# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Masaaki Okazaki' 'Kyeong A. Jung' 'Hiromi Tobita' _publ_contact_author_name 'Prof Masaaki Okazaki' _publ_contact_author_address ; International Research Center for Elements Science Institute for Chemical Research, Kyoto University Gokasho Uji Kyoto 6110011 JAPAN ; _publ_contact_author_email MOKAZAKI@SCL.KYOTO-U.AC.JP _publ_requested_journal 'Chemical Communications' _publ_section_title ; Regioselective Silylphosphination of Methyl Vinyl Ketone with Complexes Containing Cyclic and Linear Iron-Silicon-Phosphorus Reacting Sites ; data_complex3 _database_code_depnum_ccdc_archive 'CCDC 250453' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H37 Fe O2 P Si' _chemical_formula_weight 532.50 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' O O 0.0106 0.0060 '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 'P 21/c' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.7874(6) _cell_length_b 11.2168(7) _cell_length_c 25.7032(18) _cell_angle_alpha 90.00 _cell_angle_beta 97.956(4) _cell_angle_gamma 90.00 _cell_volume 2794.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19849 _cell_measurement_theta_min 3.98 _cell_measurement_theta_max 54.93 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.663 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8109 _exptl_absorpt_correction_T_max 0.9071 _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 23548 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6373 _reflns_number_gt 5515 _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^)+(0.0620P)^2^+2.9262P] 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 6373 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 0.10601(4) 0.29622(3) 0.629588(12) 0.01962(11) Uani 1 1 d . . . Si1 Si 0.27435(7) 0.33223(6) 0.69943(3) 0.02550(16) Uani 1 1 d . . . P1 P 0.27615(7) 0.20635(5) 0.59927(2) 0.02246(14) Uani 1 1 d . . . C1 C 0.1420(3) 0.4369(2) 0.60672(10) 0.0264(5) Uani 1 1 d . . . O1 O 0.1494(2) 0.53433(17) 0.59136(8) 0.0385(5) Uani 1 1 d . . . C2 C 0.2918(3) 0.2371(3) 0.76130(11) 0.0386(7) Uani 1 1 d . . . H1 H 0.2551 0.1572 0.7525 0.058 Uiso 1 1 calc R . . H2 H 0.2399 0.2739 0.7871 0.058 Uiso 1 1 calc R . . H3 H 0.3893 0.2311 0.7761 0.058 Uiso 1 1 calc R . . C3 C 0.2787(3) 0.4891(3) 0.72664(12) 0.0367(6) Uani 1 1 d . . . H4 H 0.3584 0.4979 0.7540 0.055 Uiso 1 1 calc R . . H5 H 0.1937 0.5045 0.7417 0.055 Uiso 1 1 calc R . . H6 H 0.2862 0.5462 0.6983 0.055 Uiso 1 1 calc R . . O2 O 0.4324(2) 0.31216(18) 0.67944(8) 0.0342(4) Uani 1 1 d . . . C4 C 0.4470(3) 0.2834(2) 0.62678(11) 0.0307(6) Uani 1 1 d . . . C5 C 0.5762(3) 0.2049(3) 0.62726(14) 0.0425(7) Uani 1 1 d . . . H7 H 0.6540 0.2419 0.6496 0.064 Uiso 1 1 calc R . . H8 H 0.5985 0.1971 0.5914 0.064 Uiso 1 1 calc R . . H9 H 0.5585 0.1258 0.6411 0.064 Uiso 1 1 calc R . . C6 C 0.4652(3) 0.3950(3) 0.59460(14) 0.0407(7) Uani 1 1 d . . . H10 H 0.4585 0.3881 0.5575 0.049 Uiso 1 1 calc R . . C7 C 0.4900(5) 0.5011(4) 0.6163(2) 0.0700(12) Uani 1 1 d . . . H11 H 0.4970 0.5099 0.6534 0.084 Uiso 1 1 calc R . . H12 H 0.5007 0.5685 0.5949 0.084 Uiso 1 1 calc R . . C8 C 0.3027(3) 0.0475(2) 0.61707(10) 0.0258(5) Uani 1 1 d . . . C9 C 0.3553(3) 0.0163(2) 0.66876(11) 0.0303(5) Uani 1 1 d . . . H13 H 0.3863 0.0770 0.6934 0.036 Uiso 1 1 calc R . . C10 C 0.3627(3) -0.1031(3) 0.68453(12) 0.0379(6) Uani 1 1 d . . . H14 H 0.3991 -0.1232 0.7196 0.045 Uiso 1 1 calc R . . C11 C 0.3168(4) -0.1923(3) 0.64878(14) 0.0434(7) Uani 1 1 d . . . H15 H 0.3217 -0.2734 0.6595 0.052 Uiso 1 1 calc R . . C12 C 0.2642(4) -0.1632(3) 0.59791(13) 0.0409(7) Uani 1 1 d . . . H16 H 0.2325 -0.2244 0.5736 0.049 Uiso 1 1 calc R . . C13 C 0.2573(3) -0.0436(2) 0.58173(11) 0.0327(6) Uani 1 1 d . . . H17 H 0.2215 -0.0245 0.5465 0.039 Uiso 1 1 calc R . . C14 C 0.2781(3) 0.2034(2) 0.52760(10) 0.0285(5) Uani 1 1 d . . . C15 C 0.3800(3) 0.1435(3) 0.50397(12) 0.0388(7) Uani 1 1 d . . . H18 H 0.4509 0.1009 0.5252 0.047 Uiso 1 1 calc R . . C16 C 0.3774(4) 0.1466(3) 0.44957(13) 0.0492(9) Uani 1 1 d . . . H19 H 0.4481 0.1083 0.4339 0.059 Uiso 1 1 calc R . . C17 C 0.2707(4) 0.2061(3) 0.41802(12) 0.0509(9) Uani 1 1 d . . . H20 H 0.2681 0.2068 0.3809 0.061 Uiso 1 1 calc R . . C18 C 0.1688(4) 0.2641(3) 0.44085(12) 0.0457(8) Uani 1 1 d . . . H21 H 0.0957 0.3037 0.4194 0.055 Uiso 1 1 calc R . . C19 C 0.1740(3) 0.2640(2) 0.49553(11) 0.0334(6) Uani 1 1 d . . . H22 H 0.1056 0.3059 0.5111 0.040 Uiso 1 1 calc R . . C20 C -0.0634(3) 0.1874(2) 0.59558(9) 0.0255(5) Uani 1 1 d . . . C21 C -0.1027(3) 0.3094(2) 0.59303(10) 0.0258(5) Uani 1 1 d . . . C22 C -0.0881(3) 0.3553(2) 0.64601(9) 0.0247(5) Uani 1 1 d . . . C23 C -0.0433(3) 0.2597(2) 0.68084(9) 0.0236(5) Uani 1 1 d . . . C24 C -0.0248(3) 0.1557(2) 0.65002(9) 0.0238(5) Uani 1 1 d . . . C25 C -0.0798(3) 0.1000(3) 0.55078(10) 0.0332(6) Uani 1 1 d . . . H23 H -0.1750 0.0705 0.5451 0.050 Uiso 1 1 calc R . . H24 H -0.0164 0.0329 0.5592 0.050 Uiso 1 1 calc R . . H25 H -0.0587 0.1396 0.5189 0.050 Uiso 1 1 calc R . . C26 C -0.1618(3) 0.3777(3) 0.54450(11) 0.0368(6) Uani 1 1 d . . . H26 H -0.1339 0.3394 0.5134 0.055 Uiso 1 1 calc R . . H27 H -0.1272 0.4598 0.5470 0.055 Uiso 1 1 calc R . . H28 H -0.2627 0.3784 0.5416 0.055 Uiso 1 1 calc R . . C27 C -0.1302(3) 0.4774(2) 0.66236(11) 0.0343(6) Uani 1 1 d . . . H29 H -0.2225 0.4733 0.6730 0.051 Uiso 1 1 calc R . . H30 H -0.1314 0.5327 0.6328 0.051 Uiso 1 1 calc R . . H31 H -0.0642 0.5056 0.6919 0.051 Uiso 1 1 calc R . . C28 C -0.0459(3) 0.2635(2) 0.73913(10) 0.0309(6) Uani 1 1 d . . . H32 H -0.0047 0.3383 0.7533 0.046 Uiso 1 1 calc R . . H33 H 0.0069 0.1961 0.7558 0.046 Uiso 1 1 calc R . . H34 H -0.1415 0.2585 0.7463 0.046 Uiso 1 1 calc R . . C29 C 0.0035(3) 0.0317(2) 0.67087(10) 0.0302(6) Uani 1 1 d . . . H35 H 0.0641 0.0355 0.7045 0.045 Uiso 1 1 calc R . . H36 H 0.0485 -0.0147 0.6457 0.045 Uiso 1 1 calc R . . H37 H -0.0836 -0.0067 0.6760 0.045 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 0.02516(19) 0.01631(17) 0.01845(17) 0.00077(11) 0.00679(12) -0.00321(13) Si1 0.0293(4) 0.0225(3) 0.0245(3) -0.0027(3) 0.0033(3) -0.0068(3) P1 0.0271(3) 0.0180(3) 0.0239(3) 0.0015(2) 0.0090(2) -0.0021(2) C1 0.0291(12) 0.0250(13) 0.0268(12) -0.0001(9) 0.0092(10) -0.0039(10) O1 0.0473(12) 0.0226(10) 0.0468(12) 0.0111(8) 0.0107(9) -0.0037(8) C2 0.0421(16) 0.0436(17) 0.0281(13) 0.0037(12) -0.0027(12) -0.0088(13) C3 0.0423(16) 0.0299(14) 0.0380(15) -0.0098(11) 0.0056(12) -0.0072(12) O2 0.0283(10) 0.0349(11) 0.0395(11) -0.0093(8) 0.0046(8) -0.0072(8) C4 0.0273(13) 0.0247(13) 0.0423(15) -0.0013(10) 0.0124(11) -0.0062(10) C5 0.0317(15) 0.0350(16) 0.065(2) -0.0042(14) 0.0198(14) -0.0080(12) C6 0.0330(15) 0.0340(16) 0.0575(18) 0.0048(13) 0.0149(13) -0.0092(12) C7 0.065(3) 0.050(2) 0.098(3) 0.010(2) 0.022(2) -0.0112(19) C8 0.0274(12) 0.0195(12) 0.0320(13) 0.0032(9) 0.0092(10) -0.0009(9) C9 0.0298(13) 0.0268(13) 0.0340(13) 0.0030(10) 0.0035(11) 0.0003(10) C10 0.0380(15) 0.0306(15) 0.0441(16) 0.0119(12) 0.0025(13) 0.0043(12) C11 0.0514(19) 0.0205(13) 0.0600(19) 0.0085(12) 0.0137(15) 0.0022(12) C12 0.0572(19) 0.0200(13) 0.0476(17) -0.0049(12) 0.0144(14) -0.0048(13) C13 0.0419(15) 0.0240(13) 0.0336(13) -0.0013(10) 0.0102(12) -0.0026(11) C14 0.0382(14) 0.0230(12) 0.0275(12) 0.0018(9) 0.0153(11) -0.0026(10) C15 0.0483(17) 0.0352(16) 0.0379(15) 0.0012(12) 0.0236(13) 0.0006(13) C16 0.069(2) 0.0436(18) 0.0433(17) -0.0020(14) 0.0366(17) 0.0001(16) C17 0.085(3) 0.0458(19) 0.0279(14) 0.0041(13) 0.0279(16) -0.0032(18) C18 0.071(2) 0.0375(17) 0.0309(15) 0.0092(12) 0.0155(14) 0.0036(16) C19 0.0490(17) 0.0249(13) 0.0289(13) 0.0043(10) 0.0145(12) 0.0005(12) C20 0.0260(12) 0.0289(13) 0.0223(11) -0.0035(9) 0.0060(9) -0.0079(10) C21 0.0238(12) 0.0298(13) 0.0242(12) 0.0016(10) 0.0040(9) -0.0014(10) C22 0.0248(12) 0.0253(12) 0.0252(11) -0.0020(9) 0.0079(9) -0.0008(9) C23 0.0266(12) 0.0246(12) 0.0218(11) -0.0013(9) 0.0107(9) -0.0037(9) C24 0.0288(12) 0.0211(12) 0.0230(11) -0.0012(9) 0.0092(9) -0.0059(9) C25 0.0394(15) 0.0343(15) 0.0267(12) -0.0088(11) 0.0069(11) -0.0096(12) C26 0.0375(15) 0.0448(17) 0.0272(13) 0.0046(12) 0.0014(11) 0.0048(13) C27 0.0410(16) 0.0281(14) 0.0354(14) -0.0021(11) 0.0107(12) 0.0054(12) C28 0.0430(15) 0.0305(13) 0.0220(12) -0.0022(10) 0.0141(11) -0.0048(11) C29 0.0411(15) 0.0221(12) 0.0299(13) 0.0019(10) 0.0143(11) -0.0072(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 1.737(3) . ? Fe1 C22 2.109(2) . ? Fe1 C21 2.132(3) . ? Fe1 C23 2.139(2) . ? Fe1 C24 2.141(2) . ? Fe1 C20 2.145(2) . ? Fe1 P1 2.1808(7) . ? Fe1 Si1 2.2982(8) . ? Si1 O2 1.711(2) . ? Si1 C3 1.892(3) . ? Si1 C2 1.903(3) . ? P1 C14 1.845(3) . ? P1 C8 1.849(3) . ? P1 C4 1.927(3) . ? C1 O1 1.168(3) . ? O2 C4 1.418(3) . ? C4 C6 1.525(4) . ? C4 C5 1.540(4) . ? C6 C7 1.322(5) . ? C8 C13 1.399(4) . ? C8 C9 1.401(4) . ? C9 C10 1.398(4) . ? C10 C11 1.390(5) . ? C11 C12 1.376(5) . ? C12 C13 1.403(4) . ? C14 C19 1.395(4) . ? C14 C15 1.409(4) . ? C15 C16 1.396(4) . ? C16 C17 1.400(5) . ? C17 C18 1.387(5) . ? C18 C19 1.399(4) . ? C20 C21 1.420(4) . ? C20 C24 1.442(3) . ? C20 C25 1.504(3) . ? C21 C22 1.445(3) . ? C21 C26 1.509(4) . ? C22 C23 1.427(3) . ? C22 C27 1.507(4) . ? C23 C24 1.435(3) . ? C23 C28 1.502(3) . ? C24 C29 1.503(3) . ? 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 C1 Fe1 C22 90.73(11) . . ? C1 Fe1 C21 90.85(11) . . ? C22 Fe1 C21 39.83(9) . . ? C1 Fe1 C23 124.79(11) . . ? C22 Fe1 C23 39.25(10) . . ? C21 Fe1 C23 65.79(9) . . ? C1 Fe1 C24 155.20(11) . . ? C22 Fe1 C24 66.20(10) . . ? C21 Fe1 C24 65.80(10) . . ? C23 Fe1 C24 39.19(9) . . ? C1 Fe1 C20 124.09(11) . . ? C22 Fe1 C20 66.02(10) . . ? C21 Fe1 C20 38.78(10) . . ? C23 Fe1 C20 65.56(9) . . ? C24 Fe1 C20 39.33(9) . . ? C1 Fe1 P1 95.64(9) . . ? C22 Fe1 P1 166.00(7) . . ? C21 Fe1 P1 127.36(7) . . ? C23 Fe1 P1 138.80(7) . . ? C24 Fe1 P1 105.04(7) . . ? C20 Fe1 P1 100.18(7) . . ? C1 Fe1 Si1 87.00(9) . . ? C22 Fe1 Si1 110.89(7) . . ? C21 Fe1 Si1 150.66(7) . . ? C23 Fe1 Si1 91.70(7) . . ? C24 Fe1 Si1 109.04(7) . . ? C20 Fe1 Si1 148.04(7) . . ? P1 Fe1 Si1 81.95(3) . . ? O2 Si1 C3 104.97(12) . . ? O2 Si1 C2 101.35(13) . . ? C3 Si1 C2 102.59(14) . . ? O2 Si1 Fe1 108.82(7) . . ? C3 Si1 Fe1 115.41(10) . . ? C2 Si1 Fe1 121.73(10) . . ? C14 P1 C8 102.09(12) . . ? C14 P1 C4 104.25(12) . . ? C8 P1 C4 104.84(12) . . ? C14 P1 Fe1 118.61(9) . . ? C8 P1 Fe1 116.42(8) . . ? C4 P1 Fe1 109.16(9) . . ? O1 C1 Fe1 171.8(2) . . ? C4 O2 Si1 122.08(17) . . ? O2 C4 C6 111.4(2) . . ? O2 C4 C5 108.3(2) . . ? C6 C4 C5 108.4(2) . . ? O2 C4 P1 104.82(16) . . ? C6 C4 P1 109.3(2) . . ? C5 C4 P1 114.6(2) . . ? C7 C6 C4 122.6(3) . . ? C13 C8 C9 118.4(2) . . ? C13 C8 P1 121.5(2) . . ? C9 C8 P1 119.7(2) . . ? C10 C9 C8 120.8(3) . . ? C11 C10 C9 119.9(3) . . ? C12 C11 C10 120.1(3) . . ? C11 C12 C13 120.3(3) . . ? C8 C13 C12 120.6(3) . . ? C19 C14 C15 118.7(2) . . ? C19 C14 P1 118.3(2) . . ? C15 C14 P1 123.0(2) . . ? C16 C15 C14 120.3(3) . . ? C15 C16 C17 120.1(3) . . ? C18 C17 C16 120.1(3) . . ? C17 C18 C19 119.8(3) . . ? C14 C19 C18 121.1(3) . . ? C21 C20 C24 108.4(2) . . ? C21 C20 C25 126.4(2) . . ? C24 C20 C25 124.6(2) . . ? C21 C20 Fe1 70.11(14) . . ? C24 C20 Fe1 70.19(14) . . ? C25 C20 Fe1 132.65(18) . . ? C20 C21 C22 108.0(2) . . ? C20 C21 C26 126.7(2) . . ? C22 C21 C26 125.0(2) . . ? C20 C21 Fe1 71.11(14) . . ? C22 C21 Fe1 69.23(14) . . ? C26 C21 Fe1 129.31(19) . . ? C23 C22 C21 107.8(2) . . ? C23 C22 C27 125.5(2) . . ? C21 C22 C27 126.3(2) . . ? C23 C22 Fe1 71.50(14) . . ? C21 C22 Fe1 70.94(14) . . ? C27 C22 Fe1 129.07(19) . . ? C22 C23 C24 108.4(2) . . ? C22 C23 C28 123.9(2) . . ? C24 C23 C28 126.5(2) . . ? C22 C23 Fe1 69.26(13) . . ? C24 C23 Fe1 70.51(13) . . ? C28 C23 Fe1 135.71(19) . . ? C23 C24 C20 107.4(2) . . ? C23 C24 C29 125.9(2) . . ? C20 C24 C29 125.8(2) . . ? C23 C24 Fe1 70.31(13) . . ? C20 C24 Fe1 70.48(14) . . ? C29 C24 Fe1 132.98(19) . . ? 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 C1 Fe1 Si1 O2 -77.82(12) . . . . ? C22 Fe1 Si1 O2 -167.46(11) . . . . ? C21 Fe1 Si1 O2 -164.22(16) . . . . ? C23 Fe1 Si1 O2 157.42(11) . . . . ? C24 Fe1 Si1 O2 121.52(11) . . . . ? C20 Fe1 Si1 O2 114.67(16) . . . . ? P1 Fe1 Si1 O2 18.31(8) . . . . ? C1 Fe1 Si1 C3 39.83(14) . . . . ? C22 Fe1 Si1 C3 -49.81(13) . . . . ? C21 Fe1 Si1 C3 -46.57(19) . . . . ? C23 Fe1 Si1 C3 -84.93(13) . . . . ? C24 Fe1 Si1 C3 -120.83(13) . . . . ? C20 Fe1 Si1 C3 -127.68(17) . . . . ? P1 Fe1 Si1 C3 135.96(11) . . . . ? C1 Fe1 Si1 C2 165.10(15) . . . . ? C22 Fe1 Si1 C2 75.47(15) . . . . ? C21 Fe1 Si1 C2 78.7(2) . . . . ? C23 Fe1 Si1 C2 40.35(15) . . . . ? C24 Fe1 Si1 C2 4.45(15) . . . . ? C20 Fe1 Si1 C2 -2.4(2) . . . . ? P1 Fe1 Si1 C2 -98.76(13) . . . . ? C1 Fe1 P1 C14 -62.79(13) . . . . ? C22 Fe1 P1 C14 53.9(3) . . . . ? C21 Fe1 P1 C14 32.61(13) . . . . ? C23 Fe1 P1 C14 127.70(14) . . . . ? C24 Fe1 P1 C14 103.40(12) . . . . ? C20 Fe1 P1 C14 63.36(12) . . . . ? Si1 Fe1 P1 C14 -148.95(10) . . . . ? C1 Fe1 P1 C8 174.69(13) . . . . ? C22 Fe1 P1 C8 -68.6(3) . . . . ? C21 Fe1 P1 C8 -89.90(13) . . . . ? C23 Fe1 P1 C8 5.19(15) . . . . ? C24 Fe1 P1 C8 -19.11(12) . . . . ? C20 Fe1 P1 C8 -59.15(12) . . . . ? Si1 Fe1 P1 C8 88.53(10) . . . . ? C1 Fe1 P1 C4 56.30(13) . . . . ? C22 Fe1 P1 C4 173.0(3) . . . . ? C21 Fe1 P1 C4 151.70(13) . . . . ? C23 Fe1 P1 C4 -113.20(14) . . . . ? C24 Fe1 P1 C4 -137.50(11) . . . . ? C20 Fe1 P1 C4 -177.54(11) . . . . ? Si1 Fe1 P1 C4 -29.86(10) . . . . ? C22 Fe1 C1 O1 -13.1(16) . . . . ? C21 Fe1 C1 O1 26.7(16) . . . . ? C23 Fe1 C1 O1 -34.0(17) . . . . ? C24 Fe1 C1 O1 7.7(18) . . . . ? C20 Fe1 C1 O1 48.0(17) . . . . ? P1 Fe1 C1 O1 154.4(16) . . . . ? Si1 Fe1 C1 O1 -124.0(16) . . . . ? C3 Si1 O2 C4 -121.5(2) . . . . ? C2 Si1 O2 C4 132.0(2) . . . . ? Fe1 Si1 O2 C4 2.6(2) . . . . ? Si1 O2 C4 C6 92.9(2) . . . . ? Si1 O2 C4 C5 -148.00(19) . . . . ? Si1 O2 C4 P1 -25.2(2) . . . . ? C14 P1 C4 O2 166.35(17) . . . . ? C8 P1 C4 O2 -86.74(19) . . . . ? Fe1 P1 C4 O2 38.67(19) . . . . ? C14 P1 C4 C6 46.8(2) . . . . ? C8 P1 C4 C6 153.7(2) . . . . ? Fe1 P1 C4 C6 -80.9(2) . . . . ? C14 P1 C4 C5 -75.1(2) . . . . ? C8 P1 C4 C5 31.8(2) . . . . ? Fe1 P1 C4 C5 157.24(19) . . . . ? O2 C4 C6 C7 11.7(4) . . . . ? C5 C4 C6 C7 -107.3(4) . . . . ? P1 C4 C6 C7 127.1(3) . . . . ? C14 P1 C8 C13 -29.6(2) . . . . ? C4 P1 C8 C13 -138.1(2) . . . . ? Fe1 P1 C8 C13 101.2(2) . . . . ? C14 P1 C8 C9 157.6(2) . . . . ? C4 P1 C8 C9 49.1(2) . . . . ? Fe1 P1 C8 C9 -71.6(2) . . . . ? C13 C8 C9 C10 0.2(4) . . . . ? P1 C8 C9 C10 173.2(2) . . . . ? C8 C9 C10 C11 -0.4(4) . . . . ? C9 C10 C11 C12 0.1(5) . . . . ? C10 C11 C12 C13 0.3(5) . . . . ? C9 C8 C13 C12 0.2(4) . . . . ? P1 C8 C13 C12 -172.7(2) . . . . ? C11 C12 C13 C8 -0.5(5) . . . . ? C8 P1 C14 C19 132.6(2) . . . . ? C4 P1 C14 C19 -118.5(2) . . . . ? Fe1 P1 C14 C19 3.1(3) . . . . ? C8 P1 C14 C15 -47.8(3) . . . . ? C4 P1 C14 C15 61.1(3) . . . . ? Fe1 P1 C14 C15 -177.3(2) . . . . ? C19 C14 C15 C16 0.9(4) . . . . ? P1 C14 C15 C16 -178.7(2) . . . . ? C14 C15 C16 C17 -2.1(5) . . . . ? C15 C16 C17 C18 1.2(5) . . . . ? C16 C17 C18 C19 0.8(5) . . . . ? C15 C14 C19 C18 1.1(4) . . . . ? P1 C14 C19 C18 -179.3(2) . . . . ? C17 C18 C19 C14 -1.9(5) . . . . ? C1 Fe1 C20 C21 -35.52(19) . . . . ? C22 Fe1 C20 C21 37.97(14) . . . . ? C23 Fe1 C20 C21 81.18(16) . . . . ? C24 Fe1 C20 C21 119.1(2) . . . . ? P1 Fe1 C20 C21 -139.53(13) . . . . ? Si1 Fe1 C20 C21 129.37(15) . . . . ? C1 Fe1 C20 C24 -154.63(16) . . . . ? C22 Fe1 C20 C24 -81.14(15) . . . . ? C21 Fe1 C20 C24 -119.1(2) . . . . ? C23 Fe1 C20 C24 -37.94(14) . . . . ? P1 Fe1 C20 C24 101.36(14) . . . . ? Si1 Fe1 C20 C24 10.3(2) . . . . ? C1 Fe1 C20 C25 86.1(3) . . . . ? C22 Fe1 C20 C25 159.6(3) . . . . ? C21 Fe1 C20 C25 121.6(3) . . . . ? C23 Fe1 C20 C25 -157.2(3) . . . . ? C24 Fe1 C20 C25 -119.3(3) . . . . ? P1 Fe1 C20 C25 -17.9(3) . . . . ? Si1 Fe1 C20 C25 -109.0(2) . . . . ? C24 C20 C21 C22 0.4(3) . . . . ? C25 C20 C21 C22 171.4(2) . . . . ? Fe1 C20 C21 C22 -59.64(17) . . . . ? C24 C20 C21 C26 -174.5(3) . . . . ? C25 C20 C21 C26 -3.5(4) . . . . ? Fe1 C20 C21 C26 125.5(3) . . . . ? C24 C20 C21 Fe1 60.01(17) . . . . ? C25 C20 C21 Fe1 -128.9(3) . . . . ? C1 Fe1 C21 C20 151.24(16) . . . . ? C22 Fe1 C21 C20 -118.6(2) . . . . ? C23 Fe1 C21 C20 -80.52(15) . . . . ? C24 Fe1 C21 C20 -37.38(14) . . . . ? P1 Fe1 C21 C20 53.48(16) . . . . ? Si1 Fe1 C21 C20 -123.37(16) . . . . ? C1 Fe1 C21 C22 -90.12(16) . . . . ? C23 Fe1 C21 C22 38.12(14) . . . . ? C24 Fe1 C21 C22 81.27(15) . . . . ? C20 Fe1 C21 C22 118.6(2) . . . . ? P1 Fe1 C21 C22 172.12(12) . . . . ? Si1 Fe1 C21 C22 -4.7(2) . . . . ? C1 Fe1 C21 C26 28.8(3) . . . . ? C22 Fe1 C21 C26 118.9(3) . . . . ? C23 Fe1 C21 C26 157.0(3) . . . . ? C24 Fe1 C21 C26 -159.8(3) . . . . ? C20 Fe1 C21 C26 -122.5(3) . . . . ? P1 Fe1 C21 C26 -69.0(3) . . . . ? Si1 Fe1 C21 C26 114.2(2) . . . . ? C20 C21 C22 C23 -1.6(3) . . . . ? C26 C21 C22 C23 173.4(2) . . . . ? Fe1 C21 C22 C23 -62.41(17) . . . . ? C20 C21 C22 C27 -174.2(2) . . . . ? C26 C21 C22 C27 0.8(4) . . . . ? Fe1 C21 C22 C27 125.0(3) . . . . ? C20 C21 C22 Fe1 60.83(18) . . . . ? C26 C21 C22 Fe1 -124.2(3) . . . . ? C1 Fe1 C22 C23 -152.43(16) . . . . ? C21 Fe1 C22 C23 117.1(2) . . . . ? C24 Fe1 C22 C23 36.95(14) . . . . ? C20 Fe1 C22 C23 80.14(15) . . . . ? P1 Fe1 C22 C23 90.4(3) . . . . ? Si1 Fe1 C22 C23 -65.36(14) . . . . ? C1 Fe1 C22 C21 90.45(16) . . . . ? C23 Fe1 C22 C21 -117.1(2) . . . . ? C24 Fe1 C22 C21 -80.17(15) . . . . ? C20 Fe1 C22 C21 -36.98(14) . . . . ? P1 Fe1 C22 C21 -26.8(4) . . . . ? Si1 Fe1 C22 C21 177.52(12) . . . . ? C1 Fe1 C22 C27 -31.3(2) . . . . ? C21 Fe1 C22 C27 -121.8(3) . . . . ? C23 Fe1 C22 C27 121.1(3) . . . . ? C24 Fe1 C22 C27 158.1(3) . . . . ? C20 Fe1 C22 C27 -158.7(3) . . . . ? P1 Fe1 C22 C27 -148.5(2) . . . . ? Si1 Fe1 C22 C27 55.8(2) . . . . ? C21 C22 C23 C24 2.2(3) . . . . ? C27 C22 C23 C24 174.8(2) . . . . ? Fe1 C22 C23 C24 -59.87(17) . . . . ? C21 C22 C23 C28 -166.1(2) . . . . ? C27 C22 C23 C28 6.6(4) . . . . ? Fe1 C22 C23 C28 131.9(2) . . . . ? C21 C22 C23 Fe1 62.05(17) . . . . ? C27 C22 C23 Fe1 -125.3(3) . . . . ? C1 Fe1 C23 C22 34.31(19) . . . . ? C21 Fe1 C23 C22 -38.68(14) . . . . ? C24 Fe1 C23 C22 -119.5(2) . . . . ? C20 Fe1 C23 C22 -81.41(16) . . . . ? P1 Fe1 C23 C22 -158.45(12) . . . . ? Si1 Fe1 C23 C22 121.84(13) . . . . ? C1 Fe1 C23 C24 153.78(16) . . . . ? C22 Fe1 C23 C24 119.5(2) . . . . ? C21 Fe1 C23 C24 80.80(16) . . . . ? C20 Fe1 C23 C24 38.07(15) . . . . ? P1 Fe1 C23 C24 -38.97(19) . . . . ? Si1 Fe1 C23 C24 -118.68(14) . . . . ? C1 Fe1 C23 C28 -83.5(3) . . . . ? C22 Fe1 C23 C28 -117.8(3) . . . . ? C21 Fe1 C23 C28 -156.5(3) . . . . ? C24 Fe1 C23 C28 122.7(3) . . . . ? C20 Fe1 C23 C28 160.8(3) . . . . ? P1 Fe1 C23 C28 83.7(3) . . . . ? Si1 Fe1 C23 C28 4.0(3) . . . . ? C22 C23 C24 C20 -2.0(3) . . . . ? C28 C23 C24 C20 165.9(2) . . . . ? Fe1 C23 C24 C20 -61.04(17) . . . . ? C22 C23 C24 C29 -171.5(2) . . . . ? C28 C23 C24 C29 -3.6(4) . . . . ? Fe1 C23 C24 C29 129.4(3) . . . . ? C22 C23 C24 Fe1 59.09(17) . . . . ? C28 C23 C24 Fe1 -133.1(3) . . . . ? C21 C20 C24 C23 1.0(3) . . . . ? C25 C20 C24 C23 -170.3(2) . . . . ? Fe1 C20 C24 C23 60.93(17) . . . . ? C21 C20 C24 C29 170.5(2) . . . . ? C25 C20 C24 C29 -0.7(4) . . . . ? Fe1 C20 C24 C29 -129.5(3) . . . . ? C21 C20 C24 Fe1 -59.96(17) . . . . ? C25 C20 C24 Fe1 128.8(3) . . . . ? C1 Fe1 C24 C23 -59.9(3) . . . . ? C22 Fe1 C24 C23 -37.01(15) . . . . ? C21 Fe1 C24 C23 -80.79(16) . . . . ? C20 Fe1 C24 C23 -117.7(2) . . . . ? P1 Fe1 C24 C23 154.60(13) . . . . ? Si1 Fe1 C24 C23 68.07(15) . . . . ? C1 Fe1 C24 C20 57.8(3) . . . . ? C22 Fe1 C24 C20 80.64(16) . . . . ? C21 Fe1 C24 C20 36.86(15) . . . . ? C23 Fe1 C24 C20 117.7(2) . . . . ? P1 Fe1 C24 C20 -87.75(14) . . . . ? Si1 Fe1 C24 C20 -174.28(13) . . . . ? C1 Fe1 C24 C29 179.0(2) . . . . ? C22 Fe1 C24 C29 -158.2(3) . . . . ? C21 Fe1 C24 C29 158.0(3) . . . . ? C23 Fe1 C24 C29 -121.2(3) . . . . ? C20 Fe1 C24 C29 121.2(3) . . . . ? P1 Fe1 C24 C29 33.4(2) . . . . ? Si1 Fe1 C24 C29 -53.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.746 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.074 data_complex4 _database_code_depnum_ccdc_archive 'CCDC 250454' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H37 Fe O3 P Si' _chemical_formula_weight 560.51 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' O O 0.0106 0.0060 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6625(7) _cell_length_b 12.0795(7) _cell_length_c 12.8947(7) _cell_angle_alpha 99.7325(14) _cell_angle_beta 94.253(4) _cell_angle_gamma 100.4248(17) _cell_volume 1450.36(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6692 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 54.91 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.645 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8301 _exptl_absorpt_correction_T_max 0.9383 _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measrued' _diffrn_reflns_number 14208 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6605 _reflns_number_gt 6043 _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^)+(0.0337P)^2^+1.1398P] 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 6605 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.158 _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 -0.35393(3) 0.26354(2) -0.36849(2) 0.01756(7) Uani 1 1 d . . . Si1 Si -0.14792(5) 0.39928(4) -0.32992(4) 0.01772(11) Uani 1 1 d . . . C1 C -0.1767(2) 0.54845(17) -0.33431(17) 0.0267(4) Uani 1 1 d . . . H1 H -0.2332 0.5723 -0.2776 0.040 Uiso 1 1 calc R . . H2 H -0.2268 0.5495 -0.4029 0.040 Uiso 1 1 calc R . . H3 H -0.0849 0.6013 -0.3247 0.040 Uiso 1 1 calc R . . C2 C -0.0082(2) 0.37771(18) -0.42125(16) 0.0275(4) Uani 1 1 d . . . H4 H 0.0757 0.4386 -0.3984 0.041 Uiso 1 1 calc R . . H5 H -0.0449 0.3801 -0.4936 0.041 Uiso 1 1 calc R . . H6 H 0.0175 0.3032 -0.4194 0.041 Uiso 1 1 calc R . . O1 O -0.07577(13) 0.39173(11) -0.20940(10) 0.0205(3) Uani 1 1 d . . . C3 C 0.0540(2) 0.44654(15) -0.15630(14) 0.0203(4) Uani 1 1 d . . . C4 C 0.0645(2) 0.57059(17) -0.11023(17) 0.0307(5) Uani 1 1 d . . . H7 H 0.1567 0.6006 -0.0685 0.046 Uiso 1 1 calc R . . H8 H -0.0111 0.5788 -0.0645 0.046 Uiso 1 1 calc R . . H9 H 0.0547 0.6135 -0.1675 0.046 Uiso 1 1 calc R . . C5 C 0.1561(2) 0.38794(17) -0.14283(15) 0.0247(4) Uani 1 1 d . . . H10 H 0.2421 0.4283 -0.1025 0.030 Uiso 1 1 calc R . . C6 C 0.1456(2) 0.26301(17) -0.18650(16) 0.0260(4) Uani 1 1 d . . . H11 H 0.2399 0.2498 -0.2043 0.031 Uiso 1 1 calc R . . H12 H 0.0802 0.2414 -0.2526 0.031 Uiso 1 1 calc R . . P1 P 0.08129(5) 0.17009(4) -0.09176(4) 0.02363(11) Uani 1 1 d . . . C7 C 0.1175(2) 0.03314(17) -0.16004(16) 0.0247(4) Uani 1 1 d . . . C8 C 0.1979(2) -0.03309(18) -0.11183(17) 0.0305(4) Uani 1 1 d . . . H13 H 0.2428 -0.0052 -0.0419 0.037 Uiso 1 1 calc R . . C9 C 0.2127(2) -0.13966(18) -0.1655(2) 0.0347(5) Uani 1 1 d . . . H14 H 0.2664 -0.1844 -0.1314 0.042 Uiso 1 1 calc R . . C10 C 0.1502(2) -0.18097(19) -0.26756(19) 0.0355(5) Uani 1 1 d . . . H15 H 0.1616 -0.2534 -0.3041 0.043 Uiso 1 1 calc R . . C11 C 0.0705(3) -0.1162(2) -0.31662(18) 0.0379(5) Uani 1 1 d . . . H16 H 0.0275 -0.1440 -0.3871 0.045 Uiso 1 1 calc R . . C12 C 0.0534(3) -0.01078(19) -0.26296(18) 0.0347(5) Uani 1 1 d . . . H17 H -0.0029 0.0323 -0.2969 0.042 Uiso 1 1 calc R . . C13 C 0.2256(2) 0.20736(16) 0.01643(15) 0.0237(4) Uani 1 1 d . . . C14 C 0.1918(2) 0.1832(2) 0.11425(17) 0.0318(5) Uani 1 1 d . . . H18 H 0.0962 0.1543 0.1237 0.038 Uiso 1 1 calc R . . C15 C 0.2975(3) 0.2010(2) 0.19879(18) 0.0405(6) Uani 1 1 d . . . H19 H 0.2741 0.1821 0.2648 0.049 Uiso 1 1 calc R . . C16 C 0.4357(3) 0.2463(2) 0.18643(19) 0.0400(6) Uani 1 1 d . . . H20 H 0.5076 0.2589 0.2439 0.048 Uiso 1 1 calc R . . C17 C 0.4692(2) 0.2731(2) 0.0899(2) 0.0372(5) Uani 1 1 d . . . H21 H 0.5639 0.3057 0.0817 0.045 Uiso 1 1 calc R . . C18 C 0.3653(2) 0.25266(19) 0.00534(18) 0.0306(4) Uani 1 1 d . . . H22 H 0.3898 0.2698 -0.0610 0.037 Uiso 1 1 calc R . . C19 C -0.3580(2) 0.30522(17) -0.49146(15) 0.0260(4) Uani 1 1 d . . . O2 O -0.36225(19) 0.33386(16) -0.57267(12) 0.0415(4) Uani 1 1 d . . . C20 C -0.2416(2) 0.16703(16) -0.39590(15) 0.0234(4) Uani 1 1 d . . . O3 O -0.16962(17) 0.10098(13) -0.41381(13) 0.0364(4) Uani 1 1 d . . . C21 C -0.42760(19) 0.33312(16) -0.22470(14) 0.0213(4) Uani 1 1 d . . . C22 C -0.52419(19) 0.33534(16) -0.31354(15) 0.0223(4) Uani 1 1 d . . . C23 C -0.5755(2) 0.21912(17) -0.36815(15) 0.0242(4) Uani 1 1 d . . . C24 C -0.5093(2) 0.14614(16) -0.31437(16) 0.0238(4) Uani 1 1 d . . . C25 C -0.4149(2) 0.21672(16) -0.22670(15) 0.0224(4) Uani 1 1 d . . . C26 C -0.3689(2) 0.43234(17) -0.13605(15) 0.0267(4) Uani 1 1 d . . . H23 H -0.4329 0.4335 -0.0806 0.040 Uiso 1 1 calc R . . H24 H -0.3598 0.5041 -0.1632 0.040 Uiso 1 1 calc R . . H25 H -0.2756 0.4241 -0.1066 0.040 Uiso 1 1 calc R . . C27 C -0.5747(2) 0.43881(18) -0.33989(18) 0.0304(4) Uani 1 1 d . . . H26 H -0.6582 0.4493 -0.3035 0.046 Uiso 1 1 calc R . . H27 H -0.5994 0.4280 -0.4165 0.046 Uiso 1 1 calc R . . H28 H -0.4993 0.5067 -0.3168 0.046 Uiso 1 1 calc R . . C28 C -0.6879(2) 0.1823(2) -0.46105(18) 0.0349(5) Uani 1 1 d . . . H29 H -0.6701 0.1137 -0.5065 0.052 Uiso 1 1 calc R . . H30 H -0.6857 0.2441 -0.5016 0.052 Uiso 1 1 calc R . . H31 H -0.7810 0.1649 -0.4356 0.052 Uiso 1 1 calc R . . C29 C -0.5381(3) 0.01758(18) -0.3396(2) 0.0357(5) Uani 1 1 d . . . H32 H -0.6131 -0.0128 -0.2989 0.054 Uiso 1 1 calc R . . H33 H -0.4518 -0.0098 -0.3210 0.054 Uiso 1 1 calc R . . H34 H -0.5684 -0.0085 -0.4154 0.054 Uiso 1 1 calc R . . C30 C -0.3296(2) 0.17299(19) -0.14578(16) 0.0306(4) Uani 1 1 d . . . H35 H -0.2460 0.2317 -0.1157 0.046 Uiso 1 1 calc R . . H36 H -0.2998 0.1035 -0.1797 0.046 Uiso 1 1 calc R . . H37 H -0.3876 0.1552 -0.0893 0.046 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 0.01740(13) 0.01794(13) 0.01627(13) 0.00152(9) -0.00081(9) 0.00324(10) Si1 0.0183(2) 0.0181(2) 0.0167(2) 0.00416(18) 0.00124(18) 0.00296(18) C1 0.0296(10) 0.0210(9) 0.0307(10) 0.0087(8) 0.0020(8) 0.0045(8) C2 0.0258(10) 0.0327(11) 0.0254(10) 0.0082(8) 0.0072(8) 0.0052(8) O1 0.0190(6) 0.0216(6) 0.0195(6) 0.0054(5) -0.0014(5) 0.0005(5) C3 0.0230(9) 0.0189(8) 0.0167(8) 0.0040(7) -0.0006(7) -0.0016(7) C4 0.0397(12) 0.0197(9) 0.0290(10) 0.0029(8) -0.0061(9) 0.0015(8) C5 0.0229(9) 0.0256(9) 0.0235(9) 0.0057(7) -0.0026(7) 0.0004(7) C6 0.0283(10) 0.0276(10) 0.0243(10) 0.0067(8) 0.0017(8) 0.0099(8) P1 0.0202(2) 0.0265(3) 0.0246(2) 0.00493(19) 0.00063(19) 0.00623(19) C7 0.0230(9) 0.0241(9) 0.0265(10) 0.0050(7) 0.0017(7) 0.0034(7) C8 0.0305(11) 0.0281(10) 0.0321(11) 0.0056(8) -0.0021(9) 0.0058(8) C9 0.0314(11) 0.0253(10) 0.0493(14) 0.0102(9) 0.0050(10) 0.0075(9) C10 0.0385(12) 0.0227(10) 0.0434(13) 0.0012(9) 0.0159(10) 0.0005(9) C11 0.0471(14) 0.0321(11) 0.0283(11) -0.0014(9) 0.0015(10) -0.0006(10) C12 0.0409(12) 0.0312(11) 0.0303(11) 0.0060(9) -0.0041(9) 0.0060(9) C13 0.0256(9) 0.0227(9) 0.0223(9) 0.0014(7) 0.0004(7) 0.0072(7) C14 0.0313(11) 0.0377(12) 0.0273(10) 0.0050(9) 0.0043(8) 0.0096(9) C15 0.0530(15) 0.0501(14) 0.0211(10) 0.0038(9) 0.0012(10) 0.0206(12) C16 0.0427(13) 0.0427(13) 0.0316(12) -0.0050(10) -0.0136(10) 0.0189(11) C17 0.0257(11) 0.0380(12) 0.0461(13) 0.0060(10) -0.0050(9) 0.0068(9) C18 0.0261(10) 0.0348(11) 0.0319(11) 0.0081(9) 0.0003(8) 0.0081(9) C19 0.0256(10) 0.0291(10) 0.0231(10) 0.0010(8) -0.0014(8) 0.0098(8) O2 0.0542(11) 0.0528(10) 0.0221(8) 0.0121(7) -0.0007(7) 0.0197(9) C20 0.0239(9) 0.0207(9) 0.0236(9) 0.0023(7) -0.0017(7) 0.0024(7) O3 0.0368(9) 0.0293(8) 0.0439(9) 0.0006(7) 0.0008(7) 0.0160(7) C21 0.0184(8) 0.0241(9) 0.0206(9) 0.0022(7) 0.0040(7) 0.0031(7) C22 0.0184(8) 0.0247(9) 0.0233(9) 0.0023(7) 0.0021(7) 0.0049(7) C23 0.0170(8) 0.0283(10) 0.0247(9) 0.0015(8) 0.0000(7) 0.0017(7) C24 0.0197(9) 0.0222(9) 0.0280(10) 0.0038(7) 0.0050(7) -0.0002(7) C25 0.0194(9) 0.0259(9) 0.0224(9) 0.0063(7) 0.0047(7) 0.0035(7) C26 0.0265(10) 0.0273(10) 0.0232(9) -0.0024(8) 0.0041(8) 0.0030(8) C27 0.0264(10) 0.0316(11) 0.0346(11) 0.0051(9) 0.0001(8) 0.0116(8) C28 0.0243(10) 0.0406(12) 0.0341(12) -0.0028(9) -0.0075(9) 0.0047(9) C29 0.0360(12) 0.0230(10) 0.0446(13) 0.0052(9) 0.0052(10) -0.0023(9) C30 0.0329(11) 0.0367(11) 0.0257(10) 0.0131(8) 0.0025(8) 0.0097(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C19 1.743(2) . ? Fe1 C20 1.743(2) . ? Fe1 C25 2.0975(19) . ? Fe1 C22 2.1076(19) . ? Fe1 C23 2.1117(19) . ? Fe1 C24 2.1146(19) . ? Fe1 C21 2.1298(18) . ? Fe1 Si1 2.3010(6) . ? Si1 O1 1.6792(13) . ? Si1 C2 1.881(2) . ? Si1 C1 1.882(2) . ? O1 C3 1.378(2) . ? C3 C5 1.332(3) . ? C3 C4 1.498(3) . ? C5 C6 1.501(3) . ? C6 P1 1.861(2) . ? P1 C13 1.834(2) . ? P1 C7 1.843(2) . ? C7 C12 1.395(3) . ? C7 C8 1.397(3) . ? C8 C9 1.392(3) . ? C9 C10 1.377(3) . ? C10 C11 1.385(3) . ? C11 C12 1.386(3) . ? C13 C18 1.389(3) . ? C13 C14 1.391(3) . ? C14 C15 1.398(3) . ? C15 C16 1.380(4) . ? C16 C17 1.384(4) . ? C17 C18 1.384(3) . ? C19 O2 1.157(3) . ? C20 O3 1.156(2) . ? C21 C25 1.429(3) . ? C21 C22 1.430(3) . ? C21 C26 1.503(3) . ? C22 C23 1.440(3) . ? C22 C27 1.502(3) . ? C23 C24 1.419(3) . ? C23 C28 1.505(3) . ? C24 C25 1.441(3) . ? C24 C29 1.501(3) . ? C25 C30 1.505(3) . ? 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 C19 Fe1 C20 96.27(9) . . ? C19 Fe1 C25 162.32(8) . . ? C20 Fe1 C25 97.48(8) . . ? C19 Fe1 C22 97.61(8) . . ? C20 Fe1 C22 160.99(9) . . ? C25 Fe1 C22 66.64(7) . . ? C19 Fe1 C23 96.22(9) . . ? C20 Fe1 C23 125.43(8) . . ? C25 Fe1 C23 66.67(7) . . ? C22 Fe1 C23 39.92(7) . . ? C19 Fe1 C24 127.62(9) . . ? C20 Fe1 C24 94.72(8) . . ? C25 Fe1 C24 40.00(7) . . ? C22 Fe1 C24 66.47(8) . . ? C23 Fe1 C24 39.23(8) . . ? C19 Fe1 C21 130.88(8) . . ? C20 Fe1 C21 131.82(8) . . ? C25 Fe1 C21 39.52(7) . . ? C22 Fe1 C21 39.44(7) . . ? C23 Fe1 C21 66.41(7) . . ? C24 Fe1 C21 66.38(7) . . ? C19 Fe1 Si1 83.96(7) . . ? C20 Fe1 Si1 84.58(6) . . ? C25 Fe1 Si1 108.36(5) . . ? C22 Fe1 Si1 109.74(5) . . ? C23 Fe1 Si1 149.56(6) . . ? C24 Fe1 Si1 148.13(6) . . ? C21 Fe1 Si1 90.47(5) . . ? O1 Si1 C2 105.70(8) . . ? O1 Si1 C1 110.71(8) . . ? C2 Si1 C1 104.63(9) . . ? O1 Si1 Fe1 107.45(5) . . ? C2 Si1 Fe1 115.17(7) . . ? C1 Si1 Fe1 112.97(7) . . ? C3 O1 Si1 129.50(12) . . ? C5 C3 O1 120.31(17) . . ? C5 C3 C4 124.50(17) . . ? O1 C3 C4 115.03(16) . . ? C3 C5 C6 124.98(18) . . ? C5 C6 P1 112.46(14) . . ? C13 P1 C7 99.95(9) . . ? C13 P1 C6 103.14(9) . . ? C7 P1 C6 99.25(9) . . ? C12 C7 C8 118.01(19) . . ? C12 C7 P1 118.36(16) . . ? C8 C7 P1 123.48(16) . . ? C9 C8 C7 120.5(2) . . ? C10 C9 C8 120.7(2) . . ? C9 C10 C11 119.5(2) . . ? C10 C11 C12 120.1(2) . . ? C11 C12 C7 121.2(2) . . ? C18 C13 C14 118.82(19) . . ? C18 C13 P1 124.35(16) . . ? C14 C13 P1 116.76(16) . . ? C13 C14 C15 120.4(2) . . ? C16 C15 C14 120.0(2) . . ? C15 C16 C17 119.7(2) . . ? C18 C17 C16 120.3(2) . . ? C17 C18 C13 120.7(2) . . ? O2 C19 Fe1 178.92(19) . . ? O3 C20 Fe1 178.42(18) . . ? C25 C21 C22 107.77(16) . . ? C25 C21 C26 125.89(17) . . ? C22 C21 C26 125.66(17) . . ? C25 C21 Fe1 69.02(10) . . ? C22 C21 Fe1 69.44(10) . . ? C26 C21 Fe1 134.28(13) . . ? C21 C22 C23 108.04(17) . . ? C21 C22 C27 126.26(17) . . ? C23 C22 C27 125.46(17) . . ? C21 C22 Fe1 71.12(10) . . ? C23 C22 Fe1 70.19(11) . . ? C27 C22 Fe1 128.69(14) . . ? C24 C23 C22 108.07(16) . . ? C24 C23 C28 126.45(19) . . ? C22 C23 C28 125.34(19) . . ? C24 C23 Fe1 70.49(11) . . ? C22 C23 Fe1 69.89(10) . . ? C28 C23 Fe1 128.60(15) . . ? C23 C24 C25 107.96(17) . . ? C23 C24 C29 126.38(18) . . ? C25 C24 C29 125.56(18) . . ? C23 C24 Fe1 70.27(11) . . ? C25 C24 Fe1 69.36(10) . . ? C29 C24 Fe1 128.67(15) . . ? C21 C25 C24 108.09(16) . . ? C21 C25 C30 126.39(18) . . ? C24 C25 C30 125.26(18) . . ? C21 C25 Fe1 71.46(11) . . ? C24 C25 Fe1 70.64(11) . . ? C30 C25 Fe1 128.06(14) . . ? 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 C19 Fe1 Si1 O1 -174.66(8) . . . . ? C20 Fe1 Si1 O1 -77.75(8) . . . . ? C25 Fe1 Si1 O1 18.35(8) . . . . ? C22 Fe1 Si1 O1 89.40(8) . . . . ? C23 Fe1 Si1 O1 93.34(12) . . . . ? C24 Fe1 Si1 O1 12.47(12) . . . . ? C21 Fe1 Si1 O1 54.24(7) . . . . ? C19 Fe1 Si1 C2 -57.20(10) . . . . ? C20 Fe1 Si1 C2 39.71(10) . . . . ? C25 Fe1 Si1 C2 135.81(9) . . . . ? C22 Fe1 Si1 C2 -153.14(9) . . . . ? C23 Fe1 Si1 C2 -149.20(13) . . . . ? C24 Fe1 Si1 C2 129.93(13) . . . . ? C21 Fe1 Si1 C2 171.70(9) . . . . ? C19 Fe1 Si1 C1 62.94(10) . . . . ? C20 Fe1 Si1 C1 159.85(10) . . . . ? C25 Fe1 Si1 C1 -104.05(9) . . . . ? C22 Fe1 Si1 C1 -33.00(9) . . . . ? C23 Fe1 Si1 C1 -29.05(14) . . . . ? C24 Fe1 Si1 C1 -109.93(13) . . . . ? C21 Fe1 Si1 C1 -68.16(9) . . . . ? C2 Si1 O1 C3 49.09(17) . . . . ? C1 Si1 O1 C3 -63.65(17) . . . . ? Fe1 Si1 O1 C3 172.56(14) . . . . ? Si1 O1 C3 C5 -108.63(19) . . . . ? Si1 O1 C3 C4 75.7(2) . . . . ? O1 C3 C5 C6 3.3(3) . . . . ? C4 C3 C5 C6 178.51(19) . . . . ? C3 C5 C6 P1 -92.1(2) . . . . ? C5 C6 P1 C13 -66.48(15) . . . . ? C5 C6 P1 C7 -169.06(14) . . . . ? C13 P1 C7 C12 -163.90(18) . . . . ? C6 P1 C7 C12 -58.69(19) . . . . ? C13 P1 C7 C8 20.7(2) . . . . ? C6 P1 C7 C8 125.87(18) . . . . ? C12 C7 C8 C9 -0.1(3) . . . . ? P1 C7 C8 C9 175.34(17) . . . . ? C7 C8 C9 C10 1.0(3) . . . . ? C8 C9 C10 C11 -0.7(3) . . . . ? C9 C10 C11 C12 -0.3(4) . . . . ? C10 C11 C12 C7 1.2(4) . . . . ? C8 C7 C12 C11 -1.0(3) . . . . ? P1 C7 C12 C11 -176.65(18) . . . . ? C7 P1 C13 C18 77.64(19) . . . . ? C6 P1 C13 C18 -24.4(2) . . . . ? C7 P1 C13 C14 -99.35(17) . . . . ? C6 P1 C13 C14 158.61(16) . . . . ? C18 C13 C14 C15 -1.9(3) . . . . ? P1 C13 C14 C15 175.29(18) . . . . ? C13 C14 C15 C16 2.0(4) . . . . ? C14 C15 C16 C17 -0.4(4) . . . . ? C15 C16 C17 C18 -1.3(4) . . . . ? C16 C17 C18 C13 1.4(3) . . . . ? C14 C13 C18 C17 0.2(3) . . . . ? P1 C13 C18 C17 -176.74(17) . . . . ? C20 Fe1 C19 O2 173(12) . . . . ? C25 Fe1 C19 O2 32(12) . . . . ? C22 Fe1 C19 O2 6(12) . . . . ? C23 Fe1 C19 O2 46(12) . . . . ? C24 Fe1 C19 O2 72(12) . . . . ? C21 Fe1 C19 O2 -18(12) . . . . ? Si1 Fe1 C19 O2 -103(12) . . . . ? C19 Fe1 C20 O3 -116(7) . . . . ? C25 Fe1 C20 O3 53(7) . . . . ? C22 Fe1 C20 O3 20(7) . . . . ? C23 Fe1 C20 O3 -14(7) . . . . ? C24 Fe1 C20 O3 12(7) . . . . ? C21 Fe1 C20 O3 75(7) . . . . ? Si1 Fe1 C20 O3 160(7) . . . . ? C19 Fe1 C21 C25 158.58(12) . . . . ? C20 Fe1 C21 C25 -35.88(15) . . . . ? C22 Fe1 C21 C25 119.54(16) . . . . ? C23 Fe1 C21 C25 81.39(12) . . . . ? C24 Fe1 C21 C25 38.40(11) . . . . ? Si1 Fe1 C21 C25 -119.02(10) . . . . ? C19 Fe1 C21 C22 39.04(16) . . . . ? C20 Fe1 C21 C22 -155.42(12) . . . . ? C25 Fe1 C21 C22 -119.54(16) . . . . ? C23 Fe1 C21 C22 -38.15(11) . . . . ? C24 Fe1 C21 C22 -81.13(12) . . . . ? Si1 Fe1 C21 C22 121.44(10) . . . . ? C19 Fe1 C21 C26 -81.2(2) . . . . ? C20 Fe1 C21 C26 84.3(2) . . . . ? C25 Fe1 C21 C26 120.2(2) . . . . ? C22 Fe1 C21 C26 -120.3(2) . . . . ? C23 Fe1 C21 C26 -158.4(2) . . . . ? C24 Fe1 C21 C26 158.6(2) . . . . ? Si1 Fe1 C21 C26 1.18(19) . . . . ? C25 C21 C22 C23 2.2(2) . . . . ? C26 C21 C22 C23 -168.78(18) . . . . ? Fe1 C21 C22 C23 60.79(13) . . . . ? C25 C21 C22 C27 176.81(19) . . . . ? C26 C21 C22 C27 5.8(3) . . . . ? Fe1 C21 C22 C27 -124.6(2) . . . . ? C25 C21 C22 Fe1 -58.55(13) . . . . ? C26 C21 C22 Fe1 130.43(19) . . . . ? C19 Fe1 C22 C21 -151.29(12) . . . . ? C20 Fe1 C22 C21 72.2(3) . . . . ? C25 Fe1 C22 C21 37.09(11) . . . . ? C23 Fe1 C22 C21 118.10(16) . . . . ? C24 Fe1 C22 C21 80.87(12) . . . . ? Si1 Fe1 C22 C21 -65.01(11) . . . . ? C19 Fe1 C22 C23 90.61(13) . . . . ? C20 Fe1 C22 C23 -45.9(3) . . . . ? C25 Fe1 C22 C23 -81.02(12) . . . . ? C24 Fe1 C22 C23 -37.24(11) . . . . ? C21 Fe1 C22 C23 -118.10(16) . . . . ? Si1 Fe1 C22 C23 176.89(10) . . . . ? C19 Fe1 C22 C27 -29.50(19) . . . . ? C20 Fe1 C22 C27 -166.1(2) . . . . ? C25 Fe1 C22 C27 158.9(2) . . . . ? C23 Fe1 C22 C27 -120.1(2) . . . . ? C24 Fe1 C22 C27 -157.3(2) . . . . ? C21 Fe1 C22 C27 121.8(2) . . . . ? Si1 Fe1 C22 C27 56.78(18) . . . . ? C21 C22 C23 C24 -0.9(2) . . . . ? C27 C22 C23 C24 -175.58(19) . . . . ? Fe1 C22 C23 C24 60.43(13) . . . . ? C21 C22 C23 C28 174.93(19) . . . . ? C27 C22 C23 C28 0.3(3) . . . . ? Fe1 C22 C23 C28 -123.7(2) . . . . ? C21 C22 C23 Fe1 -61.38(13) . . . . ? C27 C22 C23 Fe1 124.0(2) . . . . ? C19 Fe1 C23 C24 146.87(12) . . . . ? C20 Fe1 C23 C24 44.61(15) . . . . ? C25 Fe1 C23 C24 -37.75(11) . . . . ? C22 Fe1 C23 C24 -118.69(16) . . . . ? C21 Fe1 C23 C24 -80.99(12) . . . . ? Si1 Fe1 C23 C24 -124.48(12) . . . . ? C19 Fe1 C23 C22 -94.44(12) . . . . ? C20 Fe1 C23 C22 163.30(12) . . . . ? C25 Fe1 C23 C22 80.95(12) . . . . ? C24 Fe1 C23 C22 118.69(16) . . . . ? C21 Fe1 C23 C22 37.70(11) . . . . ? Si1 Fe1 C23 C22 -5.79(18) . . . . ? C19 Fe1 C23 C28 25.3(2) . . . . ? C20 Fe1 C23 C28 -77.0(2) . . . . ? C25 Fe1 C23 C28 -159.3(2) . . . . ? C22 Fe1 C23 C28 119.7(2) . . . . ? C24 Fe1 C23 C28 -121.6(2) . . . . ? C21 Fe1 C23 C28 157.4(2) . . . . ? Si1 Fe1 C23 C28 113.93(18) . . . . ? C22 C23 C24 C25 -0.7(2) . . . . ? C28 C23 C24 C25 -176.52(19) . . . . ? Fe1 C23 C24 C25 59.34(13) . . . . ? C22 C23 C24 C29 175.88(19) . . . . ? C28 C23 C24 C29 0.1(3) . . . . ? Fe1 C23 C24 C29 -124.1(2) . . . . ? C22 C23 C24 Fe1 -60.05(13) . . . . ? C28 C23 C24 Fe1 124.1(2) . . . . ? C19 Fe1 C24 C23 -43.31(15) . . . . ? C20 Fe1 C24 C23 -144.96(12) . . . . ? C25 Fe1 C24 C23 119.02(16) . . . . ? C22 Fe1 C24 C23 37.88(11) . . . . ? C21 Fe1 C24 C23 81.08(12) . . . . ? Si1 Fe1 C24 C23 127.73(11) . . . . ? C19 Fe1 C24 C25 -162.33(12) . . . . ? C20 Fe1 C24 C25 96.02(12) . . . . ? C22 Fe1 C24 C25 -81.15(12) . . . . ? C23 Fe1 C24 C25 -119.02(16) . . . . ? C21 Fe1 C24 C25 -37.94(11) . . . . ? Si1 Fe1 C24 C25 8.70(17) . . . . ? C19 Fe1 C24 C29 78.0(2) . . . . ? C20 Fe1 C24 C29 -23.6(2) . . . . ? C25 Fe1 C24 C29 -119.6(2) . . . . ? C22 Fe1 C24 C29 159.2(2) . . . . ? C23 Fe1 C24 C29 121.3(2) . . . . ? C21 Fe1 C24 C29 -157.6(2) . . . . ? Si1 Fe1 C24 C29 -110.93(18) . . . . ? C22 C21 C25 C24 -2.7(2) . . . . ? C26 C21 C25 C24 168.32(18) . . . . ? Fe1 C21 C25 C24 -61.48(13) . . . . ? C22 C21 C25 C30 -177.09(18) . . . . ? C26 C21 C25 C30 -6.1(3) . . . . ? Fe1 C21 C25 C30 124.1(2) . . . . ? C22 C21 C25 Fe1 58.81(13) . . . . ? C26 C21 C25 Fe1 -130.20(19) . . . . ? C23 C24 C25 C21 2.1(2) . . . . ? C29 C24 C25 C21 -174.52(19) . . . . ? Fe1 C24 C25 C21 62.01(13) . . . . ? C23 C24 C25 C30 176.59(18) . . . . ? C29 C24 C25 C30 0.0(3) . . . . ? Fe1 C24 C25 C30 -123.49(19) . . . . ? C23 C24 C25 Fe1 -59.91(13) . . . . ? C29 C24 C25 Fe1 123.5(2) . . . . ? C19 Fe1 C25 C21 -65.4(3) . . . . ? C20 Fe1 C25 C21 153.86(11) . . . . ? C22 Fe1 C25 C21 -37.02(11) . . . . ? C23 Fe1 C25 C21 -80.67(12) . . . . ? C24 Fe1 C25 C21 -117.71(16) . . . . ? Si1 Fe1 C25 C21 67.12(11) . . . . ? C19 Fe1 C25 C24 52.3(3) . . . . ? C20 Fe1 C25 C24 -88.43(12) . . . . ? C22 Fe1 C25 C24 80.69(12) . . . . ? C23 Fe1 C25 C24 37.03(11) . . . . ? C21 Fe1 C25 C24 117.71(16) . . . . ? Si1 Fe1 C25 C24 -175.17(10) . . . . ? C19 Fe1 C25 C30 172.4(2) . . . . ? C20 Fe1 C25 C30 31.70(19) . . . . ? C22 Fe1 C25 C30 -159.2(2) . . . . ? C23 Fe1 C25 C30 157.2(2) . . . . ? C24 Fe1 C25 C30 120.1(2) . . . . ? C21 Fe1 C25 C30 -122.2(2) . . . . ? Si1 Fe1 C25 C30 -55.04(18) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.691 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.079 data_complex5 _database_code_depnum_ccdc_archive 'CCDC 250455' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H37 Fe O2 P Si' _chemical_formula_weight 532.50 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' O O 0.0106 0.0060 '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 'P 21/n' _symmetry_int_tables_number 14 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 9.1251(16) _cell_length_b 15.172(2) _cell_length_c 19.699(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.714(6) _cell_angle_gamma 90.00 _cell_volume 2702.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17810 _cell_measurement_theta_min 4.96 _cell_measurement_theta_max 54.91 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.686 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8208 _exptl_absorpt_correction_T_max 0.9346 _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 25257 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.0402 _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 23 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6163 _reflns_number_gt 5212 _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^)+(0.0226P)^2^+2.8102P] 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 6163 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.0925 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _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 0.27528(3) 0.30565(2) 0.908369(16) 0.01965(9) Uani 1 1 d . . . Si1 Si 0.29319(7) 0.15613(4) 0.92489(3) 0.02511(15) Uani 1 1 d . . . P1 P 0.15656(7) 0.29328(4) 0.80437(3) 0.02181(13) Uani 1 1 d . . . C1 C 0.1177(3) 0.29660(15) 0.94756(11) 0.0236(5) Uani 1 1 d . . . O1 O 0.0197(2) 0.29721(12) 0.97963(9) 0.0365(4) Uani 1 1 d . . . C2 C 0.4280(3) 0.09050(17) 0.88036(15) 0.0387(6) Uani 1 1 d . . . H1 H 0.4554 0.0366 0.9064 0.058 Uiso 1 1 calc R . . H2 H 0.5168 0.1259 0.8775 0.058 Uiso 1 1 calc R . . H3 H 0.3818 0.0750 0.8341 0.058 Uiso 1 1 calc R . . C3 C 0.3274(3) 0.12274(19) 1.01824(14) 0.0408(7) Uani 1 1 d . . . H4 H 0.2530 0.1502 1.0429 0.061 Uiso 1 1 calc R . . H5 H 0.4262 0.1422 1.0383 0.061 Uiso 1 1 calc R . . H6 H 0.3208 0.0585 1.0219 0.061 Uiso 1 1 calc R . . O2 O 0.13801(18) 0.09540(11) 0.90000(10) 0.0359(4) Uani 1 1 d . . . C4 C -0.0055(3) 0.12096(15) 0.88630(12) 0.0253(5) Uani 1 1 d . . . C5 C -0.1013(3) 0.08815(19) 0.93696(14) 0.0407(6) Uani 1 1 d . . . H7 H -0.2050 0.1015 0.9204 0.061 Uiso 1 1 calc R . . H8 H -0.0727 0.1172 0.9812 0.061 Uiso 1 1 calc R . . H9 H -0.0889 0.0243 0.9425 0.061 Uiso 1 1 calc R . . C6 C -0.0525(3) 0.16727(15) 0.83063(12) 0.0281(5) Uani 1 1 d . . . H10 H -0.1530 0.1854 0.8223 0.034 Uiso 1 1 calc R . . C7 C 0.0502(3) 0.19122(17) 0.78083(12) 0.0329(6) Uani 1 1 d . . . H11 H -0.0076 0.1991 0.7350 0.039 Uiso 1 1 calc R . . H12 H 0.1203 0.1420 0.7778 0.039 Uiso 1 1 calc R . . C8 C 0.2621(3) 0.29921(16) 0.73129(11) 0.0283(5) Uani 1 1 d . . . C9 C 0.3497(3) 0.22754(18) 0.71839(14) 0.0383(6) Uani 1 1 d . . . H13 H 0.3512 0.1767 0.7466 0.046 Uiso 1 1 calc R . . C10 C 0.4345(4) 0.2289(2) 0.66517(15) 0.0459(7) Uani 1 1 d . . . H14 H 0.4923 0.1790 0.6567 0.055 Uiso 1 1 calc R . . C11 C 0.4352(4) 0.3033(2) 0.62418(14) 0.0446(7) Uani 1 1 d . . . H15 H 0.4951 0.3050 0.5883 0.053 Uiso 1 1 calc R . . C12 C 0.3486(3) 0.37472(19) 0.63587(14) 0.0399(7) Uani 1 1 d . . . H16 H 0.3482 0.4255 0.6077 0.048 Uiso 1 1 calc R . . C13 C 0.2618(3) 0.37280(17) 0.68864(13) 0.0340(6) Uani 1 1 d . . . H17 H 0.2016 0.4221 0.6958 0.041 Uiso 1 1 calc R . . C14 C 0.0090(3) 0.37549(16) 0.78242(12) 0.0258(5) Uani 1 1 d . . . C15 C -0.0790(3) 0.3764(2) 0.71843(13) 0.0397(7) Uani 1 1 d . . . H18 H -0.0607 0.3350 0.6844 0.048 Uiso 1 1 calc R . . C16 C -0.1920(3) 0.4369(2) 0.70441(15) 0.0511(8) Uani 1 1 d . . . H19 H -0.2507 0.4367 0.6608 0.061 Uiso 1 1 calc R . . C17 C -0.2204(3) 0.4972(2) 0.75280(16) 0.0470(8) Uani 1 1 d . . . H20 H -0.2984 0.5386 0.7427 0.056 Uiso 1 1 calc R . . C18 C -0.1353(3) 0.49764(18) 0.81617(15) 0.0383(6) Uani 1 1 d . . . H21 H -0.1543 0.5395 0.8498 0.046 Uiso 1 1 calc R . . C19 C -0.0213(3) 0.43658(16) 0.83092(13) 0.0293(5) Uani 1 1 d . . . H22 H 0.0363 0.4368 0.8748 0.035 Uiso 1 1 calc R . . C20 C 0.3318(3) 0.43111(16) 0.95375(13) 0.0312(6) Uani 1 1 d . . . C21 C 0.3990(3) 0.36133(17) 0.99584(13) 0.0317(6) Uani 1 1 d . . . C22 C 0.4972(3) 0.31607(17) 0.95795(14) 0.0338(6) Uani 1 1 d . . . C23 C 0.4862(3) 0.35431(17) 0.89134(14) 0.0334(6) Uani 1 1 d . . . C24 C 0.3840(3) 0.42670(16) 0.88953(13) 0.0313(6) Uani 1 1 d . . . C25 C 0.2349(3) 0.50107(18) 0.97842(16) 0.0450(7) Uani 1 1 d . . . H23 H 0.2945 0.5392 1.0115 0.067 Uiso 1 1 calc R . . H24 H 0.1565 0.4732 1.0004 0.067 Uiso 1 1 calc R . . H25 H 0.1904 0.5365 0.9394 0.067 Uiso 1 1 calc R . . C26 C 0.3796(4) 0.3474(2) 1.07016(14) 0.0510(8) Uani 1 1 d . . . H26 H 0.3954 0.4034 1.0950 0.076 Uiso 1 1 calc R . . H27 H 0.4516 0.3039 1.0906 0.076 Uiso 1 1 calc R . . H28 H 0.2792 0.3261 1.0730 0.076 Uiso 1 1 calc R . . C27 C 0.6199(3) 0.2542(2) 0.98674(18) 0.0502(8) Uani 1 1 d . . . H29 H 0.6099 0.2404 1.0345 0.075 Uiso 1 1 calc R . . H30 H 0.7158 0.2824 0.9846 0.075 Uiso 1 1 calc R . . H31 H 0.6135 0.1997 0.9598 0.075 Uiso 1 1 calc R . . C28 C 0.5840(3) 0.3318(2) 0.83810(18) 0.0512(8) Uani 1 1 d . . . H32 H 0.6832 0.3557 0.8520 0.077 Uiso 1 1 calc R . . H33 H 0.5424 0.3573 0.7940 0.077 Uiso 1 1 calc R . . H34 H 0.5899 0.2676 0.8337 0.077 Uiso 1 1 calc R . . C29 C 0.3548(4) 0.49462(18) 0.83317(15) 0.0460(8) Uani 1 1 d . . . H35 H 0.2494 0.4945 0.8151 0.069 Uiso 1 1 calc R . . H36 H 0.4130 0.4803 0.7963 0.069 Uiso 1 1 calc R . . H37 H 0.3830 0.5531 0.8516 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01629(15) 0.01802(16) 0.02384(16) 0.00094(13) -0.00026(11) -0.00265(12) Si1 0.0175(3) 0.0203(3) 0.0362(3) 0.0055(3) -0.0011(2) -0.0006(2) P1 0.0249(3) 0.0196(3) 0.0208(3) 0.0001(2) 0.0027(2) -0.0011(2) C1 0.0238(11) 0.0231(11) 0.0228(10) -0.0011(9) -0.0010(9) -0.0028(9) O1 0.0338(10) 0.0411(11) 0.0372(9) -0.0038(8) 0.0141(8) -0.0037(8) C2 0.0277(14) 0.0275(14) 0.0606(18) -0.0015(12) 0.0045(12) 0.0050(11) C3 0.0357(15) 0.0385(15) 0.0460(16) 0.0178(13) -0.0023(12) -0.0029(12) O2 0.0204(9) 0.0223(9) 0.0624(12) 0.0068(8) -0.0042(8) -0.0030(7) C4 0.0184(11) 0.0201(11) 0.0364(13) -0.0030(9) 0.0005(9) -0.0059(9) C5 0.0381(15) 0.0404(16) 0.0447(15) 0.0005(13) 0.0102(12) -0.0104(12) C6 0.0224(12) 0.0236(12) 0.0358(13) -0.0036(10) -0.0051(10) -0.0050(9) C7 0.0447(15) 0.0275(13) 0.0249(11) -0.0052(10) -0.0009(10) -0.0079(11) C8 0.0346(13) 0.0279(12) 0.0233(11) 0.0004(10) 0.0075(10) 0.0005(10) C9 0.0522(18) 0.0294(14) 0.0360(14) 0.0036(11) 0.0152(12) 0.0069(12) C10 0.0568(19) 0.0398(16) 0.0457(16) 0.0002(13) 0.0232(14) 0.0138(14) C11 0.0512(18) 0.0519(18) 0.0349(14) 0.0022(13) 0.0220(13) 0.0043(15) C12 0.0481(17) 0.0403(16) 0.0341(14) 0.0102(12) 0.0158(12) 0.0015(13) C13 0.0385(15) 0.0310(13) 0.0343(13) 0.0040(11) 0.0111(11) 0.0044(11) C14 0.0224(12) 0.0280(12) 0.0267(11) 0.0046(10) 0.0018(9) -0.0027(9) C15 0.0370(15) 0.0552(18) 0.0257(12) 0.0070(12) 0.0001(11) 0.0041(13) C16 0.0328(16) 0.080(2) 0.0376(15) 0.0238(16) -0.0045(12) 0.0064(15) C17 0.0294(15) 0.0522(19) 0.0594(18) 0.0315(16) 0.0063(13) 0.0103(13) C18 0.0345(15) 0.0284(13) 0.0529(16) 0.0074(12) 0.0090(12) 0.0052(11) C19 0.0268(12) 0.0236(12) 0.0361(13) 0.0028(10) -0.0007(10) 0.0005(10) C20 0.0257(13) 0.0241(12) 0.0407(14) -0.0066(10) -0.0073(10) -0.0091(10) C21 0.0270(13) 0.0301(13) 0.0345(13) -0.0026(11) -0.0085(10) -0.0077(10) C22 0.0208(12) 0.0267(13) 0.0503(15) 0.0042(12) -0.0082(10) -0.0076(10) C23 0.0210(12) 0.0300(13) 0.0483(15) 0.0015(12) 0.0018(10) -0.0108(10) C24 0.0263(12) 0.0222(12) 0.0428(14) 0.0049(10) -0.0051(10) -0.0111(10) C25 0.0461(17) 0.0290(14) 0.0553(18) -0.0170(13) -0.0093(14) 0.0003(12) C26 0.062(2) 0.0548(19) 0.0310(14) -0.0061(13) -0.0134(13) -0.0124(16) C27 0.0223(14) 0.0406(17) 0.081(2) 0.0082(15) -0.0171(14) 0.0003(12) C28 0.0303(15) 0.0531(19) 0.074(2) -0.0007(16) 0.0226(14) -0.0111(13) C29 0.0515(18) 0.0307(15) 0.0518(17) 0.0135(13) -0.0078(14) -0.0187(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 1.727(2) . ? Fe1 C21 2.106(2) . ? Fe1 C23 2.130(2) . ? Fe1 C22 2.133(2) . ? Fe1 C20 2.137(2) . ? Fe1 C24 2.144(2) . ? Fe1 P1 2.1931(7) . ? Fe1 Si1 2.2944(8) . ? Si1 O2 1.7053(18) . ? Si1 C2 1.888(3) . ? Si1 C3 1.893(3) . ? P1 C8 1.839(2) . ? P1 C14 1.843(2) . ? P1 C7 1.853(3) . ? C1 O1 1.162(3) . ? O2 C4 1.358(3) . ? C4 C6 1.324(3) . ? C4 C5 1.497(3) . ? C6 C7 1.490(4) . ? C8 C9 1.393(4) . ? C8 C13 1.397(3) . ? C9 C10 1.385(4) . ? C10 C11 1.388(4) . ? C11 C12 1.379(4) . ? C12 C13 1.389(4) . ? C14 C19 1.386(3) . ? C14 C15 1.401(3) . ? C15 C16 1.380(4) . ? C16 C17 1.371(5) . ? C17 C18 1.379(4) . ? C18 C19 1.394(4) . ? C20 C24 1.412(4) . ? C20 C21 1.431(4) . ? C20 C25 1.504(4) . ? C21 C22 1.418(4) . ? C21 C26 1.513(4) . ? C22 C23 1.426(4) . ? C22 C27 1.512(4) . ? C23 C24 1.438(4) . ? C23 C28 1.505(4) . ? C24 C29 1.512(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C21 93.05(10) . . ? C1 Fe1 C23 157.31(11) . . ? C21 Fe1 C23 66.00(10) . . ? C1 Fe1 C22 126.71(11) . . ? C21 Fe1 C22 39.09(11) . . ? C23 Fe1 C22 39.08(10) . . ? C1 Fe1 C20 93.01(11) . . ? C21 Fe1 C20 39.41(10) . . ? C23 Fe1 C20 65.45(10) . . ? C22 Fe1 C20 65.25(10) . . ? C1 Fe1 C24 125.33(11) . . ? C21 Fe1 C24 65.68(10) . . ? C23 Fe1 C24 39.33(10) . . ? C22 Fe1 C24 65.32(10) . . ? C20 Fe1 C24 38.53(10) . . ? C1 Fe1 P1 94.26(7) . . ? C21 Fe1 P1 160.38(7) . . ? C23 Fe1 P1 103.07(8) . . ? C22 Fe1 P1 138.91(8) . . ? C20 Fe1 P1 121.89(7) . . ? C24 Fe1 P1 95.38(7) . . ? C1 Fe1 Si1 84.59(8) . . ? C21 Fe1 Si1 105.09(7) . . ? C23 Fe1 Si1 108.44(8) . . ? C22 Fe1 Si1 87.89(7) . . ? C20 Fe1 Si1 144.38(7) . . ? C24 Fe1 Si1 147.76(8) . . ? P1 Fe1 Si1 93.72(3) . . ? O2 Si1 C2 98.58(11) . . ? O2 Si1 C3 99.04(11) . . ? C2 Si1 C3 106.10(13) . . ? O2 Si1 Fe1 116.92(7) . . ? C2 Si1 Fe1 119.61(9) . . ? C3 Si1 Fe1 113.69(10) . . ? C8 P1 C14 103.07(11) . . ? C8 P1 C7 99.02(12) . . ? C14 P1 C7 99.51(12) . . ? C8 P1 Fe1 118.82(8) . . ? C14 P1 Fe1 114.51(8) . . ? C7 P1 Fe1 118.79(8) . . ? O1 C1 Fe1 172.0(2) . . ? C4 O2 Si1 130.12(15) . . ? C6 C4 O2 120.8(2) . . ? C6 C4 C5 125.1(2) . . ? O2 C4 C5 114.0(2) . . ? C4 C6 C7 120.8(2) . . ? C6 C7 P1 113.19(17) . . ? C9 C8 C13 118.0(2) . . ? C9 C8 P1 118.58(19) . . ? C13 C8 P1 123.42(19) . . ? C10 C9 C8 121.3(3) . . ? C9 C10 C11 120.0(3) . . ? C12 C11 C10 119.6(3) . . ? C11 C12 C13 120.4(3) . . ? C12 C13 C8 120.8(2) . . ? C19 C14 C15 118.1(2) . . ? C19 C14 P1 119.87(17) . . ? C15 C14 P1 122.0(2) . . ? C16 C15 C14 120.6(3) . . ? C17 C16 C15 120.7(3) . . ? C16 C17 C18 119.8(3) . . ? C17 C18 C19 120.0(3) . . ? C14 C19 C18 120.9(2) . . ? C24 C20 C21 108.3(2) . . ? C24 C20 C25 127.4(2) . . ? C21 C20 C25 124.1(3) . . ? C24 C20 Fe1 71.00(14) . . ? C21 C20 Fe1 69.14(14) . . ? C25 C20 Fe1 130.15(18) . . ? C22 C21 C20 107.8(2) . . ? C22 C21 C26 127.3(3) . . ? C20 C21 C26 124.5(3) . . ? C22 C21 Fe1 71.48(14) . . ? C20 C21 Fe1 71.45(13) . . ? C26 C21 Fe1 128.05(19) . . ? C21 C22 C23 108.4(2) . . ? C21 C22 C27 126.3(3) . . ? C23 C22 C27 123.7(3) . . ? C21 C22 Fe1 69.43(14) . . ? C23 C22 Fe1 70.34(14) . . ? C27 C22 Fe1 137.35(19) . . ? C22 C23 C24 107.4(2) . . ? C22 C23 C28 125.0(3) . . ? C24 C23 C28 126.8(3) . . ? C22 C23 Fe1 70.57(14) . . ? C24 C23 Fe1 70.85(14) . . ? C28 C23 Fe1 131.60(19) . . ? C20 C24 C23 108.0(2) . . ? C20 C24 C29 125.3(3) . . ? C23 C24 C29 126.1(3) . . ? C20 C24 Fe1 70.47(14) . . ? C23 C24 Fe1 69.83(13) . . ? C29 C24 Fe1 132.13(18) . . ? 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 C1 Fe1 Si1 O2 49.11(11) . . . . ? C21 Fe1 Si1 O2 140.82(11) . . . . ? C23 Fe1 Si1 O2 -149.92(11) . . . . ? C22 Fe1 Si1 O2 176.29(12) . . . . ? C20 Fe1 Si1 O2 136.73(15) . . . . ? C24 Fe1 Si1 O2 -151.02(15) . . . . ? P1 Fe1 Si1 O2 -44.82(9) . . . . ? C1 Fe1 Si1 C2 167.87(13) . . . . ? C21 Fe1 Si1 C2 -100.43(13) . . . . ? C23 Fe1 Si1 C2 -31.17(13) . . . . ? C22 Fe1 Si1 C2 -64.95(13) . . . . ? C20 Fe1 Si1 C2 -104.52(16) . . . . ? C24 Fe1 Si1 C2 -32.27(18) . . . . ? P1 Fe1 Si1 C2 73.93(11) . . . . ? C1 Fe1 Si1 C3 -65.43(12) . . . . ? C21 Fe1 Si1 C3 26.28(13) . . . . ? C23 Fe1 Si1 C3 95.54(13) . . . . ? C22 Fe1 Si1 C3 61.75(13) . . . . ? C20 Fe1 Si1 C3 22.19(17) . . . . ? C24 Fe1 Si1 C3 94.44(17) . . . . ? P1 Fe1 Si1 C3 -159.36(10) . . . . ? C1 Fe1 P1 C8 179.03(12) . . . . ? C21 Fe1 P1 C8 67.5(3) . . . . ? C23 Fe1 P1 C8 13.78(12) . . . . ? C22 Fe1 P1 C8 -5.08(15) . . . . ? C20 Fe1 P1 C8 82.81(13) . . . . ? C24 Fe1 P1 C8 52.91(12) . . . . ? Si1 Fe1 P1 C8 -96.12(9) . . . . ? C1 Fe1 P1 C14 56.72(11) . . . . ? C21 Fe1 P1 C14 -54.9(3) . . . . ? C23 Fe1 P1 C14 -108.53(11) . . . . ? C22 Fe1 P1 C14 -127.39(13) . . . . ? C20 Fe1 P1 C14 -39.50(12) . . . . ? C24 Fe1 P1 C14 -69.40(11) . . . . ? Si1 Fe1 P1 C14 141.56(9) . . . . ? C1 Fe1 P1 C7 -60.53(13) . . . . ? C21 Fe1 P1 C7 -172.1(2) . . . . ? C23 Fe1 P1 C7 134.22(13) . . . . ? C22 Fe1 P1 C7 115.36(15) . . . . ? C20 Fe1 P1 C7 -156.75(13) . . . . ? C24 Fe1 P1 C7 173.35(13) . . . . ? Si1 Fe1 P1 C7 24.31(11) . . . . ? C21 Fe1 C1 O1 15.4(16) . . . . ? C23 Fe1 C1 O1 -6.4(17) . . . . ? C22 Fe1 C1 O1 37.0(16) . . . . ? C20 Fe1 C1 O1 -24.1(16) . . . . ? C24 Fe1 C1 O1 -46.7(16) . . . . ? P1 Fe1 C1 O1 -146.4(15) . . . . ? Si1 Fe1 C1 O1 120.2(16) . . . . ? C2 Si1 O2 C4 -146.9(2) . . . . ? C3 Si1 O2 C4 105.1(2) . . . . ? Fe1 Si1 O2 C4 -17.3(3) . . . . ? Si1 O2 C4 C6 70.9(3) . . . . ? Si1 O2 C4 C5 -112.1(2) . . . . ? O2 C4 C6 C7 1.1(3) . . . . ? C5 C4 C6 C7 -175.6(2) . . . . ? C4 C6 C7 P1 -85.2(3) . . . . ? C8 P1 C7 C6 -179.00(19) . . . . ? C14 P1 C7 C6 -74.0(2) . . . . ? Fe1 P1 C7 C6 50.9(2) . . . . ? C14 P1 C8 C9 -158.5(2) . . . . ? C7 P1 C8 C9 -56.5(2) . . . . ? Fe1 P1 C8 C9 73.6(2) . . . . ? C14 P1 C8 C13 22.9(2) . . . . ? C7 P1 C8 C13 124.9(2) . . . . ? Fe1 P1 C8 C13 -105.0(2) . . . . ? C13 C8 C9 C10 0.3(4) . . . . ? P1 C8 C9 C10 -178.4(2) . . . . ? C8 C9 C10 C11 1.0(5) . . . . ? C9 C10 C11 C12 -1.4(5) . . . . ? C10 C11 C12 C13 0.5(5) . . . . ? C11 C12 C13 C8 0.8(4) . . . . ? C9 C8 C13 C12 -1.2(4) . . . . ? P1 C8 C13 C12 177.4(2) . . . . ? C8 P1 C14 C19 -132.3(2) . . . . ? C7 P1 C14 C19 126.0(2) . . . . ? Fe1 P1 C14 C19 -1.8(2) . . . . ? C8 P1 C14 C15 50.3(2) . . . . ? C7 P1 C14 C15 -51.3(2) . . . . ? Fe1 P1 C14 C15 -179.16(19) . . . . ? C19 C14 C15 C16 0.3(4) . . . . ? P1 C14 C15 C16 177.7(2) . . . . ? C14 C15 C16 C17 0.0(5) . . . . ? C15 C16 C17 C18 0.0(5) . . . . ? C16 C17 C18 C19 -0.3(4) . . . . ? C15 C14 C19 C18 -0.6(4) . . . . ? P1 C14 C19 C18 -178.0(2) . . . . ? C17 C18 C19 C14 0.6(4) . . . . ? C1 Fe1 C20 C24 -149.74(15) . . . . ? C21 Fe1 C20 C24 119.1(2) . . . . ? C23 Fe1 C20 C24 37.66(15) . . . . ? C22 Fe1 C20 C24 80.85(16) . . . . ? P1 Fe1 C20 C24 -52.83(16) . . . . ? Si1 Fe1 C20 C24 125.35(15) . . . . ? C1 Fe1 C20 C21 91.14(17) . . . . ? C23 Fe1 C20 C21 -81.46(17) . . . . ? C22 Fe1 C20 C21 -38.27(16) . . . . ? C24 Fe1 C20 C21 -119.1(2) . . . . ? P1 Fe1 C20 C21 -171.95(13) . . . . ? Si1 Fe1 C20 C21 6.2(2) . . . . ? C1 Fe1 C20 C25 -26.4(3) . . . . ? C21 Fe1 C20 C25 -117.5(3) . . . . ? C23 Fe1 C20 C25 161.0(3) . . . . ? C22 Fe1 C20 C25 -155.8(3) . . . . ? C24 Fe1 C20 C25 123.3(3) . . . . ? P1 Fe1 C20 C25 70.5(3) . . . . ? Si1 Fe1 C20 C25 -111.3(2) . . . . ? C24 C20 C21 C22 2.2(3) . . . . ? C25 C20 C21 C22 -172.2(2) . . . . ? Fe1 C20 C21 C22 62.65(16) . . . . ? C24 C20 C21 C26 175.6(2) . . . . ? C25 C20 C21 C26 1.2(4) . . . . ? Fe1 C20 C21 C26 -123.9(3) . . . . ? C24 C20 C21 Fe1 -60.46(16) . . . . ? C25 C20 C21 Fe1 125.1(2) . . . . ? C1 Fe1 C21 C22 152.10(16) . . . . ? C23 Fe1 C21 C22 -36.92(15) . . . . ? C20 Fe1 C21 C22 -116.9(2) . . . . ? C24 Fe1 C21 C22 -80.20(16) . . . . ? P1 Fe1 C21 C22 -96.1(3) . . . . ? Si1 Fe1 C21 C22 66.89(15) . . . . ? C1 Fe1 C21 C20 -91.03(17) . . . . ? C23 Fe1 C21 C20 79.95(16) . . . . ? C22 Fe1 C21 C20 116.9(2) . . . . ? C24 Fe1 C21 C20 36.67(15) . . . . ? P1 Fe1 C21 C20 20.7(3) . . . . ? Si1 Fe1 C21 C20 -176.25(14) . . . . ? C1 Fe1 C21 C26 28.8(3) . . . . ? C23 Fe1 C21 C26 -160.3(3) . . . . ? C22 Fe1 C21 C26 -123.3(3) . . . . ? C20 Fe1 C21 C26 119.8(3) . . . . ? C24 Fe1 C21 C26 156.5(3) . . . . ? P1 Fe1 C21 C26 140.5(2) . . . . ? Si1 Fe1 C21 C26 -56.5(3) . . . . ? C20 C21 C22 C23 -2.9(3) . . . . ? C26 C21 C22 C23 -176.0(2) . . . . ? Fe1 C21 C22 C23 59.76(17) . . . . ? C20 C21 C22 C27 163.0(2) . . . . ? C26 C21 C22 C27 -10.2(4) . . . . ? Fe1 C21 C22 C27 -134.4(3) . . . . ? C20 C21 C22 Fe1 -62.63(16) . . . . ? C26 C21 C22 Fe1 124.2(3) . . . . ? C1 Fe1 C22 C21 -35.7(2) . . . . ? C23 Fe1 C22 C21 119.5(2) . . . . ? C20 Fe1 C22 C21 38.59(15) . . . . ? C24 Fe1 C22 C21 81.18(16) . . . . ? P1 Fe1 C22 C21 149.47(13) . . . . ? Si1 Fe1 C22 C21 -117.30(14) . . . . ? C1 Fe1 C22 C23 -155.15(16) . . . . ? C21 Fe1 C22 C23 -119.5(2) . . . . ? C20 Fe1 C22 C23 -80.91(17) . . . . ? C24 Fe1 C22 C23 -38.32(16) . . . . ? P1 Fe1 C22 C23 30.0(2) . . . . ? Si1 Fe1 C22 C23 123.20(15) . . . . ? C1 Fe1 C22 C27 86.0(4) . . . . ? C21 Fe1 C22 C27 121.7(4) . . . . ? C23 Fe1 C22 C27 -118.8(4) . . . . ? C20 Fe1 C22 C27 160.3(4) . . . . ? C24 Fe1 C22 C27 -157.1(4) . . . . ? P1 Fe1 C22 C27 -88.8(3) . . . . ? Si1 Fe1 C22 C27 4.4(3) . . . . ? C21 C22 C23 C24 2.5(3) . . . . ? C27 C22 C23 C24 -163.9(2) . . . . ? Fe1 C22 C23 C24 61.64(16) . . . . ? C21 C22 C23 C28 173.0(2) . . . . ? C27 C22 C23 C28 6.7(4) . . . . ? Fe1 C22 C23 C28 -127.8(3) . . . . ? C21 C22 C23 Fe1 -59.19(17) . . . . ? C27 C22 C23 Fe1 134.5(2) . . . . ? C1 Fe1 C23 C22 60.9(3) . . . . ? C21 Fe1 C23 C22 36.92(15) . . . . ? C20 Fe1 C23 C22 80.34(17) . . . . ? C24 Fe1 C23 C22 117.3(2) . . . . ? P1 Fe1 C23 C22 -160.30(14) . . . . ? Si1 Fe1 C23 C22 -61.82(16) . . . . ? C1 Fe1 C23 C24 -56.4(3) . . . . ? C21 Fe1 C23 C24 -80.33(16) . . . . ? C22 Fe1 C23 C24 -117.3(2) . . . . ? C20 Fe1 C23 C24 -36.91(15) . . . . ? P1 Fe1 C23 C24 82.44(15) . . . . ? Si1 Fe1 C23 C24 -179.07(13) . . . . ? C1 Fe1 C23 C28 -179.1(3) . . . . ? C21 Fe1 C23 C28 157.0(3) . . . . ? C22 Fe1 C23 C28 120.1(3) . . . . ? C20 Fe1 C23 C28 -159.6(3) . . . . ? C24 Fe1 C23 C28 -122.7(3) . . . . ? P1 Fe1 C23 C28 -40.2(3) . . . . ? Si1 Fe1 C23 C28 58.2(3) . . . . ? C21 C20 C24 C23 -0.7(3) . . . . ? C25 C20 C24 C23 173.5(2) . . . . ? Fe1 C20 C24 C23 -59.97(16) . . . . ? C21 C20 C24 C29 -172.3(2) . . . . ? C25 C20 C24 C29 1.9(4) . . . . ? Fe1 C20 C24 C29 128.4(2) . . . . ? C21 C20 C24 Fe1 59.30(16) . . . . ? C25 C20 C24 Fe1 -126.5(3) . . . . ? C22 C23 C24 C20 -1.1(3) . . . . ? C28 C23 C24 C20 -171.5(2) . . . . ? Fe1 C23 C24 C20 60.38(16) . . . . ? C22 C23 C24 C29 170.5(2) . . . . ? C28 C23 C24 C29 0.1(4) . . . . ? Fe1 C23 C24 C29 -128.1(2) . . . . ? C22 C23 C24 Fe1 -61.47(16) . . . . ? C28 C23 C24 Fe1 128.2(3) . . . . ? C1 Fe1 C24 C20 38.09(19) . . . . ? C21 Fe1 C24 C20 -37.50(15) . . . . ? C23 Fe1 C24 C20 -118.7(2) . . . . ? C22 Fe1 C24 C20 -80.64(16) . . . . ? P1 Fe1 C24 C20 137.19(14) . . . . ? Si1 Fe1 C24 C20 -117.07(16) . . . . ? C1 Fe1 C24 C23 156.81(15) . . . . ? C21 Fe1 C24 C23 81.22(16) . . . . ? C22 Fe1 C24 C23 38.08(16) . . . . ? C20 Fe1 C24 C23 118.7(2) . . . . ? P1 Fe1 C24 C23 -104.09(14) . . . . ? Si1 Fe1 C24 C23 1.7(2) . . . . ? C1 Fe1 C24 C29 -82.3(3) . . . . ? C21 Fe1 C24 C29 -157.9(3) . . . . ? C23 Fe1 C24 C29 120.9(3) . . . . ? C22 Fe1 C24 C29 159.0(3) . . . . ? C20 Fe1 C24 C29 -120.4(3) . . . . ? P1 Fe1 C24 C29 16.8(3) . . . . ? Si1 Fe1 C24 C29 122.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.319 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.071