Electronic Supplementary Material for Dalton Transactions This Journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof. Dr. Jose Sordo' _publ_contact_author_address ; Departamento de Quimica Inorganica Facultade de Farmacia Universidade de Santiago de Compostela 15782 Santiago de Compostela Galicia, Spain ; _publ_contact_author_email qijsordol@usc.es _publ_section_title ; New structural features in triphenylphosphinesilver(I) sulfanylcarboxylates. ; loop_ _publ_author_name _publ_author_address E.Barreiro ; Departamento de Quimica Inorganica Facultade de Farmacia Universidade de Santiago de Compostela 15782-Santaigo de Compostela, Galicia Spain ; J.S.Casas ; Departamento de Quimica Inorganica Facultade de Farmacia Universidade de Santiago de Compostela 15782-Santaigo de Compostela, Galicia Spain ; M.D.Couce ; Departamento de Quimica Inorganica Facultade de Ciencias-Quimica Universidade de Vigo 36310-Vigo, Galicia Spain ; A.Sanchez ; Departamento de Quimica Inorganica Facultade de Farmacia Universidade de Santiago de Compostela 15782-Santaigo de Compostela, Galicia Spain ; J.Sordo ; Departamento de Quimica Inorganica Facultade de Farmacia Universidade de Santiago de Compostela 15782-Santaigo de Compostela, Galicia Spain ; J.M.Varela ; Departamento de Quimica Inorganica Facultade de Farmacia Universidade de Santiago de Compostela 15782-Santaigo de Compostela, Galicia Spain ; ; E.M.Vazquez-Lopez ; ; Departamento de Quimica Inorganica Facultade de Ciencias-Quimica Universidade de Vigo 36310-Vigo, Galicia Spain ; #============================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 261747' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H22 Ag O2 P S' _chemical_formula_weight 549.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.056(4) _cell_length_b 9.356(3) _cell_length_c 19.162(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.806(6) _cell_angle_gamma 90.00 _cell_volume 2370.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max .19 _exptl_crystal_size_mid .11 _exptl_crystal_size_min .03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.676701 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11160 _diffrn_reflns_av_R_equivalents 0.1239 _diffrn_reflns_av_sigmaI/netI 0.4795 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.03 _reflns_number_total 5082 _reflns_number_gt 1028 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0061P)^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 5082 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3461 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0633 _refine_ls_goodness_of_fit_ref 0.671 _refine_ls_restrained_S_all 0.671 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.92454(6) 0.42092(9) 0.03085(5) 0.0932(4) Uani 1 1 d . . . S S 1.10290(17) 0.4327(3) 0.10497(13) 0.0664(8) Uani 1 1 d . . . O1 O 0.9973(5) 0.1682(6) 0.0233(4) 0.071(2) Uani 1 1 d . . . O2 O 1.1332(4) 0.0309(6) 0.0506(3) 0.067(2) Uani 1 1 d . . . H2 H 1.0900 -0.0347 0.0275 0.100 Uiso 1 1 d . . . C1 C 1.0887(8) 0.1496(11) 0.0573(5) 0.048(3) Uani 1 1 d . . . C2 C 1.1530(7) 0.2623(9) 0.1065(5) 0.048(3) Uani 1 1 d . . . C3 C 1.2439(7) 0.2179(9) 0.1526(5) 0.048(3) Uani 1 1 d . . . H3 H 1.2589 0.1238 0.1446 0.058 Uiso 1 1 calc R . . C4 C 1.3223(8) 0.2876(11) 0.2118(6) 0.051(3) Uani 1 1 d . . . C5 C 1.3368(7) 0.4342(11) 0.2178(5) 0.056(3) Uani 1 1 d . . . H5 H 1.2924 0.4935 0.1828 0.068 Uiso 1 1 calc R . . C6 C 1.4156(8) 0.4949(10) 0.2745(6) 0.065(3) Uani 1 1 d . . . H6 H 1.4242 0.5936 0.2760 0.078 Uiso 1 1 calc R . . C7 C 1.4819(8) 0.4105(13) 0.3291(5) 0.075(3) Uani 1 1 d . . . H7 H 1.5343 0.4511 0.3677 0.090 Uiso 1 1 calc R . . C8 C 1.4676(7) 0.2642(12) 0.3242(5) 0.070(3) Uani 1 1 d . . . H8 H 1.5111 0.2053 0.3601 0.084 Uiso 1 1 calc R . . C9 C 1.3891(8) 0.2036(10) 0.2665(5) 0.068(3) Uani 1 1 d . . . H9 H 1.3812 0.1048 0.2645 0.082 Uiso 1 1 calc R . . P P 0.75283(18) 0.4159(3) 0.02337(14) 0.0561(8) Uani 1 1 d . . . C11 C 0.6674(9) 0.3119(10) -0.0541(5) 0.054(3) Uani 1 1 d . . . C12 C 0.7105(7) 0.2583(10) -0.1044(6) 0.053(3) Uani 1 1 d . . . H12 H 0.7784 0.2749 -0.0975 0.064 Uiso 1 1 calc R . . C13 C 0.6511(11) 0.1802(10) -0.1647(7) 0.074(4) Uani 1 1 d . . . H13 H 0.6785 0.1430 -0.1987 0.089 Uiso 1 1 calc R . . C14 C 0.5523(10) 0.1587(10) -0.1737(6) 0.070(4) Uani 1 1 d . . . H14 H 0.5132 0.1052 -0.2141 0.084 Uiso 1 1 calc R . . C15 C 0.5058(9) 0.2140(13) -0.1242(7) 0.095(5) Uani 1 1 d . . . H15 H 0.4372 0.2002 -0.1328 0.114 Uiso 1 1 calc R . . C16 C 0.5650(9) 0.2883(10) -0.0635(6) 0.062(3) Uani 1 1 d . . . H16 H 0.5378 0.3228 -0.0288 0.074 Uiso 1 1 calc R . . C21 C 0.7019(7) 0.5950(11) 0.0145(6) 0.059(3) Uani 1 1 d . . . C22 C 0.6249(8) 0.6451(11) -0.0460(5) 0.062(3) Uani 1 1 d . . . H22 H 0.5909 0.5820 -0.0837 0.075 Uiso 1 1 calc R . . C23 C 0.5963(8) 0.7904(12) -0.0522(6) 0.080(4) Uani 1 1 d . . . H23 H 0.5424 0.8216 -0.0928 0.095 Uiso 1 1 calc R . . C24 C 0.6479(9) 0.8852(13) 0.0017(7) 0.089(4) Uani 1 1 d . . . H24 H 0.6309 0.9816 -0.0030 0.107 Uiso 1 1 calc R . . C25 C 0.7238(10) 0.8380(12) 0.0619(7) 0.095(4) Uani 1 1 d . . . H25 H 0.7573 0.9021 0.0993 0.114 Uiso 1 1 calc R . . C26 C 0.7523(8) 0.6954(13) 0.0686(6) 0.082(4) Uani 1 1 d . . . H26 H 0.8059 0.6658 0.1098 0.098 Uiso 1 1 calc R . . C31 C 0.7279(9) 0.3467(12) 0.1027(5) 0.059(3) Uani 1 1 d . . . C32 C 0.6532(9) 0.3917(12) 0.1297(7) 0.081(4) Uani 1 1 d . . . H32 H 0.6130 0.4690 0.1068 0.097 Uiso 1 1 calc R . . C33 C 0.6353(11) 0.3266(18) 0.1894(8) 0.108(5) Uani 1 1 d . . . H33 H 0.5864 0.3635 0.2072 0.130 Uiso 1 1 calc R . . C34 C 0.686(2) 0.216(2) 0.2198(13) 0.178(12) Uani 1 1 d . . . H34 H 0.6694 0.1680 0.2566 0.214 Uiso 1 1 calc R . . C35 C 0.7666(18) 0.165(2) 0.1989(14) 0.181(11) Uani 1 1 d . . . H35 H 0.8061 0.0892 0.2242 0.217 Uiso 1 1 calc R . . C36 C 0.7873(12) 0.2318(15) 0.1378(7) 0.131(6) Uani 1 1 d . . . H36 H 0.8392 0.1986 0.1222 0.157 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.0496(5) 0.0717(6) 0.1484(8) -0.0386(7) 0.0208(5) 0.0030(6) S 0.0604(18) 0.0405(17) 0.084(2) -0.0130(17) 0.0054(16) 0.0055(16) O1 0.057(5) 0.032(4) 0.101(6) -0.016(4) -0.001(5) 0.003(4) O2 0.044(4) 0.050(5) 0.095(5) -0.027(4) 0.010(4) 0.007(3) C1 0.055(8) 0.046(8) 0.050(8) 0.004(6) 0.026(7) 0.005(7) C2 0.028(6) 0.029(6) 0.076(8) -0.024(6) 0.001(6) -0.008(5) C3 0.037(7) 0.044(7) 0.065(8) -0.004(6) 0.020(7) -0.005(6) C4 0.059(8) 0.044(8) 0.043(8) -0.012(6) 0.008(7) -0.025(7) C5 0.058(7) 0.054(8) 0.039(7) -0.001(6) -0.006(6) -0.009(7) C6 0.080(9) 0.046(7) 0.066(9) 0.005(7) 0.020(7) -0.003(7) C7 0.081(9) 0.062(9) 0.070(8) -0.005(8) 0.012(7) -0.021(8) C8 0.053(8) 0.068(9) 0.060(8) 0.015(7) -0.019(7) 0.005(7) C9 0.073(9) 0.059(8) 0.051(8) 0.013(7) -0.007(7) -0.004(7) P 0.0523(18) 0.0513(19) 0.062(2) -0.0038(19) 0.0154(16) 0.0075(18) C11 0.075(9) 0.059(8) 0.044(8) 0.010(6) 0.040(8) 0.008(7) C12 0.053(8) 0.039(7) 0.060(9) 0.017(6) 0.010(8) -0.007(6) C13 0.102(12) 0.030(7) 0.084(10) -0.001(7) 0.023(10) -0.001(8) C14 0.080(10) 0.041(8) 0.062(9) -0.018(6) -0.012(9) -0.014(7) C15 0.074(10) 0.096(11) 0.088(11) -0.023(8) -0.007(9) 0.004(8) C16 0.062(9) 0.049(7) 0.079(10) -0.003(6) 0.031(9) 0.009(7) C21 0.033(6) 0.063(8) 0.068(8) 0.003(8) 0.000(6) 0.001(7) C22 0.066(9) 0.067(9) 0.060(8) -0.002(6) 0.029(7) 0.011(7) C23 0.074(10) 0.048(8) 0.089(10) 0.008(7) -0.008(8) -0.004(8) C24 0.065(9) 0.067(11) 0.130(13) 0.034(10) 0.027(9) -0.001(8) C25 0.130(13) 0.042(9) 0.107(11) -0.025(8) 0.031(10) 0.014(8) C26 0.051(8) 0.081(10) 0.088(9) -0.015(8) -0.010(7) -0.001(7) C31 0.058(8) 0.058(9) 0.053(9) -0.005(7) 0.008(7) -0.001(6) C32 0.088(10) 0.085(10) 0.074(10) 0.004(9) 0.035(8) -0.014(8) C33 0.143(15) 0.117(15) 0.067(13) -0.023(10) 0.039(11) -0.059(13) C34 0.33(4) 0.092(19) 0.093(16) 0.027(14) 0.04(2) -0.06(2) C35 0.28(3) 0.086(15) 0.13(2) 0.041(13) 0.02(2) 0.038(16) C36 0.252(18) 0.061(10) 0.066(11) 0.001(8) 0.037(12) 0.031(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag P 2.369(3) . ? Ag S 2.429(2) . ? Ag O1 2.599(6) . ? Ag S 2.849(3) 3_765 ? Ag Ag 3.1282(19) 3_765 ? Ag O1 4.223(6) 3_765 ? S C2 1.739(8) . ? S Ag 2.849(3) 3_765 ? O1 C1 1.241(9) . ? O2 C1 1.302(9) . ? C1 C2 1.496(11) . ? C2 C3 1.349(10) . ? C3 C4 1.442(10) . ? C4 C5 1.387(10) . ? C4 C9 1.390(11) . ? C5 C6 1.383(10) . ? C6 C7 1.388(11) . ? C7 C8 1.382(11) . ? C8 C9 1.390(11) . ? P C31 1.791(10) . ? P C21 1.808(10) . ? P C11 1.839(10) . ? C11 C12 1.395(10) . ? C11 C16 1.406(11) . ? C12 C13 1.383(11) . ? C13 C14 1.355(12) . ? C14 C15 1.419(12) . ? C15 C16 1.369(11) . ? C21 C22 1.373(10) . ? C21 C26 1.400(11) . ? C22 C23 1.411(11) . ? C23 C24 1.368(11) . ? C24 C25 1.353(12) . ? C25 C26 1.387(12) . ? C31 C32 1.385(12) . ? C31 C36 1.387(14) . ? C32 C33 1.393(13) . ? C33 C34 1.28(2) . ? C34 C35 1.40(2) . ? C35 C36 1.44(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 P Ag S 149.83(9) . . ? P Ag O1 112.97(16) . . ? S Ag O1 74.12(15) . . ? P Ag S 97.73(9) . 3_765 ? S Ag S 107.81(7) . 3_765 ? O1 Ag S 108.69(16) . 3_765 ? P Ag Ag 142.55(9) . 3_765 ? S Ag Ag 60.13(7) . 3_765 ? O1 Ag Ag 94.55(15) . 3_765 ? S Ag Ag 47.68(5) 3_765 3_765 ? P Ag O1 110.36(12) . 3_765 ? S Ag O1 78.43(11) . 3_765 ? O1 Ag O1 132.40(10) . 3_765 ? S Ag O1 45.89(10) 3_765 3_765 ? Ag Ag O1 37.85(9) 3_765 3_765 ? C2 S Ag 107.4(3) . . ? C2 S Ag 112.6(3) . 3_765 ? Ag S Ag 72.19(7) . 3_765 ? C1 O1 Ag 117.1(6) . . ? O1 C1 O2 121.0(10) . . ? O1 C1 C2 121.9(9) . . ? O2 C1 C2 117.1(9) . . ? C3 C2 C1 115.6(9) . . ? C3 C2 S 125.5(7) . . ? C1 C2 S 118.7(7) . . ? C2 C3 C4 132.7(9) . . ? C5 C4 C9 116.9(9) . . ? C5 C4 C3 124.4(10) . . ? C9 C4 C3 118.7(10) . . ? C6 C5 C4 121.9(9) . . ? C5 C6 C7 120.9(10) . . ? C8 C7 C6 117.8(10) . . ? C7 C8 C9 121.0(10) . . ? C4 C9 C8 121.4(10) . . ? C31 P C21 103.3(5) . . ? C31 P C11 103.4(5) . . ? C21 P C11 106.6(5) . . ? C31 P Ag 116.3(4) . . ? C21 P Ag 110.5(3) . . ? C11 P Ag 115.6(4) . . ? C12 C11 C16 121.4(10) . . ? C12 C11 P 115.5(9) . . ? C16 C11 P 123.1(9) . . ? C13 C12 C11 119.1(10) . . ? C14 C13 C12 119.1(12) . . ? C13 C14 C15 123.1(12) . . ? C16 C15 C14 117.8(12) . . ? C15 C16 C11 119.3(11) . . ? C22 C21 C26 116.9(10) . . ? C22 C21 P 124.7(9) . . ? C26 C21 P 117.9(9) . . ? C21 C22 C23 121.3(10) . . ? C24 C23 C22 119.9(11) . . ? C25 C24 C23 119.7(12) . . ? C24 C25 C26 120.8(12) . . ? C25 C26 C21 121.3(10) . . ? C32 C31 C36 117.5(12) . . ? C32 C31 P 126.8(11) . . ? C36 C31 P 115.7(12) . . ? C31 C32 C33 123.1(13) . . ? C34 C33 C32 120(2) . . ? C33 C34 C35 122(3) . . ? C34 C35 C36 119(3) . . ? C31 C36 C35 118.4(17) . . ? 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 S C2 C1 O1 -9.8(13) . . . . ? C2 C1 O1 O2 178.9(17) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O1 0.872(5) 1.789(6) 2.661(8) 177.6(5) 3_755 _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.884 _refine_diff_density_max 0.564 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.067 #=== END data_2 _database_code_depnum_ccdc_archive 'CCDC 261748' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H35 Ag2 Cl O2 P2 S' _chemical_formula_weight 952.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.7866(10) _cell_length_b 13.2797(12) _cell_length_c 14.8441(13) _cell_angle_alpha 113.369(2) _cell_angle_beta 104.383(2) _cell_angle_gamma 96.518(2) _cell_volume 2006.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .19 _exptl_crystal_size_mid .13 _exptl_crystal_size_min .09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 1.212 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.818497 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12024 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.1599 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28.05 _reflns_number_total 8436 _reflns_number_gt 3874 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ZORTEP _computing_publication_material SHELXL97 _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^)+(0.0152P)^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 8436 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1285 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 0.778 _refine_ls_restrained_S_all 0.778 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.20577(4) 0.56912(4) 0.16795(3) 0.04687(14) Uani 1 1 d . . . Ag2 Ag 0.13934(4) 0.33563(4) -0.02863(4) 0.05023(15) Uani 1 1 d . . . Cl Cl 0.2113(2) 0.73589(19) -0.25441(18) 0.1182(9) Uani 1 1 d . . . S S 0.27289(12) 0.52148(11) 0.01718(11) 0.0405(4) Uani 1 1 d . . . O1 O 0.0728(3) 0.6395(3) 0.0737(3) 0.0492(10) Uani 1 1 d . . . O2 O -0.0117(3) 0.6198(3) -0.0844(3) 0.0453(10) Uani 1 1 d . . . C1 C 0.0742(5) 0.6173(4) -0.0175(4) 0.0362(14) Uani 1 1 d . . . C2 C 0.1864(4) 0.5899(4) -0.0445(4) 0.0313(13) Uani 1 1 d . . . C3 C 0.2136(5) 0.6228(4) -0.1124(4) 0.0456(15) Uani 1 1 d . . . H3 H 0.1554 0.6536 -0.1401 0.055 Uiso 1 1 calc R . . C4 C 0.3145(5) 0.6206(4) -0.1521(4) 0.0430(15) Uani 1 1 d . . . C5 C 0.3237(5) 0.6712(5) -0.2184(5) 0.0523(17) Uani 1 1 d . . . C6 C 0.4164(6) 0.6714(5) -0.2576(5) 0.074(2) Uani 1 1 d . . . H6 H 0.4195 0.7078 -0.2994 0.088 Uiso 1 1 calc R . . C7 C 0.5054(6) 0.6185(6) -0.2359(5) 0.074(2) Uani 1 1 d . . . H7 H 0.5686 0.6180 -0.2630 0.089 Uiso 1 1 calc R . . C8 C 0.4993(6) 0.5668(6) -0.1742(5) 0.083(2) Uani 1 1 d . . . H8 H 0.5583 0.5296 -0.1594 0.099 Uiso 1 1 calc R . . C9 C 0.4059(5) 0.5691(6) -0.1330(5) 0.067(2) Uani 1 1 d . . . H9 H 0.4051 0.5338 -0.0900 0.080 Uiso 1 1 calc R . . P1 P 0.21165(14) 0.60067(13) 0.33662(12) 0.0445(4) Uani 1 1 d . . . C111 C 0.2421(5) 0.4867(4) 0.3685(4) 0.0383(14) Uani 1 1 d . . . C112 C 0.1714(5) 0.3797(5) 0.2996(4) 0.0569(18) Uani 1 1 d . . . H112 H 0.1115 0.3700 0.2406 0.068 Uiso 1 1 calc R . . C113 C 0.1884(6) 0.2875(5) 0.3173(5) 0.067(2) Uani 1 1 d . . . H113 H 0.1389 0.2164 0.2711 0.081 Uiso 1 1 calc R . . C114 C 0.2780(6) 0.3002(6) 0.4027(6) 0.0636(19) Uani 1 1 d . . . H114 H 0.2905 0.2375 0.4135 0.076 Uiso 1 1 calc R . . C115 C 0.3490(6) 0.4049(6) 0.4718(5) 0.0616(19) Uani 1 1 d . . . H115 H 0.4095 0.4135 0.5301 0.074 Uiso 1 1 calc R . . C116 C 0.3307(5) 0.4987(5) 0.4551(4) 0.0521(17) Uani 1 1 d . . . H116 H 0.3786 0.5701 0.5028 0.063 Uiso 1 1 calc R . . C121 C 0.0698(5) 0.6183(4) 0.3582(4) 0.0397(14) Uani 1 1 d . . . C122 C -0.0087(6) 0.6485(5) 0.2956(5) 0.0611(18) Uani 1 1 d . . . H122 H 0.0124 0.6609 0.2438 0.073 Uiso 1 1 calc R . . C123 C -0.1199(7) 0.6612(6) 0.3075(5) 0.080(2) Uani 1 1 d . . . H123 H -0.1710 0.6849 0.2654 0.096 Uiso 1 1 calc R . . C124 C -0.1553(6) 0.6400(6) 0.3789(6) 0.070(2) Uani 1 1 d . . . H124 H -0.2310 0.6466 0.3853 0.084 Uiso 1 1 calc R . . C125 C -0.0780(6) 0.6088(5) 0.4411(5) 0.073(2) Uani 1 1 d . . . H125 H -0.0997 0.5960 0.4925 0.088 Uiso 1 1 calc R . . C126 C 0.0319(6) 0.5959(5) 0.4297(5) 0.0648(19) Uani 1 1 d . . . H126 H 0.0820 0.5712 0.4715 0.078 Uiso 1 1 calc R . . C131 C 0.3227(5) 0.7256(5) 0.4385(5) 0.0478(16) Uani 1 1 d . . . C132 C 0.4268(6) 0.7581(5) 0.4192(5) 0.0654(19) Uani 1 1 d . . . H132 H 0.4368 0.7153 0.3560 0.078 Uiso 1 1 calc R . . C133 C 0.5160(6) 0.8527(6) 0.4922(6) 0.078(2) Uani 1 1 d . . . H133 H 0.5860 0.8732 0.4790 0.094 Uiso 1 1 calc R . . C134 C 0.4992(8) 0.9153(6) 0.5841(7) 0.090(3) Uani 1 1 d . . . H134 H 0.5581 0.9796 0.6336 0.108 Uiso 1 1 calc R . . C135 C 0.3986(7) 0.8856(7) 0.6039(6) 0.094(3) Uani 1 1 d . . . H135 H 0.3889 0.9289 0.6672 0.113 Uiso 1 1 calc R . . C136 C 0.3110(6) 0.7924(6) 0.5321(5) 0.075(2) Uani 1 1 d . . . H136 H 0.2416 0.7735 0.5468 0.090 Uiso 1 1 calc R . . P2 P 0.17627(13) 0.15183(12) -0.10383(12) 0.0444(4) Uani 1 1 d . . . C211 C 0.3242(5) 0.1522(5) -0.1186(4) 0.0458(16) Uani 1 1 d . . . C212 C 0.3704(6) 0.2280(6) -0.1484(6) 0.074(2) Uani 1 1 d . . . H212 H 0.3248 0.2761 -0.1621 0.089 Uiso 1 1 calc R . . C213 C 0.4834(7) 0.2344(6) -0.1587(6) 0.087(3) Uani 1 1 d . . . H213 H 0.5133 0.2873 -0.1787 0.104 Uiso 1 1 calc R . . C214 C 0.5514(7) 0.1656(7) -0.1404(6) 0.092(3) Uani 1 1 d . . . H214 H 0.6268 0.1688 -0.1494 0.111 Uiso 1 1 calc R . . C215 C 0.5081(7) 0.0924(7) -0.1090(6) 0.096(3) Uani 1 1 d . . . H215 H 0.5560 0.0468 -0.0931 0.116 Uiso 1 1 calc R . . C216 C 0.3941(6) 0.0827(6) -0.0994(5) 0.074(2) Uani 1 1 d . . . H216 H 0.3650 0.0290 -0.0800 0.089 Uiso 1 1 calc R . . C221 C 0.1664(5) 0.0647(5) -0.0351(5) 0.0430(15) Uani 1 1 d . . . C222 C 0.0976(5) -0.0459(5) -0.0843(5) 0.0596(18) Uani 1 1 d . . . H222 H 0.0511 -0.0773 -0.1538 0.071 Uiso 1 1 calc R . . C223 C 0.0986(7) -0.1086(6) -0.0293(7) 0.081(3) Uani 1 1 d . . . H223 H 0.0530 -0.1827 -0.0622 0.097 Uiso 1 1 calc R . . C224 C 0.1644(8) -0.0641(8) 0.0708(8) 0.091(3) Uani 1 1 d . . . H224 H 0.1637 -0.1073 0.1071 0.110 Uiso 1 1 calc R . . C225 C 0.2330(7) 0.0445(7) 0.1202(6) 0.083(2) Uani 1 1 d . . . H225 H 0.2789 0.0749 0.1898 0.099 Uiso 1 1 calc R . . C226 C 0.2340(6) 0.1084(5) 0.0672(5) 0.0651(19) Uani 1 1 d . . . H226 H 0.2809 0.1821 0.1009 0.078 Uiso 1 1 calc R . . C231 C 0.0722(5) 0.0698(5) -0.2355(4) 0.0468(16) Uani 1 1 d . . . C232 C -0.0352(6) 0.0978(5) -0.2604(5) 0.0624(19) Uani 1 1 d . . . H232 H -0.0536 0.1567 -0.2107 0.075 Uiso 1 1 calc R . . C233 C -0.1172(6) 0.0381(6) -0.3601(6) 0.079(2) Uani 1 1 d . . . H233 H -0.1897 0.0581 -0.3778 0.095 Uiso 1 1 calc R . . C234 C -0.0903(8) -0.0503(7) -0.4319(6) 0.090(3) Uani 1 1 d . . . H234 H -0.1451 -0.0908 -0.4984 0.108 Uiso 1 1 calc R . . C235 C 0.0158(7) -0.0792(6) -0.4066(6) 0.090(3) Uani 1 1 d . . . H235 H 0.0330 -0.1395 -0.4559 0.107 Uiso 1 1 calc R . . C236 C 0.0972(6) -0.0208(5) -0.3098(5) 0.073(2) Uani 1 1 d . . . H236 H 0.1697 -0.0413 -0.2933 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0549(3) 0.0572(3) 0.0363(3) 0.0264(2) 0.0177(2) 0.0132(3) Ag2 0.0554(3) 0.0416(3) 0.0614(4) 0.0235(3) 0.0261(3) 0.0204(2) Cl 0.178(2) 0.164(2) 0.146(2) 0.1344(18) 0.1251(18) 0.1226(18) S 0.0422(9) 0.0495(9) 0.0449(9) 0.0306(8) 0.0200(7) 0.0163(8) O1 0.056(3) 0.064(3) 0.046(3) 0.031(2) 0.029(2) 0.028(2) O2 0.036(2) 0.061(3) 0.048(3) 0.032(2) 0.013(2) 0.019(2) C1 0.049(4) 0.022(3) 0.044(4) 0.018(3) 0.019(3) 0.010(3) C2 0.030(3) 0.029(3) 0.035(3) 0.015(3) 0.011(3) 0.006(2) C3 0.052(4) 0.059(4) 0.047(4) 0.038(3) 0.022(3) 0.022(3) C4 0.041(4) 0.054(4) 0.037(4) 0.021(3) 0.014(3) 0.014(3) C5 0.066(4) 0.059(4) 0.052(4) 0.031(3) 0.033(4) 0.029(4) C6 0.092(6) 0.089(5) 0.071(5) 0.049(5) 0.054(5) 0.023(5) C7 0.054(5) 0.116(6) 0.060(5) 0.039(5) 0.033(4) 0.010(4) C8 0.060(5) 0.154(7) 0.072(5) 0.072(5) 0.035(4) 0.052(5) C9 0.044(4) 0.131(6) 0.065(5) 0.069(5) 0.033(4) 0.037(4) P1 0.0497(10) 0.0543(10) 0.0362(9) 0.0255(8) 0.0159(8) 0.0121(9) C111 0.043(4) 0.047(4) 0.033(3) 0.021(3) 0.019(3) 0.015(3) C112 0.068(5) 0.060(4) 0.042(4) 0.023(4) 0.013(4) 0.019(4) C113 0.078(5) 0.047(4) 0.061(5) 0.017(4) 0.015(4) 0.003(4) C114 0.074(5) 0.058(5) 0.084(6) 0.045(4) 0.035(4) 0.030(4) C115 0.058(5) 0.081(5) 0.068(5) 0.053(5) 0.018(4) 0.029(4) C116 0.040(4) 0.068(5) 0.051(4) 0.034(4) 0.007(3) 0.011(3) C121 0.044(4) 0.043(4) 0.037(4) 0.024(3) 0.013(3) 0.010(3) C122 0.064(5) 0.092(5) 0.048(4) 0.045(4) 0.026(4) 0.029(4) C123 0.081(6) 0.119(6) 0.057(5) 0.046(5) 0.023(4) 0.053(5) C124 0.059(5) 0.088(5) 0.069(5) 0.032(4) 0.033(4) 0.025(4) C125 0.085(6) 0.089(5) 0.091(6) 0.061(5) 0.061(5) 0.035(5) C126 0.076(5) 0.084(5) 0.075(5) 0.060(4) 0.040(4) 0.040(4) C131 0.052(4) 0.057(4) 0.047(4) 0.033(4) 0.018(3) 0.014(3) C132 0.074(5) 0.062(5) 0.046(4) 0.020(4) 0.012(4) -0.005(4) C133 0.065(5) 0.079(6) 0.092(6) 0.049(5) 0.018(5) -0.007(5) C134 0.091(7) 0.059(5) 0.080(7) 0.024(5) -0.016(6) -0.009(5) C135 0.083(6) 0.088(6) 0.068(6) 0.002(5) 0.017(5) -0.005(5) C136 0.069(5) 0.073(5) 0.060(5) 0.009(4) 0.026(4) -0.003(4) P2 0.0446(10) 0.0354(9) 0.0566(11) 0.0192(8) 0.0223(8) 0.0124(8) C211 0.045(4) 0.038(4) 0.055(4) 0.015(3) 0.024(3) 0.012(3) C212 0.046(4) 0.083(5) 0.115(7) 0.058(5) 0.035(4) 0.021(4) C213 0.070(6) 0.088(6) 0.109(7) 0.043(5) 0.047(5) 0.000(5) C214 0.051(5) 0.112(8) 0.090(7) 0.011(6) 0.039(5) 0.020(5) C215 0.073(6) 0.138(8) 0.097(7) 0.054(6) 0.043(5) 0.057(6) C216 0.064(5) 0.095(5) 0.106(6) 0.061(5) 0.056(5) 0.046(4) C221 0.043(4) 0.041(4) 0.053(4) 0.024(3) 0.024(3) 0.014(3) C222 0.059(4) 0.048(4) 0.077(5) 0.024(4) 0.033(4) 0.019(4) C223 0.103(7) 0.066(5) 0.129(8) 0.070(6) 0.072(6) 0.041(5) C224 0.104(8) 0.125(8) 0.146(9) 0.114(8) 0.092(7) 0.083(7) C225 0.090(6) 0.113(7) 0.082(6) 0.068(6) 0.038(5) 0.050(6) C226 0.066(5) 0.066(5) 0.071(5) 0.034(4) 0.028(4) 0.020(4) C231 0.041(4) 0.047(4) 0.053(4) 0.023(3) 0.016(3) 0.008(3) C232 0.057(5) 0.065(5) 0.062(5) 0.028(4) 0.017(4) 0.009(4) C233 0.061(5) 0.091(6) 0.094(7) 0.051(5) 0.021(5) 0.018(5) C234 0.089(6) 0.087(6) 0.062(6) 0.024(5) -0.002(5) -0.005(5) C235 0.090(6) 0.069(5) 0.070(6) 0.003(5) 0.012(5) 0.007(5) C236 0.069(5) 0.055(5) 0.071(5) 0.008(4) 0.018(4) 0.015(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 Ag1 P1 2.3504(16) . ? Ag1 O1 2.359(3) . ? Ag1 S 2.4300(15) . ? Ag1 O2 2.808(3) 2_565 ? Ag1 Ag2 3.1429(7) . ? Ag1 Ag2 4.6354(7) 2_565 ? Ag2 P2 2.3905(15) . ? Ag2 O2 2.470(4) 2_565 ? Ag2 S 2.5072(14) . ? Ag2 O1 2.519(3) 2_565 ? Ag2 O1 3.956(3) . ? Cl C5 1.746(6) . ? S C2 1.764(5) . ? O1 C1 1.271(6) . ? O1 Ag2 2.519(3) 2_565 ? O2 C1 1.245(6) . ? O2 Ag2 2.470(4) 2_565 ? C1 C2 1.516(7) . ? C2 C3 1.335(7) . ? C3 C4 1.451(7) . ? C4 C9 1.371(7) . ? C4 C5 1.411(7) . ? C5 C6 1.361(8) . ? C6 C7 1.369(8) . ? C7 C8 1.355(8) . ? C8 C9 1.384(8) . ? P1 C121 1.802(6) . ? P1 C111 1.802(5) . ? P1 C131 1.813(6) . ? C111 C116 1.379(6) . ? C111 C112 1.383(7) . ? C112 C113 1.375(7) . ? C113 C114 1.370(7) . ? C114 C115 1.365(7) . ? C115 C116 1.393(7) . ? C121 C122 1.354(7) . ? C121 C126 1.367(7) . ? C122 C123 1.386(8) . ? C123 C124 1.343(9) . ? C124 C125 1.352(8) . ? C125 C126 1.369(8) . ? C131 C136 1.372(8) . ? C131 C132 1.387(8) . ? C132 C133 1.383(8) . ? C133 C134 1.365(10) . ? C134 C135 1.345(10) . ? C135 C136 1.361(8) . ? P2 C211 1.810(6) . ? P2 C231 1.824(6) . ? P2 C221 1.833(6) . ? C211 C212 1.362(8) . ? C211 C216 1.370(7) . ? C212 C213 1.375(8) . ? C213 C214 1.344(9) . ? C214 C215 1.337(10) . ? C215 C216 1.383(9) . ? C221 C226 1.368(7) . ? C221 C222 1.390(7) . ? C222 C223 1.377(8) . ? C223 C224 1.335(9) . ? C224 C225 1.369(9) . ? C225 C226 1.369(8) . ? C231 C232 1.363(7) . ? C231 C236 1.393(7) . ? C232 C233 1.392(8) . ? C233 C234 1.369(9) . ? C234 C235 1.358(9) . ? C235 C236 1.359(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Ag1 O1 120.91(10) . . ? P1 Ag1 S 158.11(5) . . ? O1 Ag1 S 80.11(10) . . ? P1 Ag1 O2 90.37(8) . 2_565 ? O1 Ag1 O2 85.15(11) . 2_565 ? S Ag1 O2 98.04(8) . 2_565 ? P1 Ag1 Ag2 127.50(4) . . ? O1 Ag1 Ag2 90.80(9) . . ? S Ag1 Ag2 51.56(3) . . ? O2 Ag1 Ag2 48.64(7) 2_565 . ? P1 Ag1 Ag2 106.49(4) . 2_565 ? O1 Ag1 Ag2 18.74(9) . 2_565 ? S Ag1 Ag2 95.33(3) . 2_565 ? O2 Ag1 Ag2 72.10(7) 2_565 2_565 ? Ag2 Ag1 Ag2 91.778(14) . 2_565 ? P2 Ag2 O2 122.01(9) . 2_565 ? P2 Ag2 S 127.75(5) . . ? O2 Ag2 S 105.52(9) 2_565 . ? P2 Ag2 O1 119.68(9) . 2_565 ? O2 Ag2 O1 52.49(11) 2_565 2_565 ? S Ag2 O1 105.46(9) . 2_565 ? P2 Ag2 Ag1 147.29(4) . . ? O2 Ag2 Ag1 58.59(8) 2_565 . ? S Ag2 Ag1 49.39(3) . . ? O1 Ag2 Ag1 87.48(8) 2_565 . ? P2 Ag2 O1 175.42(7) . . ? O2 Ag2 O1 61.18(10) 2_565 . ? S Ag2 O1 51.18(6) . . ? O1 Ag2 O1 58.95(12) 2_565 . ? Ag1 Ag2 O1 36.60(5) . . ? C2 S Ag1 99.46(18) . . ? C2 S Ag2 107.37(16) . . ? Ag1 S Ag2 79.06(4) . . ? C1 O1 Ag1 116.9(3) . . ? C1 O1 Ag2 91.0(3) . 2_565 ? Ag1 O1 Ag2 143.74(17) . 2_565 ? C1 O1 Ag2 76.0(3) . . ? Ag1 O1 Ag2 52.60(7) . . ? Ag2 O1 Ag2 121.05(12) 2_565 . ? C1 O2 Ag2 93.9(3) . 2_565 ? O2 C1 O1 122.5(5) . . ? O2 C1 C2 118.9(5) . . ? O1 C1 C2 118.6(5) . . ? C3 C2 C1 116.5(5) . . ? C3 C2 S 124.9(4) . . ? C1 C2 S 118.5(4) . . ? C2 C3 C4 133.7(5) . . ? C9 C4 C5 113.9(6) . . ? C9 C4 C3 125.2(6) . . ? C5 C4 C3 120.9(5) . . ? C6 C5 C4 123.1(6) . . ? C6 C5 Cl 117.3(5) . . ? C4 C5 Cl 119.6(5) . . ? C5 C6 C7 120.5(6) . . ? C8 C7 C6 118.6(7) . . ? C7 C8 C9 120.4(7) . . ? C4 C9 C8 123.5(6) . . ? C121 P1 C111 104.0(3) . . ? C121 P1 C131 105.3(3) . . ? C111 P1 C131 105.3(3) . . ? C121 P1 Ag1 112.34(19) . . ? C111 P1 Ag1 114.57(18) . . ? C131 P1 Ag1 114.4(2) . . ? C116 C111 C112 118.4(5) . . ? C116 C111 P1 124.8(5) . . ? C112 C111 P1 116.8(4) . . ? C113 C112 C111 120.9(6) . . ? C114 C113 C112 120.2(6) . . ? C115 C114 C113 120.1(6) . . ? C114 C115 C116 119.9(6) . . ? C111 C116 C115 120.5(6) . . ? C122 C121 C126 117.0(6) . . ? C122 C121 P1 118.6(5) . . ? C126 C121 P1 124.3(5) . . ? C121 C122 C123 121.0(6) . . ? C124 C123 C122 121.2(7) . . ? C123 C124 C125 118.2(7) . . ? C124 C125 C126 120.9(7) . . ? C121 C126 C125 121.6(6) . . ? C136 C131 C132 117.3(6) . . ? C136 C131 P1 125.3(5) . . ? C132 C131 P1 117.4(5) . . ? C133 C132 C131 121.3(6) . . ? C134 C133 C132 118.6(7) . . ? C135 C134 C133 121.0(8) . . ? C134 C135 C136 120.4(8) . . ? C135 C136 C131 121.5(7) . . ? C211 P2 C231 104.2(3) . . ? C211 P2 C221 103.1(3) . . ? C231 P2 C221 106.8(3) . . ? C211 P2 Ag2 114.17(19) . . ? C231 P2 Ag2 110.36(19) . . ? C221 P2 Ag2 117.06(19) . . ? C212 C211 C216 117.7(6) . . ? C212 C211 P2 118.1(5) . . ? C216 C211 P2 124.2(5) . . ? C211 C212 C213 121.0(7) . . ? C214 C213 C212 121.1(8) . . ? C215 C214 C213 118.5(8) . . ? C214 C215 C216 121.8(8) . . ? C211 C216 C215 119.9(7) . . ? C226 C221 C222 118.9(6) . . ? C226 C221 P2 118.6(5) . . ? C222 C221 P2 122.5(5) . . ? C223 C222 C221 119.5(7) . . ? C224 C223 C222 120.7(8) . . ? C223 C224 C225 120.5(8) . . ? C224 C225 C226 119.9(8) . . ? C221 C226 C225 120.5(7) . . ? C232 C231 C236 119.4(6) . . ? C232 C231 P2 118.0(5) . . ? C236 C231 P2 122.7(5) . . ? C231 C232 C233 120.1(6) . . ? C234 C233 C232 119.4(7) . . ? C235 C234 C233 120.4(7) . . ? C234 C235 C236 120.6(7) . . ? C235 C236 C231 120.0(6) . . ? _diffrn_measured_fraction_theta_max 0.866 _diffrn_reflns_theta_full 28.05 _diffrn_measured_fraction_theta_full 0.866 _refine_diff_density_max 0.699 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.084 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 261749' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H38 Ag2 O3 P2 S' _chemical_formula_weight 948.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4962(9) _cell_length_b 17.1129(11) _cell_length_c 18.6400(11) _cell_angle_alpha 90.00 _cell_angle_beta 107.1740(10) _cell_angle_gamma 90.00 _cell_volume 4113.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max .21 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 1.121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.761479 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22070 _diffrn_reflns_av_R_equivalents 0.0737 _diffrn_reflns_av_sigmaI/netI 0.2206 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28.01 _reflns_number_total 9136 _reflns_number_gt 3340 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^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 9136 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1714 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 0.690 _refine_ls_restrained_S_all 0.690 _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 Ag1 Ag 0.18155(4) 0.53518(3) 0.11217(3) 0.04627(15) Uani 1 1 d . . . Ag2 Ag 0.18773(4) 0.46108(3) -0.04710(3) 0.04714(16) Uani 1 1 d . . . S S 0.19346(13) 0.39919(9) 0.07314(9) 0.0385(4) Uani 1 1 d . . . O1 O 0.0071(3) 0.4952(2) 0.0832(2) 0.0370(10) Uani 1 1 d . . . O2 O -0.1144(3) 0.4080(2) 0.0312(2) 0.0423(11) Uani 1 1 d . . . O3 O -0.0326(5) 0.1581(2) 0.0615(3) 0.0715(16) Uani 1 1 d . . . C1 C -0.0210(5) 0.4291(4) 0.0548(3) 0.0341(16) Uani 1 1 d . . . C2 C 0.0618(5) 0.3701(3) 0.0480(3) 0.0330(15) Uani 1 1 d . . . C3 C 0.0296(5) 0.2978(3) 0.0279(3) 0.0398(17) Uani 1 1 d . . . H3 H -0.0416 0.2901 0.0162 0.048 Uiso 1 1 calc R . . C4 C 0.0901(5) 0.2282(4) 0.0213(3) 0.0437(17) Uani 1 1 d . . . C5 C 0.0565(6) 0.1555(4) 0.0419(4) 0.0501(19) Uani 1 1 d . . . C6 C 0.1141(7) 0.0879(4) 0.0411(4) 0.066(2) Uani 1 1 d . . . H6 H 0.0934 0.0406 0.0565 0.079 Uiso 1 1 calc R . . C7 C 0.2010(7) 0.0914(5) 0.0178(5) 0.079(3) Uani 1 1 d . . . H7 H 0.2393 0.0462 0.0181 0.095 Uiso 1 1 calc R . . C8 C 0.2329(6) 0.1596(4) -0.0060(4) 0.071(2) Uani 1 1 d . . . H8 H 0.2902 0.1607 -0.0239 0.086 Uiso 1 1 calc R . . C9 C 0.1778(6) 0.2273(4) -0.0026(4) 0.057(2) Uani 1 1 d . . . H9 H 0.2009 0.2742 -0.0172 0.068 Uiso 1 1 calc R . . C10 C -0.0676(7) 0.0933(4) 0.0899(4) 0.093(3) Uani 1 1 d . . . H10A H -0.0785 0.0515 0.0541 0.139 Uiso 1 1 calc R . . H10B H -0.1318 0.1054 0.0998 0.139 Uiso 1 1 calc R . . H10C H -0.0171 0.0777 0.1357 0.139 Uiso 1 1 calc R . . P1 P 0.25155(14) 0.64407(9) 0.18729(9) 0.0410(4) Uani 1 1 d . . . C111 C 0.3673(5) 0.5319(4) -0.1343(3) 0.0447(16) Uani 1 1 d . . . C112 C 0.4507(6) 0.5173(4) -0.1614(4) 0.068(2) Uani 1 1 d . . . H112 H 0.4513 0.4724 -0.1893 0.082 Uiso 1 1 calc R . . C113 C 0.5327(6) 0.5687(6) -0.1472(5) 0.084(3) Uani 1 1 d . . . H113 H 0.5883 0.5580 -0.1656 0.100 Uiso 1 1 calc R . . C114 C 0.5335(7) 0.6345(5) -0.1070(5) 0.089(3) Uani 1 1 d . . . H114 H 0.5897 0.6685 -0.0976 0.107 Uiso 1 1 calc R . . C115 C 0.4529(7) 0.6513(5) -0.0802(5) 0.087(3) Uani 1 1 d . . . H115 H 0.4522 0.6973 -0.0538 0.105 Uiso 1 1 calc R . . C116 C 0.3719(6) 0.5991(4) -0.0928(4) 0.066(2) Uani 1 1 d . . . H116 H 0.3182 0.6097 -0.0724 0.079 Uiso 1 1 calc R . . C121 C 0.1627(5) 0.5189(3) -0.2323(3) 0.0402(16) Uani 1 1 d . . . C122 C 0.0600(5) 0.5223(4) -0.2350(3) 0.0456(18) Uani 1 1 d . . . H122 H 0.0373 0.4965 -0.1988 0.055 Uiso 1 1 calc R . . C123 C -0.0110(6) 0.5645(4) -0.2919(4) 0.059(2) Uani 1 1 d . . . H123 H -0.0802 0.5675 -0.2931 0.070 Uiso 1 1 calc R . . C124 C 0.0227(7) 0.6015(4) -0.3461(4) 0.061(2) Uani 1 1 d . . . H124 H -0.0242 0.6295 -0.3840 0.073 Uiso 1 1 calc R . . C125 C 0.1253(6) 0.5973(4) -0.3445(4) 0.055(2) Uani 1 1 d . . . H125 H 0.1479 0.6220 -0.3812 0.067 Uiso 1 1 calc R . . C126 C 0.1939(5) 0.5562(4) -0.2879(3) 0.0520(19) Uani 1 1 d . . . H126 H 0.2631 0.5533 -0.2870 0.062 Uiso 1 1 calc R . . C131 C 0.2884(5) 0.3798(4) -0.1861(4) 0.0409(17) Uani 1 1 d . . . C132 C 0.3491(6) 0.3291(5) -0.1334(4) 0.072(2) Uani 1 1 d . . . H132 H 0.3724 0.3446 -0.0834 0.087 Uiso 1 1 calc R . . C133 C 0.3757(7) 0.2567(5) -0.1529(5) 0.092(3) Uani 1 1 d . . . H133 H 0.4188 0.2246 -0.1166 0.111 Uiso 1 1 calc R . . C134 C 0.3394(7) 0.2317(5) -0.2249(5) 0.079(3) Uani 1 1 d . . . H134 H 0.3560 0.1820 -0.2381 0.095 Uiso 1 1 calc R . . C135 C 0.2781(6) 0.2803(5) -0.2780(4) 0.071(2) Uani 1 1 d . . . H135 H 0.2521 0.2632 -0.3274 0.085 Uiso 1 1 calc R . . C136 C 0.2541(5) 0.3557(4) -0.2585(4) 0.058(2) Uani 1 1 d . . . H136 H 0.2147 0.3891 -0.2953 0.070 Uiso 1 1 calc R . . P2 P 0.25264(13) 0.47154(11) -0.15243(9) 0.0425(4) Uani 1 1 d . . . C211 C 0.3039(5) 0.7243(4) 0.1445(4) 0.0402(16) Uani 1 1 d . . . C212 C 0.2833(5) 0.7234(4) 0.0674(4) 0.058(2) Uani 1 1 d . . . H212 H 0.2483 0.6811 0.0401 0.070 Uiso 1 1 calc R . . C213 C 0.3142(6) 0.7848(5) 0.0299(4) 0.073(2) Uani 1 1 d . . . H213 H 0.2993 0.7841 -0.0221 0.087 Uiso 1 1 calc R . . C214 C 0.3663(6) 0.8459(4) 0.0706(5) 0.070(2) Uani 1 1 d . . . H214 H 0.3875 0.8871 0.0460 0.084 Uiso 1 1 calc R . . C215 C 0.3881(6) 0.8478(4) 0.1465(4) 0.060(2) Uani 1 1 d . . . H215 H 0.4238 0.8900 0.1736 0.073 Uiso 1 1 calc R . . C216 C 0.3571(5) 0.7873(4) 0.1830(4) 0.0523(19) Uani 1 1 d . . . H216 H 0.3724 0.7889 0.2350 0.063 Uiso 1 1 calc R . . C221 C 0.3536(5) 0.6143(4) 0.2707(3) 0.0432(17) Uani 1 1 d . . . C222 C 0.4567(6) 0.6333(4) 0.2871(4) 0.063(2) Uani 1 1 d . . . H222 H 0.4787 0.6656 0.2546 0.075 Uiso 1 1 calc R . . C223 C 0.5280(6) 0.6051(5) 0.3509(5) 0.087(3) Uani 1 1 d . . . H223 H 0.5971 0.6200 0.3619 0.104 Uiso 1 1 calc R . . C224 C 0.4987(8) 0.5562(5) 0.3976(5) 0.092(3) Uani 1 1 d . . . H224 H 0.5476 0.5371 0.4403 0.110 Uiso 1 1 calc R . . C225 C 0.3974(8) 0.5347(6) 0.3821(5) 0.099(3) Uani 1 1 d . . . H225 H 0.3769 0.5008 0.4140 0.118 Uiso 1 1 calc R . . C226 C 0.3263(6) 0.5631(4) 0.3197(4) 0.071(2) Uani 1 1 d . . . H226 H 0.2574 0.5478 0.3095 0.086 Uiso 1 1 calc R . . C231 C 0.1570(5) 0.6902(3) 0.2258(3) 0.0388(16) Uani 1 1 d . . . C232 C 0.0530(6) 0.6787(4) 0.1891(4) 0.054(2) Uani 1 1 d . . . H232 H 0.0328 0.6485 0.1457 0.065 Uiso 1 1 calc R . . C233 C -0.0210(6) 0.7125(4) 0.2173(4) 0.061(2) Uani 1 1 d . . . H233 H -0.0910 0.7051 0.1925 0.073 Uiso 1 1 calc R . . C234 C 0.0077(7) 0.7561(4) 0.2808(4) 0.062(2) Uani 1 1 d . . . H234 H -0.0430 0.7770 0.2998 0.075 Uiso 1 1 calc R . . C235 C 0.1113(7) 0.7701(4) 0.3177(4) 0.057(2) Uani 1 1 d . . . H235 H 0.1306 0.8015 0.3603 0.068 Uiso 1 1 calc R . . C236 C 0.1848(5) 0.7366(3) 0.2901(3) 0.0479(18) Uani 1 1 d . . . H236 H 0.2546 0.7451 0.3147 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0494(4) 0.0413(3) 0.0470(3) -0.0104(3) 0.0125(3) -0.0080(3) Ag2 0.0493(4) 0.0514(3) 0.0461(3) 0.0028(3) 0.0224(3) 0.0051(3) S 0.0345(10) 0.0349(9) 0.0438(10) 0.0006(8) 0.0079(8) 0.0000(8) O1 0.040(3) 0.033(2) 0.040(2) -0.010(2) 0.013(2) -0.003(2) O2 0.032(3) 0.040(3) 0.054(3) -0.005(2) 0.011(2) -0.003(2) O3 0.119(5) 0.035(3) 0.073(4) 0.006(3) 0.048(4) -0.005(3) C1 0.039(5) 0.045(4) 0.020(3) 0.010(3) 0.012(3) 0.007(4) C2 0.038(4) 0.034(4) 0.026(3) 0.007(3) 0.008(3) -0.001(3) C3 0.042(5) 0.037(4) 0.043(4) 0.009(3) 0.015(4) 0.005(3) C4 0.046(5) 0.037(4) 0.041(4) -0.006(3) 0.002(4) 0.004(4) C5 0.062(6) 0.044(5) 0.037(4) -0.007(3) 0.005(4) -0.003(4) C6 0.092(7) 0.035(4) 0.049(5) -0.003(4) -0.012(5) 0.001(5) C7 0.060(6) 0.053(6) 0.098(7) -0.018(5) -0.018(5) 0.018(5) C8 0.057(6) 0.053(5) 0.096(6) -0.035(5) 0.012(5) 0.003(5) C9 0.055(5) 0.044(4) 0.069(5) -0.018(4) 0.013(4) -0.003(4) C10 0.141(9) 0.050(5) 0.098(7) -0.001(5) 0.054(6) -0.011(6) P1 0.0417(12) 0.0395(10) 0.0405(11) -0.0061(8) 0.0101(9) -0.0048(9) C111 0.039(4) 0.059(4) 0.035(4) 0.002(4) 0.009(3) 0.002(4) C112 0.051(5) 0.087(6) 0.072(5) -0.009(5) 0.028(4) 0.002(5) C113 0.036(5) 0.121(8) 0.099(7) -0.012(6) 0.027(5) -0.011(5) C114 0.047(6) 0.095(8) 0.115(8) -0.014(6) 0.007(6) -0.025(6) C115 0.055(6) 0.087(7) 0.109(8) -0.034(5) 0.007(6) -0.008(6) C116 0.054(6) 0.072(6) 0.071(6) -0.014(5) 0.018(4) -0.009(5) C121 0.046(5) 0.038(4) 0.035(4) 0.002(3) 0.010(3) -0.002(3) C122 0.051(5) 0.043(4) 0.042(4) 0.002(3) 0.013(4) 0.001(4) C123 0.048(5) 0.061(5) 0.058(5) -0.008(4) 0.001(4) 0.014(4) C124 0.090(7) 0.041(4) 0.037(4) -0.002(4) -0.005(4) 0.007(5) C125 0.071(6) 0.044(4) 0.048(5) 0.004(4) 0.012(4) -0.011(4) C126 0.053(5) 0.057(5) 0.042(4) 0.007(4) 0.008(4) -0.001(4) C131 0.036(4) 0.053(4) 0.038(4) 0.007(4) 0.018(3) 0.009(4) C132 0.082(7) 0.088(6) 0.047(5) -0.005(5) 0.019(5) 0.038(5) C133 0.114(9) 0.089(7) 0.079(7) 0.016(6) 0.036(6) 0.060(6) C134 0.090(8) 0.057(5) 0.107(8) -0.001(6) 0.052(7) 0.023(5) C135 0.065(6) 0.084(6) 0.065(6) -0.024(5) 0.019(5) -0.003(5) C136 0.062(6) 0.064(5) 0.054(5) 0.003(4) 0.025(4) 0.010(4) P2 0.0372(10) 0.0522(11) 0.0395(10) 0.0041(9) 0.0138(8) 0.0046(10) C211 0.040(4) 0.040(4) 0.043(4) -0.005(3) 0.016(4) 0.005(3) C212 0.056(5) 0.070(5) 0.047(5) -0.011(4) 0.013(4) -0.015(4) C213 0.088(7) 0.085(6) 0.049(5) 0.013(5) 0.027(5) -0.011(5) C214 0.074(6) 0.052(5) 0.092(7) 0.007(5) 0.036(6) -0.007(5) C215 0.066(6) 0.046(5) 0.074(6) -0.013(4) 0.027(5) -0.013(4) C216 0.060(5) 0.042(4) 0.058(5) -0.004(4) 0.023(4) -0.001(4) C221 0.050(5) 0.040(4) 0.039(4) -0.008(3) 0.012(4) -0.006(4) C222 0.054(6) 0.080(6) 0.052(5) 0.008(4) 0.012(4) -0.002(5) C223 0.054(6) 0.123(8) 0.070(6) 0.017(6) -0.004(5) 0.004(6) C224 0.080(7) 0.116(8) 0.067(6) 0.036(6) 0.001(6) 0.025(7) C225 0.099(8) 0.117(8) 0.072(6) 0.050(6) 0.012(6) 0.011(8) C226 0.058(6) 0.082(6) 0.068(6) 0.018(5) 0.010(5) -0.010(5) C231 0.044(5) 0.033(4) 0.039(4) 0.002(3) 0.012(4) -0.007(3) C232 0.062(6) 0.045(4) 0.055(5) -0.004(4) 0.019(4) -0.009(4) C233 0.042(5) 0.067(5) 0.078(6) 0.016(5) 0.025(5) 0.001(4) C234 0.084(7) 0.050(5) 0.068(6) 0.006(4) 0.045(5) 0.006(5) C235 0.078(6) 0.042(4) 0.057(5) 0.000(4) 0.030(5) -0.004(5) C236 0.046(5) 0.046(4) 0.050(5) -0.007(4) 0.014(4) -0.007(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 Ag1 P1 2.3547(17) . ? Ag1 O1 2.356(4) . ? Ag1 S 2.4577(16) . ? Ag1 O2 2.736(4) 3_565 ? Ag1 Ag2 3.2519(6) . ? Ag1 Ag2 4.7692(8) 3_565 ? Ag2 P2 2.3812(15) . ? Ag2 S 2.4593(16) . ? Ag2 O2 2.502(4) 3_565 ? Ag2 O1 2.624(4) 3_565 ? S C2 1.770(6) . ? O1 C1 1.259(6) . ? O1 Ag2 2.624(4) 3_565 ? O2 C1 1.260(7) . ? O2 Ag2 2.502(4) 3_565 ? O2 Ag1 2.736(4) 3_565 ? O3 C5 1.358(8) . ? O3 C10 1.371(7) . ? C1 C2 1.538(8) . ? C2 C3 1.329(7) . ? C3 C4 1.469(8) . ? C4 C9 1.383(8) . ? C4 C5 1.415(8) . ? C5 C6 1.395(9) . ? C6 C7 1.367(9) . ? C7 C8 1.361(9) . ? C8 C9 1.388(8) . ? P1 C221 1.819(7) . ? P1 C231 1.819(6) . ? P1 C211 1.832(6) . ? C111 C116 1.377(8) . ? C111 C112 1.386(8) . ? C111 P2 1.807(6) . ? C112 C113 1.377(9) . ? C113 C114 1.352(10) . ? C114 C115 1.354(10) . ? C115 C116 1.377(9) . ? C121 C122 1.374(8) . ? C121 C126 1.386(7) . ? C121 P2 1.810(6) . ? C122 C123 1.401(8) . ? C123 C124 1.378(8) . ? C124 C125 1.379(9) . ? C125 C126 1.374(8) . ? C131 C136 1.356(8) . ? C131 C132 1.382(8) . ? C131 P2 1.809(6) . ? C132 C133 1.369(9) . ? C133 C134 1.355(10) . ? C134 C135 1.369(9) . ? C135 C136 1.404(9) . ? C211 C216 1.373(8) . ? C211 C212 1.380(8) . ? C212 C213 1.393(9) . ? C213 C214 1.359(9) . ? C214 C215 1.359(9) . ? C215 C216 1.370(8) . ? C221 C222 1.373(8) . ? C221 C226 1.392(8) . ? C222 C223 1.377(9) . ? C223 C224 1.348(9) . ? C224 C225 1.362(11) . ? C225 C226 1.359(10) . ? C231 C232 1.383(8) . ? C231 C236 1.393(7) . ? C232 C233 1.384(8) . ? C233 C234 1.355(9) . ? C234 C235 1.385(9) . ? C235 C236 1.370(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Ag1 O1 124.37(10) . . ? P1 Ag1 S 151.12(6) . . ? O1 Ag1 S 78.77(10) . . ? P1 Ag1 O2 104.98(9) . 3_565 ? O1 Ag1 O2 81.89(12) . 3_565 ? S Ag1 O2 94.54(9) . 3_565 ? P1 Ag1 Ag2 137.52(4) . . ? O1 Ag1 Ag2 88.31(9) . . ? S Ag1 Ag2 48.62(4) . . ? O2 Ag1 Ag2 48.47(8) 3_565 . ? P1 Ag1 Ag2 110.26(5) . 3_565 ? O1 Ag1 Ag2 17.67(9) . 3_565 ? S Ag1 Ag2 95.29(4) . 3_565 ? O2 Ag1 Ag2 74.16(9) 3_565 3_565 ? Ag2 Ag1 Ag2 94.566(15) . 3_565 ? P2 Ag2 S 149.72(6) . . ? P2 Ag2 O2 106.53(10) . 3_565 ? S Ag2 O2 100.68(9) . 3_565 ? P2 Ag2 O1 110.62(9) . 3_565 ? S Ag2 O1 96.65(9) . 3_565 ? O2 Ag2 O1 51.21(12) 3_565 3_565 ? P2 Ag2 Ag1 146.96(5) . . ? S Ag2 Ag1 48.57(4) . . ? O2 Ag2 Ag1 54.92(9) 3_565 . ? O1 Ag2 Ag1 80.14(8) 3_565 . ? C2 S Ag1 101.3(2) . . ? C2 S Ag2 96.96(18) . . ? Ag1 S Ag2 82.81(5) . . ? C1 O1 Ag1 120.9(4) . . ? C1 O1 Ag2 89.6(4) . 3_565 ? Ag1 O1 Ag2 146.51(17) . 3_565 ? C1 O2 Ag2 95.3(4) . 3_565 ? C1 O2 Ag1 104.3(3) . 3_565 ? Ag2 O2 Ag1 76.61(11) 3_565 3_565 ? C5 O3 C10 120.7(6) . . ? O1 C1 O2 123.4(6) . . ? O1 C1 C2 119.2(6) . . ? O2 C1 C2 117.4(6) . . ? C3 C2 C1 116.7(6) . . ? C3 C2 S 123.7(5) . . ? C1 C2 S 119.4(4) . . ? C2 C3 C4 129.5(6) . . ? C9 C4 C5 116.8(6) . . ? C9 C4 C3 125.8(6) . . ? C5 C4 C3 117.4(6) . . ? O3 C5 C6 124.8(7) . . ? O3 C5 C4 115.1(6) . . ? C6 C5 C4 120.1(7) . . ? C7 C6 C5 120.0(7) . . ? C8 C7 C6 121.6(8) . . ? C7 C8 C9 118.4(8) . . ? C4 C9 C8 123.0(7) . . ? C221 P1 C231 103.1(3) . . ? C221 P1 C211 106.9(3) . . ? C231 P1 C211 104.6(3) . . ? C221 P1 Ag1 110.9(2) . . ? C231 P1 Ag1 111.9(2) . . ? C211 P1 Ag1 118.2(2) . . ? C116 C111 C112 116.6(7) . . ? C116 C111 P2 118.5(5) . . ? C112 C111 P2 124.8(6) . . ? C113 C112 C111 120.6(7) . . ? C114 C113 C112 120.8(8) . . ? C113 C114 C115 120.4(8) . . ? C114 C115 C116 118.9(8) . . ? C111 C116 C115 122.7(7) . . ? C122 C121 C126 118.7(6) . . ? C122 C121 P2 118.3(5) . . ? C126 C121 P2 122.9(5) . . ? C121 C122 C123 120.4(6) . . ? C124 C123 C122 119.5(7) . . ? C123 C124 C125 120.4(7) . . ? C124 C125 C126 119.3(7) . . ? C125 C126 C121 121.7(7) . . ? C136 C131 C132 118.2(6) . . ? C136 C131 P2 124.2(5) . . ? C132 C131 P2 117.5(5) . . ? C133 C132 C131 121.8(7) . . ? C134 C133 C132 120.1(8) . . ? C133 C134 C135 119.3(8) . . ? C134 C135 C136 120.5(7) . . ? C131 C136 C135 120.0(7) . . ? C111 P2 C131 105.1(3) . . ? C111 P2 C121 103.1(3) . . ? C131 P2 C121 106.6(3) . . ? C111 P2 Ag2 113.1(2) . . ? C131 P2 Ag2 114.9(2) . . ? C121 P2 Ag2 113.0(2) . . ? C216 C211 C212 117.8(6) . . ? C216 C211 P1 124.8(5) . . ? C212 C211 P1 117.4(5) . . ? C211 C212 C213 121.1(7) . . ? C214 C213 C212 118.9(7) . . ? C215 C214 C213 121.0(7) . . ? C214 C215 C216 119.7(7) . . ? C215 C216 C211 121.6(6) . . ? C222 C221 C226 116.8(7) . . ? C222 C221 P1 125.8(5) . . ? C226 C221 P1 117.2(6) . . ? C221 C222 C223 120.8(7) . . ? C224 C223 C222 120.8(8) . . ? C223 C224 C225 119.8(8) . . ? C226 C225 C224 119.7(8) . . ? C225 C226 C221 122.0(8) . . ? C232 C231 C236 118.9(6) . . ? C232 C231 P1 118.1(5) . . ? C236 C231 P1 123.0(5) . . ? C233 C232 C231 119.6(7) . . ? C234 C233 C232 120.6(7) . . ? C233 C234 C235 121.0(7) . . ? C236 C235 C234 118.6(7) . . ? C235 C236 C231 121.3(7) . . ? _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 0.332 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.082 #=== END data_4.C3H6O _database_code_depnum_ccdc_archive 'CCDC 261750' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H43 Ag2 O4 P2 S' _chemical_formula_weight 993.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6832(13) _cell_length_b 13.5698(14) _cell_length_c 15.7147(17) _cell_angle_alpha 107.707(2) _cell_angle_beta 98.165(2) _cell_angle_gamma 113.460(2) _cell_volume 2253.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max .26 _exptl_crystal_size_mid .24 _exptl_crystal_size_min .22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1006 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.669307 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12975 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.1868 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 28.08 _reflns_number_total 9092 _reflns_number_gt 3775 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^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 9092 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1257 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1198 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 0.746 _refine_ls_restrained_S_all 0.746 _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 Ag1 Ag 0.63752(5) 0.66923(4) 0.45213(4) 0.04901(18) Uani 1 1 d . . . Ag2 Ag 0.44281(5) 0.68708(4) 0.57528(4) 0.05324(19) Uani 1 1 d . . . S S 0.66738(15) 0.75675(13) 0.62046(12) 0.0424(4) Uani 1 1 d . . . O1 O 0.6340(4) 0.5181(3) 0.4968(3) 0.0434(11) Uani 1 1 d . . . O2 O 0.6101(4) 0.4403(4) 0.6004(3) 0.0534(13) Uani 1 1 d . . . C1 C 0.6354(5) 0.5265(5) 0.5780(5) 0.0388(16) Uani 1 1 d . . . C2 C 0.6709(5) 0.6454(5) 0.6554(5) 0.0370(16) Uani 1 1 d . . . C3 C 0.7032(6) 0.6568(6) 0.7432(5) 0.0463(18) Uani 1 1 d . . . H3 H 0.6993 0.5893 0.7488 0.056 Uiso 1 1 calc R . . C4 C 0.7441(6) 0.7560(6) 0.8339(5) 0.0478(18) Uani 1 1 d . . . C5 C 0.7975(7) 0.8735(7) 0.8476(5) 0.066(2) Uani 1 1 d . . . H5 H 0.8042 0.8923 0.7958 0.079 Uiso 1 1 calc R . . C6 C 0.8406(7) 0.9626(6) 0.9344(6) 0.069(2) Uani 1 1 d . . . H6 H 0.8757 1.0401 0.9407 0.082 Uiso 1 1 calc R . . C7 C 0.8318(7) 0.9373(7) 1.0099(6) 0.061(2) Uani 1 1 d . . . C8 C 0.7796(7) 0.8236(8) 1.0018(6) 0.073(2) Uani 1 1 d . . . H8 H 0.7728 0.8065 1.0544 0.088 Uiso 1 1 calc R . . C9 C 0.7369(7) 0.7344(7) 0.9134(6) 0.065(2) Uani 1 1 d . . . H9 H 0.7022 0.6572 0.9078 0.078 Uiso 1 1 calc R . . O3 O 0.8710(5) 1.0170(5) 1.1014(4) 0.0811(17) Uani 1 1 d . . . C71 C 0.9205(8) 1.1377(7) 1.1150(6) 0.101(3) Uani 1 1 d . . . H71A H 0.9911 1.1594 1.0946 0.152 Uiso 1 1 calc R . . H71B H 0.9417 1.1854 1.1803 0.152 Uiso 1 1 calc R . . H71C H 0.8618 1.1493 1.0794 0.152 Uiso 1 1 calc R . . P1 P 0.67277(16) 0.66647(15) 0.30879(13) 0.0454(5) Uani 1 1 d . . . C111 C 0.5580(6) 0.6606(5) 0.2196(5) 0.0463(18) Uani 1 1 d . . . C112 C 0.4629(7) 0.6747(6) 0.2422(6) 0.065(2) Uani 1 1 d . . . H112 H 0.4592 0.6882 0.3031 0.077 Uiso 1 1 calc R . . C113 C 0.3731(8) 0.6695(8) 0.1781(7) 0.087(3) Uani 1 1 d . . . H113 H 0.3107 0.6814 0.1957 0.105 Uiso 1 1 calc R . . C114 C 0.3772(8) 0.6468(7) 0.0892(6) 0.082(3) Uani 1 1 d . . . H114 H 0.3168 0.6422 0.0445 0.098 Uiso 1 1 calc R . . C115 C 0.4707(8) 0.6306(7) 0.0648(6) 0.075(2) Uani 1 1 d . . . H115 H 0.4732 0.6160 0.0035 0.090 Uiso 1 1 calc R . . C116 C 0.5607(7) 0.6352(6) 0.1285(5) 0.062(2) Uani 1 1 d . . . H116 H 0.6220 0.6215 0.1105 0.074 Uiso 1 1 calc R . . C121 C 0.8127(6) 0.7909(6) 0.3236(5) 0.0472(18) Uani 1 1 d . . . C122 C 0.8238(7) 0.8656(6) 0.2793(5) 0.065(2) Uani 1 1 d . . . H122 H 0.7565 0.8531 0.2363 0.078 Uiso 1 1 calc R . . C123 C 0.9338(9) 0.9588(7) 0.2979(7) 0.081(3) Uani 1 1 d . . . H123 H 0.9399 1.0087 0.2672 0.097 Uiso 1 1 calc R . . C124 C 1.0237(8) 0.9070(9) 0.4051(7) 0.110(4) Uani 1 1 d . . . H124 H 1.0918 0.9205 0.4479 0.132 Uiso 1 1 calc R . . C125 C 1.0335(9) 0.9794(8) 0.3600(7) 0.089(3) Uani 1 1 d . . . H125 H 1.1077 1.0423 0.3715 0.107 Uiso 1 1 calc R . . C126 C 0.9127(7) 0.8125(7) 0.3881(6) 0.081(3) Uani 1 1 d . . . H126 H 0.9065 0.7643 0.4204 0.097 Uiso 1 1 calc R . . C131 C 0.6872(6) 0.5361(6) 0.2457(5) 0.0469(18) Uani 1 1 d . . . C132 C 0.7833(7) 0.5417(7) 0.2137(5) 0.068(2) Uani 1 1 d . . . H132 H 0.8454 0.6144 0.2241 0.081 Uiso 1 1 calc R . . C133 C 0.7900(10) 0.4415(10) 0.1660(7) 0.096(3) Uani 1 1 d . . . H133 H 0.8549 0.4461 0.1433 0.115 Uiso 1 1 calc R . . C134 C 0.7019(11) 0.3381(10) 0.1533(7) 0.098(4) Uani 1 1 d . . . H134 H 0.7078 0.2708 0.1232 0.118 Uiso 1 1 calc R . . C135 C 0.6007(10) 0.3272(7) 0.1836(6) 0.093(3) Uani 1 1 d . . . H135 H 0.5381 0.2539 0.1710 0.112 Uiso 1 1 calc R . . C136 C 0.5962(7) 0.4302(7) 0.2337(6) 0.071(2) Uani 1 1 d . . . H136 H 0.5327 0.4266 0.2581 0.085 Uiso 1 1 calc R . . P2 P 0.33108(15) 0.78998(15) 0.61603(13) 0.0448(5) Uani 1 1 d . . . C211 C 0.4028(6) 0.9034(5) 0.7339(5) 0.0450(18) Uani 1 1 d . . . C212 C 0.5245(6) 0.9462(6) 0.7737(6) 0.062(2) Uani 1 1 d . . . H212 H 0.5671 0.9166 0.7396 0.074 Uiso 1 1 calc R . . C213 C 0.5848(8) 1.0325(8) 0.8638(7) 0.098(3) Uani 1 1 d . . . H213 H 0.6674 1.0622 0.8890 0.118 Uiso 1 1 calc R . . C214 C 0.3403(7) 0.9456(7) 0.7882(6) 0.079(3) Uani 1 1 d . . . H214 H 0.2576 0.9163 0.7643 0.095 Uiso 1 1 calc R . . C215 C 0.4015(10) 1.0310(8) 0.8776(7) 0.100(3) Uani 1 1 d . . . H215 H 0.3601 1.0605 0.9133 0.120 Uiso 1 1 calc R . . C216 C 0.5223(10) 1.0725(7) 0.9140(7) 0.098(3) Uani 1 1 d . . . H216 H 0.5622 1.1295 0.9746 0.118 Uiso 1 1 calc R . . C221 C 0.1762(6) 0.7110(6) 0.6113(5) 0.0451(18) Uani 1 1 d . . . C222 C 0.0908(7) 0.7477(6) 0.5956(5) 0.062(2) Uani 1 1 d . . . H222 H 0.1118 0.8153 0.5842 0.074 Uiso 1 1 calc R . . C223 C -0.0280(7) 0.6838(8) 0.5966(6) 0.073(2) Uani 1 1 d . . . H223 H -0.0844 0.7099 0.5869 0.087 Uiso 1 1 calc R . . C224 C -0.0593(7) 0.5832(8) 0.6119(6) 0.080(3) Uani 1 1 d . . . H224 H -0.1369 0.5408 0.6135 0.096 Uiso 1 1 calc R . . C225 C 0.0241(7) 0.5458(7) 0.6247(6) 0.074(3) Uani 1 1 d . . . H225 H 0.0022 0.4770 0.6345 0.089 Uiso 1 1 calc R . . C226 C 0.1404(6) 0.6067(6) 0.6237(5) 0.059(2) Uani 1 1 d . . . H226 H 0.1949 0.5779 0.6313 0.070 Uiso 1 1 calc R . . C231 C 0.3278(6) 0.8690(6) 0.5412(5) 0.0467(18) Uani 1 1 d . . . C232 C 0.3035(8) 0.8097(7) 0.4463(6) 0.085(3) Uani 1 1 d . . . H232 H 0.2861 0.7314 0.4230 0.102 Uiso 1 1 calc R . . C233 C 0.3046(9) 0.8649(10) 0.3858(7) 0.111(4) Uani 1 1 d . . . H233 H 0.2883 0.8241 0.3220 0.133 Uiso 1 1 calc R . . C234 C 0.3296(8) 0.9796(9) 0.4194(8) 0.085(3) Uani 1 1 d . . . H234 H 0.3295 1.0167 0.3785 0.102 Uiso 1 1 calc R . . C235 C 0.3541(8) 1.0379(8) 0.5101(8) 0.089(3) Uani 1 1 d . . . H235 H 0.3725 1.1165 0.5330 0.107 Uiso 1 1 calc R . . C236 C 0.3523(7) 0.9831(7) 0.5707(6) 0.077(3) Uani 1 1 d . . . H236 H 0.3685 1.0254 0.6341 0.093 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0622(4) 0.0506(3) 0.0420(4) 0.0254(3) 0.0213(3) 0.0265(3) Ag2 0.0655(4) 0.0486(3) 0.0550(4) 0.0179(3) 0.0189(3) 0.0372(3) S 0.0520(11) 0.0389(9) 0.0382(11) 0.0162(9) 0.0119(9) 0.0230(8) O1 0.068(3) 0.040(2) 0.031(3) 0.016(2) 0.020(3) 0.030(2) O2 0.067(3) 0.044(3) 0.058(3) 0.030(3) 0.021(3) 0.027(2) C1 0.031(4) 0.041(4) 0.052(5) 0.024(4) 0.015(4) 0.018(3) C2 0.037(4) 0.033(4) 0.043(4) 0.018(4) 0.010(4) 0.017(3) C3 0.061(5) 0.049(4) 0.043(5) 0.024(4) 0.019(4) 0.033(4) C4 0.056(5) 0.056(5) 0.041(5) 0.022(4) 0.016(4) 0.033(4) C5 0.090(6) 0.065(5) 0.036(5) 0.022(4) 0.010(5) 0.031(5) C6 0.090(6) 0.046(5) 0.053(6) 0.019(5) 0.013(5) 0.019(4) C7 0.071(6) 0.057(5) 0.056(6) 0.020(5) 0.018(5) 0.031(5) C8 0.095(7) 0.089(7) 0.041(5) 0.031(5) 0.025(5) 0.042(5) C9 0.079(6) 0.069(5) 0.056(6) 0.038(5) 0.020(5) 0.034(5) O3 0.100(4) 0.075(4) 0.047(4) 0.012(3) 0.022(3) 0.031(3) C71 0.115(8) 0.089(7) 0.063(7) -0.003(6) 0.017(6) 0.040(6) P1 0.0518(12) 0.0464(11) 0.0420(12) 0.0233(10) 0.0174(10) 0.0212(9) C111 0.053(5) 0.042(4) 0.040(5) 0.020(4) 0.010(4) 0.018(4) C112 0.077(6) 0.074(5) 0.054(6) 0.028(5) 0.025(5) 0.043(5) C113 0.084(7) 0.124(8) 0.079(8) 0.045(7) 0.023(6) 0.069(6) C114 0.087(7) 0.106(7) 0.058(7) 0.026(6) 0.001(6) 0.062(6) C115 0.098(7) 0.084(6) 0.041(5) 0.027(5) 0.015(5) 0.041(6) C116 0.069(5) 0.082(6) 0.045(5) 0.027(5) 0.013(5) 0.045(5) C121 0.042(4) 0.050(4) 0.040(5) 0.017(4) 0.010(4) 0.013(4) C122 0.081(6) 0.052(5) 0.062(6) 0.031(5) 0.025(5) 0.026(5) C123 0.092(7) 0.060(6) 0.095(8) 0.046(6) 0.043(6) 0.023(6) C124 0.054(6) 0.133(9) 0.102(9) 0.056(8) 0.004(6) 0.007(6) C125 0.078(7) 0.073(6) 0.087(8) 0.037(6) 0.027(6) 0.003(6) C126 0.063(6) 0.086(6) 0.083(7) 0.055(6) 0.009(5) 0.013(5) C131 0.059(5) 0.047(4) 0.031(4) 0.016(4) 0.010(4) 0.023(4) C132 0.091(6) 0.067(5) 0.059(6) 0.025(5) 0.034(5) 0.047(5) C133 0.126(9) 0.113(8) 0.071(7) 0.033(7) 0.034(7) 0.078(8) C134 0.150(11) 0.101(9) 0.053(6) 0.008(7) 0.004(7) 0.093(9) C135 0.133(9) 0.049(5) 0.070(7) 0.014(5) -0.017(7) 0.039(6) C136 0.070(6) 0.058(5) 0.075(7) 0.035(5) 0.005(5) 0.022(5) P2 0.0475(11) 0.0405(10) 0.0482(13) 0.0138(10) 0.0129(10) 0.0255(9) C211 0.052(5) 0.038(4) 0.045(5) 0.014(4) 0.013(4) 0.023(4) C212 0.044(5) 0.060(5) 0.065(6) 0.012(5) 0.012(5) 0.021(4) C213 0.072(7) 0.098(8) 0.065(7) -0.007(6) -0.014(6) 0.025(6) C214 0.068(6) 0.077(6) 0.066(7) -0.005(5) 0.014(5) 0.035(5) C215 0.097(8) 0.089(7) 0.071(8) -0.018(6) 0.021(7) 0.042(6) C216 0.115(9) 0.058(6) 0.057(7) -0.014(5) -0.002(7) 0.018(6) C221 0.044(4) 0.046(4) 0.041(4) 0.012(4) 0.006(4) 0.023(4) C222 0.068(5) 0.062(5) 0.065(6) 0.029(5) 0.016(5) 0.038(4) C223 0.050(5) 0.095(7) 0.081(7) 0.036(6) 0.018(5) 0.042(5) C224 0.053(6) 0.079(6) 0.090(7) 0.034(6) 0.022(5) 0.014(5) C225 0.063(6) 0.068(6) 0.087(7) 0.043(5) 0.006(5) 0.024(5) C226 0.051(5) 0.052(5) 0.057(5) 0.016(4) 0.000(4) 0.020(4) C231 0.045(4) 0.046(4) 0.053(5) 0.017(4) 0.016(4) 0.025(4) C232 0.150(9) 0.070(6) 0.076(7) 0.041(6) 0.055(7) 0.075(6) C233 0.195(11) 0.121(9) 0.077(7) 0.062(7) 0.070(8) 0.105(9) C234 0.106(8) 0.097(8) 0.094(8) 0.065(7) 0.053(7) 0.059(7) C235 0.104(7) 0.064(6) 0.109(9) 0.052(7) 0.015(7) 0.042(6) C236 0.105(7) 0.059(5) 0.075(7) 0.030(5) 0.019(6) 0.045(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O1 2.347(4) . ? Ag1 P1 2.3503(19) . ? Ag1 S 2.4489(18) . ? Ag1 O2 2.748(4) 2_666 ? Ag1 Ag2 3.3839(8) . ? Ag1 Ag2 4.3918(9) 2_666 ? Ag2 O1 2.365(4) 2_666 ? Ag2 P2 2.3784(17) . ? Ag2 S 2.5267(18) . ? Ag2 O2 2.590(5) 2_666 ? S C2 1.772(6) . ? O1 C1 1.243(7) . ? O1 Ag2 2.365(4) 2_666 ? O2 C1 1.257(7) . ? O2 Ag2 2.590(5) 2_666 ? C1 C2 1.536(8) . ? C2 C3 1.324(8) . ? C3 C4 1.476(9) . ? C4 C9 1.374(9) . ? C4 C5 1.391(9) . ? C5 C6 1.371(9) . ? C6 C7 1.340(10) . ? C7 C8 1.370(10) . ? C7 O3 1.381(8) . ? C8 C9 1.390(9) . ? O3 C71 1.432(9) . ? P1 C121 1.820(7) . ? P1 C111 1.831(7) . ? P1 C131 1.841(7) . ? C111 C112 1.371(9) . ? C111 C116 1.375(9) . ? C112 C113 1.373(10) . ? C113 C114 1.350(11) . ? C114 C115 1.375(10) . ? C115 C116 1.374(9) . ? C121 C122 1.369(9) . ? C121 C126 1.371(9) . ? C122 C123 1.374(9) . ? C123 C125 1.354(11) . ? C124 C125 1.354(12) . ? C124 C126 1.395(10) . ? C131 C132 1.367(9) . ? C131 C136 1.373(9) . ? C132 C133 1.381(11) . ? C133 C134 1.331(12) . ? C134 C135 1.402(12) . ? C135 C136 1.409(10) . ? P2 C221 1.802(7) . ? P2 C211 1.816(7) . ? P2 C231 1.823(7) . ? C211 C212 1.380(8) . ? C211 C214 1.393(9) . ? C212 C213 1.390(10) . ? C213 C216 1.344(11) . ? C214 C215 1.379(10) . ? C215 C216 1.365(11) . ? C221 C222 1.381(8) . ? C221 C226 1.389(9) . ? C222 C223 1.413(9) . ? C223 C224 1.370(10) . ? C224 C225 1.359(10) . ? C225 C226 1.379(9) . ? C231 C236 1.360(9) . ? C231 C232 1.380(10) . ? C232 C233 1.378(11) . ? C233 C234 1.364(11) . ? C234 C235 1.323(11) . ? C235 C236 1.373(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ag1 P1 118.29(11) . . ? O1 Ag1 S 78.88(11) . . ? P1 Ag1 S 155.62(6) . . ? O1 Ag1 O2 88.86(13) . 2_666 ? P1 Ag1 O2 101.16(11) . 2_666 ? S Ag1 O2 96.08(11) . 2_666 ? O1 Ag1 Ag2 87.31(10) . . ? P1 Ag1 Ag2 142.12(5) . . ? S Ag1 Ag2 48.12(4) . . ? O2 Ag1 Ag2 48.62(10) 2_666 . ? O1 Ag1 Ag2 21.34(10) . 2_666 ? P1 Ag1 Ag2 101.60(5) . 2_666 ? S Ag1 Ag2 98.58(4) . 2_666 ? O2 Ag1 Ag2 78.66(9) 2_666 2_666 ? Ag2 Ag1 Ag2 94.392(16) . 2_666 ? O1 Ag2 P2 126.91(11) 2_666 . ? O1 Ag2 S 101.61(11) 2_666 . ? P2 Ag2 S 130.63(6) . . ? O1 Ag2 O2 52.19(14) 2_666 2_666 ? P2 Ag2 O2 117.23(11) . 2_666 ? S Ag2 O2 98.26(10) . 2_666 ? O1 Ag2 Ag1 79.11(10) 2_666 . ? P2 Ag2 Ag1 141.88(5) . . ? S Ag2 Ag1 46.19(4) . . ? O2 Ag2 Ag1 52.76(9) 2_666 . ? C2 S Ag1 101.3(2) . . ? C2 S Ag2 99.3(2) . . ? Ag1 S Ag2 85.69(6) . . ? C1 O1 Ag1 119.9(4) . . ? C1 O1 Ag2 98.1(4) . 2_666 ? Ag1 O1 Ag2 137.49(19) . 2_666 ? C1 O2 Ag2 87.2(4) . 2_666 ? O1 C1 O2 122.2(6) . . ? O1 C1 C2 120.2(6) . . ? O2 C1 C2 117.6(6) . . ? C3 C2 C1 117.2(6) . . ? C3 C2 S 125.2(5) . . ? C1 C2 S 117.6(5) . . ? C2 C3 C4 132.5(6) . . ? C9 C4 C5 115.6(7) . . ? C9 C4 C3 119.2(7) . . ? C5 C4 C3 125.1(7) . . ? C6 C5 C4 122.8(7) . . ? C7 C6 C5 119.5(7) . . ? C6 C7 C8 121.0(8) . . ? C6 C7 O3 126.3(7) . . ? C8 C7 O3 112.7(8) . . ? C7 C8 C9 118.6(8) . . ? C4 C9 C8 122.5(7) . . ? C7 O3 C71 116.0(7) . . ? C121 P1 C111 105.3(3) . . ? C121 P1 C131 105.4(3) . . ? C111 P1 C131 102.0(3) . . ? C121 P1 Ag1 112.6(2) . . ? C111 P1 Ag1 118.5(2) . . ? C131 P1 Ag1 111.7(2) . . ? C112 C111 C116 118.9(7) . . ? C112 C111 P1 119.5(6) . . ? C116 C111 P1 121.5(6) . . ? C111 C112 C113 122.3(8) . . ? C114 C113 C112 118.7(8) . . ? C113 C114 C115 119.8(8) . . ? C116 C115 C114 121.8(8) . . ? C115 C116 C111 118.4(7) . . ? C122 C121 C126 118.8(7) . . ? C122 C121 P1 125.5(6) . . ? C126 C121 P1 115.7(6) . . ? C121 C122 C123 120.4(8) . . ? C125 C123 C122 121.2(9) . . ? C125 C124 C126 120.7(9) . . ? C123 C125 C124 119.0(8) . . ? C121 C126 C124 119.8(8) . . ? C132 C131 C136 120.6(7) . . ? C132 C131 P1 123.2(6) . . ? C136 C131 P1 116.2(6) . . ? C131 C132 C133 121.2(8) . . ? C134 C133 C132 118.9(10) . . ? C133 C134 C135 122.3(10) . . ? C134 C135 C136 118.2(9) . . ? C131 C136 C135 118.7(8) . . ? C221 P2 C211 104.4(3) . . ? C221 P2 C231 104.9(3) . . ? C211 P2 C231 104.3(3) . . ? C221 P2 Ag2 119.8(2) . . ? C211 P2 Ag2 111.9(2) . . ? C231 P2 Ag2 110.1(2) . . ? C212 C211 C214 118.0(7) . . ? C212 C211 P2 118.4(5) . . ? C214 C211 P2 123.5(6) . . ? C211 C212 C213 121.4(7) . . ? C216 C213 C212 119.1(9) . . ? C215 C214 C211 119.8(8) . . ? C216 C215 C214 120.4(9) . . ? C213 C216 C215 121.2(9) . . ? C222 C221 C226 118.0(6) . . ? C222 C221 P2 124.0(6) . . ? C226 C221 P2 118.0(5) . . ? C221 C222 C223 120.9(7) . . ? C224 C223 C222 119.5(7) . . ? C225 C224 C223 119.3(8) . . ? C224 C225 C226 122.0(8) . . ? C225 C226 C221 120.1(7) . . ? C236 C231 C232 116.7(7) . . ? C236 C231 P2 125.8(6) . . ? C232 C231 P2 117.4(6) . . ? C233 C232 C231 120.9(8) . . ? C234 C233 C232 119.9(9) . . ? C235 C234 C233 120.0(9) . . ? C234 C235 C236 120.3(9) . . ? C231 C236 C235 122.3(9) . . ? _diffrn_measured_fraction_theta_max 0.830 _diffrn_reflns_theta_full 28.08 _diffrn_measured_fraction_theta_full 0.830 _refine_diff_density_max 0.920 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.107 #=== END data_5 _database_code_depnum_ccdc_archive 'CCDC 261751' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H34 Ag2 Br2 O3 P2 S' _chemical_formula_weight 1092.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.7725(9) _cell_length_b 17.2472(10) _cell_length_c 17.4361(9) _cell_angle_alpha 90.00 _cell_angle_beta 116.0150(10) _cell_angle_gamma 90.00 _cell_volume 4262.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max .28 _exptl_crystal_size_mid .26 _exptl_crystal_size_min .12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 2.957 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.761479 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23200 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.1476 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 28.03 _reflns_number_total 9513 _reflns_number_gt 4049 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0138P)^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 9513 _refine_ls_number_parameters 500 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1341 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0572 _refine_ls_wR_factor_gt 0.0469 _refine_ls_goodness_of_fit_ref 0.708 _refine_ls_restrained_S_all 0.708 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.56244(2) 0.87058(2) 0.659001(19) 0.05497(11) Uani 1 1 d . . . Ag2 Ag 0.39600(2) 0.822686(19) 0.476483(19) 0.05153(10) Uani 1 1 d . . . S S 0.39643(7) 0.89892(6) 0.59407(6) 0.0411(3) Uani 1 1 d . . . Br1 Br 0.07486(4) 0.88103(4) 0.19463(3) 0.1079(2) Uani 1 1 d . . . Br2 Br 0.01945(4) 0.89263(4) 0.49078(4) 0.1110(2) Uani 1 1 d . . . O1 O 0.56429(18) 1.00800(16) 0.63732(16) 0.0484(8) Uani 1 1 d . . . O2 O 0.48508(17) 1.10124(17) 0.54452(16) 0.0528(8) Uani 1 1 d . . . O3 O 0.2549(3) 0.9596(2) 0.3072(2) 0.0713(12) Uani 1 1 d . . . H3 H 0.306(3) 0.966(3) 0.328(3) 0.07(2) Uiso 1 1 d . . . C1 C 0.4909(3) 1.0364(3) 0.5787(3) 0.0400(11) Uani 1 1 d . . . C2 C 0.3994(3) 0.9893(2) 0.5462(2) 0.0350(10) Uani 1 1 d . . . C3 C 0.3243(3) 1.0140(2) 0.4784(2) 0.0431(11) Uani 1 1 d . . . H3A H 0.3293 1.0620 0.4565 0.052 Uiso 1 1 calc R . . C4 C 0.2336(3) 0.9730(2) 0.4342(3) 0.0441(11) Uani 1 1 d . . . C5 C 0.2036(3) 0.9492(2) 0.3506(3) 0.0488(12) Uani 1 1 d . . . C6 C 0.1158(3) 0.9129(3) 0.3077(3) 0.0579(13) Uani 1 1 d . . . C7 C 0.0612(3) 0.8982(3) 0.3493(3) 0.0678(15) Uani 1 1 d . . . H7 H 0.0027 0.8744 0.3206 0.081 Uiso 1 1 calc R . . C8 C 0.0930(3) 0.9188(3) 0.4331(3) 0.0638(14) Uani 1 1 d . . . C9 C 0.1772(3) 0.9564(2) 0.4751(3) 0.0539(12) Uani 1 1 d . . . H9 H 0.1971 0.9711 0.5317 0.065 Uiso 1 1 calc R . . P1 P 0.70735(7) 0.80595(7) 0.72705(7) 0.0468(3) Uani 1 1 d . . . C111 C 0.7881(3) 0.8509(3) 0.8259(2) 0.0459(12) Uani 1 1 d . . . C112 C 0.7706(3) 0.9261(3) 0.8426(3) 0.0718(15) Uani 1 1 d . . . H112 H 0.7175 0.9518 0.8033 0.086 Uiso 1 1 calc R . . C113 C 0.8307(4) 0.9639(3) 0.9167(3) 0.0884(18) Uani 1 1 d . . . H113 H 0.8183 1.0146 0.9268 0.106 Uiso 1 1 calc R . . C114 C 0.9076(4) 0.9263(4) 0.9743(3) 0.0843(17) Uani 1 1 d . . . H114 H 0.9480 0.9515 1.0242 0.101 Uiso 1 1 calc R . . C115 C 0.9261(3) 0.8530(3) 0.9604(3) 0.0822(17) Uani 1 1 d . . . H115 H 0.9792 0.8280 1.0006 0.099 Uiso 1 1 calc R . . C116 C 0.8522(3) 0.8421(3) 0.6815(3) 0.0711(15) Uani 1 1 d . . . H116 H 0.8832 0.8658 0.7344 0.085 Uiso 1 1 calc R . . C121 C 0.7678(3) 0.8050(3) 0.6605(3) 0.0484(12) Uani 1 1 d . . . C122 C 0.8667(3) 0.8142(3) 0.8866(3) 0.0665(14) Uani 1 1 d . . . H122 H 0.8799 0.7633 0.8779 0.080 Uiso 1 1 calc R . . C123 C 0.8914(4) 0.8443(3) 0.6243(4) 0.106(2) Uani 1 1 d . . . H123 H 0.9481 0.8701 0.6386 0.127 Uiso 1 1 calc R . . C124 C 0.8472(5) 0.8088(4) 0.5474(4) 0.127(3) Uani 1 1 d . . . H124 H 0.8742 0.8093 0.5095 0.153 Uiso 1 1 calc R . . C125 C 0.7639(5) 0.7726(3) 0.5260(3) 0.110(2) Uani 1 1 d . . . H125 H 0.7335 0.7486 0.4730 0.132 Uiso 1 1 calc R . . C126 C 0.7237(3) 0.7708(3) 0.5815(3) 0.0813(17) Uani 1 1 d . . . H126 H 0.6660 0.7463 0.5655 0.098 Uiso 1 1 calc R . . C131 C 0.7026(3) 0.7049(3) 0.7524(2) 0.0485(12) Uani 1 1 d . . . C132 C 0.7693(3) 0.6521(3) 0.7586(3) 0.0673(14) Uani 1 1 d . . . H132 H 0.8192 0.6676 0.7473 0.081 Uiso 1 1 calc R . . C133 C 0.7649(4) 0.5758(3) 0.7814(3) 0.0779(16) Uani 1 1 d . . . H133 H 0.8118 0.5408 0.7863 0.093 Uiso 1 1 calc R . . C134 C 0.6915(5) 0.5528(3) 0.7965(3) 0.0887(18) Uani 1 1 d . . . H134 H 0.6877 0.5016 0.8116 0.106 Uiso 1 1 calc R . . C135 C 0.6242(4) 0.6036(4) 0.7898(3) 0.101(2) Uani 1 1 d . . . H135 H 0.5738 0.5873 0.7999 0.122 Uiso 1 1 calc R . . C136 C 0.6288(3) 0.6797(3) 0.7682(3) 0.0776(15) Uani 1 1 d . . . H136 H 0.5819 0.7143 0.7643 0.093 Uiso 1 1 calc R . . P2 P 0.35333(7) 0.72109(7) 0.37468(6) 0.0444(3) Uani 1 1 d . . . C211 C 0.4476(3) 0.6515(2) 0.4009(3) 0.0446(11) Uani 1 1 d . . . C212 C 0.5030(3) 0.6344(3) 0.4857(3) 0.0664(14) Uani 1 1 d . . . H212 H 0.4909 0.6584 0.5277 0.080 Uiso 1 1 calc R . . C213 C 0.5768(4) 0.5814(3) 0.5090(3) 0.0877(18) Uani 1 1 d . . . H213 H 0.6128 0.5691 0.5661 0.105 Uiso 1 1 calc R . . C214 C 0.5964(3) 0.5475(3) 0.4479(4) 0.0903(19) Uani 1 1 d . . . H214 H 0.6465 0.5130 0.4632 0.108 Uiso 1 1 calc R . . C215 C 0.5420(4) 0.5646(3) 0.3644(4) 0.0885(18) Uani 1 1 d . . . H215 H 0.5548 0.5411 0.3227 0.106 Uiso 1 1 calc R . . C216 C 0.4682(3) 0.6163(3) 0.3405(3) 0.0670(14) Uani 1 1 d . . . H216 H 0.4320 0.6273 0.2830 0.080 Uiso 1 1 calc R . . C221 C 0.2534(3) 0.6665(3) 0.3674(2) 0.0425(11) Uani 1 1 d . . . C222 C 0.2469(3) 0.5866(3) 0.3645(3) 0.0675(14) Uani 1 1 d . . . H222 H 0.2968 0.5576 0.3650 0.081 Uiso 1 1 calc R . . C223 C 0.1677(4) 0.5487(3) 0.3607(3) 0.0859(17) Uani 1 1 d . . . H223 H 0.1654 0.4948 0.3592 0.103 Uiso 1 1 calc R . . C224 C 0.0944(4) 0.5891(4) 0.3594(3) 0.0879(18) Uani 1 1 d . . . H224 H 0.0411 0.5635 0.3562 0.105 Uiso 1 1 calc R . . C225 C 0.0988(3) 0.6677(4) 0.3627(3) 0.0889(18) Uani 1 1 d . . . H225 H 0.0486 0.6964 0.3621 0.107 Uiso 1 1 calc R . . C226 C 0.1773(3) 0.7042(3) 0.3671(3) 0.0683(14) Uani 1 1 d . . . H226 H 0.1792 0.7581 0.3700 0.082 Uiso 1 1 calc R . . C231 C 0.3234(3) 0.7527(2) 0.2667(2) 0.0415(11) Uani 1 1 d . . . C232 C 0.3730(3) 0.8137(3) 0.2570(3) 0.0662(14) Uani 1 1 d . . . H232 H 0.4195 0.8372 0.3050 0.079 Uiso 1 1 calc R . . C233 C 0.3549(4) 0.8408(3) 0.1769(3) 0.0872(18) Uani 1 1 d . . . H233 H 0.3897 0.8822 0.1715 0.105 Uiso 1 1 calc R . . C234 C 0.2872(4) 0.8078(3) 0.1060(3) 0.0790(17) Uani 1 1 d . . . H234 H 0.2747 0.8268 0.0522 0.095 Uiso 1 1 calc R . . C235 C 0.2378(3) 0.7468(3) 0.1145(3) 0.0765(16) Uani 1 1 d . . . H235 H 0.1920 0.7231 0.0662 0.092 Uiso 1 1 calc R . . C236 C 0.2551(3) 0.7196(3) 0.1939(3) 0.0637(14) Uani 1 1 d . . . H236 H 0.2201 0.6781 0.1988 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0417(2) 0.0614(3) 0.0546(2) 0.00030(19) 0.01450(17) 0.00687(18) Ag2 0.0593(2) 0.0377(2) 0.0509(2) -0.00845(18) 0.01798(17) -0.00478(19) S 0.0382(6) 0.0414(8) 0.0468(6) 0.0005(5) 0.0216(5) -0.0050(5) Br1 0.0819(4) 0.1311(6) 0.0722(4) -0.0221(4) -0.0017(3) -0.0226(4) Br2 0.0728(4) 0.1275(6) 0.1524(6) 0.0177(5) 0.0674(4) -0.0184(4) O1 0.0330(17) 0.051(2) 0.0527(18) -0.0081(15) 0.0108(15) -0.0114(15) O2 0.0494(18) 0.043(2) 0.071(2) -0.0036(17) 0.0305(16) -0.0122(16) O3 0.046(2) 0.101(3) 0.058(2) -0.0004(19) 0.014(2) -0.010(2) C1 0.037(3) 0.044(3) 0.045(3) -0.023(2) 0.024(2) -0.013(2) C2 0.029(2) 0.036(3) 0.041(3) -0.004(2) 0.016(2) -0.003(2) C3 0.043(3) 0.039(3) 0.052(3) -0.003(2) 0.026(2) -0.005(2) C4 0.031(3) 0.043(3) 0.050(3) 0.009(2) 0.010(2) 0.000(2) C5 0.038(3) 0.045(3) 0.059(3) 0.009(3) 0.017(3) 0.005(2) C6 0.038(3) 0.049(3) 0.067(3) 0.008(3) 0.004(3) 0.003(2) C7 0.036(3) 0.056(4) 0.085(4) 0.005(3) 0.003(3) -0.003(2) C8 0.037(3) 0.065(4) 0.088(4) 0.015(3) 0.026(3) 0.002(3) C9 0.039(3) 0.056(4) 0.058(3) 0.004(2) 0.013(3) -0.003(2) P1 0.0389(7) 0.0512(9) 0.0486(7) 0.0039(6) 0.0179(6) 0.0011(6) C111 0.037(3) 0.057(4) 0.043(3) 0.007(2) 0.017(2) 0.001(2) C112 0.071(4) 0.074(5) 0.058(3) 0.001(3) 0.016(3) 0.016(3) C113 0.103(5) 0.075(5) 0.068(4) -0.008(4) 0.021(3) 0.004(4) C114 0.084(4) 0.082(5) 0.062(4) -0.017(4) 0.009(3) -0.024(4) C115 0.076(4) 0.083(5) 0.052(3) 0.002(3) -0.006(3) -0.004(3) C116 0.070(4) 0.088(5) 0.068(3) -0.002(3) 0.042(3) -0.008(3) C121 0.050(3) 0.044(3) 0.052(3) 0.006(2) 0.023(2) 0.003(2) C122 0.067(3) 0.068(4) 0.054(3) 0.005(3) 0.016(3) -0.001(3) C123 0.113(5) 0.123(6) 0.122(5) -0.036(4) 0.089(4) -0.050(4) C124 0.180(7) 0.130(7) 0.146(6) -0.054(5) 0.140(6) -0.072(5) C125 0.161(6) 0.109(6) 0.097(5) -0.042(4) 0.089(5) -0.046(5) C126 0.093(4) 0.091(5) 0.073(4) -0.020(3) 0.049(4) -0.038(3) C131 0.041(3) 0.063(4) 0.039(3) 0.005(2) 0.016(2) 0.000(3) C132 0.067(4) 0.050(4) 0.084(4) 0.016(3) 0.032(3) -0.003(3) C133 0.079(4) 0.063(5) 0.079(4) 0.003(3) 0.023(3) -0.001(3) C134 0.112(5) 0.063(5) 0.077(4) 0.016(3) 0.028(4) -0.015(4) C135 0.105(5) 0.100(6) 0.115(5) 0.040(4) 0.063(4) -0.011(4) C136 0.080(4) 0.078(5) 0.090(4) 0.022(3) 0.052(3) 0.002(3) P2 0.0491(7) 0.0377(8) 0.0451(7) -0.0054(6) 0.0197(6) -0.0062(6) C211 0.045(3) 0.040(3) 0.051(3) -0.004(2) 0.023(2) -0.006(2) C212 0.071(3) 0.062(4) 0.060(3) 0.003(3) 0.023(3) 0.003(3) C213 0.085(4) 0.078(5) 0.070(4) 0.013(3) 0.006(3) 0.014(3) C214 0.070(4) 0.089(5) 0.106(5) 0.021(4) 0.033(4) 0.033(3) C215 0.097(5) 0.091(5) 0.097(5) 0.008(4) 0.061(4) 0.031(4) C216 0.068(3) 0.073(4) 0.066(3) 0.010(3) 0.035(3) 0.017(3) C221 0.042(3) 0.040(3) 0.046(3) 0.000(2) 0.020(2) -0.004(2) C222 0.064(3) 0.049(4) 0.101(4) -0.007(3) 0.046(3) -0.008(3) C223 0.086(4) 0.049(4) 0.128(5) 0.012(3) 0.051(4) -0.014(3) C224 0.054(4) 0.084(5) 0.121(5) 0.025(4) 0.033(3) -0.009(4) C225 0.049(3) 0.085(5) 0.136(5) 0.024(4) 0.044(3) 0.011(3) C226 0.054(3) 0.055(4) 0.097(4) 0.009(3) 0.034(3) -0.005(3) C231 0.048(3) 0.035(3) 0.047(3) 0.000(2) 0.025(2) -0.001(2) C232 0.083(4) 0.069(4) 0.047(3) -0.005(3) 0.028(3) -0.020(3) C233 0.129(5) 0.070(5) 0.069(4) 0.004(3) 0.049(4) -0.024(4) C234 0.114(5) 0.074(5) 0.054(4) 0.005(3) 0.041(3) 0.007(4) C235 0.087(4) 0.088(5) 0.046(3) -0.007(3) 0.021(3) -0.010(3) C236 0.070(3) 0.058(4) 0.054(3) -0.004(3) 0.019(3) -0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P1 2.3442(11) . ? Ag1 O1 2.402(3) . ? Ag1 S 2.4033(10) . ? Ag1 Ag2 3.2208(4) . ? Ag2 P2 2.3719(11) . ? Ag2 S 2.4331(10) . ? Ag2 O2 2.445(3) 3_676 ? S C2 1.779(4) . ? Br1 C6 1.869(4) . ? Br2 C8 1.893(4) . ? O1 C1 1.260(4) . ? O2 C1 1.251(4) . ? O2 Ag2 2.445(3) 3_676 ? O3 C5 1.340(5) . ? C1 C2 1.532(5) . ? C2 C3 1.324(4) . ? C3 C4 1.473(5) . ? C4 C5 1.382(5) . ? C4 C9 1.393(5) . ? C5 C6 1.401(5) . ? C6 C7 1.370(5) . ? C7 C8 1.368(5) . ? C8 C9 1.366(5) . ? P1 C121 1.796(4) . ? P1 C131 1.808(5) . ? P1 C111 1.808(4) . ? C111 C122 1.381(5) . ? C111 C112 1.383(5) . ? C112 C113 1.384(6) . ? C113 C114 1.353(6) . ? C114 C115 1.343(6) . ? C115 C122 1.386(5) . ? C116 C121 1.374(5) . ? C116 C123 1.385(5) . ? C121 C126 1.374(5) . ? C123 C124 1.356(6) . ? C124 C125 1.352(6) . ? C125 C126 1.370(6) . ? C131 C132 1.361(5) . ? C131 C136 1.378(5) . ? C132 C133 1.384(6) . ? C133 C134 1.355(6) . ? C134 C135 1.341(6) . ? C135 C136 1.375(6) . ? P2 C221 1.792(4) . ? P2 C211 1.807(4) . ? P2 C231 1.813(4) . ? C211 C216 1.372(5) . ? C211 C212 1.380(5) . ? C212 C213 1.394(6) . ? C213 C214 1.364(6) . ? C214 C215 1.359(6) . ? C215 C216 1.377(6) . ? C221 C226 1.362(5) . ? C221 C222 1.381(5) . ? C222 C223 1.385(5) . ? C223 C224 1.341(6) . ? C224 C225 1.357(6) . ? C225 C226 1.362(5) . ? C231 C232 1.364(5) . ? C231 C236 1.377(5) . ? C232 C233 1.379(5) . ? C233 C234 1.355(6) . ? C234 C235 1.355(6) . ? C235 C236 1.371(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Ag1 O1 118.19(7) . . ? P1 Ag1 S 162.55(4) . . ? O1 Ag1 S 79.12(7) . . ? P1 Ag1 Ag2 124.70(3) . . ? O1 Ag1 Ag2 99.12(6) . . ? S Ag1 Ag2 48.64(2) . . ? P2 Ag2 S 157.64(4) . . ? P2 Ag2 O2 105.60(7) . 3_676 ? S Ag2 O2 96.75(7) . 3_676 ? P2 Ag2 Ag1 140.33(3) . . ? S Ag2 Ag1 47.85(2) . . ? O2 Ag2 Ag1 70.36(6) 3_676 . ? C2 S Ag1 98.75(12) . . ? C2 S Ag2 94.00(12) . . ? Ag1 S Ag2 83.51(3) . . ? C1 O1 Ag1 116.2(3) . . ? C1 O2 Ag2 130.6(3) . 3_676 ? O2 C1 O1 125.7(4) . . ? O2 C1 C2 115.9(4) . . ? O1 C1 C2 118.4(4) . . ? C3 C2 C1 119.3(4) . . ? C3 C2 S 120.2(3) . . ? C1 C2 S 120.4(3) . . ? C2 C3 C4 126.6(4) . . ? C5 C4 C9 118.6(4) . . ? C5 C4 C3 120.0(4) . . ? C9 C4 C3 121.5(4) . . ? O3 C5 C4 122.9(4) . . ? O3 C5 C6 117.3(5) . . ? C4 C5 C6 119.8(4) . . ? C7 C6 C5 120.3(4) . . ? C7 C6 Br1 119.8(4) . . ? C5 C6 Br1 119.8(4) . . ? C8 C7 C6 119.7(4) . . ? C9 C8 C7 120.7(4) . . ? C9 C8 Br2 120.5(4) . . ? C7 C8 Br2 118.9(4) . . ? C8 C9 C4 120.9(4) . . ? C121 P1 C131 103.9(2) . . ? C121 P1 C111 105.6(2) . . ? C131 P1 C111 105.55(19) . . ? C121 P1 Ag1 110.69(13) . . ? C131 P1 Ag1 116.50(14) . . ? C111 P1 Ag1 113.65(16) . . ? C122 C111 C112 117.6(4) . . ? C122 C111 P1 123.6(4) . . ? C112 C111 P1 118.7(4) . . ? C111 C112 C113 121.3(5) . . ? C114 C113 C112 119.4(5) . . ? C115 C114 C113 120.8(5) . . ? C114 C115 C122 120.6(5) . . ? C121 C116 C123 120.5(5) . . ? C116 C121 C126 118.1(4) . . ? C116 C121 P1 123.4(4) . . ? C126 C121 P1 118.2(4) . . ? C111 C122 C115 120.3(5) . . ? C124 C123 C116 120.1(5) . . ? C125 C124 C123 119.8(5) . . ? C124 C125 C126 120.7(5) . . ? C125 C126 C121 120.8(5) . . ? C132 C131 C136 117.7(5) . . ? C132 C131 P1 123.4(4) . . ? C136 C131 P1 118.9(4) . . ? C131 C132 C133 121.6(5) . . ? C134 C133 C132 119.3(5) . . ? C135 C134 C133 120.1(6) . . ? C134 C135 C136 120.9(6) . . ? C135 C136 C131 120.4(5) . . ? C221 P2 C211 105.7(2) . . ? C221 P2 C231 105.30(18) . . ? C211 P2 C231 105.83(19) . . ? C221 P2 Ag2 113.16(14) . . ? C211 P2 Ag2 111.69(14) . . ? C231 P2 Ag2 114.48(14) . . ? C216 C211 C212 118.5(4) . . ? C216 C211 P2 123.1(4) . . ? C212 C211 P2 118.4(4) . . ? C211 C212 C213 120.5(5) . . ? C214 C213 C212 120.0(5) . . ? C215 C214 C213 119.4(5) . . ? C214 C215 C216 121.2(5) . . ? C211 C216 C215 120.4(4) . . ? C226 C221 C222 115.2(4) . . ? C226 C221 P2 119.7(4) . . ? C222 C221 P2 125.1(4) . . ? C221 C222 C223 121.6(4) . . ? C224 C223 C222 120.5(5) . . ? C223 C224 C225 119.4(5) . . ? C224 C225 C226 119.5(5) . . ? C225 C226 C221 123.9(5) . . ? C232 C231 C236 117.7(4) . . ? C232 C231 P2 117.3(3) . . ? C236 C231 P2 125.0(4) . . ? C231 C232 C233 120.8(4) . . ? C234 C233 C232 120.8(5) . . ? C233 C234 C235 119.2(5) . . ? C234 C235 C236 120.4(5) . . ? C235 C236 C231 121.2(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O1 0.74(4) 1.91(4) 2.639(4) 170(5) 3_676 _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.494 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.065 #=== END data_6.C3H6O _database_code_depnum_ccdc_archive 'CCDC 261752' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H40 Ag2 O4 P2 S' _chemical_formula_weight 966.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.5325(12) _cell_length_b 13.1244(9) _cell_length_c 18.6677(12) _cell_angle_alpha 90.00 _cell_angle_beta 100.0680(10) _cell_angle_gamma 90.00 _cell_volume 4229.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 1.093 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22434 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.1889 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.05 _reflns_number_total 9378 _reflns_number_gt 3463 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0320P)^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 9378 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1552 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 0.701 _refine_ls_restrained_S_all 0.701 _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 Ag1 Ag 0.03233(2) 0.19067(3) 0.05974(2) 0.05675(14) Uani 1 1 d . . . P1 P 0.14327(8) 0.29497(11) 0.06701(8) 0.0539(4) Uani 1 1 d . . . C111 C 0.2114(3) 0.2864(4) 0.1526(3) 0.0520(14) Uani 1 1 d . . . C112 C 0.2332(3) 0.1915(5) 0.1800(3) 0.0689(16) Uani 1 1 d . . . H112 H 0.2125 0.1341 0.1546 0.083 Uiso 1 1 calc R . . C113 C 0.2844(4) 0.1794(5) 0.2433(4) 0.088(2) Uani 1 1 d . . . H113 H 0.2987 0.1145 0.2606 0.106 Uiso 1 1 calc R . . C114 C 0.3145(4) 0.2635(6) 0.2812(3) 0.087(2) Uani 1 1 d . . . H114 H 0.3498 0.2556 0.3242 0.104 Uiso 1 1 calc R . . C115 C 0.2931(4) 0.3585(6) 0.2565(3) 0.087(2) Uani 1 1 d . . . H115 H 0.3126 0.4152 0.2835 0.104 Uiso 1 1 calc R . . C116 C 0.2426(3) 0.3715(5) 0.1915(3) 0.0731(17) Uani 1 1 d . . . H116 H 0.2295 0.4366 0.1738 0.088 Uiso 1 1 calc R . . C121 C 0.1215(3) 0.4291(4) 0.0571(3) 0.0553(15) Uani 1 1 d . . . C122 C 0.0638(4) 0.4652(5) 0.0907(3) 0.0767(19) Uani 1 1 d . . . H122 H 0.0369 0.4199 0.1154 0.092 Uiso 1 1 calc R . . C123 C 0.0440(5) 0.5683(6) 0.0889(3) 0.099(2) Uani 1 1 d . . . H123 H 0.0045 0.5912 0.1122 0.119 Uiso 1 1 calc R . . C124 C 0.0828(5) 0.6343(6) 0.0531(4) 0.090(2) Uani 1 1 d . . . H124 H 0.0712 0.7034 0.0527 0.108 Uiso 1 1 calc R . . C125 C 0.1376(4) 0.5999(6) 0.0185(4) 0.105(3) Uani 1 1 d . . . H125 H 0.1630 0.6458 -0.0072 0.126 Uiso 1 1 calc R . . C126 C 0.1583(4) 0.4970(5) 0.0195(4) 0.093(2) Uani 1 1 d . . . H126 H 0.1969 0.4749 -0.0053 0.111 Uiso 1 1 calc R . . C131 C 0.2023(3) 0.2631(4) -0.0004(3) 0.0576(15) Uani 1 1 d . . . C132 C 0.1737(4) 0.1937(5) -0.0538(3) 0.086(2) Uani 1 1 d . . . H132 H 0.1243 0.1670 -0.0556 0.103 Uiso 1 1 calc R . . C133 C 0.2182(5) 0.1629(6) -0.1051(4) 0.116(3) Uani 1 1 d . . . H133 H 0.1983 0.1166 -0.1413 0.139 Uiso 1 1 calc R . . C134 C 0.2902(5) 0.2006(7) -0.1021(5) 0.119(3) Uani 1 1 d . . . H134 H 0.3203 0.1786 -0.1355 0.143 Uiso 1 1 calc R . . C135 C 0.3194(4) 0.2702(7) -0.0510(5) 0.114(3) Uani 1 1 d . . . H135 H 0.3686 0.2971 -0.0504 0.136 Uiso 1 1 calc R . . C136 C 0.2761(4) 0.3013(5) 0.0001(4) 0.087(2) Uani 1 1 d . . . H136 H 0.2968 0.3485 0.0354 0.104 Uiso 1 1 calc R . . Ag2 Ag -0.02618(2) -0.00218(3) 0.15088(2) 0.06392(15) Uani 1 1 d . . . P2 P -0.03343(9) -0.05345(12) 0.27211(8) 0.0609(4) Uani 1 1 d . . . C211 C -0.1303(3) -0.0420(5) 0.2947(3) 0.0637(16) Uani 1 1 d . . . C212 C -0.1756(4) 0.0388(5) 0.2656(3) 0.092(2) Uani 1 1 d . . . H212 H -0.1562 0.0848 0.2354 0.110 Uiso 1 1 calc R . . C213 C -0.2488(4) 0.0524(6) 0.2805(4) 0.115(3) Uani 1 1 d . . . H213 H -0.2786 0.1076 0.2608 0.138 Uiso 1 1 calc R . . C214 C -0.2771(4) -0.0140(8) 0.3234(4) 0.123(3) Uani 1 1 d . . . H214 H -0.3269 -0.0045 0.3330 0.147 Uiso 1 1 calc R . . C215 C -0.2351(5) -0.0950(7) 0.3531(4) 0.132(3) Uani 1 1 d . . . H215 H -0.2556 -0.1401 0.3832 0.158 Uiso 1 1 calc R . . C216 C -0.1607(4) -0.1101(6) 0.3382(3) 0.099(2) Uani 1 1 d . . . H216 H -0.1317 -0.1661 0.3576 0.119 Uiso 1 1 calc R . . C221 C 0.0266(3) 0.0250(4) 0.3403(3) 0.0628(16) Uani 1 1 d . . . C222 C 0.0049(4) 0.0567(5) 0.4040(3) 0.087(2) Uani 1 1 d . . . H222 H -0.0432 0.0383 0.4145 0.104 Uiso 1 1 calc R . . C223 C 0.0545(5) 0.1155(6) 0.4524(4) 0.104(2) Uani 1 1 d . . . H223 H 0.0386 0.1388 0.4944 0.125 Uiso 1 1 calc R . . C224 C 0.1266(5) 0.1404(6) 0.4398(4) 0.104(2) Uani 1 1 d . . . H224 H 0.1604 0.1775 0.4742 0.125 Uiso 1 1 calc R . . C225 C 0.1488(4) 0.1106(6) 0.3764(5) 0.106(3) Uani 1 1 d . . . H225 H 0.1973 0.1285 0.3667 0.127 Uiso 1 1 calc R . . C226 C 0.0992(4) 0.0543(5) 0.3274(4) 0.093(2) Uani 1 1 d . . . H226 H 0.1145 0.0349 0.2841 0.111 Uiso 1 1 calc R . . C231 C -0.0044(3) -0.1842(5) 0.2984(3) 0.0600(15) Uani 1 1 d . . . C232 C 0.0429(3) -0.2102(5) 0.3620(3) 0.0768(18) Uani 1 1 d . . . H232 H 0.0619 -0.1594 0.3950 0.092 Uiso 1 1 calc R . . C233 C 0.0631(4) -0.3104(6) 0.3781(4) 0.092(2) Uani 1 1 d . . . H233 H 0.0959 -0.3265 0.4214 0.110 Uiso 1 1 calc R . . C234 C 0.0353(4) -0.3849(6) 0.3311(5) 0.099(2) Uani 1 1 d . . . H234 H 0.0497 -0.4520 0.3421 0.118 Uiso 1 1 calc R . . C235 C -0.0130(5) -0.3642(6) 0.2683(5) 0.106(2) Uani 1 1 d . . . H235 H -0.0331 -0.4168 0.2373 0.127 Uiso 1 1 calc R . . C236 C -0.0328(4) -0.2621(6) 0.2499(4) 0.093(2) Uani 1 1 d . . . H236 H -0.0645 -0.2467 0.2059 0.111 Uiso 1 1 calc R . . O1 O -0.01424(18) 0.1032(2) -0.05317(17) 0.0507(9) Uani 1 1 d . . . O2 O -0.10172(17) -0.0060(3) -0.10829(17) 0.0534(9) Uani 1 1 d . . . O3 O -0.3439(3) 0.0553(4) -0.0304(3) 0.132(2) Uani 1 1 d . . . S S -0.09779(7) 0.14014(10) 0.07759(7) 0.0527(4) Uani 1 1 d . . . C1 C -0.0792(3) 0.0583(4) -0.0594(3) 0.0445(13) Uani 1 1 d . . . C2 C -0.1335(3) 0.0838(3) -0.0075(2) 0.0420(13) Uani 1 1 d . . . C3 C -0.2089(3) 0.0644(4) -0.0290(3) 0.0566(15) Uani 1 1 d . . . H3 H -0.2220 0.0355 -0.0750 0.068 Uiso 1 1 calc R . . C4 C -0.2732(3) 0.0820(5) 0.0090(4) 0.0734(18) Uani 1 1 d . . . C5 C -0.2837(4) 0.1159(5) 0.0741(4) 0.086(2) Uani 1 1 d . . . H5 H -0.2454 0.1387 0.1115 0.103 Uiso 1 1 calc R . . C6 C -0.3645(5) 0.1107(7) 0.0755(5) 0.129(3) Uani 1 1 d . . . H6 H -0.3886 0.1280 0.1144 0.155 Uiso 1 1 calc R . . C7 C -0.3978(5) 0.0775(8) 0.0129(6) 0.157(4) Uani 1 1 d . . . H7 H -0.4511 0.0695 -0.0011 0.188 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0550(3) 0.0553(3) 0.0570(3) -0.0018(2) 0.0015(2) -0.0125(2) P1 0.0513(9) 0.0530(10) 0.0533(9) 0.0047(8) -0.0025(7) -0.0073(8) C111 0.054(3) 0.053(4) 0.046(3) 0.002(3) 0.001(3) -0.012(3) C112 0.078(4) 0.060(4) 0.061(4) 0.013(4) -0.006(3) -0.006(4) C113 0.090(5) 0.084(5) 0.078(5) 0.026(4) -0.015(4) 0.000(4) C114 0.069(5) 0.124(7) 0.057(4) 0.031(5) -0.017(3) -0.008(5) C115 0.096(5) 0.104(6) 0.051(4) -0.006(4) -0.016(4) -0.030(5) C116 0.087(4) 0.064(4) 0.059(4) 0.005(4) -0.011(4) -0.014(4) C121 0.059(4) 0.052(4) 0.050(4) 0.003(3) -0.006(3) -0.009(3) C122 0.111(5) 0.053(4) 0.065(4) 0.004(3) 0.011(4) 0.014(4) C123 0.147(7) 0.082(6) 0.065(5) -0.006(4) 0.009(5) 0.017(6) C124 0.102(6) 0.061(5) 0.088(6) -0.010(5) -0.036(5) 0.024(5) C125 0.092(6) 0.074(6) 0.140(8) 0.036(5) -0.005(5) -0.012(5) C126 0.093(5) 0.067(5) 0.119(6) 0.032(5) 0.017(4) 0.008(5) C131 0.058(4) 0.064(4) 0.047(4) 0.007(3) -0.001(3) -0.005(3) C132 0.081(5) 0.118(6) 0.056(4) -0.012(4) 0.007(4) -0.021(5) C133 0.136(7) 0.156(8) 0.059(5) -0.034(5) 0.023(5) -0.010(6) C134 0.090(6) 0.183(9) 0.095(7) -0.001(6) 0.045(6) 0.006(7) C135 0.079(5) 0.173(9) 0.091(6) 0.010(6) 0.022(5) -0.022(6) C136 0.065(4) 0.111(6) 0.086(5) 0.006(4) 0.015(4) -0.012(4) Ag2 0.0753(3) 0.0770(3) 0.0417(2) 0.0037(3) 0.0167(2) 0.0011(3) P2 0.0653(10) 0.0771(11) 0.0424(9) 0.0048(8) 0.0152(8) 0.0078(9) C211 0.058(4) 0.094(5) 0.042(4) -0.001(3) 0.013(3) 0.008(4) C212 0.071(5) 0.124(6) 0.084(5) 0.013(4) 0.025(4) 0.028(5) C213 0.082(6) 0.157(8) 0.109(7) 0.024(6) 0.027(5) 0.041(5) C214 0.068(5) 0.209(11) 0.095(6) 0.010(7) 0.021(5) 0.044(6) C215 0.085(6) 0.203(10) 0.119(7) 0.052(7) 0.051(6) 0.015(6) C216 0.077(5) 0.138(7) 0.087(5) 0.034(5) 0.029(4) 0.019(5) C221 0.065(4) 0.060(4) 0.065(4) 0.008(3) 0.015(3) 0.009(3) C222 0.085(5) 0.126(6) 0.053(4) -0.021(4) 0.021(4) -0.022(5) C223 0.126(7) 0.126(7) 0.062(5) -0.027(5) 0.018(5) -0.017(6) C224 0.100(6) 0.110(6) 0.093(6) -0.020(5) -0.009(5) -0.022(5) C225 0.085(5) 0.113(6) 0.121(7) -0.035(6) 0.018(5) -0.009(5) C226 0.080(5) 0.111(6) 0.089(6) -0.026(5) 0.018(5) 0.002(5) C231 0.060(4) 0.076(4) 0.050(4) 0.010(4) 0.026(3) 0.002(4) C232 0.076(4) 0.077(5) 0.073(5) 0.008(4) 0.000(4) 0.008(4) C233 0.090(5) 0.077(5) 0.102(6) 0.023(5) -0.004(4) 0.015(5) C234 0.106(6) 0.087(6) 0.107(7) 0.011(6) 0.028(6) 0.009(5) C235 0.134(7) 0.085(6) 0.098(7) -0.006(5) 0.020(6) -0.007(6) C236 0.107(6) 0.110(6) 0.061(5) -0.001(5) 0.017(4) -0.001(5) O1 0.045(2) 0.059(2) 0.050(2) -0.0075(19) 0.0144(19) -0.0068(19) O2 0.050(2) 0.063(2) 0.045(2) -0.010(2) 0.0020(18) -0.004(2) O3 0.059(3) 0.219(6) 0.121(4) -0.062(4) 0.026(3) -0.039(4) S 0.0531(9) 0.0592(9) 0.0459(9) -0.0059(7) 0.0086(7) -0.0027(7) C1 0.050(4) 0.050(4) 0.032(3) 0.010(3) 0.005(3) 0.008(3) C2 0.043(3) 0.040(3) 0.041(3) 0.007(3) 0.002(3) -0.005(3) C3 0.054(4) 0.072(4) 0.044(3) -0.010(3) 0.006(3) -0.006(3) C4 0.050(4) 0.096(5) 0.076(5) -0.004(4) 0.017(4) -0.005(4) C5 0.072(5) 0.124(6) 0.068(5) -0.015(4) 0.025(4) 0.003(4) C6 0.079(6) 0.209(10) 0.114(7) -0.029(7) 0.059(6) -0.004(6) C7 0.072(6) 0.244(12) 0.171(10) -0.058(9) 0.067(7) -0.029(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P1 2.3629(14) . ? Ag1 O1 2.414(3) . ? Ag1 S 2.4539(13) . ? Ag1 O2 2.791(3) 3 ? Ag1 Ag2 3.3111(6) . ? Ag1 Ag2 4.6305(6) 3 ? P1 C121 1.804(5) . ? P1 C131 1.814(5) . ? P1 C111 1.824(5) . ? C111 C112 1.374(7) . ? C111 C116 1.390(6) . ? C112 C113 1.362(7) . ? C113 C114 1.365(8) . ? C114 C115 1.360(8) . ? C115 C116 1.382(7) . ? C121 C122 1.365(7) . ? C121 C126 1.365(7) . ? C122 C123 1.395(8) . ? C123 C124 1.349(8) . ? C124 C125 1.327(8) . ? C125 C126 1.399(8) . ? C131 C132 1.377(7) . ? C131 C136 1.386(7) . ? C132 C133 1.398(8) . ? C133 C134 1.348(9) . ? C134 C135 1.354(9) . ? C135 C136 1.380(8) . ? Ag2 P2 2.3856(15) . ? Ag2 O1 2.457(3) 3 ? Ag2 O2 2.509(3) 3 ? Ag2 S 2.5173(14) . ? P2 C221 1.821(6) . ? P2 C211 1.826(5) . ? P2 C231 1.832(6) . ? C211 C216 1.376(7) . ? C211 C212 1.378(7) . ? C212 C213 1.371(7) . ? C213 C214 1.337(9) . ? C214 C215 1.356(9) . ? C215 C216 1.395(8) . ? C221 C222 1.375(7) . ? C221 C226 1.391(7) . ? C222 C223 1.376(8) . ? C223 C224 1.364(8) . ? C224 C225 1.366(8) . ? C225 C226 1.364(8) . ? C231 C232 1.368(7) . ? C231 C236 1.397(8) . ? C232 C233 1.382(7) . ? C233 C234 1.347(8) . ? C234 C235 1.349(8) . ? C235 C236 1.411(8) . ? O1 C1 1.270(5) . ? O1 Ag2 2.457(3) 3 ? O2 C1 1.255(5) . ? O2 Ag2 2.509(3) 3 ? O3 C4 1.371(6) . ? O3 C7 1.379(8) . ? S C2 1.764(5) . ? C1 C2 1.510(6) . ? C2 C3 1.337(6) . ? C3 C4 1.451(7) . ? C4 C5 1.337(7) . ? C5 C6 1.422(8) . ? C6 C7 1.288(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Ag1 O1 118.38(8) . . ? P1 Ag1 S 157.56(5) . . ? O1 Ag1 S 79.01(8) . . ? P1 Ag1 O2 100.18(7) . 3 ? O1 Ag1 O2 86.11(10) . 3 ? S Ag1 O2 94.82(7) . 3 ? P1 Ag1 Ag2 137.66(4) . . ? O1 Ag1 Ag2 89.83(8) . . ? S Ag1 Ag2 49.06(3) . . ? O2 Ag1 Ag2 47.62(6) 3 . ? P1 Ag1 Ag2 104.78(4) . 3 ? O1 Ag1 Ag2 18.25(7) . 3 ? S Ag1 Ag2 94.98(3) . 3 ? O2 Ag1 Ag2 75.88(7) 3 3 ? Ag2 Ag1 Ag2 93.704(13) . 3 ? C121 P1 C131 106.9(3) . . ? C121 P1 C111 104.1(2) . . ? C131 P1 C111 103.2(2) . . ? C121 P1 Ag1 113.72(19) . . ? C131 P1 Ag1 113.0(2) . . ? C111 P1 Ag1 114.88(17) . . ? C112 C111 C116 118.4(5) . . ? C112 C111 P1 118.6(4) . . ? C116 C111 P1 123.0(4) . . ? C113 C112 C111 121.8(6) . . ? C112 C113 C114 119.4(6) . . ? C115 C114 C113 120.4(6) . . ? C114 C115 C116 120.5(6) . . ? C115 C116 C111 119.5(6) . . ? C122 C121 C126 117.7(6) . . ? C122 C121 P1 116.9(5) . . ? C126 C121 P1 125.4(5) . . ? C121 C122 C123 121.9(6) . . ? C124 C123 C122 119.3(7) . . ? C125 C124 C123 119.6(8) . . ? C124 C125 C126 122.0(7) . . ? C121 C126 C125 119.5(7) . . ? C132 C131 C136 117.8(6) . . ? C132 C131 P1 118.3(5) . . ? C136 C131 P1 123.8(5) . . ? C131 C132 C133 120.7(6) . . ? C134 C133 C132 119.7(7) . . ? C133 C134 C135 120.8(8) . . ? C134 C135 C136 120.1(7) . . ? C135 C136 C131 120.8(7) . . ? P2 Ag2 O1 128.47(9) . 3 ? P2 Ag2 O2 120.76(8) . 3 ? O1 Ag2 O2 53.00(10) 3 3 ? P2 Ag2 S 128.36(5) . . ? O1 Ag2 S 100.26(8) 3 . ? O2 Ag2 S 100.63(8) 3 . ? P2 Ag2 Ag1 140.87(4) . . ? O1 Ag2 Ag1 82.84(8) 3 . ? O2 Ag2 Ag1 55.25(7) 3 . ? S Ag2 Ag1 47.42(3) . . ? C221 P2 C211 103.8(3) . . ? C221 P2 C231 104.1(3) . . ? C211 P2 C231 103.9(3) . . ? C221 P2 Ag2 112.5(2) . . ? C211 P2 Ag2 113.7(2) . . ? C231 P2 Ag2 117.36(18) . . ? C216 C211 C212 118.4(5) . . ? C216 C211 P2 123.7(5) . . ? C212 C211 P2 117.9(5) . . ? C213 C212 C211 121.1(7) . . ? C214 C213 C212 119.6(8) . . ? C213 C214 C215 121.6(7) . . ? C214 C215 C216 119.4(8) . . ? C211 C216 C215 119.8(7) . . ? C222 C221 C226 117.7(6) . . ? C222 C221 P2 124.3(5) . . ? C226 C221 P2 118.0(5) . . ? C223 C222 C221 119.9(6) . . ? C224 C223 C222 121.4(7) . . ? C225 C224 C223 119.5(7) . . ? C226 C225 C224 119.5(7) . . ? C225 C226 C221 121.9(6) . . ? C232 C231 C236 118.3(6) . . ? C232 C231 P2 124.3(5) . . ? C236 C231 P2 117.4(5) . . ? C231 C232 C233 121.3(6) . . ? C234 C233 C232 119.9(7) . . ? C233 C234 C235 121.4(8) . . ? C234 C235 C236 119.6(8) . . ? C231 C236 C235 119.5(7) . . ? C1 O1 Ag1 117.5(3) . . ? C1 O1 Ag2 93.0(3) . 3 ? Ag1 O1 Ag2 143.84(14) . 3 ? C1 O2 Ag2 91.0(3) . 3 ? C4 O3 C7 106.3(6) . . ? C2 S Ag1 100.56(16) . . ? C2 S Ag2 104.06(16) . . ? Ag1 S Ag2 83.52(4) . . ? O2 C1 O1 122.8(5) . . ? O2 C1 C2 117.6(5) . . ? O1 C1 C2 119.6(5) . . ? C3 C2 C1 117.7(5) . . ? C3 C2 S 121.8(4) . . ? C1 C2 S 120.4(4) . . ? C2 C3 C4 129.4(5) . . ? C5 C4 O3 108.5(5) . . ? C5 C4 C3 137.7(6) . . ? O3 C4 C3 113.8(6) . . ? C4 C5 C6 107.3(6) . . ? C7 C6 C5 107.2(7) . . ? C6 C7 O3 110.7(8) . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 28.05 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 0.406 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.071 #=== END data_7 _database_code_depnum_ccdc_archive 'CCDC 261753' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H50 Ag O3 P3 S' _chemical_formula_weight 1063.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2174(16) _cell_length_b 20.525(3) _cell_length_c 20.943(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.790(3) _cell_angle_gamma 90.00 _cell_volume 5224.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 879 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 20.99 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 0.563 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.867293 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29034 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0692 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.03 _reflns_number_total 11647 _reflns_number_gt 7680 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+1.2743P] 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 11647 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1029 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Ag Ag 0.474886(19) 0.210747(12) 0.121514(11) 0.04443(8) Uani 1 1 d . . . S S 0.34856(8) 0.22924(4) 0.01447(4) 0.0584(3) Uani 1 1 d . . . O1 O 0.5311(3) 0.25829(19) -0.05738(15) 0.1052(11) Uani 1 1 d . . . H1 H 0.4998 0.2278 -0.0306 0.120 Uiso 1 1 d . . . O2 O 0.5085(3) 0.36356(19) -0.06995(16) 0.1214(13) Uani 1 1 d . . . C1 C 0.4757(4) 0.3126(3) -0.05089(19) 0.0794(13) Uani 1 1 d . . . C2 C 0.3729(3) 0.30625(18) -0.01723(15) 0.0567(9) Uani 1 1 d . . . C3 C 0.3086(4) 0.35900(19) -0.01603(16) 0.0680(11) Uani 1 1 d . . . H3 H 0.3328 0.3958 -0.0364 0.082 Uiso 1 1 calc R . . C4 C 0.2073(4) 0.3662(2) 0.01249(18) 0.0694(11) Uani 1 1 d . . . C5 C 0.1384(4) 0.3268(2) 0.0405(2) 0.0804(12) Uani 1 1 d . . . H5 H 0.1447 0.2818 0.0451 0.096 Uiso 1 1 calc R . . C6 C 0.0545(4) 0.3662(4) 0.0616(2) 0.1058(18) Uani 1 1 d . . . H6 H -0.0043 0.3522 0.0831 0.127 Uiso 1 1 calc R . . C7 C 0.0755(6) 0.4271(3) 0.0451(3) 0.121(2) Uani 1 1 d . . . H7 H 0.0329 0.4631 0.0537 0.145 Uiso 1 1 calc R . . O3 O 0.1685(3) 0.42961(15) 0.01380(15) 0.1006(10) Uani 1 1 d . . . P1 P 0.41315(6) 0.29914(4) 0.19630(4) 0.03821(19) Uani 1 1 d . . . C111 C 0.5025(2) 0.31727(15) 0.26990(13) 0.0390(7) Uani 1 1 d . . . C112 C 0.5593(3) 0.37529(17) 0.27947(16) 0.0554(9) Uani 1 1 d . . . H112 H 0.5488 0.4084 0.2492 0.066 Uiso 1 1 calc R . . C113 C 0.6315(3) 0.3843(2) 0.33400(19) 0.0725(11) Uani 1 1 d . . . H113 H 0.6693 0.4235 0.3401 0.087 Uiso 1 1 calc R . . C114 C 0.6479(3) 0.3358(2) 0.37917(17) 0.0670(11) Uani 1 1 d . . . H114 H 0.6960 0.3424 0.4159 0.080 Uiso 1 1 calc R . . C115 C 0.5935(3) 0.27790(19) 0.37005(16) 0.0590(10) Uani 1 1 d . . . H115 H 0.6050 0.2449 0.4004 0.071 Uiso 1 1 calc R . . C116 C 0.5214(3) 0.26850(16) 0.31585(15) 0.0508(8) Uani 1 1 d . . . H116 H 0.4849 0.2289 0.3099 0.061 Uiso 1 1 calc R . . C121 C 0.2813(3) 0.27843(15) 0.22492(15) 0.0459(8) Uani 1 1 d . . . C122 C 0.2525(3) 0.29375(18) 0.28536(17) 0.0637(10) Uani 1 1 d . . . H122 H 0.3011 0.3172 0.3137 0.076 Uiso 1 1 calc R . . C123 C 0.1522(4) 0.2744(2) 0.3040(2) 0.0931(15) Uani 1 1 d . . . H123 H 0.1343 0.2840 0.3451 0.112 Uiso 1 1 calc R . . C124 C 0.0790(4) 0.2411(3) 0.2621(3) 0.1017(16) Uani 1 1 d . . . H124 H 0.0117 0.2279 0.2748 0.122 Uiso 1 1 calc R . . C125 C 0.1052(3) 0.2273(2) 0.2013(2) 0.0861(13) Uani 1 1 d . . . H125 H 0.0545 0.2061 0.1724 0.103 Uiso 1 1 calc R . . C126 C 0.2067(3) 0.24490(18) 0.18286(17) 0.0588(9) Uani 1 1 d . . . H126 H 0.2249 0.2342 0.1421 0.071 Uiso 1 1 calc R . . C131 C 0.3908(3) 0.37971(14) 0.16089(14) 0.0432(8) Uani 1 1 d . . . C132 C 0.3039(3) 0.41892(16) 0.17412(16) 0.0600(10) Uani 1 1 d . . . H132 H 0.2514 0.4031 0.1994 0.072 Uiso 1 1 calc R . . C133 C 0.2950(4) 0.48103(19) 0.15010(19) 0.0816(13) Uani 1 1 d . . . H133 H 0.2354 0.5068 0.1583 0.098 Uiso 1 1 calc R . . C134 C 0.3731(4) 0.5055(2) 0.1141(2) 0.0848(14) Uani 1 1 d . . . H134 H 0.3681 0.5484 0.0998 0.102 Uiso 1 1 calc R . . C135 C 0.4584(4) 0.4672(2) 0.0990(2) 0.0804(13) Uani 1 1 d . . . H135 H 0.5105 0.4835 0.0738 0.097 Uiso 1 1 calc R . . C136 C 0.4667(3) 0.40256(18) 0.12222(17) 0.0619(10) Uani 1 1 d . . . H136 H 0.5232 0.3756 0.1114 0.074 Uiso 1 1 calc R . . P2 P 0.68166(7) 0.21795(5) 0.11418(4) 0.0499(2) Uani 1 1 d . . . C211 C 0.7553(3) 0.17581(18) 0.18258(16) 0.0541(9) Uani 1 1 d . . . C212 C 0.8309(3) 0.1277(2) 0.1771(2) 0.0796(12) Uani 1 1 d . . . H212 H 0.8507 0.1165 0.1368 0.096 Uiso 1 1 calc R . . C213 C 0.8786(4) 0.0954(2) 0.2313(2) 0.1033(16) Uani 1 1 d . . . H213 H 0.9290 0.0623 0.2266 0.124 Uiso 1 1 calc R . . C214 C 0.8530(4) 0.1112(2) 0.2905(2) 0.0870(13) Uani 1 1 d . . . H214 H 0.8848 0.0889 0.3264 0.104 Uiso 1 1 calc R . . C215 C 0.7804(4) 0.1600(3) 0.2969(2) 0.0920(15) Uani 1 1 d . . . H215 H 0.7646 0.1726 0.3376 0.110 Uiso 1 1 calc R . . C216 C 0.7299(3) 0.1912(2) 0.24365(19) 0.0853(14) Uani 1 1 d . . . H216 H 0.6777 0.2232 0.2489 0.102 Uiso 1 1 calc R . . C221 C 0.7316(3) 0.30248(18) 0.11751(17) 0.0560(9) Uani 1 1 d . . . C222 C 0.7750(4) 0.3337(2) 0.1724(2) 0.0845(13) Uani 1 1 d . . . H222 H 0.7869 0.3107 0.2107 0.101 Uiso 1 1 calc R . . C223 C 0.8013(4) 0.3997(3) 0.1708(3) 0.1124(18) Uani 1 1 d . . . H223 H 0.8305 0.4204 0.2082 0.135 Uiso 1 1 calc R . . C224 C 0.7848(4) 0.4340(3) 0.1154(3) 0.1101(17) Uani 1 1 d . . . H224 H 0.8023 0.4781 0.1150 0.132 Uiso 1 1 calc R . . C225 C 0.7430(4) 0.4043(2) 0.0610(3) 0.0903(14) Uani 1 1 d . . . H225 H 0.7326 0.4276 0.0228 0.108 Uiso 1 1 calc R . . C226 C 0.7157(3) 0.3394(2) 0.0620(2) 0.0701(11) Uani 1 1 d . . . H226 H 0.6856 0.3197 0.0242 0.084 Uiso 1 1 calc R . . C231 C 0.7470(3) 0.18619(18) 0.04611(16) 0.0548(9) Uani 1 1 d . . . C232 C 0.8531(3) 0.2054(2) 0.03572(19) 0.0760(12) Uani 1 1 d . . . H232 H 0.8899 0.2355 0.0633 0.091 Uiso 1 1 calc R . . C233 C 0.9042(4) 0.1808(3) -0.0142(2) 0.0919(14) Uani 1 1 d . . . H233 H 0.9744 0.1949 -0.0210 0.110 Uiso 1 1 calc R . . C234 C 0.8525(5) 0.1362(3) -0.0533(2) 0.0932(15) Uani 1 1 d . . . H234 H 0.8886 0.1189 -0.0864 0.112 Uiso 1 1 calc R . . C235 C 0.7491(5) 0.1158(2) -0.0457(2) 0.0988(15) Uani 1 1 d . . . H235 H 0.7144 0.0849 -0.0733 0.119 Uiso 1 1 calc R . . C236 C 0.6946(3) 0.1423(2) 0.00516(19) 0.0775(12) Uani 1 1 d . . . H236 H 0.6231 0.1295 0.0105 0.093 Uiso 1 1 calc R . . P3 P 0.40797(7) 0.10155(4) 0.16852(4) 0.0469(2) Uani 1 1 d . . . C311 C 0.2677(3) 0.07498(15) 0.14151(15) 0.0454(8) Uani 1 1 d . . . C312 C 0.2068(3) 0.03364(18) 0.17570(18) 0.0682(11) Uani 1 1 d . . . H312 H 0.2351 0.0197 0.2163 0.082 Uiso 1 1 calc R . . C313 C 0.1046(4) 0.0127(2) 0.1506(2) 0.0878(14) Uani 1 1 d . . . H313 H 0.0644 -0.0152 0.1743 0.105 Uiso 1 1 calc R . . C314 C 0.0619(3) 0.0322(2) 0.0915(3) 0.0894(15) Uani 1 1 d . . . H314 H -0.0077 0.0183 0.0749 0.107 Uiso 1 1 calc R . . C315 C 0.1205(4) 0.0720(2) 0.0570(2) 0.0931(15) Uani 1 1 d . . . H315 H 0.0913 0.0851 0.0163 0.112 Uiso 1 1 calc R . . C316 C 0.2235(3) 0.09368(18) 0.08108(18) 0.0675(11) Uani 1 1 d . . . H316 H 0.2632 0.1210 0.0565 0.081 Uiso 1 1 calc R . . C321 C 0.4130(3) 0.10265(16) 0.25601(17) 0.0596(10) Uani 1 1 d . . . C322 C 0.3269(4) 0.12694(17) 0.28684(16) 0.0651(11) Uani 1 1 d . . . H322 H 0.2615 0.1383 0.2627 0.078 Uiso 1 1 calc R . . C323 C 0.3357(5) 0.1348(2) 0.3531(2) 0.0886(15) Uani 1 1 d . . . H323 H 0.2767 0.1508 0.3732 0.106 Uiso 1 1 calc R . . C324 C 0.4326(6) 0.1187(2) 0.3884(2) 0.113(2) Uani 1 1 d . . . H324 H 0.4393 0.1244 0.4327 0.135 Uiso 1 1 calc R . . C325 C 0.5185(5) 0.0948(2) 0.3597(2) 0.110(2) Uani 1 1 d . . . H325 H 0.5834 0.0836 0.3844 0.132 Uiso 1 1 calc R . . C326 C 0.5101(4) 0.08689(18) 0.2933(2) 0.0859(14) Uani 1 1 d . . . H326 H 0.5698 0.0710 0.2738 0.103 Uiso 1 1 calc R . . C331 C 0.4827(3) 0.02776(18) 0.1508(2) 0.0639(10) Uani 1 1 d . . . C332 C 0.5421(5) 0.0284(3) 0.1013(3) 0.144(2) Uani 1 1 d . . . H332 H 0.5511 0.0672 0.0795 0.172 Uiso 1 1 calc R . . C333 C 0.5267(6) -0.0856(3) 0.1618(4) 0.148(3) Uani 1 1 d . . . H333 H 0.5233 -0.1243 0.1846 0.178 Uiso 1 1 calc R . . C334 C 0.5803(6) -0.0840(4) 0.1091(5) 0.167(5) Uani 1 1 d . . . H334 H 0.6089 -0.1219 0.0930 0.201 Uiso 1 1 calc R . . C335 C 0.5915(7) -0.0285(4) 0.0814(5) 0.203(4) Uani 1 1 d . . . H335 H 0.6339 -0.0263 0.0469 0.243 Uiso 1 1 calc R . . C336 C 0.4762(4) -0.0302(2) 0.1829(3) 0.1090(17) Uani 1 1 d . . . H336 H 0.4377 -0.0323 0.2190 0.131 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.04453(14) 0.04743(14) 0.04151(14) -0.00382(12) 0.00516(10) 0.00058(12) S 0.0734(6) 0.0542(6) 0.0443(5) 0.0057(4) -0.0106(5) -0.0120(4) O1 0.102(2) 0.136(3) 0.083(2) 0.015(2) 0.0369(19) 0.011(2) O2 0.112(3) 0.137(3) 0.116(3) 0.061(2) 0.013(2) -0.040(2) C1 0.082(3) 0.103(4) 0.051(2) 0.016(2) -0.003(2) -0.018(3) C2 0.073(3) 0.060(2) 0.0345(18) 0.0090(16) -0.0082(17) -0.0108(19) C3 0.096(3) 0.058(3) 0.045(2) 0.0111(18) -0.012(2) -0.016(2) C4 0.087(3) 0.065(3) 0.050(2) -0.005(2) -0.024(2) 0.010(2) C5 0.076(3) 0.094(3) 0.067(3) 0.000(3) -0.014(2) 0.005(3) C6 0.081(4) 0.153(5) 0.078(3) -0.018(4) -0.016(3) 0.028(4) C7 0.126(5) 0.135(6) 0.094(4) -0.037(4) -0.025(4) 0.055(5) O3 0.132(3) 0.079(2) 0.084(2) -0.0139(17) -0.023(2) 0.023(2) P1 0.0416(5) 0.0374(5) 0.0360(4) -0.0032(3) 0.0056(3) 0.0013(3) C111 0.0395(18) 0.0407(17) 0.0373(17) -0.0032(14) 0.0066(14) 0.0049(14) C112 0.057(2) 0.053(2) 0.054(2) 0.0026(17) -0.0097(18) -0.0057(17) C113 0.069(3) 0.070(3) 0.074(3) -0.007(2) -0.013(2) -0.015(2) C114 0.055(2) 0.094(3) 0.048(2) -0.008(2) -0.0097(18) 0.004(2) C115 0.063(2) 0.074(3) 0.041(2) 0.0055(17) 0.0072(17) 0.016(2) C116 0.061(2) 0.050(2) 0.0412(19) -0.0009(15) 0.0052(17) 0.0004(16) C121 0.0447(19) 0.045(2) 0.0482(19) -0.0021(15) 0.0077(15) 0.0000(15) C122 0.057(2) 0.078(3) 0.059(2) -0.014(2) 0.0189(19) -0.001(2) C123 0.077(3) 0.126(4) 0.084(3) -0.012(3) 0.046(3) -0.003(3) C124 0.056(3) 0.133(5) 0.122(4) -0.002(4) 0.042(3) -0.018(3) C125 0.048(3) 0.108(4) 0.101(4) -0.004(3) 0.003(2) -0.012(2) C126 0.048(2) 0.072(3) 0.056(2) 0.0004(19) 0.0028(18) -0.0050(18) C131 0.052(2) 0.0386(18) 0.0379(17) -0.0045(14) -0.0010(15) 0.0025(15) C132 0.082(3) 0.045(2) 0.053(2) -0.0019(17) 0.0072(19) 0.0152(19) C133 0.125(4) 0.048(2) 0.072(3) 0.000(2) 0.007(3) 0.023(2) C134 0.123(4) 0.043(2) 0.083(3) 0.009(2) -0.015(3) 0.002(3) C135 0.090(3) 0.074(3) 0.076(3) 0.027(2) 0.000(2) -0.020(3) C136 0.060(2) 0.060(2) 0.065(2) 0.013(2) 0.0046(19) -0.0023(19) P2 0.0390(5) 0.0660(6) 0.0455(5) -0.0057(4) 0.0084(4) 0.0013(4) C211 0.0382(19) 0.076(3) 0.049(2) -0.0029(18) 0.0082(16) 0.0040(17) C212 0.086(3) 0.091(3) 0.063(3) -0.002(2) 0.016(2) 0.026(3) C213 0.109(4) 0.115(4) 0.085(4) 0.009(3) 0.007(3) 0.053(3) C214 0.079(3) 0.115(4) 0.065(3) 0.020(3) -0.003(2) 0.014(3) C215 0.086(3) 0.139(4) 0.051(3) 0.008(3) 0.007(2) 0.027(3) C216 0.067(3) 0.130(4) 0.060(3) 0.004(3) 0.012(2) 0.038(3) C221 0.0404(19) 0.074(3) 0.055(2) -0.0105(19) 0.0110(16) -0.0053(17) C222 0.093(3) 0.087(3) 0.073(3) -0.017(2) 0.002(2) -0.015(3) C223 0.117(4) 0.109(5) 0.106(4) -0.038(4) -0.010(4) -0.031(4) C224 0.101(4) 0.095(4) 0.135(5) -0.021(4) 0.014(4) -0.030(3) C225 0.076(3) 0.085(3) 0.112(4) 0.015(3) 0.021(3) -0.012(3) C226 0.062(3) 0.076(3) 0.072(3) 0.000(2) 0.007(2) -0.014(2) C231 0.051(2) 0.070(2) 0.044(2) -0.0039(18) 0.0090(17) 0.0081(18) C232 0.067(3) 0.095(3) 0.070(3) -0.007(2) 0.026(2) 0.005(2) C233 0.088(3) 0.110(4) 0.085(3) 0.007(3) 0.045(3) 0.018(3) C234 0.118(4) 0.106(4) 0.059(3) 0.007(3) 0.026(3) 0.040(3) C235 0.128(5) 0.100(4) 0.066(3) -0.023(3) 0.000(3) 0.014(3) C236 0.077(3) 0.089(3) 0.066(3) -0.016(2) 0.010(2) 0.001(2) P3 0.0522(5) 0.0387(5) 0.0484(5) 0.0012(4) -0.0022(4) -0.0033(4) C311 0.050(2) 0.0400(18) 0.0463(19) -0.0037(15) 0.0044(16) -0.0021(15) C312 0.079(3) 0.069(3) 0.058(2) -0.0066(19) 0.013(2) -0.024(2) C313 0.081(3) 0.091(3) 0.097(4) -0.025(3) 0.036(3) -0.040(3) C314 0.049(3) 0.086(3) 0.130(4) -0.034(3) -0.007(3) -0.012(2) C315 0.086(3) 0.079(3) 0.104(4) 0.004(3) -0.040(3) -0.012(3) C316 0.073(3) 0.060(2) 0.066(3) 0.0089(19) -0.013(2) -0.017(2) C321 0.087(3) 0.0368(19) 0.051(2) 0.0056(16) -0.009(2) -0.0108(19) C322 0.106(3) 0.044(2) 0.044(2) 0.0017(16) 0.002(2) -0.026(2) C323 0.152(5) 0.061(3) 0.055(3) 0.002(2) 0.021(3) -0.037(3) C324 0.218(7) 0.058(3) 0.054(3) 0.008(2) -0.024(4) -0.030(4) C325 0.173(6) 0.068(3) 0.075(4) 0.007(3) -0.059(4) -0.001(3) C326 0.117(4) 0.055(3) 0.076(3) 0.000(2) -0.037(3) 0.007(2) C331 0.054(2) 0.050(2) 0.084(3) -0.010(2) -0.011(2) 0.0025(18) C332 0.167(6) 0.096(4) 0.183(6) 0.000(4) 0.092(5) 0.038(4) C333 0.126(6) 0.048(3) 0.257(10) -0.028(5) -0.049(6) 0.018(3) C334 0.088(5) 0.115(6) 0.288(12) -0.111(8) -0.038(6) 0.039(5) C335 0.217(9) 0.144(7) 0.267(10) -0.052(7) 0.120(8) 0.056(7) C336 0.115(4) 0.057(3) 0.152(5) -0.009(3) -0.004(4) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag P2 2.5505(9) . ? Ag P1 2.5597(8) . ? Ag P3 2.6120(9) . ? Ag S 2.6179(9) . ? Ag O1 3.997(3) . ? Ag O2 5.140(3) . ? S C2 1.752(4) . ? O1 C1 1.318(5) . ? O2 C1 1.203(5) . ? C1 C2 1.506(6) . ? C2 C3 1.339(5) . ? C3 C4 1.435(6) . ? C4 C5 1.345(6) . ? C4 O3 1.387(5) . ? C5 C6 1.412(6) . ? C6 C7 1.330(7) . ? C7 O3 1.369(7) . ? P1 C131 1.822(3) . ? P1 C121 1.825(3) . ? P1 C111 1.835(3) . ? C111 C112 1.382(4) . ? C111 C116 1.392(4) . ? C112 C113 1.383(5) . ? C113 C114 1.374(5) . ? C114 C115 1.366(5) . ? C115 C116 1.378(4) . ? C121 C122 1.383(4) . ? C121 C126 1.385(4) . ? C122 C123 1.382(5) . ? C123 C124 1.371(6) . ? C124 C125 1.373(6) . ? C125 C126 1.383(5) . ? C131 C136 1.373(4) . ? C131 C132 1.382(4) . ? C132 C133 1.371(5) . ? C133 C134 1.371(6) . ? C134 C135 1.368(6) . ? C135 C136 1.413(5) . ? P2 C231 1.823(3) . ? P2 C211 1.830(3) . ? P2 C221 1.838(4) . ? C211 C212 1.364(5) . ? C211 C216 1.383(5) . ? C212 C213 1.391(5) . ? C213 C214 1.349(6) . ? C214 C215 1.353(6) . ? C215 C216 1.376(5) . ? C221 C222 1.374(5) . ? C221 C226 1.385(5) . ? C222 C223 1.393(6) . ? C223 C224 1.356(7) . ? C224 C225 1.347(6) . ? C225 C226 1.373(5) . ? C231 C236 1.359(5) . ? C231 C232 1.393(5) . ? C232 C233 1.366(5) . ? C233 C234 1.343(6) . ? C234 C235 1.356(6) . ? C235 C236 1.419(6) . ? P3 C331 1.826(4) . ? P3 C321 1.827(4) . ? P3 C311 1.833(3) . ? C311 C312 1.376(4) . ? C311 C316 1.379(4) . ? C312 C313 1.374(5) . ? C313 C314 1.354(6) . ? C314 C315 1.344(6) . ? C315 C316 1.382(5) . ? C321 C322 1.382(5) . ? C321 C326 1.391(5) . ? C322 C323 1.390(5) . ? C323 C324 1.370(7) . ? C324 C325 1.354(7) . ? C325 C326 1.394(6) . ? C331 C332 1.325(6) . ? C331 C336 1.372(6) . ? C332 C335 1.396(8) . ? C333 C334 1.340(10) . ? C333 C336 1.387(7) . ? C334 C335 1.293(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 P2 Ag P1 110.52(3) . . ? P2 Ag P3 114.96(3) . . ? P1 Ag P3 104.76(3) . . ? P2 Ag S 116.23(3) . . ? P1 Ag S 103.68(3) . . ? P3 Ag S 105.50(3) . . ? P2 Ag O1 70.41(5) . . ? P1 Ag O1 119.31(6) . . ? P3 Ag O1 130.73(6) . . ? S Ag O1 45.91(5) . . ? P2 Ag O2 76.12(4) . . ? P1 Ag O2 95.54(5) . . ? P3 Ag O2 150.49(5) . . ? S Ag O2 47.93(4) . . ? O1 Ag O2 23.80(7) . . ? C2 S Ag 110.33(11) . . ? C1 O1 Ag 88.3(2) . . ? C1 O2 Ag 32.3(2) . . ? O2 C1 O1 120.6(5) . . ? O2 C1 C2 123.5(5) . . ? O1 C1 C2 115.9(4) . . ? C3 C2 C1 117.2(4) . . ? C3 C2 S 126.9(3) . . ? C1 C2 S 115.9(3) . . ? C2 C3 C4 128.5(4) . . ? C5 C4 O3 109.0(4) . . ? C5 C4 C3 136.4(4) . . ? O3 C4 C3 114.5(4) . . ? C4 C5 C6 107.4(5) . . ? C7 C6 C5 107.0(6) . . ? C6 C7 O3 110.5(5) . . ? C7 O3 C4 106.1(4) . . ? C131 P1 C121 104.12(15) . . ? C131 P1 C111 102.12(14) . . ? C121 P1 C111 103.98(14) . . ? C131 P1 Ag 115.82(10) . . ? C121 P1 Ag 111.12(10) . . ? C111 P1 Ag 118.08(10) . . ? C112 C111 C116 118.3(3) . . ? C112 C111 P1 122.9(2) . . ? C116 C111 P1 118.6(2) . . ? C111 C112 C113 120.2(3) . . ? C114 C113 C112 120.6(4) . . ? C115 C114 C113 119.9(3) . . ? C114 C115 C116 119.9(3) . . ? C115 C116 C111 121.1(3) . . ? C122 C121 C126 118.9(3) . . ? C122 C121 P1 124.2(3) . . ? C126 C121 P1 116.9(2) . . ? C123 C122 C121 120.5(4) . . ? C124 C123 C122 120.2(4) . . ? C123 C124 C125 119.9(4) . . ? C124 C125 C126 120.3(4) . . ? C125 C126 C121 120.2(4) . . ? C136 C131 C132 119.8(3) . . ? C136 C131 P1 117.9(2) . . ? C132 C131 P1 122.2(3) . . ? C133 C132 C131 120.2(4) . . ? C132 C133 C134 120.6(4) . . ? C135 C134 C133 120.3(4) . . ? C134 C135 C136 119.4(4) . . ? C131 C136 C135 119.6(4) . . ? C231 P2 C211 102.92(15) . . ? C231 P2 C221 101.38(16) . . ? C211 P2 C221 106.34(17) . . ? C231 P2 Ag 122.74(12) . . ? C211 P2 Ag 109.71(11) . . ? C221 P2 Ag 112.29(11) . . ? C212 C211 C216 117.4(4) . . ? C212 C211 P2 124.0(3) . . ? C216 C211 P2 118.5(3) . . ? C211 C212 C213 120.4(4) . . ? C214 C213 C212 121.3(4) . . ? C213 C214 C215 118.9(4) . . ? C214 C215 C216 120.6(4) . . ? C215 C216 C211 121.3(4) . . ? C222 C221 C226 117.2(4) . . ? C222 C221 P2 124.8(3) . . ? C226 C221 P2 117.8(3) . . ? C221 C222 C223 120.3(5) . . ? C224 C223 C222 120.7(5) . . ? C225 C224 C223 119.9(5) . . ? C224 C225 C226 119.9(5) . . ? C225 C226 C221 121.9(4) . . ? C236 C231 C232 118.4(3) . . ? C236 C231 P2 121.0(3) . . ? C232 C231 P2 120.6(3) . . ? C233 C232 C231 121.3(4) . . ? C234 C233 C232 119.7(5) . . ? C233 C234 C235 121.8(5) . . ? C234 C235 C236 118.8(5) . . ? C231 C236 C235 120.1(4) . . ? C331 P3 C321 104.31(18) . . ? C331 P3 C311 99.30(15) . . ? C321 P3 C311 104.41(16) . . ? C331 P3 Ag 116.95(14) . . ? C321 P3 Ag 112.78(11) . . ? C311 P3 Ag 117.23(11) . . ? C312 C311 C316 117.9(3) . . ? C312 C311 P3 124.1(3) . . ? C316 C311 P3 117.9(3) . . ? C313 C312 C311 120.8(4) . . ? C314 C313 C312 120.6(4) . . ? C315 C314 C313 119.6(4) . . ? C314 C315 C316 120.9(4) . . ? C311 C316 C315 120.2(4) . . ? C322 C321 C326 117.9(4) . . ? C322 C321 P3 121.5(3) . . ? C326 C321 P3 120.0(3) . . ? C321 C322 C323 121.5(4) . . ? C324 C323 C322 119.1(5) . . ? C325 C324 C323 120.9(5) . . ? C324 C325 C326 120.2(5) . . ? C321 C326 C325 120.4(5) . . ? C332 C331 C336 117.1(4) . . ? C332 C331 P3 118.4(4) . . ? C336 C331 P3 124.3(4) . . ? C331 C332 C335 120.9(6) . . ? C334 C333 C336 120.8(8) . . ? C335 C334 C333 118.4(8) . . ? C334 C335 C332 122.2(8) . . ? C331 C336 C333 120.3(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 S 0.946(3) 2.1590(11) 2.876(3) 131.7(2) . _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.417 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.056