data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H38 Au2 Fe P2 S2' _chemical_formula_weight 1166.61 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' 'S' 'S' 0.1246 0.1234 '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' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6320(17) _cell_length_b 10.140(2) _cell_length_c 13.014(3) _cell_angle_alpha 101.87(3) _cell_angle_beta 106.29(3) _cell_angle_gamma 105.48(3) _cell_volume 1004.1(3) _cell_formula_units_Z 1 _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 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.929 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 7.860 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7241 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4585 _reflns_number_gt 3925 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect(Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_data_reduction 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0398P)^2^+0.5303P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0085(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4585 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0855 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.002 _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 Au1 Au 0.45316(2) 0.71464(2) 0.374070(16) 0.04307(11) Uani 1 1 d . . . Fe1 Fe 1.0000 1.0000 0.5000 0.0336(2) Uani 1 2 d S . . P1 P 0.58653(14) 0.89405(14) 0.31757(10) 0.0346(3) Uani 1 1 d . . . S1 S 0.28008(19) 0.53924(16) 0.42048(13) 0.0528(3) Uani 1 1 d . . . C11 C 1.0796(6) 0.8811(6) 0.5992(5) 0.0444(12) Uani 1 1 d . . . H11 H 1.0668 0.8819 0.6718 0.053 Uiso 1 1 calc R . . C12 C 1.0384(7) 1.2120(6) 0.5080(6) 0.0550(15) Uani 1 1 d . . . H12 H 1.1487 1.2852 0.5222 0.066 Uiso 1 1 calc R . . C13 C 0.9724(7) 1.1793(6) 0.5904(5) 0.0514(14) Uani 1 1 d . . . H13 H 1.0292 1.2259 0.6715 0.062 Uiso 1 1 calc R . . C14 C 0.7791(5) 1.0284(5) 0.4184(4) 0.0353(10) Uani 1 1 d . . . C15 C 0.8138(6) 1.0662(6) 0.5375(4) 0.0429(11) Uani 1 1 d . . . H15 H 0.7392 1.0222 0.5748 0.051 Uiso 1 1 calc R . . C21 C 0.6314(6) 0.8398(6) 0.1893(4) 0.0409(11) Uani 1 1 d . . . C22 C 0.6481(7) 0.7065(6) 0.1569(5) 0.0480(12) Uani 1 1 d . . . H22A H 0.6370 0.6447 0.2003 0.058 Uiso 1 1 calc R . . C23 C 0.6810(8) 0.6671(7) 0.0600(6) 0.0605(16) Uani 1 1 d . . . H23A H 0.6947 0.5787 0.0391 0.073 Uiso 1 1 calc R . . C24 C 0.6943(8) 0.7543(8) -0.0066(5) 0.0614(17) Uani 1 1 d . . . H24A H 0.7140 0.7248 -0.0728 0.074 Uiso 1 1 calc R . . C25 C 0.6782(8) 0.8865(8) 0.0255(5) 0.0593(16) Uani 1 1 d . . . H25A H 0.6877 0.9471 -0.0189 0.071 Uiso 1 1 calc R . . C26 C 0.6477(7) 0.9295(7) 0.1244(5) 0.0485(13) Uani 1 1 d . . . H26A H 0.6383 1.0195 0.1464 0.058 Uiso 1 1 calc R . . C31 C 0.4379(6) 0.9898(6) 0.2801(4) 0.0383(11) Uani 1 1 d . . . C32 C 0.4818(7) 1.1364(6) 0.3259(5) 0.0472(12) Uani 1 1 d . . . H32A H 0.5934 1.1917 0.3743 0.057 Uiso 1 1 calc R . . C33 C 0.3591(9) 1.2007(8) 0.2996(6) 0.0590(15) Uani 1 1 d . . . H33A H 0.3882 1.2988 0.3316 0.071 Uiso 1 1 calc R . . C34 C 0.1948(8) 1.1203(8) 0.2265(6) 0.0636(18) Uani 1 1 d . . . H34A H 0.1136 1.1644 0.2082 0.076 Uiso 1 1 calc R . . C35 C 0.1510(7) 0.9769(8) 0.1809(6) 0.0614(17) Uani 1 1 d . . . H35A H 0.0395 0.9232 0.1315 0.074 Uiso 1 1 calc R . . C36 C 0.2698(6) 0.9090(7) 0.2068(5) 0.0484(13) Uani 1 1 d . . . H36A H 0.2379 0.8103 0.1756 0.058 Uiso 1 1 calc R . . C41 C 0.0917(7) 0.4686(6) 0.2970(5) 0.0470(12) Uani 1 1 d . . . C42 C 0.0985(8) 0.4480(7) 0.1899(5) 0.0588(15) Uani 1 1 d . . . H42A H 0.2044 0.4780 0.1812 0.071 Uiso 1 1 calc R . . C43 C -0.0490(9) 0.3840(8) 0.0963(6) 0.075(2) Uani 1 1 d . . . H43A H -0.0420 0.3703 0.0251 0.090 Uiso 1 1 calc R . . C44 C -0.2070(9) 0.3401(9) 0.1075(8) 0.087(3) Uani 1 1 d . . . H44A H -0.3070 0.2959 0.0444 0.104 Uiso 1 1 calc R . . C45 C -0.2144(9) 0.3628(9) 0.2140(8) 0.081(2) Uani 1 1 d . . . H45A H -0.3207 0.3346 0.2225 0.097 Uiso 1 1 calc R . . C46 C -0.0697(8) 0.4255(7) 0.3060(7) 0.0631(17) Uani 1 1 d . . . H46A H -0.0781 0.4401 0.3769 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.03930(13) 0.04255(15) 0.04393(15) 0.01355(9) 0.01480(9) 0.00847(8) Fe1 0.0281(4) 0.0341(5) 0.0357(5) 0.0102(4) 0.0097(4) 0.0082(4) P1 0.0303(5) 0.0389(7) 0.0324(6) 0.0095(5) 0.0107(5) 0.0098(5) S1 0.0572(8) 0.0451(8) 0.0477(8) 0.0170(6) 0.0173(6) 0.0039(6) C11 0.038(2) 0.047(3) 0.053(3) 0.028(3) 0.017(2) 0.014(2) C12 0.040(3) 0.036(3) 0.076(4) 0.018(3) 0.007(3) 0.008(2) C13 0.051(3) 0.045(3) 0.047(3) 0.001(3) 0.006(2) 0.021(2) C14 0.030(2) 0.045(3) 0.033(2) 0.013(2) 0.0107(18) 0.0153(19) C15 0.036(2) 0.052(3) 0.040(3) 0.008(2) 0.013(2) 0.019(2) C21 0.031(2) 0.048(3) 0.037(3) 0.009(2) 0.0079(19) 0.012(2) C22 0.048(3) 0.047(3) 0.044(3) 0.007(2) 0.013(2) 0.017(2) C23 0.062(4) 0.054(4) 0.061(4) 0.000(3) 0.026(3) 0.020(3) C24 0.053(3) 0.087(5) 0.041(3) 0.003(3) 0.021(3) 0.027(3) C25 0.053(3) 0.088(5) 0.050(3) 0.028(3) 0.025(3) 0.032(3) C26 0.047(3) 0.061(4) 0.043(3) 0.016(3) 0.019(2) 0.024(3) C31 0.035(2) 0.053(3) 0.032(2) 0.014(2) 0.0173(19) 0.017(2) C32 0.051(3) 0.054(3) 0.044(3) 0.016(3) 0.023(2) 0.022(2) C33 0.077(4) 0.061(4) 0.064(4) 0.028(3) 0.040(3) 0.040(3) C34 0.067(4) 0.092(5) 0.075(4) 0.051(4) 0.046(4) 0.054(4) C35 0.038(3) 0.095(5) 0.059(4) 0.035(4) 0.013(3) 0.031(3) C36 0.036(2) 0.057(3) 0.046(3) 0.013(3) 0.011(2) 0.014(2) C41 0.051(3) 0.032(3) 0.061(4) 0.017(2) 0.024(3) 0.012(2) C42 0.054(3) 0.052(4) 0.059(4) 0.007(3) 0.019(3) 0.009(3) C43 0.076(4) 0.072(5) 0.055(4) 0.010(4) 0.012(3) 0.008(4) C44 0.059(4) 0.083(6) 0.098(6) 0.044(5) 0.002(4) 0.009(4) C45 0.047(4) 0.084(5) 0.114(7) 0.052(5) 0.027(4) 0.010(3) C46 0.055(3) 0.049(4) 0.091(5) 0.027(3) 0.035(3) 0.013(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 Au1 P1 2.2546(14) . ? Au1 S1 2.3000(16) . ? Fe1 C14 2.032(4) . ? Fe1 C14 2.032(4) 2_776 ? Fe1 C15 2.038(5) . ? Fe1 C15 2.038(5) 2_776 ? Fe1 C11 2.044(5) . ? Fe1 C11 2.044(5) 2_776 ? Fe1 C12 2.061(6) . ? Fe1 C12 2.061(6) 2_776 ? Fe1 C13 2.063(5) 2_776 ? Fe1 C13 2.063(5) . ? P1 C14 1.781(5) . ? P1 C31 1.826(5) . ? P1 C21 1.827(5) . ? S1 C41 1.783(6) . ? C11 C12 1.423(8) 2_776 ? C11 C14 1.424(7) 2_776 ? C12 C13 1.404(9) . ? C12 C11 1.423(8) 2_776 ? C13 C15 1.404(8) . ? C14 C11 1.424(7) 2_776 ? C14 C15 1.440(7) . ? C21 C26 1.370(8) . ? C21 C22 1.389(8) . ? C22 C23 1.373(8) . ? C23 C24 1.364(10) . ? C24 C25 1.375(10) . ? C25 C26 1.391(8) . ? C31 C32 1.385(8) . ? C31 C36 1.398(7) . ? C32 C33 1.385(8) . ? C33 C34 1.374(10) . ? C34 C35 1.355(10) . ? C35 C36 1.385(8) . ? C41 C42 1.386(9) . ? C41 C46 1.391(8) . ? C42 C43 1.374(9) . ? C43 C44 1.376(11) . ? C44 C45 1.379(12) . ? C45 C46 1.350(11) . ? 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 P1 Au1 S1 171.33(5) . . ? C14 Fe1 C14 180.0(3) . 2_776 ? C14 Fe1 C15 41.4(2) . . ? C14 Fe1 C15 138.6(2) 2_776 . ? C14 Fe1 C15 138.6(2) . 2_776 ? C14 Fe1 C15 41.4(2) 2_776 2_776 ? C15 Fe1 C15 179.999(2) . 2_776 ? C14 Fe1 C11 139.10(19) . . ? C14 Fe1 C11 40.90(19) 2_776 . ? C15 Fe1 C11 111.0(2) . . ? C15 Fe1 C11 69.0(2) 2_776 . ? C14 Fe1 C11 40.90(19) . 2_776 ? C14 Fe1 C11 139.10(19) 2_776 2_776 ? C15 Fe1 C11 69.0(2) . 2_776 ? C15 Fe1 C11 111.0(2) 2_776 2_776 ? C11 Fe1 C11 179.999(1) . 2_776 ? C14 Fe1 C12 68.1(2) . . ? C14 Fe1 C12 111.9(2) 2_776 . ? C15 Fe1 C12 67.7(2) . . ? C15 Fe1 C12 112.3(2) 2_776 . ? C11 Fe1 C12 139.4(2) . . ? C11 Fe1 C12 40.6(2) 2_776 . ? C14 Fe1 C12 111.9(2) . 2_776 ? C14 Fe1 C12 68.1(2) 2_776 2_776 ? C15 Fe1 C12 112.3(2) . 2_776 ? C15 Fe1 C12 67.7(2) 2_776 2_776 ? C11 Fe1 C12 40.6(2) . 2_776 ? C11 Fe1 C12 139.4(2) 2_776 2_776 ? C12 Fe1 C12 179.999(1) . 2_776 ? C14 Fe1 C13 111.8(2) . 2_776 ? C14 Fe1 C13 68.2(2) 2_776 2_776 ? C15 Fe1 C13 140.0(2) . 2_776 ? C15 Fe1 C13 40.0(2) 2_776 2_776 ? C11 Fe1 C13 68.0(2) . 2_776 ? C11 Fe1 C13 112.0(2) 2_776 2_776 ? C12 Fe1 C13 140.2(3) . 2_776 ? C12 Fe1 C13 39.8(3) 2_776 2_776 ? C14 Fe1 C13 68.2(2) . . ? C14 Fe1 C13 111.8(2) 2_776 . ? C15 Fe1 C13 40.0(2) . . ? C15 Fe1 C13 140.0(2) 2_776 . ? C11 Fe1 C13 112.0(2) . . ? C11 Fe1 C13 68.0(2) 2_776 . ? C12 Fe1 C13 39.8(3) . . ? C12 Fe1 C13 140.2(3) 2_776 . ? C13 Fe1 C13 180.0(3) 2_776 . ? C14 P1 C31 105.0(2) . . ? C14 P1 C21 106.8(2) . . ? C31 P1 C21 103.4(2) . . ? C14 P1 Au1 117.20(17) . . ? C31 P1 Au1 106.87(16) . . ? C21 P1 Au1 116.13(18) . . ? C41 S1 Au1 100.93(19) . . ? C12 C11 C14 107.2(5) 2_776 2_776 ? C12 C11 Fe1 70.4(3) 2_776 . ? C14 C11 Fe1 69.1(3) 2_776 . ? C13 C12 C11 108.7(5) . 2_776 ? C13 C12 Fe1 70.2(3) . . ? C11 C12 Fe1 69.1(3) 2_776 . ? C15 C13 C12 108.8(5) . . ? C15 C13 Fe1 69.0(3) . . ? C12 C13 Fe1 70.0(3) . . ? C11 C14 C15 107.7(4) 2_776 . ? C11 C14 P1 129.1(4) 2_776 . ? C15 C14 P1 123.2(4) . . ? C11 C14 Fe1 70.0(3) 2_776 . ? C15 C14 Fe1 69.5(3) . . ? P1 C14 Fe1 127.2(3) . . ? C13 C15 C14 107.6(5) . . ? C13 C15 Fe1 70.9(3) . . ? C14 C15 Fe1 69.0(3) . . ? C26 C21 C22 119.7(5) . . ? C26 C21 P1 120.4(4) . . ? C22 C21 P1 119.9(4) . . ? C23 C22 C21 119.2(6) . . ? C24 C23 C22 121.7(6) . . ? C23 C24 C25 119.2(6) . . ? C24 C25 C26 120.1(6) . . ? C21 C26 C25 120.2(6) . . ? C32 C31 C36 119.1(5) . . ? C32 C31 P1 122.9(4) . . ? C36 C31 P1 117.9(4) . . ? C33 C32 C31 119.9(5) . . ? C34 C33 C32 120.4(6) . . ? C35 C34 C33 120.0(5) . . ? C34 C35 C36 121.0(6) . . ? C35 C36 C31 119.5(6) . . ? C42 C41 C46 117.6(6) . . ? C42 C41 S1 122.6(4) . . ? C46 C41 S1 119.8(5) . . ? C43 C42 C41 121.0(6) . . ? C44 C43 C42 120.3(7) . . ? C43 C44 C45 118.8(7) . . ? C46 C45 C44 121.0(7) . . ? C45 C46 C41 121.3(7) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.541 _refine_diff_density_min -0.967 _refine_diff_density_rms 0.160