Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Laguna, Antonio' 'Canales, Silvia' 'Concepcion Gimeno, M.' 'Crespo, Olga' 'Fortea, Angela' 'Jones, P.' _publ_contact_author_name 'Prof Antonio Laguna' _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 'ALAGUNA@POSTA.UNIZAR.ES' _publ_section_title ; Gold and Silver Complexes with the Ligands Fc(SePh)2 (Fc = ( 5-C5H4)2Fe) ; data_Luzson #(complex 5 in the MS) _database_code_CSD 176348 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H18 Au2 F30 Fe S2' _chemical_formula_weight 1798.63 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' '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 'P 21/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 10.6032(12) _cell_length_b 9.6844(10) _cell_length_c 27.385(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.836(3) _cell_angle_gamma 90.00 _cell_volume 2802.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 6242 _cell_measurement_theta_min 2 _cell_measurement_theta_max 56 _exptl_crystal_description Lath _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 5.694 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.287 _exptl_absorpt_correction_T_max 0.797 _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 0.00 0.2510 1.00 0.00 0.00 0.2350 0.00 -1.00 0.00 0.0580 0.00 1.00 0.00 0.0640 0.00 0.00 1.00 0.0180 0.00 0.00 -1.00 0.0220 _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-scans & /f-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44196 _diffrn_reflns_av_R_equivalents 0.0912 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.28 _reflns_number_total 6940 _reflns_number_gt 5170 _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^)+(0.0257P)^2^+0.4008P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 6940 _refine_ls_number_parameters 421 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0664 _refine_ls_wR_factor_gt 0.0582 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.000 _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 0.364753(14) 0.424616(14) 0.609357(5) 0.02478(5) Uani 1 1 d . . . Fe Fe 0.5000 0.0000 0.5000 0.0329(2) Uani 1 2 d S . . S S 0.51447(9) 0.29637(10) 0.56787(4) 0.0276(2) Uani 1 1 d . . . C1 C 0.4320(4) 0.1626(4) 0.53534(14) 0.0280(9) Uani 1 1 d DU . . C2 C 0.3767(4) 0.0387(4) 0.55199(16) 0.0347(10) Uani 1 1 d DU . . H2 H 0.3825 0.0051 0.5847 0.042 Uiso 1 1 calc R . . C3 C 0.3116(4) -0.0248(6) 0.5109(2) 0.0515(13) Uani 1 1 d DU . . H3 H 0.2669 -0.1098 0.5111 0.062 Uiso 1 1 calc R . . C4 C 0.3238(5) 0.0580(6) 0.46973(19) 0.0603(16) Uani 1 1 d DU . . H4 H 0.2878 0.0391 0.4375 0.072 Uiso 1 1 calc R . . C5 C 0.3989(4) 0.1750(5) 0.48412(15) 0.0452(12) Uani 1 1 d DU . . H5 H 0.4225 0.2477 0.4634 0.054 Uiso 1 1 calc R . . C11 C 0.6237(4) 0.2147(4) 0.61211(14) 0.0285(9) Uani 1 1 d DU . . C12 C 0.7503(4) 0.2436(5) 0.60762(17) 0.0457(12) Uani 1 1 d DU . . H12 H 0.7745 0.3033 0.5825 0.055 Uiso 1 1 calc R . . C13 C 0.8409(5) 0.1837(6) 0.6405(2) 0.0609(15) Uani 1 1 d DU . . H13 H 0.9280 0.2041 0.6387 0.073 Uiso 1 1 calc R . . C14 C 0.8042(5) 0.0952(6) 0.67564(17) 0.0579(15) Uani 1 1 d DU . . H14 H 0.8664 0.0512 0.6973 0.070 Uiso 1 1 calc R . . C15 C 0.6793(5) 0.0696(6) 0.67974(18) 0.0558(14) Uani 1 1 d DU . . H15 H 0.6557 0.0089 0.7047 0.067 Uiso 1 1 calc R . . C16 C 0.5862(4) 0.1300(5) 0.64842(15) 0.0360(10) Uani 1 1 d DU . . H16 H 0.4991 0.1135 0.6519 0.043 Uiso 1 1 calc R . . C21 C 0.2433(4) 0.5516(4) 0.64108(14) 0.0288(9) Uani 1 1 d DU . . C22 C 0.2486(4) 0.6936(4) 0.63235(15) 0.0344(10) Uani 1 1 d DU . . C23 C 0.1698(4) 0.7847(4) 0.65276(16) 0.0396(11) Uani 1 1 d DU . . C24 C 0.0834(4) 0.7384(4) 0.68345(16) 0.0398(11) Uani 1 1 d DU . . C25 C 0.0750(4) 0.5972(4) 0.69298(16) 0.0359(10) Uani 1 1 d DU . . C26 C 0.1538(4) 0.5081(4) 0.67157(15) 0.0328(9) Uani 1 1 d DU . . F1 F 0.3338(3) 0.7424(2) 0.60280(9) 0.0432(6) Uani 1 1 d D . . F2 F 0.1756(3) 0.9201(2) 0.64204(11) 0.0571(8) Uani 1 1 d D . . F3 F 0.0088(3) 0.8275(3) 0.70495(11) 0.0577(8) Uani 1 1 d D . . F4 F -0.0102(3) 0.5509(3) 0.72229(10) 0.0496(7) Uani 1 1 d D . . F5 F 0.1432(2) 0.3723(2) 0.68137(10) 0.0429(6) Uani 1 1 d D . . C31 C 0.5031(4) 0.4822(4) 0.66327(15) 0.0309(9) Uani 1 1 d DU . . C32 C 0.5944(4) 0.5780(4) 0.65572(18) 0.0458(12) Uani 1 1 d DU . . C33 C 0.6843(4) 0.6236(4) 0.6924(2) 0.0543(15) Uani 1 1 d DU . . C34 C 0.6834(4) 0.5678(5) 0.73827(18) 0.0492(13) Uani 1 1 d DU . . C35 C 0.5947(4) 0.4699(5) 0.74712(17) 0.0443(12) Uani 1 1 d DU . . C36 C 0.5059(4) 0.4306(4) 0.71018(15) 0.0347(9) Uani 1 1 d DU . . F6 F 0.6003(3) 0.6333(4) 0.61056(13) 0.0830(12) Uani 1 1 d D . . F7 F 0.7689(3) 0.7193(3) 0.68227(15) 0.0967(14) Uani 1 1 d D . . F8 F 0.7688(3) 0.6095(3) 0.77384(12) 0.0710(10) Uani 1 1 d D . . F9 F 0.5937(3) 0.4151(4) 0.79239(10) 0.0687(10) Uani 1 1 d D . . F10 F 0.4194(2) 0.3359(3) 0.72102(9) 0.0494(7) Uani 1 1 d D . . C41 C 0.2198(4) 0.3698(4) 0.55747(14) 0.0251(8) Uani 1 1 d DU . . C42 C 0.1964(4) 0.4379(4) 0.51366(14) 0.0289(9) Uani 1 1 d DU . . C43 C 0.1047(4) 0.3957(4) 0.47795(15) 0.0355(10) Uani 1 1 d DU . . C44 C 0.0323(4) 0.2813(4) 0.48655(15) 0.0344(10) Uani 1 1 d DU . . C45 C 0.0518(4) 0.2119(4) 0.52998(15) 0.0325(9) Uani 1 1 d DU . . C46 C 0.1454(4) 0.2566(4) 0.56444(13) 0.0263(8) Uani 1 1 d DU . . F11 F 0.2665(3) 0.5507(2) 0.50403(9) 0.0435(7) Uani 1 1 d D . . F12 F 0.0859(3) 0.4647(3) 0.43528(9) 0.0550(8) Uani 1 1 d D . . F13 F -0.0581(3) 0.2399(3) 0.45234(10) 0.0563(8) Uani 1 1 d D . . F14 F -0.0191(3) 0.1004(3) 0.53832(10) 0.0492(7) Uani 1 1 d D . . F15 F 0.1640(2) 0.1820(2) 0.60612(8) 0.0372(6) Uani 1 1 d 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 Au 0.02065(8) 0.01955(7) 0.03245(9) 0.00534(7) -0.00766(5) -0.00263(7) Fe 0.0164(4) 0.0533(6) 0.0280(4) -0.0108(4) -0.0041(3) 0.0049(4) S 0.0191(5) 0.0301(5) 0.0328(5) 0.0099(4) -0.0023(4) -0.0026(4) C1 0.019(2) 0.039(2) 0.025(2) -0.0023(17) -0.0013(16) 0.0032(17) C2 0.022(2) 0.038(2) 0.045(2) -0.0123(18) 0.0098(18) -0.0035(18) C3 0.017(2) 0.068(3) 0.069(3) -0.035(3) 0.002(2) 0.000(2) C4 0.027(3) 0.103(5) 0.048(3) -0.038(3) -0.019(2) 0.025(3) C5 0.036(3) 0.072(3) 0.027(2) 0.000(2) -0.0040(19) 0.022(2) C11 0.024(2) 0.030(2) 0.030(2) -0.0038(17) -0.0067(17) 0.0052(17) C12 0.028(2) 0.059(3) 0.049(3) 0.002(2) -0.004(2) 0.002(2) C13 0.029(3) 0.090(4) 0.061(4) -0.015(3) -0.014(2) 0.014(3) C14 0.053(3) 0.086(4) 0.032(3) -0.007(2) -0.016(2) 0.038(3) C15 0.063(3) 0.066(4) 0.037(3) 0.011(2) -0.002(2) 0.027(3) C16 0.037(3) 0.042(2) 0.028(2) 0.0051(18) -0.0032(18) 0.009(2) C21 0.027(2) 0.022(2) 0.035(2) 0.0008(16) -0.0145(17) 0.0036(16) C22 0.034(2) 0.026(2) 0.041(3) 0.0030(18) -0.0127(19) -0.0002(18) C23 0.046(3) 0.0182(19) 0.051(3) -0.0027(18) -0.019(2) 0.0027(19) C24 0.039(3) 0.026(2) 0.051(3) -0.013(2) -0.016(2) 0.011(2) C25 0.031(2) 0.035(2) 0.040(3) -0.0013(18) -0.0084(19) 0.0054(19) C26 0.032(2) 0.022(2) 0.041(2) 0.0044(18) -0.0124(19) 0.0031(17) F1 0.0520(17) 0.0225(12) 0.0551(16) 0.0086(11) 0.0037(13) -0.0056(12) F2 0.064(2) 0.0199(12) 0.084(2) 0.0002(13) -0.0152(16) 0.0019(14) F3 0.0497(18) 0.0402(16) 0.081(2) -0.0218(14) -0.0044(15) 0.0143(14) F4 0.0462(17) 0.0490(17) 0.0545(17) -0.0003(13) 0.0106(14) 0.0094(14) F5 0.0424(16) 0.0233(12) 0.0641(18) 0.0099(12) 0.0104(13) 0.0029(12) C31 0.027(2) 0.0207(18) 0.043(2) 0.0005(17) -0.0128(18) 0.0001(17) C32 0.038(3) 0.032(2) 0.063(3) 0.014(2) -0.023(2) -0.007(2) C33 0.036(3) 0.025(2) 0.095(4) 0.009(2) -0.036(3) -0.009(2) C34 0.036(3) 0.037(2) 0.069(3) -0.018(2) -0.028(2) 0.007(2) C35 0.028(3) 0.062(3) 0.040(3) -0.009(2) -0.009(2) 0.007(2) C36 0.027(2) 0.035(2) 0.040(2) -0.0067(19) -0.0073(18) 0.004(2) F6 0.057(2) 0.091(2) 0.093(3) 0.064(2) -0.0410(18) -0.0464(19) F7 0.065(2) 0.059(2) 0.154(4) 0.046(2) -0.063(2) -0.0406(19) F8 0.0440(19) 0.075(2) 0.087(2) -0.0351(18) -0.0368(16) 0.0053(16) F9 0.0450(18) 0.125(3) 0.0339(16) -0.0031(17) -0.0123(13) 0.0001(19) F10 0.0349(15) 0.073(2) 0.0393(15) 0.0096(13) -0.0032(12) -0.0130(15) C41 0.021(2) 0.0238(18) 0.029(2) 0.0021(16) -0.0040(16) 0.0017(16) C42 0.026(2) 0.032(2) 0.028(2) 0.0047(17) 0.0004(16) 0.0043(18) C43 0.031(2) 0.044(3) 0.031(2) 0.0050(18) -0.0056(17) 0.0123(19) C44 0.020(2) 0.045(2) 0.036(2) -0.0106(19) -0.0099(17) 0.0061(19) C45 0.023(2) 0.033(2) 0.042(2) -0.0076(18) 0.0020(18) -0.0061(18) C46 0.023(2) 0.031(2) 0.024(2) 0.0002(16) -0.0039(15) -0.0021(17) F11 0.0498(17) 0.0399(15) 0.0400(15) 0.0154(11) -0.0009(12) -0.0065(12) F12 0.063(2) 0.0641(19) 0.0338(15) 0.0112(13) -0.0178(13) 0.0108(16) F13 0.0375(16) 0.076(2) 0.0502(17) -0.0145(15) -0.0238(13) -0.0028(16) F14 0.0385(16) 0.0563(18) 0.0523(17) -0.0141(13) 0.0009(13) -0.0267(13) F15 0.0436(16) 0.0317(13) 0.0351(14) 0.0089(10) -0.0046(11) -0.0128(11) _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 C21 2.028(4) . y Au C31 2.068(4) . y Au C41 2.073(4) . y Au S 2.3786(11) . y Fe C1 2.013(4) 3_656 ? Fe C1 2.013(4) . ? Fe C5 2.033(5) 3_656 ? Fe C5 2.033(5) . ? Fe C2 2.047(4) 3_656 ? Fe C2 2.047(4) . ? Fe C4 2.057(5) . ? Fe C4 2.057(5) 3_656 ? Fe C3 2.058(5) 3_656 ? Fe C3 2.058(5) . ? S C1 1.762(4) . ? S C11 1.788(4) . y C1 C5 1.422(5) . ? C1 C2 1.428(6) . ? C2 C3 1.411(6) . ? C3 C4 1.397(8) . ? C4 C5 1.421(7) . ? C11 C16 1.374(5) . ? C11 C12 1.387(6) . ? C12 C13 1.388(6) . ? C13 C14 1.369(7) . ? C14 C15 1.361(7) . ? C15 C16 1.382(6) . ? C21 C26 1.382(6) . ? C21 C22 1.398(5) . ? C22 F1 1.348(5) . ? C22 C23 1.366(6) . ? C23 F2 1.346(4) . ? C23 C24 1.370(6) . ? C24 F3 1.340(5) . ? C24 C25 1.397(5) . ? C25 F4 1.335(5) . ? C25 C26 1.367(6) . ? C26 F5 1.348(4) . ? C31 C32 1.369(6) . ? C31 C36 1.376(5) . ? C32 F6 1.354(5) . ? C32 C33 1.397(6) . ? C33 F7 1.335(5) . ? C33 C34 1.368(7) . ? C34 F8 1.335(5) . ? C34 C35 1.371(6) . ? C35 F9 1.349(5) . ? C35 C36 1.376(6) . ? C36 F10 1.348(5) . ? C41 C46 1.373(5) . ? C41 C42 1.373(5) . ? C42 F11 1.359(4) . ? C42 C43 1.382(6) . ? C43 F12 1.347(5) . ? C43 C44 1.380(6) . ? C44 F13 1.344(4) . ? C44 C45 1.367(5) . ? C45 F14 1.346(4) . ? C45 C46 1.380(5) . ? C46 F15 1.351(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 C21 Au C31 88.18(15) . . y C21 Au C41 89.30(15) . . y C31 Au C41 177.31(15) . . y C21 Au S 174.03(11) . . y C31 Au S 91.16(12) . . y C41 Au S 91.44(11) . . y C1 Fe C1 180.00(18) 3_656 . ? C1 Fe C5 41.16(15) 3_656 3_656 ? C1 Fe C5 138.84(15) . 3_656 ? C1 Fe C5 138.84(15) 3_656 . ? C1 Fe C5 41.16(15) . . ? C5 Fe C5 180.0(2) 3_656 . ? C1 Fe C2 41.16(15) 3_656 3_656 ? C1 Fe C2 138.84(15) . 3_656 ? C5 Fe C2 68.90(18) 3_656 3_656 ? C5 Fe C2 111.10(19) . 3_656 ? C1 Fe C2 138.84(15) 3_656 . ? C1 Fe C2 41.16(15) . . ? C5 Fe C2 111.10(19) 3_656 . ? C5 Fe C2 68.90(18) . . ? C2 Fe C2 180.000(1) 3_656 . ? C1 Fe C4 111.68(18) 3_656 . ? C1 Fe C4 68.32(17) . . ? C5 Fe C4 139.3(2) 3_656 . ? C5 Fe C4 40.7(2) . . ? C2 Fe C4 112.42(19) 3_656 . ? C2 Fe C4 67.58(19) . . ? C1 Fe C4 68.32(17) 3_656 3_656 ? C1 Fe C4 111.68(18) . 3_656 ? C5 Fe C4 40.7(2) 3_656 3_656 ? C5 Fe C4 139.3(2) . 3_656 ? C2 Fe C4 67.58(19) 3_656 3_656 ? C2 Fe C4 112.42(19) . 3_656 ? C4 Fe C4 180.0(3) . 3_656 ? C1 Fe C3 68.32(18) 3_656 3_656 ? C1 Fe C3 111.68(18) . 3_656 ? C5 Fe C3 68.1(2) 3_656 3_656 ? C5 Fe C3 111.9(2) . 3_656 ? C2 Fe C3 40.20(17) 3_656 3_656 ? C2 Fe C3 139.80(17) . 3_656 ? C4 Fe C3 140.3(2) . 3_656 ? C4 Fe C3 39.7(2) 3_656 3_656 ? C1 Fe C3 111.68(18) 3_656 . ? C1 Fe C3 68.32(18) . . ? C5 Fe C3 111.9(2) 3_656 . ? C5 Fe C3 68.1(2) . . ? C2 Fe C3 139.80(17) 3_656 . ? C2 Fe C3 40.20(17) . . ? C4 Fe C3 39.7(2) . . ? C4 Fe C3 140.3(2) 3_656 . ? C3 Fe C3 180.000(1) 3_656 . ? C1 S C11 106.42(18) . . ? C1 S Au 107.63(13) . . y C11 S Au 109.11(13) . . y C5 C1 C2 108.2(4) . . ? C5 C1 S 120.5(3) . . ? C2 C1 S 131.0(3) . . ? C5 C1 Fe 70.1(2) . . ? C2 C1 Fe 70.7(2) . . ? S C1 Fe 129.5(2) . . ? C3 C2 C1 107.3(4) . . ? C3 C2 Fe 70.3(3) . . ? C1 C2 Fe 68.1(2) . . ? C4 C3 C2 108.8(5) . . ? C4 C3 Fe 70.1(3) . . ? C2 C3 Fe 69.5(2) . . ? C3 C4 C5 108.7(4) . . ? C3 C4 Fe 70.2(3) . . ? C5 C4 Fe 68.7(3) . . ? C4 C5 C1 107.0(4) . . ? C4 C5 Fe 70.6(3) . . ? C1 C5 Fe 68.7(2) . . ? C16 C11 C12 121.7(4) . . ? C16 C11 S 123.0(3) . . ? C12 C11 S 115.3(3) . . ? C11 C12 C13 118.7(5) . . ? C14 C13 C12 119.7(5) . . ? C15 C14 C13 120.5(5) . . ? C14 C15 C16 121.4(5) . . ? C11 C16 C15 117.8(5) . . ? C26 C21 C22 116.3(4) . . ? C26 C21 Au 124.5(3) . . ? C22 C21 Au 119.2(3) . . ? F1 C22 C23 118.9(4) . . ? F1 C22 C21 119.1(4) . . ? C23 C22 C21 122.0(4) . . ? F2 C23 C22 119.9(4) . . ? F2 C23 C24 119.8(4) . . ? C22 C23 C24 120.2(4) . . ? F3 C24 C23 120.6(4) . . ? F3 C24 C25 119.9(4) . . ? C23 C24 C25 119.5(4) . . ? F4 C25 C26 121.0(4) . . ? F4 C25 C24 119.9(4) . . ? C26 C25 C24 119.1(4) . . ? F5 C26 C25 117.8(4) . . ? F5 C26 C21 119.4(4) . . ? C25 C26 C21 122.8(4) . . ? C32 C31 C36 115.3(4) . . ? C32 C31 Au 122.9(3) . . ? C36 C31 Au 121.8(3) . . ? F6 C32 C31 119.6(4) . . ? F6 C32 C33 116.8(4) . . ? C31 C32 C33 123.6(4) . . ? F7 C33 C34 121.4(4) . . ? F7 C33 C32 120.0(5) . . ? C34 C33 C32 118.6(4) . . ? F8 C34 C33 119.6(4) . . ? F8 C34 C35 120.9(5) . . ? C33 C34 C35 119.5(4) . . ? F9 C35 C34 119.5(4) . . ? F9 C35 C36 120.6(4) . . ? C34 C35 C36 119.9(4) . . ? F10 C36 C35 117.5(4) . . ? F10 C36 C31 119.4(4) . . ? C35 C36 C31 123.0(4) . . ? C46 C41 C42 116.2(4) . . ? C46 C41 Au 120.7(3) . . ? C42 C41 Au 123.0(3) . . ? F11 C42 C41 119.6(3) . . ? F11 C42 C43 117.7(3) . . ? C41 C42 C43 122.7(4) . . ? F12 C43 C44 120.2(4) . . ? F12 C43 C42 120.7(4) . . ? C44 C43 C42 119.1(4) . . ? F13 C44 C45 120.4(4) . . ? F13 C44 C43 119.7(4) . . ? C45 C44 C43 119.9(4) . . ? F14 C45 C44 119.7(4) . . ? F14 C45 C46 121.0(4) . . ? C44 C45 C46 119.2(4) . . ? F15 C46 C41 120.0(3) . . ? F15 C46 C45 117.1(3) . . ? C41 C46 C45 122.9(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.511 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.125 ################END data_saturno #(complex 7 in MS) _database_code_CSD 176349 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H18 Ag F3 Fe O3 S3' _chemical_formula_weight 659.27 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' '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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7150(10) _cell_length_b 16.222(2) _cell_length_c 14.1250(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.916(6) _cell_angle_gamma 90.00 _cell_volume 2308.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 62 _cell_measurement_theta_min 6 _cell_measurement_theta_max 12.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.798 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.3659 _exptl_absorpt_correction_T_max 0.4668 _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-P4 _diffrn_measurement_method theta-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 297 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5190 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 2 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4030 _reflns_number_gt 3454 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _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^)+(0.0620P)^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 4030 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0826 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 0.34221(3) 0.411507(15) 0.571034(19) 0.03197(10) Uani 1 1 d . . . Fe Fe 0.02016(4) 0.27822(2) 0.52146(3) 0.01993(12) Uani 1 1 d . . . S1 S 0.33145(8) 0.25975(5) 0.53684(5) 0.02459(18) Uani 1 1 d . . . S2 S 0.14134(8) 0.46232(4) 0.61300(5) 0.02454(17) Uani 1 1 d . . . C1 C 0.1620(3) 0.25058(18) 0.4620(2) 0.0226(6) Uani 1 1 d . . . C2 C 0.0781(3) 0.31415(19) 0.4043(2) 0.0248(6) Uani 1 1 d . . . H2 H 0.1052 0.3680 0.3932 0.030 Uiso 1 1 calc R . . C3 C -0.0528(3) 0.2824(2) 0.3665(2) 0.0295(7) Uani 1 1 d . . . H3 H -0.1292 0.3116 0.3259 0.035 Uiso 1 1 calc R . . C4 C -0.0505(3) 0.2002(2) 0.3993(2) 0.0311(7) Uani 1 1 d . . . H4 H -0.1250 0.1644 0.3838 0.037 Uiso 1 1 calc R . . C5 C 0.0816(3) 0.17947(18) 0.4592(2) 0.0275(7) Uani 1 1 d . . . H5 H 0.1111 0.1281 0.4914 0.033 Uiso 1 1 calc R . . C6 C 0.0566(3) 0.37089(18) 0.6227(2) 0.0235(6) Uani 1 1 d . . . C7 C -0.0837(3) 0.35917(19) 0.5793(2) 0.0269(7) Uani 1 1 d . . . H7 H -0.1471 0.3989 0.5431 0.032 Uiso 1 1 calc R . . C8 C -0.1104(3) 0.27677(19) 0.6006(2) 0.0301(7) Uani 1 1 d . . . H8 H -0.1955 0.2515 0.5803 0.036 Uiso 1 1 calc R . . C9 C 0.0112(4) 0.2384(2) 0.6573(2) 0.0290(7) Uani 1 1 d . . . H9 H 0.0211 0.1833 0.6815 0.035 Uiso 1 1 calc R . . C10 C 0.1155(3) 0.29616(19) 0.6717(2) 0.0263(7) Uani 1 1 d . . . H10 H 0.2072 0.2870 0.7073 0.032 Uiso 1 1 calc R . . C11 C 0.4185(3) 0.24126(18) 0.4505(2) 0.0227(6) Uani 1 1 d . . . C12 C 0.5135(4) 0.2970(2) 0.4457(3) 0.0339(8) Uani 1 1 d . . . H12 H 0.5286 0.3460 0.4849 0.041 Uiso 1 1 calc R . . C13 C 0.5868(4) 0.2816(2) 0.3838(3) 0.0392(8) Uani 1 1 d . . . H13 H 0.6535 0.3194 0.3817 0.047 Uiso 1 1 calc R . . C14 C 0.5633(3) 0.2112(2) 0.3248(2) 0.0343(8) Uani 1 1 d . . . H14 H 0.6118 0.2013 0.2808 0.041 Uiso 1 1 calc R . . C15 C 0.4685(3) 0.1556(2) 0.3307(3) 0.0347(8) Uani 1 1 d . . . H15 H 0.4522 0.1073 0.2904 0.042 Uiso 1 1 calc R . . C16 C 0.3971(3) 0.16910(19) 0.3941(2) 0.0306(7) Uani 1 1 d . . . H16 H 0.3342 0.1296 0.3992 0.037 Uiso 1 1 calc R . . C21 C 0.1932(3) 0.50362(17) 0.7378(2) 0.0234(6) Uani 1 1 d . . . C22 C 0.1151(4) 0.49605(19) 0.7979(2) 0.0307(7) Uani 1 1 d . . . H22 H 0.0338 0.4664 0.7749 0.037 Uiso 1 1 calc R . . C23 C 0.1580(4) 0.5327(2) 0.8926(3) 0.0374(8) Uani 1 1 d . . . H23 H 0.1055 0.5278 0.9346 0.045 Uiso 1 1 calc R . . C24 C 0.2752(4) 0.5758(2) 0.9262(3) 0.0400(9) Uani 1 1 d . . . H24 H 0.3036 0.6003 0.9912 0.048 Uiso 1 1 calc R . . C25 C 0.3519(4) 0.5835(2) 0.8654(3) 0.0421(9) Uani 1 1 d . . . H25 H 0.4326 0.6138 0.8885 0.050 Uiso 1 1 calc R . . C26 C 0.3116(3) 0.5473(2) 0.7706(2) 0.0323(7) Uani 1 1 d . . . H26 H 0.3645 0.5524 0.7289 0.039 Uiso 1 1 calc R . . S3 S 0.34834(8) 0.51128(5) 0.33960(6) 0.02711(18) Uani 1 1 d . . . O1 O 0.2757(2) 0.47409(15) 0.39748(17) 0.0380(6) Uani 1 1 d . . . O2 O 0.4898(2) 0.49176(14) 0.37529(18) 0.0371(6) Uani 1 1 d . . . O3 O 0.3180(3) 0.59565(14) 0.3133(2) 0.0488(7) Uani 1 1 d . . . C99 C 0.2888(4) 0.4559(2) 0.2203(3) 0.0403(8) Uani 1 1 d . . . F1 F 0.3012(3) 0.37595(15) 0.2332(2) 0.0719(8) Uani 1 1 d . . . F2 F 0.3541(3) 0.47758(19) 0.16034(18) 0.0708(8) Uani 1 1 d . . . F3 F 0.1613(2) 0.47115(19) 0.17150(18) 0.0686(8) 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 0.03014(16) 0.03448(16) 0.03424(16) -0.00975(10) 0.01481(12) -0.01181(11) Fe 0.0191(2) 0.0226(2) 0.0191(2) -0.00232(15) 0.00782(18) -0.00335(17) S1 0.0202(4) 0.0302(4) 0.0233(4) -0.0016(3) 0.0073(3) -0.0015(3) S2 0.0263(4) 0.0248(4) 0.0225(4) -0.0028(3) 0.0081(3) -0.0047(3) C1 0.0203(16) 0.0274(15) 0.0224(14) -0.0029(12) 0.0102(12) -0.0013(12) C2 0.0254(17) 0.0327(15) 0.0182(14) -0.0021(12) 0.0097(13) -0.0021(13) C3 0.0225(16) 0.0447(18) 0.0197(14) -0.0042(13) 0.0051(13) -0.0024(14) C4 0.0259(17) 0.0367(17) 0.0311(17) -0.0167(14) 0.0101(14) -0.0106(14) C5 0.0295(17) 0.0230(14) 0.0330(16) -0.0103(12) 0.0145(14) -0.0046(13) C6 0.0245(16) 0.0261(15) 0.0215(14) -0.0060(12) 0.0098(13) -0.0039(13) C7 0.0230(16) 0.0309(15) 0.0275(15) -0.0070(13) 0.0097(13) -0.0013(13) C8 0.0266(17) 0.0363(17) 0.0332(17) -0.0049(13) 0.0177(15) -0.0054(14) C9 0.0370(19) 0.0295(16) 0.0246(15) -0.0002(12) 0.0159(14) -0.0044(14) C10 0.0291(17) 0.0304(15) 0.0189(14) -0.0018(12) 0.0076(13) -0.0008(14) C11 0.0178(15) 0.0273(14) 0.0217(14) 0.0023(12) 0.0051(12) 0.0044(12) C12 0.0352(19) 0.0279(16) 0.0443(19) -0.0057(14) 0.0211(17) -0.0035(15) C13 0.035(2) 0.0385(18) 0.050(2) -0.0007(16) 0.0233(18) -0.0032(16) C14 0.0271(18) 0.048(2) 0.0282(16) 0.0029(14) 0.0107(14) 0.0135(16) C15 0.0288(18) 0.0393(18) 0.0316(17) -0.0112(14) 0.0048(15) 0.0023(15) C16 0.0245(17) 0.0326(17) 0.0320(17) -0.0058(13) 0.0062(14) -0.0014(14) C21 0.0242(16) 0.0190(13) 0.0232(14) -0.0024(11) 0.0033(13) 0.0043(12) C22 0.0311(18) 0.0290(16) 0.0327(17) -0.0049(13) 0.0118(15) 0.0018(14) C23 0.045(2) 0.0387(18) 0.0305(17) -0.0033(15) 0.0162(16) 0.0075(17) C24 0.043(2) 0.0370(18) 0.0319(18) -0.0123(14) 0.0031(17) 0.0048(16) C25 0.033(2) 0.041(2) 0.044(2) -0.0147(16) 0.0029(17) -0.0072(16) C26 0.0270(18) 0.0339(17) 0.0341(17) -0.0034(14) 0.0080(15) -0.0017(14) S3 0.0273(4) 0.0280(4) 0.0291(4) -0.0023(3) 0.0135(3) -0.0067(3) O1 0.0370(14) 0.0460(13) 0.0368(13) 0.0037(11) 0.0203(11) -0.0103(11) O2 0.0256(13) 0.0409(13) 0.0422(14) -0.0116(10) 0.0080(11) -0.0110(10) O3 0.067(2) 0.0306(13) 0.0596(17) 0.0051(11) 0.0350(16) 0.0009(13) C99 0.0299(19) 0.054(2) 0.0363(19) -0.0062(17) 0.0102(16) -0.0023(17) F1 0.083(2) 0.0478(14) 0.0682(17) -0.0276(12) 0.0040(16) -0.0063(14) F2 0.0602(17) 0.121(2) 0.0394(13) -0.0184(14) 0.0279(13) -0.0225(16) F3 0.0287(13) 0.113(2) 0.0494(14) -0.0184(14) -0.0059(11) 0.0062(14) _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 O2 2.312(2) 3_666 y Ag S1 2.5037(8) . y Ag O1 2.521(2) . y Ag S2 2.5558(8) . y Fe C6 2.019(3) . ? Fe C1 2.021(3) . ? Fe C10 2.039(3) . ? Fe C2 2.041(3) . ? Fe C5 2.041(3) . ? Fe C9 2.057(3) . ? Fe C3 2.059(3) . ? Fe C7 2.062(3) . ? Fe C4 2.065(3) . ? Fe C8 2.067(3) . ? S1 C1 1.768(3) . ? S1 C11 1.795(3) . ? S2 C6 1.768(3) . ? S2 C21 1.788(3) . ? C1 C2 1.427(4) . ? C1 C5 1.432(4) . ? C2 C3 1.417(5) . ? C3 C4 1.409(5) . ? C4 C5 1.420(5) . ? C6 C7 1.431(4) . ? C6 C10 1.432(4) . ? C7 C8 1.420(4) . ? C8 C9 1.420(5) . ? C9 C10 1.419(5) . ? C11 C12 1.381(5) . ? C11 C16 1.390(4) . ? C12 C13 1.383(5) . ? C13 C14 1.384(5) . ? C14 C15 1.382(5) . ? C15 C16 1.379(5) . ? C21 C22 1.386(5) . ? C21 C26 1.388(5) . ? C22 C23 1.392(5) . ? C23 C24 1.373(5) . ? C24 C25 1.382(6) . ? C25 C26 1.388(5) . ? S3 O3 1.426(2) . ? S3 O1 1.440(2) . ? S3 O2 1.460(3) . ? S3 C99 1.823(4) . ? O2 Ag 2.312(2) 3_666 ? C99 F1 1.310(5) . ? C99 F2 1.316(4) . ? C99 F3 1.327(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 O2 Ag S1 135.24(7) 3_666 . y O2 Ag O1 88.64(8) 3_666 . y S1 Ag O1 103.25(6) . . y O2 Ag S2 109.14(6) 3_666 . y S1 Ag S2 112.01(3) . . y O1 Ag S2 96.55(6) . . y C6 Fe C1 117.89(12) . . ? C6 Fe C10 41.31(12) . . ? C1 Fe C10 106.44(13) . . ? C6 Fe C2 108.84(12) . . ? C1 Fe C2 41.13(12) . . ? C10 Fe C2 128.35(13) . . ? C6 Fe C5 151.19(13) . . ? C1 Fe C5 41.28(12) . . ? C10 Fe C5 116.07(13) . . ? C2 Fe C5 69.08(13) . . ? C6 Fe C9 68.44(12) . . ? C1 Fe C9 126.74(13) . . ? C10 Fe C9 40.54(13) . . ? C2 Fe C9 165.85(14) . . ? C5 Fe C9 106.22(13) . . ? C6 Fe C3 129.82(13) . . ? C1 Fe C3 68.44(13) . . ? C10 Fe C3 167.44(13) . . ? C2 Fe C3 40.43(13) . . ? C5 Fe C3 68.24(13) . . ? C9 Fe C3 151.65(13) . . ? C6 Fe C7 41.02(12) . . ? C1 Fe C7 152.85(12) . . ? C10 Fe C7 69.10(13) . . ? C2 Fe C7 119.62(12) . . ? C5 Fe C7 165.33(13) . . ? C9 Fe C7 68.13(13) . . ? C3 Fe C7 109.86(13) . . ? C6 Fe C4 167.38(13) . . ? C1 Fe C4 68.29(13) . . ? C10 Fe C4 150.29(13) . . ? C2 Fe C4 67.88(13) . . ? C5 Fe C4 40.45(13) . . ? C9 Fe C4 117.80(13) . . ? C3 Fe C4 39.96(13) . . ? C7 Fe C4 128.91(13) . . ? C6 Fe C8 68.21(13) . . ? C1 Fe C8 164.87(12) . . ? C10 Fe C8 68.29(13) . . ? C2 Fe C8 152.98(13) . . ? C5 Fe C8 126.94(13) . . ? C9 Fe C8 40.27(14) . . ? C3 Fe C8 119.57(14) . . ? C7 Fe C8 40.24(12) . . ? C4 Fe C8 108.79(13) . . ? C1 S1 C11 104.20(13) . . ? C1 S1 Ag 99.70(10) . . y C11 S1 Ag 107.15(10) . . y C6 S2 C21 103.48(14) . . ? C6 S2 Ag 104.04(10) . . y C21 S2 Ag 110.22(11) . . y C2 C1 C5 108.1(3) . . ? C2 C1 S1 126.8(2) . . ? C5 C1 S1 124.7(2) . . ? C2 C1 Fe 70.17(17) . . ? C5 C1 Fe 70.11(17) . . ? S1 C1 Fe 119.82(15) . . ? C3 C2 C1 107.6(3) . . ? C3 C2 Fe 70.48(18) . . ? C1 C2 Fe 68.70(16) . . ? C4 C3 C2 108.4(3) . . ? C4 C3 Fe 70.24(18) . . ? C2 C3 Fe 69.08(17) . . ? C3 C4 C5 108.8(3) . . ? C3 C4 Fe 69.80(17) . . ? C5 C4 Fe 68.87(17) . . ? C4 C5 C1 107.1(3) . . ? C4 C5 Fe 70.68(18) . . ? C1 C5 Fe 68.61(16) . . ? C7 C6 C10 108.7(3) . . ? C7 C6 S2 124.8(2) . . ? C10 C6 S2 126.5(2) . . ? C7 C6 Fe 71.08(16) . . ? C10 C6 Fe 70.07(17) . . ? S2 C6 Fe 123.36(16) . . ? C8 C7 C6 107.0(3) . . ? C8 C7 Fe 70.09(18) . . ? C6 C7 Fe 67.90(17) . . ? C9 C8 C7 108.7(3) . . ? C9 C8 Fe 69.48(18) . . ? C7 C8 Fe 69.67(17) . . ? C10 C9 C8 108.5(3) . . ? C10 C9 Fe 69.03(17) . . ? C8 C9 Fe 70.24(17) . . ? C9 C10 C6 107.1(3) . . ? C9 C10 Fe 70.43(17) . . ? C6 C10 Fe 68.62(16) . . ? C12 C11 C16 120.2(3) . . ? C12 C11 S1 119.1(2) . . ? C16 C11 S1 120.5(2) . . ? C11 C12 C13 120.0(3) . . ? C12 C13 C14 120.2(3) . . ? C15 C14 C13 119.2(3) . . ? C16 C15 C14 121.2(3) . . ? C15 C16 C11 119.1(3) . . ? C22 C21 C26 120.9(3) . . ? C22 C21 S2 121.4(2) . . ? C26 C21 S2 117.6(2) . . ? C21 C22 C23 118.7(3) . . ? C24 C23 C22 120.9(3) . . ? C23 C24 C25 119.9(3) . . ? C24 C25 C26 120.4(3) . . ? C25 C26 C21 119.1(3) . . ? O3 S3 O1 115.50(16) . . ? O3 S3 O2 114.57(17) . . ? O1 S3 O2 114.32(15) . . ? O3 S3 C99 104.81(18) . . ? O1 S3 C99 103.41(16) . . ? O2 S3 C99 101.97(15) . . ? S3 O1 Ag 133.81(15) . . y S3 O2 Ag 124.51(14) . 3_666 y F1 C99 F2 107.7(3) . . ? F1 C99 F3 107.1(3) . . ? F2 C99 F3 107.1(3) . . ? F1 C99 S3 111.8(3) . . ? F2 C99 S3 111.6(3) . . ? F3 C99 S3 111.2(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.111 _refine_diff_density_min -1.221 _refine_diff_density_rms 0.107 ####################END data_se4ag #(complex 8 in the MS) _database_code_CSD 176350 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H18 Ag F3 Fe O3 S Se2' _chemical_formula_weight 753.07 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' '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 'P 21/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 10.7367(8) _cell_length_b 16.0702(14) _cell_length_c 14.2622(12) _cell_angle_alpha 90.00 _cell_angle_beta 109.167(3) _cell_angle_gamma 90.00 _cell_volume 2324.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 6735 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 4.738 _exptl_absorpt_correction_type 'multiple scans (SADABS)' _exptl_absorpt_correction_T_min 0.732 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_process_details ? _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-scans _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19087 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6758 _reflns_number_gt 5021 _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^)+(0.0182P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6758 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0479 _refine_ls_wR_factor_gt 0.0453 _refine_ls_goodness_of_fit_ref 0.879 _refine_ls_restrained_S_all 0.879 _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 0.339321(19) 0.415672(12) 0.571410(15) 0.02370(5) Uani 1 1 d . . . Se1 Se 0.33756(2) 0.256068(15) 0.546363(18) 0.01883(6) Uani 1 1 d . . . Se2 Se 0.13305(2) 0.471947(15) 0.613020(18) 0.01808(6) Uani 1 1 d . . . Fe Fe 0.01527(3) 0.27637(2) 0.52525(3) 0.01578(8) Uani 1 1 d . . . C1 C 0.1568(2) 0.24806(15) 0.46540(18) 0.0182(5) Uani 1 1 d . . . C2 C 0.0760(2) 0.31327(15) 0.40960(17) 0.0186(5) Uani 1 1 d . . . H2 H 0.1048 0.3674 0.3994 0.022 Uiso 1 1 calc R . . C3 C -0.0549(2) 0.28285(16) 0.37205(18) 0.0220(5) Uani 1 1 d . . . H3 H -0.1295 0.3132 0.3324 0.026 Uiso 1 1 calc R . . C4 C -0.0553(3) 0.19844(16) 0.40416(19) 0.0229(6) Uani 1 1 d . . . H4 H -0.1304 0.1632 0.3891 0.027 Uiso 1 1 calc R . . C5 C 0.0745(3) 0.17645(14) 0.46204(19) 0.0221(5) Uani 1 1 d . . . H5 H 0.1025 0.1242 0.4930 0.027 Uiso 1 1 calc R . . C6 C 0.0478(2) 0.37025(15) 0.62521(17) 0.0176(5) Uani 1 1 d . . . C7 C -0.0901(2) 0.35577(15) 0.58415(18) 0.0203(5) Uani 1 1 d . . . H7 H -0.1549 0.3948 0.5487 0.024 Uiso 1 1 calc R . . C8 C -0.1131(3) 0.27189(15) 0.60610(19) 0.0216(5) Uani 1 1 d . . . H8 H -0.1963 0.2448 0.5875 0.026 Uiso 1 1 calc R . . C9 C 0.0095(3) 0.23608(16) 0.66052(18) 0.0224(6) Uani 1 1 d . . . H9 H 0.0224 0.1806 0.6847 0.027 Uiso 1 1 calc R . . C10 C 0.1094(3) 0.29576(15) 0.67316(17) 0.0199(5) Uani 1 1 d . . . H10 H 0.2009 0.2880 0.7072 0.024 Uiso 1 1 calc R . . C11 C 0.4275(2) 0.24057(14) 0.45016(18) 0.0177(5) Uani 1 1 d . . . C12 C 0.5244(3) 0.29667(15) 0.4488(2) 0.0246(6) Uani 1 1 d . . . H12 H 0.5428 0.3433 0.4922 0.030 Uiso 1 1 calc R . . C13 C 0.5949(3) 0.28460(17) 0.3839(2) 0.0278(6) Uani 1 1 d . . . H13 H 0.6618 0.3229 0.3829 0.033 Uiso 1 1 calc R . . C14 C 0.5676(3) 0.21675(16) 0.32055(19) 0.0246(6) Uani 1 1 d . . . H14 H 0.6149 0.2089 0.2754 0.030 Uiso 1 1 calc R . . C15 C 0.4713(2) 0.16035(16) 0.32321(18) 0.0226(5) Uani 1 1 d . . . H15 H 0.4532 0.1136 0.2800 0.027 Uiso 1 1 calc R . . C16 C 0.4012(2) 0.17149(15) 0.38827(19) 0.0220(5) Uani 1 1 d . . . H16 H 0.3359 0.1324 0.3905 0.026 Uiso 1 1 calc R . . C21 C 0.1970(2) 0.50833(14) 0.74940(18) 0.0170(5) Uani 1 1 d . . . C22 C 0.1190(3) 0.50041(15) 0.8097(2) 0.0235(6) Uani 1 1 d . . . H22 H 0.0355 0.4738 0.7858 0.028 Uiso 1 1 calc R . . C23 C 0.1654(3) 0.53216(16) 0.90597(19) 0.0250(6) Uani 1 1 d . . . H23 H 0.1130 0.5274 0.9480 0.030 Uiso 1 1 calc R . . C24 C 0.2872(3) 0.57059(16) 0.9406(2) 0.0291(6) Uani 1 1 d . . . H24 H 0.3183 0.5920 1.0063 0.035 Uiso 1 1 calc R . . C25 C 0.3637(3) 0.57790(16) 0.8800(2) 0.0300(6) Uani 1 1 d . . . H25 H 0.4473 0.6045 0.9041 0.036 Uiso 1 1 calc R . . C26 C 0.3195(2) 0.54680(15) 0.78435(19) 0.0234(6) Uani 1 1 d . . . H26 H 0.3725 0.5517 0.7428 0.028 Uiso 1 1 calc R . . S S 0.35119(6) 0.50973(4) 0.34189(5) 0.02113(13) Uani 1 1 d . . . O1 O 0.27655(17) 0.47453(11) 0.39990(13) 0.0265(4) Uani 1 1 d . . . O2 O 0.49015(17) 0.48785(11) 0.37683(14) 0.0273(4) Uani 1 1 d . . . O3 O 0.3240(2) 0.59515(11) 0.31430(15) 0.0341(5) Uani 1 1 d . . . C99 C 0.2905(3) 0.45222(18) 0.2252(2) 0.0289(6) Uani 1 1 d . . . F1 F 0.29864(17) 0.37117(10) 0.24021(13) 0.0449(4) Uani 1 1 d . . . F2 F 0.35856(17) 0.47164(12) 0.16546(12) 0.0475(5) Uani 1 1 d . . . F3 F 0.16456(16) 0.47080(12) 0.17602(13) 0.0469(5) 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 0.02390(11) 0.02454(10) 0.02555(11) -0.00560(8) 0.01206(9) -0.00727(8) Se1 0.01705(12) 0.02172(13) 0.01892(13) -0.00026(10) 0.00752(10) 0.00033(10) Se2 0.01974(13) 0.01776(12) 0.01666(12) -0.00119(10) 0.00588(10) -0.00214(10) Fe 0.01610(18) 0.01590(17) 0.01675(18) -0.00178(13) 0.00730(14) -0.00160(14) C1 0.0152(12) 0.0213(12) 0.0198(13) -0.0039(10) 0.0079(10) -0.0008(10) C2 0.0233(14) 0.0185(12) 0.0161(13) -0.0027(10) 0.0095(11) -0.0018(10) C3 0.0176(13) 0.0327(15) 0.0162(13) -0.0037(10) 0.0064(10) -0.0001(11) C4 0.0200(14) 0.0266(14) 0.0248(14) -0.0106(11) 0.0111(11) -0.0077(11) C5 0.0255(14) 0.0160(12) 0.0275(15) -0.0032(10) 0.0122(12) -0.0012(10) C6 0.0191(13) 0.0185(12) 0.0169(12) -0.0017(10) 0.0083(10) -0.0013(10) C7 0.0215(13) 0.0208(13) 0.0212(13) -0.0020(10) 0.0106(11) 0.0015(10) C8 0.0226(13) 0.0250(13) 0.0217(14) -0.0036(10) 0.0132(11) -0.0044(11) C9 0.0290(15) 0.0245(13) 0.0175(13) 0.0003(10) 0.0126(11) -0.0009(11) C10 0.0239(14) 0.0219(13) 0.0143(12) -0.0008(10) 0.0070(10) 0.0007(10) C11 0.0154(12) 0.0206(12) 0.0176(12) 0.0012(10) 0.0059(10) 0.0035(10) C12 0.0255(14) 0.0214(13) 0.0296(15) -0.0062(11) 0.0128(12) -0.0035(11) C13 0.0234(15) 0.0318(15) 0.0325(16) -0.0015(12) 0.0150(13) -0.0023(12) C14 0.0222(14) 0.0319(15) 0.0216(14) 0.0018(11) 0.0096(11) 0.0065(11) C15 0.0223(14) 0.0246(13) 0.0190(14) -0.0061(10) 0.0042(11) 0.0024(11) C16 0.0193(13) 0.0203(13) 0.0248(14) -0.0026(10) 0.0051(11) -0.0033(10) C21 0.0204(13) 0.0131(11) 0.0154(12) 0.0000(9) 0.0032(10) 0.0044(9) C22 0.0221(14) 0.0217(13) 0.0287(15) -0.0032(11) 0.0110(12) -0.0008(10) C23 0.0299(15) 0.0247(13) 0.0231(14) -0.0001(11) 0.0126(12) 0.0034(12) C24 0.0383(17) 0.0252(14) 0.0204(14) -0.0066(11) 0.0049(12) 0.0020(12) C25 0.0245(15) 0.0288(15) 0.0322(16) -0.0125(12) 0.0031(12) -0.0060(12) C26 0.0205(14) 0.0249(14) 0.0264(15) -0.0023(11) 0.0100(12) -0.0001(11) S 0.0228(3) 0.0206(3) 0.0229(3) -0.0021(2) 0.0115(3) -0.0044(3) O1 0.0273(10) 0.0296(10) 0.0266(10) -0.0002(8) 0.0144(8) -0.0066(8) O2 0.0199(10) 0.0291(10) 0.0319(11) -0.0066(8) 0.0073(8) -0.0066(8) O3 0.0454(13) 0.0204(10) 0.0443(13) 0.0042(9) 0.0254(11) 0.0006(9) C99 0.0194(14) 0.0400(17) 0.0286(16) -0.0066(13) 0.0095(12) -0.0008(12) F1 0.0510(12) 0.0300(10) 0.0475(12) -0.0171(8) 0.0079(9) -0.0050(8) F2 0.0407(11) 0.0774(13) 0.0304(10) -0.0131(9) 0.0200(9) -0.0110(10) F3 0.0249(9) 0.0747(13) 0.0340(11) -0.0088(9) 0.0001(8) 0.0065(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag O2 2.3267(17) 3_666 Y Ag O1 2.4999(18) . Y Ag Se1 2.5888(4) . Y Ag Se2 2.6339(3) . Y Se1 C1 1.909(2) . Y Se1 C11 1.936(2) . Y Se2 C6 1.909(2) . Y Se2 C21 1.929(2) . Y Fe C1 2.024(2) . ? Fe C6 2.026(2) . ? Fe C10 2.042(2) . ? Fe C5 2.043(2) . ? Fe C2 2.050(2) . ? Fe C9 2.055(2) . ? Fe C7 2.059(2) . ? Fe C4 2.065(2) . ? Fe C3 2.067(2) . ? Fe C8 2.069(2) . ? C1 C2 1.425(3) . ? C1 C5 1.442(3) . ? C2 C3 1.417(3) . ? C3 C4 1.432(4) . ? C4 C5 1.412(4) . ? C6 C7 1.422(3) . ? C6 C10 1.429(3) . ? C7 C8 1.424(3) . ? C8 C9 1.413(4) . ? C9 C10 1.406(3) . ? C11 C12 1.381(3) . ? C11 C16 1.388(3) . ? C12 C13 1.389(3) . ? C13 C14 1.384(4) . ? C14 C15 1.385(3) . ? C15 C16 1.385(3) . ? C21 C26 1.389(3) . ? C21 C22 1.389(3) . ? C22 C23 1.394(4) . ? C23 C24 1.383(4) . ? C24 C25 1.380(4) . ? C25 C26 1.382(3) . ? S O3 1.4315(19) . Y S O1 1.4429(16) . Y S O2 1.4525(18) . Y S C99 1.826(3) . Y O2 Ag 2.3267(17) 3_666 ? C99 F1 1.318(3) . Y C99 F2 1.329(3) . Y C99 F3 1.337(3) . Y 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 O2 Ag O1 89.40(6) 3_666 . Y O2 Ag Se1 132.32(4) 3_666 . Y O1 Ag Se1 104.62(4) . . Y O2 Ag Se2 109.39(4) 3_666 . Y O1 Ag Se2 96.55(4) . . Y Se1 Ag Se2 113.744(10) . . Y C1 Se1 C11 101.96(10) . . Y C1 Se1 Ag 96.33(7) . . Y C11 Se1 Ag 104.03(7) . . Y C6 Se2 C21 100.97(10) . . Y C6 Se2 Ag 100.97(7) . . Y C21 Se2 Ag 106.50(7) . . Y C1 Fe C6 118.96(9) . . ? C1 Fe C10 106.52(10) . . ? C6 Fe C10 41.13(9) . . ? C1 Fe C5 41.53(9) . . ? C6 Fe C5 152.79(10) . . ? C10 Fe C5 117.11(10) . . ? C1 Fe C2 40.94(9) . . ? C6 Fe C2 108.89(9) . . ? C10 Fe C2 127.35(10) . . ? C5 Fe C2 69.20(9) . . ? C1 Fe C9 125.68(10) . . ? C6 Fe C9 68.00(9) . . ? C10 Fe C9 40.13(9) . . ? C5 Fe C9 106.05(10) . . ? C2 Fe C9 164.13(10) . . ? C1 Fe C7 154.26(10) . . ? C6 Fe C7 40.73(9) . . ? C10 Fe C7 68.65(10) . . ? C5 Fe C7 163.71(10) . . ? C2 Fe C7 120.77(9) . . ? C9 Fe C7 67.80(10) . . ? C1 Fe C4 68.37(10) . . ? C6 Fe C4 166.21(10) . . ? C10 Fe C4 151.37(10) . . ? C5 Fe C4 40.21(10) . . ? C2 Fe C4 68.23(10) . . ? C9 Fe C4 118.56(10) . . ? C7 Fe C4 128.09(10) . . ? C1 Fe C3 68.22(10) . . ? C6 Fe C3 128.70(10) . . ? C10 Fe C3 165.82(10) . . ? C5 Fe C3 68.36(10) . . ? C2 Fe C3 40.25(9) . . ? C9 Fe C3 153.57(10) . . ? C7 Fe C3 109.98(10) . . ? C4 Fe C3 40.56(10) . . ? C1 Fe C8 163.20(10) . . ? C6 Fe C8 68.04(9) . . ? C10 Fe C8 67.91(10) . . ? C5 Fe C8 125.44(10) . . ? C2 Fe C8 154.78(10) . . ? C9 Fe C8 40.07(10) . . ? C7 Fe C8 40.35(9) . . ? C4 Fe C8 108.44(10) . . ? C3 Fe C8 120.85(10) . . ? C2 C1 C5 108.3(2) . . ? C2 C1 Se1 126.86(18) . . ? C5 C1 Se1 124.34(19) . . ? C2 C1 Fe 70.52(12) . . ? C5 C1 Fe 69.92(12) . . ? Se1 C1 Fe 118.99(12) . . ? C3 C2 C1 107.7(2) . . ? C3 C2 Fe 70.50(13) . . ? C1 C2 Fe 68.54(13) . . ? C2 C3 C4 108.2(2) . . ? C2 C3 Fe 69.25(14) . . ? C4 C3 Fe 69.67(14) . . ? C5 C4 C3 108.5(2) . . ? C5 C4 Fe 69.03(14) . . ? C3 C4 Fe 69.78(14) . . ? C4 C5 C1 107.2(2) . . ? C4 C5 Fe 70.76(14) . . ? C1 C5 Fe 68.55(13) . . ? C7 C6 C10 108.4(2) . . ? C7 C6 Se2 124.64(18) . . ? C10 C6 Se2 126.90(18) . . ? C7 C6 Fe 70.89(14) . . ? C10 C6 Fe 70.04(13) . . ? Se2 C6 Fe 123.41(11) . . ? C6 C7 C8 107.3(2) . . ? C6 C7 Fe 68.38(13) . . ? C8 C7 Fe 70.20(13) . . ? C9 C8 C7 108.0(2) . . ? C9 C8 Fe 69.44(13) . . ? C7 C8 Fe 69.45(12) . . ? C10 C9 C8 109.1(2) . . ? C10 C9 Fe 69.43(13) . . ? C8 C9 Fe 70.48(14) . . ? C9 C10 C6 107.2(2) . . ? C9 C10 Fe 70.44(14) . . ? C6 C10 Fe 68.83(14) . . ? C12 C11 C16 120.7(2) . . ? C12 C11 Se1 118.61(18) . . ? C16 C11 Se1 120.58(17) . . ? C11 C12 C13 119.7(2) . . ? C14 C13 C12 120.0(2) . . ? C13 C14 C15 119.8(2) . . ? C14 C15 C16 120.6(2) . . ? C15 C16 C11 119.2(2) . . ? C26 C21 C22 120.7(2) . . ? C26 C21 Se2 118.58(17) . . ? C22 C21 Se2 120.61(19) . . ? C21 C22 C23 118.9(2) . . ? C24 C23 C22 120.4(2) . . ? C25 C24 C23 120.1(3) . . ? C24 C25 C26 120.4(3) . . ? C25 C26 C21 119.5(2) . . ? O3 S O1 115.60(11) . . Y O3 S O2 114.84(11) . . Y O1 S O2 114.19(11) . . Y O3 S C99 104.79(13) . . Y O1 S C99 103.01(12) . . Y O2 S C99 102.06(11) . . Y S O1 Ag 133.41(11) . . Y S O2 Ag 124.07(10) . 3_666 Y F1 C99 F2 108.4(2) . . Y F1 C99 F3 107.9(2) . . Y F2 C99 F3 106.6(2) . . Y F1 C99 S 111.6(2) . . Y F2 C99 S 111.03(19) . . Y F3 C99 S 111.21(18) . . Y _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.625 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.095 ##################END data_silvia #(complex 12 in the MS) _database_code_CSD 176351 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H33 Ag F3 Fe O3 P S Se2' _chemical_formula_weight 1015.34 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 Orthorrombic _symmetry_space_group_name_H-M Pna21 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' _cell_length_a 24.083(8) _cell_length_b 16.552(5) _cell_length_c 9.808(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3910(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 52 _cell_measurement_theta_min 6 _cell_measurement_theta_max 12.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 2.881 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.2768 _exptl_absorpt_correction_T_max 0.3920 _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-P4 _diffrn_measurement_method theta-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 247 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6484 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4068 _reflns_number_gt 3467 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _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^)+(0.0545P)^2^+50.2083P] 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 0.39(2) _refine_ls_number_reflns 4068 _refine_ls_number_parameters 478 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1567 _refine_ls_wR_factor_gt 0.1363 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.039 _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 0.12323(4) 0.24364(6) 0.09073(15) 0.0339(3) Uani 1 1 d . . . Se1 Se 0.13255(5) 0.40538(8) 0.03867(17) 0.0362(4) Uani 1 1 d . . . Se2 Se 0.06766(5) 0.22722(7) 0.32167(18) 0.0332(3) Uani 1 1 d . . . P P 0.19688(13) 0.1523(2) 0.0160(4) 0.0321(8) Uani 1 1 d . . . Fe Fe 0.06349(7) 0.42914(11) 0.3390(3) 0.0349(5) Uani 1 1 d . . . C1 C 0.1321(5) 0.4484(9) 0.2279(18) 0.036(3) Uani 1 1 d U . . C2 C 0.1090(6) 0.5247(9) 0.268(2) 0.045(3) Uani 1 1 d U . . H2 H 0.0960 0.5660 0.2090 0.054 Uiso 1 1 calc R . . C3 C 0.1091(8) 0.5273(11) 0.413(2) 0.055(4) Uani 1 1 d U . . H3 H 0.0962 0.5707 0.4681 0.066 Uiso 1 1 calc R . . C4 C 0.1326(6) 0.4511(10) 0.463(2) 0.050(4) Uani 1 1 d U . . H4 H 0.1377 0.4362 0.5559 0.060 Uiso 1 1 calc R . . C5 C 0.1464(5) 0.4039(8) 0.3476(18) 0.038(3) Uani 1 1 d U . . H5 H 0.1623 0.3514 0.3493 0.046 Uiso 1 1 calc R . . C6 C 0.0220(4) 0.3224(7) 0.3359(19) 0.028(2) Uani 1 1 d U . . C7 C 0.0057(5) 0.3724(8) 0.2192(18) 0.036(3) Uani 1 1 d U . . H7 H 0.0101 0.3593 0.1255 0.043 Uiso 1 1 calc R . . C8 C -0.0179(6) 0.4448(9) 0.274(2) 0.048(4) Uani 1 1 d U . . H8 H -0.0317 0.4890 0.2222 0.057 Uiso 1 1 calc R . . C9 C -0.0170(7) 0.4389(10) 0.423(2) 0.055(4) Uani 1 1 d U . . H9 H -0.0306 0.4783 0.4851 0.066 Uiso 1 1 calc R . . C10 C 0.0077(6) 0.3642(10) 0.4583(19) 0.044(3) Uani 1 1 d U . . H10 H 0.0137 0.3450 0.5484 0.053 Uiso 1 1 calc R . . C11 C 0.2099(5) 0.4240(7) -0.0056(17) 0.034(3) Uani 1 1 d U . . C12 C 0.2454(6) 0.4699(9) 0.069(2) 0.043(3) Uani 1 1 d U . . H12 H 0.2324 0.4940 0.1515 0.052 Uiso 1 1 calc R . . C13 C 0.2998(6) 0.4826(10) 0.030(2) 0.052(4) Uani 1 1 d U . . H13 H 0.3241 0.5142 0.0847 0.062 Uiso 1 1 calc R . . C14 C 0.3187(7) 0.4477(10) -0.094(2) 0.052(4) Uani 1 1 d U . . H14 H 0.3556 0.4564 -0.1245 0.063 Uiso 1 1 calc R . . C15 C 0.2827(6) 0.4013(9) -0.169(2) 0.049(3) Uani 1 1 d U . . H15 H 0.2957 0.3760 -0.2495 0.059 Uiso 1 1 calc R . . C16 C 0.2280(7) 0.3902(9) -0.1293(18) 0.044(3) Uani 1 1 d U . . H16 H 0.2031 0.3603 -0.1851 0.052 Uiso 1 1 calc R . . C21 C 0.0155(5) 0.1397(8) 0.2981(19) 0.039(3) Uani 1 1 d U . . C22 C -0.0259(6) 0.1426(9) 0.202(2) 0.046(4) Uani 1 1 d U . . H22 H -0.0312 0.1906 0.1505 0.055 Uiso 1 1 calc R . . C23 C -0.0609(7) 0.0753(10) 0.179(2) 0.053(4) Uani 1 1 d U . . H23 H -0.0912 0.0791 0.1169 0.064 Uiso 1 1 calc R . . C24 C -0.0502(7) 0.0037(10) 0.247(2) 0.056(4) Uani 1 1 d U . . H24 H -0.0711 -0.0434 0.2259 0.068 Uiso 1 1 calc R . . C25 C -0.0078(7) 0.0005(9) 0.349(3) 0.056(4) Uani 1 1 d U . . H25 H -0.0017 -0.0479 0.3985 0.067 Uiso 1 1 calc R . . C26 C 0.0243(6) 0.0679(9) 0.3746(19) 0.043(3) Uani 1 1 d U . . H26 H 0.0521 0.0663 0.4432 0.052 Uiso 1 1 calc R . . C31 C 0.2614(5) 0.1583(7) 0.1189(15) 0.031(3) Uani 1 1 d U . . C32 C 0.2880(5) 0.2338(7) 0.1223(19) 0.037(3) Uani 1 1 d U . . H32 H 0.2737 0.2778 0.0710 0.045 Uiso 1 1 calc R . . C33 C 0.3363(5) 0.2440(9) 0.2024(19) 0.039(3) Uani 1 1 d U . . H33 H 0.3537 0.2954 0.2076 0.047 Uiso 1 1 calc R . . C34 C 0.3585(6) 0.1780(9) 0.2743(18) 0.043(3) Uani 1 1 d U . . H34 H 0.3919 0.1839 0.3249 0.051 Uiso 1 1 calc R . . C35 C 0.3311(6) 0.1040(9) 0.271(2) 0.050(4) Uani 1 1 d U . . H35 H 0.3454 0.0597 0.3214 0.061 Uiso 1 1 calc R . . C36 C 0.2826(5) 0.0940(8) 0.1938(19) 0.039(3) Uani 1 1 d U . . H36 H 0.2641 0.0432 0.1927 0.047 Uiso 1 1 calc R . . C41 C 0.2185(5) 0.1722(8) -0.160(2) 0.034(3) Uani 1 1 d U . . C42 C 0.2735(6) 0.1695(9) -0.2065(17) 0.039(3) Uani 1 1 d U . . H42 H 0.3025 0.1573 -0.1442 0.047 Uiso 1 1 calc R . . C43 C 0.2865(7) 0.1844(10) -0.3439(19) 0.050(4) Uani 1 1 d U . . H43 H 0.3239 0.1832 -0.3740 0.060 Uiso 1 1 calc R . . C44 C 0.2436(7) 0.2009(9) -0.436(2) 0.051(4) Uani 1 1 d U . . H44 H 0.2518 0.2103 -0.5293 0.061 Uiso 1 1 calc R . . C45 C 0.1882(6) 0.2037(10) -0.390(2) 0.049(4) Uani 1 1 d U . . H45 H 0.1592 0.2160 -0.4521 0.059 Uiso 1 1 calc R . . C46 C 0.1756(6) 0.1887(9) -0.2531(18) 0.041(3) Uani 1 1 d U . . H46 H 0.1381 0.1896 -0.2231 0.049 Uiso 1 1 calc R . . C51 C 0.1774(6) 0.0455(8) 0.0131(18) 0.038(3) Uani 1 1 d U . . C52 C 0.1257(5) 0.0222(8) 0.0719(16) 0.034(3) Uani 1 1 d U . . H52 H 0.1026 0.0614 0.1143 0.041 Uiso 1 1 calc R . . C53 C 0.1092(7) -0.0593(9) 0.0662(19) 0.051(4) Uani 1 1 d U . . H53 H 0.0752 -0.0759 0.1066 0.061 Uiso 1 1 calc R . . C54 C 0.1430(7) -0.1154(9) 0.001(2) 0.049(4) Uani 1 1 d U . . H54 H 0.1314 -0.1703 -0.0025 0.059 Uiso 1 1 calc R . . C55 C 0.1937(7) -0.0935(8) -0.059(2) 0.047(4) Uani 1 1 d U . . H55 H 0.2160 -0.1328 -0.1036 0.057 Uiso 1 1 calc R . . C56 C 0.2104(6) -0.0132(8) -0.0527(17) 0.037(3) Uani 1 1 d U . . H56 H 0.2446 0.0025 -0.0933 0.045 Uiso 1 1 calc R . . S S 0.02015(15) 0.2621(3) -0.1742(6) 0.0505(10) Uani 1 1 d . . . O1 O 0.0406(5) 0.2219(9) -0.0544(15) 0.063(4) Uani 1 1 d . . . O2 O 0.0371(7) 0.2174(11) -0.2990(18) 0.089(5) Uani 1 1 d . . . O3 O 0.0250(7) 0.3456(8) -0.182(3) 0.119(8) Uani 1 1 d . . . C100 C -0.0539(8) 0.2411(10) -0.175(3) 0.063(6) Uani 1 1 d . . . F1 F -0.0778(6) 0.2814(9) -0.0621(18) 0.098(5) Uani 1 1 d . . . F2 F -0.0772(5) 0.2728(8) -0.2906(16) 0.083(4) Uani 1 1 d . . . F3 F -0.0674(4) 0.1673(6) -0.165(2) 0.074(3) 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 0.0279(4) 0.0316(5) 0.0423(5) -0.0044(6) 0.0019(5) 0.0044(4) Se1 0.0320(6) 0.0286(6) 0.0480(9) 0.0026(7) -0.0024(7) -0.0020(5) Se2 0.0289(6) 0.0322(6) 0.0384(7) 0.0024(7) -0.0012(7) 0.0019(5) P 0.0268(15) 0.0276(16) 0.042(2) -0.0043(17) 0.0009(17) 0.0053(13) Fe 0.0279(9) 0.0290(9) 0.0479(13) -0.0070(11) 0.0048(10) 0.0004(7) C1 0.025(6) 0.031(7) 0.053(7) -0.007(6) 0.004(7) -0.005(5) C2 0.034(7) 0.030(6) 0.071(9) -0.007(7) 0.007(8) -0.010(5) C3 0.053(10) 0.040(8) 0.070(9) -0.018(8) 0.012(10) -0.004(7) C4 0.034(8) 0.058(9) 0.059(8) -0.016(7) -0.005(8) -0.003(7) C5 0.024(6) 0.040(7) 0.051(8) 0.000(6) 0.005(7) -0.001(5) C6 0.012(5) 0.027(5) 0.044(7) 0.004(6) 0.003(6) -0.005(4) C7 0.030(6) 0.031(6) 0.046(7) 0.007(6) 0.001(7) -0.001(5) C8 0.025(7) 0.030(6) 0.089(10) 0.005(7) -0.018(8) 0.000(5) C9 0.041(9) 0.042(8) 0.082(10) -0.018(8) 0.036(9) 0.009(6) C10 0.042(8) 0.042(8) 0.048(7) -0.006(7) 0.011(8) 0.000(6) C11 0.037(6) 0.014(5) 0.051(8) 0.012(5) 0.012(6) -0.003(5) C12 0.036(6) 0.041(7) 0.053(10) -0.008(7) -0.001(6) 0.004(5) C13 0.034(6) 0.049(9) 0.073(11) -0.009(9) 0.002(8) -0.001(6) C14 0.041(7) 0.052(9) 0.064(11) 0.005(8) 0.009(7) 0.003(6) C15 0.047(7) 0.048(8) 0.052(9) 0.001(8) 0.009(7) 0.011(6) C16 0.052(7) 0.035(7) 0.044(8) 0.004(6) 0.006(7) -0.001(6) C21 0.029(6) 0.030(6) 0.059(10) 0.001(7) 0.012(6) 0.002(5) C22 0.050(8) 0.032(6) 0.055(10) 0.008(8) 0.001(7) -0.004(6) C23 0.061(9) 0.050(8) 0.049(10) -0.008(7) 0.003(8) -0.016(7) C24 0.059(9) 0.036(7) 0.074(13) -0.008(8) 0.021(8) -0.021(7) C25 0.062(9) 0.028(6) 0.078(13) 0.008(8) 0.022(8) 0.003(6) C26 0.035(7) 0.043(7) 0.053(10) 0.006(7) 0.006(6) 0.010(5) C31 0.036(6) 0.026(5) 0.031(8) -0.003(5) 0.006(6) 0.003(4) C32 0.035(6) 0.016(5) 0.061(10) -0.010(6) 0.001(6) 0.008(4) C33 0.030(6) 0.034(6) 0.054(9) -0.006(7) 0.006(6) 0.001(5) C34 0.038(7) 0.046(7) 0.044(9) -0.005(7) -0.009(7) -0.005(5) C35 0.042(7) 0.035(6) 0.075(13) 0.002(8) -0.011(8) 0.007(6) C36 0.032(6) 0.024(6) 0.062(10) 0.000(7) -0.004(7) -0.001(5) C41 0.034(6) 0.026(6) 0.042(7) 0.001(7) -0.001(6) 0.001(5) C42 0.036(6) 0.037(7) 0.044(7) -0.002(7) -0.005(6) -0.002(6) C43 0.045(7) 0.052(9) 0.054(9) 0.001(9) 0.010(6) 0.000(7) C44 0.054(7) 0.049(8) 0.050(9) 0.009(9) -0.004(6) -0.015(7) C45 0.045(6) 0.059(9) 0.044(8) 0.001(9) -0.006(7) -0.003(7) C46 0.034(6) 0.040(8) 0.049(8) -0.012(7) -0.006(6) 0.001(6) C51 0.033(6) 0.031(6) 0.050(10) -0.002(7) 0.003(6) -0.001(5) C52 0.028(5) 0.032(5) 0.042(9) 0.023(7) -0.008(6) 0.003(5) C53 0.056(8) 0.044(7) 0.052(11) -0.001(8) 0.001(8) -0.013(6) C54 0.058(8) 0.029(6) 0.060(12) 0.006(7) -0.015(7) -0.008(5) C55 0.060(8) 0.025(6) 0.057(11) -0.001(7) -0.006(8) 0.000(6) C56 0.038(7) 0.033(6) 0.040(9) -0.015(7) 0.003(6) -0.001(5) S 0.0342(17) 0.066(3) 0.051(2) 0.016(3) -0.009(2) -0.0032(17) O1 0.047(7) 0.085(9) 0.057(8) 0.012(8) -0.027(7) -0.015(6) O2 0.093(11) 0.110(13) 0.065(10) 0.000(11) 0.010(10) 0.046(10) O3 0.122(12) 0.059(8) 0.18(2) 0.028(13) -0.089(16) -0.039(9) C100 0.069(11) 0.045(9) 0.076(13) 0.009(11) -0.047(12) -0.019(8) F1 0.094(10) 0.090(9) 0.110(13) -0.009(10) 0.035(10) 0.027(8) F2 0.074(7) 0.080(8) 0.096(10) 0.006(8) -0.057(8) 0.013(6) F3 0.063(5) 0.051(5) 0.106(9) -0.002(7) -0.020(8) -0.018(5) _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 2.443(3) . y Ag O1 2.473(12) . y Ag Se2 2.645(2) . y Ag Se1 2.7347(18) . y Se1 C11 1.937(13) . y Se1 C1 1.988(17) . y Se2 C6 1.926(12) . y Se2 C21 1.932(13) . y P C51 1.830(13) . ? P C41 1.831(19) . ? P C31 1.855(14) . ? Fe C1 2.006(15) . ? Fe C6 2.031(11) . ? Fe C5 2.041(13) . ? Fe C2 2.046(16) . ? Fe C7 2.049(15) . ? Fe C8 2.078(14) . ? Fe C10 2.081(17) . ? Fe C3 2.092(18) . ? Fe C4 2.095(17) . ? Fe C9 2.113(15) . ? C1 C5 1.43(2) . ? C1 C2 1.44(2) . ? C2 C3 1.42(3) . ? C3 C4 1.47(3) . ? C4 C5 1.42(2) . ? C6 C10 1.43(2) . ? C6 C7 1.47(2) . ? C7 C8 1.43(2) . ? C8 C9 1.47(3) . ? C9 C10 1.42(2) . ? C11 C12 1.36(2) . ? C11 C16 1.41(2) . ? C12 C13 1.38(2) . ? C13 C14 1.42(3) . ? C14 C15 1.37(2) . ? C15 C16 1.39(2) . ? C21 C22 1.37(2) . ? C21 C26 1.42(2) . ? C22 C23 1.42(2) . ? C23 C24 1.39(3) . ? C24 C25 1.43(3) . ? C25 C26 1.38(2) . ? C31 C36 1.39(2) . ? C31 C32 1.406(17) . ? C32 C33 1.41(2) . ? C33 C34 1.41(2) . ? C34 C35 1.39(2) . ? C35 C36 1.40(2) . ? C41 C42 1.40(2) . ? C41 C46 1.41(2) . ? C42 C43 1.41(2) . ? C43 C44 1.40(2) . ? C44 C45 1.41(2) . ? C45 C46 1.40(3) . ? C51 C56 1.411(19) . ? C51 C52 1.426(19) . ? C52 C53 1.408(19) . ? C53 C54 1.39(2) . ? C54 C55 1.40(2) . ? C55 C56 1.392(19) . ? S O3 1.389(14) . ? S O1 1.438(14) . ? S O2 1.487(17) . ? S C100 1.817(18) . ? C100 F3 1.269(18) . ? C100 F2 1.37(2) . ? C100 F1 1.42(3) . ? 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 108.7(4) . . y P Ag Se2 124.12(11) . . y O1 Ag Se2 94.1(4) . . y P Ag Se1 119.34(10) . . y O1 Ag Se1 95.8(3) . . y Se2 Ag Se1 107.58(6) . . y C11 Se1 C1 99.0(6) . . y C11 Se1 Ag 106.1(3) . . y C1 Se1 Ag 100.1(4) . . y C6 Se2 C21 104.5(5) . . y C6 Se2 Ag 105.5(5) . . y C21 Se2 Ag 107.7(5) . . y C51 P C41 103.4(7) . . ? C51 P C31 105.9(6) . . ? C41 P C31 105.4(6) . . ? C51 P Ag 114.6(5) . . y C41 P Ag 112.2(4) . . y C31 P Ag 114.3(4) . . y C1 Fe C6 122.4(6) . . ? C1 Fe C5 41.3(6) . . ? C6 Fe C5 107.7(5) . . ? C1 Fe C2 41.5(6) . . ? C6 Fe C2 158.7(7) . . ? C5 Fe C2 69.4(6) . . ? C1 Fe C7 108.7(6) . . ? C6 Fe C7 42.1(6) . . ? C5 Fe C7 126.4(6) . . ? C2 Fe C7 121.6(7) . . ? C1 Fe C8 126.1(7) . . ? C6 Fe C8 68.9(5) . . ? C5 Fe C8 163.8(8) . . ? C2 Fe C8 107.7(7) . . ? C7 Fe C8 40.6(6) . . ? C1 Fe C10 156.9(6) . . ? C6 Fe C10 40.6(7) . . ? C5 Fe C10 120.2(7) . . ? C2 Fe C10 159.4(7) . . ? C7 Fe C10 69.3(6) . . ? C8 Fe C10 68.2(7) . . ? C1 Fe C3 68.5(7) . . ? C6 Fe C3 160.0(8) . . ? C5 Fe C3 68.4(6) . . ? C2 Fe C3 40.2(7) . . ? C7 Fe C3 155.8(7) . . ? C8 Fe C3 120.4(7) . . ? C10 Fe C3 123.0(8) . . ? C1 Fe C4 68.5(7) . . ? C6 Fe C4 123.5(7) . . ? C5 Fe C4 40.0(7) . . ? C2 Fe C4 68.7(8) . . ? C7 Fe C4 162.3(6) . . ? C8 Fe C4 155.1(7) . . ? C10 Fe C4 106.0(8) . . ? C3 Fe C4 41.0(7) . . ? C1 Fe C9 163.0(7) . . ? C6 Fe C9 67.7(6) . . ? C5 Fe C9 153.8(8) . . ? C2 Fe C9 124.4(6) . . ? C7 Fe C9 68.7(7) . . ? C8 Fe C9 41.0(8) . . ? C10 Fe C9 39.4(7) . . ? C3 Fe C9 106.7(7) . . ? C4 Fe C9 119.3(8) . . ? C5 C1 C2 108.7(15) . . ? C5 C1 Se1 125.5(10) . . y C2 C1 Se1 125.1(13) . . y C5 C1 Fe 70.7(8) . . ? C2 C1 Fe 70.7(9) . . ? Se1 C1 Fe 117.0(7) . . y C3 C2 C1 107.5(17) . . ? C3 C2 Fe 71.6(11) . . ? C1 C2 Fe 67.8(8) . . ? C2 C3 C4 108.0(17) . . ? C2 C3 Fe 68.2(11) . . ? C4 C3 Fe 69.6(9) . . ? C5 C4 C3 107.3(17) . . ? C5 C4 Fe 67.9(9) . . ? C3 C4 Fe 69.4(10) . . ? C4 C5 C1 108.5(12) . . ? C4 C5 Fe 72.0(8) . . ? C1 C5 Fe 68.0(8) . . ? C10 C6 C7 108.6(11) . . ? C10 C6 Se2 126.5(12) . . y C7 C6 Se2 123.9(12) . . y C10 C6 Fe 71.6(8) . . ? C7 C6 Fe 69.6(7) . . ? Se2 C6 Fe 115.6(5) . . ? C8 C7 C6 106.7(15) . . ? C8 C7 Fe 70.8(9) . . ? C6 C7 Fe 68.3(8) . . ? C7 C8 C9 108.2(15) . . ? C7 C8 Fe 68.6(8) . . ? C9 C8 Fe 70.8(10) . . ? C10 C9 C8 107.9(15) . . ? C10 C9 Fe 69.1(9) . . ? C8 C9 Fe 68.2(9) . . ? C9 C10 C6 108.6(16) . . ? C9 C10 Fe 71.5(10) . . ? C6 C10 Fe 67.8(8) . . ? C12 C11 C16 119.6(14) . . ? C12 C11 Se1 124.9(12) . . y C16 C11 Se1 115.3(11) . . y C11 C12 C13 122.0(17) . . ? C12 C13 C14 118.7(16) . . ? C15 C14 C13 119.0(15) . . ? C14 C15 C16 121.8(18) . . ? C15 C16 C11 118.8(16) . . ? C22 C21 C26 120.0(13) . . ? C22 C21 Se2 121.9(11) . . y C26 C21 Se2 117.9(12) . . y C21 C22 C23 121.1(15) . . ? C24 C23 C22 119.0(17) . . ? C23 C24 C25 120.1(15) . . ? C26 C25 C24 119.9(16) . . ? C25 C26 C21 119.7(16) . . ? C36 C31 C32 120.0(13) . . ? C36 C31 P 123.6(10) . . ? C32 C31 P 116.3(10) . . ? C31 C32 C33 119.7(13) . . ? C34 C33 C32 119.9(13) . . ? C35 C34 C33 119.4(14) . . ? C34 C35 C36 120.9(15) . . ? C31 C36 C35 120.0(13) . . ? C42 C41 C46 119.2(16) . . ? C42 C41 P 124.8(12) . . ? C46 C41 P 116.0(11) . . ? C41 C42 C43 121.2(15) . . ? C44 C43 C42 119.3(15) . . ? C43 C44 C45 119.9(17) . . ? C46 C45 C44 120.5(16) . . ? C45 C46 C41 120.0(15) . . ? C56 C51 C52 119.5(12) . . ? C56 C51 P 121.8(11) . . ? C52 C51 P 118.6(10) . . ? C53 C52 C51 119.3(13) . . ? C54 C53 C52 119.5(15) . . ? C53 C54 C55 122.1(14) . . ? C56 C55 C54 118.7(15) . . ? C55 C56 C51 121.0(14) . . ? O3 S O1 118.6(12) . . ? O3 S O2 115.1(14) . . ? O1 S O2 110.3(8) . . ? O3 S C100 105.8(9) . . ? O1 S C100 104.7(9) . . ? O2 S C100 99.7(11) . . ? S O1 Ag 132.7(8) . . y F3 C100 F2 109.3(16) . . ? F3 C100 F1 107(2) . . ? F2 C100 F1 107.5(14) . . ? F3 C100 S 115.8(13) . . ? F2 C100 S 109.6(16) . . ? F1 C100 S 107.6(12) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.208 _refine_diff_density_min -1.569 _refine_diff_density_rms 0.159 ##############END