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 Cl3 Fe O P2 Re' _chemical_formula_weight 862.90 _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' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.419(2) _cell_length_b 15.687(3) _cell_length_c 22.166(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3275.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method ? _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 14.052 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\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 2923 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 66.93 _reflns_number_total 2923 _reflns_number_observed 2259 _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 0 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^)+(0.1145P)^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 SHELXL _refine_ls_extinction_coef 0.0 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2923 _refine_ls_number_parameters 195 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0673 _refine_ls_R_factor_obs 0.0534 _refine_ls_wR_factor_all 0.1589 _refine_ls_wR_factor_obs 0.1515 _refine_ls_goodness_of_fit_all 1.060 _refine_ls_goodness_of_fit_obs 1.160 _refine_ls_restrained_S_all 1.065 _refine_ls_restrained_S_obs 1.166 _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 Re1 Re 0.0000 0.94203(2) 0.2500 0.0328(2) Uani 1 d SD . Fe1 Fe 0.0000 0.66446(10) 0.2500 0.0389(5) Uani 1 d S . Cl1 Cl 0.0669(2) 1.05315(10) 0.31650(8) 0.0458(5) Uani 1 d . . Cl2 Cl 0.2282(3) 0.9221(3) 0.2243(2) 0.0266(7) Uani 0.50 d PD 1 O1 O 0.1775(11) 0.9255(9) 0.2247(7) 0.0266(7) Uani 0.50 d PD 2 P1 P 0.0500(2) 0.84298(10) 0.33556(6) 0.0231(4) Uani 1 d . . C1 C -0.1445(8) 0.7134(5) 0.3098(3) 0.044(2) Uani 1 d . . H1 H -0.2158(8) 0.7527(5) 0.3016(3) 0.053 Uiso 1 calc R . C2 C -0.1600(12) 0.6234(5) 0.3075(4) 0.069(3) Uani 1 d . . H2 H -0.2413(12) 0.5935(5) 0.2967(4) 0.083 Uiso 1 calc R . C3 C -0.0299(13) 0.5887(5) 0.3245(5) 0.070(3) Uani 1 d . . H3 H -0.0111(13) 0.5307(5) 0.3277(5) 0.084 Uiso 1 calc R . C4 C 0.0706(10) 0.6549(4) 0.3364(3) 0.048(2) Uani 1 d . . H4 H 0.1647(10) 0.6484(4) 0.3482(3) 0.057 Uiso 1 calc R . C5 C -0.0040(6) 0.7337(4) 0.3264(3) 0.0296(14) Uani 1 d . . C6 C 0.2359(6) 0.8417(4) 0.3560(3) 0.0272(13) Uani 1 d . . C7 C 0.3326(8) 0.7884(6) 0.3274(4) 0.056(2) Uani 1 d . . H7 H 0.3013(8) 0.7517(6) 0.2972(4) 0.067 Uiso 1 calc R . C8 C 0.4737(8) 0.7890(8) 0.3431(5) 0.066(3) Uani 1 d . . H8 H 0.5367(8) 0.7520(8) 0.3242(5) 0.079 Uiso 1 calc R . C9 C 0.5221(8) 0.8451(6) 0.3870(4) 0.054(2) Uani 1 d . . H9 H 0.6180(8) 0.8473(6) 0.3967(4) 0.065 Uiso 1 calc R . C10 C 0.4287(9) 0.8961(6) 0.4153(4) 0.059(2) Uani 1 d . . H10 H 0.4609(9) 0.9328(6) 0.4453(4) 0.070 Uiso 1 calc R . C11 C 0.2861(8) 0.8952(5) 0.4009(3) 0.046(2) Uani 1 d . . H11 H 0.2235(8) 0.9306(5) 0.4215(3) 0.055 Uiso 1 calc R . C12 C -0.0422(8) 0.8698(4) 0.4064(3) 0.0359(15) Uani 1 d . . C13 C -0.0391(14) 0.8110(7) 0.4520(5) 0.086(4) Uani 1 d . . H13 H 0.0073(14) 0.7594(7) 0.4460(5) 0.103 Uiso 1 calc R . C14 C -0.1034(18) 0.8273(8) 0.5062(5) 0.113(6) Uani 1 d . . H14 H -0.0949(18) 0.7881(8) 0.5375(5) 0.136 Uiso 1 calc R . C15 C -0.1800(12) 0.9001(6) 0.5150(4) 0.073(3) Uani 1 d . . H15 H -0.2273(12) 0.9096(6) 0.5512(4) 0.088 Uiso 1 calc R . C16 C -0.1857(9) 0.9583(5) 0.4700(3) 0.051(2) Uani 1 d . . H16 H -0.2340(9) 1.0093(5) 0.4758(3) 0.062 Uiso 1 calc R . C17 C -0.1206(8) 0.9422(4) 0.4162(3) 0.038(2) Uani 1 d . . H17 H -0.1297(8) 0.9817(4) 0.3851(3) 0.046 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 Re1 0.0540(4) 0.0114(3) 0.0331(3) 0.000 -0.0160(2) 0.000 Fe1 0.0614(11) 0.0137(8) 0.0414(9) 0.000 -0.0205(7) 0.000 Cl1 0.0703(13) 0.0249(8) 0.0424(10) -0.0153(7) 0.0095(9) -0.0162(8) Cl2 0.022(2) 0.0281(12) 0.0297(12) 0.0034(11) 0.008(2) 0.000(2) O1 0.022(2) 0.0281(12) 0.0297(12) 0.0034(11) 0.008(2) 0.000(2) P1 0.0294(8) 0.0190(7) 0.0208(7) -0.0006(6) 0.0012(6) -0.0008(6) C1 0.049(4) 0.035(4) 0.049(4) 0.011(3) -0.004(3) -0.016(3) C2 0.107(8) 0.044(5) 0.055(5) 0.020(4) -0.020(5) -0.033(5) C3 0.131(10) 0.021(4) 0.058(6) 0.015(4) -0.022(6) -0.016(5) C4 0.073(5) 0.028(4) 0.042(4) 0.007(3) -0.032(4) 0.010(4) C5 0.032(3) 0.026(3) 0.031(3) 0.003(3) -0.008(2) 0.004(3) C6 0.028(3) 0.028(3) 0.025(3) 0.002(2) -0.001(2) -0.001(3) C7 0.035(4) 0.080(6) 0.052(5) -0.029(4) -0.012(3) 0.000(4) C8 0.033(4) 0.107(9) 0.057(6) -0.025(6) 0.002(4) -0.002(5) C9 0.036(4) 0.063(6) 0.064(6) 0.004(5) -0.010(4) -0.011(4) C10 0.056(5) 0.055(5) 0.066(5) -0.015(4) -0.032(5) -0.007(4) C11 0.047(4) 0.047(4) 0.045(4) -0.011(3) -0.013(3) 0.012(4) C12 0.048(4) 0.032(4) 0.028(3) -0.002(3) 0.006(3) -0.008(3) C13 0.134(10) 0.060(7) 0.065(6) 0.026(5) 0.046(7) 0.041(6) C14 0.203(17) 0.089(8) 0.048(6) 0.034(6) 0.060(8) 0.041(9) C15 0.118(9) 0.066(6) 0.035(5) -0.007(4) 0.030(5) -0.012(6) C16 0.065(5) 0.052(4) 0.037(4) -0.019(4) 0.009(4) -0.001(4) C17 0.053(4) 0.040(4) 0.023(3) -0.007(3) 0.003(3) -0.004(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 Re1 O1 1.782(10) 3 ? Re1 O1 1.783(10) . ? Re1 Cl2 2.245(3) 3 ? Re1 Cl2 2.245(3) . ? Re1 Cl1 2.368(2) . ? Re1 Cl1 2.368(2) 3 ? Re1 P1 2.497(2) 3 ? Re1 P1 2.497(2) . ? Fe1 C5 2.011(7) . ? Fe1 C5 2.011(7) 3 ? Fe1 C4 2.033(7) 3 ? Fe1 C4 2.033(7) . ? Fe1 C1 2.048(8) . ? Fe1 C1 2.048(8) 3 ? Fe1 C3 2.054(9) . ? Fe1 C3 2.054(9) 3 ? Fe1 C2 2.076(10) . ? Fe1 C2 2.076(10) 3 ? P1 C5 1.800(7) . ? P1 C6 1.809(6) . ? P1 C12 1.843(7) . ? C1 C5 1.410(9) . ? C1 C2 1.419(11) . ? C2 C3 1.393(15) . ? C3 C4 1.429(12) . ? C4 C5 1.439(9) . ? C6 C11 1.386(9) . ? C6 C7 1.390(10) . ? C7 C8 1.373(11) . ? C8 C9 1.389(14) . ? C9 C10 1.344(13) . ? C10 C11 1.380(11) . ? C12 C13 1.367(12) . ? C12 C17 1.372(10) . ? C13 C14 1.371(14) . ? C14 C15 1.365(14) . ? C15 C16 1.352(12) . ? C16 C17 1.365(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 O1 Re1 O1 163.2(9) 3 . ? Cl2 Re1 Cl2 164.0(2) 3 . ? O1 Re1 Cl1 99.3(5) 3 . ? O1 Re1 Cl1 93.1(5) . . ? Cl2 Re1 Cl1 101.48(12) 3 . ? Cl2 Re1 Cl1 90.32(12) . . ? O1 Re1 Cl1 93.1(5) 3 3 ? O1 Re1 Cl1 99.3(5) . 3 ? Cl2 Re1 Cl1 90.32(12) 3 3 ? Cl2 Re1 Cl1 101.48(12) . 3 ? Cl1 Re1 Cl1 85.20(10) . 3 ? O1 Re1 P1 88.4(5) 3 3 ? O1 Re1 P1 81.2(5) . 3 ? Cl2 Re1 P1 85.74(11) 3 3 ? Cl2 Re1 P1 84.33(12) . 3 ? Cl1 Re1 P1 168.85(6) . 3 ? Cl1 Re1 P1 86.28(6) 3 3 ? O1 Re1 P1 81.2(5) 3 . ? O1 Re1 P1 88.4(5) . . ? Cl2 Re1 P1 84.33(12) 3 . ? Cl2 Re1 P1 85.74(11) . . ? Cl1 Re1 P1 86.28(6) . . ? Cl1 Re1 P1 168.85(6) 3 . ? P1 Re1 P1 103.02(7) 3 . ? C5 Fe1 C5 114.6(4) . 3 ? C5 Fe1 C4 145.7(3) . 3 ? C5 Fe1 C4 41.7(3) 3 3 ? C5 Fe1 C4 41.7(3) . . ? C5 Fe1 C4 145.7(3) 3 . ? C4 Fe1 C4 171.5(4) 3 . ? C5 Fe1 C1 40.6(3) . . ? C5 Fe1 C1 110.8(3) 3 . ? C4 Fe1 C1 114.8(3) 3 . ? C4 Fe1 C1 68.6(3) . . ? C5 Fe1 C1 110.8(3) . 3 ? C5 Fe1 C1 40.6(3) 3 3 ? C4 Fe1 C1 68.6(3) 3 3 ? C4 Fe1 C1 114.8(3) . 3 ? C1 Fe1 C1 136.0(4) . 3 ? C5 Fe1 C3 68.5(3) . . ? C5 Fe1 C3 172.5(3) 3 . ? C4 Fe1 C3 132.1(3) 3 . ? C4 Fe1 C3 40.9(3) . . ? C1 Fe1 C3 66.8(4) . . ? C1 Fe1 C3 145.9(4) 3 . ? C5 Fe1 C3 172.5(3) . 3 ? C5 Fe1 C3 68.5(3) 3 3 ? C4 Fe1 C3 40.9(3) 3 3 ? C4 Fe1 C3 132.1(3) . 3 ? C1 Fe1 C3 145.9(4) . 3 ? C1 Fe1 C3 66.8(4) 3 3 ? C3 Fe1 C3 109.3(6) . 3 ? C5 Fe1 C2 68.7(3) . . ? C5 Fe1 C2 134.2(3) 3 . ? C4 Fe1 C2 108.5(4) 3 . ? C4 Fe1 C2 68.7(4) . . ? C1 Fe1 C2 40.2(3) . . ? C1 Fe1 C2 174.5(3) 3 . ? C3 Fe1 C2 39.4(4) . . ? C3 Fe1 C2 114.5(4) 3 . ? C5 Fe1 C2 134.2(3) . 3 ? C5 Fe1 C2 68.7(3) 3 3 ? C4 Fe1 C2 68.7(4) 3 3 ? C4 Fe1 C2 108.5(4) . 3 ? C1 Fe1 C2 174.5(4) . 3 ? C1 Fe1 C2 40.2(3) 3 3 ? C3 Fe1 C2 114.5(4) . 3 ? C3 Fe1 C2 39.4(4) 3 3 ? C2 Fe1 C2 143.9(5) . 3 ? C5 P1 C6 106.9(3) . . ? C5 P1 C12 100.4(3) . . ? C6 P1 C12 104.2(3) . . ? C5 P1 Re1 117.0(2) . . ? C6 P1 Re1 112.3(2) . . ? C12 P1 Re1 114.6(2) . . ? C5 C1 C2 109.3(7) . . ? C5 C1 Fe1 68.3(4) . . ? C2 C1 Fe1 70.9(6) . . ? C3 C2 C1 106.7(8) . . ? C3 C2 Fe1 69.4(6) . . ? C1 C2 Fe1 68.8(5) . . ? C2 C3 C4 110.4(7) . . ? C2 C3 Fe1 71.1(5) . . ? C4 C3 Fe1 68.8(4) . . ? C3 C4 C5 105.8(7) . . ? C3 C4 Fe1 70.3(5) . . ? C5 C4 Fe1 68.3(4) . . ? C1 C5 C4 107.7(6) . . ? C1 C5 P1 120.7(5) . . ? C4 C5 P1 131.5(5) . . ? C1 C5 Fe1 71.1(4) . . ? C4 C5 Fe1 70.0(4) . . ? P1 C5 Fe1 127.2(4) . . ? C11 C6 C7 117.9(6) . . ? C11 C6 P1 120.3(5) . . ? C7 C6 P1 121.8(5) . . ? C8 C7 C6 121.0(8) . . ? C7 C8 C9 120.0(9) . . ? C10 C9 C8 119.3(7) . . ? C9 C10 C11 121.5(8) . . ? C10 C11 C6 120.3(7) . . ? C13 C12 C17 117.0(7) . . ? C13 C12 P1 117.7(6) . . ? C17 C12 P1 125.2(5) . . ? C12 C13 C14 120.8(9) . . ? C15 C14 C13 120.9(9) . . ? C16 C15 C14 118.8(8) . . ? C15 C16 C17 120.1(8) . . ? C16 C17 C12 122.1(7) . . ? _refine_diff_density_max 1.661 _refine_diff_density_min -1.626 _refine_diff_density_rms 0.217