data_s92 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H28 Fe P2' _chemical_formula_weight 554.35 _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' '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 8.6164(4) _cell_length_b 18.419(2) _cell_length_c 8.7071(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.283(11) _cell_angle_gamma 90.00 _cell_volume 1355.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method ? _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5442 _diffrn_reflns_av_R_equivalents 0.1434 _diffrn_reflns_av_sigmaI/netI 0.1489 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1969 _reflns_number_observed 1398 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 7 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^)+(0.0255P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1962 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_obs 0.0457 _refine_ls_wR_factor_all 0.1176 _refine_ls_wR_factor_obs 0.0992 _refine_ls_goodness_of_fit_all 0.909 _refine_ls_goodness_of_fit_obs 1.058 _refine_ls_restrained_S_all 1.059 _refine_ls_restrained_S_obs 1.058 _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 0.5000 0.5000 0.0000 0.0277(3) Uani 1 d S . P1 P 0.61421(11) 0.36397(6) 0.27242(12) 0.0273(3) Uani 1 d . . C1 C 0.5182(4) 0.5178(2) 0.2323(4) 0.0281(10) Uani 1 d . . H1 H 0.4344(4) 0.5167(2) 0.2852(4) 0.034 Uiso 1 calc R . C2 C 0.5707(5) 0.5793(2) 0.1642(5) 0.0408(11) Uani 1 d . . H2 H 0.5295(5) 0.6259(2) 0.1657(5) 0.049 Uiso 1 calc R . C3 C 0.6962(5) 0.5588(3) 0.0931(4) 0.0411(12) Uani 1 d . . H3 H 0.7519(5) 0.5892(3) 0.0380(4) 0.049 Uiso 1 calc R . C4 C 0.7236(4) 0.4848(3) 0.1191(4) 0.0353(11) Uani 1 d . . H4 H 0.8010(4) 0.4576(3) 0.0844(4) 0.042 Uiso 1 calc R . C5 C 0.6121(4) 0.4572(2) 0.2086(4) 0.0268(9) Uani 1 d . . C6 C 0.8100(4) 0.4342(2) 0.5298(4) 0.0259(9) Uani 1 d . . H6 H 0.8181(4) 0.4719(2) 0.4607(4) 0.031 Uiso 1 calc R . C7 C 0.8938(4) 0.4378(2) 0.6832(4) 0.0317(10) Uani 1 d . . H7 H 0.9567(4) 0.4780(2) 0.7161(4) 0.038 Uiso 1 calc R . C8 C 0.8844(4) 0.3824(2) 0.7865(5) 0.0328(10) Uani 1 d . . H8 H 0.9404(4) 0.3849(2) 0.8891(5) 0.039 Uiso 1 calc R . C9 C 0.7902(4) 0.3225(2) 0.7356(5) 0.0361(10) Uani 1 d . . H9 H 0.7824(4) 0.2849(2) 0.8050(5) 0.043 Uiso 1 calc R . C10 C 0.7082(4) 0.3185(2) 0.5834(4) 0.0336(10) Uani 1 d . . H10 H 0.6480(4) 0.2774(2) 0.5504(4) 0.040 Uiso 1 calc R . C11 C 0.7139(4) 0.3746(2) 0.4786(4) 0.0236(9) Uani 1 d . . C12 C 0.4102(4) 0.3474(2) 0.2939(4) 0.0236(9) Uani 1 d . . C13 C 0.3411(4) 0.3807(2) 0.4086(4) 0.0284(10) Uani 1 d . . H13 H 0.4009(4) 0.4121(2) 0.4806(4) 0.034 Uiso 1 calc R . C14 C 0.1856(4) 0.3675(2) 0.4159(5) 0.0358(11) Uani 1 d . . H14 H 0.1409(4) 0.3899(2) 0.4927(5) 0.043 Uiso 1 calc R . C15 C 0.0955(4) 0.3211(2) 0.3092(5) 0.0389(11) Uani 1 d . . H15 H -0.0102(4) 0.3131(2) 0.3132(5) 0.047 Uiso 1 calc R . C16 C 0.1611(4) 0.2867(2) 0.1978(5) 0.0439(12) Uani 1 d . . H16 H 0.1007(4) 0.2549(2) 0.1272(5) 0.053 Uiso 1 calc R . C17 C 0.3180(4) 0.2996(2) 0.1912(5) 0.0348(10) Uani 1 d . . H17 H 0.3626(4) 0.2756(2) 0.1163(5) 0.042 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0273(4) 0.0413(6) 0.0127(4) 0.0009(4) -0.0005(3) -0.0115(4) P1 0.0286(6) 0.0300(6) 0.0228(6) -0.0074(5) 0.0041(4) -0.0001(5) C1 0.029(2) 0.033(3) 0.021(2) -0.003(2) 0.002(2) -0.006(2) C2 0.052(3) 0.037(3) 0.026(2) 0.002(2) -0.010(2) -0.013(2) C3 0.043(3) 0.056(3) 0.019(2) 0.008(2) -0.007(2) -0.021(2) C4 0.022(2) 0.070(4) 0.014(2) 0.002(2) 0.002(2) -0.009(2) C5 0.023(2) 0.035(3) 0.019(2) -0.004(2) -0.004(2) -0.009(2) C6 0.030(2) 0.026(2) 0.023(2) -0.001(2) 0.005(2) 0.001(2) C7 0.029(2) 0.034(3) 0.029(2) -0.004(2) -0.003(2) -0.001(2) C8 0.027(2) 0.047(3) 0.024(2) 0.002(2) 0.002(2) 0.008(2) C9 0.040(2) 0.036(3) 0.031(3) 0.009(2) 0.006(2) 0.004(2) C10 0.033(2) 0.030(3) 0.036(3) 0.003(2) 0.001(2) 0.003(2) C11 0.022(2) 0.027(2) 0.023(2) -0.003(2) 0.007(2) 0.005(2) C12 0.028(2) 0.018(2) 0.025(2) -0.001(2) 0.004(2) -0.001(2) C13 0.030(2) 0.028(3) 0.026(2) -0.004(2) 0.004(2) -0.001(2) C14 0.039(2) 0.030(3) 0.041(3) -0.000(2) 0.016(2) -0.002(2) C15 0.029(2) 0.035(3) 0.054(3) -0.001(2) 0.010(2) -0.010(2) C16 0.039(3) 0.045(3) 0.048(3) -0.016(2) 0.007(2) -0.016(2) C17 0.038(2) 0.031(3) 0.037(3) -0.014(2) 0.011(2) -0.007(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 C4 2.021(3) 3_665 ? Fe1 C4 2.021(3) . ? Fe1 C1 2.024(4) . ? Fe1 C1 2.024(4) 3_665 ? Fe1 C3 2.037(4) . ? Fe1 C3 2.037(4) 3_665 ? Fe1 C5 2.041(3) 3_665 ? Fe1 C5 2.041(3) . ? Fe1 C2 2.052(4) . ? Fe1 C2 2.052(4) 3_665 ? P1 C5 1.804(4) . ? P1 C12 1.829(4) . ? P1 C11 1.843(4) . ? C1 C2 1.395(5) . ? C1 C5 1.417(5) . ? C2 C3 1.399(6) . ? C3 C4 1.394(6) . ? C4 C5 1.442(5) . ? C6 C7 1.390(5) . ? C6 C11 1.395(5) . ? C7 C8 1.373(5) . ? C8 C9 1.389(5) . ? C9 C10 1.377(5) . ? C10 C11 1.386(5) . ? C12 C17 1.389(5) . ? C12 C13 1.401(5) . ? C13 C14 1.375(5) . ? C14 C15 1.384(5) . ? C15 C16 1.370(5) . ? C16 C17 1.385(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Fe1 C4 180.0 3_665 . ? C4 Fe1 C1 111.71(14) 3_665 . ? C4 Fe1 C1 68.29(14) . . ? C4 Fe1 C1 68.29(14) 3_665 3_665 ? C4 Fe1 C1 111.71(14) . 3_665 ? C1 Fe1 C1 180.0 . 3_665 ? C4 Fe1 C3 139.8(2) 3_665 . ? C4 Fe1 C3 40.2(2) . . ? C1 Fe1 C3 67.7(2) . . ? C1 Fe1 C3 112.3(2) 3_665 . ? C4 Fe1 C3 40.2(2) 3_665 3_665 ? C4 Fe1 C3 139.8(2) . 3_665 ? C1 Fe1 C3 112.3(2) . 3_665 ? C1 Fe1 C3 67.7(2) 3_665 3_665 ? C3 Fe1 C3 180.0 . 3_665 ? C4 Fe1 C5 41.59(14) 3_665 3_665 ? C4 Fe1 C5 138.41(14) . 3_665 ? C1 Fe1 C5 139.20(14) . 3_665 ? C1 Fe1 C5 40.80(14) 3_665 3_665 ? C3 Fe1 C5 111.1(2) . 3_665 ? C3 Fe1 C5 68.9(2) 3_665 3_665 ? C4 Fe1 C5 138.41(14) 3_665 . ? C4 Fe1 C5 41.59(14) . . ? C1 Fe1 C5 40.80(14) . . ? C1 Fe1 C5 139.20(14) 3_665 . ? C3 Fe1 C5 68.9(2) . . ? C3 Fe1 C5 111.1(2) 3_665 . ? C5 Fe1 C5 180.0 3_665 . ? C4 Fe1 C2 112.5(2) 3_665 . ? C4 Fe1 C2 67.5(2) . . ? C1 Fe1 C2 40.01(15) . . ? C1 Fe1 C2 139.99(15) 3_665 . ? C3 Fe1 C2 40.0(2) . . ? C3 Fe1 C2 140.0(2) 3_665 . ? C5 Fe1 C2 111.7(2) 3_665 . ? C5 Fe1 C2 68.3(2) . . ? C4 Fe1 C2 67.5(2) 3_665 3_665 ? C4 Fe1 C2 112.5(2) . 3_665 ? C1 Fe1 C2 139.99(15) . 3_665 ? C1 Fe1 C2 40.01(15) 3_665 3_665 ? C3 Fe1 C2 140.0(2) . 3_665 ? C3 Fe1 C2 40.0(2) 3_665 3_665 ? C5 Fe1 C2 68.3(2) 3_665 3_665 ? C5 Fe1 C2 111.7(2) . 3_665 ? C2 Fe1 C2 180.0 . 3_665 ? C5 P1 C12 103.8(2) . . ? C5 P1 C11 100.0(2) . . ? C12 P1 C11 101.1(2) . . ? C2 C1 C5 109.6(4) . . ? C2 C1 Fe1 71.1(2) . . ? C5 C1 Fe1 70.2(2) . . ? C1 C2 C3 108.1(4) . . ? C1 C2 Fe1 68.9(2) . . ? C3 C2 Fe1 69.4(2) . . ? C4 C3 C2 108.3(4) . . ? C4 C3 Fe1 69.3(2) . . ? C2 C3 Fe1 70.5(2) . . ? C3 C4 C5 108.8(4) . . ? C3 C4 Fe1 70.5(2) . . ? C5 C4 Fe1 69.9(2) . . ? C1 C5 C4 105.1(4) . . ? C1 C5 P1 132.6(3) . . ? C4 C5 P1 122.3(3) . . ? C1 C5 Fe1 69.0(2) . . ? C4 C5 Fe1 68.5(2) . . ? P1 C5 Fe1 128.0(2) . . ? C7 C6 C11 120.6(4) . . ? C8 C7 C6 120.6(4) . . ? C7 C8 C9 119.1(4) . . ? C10 C9 C8 120.5(4) . . ? C9 C10 C11 121.0(4) . . ? C10 C11 C6 118.2(3) . . ? C10 C11 P1 119.5(3) . . ? C6 C11 P1 121.9(3) . . ? C17 C12 C13 117.9(3) . . ? C17 C12 P1 118.7(3) . . ? C13 C12 P1 123.4(3) . . ? C14 C13 C12 120.6(4) . . ? C13 C14 C15 120.1(4) . . ? C16 C15 C14 120.4(4) . . ? C15 C16 C17 119.4(4) . . ? C16 C17 C12 121.5(4) . . ? _refine_diff_density_max 0.518 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.080