# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2286 #[Fe2(CO)6(m-PhC=CH2)(m-PPh2)] 1a data_str686 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H17 Fe2 O6 P' _chemical_formula_weight 568.07 _chemical_melting_point ? _chemical_compound_source ? 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' '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 P21/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 14.066(3) _cell_length_b 12.748(3) _cell_length_c 14.593(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.74(3) _cell_angle_gamma 90.00 _cell_volume 2447.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17 _cell_measurement_theta_max 24 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method ? _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 1.290 _exptl_absorpt_correction_type psi scans _exptl_absorpt_correction_T_min 0.732 _exptl_absorpt_correction_T_max 1.000 _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 Nicolet R3 _diffrn_measurement_method Nicolet R3 _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 8 _diffrn_reflns_number 4248 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0672 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.08 _reflns_number_total 4075 _reflns_number_observed 2506 _reflns_observed_criterion >2sigma(I) _computing_data_collection Nicolet R3 _computing_cell_refinement Nicolet R3 _computing_data_reduction XDISK _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _refine_special_details ; Refinement on F^2^ for ALL reflections except for 8 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. Hydrogens on C8 were found from difference maps. All others were generated using HADD ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+0.1034P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4067 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_obs 0.0515 _refine_ls_wR_factor_all 0.1599 _refine_ls_wR_factor_obs 0.1225 _refine_ls_goodness_of_fit_all 1.093 _refine_ls_goodness_of_fit_obs 1.115 _refine_ls_restrained_S_all 1.116 _refine_ls_restrained_S_obs 1.115 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.16961(6) 0.17494(6) 0.52162(5) 0.0358(2) Uani 1 d . . Fe2 Fe 0.18992(6) 0.34922(6) 0.62132(6) 0.0413(3) Uani 1 d . . P P 0.23499(11) 0.32371(11) 0.48953(10) 0.0361(3) Uani 1 d . . C1 C 0.0871(5) 0.1365(4) 0.4043(4) 0.0432(13) Uani 1 d . . C2 C 0.2840(5) 0.1080(5) 0.5260(4) 0.0469(14) Uani 1 d . . C3 C 0.1474(5) 0.0654(5) 0.5898(4) 0.0481(15) Uani 1 d . . C4 C 0.2968(5) 0.2752(5) 0.6986(5) 0.0479(14) Uani 1 d . . C5 C 0.2312(5) 0.4812(5) 0.6304(5) 0.055(2) Uani 1 d . . C6 C 0.1447(5) 0.3642(6) 0.7212(5) 0.060(2) Uani 1 d . . C7 C 0.0595(4) 0.2617(4) 0.5416(4) 0.0386(12) Uani 1 d . . C8 C 0.0401(4) 0.3654(4) 0.5103(4) 0.0444(14) Uani 1 d . . H8A H -0.0173(4) 0.3972(4) 0.5272(4) 0.080 Uiso 1 d R . H8B H 0.0591(4) 0.4017(4) 0.4549(4) 0.080 Uiso 1 d R . O1 O 0.0330(4) 0.1124(4) 0.3277(3) 0.0680(13) Uani 1 d . . O2 O 0.3540(3) 0.0610(4) 0.5262(4) 0.0704(14) Uani 1 d . . O3 O 0.1429(4) -0.0108(4) 0.6295(4) 0.0741(14) Uani 1 d . . O4 O 0.3640(4) 0.2306(4) 0.7528(3) 0.0732(14) Uani 1 d . . O5 O 0.2588(4) 0.5671(4) 0.6365(4) 0.0765(15) Uani 1 d . . O6 O 0.1217(4) 0.3787(5) 0.7882(4) 0.092(2) Uani 1 d . . C10 C -0.0159(4) 0.2142(4) 0.5804(4) 0.0399(13) Uani 1 d . . C11 C 0.0073(5) 0.1678(5) 0.6731(5) 0.052(2) Uani 1 d . . H11A H 0.0769(5) 0.1669(5) 0.7168(5) 0.080 Uiso 1 d R . C12 C -0.0655(7) 0.1248(5) 0.7030(6) 0.071(2) Uani 1 d . . H12A H -0.0477(7) 0.0948(5) 0.7672(6) 0.080 Uiso 1 d R . C13 C -0.1663(7) 0.1249(6) 0.6409(7) 0.078(2) Uani 1 d . . H13A H -0.2168(7) 0.0935(6) 0.6626(7) 0.080 Uiso 1 d R . C14 C -0.1930(5) 0.1683(6) 0.5491(7) 0.072(2) Uani 1 d . . H14A H -0.2630(5) 0.1672(6) 0.5067(7) 0.080 Uiso 1 d R . C15 C -0.1184(5) 0.2145(5) 0.5191(5) 0.058(2) Uani 1 d . . H15A H -0.1376(5) 0.2482(5) 0.4562(5) 0.080 Uiso 1 d R . C20 C 0.3702(4) 0.3286(4) 0.5048(4) 0.0406(13) Uani 1 d . . C21 C 0.4426(4) 0.3771(5) 0.5846(4) 0.0471(14) Uani 1 d . . H21A H 0.4219(4) 0.4062(5) 0.6353(4) 0.080 Uiso 1 d R . C22 C 0.5439(5) 0.3791(6) 0.5944(5) 0.061(2) Uani 1 d . . H22A H 0.5924(5) 0.4144(6) 0.6493(5) 0.080 Uiso 1 d R . C23 C 0.5741(5) 0.3322(6) 0.5245(6) 0.067(2) Uani 1 d . . H23A H 0.6444(5) 0.3339(6) 0.5308(6) 0.080 Uiso 1 d R . C24 C 0.5031(6) 0.2834(6) 0.4450(5) 0.067(2) Uani 1 d . . H24A H 0.5247(6) 0.2493(6) 0.3971(5) 0.080 Uiso 1 d R . C25 C 0.4026(5) 0.2827(5) 0.4340(5) 0.054(2) Uani 1 d . . H25A H 0.3537(5) 0.2512(5) 0.3770(5) 0.080 Uiso 1 d R . C30 C 0.1791(4) 0.3993(4) 0.3763(4) 0.0403(13) Uani 1 d . . C31 C 0.1824(6) 0.5081(5) 0.3782(5) 0.065(2) Uani 1 d . . H31A H 0.2115(6) 0.5448(5) 0.4393(5) 0.080 Uiso 1 d R . C32 C 0.1412(6) 0.5648(6) 0.2906(5) 0.071(2) Uani 1 d . . H32A H 0.1463(6) 0.6399(6) 0.2909(5) 0.080 Uiso 1 d R . C33 C 0.0950(6) 0.5137(6) 0.2022(5) 0.065(2) Uani 1 d . . H33A H 0.0626(6) 0.5516(6) 0.1424(5) 0.080 Uiso 1 d R . C34 C 0.0929(5) 0.4078(6) 0.2019(5) 0.060(2) Uani 1 d . . H34A H 0.0648(5) 0.3711(6) 0.1407(5) 0.080 Uiso 1 d R . C35 C 0.1334(5) 0.3492(5) 0.2870(4) 0.055(2) Uani 1 d . . H35A H 0.1278(5) 0.2741(5) 0.2842(4) 0.080 Uiso 1 d 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 0.0369(4) 0.0349(4) 0.0361(4) -0.0005(3) 0.0135(3) -0.0005(3) Fe2 0.0433(5) 0.0436(5) 0.0398(5) -0.0088(4) 0.0181(4) -0.0064(4) P 0.0377(8) 0.0364(8) 0.0345(7) -0.0016(6) 0.0131(6) -0.0037(6) C1 0.048(3) 0.036(3) 0.049(4) 0.001(3) 0.022(3) 0.000(3) C2 0.043(3) 0.042(3) 0.052(3) 0.008(3) 0.011(3) 0.003(3) C3 0.055(4) 0.042(4) 0.048(3) 0.000(3) 0.020(3) 0.006(3) C4 0.053(4) 0.045(4) 0.048(4) -0.002(3) 0.022(3) -0.012(3) C5 0.070(4) 0.042(4) 0.054(4) -0.011(3) 0.023(3) -0.008(3) C6 0.058(4) 0.074(5) 0.050(4) -0.015(3) 0.022(3) -0.010(4) C7 0.046(3) 0.033(3) 0.039(3) -0.003(2) 0.018(2) -0.001(3) C8 0.036(3) 0.043(3) 0.055(4) 0.008(3) 0.017(3) 0.009(3) O1 0.079(3) 0.058(3) 0.049(3) -0.005(2) 0.002(2) -0.006(2) O2 0.050(3) 0.068(3) 0.096(4) 0.003(3) 0.029(3) 0.014(2) O3 0.110(4) 0.042(3) 0.083(3) 0.019(3) 0.049(3) 0.010(3) O4 0.070(3) 0.078(4) 0.059(3) 0.011(3) 0.008(3) 0.002(3) O5 0.099(4) 0.051(3) 0.076(3) -0.012(3) 0.026(3) -0.017(3) O6 0.093(4) 0.127(5) 0.074(4) -0.045(3) 0.052(3) -0.034(4) C10 0.040(3) 0.036(3) 0.046(3) -0.008(2) 0.017(3) 0.000(2) C11 0.064(4) 0.043(3) 0.058(4) -0.001(3) 0.033(3) -0.006(3) C12 0.109(7) 0.042(4) 0.088(5) -0.001(4) 0.066(5) -0.005(4) C13 0.082(6) 0.068(5) 0.115(7) -0.015(5) 0.072(6) -0.015(4) C14 0.038(4) 0.061(5) 0.126(7) -0.030(5) 0.040(4) -0.012(3) C15 0.052(4) 0.048(4) 0.077(5) -0.004(3) 0.028(4) 0.001(3) C20 0.043(3) 0.036(3) 0.045(3) -0.004(2) 0.019(3) -0.002(3) C21 0.044(3) 0.053(4) 0.048(3) -0.003(3) 0.021(3) -0.004(3) C22 0.042(4) 0.067(5) 0.066(4) -0.004(4) 0.009(3) -0.003(3) C23 0.042(4) 0.077(5) 0.088(5) 0.006(4) 0.030(4) 0.004(3) C24 0.065(5) 0.080(5) 0.063(4) -0.003(4) 0.034(4) 0.014(4) C25 0.051(4) 0.066(4) 0.050(4) -0.005(3) 0.025(3) 0.003(3) C30 0.037(3) 0.039(3) 0.048(3) 0.001(3) 0.018(3) -0.003(2) C31 0.096(6) 0.046(4) 0.052(4) 0.000(3) 0.022(4) -0.018(4) C32 0.099(6) 0.044(4) 0.068(5) 0.013(3) 0.027(4) 0.002(4) C33 0.078(5) 0.064(5) 0.056(4) 0.017(4) 0.027(4) 0.016(4) C34 0.063(4) 0.062(4) 0.044(4) 0.004(3) 0.007(3) -0.003(3) C35 0.066(4) 0.054(4) 0.044(3) -0.001(3) 0.017(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 1.763(6) . y Fe1 C2 1.802(6) . y Fe1 C3 1.805(6) . y Fe1 C7 2.007(5) . y Fe1 P 2.229(2) . y Fe1 Fe2 2.6153(12) . y Fe2 C5 1.769(7) . y Fe2 C4 1.795(7) . y Fe2 C6 1.796(7) . y Fe2 C7 2.109(5) . y Fe2 C8 2.165(6) . y Fe2 P 2.252(2) . y P C30 1.832(6) . ? P C20 1.836(6) . ? C1 O1 1.150(7) . ? C2 O2 1.152(7) . ? C3 O3 1.145(7) . ? C4 O4 1.146(7) . ? C5 O5 1.155(7) . ? C6 O6 1.148(8) . ? C7 C8 1.393(8) . y C7 C10 1.495(7) . ? C10 C15 1.402(8) . ? C10 C11 1.406(8) . ? C11 C12 1.362(9) . ? C12 C13 1.387(11) . ? C13 C14 1.373(12) . ? C14 C15 1.402(9) . ? C20 C21 1.391(8) . ? C20 C25 1.396(8) . ? C21 C22 1.382(9) . ? C22 C23 1.373(10) . ? C23 C24 1.381(10) . ? C24 C25 1.366(9) . ? C30 C35 1.388(8) . ? C30 C31 1.388(8) . ? C31 C32 1.404(9) . ? C32 C33 1.385(10) . ? C33 C34 1.350(9) . ? C34 C35 1.386(9) . ? 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 C2 100.1(3) . . ? C1 Fe1 C3 97.9(3) . . ? C2 Fe1 C3 86.6(3) . . ? C1 Fe1 C7 91.0(2) . . ? C2 Fe1 C7 168.8(3) . . ? C3 Fe1 C7 93.0(2) . . ? C1 Fe1 P 102.2(2) . . ? C2 Fe1 P 88.9(2) . . ? C3 Fe1 P 159.9(2) . . ? C7 Fe1 P 87.6(2) . . ? C1 Fe1 Fe2 132.9(2) . . ? C2 Fe1 Fe2 117.5(2) . . ? C3 Fe1 Fe2 110.9(2) . . ? C7 Fe1 Fe2 52.3(2) . . ? P Fe1 Fe2 54.70(5) . . ? C5 Fe2 C4 105.8(3) . . ? C5 Fe2 C6 92.3(3) . . ? C4 Fe2 C6 90.3(3) . . ? C5 Fe2 C7 137.9(3) . . ? C4 Fe2 C7 116.1(2) . . ? C6 Fe2 C7 90.8(3) . . ? C5 Fe2 C8 99.9(3) . . ? C4 Fe2 C8 153.7(2) . . ? C6 Fe2 C8 93.8(3) . . ? C7 Fe2 C8 38.0(2) . . ? C5 Fe2 P 91.0(2) . . ? C4 Fe2 P 91.9(2) . . ? C6 Fe2 P 175.4(2) . . ? C7 Fe2 P 84.59(15) . . ? C8 Fe2 P 82.4(2) . . ? C5 Fe2 Fe1 144.9(2) . . ? C4 Fe2 Fe1 78.8(2) . . ? C6 Fe2 Fe1 122.8(2) . . ? C7 Fe2 Fe1 48.85(15) . . ? C8 Fe2 Fe1 77.2(2) . . ? P Fe2 Fe1 53.88(4) . . ? C30 P C20 100.8(3) . . ? C30 P Fe1 124.0(2) . . ? C20 P Fe1 119.3(2) . . ? C30 P Fe2 122.3(2) . . ? C20 P Fe2 119.0(2) . . ? Fe1 P Fe2 71.43(5) . . y O1 C1 Fe1 179.4(6) . . ? O2 C2 Fe1 176.4(6) . . ? O3 C3 Fe1 170.8(6) . . ? O4 C4 Fe2 175.8(6) . . ? O5 C5 Fe2 179.6(6) . . ? O6 C6 Fe2 175.0(6) . . ? C8 C7 C10 115.2(5) . . y C8 C7 Fe1 123.1(4) . . ? C10 C7 Fe1 121.3(4) . . ? C8 C7 Fe2 73.2(3) . . y C10 C7 Fe2 126.9(4) . . ? Fe1 C7 Fe2 78.8(2) . . y C7 C8 Fe2 68.8(3) . . y C15 C10 C11 116.8(6) . . ? C15 C10 C7 117.7(5) . . ? C11 C10 C7 125.5(5) . . ? C12 C11 C10 122.2(7) . . ? C11 C12 C13 120.1(7) . . ? C14 C13 C12 120.0(7) . . ? C13 C14 C15 119.9(7) . . ? C10 C15 C14 120.9(7) . . ? C21 C20 C25 118.2(5) . . ? C21 C20 P 122.4(4) . . ? C25 C20 P 119.4(4) . . ? C22 C21 C20 121.1(6) . . ? C23 C22 C21 119.6(6) . . ? C22 C23 C24 119.9(6) . . ? C25 C24 C23 120.8(6) . . ? C24 C25 C20 120.4(6) . . ? C35 C30 C31 118.7(6) . . ? C35 C30 P 120.9(5) . . ? C31 C30 P 120.4(5) . . ? C30 C31 C32 119.7(6) . . ? C33 C32 C31 120.8(7) . . ? C34 C33 C32 118.5(6) . . ? C33 C34 C35 122.3(7) . . ? C34 C35 C30 120.0(6) . . ? _refine_diff_density_max 0.594 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.095 # [Fe2(CO)6(nPrC=CH2)(m-PPh2)] 1c data_str643 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C23 H19 Fe2 O6 P' _chemical_formula_weight 534.05 _chemical_melting_point ? _chemical_compound_source ? 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' '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.444(3) _cell_length_b 8.120(2) _cell_length_c 22.698(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.55(3) _cell_angle_gamma 90.00 _cell_volume 2476.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 12 _cell_measurement_theta_max 19 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method ? _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 1.270 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 Nicolet R3mV _diffrn_measurement_method omega _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4350 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4162 _reflns_number_observed 2061 _reflns_observed_criterion >2sigma(I) _computing_data_collection Nicolet R3 _computing_cell_refinement Nicolet R3 _computing_data_reduction XDISK _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. The protons on the beta carbon were located experimentally ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1418P)^2^+8.7196P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4157 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1671 _refine_ls_R_factor_obs 0.0971 _refine_ls_wR_factor_all 0.3418 _refine_ls_wR_factor_obs 0.2435 _refine_ls_goodness_of_fit_all 1.221 _refine_ls_goodness_of_fit_obs 1.285 _refine_ls_restrained_S_all 1.233 _refine_ls_restrained_S_obs 1.285 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.27734(10) 0.1993(2) 0.54414(6) 0.0591(5) Uani 1 d . . Fe2 Fe 0.27529(11) 0.5185(2) 0.56354(7) 0.0637(5) Uani 1 d . . P1 P 0.2228(2) 0.3189(4) 0.62719(11) 0.0587(7) Uani 1 d . . O1 O 0.1282(7) -0.0512(12) 0.5084(4) 0.087(2) Uani 1 d . . O2 O 0.4119(8) -0.0136(15) 0.6185(4) 0.110(4) Uani 1 d . . O3 O 0.4296(8) 0.1521(15) 0.4521(4) 0.119(4) Uani 1 d . . O4 O 0.3419(8) 0.7509(13) 0.4703(5) 0.106(3) Uani 1 d . . O5 O 0.4880(7) 0.4645(14) 0.5949(5) 0.102(3) Uani 1 d . . O6 O 0.2035(8) 0.7758(12) 0.6459(4) 0.099(3) Uani 1 d . . C1 C 0.1878(8) 0.0474(13) 0.5232(4) 0.061(2) Uani 1 d . . C2 C 0.3590(8) 0.0751(18) 0.5898(5) 0.074(3) Uani 1 d . . C3 C 0.3670(10) 0.1793(15) 0.4857(5) 0.076(3) Uani 1 d . . C4 C 0.3160(10) 0.6576(18) 0.5047(7) 0.087(4) Uani 1 d . . C5 C 0.4036(9) 0.4822(15) 0.5840(6) 0.074(3) Uani 1 d . . C6 C 0.2315(8) 0.6741(14) 0.6123(5) 0.064(3) Uani 1 d . . C7 C 0.2026(8) 0.3743(14) 0.4971(5) 0.068(3) Uani 1 d . . C8 C 0.1300(8) 0.4782(13) 0.5201(5) 0.063(3) Uani 1 d . . H8A H 0.0829(8) 0.4464(13) 0.5524(5) 0.080 Uiso 1 d R . H8B H 0.0997(8) 0.5703(13) 0.4977(5) 0.080 Uiso 1 d R . C9 C 0.2196(8) 0.3924(15) 0.4288(4) 0.067(3) Uani 1 d . . H9A H 0.2897(8) 0.3847(15) 0.4222(4) 0.080 Uiso 1 d R . H9B H 0.1977(8) 0.4995(15) 0.4160(4) 0.080 Uiso 1 d R . C10 C 0.1661(9) 0.2608(16) 0.3913(5) 0.077(3) Uani 1 d . . H10A H 0.1918(9) 0.1549(16) 0.4028(5) 0.080 Uiso 1 d R . H10B H 0.1816(9) 0.2778(16) 0.3507(5) 0.080 Uiso 1 d R . C11 C 0.0533(9) 0.2588(18) 0.3968(6) 0.084(4) Uani 1 d . . H11A H 0.0251(9) 0.1733(18) 0.3724(6) 0.080 Uiso 1 d R . H11B H 0.0370(9) 0.2391(18) 0.4372(6) 0.080 Uiso 1 d R . H11C H 0.0267(9) 0.3634(18) 0.3845(6) 0.080 Uiso 1 d R . C20 C 0.0940(8) 0.3104(13) 0.6538(4) 0.062(3) Uani 1 d . . C21 C 0.0719(9) 0.3994(17) 0.7066(5) 0.079(3) Uani 1 d . . H21A H 0.1230(9) 0.4615(17) 0.7269(5) 0.080 Uiso 1 d R . C22 C -0.0263(10) 0.3967(22) 0.7280(5) 0.096(4) Uani 1 d . . H22A H -0.0417(10) 0.4555(22) 0.7633(5) 0.080 Uiso 1 d R . C23 C -0.0999(10) 0.3071(20) 0.6988(6) 0.090(4) Uani 1 d . . H23A H -0.1662(10) 0.3077(20) 0.7136(6) 0.080 Uiso 1 d R . C24 C -0.0818(9) 0.2174(18) 0.6480(6) 0.083(4) Uani 1 d . . H24A H -0.1327(9) 0.1532(18) 0.6285(6) 0.080 Uiso 1 d R . C25 C 0.0185(8) 0.2185(16) 0.6256(5) 0.071(3) Uani 1 d . . H25A H 0.0337(8) 0.1604(16) 0.5901(5) 0.080 Uiso 1 d R . C30 C 0.2947(8) 0.2922(13) 0.6962(5) 0.062(2) Uani 1 d . . C31 C 0.3534(10) 0.4221(19) 0.7202(5) 0.086(4) Uani 1 d . . H31A H 0.3547(10) 0.5263(19) 0.7003(5) 0.080 Uiso 1 d R . C32 C 0.4113(11) 0.3994(23) 0.7741(6) 0.102(5) Uani 1 d . . H32A H 0.4487(11) 0.4880(23) 0.7919(6) 0.080 Uiso 1 d R . C33 C 0.4100(10) 0.2431(22) 0.8022(5) 0.095(4) Uani 1 d . . H33A H 0.4510(10) 0.2228(22) 0.8367(5) 0.080 Uiso 1 d R . C34 C 0.3526(10) 0.1157(20) 0.7777(6) 0.091(4) Uani 1 d . . H34A H 0.3522(10) 0.0108(20) 0.7972(6) 0.080 Uiso 1 d R . C35 C 0.2939(9) 0.1361(17) 0.7263(5) 0.078(3) Uani 1 d . . H35A H 0.2521(9) 0.0487(17) 0.7116(5) 0.080 Uiso 1 d 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 0.0602(9) 0.0611(10) 0.0563(9) -0.0037(7) 0.0047(6) 0.0042(7) Fe2 0.0665(10) 0.0617(10) 0.0633(9) -0.0019(7) 0.0078(7) -0.0027(7) P1 0.0585(15) 0.064(2) 0.0534(14) -0.0057(12) 0.0024(11) -0.0003(12) O1 0.092(6) 0.073(6) 0.094(6) 0.006(5) -0.007(5) -0.005(5) O2 0.098(7) 0.155(10) 0.077(6) -0.002(6) -0.003(5) 0.045(7) O3 0.106(7) 0.153(10) 0.099(7) 0.026(7) 0.050(6) 0.047(7) O4 0.130(8) 0.077(6) 0.114(8) 0.005(6) 0.035(6) -0.029(6) O5 0.071(6) 0.120(8) 0.115(7) -0.011(6) -0.008(5) -0.003(5) O6 0.120(7) 0.078(6) 0.100(6) -0.018(5) 0.028(6) 0.009(6) C1 0.070(7) 0.052(6) 0.060(6) 0.003(5) 0.005(5) 0.009(5) C2 0.047(6) 0.109(10) 0.067(6) -0.003(7) 0.003(5) -0.005(6) C3 0.088(8) 0.062(7) 0.077(7) 0.007(6) -0.005(6) 0.019(6) C4 0.073(8) 0.073(8) 0.115(11) -0.013(8) 0.023(7) -0.001(6) C5 0.064(7) 0.073(8) 0.084(8) -0.010(6) 0.002(6) -0.009(6) C6 0.069(6) 0.061(6) 0.062(6) 0.003(5) -0.005(5) -0.004(5) C7 0.061(6) 0.063(7) 0.080(7) 0.009(5) 0.013(5) 0.001(5) C8 0.058(6) 0.053(6) 0.077(7) 0.002(5) 0.010(5) 0.007(5) C9 0.063(6) 0.076(7) 0.061(6) 0.005(5) -0.003(5) 0.007(5) C10 0.092(8) 0.077(8) 0.062(6) 0.001(6) 0.004(6) 0.008(7) C11 0.082(8) 0.094(9) 0.076(8) 0.001(7) -0.005(6) -0.006(7) C20 0.070(6) 0.062(6) 0.055(5) 0.000(5) 0.004(5) 0.014(5) C21 0.080(8) 0.086(9) 0.071(7) -0.009(6) 0.002(6) -0.002(7) C22 0.080(8) 0.143(14) 0.065(7) -0.011(8) 0.014(6) 0.015(9) C23 0.066(7) 0.122(12) 0.083(8) 0.006(8) 0.014(6) 0.013(8) C24 0.060(7) 0.093(9) 0.095(9) 0.000(7) 0.011(6) 0.001(6) C25 0.064(6) 0.082(8) 0.067(6) -0.007(6) 0.010(5) -0.004(6) C30 0.066(6) 0.061(6) 0.060(6) 0.004(5) 0.003(5) 0.001(5) C31 0.092(9) 0.095(9) 0.071(7) 0.008(7) -0.005(6) -0.006(8) C32 0.090(9) 0.135(14) 0.079(8) -0.001(9) -0.017(7) -0.021(9) C33 0.090(9) 0.139(13) 0.054(7) 0.008(8) -0.015(6) 0.005(9) C34 0.090(9) 0.108(11) 0.075(8) -0.004(8) -0.005(7) 0.023(8) C35 0.077(7) 0.092(9) 0.065(7) 0.001(6) -0.007(6) 0.006(7) _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 1.780(12) . yes Fe1 C2 1.798(13) . yes Fe1 C3 1.823(14) . yes Fe1 C7 2.027(11) . yes Fe1 P1 2.260(3) . yes Fe1 Fe2 2.629(2) . yes Fe2 C6 1.790(12) . yes Fe2 C5 1.799(13) . yes Fe2 C4 1.84(2) . yes Fe2 C7 2.126(12) . yes Fe2 C8 2.188(11) . yes Fe2 P1 2.295(3) . yes P1 C30 1.831(11) . ? P1 C20 1.851(11) . ? O1 C1 1.174(13) . yes O2 C2 1.194(15) . yes O3 C3 1.173(15) . yes O4 C4 1.15(2) . yes O5 C5 1.163(14) . yes O6 C6 1.192(14) . yes C7 C8 1.402(14) . yes C7 C9 1.581(15) . yes C9 C10 1.53(2) . yes C10 C11 1.53(2) . yes C20 C25 1.40(2) . ? C20 C21 1.44(2) . ? C21 C22 1.42(2) . ? C22 C23 1.38(2) . ? C23 C24 1.39(2) . ? C24 C25 1.453(15) . ? C30 C31 1.42(2) . ? C30 C35 1.44(2) . ? C31 C32 1.44(2) . ? C32 C33 1.42(2) . ? C33 C34 1.40(2) . ? C34 C35 1.40(2) . ? 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 C2 99.4(6) . . yes C1 Fe1 C3 101.5(5) . . yes C2 Fe1 C3 87.9(5) . . yes C1 Fe1 C7 91.3(5) . . yes C2 Fe1 C7 169.3(5) . . yes C3 Fe1 C7 90.4(5) . . yes C1 Fe1 P1 106.7(3) . . yes C2 Fe1 P1 88.1(4) . . yes C3 Fe1 P1 151.7(4) . . yes C7 Fe1 P1 88.4(3) . . yes C1 Fe1 Fe2 135.9(3) . . yes C2 Fe1 Fe2 117.7(4) . . yes C3 Fe1 Fe2 102.7(4) . . yes C7 Fe1 Fe2 52.4(3) . . yes P1 Fe1 Fe2 55.38(9) . . yes C6 Fe2 C5 106.5(5) . . yes C6 Fe2 C4 97.2(5) . . yes C5 Fe2 C4 89.2(6) . . yes C6 Fe2 C7 132.5(5) . . yes C5 Fe2 C7 120.8(5) . . yes C4 Fe2 C7 87.9(5) . . yes C6 Fe2 C8 94.6(4) . . yes C5 Fe2 C8 158.4(5) . . yes C4 Fe2 C8 92.5(5) . . yes C7 Fe2 C8 37.9(4) . . yes C6 Fe2 P1 89.8(4) . . yes C5 Fe2 P1 91.7(4) . . yes C4 Fe2 P1 172.3(4) . . yes C7 Fe2 P1 85.1(3) . . yes C8 Fe2 P1 83.8(3) . . yes C6 Fe2 Fe1 143.6(4) . . yes C5 Fe2 Fe1 82.4(4) . . yes C4 Fe2 Fe1 118.6(4) . . yes C7 Fe2 Fe1 49.1(3) . . yes C8 Fe2 Fe1 77.9(3) . . yes P1 Fe2 Fe1 54.13(8) . . yes C30 P1 C20 101.2(5) . . ? C30 P1 Fe1 119.2(4) . . ? C20 P1 Fe1 125.7(4) . . ? C30 P1 Fe2 117.3(4) . . ? C20 P1 Fe2 122.5(4) . . ? Fe1 P1 Fe2 70.49(9) . . yes O1 C1 Fe1 178.7(10) . . ? O2 C2 Fe1 176.9(12) . . ? O3 C3 Fe1 172.2(10) . . ? O4 C4 Fe2 176.3(12) . . ? O5 C5 Fe2 176.3(12) . . ? O6 C6 Fe2 178.4(10) . . ? C8 C7 C9 115.5(10) . . ? C8 C7 Fe1 124.4(8) . . ? C9 C7 Fe1 120.0(7) . . ? C8 C7 Fe2 73.5(7) . . ? C9 C7 Fe2 124.7(8) . . ? Fe1 C7 Fe2 78.5(4) . . yes C7 C8 Fe2 68.6(6) . . ? C10 C9 C7 113.7(10) . . ? C11 C10 C9 114.4(10) . . ? C25 C20 C21 119.0(10) . . ? C25 C20 P1 123.0(8) . . ? C21 C20 P1 118.0(9) . . ? C22 C21 C20 119.5(12) . . ? C23 C22 C21 120.3(12) . . ? C22 C23 C24 122.2(12) . . ? C23 C24 C25 118.2(12) . . ? C20 C25 C24 120.8(11) . . ? C31 C30 C35 118.9(10) . . ? C31 C30 P1 121.1(9) . . ? C35 C30 P1 120.0(8) . . ? C30 C31 C32 120.9(13) . . ? C33 C32 C31 118.7(14) . . ? C34 C33 C32 119.8(12) . . ? C33 C34 C35 122.5(14) . . ? C34 C35 C30 119.2(13) . . ? _refine_diff_density_max 0.688 _refine_diff_density_min -1.160 _refine_diff_density_rms 0.145 # [Fe2(CO)6(m-HC=CHPh)(m-PPh2)] 2a data_str644 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H17 Fe2 O6 P' _chemical_formula_weight 568.07 _chemical_melting_point ? _chemical_compound_source ? 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' '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 P21/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 9.993(2) _cell_length_b 14.641(3) _cell_length_c 18.690(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.49(3) _cell_angle_gamma 90.00 _cell_volume 2647.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14 _cell_measurement_theta_max 23 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.92 _exptl_crystal_size_mid 0.90 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method ? _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 1.193 _exptl_absorpt_correction_type psi scans _exptl_absorpt_correction_T_min 0.570 _exptl_absorpt_correction_T_max 0.998 _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 Nicolet R3mV _diffrn_measurement_method omega-2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4945 _diffrn_reflns_av_R_equivalents 0.0826 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4668 _reflns_number_observed 3479 _reflns_observed_criterion >2sigma(I) _computing_data_collection Nicolet R3 _computing_cell_refinement Nicolet R3 _computing_data_reduction XDISK _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _refine_special_details ; Refinement on F^2^ for ALL reflections except for 9 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0834P)^2^+1.1413P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4659 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_obs 0.0490 _refine_ls_wR_factor_all 0.1558 _refine_ls_wR_factor_obs 0.1304 _refine_ls_goodness_of_fit_all 1.079 _refine_ls_goodness_of_fit_obs 1.113 _refine_ls_restrained_S_all 1.138 _refine_ls_restrained_S_obs 1.113 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.19671(6) 0.65628(4) 0.89109(3) 0.0612(2) Uani 1 d . . Fe2 Fe -0.06103(5) 0.64746(3) 0.81478(3) 0.0539(2) Uani 1 d . . P1 P 0.09144(9) 0.76287(6) 0.80947(5) 0.0509(2) Uani 1 d . . O1 O 0.1922(5) 0.5135(3) 1.0035(2) 0.1194(14) Uani 1 d . . O2 O 0.4732(4) 0.6216(3) 0.8678(3) 0.1182(14) Uani 1 d . . O3 O 0.2641(6) 0.7987(3) 1.0083(2) 0.140(2) Uani 1 d . . O4 O -0.2174(4) 0.4777(3) 0.8286(2) 0.1105(13) Uani 1 d . . O5 O -0.2813(4) 0.7313(3) 0.6957(2) 0.1110(12) Uani 1 d . . O6 O -0.1156(4) 0.7125(2) 0.9548(2) 0.0963(10) Uani 1 d . . C1 C 0.1958(5) 0.5691(3) 0.9606(2) 0.0804(12) Uani 1 d . . C2 C 0.3657(5) 0.6383(3) 0.8771(3) 0.0789(12) Uani 1 d . . C3 C 0.2380(6) 0.7447(3) 0.9623(3) 0.0910(15) Uani 1 d . . C4 C -0.1549(5) 0.5432(3) 0.8243(3) 0.0746(11) Uani 1 d . . C5 C -0.1967(5) 0.6981(3) 0.7420(2) 0.0709(11) Uani 1 d . . C6 C -0.0909(5) 0.6900(3) 0.9001(2) 0.0691(10) Uani 1 d . . C7 C 0.1118(4) 0.5634(3) 0.8151(2) 0.0587(9) Uani 1 d . . H7 H 0.1131(4) 0.5013(3) 0.8318(2) 0.080 Uiso 1 d R . C8 C 0.0516(3) 0.5759(2) 0.7393(2) 0.0522(8) Uani 1 d . . H8 H 0.0759(3) 0.6265(2) 0.7161(2) 0.080 Uiso 1 d R . C10 C -0.0115(3) 0.5024(2) 0.6858(2) 0.0529(8) Uani 1 d . . C11 C -0.0287(4) 0.4111(2) 0.7062(2) 0.0611(9) Uani 1 d . . H11A H -0.0036(4) 0.3945(2) 0.7575(2) 0.080 Uiso 1 d R . C12 C -0.0780(4) 0.3451(3) 0.6519(3) 0.0765(13) Uani 1 d . . H12A H -0.0899(4) 0.2835(3) 0.6668(3) 0.080 Uiso 1 d R . C13 C -0.1132(5) 0.3684(4) 0.5781(3) 0.091(2) Uani 1 d . . H13A H -0.1463(5) 0.3218(4) 0.5418(3) 0.080 Uiso 1 d R . C14 C -0.0988(5) 0.4581(4) 0.5571(3) 0.092(2) Uani 1 d . . H14A H -0.1233(5) 0.4739(4) 0.5056(3) 0.080 Uiso 1 d R . C15 C -0.0486(4) 0.5248(3) 0.6100(2) 0.0651(10) Uani 1 d . . H15A H -0.0394(4) 0.5868(3) 0.5954(2) 0.080 Uiso 1 d R . C20 C 0.1307(4) 0.7913(2) 0.7204(2) 0.0534(8) Uani 1 d . . C21 C 0.2497(4) 0.7615(3) 0.7017(2) 0.0656(10) Uani 1 d . . H21A H 0.3146(4) 0.7244(3) 0.7362(2) 0.080 Uiso 1 d R . C22 C 0.2736(5) 0.7847(3) 0.6325(3) 0.0808(13) Uani 1 d . . H22A H 0.3567(5) 0.7646(3) 0.6205(3) 0.080 Uiso 1 d R . C23 C 0.1798(6) 0.8373(3) 0.5827(3) 0.0824(14) Uani 1 d . . H23A H 0.1952(6) 0.8528(3) 0.5355(3) 0.080 Uiso 1 d R . C24 C 0.0624(6) 0.8683(3) 0.6010(3) 0.0852(13) Uani 1 d . . H24A H -0.0031(6) 0.9052(3) 0.5666(3) 0.080 Uiso 1 d R . C25 C 0.0373(5) 0.8459(3) 0.6689(2) 0.0743(11) Uani 1 d . . H25A H -0.0450(5) 0.8672(3) 0.6812(2) 0.080 Uiso 1 d R . C30 C 0.0648(3) 0.8790(2) 0.8414(2) 0.0528(8) Uani 1 d . . C31 C 0.1710(4) 0.9433(3) 0.8478(2) 0.0649(10) Uani 1 d . . H31A H 0.2542(4) 0.9252(3) 0.8348(2) 0.080 Uiso 1 d R . C32 C 0.1560(4) 1.0323(3) 0.8717(3) 0.0697(11) Uani 1 d . . H32A H 0.2298(4) 1.0756(3) 0.8759(3) 0.080 Uiso 1 d R . C33 C 0.0351(5) 1.0575(3) 0.8904(3) 0.0838(13) Uani 1 d . . H33A H 0.0251(5) 1.1183(3) 0.9078(3) 0.080 Uiso 1 d R . C34 C -0.0698(5) 0.9945(3) 0.8841(4) 0.100(2) Uani 1 d . . H34A H -0.1541(5) 1.0119(3) 0.8963(4) 0.080 Uiso 1 d R . C35 C -0.0564(4) 0.9062(3) 0.8593(3) 0.0794(13) Uani 1 d . . H35A H -0.1296(4) 0.8624(3) 0.8543(3) 0.080 Uiso 1 d 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 0.0719(4) 0.0542(3) 0.0507(3) 0.0006(2) 0.0026(3) -0.0021(2) Fe2 0.0600(3) 0.0529(3) 0.0520(3) -0.0012(2) 0.0203(2) -0.0060(2) P1 0.0533(5) 0.0490(5) 0.0518(5) -0.0001(4) 0.0156(4) -0.0015(4) O1 0.194(4) 0.091(2) 0.074(2) 0.025(2) 0.034(2) 0.007(3) O2 0.073(2) 0.109(3) 0.171(4) 0.030(3) 0.028(2) 0.010(2) O3 0.213(5) 0.092(3) 0.081(3) -0.028(2) -0.026(3) -0.006(3) O4 0.144(3) 0.089(2) 0.117(3) -0.016(2) 0.067(3) -0.051(2) O5 0.091(2) 0.122(3) 0.101(3) 0.019(2) -0.010(2) 0.011(2) O6 0.126(3) 0.101(2) 0.079(2) -0.009(2) 0.058(2) 0.000(2) C1 0.107(3) 0.076(3) 0.053(2) -0.002(2) 0.008(2) 0.000(3) C2 0.079(3) 0.065(3) 0.083(3) 0.009(2) 0.002(2) -0.004(2) C3 0.120(4) 0.070(3) 0.068(3) -0.003(2) -0.006(3) 0.001(3) C4 0.088(3) 0.071(3) 0.074(3) -0.006(2) 0.039(2) -0.014(2) C5 0.072(3) 0.072(3) 0.071(3) -0.005(2) 0.022(2) -0.011(2) C6 0.088(3) 0.063(2) 0.066(2) 0.002(2) 0.037(2) -0.003(2) C7 0.065(2) 0.056(2) 0.053(2) 0.002(2) 0.010(2) 0.006(2) C8 0.052(2) 0.049(2) 0.057(2) 0.000(2) 0.017(2) -0.0022(15) C10 0.046(2) 0.058(2) 0.057(2) -0.003(2) 0.018(2) 0.005(2) C11 0.061(2) 0.053(2) 0.070(2) -0.004(2) 0.019(2) 0.001(2) C12 0.068(3) 0.064(3) 0.105(4) -0.023(2) 0.036(3) -0.013(2) C13 0.083(3) 0.114(4) 0.085(4) -0.049(3) 0.037(3) -0.035(3) C14 0.086(3) 0.141(5) 0.053(2) -0.018(3) 0.022(2) -0.033(3) C15 0.058(2) 0.082(3) 0.056(2) -0.002(2) 0.016(2) -0.007(2) C20 0.058(2) 0.046(2) 0.059(2) -0.001(2) 0.020(2) -0.005(2) C21 0.068(2) 0.059(2) 0.076(3) -0.003(2) 0.029(2) 0.000(2) C22 0.094(3) 0.072(3) 0.096(3) -0.016(3) 0.059(3) -0.012(2) C23 0.128(4) 0.066(3) 0.064(3) -0.004(2) 0.044(3) -0.019(3) C24 0.108(4) 0.083(3) 0.061(3) 0.013(2) 0.013(2) 0.004(3) C25 0.079(3) 0.080(3) 0.065(3) 0.013(2) 0.022(2) 0.011(2) C30 0.053(2) 0.049(2) 0.057(2) 0.001(2) 0.016(2) -0.0004(15) C31 0.055(2) 0.056(2) 0.088(3) -0.007(2) 0.026(2) -0.005(2) C32 0.065(2) 0.053(2) 0.092(3) -0.004(2) 0.022(2) -0.007(2) C33 0.095(3) 0.050(2) 0.111(4) -0.009(2) 0.035(3) 0.003(2) C34 0.081(3) 0.068(3) 0.173(6) -0.011(3) 0.071(3) 0.005(2) C35 0.063(2) 0.061(2) 0.124(4) -0.003(2) 0.042(2) -0.009(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 C2 1.791(6) . y Fe1 C1 1.823(5) . y Fe1 C3 1.829(5) . y Fe1 C7 1.996(4) . y Fe1 P1 2.2508(12) . y Fe1 Fe2 2.6166(11) . y Fe2 C6 1.806(4) . y Fe2 C5 1.821(5) . y Fe2 C4 1.823(4) . y Fe2 C7 2.119(4) . y Fe2 C8 2.269(3) . y Fe2 P1 2.2940(11) . y P1 C30 1.843(4) . ? P1 C20 1.850(4) . ? O1 C1 1.150(6) . y O2 C2 1.157(6) . y O3 C3 1.149(6) . y O4 C4 1.159(5) . y O5 C5 1.155(5) . y O6 C6 1.157(5) . y C7 C8 1.405(5) . y C8 C10 1.496(5) . y C10 C11 1.411(5) . ? C10 C15 1.410(5) . ? C11 C12 1.400(6) . ? C12 C13 1.378(7) . ? C13 C14 1.388(8) . ? C14 C15 1.392(6) . ? C20 C21 1.392(5) . ? C20 C25 1.410(5) . ? C21 C22 1.413(6) . ? C22 C23 1.379(7) . ? C23 C24 1.378(7) . ? C24 C25 1.393(6) . ? C30 C35 1.393(5) . ? C30 C31 1.401(5) . ? C31 C32 1.398(5) . ? C32 C33 1.389(6) . ? C33 C34 1.379(6) . ? C34 C35 1.391(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 C2 Fe1 C1 100.0(2) . . y C2 Fe1 C3 99.2(2) . . y C1 Fe1 C3 91.0(2) . . y C2 Fe1 C7 92.6(2) . . y C1 Fe1 C7 87.3(2) . . y C3 Fe1 C7 168.2(2) . . y C2 Fe1 P1 107.51(15) . . y C1 Fe1 P1 152.1(2) . . y C3 Fe1 P1 89.1(2) . . y C7 Fe1 P1 86.93(11) . . y C2 Fe1 Fe2 138.5(2) . . y C1 Fe1 Fe2 100.0(2) . . y C3 Fe1 Fe2 116.4(2) . . y C7 Fe1 Fe2 52.64(10) . . y P1 Fe1 Fe2 55.63(3) . . y C6 Fe2 C5 105.2(2) . . y C6 Fe2 C4 90.0(2) . . y C5 Fe2 C4 96.2(2) . . y C6 Fe2 C7 120.8(2) . . y C5 Fe2 C7 133.8(2) . . y C4 Fe2 C7 87.3(2) . . y C6 Fe2 C8 157.8(2) . . y C5 Fe2 C8 96.7(2) . . y C4 Fe2 C8 91.2(2) . . y C7 Fe2 C8 37.14(13) . . y C6 Fe2 P1 92.42(14) . . y C5 Fe2 P1 92.64(13) . . y C4 Fe2 P1 169.8(2) . . y C7 Fe2 P1 83.00(11) . . y C8 Fe2 P1 82.83(9) . . y C6 Fe2 Fe1 81.89(15) . . y C5 Fe2 Fe1 146.56(13) . . y C4 Fe2 Fe1 116.6(2) . . y C7 Fe2 Fe1 48.46(10) . . y C8 Fe2 Fe1 77.75(9) . . y P1 Fe2 Fe1 54.08(3) . . y C30 P1 C20 99.4(2) . . ? C30 P1 Fe1 120.07(12) . . ? C20 P1 Fe1 126.67(12) . . ? C30 P1 Fe2 120.95(11) . . ? C20 P1 Fe2 119.82(12) . . ? Fe1 P1 Fe2 70.29(4) . . y O1 C1 Fe1 178.4(5) . . ? O2 C2 Fe1 176.2(4) . . ? O3 C3 Fe1 178.3(5) . . ? O4 C4 Fe2 178.1(5) . . ? O5 C5 Fe2 178.9(4) . . ? O6 C6 Fe2 175.5(4) . . ? C8 C7 Fe1 128.9(3) . . ? C8 C7 Fe2 77.2(2) . . ? Fe1 C7 Fe2 78.91(13) . . y C7 C8 C10 125.7(3) . . ? C7 C8 Fe2 65.6(2) . . ? C10 C8 Fe2 123.7(2) . . ? C11 C10 C15 118.1(4) . . ? C11 C10 C8 124.0(3) . . ? C15 C10 C8 117.7(3) . . ? C12 C11 C10 120.2(4) . . ? C13 C12 C11 120.7(4) . . ? C12 C13 C14 119.9(4) . . ? C13 C14 C15 120.4(4) . . ? C14 C15 C10 120.6(4) . . ? C21 C20 C25 117.8(4) . . ? C21 C20 P1 122.9(3) . . ? C25 C20 P1 119.3(3) . . ? C20 C21 C22 120.3(4) . . ? C23 C22 C21 120.7(4) . . ? C24 C23 C22 119.6(4) . . ? C23 C24 C25 120.4(4) . . ? C24 C25 C20 121.1(4) . . ? C35 C30 C31 118.2(3) . . ? C35 C30 P1 123.1(3) . . ? C31 C30 P1 118.7(3) . . ? C32 C31 C30 120.9(3) . . ? C33 C32 C31 119.9(4) . . ? C34 C33 C32 119.4(4) . . ? C33 C34 C35 121.0(4) . . ? C34 C35 C30 120.5(4) . . ? _refine_diff_density_max 0.532 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.077 # [Fe2(CO)5(PPh3)(m-HC=CHPh)(m-PPh2)] 3a data_sd92 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H42 Fe2 O6 P2' _chemical_formula_weight 876.45 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' '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.8886(11) _cell_length_b 12.9963(8) _cell_length_c 19.5996(13) _cell_angle_alpha 90.00 _cell_angle_beta 104.807(2) _cell_angle_gamma 90.00 _cell_volume 4159.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 12362 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 28.59 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.823 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.638 _exptl_absorpt_correction_T_max 0.976 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25146 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.0885 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.84 _reflns_number_total 9775 _reflns_number_gt 6434 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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^)+(0.0516P)^2^+4.9239P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom except H1&2 coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00015(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9775 _refine_ls_number_parameters 548 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.1150 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1470 _refine_ls_wR_factor_gt 0.1277 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.003 _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 0.31032(3) 0.51778(4) 0.23617(3) 0.01923(14) Uani 1 1 d . . . Fe2 Fe 0.18683(3) 0.39333(4) 0.23701(3) 0.02286(15) Uani 1 1 d . . . C1 C 0.3074(2) 0.3674(3) 0.2341(2) 0.0211(8) Uani 1 1 d . . . H1 H 0.311(2) 0.331(3) 0.191(2) 0.025 Uiso 1 1 d . . . C2 C 0.2967(2) 0.2992(3) 0.2866(2) 0.0232(9) Uani 1 1 d . . . H2 H 0.308(2) 0.320(3) 0.334(2) 0.028 Uiso 1 1 d . . . C3 C 0.3000(2) 0.1853(3) 0.2830(2) 0.0250(9) Uani 1 1 d . . . C4 C 0.2990(3) 0.1312(3) 0.2213(2) 0.0395(12) Uani 1 1 d . . . H4 H 0.2932 0.1676 0.1783 0.047 Uiso 1 1 calc R . . C5 C 0.3062(4) 0.0251(4) 0.2222(3) 0.0526(14) Uani 1 1 d . . . H5 H 0.3054 -0.0109 0.1798 0.063 Uiso 1 1 calc R . . C6 C 0.3145(4) -0.0287(4) 0.2845(3) 0.0545(15) Uani 1 1 d . . . H6 H 0.3188 -0.1016 0.2849 0.065 Uiso 1 1 calc R . . C7 C 0.3166(4) 0.0233(4) 0.3455(3) 0.0522(14) Uani 1 1 d . . . H7 H 0.3227 -0.0136 0.3883 0.063 Uiso 1 1 calc R . . C8 C 0.3100(3) 0.1292(3) 0.3453(2) 0.0360(11) Uani 1 1 d . . . H8 H 0.3122 0.1644 0.3882 0.043 Uiso 1 1 calc R . . C9 C 0.4123(2) 0.5364(3) 0.2849(2) 0.0224(8) Uani 1 1 d . . . O9 O 0.47892(18) 0.5456(2) 0.31741(16) 0.0352(7) Uani 1 1 d . . . C10 C 0.2781(3) 0.6485(3) 0.2168(2) 0.0291(9) Uani 1 1 d . . . O10 O 0.2595(2) 0.7324(2) 0.20337(17) 0.0440(9) Uani 1 1 d . . . C11 C 0.1558(3) 0.3111(4) 0.1604(2) 0.0314(10) Uani 1 1 d . . . O11 O 0.1336(2) 0.2597(3) 0.11246(17) 0.0486(9) Uani 1 1 d . . . C12 C 0.1213(3) 0.4920(4) 0.1917(2) 0.0349(10) Uani 1 1 d . . . O12 O 0.0762(2) 0.5533(3) 0.16188(18) 0.0511(9) Uani 1 1 d . . . C13 C 0.1282(3) 0.3299(3) 0.2888(2) 0.0310(10) Uani 1 1 d . . . O13 O 0.0923(2) 0.2894(3) 0.32301(17) 0.0481(9) Uani 1 1 d . . . P1 P 0.33878(6) 0.51018(7) 0.12992(5) 0.0191(2) Uani 1 1 d . . . C14 C 0.2512(2) 0.4724(3) 0.0587(2) 0.0238(8) Uani 1 1 d . . . C15 C 0.2490(3) 0.3807(3) 0.0206(2) 0.0326(10) Uani 1 1 d . . . H15 H 0.2959 0.3375 0.0300 0.039 Uiso 1 1 calc R . . C16 C 0.1795(3) 0.3519(4) -0.0304(2) 0.0429(12) Uani 1 1 d . . . H16 H 0.1792 0.2896 -0.0558 0.052 Uiso 1 1 calc R . . C17 C 0.1109(3) 0.4133(4) -0.0444(2) 0.0426(12) Uani 1 1 d . . . H17 H 0.0635 0.3941 -0.0800 0.051 Uiso 1 1 calc R . . C18 C 0.1111(3) 0.5027(4) -0.0067(2) 0.0400(12) Uani 1 1 d . . . H18 H 0.0636 0.5450 -0.0163 0.048 Uiso 1 1 calc R . . C19 C 0.1799(2) 0.5316(3) 0.0451(2) 0.0310(10) Uani 1 1 d . . . H19 H 0.1786 0.5925 0.0716 0.037 Uiso 1 1 calc R . . C20 C 0.3739(2) 0.6345(3) 0.10373(19) 0.0191(8) Uani 1 1 d . . . C21 C 0.3265(2) 0.6993(3) 0.0531(2) 0.0273(9) Uani 1 1 d . . . H21 H 0.2752 0.6762 0.0248 0.033 Uiso 1 1 calc R . . C22 C 0.3540(3) 0.7982(3) 0.0437(2) 0.0322(10) Uani 1 1 d . . . H22 H 0.3209 0.8429 0.0098 0.039 Uiso 1 1 calc R . . C23 C 0.4296(3) 0.8314(3) 0.0840(2) 0.0319(10) Uani 1 1 d . . . H23 H 0.4479 0.8991 0.0779 0.038 Uiso 1 1 calc R . . C24 C 0.4783(3) 0.7663(3) 0.1329(2) 0.0299(9) Uani 1 1 d . . . H24 H 0.5306 0.7886 0.1595 0.036 Uiso 1 1 calc R . . C25 C 0.4510(2) 0.6687(3) 0.1431(2) 0.0248(9) Uani 1 1 d . . . H25 H 0.4846 0.6244 0.1769 0.030 Uiso 1 1 calc R . . C26 C 0.4216(2) 0.4250(3) 0.1189(2) 0.0214(8) Uani 1 1 d . . . C27 C 0.4660(2) 0.3639(3) 0.1735(2) 0.0250(9) Uani 1 1 d . . . H27 H 0.4552 0.3671 0.2187 0.030 Uiso 1 1 calc R . . C28 C 0.5262(3) 0.2982(3) 0.1621(2) 0.0334(10) Uani 1 1 d . . . H28 H 0.5566 0.2568 0.1997 0.040 Uiso 1 1 calc R . . C29 C 0.5420(3) 0.2926(3) 0.0966(2) 0.0340(10) Uani 1 1 d . . . H29 H 0.5821 0.2459 0.0887 0.041 Uiso 1 1 calc R . . C30 C 0.4997(3) 0.3550(3) 0.0423(2) 0.0314(10) Uani 1 1 d . . . H30 H 0.5113 0.3519 -0.0026 0.038 Uiso 1 1 calc R . . C31 C 0.4402(3) 0.4219(3) 0.0531(2) 0.0286(9) Uani 1 1 d . . . H31 H 0.4121 0.4657 0.0160 0.034 Uiso 1 1 calc R . . P2 P 0.24487(6) 0.50951(8) 0.32003(5) 0.0216(2) Uani 1 1 d . . . C32 C 0.1814(2) 0.6163(3) 0.3361(2) 0.0270(9) Uani 1 1 d . . . C33 C 0.0992(3) 0.6041(4) 0.3304(3) 0.0449(12) Uani 1 1 d . . . H33 H 0.0741 0.5391 0.3173 0.054 Uiso 1 1 calc R . . C34 C 0.0518(3) 0.6871(5) 0.3437(3) 0.0632(17) Uani 1 1 d . . . H34 H -0.0051 0.6781 0.3394 0.076 Uiso 1 1 calc R . . C35 C 0.0877(4) 0.7808(4) 0.3630(3) 0.0600(16) Uani 1 1 d . . . H35 H 0.0556 0.8366 0.3723 0.072 Uiso 1 1 calc R . . C36 C 0.1688(3) 0.7940(4) 0.3689(3) 0.0490(13) Uani 1 1 d . . . H36 H 0.1934 0.8592 0.3820 0.059 Uiso 1 1 calc R . . C37 C 0.2163(3) 0.7124(4) 0.3559(2) 0.0387(11) Uani 1 1 d . . . H37 H 0.2732 0.7223 0.3606 0.046 Uiso 1 1 calc R . . C38 C 0.2885(2) 0.4652(3) 0.41079(19) 0.0227(8) Uani 1 1 d . . . C39 C 0.2368(3) 0.4465(4) 0.4549(2) 0.0342(10) Uani 1 1 d . . . H39 H 0.1797 0.4595 0.4388 0.041 Uiso 1 1 calc R . . C40 C 0.2696(3) 0.4088(4) 0.5227(2) 0.0409(12) Uani 1 1 d . . . H40 H 0.2343 0.3961 0.5525 0.049 Uiso 1 1 calc R . . C41 C 0.3522(3) 0.3893(3) 0.5474(2) 0.0349(10) Uani 1 1 d . . . H41 H 0.3735 0.3632 0.5938 0.042 Uiso 1 1 calc R . . C42 C 0.4035(3) 0.4081(3) 0.5042(2) 0.0307(10) Uani 1 1 d . . . H42 H 0.4605 0.3947 0.5207 0.037 Uiso 1 1 calc R . . C43 C 0.3719(3) 0.4468(3) 0.4365(2) 0.0271(9) Uani 1 1 d . . . H43 H 0.4078 0.4608 0.4074 0.032 Uiso 1 1 calc R . . C44 C -0.1000(6) 0.5106(8) 0.2489(6) 0.150(4) Uani 1 1 d DU . . H44A H -0.1250 0.4604 0.2124 0.225 Uiso 0.360(19) 1 calc PR A 1 H44B H -0.0492 0.5368 0.2399 0.225 Uiso 0.360(19) 1 calc PR A 1 H44C H -0.1381 0.5678 0.2480 0.225 Uiso 0.360(19) 1 calc PR A 1 H44D H -0.1074 0.4720 0.2048 0.225 Uiso 0.640(19) 1 calc PR A 2 H44E H -0.0486 0.5494 0.2582 0.225 Uiso 0.640(19) 1 calc PR A 2 H44F H -0.1459 0.5585 0.2449 0.225 Uiso 0.640(19) 1 calc PR A 2 C45 C -0.077(3) 0.448(2) 0.3361(12) 0.177(9) Uani 0.360(19) 1 d PDU A 1 H45A H -0.1109 0.3850 0.3305 0.212 Uiso 0.360(19) 1 calc PR A 1 H45B H -0.0193 0.4254 0.3463 0.212 Uiso 0.360(19) 1 calc PR A 1 O14 O -0.086(2) 0.493(2) 0.3926(10) 0.197(10) Uiso 0.360(19) 1 d PDU A 1 C46 C -0.033(2) 0.414(3) 0.4609(15) 0.230(10) Uani 0.360(19) 1 d PDU A 1 H46A H 0.0239 0.4032 0.4583 0.275 Uiso 0.360(19) 1 calc PR A 1 H46B H -0.0326 0.4447 0.5074 0.275 Uiso 0.360(19) 1 calc PR A 1 C47 C -0.079(3) 0.320(3) 0.4498(17) 0.207(13) Uani 0.360(19) 1 d PDU A 1 H47A H -0.0438 0.2630 0.4729 0.311 Uiso 0.360(19) 1 calc PR A 1 H47B H -0.0979 0.3057 0.3991 0.311 Uiso 0.360(19) 1 calc PR A 1 H47C H -0.1263 0.3254 0.4699 0.311 Uiso 0.360(19) 1 calc PR A 1 C45X C -0.0967(19) 0.4216(14) 0.3212(12) 0.203(7) Uani 0.640(19) 1 d PDU A 2 H45C H -0.1539 0.4002 0.3178 0.244 Uiso 0.640(19) 1 calc PR A 2 H45D H -0.0673 0.3594 0.3118 0.244 Uiso 0.640(19) 1 calc PR A 2 O14X O -0.0647(14) 0.4474(19) 0.3865(8) 0.216(7) Uiso 0.640(19) 1 d PDU A 2 C46X C -0.0466(14) 0.3259(15) 0.4251(11) 0.183(7) Uani 0.640(19) 1 d PDU A 2 H46C H -0.0518 0.2719 0.3887 0.220 Uiso 0.640(19) 1 calc PR A 2 H46D H 0.0089 0.3222 0.4575 0.220 Uiso 0.640(19) 1 calc PR A 2 C47X C -0.1083(10) 0.3142(10) 0.4631(7) 0.115(6) Uani 0.640(19) 1 d PDU A 2 H47D H -0.1085 0.2430 0.4794 0.173 Uiso 0.640(19) 1 calc PR A 2 H47E H -0.1621 0.3309 0.4319 0.173 Uiso 0.640(19) 1 calc PR A 2 H47F H -0.0966 0.3607 0.5038 0.173 Uiso 0.640(19) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0235(3) 0.0170(3) 0.0193(3) 0.0009(2) 0.0092(2) 0.0009(2) Fe2 0.0234(3) 0.0267(3) 0.0203(3) 0.0012(2) 0.0090(2) -0.0014(2) C1 0.0194(19) 0.020(2) 0.023(2) -0.0029(16) 0.0056(15) -0.0017(15) C2 0.027(2) 0.022(2) 0.023(2) -0.0009(17) 0.0112(17) 0.0013(16) C3 0.029(2) 0.022(2) 0.026(2) -0.0009(17) 0.0116(17) -0.0010(16) C4 0.068(3) 0.026(2) 0.030(2) 0.0018(19) 0.022(2) 0.000(2) C5 0.092(4) 0.024(3) 0.046(3) -0.010(2) 0.025(3) 0.001(3) C6 0.086(4) 0.019(3) 0.052(3) -0.003(2) 0.007(3) -0.002(3) C7 0.087(4) 0.029(3) 0.035(3) 0.009(2) 0.004(3) -0.004(3) C8 0.060(3) 0.024(2) 0.024(2) -0.0008(18) 0.011(2) -0.006(2) C9 0.031(2) 0.017(2) 0.022(2) 0.0014(15) 0.0126(18) -0.0026(16) O9 0.0322(18) 0.0390(19) 0.0324(17) 0.0015(14) 0.0044(14) -0.0079(14) C10 0.037(2) 0.030(2) 0.024(2) 0.0001(18) 0.0149(18) -0.0011(19) O10 0.074(2) 0.0220(17) 0.043(2) 0.0068(14) 0.0292(18) 0.0123(16) C11 0.029(2) 0.040(3) 0.027(2) 0.001(2) 0.0121(19) -0.0073(19) O11 0.056(2) 0.059(2) 0.0328(19) -0.0144(17) 0.0149(16) -0.0230(18) C12 0.028(2) 0.047(3) 0.032(2) 0.004(2) 0.0111(19) -0.004(2) O12 0.041(2) 0.065(3) 0.045(2) 0.0178(19) 0.0072(16) 0.0165(18) C13 0.034(2) 0.035(3) 0.024(2) -0.0007(19) 0.0065(19) -0.0025(19) O13 0.046(2) 0.061(2) 0.042(2) 0.0126(17) 0.0206(17) -0.0105(17) P1 0.0228(5) 0.0170(5) 0.0191(5) 0.0026(4) 0.0085(4) 0.0005(4) C14 0.025(2) 0.026(2) 0.022(2) 0.0034(17) 0.0095(16) -0.0052(16) C15 0.037(2) 0.034(3) 0.028(2) -0.0022(19) 0.0104(19) -0.004(2) C16 0.042(3) 0.050(3) 0.036(3) -0.010(2) 0.009(2) -0.011(2) C17 0.034(3) 0.059(3) 0.030(3) 0.005(2) 0.000(2) -0.012(2) C18 0.025(2) 0.051(3) 0.044(3) 0.022(2) 0.009(2) 0.000(2) C19 0.030(2) 0.030(2) 0.034(2) 0.0103(19) 0.0110(19) -0.0032(18) C20 0.026(2) 0.0153(19) 0.0196(19) 0.0019(15) 0.0127(16) 0.0004(15) C21 0.025(2) 0.027(2) 0.032(2) 0.0025(18) 0.0123(18) -0.0004(17) C22 0.037(2) 0.024(2) 0.039(3) 0.0151(19) 0.015(2) 0.0056(18) C23 0.039(3) 0.020(2) 0.041(3) 0.0011(19) 0.017(2) -0.0041(18) C24 0.037(2) 0.024(2) 0.031(2) -0.0041(18) 0.0134(19) -0.0078(18) C25 0.028(2) 0.025(2) 0.024(2) 0.0038(17) 0.0118(17) -0.0016(17) C26 0.025(2) 0.017(2) 0.025(2) -0.0032(16) 0.0109(16) -0.0024(15) C27 0.025(2) 0.022(2) 0.028(2) 0.0021(17) 0.0083(17) 0.0012(16) C28 0.036(2) 0.025(2) 0.040(3) 0.0017(19) 0.011(2) 0.0055(19) C29 0.030(2) 0.029(2) 0.047(3) -0.006(2) 0.016(2) 0.0028(19) C30 0.036(2) 0.029(2) 0.036(2) -0.0075(19) 0.022(2) -0.0053(19) C31 0.032(2) 0.026(2) 0.031(2) 0.0030(18) 0.0126(18) 0.0008(18) P2 0.0255(5) 0.0218(5) 0.0203(5) 0.0012(4) 0.0110(4) 0.0038(4) C32 0.032(2) 0.027(2) 0.025(2) 0.0011(17) 0.0115(18) 0.0080(18) C33 0.040(3) 0.037(3) 0.068(4) 0.001(2) 0.031(3) 0.009(2) C34 0.047(3) 0.059(4) 0.094(5) -0.003(3) 0.037(3) 0.018(3) C35 0.068(4) 0.043(3) 0.078(4) -0.011(3) 0.036(3) 0.023(3) C36 0.069(4) 0.033(3) 0.049(3) -0.012(2) 0.022(3) 0.009(3) C37 0.053(3) 0.034(3) 0.035(3) -0.004(2) 0.021(2) 0.007(2) C38 0.034(2) 0.019(2) 0.0172(19) 0.0000(15) 0.0107(17) -0.0017(16) C39 0.032(2) 0.049(3) 0.025(2) 0.001(2) 0.0138(19) -0.002(2) C40 0.046(3) 0.053(3) 0.030(2) 0.003(2) 0.020(2) -0.010(2) C41 0.053(3) 0.033(3) 0.019(2) 0.0044(19) 0.010(2) -0.005(2) C42 0.036(2) 0.027(2) 0.028(2) -0.0006(18) 0.0070(19) 0.0020(18) C43 0.034(2) 0.026(2) 0.025(2) -0.0009(17) 0.0137(18) 0.0030(18) C44 0.102(7) 0.172(10) 0.160(9) -0.030(6) 0.006(7) -0.032(7) C45 0.167(16) 0.120(15) 0.279(13) 0.080(13) 0.123(14) -0.028(13) C46 0.30(2) 0.185(19) 0.246(12) 0.021(18) 0.151(18) -0.045(17) C47 0.31(3) 0.25(3) 0.13(2) -0.001(19) 0.17(2) -0.10(2) C45X 0.149(14) 0.162(13) 0.343(15) 0.061(10) 0.144(13) 0.043(12) C46X 0.272(19) 0.119(14) 0.237(14) -0.017(10) 0.208(12) -0.002(12) C47X 0.189(14) 0.103(9) 0.080(8) -0.046(7) 0.084(8) -0.124(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 C9 1.760(4) . ? Fe1 C10 1.794(4) . ? Fe1 C1 1.955(4) . ? Fe1 P2 2.2054(11) . ? Fe1 P1 2.2558(11) . ? Fe1 Fe2 2.6427(8) . ? Fe2 C12 1.776(5) . ? Fe2 C13 1.790(4) . ? Fe2 C11 1.808(5) . ? Fe2 C1 2.079(4) . ? Fe2 C2 2.228(4) . ? Fe2 P2 2.2524(12) . ? C1 C2 1.405(5) . ? C2 C3 1.484(5) . ? C3 C4 1.394(6) . ? C3 C8 1.395(6) . ? C4 C5 1.385(6) . ? C5 C6 1.382(7) . ? C6 C7 1.366(7) . ? C7 C8 1.381(6) . ? C9 O9 1.149(5) . ? C10 O10 1.147(5) . ? C11 O11 1.136(5) . ? C12 O12 1.152(5) . ? C13 O13 1.141(5) . ? P1 C14 1.823(4) . ? P1 C26 1.839(4) . ? P1 C20 1.839(4) . ? C14 C19 1.395(6) . ? C14 C15 1.402(6) . ? C15 C16 1.384(6) . ? C16 C17 1.376(7) . ? C17 C18 1.376(7) . ? C18 C19 1.386(6) . ? C20 C21 1.389(5) . ? C20 C25 1.405(5) . ? C21 C22 1.394(6) . ? C22 C23 1.387(6) . ? C23 C24 1.381(6) . ? C24 C25 1.381(5) . ? C26 C27 1.388(5) . ? C26 C31 1.404(5) . ? C27 C28 1.390(6) . ? C28 C29 1.379(6) . ? C29 C30 1.383(6) . ? C30 C31 1.385(6) . ? P2 C32 1.829(4) . ? P2 C38 1.836(4) . ? C32 C33 1.374(6) . ? C32 C37 1.393(6) . ? C33 C34 1.406(7) . ? C34 C35 1.370(8) . ? C35 C36 1.357(7) . ? C36 C37 1.393(6) . ? C38 C43 1.391(6) . ? C38 C39 1.397(5) . ? C39 C40 1.391(6) . ? C40 C41 1.377(6) . ? C41 C42 1.380(6) . ? C42 C43 1.392(6) . ? C44 C45X 1.819(18) . ? C44 C45 1.841(18) . ? C45 O14 1.29(2) . ? O14 C46 1.74(2) . ? C46 C47 1.44(2) . ? C45X O14X 1.30(2) . ? O14X C46X 1.74(2) . ? C46X C47X 1.436(18) . ? 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 C9 Fe1 C10 100.75(19) . . ? C9 Fe1 C1 99.48(16) . . ? C10 Fe1 C1 159.57(18) . . ? C9 Fe1 P2 102.08(12) . . ? C10 Fe1 P2 91.25(13) . . ? C1 Fe1 P2 87.27(12) . . ? C9 Fe1 P1 95.60(12) . . ? C10 Fe1 P1 88.29(13) . . ? C1 Fe1 P1 86.95(12) . . ? P2 Fe1 P1 162.08(5) . . ? C9 Fe1 Fe2 138.16(12) . . ? C10 Fe1 Fe2 112.57(14) . . ? C1 Fe1 Fe2 51.15(11) . . ? P2 Fe1 Fe2 54.47(3) . . ? P1 Fe1 Fe2 109.49(3) . . ? C12 Fe2 C13 104.5(2) . . ? C12 Fe2 C11 90.0(2) . . ? C13 Fe2 C11 96.54(19) . . ? C12 Fe2 C1 126.34(17) . . ? C13 Fe2 C1 128.98(18) . . ? C11 Fe2 C1 87.67(17) . . ? C12 Fe2 C2 163.26(17) . . ? C13 Fe2 C2 91.14(17) . . ? C11 Fe2 C2 94.01(18) . . ? C1 Fe2 C2 37.87(14) . . ? C12 Fe2 P2 88.71(15) . . ? C13 Fe2 P2 95.78(14) . . ? C11 Fe2 P2 167.54(13) . . ? C1 Fe2 P2 83.11(11) . . ? C2 Fe2 P2 83.85(11) . . ? C12 Fe2 Fe1 86.97(14) . . ? C13 Fe2 Fe1 146.85(14) . . ? C11 Fe2 Fe1 114.73(13) . . ? C1 Fe2 Fe1 47.06(11) . . ? C2 Fe2 Fe1 76.58(10) . . ? P2 Fe2 Fe1 52.83(3) . . ? C2 C1 Fe1 128.5(3) . . ? C2 C1 Fe2 76.8(2) . . ? Fe1 C1 Fe2 81.79(14) . . ? C1 C2 C3 125.6(4) . . ? C1 C2 Fe2 65.3(2) . . ? C3 C2 Fe2 124.4(3) . . ? C4 C3 C8 117.9(4) . . ? C4 C3 C2 123.5(4) . . ? C8 C3 C2 118.5(4) . . ? C5 C4 C3 120.7(4) . . ? C6 C5 C4 120.2(5) . . ? C7 C6 C5 119.8(5) . . ? C6 C7 C8 120.5(5) . . ? C7 C8 C3 120.9(4) . . ? O9 C9 Fe1 178.0(4) . . ? O10 C10 Fe1 177.9(4) . . ? O11 C11 Fe2 177.7(4) . . ? O12 C12 Fe2 177.3(4) . . ? O13 C13 Fe2 178.5(4) . . ? C14 P1 C26 103.94(18) . . ? C14 P1 C20 106.23(18) . . ? C26 P1 C20 100.76(16) . . ? C14 P1 Fe1 113.33(12) . . ? C26 P1 Fe1 118.84(13) . . ? C20 P1 Fe1 112.29(12) . . ? C19 C14 C15 117.6(4) . . ? C19 C14 P1 119.3(3) . . ? C15 C14 P1 122.8(3) . . ? C16 C15 C14 121.0(4) . . ? C17 C16 C15 120.3(5) . . ? C16 C17 C18 119.7(4) . . ? C17 C18 C19 120.6(4) . . ? C18 C19 C14 120.8(4) . . ? C21 C20 C25 119.0(3) . . ? C21 C20 P1 124.3(3) . . ? C25 C20 P1 116.4(3) . . ? C20 C21 C22 120.1(4) . . ? C23 C22 C21 120.1(4) . . ? C24 C23 C22 120.1(4) . . ? C25 C24 C23 120.1(4) . . ? C24 C25 C20 120.5(4) . . ? C27 C26 C31 119.2(4) . . ? C27 C26 P1 122.1(3) . . ? C31 C26 P1 118.7(3) . . ? C26 C27 C28 120.1(4) . . ? C29 C28 C27 120.4(4) . . ? C28 C29 C30 120.0(4) . . ? C29 C30 C31 120.3(4) . . ? C30 C31 C26 120.0(4) . . ? C32 P2 C38 100.32(17) . . ? C32 P2 Fe1 121.23(13) . . ? C38 P2 Fe1 125.76(13) . . ? C32 P2 Fe2 117.83(14) . . ? C38 P2 Fe2 118.83(13) . . ? Fe1 P2 Fe2 72.71(4) . . ? C33 C32 C37 118.2(4) . . ? C33 C32 P2 121.6(3) . . ? C37 C32 P2 120.2(3) . . ? C32 C33 C34 120.5(5) . . ? C35 C34 C33 120.1(5) . . ? C36 C35 C34 120.1(5) . . ? C35 C36 C37 120.4(5) . . ? C36 C37 C32 120.7(5) . . ? C43 C38 C39 118.7(4) . . ? C43 C38 P2 121.6(3) . . ? C39 C38 P2 119.7(3) . . ? C40 C39 C38 119.5(4) . . ? C41 C40 C39 121.5(4) . . ? C40 C41 C42 119.3(4) . . ? C41 C42 C43 120.1(4) . . ? C38 C43 C42 120.9(4) . . ? C45X C44 C45 16.2(15) . . ? O14 C45 C44 124(2) . . ? C45 O14 C46 104(2) . . ? C47 C46 O14 103.9(18) . . ? O14X C45X C44 121.6(18) . . ? C45X O14X C46X 100.2(18) . . ? C47X C46X O14X 104.5(14) . . ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.770 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.095 # [Fe2(CO)5{P(OMe)3}(m-HC=CHPh)(m-PPh2)] 6 data_str642 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H26 Fe2 O8 P2' _chemical_formula_weight 664.13 _chemical_melting_point ? _chemical_compound_source ? 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' '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 P1 bar loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.954(2) _cell_length_b 11.645(2) _cell_length_c 13.745(2) _cell_angle_alpha 109.43(3) _cell_angle_beta 99.92(3) _cell_angle_gamma 102.79(3) _cell_volume 1553.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 24 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method ? _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 1.081 _exptl_absorpt_correction_type psi scans _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 0.986 _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 Nicolet R3mV _diffrn_measurement_method omega-2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5692 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5382 _reflns_number_observed 3919 _reflns_observed_criterion >2sigma(I) _computing_data_collection Nicolet R3 _computing_cell_refinement Nicolet R3 _computing_data_reduction XDISK _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _refine_special_details ; Refinement on F^2^ for ALL reflections except for 9 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1102P)^2^+1.6876P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5373 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_obs 0.0646 _refine_ls_wR_factor_all 0.1950 _refine_ls_wR_factor_obs 0.1671 _refine_ls_goodness_of_fit_all 1.079 _refine_ls_goodness_of_fit_obs 1.117 _refine_ls_restrained_S_all 1.101 _refine_ls_restrained_S_obs 1.117 _refine_ls_shift/esd_max 0.079 _refine_ls_shift/esd_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe2 Fe 0.24537(7) 0.11902(7) 0.16563(5) 0.0435(2) Uani 1 d . . Fe1 Fe 0.26330(7) 0.16904(7) 0.37018(5) 0.0416(2) Uani 1 d . . P1 P 0.31733(12) 0.00766(12) 0.26147(10) 0.0414(3) Uani 1 d . . P2 P 0.1557(2) 0.3113(2) 0.41815(12) 0.0574(4) Uani 1 d . . O1 O 0.4618(5) 0.2593(5) 0.5737(4) 0.086(2) Uani 1 d . . O2 O 0.0611(5) -0.0223(5) 0.4025(4) 0.0804(14) Uani 1 d . . O3 O -0.0333(4) -0.0063(5) 0.1377(4) 0.0810(14) Uani 1 d . . O4 O 0.1576(6) 0.2978(5) 0.0776(5) 0.112(2) Uani 1 d . . O5 O 0.2945(7) -0.0466(6) -0.0295(4) 0.111(2) Uani 1 d . . O6 O 0.0274(7) 0.2823(8) 0.3261(5) 0.141(3) Uani 1 d . . O7 O 0.2138(6) 0.4545(5) 0.4392(5) 0.099(2) Uani 1 d . . O8 O 0.0862(7) 0.3165(6) 0.5113(5) 0.107(2) Uani 1 d . . C1 C 0.3821(5) 0.2232(5) 0.4943(5) 0.0538(13) Uani 1 d . . C2 C 0.1397(6) 0.0531(6) 0.3906(4) 0.0531(13) Uani 1 d . . C3 C 0.0773(6) 0.0415(5) 0.1521(5) 0.0564(14) Uani 1 d . . C4 C 0.1942(7) 0.2303(6) 0.1137(5) 0.067(2) Uani 1 d . . C5 C 0.2778(7) 0.0203(6) 0.0460(5) 0.066(2) Uani 1 d . . C6 C -0.0719(9) 0.3318(12) 0.3249(12) 0.165(6) Uani 1 d . . H6A H -0.1333(9) 0.2945(12) 0.2557(12) 0.080 Uiso 1 d R . H6B H -0.1137(9) 0.3144(12) 0.3766(12) 0.080 Uiso 1 d R . H6C H -0.0394(9) 0.4224(12) 0.3453(12) 0.080 Uiso 1 d R . C7 C 0.3186(9) 0.5221(13) 0.5162(8) 0.125(4) Uani 1 d . . H7A H 0.3405(9) 0.6072(13) 0.5175(8) 0.080 Uiso 1 d R . H7B H 0.3044(9) 0.5243(13) 0.5838(8) 0.080 Uiso 1 d R . H7C H 0.3885(9) 0.4869(13) 0.5036(8) 0.080 Uiso 1 d R . C8 C 0.1308(10) 0.3017(9) 0.6075(6) 0.100(3) Uani 1 d . . H8A H 0.0678(10) 0.3093(9) 0.6482(6) 0.080 Uiso 1 d R . H8B H 0.1430(10) 0.2189(9) 0.5912(6) 0.080 Uiso 1 d R . H8C H 0.2118(10) 0.3663(9) 0.6486(6) 0.080 Uiso 1 d R . C9 C 0.3607(5) 0.2780(5) 0.3063(4) 0.0457(12) Uani 1 d . . H9 H 0.3421(5) 0.3536(5) 0.3195(4) 0.080 Uiso 1 d R . C10 C 0.4490(5) 0.2549(5) 0.2433(4) 0.0454(12) Uani 1 d . . H10 H 0.4946(5) 0.1959(5) 0.2500(4) 0.080 Uiso 1 d R . C11 C 0.2247(5) -0.1609(5) 0.2289(4) 0.0467(12) Uani 1 d . . C12 C 0.1164(7) -0.2298(6) 0.1407(5) 0.067(2) Uani 1 d . . H12A H 0.0897(7) -0.1906(6) 0.0927(5) 0.080 Uiso 1 d R . C13 C 0.0459(8) -0.3546(7) 0.1216(6) 0.084(2) Uani 1 d . . H13A H -0.0280(8) -0.4008(7) 0.0606(6) 0.080 Uiso 1 d R . C14 C 0.0833(8) -0.4122(7) 0.1887(7) 0.082(2) Uani 1 d . . H14A H 0.0331(8) -0.4971(7) 0.1761(7) 0.080 Uiso 1 d R . C15 C 0.1909(8) -0.3482(7) 0.2753(7) 0.088(2) Uani 1 d . . H15A H 0.2185(8) -0.3898(7) 0.3210(7) 0.080 Uiso 1 d R . C16 C 0.2615(7) -0.2213(6) 0.2956(6) 0.073(2) Uani 1 d . . H16A H 0.3353(7) -0.1757(6) 0.3568(6) 0.080 Uiso 1 d R . C21 C 0.4841(5) -0.0086(5) 0.2721(5) 0.0510(13) Uani 1 d . . C22 C 0.5832(6) 0.0594(7) 0.3680(6) 0.073(2) Uani 1 d . . H22A H 0.5660(6) 0.1171(7) 0.4288(6) 0.080 Uiso 1 d R . C23 C 0.7070(7) 0.0417(9) 0.3747(8) 0.094(3) Uani 1 d . . H23A H 0.7736(7) 0.0859(9) 0.4410(8) 0.080 Uiso 1 d R . C24 C 0.7344(8) -0.0372(10) 0.2886(10) 0.109(4) Uani 1 d . . H24A H 0.8204(8) -0.0451(10) 0.2931(10) 0.080 Uiso 1 d R . C25 C 0.6364(8) -0.1075(8) 0.1927(8) 0.089(3) Uani 1 d . . H25A H 0.6539(8) -0.1666(8) 0.1329(8) 0.080 Uiso 1 d R . C26 C 0.5116(6) -0.0906(7) 0.1843(6) 0.068(2) Uani 1 d . . H26A H 0.4451(6) -0.1353(7) 0.1179(6) 0.080 Uiso 1 d R . C31 C 0.5119(5) 0.3425(5) 0.1938(4) 0.0505(12) Uani 1 d . . C32 C 0.6057(6) 0.3108(7) 0.1399(5) 0.069(2) Uani 1 d . . H32A H 0.6260(6) 0.2330(7) 0.1336(5) 0.080 Uiso 1 d R . C33 C 0.6706(8) 0.3909(9) 0.0948(6) 0.086(2) Uani 1 d . . H33A H 0.7351(8) 0.3687(9) 0.0593(6) 0.080 Uiso 1 d R . C34 C 0.6440(9) 0.5038(9) 0.1042(7) 0.095(3) Uani 1 d . . H34A H 0.6864(9) 0.5575(9) 0.0724(7) 0.080 Uiso 1 d R . C35 C 0.5511(8) 0.5374(8) 0.1572(7) 0.087(2) Uani 1 d . . H35A H 0.5330(8) 0.6164(8) 0.1644(7) 0.080 Uiso 1 d R . C36 C 0.4863(7) 0.4577(6) 0.2011(6) 0.069(2) Uani 1 d . . H36A H 0.4227(7) 0.4815(6) 0.2372(6) 0.080 Uiso 1 d 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 Fe2 0.0458(4) 0.0416(4) 0.0408(4) 0.0148(3) 0.0007(3) 0.0190(3) Fe1 0.0394(4) 0.0413(4) 0.0412(4) 0.0137(3) 0.0046(3) 0.0147(3) P1 0.0384(7) 0.0400(7) 0.0448(7) 0.0157(5) 0.0037(5) 0.0166(5) P2 0.0671(10) 0.0588(9) 0.0514(8) 0.0174(7) 0.0156(7) 0.0351(8) O1 0.078(3) 0.104(4) 0.055(3) 0.018(3) -0.012(2) 0.032(3) O2 0.066(3) 0.070(3) 0.101(4) 0.032(3) 0.033(3) 0.007(2) O3 0.045(2) 0.090(3) 0.086(3) 0.024(3) -0.003(2) 0.010(2) O4 0.131(5) 0.078(3) 0.117(5) 0.048(3) -0.024(4) 0.040(4) O5 0.175(6) 0.130(5) 0.063(3) 0.037(3) 0.045(4) 0.100(5) O6 0.123(5) 0.200(8) 0.101(4) 0.023(5) 0.008(4) 0.123(6) O7 0.103(4) 0.061(3) 0.123(5) 0.022(3) 0.025(4) 0.029(3) O8 0.136(5) 0.126(5) 0.118(5) 0.066(4) 0.082(4) 0.086(4) C1 0.049(3) 0.052(3) 0.055(3) 0.016(3) 0.005(3) 0.017(3) C2 0.052(3) 0.052(3) 0.053(3) 0.015(3) 0.014(3) 0.020(3) C3 0.056(4) 0.049(3) 0.051(3) 0.011(2) -0.004(3) 0.018(3) C4 0.071(4) 0.059(4) 0.061(4) 0.024(3) -0.012(3) 0.021(3) C5 0.092(5) 0.070(4) 0.048(3) 0.027(3) 0.017(3) 0.045(4) C6 0.073(6) 0.157(10) 0.268(16) 0.131(11) -0.028(8) 0.019(7) C7 0.085(6) 0.215(13) 0.111(7) 0.096(8) 0.028(6) 0.059(8) C8 0.133(8) 0.108(7) 0.073(5) 0.036(5) 0.052(5) 0.039(6) C9 0.044(3) 0.038(3) 0.045(3) 0.012(2) -0.001(2) 0.010(2) C10 0.043(3) 0.040(3) 0.050(3) 0.018(2) 0.003(2) 0.012(2) C11 0.045(3) 0.044(3) 0.052(3) 0.017(2) 0.008(2) 0.020(2) C12 0.076(4) 0.046(3) 0.061(4) 0.014(3) -0.005(3) 0.016(3) C13 0.082(5) 0.054(4) 0.087(5) 0.014(4) -0.007(4) 0.008(4) C14 0.085(5) 0.048(4) 0.104(6) 0.027(4) 0.019(4) 0.009(3) C15 0.099(6) 0.064(4) 0.109(6) 0.053(4) 0.012(5) 0.021(4) C16 0.070(4) 0.064(4) 0.083(5) 0.042(4) -0.002(3) 0.016(3) C21 0.044(3) 0.053(3) 0.068(3) 0.033(3) 0.011(3) 0.024(2) C22 0.054(4) 0.082(5) 0.076(4) 0.030(4) -0.006(3) 0.026(3) C23 0.049(4) 0.114(7) 0.127(7) 0.061(6) 0.006(4) 0.032(4) C24 0.050(4) 0.146(9) 0.194(11) 0.117(9) 0.047(6) 0.056(5) C25 0.081(5) 0.104(6) 0.143(8) 0.078(6) 0.069(6) 0.066(5) C26 0.063(4) 0.076(4) 0.079(4) 0.036(4) 0.022(3) 0.038(3) C31 0.048(3) 0.051(3) 0.048(3) 0.018(2) 0.007(2) 0.011(2) C32 0.064(4) 0.065(4) 0.073(4) 0.025(3) 0.022(3) 0.011(3) C33 0.084(5) 0.101(6) 0.074(5) 0.033(4) 0.039(4) 0.016(4) C34 0.100(6) 0.106(6) 0.083(5) 0.061(5) 0.025(5) -0.001(5) C35 0.097(6) 0.078(5) 0.093(5) 0.054(4) 0.019(5) 0.015(4) C36 0.084(5) 0.058(4) 0.079(4) 0.038(3) 0.028(4) 0.026(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe2 C3 1.809(6) . y Fe2 C5 1.810(6) . y Fe2 C4 1.817(6) . y Fe2 C9 2.121(5) . y Fe2 C10 2.261(5) . y Fe2 P1 2.295(2) . y Fe2 Fe1 2.6367(11) . y Fe1 C1 1.777(6) . y Fe1 C2 1.819(6) . y Fe1 C9 1.996(5) . y Fe1 P2 2.230(2) . y Fe1 P1 2.246(2) . y P1 C11 1.860(5) . ? P1 C21 1.864(5) . ? P2 O7 1.554(6) . ? P2 O8 1.590(5) . ? P2 O6 1.607(6) . ? O1 C1 1.155(7) . ? O2 C2 1.162(7) . ? O3 C3 1.167(7) . ? O4 C4 1.163(7) . ? O5 C5 1.144(7) . ? O6 C6 1.339(11) . ? O7 C7 1.298(11) . ? O8 C8 1.409(10) . ? C9 C10 1.417(8) . y C10 C31 1.513(8) . ? C11 C16 1.387(8) . ? C11 C12 1.399(8) . ? C12 C13 1.398(9) . ? C13 C14 1.368(11) . ? C14 C15 1.379(11) . ? C15 C16 1.415(10) . ? C21 C26 1.394(9) . ? C21 C22 1.406(8) . ? C22 C23 1.408(10) . ? C23 C24 1.362(13) . ? C24 C25 1.401(13) . ? C25 C26 1.415(9) . ? C31 C36 1.405(8) . ? C31 C32 1.410(8) . ? C32 C33 1.414(10) . ? C33 C34 1.379(12) . ? C34 C35 1.400(12) . ? C35 C36 1.399(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Fe2 C5 103.8(3) . . ? C3 Fe2 C4 89.4(3) . . ? C5 Fe2 C4 97.7(3) . . ? C3 Fe2 C9 121.4(2) . . ? C5 Fe2 C9 134.5(3) . . ? C4 Fe2 C9 88.1(2) . . ? C3 Fe2 C10 158.8(2) . . ? C5 Fe2 C10 97.0(3) . . ? C4 Fe2 C10 91.6(2) . . ? C9 Fe2 C10 37.5(2) . . ? C3 Fe2 P1 91.9(2) . . ? C5 Fe2 P1 92.1(2) . . ? C4 Fe2 P1 169.5(2) . . ? C9 Fe2 P1 82.27(14) . . ? C10 Fe2 P1 83.45(14) . . ? C3 Fe2 Fe1 82.2(2) . . y C5 Fe2 Fe1 145.7(2) . . y C4 Fe2 Fe1 116.3(2) . . y C9 Fe2 Fe1 48.11(15) . . y C10 Fe2 Fe1 78.37(14) . . y P1 Fe2 Fe1 53.63(4) . . y C1 Fe1 C2 99.2(3) . . ? C1 Fe1 C9 97.7(2) . . ? C2 Fe1 C9 163.1(2) . . ? C1 Fe1 P2 98.1(2) . . ? C2 Fe1 P2 89.4(2) . . ? C9 Fe1 P2 88.6(2) . . ? C1 Fe1 P1 104.0(2) . . ? C2 Fe1 P1 89.2(2) . . ? C9 Fe1 P1 86.4(2) . . ? P2 Fe1 P1 157.83(6) . . y C1 Fe1 Fe2 140.5(2) . . y C2 Fe1 Fe2 112.4(2) . . y C9 Fe1 Fe2 52.31(14) . . y P2 Fe1 Fe2 105.17(6) . . y P1 Fe1 Fe2 55.39(4) . . y C11 P1 C21 99.3(2) . . ? C11 P1 Fe1 120.5(2) . . ? C21 P1 Fe1 125.9(2) . . ? C11 P1 Fe2 120.5(2) . . ? C21 P1 Fe2 120.1(2) . . ? Fe1 P1 Fe2 70.98(5) . . y O7 P2 O8 103.1(3) . . ? O7 P2 O6 97.2(4) . . ? O8 P2 O6 96.6(4) . . ? O7 P2 Fe1 122.6(2) . . ? O8 P2 Fe1 119.9(2) . . ? O6 P2 Fe1 112.4(2) . . ? C6 O6 P2 132.4(8) . . ? C7 O7 P2 119.0(7) . . ? C8 O8 P2 128.3(6) . . ? O1 C1 Fe1 178.2(6) . . ? O2 C2 Fe1 179.1(5) . . ? O3 C3 Fe2 175.5(5) . . ? O4 C4 Fe2 177.5(6) . . ? O5 C5 Fe2 177.0(7) . . ? C10 C9 Fe1 130.5(4) . . y C10 C9 Fe2 76.6(3) . . y Fe1 C9 Fe2 79.6(2) . . y C9 C10 C31 125.8(5) . . ? C9 C10 Fe2 65.9(3) . . y C31 C10 Fe2 121.9(3) . . ? C16 C11 C12 117.8(5) . . ? C16 C11 P1 119.4(4) . . ? C12 C11 P1 122.9(4) . . ? C11 C12 C13 121.1(6) . . ? C14 C13 C12 120.2(7) . . ? C13 C14 C15 120.4(7) . . ? C14 C15 C16 119.5(7) . . ? C11 C16 C15 121.0(6) . . ? C26 C21 C22 119.0(6) . . ? C26 C21 P1 119.9(5) . . ? C22 C21 P1 121.1(5) . . ? C23 C22 C21 119.7(7) . . ? C24 C23 C22 121.3(8) . . ? C23 C24 C25 119.8(7) . . ? C24 C25 C26 119.6(8) . . ? C21 C26 C25 120.4(7) . . ? C36 C31 C32 116.9(6) . . ? C36 C31 C10 124.0(5) . . ? C32 C31 C10 119.0(5) . . ? C31 C32 C33 121.6(7) . . ? C34 C33 C32 120.0(7) . . ? C33 C34 C35 119.5(7) . . ? C36 C35 C34 120.4(8) . . ? C35 C36 C31 121.6(7) . . ? _refine_diff_density_max 1.184 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.099 # [Fe2(CO)4{P(OMe)3}2(m-HC=CHPh)(m-PPh2)] 7 data_str683 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C90 H105 Fe6 O30 P9' _chemical_formula_weight 2280.57 _chemical_melting_point ? _chemical_compound_source ? 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' '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 P1bar loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.462(2) _cell_length_b 17.092(3) _cell_length_c 27.804(6) _cell_angle_alpha 80.91(3) _cell_angle_beta 88.26(3) _cell_angle_gamma 81.62(3) _cell_volume 5321.1(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 13 _cell_measurement_theta_max 23 _exptl_crystal_description orange _exptl_crystal_colour plate _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method ? _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 1.004 _exptl_absorpt_correction_type psi scans _exptl_absorpt_correction_T_min 0.816 _exptl_absorpt_correction_T_max 1.000 _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 Nicolet R3 _diffrn_measurement_method Nicolet R3 _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11664 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 21.00 _reflns_number_total 10961 _reflns_number_observed 7112 _reflns_observed_criterion >2sigma(I) _computing_data_collection Nicolet R3 _computing_cell_refinement Nicolet R3 _computing_data_reduction XDISK _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _refine_special_details ; Refinement on F^2^ for ALL reflections except for 10 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. Hydrogens on the alkenyl ligand were located from difference maps. All others were computed with HADD ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1189P)^2^+13.1708P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10951 _refine_ls_number_parameters 1216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_obs 0.0707 _refine_ls_wR_factor_all 0.2390 _refine_ls_wR_factor_obs 0.1877 _refine_ls_goodness_of_fit_all 1.131 _refine_ls_goodness_of_fit_obs 1.167 _refine_ls_restrained_S_all 1.163 _refine_ls_restrained_S_obs 1.167 _refine_ls_shift/esd_max 0.042 _refine_ls_shift/esd_mean 0.005 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.04084(13) 0.17675(9) 0.44106(6) 0.0493(4) Uani 1 d . . Fe2 Fe 0.03181(13) 0.33057(9) 0.40649(6) 0.0510(4) Uani 1 d . . P1 P -0.1047(2) 0.2506(2) 0.39692(11) 0.0538(8) Uani 1 d . . P2 P 0.1991(3) 0.1358(2) 0.48503(11) 0.0538(8) Uani 1 d . . P3 P -0.0384(3) 0.4383(2) 0.35806(13) 0.0665(9) Uani 1 d . . O1 O -0.1034(9) 0.1610(6) 0.5304(3) 0.105(3) Uani 1 d . . O2 O 0.0186(9) 0.0224(6) 0.4147(4) 0.097(3) Uani 1 d . . O3 O 0.2381(8) 0.3900(5) 0.4392(4) 0.088(3) Uani 1 d . . O4 O -0.0843(9) 0.3677(6) 0.4972(4) 0.097(3) Uani 1 d . . O5 O 0.3191(6) 0.1006(5) 0.4600(3) 0.066(2) Uani 1 d . . O6 O 0.1764(6) 0.0673(4) 0.5293(3) 0.064(2) Uani 1 d . . O7 O 0.2623(7) 0.1977(5) 0.5090(3) 0.069(2) Uani 1 d . . O8 O 0.0096(11) 0.5197(6) 0.3607(5) 0.130(4) Uani 1 d . . O9 O -0.1757(8) 0.4559(5) 0.3576(5) 0.122(4) Uani 1 d . . O10 O -0.0114(10) 0.4414(6) 0.3003(3) 0.110(3) Uani 1 d . . C1 C -0.0481(11) 0.1697(8) 0.4955(5) 0.072(4) Uani 1 d . . C2 C 0.0304(11) 0.0829(8) 0.4249(5) 0.067(3) Uani 1 d . . C3 C 0.1567(12) 0.3670(7) 0.4243(5) 0.070(3) Uani 1 d . . C4 C -0.0402(10) 0.3503(7) 0.4628(5) 0.063(3) Uani 1 d . . C5 C 0.3181(13) 0.0355(9) 0.4326(6) 0.104(5) Uani 1 d . . H5A H 0.3953(13) 0.0204(9) 0.4197(6) 0.080 Uiso 1 d R . H5B H 0.2940(13) -0.0093(9) 0.4538(6) 0.080 Uiso 1 d R . H5C H 0.2633(13) 0.0521(9) 0.4062(6) 0.080 Uiso 1 d R . C6 C 0.2709(11) 0.0275(7) 0.5618(5) 0.079(4) Uani 1 d . . H6A H 0.2409(11) -0.0114(7) 0.5858(5) 0.080 Uiso 1 d R . H6B H 0.3326(11) 0.0013(7) 0.5434(5) 0.080 Uiso 1 d R . H6C H 0.3016(11) 0.0661(7) 0.5776(5) 0.080 Uiso 1 d R . C7 C 0.1986(13) 0.2433(8) 0.5432(5) 0.087(4) Uani 1 d . . H7A H 0.2486(13) 0.2771(8) 0.5543(5) 0.080 Uiso 1 d R . H7B H 0.1312(13) 0.2757(8) 0.5272(5) 0.080 Uiso 1 d R . H7C H 0.1731(13) 0.2080(8) 0.5706(5) 0.080 Uiso 1 d R . C8 C -0.0062(21) 0.5530(10) 0.4069(8) 0.175(11) Uani 1 d . . H8A H 0.0268(21) 0.6021(10) 0.4039(8) 0.080 Uiso 1 d R . H8B H -0.0892(21) 0.5634(10) 0.4135(8) 0.080 Uiso 1 d R . H8C H 0.0316(21) 0.5153(10) 0.4331(8) 0.080 Uiso 1 d R . C9 C -0.2450(14) 0.5175(10) 0.3265(7) 0.136(7) Uani 1 d . . H9A H -0.3273(14) 0.5158(10) 0.3333(7) 0.080 Uiso 1 d R . H9B H -0.2253(14) 0.5681(10) 0.3319(7) 0.080 Uiso 1 d R . H9C H -0.2286(14) 0.5110(10) 0.2932(7) 0.080 Uiso 1 d R . C10 C 0.0248(23) 0.5040(12) 0.2672(7) 0.205(13) Uani 1 d . . H10A H 0.0345(23) 0.4889(12) 0.2353(7) 0.080 Uiso 1 d R . H10B H -0.0346(23) 0.5501(12) 0.2662(7) 0.080 Uiso 1 d R . H10C H 0.0981(23) 0.5167(12) 0.2775(7) 0.080 Uiso 1 d R . C31 C 0.1462(10) 0.2291(6) 0.3930(4) 0.058(3) Uani 1 d . . H31 H 0.2235(10) 0.2380(6) 0.4038(4) 0.080 Uiso 1 d R . C32 C 0.1270(10) 0.2738(6) 0.3466(4) 0.059(3) Uani 1 d . . H32 H 0.0580(10) 0.2710(6) 0.3218(4) 0.080 Uiso 1 d R . C33 C 0.2230(12) 0.3080(7) 0.3165(4) 0.068(3) Uani 1 d . . C34 C 0.3338(12) 0.3130(8) 0.3336(6) 0.085(4) Uani 1 d . . H34A H 0.3505(12) 0.2963(8) 0.3676(6) 0.080 Uiso 1 d R . C35 C 0.2048(15) 0.3316(10) 0.2666(6) 0.104(5) Uani 1 d . . H35A H 0.1296(15) 0.3272(10) 0.2538(6) 0.080 Uiso 1 d R . C36 C 0.2910(19) 0.3599(12) 0.2359(6) 0.131(7) Uani 1 d . . H36A H 0.2761(19) 0.3774(12) 0.2018(6) 0.080 Uiso 1 d R . C37 C 0.3975(19) 0.3628(11) 0.2543(9) 0.133(8) Uani 1 d . . H37A H 0.4596(19) 0.3805(11) 0.2333(9) 0.080 Uiso 1 d R . C38 C 0.4177(15) 0.3406(10) 0.3021(7) 0.111(6) Uani 1 d . . H38A H 0.4933(15) 0.3452(10) 0.3145(7) 0.080 Uiso 1 d R . C39 C -0.2513(10) 0.2588(7) 0.4260(4) 0.058(3) Uani 1 d . . C40 C -0.3138(12) 0.3319(9) 0.4311(6) 0.099(5) Uani 1 d . . H40A H -0.2789(12) 0.3795(9) 0.4203(6) 0.080 Uiso 1 d R . C41 C -0.4271(14) 0.3361(12) 0.4521(7) 0.130(7) Uani 1 d . . H41A H -0.4706(14) 0.3873(12) 0.4556(7) 0.080 Uiso 1 d R . C42 C -0.4746(12) 0.2691(14) 0.4670(6) 0.103(6) Uani 1 d . . H42A H -0.5494(12) 0.2715(14) 0.4837(6) 0.080 Uiso 1 d R . C43 C -0.4158(15) 0.2001(13) 0.4595(6) 0.118(7) Uani 1 d . . H43A H -0.4540(15) 0.1533(13) 0.4675(6) 0.080 Uiso 1 d R . C44 C -0.3030(12) 0.1929(10) 0.4390(6) 0.100(5) Uani 1 d . . H44A H -0.2610(12) 0.1414(10) 0.4352(6) 0.080 Uiso 1 d R . C45 C -0.1439(10) 0.2319(7) 0.3367(4) 0.061(3) Uani 1 d . . C46 C -0.0938(12) 0.1636(9) 0.3179(5) 0.082(4) Uani 1 d . . H46A H -0.0364(12) 0.1256(9) 0.3370(5) 0.080 Uiso 1 d R . C47 C -0.1250(13) 0.1510(11) 0.2727(6) 0.099(5) Uani 1 d . . H47A H -0.0909(13) 0.1027(11) 0.2611(6) 0.080 Uiso 1 d R . C48 C -0.2035(15) 0.2042(12) 0.2435(6) 0.101(5) Uani 1 d . . H48A H -0.2230(15) 0.1943(12) 0.2119(6) 0.080 Uiso 1 d R . C49 C -0.2531(14) 0.2696(12) 0.2610(5) 0.099(5) Uani 1 d . . H49A H -0.3091(14) 0.3077(12) 0.2414(5) 0.080 Uiso 1 d R . C50 C -0.2245(12) 0.2849(9) 0.3074(5) 0.088(4) Uani 1 d . . H50A H -0.2609(12) 0.3325(9) 0.3192(5) 0.080 Uiso 1 d R . Fe3 Fe 0.48998(12) 0.74437(8) 0.29440(5) 0.0439(4) Uani 1 d . . Fe4 Fe 0.42576(12) 0.89540(8) 0.30416(5) 0.0448(4) Uani 1 d . . P4 P 0.5940(2) 0.8419(2) 0.26855(10) 0.0440(7) Uani 1 d . . P5 P 0.3588(3) 0.6699(2) 0.32564(12) 0.0574(8) Uani 1 d . . P6 P 0.4449(3) 1.0217(2) 0.28743(12) 0.0567(8) Uani 1 d . . O11 O 0.6031(8) 0.6325(5) 0.2335(3) 0.077(2) Uani 1 d . . O12 O 0.6420(9) 0.6818(6) 0.3794(3) 0.092(3) Uani 1 d . . O13 O 0.5334(7) 0.8640(5) 0.3998(3) 0.077(2) Uani 1 d . . O14 O 0.1985(8) 0.9115(6) 0.3550(3) 0.084(3) Uani 1 d . . O15 O 0.4204(7) 0.5821(4) 0.3476(3) 0.077(2) Uani 1 d . . O16 O 0.2676(7) 0.6955(5) 0.3664(4) 0.087(3) Uani 1 d . . O17 O 0.2558(7) 0.6541(5) 0.2925(4) 0.080(3) Uani 1 d . . O18 O 0.3438(8) 1.0882(5) 0.3025(4) 0.096(3) Uani 1 d . . O19 O 0.5450(9) 1.0439(5) 0.3188(4) 0.103(3) Uani 1 d . . O20 O 0.4748(9) 1.0513(5) 0.2327(3) 0.096(3) Uani 1 d . . C11 C 0.5532(10) 0.6768(7) 0.2568(4) 0.054(3) Uani 1 d . . C12 C 0.5827(10) 0.7068(7) 0.3467(5) 0.058(3) Uani 1 d . . C13 C 0.4927(10) 0.8756(7) 0.3612(5) 0.059(3) Uani 1 d . . C14 C 0.2865(11) 0.9068(7) 0.3343(4) 0.057(3) Uani 1 d . . C15 C 0.3513(14) 0.5205(9) 0.3694(7) 0.114(6) Uani 1 d . . H15A H 0.4027(14) 0.4718(9) 0.3806(7) 0.080 Uiso 1 d R . H15B H 0.3060(14) 0.5379(9) 0.3963(7) 0.080 Uiso 1 d R . H15C H 0.2991(14) 0.5110(9) 0.3452(7) 0.080 Uiso 1 d R . C16 C 0.3086(15) 0.7122(10) 0.4125(5) 0.109(6) Uani 1 d . . H16A H 0.2436(15) 0.7272(10) 0.4333(5) 0.080 Uiso 1 d R . H16B H 0.3563(15) 0.6648(10) 0.4283(5) 0.080 Uiso 1 d R . H16C H 0.3554(15) 0.7549(10) 0.4057(5) 0.080 Uiso 1 d R . C17 C 0.2836(15) 0.6337(11) 0.2449(6) 0.124(7) Uani 1 d . . H17A H 0.2136(15) 0.6259(11) 0.2293(6) 0.080 Uiso 1 d R . H17B H 0.3184(15) 0.6761(11) 0.2256(6) 0.080 Uiso 1 d R . H17C H 0.3387(15) 0.5852(11) 0.2482(6) 0.080 Uiso 1 d R . C18 C 0.2272(12) 1.0993(8) 0.2848(6) 0.095(5) Uani 1 d . . H18A H 0.1803(12) 1.1420(8) 0.2983(6) 0.080 Uiso 1 d R . H18B H 0.2291(12) 1.1126(8) 0.2499(6) 0.080 Uiso 1 d R . H18C H 0.1934(12) 1.0508(8) 0.2938(6) 0.080 Uiso 1 d R . C19 C 0.5539(14) 1.1188(8) 0.3343(6) 0.102(5) Uani 1 d . . H19A H 0.6247(14) 1.1140(8) 0.3528(6) 0.080 Uiso 1 d R . H19B H 0.5560(14) 1.1597(8) 0.3064(6) 0.080 Uiso 1 d R . H19C H 0.4867(14) 1.1329(8) 0.3542(6) 0.080 Uiso 1 d R . C20 C 0.4954(17) 1.1292(9) 0.2118(6) 0.131(7) Uani 1 d . . H20A H 0.5116(17) 1.1305(9) 0.1776(6) 0.080 Uiso 1 d R . H20B H 0.4262(17) 1.1665(9) 0.2162(6) 0.080 Uiso 1 d R . H20C H 0.5613(17) 1.1435(9) 0.2272(6) 0.080 Uiso 1 d R . C51 C 0.3557(9) 0.8198(6) 0.2630(3) 0.047(3) Uani 1 d . . H51 H 0.2968(9) 0.8086(6) 0.2686(3) 0.080 Uiso 1 d R . C52 C 0.3476(8) 0.8937(6) 0.2321(3) 0.042(2) Uani 1 d . . H52 H 0.4208(8) 0.9112(6) 0.2040(3) 0.080 Uiso 1 d R . C53 C 0.2339(9) 0.9393(6) 0.2146(3) 0.047(3) Uani 1 d . . C54 C 0.1232(10) 0.9245(7) 0.2314(5) 0.066(3) Uani 1 d . . H54A H 0.1184(10) 0.8835(7) 0.2590(5) 0.080 Uiso 1 d R . C55 C 0.0226(11) 0.9655(8) 0.2107(5) 0.081(4) Uani 1 d . . H55A H -0.0523(11) 0.9512(8) 0.2223(5) 0.080 Uiso 1 d R . C56 C 0.0269(13) 1.0278(9) 0.1721(6) 0.092(5) Uani 1 d . . H56A H -0.0443(13) 1.0582(9) 0.1580(6) 0.080 Uiso 1 d R . C57 C 0.1343(14) 1.0451(8) 0.1541(5) 0.078(4) Uani 1 d . . H57A H 0.1386(14) 1.0873(8) 0.1272(5) 0.080 Uiso 1 d R . C58 C 0.2370(11) 1.0035(7) 0.1748(4) 0.066(3) Uani 1 d . . H58A H 0.3121(11) 1.0168(7) 0.1626(4) 0.080 Uiso 1 d R . C59 C 0.7419(9) 0.8325(5) 0.2939(4) 0.051(3) Uani 1 d . . C60 C 0.8219(10) 0.7652(6) 0.2900(4) 0.061(3) Uani 1 d . . H60A H 0.7980(10) 0.7238(6) 0.2745(4) 0.080 Uiso 1 d R . C61 C 0.9349(11) 0.7565(9) 0.3082(6) 0.085(4) Uani 1 d . . H61A H 0.9900(11) 0.7105(9) 0.3031(6) 0.080 Uiso 1 d R . C62 C 0.9699(11) 0.8106(9) 0.3328(5) 0.084(4) Uani 1 d . . H62A H 1.0472(11) 0.8017(9) 0.3467(5) 0.080 Uiso 1 d R . C63 C 0.8940(11) 0.8773(9) 0.3377(5) 0.077(4) Uani 1 d . . H63A H 0.9193(11) 0.9164(9) 0.3548(5) 0.080 Uiso 1 d R . C64 C 0.7775(10) 0.8922(6) 0.3176(4) 0.059(3) Uani 1 d . . H64A H 0.7250(10) 0.9406(6) 0.3201(4) 0.080 Uiso 1 d R . C65 C 0.6237(9) 0.8721(7) 0.2038(4) 0.055(3) Uani 1 d . . C66 C 0.5765(10) 0.8368(7) 0.1677(4) 0.059(3) Uani 1 d . . H66A H 0.5317(10) 0.7935(7) 0.1773(4) 0.080 Uiso 1 d R . C67 C 0.5951(12) 0.8632(8) 0.1188(5) 0.077(4) Uani 1 d . . H67A H 0.5641(12) 0.8384(8) 0.0942(5) 0.080 Uiso 1 d R . C68 C 0.6572(14) 0.9251(10) 0.1053(5) 0.097(5) Uani 1 d . . H68A H 0.6679(14) 0.9446(10) 0.0714(5) 0.080 Uiso 1 d R . C69 C 0.7046(13) 0.9601(9) 0.1396(6) 0.096(5) Uani 1 d . . H69A H 0.7495(13) 1.0032(9) 0.1295(6) 0.080 Uiso 1 d R . C70 C 0.6890(10) 0.9339(7) 0.1887(5) 0.073(4) Uani 1 d . . H70A H 0.7230(10) 0.9580(7) 0.2128(5) 0.080 Uiso 1 d R . Fe5 Fe 0.77630(13) 0.36162(9) 0.05975(5) 0.0483(4) Uani 1 d . . Fe6 Fe 0.84261(12) 0.23625(9) 0.01751(5) 0.0478(4) Uani 1 d . . P7 P 0.6625(2) 0.3124(2) 0.01203(10) 0.0478(7) Uani 1 d . . P8 P 0.9172(3) 0.3615(2) 0.11103(12) 0.0615(8) Uani 1 d . . P9 P 0.8125(3) 0.1587(2) -0.03402(12) 0.0600(8) Uani 1 d . . O21 O 0.6163(8) 0.3253(6) 0.1436(3) 0.088(3) Uani 1 d . . O22 O 0.7130(9) 0.5337(6) 0.0354(4) 0.093(3) Uani 1 d . . O23 O 1.0861(8) 0.1633(6) 0.0400(4) 0.092(3) Uani 1 d . . O24 O 0.7800(8) 0.1473(5) 0.1109(4) 0.084(3) Uani 1 d . . O25 O 1.0387(7) 0.3901(6) 0.0934(3) 0.090(3) Uani 1 d . . O26 O 0.9678(8) 0.2715(5) 0.1386(3) 0.087(3) Uani 1 d . . O27 O 0.8886(9) 0.4045(7) 0.1576(3) 0.103(3) Uani 1 d . . O28 O 0.7206(10) 0.0997(6) -0.0163(4) 0.121(4) Uani 1 d . . O29 O 0.7678(10) 0.2072(5) -0.0846(3) 0.108(4) Uani 1 d . . O30 O 0.9108(9) 0.0919(7) -0.0482(5) 0.118(4) Uani 1 d . . C21 C 0.6779(10) 0.3416(7) 0.1106(4) 0.052(3) Uani 1 d . . C22 C 0.7368(10) 0.4651(7) 0.0458(4) 0.057(3) Uani 1 d . . C23 C 0.9906(11) 0.1947(6) 0.0304(4) 0.052(3) Uani 1 d . . C24 C 0.8013(10) 0.1837(7) 0.0731(5) 0.059(3) Uani 1 d . . C25 C 1.0445(16) 0.4682(8) 0.0734(7) 0.127(6) Uani 1 d . . H25A H 1.1251(16) 0.4739(8) 0.0654(7) 0.080 Uiso 1 d R . H25B H 0.9981(16) 0.4804(8) 0.0443(7) 0.080 Uiso 1 d R . H25C H 1.0147(16) 0.5042(8) 0.0956(7) 0.080 Uiso 1 d R . C26 C 1.0533(14) 0.2568(10) 0.1746(6) 0.111(5) Uani 1 d . . H26A H 1.0714(14) 0.2004(10) 0.1860(6) 0.080 Uiso 1 d R . H26B H 1.1234(14) 0.2772(10) 0.1616(6) 0.080 Uiso 1 d R . H26C H 1.0236(14) 0.2837(10) 0.2013(6) 0.080 Uiso 1 d R . C27 C 0.8053(15) 0.4663(10) 0.1635(6) 0.114(6) Uani 1 d . . H27A H 0.8098(15) 0.4794(10) 0.1957(6) 0.080 Uiso 1 d R . H27B H 0.8172(15) 0.5119(10) 0.1399(6) 0.080 Uiso 1 d R . H27C H 0.7291(15) 0.4518(10) 0.1590(6) 0.080 Uiso 1 d R . C28 C 0.6996(17) 0.0316(9) -0.0353(6) 0.120(6) Uani 1 d . . H28A H 0.6378(17) 0.0082(9) -0.0168(6) 0.080 Uiso 1 d R . H28B H 0.6763(17) 0.0466(9) -0.0688(6) 0.080 Uiso 1 d R . H28C H 0.7702(17) -0.0065(9) -0.0332(6) 0.080 Uiso 1 d R . C29 C 0.7553(16) 0.1774(10) -0.1293(5) 0.116(6) Uani 1 d . . H29A H 0.7249(16) 0.2206(10) -0.1542(5) 0.080 Uiso 1 d R . H29B H 0.8318(16) 0.1537(10) -0.1390(5) 0.080 Uiso 1 d R . H29C H 0.7029(16) 0.1378(10) -0.1249(5) 0.080 Uiso 1 d R . C30 C 1.0195(15) 0.0965(11) -0.0636(7) 0.133(7) Uani 1 d . . H30A H 1.0594(15) 0.0454(11) -0.0692(7) 0.080 Uiso 1 d R . H30B H 1.0155(15) 0.1335(11) -0.0935(7) 0.080 Uiso 1 d R . H30C H 1.0619(15) 0.1162(11) -0.0399(7) 0.080 Uiso 1 d R . C71 C 0.8990(10) 0.3484(6) 0.0088(4) 0.055(3) Uani 1 d . . H71 H 0.9802(10) 0.3505(6) 0.0128(4) 0.080 Uiso 1 d R . C72 C 0.8888(9) 0.3337(6) -0.0388(4) 0.054(3) Uani 1 d . . H72 H 0.8185(9) 0.3495(6) -0.0570(4) 0.080 Uiso 1 d R . C73 C 0.9888(10) 0.3241(7) -0.0740(4) 0.060(3) Uani 1 d . . C74 C 1.1064(10) 0.3143(7) -0.0614(5) 0.066(3) Uani 1 d . . H74A H 1.1260(10) 0.3152(7) -0.0282(5) 0.080 Uiso 1 d R . C75 C 1.1951(12) 0.3049(9) -0.0948(6) 0.094(5) Uani 1 d . . H75A H 1.2765(12) 0.2949(9) -0.0855(6) 0.080 Uiso 1 d R . C76 C 1.1647(15) 0.3084(10) -0.1438(7) 0.107(6) Uani 1 d . . H76A H 1.2256(15) 0.3042(10) -0.1681(7) 0.080 Uiso 1 d R . C77 C 1.0519(14) 0.3179(9) -0.1577(5) 0.091(4) Uani 1 d . . H77A H 1.0329(14) 0.3183(9) -0.1912(5) 0.080 Uiso 1 d R . C78 C 0.9624(11) 0.3273(7) -0.1234(4) 0.069(3) Uani 1 d . . H78A H 0.8814(11) 0.3358(7) -0.1333(4) 0.080 Uiso 1 d R . C79 C 0.5285(9) 0.2746(7) 0.0384(4) 0.053(3) Uani 1 d . . C80 C 0.4329(10) 0.3295(9) 0.0466(5) 0.087(5) Uani 1 d . . H80A H 0.4379(10) 0.3858(9) 0.0405(5) 0.080 Uiso 1 d R . C81 C 0.3315(12) 0.2999(13) 0.0669(6) 0.109(6) Uani 1 d . . H81A H 0.2617(12) 0.3368(13) 0.0710(6) 0.080 Uiso 1 d R . C82 C 0.3290(15) 0.2187(14) 0.0799(5) 0.107(6) Uani 1 d . . H82A H 0.2597(15) 0.2001(14) 0.0951(5) 0.080 Uiso 1 d R . C83 C 0.4264(17) 0.1654(10) 0.0713(6) 0.112(6) Uani 1 d . . H83A H 0.4218(17) 0.1091(10) 0.0787(6) 0.080 Uiso 1 d R . C84 C 0.5252(11) 0.1915(9) 0.0517(5) 0.083(4) Uani 1 d . . H84A H 0.5944(11) 0.1541(9) 0.0476(5) 0.080 Uiso 1 d R . C85 C 0.6022(8) 0.3673(7) -0.0461(4) 0.049(3) Uani 1 d . . C86 C 0.6241(10) 0.4445(7) -0.0639(4) 0.060(3) Uani 1 d . . H86A H 0.6687(10) 0.4714(7) -0.0447(4) 0.080 Uiso 1 d R . C87 C 0.5805(12) 0.4830(8) -0.1095(5) 0.080(4) Uani 1 d . . H87A H 0.5934(12) 0.5370(8) -0.1211(5) 0.080 Uiso 1 d R . C88 C 0.5207(11) 0.4455(9) -0.1381(5) 0.076(4) Uani 1 d . . H88A H 0.4958(11) 0.4710(9) -0.1702(5) 0.080 Uiso 1 d R . C89 C 0.4974(11) 0.3698(9) -0.1200(5) 0.080(4) Uani 1 d . . H89A H 0.4500(11) 0.3444(9) -0.1390(5) 0.080 Uiso 1 d R . C90 C 0.5380(10) 0.3300(8) -0.0748(5) 0.067(3) Uani 1 d . . H90A H 0.5229(10) 0.2763(8) -0.0636(5) 0.080 Uiso 1 d 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 0.0431(9) 0.0509(9) 0.0545(10) -0.0056(7) 0.0043(7) -0.0126(7) Fe2 0.0459(9) 0.0502(9) 0.0583(10) -0.0073(7) -0.0034(8) -0.0122(7) P1 0.042(2) 0.064(2) 0.057(2) -0.0107(15) -0.0009(14) -0.0142(14) P2 0.050(2) 0.058(2) 0.054(2) -0.0029(14) -0.0003(14) -0.0146(14) P3 0.067(2) 0.052(2) 0.079(2) -0.004(2) -0.010(2) -0.009(2) O1 0.109(8) 0.124(8) 0.062(6) 0.017(6) 0.038(6) 0.010(6) O2 0.102(8) 0.065(6) 0.131(9) -0.022(6) -0.002(6) -0.023(5) O3 0.071(6) 0.091(7) 0.110(7) -0.018(5) -0.012(5) -0.037(5) O4 0.092(7) 0.118(8) 0.091(7) -0.051(6) 0.032(6) -0.016(6) O5 0.056(5) 0.065(5) 0.074(5) -0.003(4) -0.001(4) -0.001(4) O6 0.063(5) 0.063(5) 0.063(5) 0.006(4) -0.004(4) -0.018(4) O7 0.062(5) 0.064(5) 0.083(6) -0.004(4) -0.017(4) -0.021(4) O8 0.171(11) 0.082(7) 0.144(10) 0.005(7) -0.049(9) -0.051(7) O9 0.075(6) 0.075(6) 0.183(11) 0.058(7) -0.014(7) 0.015(5) O10 0.131(9) 0.119(8) 0.071(6) 0.000(6) 0.009(6) -0.006(7) C1 0.063(8) 0.083(9) 0.061(8) 0.018(7) 0.007(7) -0.014(7) C2 0.068(8) 0.061(8) 0.081(9) -0.015(7) 0.010(7) -0.030(7) C3 0.068(9) 0.061(8) 0.084(9) -0.022(7) 0.017(7) -0.012(7) C4 0.048(7) 0.060(8) 0.085(10) -0.016(7) 0.000(7) -0.010(6) C5 0.077(10) 0.110(12) 0.112(12) -0.011(10) -0.003(9) 0.026(9) C6 0.086(10) 0.071(8) 0.077(9) 0.007(7) -0.016(8) -0.018(7) C7 0.104(11) 0.091(10) 0.075(9) -0.027(8) -0.020(8) -0.018(9) C8 0.271(29) 0.070(11) 0.190(22) -0.037(13) -0.097(21) -0.006(14) C9 0.096(12) 0.106(13) 0.176(18) 0.038(13) -0.014(12) 0.027(10) C10 0.318(36) 0.146(19) 0.136(19) 0.040(16) 0.072(21) -0.064(21) C31 0.069(8) 0.060(7) 0.045(7) -0.005(6) 0.012(6) -0.014(6) C32 0.063(8) 0.058(7) 0.056(8) -0.004(6) 0.004(6) -0.020(6) C33 0.088(10) 0.064(8) 0.051(8) 0.000(6) 0.012(7) -0.021(7) C34 0.074(10) 0.080(9) 0.095(11) 0.005(8) 0.029(9) -0.018(8) C35 0.108(12) 0.129(13) 0.082(12) -0.003(10) 0.006(10) -0.058(11) C36 0.128(16) 0.183(20) 0.075(11) 0.025(11) 0.025(12) -0.057(15) C37 0.119(17) 0.119(14) 0.159(21) -0.011(14) 0.086(16) -0.039(13) C38 0.083(11) 0.133(14) 0.119(15) -0.002(12) 0.034(11) -0.050(10) C39 0.048(7) 0.048(7) 0.073(8) 0.003(6) -0.012(6) -0.003(6) C40 0.065(9) 0.080(10) 0.130(13) 0.053(9) -0.005(9) -0.011(8) C41 0.067(11) 0.124(14) 0.168(18) 0.036(13) 0.047(11) 0.021(10) C42 0.044(9) 0.183(19) 0.080(11) -0.003(12) 0.014(8) -0.027(11) C43 0.082(12) 0.167(18) 0.138(15) -0.085(14) 0.052(11) -0.067(12) C44 0.072(10) 0.124(13) 0.119(13) -0.042(10) 0.033(9) -0.049(9) C45 0.046(7) 0.076(8) 0.065(8) -0.009(7) -0.013(6) -0.023(6) C46 0.078(9) 0.110(11) 0.062(9) -0.027(8) -0.003(7) -0.006(8) C47 0.073(10) 0.148(15) 0.091(12) -0.059(11) -0.004(9) -0.018(10) C48 0.083(11) 0.171(17) 0.061(10) -0.042(11) 0.002(9) -0.032(11) C49 0.084(11) 0.162(16) 0.054(9) -0.011(10) -0.013(8) -0.030(11) C50 0.083(10) 0.089(10) 0.093(11) -0.018(8) -0.014(9) -0.007(8) Fe3 0.0375(8) 0.0457(9) 0.0490(9) -0.0059(7) -0.0020(7) -0.0094(7) Fe4 0.0357(8) 0.0497(9) 0.0506(9) -0.0112(7) -0.0022(7) -0.0076(7) P4 0.0348(15) 0.048(2) 0.050(2) -0.0097(13) -0.0018(13) -0.0091(12) P5 0.048(2) 0.053(2) 0.069(2) 0.0024(15) 0.002(2) -0.0137(14) P6 0.049(2) 0.049(2) 0.073(2) -0.014(2) -0.005(2) -0.0042(14) O11 0.085(6) 0.064(5) 0.076(6) -0.018(5) -0.003(5) 0.015(5) O12 0.096(7) 0.106(7) 0.072(6) -0.007(5) -0.047(6) -0.004(6) O13 0.074(6) 0.099(7) 0.061(6) -0.022(5) -0.019(5) -0.010(5) O14 0.051(5) 0.126(8) 0.083(6) -0.038(6) 0.015(5) -0.019(5) O15 0.065(5) 0.046(4) 0.110(7) 0.018(4) 0.004(5) -0.014(4) O16 0.065(6) 0.089(6) 0.102(7) -0.006(5) 0.037(5) -0.014(5) O17 0.055(5) 0.079(6) 0.106(7) 0.007(5) -0.013(5) -0.028(4) O18 0.072(6) 0.074(6) 0.141(9) -0.032(6) -0.018(6) 0.009(5) O19 0.107(7) 0.056(5) 0.157(10) -0.031(6) -0.055(7) -0.016(5) O20 0.151(9) 0.063(6) 0.077(6) 0.000(5) 0.017(6) -0.039(6) C11 0.044(7) 0.047(7) 0.071(8) -0.011(6) -0.008(6) -0.002(5) C12 0.052(7) 0.056(7) 0.069(8) -0.018(6) -0.005(7) -0.011(6) C13 0.047(7) 0.070(8) 0.060(8) -0.010(6) -0.016(6) -0.008(6) C14 0.046(7) 0.062(7) 0.072(8) -0.030(6) 0.002(6) -0.013(6) C15 0.117(13) 0.077(10) 0.149(15) -0.006(10) 0.020(12) -0.031(10) C16 0.140(15) 0.104(12) 0.083(11) -0.021(9) 0.057(11) -0.026(10) C17 0.124(14) 0.130(14) 0.133(16) 0.005(12) -0.054(13) -0.081(12) C18 0.090(11) 0.060(8) 0.132(13) -0.023(8) -0.051(10) 0.021(7) C19 0.121(13) 0.079(10) 0.113(12) -0.007(9) -0.028(10) -0.038(9) C20 0.197(20) 0.089(12) 0.113(14) 0.011(10) -0.018(13) -0.065(13) C51 0.043(6) 0.061(7) 0.044(6) -0.017(6) -0.003(5) -0.015(5) C52 0.043(6) 0.048(6) 0.034(6) -0.005(5) -0.001(5) -0.009(5) C53 0.054(7) 0.060(7) 0.026(6) -0.009(5) -0.013(5) -0.006(6) C54 0.039(7) 0.078(8) 0.080(9) -0.007(7) -0.007(7) -0.011(6) C55 0.051(8) 0.091(10) 0.098(11) -0.021(9) -0.010(8) 0.008(7) C56 0.066(10) 0.098(11) 0.102(12) -0.011(10) -0.037(9) 0.024(9) C57 0.092(11) 0.070(9) 0.066(9) 0.002(7) -0.027(8) 0.005(8) C58 0.073(9) 0.066(8) 0.061(8) -0.018(7) -0.018(7) -0.003(7) C59 0.039(6) 0.029(6) 0.085(8) -0.011(5) 0.004(6) -0.009(5) C60 0.063(8) 0.045(7) 0.078(8) -0.029(6) -0.012(7) 0.007(6) C61 0.040(8) 0.093(10) 0.127(12) -0.049(10) 0.005(8) 0.006(7) C62 0.038(7) 0.098(11) 0.106(11) 0.006(9) -0.014(7) -0.001(8) C63 0.063(9) 0.103(11) 0.075(9) -0.015(8) -0.026(7) -0.034(8) C64 0.066(8) 0.047(7) 0.068(8) -0.023(6) 0.008(6) -0.009(6) C65 0.033(6) 0.062(7) 0.066(8) -0.003(6) 0.011(6) -0.003(5) C66 0.052(7) 0.060(7) 0.067(9) -0.018(6) 0.008(6) -0.010(6) C67 0.075(9) 0.091(10) 0.063(9) -0.011(7) 0.004(7) -0.010(8) C68 0.107(12) 0.127(14) 0.053(9) 0.007(9) 0.016(9) -0.032(11) C69 0.087(11) 0.096(11) 0.101(13) 0.015(10) 0.031(10) -0.041(9) C70 0.064(8) 0.074(8) 0.089(10) -0.011(7) 0.013(7) -0.038(7) Fe5 0.0414(9) 0.0566(10) 0.0485(9) -0.0103(7) -0.0047(7) -0.0098(7) Fe6 0.0404(9) 0.0511(9) 0.0521(10) -0.0076(7) -0.0056(7) -0.0063(7) P7 0.037(2) 0.058(2) 0.049(2) -0.0061(14) -0.0039(13) -0.0104(13) P8 0.049(2) 0.079(2) 0.060(2) -0.016(2) -0.011(2) -0.013(2) P9 0.054(2) 0.062(2) 0.067(2) -0.021(2) -0.004(2) -0.006(2) O21 0.074(6) 0.135(8) 0.055(6) -0.002(5) 0.013(5) -0.031(6) O22 0.108(8) 0.069(6) 0.099(7) -0.017(5) -0.030(6) 0.004(6) O23 0.055(6) 0.097(7) 0.112(8) 0.000(6) -0.029(5) 0.018(5) O24 0.090(7) 0.077(6) 0.081(7) 0.007(5) 0.002(5) -0.019(5) O25 0.068(6) 0.110(8) 0.097(7) -0.012(6) -0.010(5) -0.036(5) O26 0.090(6) 0.086(6) 0.084(6) 0.003(5) -0.042(6) -0.022(5) O27 0.086(7) 0.142(9) 0.090(7) -0.067(7) -0.018(6) 0.014(6) O28 0.148(10) 0.116(8) 0.135(9) -0.076(7) 0.041(8) -0.083(8) O29 0.160(10) 0.082(6) 0.081(7) -0.032(5) -0.056(7) 0.021(6) O30 0.057(6) 0.143(10) 0.165(11) -0.079(8) 0.003(7) 0.011(6) C21 0.046(7) 0.069(7) 0.041(7) -0.006(6) -0.013(6) -0.011(6) C22 0.057(7) 0.049(7) 0.065(8) -0.016(6) -0.014(6) 0.000(6) C23 0.061(8) 0.044(6) 0.054(7) -0.015(5) -0.006(6) -0.004(6) C24 0.050(7) 0.052(7) 0.073(9) -0.006(6) -0.011(6) -0.008(6) C25 0.151(16) 0.062(10) 0.155(17) 0.017(10) 0.004(13) -0.011(10) C26 0.108(12) 0.119(13) 0.094(12) 0.023(10) -0.019(10) -0.013(10) C27 0.132(15) 0.111(13) 0.105(13) -0.049(10) -0.023(11) -0.003(12) C28 0.175(18) 0.101(12) 0.095(12) -0.006(10) 0.009(12) -0.064(12) C29 0.159(16) 0.134(14) 0.068(10) -0.024(9) -0.032(10) -0.053(12) C30 0.112(15) 0.171(18) 0.131(15) -0.112(14) -0.014(12) 0.022(13) C71 0.051(7) 0.068(7) 0.050(7) -0.015(6) 0.008(5) -0.018(6) C72 0.046(7) 0.069(7) 0.047(7) -0.013(6) 0.002(5) -0.009(6) C73 0.054(8) 0.064(7) 0.066(8) -0.019(6) 0.007(6) -0.017(6) C74 0.040(7) 0.082(9) 0.074(8) -0.012(7) 0.018(7) -0.009(6) C75 0.055(9) 0.103(11) 0.110(13) 0.007(9) 0.013(9) 0.003(8) C76 0.083(12) 0.125(13) 0.098(13) 0.003(10) 0.056(11) 0.001(10) C77 0.085(11) 0.107(11) 0.080(10) -0.023(8) 0.038(9) -0.005(9) C78 0.068(8) 0.078(8) 0.063(9) -0.014(7) 0.005(7) -0.009(7) C79 0.044(7) 0.069(8) 0.048(7) -0.011(6) -0.007(5) -0.013(6) C80 0.028(7) 0.095(10) 0.115(11) 0.035(8) 0.009(7) 0.007(7) C81 0.037(8) 0.165(18) 0.115(13) -0.003(12) 0.011(8) -0.003(9) C82 0.078(12) 0.178(19) 0.077(10) -0.002(12) 0.012(9) -0.082(13) C83 0.122(15) 0.087(11) 0.139(15) -0.027(10) 0.041(12) -0.056(11) C84 0.059(8) 0.099(11) 0.100(11) -0.015(8) 0.018(8) -0.038(8) C85 0.035(6) 0.074(8) 0.035(6) -0.004(6) 0.002(5) -0.008(5) C86 0.060(7) 0.061(8) 0.057(8) -0.001(6) -0.007(6) -0.009(6) C87 0.084(10) 0.077(9) 0.071(9) 0.011(8) 0.001(8) -0.006(8) C88 0.067(9) 0.105(11) 0.053(8) -0.011(8) -0.017(7) -0.007(8) C89 0.076(9) 0.098(11) 0.075(10) -0.021(8) -0.019(8) -0.033(8) C90 0.061(8) 0.080(8) 0.068(9) -0.014(7) -0.010(7) -0.032(7) _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 1.754(13) . y Fe1 C1 1.798(14) . y Fe1 C31 1.972(10) . y Fe1 P2 2.184(3) . y Fe1 P1 2.214(3) . y Fe1 Fe2 2.641(2) . y Fe2 C3 1.757(14) . y Fe2 C4 1.803(14) . y Fe2 C31 2.093(11) . y Fe2 P3 2.168(4) . y Fe2 C32 2.235(11) . y Fe2 P1 2.270(3) . y P1 C45 1.835(12) . ? P1 C39 1.839(12) . ? P2 O7 1.601(8) . ? P2 O6 1.602(8) . ? P2 O5 1.603(8) . ? P3 O9 1.559(10) . ? P3 O8 1.582(10) . ? P3 O10 1.621(10) . ? O1 C1 1.143(13) . ? O2 C2 1.142(13) . ? O3 C3 1.173(14) . ? O4 C4 1.130(14) . ? O5 C5 1.45(2) . ? O6 C6 1.449(13) . ? O7 C7 1.440(15) . ? O8 C8 1.48(2) . ? O9 C9 1.41(2) . ? O10 C10 1.40(2) . ? C31 C32 1.396(15) . y C32 C33 1.49(2) . ? C33 C34 1.39(2) . ? C33 C35 1.39(2) . ? C34 C38 1.37(2) . ? C35 C36 1.38(2) . ? C36 C37 1.35(2) . ? C37 C38 1.34(3) . ? C39 C44 1.34(2) . ? C39 C40 1.37(2) . ? C40 C41 1.40(2) . ? C41 C42 1.34(2) . ? C42 C43 1.31(2) . ? C43 C44 1.39(2) . ? C45 C50 1.38(2) . ? C45 C46 1.39(2) . ? C46 C47 1.38(2) . ? C47 C48 1.37(2) . ? C48 C49 1.33(2) . ? C49 C50 1.41(2) . ? Fe3 C11 1.745(13) . y Fe3 C12 1.805(13) . y Fe3 C51 1.984(10) . y Fe3 P5 2.183(3) . y Fe3 P4 2.206(3) . y Fe3 Fe4 2.633(2) . y Fe4 C13 1.744(13) . y Fe4 C14 1.779(13) . y Fe4 C51 2.110(9) . y Fe4 P6 2.177(3) . y Fe4 C52 2.225(9) . y Fe4 P4 2.279(3) . y P4 C65 1.828(11) . ? P4 C59 1.830(10) . ? P5 O16 1.589(9) . ? P5 O15 1.596(8) . ? P5 O17 1.599(9) . ? P6 O20 1.570(9) . ? P6 O19 1.586(9) . ? P6 O18 1.596(9) . ? O11 C11 1.152(12) . ? O12 C12 1.141(13) . ? O13 C13 1.160(12) . ? O14 C14 1.145(12) . ? O15 C15 1.455(15) . ? O16 C16 1.46(2) . ? O17 C17 1.43(2) . ? O18 C18 1.415(14) . ? O19 C19 1.432(15) . ? O20 C20 1.42(2) . ? C51 C52 1.405(13) . y C52 C53 1.471(14) . ? C53 C54 1.382(15) . ? C53 C58 1.43(2) . ? C54 C55 1.35(2) . ? C55 C56 1.39(2) . ? C56 C57 1.37(2) . ? C57 C58 1.37(2) . ? C59 C60 1.380(14) . ? C59 C64 1.412(14) . ? C60 C61 1.38(2) . ? C61 C62 1.35(2) . ? C62 C63 1.35(2) . ? C63 C64 1.43(2) . ? C65 C70 1.39(2) . ? C65 C66 1.41(2) . ? C66 C67 1.38(2) . ? C67 C68 1.36(2) . ? C68 C69 1.37(2) . ? C69 C70 1.38(2) . ? Fe5 C22 1.744(12) . y Fe5 C21 1.802(12) . y Fe5 C71 1.981(10) . y Fe5 P8 2.186(3) . y Fe5 P7 2.224(3) . y Fe5 Fe6 2.611(2) . y Fe6 C24 1.749(14) . y Fe6 C23 1.765(12) . y Fe6 C71 2.087(11) . y Fe6 P9 2.166(3) . y Fe6 C72 2.211(11) . y Fe6 P7 2.270(3) . y P7 C85 1.836(10) . ? P7 C79 1.840(11) . ? P8 O25 1.581(9) . ? P8 O27 1.592(9) . ? P8 O26 1.638(9) . ? P9 O30 1.571(10) . ? P9 O29 1.574(9) . ? P9 O28 1.578(10) . ? O21 C21 1.164(12) . ? O22 C22 1.156(13) . ? O23 C23 1.165(12) . ? O24 C24 1.173(13) . ? O25 C25 1.37(2) . ? O26 C26 1.39(2) . ? O27 C27 1.34(2) . ? O28 C28 1.41(2) . ? O29 C29 1.435(15) . ? O30 C30 1.31(2) . ? C71 C72 1.397(14) . y C72 C73 1.492(15) . ? C73 C74 1.38(2) . ? C73 C78 1.41(2) . ? C74 C75 1.37(2) . ? C75 C76 1.41(2) . ? C76 C77 1.34(2) . ? C77 C78 1.39(2) . ? C79 C80 1.37(2) . ? C79 C84 1.42(2) . ? C80 C81 1.40(2) . ? C81 C82 1.38(2) . ? C82 C83 1.38(2) . ? C83 C84 1.35(2) . ? C85 C90 1.386(14) . ? C85 C86 1.389(15) . ? C86 C87 1.40(2) . ? C87 C88 1.36(2) . ? C88 C89 1.37(2) . ? C89 C90 1.39(2) . ? 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 C1 99.0(6) . . ? C2 Fe1 C31 107.1(5) . . ? C1 Fe1 C31 153.8(5) . . ? C2 Fe1 P2 95.2(4) . . ? C1 Fe1 P2 89.8(4) . . ? C31 Fe1 P2 85.6(4) . . ? C2 Fe1 P1 99.7(4) . . ? C1 Fe1 P1 92.6(4) . . ? C31 Fe1 P1 85.5(4) . . ? P2 Fe1 P1 164.34(13) . . y C2 Fe1 Fe2 143.7(4) . . ? C1 Fe1 Fe2 106.9(4) . . ? C31 Fe1 Fe2 51.5(3) . . ? P2 Fe1 Fe2 109.66(10) . . y P1 Fe1 Fe2 54.90(9) . . ? C3 Fe2 C4 89.3(5) . . ? C3 Fe2 C31 86.9(5) . . ? C4 Fe2 C31 128.7(5) . . ? C3 Fe2 P3 96.3(4) . . ? C4 Fe2 P3 100.4(4) . . ? C31 Fe2 P3 130.9(3) . . ? C3 Fe2 C32 93.9(5) . . ? C4 Fe2 C32 165.3(5) . . ? C31 Fe2 C32 37.5(4) . . ? P3 Fe2 C32 93.5(3) . . ? C3 Fe2 P1 163.4(4) . . ? C4 Fe2 P1 88.9(4) . . ? C31 Fe2 P1 81.4(3) . . ? P3 Fe2 P1 100.24(13) . . ? C32 Fe2 P1 83.9(3) . . ? C3 Fe2 Fe1 110.5(4) . . ? C4 Fe2 Fe1 87.1(4) . . ? C31 Fe2 Fe1 47.5(3) . . ? P3 Fe2 Fe1 152.31(12) . . y C32 Fe2 Fe1 78.2(3) . . ? P1 Fe2 Fe1 52.95(9) . . ? C45 P1 C39 99.9(5) . . ? C45 P1 Fe1 123.2(4) . . ? C39 P1 Fe1 116.2(4) . . ? C45 P1 Fe2 122.0(4) . . ? C39 P1 Fe2 123.7(4) . . ? Fe1 P1 Fe2 72.15(10) . . y O7 P2 O6 105.1(4) . . ? O7 P2 O5 92.7(4) . . ? O6 P2 O5 104.7(4) . . ? O7 P2 Fe1 120.8(3) . . ? O6 P2 Fe1 111.2(3) . . ? O5 P2 Fe1 119.8(3) . . ? O9 P3 O8 107.6(7) . . ? O9 P3 O10 100.3(6) . . ? O8 P3 O10 94.2(7) . . ? O9 P3 Fe2 114.1(4) . . ? O8 P3 Fe2 119.8(4) . . ? O10 P3 Fe2 117.7(4) . . ? C5 O5 P2 119.0(8) . . ? C6 O6 P2 121.2(7) . . ? C7 O7 P2 119.8(8) . . ? C8 O8 P3 118.2(12) . . ? C9 O9 P3 126.2(10) . . ? C10 O10 P3 128.3(13) . . ? O1 C1 Fe1 176.4(12) . . ? O2 C2 Fe1 177.1(11) . . ? O3 C3 Fe2 175.8(12) . . ? O4 C4 Fe2 175.5(11) . . ? C32 C31 Fe1 132.6(9) . . ? C32 C31 Fe2 76.8(7) . . ? Fe1 C31 Fe2 81.0(4) . . y C31 C32 C33 122.8(11) . . ? C31 C32 Fe2 65.7(6) . . ? C33 C32 Fe2 123.8(8) . . ? C34 C33 C35 116.4(12) . . ? C34 C33 C32 124.9(11) . . ? C35 C33 C32 118.5(13) . . ? C38 C34 C33 120.1(15) . . ? C36 C35 C33 122.1(16) . . ? C37 C36 C35 119.1(17) . . ? C38 C37 C36 120.2(17) . . ? C37 C38 C34 122.0(18) . . ? C44 C39 C40 118.7(12) . . ? C44 C39 P1 119.7(10) . . ? C40 C39 P1 121.3(9) . . ? C39 C40 C41 119.8(14) . . ? C42 C41 C40 120.4(16) . . ? C43 C42 C41 118.8(15) . . ? C42 C43 C44 122.8(17) . . ? C39 C44 C43 119.3(16) . . ? C50 C45 C46 116.4(12) . . ? C50 C45 P1 121.8(10) . . ? C46 C45 P1 121.9(9) . . ? C47 C46 C45 120.6(14) . . ? C48 C47 C46 122.8(16) . . ? C49 C48 C47 117.3(14) . . ? C48 C49 C50 121.9(16) . . ? C45 C50 C49 120.9(14) . . ? C11 Fe3 C12 97.6(5) . . ? C11 Fe3 C51 112.4(4) . . ? C12 Fe3 C51 149.9(4) . . ? C11 Fe3 P5 94.3(4) . . ? C12 Fe3 P5 89.9(4) . . ? C51 Fe3 P5 86.4(3) . . ? C11 Fe3 P4 98.0(4) . . ? C12 Fe3 P4 93.1(4) . . ? C51 Fe3 P4 84.5(3) . . ? P5 Fe3 P4 166.81(13) . . y C11 Fe3 Fe4 146.9(4) . . ? C12 Fe3 Fe4 102.5(3) . . ? C51 Fe3 Fe4 52.1(3) . . ? P5 Fe3 Fe4 111.49(11) . . ? P4 Fe3 Fe4 55.33(8) . . ? C13 Fe4 C14 88.4(5) . . ? C13 Fe4 C51 131.2(5) . . ? C14 Fe4 C51 87.3(4) . . ? C13 Fe4 P6 97.7(4) . . ? C14 Fe4 P6 97.7(4) . . ? C51 Fe4 P6 131.1(3) . . ? C13 Fe4 C52 168.3(5) . . ? C14 Fe4 C52 93.8(4) . . ? C51 Fe4 C52 37.7(4) . . ? P6 Fe4 C52 93.4(3) . . ? C13 Fe4 P4 91.2(4) . . ? C14 Fe4 P4 162.8(4) . . ? C51 Fe4 P4 80.0(3) . . ? P6 Fe4 P4 99.48(12) . . y C52 Fe4 P4 83.2(3) . . ? C13 Fe4 Fe3 89.0(4) . . ? C14 Fe4 Fe3 110.0(4) . . ? C51 Fe4 Fe3 47.9(3) . . ? P6 Fe4 Fe3 151.77(11) . . ? C52 Fe4 Fe3 79.5(3) . . ? P4 Fe4 Fe3 52.78(8) . . ? C65 P4 C59 101.0(5) . . ? C65 P4 Fe3 121.8(4) . . ? C59 P4 Fe3 116.8(3) . . ? C65 P4 Fe4 120.7(3) . . ? C59 P4 Fe4 124.5(4) . . ? Fe3 P4 Fe4 71.89(10) . . y O16 P5 O15 104.9(5) . . ? O16 P5 O17 92.0(5) . . ? O15 P5 O17 103.8(5) . . ? O16 P5 Fe3 122.2(4) . . ? O15 P5 Fe3 110.8(3) . . ? O17 P5 Fe3 120.2(4) . . ? O20 P6 O19 106.5(6) . . ? O20 P6 O18 105.5(6) . . ? O19 P6 O18 95.5(5) . . ? O20 P6 Fe4 114.7(4) . . ? O19 P6 Fe4 112.1(4) . . ? O18 P6 Fe4 120.3(4) . . ? C15 O15 P5 121.4(8) . . ? C16 O16 P5 120.8(9) . . ? C17 O17 P5 119.5(9) . . ? C18 O18 P6 123.0(8) . . ? C19 O19 P6 128.6(9) . . ? C20 O20 P6 127.1(10) . . ? O11 C11 Fe3 174.8(10) . . ? O12 C12 Fe3 178.7(10) . . ? O13 C13 Fe4 177.4(10) . . ? O14 C14 Fe4 177.3(11) . . ? C52 C51 Fe3 133.4(8) . . ? C52 C51 Fe4 75.6(6) . . ? Fe3 C51 Fe4 80.0(3) . . y C51 C52 C53 122.3(9) . . ? C51 C52 Fe4 66.7(5) . . ? C53 C52 Fe4 124.8(6) . . ? C54 C53 C58 116.1(10) . . ? C54 C53 C52 126.6(10) . . ? C58 C53 C52 117.2(10) . . ? C55 C54 C53 122.8(12) . . ? C54 C55 C56 120.4(13) . . ? C57 C56 C55 119.2(12) . . ? C56 C57 C58 120.7(13) . . ? C57 C58 C53 120.7(12) . . ? C60 C59 C64 118.3(10) . . ? C60 C59 P4 119.5(8) . . ? C64 C59 P4 122.2(8) . . ? C59 C60 C61 121.2(11) . . ? C62 C61 C60 121.9(12) . . ? C61 C62 C63 118.7(12) . . ? C62 C63 C64 122.4(12) . . ? C59 C64 C63 117.4(10) . . ? C70 C65 C66 117.9(11) . . ? C70 C65 P4 120.4(10) . . ? C66 C65 P4 121.6(8) . . ? C67 C66 C65 120.8(11) . . ? C68 C67 C66 119.7(13) . . ? C67 C68 C69 120.8(13) . . ? C68 C69 C70 120.6(13) . . ? C69 C70 C65 120.2(13) . . ? C22 Fe5 C21 99.2(5) . . ? C22 Fe5 C71 98.1(5) . . ? C21 Fe5 C71 162.7(5) . . ? C22 Fe5 P8 97.8(4) . . ? C21 Fe5 P8 89.2(3) . . ? C71 Fe5 P8 88.2(3) . . ? C22 Fe5 P7 104.1(4) . . ? C21 Fe5 P7 90.6(3) . . ? C71 Fe5 P7 85.6(3) . . ? P8 Fe5 P7 157.86(14) . . y C22 Fe5 Fe6 140.8(4) . . ? C21 Fe5 Fe6 112.7(4) . . ? C71 Fe5 Fe6 51.9(3) . . ? P8 Fe5 Fe6 104.74(11) . . ? P7 Fe5 Fe6 55.30(9) . . ? C24 Fe6 C23 88.8(5) . . ? C24 Fe6 C71 124.8(5) . . ? C23 Fe6 C71 87.1(5) . . ? C24 Fe6 P9 102.8(4) . . ? C23 Fe6 P9 96.7(3) . . ? C71 Fe6 P9 132.4(3) . . ? C24 Fe6 C72 161.8(5) . . ? C23 Fe6 C72 94.3(4) . . ? C71 Fe6 C72 37.8(4) . . ? P9 Fe6 C72 94.7(3) . . ? C24 Fe6 P7 90.0(4) . . ? C23 Fe6 P7 165.8(3) . . ? C71 Fe6 P7 82.0(3) . . ? P9 Fe6 P7 97.39(12) . . y C72 Fe6 P7 82.6(3) . . ? C24 Fe6 Fe5 83.7(4) . . ? C23 Fe6 Fe5 112.2(3) . . ? C71 Fe6 Fe5 48.3(3) . . ? P9 Fe6 Fe5 150.70(11) . . ? C72 Fe6 Fe5 78.6(3) . . ? P7 Fe6 Fe5 53.67(8) . . ? C85 P7 C79 99.2(5) . . ? C85 P7 Fe5 123.8(4) . . ? C79 P7 Fe5 118.5(3) . . ? C85 P7 Fe6 122.4(3) . . ? C79 P7 Fe6 122.6(4) . . ? Fe5 P7 Fe6 71.03(10) . . y O25 P8 O27 101.5(5) . . ? O25 P8 O26 98.7(5) . . ? O27 P8 O26 98.8(6) . . ? O25 P8 Fe5 121.6(4) . . ? O27 P8 Fe5 119.3(4) . . ? O26 P8 Fe5 112.8(3) . . ? O30 P9 O29 103.8(6) . . ? O30 P9 O28 95.0(6) . . ? O29 P9 O28 106.8(7) . . ? O30 P9 Fe6 122.4(4) . . ? O29 P9 Fe6 112.3(4) . . ? O28 P9 Fe6 114.4(4) . . ? C25 O25 P8 121.2(10) . . ? C26 O26 P8 123.3(9) . . ? C27 O27 P8 129.0(10) . . ? C28 O28 P9 128.7(10) . . ? C29 O29 P9 128.2(9) . . ? C30 O30 P9 130.1(12) . . ? O21 C21 Fe5 177.1(10) . . ? O22 C22 Fe5 178.0(11) . . ? O23 C23 Fe6 176.2(10) . . ? O24 C24 Fe6 176.3(10) . . ? C72 C71 Fe5 129.8(8) . . ? C72 C71 Fe6 75.9(6) . . ? Fe5 C71 Fe6 79.8(4) . . y C71 C72 C73 124.9(10) . . ? C71 C72 Fe6 66.3(6) . . ? C73 C72 Fe6 124.0(8) . . ? C74 C73 C78 117.6(11) . . ? C74 C73 C72 124.2(11) . . ? C78 C73 C72 118.2(10) . . ? C75 C74 C73 122.1(13) . . ? C74 C75 C76 118.4(13) . . ? C77 C76 C75 121.6(13) . . ? C76 C77 C78 119.5(15) . . ? C77 C78 C73 120.8(13) . . ? C80 C79 C84 120.8(11) . . ? C80 C79 P7 118.0(9) . . ? C84 C79 P7 121.1(9) . . ? C79 C80 C81 117.4(14) . . ? C82 C81 C80 121.5(15) . . ? C83 C82 C81 119.5(13) . . ? C84 C83 C82 120.7(15) . . ? C83 C84 C79 120.0(14) . . ? C90 C85 C86 118.1(10) . . ? C90 C85 P7 119.7(9) . . ? C86 C85 P7 122.1(8) . . ? C85 C86 C87 120.3(11) . . ? C88 C87 C86 121.6(13) . . ? C87 C88 C89 117.9(12) . . ? C88 C89 C90 122.2(12) . . ? C85 C90 C89 119.9(11) . . ? _refine_diff_density_max 1.277 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.107