measurement_theta_max 27.4835 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1638 _exptl_absorpt_coefficient_mu 1.508 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8166 _exptl_absorpt_correction_T_max 0.9284 _exptl_absorpt_process_details 'Higashi' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71070 _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 26788 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5006 _reflns_number_gt 4443 _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^)+(0.0955P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.26(3) _refine_ls_number_reflns 5006 _refine_ls_number_parameters 267 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1663 _refine_ls_wR_factor_gt 0.1589 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 Fe1 Fe 0.10416(7) 0.32218(7) 0.14252(2) 0.03222(19) Uani 1 1 d . . . Fe2 Fe -0.09640(7) 0.10389(7) 0.11874(2) 0.0342(2) Uani 1 1 d . . . C1 C 0.0633(5) 0.1312(5) 0.15197(15) 0.0351(10) Uani 1 1 d . . . C2 C -0.0829(5) 0.2714(5) 0.12676(16) 0.0351(10) Uani 1 1 d . . . C3 C -0.1326(5) 0.3420(6) 0.10300(19) 0.0387(12) Uani 1 1 d . . . C4 C -0.1753(6) 0.4015(6) 0.08044(19) 0.0429(12) Uani 1 1 d . . . Si1 Si -0.23168(17) 0.50536(17) 0.04833(6) 0.0463(4) Uani 1 1 d . . . C5 C -0.0768(7) 0.6731(7) 0.0403(3) 0.0638(19) Uani 1 1 d . . . H1 H -0.0214 0.6979 0.0680 0.096 Uiso 1 1 calc R . . H2 H -0.1028 0.7417 0.0340 0.096 Uiso 1 1 calc R . . H3 H -0.0242 0.6683 0.0145 0.096 Uiso 1 1 calc R . . C6 C -0.3605(7) 0.5184(8) 0.0840(3) 0.074(2) Uani 1 1 d . . . H4 H -0.4435 0.4294 0.0856 0.111 Uiso 1 1 calc R . . H5 H -0.3815 0.5845 0.0703 0.111 Uiso 1 1 calc R . . H6 H -0.3244 0.5482 0.1148 0.111 Uiso 1 1 calc R . . C7 C -0.3032(10) 0.4201(9) -0.0077(3) 0.080(2) Uani 1 1 d . . . H7 H -0.2413 0.3942 -0.0218 0.120 Uiso 1 1 calc R . . H8 H -0.3139 0.4829 -0.0279 0.120 Uiso 1 1 calc R . . H9 H -0.3919 0.3388 -0.0027 0.120 Uiso 1 1 calc R . . C8 C 0.2111(6) 0.5305(6) 0.1197(2) 0.0456(13) Uani 1 1 d . . . C9 C 0.2984(5) 0.5007(6) 0.1455(2) 0.0460(14) Uani 1 1 d . . . H10 H 0.3477 0.5484 0.1739 0.055 Uiso 1 1 calc R . . C10 C 0.3081(6) 0.3950(7) 0.1231(2) 0.0522(15) Uani 1 1 d . . . H11 H 0.3661 0.3564 0.1329 0.063 Uiso 1 1 calc R . . C11 C 0.2265(6) 0.3582(7) 0.0833(2) 0.0514(15) Uani 1 1 d . . . H12 H 0.2162 0.2890 0.0601 0.062 Uiso 1 1 calc R . . C12 C 0.1655(6) 0.4406(6) 0.08159(19) 0.0441(12) Uani 1 1 d . . . H13 H 0.1031 0.4383 0.0571 0.053 Uiso 1 1 calc R . . C13 C 0.1772(8) 0.6405(6) 0.1290(2) 0.0623(18) Uani 1 1 d . . . H14 H 0.2494 0.7270 0.1169 0.093 Uiso 1 1 calc R . . H15 H 0.1693 0.6488 0.1620 0.093 Uiso 1 1 calc R . . H16 H 0.0909 0.6173 0.1143 0.093 Uiso 1 1 calc R . . C14 C -0.2789(6) -0.0763(6) 0.0977(2) 0.0492(14) Uani 1 1 d . . . C15 C -0.1633(7) -0.0885(7) 0.0903(2) 0.0574(16) Uani 1 1 d . . . H17 H -0.1481 -0.1603 0.1041 0.069 Uiso 1 1 calc R . . C16 C -0.0724(7) 0.0137(8) 0.0599(2) 0.0577(17) Uani 1 1 d . . . H18 H 0.0148 0.0246 0.0478 0.069 Uiso 1 1 calc R . . C17 C -0.1316(7) 0.0944(7) 0.0485(2) 0.0576(17) Uani 1 1 d . . . H19 H -0.0935 0.1730 0.0269 0.069 Uiso 1 1 calc R . . C18 C -0.2573(6) 0.0397(6) 0.07241(19) 0.0462(13) Uani 1 1 d . . . H20 H -0.3218 0.0753 0.0708 0.055 Uiso 1 1 calc R . . C19 C -0.4011(7) -0.1685(7) 0.1247(2) 0.0632(18) Uani 1 1 d . . . H21 H -0.4714 -0.2348 0.1043 0.095 Uiso 1 1 calc R . . H22 H -0.4355 -0.1154 0.1402 0.095 Uiso 1 1 calc R . . H23 H -0.3772 -0.2163 0.1474 0.095 Uiso 1 1 calc R . . P1 P 0.35181(17) 0.04665(17) 0.06919(6) 0.0506(4) Uani 1 1 d . . . F1 F 0.2785(8) 0.0922(7) 0.0315(2) 0.124(2) Uani 1 1 d . . . F2 F 0.4232(6) -0.0011(6) 0.10398(19) 0.1102(19) Uani 1 1 d . . . F3 F 0.2873(8) -0.0954(6) 0.0460(2) 0.127(2) Uani 1 1 d . . . F4 F 0.4071(11) 0.1828(6) 0.0930(2) 0.182(4) Uani 1 1 d . . . F5 F 0.4734(7) 0.0997(9) 0.0355(3) 0.156(3) Uani 1 1 d . . . F6 F 0.2255(8) -0.0142(8) 0.1015(3) 0.160(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 Fe1 0.0292(4) 0.0350(4) 0.0318(3) 0.0047(3) 0.0055(3) 0.0156(3) Fe2 0.0345(4) 0.0345(4) 0.0340(3) -0.0026(3) 0.0015(3) 0.0175(3) C1 0.040(3) 0.040(3) 0.029(2) -0.002(2) 0.001(2) 0.023(2) C2 0.033(2) 0.035(2) 0.033(2) 0.0018(19) 0.006(2) 0.014(2) C3 0.033(2) 0.036(3) 0.044(3) 0.001(2) 0.003(2) 0.014(2) C4 0.039(3) 0.042(3) 0.047(3) 0.006(2) 0.001(2) 0.019(2) Si1 0.0458(9) 0.0465(9) 0.0529(9) 0.0093(7) 0.0007(7) 0.0278(8) C5 0.065(4) 0.052(4) 0.079(5) 0.030(4) 0.029(4) 0.032(3) C6 0.049(4) 0.064(4) 0.122(7) 0.031(5) 0.025(4) 0.038(4) C7 0.100(6) 0.087(6) 0.070(4) 0.004(4) -0.023(5) 0.059(5) C8 0.041(3) 0.039(3) 0.051(3) 0.016(2) 0.009(2) 0.016(2) C9 0.028(3) 0.043(3) 0.048(3) 0.014(3) 0.004(2) 0.004(2) C10 0.028(3) 0.066(4) 0.056(3) 0.015(3) 0.013(3) 0.019(3) C11 0.050(3) 0.055(4) 0.044(3) 0.015(3) 0.027(3) 0.022(3) C12 0.037(3) 0.045(3) 0.044(3) 0.015(2) 0.002(2) 0.015(2) C13 0.070(5) 0.035(3) 0.070(4) 0.011(3) 0.003(4) 0.017(3) C14 0.050(4) 0.039(3) 0.049(3) -0.011(2) -0.009(3) 0.015(3) C15 0.068(4) 0.052(4) 0.065(4) -0.026(3) -0.019(3) 0.039(3) C16 0.055(4) 0.075(5) 0.048(3) -0.020(3) 0.000(3) 0.036(4) C17 0.061(4) 0.061(4) 0.033(3) -0.013(3) -0.005(3) 0.017(3) C18 0.048(3) 0.050(3) 0.039(3) -0.008(2) -0.007(2) 0.023(3) C19 0.061(4) 0.043(3) 0.061(4) -0.001(3) -0.006(3) 0.008(3) P1 0.0521(9) 0.0481(9) 0.0549(8) -0.0064(7) -0.0019(7) 0.0276(7) F1 0.163(6) 0.146(6) 0.113(4) -0.009(4) -0.046(5) 0.114(5) F2 0.109(4) 0.125(5) 0.104(4) 0.025(4) -0.027(3) 0.063(4) F3 0.176(7) 0.081(4) 0.122(5) -0.034(4) -0.042(5) 0.063(4) F4 0.334(12) 0.063(3) 0.111(5) -0.032(3) -0.040(6) 0.069(6) F5 0.122(6) 0.189(8) 0.164(6) 0.084(6) 0.076(5) 0.083(6) F6 0.132(6) 0.171(7) 0.204(8) 0.055(6) 0.108(6) 0.096(5) _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 1.950(5) 5 ? Fe1 C2 1.959(5) . ? Fe1 C1 1.999(5) . ? Fe1 C10 2.113(6) . ? Fe1 C9 2.126(6) . ? Fe1 C12 2.133(5) . ? Fe1 C11 2.133(5) . ? Fe1 C8 2.157(6) . ? Fe1 Fe2 2.486(2) . ? Fe1 Fe1 2.492(2) 5 ? Fe1 Fe2 2.503(2) 5 ? Fe2 C2 1.847(5) . ? Fe2 C1 1.943(5) . ? Fe2 C1 1.957(5) 5 ? Fe2 C17 2.089(6) . ? Fe2 C16 2.093(6) . ? Fe2 C18 2.094(6) . ? Fe2 C15 2.096(6) . ? Fe2 C14 2.152(6) . ? Fe2 Fe1 2.503(2) 5 ? C1 C1 1.515(10) 5 ? C1 Fe2 1.957(5) 5 ? C2 C3 1.379(7) . ? C2 Fe1 1.950(5) 5 ? C3 C4 1.207(8) . ? C4 Si1 1.857(6) . ? Si1 C5 1.853(7) . ? Si1 C6 1.864(7) . ? Si1 C7 1.874(8) . ? C8 C9 1.416(8) . ? C8 C12 1.426(8) . ? C8 C13 1.506(9) . ? C9 C10 1.420(9) . ? C10 C11 1.418(9) . ? C11 C12 1.418(9) . ? C14 C15 1.405(9) . ? C14 C18 1.422(9) . ? C14 C19 1.483(9) . ? C15 C16 1.419(10) . ? C16 C17 1.422(10) . ? C17 C18 1.425(9) . ? P1 F4 1.517(6) . ? P1 F5 1.553(6) . ? P1 F3 1.557(6) . ? P1 F2 1.560(5) . ? P1 F6 1.562(6) . ? P1 F1 1.615(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 C2 Fe1 C2 93.7(2) 5 . ? C2 Fe1 C1 95.0(2) 5 . ? C2 Fe1 C1 94.8(2) . . ? C2 Fe1 C10 113.6(2) 5 . ? C2 Fe1 C10 150.2(2) . . ? C1 Fe1 C10 94.4(2) . . ? C2 Fe1 C9 87.1(2) 5 . ? C2 Fe1 C9 138.3(2) . . ? C1 Fe1 C9 126.7(2) . . ? C10 Fe1 C9 39.2(2) . . ? C2 Fe1 C12 136.1(2) 5 . ? C2 Fe1 C12 87.3(2) . . ? C1 Fe1 C12 128.8(2) . . ? C10 Fe1 C12 65.1(2) . . ? C9 Fe1 C12 64.9(2) . . ? C2 Fe1 C11 151.4(2) 5 . ? C2 Fe1 C11 111.8(2) . . ? C1 Fe1 C11 95.5(2) . . ? C10 Fe1 C11 39.0(2) . . ? C9 Fe1 C11 65.4(3) . . ? C12 Fe1 C11 38.8(2) . . ? C2 Fe1 C8 98.5(2) 5 . ? C2 Fe1 C8 100.6(2) . . ? C1 Fe1 C8 158.8(2) . . ? C10 Fe1 C8 65.2(3) . . ? C9 Fe1 C8 38.6(2) . . ? C12 Fe1 C8 38.8(2) . . ? C11 Fe1 C8 65.3(2) . . ? C2 Fe1 Fe2 108.59(16) 5 . ? C2 Fe1 Fe2 47.27(15) . . ? C1 Fe1 Fe2 49.91(15) . . ? C10 Fe1 Fe2 126.5(2) . . ? C9 Fe1 Fe2 163.80(17) . . ? C12 Fe1 Fe2 104.02(17) . . ? C11 Fe1 Fe2 98.49(19) . . ? C8 Fe1 Fe2 137.80(17) . . ? C2 Fe1 Fe1 50.57(16) 5 5 ? C2 Fe1 Fe1 50.25(14) . 5 ? C1 Fe1 Fe1 75.86(15) . 5 ? C10 Fe1 Fe1 159.25(18) . 5 ? C9 Fe1 Fe1 135.81(17) . 5 ? C12 Fe1 Fe1 135.11(16) . 5 ? C11 Fe1 Fe1 158.01(19) . 5 ? C8 Fe1 Fe1 125.28(16) . 5 ? Fe2 Fe1 Fe1 60.38(5) . 5 ? C2 Fe1 Fe2 46.99(16) 5 5 ? C2 Fe1 Fe2 107.64(14) . 5 ? C1 Fe1 Fe2 50.01(13) . 5 ? C10 Fe1 Fe2 99.94(18) . 5 ? C9 Fe1 Fe2 103.07(16) . 5 ? C12 Fe1 Fe2 164.98(16) . 5 ? C11 Fe1 Fe2 129.25(19) . 5 ? C8 Fe1 Fe2 135.52(17) . 5 ? Fe2 Fe1 Fe2 85.60(5) . 5 ? Fe1 Fe1 Fe2 59.71(5) 5 5 ? C2 Fe2 C1 100.5(2) . . ? C2 Fe2 C1 99.8(2) . 5 ? C1 Fe2 C1 45.7(3) . 5 ? C2 Fe2 C17 95.4(3) . . ? C1 Fe2 C17 129.9(2) . . ? C1 Fe2 C17 164.7(3) 5 . ? C2 Fe2 C16 130.2(3) . . ? C1 Fe2 C16 98.7(2) . . ? C1 Fe2 C16 125.8(3) 5 . ? C17 Fe2 C16 39.8(3) . . ? C2 Fe2 C18 92.9(2) . . ? C1 Fe2 C18 164.5(2) . . ? C1 Fe2 C18 139.5(2) 5 . ? C17 Fe2 C18 39.8(2) . . ? C16 Fe2 C18 66.4(2) . . ? C2 Fe2 C15 157.8(2) . . ? C1 Fe2 C15 100.9(2) . . ? C1 Fe2 C15 99.3(3) 5 . ? C17 Fe2 C15 66.1(3) . . ? C16 Fe2 C15 39.6(3) . . ? C18 Fe2 C15 65.2(2) . . ? C2 Fe2 C14 124.2(2) . . ? C1 Fe2 C14 132.4(2) . . ? C1 Fe2 C14 105.4(2) 5 . ? C17 Fe2 C14 66.4(2) . . ? C16 Fe2 C14 66.2(3) . . ? C18 Fe2 C14 39.1(2) . . ? C15 Fe2 C14 38.6(3) . . ? C2 Fe2 Fe1 51.20(16) . . ? C1 Fe2 Fe1 51.91(16) . . ? C1 Fe2 Fe1 76.68(16) 5 . ? C17 Fe2 Fe1 112.58(19) . . ? C16 Fe2 Fe1 116.2(2) . . ? C18 Fe2 Fe1 137.27(18) . . ? C15 Fe2 Fe1 145.69(19) . . ? C14 Fe2 Fe1 175.37(18) . . ? C2 Fe2 Fe1 50.56(15) . 5 ? C1 Fe2 Fe1 76.49(15) . 5 ? C1 Fe2 Fe1 51.49(16) 5 5 ? C17 Fe2 Fe1 143.4(2) . 5 ? C16 Fe2 Fe1 175.03(19) . 5 ? C18 Fe2 Fe1 118.47(18) . 5 ? C15 Fe2 Fe1 142.0(2) . 5 ? C14 Fe2 Fe1 117.94(17) . 5 ? Fe1 Fe2 Fe1 59.91(3) . 5 ? C1 C1 Fe2 67.6(4) 5 . ? C1 C1 Fe2 66.7(3) 5 5 ? Fe2 C1 Fe2 120.7(3) . 5 ? C1 C1 Fe1 104.14(15) 5 . ? Fe2 C1 Fe1 78.19(19) . . ? Fe2 C1 Fe1 78.49(19) 5 . ? C3 C2 Fe2 133.5(4) . . ? C3 C2 Fe1 130.1(4) . 5 ? Fe2 C2 Fe1 82.4(2) . 5 ? C3 C2 Fe1 130.4(4) . . ? Fe2 C2 Fe1 81.5(2) . . ? Fe1 C2 Fe1 79.18(19) 5 . ? C4 C3 C2 177.1(6) . . ? C3 C4 Si1 175.5(5) . . ? C5 Si1 C4 105.4(3) . . ? C5 Si1 C6 111.7(3) . . ? C4 Si1 C6 107.6(3) . . ? C5 Si1 C7 111.3(4) . . ? C4 Si1 C7 108.3(3) . . ? C6 Si1 C7 112.2(4) . . ? C9 C8 C12 107.1(5) . . ? C9 C8 C13 127.1(6) . . ? C12 C8 C13 125.8(6) . . ? C9 C8 Fe1 69.5(3) . . ? C12 C8 Fe1 69.7(3) . . ? C13 C8 Fe1 128.1(4) . . ? C8 C9 C10 108.4(5) . . ? C8 C9 Fe1 71.9(3) . . ? C10 C9 Fe1 69.9(3) . . ? C11 C10 C9 108.3(6) . . ? C11 C10 Fe1 71.3(3) . . ? C9 C10 Fe1 70.9(3) . . ? C12 C11 C10 107.3(6) . . ? C12 C11 Fe1 70.6(3) . . ? C10 C11 Fe1 69.7(3) . . ? C11 C12 C8 108.9(5) . . ? C11 C12 Fe1 70.6(3) . . ? C8 C12 Fe1 71.5(3) . . ? C15 C14 C18 106.0(6) . . ? C15 C14 C19 127.1(7) . . ? C18 C14 C19 126.8(6) . . ? C15 C14 Fe2 68.5(4) . . ? C18 C14 Fe2 68.3(3) . . ? C19 C14 Fe2 129.5(4) . . ? C14 C15 C16 110.4(6) . . ? C14 C15 Fe2 72.9(3) . . ? C16 C15 Fe2 70.1(4) . . ? C15 C16 C17 106.9(6) . . ? C15 C16 Fe2 70.3(3) . . ? C17 C16 Fe2 70.0(3) . . ? C16 C17 C18 107.3(6) . . ? C16 C17 Fe2 70.3(4) . . ? C18 C17 Fe2 70.3(3) . . ? C14 C18 C17 109.3(6) . . ? C14 C18 Fe2 72.6(3) . . ? C17 C18 Fe2 69.9(3) . . ? F4 P1 F5 93.5(5) . . ? F4 P1 F3 176.8(6) . . ? F5 P1 F3 89.5(4) . . ? F4 P1 F2 91.9(4) . . ? F5 P1 F2 91.9(4) . . ? F3 P1 F2 89.0(3) . . ? F4 P1 F6 89.6(5) . . ? F5 P1 F6 176.8(5) . . ? F3 P1 F6 87.3(4) . . ? F2 P1 F6 88.4(4) . . ? F4 P1 F1 90.2(4) . . ? F5 P1 F1 86.7(4) . . ? F3 P1 F1 89.0(3) . . ? F2 P1 F1 177.6(4) . . ? F6 P1 F1 92.8(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.148 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.097