Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr M Concepcion Gimeno' _publ_contact_author_address ; Departamento de Quimica Inorganica, Inst de Ciencia de Materiales de Aragon Universidad de Zaragoza-CSIC E-50009 Zaragoza SPAIN ; _publ_contact_author_email GIMENO@UNIZAR.ES _publ_section_title ; Group 11 Complexes with Unsymmetrical P,S and P,Se Disubstituted Ferrocene Ligands ; loop_ _publ_author_name 'M. Concepcion Gimeno' 'Javier E. Aguado' 'Silvia Canales' 'P. Jones' 'Antonio Laguna' ; M.D.Villacampa ; data_diados(complex3) _database_code_depnum_ccdc_archive 'CCDC 272428' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H23 Au Cl Fe P S' _chemical_formula_weight 710.76 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' Cl Cl 0.1484 0.1585 '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 orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.1540(8) _cell_length_b 10.6559(8) _cell_length_c 25.390(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2476.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 5466 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description tablet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 6.775 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3413 _exptl_absorpt_correction_T_max 0.7370 _exptl_absorpt_process_details XPREP loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 -1.00 1.00 0.0240 0.00 1.00 -1.00 0.0240 0.00 -1.00 -2.00 0.0580 0.00 1.00 2.00 0.0620 -1.00 0.00 1.00 0.0920 1.00 0.00 -1.00 0.0990 1.00 0.00 1.00 0.1030 -1.00 0.00 -1.00 0.0810 _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w- and \f-scan' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45484 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.28 _reflns_number_total 6147 _reflns_number_gt 5536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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^)+(0.0160P)^2^] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.015(4) _refine_ls_number_reflns 6147 _refine_ls_number_parameters 298 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0430 _refine_ls_wR_factor_gt 0.0414 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au Au 0.450339(15) 0.123061(13) 0.349832(5) 0.02138(4) Uani 1 1 d . . . Fe Fe 0.32793(5) 0.51040(4) 0.34502(2) 0.01929(10) Uani 1 1 d . . . P P 0.59386(10) 0.29071(9) 0.35831(4) 0.0196(2) Uani 1 1 d . . . Cl Cl 0.30784(11) -0.05104(9) 0.33625(4) 0.0272(2) Uani 1 1 d . . . S S 0.41747(11) 0.62953(13) 0.46044(4) 0.0363(2) Uani 1 1 d . . . C11 C 0.6380(4) 0.3399(3) 0.42480(14) 0.0254(9) Uani 1 1 d DU . . C12 C 0.7461(5) 0.4303(4) 0.43380(17) 0.0365(10) Uani 1 1 d DU . . H12 H 0.7998 0.4634 0.4050 0.044 Uiso 1 1 calc R . . C13 C 0.7751(5) 0.4716(5) 0.48432(18) 0.0487(13) Uani 1 1 d DU . . H13 H 0.8486 0.5328 0.4905 0.058 Uiso 1 1 calc R . . C14 C 0.6949(6) 0.4220(5) 0.52611(17) 0.0522(14) Uani 1 1 d DU . . H14 H 0.7118 0.4518 0.5608 0.063 Uiso 1 1 calc R . . C15 C 0.5922(5) 0.3309(5) 0.51764(16) 0.0470(13) Uani 1 1 d DU . . H15 H 0.5402 0.2966 0.5466 0.056 Uiso 1 1 calc R . . C16 C 0.5633(5) 0.2885(4) 0.46716(13) 0.0328(9) Uani 1 1 d DU . . H16 H 0.4927 0.2245 0.4616 0.039 Uiso 1 1 calc R . . C21 C 0.7706(4) 0.2593(3) 0.32756(13) 0.0217(8) Uani 1 1 d DU . . C22 C 0.8197(4) 0.3261(4) 0.28439(14) 0.0277(9) Uani 1 1 d DU . . H22 H 0.7648 0.3952 0.2714 0.033 Uiso 1 1 calc R . . C23 C 0.9496(5) 0.2920(4) 0.25998(15) 0.0350(9) Uani 1 1 d DU . . H23 H 0.9836 0.3375 0.2302 0.042 Uiso 1 1 calc R . . C24 C 1.0294(5) 0.1914(4) 0.27913(15) 0.0359(10) Uani 1 1 d DU . . H24 H 1.1174 0.1672 0.2621 0.043 Uiso 1 1 calc R . . C25 C 0.9814(4) 0.1259(4) 0.32296(16) 0.0334(9) Uani 1 1 d DU . . H25 H 1.0376 0.0581 0.3364 0.040 Uiso 1 1 calc R . . C26 C 0.8518(4) 0.1593(3) 0.34714(16) 0.0259(8) Uani 1 1 d DU . . H26 H 0.8182 0.1140 0.3770 0.031 Uiso 1 1 calc R . . C31 C 0.5162(4) 0.4221(3) 0.32403(13) 0.0208(8) Uani 1 1 d DU . . C32 C 0.4080(4) 0.4087(3) 0.28371(13) 0.0232(8) Uani 1 1 d DU . . H32 H 0.3694 0.3317 0.2711 0.028 Uiso 1 1 calc R . . C33 C 0.3686(4) 0.5301(4) 0.26591(14) 0.0267(9) Uani 1 1 d DU . . H33 H 0.2994 0.5486 0.2391 0.032 Uiso 1 1 calc R . . C34 C 0.4506(4) 0.6192(4) 0.29502(13) 0.0282(7) Uani 1 1 d DU . . H34 H 0.4454 0.7077 0.2912 0.034 Uiso 1 1 calc R . . C35 C 0.5413(4) 0.5537(3) 0.33078(13) 0.0230(8) Uani 1 1 d DU . . H35 H 0.6075 0.5907 0.3551 0.028 Uiso 1 1 calc R . . C36 C 0.2814(4) 0.5673(4) 0.41947(14) 0.0244(8) Uani 1 1 d DU . . C37 C 0.2470(4) 0.4375(4) 0.41354(14) 0.0234(8) Uani 1 1 d DU . . H37 H 0.2881 0.3703 0.4331 0.028 Uiso 1 1 calc R . . C38 C 0.1409(4) 0.4265(4) 0.37332(14) 0.0256(9) Uani 1 1 d DU . . H38 H 0.0976 0.3507 0.3614 0.031 Uiso 1 1 calc R . . C39 C 0.1106(4) 0.5487(4) 0.35398(16) 0.0287(8) Uani 1 1 d DU . . H39 H 0.0442 0.5687 0.3265 0.034 Uiso 1 1 calc R . . C40 C 0.1952(4) 0.6347(4) 0.38247(13) 0.0273(8) Uani 1 1 d DU . . H40 H 0.1951 0.7231 0.3778 0.033 Uiso 1 1 calc R . . C41 C 0.3300(4) 0.6351(4) 0.52245(14) 0.0297(8) Uani 1 1 d DU . . C42 C 0.4162(5) 0.6720(4) 0.56460(16) 0.0441(12) Uani 1 1 d DU . . H42 H 0.5168 0.6901 0.5594 0.053 Uiso 1 1 calc R . . C43 C 0.3550(7) 0.6824(5) 0.61449(17) 0.0522(14) Uani 1 1 d DU . . H43 H 0.4131 0.7111 0.6431 0.063 Uiso 1 1 calc R . . C44 C 0.2105(6) 0.6516(4) 0.62288(18) 0.0485(13) Uani 1 1 d DU . . H44 H 0.1700 0.6544 0.6573 0.058 Uiso 1 1 calc R . . C45 C 0.1266(5) 0.6167(5) 0.58066(16) 0.0437(11) Uani 1 1 d DU . . H45 H 0.0258 0.5996 0.5858 0.052 Uiso 1 1 calc R . . C46 C 0.1850(5) 0.6061(4) 0.53097(15) 0.0345(10) Uani 1 1 d DU . . H46 H 0.1255 0.5788 0.5025 0.041 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 Au 0.02227(6) 0.01929(6) 0.02259(6) 0.00033(6) 0.00038(6) 0.00131(6) Fe 0.0219(3) 0.0180(2) 0.0179(2) 0.0009(2) 0.0007(2) 0.00101(19) P 0.0212(5) 0.0202(5) 0.0175(5) 0.0001(4) -0.0012(3) 0.0021(3) Cl 0.0265(5) 0.0227(5) 0.0324(5) -0.0020(4) -0.0015(4) -0.0020(4) S 0.0302(6) 0.0521(6) 0.0268(5) -0.0117(5) 0.0057(4) -0.0151(6) C11 0.030(2) 0.027(2) 0.0194(18) -0.0022(14) -0.0024(16) 0.0109(16) C12 0.028(2) 0.049(3) 0.032(2) -0.0126(19) -0.0070(18) 0.0077(19) C13 0.038(3) 0.065(3) 0.043(3) -0.024(2) -0.020(2) 0.014(2) C14 0.059(4) 0.073(4) 0.024(2) -0.015(2) -0.020(2) 0.032(3) C15 0.056(3) 0.064(3) 0.021(2) 0.008(2) -0.003(2) 0.030(2) C16 0.039(2) 0.036(2) 0.0233(19) 0.0072(16) -0.0013(19) 0.015(2) C21 0.0197(19) 0.025(2) 0.0201(17) -0.0061(15) -0.0034(14) -0.0006(16) C22 0.027(2) 0.036(2) 0.0206(19) -0.0011(16) -0.0019(16) 0.0030(17) C23 0.027(2) 0.052(3) 0.0264(19) -0.0107(17) 0.0031(19) -0.001(2) C24 0.022(2) 0.049(3) 0.037(2) -0.0233(19) 0.0029(18) 0.0015(19) C25 0.021(2) 0.033(2) 0.046(2) -0.010(2) -0.0081(16) 0.004(2) C26 0.0221(18) 0.0228(19) 0.033(2) -0.0029(17) -0.0082(18) 0.0014(14) C31 0.022(2) 0.0227(18) 0.0176(17) -0.0008(14) 0.0014(14) 0.0022(14) C32 0.026(2) 0.025(2) 0.0178(17) -0.0025(14) 0.0013(14) 0.0057(15) C33 0.027(2) 0.034(2) 0.0185(18) 0.0050(16) 0.0031(15) 0.0075(18) C34 0.0326(19) 0.0222(17) 0.0299(17) 0.0105(16) 0.0132(17) 0.005(2) C35 0.0218(19) 0.0235(18) 0.0238(17) 0.0016(14) 0.0064(16) -0.0039(17) C36 0.026(2) 0.026(2) 0.0211(19) -0.0051(15) 0.0048(15) -0.0064(17) C37 0.026(2) 0.027(2) 0.0174(18) 0.0044(15) 0.0009(15) -0.0017(17) C38 0.026(2) 0.028(2) 0.0224(18) -0.0012(15) 0.0020(16) -0.0071(17) C39 0.0217(19) 0.037(2) 0.027(2) 0.0042(19) 0.0002(17) 0.0046(16) C40 0.033(2) 0.023(2) 0.0263(18) 0.0010(17) 0.0112(15) 0.0011(19) C41 0.037(2) 0.026(2) 0.0265(18) -0.0045(18) 0.0022(16) -0.004(2) C42 0.049(3) 0.050(3) 0.033(2) -0.0095(19) 0.000(2) -0.019(2) C43 0.081(4) 0.051(3) 0.025(2) -0.005(2) -0.009(2) -0.014(3) C44 0.083(4) 0.027(3) 0.036(2) 0.0028(18) 0.025(2) 0.008(2) C45 0.046(3) 0.045(3) 0.040(2) 0.011(2) 0.0127(19) 0.004(3) C46 0.032(2) 0.043(3) 0.028(2) -0.0015(19) 0.0044(16) 0.000(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 Au P 2.2280(9) . y Au Cl 2.2939(10) . y Fe C36 2.030(4) . ? Fe C40 2.033(4) . ? Fe C32 2.033(3) . ? Fe C31 2.034(4) . ? Fe C35 2.040(4) . ? Fe C39 2.044(4) . ? Fe C37 2.044(3) . ? Fe C34 2.053(3) . ? Fe C33 2.054(3) . ? Fe C38 2.061(4) . ? P C31 1.796(4) . Y P C11 1.813(4) . Y P C21 1.827(4) . Y S C36 1.753(4) . Y S C41 1.767(4) . Y C11 C16 1.387(5) . ? C11 C12 1.399(5) . ? C12 C13 1.382(6) . ? C13 C14 1.394(7) . ? C14 C15 1.369(6) . ? C15 C16 1.385(5) . ? C21 C22 1.383(5) . ? C21 C26 1.391(5) . ? C22 C23 1.389(5) . ? C23 C24 1.385(6) . ? C24 C25 1.385(6) . ? C25 C26 1.383(5) . ? C31 C32 1.431(5) . ? C31 C35 1.431(5) . ? C32 C33 1.416(5) . ? C33 C34 1.418(5) . ? C34 C35 1.414(5) . ? C36 C40 1.421(5) . ? C36 C37 1.426(5) . ? C37 C38 1.414(5) . ? C38 C39 1.418(5) . ? C39 C40 1.401(5) . ? C41 C46 1.380(5) . ? C41 C42 1.387(5) . ? C42 C43 1.390(6) . ? C43 C44 1.379(7) . ? C44 C45 1.370(6) . ? C45 C46 1.375(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 P Au Cl 176.67(4) . . y C36 Fe C40 40.95(15) . . ? C36 Fe C32 161.35(15) . . ? C40 Fe C32 157.01(15) . . ? C36 Fe C31 124.03(15) . . ? C40 Fe C31 158.40(15) . . ? C32 Fe C31 41.20(13) . . ? C36 Fe C35 107.36(15) . . ? C40 Fe C35 120.51(16) . . ? C32 Fe C35 68.87(15) . . ? C31 Fe C35 41.14(14) . . ? C36 Fe C39 68.45(16) . . ? C40 Fe C39 40.21(15) . . ? C32 Fe C39 122.86(16) . . ? C31 Fe C39 161.10(15) . . ? C35 Fe C39 155.09(16) . . ? C36 Fe C37 40.98(14) . . ? C40 Fe C37 68.47(16) . . ? C32 Fe C37 125.43(15) . . ? C31 Fe C37 110.74(15) . . ? C35 Fe C37 125.73(14) . . ? C39 Fe C37 68.18(16) . . ? C36 Fe C34 121.46(15) . . ? C40 Fe C34 104.38(16) . . ? C32 Fe C34 68.29(15) . . ? C31 Fe C34 68.64(15) . . ? C35 Fe C34 40.43(14) . . ? C39 Fe C34 119.25(16) . . ? C37 Fe C34 159.87(15) . . ? C36 Fe C33 156.67(16) . . ? C40 Fe C33 119.96(15) . . ? C32 Fe C33 40.55(14) . . ? C31 Fe C33 68.73(14) . . ? C35 Fe C33 68.26(14) . . ? C39 Fe C33 105.38(16) . . ? C37 Fe C33 159.55(16) . . ? C34 Fe C33 40.39(15) . . ? C36 Fe C38 68.32(15) . . ? C40 Fe C38 67.85(16) . . ? C32 Fe C38 109.61(15) . . ? C31 Fe C38 126.49(15) . . ? C35 Fe C38 162.90(15) . . ? C39 Fe C38 40.43(15) . . ? C37 Fe C38 40.30(14) . . ? C34 Fe C38 156.18(15) . . ? C33 Fe C38 122.42(15) . . ? C31 P C11 108.31(16) . . Y C31 P C21 106.64(17) . . Y C11 P C21 104.69(17) . . Y C31 P Au 110.18(12) . . Y C11 P Au 116.94(13) . . Y C21 P Au 109.50(12) . . Y C36 S C41 102.67(18) . . Y C16 C11 C12 119.6(4) . . ? C16 C11 P 119.9(3) . . ? C12 C11 P 120.6(3) . . ? C13 C12 C11 120.5(4) . . ? C12 C13 C14 119.0(5) . . ? C15 C14 C13 120.7(4) . . ? C14 C15 C16 120.5(4) . . ? C15 C16 C11 119.7(4) . . ? C22 C21 C26 120.3(4) . . ? C22 C21 P 122.2(3) . . ? C26 C21 P 117.4(3) . . ? C21 C22 C23 119.8(4) . . ? C24 C23 C22 119.8(4) . . ? C25 C24 C23 120.3(4) . . ? C26 C25 C24 119.9(4) . . ? C25 C26 C21 119.8(4) . . ? C32 C31 C35 107.1(3) . . ? C32 C31 P 122.9(3) . . ? C35 C31 P 130.0(3) . . ? C32 C31 Fe 69.37(19) . . ? C35 C31 Fe 69.6(2) . . ? P C31 Fe 124.69(19) . . ? C33 C32 C31 108.3(3) . . ? C33 C32 Fe 70.5(2) . . ? C31 C32 Fe 69.43(19) . . ? C32 C33 C34 108.1(3) . . ? C32 C33 Fe 68.96(19) . . ? C34 C33 Fe 69.79(19) . . ? C35 C34 C33 108.4(3) . . ? C35 C34 Fe 69.3(2) . . ? C33 C34 Fe 69.8(2) . . ? C34 C35 C31 108.2(3) . . ? C34 C35 Fe 70.3(2) . . ? C31 C35 Fe 69.2(2) . . ? C40 C36 C37 107.3(4) . . ? C40 C36 S 126.5(3) . . ? C37 C36 S 125.9(3) . . ? C40 C36 Fe 69.6(2) . . ? C37 C36 Fe 70.0(2) . . ? S C36 Fe 121.1(2) . . ? C38 C37 C36 107.9(3) . . ? C38 C37 Fe 70.5(2) . . ? C36 C37 Fe 69.0(2) . . ? C37 C38 C39 108.0(3) . . ? C37 C38 Fe 69.2(2) . . ? C39 C38 Fe 69.1(2) . . ? C40 C39 C38 108.2(3) . . ? C40 C39 Fe 69.5(2) . . ? C38 C39 Fe 70.4(2) . . ? C39 C40 C36 108.5(4) . . ? C39 C40 Fe 70.3(2) . . ? C36 C40 Fe 69.4(2) . . ? C46 C41 C42 119.3(4) . . ? C46 C41 S 124.6(3) . . ? C42 C41 S 116.0(3) . . ? C41 C42 C43 119.8(4) . . ? C44 C43 C42 120.6(4) . . ? C45 C44 C43 118.8(4) . . ? C44 C45 C46 121.5(4) . . ? C45 C46 C41 120.0(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.739 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.100 ################################################# data_con6as(complex5) _database_code_depnum_ccdc_archive 'CCDC 272429' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H23 Au Cl Fe P Se' _chemical_formula_weight 757.66 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' Cl Cl 0.1484 0.1585 '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' Se Se -0.0929 2.2259 '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 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 10.0410(7) _cell_length_b 22.0090(15) _cell_length_c 11.8345(8) _cell_angle_alpha 90.00 _cell_angle_beta 106.2200(10) _cell_angle_gamma 90.00 _cell_volume 2511.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3059 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 25.1 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.004 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 8.048 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2115 _exptl_absorpt_correction_T_max 0.7390 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker SMART APEX CCD' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.28 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16363 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0955 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 28.56 _reflns_number_total 5936 _reflns_number_gt 3885 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SAINT' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material SHELXL-97 _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^)+(0.0244P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5936 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0768 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 0.824 _refine_ls_restrained_S_all 0.824 _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 Au Au 0.10991(3) 0.522909(11) 0.34659(2) 0.02919(8) Uani 1 1 d . . . Cl Cl 0.0510(2) 0.43227(7) 0.41361(15) 0.0443(4) Uani 1 1 d . . . P P 0.17725(17) 0.60849(7) 0.27941(13) 0.0253(4) Uani 1 1 d . . . Se Se 0.66415(8) 0.57656(3) 0.77561(6) 0.0437(2) Uani 1 1 d . . . Fe Fe 0.43233(9) 0.64316(4) 0.53389(8) 0.0318(2) Uani 1 1 d . . . C1 C 0.4999(7) 0.6209(3) 0.7070(5) 0.0352(16) Uani 1 1 d . . . C2 C 0.4912(8) 0.6856(4) 0.6930(6) 0.049(2) Uani 1 1 d . . . H2 H 0.5654 0.7137 0.7184 0.059 Uiso 1 1 calc R . . C3 C 0.3518(9) 0.6999(5) 0.6345(7) 0.069(3) Uani 1 1 d . . . H3 H 0.3154 0.7393 0.6126 0.082 Uiso 1 1 calc R . . C4 C 0.2785(8) 0.6465(5) 0.6150(6) 0.069(3) Uani 1 1 d . . . H4 H 0.1817 0.6439 0.5777 0.082 Uiso 1 1 calc R . . C5 C 0.3641(8) 0.5965(4) 0.6568(5) 0.052(2) Uani 1 1 d . . . H5 H 0.3375 0.5549 0.6526 0.062 Uiso 1 1 calc R . . C9 C 0.5546(8) 0.6788(4) 0.4406(6) 0.057(2) Uani 1 1 d . . . H9 H 0.6205 0.7105 0.4658 0.068 Uiso 1 1 calc R . . C10 C 0.4125(7) 0.6877(3) 0.3794(5) 0.0396(17) Uani 1 1 d . . . H10 H 0.3677 0.7256 0.3569 0.047 Uiso 1 1 calc R . . C6 C 0.3495(6) 0.6289(3) 0.3580(5) 0.0280(14) Uani 1 1 d . . . C7 C 0.4562(7) 0.5858(3) 0.4065(5) 0.0359(16) Uani 1 1 d . . . H7 H 0.4450 0.5429 0.4049 0.043 Uiso 1 1 calc R . . C8 C 0.5832(7) 0.6178(4) 0.4581(6) 0.047(2) Uani 1 1 d . . . H8 H 0.6704 0.6002 0.4970 0.057 Uiso 1 1 calc R . . C11 C 0.6684(7) 0.5873(3) 0.9385(5) 0.0329(16) Uani 1 1 d . . . C12 C 0.6666(10) 0.5378(4) 1.0043(6) 0.066(3) Uani 1 1 d . . . H12 H 0.6584 0.4985 0.9699 0.080 Uiso 1 1 calc R . . C13 C 0.6769(11) 0.5445(4) 1.1252(7) 0.085(3) Uani 1 1 d . . . H13 H 0.6733 0.5097 1.1718 0.102 Uiso 1 1 calc R . . C14 C 0.6922(8) 0.6011(4) 1.1750(7) 0.061(2) Uani 1 1 d . . . H14 H 0.7006 0.6058 1.2565 0.073 Uiso 1 1 calc R . . C15 C 0.6952(9) 0.6502(4) 1.1073(7) 0.064(2) Uani 1 1 d . . . H15 H 0.7038 0.6897 1.1409 0.077 Uiso 1 1 calc R . . C16 C 0.6859(8) 0.6431(3) 0.9907(6) 0.055(2) Uani 1 1 d . . . H16 H 0.6917 0.6779 0.9448 0.065 Uiso 1 1 calc R . . C21 C 0.1808(6) 0.6050(3) 0.1264(5) 0.0286(15) Uani 1 1 d . . . C22 C 0.0642(7) 0.5832(3) 0.0433(5) 0.0367(16) Uani 1 1 d . . . H22 H -0.0133 0.5693 0.0673 0.044 Uiso 1 1 calc R . . C23 C 0.0606(8) 0.5815(3) -0.0743(6) 0.0463(19) Uani 1 1 d . . . H23 H -0.0185 0.5657 -0.1308 0.056 Uiso 1 1 calc R . . C24 C 0.1710(8) 0.6027(3) -0.1094(6) 0.0451(19) Uani 1 1 d . . . H24 H 0.1678 0.6019 -0.1904 0.054 Uiso 1 1 calc R . . C25 C 0.2862(8) 0.6251(3) -0.0283(6) 0.0446(19) Uani 1 1 d . . . H25 H 0.3619 0.6405 -0.0529 0.054 Uiso 1 1 calc R . . C26 C 0.2913(7) 0.6249(3) 0.0898(6) 0.0358(16) Uani 1 1 d . . . H26 H 0.3726 0.6389 0.1463 0.043 Uiso 1 1 calc R . . C31 C 0.0694(6) 0.6739(3) 0.2846(5) 0.0260(14) Uani 1 1 d . . . C32 C 0.0642(7) 0.7227(3) 0.2095(6) 0.0352(16) Uani 1 1 d . . . H32 H 0.1141 0.7214 0.1521 0.042 Uiso 1 1 calc R . . C33 C -0.0146(7) 0.7736(3) 0.2186(6) 0.0453(19) Uani 1 1 d . . . H33 H -0.0191 0.8072 0.1671 0.054 Uiso 1 1 calc R . . C34 C -0.0855(7) 0.7752(3) 0.3021(7) 0.0468(19) Uani 1 1 d . . . H34 H -0.1368 0.8105 0.3098 0.056 Uiso 1 1 calc R . . C35 C -0.0834(7) 0.7269(3) 0.3739(6) 0.0411(18) Uani 1 1 d . . . H35 H -0.1349 0.7283 0.4301 0.049 Uiso 1 1 calc R . . C36 C -0.0069(6) 0.6760(3) 0.3659(5) 0.0358(16) Uani 1 1 d . . . H36 H -0.0062 0.6423 0.4161 0.043 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 Au 0.03699(15) 0.02564(13) 0.02588(12) 0.00299(12) 0.01034(10) -0.00229(13) Cl 0.0649(13) 0.0296(9) 0.0443(10) 0.0045(8) 0.0248(9) -0.0058(9) P 0.0277(9) 0.0269(9) 0.0211(8) 0.0034(7) 0.0063(7) -0.0019(7) Se 0.0512(5) 0.0505(5) 0.0291(4) -0.0028(3) 0.0108(3) 0.0153(4) Fe 0.0275(6) 0.0458(6) 0.0227(5) -0.0027(4) 0.0082(4) -0.0010(4) C1 0.034(4) 0.052(5) 0.020(3) -0.009(3) 0.007(3) -0.010(3) C2 0.054(5) 0.053(5) 0.037(4) -0.014(4) 0.005(4) 0.019(4) C3 0.062(7) 0.093(7) 0.049(5) -0.013(5) 0.013(5) 0.039(6) C4 0.029(5) 0.154(10) 0.026(4) 0.015(6) 0.011(4) 0.014(6) C5 0.043(5) 0.092(6) 0.019(3) 0.003(4) 0.006(3) -0.030(5) C9 0.046(5) 0.084(7) 0.042(5) 0.005(5) 0.013(4) -0.022(5) C10 0.043(5) 0.048(4) 0.029(4) 0.007(3) 0.013(3) -0.009(4) C6 0.030(4) 0.036(4) 0.020(3) -0.003(3) 0.010(3) -0.002(3) C7 0.039(4) 0.046(4) 0.025(3) 0.002(3) 0.013(3) 0.007(3) C8 0.026(4) 0.081(6) 0.037(4) -0.003(4) 0.012(3) -0.001(4) C11 0.032(4) 0.045(4) 0.022(3) 0.000(3) 0.008(3) 0.004(3) C12 0.124(8) 0.043(5) 0.033(4) -0.002(4) 0.022(5) 0.004(5) C13 0.150(10) 0.066(6) 0.047(5) 0.014(5) 0.040(6) 0.007(6) C14 0.060(6) 0.094(7) 0.030(4) -0.010(5) 0.015(4) 0.009(5) C15 0.075(7) 0.079(6) 0.040(5) -0.023(5) 0.020(4) -0.018(5) C16 0.080(6) 0.041(5) 0.042(5) 0.001(4) 0.017(4) -0.014(4) C21 0.032(4) 0.029(4) 0.024(3) 0.000(3) 0.007(3) 0.010(3) C22 0.030(4) 0.046(4) 0.031(4) -0.003(3) 0.004(3) -0.001(3) C23 0.041(5) 0.067(5) 0.026(4) -0.001(4) 0.002(3) 0.009(4) C24 0.052(5) 0.062(5) 0.022(3) -0.002(4) 0.012(3) 0.014(4) C25 0.049(5) 0.048(5) 0.045(4) 0.010(4) 0.028(4) 0.005(4) C26 0.028(4) 0.045(4) 0.033(4) -0.002(3) 0.007(3) -0.005(3) C31 0.024(4) 0.028(3) 0.024(3) 0.002(3) 0.002(3) -0.001(3) C32 0.038(4) 0.036(4) 0.041(4) 0.003(3) 0.026(3) 0.001(3) C33 0.050(5) 0.032(4) 0.059(5) 0.010(4) 0.024(4) 0.003(4) C34 0.038(5) 0.039(4) 0.065(5) -0.011(4) 0.017(4) 0.004(4) C35 0.038(4) 0.051(5) 0.041(4) -0.004(4) 0.022(3) 0.006(4) C36 0.034(4) 0.044(4) 0.030(4) 0.008(3) 0.010(3) -0.001(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 Au P 2.2220(15) . y Au Cl 2.2847(16) . y P C6 1.778(6) . y P C31 1.813(6) . y P C21 1.823(6) . y Se C1 1.893(7) . y Se C11 1.931(6) . y Fe C9 2.025(7) . ? Fe C1 2.031(6) . ? Fe C7 2.032(6) . ? Fe C4 2.035(7) . ? Fe C10 2.035(6) . ? Fe C2 2.037(7) . ? Fe C6 2.039(6) . ? Fe C3 2.042(8) . ? Fe C8 2.042(7) . ? Fe C5 2.048(7) . ? C1 C5 1.432(9) . ? C1 C2 1.434(9) . ? C2 C3 1.412(10) . ? C3 C4 1.371(12) . ? C4 C5 1.400(11) . ? C9 C8 1.377(10) . ? C9 C10 1.422(9) . ? C10 C6 1.432(8) . ? C6 C7 1.426(8) . ? C7 C8 1.436(9) . ? C11 C12 1.342(9) . ? C11 C16 1.365(9) . ? C12 C13 1.412(10) . ? C13 C14 1.368(11) . ? C14 C15 1.351(11) . ? C15 C16 1.366(9) . ? C21 C26 1.371(8) . ? C21 C22 1.387(8) . ? C22 C23 1.383(8) . ? C23 C24 1.369(9) . ? C24 C25 1.372(9) . ? C25 C26 1.384(9) . ? C31 C32 1.385(8) . ? C31 C36 1.388(8) . ? C32 C33 1.394(8) . ? C33 C34 1.370(9) . ? C34 C35 1.357(9) . ? C35 C36 1.376(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 P Au Cl 176.81(6) . . y C6 P C31 106.5(3) . . y C6 P C21 104.1(3) . . y C31 P C21 104.1(3) . . y C6 P Au 112.1(2) . . y C31 P Au 114.7(2) . . y C21 P Au 114.3(2) . . y C1 Se C11 98.0(3) . . y C9 Fe C1 124.1(3) . . ? C9 Fe C7 67.7(3) . . ? C1 Fe C7 121.6(3) . . ? C9 Fe C4 154.0(4) . . ? C1 Fe C4 67.5(3) . . ? C7 Fe C4 129.4(4) . . ? C9 Fe C10 41.0(3) . . ? C1 Fe C10 160.8(3) . . ? C7 Fe C10 68.6(3) . . ? C4 Fe C10 120.6(3) . . ? C9 Fe C2 105.3(3) . . ? C1 Fe C2 41.3(3) . . ? C7 Fe C2 155.2(3) . . ? C4 Fe C2 67.0(3) . . ? C10 Fe C2 122.7(3) . . ? C9 Fe C6 68.8(3) . . ? C1 Fe C6 156.8(3) . . ? C7 Fe C6 41.0(2) . . ? C4 Fe C6 109.9(3) . . ? C10 Fe C6 41.2(2) . . ? C2 Fe C6 160.9(3) . . ? C9 Fe C3 118.7(4) . . ? C1 Fe C3 68.5(3) . . ? C7 Fe C3 163.9(3) . . ? C4 Fe C3 39.3(3) . . ? C10 Fe C3 105.9(3) . . ? C2 Fe C3 40.5(3) . . ? C6 Fe C3 125.1(3) . . ? C9 Fe C8 39.6(3) . . ? C1 Fe C8 107.3(3) . . ? C7 Fe C8 41.3(3) . . ? C4 Fe C8 166.2(4) . . ? C10 Fe C8 68.6(3) . . ? C2 Fe C8 118.2(3) . . ? C6 Fe C8 69.6(3) . . ? C3 Fe C8 152.4(4) . . ? C9 Fe C5 162.8(3) . . ? C1 Fe C5 41.1(2) . . ? C7 Fe C5 110.3(3) . . ? C4 Fe C5 40.1(3) . . ? C10 Fe C5 155.7(3) . . ? C2 Fe C5 69.0(3) . . ? C6 Fe C5 121.7(3) . . ? C3 Fe C5 68.1(4) . . ? C8 Fe C5 127.6(3) . . ? C5 C1 C2 107.7(7) . . ? C5 C1 Se 126.8(6) . . y C2 C1 Se 125.4(5) . . y C5 C1 Fe 70.1(4) . . ? C2 C1 Fe 69.6(4) . . ? Se C1 Fe 124.2(3) . . ? C3 C2 C1 107.3(7) . . ? C3 C2 Fe 69.9(4) . . ? C1 C2 Fe 69.1(4) . . ? C4 C3 C2 107.7(8) . . ? C4 C3 Fe 70.1(5) . . ? C2 C3 Fe 69.6(4) . . ? C3 C4 C5 111.5(8) . . ? C3 C4 Fe 70.6(5) . . ? C5 C4 Fe 70.5(4) . . ? C4 C5 C1 105.7(8) . . ? C4 C5 Fe 69.4(4) . . ? C1 C5 Fe 68.8(4) . . ? C8 C9 C10 110.5(7) . . ? C8 C9 Fe 70.9(4) . . ? C10 C9 Fe 69.9(4) . . ? C9 C10 C6 107.2(7) . . ? C9 C10 Fe 69.1(4) . . ? C6 C10 Fe 69.6(3) . . ? C7 C6 C10 106.6(6) . . ? C7 C6 P 123.6(5) . . y C10 C6 P 129.6(5) . . y C7 C6 Fe 69.2(3) . . ? C10 C6 Fe 69.3(3) . . ? P C6 Fe 129.3(3) . . ? C6 C7 C8 108.8(6) . . ? C6 C7 Fe 69.7(3) . . ? C8 C7 Fe 69.7(4) . . ? C9 C8 C7 106.9(7) . . ? C9 C8 Fe 69.5(4) . . ? C7 C8 Fe 69.0(4) . . ? C12 C11 C16 119.3(6) . . ? C12 C11 Se 118.7(5) . . y C16 C11 Se 121.7(5) . . y C11 C12 C13 119.6(7) . . ? C14 C13 C12 120.0(8) . . ? C15 C14 C13 119.4(7) . . ? C14 C15 C16 120.1(8) . . ? C11 C16 C15 121.6(7) . . ? C26 C21 C22 118.9(6) . . ? C26 C21 P 122.9(5) . . y C22 C21 P 118.2(5) . . y C23 C22 C21 120.2(6) . . ? C24 C23 C22 120.0(7) . . ? C23 C24 C25 120.4(6) . . ? C24 C25 C26 119.5(6) . . ? C21 C26 C25 121.0(6) . . ? C32 C31 C36 119.3(6) . . ? C32 C31 P 120.6(5) . . y C36 C31 P 120.0(5) . . y C31 C32 C33 119.6(6) . . ? C34 C33 C32 119.8(7) . . ? C35 C34 C33 120.8(7) . . ? C34 C35 C36 120.4(6) . . ? C35 C36 C31 120.1(6) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 28.56 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.822 _refine_diff_density_min -1.122 _refine_diff_density_rms 0.162 ################################## data_lola28(complex4) _database_code_depnum_ccdc_archive 'CCDC 272430' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H30 Au F5 Fe P S' _chemical_formula_weight 885.46 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' F F 0.0171 0.0103 '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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.212(6) _cell_length_b 12.970(3) _cell_length_c 22.518(5) _cell_angle_alpha 90.00 _cell_angle_beta 132.70(3) _cell_angle_gamma 90.00 _cell_volume 6699(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 54 _cell_measurement_theta_min 9 _cell_measurement_theta_max 15 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3464 _exptl_absorpt_coefficient_mu 4.972 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.694 _exptl_absorpt_correction_T_max 0.767 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 Stoe AED-2' _diffrn_measurement_method Omega/theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 7063 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 2 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.63 _diffrn_reflns_theta_max 25.06 _reflns_number_total 5916 _reflns_number_gt 3999 _reflns_threshold_expression >2sigma(I) _computing_data_collection Dif4 _computing_cell_refinement Dif4 _computing_data_reduction REdu4 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens xp' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Extensive regions of badly resolved residual electron density could not be clearly identified as disordered solvent molecules, so the main peaks were refined as partially occupied carbons. For the calculation of composition etc., the solvent content was estimated as half a hexane molecule per asymmetric unit." ; _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^)+(0.0433P)^2^+8.3826P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5916 _refine_ls_number_parameters 413 _refine_ls_number_restraints 85 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0826 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au Au 0.089576(9) 0.24982(2) 0.272384(12) 0.02685(8) Uani 1 1 d . . . Fe Fe 0.15816(4) 0.20120(7) 0.16335(5) 0.0314(2) Uani 1 1 d . . . P P 0.05168(6) 0.14853(12) 0.16417(9) 0.0264(3) Uani 1 1 d . . . S S 0.25880(7) 0.07750(15) 0.17560(11) 0.0432(4) Uani 1 1 d . . . C1 C 0.0749(2) 0.1806(4) 0.1119(3) 0.0270(13) Uani 1 1 d U . . C2 C 0.0824(3) 0.2812(5) 0.0961(4) 0.0359(16) Uani 1 1 d U . . H2 H 0.0763 0.3421 0.1112 0.043 Uiso 1 1 calc R . . C3 C 0.1004(3) 0.2738(5) 0.0542(4) 0.0464(19) Uani 1 1 d U . . H3 H 0.1083 0.3289 0.0363 0.056 Uiso 1 1 calc R . . C4 C 0.1047(3) 0.1688(6) 0.0434(4) 0.0416(16) Uani 1 1 d U . . H4 H 0.1163 0.1423 0.0178 0.050 Uiso 1 1 calc R . . C5 C 0.0886(2) 0.1109(5) 0.0783(3) 0.0329(14) Uani 1 1 d U . . H5 H 0.0870 0.0393 0.0791 0.039 Uiso 1 1 calc R . . C6 C 0.2227(3) 0.1107(6) 0.2594(4) 0.0422(16) Uani 1 1 d U . . H6 H 0.2198 0.0413 0.2664 0.051 Uiso 1 1 calc R . . C7 C 0.2115(3) 0.1954(7) 0.2866(4) 0.0513(18) Uani 1 1 d U . . H7 H 0.1999 0.1910 0.3152 0.062 Uiso 1 1 calc R . . C8 C 0.2205(3) 0.2859(6) 0.2641(5) 0.055(2) Uani 1 1 d U . . H8 H 0.2160 0.3520 0.2752 0.066 Uiso 1 1 calc R . . C9 C 0.2381(3) 0.2615(5) 0.2208(4) 0.0464(17) Uani 1 1 d U . . H9 H 0.2467 0.3075 0.1985 0.056 Uiso 1 1 calc R . . C10 C 0.2392(2) 0.1521(5) 0.2194(4) 0.0314(14) Uani 1 1 d U . . C11 C 0.1275(2) 0.3367(4) 0.3739(3) 0.0258(13) Uani 1 1 d DU . . C12 C 0.1865(3) 0.3563(4) 0.4302(3) 0.0320(14) Uani 1 1 d DU . . C13 C 0.2135(3) 0.4143(5) 0.4979(3) 0.0331(15) Uani 1 1 d DU . . C14 C 0.1812(3) 0.4567(5) 0.5121(4) 0.0360(15) Uani 1 1 d DU . . C15 C 0.1226(3) 0.4401(5) 0.4583(4) 0.0381(16) Uani 1 1 d DU . . C16 C 0.0974(2) 0.3812(5) 0.3909(4) 0.0333(15) Uani 1 1 d DU . . F1 F 0.22093(15) 0.3169(4) 0.4191(2) 0.0542(12) Uani 1 1 d D . . F2 F 0.27132(15) 0.4323(4) 0.5504(2) 0.0589(13) Uani 1 1 d D . . F3 F 0.20675(16) 0.5170(3) 0.5778(2) 0.0527(11) Uani 1 1 d D . . F4 F 0.09098(18) 0.4820(4) 0.4731(3) 0.0662(13) Uani 1 1 d D . . F5 F 0.03907(15) 0.3685(3) 0.3401(2) 0.0551(12) Uani 1 1 d D . . C21 C 0.3353(3) 0.0626(4) 0.2581(4) 0.0337(14) Uani 1 1 d DU . . C22 C 0.3664(3) 0.0272(5) 0.2403(5) 0.0496(19) Uani 1 1 d DU . . H22 H 0.3472 0.0095 0.1873 0.060 Uiso 1 1 calc R . . C23 C 0.4267(3) 0.0170(6) 0.3006(6) 0.060(2) Uani 1 1 d DU . . H23 H 0.4478 -0.0076 0.2882 0.072 Uiso 1 1 calc R . . C24 C 0.4549(3) 0.0441(5) 0.3795(6) 0.055(2) Uani 1 1 d DU . . H24 H 0.4953 0.0394 0.4201 0.066 Uiso 1 1 calc R . . C25 C 0.4235(3) 0.0770(5) 0.3967(5) 0.0478(17) Uani 1 1 d DU . . H25 H 0.4426 0.0938 0.4497 0.057 Uiso 1 1 calc R . . C26 C 0.3633(3) 0.0865(5) 0.3370(4) 0.0399(16) Uani 1 1 d DU . . H26 H 0.3422 0.1087 0.3500 0.048 Uiso 1 1 calc R . . C31 C -0.0272(2) 0.1447(5) 0.0868(3) 0.0294(13) Uani 1 1 d DU . . C32 C -0.0574(3) 0.1128(6) 0.1084(4) 0.0506(19) Uani 1 1 d DU . . H32 H -0.0371 0.0947 0.1617 0.061 Uiso 1 1 calc R . . C33 C -0.1176(3) 0.1078(6) 0.0511(5) 0.060(2) Uani 1 1 d DU . . H33 H -0.1377 0.0856 0.0658 0.072 Uiso 1 1 calc R . . C34 C -0.1476(3) 0.1354(6) -0.0268(4) 0.0480(18) Uani 1 1 d DU . . H34 H -0.1881 0.1322 -0.0650 0.058 Uiso 1 1 calc R . . C35 C -0.1186(3) 0.1676(6) -0.0489(4) 0.0486(18) Uani 1 1 d DU . . H35 H -0.1393 0.1861 -0.1022 0.058 Uiso 1 1 calc R . . C36 C -0.0578(3) 0.1727(5) 0.0086(4) 0.0386(16) Uani 1 1 d DU . . H36 H -0.0381 0.1954 -0.0065 0.046 Uiso 1 1 calc R . . C41 C 0.0723(2) 0.0142(5) 0.1914(3) 0.0276(13) Uani 1 1 d DU . . C42 C 0.0392(3) -0.0640(5) 0.1363(4) 0.0391(16) Uani 1 1 d DU . . H42 H 0.0041 -0.0489 0.0847 0.047 Uiso 1 1 calc R . . C43 C 0.0580(4) -0.1643(6) 0.1574(5) 0.054(2) Uani 1 1 d DU . . H43 H 0.0357 -0.2170 0.1201 0.065 Uiso 1 1 calc R . . C44 C 0.1096(4) -0.1866(6) 0.2335(5) 0.061(2) Uani 1 1 d DU . . H44 H 0.1220 -0.2548 0.2477 0.073 Uiso 1 1 calc R . . C45 C 0.1429(3) -0.1111(6) 0.2879(5) 0.065(2) Uani 1 1 d DU . . H45 H 0.1783 -0.1271 0.3391 0.078 Uiso 1 1 calc R . . C46 C 0.1244(3) -0.0102(5) 0.2679(4) 0.0469(19) Uani 1 1 d DU . . H46 H 0.1471 0.0417 0.3059 0.056 Uiso 1 1 calc R . . C100 C 0.2195(6) 0.6970(11) 0.4653(8) 0.043(3) Uiso 0.50 1 d PU . . C101 C 0.1752(10) 0.2666(15) 0.9583(13) 0.088(6) Uiso 0.50 1 d PU . . C102 C 0.5482(9) 0.1807(16) 0.3321(13) 0.085(6) Uiso 0.50 1 d PU . . C103 C 0.5000 0.170(7) 0.2500 0.22(4) Uiso 0.50 2 d SPU . . C104 C 0.5000 0.219(7) 0.2500 0.20(4) Uiso 0.50 2 d SPU . . C105 C 0.4651(14) 0.343(3) 0.1995(19) 0.175(13) Uiso 0.50 1 d PU . . C106 C 0.2500 0.7500 0.5000 0.107(11) Uiso 0.50 2 d SPU . . C107 C 0.1141(14) 0.295(2) 0.8896(18) 0.136(10) Uiso 0.50 1 d PU . . 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 Au 0.02043(11) 0.02743(12) 0.02471(11) -0.00562(13) 0.01214(9) -0.00128(12) Fe 0.0200(4) 0.0325(5) 0.0350(5) -0.0065(4) 0.0160(4) -0.0017(4) P 0.0183(7) 0.0279(9) 0.0224(7) -0.0040(7) 0.0095(7) -0.0013(7) S 0.0361(9) 0.0475(11) 0.0445(10) -0.0064(9) 0.0268(9) 0.0040(8) C1 0.017(3) 0.027(3) 0.022(3) 0.000(2) 0.007(2) 0.001(2) C2 0.027(3) 0.027(4) 0.046(4) 0.006(3) 0.022(3) 0.008(3) C3 0.041(4) 0.050(5) 0.047(4) 0.013(3) 0.029(3) 0.001(3) C4 0.025(3) 0.060(5) 0.030(3) -0.005(3) 0.015(3) -0.002(3) C5 0.022(3) 0.035(4) 0.029(3) -0.011(3) 0.012(3) -0.006(3) C6 0.031(4) 0.052(4) 0.036(4) 0.001(3) 0.020(3) 0.003(3) C7 0.025(4) 0.079(5) 0.034(4) -0.016(4) 0.014(3) 0.001(4) C8 0.025(4) 0.049(4) 0.057(5) -0.031(4) 0.015(3) -0.002(3) C9 0.024(3) 0.034(4) 0.064(4) -0.013(4) 0.024(3) -0.012(3) C10 0.020(3) 0.032(3) 0.034(3) -0.007(3) 0.015(3) -0.002(3) C11 0.024(3) 0.029(3) 0.024(3) -0.003(2) 0.016(3) -0.003(3) C12 0.029(3) 0.040(4) 0.028(3) -0.002(3) 0.020(3) 0.006(3) C13 0.023(3) 0.041(4) 0.028(3) -0.009(3) 0.014(3) -0.001(3) C14 0.035(3) 0.042(4) 0.022(3) -0.007(3) 0.016(3) 0.000(3) C15 0.040(4) 0.039(4) 0.048(4) -0.002(3) 0.035(3) 0.010(3) C16 0.020(3) 0.040(4) 0.034(3) -0.004(3) 0.016(3) 0.000(3) F1 0.029(2) 0.083(3) 0.051(2) -0.025(2) 0.027(2) -0.002(2) F2 0.0217(19) 0.094(4) 0.039(2) -0.029(2) 0.0119(18) -0.010(2) F3 0.045(2) 0.069(3) 0.032(2) -0.024(2) 0.0212(19) -0.004(2) F4 0.048(3) 0.095(4) 0.064(3) -0.029(3) 0.041(2) 0.004(2) F5 0.024(2) 0.077(3) 0.058(3) -0.026(2) 0.025(2) -0.006(2) C21 0.032(3) 0.020(3) 0.052(4) 0.004(3) 0.030(3) 0.003(3) C22 0.054(4) 0.034(4) 0.076(5) -0.009(4) 0.050(4) 0.001(4) C23 0.052(4) 0.033(4) 0.111(6) 0.000(5) 0.062(5) 0.005(4) C24 0.033(4) 0.034(4) 0.095(5) 0.010(4) 0.042(4) 0.004(3) C25 0.034(3) 0.040(4) 0.061(4) 0.009(4) 0.028(3) 0.003(3) C26 0.036(3) 0.041(4) 0.051(4) 0.005(3) 0.033(3) 0.004(3) C31 0.023(3) 0.032(3) 0.029(3) -0.007(3) 0.016(3) 0.002(3) C32 0.034(4) 0.078(6) 0.036(4) -0.006(4) 0.022(3) -0.005(4) C33 0.035(4) 0.090(7) 0.068(5) -0.019(5) 0.039(4) -0.009(4) C34 0.017(3) 0.053(5) 0.052(4) -0.016(4) 0.014(3) -0.002(3) C35 0.028(3) 0.057(5) 0.037(4) 0.003(3) 0.013(3) 0.003(3) C36 0.027(3) 0.041(4) 0.038(3) 0.002(3) 0.018(3) -0.002(3) C41 0.025(3) 0.028(3) 0.032(3) -0.002(3) 0.020(3) -0.004(3) C42 0.044(4) 0.036(4) 0.033(3) -0.008(3) 0.024(3) -0.007(3) C43 0.074(5) 0.036(4) 0.057(4) -0.018(4) 0.046(4) -0.013(4) C44 0.084(6) 0.035(4) 0.082(5) 0.008(4) 0.064(5) 0.016(4) C45 0.046(5) 0.049(5) 0.056(5) 0.014(4) 0.017(4) 0.015(4) C46 0.033(4) 0.035(4) 0.040(4) 0.000(3) 0.012(3) 0.000(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 Au C11 2.056(6) . y Au P 2.2701(16) . y Fe C10 2.016(6) . ? Fe C1 2.020(6) . ? Fe C2 2.026(6) . ? Fe C5 2.029(6) . ? Fe C9 2.032(6) . ? Fe C4 2.035(6) . ? Fe C8 2.038(7) . ? Fe C3 2.042(7) . ? Fe C6 2.050(7) . ? Fe C7 2.053(7) . ? P C1 1.800(6) . y P C31 1.811(6) . y P C41 1.814(6) . y S C10 1.761(6) . y S C21 1.782(6) . y C1 C2 1.412(9) . ? C1 C5 1.418(8) . ? C2 C3 1.393(10) . ? C3 C4 1.406(10) . ? C4 C5 1.404(9) . ? C6 C10 1.412(9) . ? C6 C7 1.412(10) . ? C7 C8 1.380(12) . ? C8 C9 1.441(11) . ? C9 C10 1.420(8) . ? C11 C16 1.360(8) . ? C11 C12 1.377(8) . ? C12 F1 1.358(6) . ? C12 C13 1.363(8) . ? C13 F2 1.347(7) . ? C13 C14 1.362(8) . ? C14 F3 1.357(7) . ? C14 C15 1.362(9) . ? C15 F4 1.350(7) . ? C15 C16 1.374(9) . ? C16 F5 1.351(6) . ? C21 C22 1.356(9) . ? C21 C26 1.383(9) . ? C22 C23 1.392(10) . ? C23 C24 1.391(11) . ? C24 C25 1.343(10) . ? C25 C26 1.388(9) . ? C31 C36 1.365(8) . ? C31 C32 1.385(9) . ? C32 C33 1.383(9) . ? C33 C34 1.361(10) . ? C34 C35 1.360(10) . ? C35 C36 1.396(8) . ? C41 C42 1.377(8) . ? C41 C46 1.384(8) . ? C42 C43 1.372(10) . ? C43 C44 1.367(11) . ? C44 C45 1.347(11) . ? C45 C46 1.376(10) . ? C100 C106 0.989(14) . ? C100 C101 1.37(2) 6_565 ? C100 C100 1.98(3) 7_566 ? C101 C100 1.37(2) 6_566 ? C101 C107 1.47(3) . ? C101 C106 1.85(2) 4_546 ? C102 C103 1.39(2) . ? C102 C104 1.47(4) . ? C102 C107 1.55(3) 8 ? C103 C104 0.64(13) . ? C103 C102 1.39(2) 2_655 ? C104 C102 1.47(4) 2_655 ? C104 C105 1.84(7) 2_655 ? C104 C105 1.84(7) . ? C105 C105 1.79(6) 2_655 ? C106 C100 0.989(14) 7_566 ? C106 C101 1.85(2) 4_556 ? C106 C101 1.85(2) 6_565 ? C107 C102 1.55(3) 8_456 ? 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 C11 Au P 177.13(17) . . y C10 Fe C1 153.7(3) . . ? C10 Fe C2 164.2(3) . . ? C1 Fe C2 40.9(2) . . ? C10 Fe C5 119.6(3) . . ? C1 Fe C5 41.0(2) . . ? C2 Fe C5 68.3(3) . . ? C10 Fe C9 41.1(2) . . ? C1 Fe C9 164.1(3) . . ? C2 Fe C9 125.8(3) . . ? C5 Fe C9 152.8(3) . . ? C10 Fe C4 108.5(3) . . ? C1 Fe C4 68.5(3) . . ? C2 Fe C4 67.9(3) . . ? C5 Fe C4 40.4(2) . . ? C9 Fe C4 118.1(3) . . ? C10 Fe C8 68.1(3) . . ? C1 Fe C8 126.5(3) . . ? C2 Fe C8 107.8(3) . . ? C5 Fe C8 164.8(3) . . ? C9 Fe C8 41.5(3) . . ? C4 Fe C8 153.3(4) . . ? C10 Fe C3 127.4(3) . . ? C1 Fe C3 68.2(3) . . ? C2 Fe C3 40.0(3) . . ? C5 Fe C3 67.9(3) . . ? C9 Fe C3 106.8(3) . . ? C4 Fe C3 40.3(3) . . ? C8 Fe C3 119.3(3) . . ? C10 Fe C6 40.6(2) . . ? C1 Fe C6 119.4(3) . . ? C2 Fe C6 153.5(3) . . ? C5 Fe C6 108.8(3) . . ? C9 Fe C6 69.2(3) . . ? C4 Fe C6 128.0(3) . . ? C8 Fe C6 67.7(3) . . ? C3 Fe C6 165.4(3) . . ? C10 Fe C7 67.6(3) . . ? C1 Fe C7 108.6(3) . . ? C2 Fe C7 119.7(3) . . ? C5 Fe C7 128.5(3) . . ? C9 Fe C7 68.5(3) . . ? C4 Fe C7 165.9(3) . . ? C8 Fe C7 39.4(3) . . ? C3 Fe C7 152.8(3) . . ? C6 Fe C7 40.3(3) . . ? C1 P C31 105.3(3) . . y C1 P C41 103.6(3) . . y C31 P C41 103.7(3) . . y C1 P Au 114.84(19) . . y C31 P Au 115.33(19) . . y C41 P Au 112.7(2) . . y C10 S C21 101.8(3) . . y C2 C1 C5 107.1(5) . . ? C2 C1 P 125.9(5) . . ? C5 C1 P 127.0(5) . . ? C2 C1 Fe 69.8(3) . . ? C5 C1 Fe 69.8(3) . . ? P C1 Fe 126.0(3) . . ? C3 C2 C1 108.7(6) . . ? C3 C2 Fe 70.6(4) . . ? C1 C2 Fe 69.4(3) . . ? C2 C3 C4 108.2(6) . . ? C2 C3 Fe 69.3(4) . . ? C4 C3 Fe 69.6(4) . . ? C5 C4 C3 108.1(6) . . ? C5 C4 Fe 69.6(4) . . ? C3 C4 Fe 70.1(4) . . ? C4 C5 C1 108.0(6) . . ? C4 C5 Fe 70.0(4) . . ? C1 C5 Fe 69.2(3) . . ? C10 C6 C7 106.5(7) . . ? C10 C6 Fe 68.4(4) . . ? C7 C6 Fe 70.0(4) . . ? C8 C7 C6 109.3(7) . . ? C8 C7 Fe 69.7(4) . . ? C6 C7 Fe 69.8(4) . . ? C7 C8 C9 109.1(6) . . ? C7 C8 Fe 70.9(4) . . ? C9 C8 Fe 69.0(4) . . ? C10 C9 C8 105.1(7) . . ? C10 C9 Fe 68.9(3) . . ? C8 C9 Fe 69.5(4) . . ? C6 C10 C9 109.9(6) . . ? C6 C10 S 124.3(5) . . ? C9 C10 S 125.8(5) . . ? C6 C10 Fe 71.0(4) . . ? C9 C10 Fe 70.1(4) . . ? S C10 Fe 126.0(3) . . ? C16 C11 C12 114.2(5) . . ? C16 C11 Au 124.0(4) . . ? C12 C11 Au 121.8(4) . . ? F1 C12 C13 116.5(5) . . ? F1 C12 C11 119.5(5) . . ? C13 C12 C11 124.0(6) . . ? F2 C13 C14 119.2(5) . . ? F2 C13 C12 121.5(5) . . ? C14 C13 C12 119.3(6) . . ? F3 C14 C13 120.6(6) . . ? F3 C14 C15 120.0(6) . . ? C13 C14 C15 119.4(6) . . ? F4 C15 C14 119.0(6) . . ? F4 C15 C16 121.9(6) . . ? C14 C15 C16 119.1(6) . . ? F5 C16 C11 120.0(5) . . ? F5 C16 C15 115.9(5) . . ? C11 C16 C15 124.1(6) . . ? C22 C21 C26 120.0(6) . . ? C22 C21 S 116.7(6) . . ? C26 C21 S 123.2(5) . . ? C21 C22 C23 120.6(8) . . ? C24 C23 C22 119.2(7) . . ? C25 C24 C23 119.7(7) . . ? C24 C25 C26 121.5(8) . . ? C21 C26 C25 119.0(6) . . ? C36 C31 C32 119.0(6) . . ? C36 C31 P 122.7(5) . . ? C32 C31 P 118.3(5) . . ? C33 C32 C31 120.3(7) . . ? C34 C33 C32 120.0(7) . . ? C35 C34 C33 120.4(6) . . ? C34 C35 C36 119.9(7) . . ? C31 C36 C35 120.4(6) . . ? C42 C41 C46 118.8(6) . . ? C42 C41 P 121.8(5) . . ? C46 C41 P 119.2(5) . . ? C43 C42 C41 120.2(7) . . ? C44 C43 C42 119.9(7) . . ? C45 C44 C43 120.8(7) . . ? C44 C45 C46 120.0(7) . . ? C45 C46 C41 120.2(7) . . ? C106 C100 C101 101.9(15) . 6_565 ? C106 C100 C100 0.0(10) . 7_566 ? C101 C100 C100 101.9(15) 6_565 7_566 ? C100 C101 C107 122(2) 6_566 . ? C100 C101 C106 31.6(8) 6_566 4_546 ? C107 C101 C106 148.7(19) . 4_546 ? C103 C102 C104 26(5) . . ? C103 C102 C107 140(2) . 8 ? C104 C102 C107 129(3) . 8 ? C104 C103 C102 84(4) . 2_655 ? C104 C103 C102 84(4) . . ? C102 C103 C102 168(8) 2_655 . ? C103 C104 C102 70(4) . 2_655 ? C103 C104 C102 70(4) . . ? C102 C104 C102 140(7) 2_655 . ? C103 C104 C105 150.9(18) . 2_655 ? C102 C104 C105 139(5) 2_655 2_655 ? C102 C104 C105 81(2) . 2_655 ? C103 C104 C105 150.9(18) . . ? C102 C104 C105 81(2) 2_655 . ? C102 C104 C105 139(5) . . ? C105 C104 C105 58(4) 2_655 . ? C105 C105 C104 60.9(18) 2_655 . ? C100 C106 C100 180(2) 7_566 . ? C100 C106 C101 46.4(10) 7_566 4_556 ? C100 C106 C101 133.6(10) . 4_556 ? C100 C106 C101 133.6(10) 7_566 6_565 ? C100 C106 C101 46.4(10) . 6_565 ? C101 C106 C101 180.000(3) 4_556 6_565 ? C101 C107 C102 166(3) . 8_456 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C24 H24 F4 0.93 2.46 3.315(8) 152.2 3_545 C46 H46 F2 0.93 2.43 3.208(8) 141.5 7_556 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.012 _refine_diff_density_min -1.201 _refine_diff_density_rms 0.112 ################################################# data_con20as(complex6) _database_code_depnum_ccdc_archive 'CCDC 272431' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H23 Au F5 Fe P Se' _chemical_formula_weight 889.27 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' F F 0.0171 0.0103 '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' Se Se -0.0929 2.2259 '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 11.7891(5) _cell_length_b 14.7442(6) _cell_length_c 18.4764(8) _cell_angle_alpha 73.3850(10) _cell_angle_beta 84.7880(10) _cell_angle_gamma 76.9320(10) _cell_volume 2996.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7589 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 28 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.971 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 6.697 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2231 _exptl_absorpt_correction_T_max 0.4332 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20097 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 28.71 _reflns_number_total 13522 _reflns_number_gt 10205 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.02 (Bruker AXS, 1999)' _computing_data_reduction 'SAINT+ v. 6.02 (Bruker AXS, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material SHELXL-97 _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^)+(0.0468P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens riding _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13522 _refine_ls_number_parameters 775 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.811949(19) 0.829772(16) 0.937697(12) 0.03242(7) Uani 1 1 d . . . Se1 Se 1.21484(6) 0.42208(5) 0.90025(4) 0.04467(16) Uani 1 1 d . . . P1 P 0.75165(12) 0.79711(10) 0.83596(8) 0.0291(3) Uani 1 1 d . . . Fe1 Fe 0.99498(7) 0.62177(6) 0.82801(5) 0.0363(2) Uani 1 1 d . . . C1 C 1.1617(5) 0.5570(5) 0.8582(4) 0.0437(15) Uani 1 1 d . . . C2 C 1.1151(5) 0.6248(5) 0.9002(4) 0.0504(17) Uani 1 1 d . . . H2 H 1.1062 0.6108 0.9536 0.061 Uiso 1 1 calc R . . C3 C 1.0849(6) 0.7156(5) 0.8485(5) 0.062(2) Uani 1 1 d . . . H3 H 1.0528 0.7744 0.8612 0.074 Uiso 1 1 calc R . . C4 C 1.1086(6) 0.7068(6) 0.7767(5) 0.064(2) Uani 1 1 d . . . H4 H 1.0949 0.7583 0.7317 0.077 Uiso 1 1 calc R . . C5 C 1.1574(6) 0.6076(5) 0.7804(4) 0.0545(18) Uani 1 1 d . . . H5 H 1.1820 0.5810 0.7390 0.065 Uiso 1 1 calc R . . C6 C 0.8226(5) 0.6797(4) 0.8261(3) 0.0322(13) Uani 1 1 d . . . C7 C 0.8596(6) 0.6534(5) 0.7590(3) 0.0413(15) Uani 1 1 d . . . H7 H 0.8542 0.6961 0.7094 0.050 Uiso 1 1 calc R . . C8 C 0.9055(6) 0.5540(5) 0.7773(4) 0.0471(16) Uani 1 1 d . . . H8 H 0.9367 0.5174 0.7426 0.056 Uiso 1 1 calc R . . C9 C 0.8977(6) 0.5182(5) 0.8552(4) 0.0488(17) Uani 1 1 d . . . H9 H 0.9229 0.4525 0.8829 0.059 Uiso 1 1 calc R . . C10 C 0.8468(5) 0.5944(4) 0.8864(3) 0.0385(14) Uani 1 1 d . . . H10 H 0.8314 0.5897 0.9386 0.046 Uiso 1 1 calc R . . C11 C 1.3749(5) 0.4218(5) 0.9163(3) 0.0411(15) Uani 1 1 d . . . C12 C 1.4432(7) 0.3346(5) 0.9504(4) 0.062(2) Uani 1 1 d . . . H12 H 1.4099 0.2790 0.9680 0.074 Uiso 1 1 calc R . . C13 C 1.5591(8) 0.3263(7) 0.9594(5) 0.083(3) Uani 1 1 d . . . H13 H 1.6070 0.2649 0.9811 0.099 Uiso 1 1 calc R . . C14 C 1.6059(7) 0.4083(7) 0.9367(4) 0.072(2) Uani 1 1 d . . . H14 H 1.6862 0.4035 0.9434 0.086 Uiso 1 1 calc R . . C15 C 1.5371(7) 0.4959(6) 0.9047(4) 0.061(2) Uani 1 1 d . . . H15 H 1.5692 0.5523 0.8895 0.073 Uiso 1 1 calc R . . C16 C 1.4212(6) 0.5028(5) 0.8945(4) 0.0521(17) Uani 1 1 d . . . H16 H 1.3731 0.5639 0.8722 0.063 Uiso 1 1 calc R . . C21 C 0.8901(5) 0.8600(4) 1.0202(3) 0.0330(13) Uani 1 1 d . . . C22 C 0.9853(6) 0.7976(4) 1.0551(3) 0.0394(14) Uani 1 1 d . . . C23 C 1.0512(6) 0.8154(5) 1.1047(3) 0.0438(15) Uani 1 1 d . . . C24 C 1.0170(6) 0.9003(5) 1.1237(4) 0.0476(17) Uani 1 1 d . . . C25 C 0.9219(6) 0.9670(5) 1.0913(4) 0.0421(15) Uani 1 1 d . . . C26 C 0.8620(5) 0.9439(4) 1.0410(3) 0.0352(13) Uani 1 1 d . . . F1 F 1.0235(4) 0.7118(3) 1.0379(2) 0.0628(12) Uani 1 1 d . . . F2 F 1.1448(4) 0.7505(3) 1.1355(2) 0.0759(14) Uani 1 1 d . . . F3 F 1.0790(4) 0.9198(3) 1.1729(2) 0.0670(12) Uani 1 1 d . . . F4 F 0.8905(4) 1.0516(3) 1.1089(2) 0.0665(12) Uani 1 1 d . . . F5 F 0.7705(3) 1.0156(3) 1.0082(2) 0.0565(10) Uani 1 1 d . . . C31 C 0.7917(5) 0.8814(4) 0.7501(3) 0.0291(12) Uani 1 1 d . . . C32 C 0.8788(5) 0.9283(4) 0.7515(3) 0.0382(14) Uani 1 1 d . . . H32 H 0.9149 0.9181 0.7979 0.046 Uiso 1 1 calc R . . C33 C 0.9148(6) 0.9896(5) 0.6875(4) 0.0520(17) Uani 1 1 d . . . H33 H 0.9752 1.0218 0.6897 0.062 Uiso 1 1 calc R . . C34 C 0.8635(6) 1.0050(5) 0.6193(4) 0.0542(18) Uani 1 1 d . . . H34 H 0.8902 1.0455 0.5742 0.065 Uiso 1 1 calc R . . C35 C 0.7731(6) 0.9606(5) 0.6179(4) 0.0572(19) Uani 1 1 d . . . H35 H 0.7339 0.9735 0.5722 0.069 Uiso 1 1 calc R . . C36 C 0.7393(6) 0.8976(4) 0.6826(3) 0.0423(15) Uani 1 1 d . . . H36 H 0.6793 0.8650 0.6807 0.051 Uiso 1 1 calc R . . C41 C 0.5979(5) 0.8028(4) 0.8298(3) 0.0325(13) Uani 1 1 d . . . C42 C 0.5199(6) 0.8621(5) 0.8640(4) 0.0504(17) Uani 1 1 d . . . H42 H 0.5472 0.8968 0.8924 0.060 Uiso 1 1 calc R . . C43 C 0.4006(6) 0.8724(6) 0.8576(5) 0.068(2) Uani 1 1 d . . . H43 H 0.3469 0.9172 0.8787 0.081 Uiso 1 1 calc R . . C44 C 0.3619(6) 0.8186(6) 0.8213(4) 0.059(2) Uani 1 1 d . . . H44 H 0.2806 0.8236 0.8185 0.071 Uiso 1 1 calc R . . C45 C 0.4387(6) 0.7572(5) 0.7888(4) 0.0567(19) Uani 1 1 d . . . H45 H 0.4105 0.7197 0.7631 0.068 Uiso 1 1 calc R . . C46 C 0.5569(6) 0.7484(4) 0.7926(4) 0.0435(15) Uani 1 1 d . . . H46 H 0.6100 0.7052 0.7697 0.052 Uiso 1 1 calc R . . Au2 Au 0.507629(19) 0.789199(16) 0.429742(13) 0.03341(7) Uani 1 1 d . . . Se2 Se 0.30941(6) 0.38102(5) 0.42055(4) 0.04739(17) Uani 1 1 d . . . P2 P 0.60090(12) 0.74055(11) 0.33033(8) 0.0301(3) Uani 1 1 d . . . Fe2 Fe 0.44323(6) 0.56858(6) 0.34198(4) 0.02934(18) Uani 1 1 d . . . C51 C 0.2988(5) 0.5132(5) 0.3714(3) 0.0383(14) Uani 1 1 d . . . C52 C 0.3042(5) 0.5548(5) 0.2920(3) 0.0408(15) Uani 1 1 d . . . H52 H 0.3065 0.5219 0.2544 0.049 Uiso 1 1 calc R . . C53 C 0.3055(5) 0.6535(5) 0.2791(4) 0.0455(17) Uani 1 1 d . . . H53 H 0.3101 0.6984 0.2310 0.055 Uiso 1 1 calc R . . C54 C 0.2990(5) 0.6746(5) 0.3500(4) 0.0398(14) Uani 1 1 d . . . H54 H 0.2971 0.7359 0.3578 0.048 Uiso 1 1 calc R . . C55 C 0.2957(5) 0.5879(4) 0.4066(3) 0.0375(14) Uani 1 1 d . . . H55 H 0.2921 0.5804 0.4595 0.045 Uiso 1 1 calc R . . C56 C 0.5910(4) 0.6194(4) 0.3352(3) 0.0304(12) Uani 1 1 d . . . C57 C 0.5849(5) 0.5463(4) 0.4047(3) 0.0342(13) Uani 1 1 d . . . H57 H 0.5841 0.5546 0.4539 0.041 Uiso 1 1 calc R . . C58 C 0.5804(5) 0.4601(4) 0.3880(4) 0.0417(15) Uani 1 1 d . . . H58 H 0.5764 0.3998 0.4235 0.050 Uiso 1 1 calc R . . C59 C 0.5830(5) 0.4799(5) 0.3075(4) 0.0444(16) Uani 1 1 d . . . H59 H 0.5809 0.4346 0.2803 0.053 Uiso 1 1 calc R . . C60 C 0.5893(5) 0.5773(5) 0.2753(3) 0.0379(14) Uani 1 1 d . . . H60 H 0.5919 0.6092 0.2228 0.046 Uiso 1 1 calc R . . C61 C 0.1479(5) 0.3761(5) 0.4282(3) 0.0389(14) Uani 1 1 d . . . C62 C 0.1223(6) 0.2852(5) 0.4409(4) 0.0529(18) Uani 1 1 d . . . H62 H 0.1831 0.2292 0.4465 0.064 Uiso 1 1 calc R . . C63 C 0.0066(7) 0.2775(6) 0.4453(4) 0.059(2) Uani 1 1 d . . . H63 H -0.0121 0.2156 0.4552 0.071 Uiso 1 1 calc R . . C64 C -0.0808(7) 0.3583(7) 0.4354(4) 0.066(2) Uani 1 1 d . . . H64 H -0.1596 0.3525 0.4366 0.080 Uiso 1 1 calc R . . C65 C -0.0556(6) 0.4472(6) 0.4239(4) 0.062(2) Uani 1 1 d . . . H65 H -0.1165 0.5029 0.4188 0.074 Uiso 1 1 calc R . . C66 C 0.0602(6) 0.4556(5) 0.4196(4) 0.0487(17) Uani 1 1 d . . . H66 H 0.0781 0.5177 0.4106 0.058 Uiso 1 1 calc R . . C71 C 0.4221(5) 0.8361(4) 0.5175(3) 0.0308(12) Uani 1 1 d . . . C72 C 0.4693(6) 0.8844(4) 0.5566(3) 0.0411(15) Uani 1 1 d . . . C73 C 0.4075(6) 0.9269(4) 0.6095(3) 0.0416(15) Uani 1 1 d . . . C74 C 0.2922(6) 0.9229(4) 0.6243(3) 0.0433(15) Uani 1 1 d . . . C75 C 0.2420(6) 0.8758(5) 0.5866(4) 0.0457(16) Uani 1 1 d . . . C76 C 0.3071(6) 0.8333(4) 0.5345(3) 0.0391(14) Uani 1 1 d . . . F6 F 0.5812(3) 0.8917(3) 0.5444(2) 0.0528(10) Uani 1 1 d . . . F7 F 0.4576(4) 0.9738(3) 0.6460(2) 0.0634(11) Uani 1 1 d . . . F8 F 0.2301(4) 0.9650(3) 0.6745(2) 0.0652(12) Uani 1 1 d . . . F9 F 0.1276(3) 0.8732(3) 0.6002(2) 0.0649(12) Uani 1 1 d . . . F10 F 0.2510(3) 0.7890(3) 0.4997(2) 0.0499(9) Uani 1 1 d . . . C81 C 0.7551(5) 0.7393(4) 0.3253(3) 0.0336(13) Uani 1 1 d . . . C82 C 0.7933(6) 0.7971(5) 0.3598(4) 0.0486(16) Uani 1 1 d . . . H82 H 0.7398 0.8355 0.3864 0.058 Uiso 1 1 calc R . . C83 C 0.9114(6) 0.7994(6) 0.3555(4) 0.062(2) Uani 1 1 d . . . H83 H 0.9381 0.8392 0.3797 0.075 Uiso 1 1 calc R . . C84 C 0.9876(6) 0.7460(6) 0.3177(5) 0.065(2) Uani 1 1 d . . . H84 H 1.0676 0.7492 0.3145 0.078 Uiso 1 1 calc R . . C85 C 0.9512(6) 0.6873(5) 0.2836(5) 0.061(2) Uani 1 1 d . . . H85 H 1.0057 0.6494 0.2571 0.074 Uiso 1 1 calc R . . C86 C 0.8347(5) 0.6831(5) 0.2878(4) 0.0460(16) Uani 1 1 d . . . H86 H 0.8094 0.6414 0.2648 0.055 Uiso 1 1 calc R . . C91 C 0.5481(5) 0.8132(4) 0.2384(3) 0.0368(13) Uani 1 1 d . . . C92 C 0.6171(6) 0.8216(5) 0.1726(3) 0.0461(16) Uani 1 1 d . . . H92 H 0.6974 0.7914 0.1756 0.055 Uiso 1 1 calc R . . C93 C 0.5717(6) 0.8722(5) 0.1043(4) 0.0503(17) Uani 1 1 d . . . H93 H 0.6207 0.8783 0.0601 0.060 Uiso 1 1 calc R . . C94 C 0.4551(6) 0.9148(5) 0.0987(4) 0.0515(18) Uani 1 1 d . . . H94 H 0.4231 0.9476 0.0504 0.062 Uiso 1 1 calc R . . C95 C 0.3854(6) 0.9103(5) 0.1620(4) 0.0527(18) Uani 1 1 d . . . H95 H 0.3054 0.9413 0.1581 0.063 Uiso 1 1 calc R . . C96 C 0.4315(5) 0.8603(4) 0.2321(4) 0.0437(16) Uani 1 1 d . . . H96 H 0.3831 0.8581 0.2763 0.052 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 0.03111(12) 0.04278(13) 0.02934(13) -0.01823(10) -0.00235(9) -0.00843(10) Se1 0.0441(4) 0.0526(4) 0.0357(4) -0.0161(3) -0.0010(3) -0.0018(3) P1 0.0275(7) 0.0367(8) 0.0279(8) -0.0139(6) -0.0005(6) -0.0096(6) Fe1 0.0344(5) 0.0401(5) 0.0328(5) -0.0134(4) 0.0030(4) -0.0019(4) C1 0.034(3) 0.053(4) 0.043(4) -0.019(3) 0.001(3) -0.001(3) C2 0.031(3) 0.068(5) 0.064(5) -0.040(4) 0.000(3) -0.005(3) C3 0.040(4) 0.050(4) 0.099(7) -0.028(4) 0.002(4) -0.008(3) C4 0.032(4) 0.059(5) 0.082(6) 0.007(4) 0.007(4) -0.006(3) C5 0.036(4) 0.071(5) 0.048(4) -0.013(4) 0.009(3) -0.001(3) C6 0.031(3) 0.042(3) 0.026(3) -0.013(3) 0.002(2) -0.010(3) C7 0.050(4) 0.050(4) 0.025(3) -0.015(3) -0.006(3) -0.004(3) C8 0.052(4) 0.046(4) 0.050(4) -0.027(3) -0.006(3) -0.005(3) C9 0.055(4) 0.033(3) 0.054(4) -0.010(3) -0.004(3) -0.002(3) C10 0.036(3) 0.045(4) 0.033(3) -0.010(3) 0.005(3) -0.010(3) C11 0.040(4) 0.047(4) 0.035(3) -0.016(3) -0.003(3) 0.000(3) C12 0.052(5) 0.052(4) 0.075(5) -0.013(4) -0.015(4) 0.002(4) C13 0.060(6) 0.069(6) 0.106(8) -0.015(5) -0.019(5) 0.006(5) C14 0.051(5) 0.095(7) 0.065(5) -0.021(5) -0.015(4) -0.003(5) C15 0.054(5) 0.066(5) 0.059(5) -0.010(4) 0.000(4) -0.013(4) C16 0.049(4) 0.057(4) 0.047(4) -0.014(3) -0.005(3) -0.004(4) C21 0.033(3) 0.047(3) 0.025(3) -0.017(3) -0.003(2) -0.011(3) C22 0.050(4) 0.040(3) 0.033(3) -0.017(3) -0.003(3) -0.009(3) C23 0.039(4) 0.056(4) 0.039(4) -0.018(3) -0.014(3) -0.004(3) C24 0.045(4) 0.071(5) 0.041(4) -0.029(3) -0.007(3) -0.020(4) C25 0.040(4) 0.048(4) 0.049(4) -0.032(3) 0.011(3) -0.011(3) C26 0.024(3) 0.046(3) 0.038(3) -0.017(3) 0.000(2) -0.007(3) F1 0.080(3) 0.044(2) 0.068(3) -0.029(2) -0.030(2) 0.010(2) F2 0.071(3) 0.081(3) 0.074(3) -0.030(2) -0.045(2) 0.015(2) F3 0.059(3) 0.097(3) 0.067(3) -0.046(2) -0.020(2) -0.024(2) F4 0.058(3) 0.072(3) 0.092(3) -0.062(3) 0.000(2) -0.010(2) F5 0.047(2) 0.057(2) 0.069(3) -0.033(2) -0.016(2) 0.0059(19) C31 0.026(3) 0.033(3) 0.031(3) -0.012(2) -0.001(2) -0.006(2) C32 0.039(3) 0.044(3) 0.038(3) -0.013(3) -0.006(3) -0.019(3) C33 0.045(4) 0.055(4) 0.059(5) -0.008(3) -0.003(3) -0.025(3) C34 0.057(5) 0.051(4) 0.048(4) 0.002(3) -0.001(3) -0.020(4) C35 0.064(5) 0.063(5) 0.043(4) 0.003(3) -0.016(3) -0.029(4) C36 0.046(4) 0.045(4) 0.039(4) -0.005(3) -0.012(3) -0.019(3) C41 0.030(3) 0.030(3) 0.037(3) -0.008(2) 0.003(2) -0.008(2) C42 0.039(4) 0.061(4) 0.060(4) -0.030(4) 0.003(3) -0.012(3) C43 0.034(4) 0.093(6) 0.084(6) -0.046(5) 0.007(4) -0.006(4) C44 0.031(4) 0.070(5) 0.075(5) -0.011(4) -0.006(4) -0.016(4) C45 0.052(4) 0.051(4) 0.076(5) -0.015(4) -0.016(4) -0.023(4) C46 0.041(4) 0.042(3) 0.055(4) -0.018(3) -0.011(3) -0.014(3) Au2 0.02898(12) 0.03926(13) 0.03393(13) -0.01327(10) 0.00145(9) -0.00781(10) Se2 0.0390(4) 0.0463(4) 0.0562(4) -0.0046(3) -0.0123(3) -0.0153(3) P2 0.0227(7) 0.0364(8) 0.0313(8) -0.0086(6) -0.0005(6) -0.0071(6) Fe2 0.0214(4) 0.0401(4) 0.0280(4) -0.0098(3) -0.0030(3) -0.0079(3) C51 0.022(3) 0.055(4) 0.042(4) -0.015(3) 0.001(3) -0.015(3) C52 0.025(3) 0.061(4) 0.041(4) -0.012(3) -0.009(3) -0.016(3) C53 0.021(3) 0.058(4) 0.048(4) 0.006(3) -0.014(3) -0.013(3) C54 0.017(3) 0.045(4) 0.053(4) -0.011(3) -0.005(3) -0.001(3) C55 0.023(3) 0.049(4) 0.041(4) -0.014(3) 0.001(2) -0.008(3) C56 0.017(3) 0.041(3) 0.037(3) -0.014(3) -0.002(2) -0.008(2) C57 0.021(3) 0.039(3) 0.042(4) -0.010(3) -0.008(2) -0.004(2) C58 0.024(3) 0.036(3) 0.063(4) -0.010(3) -0.010(3) -0.003(3) C59 0.030(3) 0.054(4) 0.060(4) -0.034(3) 0.005(3) -0.009(3) C60 0.034(3) 0.053(4) 0.033(3) -0.019(3) 0.005(3) -0.013(3) C61 0.042(4) 0.056(4) 0.025(3) -0.009(3) 0.000(3) -0.027(3) C62 0.061(5) 0.057(4) 0.045(4) -0.008(3) -0.001(3) -0.027(4) C63 0.072(5) 0.066(5) 0.054(5) -0.015(4) 0.005(4) -0.046(5) C64 0.048(5) 0.106(7) 0.053(5) -0.019(5) 0.012(4) -0.040(5) C65 0.046(4) 0.087(6) 0.061(5) -0.025(4) 0.008(4) -0.029(4) C66 0.048(4) 0.054(4) 0.049(4) -0.012(3) 0.000(3) -0.022(3) C71 0.029(3) 0.033(3) 0.027(3) -0.004(2) -0.002(2) -0.005(2) C72 0.042(4) 0.040(3) 0.038(4) -0.005(3) -0.006(3) -0.007(3) C73 0.053(4) 0.034(3) 0.043(4) -0.018(3) -0.009(3) -0.004(3) C74 0.049(4) 0.041(3) 0.035(4) -0.013(3) 0.006(3) -0.001(3) C75 0.041(4) 0.052(4) 0.043(4) -0.009(3) -0.001(3) -0.012(3) C76 0.044(4) 0.043(3) 0.032(3) -0.010(3) -0.003(3) -0.011(3) F6 0.033(2) 0.073(3) 0.063(3) -0.032(2) -0.0009(18) -0.0148(19) F7 0.071(3) 0.064(3) 0.071(3) -0.040(2) -0.011(2) -0.016(2) F8 0.065(3) 0.078(3) 0.060(3) -0.043(2) 0.008(2) -0.002(2) F9 0.041(2) 0.092(3) 0.071(3) -0.038(2) 0.022(2) -0.021(2) F10 0.046(2) 0.062(2) 0.055(2) -0.0267(19) 0.0011(18) -0.0241(19) C81 0.019(3) 0.039(3) 0.039(3) -0.002(3) -0.004(2) -0.008(2) C82 0.037(4) 0.059(4) 0.059(4) -0.025(3) 0.003(3) -0.019(3) C83 0.046(4) 0.076(5) 0.073(5) -0.013(4) -0.016(4) -0.032(4) C84 0.025(4) 0.061(5) 0.090(6) 0.009(4) -0.009(4) -0.010(3) C85 0.027(3) 0.052(4) 0.093(6) -0.013(4) 0.008(4) 0.003(3) C86 0.025(3) 0.042(4) 0.070(5) -0.020(3) 0.000(3) -0.001(3) C91 0.028(3) 0.036(3) 0.045(4) -0.008(3) -0.002(3) -0.007(3) C92 0.031(3) 0.056(4) 0.044(4) -0.012(3) -0.003(3) 0.004(3) C93 0.048(4) 0.063(4) 0.034(4) -0.006(3) 0.004(3) -0.010(3) C94 0.059(5) 0.047(4) 0.040(4) 0.003(3) -0.012(3) -0.009(3) C95 0.030(3) 0.047(4) 0.066(5) 0.003(3) -0.008(3) 0.000(3) C96 0.027(3) 0.040(3) 0.049(4) 0.005(3) -0.002(3) 0.002(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 C21 2.049(5) . y Au1 P1 2.2773(14) . y Se1 C1 1.896(7) . y Se1 C11 1.935(6) . y P1 C6 1.797(6) . y P1 C41 1.808(6) . y P1 C31 1.813(6) . y Fe1 C6 2.018(6) . ? Fe1 C7 2.021(6) . ? Fe1 C5 2.026(6) . ? Fe1 C10 2.027(6) . ? Fe1 C4 2.029(7) . ? Fe1 C1 2.033(6) . ? Fe1 C9 2.036(7) . ? Fe1 C8 2.044(6) . ? Fe1 C2 2.047(6) . ? Fe1 C3 2.053(7) . ? C1 C5 1.418(9) . ? C1 C2 1.421(8) . ? C2 C3 1.395(10) . ? C3 C4 1.366(10) . ? C4 C5 1.431(10) . ? C6 C7 1.407(7) . ? C6 C10 1.414(8) . ? C7 C8 1.394(8) . ? C8 C9 1.385(9) . ? C9 C10 1.400(8) . ? C11 C12 1.364(9) . ? C11 C16 1.365(9) . ? C12 C13 1.365(11) . ? C13 C14 1.382(12) . ? C14 C15 1.361(10) . ? C15 C16 1.373(10) . ? C21 C22 1.360(8) . ? C21 C26 1.361(8) . ? C22 F1 1.361(6) . ? C22 C23 1.368(8) . ? C23 F2 1.335(7) . ? C23 C24 1.360(9) . ? C24 F3 1.344(7) . ? C24 C25 1.367(9) . ? C25 F4 1.342(6) . ? C25 C26 1.373(8) . ? C26 F5 1.374(7) . ? C31 C32 1.368(7) . ? C31 C36 1.376(7) . ? C32 C33 1.367(8) . ? C33 C34 1.384(9) . ? C34 C35 1.377(9) . ? C35 C36 1.377(8) . ? C41 C42 1.362(8) . ? C41 C46 1.379(8) . ? C42 C43 1.392(9) . ? C43 C44 1.346(10) . ? C44 C45 1.358(10) . ? C45 C46 1.376(9) . ? Au2 C71 2.037(5) . y Au2 P2 2.2643(15) . y Se2 C51 1.881(6) . y Se2 C61 1.913(6) . y P2 C56 1.792(6) . y P2 C81 1.807(5) . y P2 C91 1.808(6) . y Fe2 C51 2.017(5) . ? Fe2 C56 2.027(5) . ? Fe2 C52 2.028(5) . ? Fe2 C55 2.031(6) . ? Fe2 C60 2.031(6) . ? Fe2 C57 2.032(5) . ? Fe2 C59 2.035(6) . ? Fe2 C53 2.036(6) . ? Fe2 C58 2.049(6) . ? Fe2 C54 2.060(6) . ? C51 C52 1.421(8) . ? C51 C55 1.422(8) . ? C52 C53 1.409(9) . ? C53 C54 1.424(9) . ? C54 C55 1.407(8) . ? C56 C60 1.421(7) . ? C56 C57 1.429(8) . ? C57 C58 1.404(8) . ? C58 C59 1.430(9) . ? C59 C60 1.404(8) . ? C61 C66 1.357(9) . ? C61 C62 1.391(9) . ? C62 C63 1.387(10) . ? C63 C64 1.367(11) . ? C64 C65 1.362(11) . ? C65 C66 1.392(9) . ? C71 C76 1.371(8) . ? C71 C72 1.373(8) . ? C72 F6 1.342(7) . ? C72 C73 1.376(8) . ? C73 F7 1.344(7) . ? C73 C74 1.374(9) . ? C74 F8 1.335(7) . ? C74 C75 1.361(9) . ? C75 F9 1.357(7) . ? C75 C76 1.379(9) . ? C76 F10 1.339(7) . ? C81 C82 1.369(8) . ? C81 C86 1.380(8) . ? C82 C83 1.395(9) . ? C83 C84 1.340(11) . ? C84 C85 1.363(11) . ? C85 C86 1.383(9) . ? C91 C92 1.391(8) . ? C91 C96 1.392(8) . ? C92 C93 1.356(8) . ? C93 C94 1.376(9) . ? C94 C95 1.361(9) . ? C95 C96 1.384(8) . ? 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 C21 Au1 P1 171.17(16) . . y C1 Se1 C11 98.7(3) . . y C6 P1 C41 105.0(3) . . y C6 P1 C31 104.7(2) . . y C41 P1 C31 105.8(3) . . y C6 P1 Au1 112.93(18) . . y C41 P1 Au1 117.99(19) . . y C31 P1 Au1 109.40(18) . . y C6 Fe1 C7 40.8(2) . . ? C6 Fe1 C5 152.6(3) . . ? C7 Fe1 C5 117.5(3) . . ? C6 Fe1 C10 40.9(2) . . ? C7 Fe1 C10 68.2(2) . . ? C5 Fe1 C10 163.6(3) . . ? C6 Fe1 C4 119.4(3) . . ? C7 Fe1 C4 107.9(3) . . ? C5 Fe1 C4 41.3(3) . . ? C10 Fe1 C4 154.4(3) . . ? C6 Fe1 C1 165.7(2) . . ? C7 Fe1 C1 152.0(2) . . ? C5 Fe1 C1 40.9(2) . . ? C10 Fe1 C1 127.4(3) . . ? C4 Fe1 C1 68.2(3) . . ? C6 Fe1 C9 68.0(2) . . ? C7 Fe1 C9 67.2(3) . . ? C5 Fe1 C9 125.4(3) . . ? C10 Fe1 C9 40.3(2) . . ? C4 Fe1 C9 163.5(3) . . ? C1 Fe1 C9 108.2(3) . . ? C6 Fe1 C8 68.1(2) . . ? C7 Fe1 C8 40.1(2) . . ? C5 Fe1 C8 106.0(3) . . ? C10 Fe1 C8 67.7(3) . . ? C4 Fe1 C8 126.5(3) . . ? C1 Fe1 C8 118.5(3) . . ? C9 Fe1 C8 39.7(3) . . ? C6 Fe1 C2 128.3(2) . . ? C7 Fe1 C2 165.4(3) . . ? C5 Fe1 C2 68.7(3) . . ? C10 Fe1 C2 109.9(3) . . ? C4 Fe1 C2 67.2(3) . . ? C1 Fe1 C2 40.8(2) . . ? C9 Fe1 C2 121.4(3) . . ? C8 Fe1 C2 153.9(3) . . ? C6 Fe1 C3 109.9(3) . . ? C7 Fe1 C3 127.9(3) . . ? C5 Fe1 C3 67.9(3) . . ? C10 Fe1 C3 122.2(3) . . ? C4 Fe1 C3 39.1(3) . . ? C1 Fe1 C3 67.5(3) . . ? C9 Fe1 C3 156.0(3) . . ? C8 Fe1 C3 163.7(3) . . ? C2 Fe1 C3 39.8(3) . . ? C5 C1 C2 108.0(6) . . ? C5 C1 Se1 126.7(5) . . y C2 C1 Se1 125.3(5) . . y C5 C1 Fe1 69.3(4) . . ? C2 C1 Fe1 70.2(4) . . ? Se1 C1 Fe1 124.6(3) . . y C3 C2 C1 107.4(7) . . ? C3 C2 Fe1 70.3(4) . . ? C1 C2 Fe1 69.1(4) . . ? C4 C3 C2 109.5(7) . . ? C4 C3 Fe1 69.5(4) . . ? C2 C3 Fe1 69.9(4) . . ? C3 C4 C5 109.0(7) . . ? C3 C4 Fe1 71.4(4) . . ? C5 C4 Fe1 69.2(4) . . ? C1 C5 C4 106.1(6) . . ? C1 C5 Fe1 69.8(4) . . ? C4 C5 Fe1 69.4(4) . . ? C7 C6 C10 107.1(5) . . ? C7 C6 P1 127.9(4) . . y C10 C6 P1 125.0(4) . . y C7 C6 Fe1 69.7(3) . . ? C10 C6 Fe1 69.9(3) . . ? P1 C6 Fe1 127.6(3) . . y C8 C7 C6 108.7(5) . . ? C8 C7 Fe1 70.8(4) . . ? C6 C7 Fe1 69.5(3) . . ? C9 C8 C7 107.8(5) . . ? C9 C8 Fe1 69.9(4) . . ? C7 C8 Fe1 69.1(4) . . ? C8 C9 C10 109.1(6) . . ? C8 C9 Fe1 70.4(4) . . ? C10 C9 Fe1 69.5(4) . . ? C9 C10 C6 107.4(5) . . ? C9 C10 Fe1 70.2(4) . . ? C6 C10 Fe1 69.2(3) . . ? C12 C11 C16 119.8(7) . . ? C12 C11 Se1 116.6(5) . . y C16 C11 Se1 123.6(5) . . y C11 C12 C13 120.7(8) . . ? C12 C13 C14 119.3(8) . . ? C15 C14 C13 120.1(8) . . ? C14 C15 C16 120.0(8) . . ? C11 C16 C15 120.1(7) . . ? C22 C21 C26 113.3(5) . . ? C22 C21 Au1 120.7(4) . . y C26 C21 Au1 125.8(4) . . y C21 C22 F1 118.8(5) . . ? C21 C22 C23 125.3(6) . . ? F1 C22 C23 115.8(6) . . ? F2 C23 C24 120.5(6) . . ? F2 C23 C22 121.4(6) . . ? C24 C23 C22 118.2(6) . . ? F3 C24 C23 119.8(6) . . ? F3 C24 C25 120.0(6) . . ? C23 C24 C25 120.2(6) . . ? F4 C25 C24 119.8(6) . . ? F4 C25 C26 122.5(6) . . ? C24 C25 C26 117.7(5) . . ? C21 C26 C25 125.3(6) . . ? C21 C26 F5 119.9(5) . . ? C25 C26 F5 114.7(5) . . ? C32 C31 C36 118.8(5) . . ? C32 C31 P1 119.2(4) . . ? C36 C31 P1 122.0(4) . . ? C33 C32 C31 121.2(6) . . ? C32 C33 C34 120.2(6) . . ? C35 C34 C33 118.9(6) . . ? C34 C35 C36 120.1(6) . . ? C31 C36 C35 120.7(6) . . ? C42 C41 C46 118.9(6) . . ? C42 C41 P1 118.8(5) . . ? C46 C41 P1 122.4(5) . . ? C41 C42 C43 120.8(7) . . ? C44 C43 C42 119.6(7) . . ? C43 C44 C45 120.2(7) . . ? C44 C45 C46 120.9(7) . . ? C45 C46 C41 119.6(6) . . ? C71 Au2 P2 178.62(16) . . y C51 Se2 C61 99.8(3) . . y C56 P2 C81 105.4(3) . . y C56 P2 C91 105.4(3) . . y C81 P2 C91 105.0(3) . . y C56 P2 Au2 111.82(19) . . y C81 P2 Au2 113.0(2) . . y C91 P2 Au2 115.4(2) . . y C51 Fe2 C56 168.4(2) . . ? C51 Fe2 C52 41.1(2) . . ? C56 Fe2 C52 150.2(2) . . ? C51 Fe2 C55 41.2(2) . . ? C56 Fe2 C55 130.8(2) . . ? C52 Fe2 C55 68.8(2) . . ? C51 Fe2 C60 148.4(2) . . ? C56 Fe2 C60 41.0(2) . . ? C52 Fe2 C60 115.3(2) . . ? C55 Fe2 C60 168.7(2) . . ? C51 Fe2 C57 128.4(2) . . ? C56 Fe2 C57 41.2(2) . . ? C52 Fe2 C57 165.5(2) . . ? C55 Fe2 C57 109.8(2) . . ? C60 Fe2 C57 69.0(2) . . ? C51 Fe2 C59 115.4(3) . . ? C56 Fe2 C59 68.3(2) . . ? C52 Fe2 C59 105.5(3) . . ? C55 Fe2 C59 150.5(3) . . ? C60 Fe2 C59 40.4(2) . . ? C57 Fe2 C59 68.2(2) . . ? C51 Fe2 C53 68.7(2) . . ? C56 Fe2 C53 118.8(2) . . ? C52 Fe2 C53 40.6(2) . . ? C55 Fe2 C53 68.2(3) . . ? C60 Fe2 C53 107.5(3) . . ? C57 Fe2 C53 153.5(3) . . ? C59 Fe2 C53 127.1(3) . . ? C51 Fe2 C58 106.4(2) . . ? C56 Fe2 C58 68.7(2) . . ? C52 Fe2 C58 126.7(3) . . ? C55 Fe2 C58 118.0(3) . . ? C60 Fe2 C58 68.8(3) . . ? C57 Fe2 C58 40.2(2) . . ? C59 Fe2 C58 41.0(2) . . ? C53 Fe2 C58 165.1(3) . . ? C51 Fe2 C54 68.6(2) . . ? C56 Fe2 C54 110.5(2) . . ? C52 Fe2 C54 68.5(3) . . ? C55 Fe2 C54 40.2(2) . . ? C60 Fe2 C54 129.9(2) . . ? C57 Fe2 C54 120.4(2) . . ? C59 Fe2 C54 166.4(3) . . ? C53 Fe2 C54 40.7(3) . . ? C58 Fe2 C54 152.3(3) . . ? C52 C51 C55 107.6(6) . . ? C52 C51 Se2 125.8(5) . . ? C55 C51 Se2 126.3(5) . . ? C52 C51 Fe2 69.9(3) . . ? C55 C51 Fe2 69.9(3) . . ? Se2 C51 Fe2 120.9(3) . . ? C53 C52 C51 107.8(6) . . ? C53 C52 Fe2 70.0(3) . . ? C51 C52 Fe2 69.0(3) . . ? C52 C53 C54 108.6(5) . . ? C52 C53 Fe2 69.4(3) . . ? C54 C53 Fe2 70.6(3) . . ? C55 C54 C53 107.3(6) . . ? C55 C54 Fe2 68.8(3) . . ? C53 C54 Fe2 68.8(3) . . ? C54 C55 C51 108.6(6) . . ? C54 C55 Fe2 71.0(3) . . ? C51 C55 Fe2 68.9(3) . . ? C60 C56 C57 107.7(5) . . ? C60 C56 P2 128.9(4) . . y C57 C56 P2 123.4(4) . . y C60 C56 Fe2 69.6(3) . . ? C57 C56 Fe2 69.6(3) . . ? P2 C56 Fe2 126.9(3) . . ? C58 C57 C56 108.5(5) . . ? C58 C57 Fe2 70.6(3) . . ? C56 C57 Fe2 69.2(3) . . ? C57 C58 C59 107.2(5) . . ? C57 C58 Fe2 69.2(3) . . ? C59 C58 Fe2 69.0(3) . . ? C60 C59 C58 108.9(5) . . ? C60 C59 Fe2 69.6(3) . . ? C58 C59 Fe2 70.0(3) . . ? C59 C60 C56 107.7(5) . . ? C59 C60 Fe2 70.0(3) . . ? C56 C60 Fe2 69.4(3) . . ? C66 C61 C62 120.0(6) . . ? C66 C61 Se2 123.6(5) . . y C62 C61 Se2 116.4(5) . . y C63 C62 C61 118.9(7) . . ? C64 C63 C62 120.6(7) . . ? C65 C64 C63 120.4(7) . . ? C64 C65 C66 119.5(8) . . ? C61 C66 C65 120.6(7) . . ? C76 C71 C72 115.0(5) . . ? C76 C71 Au2 121.6(4) . . y C72 C71 Au2 122.8(4) . . y F6 C72 C71 120.2(6) . . ? F6 C72 C73 116.4(6) . . ? C71 C72 C73 123.4(6) . . ? F7 C73 C74 119.3(6) . . ? F7 C73 C72 121.1(6) . . ? C74 C73 C72 119.5(6) . . ? F8 C74 C75 120.5(6) . . ? F8 C74 C73 120.5(6) . . ? C75 C74 C73 118.9(6) . . ? F9 C75 C74 119.1(6) . . ? F9 C75 C76 121.1(6) . . ? C74 C75 C76 119.8(6) . . ? F10 C76 C71 120.7(5) . . ? F10 C76 C75 116.0(6) . . ? C71 C76 C75 123.3(6) . . ? C82 C81 C86 119.2(5) . . ? C82 C81 P2 118.2(5) . . y C86 C81 P2 122.6(5) . . y C81 C82 C83 119.6(7) . . ? C84 C83 C82 120.7(7) . . ? C83 C84 C85 120.5(7) . . ? C84 C85 C86 119.8(7) . . ? C81 C86 C85 120.2(7) . . ? C92 C91 C96 117.8(6) . . ? C92 C91 P2 123.4(5) . . y C96 C91 P2 118.8(5) . . y C93 C92 C91 121.2(6) . . ? C92 C93 C94 120.2(6) . . ? C95 C94 C93 120.3(6) . . ? C94 C95 C96 119.8(6) . . ? C95 C96 C91 120.6(6) . . ? _diffrn_measured_fraction_theta_max 0.873 _diffrn_reflns_theta_full 28.71 _diffrn_measured_fraction_theta_full 0.873 _refine_diff_density_max 2.175 _refine_diff_density_min -1.490 _refine_diff_density_rms 0.153 ########################################################## data_getnit(complex15) _database_code_depnum_ccdc_archive 'CCDC 272432' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29.25 H23.50 Ag Cl0.50 F3 Fe O3 P S2' _chemical_formula_weight 756.52 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' F F 0.0171 0.0103 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 11.5500(10) _cell_length_b 12.6343(10) _cell_length_c 19.8830(16) _cell_angle_alpha 87.345(3) _cell_angle_beta 87.028(3) _cell_angle_gamma 80.112(3) _cell_volume 2852.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 7750 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1514 _exptl_absorpt_coefficient_mu 1.496 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.586 _exptl_absorpt_correction_T_max 0.918 _exptl_absorpt_process_details ; Program XPREP Based on indexed faces FACE -1.00 0.00 0.00 0.132 FACE 1.00 0.00 0.00 0.141 FACE 0.00 0.00 -1.00 0.020 FACE 0.00 0.00 1.00 0.039 FACE 0.00 -1.00 1.00 0.207 FACE 0.00 1.00 -1.00 0.148 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w- and \f-scan' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36536 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _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 1.64 _diffrn_reflns_theta_max 30.03 _reflns_number_total 16266 _reflns_number_gt 12237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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. The dichloromethane is disordered over an inversion centre. ; _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^)+(0.0410P)^2^] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16266 _refine_ls_number_parameters 743 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.010 _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 Ag Ag 0.430314(14) 0.610527(14) 0.059461(8) 0.02162(5) Uani 1 1 d . . . Fe Fe 0.45801(3) 0.89819(3) 0.134491(15) 0.01703(7) Uani 1 1 d . . . P P 0.30549(5) 0.68785(5) 0.15023(3) 0.01740(11) Uani 1 1 d . . . S1 S 0.54174(5) 0.76405(5) -0.00130(3) 0.02079(11) Uani 1 1 d . . . C11 C 0.67692(19) 0.72591(18) -0.04881(11) 0.0202(4) Uani 1 1 d . . . C12 C 0.6682(2) 0.7005(2) -0.11543(13) 0.0359(6) Uani 1 1 d . . . H12 H 0.5934 0.7000 -0.1330 0.043 Uiso 1 1 calc R . . C13 C 0.7697(3) 0.6760(3) -0.15608(14) 0.0423(7) Uani 1 1 d . . . H13 H 0.7642 0.6582 -0.2016 0.051 Uiso 1 1 calc R . . C14 C 0.8793(2) 0.6772(2) -0.13082(14) 0.0343(6) Uani 1 1 d . . . H14 H 0.9485 0.6617 -0.1590 0.041 Uiso 1 1 calc R . . C15 C 0.8867(2) 0.7011(2) -0.06457(14) 0.0340(6) Uani 1 1 d . . . H15 H 0.9616 0.7004 -0.0468 0.041 Uiso 1 1 calc R . . C16 C 0.7856(2) 0.7263(2) -0.02317(12) 0.0276(5) Uani 1 1 d . . . H16 H 0.7913 0.7436 0.0224 0.033 Uiso 1 1 calc R . . C21 C 0.3467(2) 0.63057(19) 0.23305(11) 0.0218(4) Uani 1 1 d . . . C22 C 0.2788(2) 0.6605(2) 0.29191(12) 0.0315(6) Uani 1 1 d . . . H22 H 0.2072 0.7101 0.2893 0.038 Uiso 1 1 calc R . . C23 C 0.3175(3) 0.6166(2) 0.35436(13) 0.0394(7) Uani 1 1 d . . . H23 H 0.2721 0.6364 0.3945 0.047 Uiso 1 1 calc R . . C24 C 0.4213(3) 0.5447(3) 0.35769(14) 0.0413(7) Uani 1 1 d . . . H24 H 0.4474 0.5159 0.4003 0.050 Uiso 1 1 calc R . . C25 C 0.4875(3) 0.5141(2) 0.30031(15) 0.0381(6) Uani 1 1 d . . . H25 H 0.5589 0.4643 0.3033 0.046 Uiso 1 1 calc R . . C26 C 0.4497(2) 0.5566(2) 0.23787(13) 0.0295(5) Uani 1 1 d . . . H26 H 0.4949 0.5346 0.1981 0.035 Uiso 1 1 calc R . . C31 C 0.14887(19) 0.68596(18) 0.14620(11) 0.0196(4) Uani 1 1 d . . . C32 C 0.0628(2) 0.7650(2) 0.17551(12) 0.0253(5) Uani 1 1 d . . . H32 H 0.0851 0.8233 0.1973 0.030 Uiso 1 1 calc R . . C33 C -0.0545(2) 0.7569(2) 0.17234(13) 0.0282(5) Uani 1 1 d . . . H33 H -0.1129 0.8097 0.1925 0.034 Uiso 1 1 calc R . . C34 C -0.0880(2) 0.6731(2) 0.14027(13) 0.0276(5) Uani 1 1 d . . . H34 H -0.1690 0.6682 0.1389 0.033 Uiso 1 1 calc R . . C35 C -0.0037(2) 0.5961(2) 0.11003(13) 0.0276(5) Uani 1 1 d . . . H35 H -0.0267 0.5391 0.0872 0.033 Uiso 1 1 calc R . . C36 C 0.11427(19) 0.60278(19) 0.11337(12) 0.0229(5) Uani 1 1 d . . . H36 H 0.1722 0.5498 0.0929 0.027 Uiso 1 1 calc R . . C41 C 0.58306(18) 0.82714(18) 0.06906(11) 0.0187(4) Uani 1 1 d . . . C42 C 0.58993(18) 0.93867(19) 0.07137(12) 0.0216(5) Uani 1 1 d . . . H42 H 0.5815 0.9898 0.0346 0.026 Uiso 1 1 calc R . . C43 C 0.61165(19) 0.9590(2) 0.13888(12) 0.0244(5) Uani 1 1 d . . . H43 H 0.6203 1.0266 0.1551 0.029 Uiso 1 1 calc R . . C44 C 0.61821(19) 0.8611(2) 0.17808(12) 0.0240(5) Uani 1 1 d . . . H44 H 0.6315 0.8522 0.2249 0.029 Uiso 1 1 calc R . . C45 C 0.60140(18) 0.77912(19) 0.13501(11) 0.0211(4) Uani 1 1 d . . . H45 H 0.6022 0.7056 0.1477 0.025 Uiso 1 1 calc R . . C46 C 0.31185(18) 0.82886(18) 0.15417(11) 0.0186(4) Uani 1 1 d . . . C47 C 0.29697(18) 0.90046(18) 0.09572(12) 0.0210(4) Uani 1 1 d . . . H47 H 0.2830 0.8807 0.0517 0.025 Uiso 1 1 calc R . . C48 C 0.30651(19) 1.00520(19) 0.11442(13) 0.0246(5) Uani 1 1 d . . . H48 H 0.2997 1.0676 0.0854 0.029 Uiso 1 1 calc R . . C49 C 0.32805(19) 1.00058(19) 0.18413(13) 0.0257(5) Uani 1 1 d . . . H49 H 0.3386 1.0596 0.2097 0.031 Uiso 1 1 calc R . . C50 C 0.33122(19) 0.89249(19) 0.20953(12) 0.0221(5) Uani 1 1 d . . . H50 H 0.3438 0.8671 0.2547 0.026 Uiso 1 1 calc R . . S2 S 0.70143(5) 0.44964(5) 0.08166(3) 0.02155(11) Uani 1 1 d . . . C99 C 0.7302(2) 0.3084(2) 0.10748(15) 0.0358(6) Uani 1 1 d . . . O1 O 0.58789(14) 0.45837(14) 0.04957(8) 0.0264(4) Uani 1 1 d . . . O2 O 0.79849(17) 0.46181(18) 0.03676(10) 0.0426(5) Uani 1 1 d . . . O3 O 0.69240(16) 0.50436(17) 0.14375(9) 0.0391(5) Uani 1 1 d . . . F1 F 0.83207(14) 0.28476(14) 0.13798(9) 0.0472(4) Uani 1 1 d . . . F2 F 0.73803(18) 0.24624(15) 0.05489(12) 0.0652(6) Uani 1 1 d . . . F3 F 0.64691(18) 0.28176(19) 0.15012(12) 0.0743(7) Uani 1 1 d . . . Ag' Ag 0.919012(16) -0.115729(15) 0.516554(9) 0.02771(5) Uani 1 1 d . . . Fe' Fe 0.73823(3) -0.31894(3) 0.433113(16) 0.02084(7) Uani 1 1 d . . . P' P 0.83622(5) -0.24872(5) 0.58226(3) 0.02047(12) Uani 1 1 d . . . S1' S 0.93594(5) -0.16964(5) 0.38589(3) 0.02423(12) Uani 1 1 d . . . C111 C 0.9454(2) -0.06288(19) 0.32531(11) 0.0219(5) Uani 1 1 d . . . C112 C 1.0519(2) -0.0253(2) 0.31827(12) 0.0252(5) Uani 1 1 d . . . H112 H 1.1135 -0.0530 0.3473 0.030 Uiso 1 1 calc R . . C113 C 1.0681(2) 0.0519(2) 0.26931(13) 0.0294(5) Uani 1 1 d . . . H113 H 1.1406 0.0781 0.2652 0.035 Uiso 1 1 calc R . . C114 C 0.9799(2) 0.0917(2) 0.22598(13) 0.0316(6) Uani 1 1 d . . . H114 H 0.9924 0.1436 0.1915 0.038 Uiso 1 1 calc R . . C115 C 0.8725(2) 0.0554(2) 0.23305(14) 0.0335(6) Uani 1 1 d . . . H115 H 0.8115 0.0828 0.2035 0.040 Uiso 1 1 calc R . . C116 C 0.8547(2) -0.0209(2) 0.28321(13) 0.0285(5) Uani 1 1 d . . . H116 H 0.7809 -0.0444 0.2888 0.034 Uiso 1 1 calc R . . C121 C 0.7009(2) -0.20010(19) 0.63090(11) 0.0226(5) Uani 1 1 d . . . C122 C 0.6418(2) -0.2685(2) 0.67193(12) 0.0279(5) Uani 1 1 d . . . H122 H 0.6731 -0.3430 0.6759 0.034 Uiso 1 1 calc R . . C123 C 0.5374(2) -0.2278(2) 0.70705(13) 0.0339(6) Uani 1 1 d . . . H123 H 0.4977 -0.2744 0.7351 0.041 Uiso 1 1 calc R . . C124 C 0.4917(2) -0.1198(3) 0.70109(13) 0.0386(7) Uani 1 1 d . . . H124 H 0.4196 -0.0924 0.7244 0.046 Uiso 1 1 calc R . . C125 C 0.5496(2) -0.0515(2) 0.66173(14) 0.0372(7) Uani 1 1 d . . . H125 H 0.5182 0.0231 0.6587 0.045 Uiso 1 1 calc R . . C126 C 0.6540(2) -0.0910(2) 0.62628(12) 0.0280(5) Uani 1 1 d . . . H126 H 0.6933 -0.0434 0.5989 0.034 Uiso 1 1 calc R . . C131 C 0.93278(19) -0.33235(19) 0.64104(11) 0.0215(5) Uani 1 1 d . . . C132 C 0.9128(2) -0.4334(2) 0.66520(12) 0.0252(5) Uani 1 1 d . . . H132 H 0.8479 -0.4618 0.6503 0.030 Uiso 1 1 calc R . . C133 C 0.9878(2) -0.4929(2) 0.71106(12) 0.0283(5) Uani 1 1 d . . . H133 H 0.9731 -0.5612 0.7279 0.034 Uiso 1 1 calc R . . C134 C 1.0845(2) -0.4526(2) 0.73246(12) 0.0286(5) Uani 1 1 d . . . H134 H 1.1353 -0.4926 0.7641 0.034 Uiso 1 1 calc R . . C135 C 1.1054(2) -0.3531(2) 0.70680(12) 0.0290(5) Uani 1 1 d . . . H135 H 1.1719 -0.3258 0.7204 0.035 Uiso 1 1 calc R . . C136 C 1.0305(2) -0.2932(2) 0.66167(12) 0.0244(5) Uani 1 1 d . . . H136 H 1.0458 -0.2252 0.6447 0.029 Uiso 1 1 calc R . . C141 C 0.7939(2) -0.19792(19) 0.37763(11) 0.0227(5) Uani 1 1 d . . . C142 C 0.7640(2) -0.2757(2) 0.33424(12) 0.0305(6) Uani 1 1 d . . . H142 H 0.8158 -0.3159 0.3024 0.037 Uiso 1 1 calc R . . C143 C 0.6445(2) -0.2820(2) 0.34718(14) 0.0366(6) Uani 1 1 d . . . H143 H 0.6017 -0.3270 0.3251 0.044 Uiso 1 1 calc R . . C144 C 0.5983(2) -0.2102(2) 0.39845(15) 0.0361(6) Uani 1 1 d . . . H144 H 0.5198 -0.1994 0.4169 0.043 Uiso 1 1 calc R . . C145 C 0.6904(2) -0.1570(2) 0.41763(13) 0.0279(5) Uani 1 1 d . . . H145 H 0.6842 -0.1043 0.4508 0.034 Uiso 1 1 calc R . . C146 C 0.79660(19) -0.34692(18) 0.52838(11) 0.0198(4) Uani 1 1 d . . . C147 C 0.8792(2) -0.40434(19) 0.48079(11) 0.0235(5) Uani 1 1 d . . . H147 H 0.9589 -0.3957 0.4727 0.028 Uiso 1 1 calc R . . C148 C 0.8209(2) -0.4761(2) 0.44804(12) 0.0283(5) Uani 1 1 d . . . H148 H 0.8553 -0.5245 0.4145 0.034 Uiso 1 1 calc R . . C149 C 0.7033(2) -0.4638(2) 0.47348(12) 0.0277(5) Uani 1 1 d . . . H149 H 0.6449 -0.5018 0.4599 0.033 Uiso 1 1 calc R . . C150 C 0.6875(2) -0.38373(19) 0.52354(11) 0.0230(5) Uani 1 1 d . . . H150 H 0.6167 -0.3595 0.5490 0.028 Uiso 1 1 calc R . . S2' S 0.79488(5) 0.16585(5) 0.50967(3) 0.02666(13) Uani 1 1 d . . . C199 C 0.6847(2) 0.1817(2) 0.44598(15) 0.0361(6) Uani 1 1 d . . . O1' O 0.88085(15) 0.07240(14) 0.48763(10) 0.0316(4) Uani 1 1 d . . . O2' O 0.84149(16) 0.26414(15) 0.50358(10) 0.0342(4) Uani 1 1 d . . . O3' O 0.72949(17) 0.14523(16) 0.57114(10) 0.0395(5) Uani 1 1 d . . . F1' F 0.62614(17) 0.10020(16) 0.44976(11) 0.0610(6) Uani 1 1 d . . . F2' F 0.60689(15) 0.27072(16) 0.45543(11) 0.0559(5) Uani 1 1 d . . . F3' F 0.73208(16) 0.18924(19) 0.38423(9) 0.0599(6) Uani 1 1 d . . . Cl1 Cl 0.87506(19) -0.02058(19) 0.04997(12) 0.0533(5) Uani 0.50 1 d PDU A -1 Cl2 Cl 1.0748(3) 0.0170(4) -0.03641(19) 0.1130(14) Uani 0.50 1 d PDU A -1 C299 C 1.0148(11) -0.0306(15) 0.0343(7) 0.157(6) Uiso 0.50 1 d PD A -1 H29A H 1.0477 -0.1083 0.0379 0.189 Uiso 0.50 1 calc PR A -1 H29B H 1.0459 0.0031 0.0719 0.189 Uiso 0.50 1 calc PR A -1 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 Ag 0.02026(8) 0.02315(9) 0.02079(8) -0.00562(6) 0.00018(6) -0.00087(6) Fe 0.01438(14) 0.01759(16) 0.01950(15) -0.00118(12) 0.00064(11) -0.00409(11) P 0.0165(2) 0.0172(3) 0.0188(3) -0.0016(2) 0.0015(2) -0.0041(2) S1 0.0177(2) 0.0253(3) 0.0200(3) -0.0021(2) 0.0011(2) -0.0058(2) C11 0.0214(10) 0.0174(11) 0.0208(10) 0.0022(8) 0.0027(8) -0.0026(8) C12 0.0310(13) 0.0493(18) 0.0277(13) -0.0129(12) 0.0000(10) -0.0045(12) C13 0.0454(16) 0.054(2) 0.0261(13) -0.0145(13) 0.0066(12) -0.0022(14) C14 0.0345(14) 0.0326(15) 0.0340(14) -0.0015(11) 0.0164(11) -0.0058(11) C15 0.0211(12) 0.0408(16) 0.0393(15) -0.0060(12) 0.0051(10) -0.0040(11) C16 0.0218(11) 0.0371(15) 0.0238(12) -0.0015(10) 0.0024(9) -0.0053(10) C21 0.0264(11) 0.0210(12) 0.0204(10) 0.0019(9) -0.0003(9) -0.0113(9) C22 0.0393(14) 0.0331(15) 0.0242(12) -0.0024(10) 0.0056(10) -0.0139(11) C23 0.0590(19) 0.0443(17) 0.0223(12) 0.0005(11) 0.0055(12) -0.0322(15) C24 0.0530(18) 0.0476(18) 0.0319(14) 0.0194(13) -0.0166(13) -0.0334(15) C25 0.0366(15) 0.0358(16) 0.0443(16) 0.0164(13) -0.0145(13) -0.0134(12) C26 0.0281(12) 0.0300(14) 0.0311(13) 0.0060(10) -0.0032(10) -0.0081(10) C31 0.0180(10) 0.0202(11) 0.0204(10) 0.0016(8) 0.0013(8) -0.0045(8) C32 0.0224(11) 0.0219(12) 0.0316(12) -0.0037(10) 0.0021(9) -0.0040(9) C33 0.0198(11) 0.0276(13) 0.0353(13) 0.0014(10) 0.0051(10) -0.0007(9) C34 0.0178(11) 0.0331(14) 0.0323(13) 0.0084(10) -0.0045(9) -0.0072(9) C35 0.0260(12) 0.0284(13) 0.0315(13) -0.0006(10) -0.0066(10) -0.0116(10) C36 0.0207(11) 0.0227(12) 0.0256(11) -0.0013(9) -0.0013(9) -0.0048(9) C41 0.0130(9) 0.0226(11) 0.0204(10) -0.0020(8) 0.0011(8) -0.0028(8) C42 0.0161(10) 0.0257(12) 0.0240(11) 0.0001(9) 0.0011(8) -0.0070(8) C43 0.0198(11) 0.0299(13) 0.0262(12) -0.0038(10) 0.0006(9) -0.0118(9) C44 0.0167(10) 0.0319(13) 0.0238(11) -0.0010(10) -0.0034(8) -0.0043(9) C45 0.0135(9) 0.0251(12) 0.0232(11) 0.0032(9) 0.0003(8) -0.0010(8) C46 0.0141(9) 0.0197(11) 0.0219(10) -0.0011(8) 0.0031(8) -0.0035(8) C47 0.0145(10) 0.0214(11) 0.0271(11) 0.0013(9) -0.0010(8) -0.0033(8) C48 0.0169(10) 0.0186(11) 0.0371(13) 0.0043(10) -0.0004(9) -0.0016(8) C49 0.0194(10) 0.0208(12) 0.0367(13) -0.0083(10) 0.0063(9) -0.0030(9) C50 0.0212(10) 0.0227(12) 0.0231(11) -0.0048(9) 0.0049(9) -0.0068(9) S2 0.0210(3) 0.0218(3) 0.0220(3) -0.0025(2) -0.0060(2) -0.0018(2) C99 0.0291(13) 0.0312(15) 0.0475(16) 0.0076(12) -0.0162(12) -0.0042(11) O1 0.0233(8) 0.0253(9) 0.0289(9) -0.0084(7) -0.0130(7) 0.0058(7) O2 0.0358(11) 0.0616(15) 0.0334(10) 0.0082(10) 0.0008(8) -0.0199(10) O3 0.0319(10) 0.0485(12) 0.0365(10) -0.0216(9) -0.0135(8) 0.0032(8) F1 0.0372(9) 0.0442(10) 0.0586(11) 0.0115(8) -0.0276(8) 0.0020(8) F2 0.0722(13) 0.0269(9) 0.0956(16) -0.0205(10) -0.0462(12) 0.0116(9) F3 0.0510(12) 0.0796(16) 0.0936(17) 0.0524(13) -0.0068(11) -0.0284(11) Ag' 0.02951(10) 0.02619(10) 0.02950(10) 0.00479(7) -0.00149(7) -0.01205(7) Fe' 0.02358(16) 0.01947(17) 0.01985(15) 0.00465(12) -0.00271(12) -0.00559(12) P' 0.0221(3) 0.0192(3) 0.0200(3) 0.0017(2) -0.0006(2) -0.0039(2) S1' 0.0237(3) 0.0272(3) 0.0219(3) 0.0061(2) -0.0019(2) -0.0065(2) C111 0.0257(11) 0.0206(11) 0.0196(10) -0.0004(9) 0.0025(9) -0.0061(9) C112 0.0219(11) 0.0267(13) 0.0265(12) -0.0022(10) 0.0011(9) -0.0036(9) C113 0.0241(12) 0.0261(13) 0.0381(14) -0.0048(11) 0.0074(10) -0.0061(10) C114 0.0402(14) 0.0241(13) 0.0300(13) 0.0068(10) 0.0036(11) -0.0073(11) C115 0.0364(14) 0.0299(14) 0.0354(14) 0.0129(11) -0.0091(11) -0.0105(11) C116 0.0261(12) 0.0300(14) 0.0316(13) 0.0067(10) -0.0073(10) -0.0113(10) C121 0.0228(11) 0.0248(12) 0.0194(10) -0.0011(9) -0.0024(8) -0.0016(9) C122 0.0297(12) 0.0280(13) 0.0255(12) -0.0025(10) 0.0024(10) -0.0036(10) C123 0.0288(13) 0.0471(17) 0.0257(12) -0.0046(11) 0.0047(10) -0.0074(12) C124 0.0248(13) 0.058(2) 0.0291(13) -0.0164(13) -0.0020(10) 0.0082(12) C125 0.0393(15) 0.0317(15) 0.0366(14) -0.0069(12) -0.0084(12) 0.0093(12) C126 0.0318(13) 0.0261(13) 0.0254(12) -0.0005(10) -0.0051(10) -0.0019(10) C131 0.0196(10) 0.0232(12) 0.0209(11) -0.0009(9) -0.0001(8) -0.0013(8) C132 0.0226(11) 0.0268(13) 0.0259(12) 0.0040(10) -0.0016(9) -0.0043(9) C133 0.0297(12) 0.0274(13) 0.0266(12) 0.0058(10) -0.0002(10) -0.0041(10) C134 0.0310(13) 0.0330(14) 0.0196(11) 0.0002(10) -0.0025(9) 0.0006(10) C135 0.0276(12) 0.0356(15) 0.0244(12) -0.0079(10) -0.0056(10) -0.0041(10) C136 0.0259(11) 0.0236(12) 0.0243(11) -0.0039(9) 0.0012(9) -0.0059(9) C141 0.0250(11) 0.0224(12) 0.0209(11) 0.0069(9) -0.0027(9) -0.0065(9) C142 0.0446(15) 0.0292(14) 0.0194(11) 0.0076(10) -0.0074(10) -0.0110(11) C143 0.0410(15) 0.0398(16) 0.0339(14) 0.0176(12) -0.0192(12) -0.0208(12) C144 0.0236(12) 0.0363(16) 0.0473(16) 0.0233(13) -0.0075(11) -0.0068(11) C145 0.0269(12) 0.0213(12) 0.0334(13) 0.0086(10) -0.0012(10) -0.0007(9) C146 0.0217(10) 0.0194(11) 0.0180(10) 0.0034(8) -0.0016(8) -0.0031(8) C147 0.0236(11) 0.0230(12) 0.0213(11) 0.0028(9) 0.0001(9) 0.0019(9) C148 0.0408(14) 0.0201(12) 0.0225(11) 0.0008(9) -0.0023(10) -0.0011(10) C149 0.0405(14) 0.0220(12) 0.0228(11) 0.0058(9) -0.0054(10) -0.0118(10) C150 0.0251(11) 0.0230(12) 0.0212(11) 0.0045(9) 0.0007(9) -0.0071(9) S2' 0.0237(3) 0.0223(3) 0.0336(3) 0.0023(2) -0.0034(2) -0.0029(2) C199 0.0258(13) 0.0367(16) 0.0461(16) 0.0016(13) -0.0083(12) -0.0049(11) O1' 0.0254(9) 0.0221(9) 0.0467(11) -0.0002(8) -0.0015(8) -0.0028(7) O2' 0.0333(10) 0.0255(10) 0.0445(11) 0.0018(8) -0.0055(8) -0.0066(8) O3' 0.0396(11) 0.0364(11) 0.0415(11) 0.0061(9) 0.0051(9) -0.0073(9) F1' 0.0513(11) 0.0538(12) 0.0860(15) -0.0001(11) -0.0287(11) -0.0249(9) F2' 0.0339(9) 0.0501(12) 0.0782(14) -0.0004(10) -0.0152(9) 0.0115(8) F3' 0.0457(11) 0.0961(17) 0.0379(10) 0.0003(10) -0.0092(8) -0.0106(10) Cl1 0.0440(11) 0.0579(12) 0.0551(13) 0.0127(9) -0.0125(9) -0.0011(9) Cl2 0.080(2) 0.172(4) 0.086(2) 0.052(2) 0.0112(18) -0.037(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 Ag P 2.3875(6) . Y Ag O1 2.4055(15) 2_665 Y Ag O1 2.4172(15) . Y Ag S1 2.7123(6) . Y Fe C41 2.013(2) . ? Fe C45 2.037(2) . ? Fe C42 2.042(2) . ? Fe C50 2.043(2) . ? Fe C46 2.044(2) . ? Fe C47 2.045(2) . ? Fe C49 2.049(2) . ? Fe C44 2.056(2) . ? Fe C43 2.059(2) . ? Fe C48 2.064(2) . ? P C46 1.801(2) . Y P C31 1.819(2) . Y P C21 1.821(2) . Y S1 C41 1.767(2) . Y S1 C11 1.787(2) . Y C11 C16 1.380(3) . ? C11 C12 1.390(3) . ? C12 C13 1.387(4) . ? C13 C14 1.388(4) . ? C14 C15 1.375(4) . ? C15 C16 1.393(3) . ? C21 C26 1.386(3) . ? C21 C22 1.404(3) . ? C22 C23 1.399(4) . ? C23 C24 1.377(5) . ? C24 C25 1.373(4) . ? C25 C26 1.391(4) . ? C31 C36 1.387(3) . ? C31 C32 1.406(3) . ? C32 C33 1.381(3) . ? C33 C34 1.380(4) . ? C34 C35 1.388(3) . ? C35 C36 1.385(3) . ? C41 C42 1.428(3) . ? C41 C45 1.429(3) . ? C42 C43 1.421(3) . ? C43 C44 1.424(4) . ? C44 C45 1.419(3) . ? C46 C47 1.438(3) . ? C46 C50 1.441(3) . ? C47 C48 1.415(3) . ? C48 C49 1.417(3) . ? C49 C50 1.429(3) . ? S2 O2 1.421(2) . Y S2 O3 1.4333(18) . Y S2 O1 1.4729(16) . Y S2 C99 1.813(3) . ? C99 F3 1.325(3) . ? C99 F2 1.327(3) . ? C99 F1 1.334(3) . ? O1 Ag 2.4055(15) 2_665 ? Ag' P' 2.3798(7) . Y Ag' O1' 2.3905(18) . Y Ag' O1' 2.4618(18) 2_756 Y Ag' S1' 2.7051(6) . Y Fe' C141 2.019(2) . ? Fe' C142 2.037(2) . ? Fe' C146 2.039(2) . ? Fe' C145 2.039(2) . ? Fe' C150 2.041(2) . ? Fe' C147 2.043(2) . ? Fe' C149 2.059(3) . ? Fe' C144 2.059(3) . ? Fe' C143 2.062(3) . ? Fe' C148 2.065(2) . ? P' C146 1.807(2) . Y P' C121 1.823(2) . Y P' C131 1.828(2) . Y S1' C141 1.755(2) . Y S1' C111 1.780(2) . Y C111 C112 1.391(3) . ? C111 C116 1.392(3) . ? C112 C113 1.375(4) . ? C113 C114 1.382(4) . ? C114 C115 1.392(4) . ? C115 C116 1.387(4) . ? C121 C126 1.393(3) . ? C121 C122 1.399(4) . ? C122 C123 1.393(3) . ? C123 C124 1.378(4) . ? C124 C125 1.374(5) . ? C125 C126 1.392(4) . ? C131 C136 1.395(3) . ? C131 C132 1.396(3) . ? C132 C133 1.393(3) . ? C133 C134 1.398(4) . ? C134 C135 1.390(4) . ? C135 C136 1.385(3) . ? C141 C142 1.434(3) . ? C141 C145 1.434(3) . ? C142 C143 1.406(4) . ? C143 C144 1.417(4) . ? C144 C145 1.429(4) . ? C146 C150 1.426(3) . ? C146 C147 1.437(3) . ? C147 C148 1.417(3) . ? C148 C149 1.410(4) . ? C149 C150 1.434(3) . ? S2' O2' 1.434(2) . Y S2' O3' 1.440(2) . Y S2' O1' 1.4738(18) . Y S2' C199 1.822(3) . ? C199 F1' 1.323(3) . ? C199 F3' 1.324(3) . ? C199 F2' 1.328(3) . ? O1' Ag' 2.4618(18) 2_756 ? Cl1 C299 1.612(12) . ? Cl2 C299 1.668(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 P Ag O1 138.60(4) . 2_665 Y P Ag O1 134.71(4) . . Y O1 Ag O1 74.92(6) 2_665 . Y P Ag S1 108.80(2) . . Y O1 Ag S1 88.95(5) 2_665 . Y O1 Ag S1 98.82(5) . . Y C41 Fe C45 41.33(9) . . ? C41 Fe C42 41.23(9) . . ? C45 Fe C42 69.25(9) . . ? C41 Fe C50 151.96(10) . . ? C45 Fe C50 117.47(10) . . ? C42 Fe C50 165.31(9) . . ? C41 Fe C46 118.11(9) . . ? C45 Fe C46 107.93(9) . . ? C42 Fe C46 152.09(9) . . ? C50 Fe C46 41.29(8) . . ? C41 Fe C47 108.66(9) . . ? C45 Fe C47 129.61(9) . . ? C42 Fe C47 118.11(9) . . ? C50 Fe C47 68.87(9) . . ? C46 Fe C47 41.18(9) . . ? C41 Fe C49 166.15(10) . . ? C45 Fe C49 150.98(10) . . ? C42 Fe C49 127.28(10) . . ? C50 Fe C49 40.88(10) . . ? C46 Fe C49 68.95(9) . . ? C47 Fe C49 68.03(9) . . ? C41 Fe C44 68.80(9) . . ? C45 Fe C44 40.56(9) . . ? C42 Fe C44 68.65(9) . . ? C50 Fe C44 107.25(10) . . ? C46 Fe C44 128.21(10) . . ? C47 Fe C44 167.47(10) . . ? C49 Fe C44 117.41(10) . . ? C41 Fe C43 68.58(9) . . ? C45 Fe C43 68.36(10) . . ? C42 Fe C43 40.56(9) . . ? C50 Fe C43 127.41(9) . . ? C46 Fe C43 166.17(9) . . ? C47 Fe C43 151.19(10) . . ? C49 Fe C43 107.42(10) . . ? C44 Fe C43 40.51(10) . . ? C41 Fe C48 128.63(10) . . ? C45 Fe C48 167.59(9) . . ? C42 Fe C48 107.68(10) . . ? C50 Fe C48 68.56(10) . . ? C46 Fe C48 68.80(9) . . ? C47 Fe C48 40.27(9) . . ? C49 Fe C48 40.32(10) . . ? C44 Fe C48 150.74(10) . . ? C43 Fe C48 117.68(10) . . ? C46 P C31 103.23(10) . . Y C46 P C21 104.98(10) . . Y C31 P C21 105.92(10) . . Y C46 P Ag 110.42(7) . . Y C31 P Ag 117.02(7) . . Y C21 P Ag 114.07(8) . . Y C41 S1 C11 103.97(10) . . Y C41 S1 Ag 101.43(8) . . Y C11 S1 Ag 119.83(8) . . Y C16 C11 C12 120.4(2) . . ? C16 C11 S1 122.95(17) . . ? C12 C11 S1 116.61(18) . . ? C13 C12 C11 119.4(2) . . ? C12 C13 C14 120.5(2) . . ? C15 C14 C13 119.4(2) . . ? C14 C15 C16 120.8(2) . . ? C11 C16 C15 119.5(2) . . ? C26 C21 C22 119.3(2) . . ? C26 C21 P 118.56(18) . . ? C22 C21 P 122.15(19) . . ? C23 C22 C21 119.4(3) . . ? C24 C23 C22 120.0(3) . . ? C25 C24 C23 121.0(3) . . ? C24 C25 C26 119.6(3) . . ? C21 C26 C25 120.7(3) . . ? C36 C31 C32 119.4(2) . . ? C36 C31 P 118.28(16) . . ? C32 C31 P 122.31(17) . . ? C33 C32 C31 119.3(2) . . ? C34 C33 C32 120.8(2) . . ? C33 C34 C35 120.2(2) . . ? C36 C35 C34 119.5(2) . . ? C35 C36 C31 120.7(2) . . ? C42 C41 C45 108.42(19) . . ? C42 C41 S1 125.11(18) . . ? C45 C41 S1 126.09(18) . . ? C42 C41 Fe 70.46(12) . . ? C45 C41 Fe 70.25(12) . . ? S1 C41 Fe 119.57(11) . . ? C43 C42 C41 107.3(2) . . ? C43 C42 Fe 70.36(13) . . ? C41 C42 Fe 68.31(12) . . ? C42 C43 C44 108.6(2) . . ? C42 C43 Fe 69.08(13) . . ? C44 C43 Fe 69.63(13) . . ? C45 C44 C43 108.1(2) . . ? C45 C44 Fe 69.03(12) . . ? C43 C44 Fe 69.86(13) . . ? C44 C45 C41 107.6(2) . . ? C44 C45 Fe 70.41(13) . . ? C41 C45 Fe 68.42(12) . . ? C47 C46 C50 106.8(2) . . ? C47 C46 P 121.91(16) . . ? C50 C46 P 131.27(18) . . ? C47 C46 Fe 69.46(12) . . ? C50 C46 Fe 69.33(12) . . ? P C46 Fe 125.88(11) . . ? C48 C47 C46 108.9(2) . . ? C48 C47 Fe 70.57(13) . . ? C46 C47 Fe 69.36(12) . . ? C47 C48 C49 107.9(2) . . ? C47 C48 Fe 69.16(12) . . ? C49 C48 Fe 69.28(13) . . ? C48 C49 C50 108.7(2) . . ? C48 C49 Fe 70.40(13) . . ? C50 C49 Fe 69.35(12) . . ? C49 C50 C46 107.6(2) . . ? C49 C50 Fe 69.77(13) . . ? C46 C50 Fe 69.37(12) . . ? O2 S2 O3 117.03(13) . . ? O2 S2 O1 114.94(11) . . ? O3 S2 O1 113.06(10) . . ? O2 S2 C99 103.54(14) . . ? O3 S2 C99 104.04(13) . . ? O1 S2 C99 101.71(11) . . ? F3 C99 F2 108.0(3) . . ? F3 C99 F1 107.6(2) . . ? F2 C99 F1 107.3(2) . . ? F3 C99 S2 112.1(2) . . ? F2 C99 S2 111.3(2) . . ? F1 C99 S2 110.36(19) . . ? S2 O1 Ag 122.88(9) . 2_665 Y S2 O1 Ag 124.12(9) . . Y Ag O1 Ag 105.08(6) 2_665 . Y P' Ag' O1' 140.65(4) . . Y P' Ag' O1' 130.38(5) . 2_756 Y O1' Ag' O1' 78.82(6) . 2_756 Y P' Ag' S1' 108.83(2) . . Y O1' Ag' S1' 92.61(5) . . Y O1' Ag' S1' 92.86(5) 2_756 . Y C141 Fe' C142 41.40(10) . . ? C141 Fe' C146 117.21(9) . . ? C142 Fe' C146 150.98(10) . . ? C141 Fe' C145 41.38(9) . . ? C142 Fe' C145 69.28(11) . . ? C146 Fe' C145 108.07(10) . . ? C141 Fe' C150 150.71(10) . . ? C142 Fe' C150 166.73(10) . . ? C146 Fe' C150 40.91(9) . . ? C145 Fe' C150 117.06(10) . . ? C141 Fe' C147 108.06(10) . . ? C142 Fe' C147 117.16(10) . . ? C146 Fe' C147 41.22(8) . . ? C145 Fe' C147 129.89(10) . . ? C150 Fe' C147 68.78(9) . . ? C141 Fe' C149 167.00(10) . . ? C142 Fe' C149 128.13(10) . . ? C146 Fe' C149 68.73(9) . . ? C145 Fe' C149 150.42(10) . . ? C150 Fe' C149 40.96(9) . . ? C147 Fe' C149 68.10(10) . . ? C141 Fe' C144 68.87(10) . . ? C142 Fe' C144 68.24(11) . . ? C146 Fe' C144 129.59(11) . . ? C145 Fe' C144 40.81(11) . . ? C150 Fe' C144 108.25(10) . . ? C147 Fe' C144 168.73(11) . . ? C149 Fe' C144 117.32(11) . . ? C141 Fe' C143 68.44(10) . . ? C142 Fe' C143 40.11(11) . . ? C146 Fe' C143 167.74(11) . . ? C145 Fe' C143 68.33(11) . . ? C150 Fe' C143 129.18(10) . . ? C147 Fe' C143 149.91(11) . . ? C149 Fe' C143 108.24(10) . . ? C144 Fe' C143 40.22(12) . . ? C141 Fe' C148 129.28(10) . . ? C142 Fe' C148 108.01(10) . . ? C146 Fe' C148 68.47(9) . . ? C145 Fe' C148 168.37(10) . . ? C150 Fe' C148 68.16(10) . . ? C147 Fe' C148 40.36(10) . . ? C149 Fe' C148 39.98(10) . . ? C144 Fe' C148 149.80(11) . . ? C143 Fe' C148 117.40(11) . . ? C146 P' C121 104.42(11) . . Y C146 P' C131 102.42(10) . . Y C121 P' C131 105.91(10) . . Y C146 P' Ag' 110.25(8) . . Y C121 P' Ag' 115.74(8) . . Y C131 P' Ag' 116.63(8) . . Y C141 S1' C111 103.68(11) . . Y C141 S1' Ag' 99.66(8) . . Y C111 S1' Ag' 116.03(8) . . Y C112 C111 C116 119.7(2) . . ? C112 C111 S1' 117.02(18) . . ? C116 C111 S1' 123.17(18) . . ? C113 C112 C111 120.1(2) . . ? C112 C113 C114 120.5(2) . . ? C113 C114 C115 119.8(2) . . ? C116 C115 C114 120.0(2) . . ? C115 C116 C111 119.8(2) . . ? C126 C121 C122 118.9(2) . . ? C126 C121 P' 118.64(19) . . ? C122 C121 P' 122.47(18) . . ? C123 C122 C121 120.3(2) . . ? C124 C123 C122 119.8(3) . . ? C125 C124 C123 120.5(2) . . ? C124 C125 C126 120.3(3) . . ? C125 C126 C121 120.2(3) . . ? C136 C131 C132 119.3(2) . . ? C136 C131 P' 118.17(19) . . ? C132 C131 P' 122.53(18) . . ? C133 C132 C131 120.2(2) . . ? C132 C133 C134 120.3(2) . . ? C135 C134 C133 119.1(2) . . ? C136 C135 C134 120.8(2) . . ? C135 C136 C131 120.3(2) . . ? C142 C141 C145 107.8(2) . . ? C142 C141 S1' 125.35(19) . . ? C145 C141 S1' 126.56(19) . . ? C142 C141 Fe' 69.95(14) . . ? C145 C141 Fe' 70.04(14) . . ? S1' C141 Fe' 120.44(12) . . ? C143 C142 C141 107.9(2) . . ? C143 C142 Fe' 70.93(15) . . ? C141 C142 Fe' 68.65(13) . . ? C142 C143 C144 108.9(2) . . ? C142 C143 Fe' 68.96(14) . . ? C144 C143 Fe' 69.76(15) . . ? C143 C144 C145 108.1(2) . . ? C143 C144 Fe' 70.02(15) . . ? C145 C144 Fe' 68.84(14) . . ? C144 C145 C141 107.3(2) . . ? C144 C145 Fe' 70.35(15) . . ? C141 C145 Fe' 68.57(14) . . ? C150 C146 C147 107.4(2) . . ? C150 C146 P' 130.20(17) . . ? C147 C146 P' 122.38(17) . . ? C150 C146 Fe' 69.64(13) . . ? C147 C146 Fe' 69.58(13) . . ? P' C146 Fe' 126.45(12) . . ? C148 C147 C146 108.0(2) . . ? C148 C147 Fe' 70.65(14) . . ? C146 C147 Fe' 69.21(12) . . ? C149 C148 C147 108.7(2) . . ? C149 C148 Fe' 69.76(14) . . ? C147 C148 Fe' 68.99(13) . . ? C148 C149 C150 108.0(2) . . ? C148 C149 Fe' 70.26(14) . . ? C150 C149 Fe' 68.86(14) . . ? C146 C150 C149 107.9(2) . . ? C146 C150 Fe' 69.45(13) . . ? C149 C150 Fe' 70.18(13) . . ? O2' S2' O3' 117.47(12) . . ? O2' S2' O1' 112.63(11) . . ? O3' S2' O1' 113.63(12) . . ? O2' S2' C199 104.12(13) . . ? O3' S2' C199 103.49(13) . . ? O1' S2' C199 103.43(12) . . ? F1' C199 F3' 108.8(3) . . ? F1' C199 F2' 107.3(2) . . ? F3' C199 F2' 107.4(2) . . ? F1' C199 S2' 111.0(2) . . ? F3' C199 S2' 112.00(18) . . ? F2' C199 S2' 110.2(2) . . ? S2' O1' Ag' 135.99(11) . . Y S2' O1' Ag' 110.10(10) . 2_756 Y Ag' O1' Ag' 101.18(6) . 2_756 y Cl1 C299 Cl2 124.0(10) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.018 _refine_diff_density_min -1.080 _refine_diff_density_rms 0.099 ############################################################### data_con9as(complex16) _database_code_depnum_ccdc_archive 'CCDC 272433' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H23 Ag F3 Fe O3 P S Se' _chemical_formula_weight 782.18 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' F F 0.0171 0.0103 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 9.7756(9) _cell_length_b 12.0232(11) _cell_length_c 12.7493(12) _cell_angle_alpha 66.8900(10) _cell_angle_beta 86.717(2) _cell_angle_gamma 84.285(2) _cell_volume 1371.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1783 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 24.41 _exptl_crystal_description prims _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 2.757 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7332 _exptl_absorpt_correction_T_max 0.8096 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9061 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.1296 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.74 _reflns_number_total 6158 _reflns_number_gt 3488 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.02 (Bruker AXS, 1999)' _computing_data_reduction 'SAINT+ v. 6.02 (Bruker AXS, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v 6.10 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v 6.10 (Bruker, 2000)' _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^)+(0.0421P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6158 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1114 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 0.807 _refine_ls_restrained_S_all 0.807 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.27335(5) 0.44936(5) 1.09369(4) 0.03821(16) Uani 1 1 d . . . Se Se 0.43345(6) 0.62773(6) 1.05620(5) 0.03358(17) Uani 1 1 d . . . P P 0.70138(16) 0.75413(14) 0.75953(13) 0.0294(4) Uani 1 1 d . . . Fe Fe 0.35618(8) 0.84664(8) 0.78821(7) 0.0302(2) Uani 1 1 d . . . C1 C 0.3441(6) 0.7792(5) 0.9612(5) 0.0291(14) Uani 1 1 d . . . C2 C 0.4081(6) 0.8907(6) 0.9172(5) 0.0355(16) Uani 1 1 d . . . H2 H 0.4987 0.9023 0.9319 0.043 Uiso 1 1 calc R . . C3 C 0.3099(7) 0.9811(6) 0.8471(6) 0.0441(18) Uani 1 1 d . . . H3 H 0.3230 1.0649 0.8084 0.053 Uiso 1 1 calc R . . C4 C 0.1908(7) 0.9263(6) 0.8444(5) 0.0415(17) Uani 1 1 d . . . H4 H 0.1112 0.9659 0.8015 0.050 Uiso 1 1 calc R . . C5 C 0.2095(6) 0.8029(5) 0.9161(5) 0.0328(15) Uani 1 1 d . . . H5 H 0.1437 0.7451 0.9317 0.039 Uiso 1 1 calc R . . C6 C 0.5270(6) 0.7996(6) 0.7105(5) 0.0305(14) Uani 1 1 d . . . C7 C 0.4654(6) 0.9164(6) 0.6386(5) 0.0364(16) Uani 1 1 d . . . H7 H 0.5088 0.9901 0.6106 0.044 Uiso 1 1 calc R . . C8 C 0.3281(6) 0.9030(6) 0.6164(5) 0.0389(16) Uani 1 1 d . . . H8 H 0.2643 0.9663 0.5713 0.047 Uiso 1 1 calc R . . C9 C 0.3033(6) 0.7794(6) 0.6731(5) 0.0353(15) Uani 1 1 d . . . H9 H 0.2199 0.7451 0.6731 0.042 Uiso 1 1 calc R . . C10 C 0.4241(6) 0.7164(6) 0.7295(5) 0.0327(15) Uani 1 1 d . . . H10 H 0.4357 0.6316 0.7734 0.039 Uiso 1 1 calc R . . C11 C 0.4127(7) 0.6410(6) 1.2036(5) 0.0376(16) Uani 1 1 d . . . C12 C 0.3088(8) 0.5871(6) 1.2787(6) 0.054(2) Uani 1 1 d . . . H12 H 0.2443 0.5459 1.2575 0.064 Uiso 1 1 calc R . . C13 C 0.2989(9) 0.5933(7) 1.3858(7) 0.063(2) Uani 1 1 d . . . H13 H 0.2276 0.5560 1.4378 0.076 Uiso 1 1 calc R . . C14 C 0.3912(9) 0.6525(8) 1.4162(7) 0.064(2) Uani 1 1 d . . . H14 H 0.3878 0.6531 1.4906 0.077 Uiso 1 1 calc R . . C15 C 0.4884(8) 0.7109(9) 1.3385(8) 0.076(3) Uani 1 1 d . . . H15 H 0.5476 0.7584 1.3569 0.092 Uiso 1 1 calc R . . C16 C 0.5026(8) 0.7022(8) 1.2337(7) 0.068(3) Uani 1 1 d . . . H16 H 0.5749 0.7389 1.1826 0.082 Uiso 1 1 calc R . . C21 C 0.7940(6) 0.7789(5) 0.6244(5) 0.0325(15) Uani 1 1 d . . . C22 C 0.9178(6) 0.8346(5) 0.5959(5) 0.0330(15) Uani 1 1 d . . . H22 H 0.9542 0.8657 0.6454 0.040 Uiso 1 1 calc R . . C23 C 0.9870(7) 0.8438(6) 0.4949(6) 0.0440(17) Uani 1 1 d . . . H23 H 1.0700 0.8828 0.4747 0.053 Uiso 1 1 calc R . . C24 C 0.9361(7) 0.7969(7) 0.4244(6) 0.0493(19) Uani 1 1 d . . . H24 H 0.9854 0.8009 0.3567 0.059 Uiso 1 1 calc R . . C25 C 0.8141(7) 0.7445(7) 0.4518(6) 0.0454(18) Uani 1 1 d . . . H25 H 0.7776 0.7146 0.4015 0.054 Uiso 1 1 calc R . . C26 C 0.7439(7) 0.7346(6) 0.5504(6) 0.0410(17) Uani 1 1 d . . . H26 H 0.6599 0.6969 0.5683 0.049 Uiso 1 1 calc R . . C31 C 0.7551(6) 0.8670(6) 0.8066(5) 0.0330(15) Uani 1 1 d . . . C32 C 0.8039(7) 0.8272(7) 0.9160(6) 0.0464(18) Uani 1 1 d . . . H32 H 0.8122 0.7429 0.9623 0.056 Uiso 1 1 calc R . . C33 C 0.8410(7) 0.9099(7) 0.9591(6) 0.0462(18) Uani 1 1 d . . . H33 H 0.8725 0.8821 1.0350 0.055 Uiso 1 1 calc R . . C34 C 0.8318(7) 1.0308(7) 0.8918(7) 0.0474(19) Uani 1 1 d . . . H34 H 0.8585 1.0869 0.9209 0.057 Uiso 1 1 calc R . . C35 C 0.7848(7) 1.0723(6) 0.7828(6) 0.0465(18) Uani 1 1 d . . . H35 H 0.7775 1.1568 0.7373 0.056 Uiso 1 1 calc R . . C36 C 0.7474(6) 0.9907(6) 0.7384(6) 0.0404(16) Uani 1 1 d . . . H36 H 0.7169 1.0192 0.6621 0.048 Uiso 1 1 calc R . . S S -0.07240(16) 0.49311(15) 1.14873(14) 0.0343(4) Uani 1 1 d . . . O1 O 0.0386(4) 0.5657(4) 1.0898(4) 0.0399(11) Uani 1 1 d . . . O2 O -0.0341(4) 0.3646(4) 1.1988(4) 0.0458(12) Uani 1 1 d . . . O3 O -0.2026(4) 0.5264(4) 1.0929(4) 0.0394(11) Uani 1 1 d . . . C40 C -0.1071(8) 0.5369(7) 1.2687(6) 0.0502(19) Uani 1 1 d . . . F1 F -0.0039(5) 0.5058(5) 1.3395(4) 0.0760(14) Uani 1 1 d . . . F2 F -0.1373(5) 0.6560(4) 1.2340(4) 0.0736(14) Uani 1 1 d . . . F3 F -0.2170(4) 0.4847(5) 1.3311(4) 0.0752(15) Uani 1 1 d . . . 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 Ag 0.0434(3) 0.0335(3) 0.0334(3) -0.0085(2) -0.0010(2) -0.0030(2) Se 0.0339(4) 0.0327(4) 0.0301(4) -0.0091(3) 0.0049(3) -0.0008(3) P 0.0276(9) 0.0305(9) 0.0279(9) -0.0090(7) 0.0048(7) -0.0051(7) Fe 0.0293(5) 0.0290(5) 0.0277(5) -0.0068(4) 0.0063(4) -0.0027(4) C1 0.031(3) 0.028(3) 0.025(3) -0.007(3) 0.005(3) -0.005(3) C2 0.037(4) 0.031(4) 0.042(4) -0.019(3) 0.016(3) -0.009(3) C3 0.065(5) 0.029(4) 0.038(4) -0.015(3) 0.012(4) -0.001(3) C4 0.045(4) 0.042(4) 0.030(4) -0.009(3) 0.000(3) 0.012(3) C5 0.026(3) 0.033(4) 0.031(4) -0.005(3) 0.012(3) -0.002(3) C6 0.026(3) 0.039(4) 0.025(3) -0.011(3) 0.010(3) -0.005(3) C7 0.029(4) 0.047(4) 0.028(4) -0.009(3) 0.010(3) -0.007(3) C8 0.032(4) 0.049(4) 0.026(4) -0.004(3) 0.000(3) 0.000(3) C9 0.025(3) 0.050(4) 0.031(4) -0.016(3) 0.006(3) -0.005(3) C10 0.031(4) 0.037(4) 0.030(4) -0.011(3) 0.005(3) -0.010(3) C11 0.040(4) 0.039(4) 0.032(4) -0.014(3) 0.001(3) 0.002(3) C12 0.075(5) 0.039(4) 0.049(5) -0.017(4) 0.024(4) -0.028(4) C13 0.100(7) 0.053(5) 0.045(5) -0.027(4) 0.028(5) -0.024(5) C14 0.083(6) 0.070(6) 0.035(5) -0.018(4) -0.008(4) 0.007(5) C15 0.046(5) 0.128(9) 0.078(7) -0.066(7) -0.011(5) -0.002(5) C16 0.040(5) 0.117(8) 0.066(6) -0.055(6) 0.007(4) -0.016(5) C21 0.035(4) 0.025(3) 0.030(4) -0.004(3) 0.003(3) 0.002(3) C22 0.027(3) 0.034(4) 0.034(4) -0.009(3) 0.003(3) -0.001(3) C23 0.037(4) 0.048(4) 0.042(4) -0.012(4) 0.010(3) -0.009(3) C24 0.038(4) 0.065(5) 0.042(5) -0.021(4) 0.015(3) 0.001(4) C25 0.049(4) 0.061(5) 0.034(4) -0.027(4) 0.006(3) -0.010(4) C26 0.040(4) 0.042(4) 0.043(4) -0.018(3) 0.006(3) -0.008(3) C31 0.030(4) 0.033(4) 0.030(4) -0.007(3) 0.007(3) -0.004(3) C32 0.042(4) 0.048(4) 0.050(5) -0.019(4) 0.003(3) -0.010(3) C33 0.043(4) 0.053(5) 0.051(5) -0.029(4) 0.002(3) -0.005(4) C34 0.041(4) 0.056(5) 0.058(5) -0.036(4) 0.009(4) -0.010(4) C35 0.049(5) 0.027(4) 0.062(5) -0.017(4) 0.006(4) -0.006(3) C36 0.038(4) 0.038(4) 0.045(4) -0.016(3) 0.004(3) -0.006(3) S 0.0289(9) 0.0413(10) 0.0297(9) -0.0115(8) 0.0046(7) -0.0013(7) O1 0.040(3) 0.035(3) 0.039(3) -0.009(2) 0.008(2) -0.006(2) O2 0.044(3) 0.032(3) 0.048(3) -0.002(2) 0.001(2) 0.001(2) O3 0.032(2) 0.044(3) 0.038(3) -0.013(2) 0.001(2) 0.002(2) C40 0.046(5) 0.065(6) 0.040(5) -0.021(4) 0.007(4) -0.004(4) F1 0.069(3) 0.119(4) 0.051(3) -0.043(3) -0.009(2) -0.007(3) F2 0.094(4) 0.066(3) 0.077(4) -0.048(3) 0.011(3) -0.004(3) F3 0.070(3) 0.113(4) 0.047(3) -0.035(3) 0.027(2) -0.029(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 Ag O3 2.414(4) 2_567 ? Ag P 2.4264(17) 2_667 ? Ag O1 2.558(4) . ? Ag Se 2.6562(8) . ? Se C1 1.902(6) . ? Se C11 1.945(6) . ? P C6 1.806(6) . ? P C31 1.815(6) . ? P C21 1.830(6) . ? P Ag 2.4264(17) 2_667 ? Fe C2 2.019(6) . ? Fe C10 2.028(6) . ? Fe C1 2.030(6) . ? Fe C4 2.035(6) . ? Fe C3 2.037(6) . ? Fe C6 2.038(5) . ? Fe C7 2.042(6) . ? Fe C9 2.043(6) . ? Fe C5 2.049(5) . ? Fe C8 2.049(6) . ? C1 C5 1.424(8) . ? C1 C2 1.428(8) . ? C2 C3 1.425(9) . ? C3 C4 1.402(9) . ? C4 C5 1.404(8) . ? C6 C10 1.434(8) . ? C6 C7 1.434(8) . ? C7 C8 1.425(8) . ? C8 C9 1.413(8) . ? C9 C10 1.406(8) . ? C11 C16 1.360(9) . ? C11 C12 1.379(8) . ? C12 C13 1.394(9) . ? C13 C14 1.362(10) . ? C14 C15 1.362(11) . ? C15 C16 1.378(10) . ? C21 C26 1.383(8) . ? C21 C22 1.402(7) . ? C22 C23 1.389(8) . ? C23 C24 1.370(9) . ? C24 C25 1.368(9) . ? C25 C26 1.366(8) . ? C31 C32 1.382(9) . ? C31 C36 1.394(8) . ? C32 C33 1.395(8) . ? C33 C34 1.365(10) . ? C34 C35 1.370(9) . ? C35 C36 1.396(8) . ? S O3 1.437(4) . ? S O2 1.440(4) . ? S O1 1.444(4) . ? S C40 1.808(7) . ? O3 Ag 2.414(4) 2_567 ? C40 F1 1.317(8) . ? C40 F2 1.330(8) . ? C40 F3 1.351(7) . ? 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 O3 Ag P 118.21(11) 2_567 2_667 ? O3 Ag O1 81.11(13) 2_567 . ? P Ag O1 115.38(10) 2_667 . ? O3 Ag Se 105.14(10) 2_567 . ? P Ag Se 127.11(5) 2_667 . ? O1 Ag Se 99.21(9) . . ? C1 Se C11 100.5(3) . . ? C1 Se Ag 110.48(17) . . ? C11 Se Ag 99.3(2) . . ? C6 P C31 107.9(3) . . ? C6 P C21 100.7(3) . . ? C31 P C21 105.5(3) . . ? C6 P Ag 112.7(2) . 2_667 ? C31 P Ag 112.4(2) . 2_667 ? C21 P Ag 116.72(19) . 2_667 ? C2 Fe C10 135.0(3) . . ? C2 Fe C1 41.3(2) . . ? C10 Fe C1 111.7(2) . . ? C2 Fe C4 69.1(3) . . ? C10 Fe C4 146.0(3) . . ? C1 Fe C4 68.6(2) . . ? C2 Fe C3 41.1(3) . . ? C10 Fe C3 173.7(3) . . ? C1 Fe C3 68.5(3) . . ? C4 Fe C3 40.3(2) . . ? C2 Fe C6 110.8(2) . . ? C10 Fe C6 41.3(2) . . ? C1 Fe C6 119.0(2) . . ? C4 Fe C6 169.1(3) . . ? C3 Fe C6 132.7(3) . . ? C2 Fe C7 116.8(2) . . ? C10 Fe C7 68.5(2) . . ? C1 Fe C7 151.0(2) . . ? C4 Fe C7 128.4(3) . . ? C3 Fe C7 108.1(3) . . ? C6 Fe C7 41.2(2) . . ? C2 Fe C9 172.5(3) . . ? C10 Fe C9 40.4(2) . . ? C1 Fe C9 131.6(2) . . ? C4 Fe C9 112.2(3) . . ? C3 Fe C9 144.2(3) . . ? C6 Fe C9 69.3(2) . . ? C7 Fe C9 68.5(2) . . ? C2 Fe C5 69.0(2) . . ? C10 Fe C5 117.0(2) . . ? C1 Fe C5 40.8(2) . . ? C4 Fe C5 40.2(2) . . ? C3 Fe C5 67.6(2) . . ? C6 Fe C5 150.6(2) . . ? C7 Fe C5 166.6(3) . . ? C9 Fe C5 107.0(2) . . ? C2 Fe C8 147.0(3) . . ? C10 Fe C8 67.9(3) . . ? C1 Fe C8 168.1(2) . . ? C4 Fe C8 104.6(3) . . ? C3 Fe C8 113.2(3) . . ? C6 Fe C8 69.1(2) . . ? C7 Fe C8 40.8(2) . . ? C9 Fe C8 40.4(2) . . ? C5 Fe C8 127.8(2) . . ? C5 C1 C2 107.8(6) . . ? C5 C1 Se 128.2(4) . . ? C2 C1 Se 123.9(5) . . ? C5 C1 Fe 70.3(3) . . ? C2 C1 Fe 68.9(3) . . ? Se C1 Fe 123.6(3) . . ? C3 C2 C1 106.7(6) . . ? C3 C2 Fe 70.1(4) . . ? C1 C2 Fe 69.7(3) . . ? C4 C3 C2 108.9(6) . . ? C4 C3 Fe 69.8(4) . . ? C2 C3 Fe 68.7(4) . . ? C3 C4 C5 108.2(6) . . ? C3 C4 Fe 69.9(4) . . ? C5 C4 Fe 70.4(3) . . ? C4 C5 C1 108.3(5) . . ? C4 C5 Fe 69.4(3) . . ? C1 C5 Fe 68.9(3) . . ? C10 C6 C7 105.9(5) . . ? C10 C6 P 123.8(5) . . ? C7 C6 P 130.0(4) . . ? C10 C6 Fe 69.0(3) . . ? C7 C6 Fe 69.6(3) . . ? P C6 Fe 130.4(3) . . ? C8 C7 C6 108.4(5) . . ? C8 C7 Fe 69.9(3) . . ? C6 C7 Fe 69.3(3) . . ? C9 C8 C7 108.2(6) . . ? C9 C8 Fe 69.6(4) . . ? C7 C8 Fe 69.4(3) . . ? C10 C9 C8 107.8(6) . . ? C10 C9 Fe 69.2(4) . . ? C8 C9 Fe 70.0(4) . . ? C9 C10 C6 109.6(6) . . ? C9 C10 Fe 70.4(4) . . ? C6 C10 Fe 69.7(3) . . ? C16 C11 C12 119.6(7) . . ? C16 C11 Se 119.9(5) . . ? C12 C11 Se 120.5(5) . . ? C11 C12 C13 119.7(7) . . ? C14 C13 C12 120.2(7) . . ? C13 C14 C15 119.1(7) . . ? C14 C15 C16 121.2(8) . . ? C11 C16 C15 119.9(8) . . ? C26 C21 C22 118.7(5) . . ? C26 C21 P 118.5(4) . . ? C22 C21 P 122.6(5) . . ? C23 C22 C21 119.5(6) . . ? C24 C23 C22 120.4(6) . . ? C25 C24 C23 119.7(6) . . ? C26 C25 C24 121.1(6) . . ? C25 C26 C21 120.5(6) . . ? C32 C31 C36 119.2(6) . . ? C32 C31 P 117.7(5) . . ? C36 C31 P 123.1(5) . . ? C31 C32 C33 120.5(7) . . ? C34 C33 C32 119.7(7) . . ? C33 C34 C35 120.7(7) . . ? C34 C35 C36 120.2(7) . . ? C31 C36 C35 119.6(7) . . ? O3 S O2 114.8(3) . . ? O3 S O1 116.2(3) . . ? O2 S O1 114.4(3) . . ? O3 S C40 101.8(3) . . ? O2 S C40 104.9(3) . . ? O1 S C40 102.2(3) . . ? S O1 Ag 115.9(2) . . ? S O3 Ag 133.1(2) . 2_567 ? F1 C40 F2 108.2(7) . . ? F1 C40 F3 106.4(6) . . ? F2 C40 F3 106.1(6) . . ? F1 C40 S 113.2(5) . . ? F2 C40 S 111.1(5) . . ? F3 C40 S 111.4(5) . . ? _diffrn_measured_fraction_theta_max 0.865 _diffrn_reflns_theta_full 28.74 _diffrn_measured_fraction_theta_full 0.865 _refine_diff_density_max 1.083 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.141 ############################################################## data_amacha(complex18) _database_code_depnum_ccdc_archive 'CCDC 272434' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47.50 H39 Ag Cl F3 Fe O3 P2 S2' _chemical_formula_weight 1040.02 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' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 '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' Ag Ag -0.8971 1.1015 '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 10.7313(8) _cell_length_b 18.2674(14) _cell_length_c 22.6389(16) _cell_angle_alpha 90.00 _cell_angle_beta 97.837(3) _cell_angle_gamma 90.00 _cell_volume 4396.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 6297 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2108 _exptl_absorpt_coefficient_mu 1.059 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7007 _exptl_absorpt_correction_T_max 0.9415 _exptl_absorpt_process_details XPREP loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1.00 0.00 1.00 0.0350 1.00 0.00 -1.00 0.0270 -1.00 -1.00 1.00 0.1070 1.00 1.00 -1.00 0.0990 0.00 0.00 1.00 0.0940 1.00 -1.00 -1.00 0.1000 -1.00 1.00 1.00 0.1100 0.00 -1.00 -8.00 0.1090 _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w- and \f-scan' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 84636 _diffrn_reflns_av_R_equivalents 0.0696 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 28.29 _reflns_number_total 10919 _reflns_number_gt 8274 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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. The dichloromethane is disordered 1:1 over an inversion centre. The triflate is disordered over two sites with relative occupation 0.85:0.15. The minor component was refined isotropically. A system of restraints was used to ensure stability of refinement. ; _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^)+(0.0378P)^2^+1.7580P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10919 _refine_ls_number_parameters 583 _refine_ls_number_restraints 190 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0800 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.015 _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 Ag Ag 0.501659(15) 0.291303(9) 0.249246(7) 0.02126(5) Uani 1 1 d . . . Fe Fe 0.81834(3) 0.179011(17) 0.330544(13) 0.01994(7) Uani 1 1 d . A . P1 P 0.68397(5) 0.34447(3) 0.31291(2) 0.01895(11) Uani 1 1 d . A . P2 P 0.38235(5) 0.34343(3) 0.15949(2) 0.02051(12) Uani 1 1 d . A . S1 S 0.54910(5) 0.14781(3) 0.24525(2) 0.02303(12) Uani 1 1 d . A . C1 C 0.7660(2) 0.27734(12) 0.36180(10) 0.0227(5) Uani 1 1 d U . . C2 C 0.8991(2) 0.26625(13) 0.37784(11) 0.0302(5) Uani 1 1 d U A . H2 H 0.9639 0.2969 0.3671 0.036 Uiso 1 1 calc R . . C3 C 0.9160(3) 0.20161(14) 0.41238(11) 0.0376(6) Uani 1 1 d U . . H3 H 0.9948 0.1814 0.4288 0.045 Uiso 1 1 calc R A . C4 C 0.7972(3) 0.17211(14) 0.41849(10) 0.0368(6) Uani 1 1 d U A . H4 H 0.7824 0.1288 0.4397 0.044 Uiso 1 1 calc R . . C5 C 0.7029(2) 0.21819(12) 0.38737(10) 0.0278(5) Uani 1 1 d U A . H5 H 0.6146 0.2111 0.3841 0.033 Uiso 1 1 calc R . . C6 C 0.7135(2) 0.13618(11) 0.25785(9) 0.0210(4) Uani 1 1 d U . . C7 C 0.8060(2) 0.18493(12) 0.24022(9) 0.0224(4) Uani 1 1 d U A . H7 H 0.7897 0.2276 0.2164 0.027 Uiso 1 1 calc R . . C8 C 0.9264(2) 0.15838(13) 0.26458(10) 0.0262(5) Uani 1 1 d U . . H8 H 1.0048 0.1803 0.2601 0.031 Uiso 1 1 calc R A . C9 C 0.9090(2) 0.09298(13) 0.29695(10) 0.0256(5) Uani 1 1 d U A . H9 H 0.9742 0.0639 0.3177 0.031 Uiso 1 1 calc R . . C10 C 0.7781(2) 0.07854(12) 0.29295(10) 0.0241(5) Uani 1 1 d U A . H10 H 0.7402 0.0383 0.3103 0.029 Uiso 1 1 calc R . . C11 C 0.5082(2) 0.12082(12) 0.16932(10) 0.0253(5) Uani 1 1 d U . . C12 C 0.5950(2) 0.09536(13) 0.13415(11) 0.0315(5) Uani 1 1 d U A . H12 H 0.6811 0.0904 0.1504 0.038 Uiso 1 1 calc R . . C13 C 0.5551(3) 0.07719(15) 0.07484(12) 0.0420(7) Uani 1 1 d U . . H13 H 0.6143 0.0603 0.0504 0.050 Uiso 1 1 calc R A . C14 C 0.4296(3) 0.08361(16) 0.05130(13) 0.0466(7) Uani 1 1 d U A . H14 H 0.4027 0.0709 0.0109 0.056 Uiso 1 1 calc R . . C15 C 0.3433(3) 0.10863(15) 0.08683(12) 0.0414(7) Uani 1 1 d U . . H15 H 0.2573 0.1132 0.0706 0.050 Uiso 1 1 calc R A . C16 C 0.3816(2) 0.12714(13) 0.14600(11) 0.0297(5) Uani 1 1 d U A . H16 H 0.3220 0.1439 0.1704 0.036 Uiso 1 1 calc R . . C21 C 0.65118(19) 0.42007(12) 0.36159(9) 0.0200(4) Uani 1 1 d U . . C22 C 0.6042(2) 0.48467(12) 0.33429(10) 0.0253(5) Uani 1 1 d U A . H22 H 0.5945 0.4887 0.2921 0.030 Uiso 1 1 calc R . . C23 C 0.5715(2) 0.54311(13) 0.36815(11) 0.0287(5) Uani 1 1 d U . . H23 H 0.5397 0.5870 0.3492 0.034 Uiso 1 1 calc R A . C24 C 0.5855(2) 0.53725(13) 0.42979(11) 0.0306(5) Uani 1 1 d U A . H24 H 0.5631 0.5771 0.4532 0.037 Uiso 1 1 calc R . . C25 C 0.6318(2) 0.47355(14) 0.45710(11) 0.0319(5) Uani 1 1 d U . . H25 H 0.6416 0.4699 0.4993 0.038 Uiso 1 1 calc R A . C26 C 0.6642(2) 0.41448(13) 0.42334(10) 0.0261(5) Uani 1 1 d U A . H26 H 0.6952 0.3706 0.4425 0.031 Uiso 1 1 calc R . . C31 C 0.8021(2) 0.38355(12) 0.27168(9) 0.0215(4) Uani 1 1 d U . . C32 C 0.9076(2) 0.42073(13) 0.30047(10) 0.0264(5) Uani 1 1 d U A . H32 H 0.9170 0.4276 0.3424 0.032 Uiso 1 1 calc R . . C33 C 0.9980(2) 0.44749(13) 0.26799(12) 0.0314(5) Uani 1 1 d U . . H33 H 1.0698 0.4721 0.2879 0.038 Uiso 1 1 calc R A . C34 C 0.9844(2) 0.43861(13) 0.20661(11) 0.0312(5) Uani 1 1 d U A . H34 H 1.0471 0.4568 0.1846 0.037 Uiso 1 1 calc R . . C35 C 0.8801(2) 0.40341(13) 0.17750(11) 0.0287(5) Uani 1 1 d U . . H35 H 0.8705 0.3978 0.1354 0.034 Uiso 1 1 calc R A . C36 C 0.7884(2) 0.37608(12) 0.20976(10) 0.0241(5) Uani 1 1 d U A . H36 H 0.7163 0.3522 0.1895 0.029 Uiso 1 1 calc R . . C41 C 0.3288(2) 0.43603(12) 0.17310(10) 0.0228(4) Uani 1 1 d U . . C42 C 0.3385(2) 0.46042(13) 0.23148(10) 0.0257(5) Uani 1 1 d U A . H42 H 0.3728 0.4292 0.2631 0.031 Uiso 1 1 calc R . . C43 C 0.2980(2) 0.53054(13) 0.24412(12) 0.0326(5) Uani 1 1 d U . . H43 H 0.3044 0.5468 0.2843 0.039 Uiso 1 1 calc R A . C44 C 0.2489(2) 0.57630(14) 0.19839(13) 0.0366(6) Uani 1 1 d U A . H44 H 0.2236 0.6245 0.2070 0.044 Uiso 1 1 calc R . . C45 C 0.2363(2) 0.55229(14) 0.14001(13) 0.0367(6) Uani 1 1 d U . . H45 H 0.2009 0.5837 0.1087 0.044 Uiso 1 1 calc R A . C46 C 0.2753(2) 0.48204(13) 0.12699(11) 0.0311(5) Uani 1 1 d U A . H46 H 0.2656 0.4654 0.0869 0.037 Uiso 1 1 calc R . . C51 C 0.2395(2) 0.30099(11) 0.12112(10) 0.0212(4) Uani 1 1 d U . . C52 C 0.2148(2) 0.29222(14) 0.05964(10) 0.0306(5) Uani 1 1 d U A . H52 H 0.2761 0.3062 0.0353 0.037 Uiso 1 1 calc R . . C53 C 0.1005(2) 0.26311(15) 0.03363(11) 0.0351(6) Uani 1 1 d U . . H53 H 0.0843 0.2571 -0.0084 0.042 Uiso 1 1 calc R A . C54 C 0.0104(2) 0.24295(14) 0.06871(11) 0.0320(5) Uani 1 1 d U A . H54 H -0.0681 0.2238 0.0509 0.038 Uiso 1 1 calc R . . C55 C 0.0352(2) 0.25073(14) 0.12973(11) 0.0323(5) Uani 1 1 d U . . H55 H -0.0265 0.2363 0.1538 0.039 Uiso 1 1 calc R A . C56 C 0.1489(2) 0.27932(12) 0.15663(10) 0.0272(5) Uani 1 1 d U A . H56 H 0.1650 0.2841 0.1988 0.033 Uiso 1 1 calc R . . C61 C 0.4885(2) 0.35186(13) 0.10312(9) 0.0236(5) Uani 1 1 d U . . C62 C 0.5320(2) 0.41843(14) 0.08399(11) 0.0333(6) Uani 1 1 d U A . H62 H 0.5005 0.4630 0.0978 0.040 Uiso 1 1 calc R . . C63 C 0.6215(3) 0.42011(16) 0.04475(12) 0.0413(7) Uani 1 1 d U . . H63 H 0.6492 0.4658 0.0313 0.050 Uiso 1 1 calc R A . C64 C 0.6699(2) 0.35598(17) 0.02533(11) 0.0401(6) Uani 1 1 d U A . H64 H 0.7321 0.3574 -0.0008 0.048 Uiso 1 1 calc R . . C65 C 0.6275(2) 0.28960(16) 0.04403(11) 0.0359(6) Uani 1 1 d U . . H65 H 0.6598 0.2453 0.0302 0.043 Uiso 1 1 calc R A . C66 C 0.5380(2) 0.28731(14) 0.08284(11) 0.0302(5) Uani 1 1 d U A . H66 H 0.5101 0.2414 0.0957 0.036 Uiso 1 1 calc R . . C98 C 0.4916(6) 0.0545(4) 0.5135(4) 0.083(3) Uani 0.50 1 d P . . H98A H 0.4275 0.0884 0.4973 0.100 Uiso 0.50 1 d PR . . H98B H 0.5444 0.0781 0.5456 0.100 Uiso 0.50 1 d PR . . Cl Cl 0.58034(10) 0.02766(8) 0.45877(6) 0.1022(4) Uani 1 1 d . . . S2 S 0.28382(14) 0.27382(7) 0.36208(6) 0.0351(3) Uani 0.851(3) 1 d PDU A 1 O1 O 0.4049(2) 0.27250(14) 0.34278(10) 0.0482(7) Uani 0.851(3) 1 d PDU A 1 O2 O 0.1819(3) 0.28048(18) 0.31358(13) 0.0755(11) Uani 0.851(3) 1 d PDU A 1 O3 O 0.2625(4) 0.22245(13) 0.40636(15) 0.0884(14) Uani 0.851(3) 1 d PDU A 1 C99 C 0.2793(3) 0.3605(2) 0.40119(15) 0.0320(12) Uani 0.851(3) 1 d PDU A 1 F1 F 0.3000(3) 0.41657(11) 0.36721(10) 0.0667(8) Uani 0.851(3) 1 d PDU A 1 F2 F 0.1705(2) 0.37103(13) 0.42127(12) 0.0689(8) Uani 0.851(3) 1 d PDU A 1 F3 F 0.3681(2) 0.36326(13) 0.44757(9) 0.0657(7) Uani 0.851(3) 1 d PDU A 1 S2' S 0.3020(8) 0.2596(4) 0.3738(3) 0.030(2) Uiso 0.149(3) 1 d PDU A 2 O1' O 0.3196(12) 0.2788(6) 0.3104(5) 0.036(3) Uiso 0.149(3) 1 d PDU A 2 O2' O 0.1821(12) 0.2293(9) 0.3671(8) 0.060(5) Uiso 0.149(3) 1 d PDU A 2 O3' O 0.4021(13) 0.2317(9) 0.4107(7) 0.067(5) Uiso 0.149(3) 1 d PDU A 2 C99' C 0.2756(16) 0.3513(8) 0.4008(7) 0.042(8) Uiso 0.149(3) 1 d PDU A 2 F1' F 0.1802(11) 0.3876(6) 0.3711(5) 0.052(3) Uiso 0.149(3) 1 d PDU A 2 F2' F 0.2586(13) 0.3532(7) 0.4576(5) 0.053(3) Uiso 0.149(3) 1 d PDU A 2 F3' F 0.3705(15) 0.3964(9) 0.3980(8) 0.088(5) Uiso 0.149(3) 1 d PDU 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 Ag 0.02245(8) 0.02052(8) 0.02024(8) -0.00003(6) 0.00087(6) -0.00123(7) Fe 0.02334(16) 0.01959(16) 0.01667(15) -0.00065(12) 0.00199(12) 0.00222(13) P1 0.0201(3) 0.0180(3) 0.0188(3) -0.0017(2) 0.0027(2) -0.0021(2) P2 0.0220(3) 0.0208(3) 0.0188(3) 0.0011(2) 0.0030(2) -0.0002(2) S1 0.0225(3) 0.0199(3) 0.0262(3) -0.0028(2) 0.0017(2) 0.0011(2) C1 0.0270(11) 0.0221(11) 0.0189(10) -0.0043(8) 0.0028(9) 0.0015(9) C2 0.0312(13) 0.0279(12) 0.0285(12) -0.0081(10) -0.0061(10) 0.0024(10) C3 0.0484(16) 0.0373(15) 0.0228(12) -0.0077(10) -0.0109(11) 0.0135(12) C4 0.0625(18) 0.0309(14) 0.0182(11) 0.0026(9) 0.0101(11) 0.0116(13) C5 0.0403(14) 0.0249(12) 0.0204(11) -0.0005(9) 0.0124(10) 0.0031(10) C6 0.0228(11) 0.0198(11) 0.0198(10) -0.0030(8) 0.0007(8) 0.0027(9) C7 0.0285(11) 0.0226(11) 0.0165(10) -0.0004(8) 0.0040(9) 0.0009(9) C8 0.0246(11) 0.0314(12) 0.0240(11) -0.0022(9) 0.0082(9) 0.0011(9) C9 0.0271(12) 0.0264(12) 0.0226(11) -0.0027(9) 0.0013(9) 0.0088(9) C10 0.0313(12) 0.0174(10) 0.0238(11) -0.0017(8) 0.0038(9) 0.0021(9) C11 0.0301(12) 0.0147(10) 0.0296(12) -0.0023(9) -0.0019(9) -0.0004(9) C12 0.0308(13) 0.0280(12) 0.0332(13) -0.0061(10) -0.0045(10) 0.0095(10) C13 0.0471(16) 0.0415(16) 0.0347(14) -0.0141(12) -0.0041(12) 0.0132(13) C14 0.0531(18) 0.0447(17) 0.0363(15) -0.0162(13) -0.0145(13) 0.0068(14) C15 0.0359(14) 0.0355(15) 0.0471(16) -0.0089(12) -0.0147(12) 0.0023(12) C16 0.0267(12) 0.0209(11) 0.0397(14) -0.0034(10) -0.0019(10) -0.0008(9) C21 0.0185(10) 0.0204(11) 0.0218(10) -0.0033(8) 0.0047(8) -0.0029(8) C22 0.0298(12) 0.0229(11) 0.0230(11) -0.0013(9) 0.0035(9) -0.0016(9) C23 0.0334(13) 0.0191(11) 0.0342(13) 0.0013(9) 0.0066(10) 0.0003(9) C24 0.0333(13) 0.0264(12) 0.0334(13) -0.0107(10) 0.0093(10) 0.0016(10) C25 0.0365(14) 0.0367(14) 0.0225(12) -0.0052(10) 0.0041(10) 0.0037(11) C26 0.0292(12) 0.0263(12) 0.0225(11) 0.0002(9) 0.0020(9) 0.0050(9) C31 0.0228(11) 0.0177(10) 0.0244(11) -0.0010(8) 0.0049(9) 0.0004(8) C32 0.0259(12) 0.0259(12) 0.0280(12) -0.0046(9) 0.0054(9) -0.0028(9) C33 0.0247(12) 0.0252(12) 0.0449(14) -0.0036(10) 0.0070(11) -0.0051(10) C34 0.0291(12) 0.0265(12) 0.0413(14) 0.0042(10) 0.0170(11) 0.0017(10) C35 0.0343(13) 0.0264(12) 0.0276(12) 0.0037(9) 0.0117(10) 0.0050(10) C36 0.0266(11) 0.0205(11) 0.0255(11) -0.0001(9) 0.0042(9) 0.0003(9) C41 0.0195(10) 0.0198(11) 0.0296(12) 0.0019(9) 0.0054(9) -0.0017(9) C42 0.0240(11) 0.0255(12) 0.0286(12) 0.0003(9) 0.0069(9) -0.0011(9) C43 0.0304(13) 0.0266(13) 0.0438(15) -0.0062(11) 0.0160(11) -0.0025(10) C44 0.0311(13) 0.0203(12) 0.0615(18) 0.0006(11) 0.0180(12) 0.0005(10) C45 0.0306(13) 0.0271(13) 0.0522(16) 0.0116(11) 0.0054(12) 0.0026(10) C46 0.0293(13) 0.0289(13) 0.0342(13) 0.0037(10) 0.0007(10) 0.0004(10) C51 0.0220(11) 0.0184(10) 0.0232(11) -0.0001(8) 0.0030(9) -0.0002(8) C52 0.0275(12) 0.0410(14) 0.0235(12) 0.0028(10) 0.0043(9) -0.0050(11) C53 0.0337(13) 0.0464(15) 0.0242(12) -0.0014(11) 0.0005(10) -0.0074(12) C54 0.0259(12) 0.0308(13) 0.0387(14) -0.0070(11) 0.0022(10) -0.0060(10) C55 0.0310(13) 0.0317(14) 0.0372(14) -0.0029(11) 0.0149(11) -0.0066(11) C56 0.0319(13) 0.0282(13) 0.0230(11) -0.0015(9) 0.0088(10) -0.0048(10) C61 0.0197(10) 0.0321(12) 0.0184(10) 0.0004(9) -0.0003(8) -0.0019(9) C62 0.0358(14) 0.0347(14) 0.0304(13) -0.0013(10) 0.0080(11) -0.0065(11) C63 0.0425(16) 0.0480(17) 0.0357(15) 0.0029(12) 0.0132(12) -0.0145(13) C64 0.0299(13) 0.0667(19) 0.0251(13) -0.0036(12) 0.0089(10) -0.0096(13) C65 0.0287(13) 0.0504(16) 0.0293(13) -0.0067(11) 0.0065(10) 0.0041(12) C66 0.0273(12) 0.0353(13) 0.0281(12) -0.0004(10) 0.0043(10) -0.0002(10) C98 0.035(4) 0.080(6) 0.128(7) -0.049(5) -0.013(4) 0.010(4) Cl 0.0533(6) 0.1323(11) 0.1219(10) -0.0469(8) 0.0158(6) -0.0064(6) S2 0.0466(7) 0.0295(6) 0.0344(6) -0.0067(5) 0.0240(5) -0.0078(5) O1 0.0454(15) 0.0626(16) 0.0420(14) 0.0052(11) 0.0251(12) 0.0112(12) O2 0.0458(16) 0.114(3) 0.0657(19) -0.0556(18) 0.0045(14) -0.0188(16) O3 0.180(4) 0.0274(14) 0.080(2) -0.0026(13) 0.097(3) -0.0161(17) C99 0.0328(19) 0.0356(19) 0.0284(18) -0.0078(13) 0.0075(12) -0.0130(14) F1 0.121(2) 0.0312(11) 0.0531(14) 0.0074(9) 0.0285(14) 0.0032(12) F2 0.0549(14) 0.0717(16) 0.0875(19) -0.0393(14) 0.0357(13) -0.0018(12) F3 0.0734(17) 0.0777(16) 0.0393(12) -0.0178(11) -0.0169(11) -0.0093(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag P2 2.4424(6) . ? Ag P1 2.4656(6) . ? Ag O1 2.506(2) . ? Ag O1' 2.554(11) . ? Ag S1 2.6741(6) . ? Fe C6 2.020(2) . ? Fe C7 2.034(2) . ? Fe C5 2.034(2) . ? Fe C1 2.037(2) . ? Fe C4 2.038(2) . ? Fe C3 2.043(2) . ? Fe C10 2.044(2) . ? Fe C2 2.045(2) . ? Fe C8 2.047(2) . ? Fe C9 2.049(2) . ? P1 C1 1.799(2) . ? P1 C31 1.819(2) . ? P1 C21 1.831(2) . ? P2 C41 1.826(2) . ? P2 C51 1.828(2) . ? P2 C61 1.830(2) . ? S1 C6 1.761(2) . ? S1 C11 1.785(2) . ? C1 C5 1.438(3) . ? C1 C2 1.439(3) . ? C2 C3 1.414(4) . ? C3 C4 1.409(4) . ? C4 C5 1.426(3) . ? C6 C7 1.430(3) . ? C6 C10 1.439(3) . ? C7 C8 1.419(3) . ? C8 C9 1.427(3) . ? C9 C10 1.421(3) . ? C11 C12 1.386(3) . ? C11 C16 1.394(3) . ? C12 C13 1.393(3) . ? C13 C14 1.384(4) . ? C14 C15 1.384(4) . ? C15 C16 1.388(3) . ? C21 C26 1.390(3) . ? C21 C22 1.394(3) . ? C22 C23 1.387(3) . ? C23 C24 1.387(3) . ? C24 C25 1.378(3) . ? C25 C26 1.394(3) . ? C31 C36 1.396(3) . ? C31 C32 1.402(3) . ? C32 C33 1.384(3) . ? C33 C34 1.387(4) . ? C34 C35 1.379(4) . ? C35 C36 1.395(3) . ? C41 C42 1.385(3) . ? C41 C46 1.401(3) . ? C42 C43 1.395(3) . ? C43 C44 1.378(4) . ? C44 C45 1.381(4) . ? C45 C46 1.394(4) . ? C51 C52 1.390(3) . ? C51 C56 1.401(3) . ? C52 C53 1.391(3) . ? C53 C54 1.382(3) . ? C54 C55 1.378(3) . ? C55 C56 1.389(3) . ? C61 C62 1.392(3) . ? C61 C66 1.396(3) . ? C62 C63 1.394(3) . ? C63 C64 1.378(4) . ? C64 C65 1.382(4) . ? C65 C66 1.388(3) . ? C98 Cl 1.734(8) . ? C98 Cl 1.838(9) 3_656 ? Cl C98 1.838(9) 3_656 ? S2 O3 1.414(3) . ? S2 O1 1.426(2) . ? S2 O2 1.446(3) . ? S2 C99 1.818(4) . ? C99 F1 1.317(4) . ? C99 F3 1.319(4) . ? C99 F2 1.324(4) . ? S2' O3' 1.367(12) . ? S2' O2' 1.389(12) . ? S2' O1' 1.514(11) . ? S2' C99' 1.819(14) . ? C99' F3' 1.318(14) . ? C99' F2' 1.323(13) . ? C99' F1' 1.324(14) . ? 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 P2 Ag P1 128.09(2) . . ? P2 Ag O1 121.72(6) . . ? P1 Ag O1 86.98(6) . . ? P2 Ag O1' 97.7(3) . . ? P1 Ag O1' 108.8(3) . . ? O1 Ag O1' 25.0(3) . . ? P2 Ag S1 115.760(19) . . ? P1 Ag S1 105.447(18) . . ? O1 Ag S1 89.83(6) . . ? O1' Ag S1 95.4(3) . . ? C6 Fe C7 41.31(9) . . ? C6 Fe C5 109.39(10) . . ? C7 Fe C5 130.95(9) . . ? C6 Fe C1 118.36(9) . . ? C7 Fe C1 108.60(9) . . ? C5 Fe C1 41.37(9) . . ? C6 Fe C4 130.38(11) . . ? C7 Fe C4 169.95(11) . . ? C5 Fe C4 41.00(10) . . ? C1 Fe C4 69.06(9) . . ? C6 Fe C3 167.71(10) . . ? C7 Fe C3 148.90(11) . . ? C5 Fe C3 68.69(11) . . ? C1 Fe C3 68.81(9) . . ? C4 Fe C3 40.38(11) . . ? C6 Fe C10 41.46(8) . . ? C7 Fe C10 69.40(9) . . ? C5 Fe C10 117.83(10) . . ? C1 Fe C10 152.06(9) . . ? C4 Fe C10 107.80(10) . . ? C3 Fe C10 127.75(10) . . ? C6 Fe C2 151.32(9) . . ? C7 Fe C2 116.73(10) . . ? C5 Fe C2 69.24(10) . . ? C1 Fe C2 41.28(9) . . ? C4 Fe C2 68.43(11) . . ? C3 Fe C2 40.48(10) . . ? C10 Fe C2 165.42(9) . . ? C6 Fe C8 69.04(9) . . ? C7 Fe C8 40.71(9) . . ? C5 Fe C8 168.78(9) . . ? C1 Fe C8 128.77(9) . . ? C4 Fe C8 148.32(10) . . ? C3 Fe C8 115.30(11) . . ? C10 Fe C8 68.87(9) . . ? C2 Fe C8 106.49(10) . . ? C6 Fe C9 68.93(9) . . ? C7 Fe C9 68.70(9) . . ? C5 Fe C9 149.99(9) . . ? C1 Fe C9 166.57(9) . . ? C4 Fe C9 115.91(10) . . ? C3 Fe C9 106.31(10) . . ? C10 Fe C9 40.62(9) . . ? C2 Fe C9 127.11(10) . . ? C8 Fe C9 40.78(9) . . ? C1 P1 C31 105.46(10) . . ? C1 P1 C21 105.18(10) . . ? C31 P1 C21 102.55(10) . . ? C1 P1 Ag 111.94(7) . . ? C31 P1 Ag 114.05(7) . . ? C21 P1 Ag 116.53(7) . . ? C41 P2 C51 102.15(10) . . ? C41 P2 C61 106.25(10) . . ? C51 P2 C61 105.42(10) . . ? C41 P2 Ag 111.23(7) . . ? C51 P2 Ag 122.71(7) . . ? C61 P2 Ag 107.90(7) . . ? C6 S1 C11 103.43(11) . . ? C6 S1 Ag 107.69(7) . . ? C11 S1 Ag 106.29(7) . . ? C5 C1 C2 107.3(2) . . ? C5 C1 P1 122.84(18) . . ? C2 C1 P1 129.53(18) . . ? C5 C1 Fe 69.18(12) . . ? C2 C1 Fe 69.66(13) . . ? P1 C1 Fe 121.48(11) . . ? C3 C2 C1 107.8(2) . . ? C3 C2 Fe 69.66(14) . . ? C1 C2 Fe 69.06(13) . . ? C4 C3 C2 108.9(2) . . ? C4 C3 Fe 69.64(14) . . ? C2 C3 Fe 69.87(13) . . ? C3 C4 C5 108.5(2) . . ? C3 C4 Fe 69.98(14) . . ? C5 C4 Fe 69.33(13) . . ? C4 C5 C1 107.5(2) . . ? C4 C5 Fe 69.67(13) . . ? C1 C5 Fe 69.45(12) . . ? C7 C6 C10 108.04(19) . . ? C7 C6 S1 126.69(16) . . ? C10 C6 S1 125.05(17) . . ? C7 C6 Fe 69.86(12) . . ? C10 C6 Fe 70.17(12) . . ? S1 C6 Fe 121.31(11) . . ? C8 C7 C6 107.95(19) . . ? C8 C7 Fe 70.13(12) . . ? C6 C7 Fe 68.83(12) . . ? C7 C8 C9 108.1(2) . . ? C7 C8 Fe 69.17(12) . . ? C9 C8 Fe 69.69(13) . . ? C10 C9 C8 108.7(2) . . ? C10 C9 Fe 69.52(12) . . ? C8 C9 Fe 69.53(13) . . ? C9 C10 C6 107.3(2) . . ? C9 C10 Fe 69.86(13) . . ? C6 C10 Fe 68.38(12) . . ? C12 C11 C16 120.5(2) . . ? C12 C11 S1 123.34(18) . . ? C16 C11 S1 116.17(18) . . ? C11 C12 C13 119.4(2) . . ? C14 C13 C12 120.4(3) . . ? C15 C14 C13 119.8(2) . . ? C14 C15 C16 120.5(2) . . ? C15 C16 C11 119.3(2) . . ? C26 C21 C22 119.3(2) . . ? C26 C21 P1 123.29(17) . . ? C22 C21 P1 117.34(16) . . ? C23 C22 C21 120.7(2) . . ? C24 C23 C22 119.7(2) . . ? C25 C24 C23 120.0(2) . . ? C24 C25 C26 120.6(2) . . ? C21 C26 C25 119.8(2) . . ? C36 C31 C32 118.8(2) . . ? C36 C31 P1 119.46(17) . . ? C32 C31 P1 121.76(17) . . ? C33 C32 C31 120.3(2) . . ? C32 C33 C34 120.3(2) . . ? C35 C34 C33 120.1(2) . . ? C34 C35 C36 120.1(2) . . ? C35 C36 C31 120.4(2) . . ? C42 C41 C46 119.2(2) . . ? C42 C41 P2 118.34(17) . . ? C46 C41 P2 122.44(18) . . ? C41 C42 C43 120.4(2) . . ? C44 C43 C42 120.1(2) . . ? C43 C44 C45 120.2(2) . . ? C44 C45 C46 120.1(2) . . ? C45 C46 C41 119.9(2) . . ? C52 C51 C56 119.3(2) . . ? C52 C51 P2 123.93(17) . . ? C56 C51 P2 116.74(17) . . ? C51 C52 C53 120.3(2) . . ? C54 C53 C52 120.2(2) . . ? C55 C54 C53 119.6(2) . . ? C54 C55 C56 121.0(2) . . ? C55 C56 C51 119.5(2) . . ? C62 C61 C66 118.5(2) . . ? C62 C61 P2 123.87(18) . . ? C66 C61 P2 117.33(18) . . ? C61 C62 C63 120.4(2) . . ? C64 C63 C62 120.5(3) . . ? C63 C64 C65 119.6(2) . . ? C64 C65 C66 120.4(3) . . ? C65 C66 C61 120.6(2) . . ? Cl C98 Cl 108.1(4) . 3_656 ? C98 Cl C98 71.9(4) . 3_656 ? O3 S2 O1 116.6(2) . . ? O3 S2 O2 114.5(2) . . ? O1 S2 O2 113.29(18) . . ? O3 S2 C99 102.43(17) . . ? O1 S2 C99 104.46(17) . . ? O2 S2 C99 103.24(19) . . ? S2 O1 Ag 139.15(17) . . ? F1 C99 F3 105.9(3) . . ? F1 C99 F2 108.3(3) . . ? F3 C99 F2 107.2(3) . . ? F1 C99 S2 112.0(2) . . ? F3 C99 S2 110.9(3) . . ? F2 C99 S2 112.1(3) . . ? O3' S2' O2' 123.9(12) . . ? O3' S2' O1' 118.4(10) . . ? O2' S2' O1' 102.8(10) . . ? O3' S2' C99' 106.4(9) . . ? O2' S2' C99' 102.7(10) . . ? O1' S2' C99' 98.7(8) . . ? S2' O1' Ag 137.6(8) . . ? F3' C99' F2' 104.0(14) . . ? F3' C99' F1' 102.2(14) . . ? F2' C99' F1' 106.4(13) . . ? F3' C99' S2' 113.7(13) . . ? F2' C99' S2' 113.5(11) . . ? F1' C99' S2' 115.8(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.658 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.078 ############################################# data_lol6as(complex19) _database_code_depnum_ccdc_archive 'CCDC 272435' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H38 Ag F3 Fe O3 P2 S Se' _chemical_formula_weight 1044.45 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' F F 0.0171 0.0103 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 12.9511(14) _cell_length_b 16.8249(19) _cell_length_c 20.548(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.689(3) _cell_angle_gamma 90.00 _cell_volume 4288.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2504 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 19.5 _exptl_crystal_description prism _exptl_crystal_colour yelow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.821 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.822258 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; SADABS; Area-Detector Absorption Correction. Bruker-AXS within SAINT+ package, v. 6.02 (1999). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28043 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.1101 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.36 _reflns_number_total 10106 _reflns_number_gt 6060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ 6.02 (Bruker AXS, 1999)' _computing_data_reduction 'SAINT+ 6.02 (Bruker AXS, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.10 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.10 (Bruker, 2000)' _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^)+(0.0499P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10106 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1287 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.21556(3) 0.78920(2) 0.38978(2) 0.03619(12) Uani 1 1 d . . . Fe1 Fe 0.20073(5) 1.02553(4) 0.45107(3) 0.02988(18) Uani 1 1 d . . . Se1 Se 0.22233(4) 0.84107(3) 0.52332(3) 0.03404(14) Uani 1 1 d . . . P1 P 0.17971(10) 0.90513(8) 0.31695(6) 0.0289(3) Uani 1 1 d . . . P2 P 0.30883(10) 0.66333(7) 0.40971(7) 0.0291(3) Uani 1 1 d . . . C1 C 0.1296(4) 0.9873(3) 0.3545(2) 0.0309(12) Uani 1 1 d . . . C2 C 0.1567(4) 1.0698(3) 0.3549(3) 0.0382(13) Uani 1 1 d . . . H2 H 0.2024 1.0927 0.3326 0.046 Uiso 1 1 calc R . . C3 C 0.1015(5) 1.1106(3) 0.3954(3) 0.0471(15) Uani 1 1 d . . . H3 H 0.1054 1.1648 0.4043 0.056 Uiso 1 1 calc R . . C4 C 0.0403(4) 1.0559(3) 0.4197(3) 0.0398(13) Uani 1 1 d . . . H4 H -0.0042 1.0676 0.4467 0.048 Uiso 1 1 calc R . . C5 C 0.0580(4) 0.9791(3) 0.3956(2) 0.0355(12) Uani 1 1 d . . . H5 H 0.0281 0.9318 0.4051 0.043 Uiso 1 1 calc R . . C6 C 0.3476(4) 0.9731(3) 0.4884(3) 0.0348(12) Uani 1 1 d . . . H6 H 0.3828 0.9415 0.4643 0.042 Uiso 1 1 calc R . . C7 C 0.3578(4) 1.0569(3) 0.4967(3) 0.0419(14) Uani 1 1 d . . . H7 H 0.4002 1.0901 0.4788 0.050 Uiso 1 1 calc R . . C8 C 0.2910(4) 1.0805(3) 0.5375(3) 0.0434(14) Uani 1 1 d . . . H8 H 0.2827 1.1321 0.5512 0.052 Uiso 1 1 calc R . . C9 C 0.2395(4) 1.0127(3) 0.5535(2) 0.0362(13) Uani 1 1 d . . . H9 H 0.1911 1.0116 0.5792 0.043 Uiso 1 1 calc R . . C10 C 0.2749(4) 0.9461(3) 0.5231(2) 0.0299(11) Uani 1 1 d . . . C11 C 0.3372(4) 0.7951(3) 0.5943(2) 0.0352(12) Uani 1 1 d . . . C12 C 0.3179(5) 0.7220(3) 0.6194(3) 0.0427(14) Uani 1 1 d . . . H12 H 0.2512 0.6974 0.6024 0.051 Uiso 1 1 calc R . . C13 C 0.3976(6) 0.6859(3) 0.6697(3) 0.0566(18) Uani 1 1 d . . . H13 H 0.3848 0.6364 0.6859 0.068 Uiso 1 1 calc R . . C14 C 0.4948(6) 0.7214(4) 0.6962(3) 0.0618(19) Uani 1 1 d . . . H14 H 0.5475 0.6971 0.7310 0.074 Uiso 1 1 calc R . . C15 C 0.5147(5) 0.7942(4) 0.6709(3) 0.0588(18) Uani 1 1 d . . . H15 H 0.5819 0.8180 0.6879 0.071 Uiso 1 1 calc R . . C16 C 0.4355(4) 0.8319(3) 0.6207(3) 0.0479(15) Uani 1 1 d . . . H16 H 0.4484 0.8816 0.6049 0.058 Uiso 1 1 calc R . . C21 C 0.0845(4) 0.8925(3) 0.2334(2) 0.0299(11) Uani 1 1 d . . . C22 C 0.0008(4) 0.9437(4) 0.2062(3) 0.0457(15) Uani 1 1 d . . . H22 H -0.0104 0.9871 0.2314 0.055 Uiso 1 1 calc R . . C23 C -0.0677(5) 0.9307(4) 0.1410(3) 0.0584(18) Uani 1 1 d . . . H23 H -0.1242 0.9657 0.1227 0.070 Uiso 1 1 calc R . . C24 C -0.0519(5) 0.8671(4) 0.1041(3) 0.0591(18) Uani 1 1 d . . . H24 H -0.0982 0.8583 0.0608 0.071 Uiso 1 1 calc R . . C25 C 0.0315(5) 0.8163(4) 0.1301(3) 0.0520(16) Uani 1 1 d . . . H25 H 0.0428 0.7734 0.1044 0.062 Uiso 1 1 calc R . . C26 C 0.0990(5) 0.8283(3) 0.1944(3) 0.0434(14) Uani 1 1 d . . . H26 H 0.1552 0.7929 0.2120 0.052 Uiso 1 1 calc R . . C31 C 0.2975(4) 0.9443(3) 0.2969(2) 0.0325(12) Uani 1 1 d . . . C32 C 0.2876(4) 1.0032(3) 0.2479(2) 0.0380(13) Uani 1 1 d . . . H32 H 0.2196 1.0216 0.2239 0.046 Uiso 1 1 calc R . . C33 C 0.3776(5) 1.0342(4) 0.2347(3) 0.0524(16) Uani 1 1 d . . . H33 H 0.3701 1.0741 0.2023 0.063 Uiso 1 1 calc R . . C34 C 0.4777(5) 1.0073(4) 0.2685(3) 0.0565(18) Uani 1 1 d . . . H34 H 0.5381 1.0295 0.2597 0.068 Uiso 1 1 calc R . . C35 C 0.4897(4) 0.9475(4) 0.3154(3) 0.0531(17) Uani 1 1 d . . . H35 H 0.5580 0.9282 0.3375 0.064 Uiso 1 1 calc R . . C36 C 0.3998(4) 0.9160(3) 0.3297(3) 0.0422(14) Uani 1 1 d . . . H36 H 0.4082 0.8755 0.3615 0.051 Uiso 1 1 calc R . . C41 C 0.4535(4) 0.6784(3) 0.4375(3) 0.0347(12) Uani 1 1 d . . . C42 C 0.5090(5) 0.6888(4) 0.5060(3) 0.0509(16) Uani 1 1 d . . . H42 H 0.4731 0.6844 0.5390 0.061 Uiso 1 1 calc R . . C43 C 0.6189(5) 0.7057(4) 0.5242(4) 0.0611(18) Uani 1 1 d . . . H43 H 0.6567 0.7115 0.5699 0.073 Uiso 1 1 calc R . . C44 C 0.6714(5) 0.7138(3) 0.4764(4) 0.0594(19) Uani 1 1 d . . . H44 H 0.7452 0.7233 0.4895 0.071 Uiso 1 1 calc R . . C45 C 0.6167(5) 0.7079(3) 0.4092(4) 0.0540(16) Uani 1 1 d . . . H45 H 0.6525 0.7167 0.3766 0.065 Uiso 1 1 calc R . . C46 C 0.5083(4) 0.6890(3) 0.3892(3) 0.0407(14) Uani 1 1 d . . . H46 H 0.4721 0.6833 0.3433 0.049 Uiso 1 1 calc R . . C51 C 0.2732(4) 0.6026(3) 0.4726(3) 0.0358(12) Uani 1 1 d . . . C52 C 0.1697(5) 0.6087(3) 0.4760(3) 0.0475(15) Uani 1 1 d . . . H52 H 0.1240 0.6472 0.4505 0.057 Uiso 1 1 calc R . . C53 C 0.1326(7) 0.5576(5) 0.5175(4) 0.077(2) Uani 1 1 d . . . H53 H 0.0619 0.5613 0.5195 0.092 Uiso 1 1 calc R . . C54 C 0.2012(10) 0.5017(5) 0.5556(4) 0.099(4) Uani 1 1 d . . . H54 H 0.1766 0.4670 0.5832 0.119 Uiso 1 1 calc R . . C55 C 0.3053(9) 0.4970(4) 0.5532(4) 0.087(3) Uani 1 1 d . . . H55 H 0.3515 0.4598 0.5802 0.104 Uiso 1 1 calc R . . C56 C 0.3429(6) 0.5458(3) 0.5118(3) 0.0551(17) Uani 1 1 d . . . H56 H 0.4135 0.5413 0.5097 0.066 Uiso 1 1 calc R . . C61 C 0.2882(4) 0.5946(3) 0.3390(3) 0.0336(12) Uani 1 1 d . . . C62 C 0.3284(5) 0.5178(3) 0.3470(3) 0.0512(16) Uani 1 1 d . . . H62 H 0.3749 0.5021 0.3886 0.061 Uiso 1 1 calc R . . C63 C 0.2999(6) 0.4644(4) 0.2939(3) 0.0611(18) Uani 1 1 d . . . H63 H 0.3251 0.4124 0.3003 0.073 Uiso 1 1 calc R . . C64 C 0.2359(5) 0.4872(4) 0.2326(3) 0.0593(18) Uani 1 1 d . . . H64 H 0.2183 0.4513 0.1966 0.071 Uiso 1 1 calc R . . C65 C 0.1974(6) 0.5623(5) 0.2238(4) 0.083(2) Uani 1 1 d . . . H65 H 0.1530 0.5777 0.1816 0.100 Uiso 1 1 calc R . . C66 C 0.2225(5) 0.6163(4) 0.2761(3) 0.0633(19) Uani 1 1 d . . . H66 H 0.1951 0.6676 0.2690 0.076 Uiso 1 1 calc R . . C71 C -0.1241(6) 0.7214(5) 0.2967(5) 0.084(2) Uani 1 1 d . . . F1 F -0.0597(5) 0.6613(4) 0.2927(3) 0.170(3) Uani 1 1 d . . . F2 F -0.2204(4) 0.6957(3) 0.2778(3) 0.131(2) Uani 1 1 d . . . F3 F -0.1169(5) 0.7790(5) 0.2553(3) 0.149(3) Uani 1 1 d . . . S1 S -0.08674(11) 0.75695(9) 0.38441(8) 0.0444(4) Uani 1 1 d . . . O1 O 0.0220(3) 0.7783(3) 0.3942(2) 0.0791(15) Uani 1 1 d . . . O2 O -0.1600(4) 0.8207(3) 0.3798(3) 0.0923(17) Uani 1 1 d . . . O3 O -0.1050(4) 0.6916(3) 0.4216(3) 0.0955(18) Uani 1 1 d . . . 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 Ag1 0.0379(2) 0.0294(2) 0.0406(3) 0.00754(18) 0.01015(19) 0.00686(17) Fe1 0.0285(4) 0.0314(4) 0.0278(4) 0.0017(3) 0.0050(3) 0.0047(3) Se1 0.0351(3) 0.0375(3) 0.0264(3) 0.0018(2) 0.0038(2) -0.0008(2) P1 0.0295(7) 0.0285(7) 0.0284(7) 0.0049(6) 0.0076(6) 0.0043(5) P2 0.0295(7) 0.0261(7) 0.0316(7) 0.0014(6) 0.0085(6) 0.0023(5) C1 0.032(3) 0.034(3) 0.024(3) 0.005(2) 0.005(2) 0.008(2) C2 0.048(3) 0.036(3) 0.030(3) 0.010(2) 0.010(3) 0.006(2) C3 0.060(4) 0.038(3) 0.035(3) 0.003(3) 0.000(3) 0.020(3) C4 0.033(3) 0.051(4) 0.037(3) -0.007(3) 0.012(3) 0.010(3) C5 0.025(3) 0.047(3) 0.031(3) -0.003(2) 0.002(2) 0.005(2) C6 0.025(3) 0.045(3) 0.033(3) 0.005(2) 0.006(2) 0.006(2) C7 0.029(3) 0.046(4) 0.046(4) 0.008(3) 0.002(3) -0.007(2) C8 0.039(3) 0.046(4) 0.039(3) -0.009(3) 0.001(3) 0.001(3) C9 0.033(3) 0.047(4) 0.024(3) 0.000(2) 0.002(2) 0.003(2) C10 0.025(3) 0.034(3) 0.027(3) 0.006(2) 0.002(2) 0.007(2) C11 0.044(3) 0.035(3) 0.023(3) -0.003(2) 0.002(2) 0.002(2) C12 0.059(4) 0.043(4) 0.025(3) -0.001(2) 0.011(3) -0.002(3) C13 0.095(5) 0.035(3) 0.035(4) 0.009(3) 0.010(4) 0.001(3) C14 0.080(5) 0.048(4) 0.041(4) 0.002(3) -0.010(3) 0.025(3) C15 0.052(4) 0.053(4) 0.052(4) -0.005(3) -0.017(3) 0.002(3) C16 0.049(4) 0.033(3) 0.051(4) 0.003(3) -0.003(3) -0.006(3) C21 0.031(3) 0.032(3) 0.026(3) 0.004(2) 0.008(2) -0.006(2) C22 0.034(3) 0.065(4) 0.037(3) 0.002(3) 0.008(3) 0.012(3) C23 0.037(4) 0.089(5) 0.042(4) 0.011(4) 0.001(3) 0.009(3) C24 0.045(4) 0.083(5) 0.041(4) -0.001(4) -0.002(3) -0.020(4) C25 0.061(4) 0.052(4) 0.040(4) -0.011(3) 0.010(3) -0.020(3) C26 0.050(4) 0.032(3) 0.045(4) 0.002(3) 0.007(3) -0.003(3) C31 0.032(3) 0.042(3) 0.022(3) -0.005(2) 0.004(2) -0.001(2) C32 0.037(3) 0.050(4) 0.028(3) 0.001(2) 0.011(2) -0.006(2) C33 0.062(4) 0.049(4) 0.051(4) -0.007(3) 0.024(3) -0.024(3) C34 0.049(4) 0.073(5) 0.056(4) -0.034(4) 0.028(3) -0.030(3) C35 0.028(3) 0.092(5) 0.038(4) -0.026(3) 0.007(3) 0.001(3) C36 0.037(3) 0.063(4) 0.026(3) -0.006(3) 0.008(3) 0.002(3) C41 0.034(3) 0.024(3) 0.046(3) -0.006(2) 0.012(3) 0.004(2) C42 0.045(4) 0.063(4) 0.043(4) -0.014(3) 0.011(3) -0.002(3) C43 0.044(4) 0.067(5) 0.060(5) -0.017(3) -0.005(3) -0.003(3) C44 0.033(3) 0.043(4) 0.099(6) -0.010(4) 0.014(4) 0.002(3) C45 0.046(4) 0.045(4) 0.078(5) -0.005(3) 0.029(4) -0.007(3) C46 0.034(3) 0.038(3) 0.054(4) -0.003(3) 0.018(3) -0.004(2) C51 0.044(3) 0.028(3) 0.036(3) -0.004(2) 0.012(3) -0.002(2) C52 0.059(4) 0.046(4) 0.041(4) -0.013(3) 0.018(3) -0.023(3) C53 0.110(6) 0.079(6) 0.057(5) -0.030(4) 0.051(5) -0.059(5) C54 0.199(11) 0.066(6) 0.046(5) -0.008(4) 0.057(7) -0.067(7) C55 0.177(10) 0.041(4) 0.041(4) 0.005(3) 0.030(6) -0.006(5) C56 0.088(5) 0.034(3) 0.041(4) 0.004(3) 0.016(3) 0.009(3) C61 0.031(3) 0.039(3) 0.034(3) 0.002(2) 0.013(2) -0.006(2) C62 0.071(4) 0.040(4) 0.049(4) 0.000(3) 0.028(3) 0.016(3) C63 0.096(5) 0.040(4) 0.063(5) -0.008(3) 0.048(4) 0.001(3) C64 0.068(5) 0.070(5) 0.043(4) -0.021(3) 0.021(4) -0.024(4) C65 0.092(6) 0.069(6) 0.056(5) -0.014(4) -0.029(4) -0.004(4) C66 0.080(5) 0.055(4) 0.040(4) 0.000(3) -0.007(3) 0.016(3) C71 0.057(5) 0.090(7) 0.103(7) -0.024(5) 0.018(5) -0.019(5) F1 0.126(5) 0.185(7) 0.188(6) -0.126(5) 0.027(4) 0.020(4) F2 0.077(3) 0.172(5) 0.121(4) -0.045(4) -0.010(3) -0.054(3) F3 0.143(5) 0.234(8) 0.070(4) 0.018(4) 0.033(3) -0.054(5) S1 0.0322(8) 0.0496(9) 0.0542(10) -0.0019(7) 0.0167(7) -0.0039(6) O1 0.039(3) 0.117(4) 0.080(3) -0.027(3) 0.016(2) -0.025(3) O2 0.095(4) 0.069(4) 0.131(5) -0.008(3) 0.062(4) 0.029(3) O3 0.069(3) 0.110(4) 0.108(4) 0.062(3) 0.027(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 Ag1 P2 2.4141(13) . y Ag1 P1 2.4208(13) . y Ag1 O1 2.541(4) . y Ag1 Se1 2.8566(7) . y Fe1 C10 2.020(5) . ? Fe1 C5 2.029(5) . ? Fe1 C9 2.029(5) . ? Fe1 C2 2.034(5) . ? Fe1 C1 2.037(5) . ? Fe1 C6 2.037(5) . ? Fe1 C3 2.040(5) . ? Fe1 C8 2.044(5) . ? Fe1 C7 2.049(5) . ? Fe1 C4 2.056(5) . ? Se1 C10 1.895(5) . y Se1 C11 1.922(5) . y P1 C1 1.794(5) . ? P1 C31 1.814(5) . ? P1 C21 1.816(5) . ? P2 C51 1.809(5) . ? P2 C41 1.813(5) . ? P2 C61 1.817(5) . ? C1 C5 1.430(7) . ? C1 C2 1.430(7) . ? C2 C3 1.419(7) . ? C3 C4 1.396(8) . ? C4 C5 1.425(7) . ? C6 C10 1.409(7) . ? C6 C7 1.422(7) . ? C7 C8 1.422(7) . ? C8 C9 1.407(7) . ? C9 C10 1.421(7) . ? C11 C16 1.379(7) . ? C11 C12 1.384(7) . ? C12 C13 1.375(7) . ? C13 C14 1.358(9) . ? C14 C15 1.383(9) . ? C15 C16 1.382(7) . ? C21 C22 1.372(7) . ? C21 C26 1.389(7) . ? C22 C23 1.396(8) . ? C23 C24 1.362(9) . ? C24 C25 1.361(8) . ? C25 C26 1.372(7) . ? C31 C36 1.386(7) . ? C31 C32 1.393(7) . ? C32 C33 1.373(7) . ? C33 C34 1.359(8) . ? C34 C35 1.370(8) . ? C35 C36 1.385(7) . ? C41 C46 1.387(7) . ? C41 C42 1.395(7) . ? C42 C43 1.393(8) . ? C43 C44 1.351(9) . ? C44 C45 1.363(9) . ? C45 C46 1.381(7) . ? C51 C52 1.366(7) . ? C51 C56 1.399(7) . ? C52 C53 1.390(8) . ? C53 C54 1.373(11) . ? C54 C55 1.366(12) . ? C55 C56 1.370(9) . ? C61 C66 1.377(7) . ? C61 C62 1.385(7) . ? C62 C63 1.380(8) . ? C63 C64 1.349(8) . ? C64 C65 1.352(9) . ? C65 C66 1.372(9) . ? C71 F2 1.271(8) . ? C71 F3 1.309(10) . ? C71 F1 1.328(9) . ? C71 S1 1.828(9) . ? S1 O3 1.397(5) . ? S1 O1 1.410(4) . ? S1 O2 1.417(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Ag1 P1 144.05(5) . . y P2 Ag1 O1 112.44(12) . . y P1 Ag1 O1 93.66(12) . . y P2 Ag1 Se1 103.25(4) . . y P1 Ag1 Se1 107.17(4) . . y O1 Ag1 Se1 75.30(10) . . y C10 Fe1 C5 108.8(2) . . ? C10 Fe1 C9 41.10(19) . . ? C5 Fe1 C9 117.1(2) . . ? C10 Fe1 C2 153.6(2) . . ? C5 Fe1 C2 68.9(2) . . ? C9 Fe1 C2 164.3(2) . . ? C10 Fe1 C1 119.5(2) . . ? C5 Fe1 C1 41.18(19) . . ? C9 Fe1 C1 152.2(2) . . ? C2 Fe1 C1 41.15(19) . . ? C10 Fe1 C6 40.64(19) . . ? C5 Fe1 C6 130.3(2) . . ? C9 Fe1 C6 68.8(2) . . ? C2 Fe1 C6 119.7(2) . . ? C1 Fe1 C6 110.0(2) . . ? C10 Fe1 C3 164.8(2) . . ? C5 Fe1 C3 68.2(2) . . ? C9 Fe1 C3 125.8(2) . . ? C2 Fe1 C3 40.8(2) . . ? C1 Fe1 C3 68.8(2) . . ? C6 Fe1 C3 152.2(2) . . ? C10 Fe1 C8 68.3(2) . . ? C5 Fe1 C8 149.7(2) . . ? C9 Fe1 C8 40.4(2) . . ? C2 Fe1 C8 127.5(2) . . ? C1 Fe1 C8 167.0(2) . . ? C6 Fe1 C8 68.3(2) . . ? C3 Fe1 C8 106.3(2) . . ? C10 Fe1 C7 68.5(2) . . ? C5 Fe1 C7 168.7(2) . . ? C9 Fe1 C7 68.6(2) . . ? C2 Fe1 C7 108.3(2) . . ? C1 Fe1 C7 129.7(2) . . ? C6 Fe1 C7 40.7(2) . . ? C3 Fe1 C7 117.3(2) . . ? C8 Fe1 C7 40.7(2) . . ? C10 Fe1 C4 128.3(2) . . ? C5 Fe1 C4 40.8(2) . . ? C9 Fe1 C4 106.2(2) . . ? C2 Fe1 C4 68.1(2) . . ? C1 Fe1 C4 68.8(2) . . ? C6 Fe1 C4 167.6(2) . . ? C3 Fe1 C4 39.9(2) . . ? C8 Fe1 C4 115.8(2) . . ? C7 Fe1 C4 149.4(2) . . ? C10 Se1 C11 100.2(2) . . y C10 Se1 Ag1 101.19(15) . . y C11 Se1 Ag1 114.17(15) . . y C1 P1 C31 104.4(2) . . ? C1 P1 C21 105.4(2) . . ? C31 P1 C21 102.4(2) . . ? C1 P1 Ag1 112.60(16) . . ? C31 P1 Ag1 114.08(17) . . ? C21 P1 Ag1 116.60(16) . . ? C51 P2 C41 107.9(3) . . ? C51 P2 C61 101.7(2) . . ? C41 P2 C61 104.0(2) . . ? C51 P2 Ag1 113.53(17) . . ? C41 P2 Ag1 110.61(16) . . ? C61 P2 Ag1 118.14(17) . . ? C5 C1 C2 106.8(4) . . ? C5 C1 P1 123.8(4) . . ? C2 C1 P1 129.2(4) . . ? C5 C1 Fe1 69.1(3) . . ? C2 C1 Fe1 69.3(3) . . ? P1 C1 Fe1 123.0(2) . . ? C3 C2 C1 108.0(5) . . ? C3 C2 Fe1 69.9(3) . . ? C1 C2 Fe1 69.5(3) . . ? C4 C3 C2 108.9(5) . . ? C4 C3 Fe1 70.7(3) . . ? C2 C3 Fe1 69.4(3) . . ? C3 C4 C5 108.0(5) . . ? C3 C4 Fe1 69.5(3) . . ? C5 C4 Fe1 68.6(3) . . ? C4 C5 C1 108.3(5) . . ? C4 C5 Fe1 70.6(3) . . ? C1 C5 Fe1 69.7(3) . . ? C10 C6 C7 108.1(5) . . ? C10 C6 Fe1 69.0(3) . . ? C7 C6 Fe1 70.1(3) . . ? C8 C7 C6 107.2(5) . . ? C8 C7 Fe1 69.5(3) . . ? C6 C7 Fe1 69.2(3) . . ? C9 C8 C7 108.7(5) . . ? C9 C8 Fe1 69.2(3) . . ? C7 C8 Fe1 69.9(3) . . ? C8 C9 C10 107.5(5) . . ? C8 C9 Fe1 70.4(3) . . ? C10 C9 Fe1 69.1(3) . . ? C6 C10 C9 108.4(5) . . ? C6 C10 Se1 126.5(4) . . ? C9 C10 Se1 124.9(4) . . ? C6 C10 Fe1 70.3(3) . . ? C9 C10 Fe1 69.8(3) . . ? Se1 C10 Fe1 121.5(2) . . ? C16 C11 C12 119.8(5) . . ? C16 C11 Se1 123.0(4) . . ? C12 C11 Se1 117.2(4) . . ? C13 C12 C11 119.7(6) . . ? C14 C13 C12 121.1(6) . . ? C13 C14 C15 119.3(6) . . ? C16 C15 C14 120.6(6) . . ? C11 C16 C15 119.4(5) . . ? C22 C21 C26 118.4(5) . . ? C22 C21 P1 123.6(4) . . ? C26 C21 P1 118.0(4) . . ? C21 C22 C23 120.2(6) . . ? C24 C23 C22 120.1(6) . . ? C25 C24 C23 120.3(6) . . ? C24 C25 C26 120.1(6) . . ? C25 C26 C21 121.0(6) . . ? C36 C31 C32 118.1(5) . . ? C36 C31 P1 121.0(4) . . ? C32 C31 P1 120.9(4) . . ? C33 C32 C31 120.4(5) . . ? C34 C33 C32 120.7(6) . . ? C33 C34 C35 120.2(6) . . ? C34 C35 C36 119.8(6) . . ? C35 C36 C31 120.7(6) . . ? C46 C41 C42 119.0(5) . . ? C46 C41 P2 119.2(4) . . ? C42 C41 P2 121.4(4) . . ? C43 C42 C41 119.2(6) . . ? C44 C43 C42 120.8(6) . . ? C43 C44 C45 120.4(6) . . ? C44 C45 C46 120.4(6) . . ? C45 C46 C41 120.1(6) . . ? C52 C51 C56 120.2(5) . . ? C52 C51 P2 116.7(4) . . ? C56 C51 P2 122.8(4) . . ? C51 C52 C53 120.1(7) . . ? C54 C53 C52 119.5(8) . . ? C55 C54 C53 120.2(7) . . ? C54 C55 C56 121.3(8) . . ? C55 C56 C51 118.8(7) . . ? C66 C61 C62 118.0(5) . . ? C66 C61 P2 119.4(4) . . ? C62 C61 P2 122.3(4) . . ? C63 C62 C61 120.4(6) . . ? C64 C63 C62 120.5(6) . . ? C63 C64 C65 119.6(6) . . ? C64 C65 C66 121.2(6) . . ? C65 C66 C61 120.2(6) . . ? F2 C71 F3 107.4(8) . . ? F2 C71 F1 107.6(7) . . ? F3 C71 F1 111.2(9) . . ? F2 C71 S1 111.7(6) . . ? F3 C71 S1 110.4(6) . . ? F1 C71 S1 108.5(6) . . ? O3 S1 O1 116.2(3) . . ? O3 S1 O2 114.6(3) . . ? O1 S1 O2 116.0(3) . . ? O3 S1 C71 104.1(4) . . ? O1 S1 C71 101.2(3) . . ? O2 S1 C71 101.5(4) . . ? S1 O1 Ag1 165.4(3) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.730 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.112 ############################################END