Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Victorio Cadierno' _publ_contact_author_address ; Departamento de Quimica Organica e Inorganica Universidad de Oviedo Facultad de Quimica Oviedo 33071 SPAIN ; _publ_contact_author_email VCM@UNIOVI.ES _publ_section_title ; Silver(I) complexes of N-thiophosphorylated bis(iminophosphorane) ligands: From monomers to polymers ; loop_ _publ_author_name _publ_author_address 'Victorio Cadierno' ; Departamento de Quimica Organica e Inorganica Facultad de Quimica Universidad de Oviedo Avda. Julian Claveria, 8 33006 Oviedo Spain ; 'Josefina Diez' ; Departamento de Quimica Organica e Inorganica Facultad de Quimica Universidad de Oviedo Avda. Julian Claveria, 8 33006 Oviedo Spain ; 'Joaquin Garcia-Alvarez' ; Departamento de Quimica Organica e Inorganica Facultad de Quimica Universidad de Oviedo Avda. Julian Claveria, 8 33006 Oviedo Spain ; 'Jose Gimeno' ; Departamento de Quimica Organica e Inorganica Facultad de Quimica Universidad de Oviedo Avda. Julian Claveria, 8 33006 Oviedo Spain ; #========================================================================== data_1b _database_code_depnum_ccdc_archive 'CCDC 639179' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H42 N2 O4 P4 S2' _chemical_formula_sum 'C49 H42 N2 O4 P4 S2' _chemical_formula_weight 910.85 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 29.2141(9) _cell_length_b 9.1678(2) _cell_length_c 20.1846(6) _cell_angle_alpha 90.00 _cell_angle_beta 123.056(2) _cell_angle_gamma 90.00 _cell_volume 4531.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5358 _cell_measurement_theta_min 0.883 _cell_measurement_theta_max 70.076 _exptl_crystal_description Prismatic _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 2.777 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.758 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_process_details 'Sortav (Blessing 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95 mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17433 _diffrn_reflns_av_R_equivalents 0.067 _diffrn_reflns_av_sigmaI/netI 0.0835 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 69.52 _reflns_number_total 4120 _reflns_number_gt 2642 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collet (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowki & Minor 1997)' _computing_data_reduction 'HKL Denzo and scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2006)' _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. ; _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^)+(0.0386P)^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 4120 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1139 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _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 C1 C 0.0000 0.1381(5) 0.2500 0.0432(10) Uani 1 2 d S . . C2 C 0.09106(12) 0.1244(3) 0.23222(17) 0.0435(7) Uani 1 1 d . . . C3 C 0.14618(15) 0.0903(4) 0.2779(2) 0.0599(9) Uani 1 1 d . . . C4 C 0.1700(2) 0.0126(5) 0.2456(3) 0.0795(12) Uani 1 1 d . . . C5 C 0.1390(2) -0.0302(5) 0.1679(3) 0.0818(14) Uani 1 1 d . . . C6 C 0.0848(2) 0.0036(4) 0.1217(2) 0.0690(11) Uani 1 1 d . . . C7 C 0.06035(16) 0.0784(4) 0.1536(2) 0.0562(9) Uani 1 1 d . . . C8 C 0.04664(12) 0.4093(3) 0.23042(17) 0.0405(7) Uani 1 1 d . . . C9 C 0.00914(14) 0.4278(4) 0.14928(19) 0.0512(8) Uani 1 1 d . . . C10 C -0.00300(15) 0.5666(4) 0.1169(2) 0.0598(9) Uani 1 1 d . . . C11 C 0.02210(15) 0.6863(4) 0.1638(2) 0.0636(10) Uani 1 1 d . . . C12 C 0.05937(15) 0.6699(4) 0.2441(2) 0.0627(10) Uani 1 1 d . . . C13 C 0.07149(14) 0.5311(4) 0.2773(2) 0.0525(8) Uani 1 1 d . . . C14 C 0.12736(13) 0.3725(3) 0.52890(17) 0.0466(7) Uani 1 1 d . . . C15 C 0.15596(15) 0.4669(4) 0.5110(2) 0.0556(9) Uani 1 1 d . . . C16 C 0.16406(17) 0.6088(4) 0.5389(2) 0.0682(11) Uani 1 1 d . . . C17 C 0.14462(19) 0.6545(5) 0.5833(2) 0.0758(12) Uani 1 1 d . . . C18 C 0.11721(19) 0.5597(5) 0.6014(2) 0.0748(12) Uani 1 1 d . . . C19 C 0.10816(16) 0.4162(4) 0.5744(2) 0.0589(9) Uani 1 1 d . . . C20 C 0.22610(12) 0.0808(4) 0.55111(18) 0.0500(8) Uani 1 1 d . . . C21 C 0.24564(15) -0.0524(4) 0.5462(2) 0.0682(11) Uani 1 1 d . . . C22 C 0.28252(18) -0.1257(5) 0.6158(3) 0.0887(15) Uani 1 1 d . . . C23 C 0.29787(18) -0.0661(6) 0.6872(3) 0.0862(15) Uani 1 1 d . . . C24 C 0.27840(17) 0.0678(7) 0.6911(2) 0.0839(14) Uani 1 1 d . . . C25 C 0.24218(15) 0.1422(5) 0.6222(2) 0.0669(11) Uani 1 1 d . . . N1 N 0.10303(10) 0.2538(3) 0.36739(13) 0.0427(6) Uani 1 1 d . . . O1 O 0.19006(8) 0.1577(2) 0.48087(11) 0.0480(5) Uani 1 1 d . . . O2 O 0.11630(8) 0.2267(2) 0.50356(11) 0.0477(5) Uani 1 1 d . . . P1 P 0.06232(3) 0.23225(8) 0.27568(4) 0.03776(19) Uani 1 1 d . . . P2 P 0.12521(3) 0.14825(8) 0.44059(4) 0.0415(2) Uani 1 1 d . . . S1 S 0.09814(4) -0.04861(9) 0.42856(5) 0.0585(3) Uani 1 1 d . . . H15 H 0.1673(13) 0.435(3) 0.4778(18) 0.055(10) Uiso 1 1 d . . . H1A H 0.0093(12) 0.080(3) 0.2905(15) 0.048(9) Uiso 1 1 d . . . H18 H 0.1040(14) 0.588(4) 0.631(2) 0.072(12) Uiso 1 1 d . . . H11 H 0.0126(14) 0.784(4) 0.138(2) 0.075(11) Uiso 1 1 d . . . H19 H 0.0858(13) 0.345(4) 0.5832(18) 0.063(10) Uiso 1 1 d . . . H6 H 0.0638(14) -0.031(4) 0.065(2) 0.078(12) Uiso 1 1 d . . . H3 H 0.1649(12) 0.117(3) 0.3301(17) 0.048(9) Uiso 1 1 d . . . H9 H -0.0091(13) 0.343(4) 0.1159(18) 0.063(10) Uiso 1 1 d . . . H13 H 0.0947(13) 0.522(3) 0.3344(19) 0.059(10) Uiso 1 1 d . . . H21 H 0.2350(14) -0.090(4) 0.496(2) 0.073(12) Uiso 1 1 d . . . H16 H 0.1835(14) 0.667(4) 0.525(2) 0.069(12) Uiso 1 1 d . . . H24 H 0.2862(16) 0.101(4) 0.741(2) 0.091(14) Uiso 1 1 d . . . H25 H 0.2281(14) 0.230(4) 0.625(2) 0.074(12) Uiso 1 1 d . . . H7 H 0.0194(14) 0.095(3) 0.1216(19) 0.068(11) Uiso 1 1 d . . . H5 H 0.1555(17) -0.073(4) 0.148(2) 0.096(15) Uiso 1 1 d . . . H17 H 0.1493(15) 0.752(4) 0.598(2) 0.084(13) Uiso 1 1 d . . . H12 H 0.0744(16) 0.757(4) 0.279(2) 0.094(13) Uiso 1 1 d . . . H10 H -0.0261(15) 0.578(4) 0.065(2) 0.082(13) Uiso 1 1 d . . . H22 H 0.2962(17) -0.220(5) 0.614(2) 0.106(16) Uiso 1 1 d . . . H23 H 0.322(2) -0.131(6) 0.732(3) 0.16(2) Uiso 1 1 d . . . H4 H 0.209(2) -0.014(5) 0.280(3) 0.120(17) Uiso 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 C1 0.050(3) 0.037(2) 0.044(2) 0.000 0.026(2) 0.000 C2 0.0517(18) 0.0409(17) 0.0473(17) 0.0002(14) 0.0331(15) -0.0012(14) C3 0.053(2) 0.073(3) 0.060(2) -0.0040(19) 0.0346(19) 0.0060(18) C4 0.069(3) 0.090(3) 0.095(3) -0.007(3) 0.055(3) 0.012(2) C5 0.107(4) 0.069(3) 0.110(4) -0.013(3) 0.085(4) 0.004(3) C6 0.095(3) 0.061(2) 0.069(3) -0.017(2) 0.057(3) -0.008(2) C7 0.063(2) 0.055(2) 0.054(2) -0.0091(17) 0.0339(19) -0.0051(18) C8 0.0410(16) 0.0381(16) 0.0452(17) 0.0024(13) 0.0252(14) -0.0023(13) C9 0.057(2) 0.048(2) 0.0465(18) 0.0041(16) 0.0261(16) -0.0042(16) C10 0.054(2) 0.061(2) 0.055(2) 0.0174(19) 0.0230(18) 0.0046(18) C11 0.061(2) 0.049(2) 0.082(3) 0.018(2) 0.040(2) 0.0063(18) C12 0.063(2) 0.0401(19) 0.078(3) -0.0007(19) 0.034(2) -0.0041(17) C13 0.054(2) 0.0459(19) 0.052(2) 0.0006(16) 0.0253(17) -0.0026(15) C14 0.0515(18) 0.0481(19) 0.0358(15) 0.0019(14) 0.0209(14) 0.0035(15) C15 0.067(2) 0.050(2) 0.052(2) -0.0051(16) 0.0343(19) -0.0055(17) C16 0.077(3) 0.054(2) 0.064(2) -0.0083(19) 0.032(2) -0.010(2) C17 0.092(3) 0.053(2) 0.061(2) -0.012(2) 0.028(2) 0.007(2) C18 0.087(3) 0.082(3) 0.055(2) -0.008(2) 0.038(2) 0.021(2) C19 0.067(2) 0.066(2) 0.0472(19) -0.0003(17) 0.0338(18) 0.0079(19) C20 0.0410(17) 0.060(2) 0.0437(18) 0.0065(15) 0.0200(15) -0.0049(15) C21 0.053(2) 0.066(3) 0.062(2) -0.006(2) 0.0165(19) 0.0014(19) C22 0.061(3) 0.064(3) 0.091(3) 0.006(3) 0.009(2) 0.007(2) C23 0.053(3) 0.100(4) 0.075(3) 0.031(3) 0.015(2) -0.001(3) C24 0.059(2) 0.129(4) 0.048(2) 0.005(3) 0.019(2) 0.005(3) C25 0.051(2) 0.091(3) 0.046(2) 0.000(2) 0.0187(17) 0.009(2) N1 0.0469(14) 0.0441(14) 0.0354(12) -0.0005(11) 0.0215(11) -0.0049(12) O1 0.0398(11) 0.0594(14) 0.0413(11) 0.0067(10) 0.0198(9) -0.0007(10) O2 0.0567(13) 0.0488(13) 0.0450(11) 0.0000(10) 0.0326(10) -0.0058(10) P1 0.0385(4) 0.0379(4) 0.0364(4) -0.0002(3) 0.0201(3) -0.0003(3) P2 0.0415(4) 0.0417(4) 0.0376(4) -0.0003(3) 0.0192(3) -0.0033(3) S1 0.0570(5) 0.0416(5) 0.0574(5) 0.0042(4) 0.0187(4) -0.0057(4) _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 C1 P1 1.816(2) . ? C1 P1 1.816(2) 2 ? C1 H1A 0.88(2) . ? C2 C3 1.386(4) . ? C2 C7 1.396(4) . ? C2 P1 1.804(3) . ? C3 C4 1.382(5) . ? C3 H3 0.92(3) . ? C4 C5 1.374(6) . ? C4 H4 0.98(5) . ? C5 C6 1.366(6) . ? C5 H5 0.87(4) . ? C6 C7 1.377(5) . ? C6 H6 1.00(4) . ? C7 H7 1.02(3) . ? C8 C13 1.387(4) . ? C8 C9 1.398(4) . ? C8 P1 1.795(3) . ? C9 C10 1.386(4) . ? C9 H9 0.97(3) . ? C10 C11 1.372(5) . ? C10 H10 0.89(4) . ? C11 C12 1.381(5) . ? C11 H11 1.00(3) . ? C12 C13 1.391(4) . ? C12 H12 0.99(4) . ? C13 H13 0.97(3) . ? C14 C19 1.371(4) . ? C14 C15 1.381(4) . ? C14 O2 1.405(4) . ? C15 C16 1.386(5) . ? C15 H15 0.94(3) . ? C16 C17 1.362(6) . ? C16 H16 0.92(3) . ? C17 C18 1.360(6) . ? C17 H17 0.93(4) . ? C18 C19 1.393(5) . ? C18 H18 0.91(3) . ? C19 H19 1.01(3) . ? C20 C25 1.364(5) . ? C20 C21 1.375(5) . ? C20 O1 1.410(3) . ? C21 C22 1.391(5) . ? C21 H21 0.95(3) . ? C22 C23 1.369(7) . ? C22 H22 0.97(4) . ? C23 C24 1.374(7) . ? C23 H23 0.98(5) . ? C24 C25 1.383(5) . ? C24 H24 0.95(4) . ? C25 H25 0.92(3) . ? N1 P1 1.574(2) . ? N1 P2 1.579(2) . ? O1 P2 1.605(2) . ? O2 P2 1.601(2) . ? P2 S1 1.9319(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 C1 P1 123.2(2) . 2 ? P1 C1 H1A 105.4(19) . . ? P1 C1 H1A 107.7(19) 2 . ? C3 C2 C7 118.8(3) . . ? C3 C2 P1 118.7(2) . . ? C7 C2 P1 122.5(3) . . ? C4 C3 C2 120.2(4) . . ? C4 C3 H3 123(2) . . ? C2 C3 H3 117.0(19) . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4 122(3) . . ? C3 C4 H4 118(3) . . ? C6 C5 C4 120.7(4) . . ? C6 C5 H5 121(3) . . ? C4 C5 H5 118(3) . . ? C5 C6 C7 119.9(4) . . ? C5 C6 H6 118(2) . . ? C7 C6 H6 122(2) . . ? C6 C7 C2 120.4(4) . . ? C6 C7 H7 120.7(18) . . ? C2 C7 H7 118.7(18) . . ? C13 C8 C9 119.1(3) . . ? C13 C8 P1 119.2(2) . . ? C9 C8 P1 121.7(2) . . ? C10 C9 C8 120.0(3) . . ? C10 C9 H9 120.1(19) . . ? C8 C9 H9 119.9(19) . . ? C11 C10 C9 120.4(3) . . ? C11 C10 H10 120(2) . . ? C9 C10 H10 120(3) . . ? C10 C11 C12 120.4(3) . . ? C10 C11 H11 118(2) . . ? C12 C11 H11 122(2) . . ? C11 C12 C13 119.7(4) . . ? C11 C12 H12 120(2) . . ? C13 C12 H12 120(2) . . ? C8 C13 C12 120.4(3) . . ? C8 C13 H13 120.3(19) . . ? C12 C13 H13 119.0(19) . . ? C19 C14 C15 121.3(3) . . ? C19 C14 O2 115.1(3) . . ? C15 C14 O2 123.5(3) . . ? C14 C15 C16 118.3(4) . . ? C14 C15 H15 119.4(19) . . ? C16 C15 H15 122.2(19) . . ? C17 C16 C15 121.1(4) . . ? C17 C16 H16 124(2) . . ? C15 C16 H16 115(2) . . ? C18 C17 C16 119.9(4) . . ? C18 C17 H17 122(2) . . ? C16 C17 H17 118(2) . . ? C17 C18 C19 120.8(4) . . ? C17 C18 H18 121(2) . . ? C19 C18 H18 118(2) . . ? C14 C19 C18 118.6(4) . . ? C14 C19 H19 118.0(18) . . ? C18 C19 H19 123.2(18) . . ? C25 C20 C21 121.6(3) . . ? C25 C20 O1 119.4(3) . . ? C21 C20 O1 118.9(3) . . ? C20 C21 C22 118.7(4) . . ? C20 C21 H21 119(2) . . ? C22 C21 H21 122(2) . . ? C23 C22 C21 119.9(5) . . ? C23 C22 H22 120(3) . . ? C21 C22 H22 120(3) . . ? C22 C23 C24 120.6(4) . . ? C22 C23 H23 112(3) . . ? C24 C23 H23 127(3) . . ? C23 C24 C25 119.8(5) . . ? C23 C24 H24 119(3) . . ? C25 C24 H24 121(3) . . ? C20 C25 C24 119.4(4) . . ? C20 C25 H25 121(2) . . ? C24 C25 H25 120(2) . . ? P1 N1 P2 133.20(16) . . ? C20 O1 P2 120.66(18) . . ? C14 O2 P2 127.74(18) . . ? N1 P1 C8 107.73(13) . . ? N1 P1 C2 112.76(14) . . ? C8 P1 C2 107.77(13) . . ? N1 P1 C1 113.07(9) . . ? C8 P1 C1 110.29(15) . . ? C2 P1 C1 105.11(14) . . ? N1 P2 O2 107.82(12) . . ? N1 P2 O1 102.07(12) . . ? O2 P2 O1 103.41(11) . . ? N1 P2 S1 121.58(10) . . ? O2 P2 S1 106.68(9) . . ? O1 P2 S1 113.78(9) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 69.52 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.324 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.062 #==END #========================================================================== data_7a _database_code_depnum_ccdc_archive 'CCDC 639180' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H84 Ag2 N4 O8 P8 S4, 2(F6 Sb1)' _chemical_formula_sum 'C66 H84 Ag2 F12 N4 O8 P8 S4 Sb2' _chemical_formula_weight 2124.61 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.0562 5.8946 '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 11.1280(11) _cell_length_b 11.3219(9) _cell_length_c 18.1350(2) _cell_angle_alpha 87.206(6) _cell_angle_beta 77.029(9) _cell_angle_gamma 70.753(7) _cell_volume 2101.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4614 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.175 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 11.774 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.446 _exptl_absorpt_correction_T_max 0.772 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95 mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40313 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_av_sigmaI/netI 0.0773 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 58.97 _reflns_number_total 6029 _reflns_number_gt 5304 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collet (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowki & Minor 1997)' _computing_data_reduction 'HKL Denzo and scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2006)' _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. ; _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^)+(0.0706P)^2^+4.6127P] 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 6029 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1582 _refine_ls_wR_factor_gt 0.1034 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _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 C1 C 0.4385(5) 0.4181(5) 0.2641(3) 0.0248(12) Uani 1 1 d . . . H1A H 0.4867 0.3710 0.3003 0.030 Uiso 1 1 calc R . . H1B H 0.4449 0.3594 0.2250 0.030 Uiso 1 1 calc R . . C2 C 0.2315(7) 0.3659(6) 0.3759(3) 0.0331(14) Uani 1 1 d . . . C3 C 0.3215(7) 0.2505(6) 0.3837(4) 0.0440(17) Uani 1 1 d . . . H3 H 0.4068 0.2304 0.3557 0.053 Uiso 1 1 calc R . . C4 C 0.2851(8) 0.1646(7) 0.4332(4) 0.0506(19) Uani 1 1 d . . . H4 H 0.3460 0.0873 0.4385 0.061 Uiso 1 1 calc R . . C5 C 0.1586(8) 0.1944(7) 0.4744(4) 0.0448(17) Uani 1 1 d . . . H5 H 0.1339 0.1375 0.5079 0.054 Uiso 1 1 calc R . . C6 C 0.0693(8) 0.3080(7) 0.4658(4) 0.0436(17) Uani 1 1 d . . . H6 H -0.0163 0.3277 0.4934 0.052 Uiso 1 1 calc R . . C7 C 0.1044(6) 0.3928(6) 0.4172(4) 0.0322(14) Uani 1 1 d . . . H7 H 0.0424 0.4694 0.4118 0.039 Uiso 1 1 calc R . . C8 C 0.2491(6) 0.6158(6) 0.3692(3) 0.0282(13) Uani 1 1 d . . . C9 C 0.3096(7) 0.5981(7) 0.4306(4) 0.0391(15) Uani 1 1 d . . . H9 H 0.3572 0.5179 0.4424 0.047 Uiso 1 1 calc R . . C10 C 0.2986(8) 0.6996(7) 0.4734(4) 0.0476(18) Uani 1 1 d . . . H10 H 0.3397 0.6880 0.5138 0.057 Uiso 1 1 calc R . . C11 C 0.2269(8) 0.8184(7) 0.4569(4) 0.0504(19) Uani 1 1 d . . . H11 H 0.2207 0.8867 0.4858 0.060 Uiso 1 1 calc R . . C12 C 0.1644(8) 0.8367(7) 0.3975(4) 0.0488(19) Uani 1 1 d . . . H12 H 0.1145 0.9169 0.3872 0.059 Uiso 1 1 calc R . . C13 C 0.1758(6) 0.7353(6) 0.3533(3) 0.0336(14) Uani 1 1 d . . . H13 H 0.1344 0.7476 0.3130 0.040 Uiso 1 1 calc R . . C14 C 0.0423(8) 0.2599(7) 0.2236(4) 0.0517(19) Uani 1 1 d . . . H14A H 0.0712 0.2487 0.1690 0.062 Uiso 1 1 calc R . . H14B H -0.0495 0.2680 0.2374 0.062 Uiso 1 1 calc R . . C15 C 0.1192(12) 0.1507(8) 0.2611(5) 0.080(3) Uani 1 1 d . . . H15A H 0.1081 0.0759 0.2455 0.120 Uiso 1 1 calc R . . H15B H 0.0894 0.1621 0.3150 0.120 Uiso 1 1 calc R . . H15C H 0.2099 0.1434 0.2471 0.120 Uiso 1 1 calc R . . C16 C -0.0851(7) 0.6291(7) 0.2013(4) 0.0469(18) Uani 1 1 d . . . H16A H -0.0697 0.6627 0.2452 0.056 Uiso 1 1 calc R . . H16B H -0.1424 0.5802 0.2190 0.056 Uiso 1 1 calc R . . C17 C -0.1488(7) 0.7349(7) 0.1543(4) 0.0468(18) Uani 1 1 d . . . H17A H -0.1644 0.7013 0.1111 0.070 Uiso 1 1 calc R . . H17B H -0.0923 0.7839 0.1376 0.070 Uiso 1 1 calc R . . H17C H -0.2302 0.7869 0.1843 0.070 Uiso 1 1 calc R . . C18 C 0.5834(6) 0.5774(6) 0.2919(3) 0.0297(13) Uani 1 1 d . . . C19 C 0.6748(7) 0.4887(7) 0.3244(4) 0.0394(16) Uani 1 1 d . . . H19 H 0.7004 0.4045 0.3106 0.047 Uiso 1 1 calc R . . C20 C 0.7275(8) 0.5267(9) 0.3777(4) 0.057(2) Uani 1 1 d . . . H20 H 0.7904 0.4679 0.3987 0.069 Uiso 1 1 calc R . . C21 C 0.6877(10) 0.6497(9) 0.3995(5) 0.066(3) Uani 1 1 d . . . H21 H 0.7227 0.6743 0.4358 0.080 Uiso 1 1 calc R . . C22 C 0.5968(10) 0.7368(9) 0.3683(5) 0.064(3) Uani 1 1 d . . . H22 H 0.5702 0.8204 0.3837 0.076 Uiso 1 1 calc R . . C23 C 0.5430(8) 0.7027(7) 0.3136(4) 0.0493(19) Uani 1 1 d . . . H23 H 0.4815 0.7626 0.2922 0.059 Uiso 1 1 calc R . . C24 C 0.6584(5) 0.4406(6) 0.1500(3) 0.0273(13) Uani 1 1 d . . . C25 C 0.7069(7) 0.3110(6) 0.1478(4) 0.0375(15) Uani 1 1 d . . . H25 H 0.6638 0.2654 0.1812 0.045 Uiso 1 1 calc R . . C26 C 0.8202(8) 0.2500(7) 0.0956(4) 0.0471(18) Uani 1 1 d . . . H26 H 0.8545 0.1631 0.0946 0.057 Uiso 1 1 calc R . . C27 C 0.8810(7) 0.3168(7) 0.0461(4) 0.0454(17) Uani 1 1 d . . . H27 H 0.9567 0.2747 0.0110 0.054 Uiso 1 1 calc R . . C28 C 0.8335(6) 0.4452(7) 0.0465(4) 0.0405(17) Uani 1 1 d . . . H28 H 0.8768 0.4897 0.0123 0.049 Uiso 1 1 calc R . . C29 C 0.7211(6) 0.5073(6) 0.0982(3) 0.0348(15) Uani 1 1 d . . . H29 H 0.6870 0.5941 0.0983 0.042 Uiso 1 1 calc R . . C30 C 0.4924(13) 0.9335(10) 0.0933(7) 0.092(4) Uani 1 1 d . . . H30A H 0.5269 0.9092 0.0402 0.110 Uiso 1 1 calc R . . H30B H 0.4024 0.9870 0.0988 0.110 Uiso 1 1 calc R . . C31 C 0.5620(15) 1.0013(10) 0.1139(7) 0.110(5) Uani 1 1 d . . . H31A H 0.5558 1.0731 0.0827 0.165 Uiso 1 1 calc R . . H31B H 0.6518 0.9500 0.1075 0.165 Uiso 1 1 calc R . . H31C H 0.5271 1.0282 0.1660 0.165 Uiso 1 1 calc R . . C32 C 0.1437(7) 0.8485(7) 0.1449(4) 0.0465(17) Uani 1 1 d . . . H32A H 0.0764 0.8659 0.1912 0.056 Uiso 1 1 calc R . . H32B H 0.1560 0.7656 0.1261 0.056 Uiso 1 1 calc R . . C33 C 0.1004(9) 0.9430(7) 0.0872(5) 0.060(2) Uani 1 1 d . . . H33A H 0.0202 0.9394 0.0777 0.089 Uiso 1 1 calc R . . H33B H 0.1661 0.9249 0.0410 0.089 Uiso 1 1 calc R . . H33C H 0.0870 1.0252 0.1059 0.089 Uiso 1 1 calc R . . Ag1 Ag 0.36402(5) 0.50271(5) 0.04968(3) 0.0463(2) Uani 1 1 d . . . F1 F 0.6625(6) 0.2071(4) 0.3335(3) 0.0808(16) Uani 1 1 d . . . F2 F 0.6233(6) 0.0124(7) 0.2866(4) 0.102(2) Uani 1 1 d . . . F3 F 0.6574(6) 0.0200(5) 0.4229(2) 0.0738(15) Uani 1 1 d . . . F4 F 0.8461(6) 0.0529(5) 0.2312(3) 0.0855(18) Uani 1 1 d . . . F5 F 0.8778(5) 0.0602(6) 0.3701(3) 0.0900(18) Uani 1 1 d . . . F6 F 0.8431(7) -0.1356(5) 0.3209(4) 0.103(2) Uani 1 1 d . . . N1 N 0.1740(5) 0.5303(5) 0.2558(3) 0.0309(11) Uani 1 1 d . . . N2 N 0.4168(5) 0.6418(5) 0.1908(3) 0.0349(12) Uani 1 1 d . . . O1 O 0.0616(5) 0.3721(4) 0.2481(2) 0.0388(11) Uani 1 1 d . . . O2 O 0.0382(4) 0.5495(4) 0.1561(2) 0.0343(10) Uani 1 1 d . . . O3 O 0.2632(4) 0.8512(4) 0.1609(2) 0.0380(10) Uani 1 1 d . . . O4 O 0.4945(5) 0.8214(5) 0.1366(3) 0.0463(12) Uani 1 1 d . . . P1 P 0.26739(14) 0.48415(13) 0.31217(8) 0.0235(3) Uani 1 1 d . . . P2 P 0.13781(15) 0.45275(14) 0.19806(8) 0.0285(4) Uani 1 1 d . . . P3 P 0.51739(15) 0.52905(13) 0.22090(8) 0.0258(3) Uani 1 1 d . . . P4 P 0.39734(16) 0.74832(14) 0.13262(9) 0.0307(4) Uani 1 1 d . . . S1 S 0.28194(17) 0.34510(15) 0.11879(9) 0.0386(4) Uani 1 1 d . . . S2 S 0.41339(16) 0.69831(15) 0.02541(9) 0.0377(4) Uani 1 1 d . . . Sb1 Sb 0.75190(4) 0.03564(4) 0.32711(2) 0.03921(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 C1 0.021(3) 0.027(3) 0.023(3) 0.001(2) -0.003(2) -0.005(2) C2 0.050(4) 0.033(3) 0.021(3) -0.002(2) -0.011(3) -0.016(3) C3 0.037(4) 0.041(4) 0.046(4) 0.005(3) 0.002(3) -0.010(3) C4 0.065(5) 0.029(4) 0.050(4) 0.013(3) -0.007(4) -0.010(3) C5 0.061(5) 0.049(4) 0.029(4) 0.008(3) -0.002(3) -0.030(4) C6 0.055(4) 0.048(4) 0.030(4) 0.003(3) 0.000(3) -0.027(4) C7 0.017(3) 0.035(3) 0.038(4) 0.001(3) 0.005(3) -0.007(3) C8 0.033(3) 0.040(4) 0.013(3) -0.003(2) 0.002(2) -0.017(3) C9 0.048(4) 0.046(4) 0.028(3) -0.001(3) -0.009(3) -0.020(3) C10 0.060(5) 0.061(5) 0.032(4) -0.003(3) -0.015(3) -0.029(4) C11 0.073(5) 0.048(4) 0.032(4) -0.012(3) -0.003(4) -0.026(4) C12 0.067(5) 0.031(4) 0.042(4) -0.005(3) 0.000(4) -0.015(4) C13 0.040(4) 0.033(3) 0.027(3) 0.001(3) -0.005(3) -0.013(3) C14 0.057(5) 0.061(5) 0.050(4) -0.010(4) -0.008(4) -0.037(4) C15 0.138(10) 0.048(5) 0.059(6) 0.000(4) -0.021(6) -0.038(6) C16 0.041(4) 0.062(5) 0.026(3) -0.013(3) -0.002(3) -0.003(4) C17 0.035(4) 0.053(4) 0.056(5) 0.011(4) -0.023(3) -0.011(3) C18 0.031(3) 0.042(4) 0.021(3) 0.004(3) -0.004(2) -0.020(3) C19 0.042(4) 0.055(4) 0.029(3) 0.007(3) -0.012(3) -0.024(3) C20 0.065(5) 0.098(7) 0.032(4) 0.018(4) -0.023(4) -0.050(5) C21 0.098(7) 0.089(7) 0.051(5) 0.010(5) -0.031(5) -0.073(6) C22 0.097(7) 0.070(6) 0.043(5) -0.015(4) -0.008(5) -0.056(6) C23 0.062(5) 0.047(4) 0.046(4) -0.007(3) 0.001(4) -0.034(4) C24 0.021(3) 0.044(4) 0.018(3) -0.002(2) -0.005(2) -0.012(3) C25 0.045(4) 0.034(4) 0.030(3) 0.000(3) -0.008(3) -0.010(3) C26 0.055(5) 0.039(4) 0.038(4) -0.005(3) -0.013(3) 0.001(3) C27 0.035(4) 0.065(5) 0.030(4) -0.005(3) -0.002(3) -0.012(4) C28 0.033(4) 0.066(5) 0.027(3) -0.003(3) 0.005(3) -0.027(4) C29 0.042(4) 0.047(4) 0.021(3) 0.003(3) -0.008(3) -0.021(3) C30 0.138(10) 0.085(7) 0.109(8) 0.070(7) -0.084(8) -0.084(7) C31 0.190(14) 0.078(7) 0.128(10) 0.059(7) -0.105(10) -0.091(9) C32 0.048(4) 0.041(4) 0.042(4) -0.009(3) 0.000(3) -0.009(3) C33 0.067(5) 0.046(4) 0.056(5) -0.005(4) -0.035(4) 0.008(4) Ag1 0.0539(4) 0.0496(3) 0.0379(3) 0.0035(2) -0.0092(2) -0.0211(3) F1 0.099(4) 0.039(3) 0.080(4) 0.009(2) 0.001(3) -0.006(3) F2 0.082(4) 0.150(6) 0.087(4) -0.015(4) -0.044(3) -0.038(4) F3 0.099(4) 0.073(3) 0.038(2) 0.009(2) 0.001(2) -0.025(3) F4 0.101(4) 0.092(4) 0.035(3) 0.009(2) 0.005(3) -0.008(3) F5 0.057(3) 0.130(5) 0.084(4) -0.016(3) -0.031(3) -0.019(3) F6 0.145(6) 0.044(3) 0.089(4) -0.009(3) -0.008(4) 0.000(3) N1 0.041(3) 0.028(3) 0.026(3) -0.004(2) -0.007(2) -0.013(2) N2 0.041(3) 0.036(3) 0.025(3) 0.003(2) -0.007(2) -0.010(2) O1 0.053(3) 0.043(3) 0.027(2) -0.0036(19) -0.002(2) -0.028(2) O2 0.032(2) 0.047(3) 0.023(2) -0.0044(18) -0.0075(18) -0.010(2) O3 0.045(3) 0.031(2) 0.035(2) -0.0042(19) -0.014(2) -0.004(2) O4 0.065(3) 0.048(3) 0.042(3) 0.020(2) -0.027(2) -0.033(3) P1 0.0262(8) 0.0253(7) 0.0192(7) -0.0004(6) -0.0035(6) -0.0096(6) P2 0.0331(8) 0.0315(8) 0.0226(8) -0.0021(6) -0.0064(6) -0.0124(7) P3 0.0307(8) 0.0272(8) 0.0203(7) 0.0010(6) -0.0051(6) -0.0112(6) P4 0.0343(9) 0.0296(8) 0.0286(8) 0.0053(6) -0.0079(7) -0.0109(7) S1 0.0461(10) 0.0373(9) 0.0265(8) -0.0093(6) 0.0007(7) -0.0103(7) S2 0.0416(9) 0.0372(9) 0.0281(8) 0.0024(6) -0.0022(7) -0.0085(7) Sb1 0.0489(3) 0.0344(3) 0.0302(3) 0.00075(19) -0.0098(2) -0.0075(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 C1 P3 1.812(6) . ? C1 P1 1.824(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.383(9) . ? C2 C7 1.384(9) . ? C2 P1 1.812(6) . ? C3 C4 1.388(10) . ? C3 H3 0.9300 . ? C4 C5 1.375(11) . ? C4 H4 0.9300 . ? C5 C6 1.369(10) . ? C5 H5 0.9300 . ? C6 C7 1.364(9) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.386(9) . ? C8 C9 1.400(9) . ? C8 P1 1.786(6) . ? C9 C10 1.374(10) . ? C9 H9 0.9300 . ? C10 C11 1.377(11) . ? C10 H10 0.9300 . ? C11 C12 1.380(11) . ? C11 H11 0.9300 . ? C12 C13 1.387(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O1 1.461(8) . ? C14 C15 1.486(12) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 O2 1.456(8) . ? C16 C17 1.509(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C23 1.387(10) . ? C18 C19 1.389(9) . ? C18 P3 1.804(6) . ? C19 C20 1.389(10) . ? C19 H19 0.9300 . ? C20 C21 1.364(13) . ? C20 H20 0.9300 . ? C21 C22 1.365(13) . ? C21 H21 0.9300 . ? C22 C23 1.395(11) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.385(9) . ? C24 C29 1.387(9) . ? C24 P3 1.817(6) . ? C25 C26 1.384(10) . ? C25 H25 0.9300 . ? C26 C27 1.355(11) . ? C26 H26 0.9300 . ? C27 C28 1.374(11) . ? C27 H27 0.9300 . ? C28 C29 1.377(9) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.371(13) . ? C30 O4 1.455(9) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 O3 1.433(9) . ? C32 C33 1.50(1) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? Ag1 S1 2.4355(18) . ? Ag1 S2 2.4492(17) . ? Ag1 S2 2.8707(17) 2_665 ? Ag1 Ag1 3.1385(11) 2_665 ? F1 Sb1 1.862(5) . ? F2 Sb1 1.843(5) . ? F3 Sb1 1.851(4) . ? F4 Sb1 1.856(5) . ? F5 Sb1 1.848(5) . ? F6 Sb1 1.864(5) . ? N1 P1 1.570(5) . ? N1 P2 1.594(5) . ? N2 P4 1.556(5) . ? N2 P3 1.563(5) . ? O1 P2 1.569(4) . ? O2 P2 1.582(4) . ? O3 P4 1.555(5) . ? O4 P4 1.578(5) . ? P2 S1 1.993(2) . ? P4 S2 2.004(2) . ? S2 Ag1 2.8707(17) 2_665 ? 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 P3 C1 P1 116.1(3) . . ? P3 C1 H1A 108.3 . . ? P1 C1 H1A 108.3 . . ? P3 C1 H1B 108.3 . . ? P1 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? C3 C2 C7 118.7(6) . . ? C3 C2 P1 124.2(5) . . ? C7 C2 P1 117.1(5) . . ? C2 C3 C4 120.4(7) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.7(7) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C6 C5 C4 119.8(6) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C7 C6 C5 120.7(7) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C2 120.6(6) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? C13 C8 C9 119.6(6) . . ? C13 C8 P1 120.7(5) . . ? C9 C8 P1 119.7(5) . . ? C10 C9 C8 119.8(7) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 120.4(7) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C12 120.3(7) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C13 119.9(7) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C8 C13 C12 119.9(6) . . ? C8 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? O1 C14 C15 108.2(6) . . ? O1 C14 H14A 110.0 . . ? C15 C14 H14A 110.0 . . ? O1 C14 H14B 110.0 . . ? C15 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C16 C17 109.8(6) . . ? O2 C16 H16A 109.7 . . ? C17 C16 H16A 109.7 . . ? O2 C16 H16B 109.7 . . ? C17 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 120.4(6) . . ? C23 C18 P3 120.0(5) . . ? C19 C18 P3 119.6(5) . . ? C20 C19 C18 119.4(7) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C21 C20 C19 120.4(8) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 120.2(7) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 121.2(8) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C18 C23 C22 118.4(8) . . ? C18 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C25 C24 C29 119.7(6) . . ? C25 C24 P3 122.6(5) . . ? C29 C24 P3 117.7(5) . . ? C26 C25 C24 119.4(6) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C27 C26 C25 120.0(7) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 121.5(6) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C27 C28 C29 119.2(6) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C28 C29 C24 120.2(6) . . ? C28 C29 H29 119.9 . . ? C24 C29 H29 119.9 . . ? C31 C30 O4 114.8(8) . . ? C31 C30 H30A 108.6 . . ? O4 C30 H30A 108.6 . . ? C31 C30 H30B 108.6 . . ? O4 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O3 C32 C33 111.3(6) . . ? O3 C32 H32A 109.4 . . ? C33 C32 H32A 109.4 . . ? O3 C32 H32B 109.4 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? S1 Ag1 S2 159.21(6) . . ? S1 Ag1 S2 87.74(5) . 2_665 ? S2 Ag1 S2 108.19(5) . 2_665 ? S1 Ag1 Ag1 133.91(5) . 2_665 ? S2 Ag1 Ag1 60.34(4) . 2_665 ? S2 Ag1 Ag1 47.85(4) 2_665 2_665 ? P1 N1 P2 130.2(3) . . ? P4 N2 P3 146.0(4) . . ? C14 O1 P2 126.4(4) . . ? C16 O2 P2 118.5(4) . . ? C32 O3 P4 123.6(4) . . ? C30 O4 P4 121.4(5) . . ? N1 P1 C8 107.8(3) . . ? N1 P1 C2 114.0(3) . . ? C8 P1 C2 107.2(3) . . ? N1 P1 C1 112.8(3) . . ? C8 P1 C1 108.6(3) . . ? C2 P1 C1 106.2(3) . . ? O1 P2 O2 106.9(3) . . ? O1 P2 N1 105.9(2) . . ? O2 P2 N1 107.6(3) . . ? O1 P2 S1 110.28(19) . . ? O2 P2 S1 107.38(17) . . ? N1 P2 S1 118.2(2) . . ? N2 P3 C18 112.2(3) . . ? N2 P3 C1 109.8(3) . . ? C18 P3 C1 107.3(3) . . ? N2 P3 C24 115.6(3) . . ? C18 P3 C24 105.3(3) . . ? C1 P3 C24 106.1(3) . . ? O3 P4 N2 109.5(3) . . ? O3 P4 O4 101.3(3) . . ? N2 P4 O4 108.0(3) . . ? O3 P4 S2 109.28(18) . . ? N2 P4 S2 116.8(2) . . ? O4 P4 S2 110.7(2) . . ? P2 S1 Ag1 100.35(8) . . ? P4 S2 Ag1 98.52(8) . . ? P4 S2 Ag1 120.27(9) . 2_665 ? Ag1 S2 Ag1 71.81(5) . 2_665 ? F2 Sb1 F5 178.5(3) . . ? F2 Sb1 F3 89.2(3) . . ? F5 Sb1 F3 89.4(3) . . ? F2 Sb1 F4 90.9(3) . . ? F5 Sb1 F4 90.4(3) . . ? F3 Sb1 F4 179.5(2) . . ? F2 Sb1 F1 89.1(3) . . ? F5 Sb1 F1 90.4(3) . . ? F3 Sb1 F1 89.4(2) . . ? F4 Sb1 F1 90.1(2) . . ? F2 Sb1 F6 91.5(3) . . ? F5 Sb1 F6 89.0(3) . . ? F3 Sb1 F6 90.8(3) . . ? F4 Sb1 F6 89.7(3) . . ? F1 Sb1 F6 179.4(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 C2 C3 C4 -1.1(11) . . . . ? P1 C2 C3 C4 -179.1(6) . . . . ? C2 C3 C4 C5 0.3(12) . . . . ? C3 C4 C5 C6 0.5(12) . . . . ? C4 C5 C6 C7 -0.5(11) . . . . ? C5 C6 C7 C2 -0.4(10) . . . . ? C3 C2 C7 C6 1.1(10) . . . . ? P1 C2 C7 C6 179.3(5) . . . . ? C13 C8 C9 C10 -1.6(9) . . . . ? P1 C8 C9 C10 178.3(5) . . . . ? C8 C9 C10 C11 0.8(11) . . . . ? C9 C10 C11 C12 0.7(11) . . . . ? C10 C11 C12 C13 -1.4(11) . . . . ? C9 C8 C13 C12 0.8(9) . . . . ? P1 C8 C13 C12 -179.0(5) . . . . ? C11 C12 C13 C8 0.6(10) . . . . ? C23 C18 C19 C20 -1.4(10) . . . . ? P3 C18 C19 C20 178.5(5) . . . . ? C18 C19 C20 C21 1.6(11) . . . . ? C19 C20 C21 C22 -0.9(12) . . . . ? C20 C21 C22 C23 -0.2(13) . . . . ? C19 C18 C23 C22 0.3(10) . . . . ? P3 C18 C23 C22 -179.6(5) . . . . ? C21 C22 C23 C18 0.5(12) . . . . ? C29 C24 C25 C26 2.3(9) . . . . ? P3 C24 C25 C26 -175.4(5) . . . . ? C24 C25 C26 C27 -1.5(10) . . . . ? C25 C26 C27 C28 0.5(11) . . . . ? C26 C27 C28 C29 -0.4(11) . . . . ? C27 C28 C29 C24 1.3(10) . . . . ? C25 C24 C29 C28 -2.3(9) . . . . ? P3 C24 C29 C28 175.6(5) . . . . ? C15 C14 O1 P2 111.0(7) . . . . ? C17 C16 O2 P2 165.4(5) . . . . ? C33 C32 O3 P4 -106.4(6) . . . . ? C31 C30 O4 P4 167.0(10) . . . . ? P2 N1 P1 C8 -172.7(4) . . . . ? P2 N1 P1 C2 -53.9(5) . . . . ? P2 N1 P1 C1 67.4(5) . . . . ? C13 C8 P1 N1 -7.8(6) . . . . ? C9 C8 P1 N1 172.3(5) . . . . ? C13 C8 P1 C2 -130.9(5) . . . . ? C9 C8 P1 C2 49.2(6) . . . . ? C13 C8 P1 C1 114.7(5) . . . . ? C9 C8 P1 C1 -65.1(5) . . . . ? C3 C2 P1 N1 125.3(6) . . . . ? C7 C2 P1 N1 -52.8(6) . . . . ? C3 C2 P1 C8 -115.6(6) . . . . ? C7 C2 P1 C8 66.4(5) . . . . ? C3 C2 P1 C1 0.4(6) . . . . ? C7 C2 P1 C1 -177.7(5) . . . . ? P3 C1 P1 N1 74.0(4) . . . . ? P3 C1 P1 C8 -45.5(4) . . . . ? P3 C1 P1 C2 -160.4(3) . . . . ? C14 O1 P2 O2 85.4(6) . . . . ? C14 O1 P2 N1 -160.1(6) . . . . ? C14 O1 P2 S1 -31.1(6) . . . . ? C16 O2 P2 O1 53.9(5) . . . . ? C16 O2 P2 N1 -59.5(5) . . . . ? C16 O2 P2 S1 172.2(4) . . . . ? P1 N1 P2 O1 65.8(5) . . . . ? P1 N1 P2 O2 179.9(4) . . . . ? P1 N1 P2 S1 -58.4(5) . . . . ? P4 N2 P3 C18 86.6(7) . . . . ? P4 N2 P3 C1 -154.2(6) . . . . ? P4 N2 P3 C24 -34.2(8) . . . . ? C23 C18 P3 N2 0.2(6) . . . . ? C19 C18 P3 N2 -179.7(5) . . . . ? C23 C18 P3 C1 -120.6(5) . . . . ? C19 C18 P3 C1 59.6(5) . . . . ? C23 C18 P3 C24 126.7(5) . . . . ? C19 C18 P3 C24 -53.2(5) . . . . ? P1 C1 P3 N2 -33.5(4) . . . . ? P1 C1 P3 C18 88.7(4) . . . . ? P1 C1 P3 C24 -159.1(3) . . . . ? C25 C24 P3 N2 -137.0(5) . . . . ? C29 C24 P3 N2 45.3(6) . . . . ? C25 C24 P3 C18 98.6(5) . . . . ? C29 C24 P3 C18 -79.2(5) . . . . ? C25 C24 P3 C1 -15.0(6) . . . . ? C29 C24 P3 C1 167.2(5) . . . . ? C32 O3 P4 N2 -87.8(5) . . . . ? C32 O3 P4 O4 158.2(5) . . . . ? C32 O3 P4 S2 41.3(5) . . . . ? P3 N2 P4 O3 -159.5(6) . . . . ? P3 N2 P4 O4 -49.9(7) . . . . ? P3 N2 P4 S2 75.6(7) . . . . ? C30 O4 P4 O3 -59.7(8) . . . . ? C30 O4 P4 N2 -174.8(8) . . . . ? C30 O4 P4 S2 56.1(8) . . . . ? O1 P2 S1 Ag1 176.3(2) . . . . ? O2 P2 S1 Ag1 60.10(19) . . . . ? N1 P2 S1 Ag1 -61.8(2) . . . . ? S2 Ag1 S1 P2 26.9(2) . . . . ? S2 Ag1 S1 P2 167.84(8) 2_665 . . . ? Ag1 Ag1 S1 P2 153.81(6) 2_665 . . . ? O3 P4 S2 Ag1 -101.5(2) . . . . ? N2 P4 S2 Ag1 23.5(3) . . . . ? O4 P4 S2 Ag1 147.7(2) . . . . ? O3 P4 S2 Ag1 -175.35(19) . . . 2_665 ? N2 P4 S2 Ag1 -50.3(3) . . . 2_665 ? O4 P4 S2 Ag1 73.9(2) . . . 2_665 ? S1 Ag1 S2 P4 19.3(2) . . . . ? S2 Ag1 S2 P4 -119.16(8) 2_665 . . . ? Ag1 Ag1 S2 P4 -119.16(8) 2_665 . . . ? S1 Ag1 S2 Ag1 138.46(17) . . . 2_665 ? S2 Ag1 S2 Ag1 0.0 2_665 . . 2_665 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 58.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.157 _refine_diff_density_min -0.825 _refine_diff_density_rms 0.141 #==END #========================================================================== data_8b _database_code_depnum_ccdc_archive 'CCDC 639181' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C50 H44 Ag N2 O4 P4 S2), 2(F6 Sb), C H2 Cl2' _chemical_formula_sum 'C101 H90 Ag2 Cl2 F12 N4 O8 P8 S4 Sb2' _chemical_formula_weight 2621.91 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.0562 5.8946 '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 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 25.8436(10) _cell_length_b 10.8312(5) _cell_length_c 20.3081(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.556(5) _cell_angle_gamma 90.00 _cell_volume 5356.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8760 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2620 _exptl_absorpt_coefficient_mu 9.821 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95 mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90615 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 68.43 _reflns_number_total 9770 _reflns_number_gt 8972 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collet (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowki & Minor 1997)' _computing_data_reduction 'HKL Denzo and scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2006)' _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. A dichlorometane solvent molecule was found to be disordered over two positions related by the crystallographic symmetry operation (1-x, y, 1/2-z), with 0.5 site occupancy factors. Bond distances between C and Cl atoms in the dichlorometane molecule of solvation were restrained to a target value of 1.6(0.02) A. The anisotropic displacement parameters of this solvent molecule were constrained to be equal. Some terminal atoms of a phenyl group (atoms C4, C5 and C6)showed quite large displacement ellipsoids and were finally constrained to have equal ansisotropic displacement parameters. ; _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^)+(0.0696P)^2^+15.4293P] 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 9764 _refine_ls_number_parameters 634 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1206 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.046 _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 C1 C 0.24884(17) 0.3893(4) 0.3372(2) 0.0354(10) Uani 1 1 d . . . H1A H 0.2395 0.4763 0.3343 0.042 Uiso 1 1 calc R . . H1B H 0.2405 0.3581 0.2900 0.042 Uiso 1 1 calc R . . C2 C 0.21405(16) 0.3198(4) 0.3737(2) 0.0326(9) Uani 1 1 d . . . H2A H 0.2217 0.3530 0.4204 0.039 Uiso 1 1 calc R . . H2B H 0.2245 0.2333 0.3782 0.039 Uiso 1 1 calc R . . C3 C 0.35793(18) 0.4582(5) 0.3382(3) 0.0386(10) Uani 1 1 d . . . C4 C 0.4122(3) 0.4308(8) 0.3489(5) 0.0911(17) Uani 1 1 d . . . H4 H 0.4288 0.3641 0.3768 0.109 Uiso 1 1 calc R . . C5 C 0.4420(3) 0.5036(7) 0.3178(5) 0.0911(17) Uani 1 1 d . . . H5 H 0.4790 0.4871 0.3264 0.109 Uiso 1 1 calc R . . C6 C 0.4174(3) 0.5990(8) 0.2748(5) 0.0911(17) Uani 1 1 d . . . H6 H 0.4374 0.6460 0.2534 0.109 Uiso 1 1 calc R . . C7 C 0.3639(2) 0.6251(5) 0.2633(3) 0.0518(13) Uani 1 1 d . . . H7 H 0.3472 0.6898 0.2338 0.062 Uiso 1 1 calc R . . C8 C 0.33357(19) 0.5562(5) 0.2952(3) 0.0402(11) Uani 1 1 d . . . H8 H 0.2970 0.5758 0.2876 0.048 Uiso 1 1 calc R . . C9 C 0.33967(16) 0.2103(4) 0.3811(2) 0.0343(9) Uani 1 1 d . . . C10 C 0.34951(18) 0.1369(4) 0.4404(2) 0.0354(10) Uani 1 1 d . . . H10 H 0.3463 0.1705 0.4809 0.042 Uiso 1 1 calc R . . C11 C 0.3642(2) 0.0135(4) 0.4391(3) 0.0430(11) Uani 1 1 d . . . H11 H 0.3701 -0.0360 0.4784 0.052 Uiso 1 1 calc R . . C12 C 0.3700(2) -0.0346(5) 0.3794(3) 0.0485(12) Uani 1 1 d . . . H12 H 0.3806 -0.1165 0.3787 0.058 Uiso 1 1 calc R . . C13 C 0.3601(2) 0.0375(5) 0.3204(3) 0.0497(12) Uani 1 1 d . . . H13 H 0.3639 0.0039 0.2801 0.060 Uiso 1 1 calc R . . C14 C 0.3447(2) 0.1602(5) 0.3211(3) 0.0434(11) Uani 1 1 d . . . H14 H 0.3378 0.2085 0.2813 0.052 Uiso 1 1 calc R . . C15 C 0.3024(2) 0.5092(4) 0.5945(2) 0.0362(10) Uani 1 1 d . . . C16 C 0.2843(2) 0.6117(4) 0.6215(2) 0.0428(11) Uani 1 1 d . . . H16 H 0.3034 0.6860 0.6278 0.051 Uiso 1 1 calc R . . C17 C 0.2373(2) 0.6010(4) 0.6387(2) 0.0454(12) Uani 1 1 d . . . H17 H 0.2244 0.6690 0.6565 0.054 Uiso 1 1 calc R . . C18 C 0.2091(3) 0.4900(4) 0.6298(3) 0.0467(12) Uani 1 1 d . . . H18 H 0.1777 0.4833 0.6422 0.056 Uiso 1 1 calc R . . C19 C 0.2280(2) 0.3883(4) 0.6022(3) 0.0439(11) Uani 1 1 d . . . H19 H 0.2086 0.3144 0.5956 0.053 Uiso 1 1 calc R . . C20 C 0.2751(2) 0.3959(4) 0.5845(2) 0.0400(11) Uani 1 1 d . . . H20 H 0.2881 0.3281 0.5666 0.048 Uiso 1 1 calc R . . C21 C 0.4442(2) 0.6650(6) 0.5438(4) 0.068(2) Uani 1 1 d . . . C22 C 0.4441(3) 0.7153(8) 0.6059(5) 0.088(2) Uani 1 1 d . . . H22 H 0.4251 0.6772 0.6319 0.106 Uiso 1 1 calc R . . C23 C 0.4729(4) 0.8235(10) 0.6292(7) 0.125(4) Uani 1 1 d . . . H23 H 0.4740 0.8591 0.6713 0.150 Uiso 1 1 calc R . . C24 C 0.4996(4) 0.8769(9) 0.5888(7) 0.111(4) Uani 1 1 d . . . H24 H 0.5183 0.9505 0.6043 0.134 Uiso 1 1 calc R . . C25 C 0.5007(3) 0.8286(7) 0.5269(6) 0.089(3) Uani 1 1 d . . . H25 H 0.5196 0.8681 0.5012 0.107 Uiso 1 1 calc R . . C26 C 0.4712(3) 0.7134(8) 0.5023(5) 0.099(3) Uani 1 1 d . . . H26 H 0.4709 0.6754 0.4611 0.119 Uiso 1 1 calc R . . C27 C 0.13034(16) 0.2676(4) 0.2412(2) 0.0273(8) Uani 1 1 d . . . C28 C 0.1454(2) 0.1448(4) 0.2355(3) 0.0396(10) Uani 1 1 d . . . H28 H 0.1594 0.0963 0.2753 0.047 Uiso 1 1 calc R . . C29 C 0.1393(2) 0.0960(5) 0.1705(3) 0.0487(13) Uani 1 1 d . . . H29 H 0.1494 0.0147 0.1664 0.058 Uiso 1 1 calc R . . C30 C 0.1184(2) 0.1679(5) 0.1119(3) 0.0539(14) Uani 1 1 d . . . H30 H 0.1147 0.1349 0.0683 0.065 Uiso 1 1 calc R . . C31 C 0.1024(3) 0.2893(5) 0.1168(3) 0.0531(13) Uani 1 1 d . . . H31 H 0.0878 0.3369 0.0768 0.064 Uiso 1 1 calc R . . C32 C 0.1085(2) 0.3387(4) 0.1818(2) 0.0379(10) Uani 1 1 d . . . H32 H 0.0979 0.4197 0.1855 0.045 Uiso 1 1 calc R . . C33 C 0.10621(17) 0.2325(4) 0.3684(2) 0.0303(9) Uani 1 1 d . . . C34 C 0.13332(19) 0.1547(4) 0.4225(2) 0.0352(10) Uani 1 1 d . . . H34 H 0.1714 0.1563 0.4416 0.042 Uiso 1 1 calc R . . C35 C 0.1031(2) 0.0733(5) 0.4486(3) 0.0444(11) Uani 1 1 d . . . H35 H 0.1213 0.0205 0.4851 0.053 Uiso 1 1 calc R . . C36 C 0.0475(2) 0.0699(5) 0.4216(3) 0.0466(12) Uani 1 1 d . . . H36 H 0.0278 0.0139 0.4387 0.056 Uiso 1 1 calc R . . C37 C 0.0202(2) 0.1505(7) 0.3683(4) 0.0666(18) Uani 1 1 d . . . H37 H -0.0179 0.1489 0.3497 0.080 Uiso 1 1 calc R . . C38 C 0.0496(2) 0.2331(6) 0.3429(3) 0.0590(16) Uani 1 1 d . . . H38 H 0.0311 0.2894 0.3084 0.071 Uiso 1 1 calc R . . C39 C 0.00219(17) 0.6221(4) 0.3670(2) 0.0326(9) Uani 1 1 d . . . C40 C -0.0192(2) 0.5675(6) 0.4134(3) 0.0488(12) Uani 1 1 d . . . H40 H -0.0096 0.4874 0.4293 0.059 Uiso 1 1 calc R . . C41 C -0.0560(2) 0.6360(7) 0.4358(3) 0.0608(17) Uani 1 1 d . . . H41 H -0.0712 0.6008 0.4669 0.073 Uiso 1 1 calc R . . C42 C -0.0699(2) 0.7533(7) 0.4129(3) 0.0596(17) Uani 1 1 d . . . H42 H -0.0946 0.7975 0.4282 0.072 Uiso 1 1 calc R . . C43 C -0.0475(2) 0.8068(6) 0.3671(3) 0.0558(14) Uani 1 1 d . . . H43 H -0.0567 0.8874 0.3520 0.067 Uiso 1 1 calc R . . C44 C -0.01118(19) 0.7407(5) 0.3433(3) 0.0425(11) Uani 1 1 d . . . H44 H 0.0038 0.7760 0.3120 0.051 Uiso 1 1 calc R . . C45 C 0.14690(16) 0.7540(4) 0.3175(2) 0.0284(8) Uani 1 1 d . . . C46 C 0.17219(19) 0.8442(4) 0.3646(2) 0.0359(10) Uani 1 1 d . . . H46 H 0.1594 0.8648 0.4008 0.043 Uiso 1 1 calc R . . C47 C 0.2176(2) 0.9046(5) 0.3571(3) 0.0520(14) Uani 1 1 d . . . H47 H 0.2358 0.9651 0.3889 0.062 Uiso 1 1 calc R . . C48 C 0.2353(2) 0.8747(5) 0.3028(3) 0.0543(15) Uani 1 1 d . . . H48 H 0.2649 0.9167 0.2971 0.065 Uiso 1 1 calc R . . C49 C 0.2097(2) 0.7830(5) 0.2567(3) 0.0484(13) Uani 1 1 d . . . H49 H 0.2226 0.7626 0.2205 0.058 Uiso 1 1 calc R . . C50 C 0.16494(19) 0.7205(4) 0.2632(2) 0.0355(9) Uani 1 1 d . . . H50 H 0.1476 0.6582 0.2321 0.043 Uiso 1 1 calc R . . Ag1 Ag 0.225228(12) 0.63993(3) 0.463633(16) 0.03461(11) Uani 1 1 d . . . F1 F 0.33042(13) 0.9246(3) 0.5951(2) 0.0649(9) Uani 1 1 d . . . F2 F 0.26427(14) 0.8998(3) 0.67028(15) 0.0549(8) Uani 1 1 d . . . F3 F 0.22275(12) 0.8860(3) 0.53280(14) 0.0461(7) Uani 1 1 d . . . F4 F 0.20136(12) 1.0815(2) 0.59694(15) 0.0432(6) Uani 1 1 d . . . F5 F 0.26570(12) 1.1036(3) 0.52157(15) 0.0467(7) Uani 1 1 d . . . F6 F 0.30732(14) 1.1194(3) 0.65987(16) 0.0551(8) Uani 1 1 d . . . N1 N 0.33567(15) 0.4044(3) 0.4646(2) 0.0328(8) Uani 1 1 d . . . N2 N 0.11872(14) 0.4693(3) 0.31349(18) 0.0303(7) Uani 1 1 d . . . O1 O 0.35154(13) 0.5188(3) 0.57984(17) 0.0390(7) Uani 1 1 d . . . O2 O 0.41678(13) 0.5494(3) 0.5189(2) 0.0498(9) Uani 1 1 d . . . O3 O 0.03503(11) 0.5484(3) 0.33949(15) 0.0328(6) Uani 1 1 d . . . O4 O 0.09922(11) 0.6983(3) 0.32196(15) 0.0303(6) Uani 1 1 d . . . P1 P 0.32179(4) 0.37051(10) 0.38469(6) 0.0311(2) Uani 1 1 d . . . P2 P 0.35235(4) 0.53343(10) 0.50200(6) 0.0339(2) Uani 1 1 d . . . P3 P 0.14118(4) 0.33216(9) 0.32616(5) 0.0253(2) Uani 1 1 d . . . P4 P 0.09955(4) 0.56715(10) 0.35763(5) 0.0263(2) Uani 1 1 d . . . S1 S 0.31365(4) 0.68429(10) 0.45507(6) 0.0361(2) Uani 1 1 d . . . S2 S 0.13586(4) 0.57201(11) 0.46036(5) 0.0366(2) Uani 1 1 d . . . Sb1 Sb 0.265962(12) 1.00112(2) 0.596374(14) 0.03287(10) Uani 1 1 d . . . C51 C 0.4366(9) 0.8727(15) 0.1619(8) 0.1254(15) Uani 0.50 1 d PD A -1 H51A H 0.4028 0.8695 0.1728 0.151 Uiso 0.50 1 calc PR A -1 H51B H 0.4342 0.9447 0.1326 0.151 Uiso 0.50 1 calc PR A -1 Cl1 Cl 0.4885(4) 0.8968(4) 0.2374(2) 0.1254(15) Uani 0.50 1 d PD A -1 Cl2 Cl 0.4379(3) 0.7508(4) 0.1149(2) 0.1254(15) Uani 0.50 1 d PD 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 C1 0.021(2) 0.045(2) 0.041(2) 0.015(2) 0.0108(18) 0.0005(18) C2 0.0225(19) 0.040(2) 0.036(2) 0.0092(18) 0.0111(17) 0.0002(17) C3 0.027(2) 0.046(3) 0.044(3) 0.014(2) 0.0144(19) -0.0036(19) C4 0.046(2) 0.105(3) 0.138(4) 0.073(3) 0.051(2) 0.012(2) C5 0.046(2) 0.105(3) 0.138(4) 0.073(3) 0.051(2) 0.012(2) C6 0.046(2) 0.105(3) 0.138(4) 0.073(3) 0.051(2) 0.012(2) C7 0.053(3) 0.056(3) 0.047(3) 0.019(2) 0.017(2) -0.009(2) C8 0.031(2) 0.045(3) 0.043(3) 0.008(2) 0.0111(19) -0.0073(19) C9 0.0202(19) 0.036(2) 0.046(2) 0.0051(19) 0.0102(18) -0.0020(16) C10 0.028(2) 0.039(2) 0.040(2) 0.0067(19) 0.0123(18) -0.0021(17) C11 0.036(2) 0.036(2) 0.053(3) 0.006(2) 0.010(2) -0.0028(19) C12 0.034(2) 0.038(3) 0.068(4) -0.007(2) 0.010(2) -0.002(2) C13 0.041(3) 0.056(3) 0.051(3) -0.013(3) 0.015(2) -0.004(2) C14 0.035(2) 0.050(3) 0.044(3) 0.000(2) 0.011(2) -0.003(2) C15 0.045(3) 0.029(2) 0.029(2) 0.0041(16) 0.0061(19) -0.0038(18) C16 0.064(3) 0.028(2) 0.030(2) 0.0013(18) 0.008(2) -0.007(2) C17 0.078(4) 0.032(2) 0.029(2) 0.0000(18) 0.022(2) 0.001(2) C18 0.073(4) 0.041(3) 0.035(3) 0.003(2) 0.029(3) -0.005(2) C19 0.063(3) 0.031(2) 0.041(3) 0.0034(19) 0.021(2) -0.012(2) C20 0.057(3) 0.027(2) 0.033(2) 0.0010(18) 0.011(2) -0.004(2) C21 0.021(2) 0.061(4) 0.103(5) 0.031(4) -0.004(3) -0.002(2) C22 0.056(4) 0.087(5) 0.111(6) -0.034(5) 0.013(4) -0.019(4) C23 0.070(5) 0.109(7) 0.183(11) -0.048(8) 0.028(7) -0.036(5) C24 0.056(5) 0.074(5) 0.174(11) 0.006(6) -0.001(6) -0.007(4) C25 0.056(4) 0.057(4) 0.128(7) 0.029(5) -0.005(4) -0.005(3) C26 0.041(3) 0.090(5) 0.143(8) 0.059(5) -0.001(4) -0.018(3) C27 0.0234(19) 0.032(2) 0.032(2) 0.0014(16) 0.0168(16) 0.0018(16) C28 0.039(3) 0.034(2) 0.054(3) 0.000(2) 0.027(2) 0.0050(19) C29 0.052(3) 0.038(3) 0.069(4) -0.013(2) 0.037(3) 0.003(2) C30 0.064(3) 0.059(3) 0.048(3) -0.021(3) 0.032(3) 0.002(3) C31 0.078(4) 0.053(3) 0.036(3) -0.002(2) 0.028(3) 0.006(3) C32 0.049(3) 0.035(2) 0.036(2) -0.0017(18) 0.022(2) 0.005(2) C33 0.027(2) 0.039(2) 0.031(2) 0.0039(17) 0.0180(17) -0.0028(17) C34 0.031(2) 0.044(2) 0.035(2) 0.0061(19) 0.0167(18) -0.0039(19) C35 0.054(3) 0.047(3) 0.038(3) 0.012(2) 0.024(2) -0.002(2) C36 0.046(3) 0.055(3) 0.047(3) 0.003(2) 0.027(2) -0.015(2) C37 0.030(3) 0.093(5) 0.074(4) 0.027(4) 0.014(3) -0.016(3) C38 0.032(3) 0.082(4) 0.060(3) 0.033(3) 0.011(2) -0.006(3) C39 0.025(2) 0.047(3) 0.028(2) -0.0104(18) 0.0114(17) -0.0066(18) C40 0.041(3) 0.061(3) 0.052(3) 0.000(2) 0.025(2) -0.006(2) C41 0.041(3) 0.105(5) 0.048(3) -0.009(3) 0.028(3) -0.006(3) C42 0.035(3) 0.088(5) 0.057(3) -0.037(3) 0.017(2) 0.000(3) C43 0.032(3) 0.059(3) 0.076(4) -0.014(3) 0.018(3) 0.002(2) C44 0.030(2) 0.051(3) 0.050(3) 0.001(2) 0.017(2) 0.004(2) C45 0.028(2) 0.028(2) 0.028(2) 0.0062(16) 0.0078(16) 0.0041(16) C46 0.040(2) 0.031(2) 0.034(2) 0.0027(18) 0.0085(19) 0.0031(18) C47 0.044(3) 0.038(3) 0.054(3) 0.013(2) -0.009(2) -0.009(2) C48 0.038(3) 0.061(3) 0.063(4) 0.031(3) 0.015(3) -0.004(2) C49 0.041(3) 0.066(3) 0.043(3) 0.022(2) 0.021(2) 0.005(2) C50 0.038(2) 0.038(2) 0.033(2) 0.0062(18) 0.0151(19) 0.0056(19) Ag1 0.02659(17) 0.03972(19) 0.03621(18) 0.00306(13) 0.00877(13) -0.00294(12) F1 0.0450(17) 0.0554(19) 0.090(3) -0.0089(18) 0.0178(17) 0.0110(15) F2 0.082(2) 0.0378(15) 0.0381(15) 0.0088(12) 0.0113(15) -0.0113(15) F3 0.0560(17) 0.0384(14) 0.0417(15) -0.0152(12) 0.0136(13) -0.0091(12) F4 0.0568(17) 0.0365(14) 0.0469(15) -0.0011(11) 0.0314(13) -0.0015(12) F5 0.0548(17) 0.0520(16) 0.0424(15) 0.0074(13) 0.0285(13) -0.0044(13) F6 0.069(2) 0.0374(15) 0.0497(17) -0.0108(13) 0.0077(15) -0.0180(14) N1 0.0327(19) 0.0283(18) 0.041(2) 0.0074(15) 0.0171(16) -0.0006(14) N2 0.0323(18) 0.0316(17) 0.0295(18) -0.0004(14) 0.0136(15) 0.0030(15) O1 0.0380(17) 0.0318(15) 0.0372(17) 0.0042(13) -0.0007(14) -0.0035(13) O2 0.0241(16) 0.0390(18) 0.079(3) 0.0188(17) 0.0077(16) -0.0025(13) O3 0.0246(14) 0.0420(17) 0.0337(15) -0.0095(13) 0.0123(12) -0.0034(12) O4 0.0257(14) 0.0326(15) 0.0353(15) 0.0008(12) 0.0137(12) 0.0032(11) P1 0.0207(5) 0.0349(6) 0.0386(6) 0.0116(4) 0.0110(4) -0.0004(4) P2 0.0240(5) 0.0277(5) 0.0460(6) 0.0095(5) 0.0063(4) -0.0016(4) P3 0.0207(5) 0.0307(5) 0.0269(5) 0.0040(4) 0.0113(4) 0.0011(4) P4 0.0237(5) 0.0326(5) 0.0250(5) -0.0022(4) 0.0113(4) -0.0013(4) S1 0.0268(5) 0.0290(5) 0.0507(6) 0.0125(4) 0.0105(4) 0.0009(4) S2 0.0329(5) 0.0551(7) 0.0244(5) -0.0030(4) 0.0131(4) -0.0105(5) Sb1 0.04288(18) 0.02587(16) 0.03049(17) -0.00333(10) 0.01312(13) -0.00538(11) C51 0.200(5) 0.0808(18) 0.062(2) -0.0014(13) 0.000(2) 0.025(2) Cl1 0.200(5) 0.0808(18) 0.062(2) -0.0014(13) 0.000(2) 0.025(2) Cl2 0.200(5) 0.0808(18) 0.062(2) -0.0014(13) 0.000(2) 0.025(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 C1 C2 1.539(6) . ? C1 P1 1.819(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 P3 1.811(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.377(8) . ? C3 C8 1.384(7) . ? C3 P1 1.805(4) . ? C4 C5 1.394(8) . ? C4 H4 0.9300 . ? C5 C6 1.364(9) . ? C5 H5 0.9300 . ? C6 C7 1.355(9) . ? C6 H6 0.9300 . ? C7 C8 1.388(7) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C14 1.379(7) . ? C9 C10 1.392(6) . ? C9 P1 1.803(5) . ? C10 C11 1.393(7) . ? C10 H10 0.9300 . ? C11 C12 1.372(8) . ? C11 H11 0.9300 . ? C12 C13 1.382(8) . ? C12 H12 0.9300 . ? C13 C14 1.389(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.388(7) . ? C15 C20 1.396(6) . ? C15 O1 1.401(6) . ? C16 C17 1.375(8) . ? C16 H16 0.9300 . ? C17 C18 1.387(7) . ? C17 H17 0.9300 . ? C18 C19 1.396(7) . ? C18 H18 0.9300 . ? C19 C20 1.383(7) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C26 1.366(11) . ? C21 C22 1.376(11) . ? C21 O2 1.445(7) . ? C22 C23 1.384(12) . ? C22 H22 0.9300 . ? C23 C24 1.365(16) . ? C23 H23 0.9300 . ? C24 C25 1.371(15) . ? C24 H24 0.9300 . ? C25 C26 1.459(11) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C32 1.382(6) . ? C27 C28 1.402(6) . ? C27 P3 1.795(4) . ? C28 C29 1.381(7) . ? C28 H28 0.9300 . ? C29 C30 1.372(8) . ? C29 H29 0.9300 . ? C30 C31 1.392(8) . ? C30 H30 0.9300 . ? C31 C32 1.382(7) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.376(6) . ? C33 C38 1.380(7) . ? C33 P3 1.799(4) . ? C34 C35 1.394(6) . ? C34 H34 0.9300 . ? C35 C36 1.357(7) . ? C35 H35 0.9300 . ? C36 C37 1.385(8) . ? C36 H36 0.9300 . ? C37 C38 1.381(8) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C44 1.375(7) . ? C39 C40 1.376(7) . ? C39 O3 1.409(5) . ? C40 C41 1.397(8) . ? C40 H40 0.9300 . ? C41 C42 1.359(10) . ? C41 H41 0.9300 . ? C42 C43 1.379(9) . ? C42 H42 0.9300 . ? C43 C44 1.388(7) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C46 1.370(6) . ? C45 C50 1.382(6) . ? C45 O4 1.401(5) . ? C46 C47 1.396(7) . ? C46 H46 0.9300 . ? C47 C48 1.365(9) . ? C47 H47 0.9300 . ? C48 C49 1.374(9) . ? C48 H48 0.9300 . ? C49 C50 1.385(7) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? Ag1 S1 2.3977(11) . ? Ag1 S2 2.4036(11) . ? F1 Sb1 1.869(3) . ? F2 Sb1 1.871(3) . ? F3 Sb1 1.872(3) . ? F4 Sb1 1.886(3) . ? F5 Sb1 1.880(3) . ? F6 Sb1 1.877(3) . ? N1 P2 1.580(4) . ? N1 P1 1.584(4) . ? N2 P4 1.572(4) . ? N2 P3 1.584(4) . ? O1 P2 1.596(4) . ? O2 P2 1.593(3) . ? O3 P4 1.596(3) . ? O4 P4 1.593(3) . ? P2 S1 1.9850(15) . ? P4 S2 1.9811(14) . ? C51 Cl2 1.636(14) . ? C51 Cl1 1.686(14) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? 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 C2 C1 P1 111.0(3) . . ? C2 C1 H1A 109.4 . . ? P1 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? P1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C1 C2 P3 112.2(3) . . ? C1 C2 H2A 109.2 . . ? P3 C2 H2A 109.2 . . ? C1 C2 H2B 109.2 . . ? P3 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C4 C3 C8 119.3(5) . . ? C4 C3 P1 118.7(4) . . ? C8 C3 P1 121.9(3) . . ? C3 C4 C5 119.6(6) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 120.6(6) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C7 C6 C5 119.8(5) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 120.8(5) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C3 C8 C7 119.8(5) . . ? C3 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C14 C9 C10 119.6(4) . . ? C14 C9 P1 121.0(4) . . ? C10 C9 P1 119.3(4) . . ? C9 C10 C11 120.3(5) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 119.4(5) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 120.7(5) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C14 120.0(5) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C9 C14 C13 119.9(5) . . ? C9 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C20 122.6(5) . . ? C16 C15 O1 118.3(4) . . ? C20 C15 O1 119.0(4) . . ? C17 C16 C15 118.5(4) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? C16 C17 C18 120.7(5) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C19 119.9(5) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 120.9(5) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C15 117.5(5) . . ? C19 C20 H20 121.3 . . ? C15 C20 H20 121.3 . . ? C26 C21 C22 124.9(8) . . ? C26 C21 O2 114.2(8) . . ? C22 C21 O2 120.9(6) . . ? C21 C22 C23 118.9(10) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C24 C23 C22 118.4(12) . . ? C24 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C23 C24 C25 124.0(9) . . ? C23 C24 H24 118.0 . . ? C25 C24 H24 118.0 . . ? C24 C25 C26 118.1(9) . . ? C24 C25 H25 120.9 . . ? C26 C25 H25 120.9 . . ? C21 C26 C25 115.7(10) . . ? C21 C26 H26 122.2 . . ? C25 C26 H26 122.2 . . ? C32 C27 C28 120.0(4) . . ? C32 C27 P3 120.6(3) . . ? C28 C27 P3 119.4(3) . . ? C29 C28 C27 119.7(5) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C30 C29 C28 119.8(5) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 121.0(5) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C32 C31 C30 119.4(5) . . ? C32 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? C27 C32 C31 120.0(5) . . ? C27 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C38 119.7(4) . . ? C34 C33 P3 123.1(3) . . ? C38 C33 P3 117.2(3) . . ? C33 C34 C35 119.3(4) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C36 C35 C34 121.1(5) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C35 C36 C37 119.4(5) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C38 C37 C36 120.1(5) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C33 C38 C37 120.2(5) . . ? C33 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C44 C39 C40 122.0(4) . . ? C44 C39 O3 120.3(4) . . ? C40 C39 O3 117.5(4) . . ? C39 C40 C41 117.9(6) . . ? C39 C40 H40 121.0 . . ? C41 C40 H40 121.0 . . ? C42 C41 C40 121.1(5) . . ? C42 C41 H41 119.5 . . ? C40 C41 H41 119.5 . . ? C41 C42 C43 120.1(5) . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C42 C43 C44 120.2(6) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C39 C44 C43 118.7(5) . . ? C39 C44 H44 120.6 . . ? C43 C44 H44 120.6 . . ? C46 C45 C50 122.3(4) . . ? C46 C45 O4 119.1(4) . . ? C50 C45 O4 118.5(4) . . ? C45 C46 C47 118.7(5) . . ? C45 C46 H46 120.7 . . ? C47 C46 H46 120.7 . . ? C48 C47 C46 119.9(5) . . ? C48 C47 H47 120.1 . . ? C46 C47 H47 120.1 . . ? C47 C48 C49 120.5(5) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C48 C49 C50 121.0(5) . . ? C48 C49 H49 119.5 . . ? C50 C49 H49 119.5 . . ? C45 C50 C49 117.7(5) . . ? C45 C50 H50 121.2 . . ? C49 C50 H50 121.2 . . ? S1 Ag1 S2 171.74(4) . . ? P2 N1 P1 129.0(2) . . ? P4 N2 P3 135.1(2) . . ? C15 O1 P2 122.1(3) . . ? C21 O2 P2 121.6(3) . . ? C39 O3 P4 123.9(3) . . ? C45 O4 P4 122.8(2) . . ? N1 P1 C9 106.9(2) . . ? N1 P1 C3 115.8(2) . . ? C9 P1 C3 107.5(2) . . ? N1 P1 C1 110.9(2) . . ? C9 P1 C1 108.7(2) . . ? C3 P1 C1 106.9(2) . . ? N1 P2 O2 107.2(2) . . ? N1 P2 O1 107.24(18) . . ? O2 P2 O1 99.0(2) . . ? N1 P2 S1 119.01(15) . . ? O2 P2 S1 109.66(13) . . ? O1 P2 S1 112.69(14) . . ? N2 P3 C27 106.15(19) . . ? N2 P3 C33 115.13(19) . . ? C27 P3 C33 106.46(19) . . ? N2 P3 C2 114.5(2) . . ? C27 P3 C2 106.5(2) . . ? C33 P3 C2 107.5(2) . . ? N2 P4 O4 107.25(17) . . ? N2 P4 O3 106.69(18) . . ? O4 P4 O3 99.33(16) . . ? N2 P4 S2 119.34(15) . . ? O4 P4 S2 112.57(12) . . ? O3 P4 S2 109.67(12) . . ? P2 S1 Ag1 98.01(5) . . ? P4 S2 Ag1 98.59(5) . . ? F1 Sb1 F2 90.67(16) . . ? F1 Sb1 F3 91.35(14) . . ? F2 Sb1 F3 89.66(13) . . ? F1 Sb1 F6 90.42(15) . . ? F2 Sb1 F6 90.57(13) . . ? F3 Sb1 F6 178.21(14) . . ? F1 Sb1 F5 90.72(15) . . ? F2 Sb1 F5 178.52(14) . . ? F3 Sb1 F5 89.78(13) . . ? F6 Sb1 F5 89.95(14) . . ? F1 Sb1 F4 178.78(14) . . ? F2 Sb1 F4 90.42(14) . . ? F3 Sb1 F4 89.23(13) . . ? F6 Sb1 F4 89.00(14) . . ? F5 Sb1 F4 88.20(12) . . ? Cl2 C51 Cl1 119.3(11) . . ? Cl2 C51 H51A 107.5 . . ? Cl1 C51 H51A 107.5 . . ? Cl2 C51 H51B 107.5 . . ? Cl1 C51 H51B 107.5 . . ? H51A C51 H51B 107.0 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 68.43 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.316 _refine_diff_density_min -1.421 _refine_diff_density_rms 0.152 #==END #========================================================================== data_9a _database_code_depnum_ccdc_archive 'CCDC 639182' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H48 Ag N2 O4 P4 S2, F6 Sb' _chemical_formula_sum 'C36 H48 Ag F6 N2 O4 P4 S2 Sb' _chemical_formula_weight 1104.38 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.0562 5.8946 '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 12.1650(2) _cell_length_b 12.5716(2) _cell_length_c 16.4500(4) _cell_angle_alpha 80.715(1) _cell_angle_beta 80.171(1) _cell_angle_gamma 68.973(1) _cell_volume 2300.02(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7957 _cell_measurement_theta_min 2.209 _cell_measurement_theta_max 68.251 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 10.781 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.809 _exptl_absorpt_correction_T_max 1.368 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95 mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46637 _diffrn_reflns_av_r_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 68.51 _reflns_number_total 8383 _reflns_number_gt 7027 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collet (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowki & Minor 1997)' _computing_data_reduction 'HKL Denzo and scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2006)' _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. ; _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^)+(0.1663P)^2^+3.1773P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0066(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8383 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.2505 _refine_ls_wR_factor_gt 0.2396 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 C1 C 0.4225(6) 1.4585(7) 0.1075(4) 0.0648(15) Uani 1 1 d . . . H1A H 0.4436 1.5025 0.1417 0.078 Uiso 1 1 calc R . . H1B H 0.4774 1.3803 0.1133 0.078 Uiso 1 1 calc R . . C2 C 0.4359(6) 1.5090(7) 0.0163(4) 0.0693(17) Uani 1 1 d . . . H2A H 0.4037 1.4730 -0.0170 0.083 Uiso 1 1 calc R . . H2B H 0.3909 1.5905 0.0117 0.083 Uiso 1 1 calc R . . C3 C 0.5629(6) 1.0162(5) 0.3834(3) 0.0539(13) Uani 1 1 d . . . H3A H 0.6132 1.0594 0.3881 0.065 Uiso 1 1 calc R . . H3B H 0.4899 1.0701 0.3643 0.065 Uiso 1 1 calc R . . C4 C 0.5339(6) 0.9576(5) 0.4691(3) 0.0538(13) Uani 1 1 d . . . H4A H 0.4871 0.9112 0.4641 0.065 Uiso 1 1 calc R . . H4B H 0.6072 0.9069 0.4896 0.065 Uiso 1 1 calc R . . C5 C 0.2754(5) 1.3969(5) 0.2506(4) 0.0559(13) Uani 1 1 d . . . C6 C 0.1678(6) 1.3868(6) 0.2924(4) 0.0688(17) Uani 1 1 d . . . H6 H 0.1015 1.4099 0.2642 0.083 Uiso 1 1 calc R . . C7 C 0.1602(7) 1.3437(7) 0.3735(5) 0.083(2) Uani 1 1 d . . . H7 H 0.0895 1.3354 0.4003 0.100 Uiso 1 1 calc R . . C8 C 0.2576(8) 1.3123(6) 0.4162(5) 0.083(2) Uani 1 1 d . . . H8 H 0.2512 1.2864 0.4725 0.100 Uiso 1 1 calc R . . C9 C 0.3620(8) 1.3191(7) 0.3762(5) 0.082(2) Uani 1 1 d . . . H9 H 0.4277 1.2953 0.4049 0.099 Uiso 1 1 calc R . . C10 C 0.3729(6) 1.3613(6) 0.2923(4) 0.0681(16) Uani 1 1 d . . . H10 H 0.4452 1.3652 0.2653 0.082 Uiso 1 1 calc R . . C11 C 0.1783(5) 1.6062(5) 0.1444(4) 0.0549(12) Uani 1 1 d . . . C12 C 0.0840(8) 1.6465(8) 0.1002(6) 0.089(2) Uani 1 1 d . . . H12 H 0.0720 1.5987 0.0676 0.107 Uiso 1 1 calc R . . C13 C 0.0069(9) 1.7563(9) 0.1032(7) 0.107(3) Uani 1 1 d . . . H13 H -0.0597 1.7810 0.0752 0.128 Uiso 1 1 calc R . . C14 C 0.0263(8) 1.8309(7) 0.1473(6) 0.085(2) Uani 1 1 d . . . H14 H -0.0249 1.9064 0.1478 0.102 Uiso 1 1 calc R . . C15 C 0.1215(10) 1.7919(8) 0.1899(7) 0.099(3) Uani 1 1 d . . . H15 H 0.1352 1.8409 0.2206 0.119 Uiso 1 1 calc R . . C16 C 0.1999(8) 1.6785(7) 0.1884(6) 0.084(2) Uani 1 1 d . . . H16 H 0.2659 1.6528 0.2170 0.101 Uiso 1 1 calc R . . C17 C 0.0797(9) 1.2365(9) 0.1248(8) 0.106(3) Uani 1 1 d . . . H17A H 0.0307 1.2983 0.0893 0.127 Uiso 1 1 calc R . . H17B H 0.0728 1.2642 0.1778 0.127 Uiso 1 1 calc R . . C18 C 0.0372(11) 1.1410(12) 0.1373(9) 0.127(4) Uani 1 1 d . . . H18A H 0.0511 1.1086 0.0860 0.191 Uiso 1 1 calc R . . H18B H -0.0464 1.1671 0.1561 0.191 Uiso 1 1 calc R . . H18C H 0.0784 1.0839 0.1783 0.191 Uiso 1 1 calc R . . C19 C 0.244(2) 1.3943(18) -0.1031(9) 0.185(9) Uani 1 1 d . . . H19A H 0.2504 1.4537 -0.0753 0.222 Uiso 1 1 calc R . . H19B H 0.3218 1.3575 -0.1315 0.222 Uiso 1 1 calc R . . C20 C 0.180(4) 1.446(3) -0.159(2) 0.36(3) Uani 1 1 d . . . H20A H 0.2259 1.4746 -0.2045 0.547 Uiso 1 1 calc R . . H20B H 0.1145 1.5084 -0.1375 0.547 Uiso 1 1 calc R . . H20C H 0.1503 1.3938 -0.1776 0.547 Uiso 1 1 calc R . . C21 C 0.4505(16) 0.6666(11) 0.3879(10) 0.139(5) Uani 1 1 d . . . H21A H 0.4438 0.6994 0.4387 0.167 Uiso 1 1 calc R . . H21B H 0.5342 0.6291 0.3703 0.167 Uiso 1 1 calc R . . C22 C 0.392(2) 0.5824(15) 0.4043(10) 0.169(7) Uani 1 1 d . . . H22A H 0.3122 0.6166 0.4293 0.254 Uiso 1 1 calc R . . H22B H 0.4342 0.5193 0.4414 0.254 Uiso 1 1 calc R . . H22C H 0.3915 0.5553 0.3532 0.254 Uiso 1 1 calc R . . C23 C 0.2227(10) 0.995(2) 0.3383(13) 0.197(10) Uani 1 1 d . . . H23A H 0.1942 1.0615 0.2989 0.236 Uiso 1 1 calc R . . H23B H 0.1979 0.9349 0.3250 0.236 Uiso 1 1 calc R . . C24 C 0.1724(12) 1.0213(15) 0.4159(11) 0.156(6) Uani 1 1 d . . . H24A H 0.2027 0.9564 0.4555 0.234 Uiso 1 1 calc R . . H24B H 0.0879 1.0416 0.4193 0.234 Uiso 1 1 calc R . . H24C H 0.1909 1.0849 0.4276 0.234 Uiso 1 1 calc R . . C25 C 0.7750(5) 0.8228(5) 0.3431(3) 0.0546(13) Uani 1 1 d . . . C26 C 0.8520(7) 0.8665(7) 0.3680(4) 0.0718(17) Uani 1 1 d . . . H26 H 0.8334 0.9454 0.3658 0.086 Uiso 1 1 calc R . . C27 C 0.9555(7) 0.7933(9) 0.3959(5) 0.089(2) Uani 1 1 d . . . H27 H 1.0061 0.8234 0.4133 0.107 Uiso 1 1 calc R . . C28 C 0.9860(8) 0.6784(9) 0.3987(6) 0.097(3) Uani 1 1 d . . . H28 H 1.0580 0.6302 0.4161 0.117 Uiso 1 1 calc R . . C29 C 0.9105(8) 0.6335(8) 0.3758(6) 0.093(3) Uani 1 1 d . . . H29 H 0.9304 0.5544 0.3789 0.111 Uiso 1 1 calc R . . C30 C 0.8037(7) 0.7056(6) 0.3477(5) 0.0721(17) Uani 1 1 d . . . H30 H 0.7523 0.6748 0.3322 0.087 Uiso 1 1 calc R . . C31 C 0.6729(5) 0.9969(5) 0.2114(3) 0.0504(12) Uani 1 1 d . . . C32 C 0.6959(5) 0.9452(6) 0.1395(4) 0.0595(14) Uani 1 1 d . . . H32 H 0.6894 0.8733 0.1414 0.071 Uiso 1 1 calc R . . C33 C 0.7288(6) 1.0008(7) 0.0637(4) 0.0695(17) Uani 1 1 d . . . H33 H 0.7445 0.9658 0.0153 0.083 Uiso 1 1 calc R . . C34 C 0.7380(6) 1.1059(7) 0.0607(4) 0.0734(19) Uani 1 1 d . . . H34 H 0.7595 1.1426 0.0100 0.088 Uiso 1 1 calc R . . C35 C 0.7152(7) 1.1600(7) 0.1335(4) 0.0720(17) Uani 1 1 d . . . H35 H 0.7211 1.2322 0.1315 0.086 Uiso 1 1 calc R . . C36 C 0.6839(6) 1.1034(6) 0.2079(4) 0.0615(14) Uani 1 1 d . . . H36 H 0.6699 1.1374 0.2566 0.074 Uiso 1 1 calc R . . Ag1 Ag 0.44054(7) 1.01613(9) 0.10152(5) 0.1206(4) Uani 1 1 d . . . F1 F 0.8565(9) 0.2530(8) 0.4595(5) 0.154(3) Uani 1 1 d . . . F2 F 0.7294(10) 0.3260(7) 0.2614(5) 0.161(3) Uani 1 1 d . . . F3 F 0.9262(9) 0.3257(11) 0.3070(6) 0.184(4) Uani 1 1 d . . . F4 F 0.6664(8) 0.2494(11) 0.4084(6) 0.175(4) Uani 1 1 d . . . F5 F 0.8698(11) 0.1376(7) 0.3352(7) 0.181(4) Uani 1 1 d . . . F6 F 0.7169(10) 0.4422(7) 0.3807(7) 0.178(4) Uani 1 1 d . . . N1 N 0.2233(5) 1.4022(5) 0.0884(4) 0.0686(14) Uani 1 1 d . . . N2 N 0.5669(5) 0.8386(4) 0.2940(3) 0.0602(12) Uani 1 1 d . . . O1 O 0.1955(5) 1.2066(5) 0.0894(5) 0.109(2) Uani 1 1 d . . . O2 O 0.2229(7) 1.3105(7) -0.0385(4) 0.105(2) Uani 1 1 d . . . O3 O 0.4055(8) 0.7490(10) 0.3306(9) 0.182(6) Uani 1 1 d . . . O4 O 0.3526(5) 0.9553(8) 0.3292(5) 0.118(3) Uani 1 1 d . . . P1 P 0.27494(12) 1.45885(14) 0.14406(9) 0.0543(4) Uani 1 1 d . . . P2 P 0.26513(14) 1.28798(16) 0.04720(10) 0.0634(4) Uani 1 1 d . . . P3 P 0.63693(12) 0.91656(12) 0.30742(8) 0.0490(3) Uani 1 1 d . . . P4 P 0.43688(15) 0.85174(15) 0.28438(10) 0.0644(4) Uani 1 1 d . . . S1 S 0.43765(18) 1.1976(2) 0.04178(17) 0.0973(7) Uani 1 1 d . . . S2 S 0.4009(3) 0.8507(3) 0.17178(18) 0.1145(9) Uani 1 1 d . . . Sb1 Sb 0.79489(5) 0.29080(4) 0.36045(3) 0.0779(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 C1 0.055(3) 0.092(4) 0.049(3) -0.002(3) -0.003(2) -0.031(3) C2 0.052(3) 0.104(5) 0.049(3) 0.006(3) -0.003(3) -0.031(3) C3 0.066(3) 0.051(3) 0.037(3) -0.001(2) -0.001(2) -0.014(2) C4 0.066(3) 0.049(3) 0.035(2) -0.006(2) 0.001(2) -0.009(2) C5 0.058(3) 0.058(3) 0.048(3) -0.005(2) -0.003(2) -0.018(3) C6 0.059(3) 0.080(4) 0.055(3) 0.006(3) 0.000(3) -0.017(3) C7 0.076(5) 0.079(4) 0.067(4) 0.011(3) 0.015(4) -0.013(4) C8 0.100(6) 0.067(4) 0.057(4) 0.014(3) -0.001(4) -0.009(4) C9 0.102(6) 0.067(4) 0.066(4) 0.013(3) -0.034(4) -0.013(4) C10 0.068(4) 0.069(4) 0.062(4) 0.004(3) -0.008(3) -0.022(3) C11 0.056(3) 0.063(3) 0.046(3) 0.000(2) -0.003(2) -0.024(3) C12 0.088(5) 0.086(5) 0.091(6) -0.025(4) -0.035(4) -0.010(4) C13 0.093(6) 0.097(6) 0.120(8) -0.035(6) -0.045(6) 0.005(5) C14 0.077(5) 0.077(5) 0.094(6) -0.009(4) -0.004(4) -0.022(4) C15 0.116(7) 0.074(5) 0.124(8) -0.018(5) -0.034(6) -0.039(5) C16 0.091(5) 0.071(4) 0.100(6) -0.010(4) -0.042(5) -0.026(4) C17 0.084(6) 0.106(6) 0.129(8) -0.041(6) 0.038(6) -0.045(5) C18 0.110(8) 0.140(9) 0.157(11) -0.041(8) 0.021(7) -0.080(7) C19 0.32(3) 0.219(18) 0.078(7) 0.034(10) -0.052(12) -0.170(19) C20 0.38(5) 0.30(4) 0.25(3) 0.16(3) -0.09(3) 0.01(3) C21 0.189(14) 0.108(8) 0.132(10) 0.037(7) -0.037(10) -0.078(9) C22 0.27(2) 0.147(12) 0.130(12) 0.017(9) -0.039(13) -0.132(14) C23 0.063(6) 0.30(2) 0.231(19) -0.156(19) -0.018(9) -0.012(9) C24 0.097(8) 0.160(12) 0.187(15) -0.071(12) 0.017(9) -0.008(8) C25 0.054(3) 0.059(3) 0.041(3) -0.008(2) -0.002(2) -0.009(2) C26 0.073(4) 0.075(4) 0.065(4) -0.006(3) -0.014(3) -0.020(3) C27 0.068(4) 0.122(7) 0.078(5) -0.009(5) -0.019(4) -0.030(5) C28 0.066(5) 0.110(7) 0.087(6) 0.006(5) -0.010(4) -0.002(5) C29 0.082(5) 0.073(5) 0.095(6) -0.007(4) -0.014(4) 0.007(4) C30 0.073(4) 0.063(4) 0.070(4) -0.015(3) -0.006(3) -0.009(3) C31 0.047(3) 0.059(3) 0.037(2) -0.006(2) -0.003(2) -0.010(2) C32 0.058(3) 0.070(3) 0.042(3) -0.014(3) -0.002(2) -0.012(3) C33 0.068(4) 0.092(5) 0.041(3) -0.007(3) 0.003(3) -0.022(3) C34 0.066(4) 0.103(5) 0.042(3) 0.005(3) -0.001(3) -0.025(4) C35 0.078(4) 0.076(4) 0.059(4) 0.005(3) -0.008(3) -0.029(3) C36 0.073(4) 0.069(4) 0.041(3) -0.005(2) -0.002(3) -0.026(3) Ag1 0.0976(5) 0.1718(9) 0.0828(5) 0.0293(5) -0.0298(4) -0.0445(5) F1 0.170(7) 0.192(8) 0.115(5) 0.000(5) -0.066(5) -0.066(6) F2 0.267(11) 0.143(6) 0.109(5) 0.012(4) -0.080(6) -0.099(6) F3 0.169(7) 0.271(12) 0.156(7) -0.054(7) 0.056(6) -0.150(8) F4 0.144(6) 0.270(11) 0.151(7) 0.000(7) 0.000(5) -0.137(7) F5 0.236(11) 0.096(5) 0.194(9) -0.026(5) -0.039(8) -0.026(5) F6 0.218(10) 0.116(5) 0.177(8) -0.053(5) -0.039(7) -0.006(6) N1 0.058(3) 0.081(4) 0.069(3) -0.018(3) -0.007(2) -0.021(3) N2 0.058(3) 0.062(3) 0.057(3) -0.012(2) -0.005(2) -0.015(2) O1 0.079(4) 0.089(4) 0.160(7) -0.050(4) 0.038(4) -0.037(3) O2 0.128(5) 0.124(5) 0.068(3) -0.011(3) -0.033(3) -0.040(4) O3 0.117(6) 0.178(9) 0.241(13) 0.115(9) -0.038(7) -0.088(6) O4 0.059(3) 0.170(7) 0.120(5) -0.083(5) -0.011(3) -0.005(3) P1 0.0491(7) 0.0712(9) 0.0441(7) -0.0042(6) -0.0011(5) -0.0254(6) P2 0.0571(8) 0.0866(11) 0.0477(8) -0.0138(7) -0.0013(6) -0.0256(8) P3 0.0534(7) 0.0529(7) 0.0357(6) -0.0078(5) -0.0012(5) -0.0128(6) P4 0.0643(9) 0.0727(10) 0.0557(9) 0.0030(7) -0.0023(7) -0.0294(8) S1 0.0602(10) 0.1130(16) 0.1112(17) -0.0349(13) 0.0074(10) -0.0189(10) S2 0.1152(19) 0.168(3) 0.0934(16) -0.0407(17) -0.0148(13) -0.0757(19) Sb1 0.0816(4) 0.0849(4) 0.0758(4) -0.0089(2) -0.0071(2) -0.0396(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 C1 C2 1.537(9) . ? C1 P1 1.792(6) . ? C2 C2 1.506(12) 2_685 ? C3 C4 1.528(7) . ? C3 P3 1.804(6) . ? C4 C4 1.511(10) 2_676 ? C5 C10 1.369(9) . ? C5 C6 1.410(9) . ? C5 P1 1.799(6) . ? C6 C7 1.358(10) . ? C7 C8 1.383(13) . ? C8 C9 1.353(13) . ? C9 C10 1.397(10) . ? C11 C12 1.360(10) . ? C11 C16 1.366(10) . ? C11 P1 1.803(6) . ? C12 C13 1.366(12) . ? C13 C14 1.377(13) . ? C14 C15 1.353(13) . ? C15 C16 1.404(12) . ? C17 O1 1.369(10) . ? C17 C18 1.442(14) . ? C19 C20 1.24(3) . ? C19 O2 1.429(16) . ? C21 O3 1.310(15) . ? C21 C22 1.440(19) . ? C23 C24 1.36(2) . ? C23 O4 1.465(13) . ? C25 C30 1.380(9) . ? C25 C26 1.386(10) . ? C25 P3 1.802(6) . ? C26 C27 1.368(11) . ? C27 C28 1.352(14) . ? C28 C29 1.366(15) . ? C29 C30 1.395(11) . ? C31 C32 1.380(8) . ? C31 C36 1.384(9) . ? C31 P3 1.809(6) . ? C32 C33 1.397(9) . ? C33 C34 1.358(11) . ? C34 C35 1.411(11) . ? C35 C36 1.380(9) . ? Ag1 S1 2.324(3) . ? Ag1 S2 2.376(4) . ? F1 Sb1 1.831(7) . ? F2 Sb1 1.855(7) . ? F3 Sb1 1.848(7) . ? F4 Sb1 1.835(7) . ? F5 Sb1 1.892(8) . ? F6 Sb1 1.854(8) . ? N1 P2 1.566(6) . ? N1 P1 1.571(6) . ? N2 P4 1.563(6) . ? N2 P3 1.571(6) . ? O1 P2 1.561(6) . ? O2 P2 1.531(6) . ? O3 P4 1.526(8) . ? O4 P4 1.544(6) . ? P2 S1 1.990(3) . ? P4 S2 1.978(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 C2 C1 P1 112.7(4) . . ? C2 C2 C1 111.4(7) 2_685 . ? C4 C3 P3 113.1(4) . . ? C4 C4 C3 112.5(6) 2_676 . ? C10 C5 C6 119.3(6) . . ? C10 C5 P1 123.8(5) . . ? C6 C5 P1 116.9(5) . . ? C7 C6 C5 120.4(7) . . ? C6 C7 C8 120.0(7) . . ? C9 C8 C7 120.0(7) . . ? C8 C9 C10 121.2(7) . . ? C5 C10 C9 119.0(7) . . ? C12 C11 C16 119.5(7) . . ? C12 C11 P1 120.2(5) . . ? C16 C11 P1 120.3(5) . . ? C11 C12 C13 120.8(8) . . ? C12 C13 C14 120.8(9) . . ? C15 C14 C13 118.5(8) . . ? C14 C15 C16 120.9(8) . . ? C11 C16 C15 119.4(7) . . ? O1 C17 C18 111.8(9) . . ? C20 C19 O2 127(3) . . ? O3 C21 C22 112.5(14) . . ? C24 C23 O4 112.9(13) . . ? C30 C25 C26 119.2(6) . . ? C30 C25 P3 119.8(5) . . ? C26 C25 P3 121.0(5) . . ? C27 C26 C25 119.8(8) . . ? C28 C27 C26 121.6(9) . . ? C27 C28 C29 119.6(8) . . ? C28 C29 C30 120.3(8) . . ? C25 C30 C29 119.5(8) . . ? C32 C31 C36 119.5(5) . . ? C32 C31 P3 117.3(5) . . ? C36 C31 P3 123.2(4) . . ? C31 C32 C33 120.1(6) . . ? C34 C33 C32 120.0(6) . . ? C33 C34 C35 120.8(6) . . ? C36 C35 C34 118.4(7) . . ? C35 C36 C31 121.2(6) . . ? S1 Ag1 S2 167.99(10) . . ? P2 N1 P1 137.0(4) . . ? P4 N2 P3 138.1(4) . . ? C17 O1 P2 127.8(6) . . ? C19 O2 P2 124.7(9) . . ? C21 O3 P4 135.2(10) . . ? C23 O4 P4 125.6(8) . . ? N1 P1 C1 114.7(3) . . ? N1 P1 C5 114.1(3) . . ? C1 P1 C5 106.8(3) . . ? N1 P1 C11 106.3(3) . . ? C1 P1 C11 107.7(3) . . ? C5 P1 C11 106.8(3) . . ? O2 P2 O1 97.8(5) . . ? O2 P2 N1 110.4(4) . . ? O1 P2 N1 112.3(3) . . ? O2 P2 S1 111.0(3) . . ? O1 P2 S1 107.9(3) . . ? N1 P2 S1 116.0(2) . . ? N2 P3 C25 107.2(3) . . ? N2 P3 C3 114.9(3) . . ? C25 P3 C3 107.3(3) . . ? N2 P3 C31 111.7(3) . . ? C25 P3 C31 107.3(3) . . ? C3 P3 C31 108.1(3) . . ? O3 P4 O4 104.9(7) . . ? O3 P4 N2 110.6(4) . . ? O4 P4 N2 107.7(3) . . ? O3 P4 S2 100.9(6) . . ? O4 P4 S2 114.3(3) . . ? N2 P4 S2 117.5(2) . . ? P2 S1 Ag1 103.12(12) . . ? P4 S2 Ag1 100.90(12) . . ? F1 Sb1 F4 90.7(4) . . ? F1 Sb1 F3 91.5(5) . . ? F4 Sb1 F3 176.1(4) . . ? F1 Sb1 F6 92.5(5) . . ? F4 Sb1 F6 92.3(6) . . ? F3 Sb1 F6 90.8(6) . . ? F1 Sb1 F2 178.1(4) . . ? F4 Sb1 F2 87.5(5) . . ? F3 Sb1 F2 90.3(5) . . ? F6 Sb1 F2 88.3(4) . . ? F1 Sb1 F5 90.4(5) . . ? F4 Sb1 F5 87.0(6) . . ? F3 Sb1 F5 89.8(5) . . ? F6 Sb1 F5 177.0(4) . . ? F2 Sb1 F5 88.8(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 C1 C2 C2 -171.2(8) . . . 2_685 ? P3 C3 C4 C4 -176.9(6) . . . 2_676 ? C10 C5 C6 C7 0.9(11) . . . . ? P1 C5 C6 C7 -178.3(6) . . . . ? C5 C6 C7 C8 1.7(12) . . . . ? C6 C7 C8 C9 -3.3(13) . . . . ? C7 C8 C9 C10 2.2(13) . . . . ? C6 C5 C10 C9 -1.9(10) . . . . ? P1 C5 C10 C9 177.1(6) . . . . ? C8 C9 C10 C5 0.4(12) . . . . ? C16 C11 C12 C13 -3.9(14) . . . . ? P1 C11 C12 C13 176.8(9) . . . . ? C11 C12 C13 C14 3.7(18) . . . . ? C12 C13 C14 C15 -2.2(17) . . . . ? C13 C14 C15 C16 0.9(16) . . . . ? C12 C11 C16 C15 2.6(13) . . . . ? P1 C11 C16 C15 -178.1(7) . . . . ? C14 C15 C16 C11 -1.2(16) . . . . ? C30 C25 C26 C27 0.6(10) . . . . ? P3 C25 C26 C27 179.1(6) . . . . ? C25 C26 C27 C28 1.0(13) . . . . ? C26 C27 C28 C29 -2.1(14) . . . . ? C27 C28 C29 C30 1.5(14) . . . . ? C26 C25 C30 C29 -1.2(11) . . . . ? P3 C25 C30 C29 -179.7(6) . . . . ? C28 C29 C30 C25 0.1(13) . . . . ? C36 C31 C32 C33 -0.6(9) . . . . ? P3 C31 C32 C33 -177.5(5) . . . . ? C31 C32 C33 C34 -0.2(10) . . . . ? C32 C33 C34 C35 0.3(11) . . . . ? C33 C34 C35 C36 0.3(11) . . . . ? C34 C35 C36 C31 -1.1(11) . . . . ? C32 C31 C36 C35 1.3(10) . . . . ? P3 C31 C36 C35 177.9(5) . . . . ? C18 C17 O1 P2 164.5(10) . . . . ? C20 C19 O2 P2 -152(3) . . . . ? C22 C21 O3 P4 -173.9(16) . . . . ? C24 C23 O4 P4 136.1(15) . . . . ? P2 N1 P1 C1 48.9(7) . . . . ? P2 N1 P1 C5 -74.8(7) . . . . ? P2 N1 P1 C11 167.9(6) . . . . ? C2 C1 P1 N1 52.3(7) . . . . ? C2 C1 P1 C5 179.8(5) . . . . ? C2 C1 P1 C11 -65.8(6) . . . . ? C10 C5 P1 N1 129.6(6) . . . . ? C6 C5 P1 N1 -51.3(6) . . . . ? C10 C5 P1 C1 1.8(7) . . . . ? C6 C5 P1 C1 -179.2(5) . . . . ? C10 C5 P1 C11 -113.3(6) . . . . ? C6 C5 P1 C11 65.8(6) . . . . ? C12 C11 P1 N1 -1.0(7) . . . . ? C16 C11 P1 N1 179.7(6) . . . . ? C12 C11 P1 C1 122.4(7) . . . . ? C16 C11 P1 C1 -56.9(7) . . . . ? C12 C11 P1 C5 -123.2(7) . . . . ? C16 C11 P1 C5 57.5(7) . . . . ? C19 O2 P2 O1 170.4(14) . . . . ? C19 O2 P2 N1 53.1(15) . . . . ? C19 O2 P2 S1 -77.0(15) . . . . ? C17 O1 P2 O2 -83.0(11) . . . . ? C17 O1 P2 N1 32.8(11) . . . . ? C17 O1 P2 S1 161.8(10) . . . . ? P1 N1 P2 O2 -142.3(6) . . . . ? P1 N1 P2 O1 109.7(7) . . . . ? P1 N1 P2 S1 -14.9(7) . . . . ? P4 N2 P3 C25 162.6(5) . . . . ? P4 N2 P3 C3 43.4(6) . . . . ? P4 N2 P3 C31 -80.1(6) . . . . ? C30 C25 P3 N2 4.6(6) . . . . ? C26 C25 P3 N2 -173.9(5) . . . . ? C30 C25 P3 C3 128.5(5) . . . . ? C26 C25 P3 C3 -50.0(6) . . . . ? C30 C25 P3 C31 -115.5(5) . . . . ? C26 C25 P3 C31 66.0(6) . . . . ? C4 C3 P3 N2 57.7(5) . . . . ? C4 C3 P3 C25 -61.4(5) . . . . ? C4 C3 P3 C31 -176.8(4) . . . . ? C32 C31 P3 N2 -33.2(5) . . . . ? C36 C31 P3 N2 150.1(5) . . . . ? C32 C31 P3 C25 84.0(5) . . . . ? C36 C31 P3 C25 -92.8(5) . . . . ? C32 C31 P3 C3 -160.5(5) . . . . ? C36 C31 P3 C3 22.7(6) . . . . ? C21 O3 P4 O4 -99.6(19) . . . . ? C21 O3 P4 N2 16(2) . . . . ? C21 O3 P4 S2 141.4(19) . . . . ? C23 O4 P4 O3 -59.4(15) . . . . ? C23 O4 P4 N2 -177.2(14) . . . . ? C23 O4 P4 S2 50.2(15) . . . . ? P3 N2 P4 O3 -140.4(8) . . . . ? P3 N2 P4 O4 -26.2(7) . . . . ? P3 N2 P4 S2 104.6(5) . . . . ? O2 P2 S1 Ag1 -105.5(3) . . . . ? O1 P2 S1 Ag1 0.5(3) . . . . ? N1 P2 S1 Ag1 127.4(3) . . . . ? S2 Ag1 S1 P2 -13.2(5) . . . . ? O3 P4 S2 Ag1 177.3(5) . . . . ? O4 P4 S2 Ag1 65.3(4) . . . . ? N2 P4 S2 Ag1 -62.4(3) . . . . ? S1 Ag1 S2 P4 -90.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 68.51 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 3.059 _refine_diff_density_min -2.110 _refine_diff_density_rms 0.155 #==END #========================================================================== data_11b _database_code_depnum_ccdc_archive 'CCDC 639183' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H48 Ag Fe N2 O4 P4 S2, F6 Sb, 2(C H2 Cl2)' _chemical_formula_sum 'C60 H52 Ag Cl4 F6 Fe N2 O4 P4 S2 Sb' _chemical_formula_weight 1594.31 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 17.9823(3) _cell_length_b 15.1788(3) _cell_length_c 24.4432(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.802(1) _cell_angle_gamma 90.00 _cell_volume 6505.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10820 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 11.011 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.664 _exptl_absorpt_correction_T_max 1.512 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95 mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74429 _diffrn_reflns_av_R_equivalents 0.0965 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 68.53 _reflns_number_total 11918 _reflns_number_gt 9020 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collet (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowki & Minor 1997)' _computing_data_reduction 'HKL Denzo and scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2006)' _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. ; _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^)+(0.1231P)^2^+22.3918P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00016(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11918 _refine_ls_number_parameters 768 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0743 _refine_ls_wR_factor_ref 0.2171 _refine_ls_wR_factor_gt 0.2007 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 C1 C -0.1838(4) 0.0007(5) -0.0480(3) 0.0347(15) Uani 1 1 d . . . C2 C -0.1581(4) -0.0615(5) -0.0796(3) 0.0418(17) Uani 1 1 d . . . H2 H -0.1433 -0.0456 -0.1124 0.050 Uiso 1 1 calc R . . C3 C -0.1545(4) -0.1489(5) -0.0623(4) 0.051(2) Uani 1 1 d . . . H3 H -0.1373 -0.1917 -0.0838 0.061 Uiso 1 1 calc R . . C4 C -0.1760(4) -0.1726(5) -0.0138(4) 0.050(2) Uani 1 1 d . . . H4 H -0.1723 -0.2309 -0.0019 0.060 Uiso 1 1 calc R . . C5 C -0.2027(5) -0.1099(6) 0.0165(4) 0.055(2) Uani 1 1 d . . . H5 H -0.2180 -0.1263 0.0490 0.066 Uiso 1 1 calc R . . C6 C -0.2078(5) -0.0216(5) 0.0003(3) 0.0466(18) Uani 1 1 d . . . H6 H -0.2266 0.0208 0.0211 0.056 Uiso 1 1 calc R . . C7 C -0.1160(4) 0.2394(5) 0.0553(3) 0.0360(15) Uani 1 1 d . . . C8 C -0.0451(5) 0.2303(6) 0.0892(3) 0.052(2) Uani 1 1 d . . . H8 H -0.0175 0.1786 0.0889 0.063 Uiso 1 1 calc R . . C9 C -0.0151(5) 0.2995(7) 0.1241(4) 0.064(3) Uani 1 1 d . . . H9 H 0.0329 0.2939 0.1478 0.077 Uiso 1 1 calc R . . C10 C -0.0557(5) 0.3765(7) 0.1242(4) 0.058(2) Uani 1 1 d . . . H10 H -0.0345 0.4231 0.1471 0.070 Uiso 1 1 calc R . . C11 C -0.1276(5) 0.3843(6) 0.0903(3) 0.0493(19) Uani 1 1 d . . . H11 H -0.1556 0.4356 0.0911 0.059 Uiso 1 1 calc R . . C12 C -0.1583(4) 0.3157(5) 0.0550(3) 0.0418(17) Uani 1 1 d . . . H12 H -0.2065 0.3208 0.0315 0.050 Uiso 1 1 calc R . . C13 C -0.0372(4) 0.3453(4) -0.0902(3) 0.0364(15) Uani 1 1 d . . . C14 C -0.0171(4) 0.3784(5) -0.0359(3) 0.0449(18) Uani 1 1 d . . . H14 H -0.0539 0.3841 -0.0148 0.054 Uiso 1 1 calc R . . C15 C 0.0572(5) 0.4029(5) -0.0131(4) 0.053(2) Uani 1 1 d . . . H15 H 0.0704 0.4246 0.0234 0.064 Uiso 1 1 calc R . . C16 C 0.1114(5) 0.3951(6) -0.0442(4) 0.060(2) Uani 1 1 d . . . H16 H 0.1614 0.4114 -0.0286 0.072 Uiso 1 1 calc R . . C17 C 0.0927(5) 0.3636(7) -0.0982(5) 0.065(3) Uani 1 1 d . . . H17 H 0.1299 0.3595 -0.1191 0.078 Uiso 1 1 calc R . . C18 C 0.0185(4) 0.3379(5) -0.1214(4) 0.0476(19) Uani 1 1 d . . . H18 H 0.0060 0.3158 -0.1578 0.057 Uiso 1 1 calc R . . C19 C -0.1903(4) 0.4119(4) -0.1275(3) 0.0345(15) Uani 1 1 d . . . C20 C -0.1585(5) 0.4884(5) -0.1434(4) 0.051(2) Uani 1 1 d . . . H20 H -0.1077 0.4893 -0.1460 0.061 Uiso 1 1 calc R . . C21 C -0.2033(5) 0.5637(6) -0.1553(4) 0.058(2) Uani 1 1 d . . . H21 H -0.1821 0.6151 -0.1658 0.070 Uiso 1 1 calc R . . C22 C -0.2761(6) 0.5628(6) -0.1519(4) 0.057(2) Uani 1 1 d . . . H22 H -0.3052 0.6137 -0.1603 0.068 Uiso 1 1 calc R . . C23 C -0.3096(5) 0.4866(6) -0.1358(3) 0.053(2) Uani 1 1 d . . . H23 H -0.3607 0.4865 -0.1338 0.064 Uiso 1 1 calc R . . C24 C -0.2658(4) 0.4113(5) -0.1230(3) 0.0376(15) Uani 1 1 d . . . H24 H -0.2868 0.3606 -0.1113 0.045 Uiso 1 1 calc R . . C25 C -0.1401(4) 0.2657(5) -0.1847(3) 0.0341(15) Uani 1 1 d . . . C26 C -0.1269(4) 0.1748(5) -0.1954(3) 0.0415(17) Uani 1 1 d . . . H26 H -0.1150 0.1304 -0.1687 0.050 Uiso 1 1 calc R . . C27 C -0.1354(4) 0.1648(5) -0.2541(3) 0.0445(18) Uani 1 1 d . . . H27 H -0.1300 0.1125 -0.2727 0.053 Uiso 1 1 calc R . . C28 C -0.1533(4) 0.2473(5) -0.2795(3) 0.0416(17) Uani 1 1 d . . . H28 H -0.1617 0.2587 -0.3178 0.050 Uiso 1 1 calc R . . C29 C -0.1566(4) 0.3102(5) -0.2377(3) 0.0375(16) Uani 1 1 d . . . H29 H -0.1676 0.3698 -0.2435 0.045 Uiso 1 1 calc R . . C30 C -0.3169(4) 0.1950(6) -0.1908(3) 0.0452(18) Uani 1 1 d . . . H30 H -0.3113 0.2001 -0.1522 0.054 Uiso 1 1 calc R . . C31 C -0.3063(4) 0.1175(5) -0.2193(3) 0.0456(18) Uani 1 1 d . . . H31 H -0.2924 0.0630 -0.2028 0.055 Uiso 1 1 calc R . . C32 C -0.3203(4) 0.1362(5) -0.2780(3) 0.0428(17) Uani 1 1 d . . . H32 H -0.3170 0.0965 -0.3064 0.051 Uiso 1 1 calc R . . C33 C -0.3403(4) 0.2271(5) -0.2850(3) 0.0348(15) Uani 1 1 d . . . C34 C -0.3376(4) 0.2645(5) -0.2304(3) 0.0360(15) Uani 1 1 d . . . H34 H -0.3475 0.3227 -0.2226 0.043 Uiso 1 1 calc R . . C35 C -0.4678(4) 0.3048(5) -0.3628(3) 0.0366(15) Uani 1 1 d . . . C36 C -0.5012(4) 0.3494(5) -0.4126(3) 0.0465(18) Uani 1 1 d . . . H36 H -0.4719 0.3671 -0.4376 0.056 Uiso 1 1 calc R . . C37 C -0.5793(5) 0.3666(6) -0.4234(4) 0.059(2) Uani 1 1 d . . . H37 H -0.6026 0.3953 -0.4564 0.071 Uiso 1 1 calc R . . C38 C -0.6218(5) 0.3419(7) -0.3865(5) 0.067(3) Uani 1 1 d . . . H38 H -0.6735 0.3552 -0.3940 0.081 Uiso 1 1 calc R . . C39 C -0.5890(5) 0.2971(7) -0.3379(4) 0.061(2) Uani 1 1 d . . . H39 H -0.6186 0.2798 -0.3131 0.074 Uiso 1 1 calc R . . C40 C -0.5119(4) 0.2782(5) -0.3263(3) 0.0451(18) Uani 1 1 d . . . H40 H -0.4897 0.2476 -0.2938 0.054 Uiso 1 1 calc R . . C41 C -0.3217(4) 0.3897(5) -0.3439(3) 0.0347(15) Uani 1 1 d . . . C42 C -0.3486(5) 0.4555(5) -0.3136(3) 0.0476(18) Uani 1 1 d . . . H42 H -0.3904 0.4451 -0.2979 0.057 Uiso 1 1 calc R . . C43 C -0.3120(5) 0.5371(6) -0.3070(4) 0.055(2) Uani 1 1 d . . . H43 H -0.3301 0.5817 -0.2874 0.066 Uiso 1 1 calc R . . C44 C -0.2501(5) 0.5519(6) -0.3292(4) 0.056(2) Uani 1 1 d . . . H44 H -0.2248 0.6057 -0.3235 0.067 Uiso 1 1 calc R . . C45 C -0.2249(5) 0.4870(5) -0.3601(3) 0.0473(19) Uani 1 1 d . . . H45 H -0.1834 0.4979 -0.3760 0.057 Uiso 1 1 calc R . . C46 C -0.2604(4) 0.4060(5) -0.3675(3) 0.0394(16) Uani 1 1 d . . . H46 H -0.2430 0.3626 -0.3885 0.047 Uiso 1 1 calc R . . C47 C -0.3183(4) -0.0108(5) -0.4427(3) 0.0375(16) Uani 1 1 d . . . C48 C -0.3167(5) -0.0771(5) -0.4044(3) 0.0494(19) Uani 1 1 d . . . H48 H -0.3124 -0.0643 -0.3666 0.059 Uiso 1 1 calc R . . C49 C -0.3215(5) -0.1636(5) -0.4230(4) 0.053(2) Uani 1 1 d . . . H49 H -0.3214 -0.2091 -0.3975 0.064 Uiso 1 1 calc R . . C50 C -0.3265(4) -0.1832(5) -0.4785(4) 0.049(2) Uani 1 1 d . . . H50 H -0.3297 -0.2414 -0.4906 0.059 Uiso 1 1 calc R . . C51 C -0.3266(4) -0.1157(5) -0.5158(3) 0.0473(19) Uani 1 1 d . . . H51 H -0.3299 -0.1286 -0.5534 0.057 Uiso 1 1 calc R . . C52 C -0.3219(4) -0.0284(5) -0.4983(3) 0.0406(16) Uani 1 1 d . . . H52 H -0.3212 0.0170 -0.5237 0.049 Uiso 1 1 calc R . . C53 C -0.4050(4) 0.2454(5) -0.5274(3) 0.0388(16) Uani 1 1 d . . . C54 C -0.4818(5) 0.2466(7) -0.5518(4) 0.073(3) Uani 1 1 d . . . H54 H -0.5129 0.1991 -0.5481 0.088 Uiso 1 1 calc R . . C55 C -0.5118(6) 0.3217(7) -0.5824(5) 0.084(4) Uani 1 1 d . . . H55 H -0.5635 0.3236 -0.5991 0.101 Uiso 1 1 calc R . . C56 C -0.4664(6) 0.3923(6) -0.5880(4) 0.064(2) Uani 1 1 d . . . H56 H -0.4870 0.4416 -0.6084 0.077 Uiso 1 1 calc R . . C57 C -0.3900(5) 0.3888(6) -0.5631(4) 0.056(2) Uani 1 1 d . . . H57 H -0.3588 0.4362 -0.5670 0.067 Uiso 1 1 calc R . . C58 C -0.3587(5) 0.3159(6) -0.5322(4) 0.051(2) Uani 1 1 d . . . H58 H -0.3071 0.3147 -0.5149 0.062 Uiso 1 1 calc R . . C59 C 0.0206(8) -0.0425(13) 0.7902(8) 0.144(8) Uani 1 1 d . . . H59A H 0.0538 -0.0936 0.7961 0.172 Uiso 1 1 calc R . . H59B H -0.0297 -0.0626 0.7713 0.172 Uiso 1 1 calc R . . C60 C 0.5505(6) -0.0366(8) 0.7103(6) 0.085(3) Uani 1 1 d . . . H60A H 0.5692 -0.0050 0.6816 0.102 Uiso 1 1 calc R . . H60B H 0.5943 -0.0562 0.7384 0.102 Uiso 1 1 calc R . . Ag1 Ag 0.0000 0.0000 0.0000 0.0361(2) Uani 1 2 d S . . Ag2 Ag -0.5000 0.0000 -0.5000 0.0387(2) Uani 1 2 d S . . Cl1 Cl 0.0494(3) 0.0203(4) 0.75094(15) 0.160(2) Uani 1 1 d . . . Cl2 Cl 0.01449(19) 0.0001(2) 0.85820(14) 0.0905(9) Uani 1 1 d . . . Cl3 Cl 0.49596(18) 0.0353(2) 0.74178(15) 0.0979(10) Uani 1 1 d . . . Cl4 Cl 0.49921(17) -0.1276(2) 0.68047(14) 0.0915(9) Uani 1 1 d . . . F5 F -0.2410(6) 0.7564(8) -0.1945(5) 0.182(6) Uani 1 1 d . A . F3 F -0.2648(5) 0.9097(6) -0.2154(7) 0.207(7) Uani 1 1 d . A . Fe1 Fe -0.23421(6) 0.21335(7) -0.23542(4) 0.0313(3) Uani 1 1 d . . . N1 N -0.1676(3) 0.2507(4) -0.0753(2) 0.0311(12) Uani 1 1 d . . . N2 N -0.3403(3) 0.2317(4) -0.3995(2) 0.0333(12) Uani 1 1 d . . . O1 O -0.1916(2) 0.0879(3) -0.06710(18) 0.0333(10) Uani 1 1 d . . . O2 O -0.1488(2) 0.1705(3) 0.01963(18) 0.0333(10) Uani 1 1 d . . . O3 O -0.3098(2) 0.0761(3) -0.42194(19) 0.0351(10) Uani 1 1 d . . . O4 O -0.3721(3) 0.1691(3) -0.49933(19) 0.0361(11) Uani 1 1 d . . . Sb1 Sb -0.21249(4) 0.83046(5) -0.24421(3) 0.0654(2) Uani 1 1 d . . . P1 P -0.13455(9) 0.31234(11) -0.11700(7) 0.0300(4) Uani 1 1 d . . . P2 P -0.13409(9) 0.16515(11) -0.04275(7) 0.0302(4) Uani 1 1 d . . . P3 P -0.36686(9) 0.28314(11) -0.35021(7) 0.0303(4) Uani 1 1 d . . . P4 P -0.37380(9) 0.14983(11) -0.43551(7) 0.0307(4) Uani 1 1 d . . . S1 S -0.02584(9) 0.14002(12) -0.04245(7) 0.0364(4) Uani 1 1 d . . . S2 S -0.47440(9) 0.10598(12) -0.42680(8) 0.0412(4) Uani 1 1 d . . . F1 F -0.1806(5) 0.8980(12) -0.2795(7) 0.267(10) Uani 1 1 d . A . F2 F -0.1242(5) 0.8562(10) -0.1936(4) 0.177(5) Uani 1 1 d . A . F6B F -0.1473(10) 0.7267(11) -0.2479(7) 0.113(3) Uiso 0.50 1 d PU A 1 F4 F -0.3001(8) 0.8056(13) -0.2930(4) 0.260(10) Uani 1 1 d . A . F6A F -0.1845(10) 0.7653(11) -0.2979(7) 0.113(3) Uiso 0.50 1 d PU 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 C1 0.024(3) 0.037(4) 0.041(4) 0.002(3) 0.002(3) -0.002(3) C2 0.031(3) 0.049(5) 0.044(4) -0.004(3) 0.006(3) -0.001(3) C3 0.030(4) 0.042(5) 0.078(6) -0.008(4) 0.006(4) 0.005(3) C4 0.042(4) 0.035(4) 0.064(5) 0.012(4) -0.007(4) -0.006(3) C5 0.066(5) 0.050(5) 0.051(5) 0.007(4) 0.013(4) -0.011(4) C6 0.057(5) 0.039(4) 0.047(4) 0.003(3) 0.019(4) -0.005(4) C7 0.033(3) 0.044(4) 0.030(3) 0.003(3) 0.007(3) -0.003(3) C8 0.041(4) 0.065(6) 0.044(4) -0.007(4) -0.004(3) 0.010(4) C9 0.041(4) 0.091(7) 0.052(5) -0.016(5) -0.007(4) -0.003(5) C10 0.048(5) 0.069(6) 0.059(5) -0.021(5) 0.017(4) -0.016(4) C11 0.053(5) 0.047(5) 0.052(5) -0.006(4) 0.019(4) -0.003(4) C12 0.035(4) 0.047(4) 0.045(4) 0.004(3) 0.013(3) 0.000(3) C13 0.032(3) 0.029(4) 0.046(4) 0.007(3) 0.003(3) 0.003(3) C14 0.037(4) 0.040(4) 0.055(5) 0.003(3) 0.003(3) -0.003(3) C15 0.044(4) 0.042(5) 0.064(5) 0.001(4) -0.011(4) -0.008(4) C16 0.044(5) 0.044(5) 0.081(6) 0.016(5) -0.010(4) -0.014(4) C17 0.029(4) 0.071(6) 0.098(8) 0.018(6) 0.019(4) 0.003(4) C18 0.033(4) 0.053(5) 0.056(5) 0.011(4) 0.007(3) 0.001(3) C19 0.039(4) 0.031(4) 0.030(3) -0.002(3) -0.001(3) 0.004(3) C20 0.056(5) 0.038(4) 0.059(5) 0.012(4) 0.013(4) 0.003(4) C21 0.066(6) 0.040(5) 0.069(6) 0.012(4) 0.014(5) 0.007(4) C22 0.075(6) 0.038(5) 0.052(5) 0.006(4) 0.002(4) 0.020(4) C23 0.048(5) 0.065(6) 0.043(4) -0.003(4) 0.004(4) 0.022(4) C24 0.039(4) 0.038(4) 0.034(3) -0.002(3) 0.004(3) 0.006(3) C25 0.027(3) 0.042(4) 0.031(3) -0.001(3) 0.003(3) 0.004(3) C26 0.044(4) 0.040(4) 0.041(4) 0.004(3) 0.011(3) 0.013(3) C27 0.044(4) 0.050(5) 0.040(4) -0.007(3) 0.009(3) 0.017(3) C28 0.031(3) 0.059(5) 0.036(4) 0.006(3) 0.008(3) 0.007(3) C29 0.030(3) 0.051(4) 0.031(3) 0.005(3) 0.005(3) -0.001(3) C30 0.039(4) 0.057(5) 0.037(4) 0.003(4) 0.005(3) -0.013(4) C31 0.050(4) 0.036(4) 0.045(4) 0.008(3) -0.002(3) -0.008(3) C32 0.048(4) 0.036(4) 0.044(4) -0.004(3) 0.009(3) -0.009(3) C33 0.032(3) 0.041(4) 0.032(3) -0.003(3) 0.007(3) -0.007(3) C34 0.030(3) 0.038(4) 0.040(4) -0.002(3) 0.007(3) 0.001(3) C35 0.031(3) 0.033(4) 0.043(4) -0.010(3) 0.002(3) 0.004(3) C36 0.035(4) 0.043(4) 0.055(5) -0.004(4) -0.003(3) 0.005(3) C37 0.045(5) 0.049(5) 0.074(6) -0.018(4) -0.008(4) 0.014(4) C38 0.024(4) 0.071(6) 0.101(8) -0.034(6) -0.001(4) 0.008(4) C39 0.034(4) 0.070(6) 0.080(6) -0.021(5) 0.013(4) -0.003(4) C40 0.029(3) 0.050(5) 0.057(5) -0.012(4) 0.012(3) -0.003(3) C41 0.034(3) 0.036(4) 0.031(3) -0.004(3) 0.001(3) -0.001(3) C42 0.046(4) 0.043(5) 0.055(5) -0.006(4) 0.014(4) 0.002(3) C43 0.069(6) 0.039(5) 0.055(5) -0.014(4) 0.008(4) -0.002(4) C44 0.068(6) 0.038(5) 0.057(5) -0.003(4) 0.005(4) -0.017(4) C45 0.055(5) 0.043(5) 0.042(4) 0.000(3) 0.007(4) -0.013(4) C46 0.037(4) 0.046(4) 0.032(3) 0.000(3) 0.001(3) -0.002(3) C47 0.023(3) 0.040(4) 0.047(4) -0.008(3) 0.002(3) -0.001(3) C48 0.058(5) 0.042(5) 0.046(4) -0.001(4) 0.006(4) 0.006(4) C49 0.058(5) 0.034(4) 0.061(5) 0.005(4) 0.000(4) 0.004(4) C50 0.040(4) 0.036(4) 0.068(5) -0.011(4) 0.003(4) 0.005(3) C51 0.039(4) 0.048(5) 0.054(5) -0.019(4) 0.006(3) 0.003(3) C52 0.034(4) 0.038(4) 0.050(4) -0.005(3) 0.009(3) 0.003(3) C53 0.042(4) 0.037(4) 0.036(4) -0.003(3) 0.005(3) -0.001(3) C54 0.044(5) 0.071(7) 0.088(7) 0.022(6) -0.022(5) -0.017(5) C55 0.056(6) 0.083(8) 0.094(8) 0.039(6) -0.024(5) 0.003(5) C56 0.070(6) 0.051(5) 0.064(6) 0.013(4) -0.001(5) 0.006(5) C57 0.049(5) 0.044(5) 0.074(6) 0.008(4) 0.010(4) 0.002(4) C58 0.037(4) 0.055(5) 0.061(5) 0.005(4) 0.010(4) 0.004(4) C59 0.076(9) 0.179(17) 0.194(18) -0.096(15) 0.070(11) -0.043(10) C60 0.055(6) 0.094(8) 0.108(9) 0.012(7) 0.024(6) -0.016(6) Ag1 0.0310(4) 0.0352(4) 0.0412(4) 0.0073(3) 0.0063(3) 0.0071(3) Ag2 0.0331(4) 0.0359(4) 0.0439(4) -0.0094(3) 0.0017(3) -0.0060(3) Cl1 0.136(3) 0.276(6) 0.071(2) 0.046(3) 0.028(2) 0.110(4) Cl2 0.0867(19) 0.110(2) 0.0830(18) 0.0006(16) 0.0366(16) 0.0227(17) Cl3 0.0715(17) 0.118(3) 0.114(2) -0.012(2) 0.0405(17) -0.0265(17) Cl4 0.0690(16) 0.092(2) 0.111(2) 0.0048(17) 0.0145(15) -0.0200(15) F5 0.120(7) 0.185(10) 0.264(13) 0.151(10) 0.088(8) 0.050(7) F3 0.097(6) 0.094(6) 0.45(2) -0.006(9) 0.108(10) 0.036(5) Fe1 0.0309(5) 0.0314(6) 0.0309(5) -0.0004(4) 0.0054(4) 0.0017(4) N1 0.027(3) 0.035(3) 0.031(3) 0.005(2) 0.005(2) 0.002(2) N2 0.028(3) 0.035(3) 0.035(3) -0.008(2) 0.003(2) -0.005(2) O1 0.032(2) 0.032(3) 0.033(2) 0.0022(19) 0.0011(18) -0.0013(19) O2 0.031(2) 0.038(3) 0.032(2) -0.0010(19) 0.0085(18) -0.0035(19) O3 0.030(2) 0.035(3) 0.038(2) -0.008(2) 0.0015(19) 0.0026(19) O4 0.037(2) 0.034(3) 0.037(2) -0.006(2) 0.008(2) 0.000(2) Sb1 0.0749(5) 0.0631(4) 0.0608(4) -0.0007(3) 0.0209(3) 0.0030(3) P1 0.0238(7) 0.0343(9) 0.0304(8) 0.0041(7) 0.0029(6) 0.0012(6) P2 0.0248(8) 0.0335(9) 0.0314(8) 0.0049(7) 0.0045(6) 0.0012(6) P3 0.0253(8) 0.0317(9) 0.0328(8) -0.0046(7) 0.0039(6) -0.0018(6) P4 0.0250(8) 0.0333(9) 0.0323(8) -0.0067(7) 0.0031(6) -0.0023(7) S1 0.0258(7) 0.0367(9) 0.0466(9) 0.0120(7) 0.0078(7) 0.0061(7) S2 0.0304(8) 0.0456(10) 0.0484(10) -0.0164(8) 0.0105(7) -0.0091(7) F1 0.078(6) 0.41(2) 0.329(18) -0.209(18) 0.083(9) -0.132(10) F2 0.071(5) 0.376(18) 0.088(5) -0.008(8) 0.024(4) -0.012(7) F4 0.192(11) 0.50(3) 0.081(6) -0.017(10) 0.005(6) -0.222(15) _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 C1 C2 1.363(10) . ? C1 C6 1.386(10) . ? C1 O1 1.399(8) . ? C2 C3 1.389(12) . ? C3 C4 1.374(12) . ? C4 C5 1.357(12) . ? C5 C6 1.396(12) . ? C7 C8 1.365(10) . ? C7 C12 1.385(10) . ? C7 O2 1.405(8) . ? C8 C9 1.385(12) . ? C9 C10 1.378(14) . ? C10 C11 1.378(12) . ? C11 C12 1.386(11) . ? C13 C14 1.390(11) . ? C13 C18 1.393(11) . ? C13 P1 1.798(7) . ? C14 C15 1.379(10) . ? C15 C16 1.367(13) . ? C16 C17 1.374(14) . ? C17 C18 1.386(12) . ? C19 C24 1.385(10) . ? C19 C20 1.387(11) . ? C19 P1 1.801(7) . ? C20 C21 1.391(12) . ? C21 C22 1.331(13) . ? C22 C23 1.400(13) . ? C23 C24 1.385(11) . ? C25 C29 1.432(9) . ? C25 C26 1.434(10) . ? C25 P1 1.783(7) . ? C25 Fe1 2.025(7) . ? C26 C27 1.417(10) . ? C26 Fe1 2.046(7) . ? C27 C28 1.404(11) . ? C27 Fe1 2.066(7) . ? C28 C29 1.409(11) . ? C28 Fe1 2.059(7) . ? C29 Fe1 2.036(7) . ? C30 C31 1.401(12) . ? C30 C34 1.425(11) . ? C30 Fe1 2.049(8) . ? C31 C32 1.429(11) . ? C31 Fe1 2.043(8) . ? C32 C33 1.427(11) . ? C32 Fe1 2.034(7) . ? C33 C34 1.440(9) . ? C33 P3 1.777(7) . ? C33 Fe1 2.031(7) . ? C34 Fe1 2.044(7) . ? C35 C40 1.378(11) . ? C35 C36 1.406(11) . ? C35 P3 1.804(7) . ? C36 C37 1.395(11) . ? C37 C38 1.358(14) . ? C38 C39 1.382(15) . ? C39 C40 1.382(11) . ? C41 C46 1.375(10) . ? C41 C42 1.392(10) . ? C41 P3 1.801(7) . ? C42 C43 1.395(12) . ? C43 C44 1.360(13) . ? C44 C45 1.377(12) . ? C45 C46 1.378(11) . ? C47 C48 1.369(11) . ? C47 C52 1.373(10) . ? C47 O3 1.409(8) . ? C48 C49 1.386(11) . ? C49 C50 1.371(12) . ? C50 C51 1.370(12) . ? C51 C52 1.390(11) . ? C53 C58 1.377(11) . ? C53 C54 1.378(11) . ? C53 O4 1.407(9) . ? C54 C55 1.403(13) . ? C55 C56 1.373(14) . ? C56 C57 1.376(13) . ? C57 C58 1.386(12) . ? C59 Cl1 1.52(2) . ? C59 Cl2 1.810(16) . ? C60 Cl4 1.730(12) . ? C60 Cl3 1.754(13) . ? Ag1 S1 2.3657(17) . ? Ag1 S1 2.3657(17) 3 ? Ag2 S2 2.3740(17) . ? Ag2 S2 2.3741(17) 3_454 ? F5 Sb1 1.811(8) . ? F3 Sb1 1.767(10) . ? N1 P2 1.572(5) . ? N1 P1 1.592(5) . ? N2 P4 1.564(5) . ? N2 P3 1.595(6) . ? O1 P2 1.590(5) . ? O2 P2 1.606(5) . ? O3 P4 1.587(5) . ? O4 P4 1.594(5) . ? Sb1 F1 1.531(18) . ? Sb1 F4 1.793(10) . ? Sb1 F6A 1.802(16) . ? Sb1 F2 1.826(9) . ? Sb1 F6B 1.977(17) . ? P2 S1 1.982(2) . ? P4 S2 1.983(2) . ? 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 C2 C1 C6 121.4(7) . . ? C2 C1 O1 119.2(6) . . ? C6 C1 O1 119.2(6) . . ? C1 C2 C3 119.2(8) . . ? C4 C3 C2 120.6(8) . . ? C5 C4 C3 119.3(8) . . ? C4 C5 C6 121.7(8) . . ? C1 C6 C5 117.7(8) . . ? C8 C7 C12 121.8(7) . . ? C8 C7 O2 120.6(7) . . ? C12 C7 O2 117.7(6) . . ? C7 C8 C9 118.8(8) . . ? C10 C9 C8 120.6(8) . . ? C9 C10 C11 119.9(8) . . ? C10 C11 C12 120.1(8) . . ? C7 C12 C11 118.8(7) . . ? C14 C13 C18 119.0(7) . . ? C14 C13 P1 118.4(6) . . ? C18 C13 P1 122.6(6) . . ? C15 C14 C13 120.5(8) . . ? C16 C15 C14 119.8(8) . . ? C15 C16 C17 120.8(8) . . ? C16 C17 C18 120.0(9) . . ? C17 C18 C13 119.8(8) . . ? C24 C19 C20 120.0(7) . . ? C24 C19 P1 120.5(5) . . ? C20 C19 P1 119.4(6) . . ? C19 C20 C21 119.4(8) . . ? C22 C21 C20 120.7(9) . . ? C21 C22 C23 121.1(8) . . ? C24 C23 C22 119.1(8) . . ? C23 C24 C19 119.6(7) . . ? C29 C25 C26 107.4(6) . . ? C29 C25 P1 127.6(6) . . ? C26 C25 P1 125.0(5) . . ? C29 C25 Fe1 69.7(4) . . ? C26 C25 Fe1 70.2(4) . . ? P1 C25 Fe1 126.2(4) . . ? C27 C26 C25 107.6(6) . . ? C27 C26 Fe1 70.6(4) . . ? C25 C26 Fe1 68.6(4) . . ? C28 C27 C26 108.4(7) . . ? C28 C27 Fe1 69.8(4) . . ? C26 C27 Fe1 69.1(4) . . ? C27 C28 C29 109.0(6) . . ? C27 C28 Fe1 70.4(4) . . ? C29 C28 Fe1 69.0(4) . . ? C28 C29 C25 107.6(7) . . ? C28 C29 Fe1 70.7(4) . . ? C25 C29 Fe1 69.0(4) . . ? C31 C30 C34 109.1(7) . . ? C31 C30 Fe1 69.8(5) . . ? C34 C30 Fe1 69.4(4) . . ? C30 C31 C32 108.7(7) . . ? C30 C31 Fe1 70.2(4) . . ? C32 C31 Fe1 69.1(4) . . ? C33 C32 C31 107.1(7) . . ? C33 C32 Fe1 69.3(4) . . ? C31 C32 Fe1 69.8(4) . . ? C32 C33 C34 108.4(6) . . ? C32 C33 P3 125.4(5) . . ? C34 C33 P3 126.1(6) . . ? C32 C33 Fe1 69.6(4) . . ? C34 C33 Fe1 69.8(4) . . ? P3 C33 Fe1 127.9(4) . . ? C30 C34 C33 106.7(7) . . ? C30 C34 Fe1 69.8(4) . . ? C33 C34 Fe1 68.8(4) . . ? C40 C35 C36 120.4(7) . . ? C40 C35 P3 122.5(6) . . ? C36 C35 P3 117.1(6) . . ? C37 C36 C35 118.2(8) . . ? C38 C37 C36 120.8(9) . . ? C37 C38 C39 120.8(8) . . ? C38 C39 C40 119.8(9) . . ? C35 C40 C39 120.0(8) . . ? C46 C41 C42 120.0(7) . . ? C46 C41 P3 120.9(5) . . ? C42 C41 P3 119.1(6) . . ? C41 C42 C43 119.2(8) . . ? C44 C43 C42 120.5(8) . . ? C43 C44 C45 119.9(8) . . ? C44 C45 C46 120.7(8) . . ? C41 C46 C45 119.7(7) . . ? C48 C47 C52 121.5(7) . . ? C48 C47 O3 117.3(7) . . ? C52 C47 O3 121.0(7) . . ? C47 C48 C49 118.8(8) . . ? C50 C49 C48 121.0(8) . . ? C51 C50 C49 119.1(7) . . ? C50 C51 C52 121.1(8) . . ? C47 C52 C51 118.5(8) . . ? C58 C53 C54 121.3(8) . . ? C58 C53 O4 119.0(6) . . ? C54 C53 O4 119.6(7) . . ? C53 C54 C55 118.2(9) . . ? C56 C55 C54 121.4(9) . . ? C55 C56 C57 118.9(8) . . ? C56 C57 C58 121.2(8) . . ? C53 C58 C57 119.1(8) . . ? Cl1 C59 Cl2 117(1) . . ? Cl4 C60 Cl3 112.6(6) . . ? S1 Ag1 S1 180. 3 . . . ? S2 Ag2 S2 180.3_454 ? C25 Fe1 C33 150.6(3) . . ? C25 Fe1 C32 167.7(3) . . ? C33 Fe1 C32 41.1(3) . . ? C25 Fe1 C29 41.3(3) . . ? C33 Fe1 C29 117.9(3) . . ? C32 Fe1 C29 148.2(3) . . ? C25 Fe1 C31 129.9(3) . . ? C33 Fe1 C31 68.7(3) . . ? C32 Fe1 C31 41.0(3) . . ? C29 Fe1 C31 170.7(3) . . ? C25 Fe1 C34 117.6(3) . . ? C33 Fe1 C34 41.4(3) . . ? C32 Fe1 C34 69.5(3) . . ? C29 Fe1 C34 111.4(3) . . ? C31 Fe1 C34 68.6(3) . . ? C25 Fe1 C26 41.2(3) . . ? C33 Fe1 C26 167.5(3) . . ? C32 Fe1 C26 127.6(3) . . ? C29 Fe1 C26 68.9(3) . . ? C31 Fe1 C26 106.0(3) . . ? C34 Fe1 C26 148.7(3) . . ? C25 Fe1 C30 109.6(3) . . ? C33 Fe1 C30 68.6(3) . . ? C32 Fe1 C30 68.6(3) . . ? C29 Fe1 C30 134.1(3) . . ? C31 Fe1 C30 40.1(3) . . ? C34 Fe1 C30 40.8(3) . . ? C26 Fe1 C30 115.2(3) . . ? C25 Fe1 C28 68.3(3) . . ? C33 Fe1 C28 109.9(3) . . ? C32 Fe1 C28 114.9(3) . . ? C29 Fe1 C28 40.2(3) . . ? C31 Fe1 C28 146.2(3) . . ? C34 Fe1 C28 133.9(3) . . ? C26 Fe1 C28 67.7(3) . . ? C30 Fe1 C28 173.3(3) . . ? C25 Fe1 C27 68.4(3) . . ? C33 Fe1 C27 130.2(3) . . ? C32 Fe1 C27 106.0(3) . . ? C29 Fe1 C27 67.9(3) . . ? C31 Fe1 C27 113.7(3) . . ? C34 Fe1 C27 170.8(3) . . ? C26 Fe1 C27 40.3(3) . . ? C30 Fe1 C27 146.1(3) . . ? C28 Fe1 C27 39.8(3) . . ? P2 N1 P1 130.9(4) . . ? P4 N2 P3 132.3(4) . . ? C1 O1 P2 124.3(4) . . ? C7 O2 P2 119.5(4) . . ? C47 O3 P4 124.7(4) . . ? C53 O4 P4 122.2(4) . . ? F1 Sb1 F3 93.9(7) . . ? F1 Sb1 F4 98.7(6) . . ? F3 Sb1 F4 86.6(8) . . ? F1 Sb1 F6A 75.9(7) . . ? F3 Sb1 F6A 157.4(8) . . ? F4 Sb1 F6A 75.3(8) . . ? F1 Sb1 F5 172.3(6) . . ? F3 Sb1 F5 84.2(6) . . ? F4 Sb1 F5 88.7(6) . . ? F6A Sb1 F5 108.4(7) . . ? F1 Sb1 F2 81.9(6) . . ? F3 Sb1 F2 92.6(6) . . ? F4 Sb1 F2 179.0(5) . . ? F6A Sb1 F2 105.6(6) . . ? F5 Sb1 F2 90.7(5) . . ? F1 Sb1 F6B 102.0(7) . . ? F3 Sb1 F6B 159.0(7) . . ? F4 Sb1 F6B 104.2(8) . . ? F6A Sb1 F6B 42.7(6) . . ? F5 Sb1 F6B 78.2(6) . . ? F2 Sb1 F6B 76.5(6) . . ? N1 P1 C25 114.1(3) . . ? N1 P1 C13 113.7(3) . . ? C25 P1 C13 107.4(3) . . ? N1 P1 C19 108.0(3) . . ? C25 P1 C19 106.6(3) . . ? C13 P1 C19 106.5(3) . . ? N1 P2 O1 106.0(3) . . ? N1 P2 O2 108.3(3) . . ? O1 P2 O2 99.3(2) . . ? N1 P2 S1 115.3(2) . . ? O1 P2 S1 114.6(2) . . ? O2 P2 S1 111.97(18) . . ? N2 P3 C33 112.2(3) . . ? N2 P3 C41 107.5(3) . . ? C33 P3 C41 109.0(3) . . ? N2 P3 C35 114.8(3) . . ? C33 P3 C35 107.5(3) . . ? C41 P3 C35 105.6(3) . . ? N2 P4 O3 105.8(3) . . ? N2 P4 O4 108.5(3) . . ? O3 P4 O4 99.4(3) . . ? N2 P4 S2 116.9(2) . . ? O3 P4 S2 112.2(2) . . ? O4 P4 S2 112.48(19) . . ? P2 S1 Ag1 105.77(9) . . ? P4 S2 Ag2 100.11(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.4(11) . . . . ? O1 C1 C2 C3 -176.3(6) . . . . ? C1 C2 C3 C4 -0.3(11) . . . . ? C2 C3 C4 C5 1.6(12) . . . . ? C3 C4 C5 C6 -1.0(13) . . . . ? C2 C1 C6 C5 1.9(12) . . . . ? O1 C1 C6 C5 176.8(7) . . . . ? C4 C5 C6 C1 -0.7(13) . . . . ? C12 C7 C8 C9 -0.1(13) . . . . ? O2 C7 C8 C9 -179.4(7) . . . . ? C7 C8 C9 C10 -0.7(14) . . . . ? C8 C9 C10 C11 1.6(15) . . . . ? C9 C10 C11 C12 -1.8(13) . . . . ? C8 C7 C12 C11 -0.1(11) . . . . ? O2 C7 C12 C11 179.3(6) . . . . ? C10 C11 C12 C7 1.0(12) . . . . ? C18 C13 C14 C15 -0.5(11) . . . . ? P1 C13 C14 C15 178.7(6) . . . . ? C13 C14 C15 C16 0.4(12) . . . . ? C14 C15 C16 C17 0.3(13) . . . . ? C15 C16 C17 C18 -1.0(14) . . . . ? C16 C17 C18 C13 0.9(13) . . . . ? C14 C13 C18 C17 -0.1(11) . . . . ? P1 C13 C18 C17 -179.3(7) . . . . ? C24 C19 C20 C21 -0.9(12) . . . . ? P1 C19 C20 C21 175.5(7) . . . . ? C19 C20 C21 C22 -0.3(14) . . . . ? C20 C21 C22 C23 0.5(14) . . . . ? C21 C22 C23 C24 0.5(13) . . . . ? C22 C23 C24 C19 -1.6(11) . . . . ? C20 C19 C24 C23 1.8(10) . . . . ? P1 C19 C24 C23 -174.6(6) . . . . ? C29 C25 C26 C27 0.1(8) . . . . ? P1 C25 C26 C27 -179.0(5) . . . . ? Fe1 C25 C26 C27 60.1(5) . . . . ? C29 C25 C26 Fe1 -60.1(5) . . . . ? P1 C25 C26 Fe1 120.9(5) . . . . ? C25 C26 C27 C28 0.1(9) . . . . ? Fe1 C26 C27 C28 58.9(5) . . . . ? C25 C26 C27 Fe1 -58.9(5) . . . . ? C26 C27 C28 C29 -0.2(9) . . . . ? Fe1 C27 C28 C29 58.3(5) . . . . ? C26 C27 C28 Fe1 -58.5(5) . . . . ? C27 C28 C29 C25 0.2(8) . . . . ? Fe1 C28 C29 C25 59.4(5) . . . . ? C27 C28 C29 Fe1 -59.2(5) . . . . ? C26 C25 C29 C28 -0.2(8) . . . . ? P1 C25 C29 C28 178.8(5) . . . . ? Fe1 C25 C29 C28 -60.5(5) . . . . ? C26 C25 C29 Fe1 60.3(5) . . . . ? P1 C25 C29 Fe1 -120.7(6) . . . . ? C34 C30 C31 C32 -0.2(9) . . . . ? Fe1 C30 C31 C32 -58.6(5) . . . . ? C34 C30 C31 Fe1 58.4(5) . . . . ? C30 C31 C32 C33 -0.3(9) . . . . ? Fe1 C31 C32 C33 -59.5(5) . . . . ? C30 C31 C32 Fe1 59.2(5) . . . . ? C31 C32 C33 C34 0.6(8) . . . . ? Fe1 C32 C33 C34 -59.2(5) . . . . ? C31 C32 C33 P3 -177.4(5) . . . . ? Fe1 C32 C33 P3 122.7(5) . . . . ? C31 C32 C33 Fe1 59.9(5) . . . . ? C31 C30 C34 C33 0.6(8) . . . . ? Fe1 C30 C34 C33 59.2(4) . . . . ? C31 C30 C34 Fe1 -58.6(5) . . . . ? C32 C33 C34 C30 -0.7(8) . . . . ? P3 C33 C34 C30 177.3(5) . . . . ? Fe1 C33 C34 C30 -59.8(5) . . . . ? C32 C33 C34 Fe1 59.1(5) . . . . ? P3 C33 C34 Fe1 -122.9(5) . . . . ? C40 C35 C36 C37 0.6(11) . . . . ? P3 C35 C36 C37 179.7(6) . . . . ? C35 C36 C37 C38 0.9(12) . . . . ? C36 C37 C38 C39 -1.6(14) . . . . ? C37 C38 C39 C40 0.8(14) . . . . ? C36 C35 C40 C39 -1.4(11) . . . . ? P3 C35 C40 C39 179.6(6) . . . . ? C38 C39 C40 C35 0.7(13) . . . . ? C46 C41 C42 C43 -0.8(11) . . . . ? P3 C41 C42 C43 177.8(6) . . . . ? C41 C42 C43 C44 -1.1(13) . . . . ? C42 C43 C44 C45 2.4(13) . . . . ? C43 C44 C45 C46 -1.8(13) . . . . ? C42 C41 C46 C45 1.4(11) . . . . ? P3 C41 C46 C45 -177.3(6) . . . . ? C44 C45 C46 C41 -0.1(12) . . . . ? C52 C47 C48 C49 -2.3(12) . . . . ? O3 C47 C48 C49 -177.1(7) . . . . ? C47 C48 C49 C50 1.1(13) . . . . ? C48 C49 C50 C51 0.0(13) . . . . ? C49 C50 C51 C52 -0.1(12) . . . . ? C48 C47 C52 C51 2.3(11) . . . . ? O3 C47 C52 C51 176.9(6) . . . . ? C50 C51 C52 C47 -1.1(11) . . . . ? C58 C53 C54 C55 0.8(16) . . . . ? O4 C53 C54 C55 -176.2(9) . . . . ? C53 C54 C55 C56 -0.1(19) . . . . ? C54 C55 C56 C57 0.0(18) . . . . ? C55 C56 C57 C58 -0.5(16) . . . . ? C54 C53 C58 C57 -1.3(13) . . . . ? O4 C53 C58 C57 175.7(7) . . . . ? C56 C57 C58 C53 1.2(14) . . . . ? C29 C25 Fe1 C33 -54.7(7) . . . . ? C26 C25 Fe1 C33 -172.9(5) . . . . ? P1 C25 Fe1 C33 67.7(8) . . . . ? C29 C25 Fe1 C32 145.4(13) . . . . ? C26 C25 Fe1 C32 27.2(15) . . . . ? P1 C25 Fe1 C32 -92.2(14) . . . . ? C26 C25 Fe1 C29 -118.2(6) . . . . ? P1 C25 Fe1 C29 122.4(7) . . . . ? C29 C25 Fe1 C31 -176.0(5) . . . . ? C26 C25 Fe1 C31 65.8(5) . . . . ? P1 C25 Fe1 C31 -53.6(6) . . . . ? C29 C25 Fe1 C34 -91.7(5) . . . . ? C26 C25 Fe1 C34 150.1(4) . . . . ? P1 C25 Fe1 C34 30.6(6) . . . . ? C29 C25 Fe1 C26 118.2(6) . . . . ? P1 C25 Fe1 C26 -119.4(7) . . . . ? C29 C25 Fe1 C30 -135.6(4) . . . . ? C26 C25 Fe1 C30 106.2(5) . . . . ? P1 C25 Fe1 C30 -13.2(6) . . . . ? C29 C25 Fe1 C28 37.7(4) . . . . ? C26 C25 Fe1 C28 -80.5(4) . . . . ? P1 C25 Fe1 C28 160.0(6) . . . . ? C29 C25 Fe1 C27 80.6(5) . . . . ? C26 C25 Fe1 C27 -37.6(4) . . . . ? P1 C25 Fe1 C27 -157.0(6) . . . . ? C32 C33 Fe1 C25 -173.6(5) . . . . ? C34 C33 Fe1 C25 -53.9(7) . . . . ? P3 C33 Fe1 C25 66.8(8) . . . . ? C34 C33 Fe1 C32 119.7(6) . . . . ? P3 C33 Fe1 C32 -119.6(7) . . . . ? C32 C33 Fe1 C29 148.9(4) . . . . ? C34 C33 Fe1 C29 -91.4(5) . . . . ? P3 C33 Fe1 C29 29.2(6) . . . . ? C32 C33 Fe1 C31 -38.3(4) . . . . ? C34 C33 Fe1 C31 81.4(5) . . . . ? P3 C33 Fe1 C31 -158.0(6) . . . . ? C32 C33 Fe1 C34 -119.7(6) . . . . ? P3 C33 Fe1 C34 120.7(7) . . . . ? C32 C33 Fe1 C26 28.5(15) . . . . ? C34 C33 Fe1 C26 148.2(13) . . . . ? P3 C33 Fe1 C26 -91.1(14) . . . . ? C32 C33 Fe1 C30 -81.5(5) . . . . ? C34 C33 Fe1 C30 38.2(4) . . . . ? P3 C33 Fe1 C30 158.9(6) . . . . ? C32 C33 Fe1 C28 105.5(5) . . . . ? C34 C33 Fe1 C28 -134.8(4) . . . . ? P3 C33 Fe1 C28 -14.2(6) . . . . ? C32 C33 Fe1 C27 65.2(5) . . . . ? C34 C33 Fe1 C27 -175.0(4) . . . . ? P3 C33 Fe1 C27 -54.4(7) . . . . ? C33 C32 Fe1 C25 165.1(12) . . . . ? C31 C32 Fe1 C25 46.8(16) . . . . ? C31 C32 Fe1 C33 -118.3(6) . . . . ? C33 C32 Fe1 C29 -60.1(7) . . . . ? C31 C32 Fe1 C29 -178.4(6) . . . . ? C33 C32 Fe1 C31 118.3(6) . . . . ? C33 C32 Fe1 C34 37.8(4) . . . . ? C31 C32 Fe1 C34 -80.5(5) . . . . ? C33 C32 Fe1 C26 -172.5(4) . . . . ? C31 C32 Fe1 C26 69.2(6) . . . . ? C33 C32 Fe1 C30 81.6(5) . . . . ? C31 C32 Fe1 C30 -36.7(5) . . . . ? C33 C32 Fe1 C28 -92.2(5) . . . . ? C31 C32 Fe1 C28 149.5(5) . . . . ? C33 C32 Fe1 C27 -133.8(4) . . . . ? C31 C32 Fe1 C27 107.9(5) . . . . ? C28 C29 Fe1 C25 118.5(6) . . . . ? C28 C29 Fe1 C33 -88.4(5) . . . . ? C25 C29 Fe1 C33 153.1(4) . . . . ? C28 C29 Fe1 C32 -48.2(8) . . . . ? C25 C29 Fe1 C32 -166.7(5) . . . . ? C28 C29 Fe1 C31 138.1(19) . . . . ? C25 C29 Fe1 C31 20(2) . . . . ? C28 C29 Fe1 C34 -133.6(4) . . . . ? C25 C29 Fe1 C34 107.8(4) . . . . ? C28 C29 Fe1 C26 80.0(4) . . . . ? C25 C29 Fe1 C26 -38.5(4) . . . . ? C28 C29 Fe1 C30 -174.8(4) . . . . ? C25 C29 Fe1 C30 66.7(6) . . . . ? C25 C29 Fe1 C28 -118.5(6) . . . . ? C28 C29 Fe1 C27 36.5(4) . . . . ? C25 C29 Fe1 C27 -82.0(4) . . . . ? C30 C31 Fe1 C25 71.6(5) . . . . ? C32 C31 Fe1 C25 -168.3(4) . . . . ? C30 C31 Fe1 C33 -81.7(5) . . . . ? C32 C31 Fe1 C33 38.4(5) . . . . ? C30 C31 Fe1 C32 -120.1(7) . . . . ? C30 C31 Fe1 C29 55(2) . . . . ? C32 C31 Fe1 C29 174.9(18) . . . . ? C30 C31 Fe1 C34 -37.1(4) . . . . ? C32 C31 Fe1 C34 83.0(5) . . . . ? C30 C31 Fe1 C26 110.3(5) . . . . ? C32 C31 Fe1 C26 -129.6(5) . . . . ? C32 C31 Fe1 C30 120.1(7) . . . . ? C30 C31 Fe1 C28 -176.0(5) . . . . ? C32 C31 Fe1 C28 -55.9(7) . . . . ? C30 C31 Fe1 C27 152.5(4) . . . . ? C32 C31 Fe1 C27 -87.4(5) . . . . ? C30 C34 Fe1 C25 -88.5(5) . . . . ? C33 C34 Fe1 C25 153.5(4) . . . . ? C30 C34 Fe1 C33 118.1(6) . . . . ? C30 C34 Fe1 C32 80.5(5) . . . . ? C33 C34 Fe1 C32 -37.6(4) . . . . ? C30 C34 Fe1 C29 -133.6(4) . . . . ? C33 C34 Fe1 C29 108.3(4) . . . . ? C30 C34 Fe1 C31 36.5(4) . . . . ? C33 C34 Fe1 C31 -81.6(4) . . . . ? C30 C34 Fe1 C26 -49.2(8) . . . . ? C33 C34 Fe1 C26 -167.3(5) . . . . ? C33 C34 Fe1 C30 -118.1(6) . . . . ? C30 C34 Fe1 C28 -174.1(5) . . . . ? C33 C34 Fe1 C28 67.8(6) . . . . ? C30 C34 Fe1 C27 142.5(19) . . . . ? C33 C34 Fe1 C27 24(2) . . . . ? C27 C26 Fe1 C25 -118.8(6) . . . . ? C27 C26 Fe1 C33 45.0(15) . . . . ? C25 C26 Fe1 C33 163.8(12) . . . . ? C27 C26 Fe1 C32 68.3(6) . . . . ? C25 C26 Fe1 C32 -172.9(4) . . . . ? C27 C26 Fe1 C29 -80.2(5) . . . . ? C25 C26 Fe1 C29 38.6(4) . . . . ? C27 C26 Fe1 C31 107.9(5) . . . . ? C25 C26 Fe1 C31 -133.3(4) . . . . ? C27 C26 Fe1 C34 -177.1(6) . . . . ? C25 C26 Fe1 C34 -58.3(7) . . . . ? C27 C26 Fe1 C30 149.8(5) . . . . ? C25 C26 Fe1 C30 -91.4(5) . . . . ? C27 C26 Fe1 C28 -36.8(5) . . . . ? C25 C26 Fe1 C28 82.0(5) . . . . ? C25 C26 Fe1 C27 118.8(6) . . . . ? C31 C30 Fe1 C25 -129.4(4) . . . . ? C34 C30 Fe1 C25 109.9(4) . . . . ? C31 C30 Fe1 C33 81.9(5) . . . . ? C34 C30 Fe1 C33 -38.8(4) . . . . ? C31 C30 Fe1 C32 37.6(4) . . . . ? C34 C30 Fe1 C32 -83.1(5) . . . . ? C31 C30 Fe1 C29 -169.4(4) . . . . ? C34 C30 Fe1 C29 69.8(5) . . . . ? C34 C30 Fe1 C31 -120.7(6) . . . . ? C31 C30 Fe1 C34 120.7(6) . . . . ? C31 C30 Fe1 C26 -85.0(5) . . . . ? C34 C30 Fe1 C26 154.2(4) . . . . ? C31 C30 Fe1 C28 160(2) . . . . ? C34 C30 Fe1 C28 40(3) . . . . ? C31 C30 Fe1 C27 -49.3(7) . . . . ? C34 C30 Fe1 C27 -170.0(5) . . . . ? C27 C28 Fe1 C25 81.9(5) . . . . ? C29 C28 Fe1 C25 -38.6(4) . . . . ? C27 C28 Fe1 C33 -129.5(4) . . . . ? C29 C28 Fe1 C33 110.0(4) . . . . ? C27 C28 Fe1 C32 -85.2(5) . . . . ? C29 C28 Fe1 C32 154.3(4) . . . . ? C27 C28 Fe1 C29 120.5(6) . . . . ? C27 C28 Fe1 C31 -48.4(7) . . . . ? C29 C28 Fe1 C31 -168.9(5) . . . . ? C27 C28 Fe1 C34 -170.2(4) . . . . ? C29 C28 Fe1 C34 69.3(5) . . . . ? C27 C28 Fe1 C26 37.3(4) . . . . ? C29 C28 Fe1 C26 -83.2(4) . . . . ? C27 C28 Fe1 C30 154(2) . . . . ? C29 C28 Fe1 C30 34(3) . . . . ? C29 C28 Fe1 C27 -120.5(6) . . . . ? C28 C27 Fe1 C25 -81.6(5) . . . . ? C26 C27 Fe1 C25 38.4(5) . . . . ? C28 C27 Fe1 C33 71.6(6) . . . . ? C26 C27 Fe1 C33 -168.4(4) . . . . ? C28 C27 Fe1 C32 110.0(5) . . . . ? C26 C27 Fe1 C32 -130.0(5) . . . . ? C28 C27 Fe1 C29 -36.9(4) . . . . ? C26 C27 Fe1 C29 83.1(5) . . . . ? C28 C27 Fe1 C31 153.0(4) . . . . ? C26 C27 Fe1 C31 -87.0(5) . . . . ? C28 C27 Fe1 C34 51(2) . . . . ? C26 C27 Fe1 C34 170.6(18) . . . . ? C28 C27 Fe1 C26 -120.0(7) . . . . ? C28 C27 Fe1 C30 -174.8(5) . . . . ? C26 C27 Fe1 C30 -54.8(7) . . . . ? C26 C27 Fe1 C28 120.0(7) . . . . ? C2 C1 O1 P2 -104.0(7) . . . . ? C6 C1 O1 P2 81.0(8) . . . . ? C8 C7 O2 P2 -89.5(7) . . . . ? C12 C7 O2 P2 91.1(7) . . . . ? C48 C47 O3 P4 -114.7(7) . . . . ? C52 C47 O3 P4 70.5(8) . . . . ? C58 C53 O4 P4 98.6(7) . . . . ? C54 C53 O4 P4 -84.3(9) . . . . ? P2 N1 P1 C25 74.1(5) . . . . ? P2 N1 P1 C13 -49.5(6) . . . . ? P2 N1 P1 C19 -167.5(4) . . . . ? C29 C25 P1 N1 142.5(6) . . . . ? C26 C25 P1 N1 -38.6(7) . . . . ? Fe1 C25 P1 N1 51.3(5) . . . . ? C29 C25 P1 C13 -90.5(6) . . . . ? C26 C25 P1 C13 88.3(7) . . . . ? Fe1 C25 P1 C13 178.2(4) . . . . ? C29 C25 P1 C19 23.3(7) . . . . ? C26 C25 P1 C19 -157.8(6) . . . . ? Fe1 C25 P1 C19 -67.9(5) . . . . ? C14 C13 P1 N1 -48.4(7) . . . . ? C18 C13 P1 N1 130.7(6) . . . . ? C14 C13 P1 C25 -175.7(6) . . . . ? C18 C13 P1 C25 3.5(7) . . . . ? C14 C13 P1 C19 70.4(6) . . . . ? C18 C13 P1 C19 -110.4(6) . . . . ? C24 C19 P1 N1 -28.0(6) . . . . ? C20 C19 P1 N1 155.6(6) . . . . ? C24 C19 P1 C25 95.1(6) . . . . ? C20 C19 P1 C25 -81.3(7) . . . . ? C24 C19 P1 C13 -150.5(5) . . . . ? C20 C19 P1 C13 33.1(7) . . . . ? P1 N1 P2 O1 -116.0(5) . . . . ? P1 N1 P2 O2 138.2(4) . . . . ? P1 N1 P2 S1 11.9(5) . . . . ? C1 O1 P2 N1 -178.0(5) . . . . ? C1 O1 P2 O2 -65.8(5) . . . . ? C1 O1 P2 S1 53.7(5) . . . . ? C7 O2 P2 N1 -61.5(5) . . . . ? C7 O2 P2 O1 -171.9(5) . . . . ? C7 O2 P2 S1 66.7(5) . . . . ? P4 N2 P3 C33 78.6(5) . . . . ? P4 N2 P3 C41 -161.5(5) . . . . ? P4 N2 P3 C35 -44.4(6) . . . . ? C32 C33 P3 N2 -19.1(7) . . . . ? C34 C33 P3 N2 163.1(5) . . . . ? Fe1 C33 P3 N2 71.6(5) . . . . ? C32 C33 P3 C41 -138.0(6) . . . . ? C34 C33 P3 C41 44.2(7) . . . . ? Fe1 C33 P3 C41 -47.3(6) . . . . ? C32 C33 P3 C35 108.0(6) . . . . ? C34 C33 P3 C35 -69.8(6) . . . . ? Fe1 C33 P3 C35 -161.4(4) . . . . ? C46 C41 P3 N2 -16.5(6) . . . . ? C42 C41 P3 N2 164.9(6) . . . . ? C46 C41 P3 C33 105.3(6) . . . . ? C42 C41 P3 C33 -73.3(6) . . . . ? C46 C41 P3 C35 -139.4(6) . . . . ? C42 C41 P3 C35 41.9(7) . . . . ? C40 C35 P3 N2 124.3(6) . . . . ? C36 C35 P3 N2 -54.7(7) . . . . ? C40 C35 P3 C33 -1.3(7) . . . . ? C36 C35 P3 C33 179.7(6) . . . . ? C40 C35 P3 C41 -117.5(6) . . . . ? C36 C35 P3 C41 63.4(6) . . . . ? P3 N2 P4 O3 -117.5(5) . . . . ? P3 N2 P4 O4 136.6(5) . . . . ? P3 N2 P4 S2 8.2(6) . . . . ? C47 O3 P4 N2 175.5(5) . . . . ? C47 O3 P4 O4 -72.2(6) . . . . ? C47 O3 P4 S2 46.9(6) . . . . ? C53 O4 P4 N2 -53.4(6) . . . . ? C53 O4 P4 O3 -163.6(5) . . . . ? C53 O4 P4 S2 77.5(5) . . . . ? N1 P2 S1 Ag1 -173.3(2) . . . . ? O1 P2 S1 Ag1 -49.9(2) . . . . ? O2 P2 S1 Ag1 62.3(2) . . . . ? S1 Ag1 S1 P2 70(28) 3 . . . ? N2 P4 S2 Ag2 172.0(2) . . . . ? O3 P4 S2 Ag2 -65.6(2) . . . . ? O4 P4 S2 Ag2 45.5(2) . . . . ? S2 Ag2 S2 P4 -58(100) 3_454 . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 68.53 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.238 _refine_diff_density_min -2.437 _refine_diff_density_rms 0.155 #==END