Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'ProfD Xian-He Bu' _publ_contact_author_address ; Department of Chemistry Nankai University Tianjin 300071 CHINA ; _publ_contact_author_email BUXH@NANKAI.EDU.CN _publ_section_title ; Novel Dithioether-Silver(I) Coordination Architectures: Structural Diversities by Varying the Spacers and Terminal Groups of Ligands ; loop_ _publ_author_name 'Xian-He Bu' 'Wen-Ping Du' 'Jiao Jiao' 'Jian-Rong Li' 'Xiu-Hua Xu' ; Ruo-Hua Zhang ; data_030312a _database_code_depnum_ccdc_archive 'CCDC 231504' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H36 Ag2 Cl2 O8 S6' _chemical_formula_weight 823.44 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'P -3c1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' _cell_length_a 10.881(3) _cell_length_b 10.881(3) _cell_length_c 15.660(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1606(1) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 606 _cell_measurement_theta_min 3.75 _cell_measurement_theta_max 22.64 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 1.809 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.5783 _exptl_absorpt_correction_T_max 0.6707 _exptl_absorpt_process_details SADABS _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 'Bruker CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4145 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 25.02 _reflns_number_total 934 _reflns_number_gt 665 _reflns_threshold_expression I>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^)+(0.0501P)^2^+0.8335P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 934 _refine_ls_number_parameters 61 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.096 _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 0.3333 0.6667 0.19990(5) 0.0566(3) Uani 1 3 d S . . S1 S 0.25645(13) 0.84633(13) 0.22364(7) 0.0446(3) Uani 1 1 d . . . C1 C 0.0804(8) 0.7889(10) 0.0904(4) 0.120(3) Uani 1 1 d . . . H1A H 0.0741 0.6977 0.0895 0.180 Uiso 1 1 calc R . . H1B H 0.0648 0.8126 0.0338 0.180 Uiso 1 1 calc R . . H1C H 0.0097 0.7861 0.1283 0.180 Uiso 1 1 calc R . . C2 C 0.2217(6) 0.8964(6) 0.1200(3) 0.0628(14) Uani 1 1 d . . . H2A H 0.2268 0.9878 0.1240 0.075 Uiso 1 1 calc R . . H2B H 0.2929 0.9048 0.0795 0.075 Uiso 1 1 calc R . . C3 C 0.4242(6) 1.0000 0.2500 0.0448(16) Uani 1 2 d S . . H3A H 0.4882 1.0228 0.2019 0.054 Uiso 0.50 1 calc PR . . H3B H 0.4654 0.9772 0.2981 0.054 Uiso 0.50 1 calc PR . . Cl1 Cl 0.3333 0.6667 -0.05394(15) 0.0683(7) Uani 1 3 d SD . . O1 O 0.3333 0.6667 0.0346(4) 0.116(3) Uani 1 3 d SDU . . O2 O 0.385(2) 0.5748(18) -0.0784(11) 0.165(5) Uani 0.50 1 d PDU . . O2' O 0.4575(13) 0.681(2) -0.0921(10) 0.165(5) Uani 0.50 1 d PDU . . 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 0.0464(3) 0.0464(3) 0.0768(6) 0.000 0.000 0.02321(16) S1 0.0448(7) 0.0431(7) 0.0463(7) -0.0006(5) -0.0019(5) 0.0223(5) C1 0.083(5) 0.156(8) 0.086(5) -0.003(5) -0.037(4) 0.034(5) C2 0.080(4) 0.063(3) 0.048(3) 0.001(3) -0.014(3) 0.038(3) C3 0.042(3) 0.047(4) 0.047(4) -0.005(3) -0.0027(15) 0.0237(19) Cl1 0.0832(11) 0.0832(11) 0.0387(14) 0.000 0.000 0.0416(6) O1 0.147(4) 0.147(4) 0.055(5) 0.000 0.000 0.073(2) O2 0.182(9) 0.169(9) 0.174(7) -0.030(7) 0.037(7) 0.111(7) O2' 0.153(8) 0.189(9) 0.160(7) -0.017(7) 0.050(6) 0.090(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 S1 2.509(1) . ? Ag1 S1 2.509(1) 2_665 ? Ag1 S1 2.509(1) 3_565 ? Ag1 O1 2.589(7) . ? S1 C3 1.802(4) . ? S1 C2 1.811(5) . ? C1 C2 1.466(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 S1 1.802(4) 5_675 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? Cl1 O1 1.387(7) . ? Cl1 O2' 1.413(9) 2_665 ? Cl1 O2' 1.413(9) 3_565 ? Cl1 O2' 1.413(9) . ? Cl1 O2 1.421(9) 3_565 ? Cl1 O2 1.421(9) 2_665 ? Cl1 O2 1.421(9) . ? O2 O2' 1.05(2) . ? O2 O2' 1.62(2) 3_565 ? O2' O2 1.62(2) 2_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ag1 S1 117.84(2) . 2_665 ? S1 Ag1 S1 117.84(2) . 3_565 ? S1 Ag1 S1 117.84(2) 2_665 3_565 ? S1 Ag1 O1 98.52(3) . . ? S1 Ag1 O1 98.52(3) 2_665 . ? S1 Ag1 O1 98.52(3) 3_565 . ? C3 S1 C2 101.1(2) . . ? C3 S1 Ag1 100.3(2) . . ? C2 S1 Ag1 107.6(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 S1 109.7(5) . . ? C1 C2 H2A 109.7 . . ? S1 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? S1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? S1 C3 S1 113.4(3) . 5_675 ? S1 C3 H3A 108.9 . . ? S1 C3 H3A 108.9 5_675 . ? S1 C3 H3B 108.9 . . ? S1 C3 H3B 108.9 5_675 . ? H3A C3 H3B 107.7 . . ? O1 Cl1 O2' 115.0(7) . 2_665 ? O1 Cl1 O2' 115.0(7) . 3_565 ? O2' Cl1 O2' 103.4(9) 2_665 3_565 ? O1 Cl1 O2' 115.0(7) . . ? O2' Cl1 O2' 103.4(9) 2_665 . ? O2' Cl1 O2' 103.4(9) 3_565 . ? O1 Cl1 O2 105.6(7) . 3_565 ? O2' Cl1 O2 69.9(7) 2_665 3_565 ? O2' Cl1 O2 43.2(7) 3_565 3_565 ? O2' Cl1 O2 136.9(9) . 3_565 ? O1 Cl1 O2 105.6(7) . 2_665 ? O2' Cl1 O2 43.2(7) 2_665 2_665 ? O2' Cl1 O2 136.9(9) 3_565 2_665 ? O2' Cl1 O2 69.9(7) . 2_665 ? O2 Cl1 O2 113.0(6) 3_565 2_665 ? O1 Cl1 O2 105.6(7) . . ? O2' Cl1 O2 136.9(9) 2_665 . ? O2' Cl1 O2 69.9(7) 3_565 . ? O2' Cl1 O2 43.2(7) . . ? O2 Cl1 O2 113.0(6) 3_565 . ? O2 Cl1 O2 113.0(6) 2_665 . ? Cl1 O1 Ag1 180.0 . . ? O2' O2 Cl1 68.0(8) . . ? O2' O2 O2' 111(2) . 3_565 ? Cl1 O2 O2' 54.8(5) . 3_565 ? O2 O2' Cl1 68.8(8) . . ? O2 O2' O2 124(1) . 2_665 ? Cl1 O2' O2 55.3(5) . 2_665 ? 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 S1 Ag1 S1 C3 153.59(3) 2_665 . . . ? S1 Ag1 S1 C3 2.38(9) 3_565 . . . ? O1 Ag1 S1 C3 -102.01(4) . . . . ? S1 Ag1 S1 C2 -101.1(2) 2_665 . . . ? S1 Ag1 S1 C2 107.7(2) 3_565 . . . ? O1 Ag1 S1 C2 3.3(2) . . . . ? C3 S1 C2 C1 -174.6(5) . . . . ? Ag1 S1 C2 C1 80.7(5) . . . . ? C2 S1 C3 S1 72.0(2) . . . 5_675 ? Ag1 S1 C3 S1 -177.53(6) . . . 5_675 ? O2' Cl1 O1 Ag1 -36(100) 2_665 . . . ? O2' Cl1 O1 Ag1 -156(100) 3_565 . . . ? O2' Cl1 O1 Ag1 84(100) . . . . ? O2 Cl1 O1 Ag1 -111(100) 3_565 . . . ? O2 Cl1 O1 Ag1 9(100) 2_665 . . . ? O2 Cl1 O1 Ag1 129(100) . . . . ? S1 Ag1 O1 Cl1 47(100) . . . . ? S1 Ag1 O1 Cl1 167(100) 2_665 . . . ? S1 Ag1 O1 Cl1 -73(100) 3_565 . . . ? O1 Cl1 O2 O2' -110.1(14) . . . . ? O2' Cl1 O2 O2' 50.1(17) 2_665 . . . ? O2' Cl1 O2 O2' 138(2) 3_565 . . . ? O2 Cl1 O2 O2' 134.9(10) 3_565 . . . ? O2 Cl1 O2 O2' 5(2) 2_665 . . . ? O1 Cl1 O2 O2' 111.4(9) . . . 3_565 ? O2' Cl1 O2 O2' -88.3(14) 2_665 . . 3_565 ? O2' Cl1 O2 O2' -138(2) . . . 3_565 ? O2 Cl1 O2 O2' -3.6(16) 3_565 . . 3_565 ? O2 Cl1 O2 O2' -133.6(9) 2_665 . . 3_565 ? O2' O2 O2' Cl1 35.4(15) 3_565 . . . ? Cl1 O2 O2' O2 -5(2) . . . 2_665 ? O2' O2 O2' O2 31(4) 3_565 . . 2_665 ? O1 Cl1 O2' O2 86.4(15) . . . . ? O2' Cl1 O2' O2 -147.4(11) 2_665 . . . ? O2' Cl1 O2' O2 -40(2) 3_565 . . . ? O2 Cl1 O2' O2 -72.5(15) 3_565 . . . ? O2 Cl1 O2' O2 -175(2) 2_665 . . . ? O1 Cl1 O2' O2 -98.4(9) . . . 2_665 ? O2' Cl1 O2' O2 27.8(14) 2_665 . . 2_665 ? O2' Cl1 O2' O2 135.4(8) 3_565 . . 2_665 ? O2 Cl1 O2' O2 102.7(13) 3_565 . . 2_665 ? O2 Cl1 O2' O2 175(2) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.388 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.086 data_021209d _database_code_depnum_ccdc_archive 'CCDC 231505' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H56 Ag4 Cl4 O16 S8' _chemical_formula_weight 1430.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.628(4) _cell_length_b 12.126(4) _cell_length_c 16.977(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.443(6) _cell_angle_gamma 90.00 _cell_volume 2452(1) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 971 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 26.12 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.938 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 2.190 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6216 _exptl_absorpt_correction_T_max 0.6685 _exptl_absorpt_process_details SADABS _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 'Bruker CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11377 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.0994 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 26.43 _reflns_number_total 4874 _reflns_number_gt 2586 _reflns_threshold_expression I>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^)+(0.0230P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00100(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4874 _refine_ls_number_parameters 295 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.1200 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.963 _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 0.67773(4) 0.58894(4) 0.53210(3) 0.05354(18) Uani 1 1 d . . . Ag2 Ag 0.36903(4) 0.69829(4) 0.32059(3) 0.05892(19) Uani 1 1 d . . . S1 S 0.58285(12) 0.70881(12) 0.41212(9) 0.0443(4) Uani 1 1 d . . . S2 S 0.36596(14) 0.89067(13) 0.37967(10) 0.0556(5) Uani 1 1 d . . . S3 S 0.29069(13) 0.57662(13) 0.19411(9) 0.0492(4) Uani 1 1 d . . . S4 S 0.24361(12) 0.57305(12) 0.38250(8) 0.0382(4) Uani 1 1 d . . . C1 C 0.7883(6) 0.7153(7) 0.3856(5) 0.103(3) Uani 1 1 d . . . H1A H 0.8110 0.7783 0.4216 0.154 Uiso 1 1 calc R . . H1B H 0.8253 0.7166 0.3445 0.154 Uiso 1 1 calc R . . H1C H 0.8086 0.6491 0.4182 0.154 Uiso 1 1 calc R . . C2 C 0.6667(6) 0.7180(6) 0.3439(4) 0.078(2) Uani 1 1 d . . . H2A H 0.6460 0.6575 0.3043 0.093 Uiso 1 1 calc R . . H2B H 0.6475 0.7860 0.3122 0.093 Uiso 1 1 calc R . . C3 C 0.5885(5) 0.8474(5) 0.4552(4) 0.0586(18) Uani 1 1 d . . . H3A H 0.5709 0.8431 0.5065 0.070 Uiso 1 1 calc R . . H3B H 0.6646 0.8751 0.4692 0.070 Uiso 1 1 calc R . . C4 C 0.5107(5) 0.9272(5) 0.3982(4) 0.0607(18) Uani 1 1 d . . . H4A H 0.5247 0.9290 0.3454 0.073 Uiso 1 1 calc R . . H4B H 0.5248 1.0004 0.4225 0.073 Uiso 1 1 calc R . . C5 C 0.2959(6) 0.9781(5) 0.2930(4) 0.073(2) Uani 1 1 d . . . H5A H 0.2980 1.0539 0.3119 0.087 Uiso 1 1 calc R . . H5B H 0.3338 0.9747 0.2519 0.087 Uiso 1 1 calc R . . C6 C 0.1749(7) 0.9410(7) 0.2539(5) 0.120(3) Uani 1 1 d . . . H6A H 0.1732 0.8682 0.2313 0.180 Uiso 1 1 calc R . . H6B H 0.1359 0.9911 0.2100 0.180 Uiso 1 1 calc R . . H6C H 0.1391 0.9402 0.2957 0.180 Uiso 1 1 calc R . . C7 C 0.1371(7) 0.5892(6) 0.0344(4) 0.094(3) Uani 1 1 d . . . H7A H 0.1971 0.5662 0.0152 0.142 Uiso 1 1 calc R . . H7B H 0.0861 0.6354 -0.0070 0.142 Uiso 1 1 calc R . . H7C H 0.0977 0.5255 0.0438 0.142 Uiso 1 1 calc R . . C8 C 0.1846(5) 0.6526(5) 0.1147(3) 0.0571(18) Uani 1 1 d . . . H8A H 0.1242 0.6714 0.1356 0.069 Uiso 1 1 calc R . . H8B H 0.2170 0.7209 0.1035 0.069 Uiso 1 1 calc R . . C9 C 0.2052(5) 0.4810(4) 0.2285(3) 0.0470(16) Uani 1 1 d . . . H9A H 0.1501 0.4492 0.1794 0.056 Uiso 1 1 calc R . . H9B H 0.2531 0.4214 0.2584 0.056 Uiso 1 1 calc R . . C10 C 0.1439(4) 0.5270(5) 0.2837(3) 0.0398(15) Uani 1 1 d . . . H10A H 0.0955 0.4707 0.2939 0.048 Uiso 1 1 calc R . . H10B H 0.0972 0.5884 0.2558 0.048 Uiso 1 1 calc R . . C11 C 0.1549(5) 0.6556(5) 0.4253(4) 0.0538(17) Uani 1 1 d . . . H11A H 0.2024 0.7039 0.4681 0.065 Uiso 1 1 calc R . . H11B H 0.1065 0.7016 0.3812 0.065 Uiso 1 1 calc R . . C12 C 0.0844(5) 0.5893(6) 0.4618(4) 0.073(2) Uani 1 1 d . . . H12A H 0.0390 0.5393 0.4205 0.109 Uiso 1 1 calc R . . H12B H 0.0368 0.6374 0.4800 0.109 Uiso 1 1 calc R . . H12C H 0.1318 0.5481 0.5086 0.109 Uiso 1 1 calc R . . Cl2 Cl 0.54676(15) 0.35943(16) 0.37988(11) 0.0573(5) Uani 1 1 d D . . O5 O 0.6461(9) 0.4282(14) 0.3972(10) 0.085(6) Uani 0.51(2) 1 d PD A 1 O6 O 0.4555(10) 0.4270(11) 0.3745(14) 0.161(9) Uani 0.51(2) 1 d PD A 1 O7 O 0.5376(11) 0.3053(17) 0.3047(8) 0.121(8) Uani 0.51(2) 1 d PD A 1 O8 O 0.5688(12) 0.2848(14) 0.4462(9) 0.128(9) Uani 0.51(2) 1 d PD A 1 O5' O 0.6583(10) 0.3934(19) 0.3871(12) 0.132(10) Uani 0.49(2) 1 d PD A 2 O6' O 0.5260(11) 0.3784(18) 0.4562(7) 0.107(9) Uani 0.49(2) 1 d PD A 2 O7' O 0.4670(11) 0.4194(11) 0.3146(9) 0.120(8) Uani 0.49(2) 1 d PD A 2 O8' O 0.5367(13) 0.2441(8) 0.3622(13) 0.144(9) Uani 0.49(2) 1 d PD A 2 Cl1 Cl 0.88125(15) 0.77083(13) 0.64523(11) 0.0575(5) Uani 1 1 d . . . O1 O 0.7671(4) 0.7504(4) 0.6385(3) 0.0848(15) Uani 1 1 d . . . O2 O 0.9164(5) 0.6856(4) 0.6017(3) 0.0968(17) Uani 1 1 d . . . O3 O 0.9464(4) 0.7674(4) 0.7306(3) 0.0985(18) Uani 1 1 d . . . O4 O 0.8918(5) 0.8750(4) 0.6121(3) 0.1062(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0504(3) 0.0533(3) 0.0497(3) 0.0133(2) 0.0069(2) 0.0072(3) Ag2 0.0490(3) 0.0501(3) 0.0681(4) -0.0041(3) 0.0068(3) -0.0112(3) S1 0.0381(10) 0.0444(9) 0.0450(10) 0.0051(7) 0.0066(7) 0.0030(8) S2 0.0482(11) 0.0525(11) 0.0675(12) 0.0005(8) 0.0211(9) 0.0052(9) S3 0.0464(10) 0.0573(11) 0.0463(10) -0.0019(8) 0.0187(8) 0.0017(8) S4 0.0344(9) 0.0424(9) 0.0354(9) 0.0016(7) 0.0085(7) 0.0030(7) C1 0.072(6) 0.133(8) 0.116(7) 0.059(6) 0.047(5) 0.030(6) C2 0.072(6) 0.101(6) 0.066(5) 0.031(4) 0.031(4) 0.021(5) C3 0.047(4) 0.048(4) 0.068(5) -0.003(3) 0.001(4) -0.004(3) C4 0.053(5) 0.039(4) 0.088(5) -0.008(3) 0.021(4) -0.001(3) C5 0.086(6) 0.054(5) 0.078(5) 0.010(4) 0.028(4) 0.017(4) C6 0.071(7) 0.110(8) 0.133(8) -0.007(6) -0.027(5) 0.025(6) C7 0.118(7) 0.081(6) 0.057(5) 0.003(4) -0.006(4) -0.021(5) C8 0.063(5) 0.055(4) 0.054(4) 0.008(3) 0.021(4) -0.006(4) C9 0.060(4) 0.037(4) 0.037(4) -0.001(3) 0.008(3) -0.002(3) C10 0.027(3) 0.053(4) 0.035(3) 0.003(3) 0.004(3) -0.002(3) C11 0.054(5) 0.049(4) 0.054(4) -0.006(3) 0.012(3) 0.018(3) C12 0.056(5) 0.089(6) 0.087(5) -0.010(4) 0.042(4) -0.011(4) Cl2 0.0421(12) 0.0789(14) 0.0479(12) -0.0065(10) 0.0110(9) 0.0096(10) O5 0.044(9) 0.122(12) 0.084(10) -0.027(8) 0.015(8) -0.030(8) O6 0.129(13) 0.211(16) 0.18(2) 0.090(14) 0.103(14) 0.109(11) O7 0.133(12) 0.168(19) 0.070(10) -0.058(11) 0.043(9) -0.022(11) O8 0.157(13) 0.136(17) 0.093(13) 0.066(13) 0.044(10) -0.006(11) O5' 0.096(15) 0.169(19) 0.16(2) 0.016(14) 0.079(14) 0.022(13) O6' 0.095(12) 0.17(2) 0.069(10) -0.045(11) 0.051(9) -0.037(13) O7' 0.070(10) 0.185(15) 0.077(12) 0.037(11) -0.012(7) 0.045(9) O8' 0.181(16) 0.115(13) 0.12(2) -0.034(11) 0.031(13) -0.014(11) Cl1 0.0548(12) 0.0487(11) 0.0622(12) -0.0030(9) 0.0104(10) -0.0093(9) O1 0.046(3) 0.087(4) 0.112(4) -0.016(3) 0.014(3) -0.007(3) O2 0.120(5) 0.074(4) 0.118(4) -0.019(3) 0.069(4) -0.001(3) O3 0.084(4) 0.115(5) 0.065(4) -0.002(3) -0.017(3) -0.025(3) O4 0.137(5) 0.060(4) 0.128(5) 0.027(3) 0.053(4) -0.008(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 S4 2.447(2) 3_666 ? Ag1 S1 2.464(2) . ? Ag2 S3 2.520(2) . ? Ag2 S2 2.545(2) . ? Ag2 S1 2.632(2) . ? Ag2 S4 2.651(2) . ? S1 C2 1.814(6) . ? S1 C3 1.824(6) . ? S2 C5 1.790(6) . ? S2 C4 1.803(6) . ? S3 C8 1.805(6) . ? S3 C9 1.809(6) . ? S4 C10 1.818(5) . ? S4 C11 1.823(5) . ? S4 Ag1 2.447(2) 3_666 ? C1 C2 1.463(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.486(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.517(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.505(8) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.507(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.480(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? Cl2 O6 1.393(8) . ? Cl2 O8 1.399(7) . ? Cl2 O7 1.406(7) . ? Cl2 O6' 1.424(7) . ? Cl2 O7' 1.425(7) . ? Cl2 O8' 1.427(8) . ? Cl2 O5' 1.433(9) . ? Cl2 O5 1.453(8) . ? Cl1 O4 1.406(5) . ? Cl1 O3 1.410(4) . ? Cl1 O2 1.424(5) . ? Cl1 O1 1.429(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 S4 Ag1 S1 162.36(5) 3_666 . ? S3 Ag2 S2 145.02(6) . . ? S3 Ag2 S1 124.47(5) . . ? S2 Ag2 S1 82.54(5) . . ? S3 Ag2 S4 83.43(5) . . ? S2 Ag2 S4 106.22(5) . . ? S1 Ag2 S4 115.12(5) . . ? C2 S1 C3 104.2(3) . . ? C2 S1 Ag1 109.7(2) . . ? C3 S1 Ag1 105.6(2) . . ? C2 S1 Ag2 109.1(2) . . ? C3 S1 Ag2 100.2(2) . . ? Ag1 S1 Ag2 125.48(6) . . ? C5 S2 C4 101.1(3) . . ? C5 S2 Ag2 106.7(2) . . ? C4 S2 Ag2 98.4(2) . . ? C8 S3 C9 101.2(3) . . ? C8 S3 Ag2 108.7(2) . . ? C9 S3 Ag2 101.97(18) . . ? C10 S4 C11 102.0(3) . . ? C10 S4 Ag1 108.64(19) . 3_666 ? C11 S4 Ag1 112.7(2) . 3_666 ? C10 S4 Ag2 97.59(17) . . ? C11 S4 Ag2 111.8(2) . . ? Ag1 S4 Ag2 121.10(6) 3_666 . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 S1 115.5(5) . . ? C1 C2 H2A 108.4 . . ? S1 C2 H2A 108.4 . . ? C1 C2 H2B 108.4 . . ? S1 C2 H2B 108.4 . . ? H2A C2 H2B 107.5 . . ? C4 C3 S1 114.2(4) . . ? C4 C3 H3A 108.7 . . ? S1 C3 H3A 108.7 . . ? C4 C3 H3B 108.7 . . ? S1 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C3 C4 S2 111.4(4) . . ? C3 C4 H4A 109.3 . . ? S2 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? S2 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C6 C5 S2 109.5(5) . . ? C6 C5 H5A 109.8 . . ? S2 C5 H5A 109.8 . . ? C6 C5 H5B 109.8 . . ? S2 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C7 C8 S3 112.9(5) . . ? C7 C8 H8A 109.0 . . ? S3 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? S3 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C10 C9 S3 116.7(4) . . ? C10 C9 H9A 108.1 . . ? S3 C9 H9A 108.1 . . ? C10 C9 H9B 108.1 . . ? S3 C9 H9B 108.1 . . ? H9A C9 H9B 107.3 . . ? C9 C10 S4 110.2(4) . . ? C9 C10 H10A 109.6 . . ? S4 C10 H10A 109.6 . . ? C9 C10 H10B 109.6 . . ? S4 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C12 C11 S4 113.8(4) . . ? C12 C11 H11A 108.8 . . ? S4 C11 H11A 108.8 . . ? C12 C11 H11B 108.8 . . ? S4 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O6 Cl2 O8 111.8(7) . . ? O6 Cl2 O7 113.5(7) . . ? O8 Cl2 O7 111.3(8) . . ? O6 Cl2 O6' 64.2(7) . . ? O8 Cl2 O6' 54.5(6) . . ? O7 Cl2 O6' 156.6(7) . . ? O6 Cl2 O7' 45.1(6) . . ? O8 Cl2 O7' 149.0(8) . . ? O7 Cl2 O7' 73.0(7) . . ? O6' Cl2 O7' 109.2(7) . . ? O6 Cl2 O8' 123.3(10) . . ? O8 Cl2 O8' 61.0(7) . . ? O7 Cl2 O8' 51.5(7) . . ? O6' Cl2 O8' 108.6(7) . . ? O7' Cl2 O8' 110.3(7) . . ? O6 Cl2 O5' 127.3(12) . . ? O8 Cl2 O5' 101.0(11) . . ? O7 Cl2 O5' 89.6(10) . . ? O6' Cl2 O5' 110.5(8) . . ? O7' Cl2 O5' 109.8(8) . . ? O8' Cl2 O5' 108.4(8) . . ? O6 Cl2 O5 108.4(8) . . ? O8 Cl2 O5 106.3(7) . . ? O7 Cl2 O5 104.9(7) . . ? O6' Cl2 O5 97.5(9) . . ? O7' Cl2 O5 101.8(10) . . ? O8' Cl2 O5 128.0(10) . . ? O5' Cl2 O5 19.9(13) . . ? O4 Cl1 O3 109.7(3) . . ? O4 Cl1 O2 110.9(3) . . ? O3 Cl1 O2 109.6(3) . . ? O4 Cl1 O1 110.6(3) . . ? O3 Cl1 O1 107.8(3) . . ? O2 Cl1 O1 108.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S4 Ag1 S1 C2 -69.0(3) 3_666 . . . ? S4 Ag1 S1 C3 179.2(3) 3_666 . . . ? S4 Ag1 S1 Ag2 64.1(2) 3_666 . . . ? S3 Ag2 S1 C2 45.4(3) . . . . ? S2 Ag2 S1 C2 -110.4(3) . . . . ? S4 Ag2 S1 C2 145.1(3) . . . . ? S3 Ag2 S1 C3 154.5(2) . . . . ? S2 Ag2 S1 C3 -1.3(2) . . . . ? S4 Ag2 S1 C3 -105.8(2) . . . . ? S3 Ag2 S1 Ag1 -87.90(9) . . . . ? S2 Ag2 S1 Ag1 116.26(8) . . . . ? S4 Ag2 S1 Ag1 11.80(9) . . . . ? S3 Ag2 S2 C5 -12.9(3) . . . . ? S1 Ag2 S2 C5 131.0(3) . . . . ? S4 Ag2 S2 C5 -114.9(3) . . . . ? S3 Ag2 S2 C4 -117.3(2) . . . . ? S1 Ag2 S2 C4 26.7(2) . . . . ? S4 Ag2 S2 C4 140.7(2) . . . . ? S2 Ag2 S3 C8 -4.7(2) . . . . ? S1 Ag2 S3 C8 -139.6(2) . . . . ? S4 Ag2 S3 C8 104.3(2) . . . . ? S2 Ag2 S3 C9 -111.1(2) . . . . ? S1 Ag2 S3 C9 114.0(2) . . . . ? S4 Ag2 S3 C9 -2.0(2) . . . . ? S3 Ag2 S4 C10 -23.10(19) . . . . ? S2 Ag2 S4 C10 122.53(19) . . . . ? S1 Ag2 S4 C10 -148.21(18) . . . . ? S3 Ag2 S4 C11 -129.3(2) . . . . ? S2 Ag2 S4 C11 16.3(2) . . . . ? S1 Ag2 S4 C11 105.6(2) . . . . ? S3 Ag2 S4 Ag1 94.10(7) . . . 3_666 ? S2 Ag2 S4 Ag1 -120.27(7) . . . 3_666 ? S1 Ag2 S4 Ag1 -31.02(8) . . . 3_666 ? C3 S1 C2 C1 78.5(6) . . . . ? Ag1 S1 C2 C1 -34.2(7) . . . . ? Ag2 S1 C2 C1 -175.2(5) . . . . ? C2 S1 C3 C4 79.8(5) . . . . ? Ag1 S1 C3 C4 -164.6(4) . . . . ? Ag2 S1 C3 C4 -33.1(5) . . . . ? S1 C3 C4 S2 65.8(6) . . . . ? C5 S2 C4 C3 -167.0(5) . . . . ? Ag2 S2 C4 C3 -58.0(4) . . . . ? C4 S2 C5 C6 166.4(5) . . . . ? Ag2 S2 C5 C6 64.0(5) . . . . ? C9 S3 C8 C7 -76.5(5) . . . . ? Ag2 S3 C8 C7 176.7(4) . . . . ? C8 S3 C9 C10 -75.5(5) . . . . ? Ag2 S3 C9 C10 36.6(4) . . . . ? S3 C9 C10 S4 -64.7(5) . . . . ? C11 S4 C10 C9 165.8(4) . . . . ? Ag1 S4 C10 C9 -75.0(4) 3_666 . . . ? Ag2 S4 C10 C9 51.5(4) . . . . ? C10 S4 C11 C12 77.6(5) . . . . ? Ag1 S4 C11 C12 -38.8(5) 3_666 . . . ? Ag2 S4 C11 C12 -179.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.548 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.097 data_021129e _database_code_depnum_ccdc_archive 'CCDC 231506' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H16 Ag Cl O4 S2' _chemical_formula_weight 371.64 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 2(1)2(1)2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.506(2) _cell_length_b 11.300(4) _cell_length_c 15.348(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1301.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 782 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 21.17 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 2.066 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.775922 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6077 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 26.47 _reflns_number_total 2592 _reflns_number_gt 1817 _reflns_threshold_expression I>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^)+(0.0552P)^2^+0.5685P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(8) _refine_ls_number_reflns 2592 _refine_ls_number_parameters 166 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.1009 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.136 _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 0.82085(9) 0.76521(7) 0.07579(4) 0.0559(3) Uani 1 1 d . . . S1 S 0.5194(3) 0.66796(19) 0.05102(13) 0.0426(5) Uani 1 1 d . . . S2 S -0.0180(4) 0.7784(3) 0.21834(14) 0.0605(7) Uani 1 1 d . . . C1 C 0.6588(19) 0.4562(10) 0.1126(9) 0.097(4) Uani 1 1 d . A . H1A H 0.6157 0.4832 0.1680 0.146 Uiso 1 1 calc R . . H1B H 0.7815 0.4784 0.1059 0.146 Uiso 1 1 calc R . . H1C H 0.6485 0.3716 0.1095 0.146 Uiso 1 1 calc R . . C2 C 0.5477(15) 0.5127(9) 0.0392(7) 0.067(3) Uani 1 1 d . . . H2A H 0.4313 0.4755 0.0378 0.080 Uiso 1 1 calc R A . H2B H 0.6054 0.4970 -0.0162 0.080 Uiso 1 1 calc R . . C3 C 0.3919(12) 0.6824(9) 0.1520(5) 0.047(2) Uani 1 1 d . . . H3A H 0.4649 0.6562 0.2004 0.057 Uiso 1 1 calc R A . H3B H 0.3635 0.7652 0.1613 0.057 Uiso 1 1 calc R . . C4 C 0.2230(14) 0.6124(9) 0.1509(7) 0.061(3) Uani 1 1 d . A . H4A H 0.2516 0.5287 0.1517 0.073 Uiso 1 1 calc R . . H4B H 0.1589 0.6289 0.0974 0.073 Uiso 1 1 calc R . . C5 C 0.1028(13) 0.6412(12) 0.2287(6) 0.074(3) Uani 1 1 d . . . H5A H 0.1755 0.6447 0.2809 0.089 Uiso 1 1 calc R A . H5B H 0.0179 0.5773 0.2362 0.089 Uiso 1 1 calc R . . C6 C -0.1834(12) 0.7595(10) 0.3015(5) 0.059(2) Uani 1 1 d . . . H6A H -0.2755 0.8186 0.2928 0.070 Uiso 1 1 calc R A . H6B H -0.2382 0.6824 0.2939 0.070 Uiso 1 1 calc R . . C7 C -0.1178(14) 0.7688(12) 0.3933(6) 0.076(3) Uani 1 1 d . A . H7A H -0.0758 0.8477 0.4040 0.114 Uiso 1 1 calc R . . H7B H -0.0222 0.7136 0.4022 0.114 Uiso 1 1 calc R . . H7C H -0.2134 0.7509 0.4328 0.114 Uiso 1 1 calc R . . Cl1 Cl 0.5402(4) 1.0137(2) 0.10595(14) 0.0538(6) Uani 1 1 d D . . O1 O 0.5492(13) 1.1366(5) 0.1032(6) 0.103(3) Uani 1 1 d DU A . O2' O 0.365(3) 0.9893(14) 0.146(2) 0.129(13) Uani 0.52(3) 1 d PDU A 1 O3' O 0.670(3) 0.9549(13) 0.1551(16) 0.122(14) Uani 0.52(3) 1 d PDU A 1 O4' O 0.530(4) 0.9612(16) 0.0217(8) 0.129(12) Uani 0.52(3) 1 d PDU A 1 O2 O 0.516(5) 0.9736(15) 0.1921(7) 0.115(14) Uani 0.48(3) 1 d PD A 2 O3 O 0.7247(17) 0.9798(16) 0.082(2) 0.133(13) Uani 0.48(3) 1 d PD A 2 O4 O 0.429(3) 0.9575(16) 0.0463(14) 0.104(11) Uani 0.48(3) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0445(4) 0.0805(5) 0.0428(3) 0.0098(4) -0.0025(3) 0.0010(4) S1 0.0362(13) 0.0548(13) 0.0369(11) 0.0040(9) 0.0006(9) -0.0001(11) S2 0.0579(15) 0.0799(18) 0.0436(11) 0.0081(12) -0.0032(11) -0.0147(15) C1 0.116(11) 0.062(7) 0.115(10) 0.023(7) -0.003(9) 0.028(8) C2 0.067(7) 0.069(7) 0.065(6) -0.004(6) 0.016(6) 0.005(6) C3 0.057(6) 0.054(5) 0.031(4) -0.003(4) -0.001(4) -0.007(5) C4 0.055(7) 0.062(7) 0.067(6) 0.000(5) 0.001(5) 0.013(5) C5 0.050(6) 0.130(10) 0.042(5) 0.018(6) 0.007(5) 0.024(7) C6 0.050(5) 0.074(6) 0.053(5) -0.003(5) 0.011(4) -0.004(7) C7 0.073(7) 0.109(9) 0.047(5) -0.005(6) 0.007(5) -0.009(7) Cl1 0.0656(17) 0.0485(14) 0.0475(13) -0.0040(10) -0.0022(12) 0.0104(12) O1 0.141(8) 0.051(4) 0.116(7) 0.008(4) 0.003(7) 0.002(5) O2' 0.15(2) 0.080(13) 0.16(3) 0.013(14) 0.06(2) -0.007(15) O3' 0.17(3) 0.079(12) 0.12(2) -0.023(14) -0.07(2) 0.044(17) O4' 0.22(3) 0.110(17) 0.057(10) -0.045(11) 0.022(17) 0.013(19) O2 0.21(4) 0.087(15) 0.045(10) 0.014(9) 0.017(15) -0.03(2) O3 0.095(16) 0.137(19) 0.17(3) -0.06(2) 0.064(19) 0.010(13) O4 0.11(2) 0.132(19) 0.067(15) 0.006(13) -0.053(15) -0.032(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 S2 2.504(2) 1_655 ? Ag1 O3 2.53(2) . ? Ag1 S1 2.544(2) . ? Ag1 S1 2.565(2) 4_565 ? S1 C2 1.78(1) . ? S1 C3 1.829(9) . ? S1 Ag1 2.565(2) 4_465 ? S2 C6 1.793(8) . ? S2 C5 1.80(1) . ? S2 Ag1 2.504(2) 1_455 ? C1 C2 1.54(2) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.495(13) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.531(13) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.497(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? Cl1 O1 1.390(6) . ? Cl1 O4 1.393(9) . ? Cl1 O3' 1.401(9) . ? Cl1 O2 1.410(8) . ? Cl1 O4' 1.426(9) . ? Cl1 O2' 1.474(9) . ? Cl1 O3 1.482(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 S2 Ag1 O3 92.7(7) 1_655 . ? S2 Ag1 S1 125.85(8) 1_655 . ? O3 Ag1 S1 99.6(4) . . ? S2 Ag1 S1 111.40(8) 1_655 4_565 ? O3 Ag1 S1 85.0(6) . 4_565 ? S1 Ag1 S1 122.04(5) . 4_565 ? C2 S1 C3 103.7(5) . . ? C2 S1 Ag1 109.6(4) . . ? C3 S1 Ag1 107.5(3) . . ? C2 S1 Ag1 106.4(4) . 4_465 ? C3 S1 Ag1 108.2(3) . 4_465 ? Ag1 S1 Ag1 120.20(8) . 4_465 ? C6 S2 C5 100.6(5) . . ? C6 S2 Ag1 106.3(3) . 1_455 ? C5 S2 Ag1 105.6(4) . 1_455 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 S1 113.5(8) . . ? C1 C2 H2A 108.9 . . ? S1 C2 H2A 108.9 . . ? C1 C2 H2B 108.9 . . ? S1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C4 C3 S1 112.8(6) . . ? C4 C3 H3A 109.0 . . ? S1 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? S1 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C3 C4 C5 112.3(9) . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C4 C5 S2 114.2(7) . . ? C4 C5 H5A 108.7 . . ? S2 C5 H5A 108.7 . . ? C4 C5 H5B 108.7 . . ? S2 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C7 C6 S2 115.7(7) . . ? C7 C6 H6A 108.3 . . ? S2 C6 H6A 108.3 . . ? C7 C6 H6B 108.3 . . ? S2 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 Cl1 O4 117.7(9) . . ? O1 Cl1 O3' 117.2(8) . . ? O4 Cl1 O3' 123.7(11) . . ? O1 Cl1 O2 110.8(7) . . ? O4 Cl1 O2 113.1(9) . . ? O3' Cl1 O2 55.4(10) . . ? O1 Cl1 O4' 113.0(9) . . ? O4 Cl1 O4' 35.0(11) . . ? O3' Cl1 O4' 109.2(9) . . ? O2 Cl1 O4' 135.3(11) . . ? O1 Cl1 O2' 104.1(7) . . ? O4 Cl1 O2' 69.6(11) . . ? O3' Cl1 O2' 108.0(9) . . ? O2 Cl1 O2' 55.7(10) . . ? O4' Cl1 O2' 104.3(9) . . ? O1 Cl1 O3 101.8(8) . . ? O4 Cl1 O3 106.3(9) . . ? O3' Cl1 O3 50.2(10) . . ? O2 Cl1 O3 105.6(10) . . ? O4' Cl1 O3 73.8(11) . . ? O2' Cl1 O3 152.3(10) . . ? Cl1 O3 Ag1 121.6(10) . . ? 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 S2 Ag1 S1 C2 -82.0(4) 1_655 . . . ? O3 Ag1 S1 C2 177.6(8) . . . . ? S1 Ag1 S1 C2 87.5(4) 4_565 . . . ? S2 Ag1 S1 C3 30.1(4) 1_655 . . . ? O3 Ag1 S1 C3 -70.3(8) . . . . ? S1 Ag1 S1 C3 -160.3(3) 4_565 . . . ? S2 Ag1 S1 Ag1 154.34(11) 1_655 . . 4_465 ? O3 Ag1 S1 Ag1 53.9(8) . . . 4_465 ? S1 Ag1 S1 Ag1 -36.14(10) 4_565 . . 4_465 ? C3 S1 C2 C1 -63.7(9) . . . . ? Ag1 S1 C2 C1 50.8(8) . . . . ? Ag1 S1 C2 C1 -177.8(7) 4_465 . . . ? C2 S1 C3 C4 -54.9(8) . . . . ? Ag1 S1 C3 C4 -171.0(6) . . . . ? Ag1 S1 C3 C4 57.8(7) 4_465 . . . ? S1 C3 C4 C5 -170.4(7) . . . . ? C3 C4 C5 S2 77.5(10) . . . . ? C6 S2 C5 C4 164.1(8) . . . . ? Ag1 S2 C5 C4 53.7(9) 1_455 . . . ? C5 S2 C6 C7 72.4(9) . . . . ? Ag1 S2 C6 C7 -177.8(8) 1_455 . . . ? O1 Cl1 O3 Ag1 178.6(15) . . . . ? O4 Cl1 O3 Ag1 -57.6(19) . . . . ? O3' Cl1 O3 Ag1 63.0(17) . . . . ? O2 Cl1 O3 Ag1 62.8(18) . . . . ? O4' Cl1 O3 Ag1 -70.6(15) . . . . ? O2' Cl1 O3 Ag1 19(3) . . . . ? S2 Ag1 O3 Cl1 -103(2) 1_655 . . . ? S1 Ag1 O3 Cl1 24(2) . . . . ? S1 Ag1 O3 Cl1 145(2) 4_565 . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.47 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.945 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.102 data_14_b _database_code_depnum_ccdc_archive 'CCDC 231507' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H36 Ag Cl O4 S4' _chemical_formula_weight 564.01 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(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 13.535(15) _cell_length_b 9.765(10) _cell_length_c 19.45(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.014(19) _cell_angle_gamma 90.00 _cell_volume 2514(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 836 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 22.43 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 1.257 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7042 _exptl_absorpt_correction_T_max 0.7358 _exptl_absorpt_process_details SADABS _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 'Bruker CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10268 _diffrn_reflns_av_R_equivalents 0.0960 _diffrn_reflns_av_sigmaI/netI 0.1424 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4325 _reflns_number_gt 1860 _reflns_threshold_expression I>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_publication_material 'Bruker SHELXTL' _computing_molecular_graphics '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^)+(0.0604P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0025(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4325 _refine_ls_number_parameters 292 _refine_ls_number_restraints 194 _refine_ls_R_factor_all 0.1768 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.1674 _refine_ls_wR_factor_gt 0.1289 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 1.013 _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 0.74275(5) 0.75156(8) 0.17048(4) 0.0545(3) Uani 1 1 d . . . S1 S 0.86345(17) 0.7492(3) 0.29328(11) 0.0571(7) Uani 1 1 d . . . S2 S 1.16424(19) 0.2069(3) 0.43217(13) 0.0562(8) Uani 1 1 d . . . C1 C 0.7455(10) 0.8995(16) 0.3647(6) 0.132(6) Uani 1 1 d U . . H1A H 0.7078 0.9016 0.4013 0.198 Uiso 1 1 calc R . . H1B H 0.7010 0.9165 0.3202 0.198 Uiso 1 1 calc R . . H1C H 0.7970 0.9687 0.3733 0.198 Uiso 1 1 calc R . . C2 C 0.7926(10) 0.7647(12) 0.3633(5) 0.102(4) Uani 1 1 d U . . H2A H 0.7405 0.6949 0.3569 0.122 Uiso 1 1 calc R . . H2B H 0.8379 0.7485 0.4082 0.122 Uiso 1 1 calc R . . C3 C 0.9008(7) 0.5705(9) 0.3015(5) 0.061(3) Uani 1 1 d . . . H3A H 0.8404 0.5145 0.2960 0.073 Uiso 1 1 calc R . . H3B H 0.9343 0.5476 0.2635 0.073 Uiso 1 1 calc R . . C4 C 0.9696(7) 0.5348(9) 0.3699(5) 0.059(3) Uani 1 1 d . . . H4A H 0.9313 0.5324 0.4068 0.071 Uiso 1 1 calc R . . H4B H 1.0214 0.6045 0.3818 0.071 Uiso 1 1 calc R . . C5 C 1.0197(7) 0.3940(10) 0.3649(5) 0.057(3) Uani 1 1 d . . . H5A H 0.9680 0.3255 0.3493 0.069 Uiso 1 1 calc R . . H5B H 1.0625 0.3985 0.3306 0.069 Uiso 1 1 calc R . . C6 C 1.0835(7) 0.3526(10) 0.4369(5) 0.059(3) Uani 1 1 d . . . H6A H 1.0387 0.3311 0.4684 0.070 Uiso 1 1 calc R . . H6B H 1.1251 0.4298 0.4567 0.070 Uiso 1 1 calc R . . C7 C 1.0693(10) 0.0732(12) 0.4083(7) 0.103(4) Uani 1 1 d . . . H7A H 1.0252 0.0730 0.4417 0.124 Uiso 1 1 calc R . . H7B H 1.0284 0.0929 0.3622 0.124 Uiso 1 1 calc R . . C8 C 1.1136(11) -0.0573(14) 0.4073(8) 0.148(6) Uani 1 1 d U . . H8A H 1.0615 -0.1248 0.3943 0.223 Uiso 1 1 calc R . . H8B H 1.1528 -0.0781 0.4532 0.223 Uiso 1 1 calc R . . H8C H 1.1566 -0.0578 0.3738 0.223 Uiso 1 1 calc R . . S3 S 0.6349(2) 0.5290(3) 0.16483(15) 0.0643(8) Uani 1 1 d D . . C9 C 0.5114(9) 0.6791(14) 0.2345(7) 0.108(5) Uani 1 1 d . . . H9A H 0.4742 0.6761 0.2714 0.162 Uiso 1 1 calc R A . H9B H 0.4663 0.6997 0.1907 0.162 Uiso 1 1 calc R . . H9C H 0.5625 0.7486 0.2447 0.162 Uiso 1 1 calc R . . C10 C 0.5593(9) 0.5458(12) 0.2293(7) 0.091(4) Uani 1 1 d . A . H10A H 0.5064 0.4771 0.2197 0.109 Uiso 1 1 calc R . . H10B H 0.6013 0.5246 0.2748 0.109 Uiso 1 1 calc R . . C11 C 0.5244(10) 0.529(3) 0.0983(4) 0.138(8) Uani 0.71(2) 1 d PDU A 1 H11A H 0.4846 0.4486 0.1032 0.166 Uiso 0.71(2) 1 calc PR A 1 H11B H 0.4842 0.6093 0.1037 0.166 Uiso 0.71(2) 1 calc PR A 1 C12 C 0.5493(10) 0.530(3) 0.0252(5) 0.176(9) Uani 0.71(2) 1 d PDU . 1 H12A H 0.6077 0.4736 0.0240 0.211 Uiso 0.71(2) 1 calc PR A 1 H12B H 0.5627 0.6227 0.0113 0.211 Uiso 0.71(2) 1 calc PR A 1 C11' C 0.560(4) 0.5947(18) 0.0846(12) 0.134(13) Uani 0.29(2) 1 d PDU A 2 H11C H 0.5052 0.6500 0.0945 0.160 Uiso 0.29(2) 1 calc PR A 2 H11D H 0.6013 0.6515 0.0608 0.160 Uiso 0.29(2) 1 calc PR A 2 C12' C 0.518(5) 0.472(2) 0.0382(8) 0.177(14) Uani 0.29(2) 1 d PDU . 2 H12C H 0.4620 0.4311 0.0547 0.213 Uiso 0.29(2) 1 calc PR A 2 H12D H 0.5701 0.4032 0.0394 0.213 Uiso 0.29(2) 1 calc PR A 2 S4 S 0.64584(18) 0.9776(3) 0.15833(14) 0.0566(8) Uani 1 1 d . . . C13 C 0.8012(8) 1.1490(11) 0.2143(6) 0.090(4) Uani 1 1 d . . . H13A H 0.8444 1.2236 0.2076 0.135 Uiso 1 1 calc R A . H13B H 0.8414 1.0692 0.2293 0.135 Uiso 1 1 calc R . . H13C H 0.7641 1.1734 0.2495 0.135 Uiso 1 1 calc R . . C14 C 0.7288(7) 1.1189(10) 0.1464(5) 0.072(3) Uani 1 1 d . A . H14A H 0.7661 1.0951 0.1106 0.086 Uiso 1 1 calc R . . H14B H 0.6887 1.1997 0.1308 0.086 Uiso 1 1 calc R . . C15 C 0.5542(8) 0.9655(10) 0.0756(6) 0.082(4) Uani 1 1 d D A . H15A H 0.5064 0.8949 0.0796 0.099 Uiso 1 1 d R . . C16 C 0.4957(13) 1.0878(17) 0.0420(10) 0.080(7) Uani 0.50 1 d PD A 1 H16A H 0.5418 1.1480 0.0254 0.096 Uiso 0.50 1 d PR A 1 H16B H 0.4753 1.1313 0.0810 0.096 Uiso 0.50 1 d PR A 1 C16' C 0.5917(13) 0.940(2) 0.0101(9) 0.087(8) Uani 0.50 1 d PD A 2 H16D H 0.6341 1.0155 0.0035 0.131 Uiso 0.50 1 d PR A 2 H16E H 0.6297 0.8564 0.0128 0.131 Uiso 0.50 1 d PR A 2 Cl1 Cl 0.7476(2) 0.1865(4) 0.92885(17) 0.0810(9) Uani 1 1 d D . . O1 O 0.6763(6) 0.2625(8) 0.9561(5) 0.140(4) Uani 1 1 d DU B 1 O2 O 0.7006(13) 0.098(3) 0.8742(13) 0.197(14) Uani 0.57(2) 1 d PDU B 1 O3 O 0.8122(15) 0.2820(16) 0.9006(14) 0.156(10) Uani 0.57(2) 1 d PDU B 1 O4 O 0.8110(16) 0.114(3) 0.9844(8) 0.151(11) Uani 0.57(2) 1 d PDU B 1 O2' O 0.754(2) 0.199(3) 0.8569(8) 0.163(15) Uani 0.43(2) 1 d PDU B 2 O3' O 0.8481(10) 0.198(3) 0.9693(15) 0.132(14) Uani 0.43(2) 1 d PDU B 2 O4' O 0.7259(19) 0.0408(12) 0.9369(15) 0.106(9) Uani 0.43(2) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0544(5) 0.0562(5) 0.0507(5) 0.0074(5) 0.0062(3) 0.0025(4) S1 0.0598(14) 0.0660(17) 0.0403(13) 0.0050(16) -0.0015(11) 0.0085(16) S2 0.0660(16) 0.0576(19) 0.0449(15) 0.0054(12) 0.0109(13) 0.0014(12) C1 0.161(13) 0.164(14) 0.079(10) 0.019(10) 0.044(9) 0.077(11) C2 0.150(11) 0.111(11) 0.049(6) 0.013(8) 0.031(7) 0.058(9) C3 0.068(7) 0.066(7) 0.045(6) 0.002(5) -0.002(5) 0.016(6) C4 0.069(7) 0.053(7) 0.054(7) 0.001(5) 0.012(6) 0.010(5) C5 0.060(6) 0.068(8) 0.044(6) 0.005(5) 0.011(5) 0.008(5) C6 0.073(6) 0.057(7) 0.049(7) -0.006(5) 0.020(6) -0.001(6) C7 0.119(11) 0.062(9) 0.129(12) -0.005(9) 0.025(10) -0.012(8) C8 0.154(13) 0.084(11) 0.176(16) 0.008(11) -0.037(12) -0.020(10) S3 0.0618(18) 0.0491(19) 0.075(2) 0.0012(15) -0.0011(17) -0.0041(14) C9 0.099(9) 0.092(10) 0.153(14) 0.021(10) 0.072(9) -0.008(8) C10 0.097(9) 0.078(10) 0.108(10) 0.009(8) 0.044(8) -0.025(8) C11 0.141(11) 0.128(11) 0.134(11) -0.001(8) 0.001(8) 0.005(8) C12 0.158(12) 0.173(12) 0.187(13) -0.030(9) 0.015(9) 0.014(9) C11' 0.131(15) 0.140(15) 0.132(15) 0.003(9) 0.033(9) -0.007(9) C12' 0.177(16) 0.183(16) 0.170(16) -0.002(10) 0.033(10) 0.020(10) S4 0.0562(17) 0.0554(19) 0.0573(18) 0.0035(14) 0.0100(15) 0.0096(13) C13 0.105(9) 0.062(8) 0.099(10) -0.012(7) 0.013(8) -0.016(7) C14 0.097(8) 0.049(7) 0.068(8) 0.006(6) 0.013(7) -0.006(6) C15 0.064(7) 0.059(8) 0.101(10) 0.035(7) -0.034(7) 0.017(6) C16 0.056(13) 0.109(19) 0.073(16) 0.031(15) 0.008(12) 0.025(13) C16' 0.040(12) 0.13(2) 0.078(18) -0.025(16) -0.014(13) 0.003(13) Cl1 0.0707(19) 0.098(3) 0.076(2) 0.0062(19) 0.0180(18) 0.0167(19) O1 0.106(6) 0.153(9) 0.172(10) -0.026(7) 0.053(7) 0.047(6) O2 0.18(2) 0.25(3) 0.13(2) -0.12(2) -0.029(18) 0.00(2) O3 0.17(2) 0.17(2) 0.13(2) 0.034(16) 0.056(17) 0.001(15) O4 0.130(19) 0.18(3) 0.135(18) 0.048(18) 0.016(16) 0.069(18) O2' 0.19(3) 0.22(4) 0.10(2) 0.01(2) 0.07(2) 0.07(3) O3' 0.074(14) 0.14(3) 0.18(3) -0.08(2) 0.023(16) 0.018(15) O4' 0.119(19) 0.098(18) 0.10(2) -0.004(14) 0.013(16) -0.006(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 S4 2.553(3) . ? Ag1 S1 2.598(3) . ? Ag1 S3 2.607(3) . ? Ag1 S2 2.609(3) 2_755 ? S1 C3 1.815(9) . ? S1 C2 1.83(1) . ? S2 C6 1.808(9) . ? S2 C7 1.82(1) . ? S2 Ag1 2.609(3) 2_745 ? C1 C2 1.465(13) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.498(11) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.545(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.539(12) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.410(14) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? S3 C11 1.762(9) . ? S3 C10 1.784(11) . ? S3 C11' 1.792(10) . ? C9 C10 1.466(14) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.529(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C12 1.595(10) 3_665 ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C11' C12' 1.536(10) . ? C11' H11C 0.9700 . ? C11' H11D 0.9700 . ? C12' C12' 1.562(11) 3_665 ? C12' H12C 0.9700 . ? C12' H12D 0.9700 . ? S4 C15 1.819(10) . ? S4 C14 1.824(10) . ? C13 C14 1.500(13) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16' 1.488(10) . ? C15 C16 1.505(9) . ? C15 H15A 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? Cl1 O1 1.406(6) . ? Cl1 O2 1.414(9) . ? Cl1 O4 1.420(9) . ? Cl1 O2' 1.425(10) . ? Cl1 O3' 1.426(10) . ? Cl1 O3 1.462(9) . ? Cl1 O4' 1.467(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 S4 Ag1 S1 107.78(9) . . ? S4 Ag1 S3 116.4(1) . . ? S1 Ag1 S3 105.7(1) . . ? S4 Ag1 S2 113.21(9) . 2_755 ? S1 Ag1 S2 113.0(1) . 2_755 ? S3 Ag1 S2 100.6(1) . 2_755 ? C3 S1 C2 101.2(5) . . ? C3 S1 Ag1 101.5(3) . . ? C2 S1 Ag1 110.9(4) . . ? C6 S2 C7 100.1(6) . . ? C6 S2 Ag1 107.5(3) . 2_745 ? C7 S2 Ag1 110.6(4) . 2_745 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 S1 112.7(8) . . ? C1 C2 H2A 109.1 . . ? S1 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? S1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? C4 C3 S1 114.3(7) . . ? C4 C3 H3A 108.7 . . ? S1 C3 H3A 108.7 . . ? C4 C3 H3B 108.7 . . ? S1 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C3 C4 C5 110.6(8) . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C6 C5 C4 110.3(7) . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5A 109.6 . . ? C6 C5 H5B 109.6 . . ? C4 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C5 C6 S2 113.0(6) . . ? C5 C6 H6A 109.0 . . ? S2 C6 H6A 109.0 . . ? C5 C6 H6B 109.0 . . ? S2 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C8 C7 S2 111.8(10) . . ? C8 C7 H7A 109.3 . . ? S2 C7 H7A 109.3 . . ? C8 C7 H7B 109.3 . . ? S2 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 S3 C10 89.6(6) . . ? C11 S3 C11' 28.5(15) . . ? C10 S3 C11' 106.0(19) . . ? C11 S3 Ag1 114.3(8) . . ? C10 S3 Ag1 107.0(4) . . ? C11' S3 Ag1 87.0(12) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C9 C10 S3 117.1(8) . . ? C9 C10 H10A 108.0 . . ? S3 C10 H10A 108.0 . . ? C9 C10 H10B 108.0 . . ? S3 C10 H10B 108.0 . . ? H10A C10 H10B 107.3 . . ? C12 C11 S3 111.5(8) . . ? C12 C11 H11A 109.3 . . ? S3 C11 H11A 109.3 . . ? C12 C11 H11B 109.3 . . ? S3 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C12 104.5(8) . 3_665 ? C11 C12 H12A 110.8 . . ? C12 C12 H12A 110.8 3_665 . ? C11 C12 H12B 110.8 . . ? C12 C12 H12B 110.8 3_665 . ? H12A C12 H12B 108.9 . . ? C12' C11' S3 107.8(11) . . ? C12' C11' H11C 110.1 . . ? S3 C11' H11C 110.1 . . ? C12' C11' H11D 110.1 . . ? S3 C11' H11D 110.1 . . ? H11C C11' H11D 108.5 . . ? C11' C12' C12' 107.0(10) . 3_665 ? C11' C12' H12C 110.3 . . ? C12' C12' H12C 110.3 3_665 . ? C11' C12' H12D 110.3 . . ? C12' C12' H12D 110.3 3_665 . ? H12C C12' H12D 108.6 . . ? C15 S4 C14 105.1(5) . . ? C15 S4 Ag1 105.6(3) . . ? C14 S4 Ag1 110.4(4) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C13 C14 S4 110.1(7) . . ? C13 C14 H14A 109.6 . . ? S4 C14 H14A 109.6 . . ? C13 C14 H14B 109.6 . . ? S4 C14 H14B 109.6 . . ? H14A C14 H14B 108.2 . . ? C16' C15 C16 90.2(7) . . ? C16' C15 S4 118.5(10) . . ? C16 C15 S4 122.2(11) . . ? C16' C15 H15A 107.7 . . ? C16 C15 H15A 107.6 . . ? S4 C15 H15A 108.8 . . ? C15 C16 H16A 108.2 . . ? C15 C16 H16B 102.7 . . ? H16A C16 H16B 108.0 . . ? C15 C16' H16D 107.8 . . ? C15 C16' H16E 111.7 . . ? H16D C16' H16E 109.5 . . ? O1 Cl1 O2 111.7(8) . . ? O1 Cl1 O4 109.2(8) . . ? O2 Cl1 O4 111.9(9) . . ? O1 Cl1 O2' 120.6(13) . . ? O2 Cl1 O2' 54.7(11) . . ? O4 Cl1 O2' 129.9(14) . . ? O1 Cl1 O3' 113.7(12) . . ? O2 Cl1 O3' 133.5(13) . . ? O4 Cl1 O3' 42.5(10) . . ? O2' Cl1 O3' 107.0(11) . . ? O1 Cl1 O3 108.4(8) . . ? O2 Cl1 O3 108.5(9) . . ? O4 Cl1 O3 106.9(8) . . ? O2' Cl1 O3 54.2(11) . . ? O3' Cl1 O3 65.3(11) . . ? O1 Cl1 O4' 107.7(10) . . ? O2 Cl1 O4' 54.5(10) . . ? O4 Cl1 O4' 62.5(10) . . ? O2' Cl1 O4' 104.0(11) . . ? O3' Cl1 O4' 101.8(10) . . ? O3 Cl1 O4' 143.8(11) . . ? 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 S4 Ag1 S1 C3 166.4(3) . . . . ? S3 Ag1 S1 C3 41.3(3) . . . . ? S2 Ag1 S1 C3 -67.8(3) 2_755 . . . ? S4 Ag1 S1 C2 59.5(4) . . . . ? S3 Ag1 S1 C2 -65.6(4) . . . . ? S2 Ag1 S1 C2 -174.6(4) 2_755 . . . ? C3 S1 C2 C1 -175.1(10) . . . . ? Ag1 S1 C2 C1 -68.1(11) . . . . ? C2 S1 C3 C4 -63.7(8) . . . . ? Ag1 S1 C3 C4 -178.0(6) . . . . ? S1 C3 C4 C5 -164.8(6) . . . . ? C3 C4 C5 C6 -175.4(8) . . . . ? C4 C5 C6 S2 -168.5(6) . . . . ? C7 S2 C6 C5 -67.6(8) . . . . ? Ag1 S2 C6 C5 47.9(7) 2_745 . . . ? C6 S2 C7 C8 -174.5(10) . . . . ? Ag1 S2 C7 C8 72.3(11) 2_745 . . . ? S4 Ag1 S3 C11 43.4(5) . . . . ? S1 Ag1 S3 C11 163.0(5) . . . . ? S2 Ag1 S3 C11 -79.3(5) 2_755 . . . ? S4 Ag1 S3 C10 -54.0(5) . . . . ? S1 Ag1 S3 C10 65.5(5) . . . . ? S2 Ag1 S3 C10 -176.7(4) 2_755 . . . ? S4 Ag1 S3 C11' 51.8(16) . . . . ? S1 Ag1 S3 C11' 171.4(15) . . . . ? S2 Ag1 S3 C11' -70.9(16) 2_755 . . . ? C11 S3 C10 C9 -72.6(13) . . . . ? C11' S3 C10 C9 -49.0(14) . . . . ? Ag1 S3 C10 C9 42.8(11) . . . . ? C10 S3 C11 C12 174.3(19) . . . . ? C11' S3 C11 C12 48(2) . . . . ? Ag1 S3 C11 C12 66(2) . . . . ? S3 C11 C12 C12 157.4(19) . . . 3_665 ? C11 S3 C11' C12' -46(3) . . . . ? C10 S3 C11' C12' -103(4) . . . . ? Ag1 S3 C11' C12' 150(5) . . . . ? S3 C11' C12' C12' -163(5) . . . 3_665 ? S1 Ag1 S4 C15 -174.4(4) . . . . ? S3 Ag1 S4 C15 -56.0(4) . . . . ? S2 Ag1 S4 C15 59.8(4) 2_755 . . . ? S1 Ag1 S4 C14 72.5(4) . . . . ? S3 Ag1 S4 C14 -169.1(4) . . . . ? S2 Ag1 S4 C14 -53.3(4) 2_755 . . . ? C15 S4 C14 C13 173.8(7) . . . . ? Ag1 S4 C14 C13 -72.8(8) . . . . ? C14 S4 C15 C16' 59.1(13) . . . . ? Ag1 S4 C15 C16' -57.6(12) . . . . ? C14 S4 C15 C16 -51.1(12) . . . . ? Ag1 S4 C15 C16 -167.8(10) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.987 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.102 data_15 _database_code_depnum_ccdc_archive 'CCDC 231508' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H16 Ag Cl N0 O4 S2' _chemical_formula_weight 467.72 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.61(1) _cell_length_b 6.244(2) _cell_length_c 17.561(6) _cell_angle_alpha 90.00 _cell_angle_beta 114.498(6) _cell_angle_gamma 90.00 _cell_volume 3552(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 701 _cell_measurement_theta_min 2.5145 _cell_measurement_theta_max 22.0562 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 1.535 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.7489 _exptl_absorpt_correction_T_max 0.7697 _exptl_absorpt_process_details SADABS _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 'Bruker CCD area detector' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9709 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.0844 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 26.43 _reflns_number_total 3639 _reflns_number_gt 2110 _reflns_threshold_expression I>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^)+(0.0586P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3639 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1114 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1252 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 Ag1 Ag 0.504307(15) 0.70409(9) 0.54992(3) 0.0482(2) Uani 1 1 d . . . S1 S 0.43257(5) 0.6506(2) 0.52771(10) 0.0363(4) Uani 1 1 d . . . S2 S 0.56887(5) 0.7950(3) 0.53975(9) 0.0372(4) Uani 1 1 d . . . Cl1 Cl 0.54313(5) 1.1971(3) 0.68705(9) 0.0439(4) Uani 1 1 d . . . C1 C 0.6714(2) 0.5725(14) 0.6126(5) 0.078(2) Uani 1 1 d . . . H1A H 0.6584 0.4409 0.5953 0.093 Uiso 1 1 calc R . . C2 C 0.7092(3) 0.604(2) 0.6129(7) 0.115(4) Uani 1 1 d . . . H2A H 0.7215 0.4964 0.5946 0.139 Uiso 1 1 calc R . . C3 C 0.7289(3) 0.793(2) 0.6396(8) 0.122(5) Uani 1 1 d . . . H3A H 0.7550 0.8138 0.6408 0.147 Uiso 1 1 calc R . . C4 C 0.7104(3) 0.9507(19) 0.6647(6) 0.112(4) Uani 1 1 d . . . H4A H 0.7239 1.0808 0.6825 0.134 Uiso 1 1 calc R . . C5 C 0.6719(3) 0.9221(15) 0.6644(5) 0.083(3) Uani 1 1 d . . . H5A H 0.6596 1.0310 0.6821 0.100 Uiso 1 1 calc R . . C6 C 0.6520(2) 0.7291(12) 0.6372(4) 0.0507(17) Uani 1 1 d . . . C7 C 0.60980(18) 0.6941(11) 0.6354(4) 0.0492(17) Uani 1 1 d . . . H7A H 0.6083 0.7654 0.6831 0.059 Uiso 1 1 calc R . . H7B H 0.6057 0.5420 0.6404 0.059 Uiso 1 1 calc R . . C8 C 0.57422(17) 0.6317(9) 0.4611(4) 0.0361(14) Uani 1 1 d . . . H8A H 0.6014 0.6548 0.4625 0.043 Uiso 1 1 calc R . . H8B H 0.5541 0.6778 0.4067 0.043 Uiso 1 1 calc R . . C9 C 0.42845(19) 0.7461(11) 0.6224(4) 0.0496(18) Uani 1 1 d . . . H9A H 0.4459 0.6589 0.6696 0.059 Uiso 1 1 calc R . . H9B H 0.4384 0.8925 0.6334 0.059 Uiso 1 1 calc R . . C10 C 0.38489(18) 0.7376(10) 0.6149(4) 0.0415(16) Uani 1 1 d . . . C11 C 0.3564(2) 0.8917(13) 0.5725(5) 0.077(2) Uani 1 1 d . . . H11A H 0.3639 1.0027 0.5462 0.093 Uiso 1 1 calc R . . C12 C 0.3170(3) 0.8843(16) 0.5682(6) 0.096(3) Uani 1 1 d . . . H12A H 0.2984 0.9928 0.5408 0.115 Uiso 1 1 calc R . . C13 C 0.3050(2) 0.7212(16) 0.6034(6) 0.084(3) Uani 1 1 d . . . H13A H 0.2781 0.7157 0.5993 0.101 Uiso 1 1 calc R . . C14 C 0.3324(2) 0.5653(15) 0.6448(5) 0.076(3) Uani 1 1 d . . . H14A H 0.3244 0.4536 0.6699 0.092 Uiso 1 1 calc R . . C15 C 0.3721(2) 0.5715(12) 0.6499(4) 0.0579(19) Uani 1 1 d . . . H15A H 0.3905 0.4621 0.6774 0.069 Uiso 1 1 calc R . . O1 O 0.51132(17) 1.0609(11) 0.6353(4) 0.109(2) Uani 1 1 d . . . O2 O 0.52782(19) 1.4151(10) 0.6704(4) 0.112(2) Uani 1 1 d . . . O3 O 0.5528(2) 1.1673(11) 0.7702(3) 0.103(2) Uani 1 1 d . . . O4 O 0.57854(19) 1.1800(11) 0.6707(4) 0.110(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0476(3) 0.0478(3) 0.0624(4) -0.0123(3) 0.0361(3) -0.0120(3) S1 0.0412(8) 0.0289(9) 0.0455(10) -0.0046(7) 0.0248(8) -0.0059(7) S2 0.0433(8) 0.0302(8) 0.0455(9) -0.0052(7) 0.0257(7) -0.0073(7) Cl1 0.0535(10) 0.0440(10) 0.0389(9) -0.0055(8) 0.0240(8) -0.0081(8) C1 0.051(5) 0.069(6) 0.101(7) 0.005(5) 0.019(5) 0.004(4) C2 0.044(5) 0.124(10) 0.174(11) 0.005(8) 0.041(6) 0.009(6) C3 0.043(6) 0.149(13) 0.162(12) 0.053(10) 0.030(6) -0.004(7) C4 0.069(7) 0.095(9) 0.140(10) 0.019(7) 0.012(6) -0.040(6) C5 0.070(6) 0.081(7) 0.083(6) -0.007(5) 0.015(5) -0.032(5) C6 0.043(4) 0.056(5) 0.040(4) 0.005(3) 0.004(3) -0.008(4) C7 0.054(4) 0.053(4) 0.038(4) 0.003(3) 0.016(3) -0.009(3) C8 0.037(3) 0.039(4) 0.038(4) -0.001(3) 0.021(3) -0.003(3) C9 0.044(4) 0.053(5) 0.060(5) -0.020(3) 0.030(3) -0.007(3) C10 0.042(4) 0.041(4) 0.047(4) -0.012(3) 0.025(3) -0.008(3) C11 0.077(6) 0.050(5) 0.124(7) 0.020(5) 0.061(5) 0.008(5) C12 0.064(6) 0.088(7) 0.142(9) 0.031(6) 0.049(6) 0.033(5) C13 0.047(5) 0.111(8) 0.106(7) 0.007(6) 0.043(5) 0.001(5) C14 0.055(5) 0.110(8) 0.080(6) 0.016(5) 0.045(4) -0.008(5) C15 0.055(4) 0.067(5) 0.059(5) 0.009(4) 0.031(4) 0.009(4) O1 0.086(4) 0.108(6) 0.142(6) -0.081(5) 0.057(4) -0.038(4) O2 0.112(5) 0.066(5) 0.126(5) 0.031(4) 0.017(4) 0.010(4) O3 0.127(5) 0.131(6) 0.048(4) 0.024(3) 0.034(3) -0.019(4) O4 0.100(4) 0.116(6) 0.156(6) -0.047(4) 0.094(5) -0.028(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 S1 2.442(2) . ? Ag1 S2 2.445(2) . ? Ag1 Ag1 3.036(1) 5_666 ? S1 C8 1.801(6) 5_666 ? S1 C9 1.829(6) . ? S2 C8 1.790(5) . ? S2 C7 1.820(6) . ? Cl1 O3 1.366(5) . ? Cl1 O1 1.406(5) . ? Cl1 O4 1.408(5) . ? Cl1 O2 1.450(6) . ? C1 C2 1.358(11) . ? C1 C6 1.367(10) . ? C1 H1A 0.9300 . ? C2 C3 1.349(15) . ? C2 H2A 0.9300 . ? C3 C4 1.358(15) . ? C3 H3A 0.9300 . ? C4 C5 1.380(12) . ? C4 H4A 0.9300 . ? C5 C6 1.379(10) . ? C5 H5A 0.9300 . ? C6 C7 1.506(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 S1 1.801(6) 5_666 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.502(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.372(9) . ? C10 C15 1.376(9) . ? C11 C12 1.375(10) . ? C11 H11A 0.9300 . ? C12 C13 1.349(11) . ? C12 H12A 0.9300 . ? C13 C14 1.357(11) . ? C13 H13A 0.9300 . ? C14 C15 1.378(9) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? 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 S1 Ag1 S2 166.65(6) . . ? S1 Ag1 Ag1 86.82(4) . 5_666 ? S2 Ag1 Ag1 91.46(4) . 5_666 ? C8 S1 C9 98.9(3) 5_666 . ? C8 S1 Ag1 107.2(2) 5_666 . ? C9 S1 Ag1 106.4(2) . . ? C8 S2 C7 102.4(3) . . ? C8 S2 Ag1 109.2(2) . . ? C7 S2 Ag1 105.6(2) . . ? O3 Cl1 O1 112.8(4) . . ? O3 Cl1 O4 110.9(4) . . ? O1 Cl1 O4 111.8(3) . . ? O3 Cl1 O2 104.5(4) . . ? O1 Cl1 O2 107.6(4) . . ? O4 Cl1 O2 108.9(4) . . ? C2 C1 C6 121.6(9) . . ? C2 C1 H1A 119.2 . . ? C6 C1 H1A 119.2 . . ? C3 C2 C1 120.0(11) . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C2 C3 C4 119.6(10) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C3 C4 C5 121.2(10) . . ? C3 C4 H4A 119.4 . . ? C5 C4 H4A 119.4 . . ? C6 C5 C4 118.8(9) . . ? C6 C5 H5A 120.6 . . ? C4 C5 H5A 120.6 . . ? C1 C6 C5 118.7(7) . . ? C1 C6 C7 121.4(7) . . ? C5 C6 C7 120.0(7) . . ? C6 C7 S2 112.3(4) . . ? C6 C7 H7A 109.1 . . ? S2 C7 H7A 109.1 . . ? C6 C7 H7B 109.1 . . ? S2 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? S2 C8 S1 114.3(3) . 5_666 ? S2 C8 H8A 108.7 . . ? S1 C8 H8A 108.7 5_666 . ? S2 C8 H8B 108.7 . . ? S1 C8 H8B 108.7 5_666 . ? H8A C8 H8B 107.6 . . ? C10 C9 S1 112.2(4) . . ? C10 C9 H9A 109.2 . . ? S1 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? S1 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C15 117.7(6) . . ? C11 C10 C9 121.8(6) . . ? C15 C10 C9 120.5(6) . . ? C10 C11 C12 120.9(7) . . ? C10 C11 H11A 119.5 . . ? C12 C11 H11A 119.5 . . ? C13 C12 C11 120.7(8) . . ? C13 C12 H12A 119.7 . . ? C11 C12 H12A 119.7 . . ? C12 C13 C14 119.6(7) . . ? C12 C13 H13A 120.2 . . ? C14 C13 H13A 120.2 . . ? C13 C14 C15 120.3(7) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C10 C15 C14 120.8(7) . . ? C10 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? 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 S2 Ag1 S1 C8 123.1(3) . . . 5_666 ? Ag1 Ag1 S1 C8 40.26(19) 5_666 . . 5_666 ? S2 Ag1 S1 C9 -131.8(3) . . . . ? Ag1 Ag1 S1 C9 145.3(2) 5_666 . . . ? S1 Ag1 S2 C8 -68.0(3) . . . . ? Ag1 Ag1 S2 C8 14.3(2) 5_666 . . . ? S1 Ag1 S2 C7 -177.5(3) . . . . ? Ag1 Ag1 S2 C7 -95.1(2) 5_666 . . . ? C6 C1 C2 C3 1.5(15) . . . . ? C1 C2 C3 C4 -1.2(18) . . . . ? C2 C3 C4 C5 0.7(18) . . . . ? C3 C4 C5 C6 -0.5(15) . . . . ? C2 C1 C6 C5 -1.3(12) . . . . ? C2 C1 C6 C7 179.0(7) . . . . ? C4 C5 C6 C1 0.8(11) . . . . ? C4 C5 C6 C7 -179.5(7) . . . . ? C1 C6 C7 S2 -95.5(7) . . . . ? C5 C6 C7 S2 84.8(7) . . . . ? C8 S2 C7 C6 63.2(6) . . . . ? Ag1 S2 C7 C6 177.5(4) . . . . ? C7 S2 C8 S1 60.7(4) . . . 5_666 ? Ag1 S2 C8 S1 -50.9(4) . . . 5_666 ? C8 S1 C9 C10 -73.3(5) 5_666 . . . ? Ag1 S1 C9 C10 175.8(4) . . . . ? S1 C9 C10 C11 -79.5(7) . . . . ? S1 C9 C10 C15 99.8(6) . . . . ? C15 C10 C11 C12 2.5(12) . . . . ? C9 C10 C11 C12 -178.2(7) . . . . ? C10 C11 C12 C13 -2.1(14) . . . . ? C11 C12 C13 C14 1.3(16) . . . . ? C12 C13 C14 C15 -0.9(14) . . . . ? C11 C10 C15 C14 -2.2(10) . . . . ? C9 C10 C15 C14 178.5(6) . . . . ? C13 C14 C15 C10 1.4(12) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.934 _refine_diff_density_min -1.139 _refine_diff_density_rms 0.488 data_030802b _database_code_depnum_ccdc_archive 'CCDC 231509' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 Ag Cl O4 S4' _chemical_formula_weight 756.17 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(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 14.908(6) _cell_length_b 18.868(7) _cell_length_c 13.658(5) _cell_angle_alpha 90.00 _cell_angle_beta 116.710(6) _cell_angle_gamma 90.00 _cell_volume 3432(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 997 _cell_measurement_theta_min 3.3396 _cell_measurement_theta_max 22.3781 _exptl_crystal_description Mast _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.943 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7524 _exptl_absorpt_correction_T_max 0.8054 _exptl_absorpt_process_details sadabs _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 'Bruker CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19635 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.50 _reflns_number_total 7061 _reflns_number_gt 3850 _reflns_threshold_expression I>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^)+(0.0659P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7061 _refine_ls_number_parameters 497 _refine_ls_number_restraints 684 _refine_ls_R_factor_all 0.1126 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1406 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.050 _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 0.35563(3) 0.34752(2) 0.15729(3) 0.07568(19) Uani 1 1 d . A . S1 S 0.47637(9) 0.45564(6) 0.20316(9) 0.0647(3) Uani 1 1 d . A . S2 S 0.49614(9) 0.27863(6) 0.14816(9) 0.0669(3) Uani 1 1 d D . . S3 S 0.25357(9) 0.35340(6) 0.26261(9) 0.0653(3) Uani 1 1 d . . . S4 S 0.18588(9) 0.34797(7) -0.01856(9) 0.0698(3) Uani 1 1 d D . . C1 C 0.2473(4) 0.5476(3) -0.0058(4) 0.0806(14) Uani 1 1 d . . . H1A H 0.2344 0.5141 -0.0605 0.097 Uiso 1 1 calc R . . C2 C 0.1695(4) 0.5897(3) -0.0090(6) 0.1045(19) Uani 1 1 d . . . H2A H 0.1052 0.5849 -0.0663 0.125 Uiso 1 1 calc R . . C3 C 0.1876(5) 0.6377(3) 0.0714(7) 0.116(2) Uani 1 1 d . . . H3A H 0.1356 0.6659 0.0692 0.139 Uiso 1 1 calc R . . C4 C 0.2814(5) 0.6450(3) 0.1553(6) 0.110(2) Uani 1 1 d . . . H4A H 0.2929 0.6773 0.2111 0.132 Uiso 1 1 calc R . . C5 C 0.3591(4) 0.6047(3) 0.1580(5) 0.0860(16) Uani 1 1 d . . . H5A H 0.4233 0.6110 0.2148 0.103 Uiso 1 1 calc R . . C6 C 0.3433(4) 0.5550(2) 0.0773(4) 0.0642(12) Uani 1 1 d . . . C7 C 0.4278(4) 0.5117(3) 0.0811(4) 0.0746(14) Uani 1 1 d . . . H7A H 0.4807 0.5425 0.0830 0.090 Uiso 1 1 calc R . . H7B H 0.4049 0.4824 0.0160 0.090 Uiso 1 1 calc R . . C8 C 0.5792(3) 0.4124(3) 0.1907(4) 0.0736(13) Uani 1 1 d . . . H8A H 0.6158 0.4478 0.1716 0.088 Uiso 1 1 calc R A . H8B H 0.6247 0.3931 0.2617 0.088 Uiso 1 1 calc R . . C9 C 0.5488(4) 0.3536(2) 0.1071(4) 0.0693(12) Uani 1 1 d . A . H9A H 0.6070 0.3380 0.0988 0.083 Uiso 1 1 calc R . . H9B H 0.4995 0.3713 0.0368 0.083 Uiso 1 1 calc R . . C10 C 0.4394(13) 0.2219(18) 0.0269(19) 0.070(7) Uani 0.43(2) 1 d PDU A 1 H10A H 0.4037 0.1832 0.0407 0.084 Uiso 0.43(2) 1 calc PR A 1 H10B H 0.3915 0.2490 -0.0346 0.084 Uiso 0.43(2) 1 calc PR A 1 C11 C 0.5202(12) 0.1921(8) -0.0009(12) 0.090(7) Uani 0.43(2) 1 d PGDU A 1 C12 C 0.5623(15) 0.2275(7) -0.0595(15) 0.076(5) Uani 0.43(2) 1 d PGU A 1 H12A H 0.5350 0.2702 -0.0940 0.091 Uiso 0.43(2) 1 calc PR A 1 C13 C 0.6452(14) 0.1990(9) -0.0665(14) 0.104(6) Uani 0.43(2) 1 d PGU A 1 H13A H 0.6734 0.2227 -0.1057 0.125 Uiso 0.43(2) 1 calc PR A 1 C14 C 0.6860(14) 0.1352(11) -0.0149(14) 0.124(7) Uani 0.43(2) 1 d PGU A 1 H14A H 0.7415 0.1162 -0.0196 0.149 Uiso 0.43(2) 1 calc PR A 1 C15 C 0.6439(19) 0.0998(10) 0.0437(17) 0.135(7) Uani 0.43(2) 1 d PGU A 1 H15A H 0.6712 0.0571 0.0782 0.162 Uiso 0.43(2) 1 calc PR A 1 C16 C 0.5610(17) 0.1283(9) 0.0507(15) 0.104(5) Uani 0.43(2) 1 d PGU A 1 H16A H 0.5328 0.1046 0.0899 0.124 Uiso 0.43(2) 1 calc PR A 1 C10' C 0.4361(10) 0.2361(12) 0.0133(14) 0.071(6) Uani 0.57(2) 1 d PDU A 2 H10C H 0.3778 0.2095 0.0060 0.085 Uiso 0.57(2) 1 calc PR A 2 H10D H 0.4140 0.2719 -0.0438 0.085 Uiso 0.57(2) 1 calc PR A 2 C11' C 0.5104(9) 0.1869(7) 0.0008(8) 0.075(4) Uani 0.57(2) 1 d PGDU A 2 C12' C 0.5779(12) 0.2162(7) -0.0324(13) 0.099(5) Uani 0.57(2) 1 d PGU A 2 H12B H 0.5764 0.2645 -0.0461 0.119 Uiso 0.57(2) 1 calc PR A 2 C13' C 0.6475(11) 0.1731(10) -0.0453(13) 0.122(5) Uani 0.57(2) 1 d PGU A 2 H13B H 0.6926 0.1927 -0.0675 0.146 Uiso 0.57(2) 1 calc PR A 2 C14' C 0.6497(11) 0.1008(10) -0.0249(10) 0.141(7) Uani 0.57(2) 1 d PGU A 2 H14B H 0.6963 0.0720 -0.0335 0.169 Uiso 0.57(2) 1 calc PR A 2 C15' C 0.5822(14) 0.0715(7) 0.0084(9) 0.132(6) Uani 0.57(2) 1 d PGU A 2 H15B H 0.5837 0.0232 0.0220 0.159 Uiso 0.57(2) 1 calc PR A 2 C16' C 0.5126(11) 0.1146(7) 0.0212(8) 0.103(5) Uani 0.57(2) 1 d PGU A 2 H16B H 0.4675 0.0950 0.0435 0.123 Uiso 0.57(2) 1 calc PR A 2 C17 C 0.0845(5) 0.5103(3) 0.2323(4) 0.0871(16) Uani 1 1 d . A . H17A H 0.0786 0.5214 0.1633 0.105 Uiso 1 1 calc R . . C18 C 0.0104(5) 0.5322(3) 0.2611(6) 0.111(2) Uani 1 1 d . . . H18A H -0.0445 0.5581 0.2120 0.134 Uiso 1 1 calc R . . C19 C 0.0191(6) 0.5157(4) 0.3607(7) 0.122(2) Uani 1 1 d . . . H19A H -0.0311 0.5292 0.3795 0.146 Uiso 1 1 calc R . . C20 C 0.1001(6) 0.4798(4) 0.4340(6) 0.115(2) Uani 1 1 d . . . H20A H 0.1067 0.4705 0.5038 0.138 Uiso 1 1 calc R . . C21 C 0.1723(5) 0.4572(3) 0.4054(4) 0.0848(16) Uani 1 1 d . A . H21A H 0.2265 0.4312 0.4553 0.102 Uiso 1 1 calc R . . C22 C 0.1659(4) 0.4725(2) 0.3042(4) 0.0638(12) Uani 1 1 d . . . C23 C 0.2462(4) 0.4490(2) 0.2747(4) 0.0721(13) Uani 1 1 d . A . H23A H 0.3104 0.4661 0.3301 0.086 Uiso 1 1 calc R . . H23B H 0.2344 0.4707 0.2056 0.086 Uiso 1 1 calc R . . C24 C 0.1310(3) 0.3341(2) 0.1529(4) 0.0667(12) Uani 1 1 d . A . H24A H 0.1252 0.2832 0.1423 0.080 Uiso 1 1 calc R . . H24B H 0.0810 0.3487 0.1758 0.080 Uiso 1 1 calc R . . C25 C 0.1062(4) 0.3686(2) 0.0435(4) 0.0690(13) Uani 1 1 d . A . H25A H 0.1070 0.4196 0.0531 0.083 Uiso 1 1 calc R . . H25B H 0.0381 0.3554 -0.0074 0.083 Uiso 1 1 calc R . . C26 C 0.1616(9) 0.2555(6) -0.0616(18) 0.063(5) Uani 0.51(2) 1 d PDU A 1 H26A H 0.1843 0.2464 -0.1168 0.076 Uiso 0.51(2) 1 calc PR A 1 H26B H 0.1993 0.2250 0.0006 0.076 Uiso 0.51(2) 1 calc PR A 1 C27 C 0.0492(9) 0.2380(9) -0.1087(16) 0.083(5) Uani 0.51(2) 1 d PGDU A 1 C28 C 0.0092(10) 0.1936(8) -0.0571(15) 0.110(6) Uani 0.51(2) 1 d PGU A 1 H28A H 0.0492 0.1782 0.0141 0.132 Uiso 0.51(2) 1 calc PR A 1 C29 C -0.0904(10) 0.1721(8) -0.1121(18) 0.134(7) Uani 0.51(2) 1 d PGU A 1 H29A H -0.1172 0.1424 -0.0776 0.161 Uiso 0.51(2) 1 calc PR A 1 C30 C -0.1501(7) 0.1952(10) -0.2185(17) 0.135(8) Uani 0.51(2) 1 d PGU A 1 H30A H -0.2168 0.1808 -0.2553 0.162 Uiso 0.51(2) 1 calc PR A 1 C31 C -0.1101(12) 0.2397(11) -0.2701(14) 0.130(7) Uani 0.51(2) 1 d PGU A 1 H31A H -0.1501 0.2551 -0.3413 0.156 Uiso 0.51(2) 1 calc PR A 1 C32 C -0.0104(13) 0.2611(10) -0.2151(16) 0.101(5) Uani 0.51(2) 1 d PGU A 1 H32A H 0.0163 0.2908 -0.2496 0.122 Uiso 0.51(2) 1 calc PR A 1 C26' C 0.1554(13) 0.2541(7) -0.0413(19) 0.082(6) Uani 0.49(2) 1 d PDU A 2 H26C H 0.2038 0.2306 -0.0594 0.099 Uiso 0.49(2) 1 calc PR A 2 H26D H 0.1597 0.2331 0.0255 0.099 Uiso 0.49(2) 1 calc PR A 2 C27' C 0.0492(9) 0.2428(9) -0.1346(13) 0.078(5) Uani 0.49(2) 1 d PGDU A 2 C28' C -0.0096(12) 0.1970(9) -0.1079(14) 0.105(5) Uani 0.49(2) 1 d PGU A 2 H28B H 0.0186 0.1727 -0.0417 0.126 Uiso 0.49(2) 1 calc PR A 2 C29' C -0.1104(11) 0.1876(10) -0.1803(17) 0.134(7) Uani 0.49(2) 1 d PGU A 2 H29B H -0.1497 0.1570 -0.1625 0.161 Uiso 0.49(2) 1 calc PR A 2 C30' C -0.1525(8) 0.2240(10) -0.2794(16) 0.131(7) Uani 0.49(2) 1 d PGU A 2 H30B H -0.2199 0.2177 -0.3278 0.158 Uiso 0.49(2) 1 calc PR A 2 C31' C -0.0937(11) 0.2698(10) -0.3060(12) 0.109(6) Uani 0.49(2) 1 d PGU A 2 H31B H -0.1219 0.2942 -0.3723 0.131 Uiso 0.49(2) 1 calc PR A 2 C32' C 0.0071(11) 0.2792(9) -0.2336(14) 0.090(5) Uani 0.49(2) 1 d PGU A 2 H32B H 0.0464 0.3099 -0.2515 0.108 Uiso 0.49(2) 1 calc PR A 2 Cl1 Cl 0.29506(10) 0.37541(7) 0.74271(11) 0.0797(4) Uani 1 1 d D . . O1 O 0.3623(9) 0.3768(7) 0.8530(6) 0.182(6) Uani 0.678(13) 1 d PDU B 1 O2 O 0.2558(8) 0.4449(4) 0.7167(11) 0.187(5) Uani 0.678(13) 1 d PDU B 1 O3 O 0.2207(9) 0.3270(6) 0.7261(11) 0.178(6) Uani 0.678(13) 1 d PDU B 1 O4 O 0.3436(9) 0.3582(8) 0.6809(10) 0.192(6) Uani 0.678(13) 1 d PDU B 1 O1' O 0.3400(19) 0.3076(8) 0.759(2) 0.240(14) Uani 0.322(13) 1 d PDU B 2 O2' O 0.3294(14) 0.4142(11) 0.8400(12) 0.124(8) Uani 0.322(13) 1 d PDU B 2 O3' O 0.1894(7) 0.3676(12) 0.6943(17) 0.155(10) Uani 0.322(13) 1 d PDU B 2 O4' O 0.3190(18) 0.4115(14) 0.6669(12) 0.176(12) Uani 0.322(13) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0554(3) 0.0911(3) 0.0854(3) -0.0050(2) 0.0359(2) -0.00340(19) S1 0.0636(8) 0.0646(7) 0.0670(7) 0.0017(5) 0.0305(6) 0.0004(6) S2 0.0614(8) 0.0663(8) 0.0633(7) 0.0003(5) 0.0194(6) 0.0090(6) S3 0.0635(7) 0.0786(8) 0.0564(7) 0.0094(5) 0.0291(6) 0.0041(6) S4 0.0626(8) 0.0859(9) 0.0539(7) -0.0009(6) 0.0198(6) 0.0035(6) C1 0.083(4) 0.073(3) 0.087(4) 0.004(3) 0.039(3) 0.001(3) C2 0.059(4) 0.094(4) 0.134(5) -0.006(4) 0.020(3) 0.005(3) C3 0.077(5) 0.078(4) 0.189(8) -0.010(4) 0.057(5) 0.013(3) C4 0.085(5) 0.089(5) 0.148(6) -0.036(4) 0.046(4) 0.001(4) C5 0.061(3) 0.079(4) 0.110(4) -0.016(3) 0.031(3) 0.004(3) C6 0.063(3) 0.061(3) 0.074(3) 0.010(2) 0.034(3) 0.003(2) C7 0.083(4) 0.076(3) 0.078(3) 0.013(2) 0.048(3) 0.013(3) C8 0.054(3) 0.075(3) 0.084(3) 0.005(3) 0.024(2) -0.003(2) C9 0.052(3) 0.082(3) 0.076(3) -0.004(2) 0.031(2) 0.002(2) C10 0.076(11) 0.055(11) 0.062(10) 0.009(9) 0.016(8) 0.022(8) C11 0.104(12) 0.059(10) 0.072(12) 0.000(10) 0.008(10) 0.009(10) C12 0.094(10) 0.081(9) 0.040(8) 0.016(6) 0.020(7) 0.015(8) C13 0.135(12) 0.106(12) 0.068(10) 0.014(8) 0.042(9) 0.036(10) C14 0.171(15) 0.116(15) 0.090(11) 0.008(10) 0.064(11) 0.073(12) C15 0.173(16) 0.142(13) 0.101(12) 0.057(11) 0.071(12) 0.080(12) C16 0.121(13) 0.101(11) 0.092(11) 0.029(9) 0.051(10) 0.027(10) C10' 0.072(8) 0.057(10) 0.063(8) 0.000(7) 0.011(6) -0.006(6) C11' 0.086(8) 0.086(9) 0.038(6) -0.004(7) 0.015(6) 0.022(7) C12' 0.129(11) 0.090(9) 0.063(9) -0.005(7) 0.029(8) 0.031(8) C13' 0.128(10) 0.156(13) 0.087(9) -0.005(9) 0.053(8) 0.060(9) C14' 0.158(13) 0.154(15) 0.076(8) -0.001(9) 0.022(9) 0.094(11) C15' 0.148(13) 0.126(11) 0.071(7) -0.001(7) 0.002(8) 0.077(10) C16' 0.103(10) 0.098(9) 0.058(6) -0.008(6) -0.006(6) 0.024(8) C17 0.112(5) 0.078(4) 0.067(3) -0.001(3) 0.036(3) 0.008(3) C18 0.107(5) 0.105(5) 0.104(5) -0.008(4) 0.032(4) 0.036(4) C19 0.131(7) 0.132(6) 0.132(6) -0.002(5) 0.086(6) 0.017(5) C20 0.154(7) 0.113(5) 0.119(5) 0.018(4) 0.097(6) 0.016(5) C21 0.110(5) 0.081(4) 0.080(4) 0.014(3) 0.057(3) 0.012(3) C22 0.080(3) 0.054(3) 0.057(3) -0.009(2) 0.031(3) -0.013(2) C23 0.073(3) 0.078(3) 0.069(3) -0.011(2) 0.035(3) -0.021(3) C24 0.057(3) 0.063(3) 0.091(4) -0.016(2) 0.042(3) -0.010(2) C25 0.056(3) 0.067(3) 0.067(3) -0.011(2) 0.013(2) 0.009(2) C26 0.054(8) 0.075(8) 0.049(7) -0.008(5) 0.014(6) 0.021(6) C27 0.067(9) 0.085(9) 0.086(9) -0.037(7) 0.026(7) 0.012(8) C28 0.085(9) 0.090(9) 0.125(14) -0.047(9) 0.021(9) -0.007(8) C29 0.092(11) 0.117(11) 0.152(15) -0.052(10) 0.019(11) -0.002(9) C30 0.062(9) 0.142(13) 0.143(16) -0.042(12) -0.006(10) -0.002(9) C31 0.066(10) 0.152(15) 0.121(13) -0.037(10) -0.004(9) -0.001(10) C32 0.074(9) 0.122(11) 0.100(11) -0.029(9) 0.032(8) -0.004(8) C26' 0.061(9) 0.119(12) 0.076(11) -0.020(8) 0.038(8) 0.019(8) C27' 0.062(9) 0.090(9) 0.073(9) -0.033(7) 0.022(7) 0.006(7) C28' 0.085(10) 0.107(10) 0.105(12) -0.039(9) 0.027(8) -0.020(8) C29' 0.075(11) 0.156(12) 0.135(15) -0.034(11) 0.015(11) -0.034(10) C30' 0.061(9) 0.171(15) 0.133(13) -0.046(11) 0.018(9) -0.027(10) C31' 0.073(9) 0.125(13) 0.098(10) -0.040(9) 0.009(8) -0.009(8) C32' 0.062(8) 0.116(11) 0.072(8) -0.039(7) 0.011(7) -0.001(7) Cl1 0.0757(9) 0.0775(9) 0.0705(9) 0.0002(7) 0.0192(7) -0.0059(7) O1 0.180(10) 0.201(13) 0.079(6) 0.016(6) -0.018(5) 0.020(9) O2 0.177(10) 0.109(7) 0.231(12) 0.041(7) 0.052(8) 0.034(6) O3 0.181(12) 0.109(9) 0.281(14) -0.077(8) 0.137(11) -0.080(8) O4 0.228(13) 0.210(15) 0.211(13) -0.016(10) 0.161(11) 0.007(10) O1' 0.32(3) 0.122(16) 0.24(2) 0.042(15) 0.09(2) 0.123(18) O2' 0.138(16) 0.115(14) 0.136(17) -0.067(12) 0.077(14) -0.062(12) O3' 0.061(10) 0.16(2) 0.191(18) -0.057(16) 0.007(10) 0.000(11) O4' 0.21(2) 0.20(2) 0.103(13) 0.066(15) 0.060(13) -0.03(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 S2 2.515(1) . ? Ag1 S3 2.523(1) . ? Ag1 S4 2.590(1) . ? Ag1 S1 2.604(1) . ? S1 C8 1.810(5) . ? S1 C7 1.827(5) . ? S2 C9 1.824(5) . ? S2 C10 1.83(1) . ? S2 C10' 1.83(1) . ? S3 C24 1.804(5) . ? S3 C23 1.819(5) . ? S4 C25 1.785(5) . ? S4 C26' 1.82(1) . ? S4 C26 1.83(1) . ? C1 C6 1.377(7) . ? C1 C2 1.390(8) . ? C1 H1A 0.9300 . ? C2 C3 1.355(8) . ? C2 H2A 0.9300 . ? C3 C4 1.358(9) . ? C3 H3A 0.9300 . ? C4 C5 1.372(7) . ? C4 H4A 0.9300 . ? C5 C6 1.384(7) . ? C5 H5A 0.9300 . ? C6 C7 1.483(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.508(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.523(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 H12A 0.9300 . ? C13 C14 1.3900 . ? C13 H13A 0.9300 . ? C14 C15 1.3900 . ? C14 H14A 0.9300 . ? C15 C16 1.3900 . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C10' C11' 1.512(9) . ? C10' H10C 0.9700 . ? C10' H10D 0.9700 . ? C11' C12' 1.3900 . ? C11' C16' 1.3900 . ? C12' C13' 1.3900 . ? C12' H12B 0.9300 . ? C13' C14' 1.3900 . ? C13' H13B 0.9300 . ? C14' C15' 1.3900 . ? C14' H14B 0.9300 . ? C15' C16' 1.3900 . ? C15' H15B 0.9300 . ? C16' H16B 0.9300 . ? C17 C22 1.369(7) . ? C17 C18 1.391(8) . ? C17 H17A 0.9300 . ? C18 C19 1.343(8) . ? C18 H18A 0.9300 . ? C19 C20 1.354(9) . ? C19 H19A 0.9300 . ? C20 C21 1.367(8) . ? C20 H20A 0.9300 . ? C21 C22 1.372(6) . ? C21 H21A 0.9300 . ? C22 C23 1.492(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.515(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.536(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.3900 . ? C27 C32 1.3900 . ? C28 C29 1.3900 . ? C28 H28A 0.9300 . ? C29 C30 1.3900 . ? C29 H29A 0.9300 . ? C30 C31 1.3900 . ? C30 H30A 0.9300 . ? C31 C32 1.3900 . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C26' C27' 1.537(9) . ? C26' H26C 0.9700 . ? C26' H26D 0.9700 . ? C27' C28' 1.3900 . ? C27' C32' 1.3900 . ? C28' C29' 1.3900 . ? C28' H28B 0.9300 . ? C29' C30' 1.3900 . ? C29' H29B 0.9300 . ? C30' C31' 1.3900 . ? C30' H30B 0.9300 . ? C31' C32' 1.3900 . ? C31' H31B 0.9300 . ? C32' H32B 0.9300 . ? Cl1 O3 1.374(7) . ? Cl1 O4 1.376(7) . ? Cl1 O1 1.384(7) . ? Cl1 O2' 1.397(9) . ? Cl1 O4' 1.413(9) . ? Cl1 O1' 1.415(8) . ? Cl1 O2 1.415(6) . ? Cl1 O3' 1.416(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 S2 Ag1 S3 141.27(4) . . ? S2 Ag1 S4 116.36(5) . . ? S3 Ag1 S4 86.58(5) . . ? S2 Ag1 S1 85.17(5) . . ? S3 Ag1 S1 110.93(4) . . ? S4 Ag1 S1 120.14(4) . . ? C8 S1 C7 100.4(2) . . ? C8 S1 Ag1 98.5(2) . . ? C7 S1 Ag1 106.7(2) . . ? C9 S2 C10 105(1) . . ? C9 S2 C10' 96.5(9) . . ? C10 S2 C10' 10(2) . . ? C9 S2 Ag1 95.60(15) . . ? C10 S2 Ag1 106.9(5) . . ? C10' S2 Ag1 103.6(4) . . ? C24 S3 C23 101.3(2) . . ? C24 S3 Ag1 99.35(15) . . ? C23 S3 Ag1 99.89(15) . . ? C25 S4 C26' 97.1(10) . . ? C25 S4 C26 106.5(7) . . ? C26' S4 C26 10.4(17) . . ? C25 S4 Ag1 98.15(15) . . ? C26' S4 Ag1 102.7(5) . . ? C26 S4 Ag1 105.4(5) . . ? C6 C1 C2 120.8(5) . . ? C6 C1 H1A 119.6 . . ? C2 C1 H1A 119.6 . . ? C3 C2 C1 119.8(6) . . ? C3 C2 H2A 120.1 . . ? C1 C2 H2A 120.1 . . ? C2 C3 C4 120.4(6) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C3 C4 C5 120.2(6) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C4 C5 C6 120.9(5) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C1 C6 C5 117.8(5) . . ? C1 C6 C7 121.7(5) . . ? C5 C6 C7 120.5(5) . . ? C6 C7 S1 109.4(3) . . ? C6 C7 H7A 109.8 . . ? S1 C7 H7A 109.8 . . ? C6 C7 H7B 109.8 . . ? S1 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? C9 C8 S1 115.1(3) . . ? C9 C8 H8A 108.5 . . ? S1 C8 H8A 108.5 . . ? C9 C8 H8B 108.5 . . ? S1 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C8 C9 S2 111.2(3) . . ? C8 C9 H9A 109.4 . . ? S2 C9 H9A 109.4 . . ? C8 C9 H9B 109.4 . . ? S2 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C11 C10 S2 110.2(10) . . ? C11 C10 H10A 109.6 . . ? S2 C10 H10A 109.6 . . ? C11 C10 H10B 109.6 . . ? S2 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C12 C11 C16 120.0 . . ? C12 C11 C10 125.4(18) . . ? C16 C11 C10 114.1(18) . . ? C13 C12 C11 120.0 . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C11 120.0 . . ? C15 C16 H16A 120.0 . . ? C11 C16 H16A 120.0 . . ? C11' C10' S2 109.3(8) . . ? C11' C10' H10C 109.8 . . ? S2 C10' H10C 109.8 . . ? C11' C10' H10D 109.8 . . ? S2 C10' H10D 109.8 . . ? H10C C10' H10D 108.3 . . ? C12' C11' C16' 120.0 . . ? C12' C11' C10' 117.8(14) . . ? C16' C11' C10' 122.2(13) . . ? C11' C12' C13' 120.0 . . ? C11' C12' H12B 120.0 . . ? C13' C12' H12B 120.0 . . ? C14' C13' C12' 120.0 . . ? C14' C13' H13B 120.0 . . ? C12' C13' H13B 120.0 . . ? C15' C14' C13' 120.0 . . ? C15' C14' H14B 120.0 . . ? C13' C14' H14B 120.0 . . ? C14' C15' C16' 120.0 . . ? C14' C15' H15B 120.0 . . ? C16' C15' H15B 120.0 . . ? C15' C16' C11' 120.0 . . ? C15' C16' H16B 120.0 . . ? C11' C16' H16B 120.0 . . ? C22 C17 C18 120.9(5) . . ? C22 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C19 C18 C17 119.3(6) . . ? C19 C18 H18A 120.4 . . ? C17 C18 H18A 120.4 . . ? C18 C19 C20 120.9(6) . . ? C18 C19 H19A 119.6 . . ? C20 C19 H19A 119.6 . . ? C19 C20 C21 120.0(6) . . ? C19 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? C20 C21 C22 121.0(6) . . ? C20 C21 H21A 119.5 . . ? C22 C21 H21A 119.5 . . ? C17 C22 C21 118.0(5) . . ? C17 C22 C23 121.4(4) . . ? C21 C22 C23 120.6(5) . . ? C22 C23 S3 114.0(3) . . ? C22 C23 H23A 108.7 . . ? S3 C23 H23A 108.7 . . ? C22 C23 H23B 108.7 . . ? S3 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C25 C24 S3 116.1(3) . . ? C25 C24 H24A 108.3 . . ? S3 C24 H24A 108.3 . . ? C25 C24 H24B 108.3 . . ? S3 C24 H24B 108.3 . . ? H24A C24 H24B 107.4 . . ? C24 C25 S4 117.0(3) . . ? C24 C25 H25A 108.0 . . ? S4 C25 H25A 108.0 . . ? C24 C25 H25B 108.0 . . ? S4 C25 H25B 108.0 . . ? H25A C25 H25B 107.3 . . ? C27 C26 S4 111.1(9) . . ? C27 C26 H26A 109.4 . . ? S4 C26 H26A 109.4 . . ? C27 C26 H26B 109.4 . . ? S4 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C32 120.0 . . ? C28 C27 C26 123.6(14) . . ? C32 C27 C26 115.8(14) . . ? C27 C28 C29 120.0 . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C29 C30 C31 120.0 . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? C32 C31 C30 120.0 . . ? C32 C31 H31A 120.0 . . ? C30 C31 H31A 120.0 . . ? C31 C32 C27 120.0 . . ? C31 C32 H32A 120.0 . . ? C27 C32 H32A 120.0 . . ? C27' C26' S4 111.2(10) . . ? C27' C26' H26C 109.4 . . ? S4 C26' H26C 109.4 . . ? C27' C26' H26D 109.4 . . ? S4 C26' H26D 109.4 . . ? H26C C26' H26D 108.0 . . ? C28' C27' C32' 120.0 . . ? C28' C27' C26' 113.8(14) . . ? C32' C27' C26' 125.8(13) . . ? C27' C28' C29' 120.0 . . ? C27' C28' H28B 120.0 . . ? C29' C28' H28B 120.0 . . ? C28' C29' C30' 120.0 . . ? C28' C29' H29B 120.0 . . ? C30' C29' H29B 120.0 . . ? C31' C30' C29' 120.0 . . ? C31' C30' H30B 120.0 . . ? C29' C30' H30B 120.0 . . ? C32' C31' C30' 120.0 . . ? C32' C31' H31B 120.0 . . ? C30' C31' H31B 120.0 . . ? C31' C32' C27' 120.0 . . ? C31' C32' H32B 120.0 . . ? C27' C32' H32B 120.0 . . ? O3 Cl1 O4 110.5(6) . . ? O3 Cl1 O1 109.1(7) . . ? O4 Cl1 O1 110.4(7) . . ? O3 Cl1 O2' 115.3(9) . . ? O4 Cl1 O2' 129.7(9) . . ? O1 Cl1 O2' 34.8(8) . . ? O3 Cl1 O4' 130.6(10) . . ? O4 Cl1 O4' 44.6(9) . . ? O1 Cl1 O4' 119.4(11) . . ? O2' Cl1 O4' 109.9(8) . . ? O3 Cl1 O1' 73.4(10) . . ? O4 Cl1 O1' 62.9(10) . . ? O1 Cl1 O1' 77.5(9) . . ? O2' Cl1 O1' 112.1(8) . . ? O4' Cl1 O1' 107.3(9) . . ? O3 Cl1 O2 111.3(6) . . ? O4 Cl1 O2 109.7(6) . . ? O1 Cl1 O2 105.7(5) . . ? O2' Cl1 O2 71.8(9) . . ? O4' Cl1 O2 65.2(10) . . ? O1' Cl1 O2 172.5(11) . . ? O3 Cl1 O3' 37.6(8) . . ? O4 Cl1 O3' 118.1(11) . . ? O1 Cl1 O3' 128.3(11) . . ? O2' Cl1 O3' 110.7(8) . . ? O4' Cl1 O3' 107.6(8) . . ? O1' Cl1 O3' 109.1(9) . . ? O2 Cl1 O3' 74.4(9) . . ? 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 S2 Ag1 S1 C8 3.20(16) . . . . ? S3 Ag1 S1 C8 146.89(16) . . . . ? S4 Ag1 S1 C8 -114.60(17) . . . . ? S2 Ag1 S1 C7 106.74(16) . . . . ? S3 Ag1 S1 C7 -109.57(16) . . . . ? S4 Ag1 S1 C7 -11.05(17) . . . . ? S3 Ag1 S2 C9 -146.33(16) . . . . ? S4 Ag1 S2 C9 92.92(16) . . . . ? S1 Ag1 S2 C9 -28.45(16) . . . . ? S3 Ag1 S2 C10 105.8(13) . . . . ? S4 Ag1 S2 C10 -15.0(13) . . . . ? S1 Ag1 S2 C10 -136.3(13) . . . . ? S3 Ag1 S2 C10' 115.6(9) . . . . ? S4 Ag1 S2 C10' -5.2(9) . . . . ? S1 Ag1 S2 C10' -126.6(9) . . . . ? S2 Ag1 S3 C24 -117.25(16) . . . . ? S4 Ag1 S3 C24 12.28(15) . . . . ? S1 Ag1 S3 C24 133.32(15) . . . . ? S2 Ag1 S3 C23 139.45(17) . . . . ? S4 Ag1 S3 C23 -91.03(17) . . . . ? S1 Ag1 S3 C23 30.01(17) . . . . ? S2 Ag1 S4 C25 157.59(16) . . . . ? S3 Ag1 S4 C25 10.19(17) . . . . ? S1 Ag1 S4 C25 -102.09(17) . . . . ? S2 Ag1 S4 C26' 58.3(10) . . . . ? S3 Ag1 S4 C26' -89.1(10) . . . . ? S1 Ag1 S4 C26' 158.6(10) . . . . ? S2 Ag1 S4 C26 47.9(8) . . . . ? S3 Ag1 S4 C26 -99.5(8) . . . . ? S1 Ag1 S4 C26 148.2(8) . . . . ? C6 C1 C2 C3 -1.2(9) . . . . ? C1 C2 C3 C4 0.0(11) . . . . ? C2 C3 C4 C5 1.4(11) . . . . ? C3 C4 C5 C6 -1.6(10) . . . . ? C2 C1 C6 C5 1.0(7) . . . . ? C2 C1 C6 C7 -178.7(5) . . . . ? C4 C5 C6 C1 0.4(8) . . . . ? C4 C5 C6 C7 -179.9(5) . . . . ? C1 C6 C7 S1 -116.5(4) . . . . ? C5 C6 C7 S1 63.8(5) . . . . ? C8 S1 C7 C6 -177.8(4) . . . . ? Ag1 S1 C7 C6 80.0(4) . . . . ? C7 S1 C8 C9 -76.9(4) . . . . ? Ag1 S1 C8 C9 31.9(4) . . . . ? S1 C8 C9 S2 -66.8(4) . . . . ? C10 S2 C9 C8 168.1(7) . . . . ? C10' S2 C9 C8 163.3(5) . . . . ? Ag1 S2 C9 C8 58.8(3) . . . . ? C9 S2 C10 C11 65(2) . . . . ? C10' S2 C10 C11 94(6) . . . . ? Ag1 S2 C10 C11 166.1(18) . . . . ? S2 C10 C11 C12 -82(2) . . . . ? S2 C10 C11 C16 89(2) . . . . ? C16 C11 C12 C13 0.0 . . . . ? C10 C11 C12 C13 170.9(13) . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C11 0.0 . . . . ? C12 C11 C16 C15 0.0 . . . . ? C10 C11 C16 C15 -171.9(11) . . . . ? C9 S2 C10' C11' 87.9(16) . . . . ? C10 S2 C10' C11' -64(5) . . . . ? Ag1 S2 C10' C11' -174.7(14) . . . . ? S2 C10' C11' C12' -83.3(15) . . . . ? S2 C10' C11' C16' 96.8(13) . . . . ? C16' C11' C12' C13' 0.0 . . . . ? C10' C11' C12' C13' -179.9(9) . . . . ? C11' C12' C13' C14' 0.0 . . . . ? C12' C13' C14' C15' 0.0 . . . . ? C13' C14' C15' C16' 0.0 . . . . ? C14' C15' C16' C11' 0.0 . . . . ? C12' C11' C16' C15' 0.0 . . . . ? C10' C11' C16' C15' 179.9(9) . . . . ? C22 C17 C18 C19 -0.3(10) . . . . ? C17 C18 C19 C20 1.8(11) . . . . ? C18 C19 C20 C21 -2.8(12) . . . . ? C19 C20 C21 C22 2.2(10) . . . . ? C18 C17 C22 C21 -0.2(8) . . . . ? C18 C17 C22 C23 -179.6(5) . . . . ? C20 C21 C22 C17 -0.8(8) . . . . ? C20 C21 C22 C23 178.6(5) . . . . ? C17 C22 C23 S3 -113.3(5) . . . . ? C21 C22 C23 S3 67.3(5) . . . . ? C24 S3 C23 C22 61.2(4) . . . . ? Ag1 S3 C23 C22 162.9(3) . . . . ? C23 S3 C24 C25 61.5(4) . . . . ? Ag1 S3 C24 C25 -40.7(3) . . . . ? S3 C24 C25 S4 59.7(4) . . . . ? C26' S4 C25 C24 64.9(6) . . . . ? C26 S4 C25 C24 69.7(7) . . . . ? Ag1 S4 C25 C24 -39.1(4) . . . . ? C25 S4 C26 C27 39.5(17) . . . . ? C26' S4 C26 C27 67(4) . . . . ? Ag1 S4 C26 C27 143.1(14) . . . . ? S4 C26 C27 C28 -111.3(14) . . . . ? S4 C26 C27 C32 77.8(17) . . . . ? C32 C27 C28 C29 0.0 . . . . ? C26 C27 C28 C29 -170.5(16) . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C27 0.0 . . . . ? C28 C27 C32 C31 0.0 . . . . ? C26 C27 C32 C31 171.3(14) . . . . ? C25 S4 C26' C27' 72.5(19) . . . . ? C26 S4 C26' C27' -81(5) . . . . ? Ag1 S4 C26' C27' 172.6(16) . . . . ? S4 C26' C27' C28' -130.4(15) . . . . ? S4 C26' C27' C32' 43(2) . . . . ? C32' C27' C28' C29' 0.0 . . . . ? C26' C27' C28' C29' 173.4(15) . . . . ? C27' C28' C29' C30' 0.0 . . . . ? C28' C29' C30' C31' 0.0 . . . . ? C29' C30' C31' C32' 0.0 . . . . ? C30' C31' C32' C27' 0.0 . . . . ? C28' C27' C32' C31' 0.0 . . . . ? C26' C27' C32' C31' -172.5(18) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.601 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.104 data_167 _database_code_depnum_ccdc_archive 'CCDC 231510' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H60 Ag2 Cl2 O8 S6' _chemical_formula_weight 1279.99 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 15.625(3) _cell_length_b 15.625(3) _cell_length_c 39.55(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8362(4) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 770 _cell_measurement_theta_min 3.0308 _cell_measurement_theta_max 25.7159 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour COLOrLESS _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3924 _exptl_absorpt_coefficient_mu 1.073 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8140 _exptl_absorpt_correction_T_max 0.8303 _exptl_absorpt_process_details SADABS _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 'Bruker CCD AREA DETECTOR' _diffrn_measurement_method 'PHI AND OMEGA SCANS' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11372 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.50 _reflns_number_total 1713 _reflns_number_gt 1255 _reflns_threshold_expression I>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^)+(0.0805P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1713 _refine_ls_number_parameters 132 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1230 _refine_ls_wR_factor_gt 0.1141 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.123 _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 1.0000 1.0000 0.406506(15) 0.0456(2) Uani 1 3 d S . . S1 S 0.82121(7) 0.87050(7) 0.40958(3) 0.0407(3) Uani 1 1 d . . . C1 C 0.8244(4) 1.0004(4) 0.33182(14) 0.0686(14) Uani 1 1 d . . . H1 H 0.8699 0.9857 0.3222 0.082 Uiso 1 1 calc R . . C2 C 0.8195(6) 1.0825(5) 0.32075(16) 0.0876(19) Uani 1 1 d . . . H2 H 0.8610 1.1217 0.3035 0.105 Uiso 1 1 calc R . . C3 C 0.7557(6) 1.1056(5) 0.33468(18) 0.087(2) Uani 1 1 d . . . H3 H 0.7540 1.1613 0.3274 0.104 Uiso 1 1 calc R . . C4 C 0.6922(4) 1.0465(5) 0.35999(16) 0.0758(17) Uani 1 1 d . . . H4 H 0.6476 1.0624 0.3696 0.091 Uiso 1 1 calc R . . C5 C 0.6953(4) 0.9643(4) 0.37095(13) 0.0633(13) Uani 1 1 d . . . H5 H 0.6524 0.9245 0.3878 0.076 Uiso 1 1 calc R . . C6 C 0.7621(4) 0.9411(3) 0.35690(11) 0.0510(12) Uani 1 1 d . . . C7 C 0.7649(4) 0.8506(4) 0.36790(13) 0.0638(14) Uani 1 1 d . . . H7A H 0.8027 0.8361 0.3518 0.077 Uiso 1 1 calc R . . H7B H 0.6983 0.7944 0.3686 0.077 Uiso 1 1 calc R . . C8 C 0.8275(3) 0.7584(3) 0.41397(11) 0.0468(10) Uani 1 1 d . . . H8A H 0.8619 0.7519 0.3946 0.056 Uiso 1 1 calc R . . H8B H 0.8656 0.7635 0.4340 0.056 Uiso 1 1 calc R . . C9 C 0.7262(4) 0.6667 0.4167 0.0518(15) Uani 1 2 d S . . H9A H 0.6922 0.6716 0.4364 0.062 Uiso 0.50 1 calc PR . . H9B H 0.6872 0.6617 0.3969 0.062 Uiso 0.50 1 calc PR . . Cl1 Cl 1.0000 1.0000 0.5000 0.0482(6) Uani 1 6 d SDU . . O2 O 0.9037(4) 0.9467(15) 0.5106(3) 0.191(7) Uani 0.50 1 d PDU . . O1 O 1.0000 1.0000 0.4627(2) 0.494(14) Uani 0.50 3 d SPDU . . Cl2 Cl 0.6667 0.2915(7) 0.5833 0.141(5) Uani 0.33 2 d SPDU . . O5 O 0.6407(14) 0.326(2) 0.5534(3) 0.109(7) Uani 0.33 1 d PDU . . O6 O 0.7730(7) 0.3333 0.5833 0.191(12) Uani 0.33 2 d SPDU . . O7 O 0.6179(13) 0.1857(9) 0.5826(10) 0.161(17) Uani 0.17 1 d PDU . . 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 0.0409(3) 0.0409(3) 0.0550(4) 0.000 0.000 0.02045(14) S1 0.0393(6) 0.0346(6) 0.0468(6) -0.0031(4) -0.0064(4) 0.0174(5) C1 0.065(3) 0.067(3) 0.064(3) -0.006(3) -0.013(3) 0.026(3) C2 0.100(5) 0.068(4) 0.074(4) 0.013(3) -0.010(4) 0.027(4) C3 0.110(5) 0.066(4) 0.093(4) -0.003(3) -0.045(4) 0.050(4) C4 0.073(4) 0.082(4) 0.087(4) -0.031(3) -0.038(3) 0.049(3) C5 0.060(3) 0.059(3) 0.068(3) -0.007(2) -0.020(2) 0.027(3) C6 0.055(3) 0.044(3) 0.052(3) -0.010(2) -0.026(2) 0.023(2) C7 0.076(4) 0.047(3) 0.067(3) -0.013(2) -0.029(3) 0.031(3) C8 0.046(2) 0.033(2) 0.060(3) 0.0077(19) 0.001(2) 0.019(2) C9 0.044(3) 0.037(3) 0.072(4) 0.001(3) 0.0007(15) 0.0183(16) Cl1 0.0563(10) 0.0563(10) 0.0320(12) 0.000 0.000 0.0281(5) O2 0.154(10) 0.195(11) 0.200(12) 0.004(9) 0.045(8) 0.069(8) O1 0.495(13) 0.495(13) 0.494(19) 0.000 0.000 0.247(7) Cl2 0.164(7) 0.178(8) 0.077(5) -0.004(3) -0.008(6) 0.082(3) O5 0.109(12) 0.137(10) 0.100(8) -0.008(10) -0.008(7) 0.075(8) O6 0.183(14) 0.194(14) 0.200(16) 0.000(10) 0.000(5) 0.097(7) O7 0.166(19) 0.155(19) 0.149(19) 0.004(11) 0.000(11) 0.071(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 Ag1 O1 2.22(1) . ? Ag1 S1 2.502(1) . ? Ag1 S1 2.502(1) 2_765 ? Ag1 S1 2.502(1) 3_675 ? S1 C8 1.811(4) . ? S1 C7 1.821(5) . ? C1 C6 1.374(7) . ? C1 C2 1.394(9) . ? C2 C3 1.336(9) . ? C3 C4 1.387(9) . ? C4 C5 1.379(8) . ? C5 C6 1.382(7) . ? C6 C7 1.502(7) . ? C8 C9 1.518(5) . ? C9 C8 1.518(5) 11_565 ? Cl1 O2 1.371(4) 19_776 ? Cl1 O2 1.371(3) 20_566 ? Cl1 O2 1.371(3) 21_656 ? Cl1 O2 1.371(3) 3_675 ? Cl1 O2 1.371(4) . ? Cl1 O2 1.371(3) ? ? Cl1 O2 1.371(3) 2_765 ? Cl1 O1 1.476(10) . ? Cl1 O1 1.476(10) 19_776 ? O2 O2 1.553(11) 21_656 ? O2 O2 1.553(11) 20_566 ? O2 O1 1.679(15) 19_776 ? O1 O2 1.679(15) ? ? O1 O2 1.679(15) 19_776 ? O1 O2 1.679(15) 20_566 ? O1 O2 1.679(15) 21_656 ? Cl2 Cl2 1.132(18) 2_655 ? Cl2 Cl2 1.132(18) 3_665 ? Cl2 O5 1.227(17) 16_545 ? Cl2 O5 1.227(17) 2_655 ? Cl2 O7 1.433(10) . ? Cl2 O7 1.433(10) 18_655 ? Cl2 O5 1.440(9) 18_655 ? Cl2 O5 1.440(9) . ? Cl2 O6 1.449(10) . ? Cl2 O6 1.449(10) 3_665 ? Cl2 O5 1.52(2) 17 ? Cl2 O5 1.52(2) 3_665 ? O5 O5 0.63(3) 3_665 ? O5 O5 0.63(3) 2_655 ? O5 Cl2 1.227(17) 3_665 ? O5 Cl2 1.52(2) 2_655 ? O6 O7 1.34(3) 2_655 ? O6 O7 1.34(3) 18_655 ? O6 Cl2 1.449(9) 2_655 ? O7 O7 1.32(4) 18_655 ? O7 O6 1.34(3) 3_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ag1 S1 87.21(3) . . ? O1 Ag1 S1 87.21(3) . 2_765 ? S1 Ag1 S1 119.766(5) . 2_765 ? O1 Ag1 S1 87.21(3) . 3_675 ? S1 Ag1 S1 119.766(5) . 3_675 ? S1 Ag1 S1 119.766(5) 2_765 3_675 ? C8 S1 C7 100.2(2) . . ? C8 S1 Ag1 102.0(1) . . ? C7 S1 Ag1 110.1(2) . . ? C6 C1 C2 120.1(6) . . ? C3 C2 C1 120.7(6) . . ? C2 C3 C4 120.0(6) . . ? C5 C4 C3 120.0(6) . . ? C4 C5 C6 120.0(5) . . ? C1 C6 C5 119.1(5) . . ? C1 C6 C7 120.0(5) . . ? C5 C6 C7 120.8(5) . . ? C6 C7 S1 109.9(3) . . ? C9 C8 S1 112.6(3) . . ? C8 C9 C8 110.4(5) 11_565 . ? O2 Cl1 O2 111.0(5) 19_776 20_566 ? O2 Cl1 O2 111.0(5) 19_776 21_656 ? O2 Cl1 O2 111.0(5) 20_566 21_656 ? O2 Cl1 O2 69.0(5) 19_776 3_675 ? O2 Cl1 O2 69.0(5) 20_566 3_675 ? O2 Cl1 O2 180.0(10) 21_656 3_675 ? O2 Cl1 O2 180.000(4) 19_776 . ? O2 Cl1 O2 69.0(5) 20_566 . ? O2 Cl1 O2 69.0(5) 21_656 . ? O2 Cl1 O2 111.0(5) 3_675 . ? O2 Cl1 O2 56.8(2) 19_776 ? ? O2 Cl1 O2 144.3(11) 20_566 ? ? O2 Cl1 O2 56.83(19) 21_656 ? ? O2 Cl1 O2 123.2(2) 3_675 ? ? O2 Cl1 O2 123.2(2) . ? ? O2 Cl1 O2 69.0(5) 19_776 2_765 ? O2 Cl1 O2 180.0(10) 20_566 2_765 ? O2 Cl1 O2 69.0(5) 21_656 2_765 ? O2 Cl1 O2 111.0(5) 3_675 2_765 ? O2 Cl1 O2 111.0(5) . 2_765 ? O2 Cl1 O2 35.7(11) ? 2_765 ? O2 Cl1 O1 72.1(6) 19_776 . ? O2 Cl1 O1 72.1(6) 20_566 . ? O2 Cl1 O1 72.1(6) 21_656 . ? O2 Cl1 O1 107.9(6) 3_675 . ? O2 Cl1 O1 107.9(6) . . ? O2 Cl1 O1 72.1(6) ? . ? O2 Cl1 O1 107.9(6) 2_765 . ? O2 Cl1 O1 107.9(6) 19_776 19_776 ? O2 Cl1 O1 107.9(6) 20_566 19_776 ? O2 Cl1 O1 107.9(6) 21_656 19_776 ? O2 Cl1 O1 72.1(6) 3_675 19_776 ? O2 Cl1 O1 72.1(6) . 19_776 ? O2 Cl1 O1 107.9(6) ? 19_776 ? O2 Cl1 O1 72.1(6) 2_765 19_776 ? O1 Cl1 O1 180.000(6) . 19_776 ? Cl1 O2 O2 55.5(3) . 21_656 ? Cl1 O2 O2 55.5(3) . 20_566 ? O2 O2 O2 93.4(12) 21_656 20_566 ? Cl1 O2 O1 56.8(3) . 19_776 ? O2 O2 O1 90.8(4) 21_656 19_776 ? O2 O2 O1 90.8(4) 20_566 19_776 ? Cl1 O1 O2 51.0(4) . ? ? Cl1 O1 O2 51.0(4) . 19_776 ? O2 O1 O2 45.8(3) ? 19_776 ? Cl1 O1 O2 51.0(4) . 20_566 ? O2 O1 O2 102.1(9) ? 20_566 ? O2 O1 O2 84.7(7) 19_776 20_566 ? Cl1 O1 O2 51.0(4) . 21_656 ? O2 O1 O2 45.8(3) ? 21_656 ? O2 O1 O2 84.7(7) 19_776 21_656 ? O2 O1 O2 84.7(7) 20_566 21_656 ? Cl1 O1 Ag1 180.0 . . ? O2 O1 Ag1 129.0(4) ? . ? O2 O1 Ag1 129.0(4) 19_776 . ? O2 O1 Ag1 129.0(4) 20_566 . ? O2 O1 Ag1 129.0(4) 21_656 . ? Cl2 Cl2 Cl2 60.000(1) 2_655 3_665 ? Cl2 Cl2 O5 80.0(9) 2_655 16_545 ? Cl2 Cl2 O5 75.2(11) 3_665 16_545 ? Cl2 Cl2 O5 75.2(11) 2_655 2_655 ? Cl2 Cl2 O5 80.0(9) 3_665 2_655 ? O5 Cl2 O5 151.2(16) 16_545 2_655 ? Cl2 Cl2 O7 177.1(13) 2_655 . ? Cl2 Cl2 O7 122.6(9) 3_665 . ? O5 Cl2 O7 102(2) 16_545 . ? O5 Cl2 O7 104(2) 2_655 . ? Cl2 Cl2 O7 122.6(9) 2_655 18_655 ? Cl2 Cl2 O7 177.1(13) 3_665 18_655 ? O5 Cl2 O7 104(2) 16_545 18_655 ? O5 Cl2 O7 102(2) 2_655 18_655 ? O7 Cl2 O7 54.9(18) . 18_655 ? Cl2 Cl2 O5 55.4(9) 2_655 18_655 ? Cl2 Cl2 O5 71.1(12) 3_665 18_655 ? O5 Cl2 O5 25.7(13) 16_545 18_655 ? O5 Cl2 O5 130.2(9) 2_655 18_655 ? O7 Cl2 O5 126(2) . 18_655 ? O7 Cl2 O5 109.1(9) 18_655 18_655 ? Cl2 Cl2 O5 71.1(12) 2_655 . ? Cl2 Cl2 O5 55.4(9) 3_665 . ? O5 Cl2 O5 130.2(9) 16_545 . ? O5 Cl2 O5 25.7(13) 2_655 . ? O7 Cl2 O5 109.1(9) . . ? O7 Cl2 O5 126(2) 18_655 . ? O5 Cl2 O5 118(2) 18_655 . ? Cl2 Cl2 O6 67.0(4) 2_655 . ? Cl2 Cl2 O6 127.0(4) 3_665 . ? O5 Cl2 O6 96.4(14) 16_545 . ? O5 Cl2 O6 87.1(14) 2_655 . ? O7 Cl2 O6 110.4(10) . . ? O7 Cl2 O6 55.6(10) 18_655 . ? O5 Cl2 O6 79.6(10) 18_655 . ? O5 Cl2 O6 107.8(7) . . ? Cl2 Cl2 O6 127.0(4) 2_655 3_665 ? Cl2 Cl2 O6 67.0(4) 3_665 3_665 ? O5 Cl2 O6 87.1(14) 16_545 3_665 ? O5 Cl2 O6 96.4(14) 2_655 3_665 ? O7 Cl2 O6 55.6(10) . 3_665 ? O7 Cl2 O6 110.4(10) 18_655 3_665 ? O5 Cl2 O6 107.8(7) 18_655 3_665 ? O5 Cl2 O6 79.6(10) . 3_665 ? O6 Cl2 O6 166.0(9) . 3_665 ? Cl2 Cl2 O5 63.9(11) 2_655 17 ? Cl2 Cl2 O5 52.8(7) 3_665 17 ? O5 Cl2 O5 23.6(10) 16_545 17 ? O5 Cl2 O5 128.1(12) 2_655 17 ? O7 Cl2 O5 118.4(15) . 17 ? O7 Cl2 O5 126.5(19) 18_655 17 ? O5 Cl2 O5 24.3(10) 18_655 17 ? O5 Cl2 O5 106.9(14) . 17 ? O6 Cl2 O5 103.8(10) . 17 ? O6 Cl2 O5 84.8(9) 3_665 17 ? Cl2 Cl2 O5 52.8(7) 2_655 3_665 ? Cl2 Cl2 O5 63.9(11) 3_665 3_665 ? O5 Cl2 O5 128.1(12) 16_545 3_665 ? O5 Cl2 O5 23.6(10) 2_655 3_665 ? O7 Cl2 O5 126.5(19) . 3_665 ? O7 Cl2 O5 118.4(15) 18_655 3_665 ? O5 Cl2 O5 106.9(14) 18_655 3_665 ? O5 Cl2 O5 24.3(10) . 3_665 ? O6 Cl2 O5 84.8(9) . 3_665 ? O6 Cl2 O5 103.8(9) 3_665 3_665 ? O5 Cl2 O5 106(2) 17 3_665 ? O5 O5 O5 60.00(3) 3_665 2_655 ? O5 O5 Cl2 97(2) 3_665 3_665 ? O5 O5 Cl2 105.1(8) 2_655 3_665 ? O5 O5 Cl2 85(2) 3_665 . ? O5 O5 Cl2 57.8(16) 2_655 . ? Cl2 O5 Cl2 49.4(9) 3_665 . ? O5 O5 Cl2 51.3(8) 3_665 2_655 ? O5 O5 Cl2 71(2) 2_655 2_655 ? Cl2 O5 Cl2 47.3(9) 3_665 2_655 ? Cl2 O5 Cl2 44.9(7) . 2_655 ? O7 O6 O7 169.1(14) 2_655 18_655 ? O7 O6 Cl2 107.6(10) 2_655 . ? O7 O6 Cl2 61.6(7) 18_655 . ? O7 O6 Cl2 61.6(7) 2_655 2_655 ? O7 O6 Cl2 107.6(10) 18_655 2_655 ? Cl2 O6 Cl2 46.0(9) . 2_655 ? O7 O7 O6 125.3(8) 18_655 3_665 ? O7 O7 Cl2 62.6(9) 18_655 . ? O6 O7 Cl2 62.8(8) 3_665 . ? 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 O1 Ag1 S1 C8 -84.97(15) . . . . ? S1 Ag1 S1 C8 0.22(16) 2_765 . . . ? S1 Ag1 S1 C8 -170.16(14) 3_675 . . . ? O1 Ag1 S1 C7 169.37(18) . . . . ? S1 Ag1 S1 C7 -105.44(18) 2_765 . . . ? S1 Ag1 S1 C7 84.18(19) 3_675 . . . ? C6 C1 C2 C3 1.2(9) . . . . ? C1 C2 C3 C4 -1.2(9) . . . . ? C2 C3 C4 C5 0.4(9) . . . . ? C3 C4 C5 C6 0.5(8) . . . . ? C2 C1 C6 C5 -0.3(7) . . . . ? C2 C1 C6 C7 177.7(5) . . . . ? C4 C5 C6 C1 -0.5(7) . . . . ? C4 C5 C6 C7 -178.5(4) . . . . ? C1 C6 C7 S1 107.8(5) . . . . ? C5 C6 C7 S1 -74.2(5) . . . . ? C8 S1 C7 C6 -173.8(4) . . . . ? Ag1 S1 C7 C6 -66.9(4) . . . . ? C7 S1 C8 C9 -67.2(3) . . . . ? Ag1 S1 C8 C9 179.6(2) . . . . ? S1 C8 C9 C8 178.5(3) . . . 11_565 ? O2 Cl1 O2 O2 -123(42) 19_776 . . 21_656 ? O2 Cl1 O2 O2 124.0(14) 20_566 . . 21_656 ? O2 Cl1 O2 O2 180.000(1) 3_675 . . 21_656 ? O2 Cl1 O2 O2 -17.9(4) ? . . 21_656 ? O2 Cl1 O2 O2 -56.0(14) 2_765 . . 21_656 ? O1 Cl1 O2 O2 62.0(7) . . . 21_656 ? O1 Cl1 O2 O2 -118.0(7) 19_776 . . 21_656 ? O2 Cl1 O2 O2 113(18) 19_776 . . 20_566 ? O2 Cl1 O2 O2 -124.0(14) 21_656 . . 20_566 ? O2 Cl1 O2 O2 56.0(14) 3_675 . . 20_566 ? O2 Cl1 O2 O2 -142.0(10) ? . . 20_566 ? O2 Cl1 O2 O2 180.000(2) 2_765 . . 20_566 ? O1 Cl1 O2 O2 -62.0(7) . . . 20_566 ? O1 Cl1 O2 O2 118.0(7) 19_776 . . 20_566 ? O2 Cl1 O2 O1 -5(7) 19_776 . . 19_776 ? O2 Cl1 O2 O1 -118.0(7) 20_566 . . 19_776 ? O2 Cl1 O2 O1 118.0(7) 21_656 . . 19_776 ? O2 Cl1 O2 O1 -62.0(7) 3_675 . . 19_776 ? O2 Cl1 O2 O1 100.0(3) ? . . 19_776 ? O2 Cl1 O2 O1 62.0(7) 2_765 . . 19_776 ? O1 Cl1 O2 O1 180.000(4) . . . 19_776 ? O2 Cl1 O1 O2 60.00(3) 19_776 . . ? ? O2 Cl1 O1 O2 180.00(2) 20_566 . . ? ? O2 Cl1 O1 O2 -60.00(3) 21_656 . . ? ? O2 Cl1 O1 O2 120.00(3) 3_675 . . ? ? O2 Cl1 O1 O2 -120.00(3) . . . ? ? O2 Cl1 O1 O2 0.00(2) 2_765 . . ? ? O1 Cl1 O1 O2 0(100) 19_776 . . ? ? O2 Cl1 O1 O2 120.000(1) 20_566 . . 19_776 ? O2 Cl1 O1 O2 -120.000(4) 21_656 . . 19_776 ? O2 Cl1 O1 O2 60.000(3) 3_675 . . 19_776 ? O2 Cl1 O1 O2 180.000(4) . . . 19_776 ? O2 Cl1 O1 O2 -60.000(2) ? . . 19_776 ? O2 Cl1 O1 O2 -60.000(1) 2_765 . . 19_776 ? O1 Cl1 O1 O2 0(100) 19_776 . . 19_776 ? O2 Cl1 O1 O2 -120.00(3) 19_776 . . 20_566 ? O2 Cl1 O1 O2 120.00(3) 21_656 . . 20_566 ? O2 Cl1 O1 O2 -60.00(3) 3_675 . . 20_566 ? O2 Cl1 O1 O2 60.00(2) . . . 20_566 ? O2 Cl1 O1 O2 180.00(2) ? . . 20_566 ? O2 Cl1 O1 O2 180.00(2) 2_765 . . 20_566 ? O1 Cl1 O1 O2 0(100) 19_776 . . 20_566 ? O2 Cl1 O1 O2 120.000(9) 19_776 . . 21_656 ? O2 Cl1 O1 O2 -120.000(6) 20_566 . . 21_656 ? O2 Cl1 O1 O2 180.000(8) 3_675 . . 21_656 ? O2 Cl1 O1 O2 -60.000(9) . . . 21_656 ? O2 Cl1 O1 O2 60.000(6) ? . . 21_656 ? O2 Cl1 O1 O2 60.000(6) 2_765 . . 21_656 ? O1 Cl1 O1 O2 0(100) 19_776 . . 21_656 ? O2 Cl1 O1 Ag1 -30(100) 19_776 . . . ? O2 Cl1 O1 Ag1 90(100) 20_566 . . . ? O2 Cl1 O1 Ag1 -150(100) 21_656 . . . ? O2 Cl1 O1 Ag1 30(100) 3_675 . . . ? O2 Cl1 O1 Ag1 150(100) . . . . ? O2 Cl1 O1 Ag1 -90(100) ? . . . ? O2 Cl1 O1 Ag1 -90(100) 2_765 . . . ? O1 Cl1 O1 Ag1 0(100) 19_776 . . . ? S1 Ag1 O1 Cl1 -161(100) . . . . ? S1 Ag1 O1 Cl1 79(100) 2_765 . . . ? S1 Ag1 O1 Cl1 -41(100) 3_675 . . . ? S1 Ag1 O1 O2 109.0(11) . . . ? ? S1 Ag1 O1 O2 -11.0(11) 2_765 . . ? ? S1 Ag1 O1 O2 -131.0(11) 3_675 . . ? ? S1 Ag1 O1 O2 169.0(11) . . . 19_776 ? S1 Ag1 O1 O2 49.0(11) 2_765 . . 19_776 ? S1 Ag1 O1 O2 -71.0(11) 3_675 . . 19_776 ? S1 Ag1 O1 O2 -71.0(11) . . . 20_566 ? S1 Ag1 O1 O2 169.0(11) 2_765 . . 20_566 ? S1 Ag1 O1 O2 49.0(11) 3_675 . . 20_566 ? S1 Ag1 O1 O2 49.0(11) . . . 21_656 ? S1 Ag1 O1 O2 -71.0(11) 2_765 . . 21_656 ? S1 Ag1 O1 O2 169.0(11) 3_675 . . 21_656 ? Cl2 Cl2 O5 O5 37(4) 2_655 . . 3_665 ? Cl2 Cl2 O5 O5 103(4) 3_665 . . 3_665 ? O5 Cl2 O5 O5 95.2(19) 16_545 . . 3_665 ? O5 Cl2 O5 O5 -57.7(9) 2_655 . . 3_665 ? O7 Cl2 O5 O5 -140(4) . . . 3_665 ? O7 Cl2 O5 O5 -80(5) 18_655 . . 3_665 ? O5 Cl2 O5 O5 68(4) 18_655 . . 3_665 ? O6 Cl2 O5 O5 -20(4) . . . 3_665 ? O6 Cl2 O5 O5 172(4) 3_665 . . 3_665 ? O5 Cl2 O5 O5 91(5) 17 . . 3_665 ? Cl2 Cl2 O5 O5 95(5) 2_655 . . 2_655 ? Cl2 Cl2 O5 O5 161(5) 3_665 . . 2_655 ? O5 Cl2 O5 O5 153(3) 16_545 . . 2_655 ? O7 Cl2 O5 O5 -82(5) . . . 2_655 ? O7 Cl2 O5 O5 -22(6) 18_655 . . 2_655 ? O5 Cl2 O5 O5 125(5) 18_655 . . 2_655 ? O6 Cl2 O5 O5 38(5) . . . 2_655 ? O6 Cl2 O5 O5 -130(5) 3_665 . . 2_655 ? O5 Cl2 O5 O5 149(6) 17 . . 2_655 ? O5 Cl2 O5 O5 57.7(10) 3_665 . . 2_655 ? Cl2 Cl2 O5 Cl2 -66.0(8) 2_655 . . 3_665 ? O5 Cl2 O5 Cl2 -8(3) 16_545 . . 3_665 ? O5 Cl2 O5 Cl2 -161(5) 2_655 . . 3_665 ? O7 Cl2 O5 Cl2 117.0(12) . . . 3_665 ? O7 Cl2 O5 Cl2 176.9(11) 18_655 . . 3_665 ? O5 Cl2 O5 Cl2 -35.6(5) 18_655 . . 3_665 ? O6 Cl2 O5 Cl2 -123.1(7) . . . 3_665 ? O6 Cl2 O5 Cl2 69.1(6) 3_665 . . 3_665 ? O5 Cl2 O5 Cl2 -12.1(8) 17 . . 3_665 ? O5 Cl2 O5 Cl2 -103(4) 3_665 . . 3_665 ? Cl2 Cl2 O5 Cl2 66.0(8) 3_665 . . 2_655 ? O5 Cl2 O5 Cl2 58(2) 16_545 . . 2_655 ? O5 Cl2 O5 Cl2 -95(5) 2_655 . . 2_655 ? O7 Cl2 O5 Cl2 -177.0(13) . . . 2_655 ? O7 Cl2 O5 Cl2 -117.1(14) 18_655 . . 2_655 ? O5 Cl2 O5 Cl2 30.4(3) 18_655 . . 2_655 ? O6 Cl2 O5 Cl2 -57.1(7) . . . 2_655 ? O6 Cl2 O5 Cl2 135.2(5) 3_665 . . 2_655 ? O5 Cl2 O5 Cl2 53.9(11) 17 . . 2_655 ? O5 Cl2 O5 Cl2 -37(4) 3_665 . . 2_655 ? Cl2 Cl2 O6 O7 -1.3(18) 2_655 . . 2_655 ? Cl2 Cl2 O6 O7 -1.3(18) 3_665 . . 2_655 ? O5 Cl2 O6 O7 -77.6(19) 16_545 . . 2_655 ? O5 Cl2 O6 O7 73.8(19) 2_655 . . 2_655 ? O7 Cl2 O6 O7 177(4) . . . 2_655 ? O7 Cl2 O6 O7 -179.89(16) 18_655 . . 2_655 ? O5 Cl2 O6 O7 -58.0(14) 18_655 . . 2_655 ? O5 Cl2 O6 O7 58(3) . . . 2_655 ? O6 Cl2 O6 O7 178.7(18) 3_665 . . 2_655 ? O5 Cl2 O6 O7 -55(2) 17 . . 2_655 ? O5 Cl2 O6 O7 50.2(17) 3_665 . . 2_655 ? Cl2 Cl2 O6 O7 179(2) 2_655 . . 18_655 ? Cl2 Cl2 O6 O7 179(2) 3_665 . . 18_655 ? O5 Cl2 O6 O7 102(2) 16_545 . . 18_655 ? O5 Cl2 O6 O7 -106(2) 2_655 . . 18_655 ? O7 Cl2 O6 O7 -3(4) . . . 18_655 ? O5 Cl2 O6 O7 121.9(16) 18_655 . . 18_655 ? O5 Cl2 O6 O7 -122(3) . . . 18_655 ? O6 Cl2 O6 O7 -1(2) 3_665 . . 18_655 ? O5 Cl2 O6 O7 125(3) 17 . . 18_655 ? O5 Cl2 O6 O7 -129.9(18) 3_665 . . 18_655 ? Cl2 Cl2 O6 Cl2 0.0 3_665 . . 2_655 ? O5 Cl2 O6 Cl2 -76.2(8) 16_545 . . 2_655 ? O5 Cl2 O6 Cl2 75.1(8) 2_655 . . 2_655 ? O7 Cl2 O6 Cl2 178.7(17) . . . 2_655 ? O7 Cl2 O6 Cl2 -179(2) 18_655 . . 2_655 ? O5 Cl2 O6 Cl2 -56.7(11) 18_655 . . 2_655 ? O5 Cl2 O6 Cl2 59.7(12) . . . 2_655 ? O6 Cl2 O6 Cl2 180.000(1) 3_665 . . 2_655 ? O5 Cl2 O6 Cl2 -53.5(11) 17 . . 2_655 ? O5 Cl2 O6 Cl2 51.6(9) 3_665 . . 2_655 ? Cl2 Cl2 O7 O7 27(33) 2_655 . . 18_655 ? Cl2 Cl2 O7 O7 -178(2) 3_665 . . 18_655 ? O5 Cl2 O7 O7 -99(4) 16_545 . . 18_655 ? O5 Cl2 O7 O7 95(4) 2_655 . . 18_655 ? O5 Cl2 O7 O7 -89(3) 18_655 . . 18_655 ? O5 Cl2 O7 O7 121(3) . . . 18_655 ? O6 Cl2 O7 O7 3(4) . . . 18_655 ? O6 Cl2 O7 O7 -177(4) 3_665 . . 18_655 ? O5 Cl2 O7 O7 -117(3) 17 . . 18_655 ? O5 Cl2 O7 O7 102(2) 3_665 . . 18_655 ? Cl2 Cl2 O7 O6 -156(29) 2_655 . . 3_665 ? Cl2 Cl2 O7 O6 -2(2) 3_665 . . 3_665 ? O5 Cl2 O7 O6 78.2(10) 16_545 . . 3_665 ? O5 Cl2 O7 O6 -88.4(11) 2_655 . . 3_665 ? O7 Cl2 O7 O6 177(4) 18_655 . . 3_665 ? O5 Cl2 O7 O6 88(2) 18_655 . . 3_665 ? O5 Cl2 O7 O6 -62.1(16) . . . 3_665 ? O6 Cl2 O7 O6 179.6(5) . . . 3_665 ? O5 Cl2 O7 O6 60.3(19) 17 . . 3_665 ? O5 Cl2 O7 O6 -81(2) 3_665 . . 3_665 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.961 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.092 data_14 _database_code_depnum_ccdc_archive 'CCDC 231511' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H33 Ag Cl O4 S3' _chemical_formula_weight 661.03 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(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 9.604(5) _cell_length_b 23.66(1) _cell_length_c 12.399(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.660(9) _cell_angle_gamma 90.00 _cell_volume 2798(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 799 _cell_measurement_theta_min 2.3021 _cell_measurement_theta_max 23.0988 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 1.072 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8142 _exptl_absorpt_correction_T_max 0.8305 _exptl_absorpt_process_details SADABS _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 'Bruker CCD area detector' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15215 _diffrn_reflns_av_R_equivalents 0.0891 _diffrn_reflns_av_sigmaI/netI 0.1215 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.51 _reflns_number_total 5742 _reflns_number_gt 2980 _reflns_threshold_expression I>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_publication_material 'Bruker SHELXTL' _computing_molecular_graphics '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^)+(0.0480P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5742 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1352 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _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 0.11866(5) 0.02630(2) 0.28572(4) 0.05191(18) Uani 1 1 d . . . S1 S 0.22365(17) 0.09079(7) 0.43400(12) 0.0530(4) Uani 1 1 d . . . S2 S 0.01693(16) -0.06087(6) 0.36407(11) 0.0437(4) Uani 1 1 d . . . S3 S 0.17064(15) 0.03171(6) 0.09203(11) 0.0434(4) Uani 1 1 d . . . Cl1 Cl -0.23604(18) 0.07861(7) 0.25952(13) 0.0552(4) Uani 1 1 d . . . C1 C 0.2776(7) -0.0929(3) 0.0576(5) 0.0555(17) Uani 1 1 d . . . H1A H 0.2152 -0.0819 -0.0017 0.067 Uiso 1 1 calc R . . C2 C 0.2852(8) -0.1488(3) 0.0864(5) 0.069(2) Uani 1 1 d . . . H2A H 0.2262 -0.1751 0.0490 0.082 Uiso 1 1 calc R . . C3 C 0.3802(8) -0.1651(3) 0.1702(6) 0.068(2) Uani 1 1 d . . . H3A H 0.3867 -0.2032 0.1892 0.081 Uiso 1 1 calc R . . C4 C 0.4648(7) -0.1277(3) 0.2264(5) 0.0626(19) Uani 1 1 d . . . H4A H 0.5297 -0.1398 0.2832 0.075 Uiso 1 1 calc R . . C5 C 0.4553(6) -0.0705(3) 0.1991(5) 0.0578(17) Uani 1 1 d . . . H5A H 0.5131 -0.0443 0.2382 0.069 Uiso 1 1 calc R . . C6 C 0.3594(6) -0.0528(3) 0.1137(5) 0.0473(15) Uani 1 1 d . . . C7 C 0.3455(7) 0.0084(3) 0.0813(5) 0.0597(18) Uani 1 1 d . . . H7A H 0.3667 0.0129 0.0072 0.072 Uiso 1 1 calc R . . H7B H 0.4115 0.0310 0.1282 0.072 Uiso 1 1 calc R . . C9 C -0.1999(6) -0.1112(2) 0.0693(4) 0.0460(15) Uani 1 1 d . . . H9A H -0.2894 -0.0946 0.0807 0.055 Uiso 1 1 calc R . . H9B H -0.2043 -0.1513 0.0856 0.055 Uiso 1 1 calc R . . C10 C -0.0866(6) -0.0845(3) 0.1469(4) 0.0476(15) Uani 1 1 d . . . H10A H -0.0768 -0.0451 0.1272 0.057 Uiso 1 1 calc R . . H10B H 0.0018 -0.1032 0.1402 0.057 Uiso 1 1 calc R . . C11 C -0.1175(6) -0.0879(2) 0.2646(4) 0.0457(15) Uani 1 1 d . . . H11A H -0.1342 -0.1271 0.2817 0.055 Uiso 1 1 calc R . . H11B H -0.2034 -0.0672 0.2711 0.055 Uiso 1 1 calc R . . C12 C 0.1544(6) -0.1130(2) 0.3592(5) 0.0486(15) Uani 1 1 d . . . H12A H 0.1813 -0.1140 0.2862 0.058 Uiso 1 1 calc R . . H12B H 0.2357 -0.1013 0.4077 0.058 Uiso 1 1 calc R . . C13 C 0.1135(5) -0.1715(2) 0.3900(4) 0.0405(14) Uani 1 1 d . . . C14 C 0.1175(6) -0.1878(3) 0.4979(5) 0.0490(16) Uani 1 1 d . . . H14A H 0.1434 -0.1617 0.5528 0.059 Uiso 1 1 calc R . . C15 C 0.0839(7) -0.2412(3) 0.5237(5) 0.0565(17) Uani 1 1 d . . . H15A H 0.0876 -0.2515 0.5963 0.068 Uiso 1 1 calc R . . C16 C 0.0452(6) -0.2799(3) 0.4459(6) 0.0587(18) Uani 1 1 d . . . H16A H 0.0221 -0.3165 0.4647 0.070 Uiso 1 1 calc R . . C17 C 0.0405(7) -0.2648(3) 0.3402(6) 0.0581(17) Uani 1 1 d . . . H17A H 0.0136 -0.2913 0.2864 0.070 Uiso 1 1 calc R . . C18 C 0.0746(6) -0.2111(3) 0.3113(5) 0.0507(16) Uani 1 1 d . . . H18A H 0.0714 -0.2015 0.2383 0.061 Uiso 1 1 calc R . . C19 C 0.4461(7) 0.0150(3) 0.4637(5) 0.069(2) Uani 1 1 d . . . H19A H 0.4931 0.0377 0.4137 0.083 Uiso 1 1 calc R . . H19B H 0.3901 -0.0129 0.4210 0.083 Uiso 1 1 calc R . . C20 C 0.3514(9) 0.0517(3) 0.5148(6) 0.090(3) Uani 1 1 d . . . H20A H 0.4086 0.0783 0.5600 0.108 Uiso 1 1 calc R . . H20B H 0.3031 0.0284 0.5631 0.108 Uiso 1 1 calc R . . C21 C 0.3109(8) 0.1493(3) 0.3843(5) 0.077(2) Uani 1 1 d . . . H21A H 0.3877 0.1357 0.3470 0.092 Uiso 1 1 calc R . . H21B H 0.2462 0.1693 0.3318 0.092 Uiso 1 1 calc R . . C22 C 0.3683(7) 0.1902(3) 0.4724(5) 0.0526(16) Uani 1 1 d . . . C23 C 0.5031(7) 0.2077(3) 0.4791(5) 0.0653(19) Uani 1 1 d . . . H23A H 0.5618 0.1936 0.4310 0.078 Uiso 1 1 calc R . . C24 C 0.5534(7) 0.2463(3) 0.5566(6) 0.0627(18) Uani 1 1 d . . . H24A H 0.6463 0.2580 0.5600 0.075 Uiso 1 1 calc R . . C25 C 0.4709(7) 0.2679(3) 0.6284(5) 0.0584(17) Uani 1 1 d . . . H25A H 0.5065 0.2942 0.6801 0.070 Uiso 1 1 calc R . . C26 C 0.3358(7) 0.2503(3) 0.6236(5) 0.0598(18) Uani 1 1 d . . . H26A H 0.2779 0.2646 0.6722 0.072 Uiso 1 1 calc R . . C27 C 0.2844(7) 0.2111(3) 0.5461(6) 0.0600(18) Uani 1 1 d . . . H27A H 0.1921 0.1987 0.5437 0.072 Uiso 1 1 calc R . . O1 O -0.1093(6) 0.0917(3) 0.2219(5) 0.122(2) Uani 1 1 d . . . O2 O -0.3173(8) 0.1260(3) 0.2553(6) 0.139(3) Uani 1 1 d . . . O3 O -0.3004(8) 0.0350(2) 0.1969(5) 0.120(2) Uani 1 1 d . . . O4 O -0.2068(7) 0.0586(2) 0.3681(4) 0.116(2) Uani 1 1 d . . . C8 C -0.1773(7) -0.1041(2) -0.0484(4) 0.0516(16) Uani 1 1 d . . . H8A H -0.2526 -0.1232 -0.0932 0.062 Uiso 1 1 calc R . . H8B H -0.0902 -0.1226 -0.0604 0.062 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 0.0567(3) 0.0474(3) 0.0519(3) 0.0033(2) 0.0077(2) -0.0059(2) S1 0.0609(11) 0.0472(10) 0.0523(10) -0.0012(7) 0.0121(8) -0.0050(8) S2 0.0494(10) 0.0423(9) 0.0415(8) 0.0016(6) 0.0136(7) -0.0033(7) S3 0.0420(9) 0.0446(9) 0.0443(8) 0.0055(7) 0.0076(6) -0.0013(7) Cl1 0.0613(11) 0.0473(10) 0.0575(10) 0.0009(8) 0.0092(8) 0.0019(8) C1 0.060(4) 0.069(5) 0.038(4) -0.003(3) 0.006(3) 0.012(4) C2 0.087(6) 0.068(6) 0.052(4) -0.019(4) 0.012(4) 0.014(4) C3 0.074(5) 0.058(5) 0.075(5) -0.005(4) 0.025(4) 0.017(4) C4 0.056(5) 0.080(6) 0.054(4) 0.016(4) 0.012(3) 0.025(4) C5 0.041(4) 0.078(6) 0.055(4) 0.001(4) 0.011(3) 0.007(4) C6 0.040(4) 0.058(4) 0.046(4) 0.004(3) 0.014(3) 0.014(3) C7 0.049(4) 0.063(5) 0.069(4) 0.016(3) 0.016(3) 0.004(3) C9 0.050(4) 0.044(4) 0.043(4) 0.011(3) 0.004(3) -0.006(3) C10 0.042(4) 0.056(4) 0.047(4) 0.010(3) 0.011(3) -0.003(3) C11 0.041(4) 0.049(4) 0.050(4) 0.009(3) 0.018(3) -0.001(3) C12 0.038(4) 0.054(4) 0.055(4) 0.010(3) 0.009(3) -0.007(3) C13 0.031(3) 0.042(4) 0.048(4) 0.003(3) 0.002(3) 0.002(3) C14 0.039(4) 0.062(5) 0.046(4) 0.004(3) 0.004(3) -0.001(3) C15 0.053(4) 0.060(5) 0.059(4) 0.024(4) 0.016(3) 0.007(3) C16 0.053(4) 0.039(4) 0.089(6) 0.009(4) 0.031(4) 0.005(3) C17 0.055(5) 0.046(4) 0.074(5) -0.015(4) 0.015(3) -0.003(3) C18 0.049(4) 0.055(5) 0.049(4) 0.006(3) 0.009(3) -0.002(3) C19 0.062(5) 0.074(5) 0.067(5) -0.022(4) -0.006(3) 0.006(4) C20 0.106(7) 0.084(6) 0.076(6) -0.021(4) -0.007(5) -0.002(5) C21 0.098(6) 0.072(5) 0.058(5) 0.009(4) 0.001(4) -0.035(4) C22 0.068(5) 0.043(4) 0.047(4) 0.007(3) 0.005(3) -0.008(3) C23 0.067(5) 0.060(5) 0.073(5) -0.003(4) 0.024(4) -0.016(4) C24 0.051(4) 0.048(4) 0.091(5) 0.005(4) 0.015(4) -0.014(3) C25 0.063(5) 0.043(4) 0.067(5) -0.002(3) -0.004(4) 0.001(3) C26 0.055(5) 0.049(4) 0.076(5) -0.001(4) 0.008(4) 0.011(4) C27 0.037(4) 0.053(4) 0.086(5) 0.016(4) -0.009(3) -0.011(3) O1 0.068(4) 0.155(6) 0.143(5) 0.045(4) 0.022(4) -0.016(4) O2 0.149(6) 0.097(5) 0.176(6) 0.012(4) 0.035(5) 0.075(5) O3 0.155(6) 0.087(5) 0.115(5) -0.027(4) -0.003(4) -0.032(4) O4 0.181(7) 0.094(4) 0.070(4) 0.031(3) -0.001(4) -0.029(4) C8 0.055(4) 0.049(4) 0.051(4) 0.001(3) 0.005(3) -0.007(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 S1 2.509(2) . ? Ag1 S3 2.512(2) . ? Ag1 S2 2.524(2) . ? S1 C20 1.755(8) . ? S1 C21 1.766(6) . ? S2 C11 1.796(6) . ? S2 C12 1.813(6) . ? S3 C7 1.788(6) . ? S3 C8 1.800(6) 3 ? Cl1 O2 1.364(5) . ? Cl1 O1 1.389(5) . ? Cl1 O3 1.392(5) . ? Cl1 O4 1.424(5) . ? C1 C2 1.368(9) . ? C1 C6 1.369(8) . ? C1 H1A 0.9300 . ? C2 C3 1.358(9) . ? C2 H2A 0.9300 . ? C3 C4 1.342(9) . ? C3 H3A 0.9300 . ? C4 C5 1.395(9) . ? C4 H4A 0.9300 . ? C5 C6 1.385(8) . ? C5 H5A 0.9300 . ? C6 C7 1.503(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C10 1.506(8) . ? C9 C8 1.510(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.524(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.500(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C18 1.373(8) . ? C13 C14 1.388(7) . ? C14 C15 1.351(8) . ? C14 H14A 0.9300 . ? C15 C16 1.351(9) . ? C15 H15A 0.9300 . ? C16 C17 1.354(8) . ? C16 H16A 0.9300 . ? C17 C18 1.370(8) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.454(10) . ? C19 C19 1.473(13) 3_656 ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.514(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.352(9) . ? C22 C27 1.379(9) . ? C23 C24 1.372(9) . ? C23 H23A 0.9300 . ? C24 C25 1.358(9) . ? C24 H24A 0.9300 . ? C25 C26 1.357(9) . ? C25 H25A 0.9300 . ? C26 C27 1.385(8) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C8 S3 1.800(6) 3 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ag1 S3 124.19(6) . . ? S1 Ag1 S2 110.82(6) . . ? S3 Ag1 S2 122.56(5) . . ? C20 S1 C21 106.5(4) . . ? C20 S1 Ag1 107.0(3) . . ? C21 S1 Ag1 112.8(2) . . ? C11 S2 C12 101.7(3) . . ? C11 S2 Ag1 107.8(2) . . ? C12 S2 Ag1 103.1(2) . . ? C7 S3 C8 101.8(3) . 3 ? C7 S3 Ag1 110.4(2) . . ? C8 S3 Ag1 110.71(19) 3 . ? O2 Cl1 O1 108.9(4) . . ? O2 Cl1 O3 111.9(5) . . ? O1 Cl1 O3 109.2(4) . . ? O2 Cl1 O4 111.0(4) . . ? O1 Cl1 O4 107.9(4) . . ? O3 Cl1 O4 107.9(4) . . ? C2 C1 C6 121.8(6) . . ? C2 C1 H1A 119.1 . . ? C6 C1 H1A 119.1 . . ? C3 C2 C1 119.1(7) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C4 C3 C2 121.4(7) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C4 C5 119.8(7) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C6 C5 C4 119.8(7) . . ? C6 C5 H5A 120.1 . . ? C4 C5 H5A 120.1 . . ? C1 C6 C5 118.1(6) . . ? C1 C6 C7 120.2(6) . . ? C5 C6 C7 121.7(6) . . ? C6 C7 S3 109.4(4) . . ? C6 C7 H7A 109.8 . . ? S3 C7 H7A 109.8 . . ? C6 C7 H7B 109.8 . . ? S3 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? C10 C9 C8 113.4(5) . . ? C10 C9 H9A 108.9 . . ? C8 C9 H9A 108.9 . . ? C10 C9 H9B 108.9 . . ? C8 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C9 C10 C11 112.5(5) . . ? C9 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? C9 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C10 C11 S2 115.8(4) . . ? C10 C11 H11A 108.3 . . ? S2 C11 H11A 108.3 . . ? C10 C11 H11B 108.3 . . ? S2 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? C13 C12 S2 114.0(4) . . ? C13 C12 H12A 108.8 . . ? S2 C12 H12A 108.8 . . ? C13 C12 H12B 108.8 . . ? S2 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C18 C13 C14 118.1(6) . . ? C18 C13 C12 120.4(5) . . ? C14 C13 C12 121.5(5) . . ? C15 C14 C13 120.4(6) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 121.3(6) . . ? C14 C15 H15A 119.4 . . ? C16 C15 H15A 119.4 . . ? C15 C16 C17 119.1(6) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? C16 C17 C18 121.1(6) . . ? C16 C17 H17A 119.5 . . ? C18 C17 H17A 119.5 . . ? C17 C18 C13 120.0(6) . . ? C17 C18 H18A 120.0 . . ? C13 C18 H18A 120.0 . . ? C20 C19 C19 116.9(8) . 3_656 ? C20 C19 H19A 108.1 . . ? C19 C19 H19A 108.1 3_656 . ? C20 C19 H19B 108.1 . . ? C19 C19 H19B 108.1 3_656 . ? H19A C19 H19B 107.3 . . ? C19 C20 S1 119.8(6) . . ? C19 C20 H20A 107.4 . . ? S1 C20 H20A 107.4 . . ? C19 C20 H20B 107.4 . . ? S1 C20 H20B 107.4 . . ? H20A C20 H20B 106.9 . . ? C22 C21 S1 113.4(4) . . ? C22 C21 H21A 108.9 . . ? S1 C21 H21A 108.9 . . ? C22 C21 H21B 108.9 . . ? S1 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C23 C22 C27 118.6(6) . . ? C23 C22 C21 120.4(6) . . ? C27 C22 C21 121.0(6) . . ? C22 C23 C24 120.3(7) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C25 C24 C23 121.6(7) . . ? C25 C24 H24A 119.2 . . ? C23 C24 H24A 119.2 . . ? C26 C25 C24 118.9(6) . . ? C26 C25 H25A 120.5 . . ? C24 C25 H25A 120.5 . . ? C25 C26 C27 119.9(6) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? C22 C27 C26 120.8(6) . . ? C22 C27 H27A 119.6 . . ? C26 C27 H27A 119.6 . . ? C9 C8 S3 114.2(4) . 3 ? C9 C8 H8A 108.7 . . ? S3 C8 H8A 108.7 3 . ? C9 C8 H8B 108.7 . . ? S3 C8 H8B 108.7 3 . ? H8A C8 H8B 107.6 . . ? 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 S3 Ag1 S1 C20 -105.0(3) . . . . ? S2 Ag1 S1 C20 57.6(3) . . . . ? S3 Ag1 S1 C21 11.8(3) . . . . ? S2 Ag1 S1 C21 174.4(3) . . . . ? S1 Ag1 S2 C11 155.0(2) . . . . ? S3 Ag1 S2 C11 -42.0(2) . . . . ? S1 Ag1 S2 C12 -97.9(2) . . . . ? S3 Ag1 S2 C12 65.1(2) . . . . ? S1 Ag1 S3 C7 70.9(3) . . . . ? S2 Ag1 S3 C7 -89.8(2) . . . . ? S1 Ag1 S3 C8 -41.1(2) . . . 3 ? S2 Ag1 S3 C8 158.2(2) . . . 3 ? C6 C1 C2 C3 -2.5(10) . . . . ? C1 C2 C3 C4 1.1(10) . . . . ? C2 C3 C4 C5 0.5(10) . . . . ? C3 C4 C5 C6 -0.6(9) . . . . ? C2 C1 C6 C5 2.3(9) . . . . ? C2 C1 C6 C7 -178.5(6) . . . . ? C4 C5 C6 C1 -0.7(8) . . . . ? C4 C5 C6 C7 -179.9(5) . . . . ? C1 C6 C7 S3 60.3(7) . . . . ? C5 C6 C7 S3 -120.6(6) . . . . ? C8 S3 C7 C6 -179.2(4) 3 . . . ? Ag1 S3 C7 C6 63.2(5) . . . . ? C8 C9 C10 C11 175.3(5) . . . . ? C9 C10 C11 S2 176.3(4) . . . . ? C12 S2 C11 C10 -69.6(5) . . . . ? Ag1 S2 C11 C10 38.5(5) . . . . ? C11 S2 C12 C13 -61.7(5) . . . . ? Ag1 S2 C12 C13 -173.4(4) . . . . ? S2 C12 C13 C18 100.5(6) . . . . ? S2 C12 C13 C14 -81.3(6) . . . . ? C18 C13 C14 C15 0.1(8) . . . . ? C12 C13 C14 C15 -178.1(5) . . . . ? C13 C14 C15 C16 -0.4(9) . . . . ? C14 C15 C16 C17 0.2(9) . . . . ? C15 C16 C17 C18 0.2(9) . . . . ? C16 C17 C18 C13 -0.4(9) . . . . ? C14 C13 C18 C17 0.3(8) . . . . ? C12 C13 C18 C17 178.5(5) . . . . ? C19 C19 C20 S1 177.9(7) 3_656 . . . ? C21 S1 C20 C19 -78.1(7) . . . . ? Ag1 S1 C20 C19 42.8(8) . . . . ? C20 S1 C21 C22 -65.9(6) . . . . ? Ag1 S1 C21 C22 177.0(5) . . . . ? S1 C21 C22 C23 129.9(6) . . . . ? S1 C21 C22 C27 -51.2(8) . . . . ? C27 C22 C23 C24 -1.2(10) . . . . ? C21 C22 C23 C24 177.7(6) . . . . ? C22 C23 C24 C25 0.2(10) . . . . ? C23 C24 C25 C26 0.5(10) . . . . ? C24 C25 C26 C27 -0.1(10) . . . . ? C23 C22 C27 C26 1.6(9) . . . . ? C21 C22 C27 C26 -177.3(6) . . . . ? C25 C26 C27 C22 -1.0(10) . . . . ? C10 C9 C8 S3 -59.9(6) . . . 3 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.51 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.914 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.090