Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Shim Sung Lee' _publ_contact_author_address ; Department of Chemistry Gyeongsang University Chinju 660-701 SOUTH KOREA ; _publ_contact_author_email SSLEE@GSNU.AC.KR _publ_section_title ; Donor Effect on Supramolecular Structures of Silver(I) Perchlorate Complexes of Macrocycles with O2S2X (X=S, O and NH) Donor Sets ; loop_ _publ_author_name 'Shim Sung Lee.' 'Kyu Seong Choi.' 'Ok-Sang Jung.' 'Ji-Eun Lee.' ; So Young Lee ; 'Ki-Min Park.' 'Joobeom Seo.' 'Mi Ryoung Song.' 'Il Yoon.' data_1 _database_code_depnum_ccdc_archive 'CCDC 271048' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H48 Ag Cl O8 S6' _chemical_formula_weight 992.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9985(7) _cell_length_b 11.6633(9) _cell_length_c 12.3578(9) _cell_angle_alpha 116.7000(10) _cell_angle_beta 95.460(2) _cell_angle_gamma 106.721(2) _cell_volume 1070.83(14) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4933 _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 28.31 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 0.876 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7054 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.31 _reflns_number_total 4933 _reflns_number_gt 3840 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0452P)^2^+0.6307P] 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 4933 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1093 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.5000 0.5000 0.5000 0.07097(14) Uani 1 2 d S . . S1 S 0.19011(8) 0.39499(7) 0.36132(6) 0.04745(16) Uani 1 1 d . . . S2 S 0.42230(9) 0.73917(7) 0.56042(7) 0.05649(19) Uani 1 1 d . . . S3 S 0.39199(9) 0.54930(8) 0.71530(7) 0.05309(18) Uani 1 1 d . . . O1 O 0.0714(2) 0.0584(2) 0.25980(18) 0.0553(5) Uani 1 1 d . . . O2 O 0.1939(3) 0.1272(2) 0.50653(19) 0.0571(5) Uani 1 1 d . . . C1 C 0.0268(4) -0.0376(3) 0.3030(3) 0.0635(8) Uani 1 1 d . . . H1A H -0.0021 -0.1300 0.2346 0.076 Uiso 1 1 calc R . . H1B H -0.0643 -0.0316 0.3367 0.076 Uiso 1 1 calc R . . C2 C -0.0431(3) 0.0501(3) 0.1732(2) 0.0479(6) Uani 1 1 d . . . C3 C -0.1971(3) -0.0513(3) 0.1183(3) 0.0562(7) Uani 1 1 d . . . H3 H -0.2291 -0.1219 0.1407 0.067 Uiso 1 1 calc R . . C4 C -0.3038(4) -0.0495(3) 0.0316(3) 0.0647(8) Uani 1 1 d . . . H4 H -0.4102 -0.1192 -0.0063 0.078 Uiso 1 1 calc R . . C5 C -0.2588(4) 0.0510(4) -0.0009(3) 0.0670(9) Uani 1 1 d . . . H5 H -0.3341 0.0517 -0.0609 0.080 Uiso 1 1 calc R . . C6 C -0.1046(4) 0.1517(3) 0.0525(3) 0.0582(7) Uani 1 1 d . . . H6 H -0.0731 0.2207 0.0280 0.070 Uiso 1 1 calc R . . C7 C 0.0043(3) 0.1530(3) 0.1412(2) 0.0480(6) Uani 1 1 d . . . C8 C 0.1714(3) 0.2605(3) 0.2024(3) 0.0529(6) Uani 1 1 d . . . H8A H 0.1994 0.3024 0.1521 0.063 Uiso 1 1 calc R . . H8B H 0.2457 0.2167 0.2064 0.063 Uiso 1 1 calc R . . C9 C 0.2059(5) 0.5346(3) 0.3279(3) 0.0722(9) Uani 1 1 d . . . H9A H 0.2916 0.5451 0.2882 0.087 Uiso 1 1 calc R . . H9B H 0.1079 0.5093 0.2696 0.087 Uiso 1 1 calc R . . C10 C 0.2361(5) 0.6682(3) 0.4402(4) 0.0773(11) Uani 1 1 d . . . H10A H 0.1479 0.6576 0.4775 0.093 Uiso 1 1 calc R . . H10B H 0.2369 0.7343 0.4140 0.093 Uiso 1 1 calc R . . C11 C 0.3430(4) 0.7615(3) 0.6946(3) 0.0667(8) Uani 1 1 d . . . H11A H 0.4305 0.8208 0.7690 0.080 Uiso 1 1 calc R . . H11B H 0.2702 0.8085 0.6984 0.080 Uiso 1 1 calc R . . C12 C 0.2561(4) 0.6310(3) 0.6971(3) 0.0595(7) Uani 1 1 d . . . H12A H 0.1730 0.5677 0.6204 0.071 Uiso 1 1 calc R . . H12B H 0.2063 0.6533 0.7653 0.071 Uiso 1 1 calc R . . C13 C 0.2476(4) 0.3915(3) 0.6952(3) 0.0569(7) Uani 1 1 d . . . H13A H 0.1874 0.4132 0.7568 0.068 Uiso 1 1 calc R . . H13B H 0.1737 0.3403 0.6134 0.068 Uiso 1 1 calc R . . C14 C 0.3373(3) 0.3062(3) 0.7100(3) 0.0519(6) Uani 1 1 d . . . C15 C 0.4482(4) 0.3570(4) 0.8214(3) 0.0675(8) Uani 1 1 d . . . H15 H 0.4656 0.4467 0.8901 0.081 Uiso 1 1 calc R . . C16 C 0.5354(4) 0.2822(4) 0.8372(4) 0.0745(10) Uani 1 1 d . . . H16 H 0.6124 0.3197 0.9152 0.089 Uiso 1 1 calc R . . C17 C 0.5091(4) 0.1541(4) 0.7392(4) 0.0728(10) Uani 1 1 d . . . H17 H 0.5684 0.1014 0.7490 0.087 Uiso 1 1 calc R . . C18 C 0.3986(4) 0.0994(4) 0.6266(3) 0.0631(8) Uani 1 1 d . . . H18 H 0.3822 0.0096 0.5585 0.076 Uiso 1 1 calc R . . C19 C 0.3112(3) 0.1749(3) 0.6121(3) 0.0508(6) Uani 1 1 d . . . C20 C 0.1662(4) -0.0042(3) 0.4021(3) 0.0628(8) Uani 1 1 d . . . H20A H 0.1432 -0.0732 0.4268 0.075 Uiso 1 1 calc R . . H20B H 0.2599 -0.0021 0.3707 0.075 Uiso 1 1 calc R . . Cl Cl 0.0166(3) 0.4550(2) -0.0309(2) 0.0817(5) Uani 0.50 1 d P . . O3 O -0.0802(7) 0.4488(5) 0.0554(4) 0.1564(17) Uani 1 1 d . . . O4 O -0.0848(8) 0.3429(7) -0.1451(6) 0.109(2) Uani 0.50 1 d P . . O5 O 0.1423(7) 0.4195(7) 0.0043(7) 0.111(2) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.0591(2) 0.0979(3) 0.0616(2) 0.0335(2) 0.01706(16) 0.0470(2) S1 0.0494(4) 0.0386(3) 0.0444(3) 0.0146(3) 0.0092(3) 0.0144(3) S2 0.0583(4) 0.0391(3) 0.0599(4) 0.0208(3) 0.0078(3) 0.0111(3) S3 0.0503(4) 0.0516(4) 0.0542(4) 0.0246(3) 0.0141(3) 0.0176(3) O1 0.0481(10) 0.0574(12) 0.0508(11) 0.0276(10) 0.0075(9) 0.0075(9) O2 0.0630(12) 0.0526(11) 0.0528(11) 0.0242(9) 0.0082(9) 0.0233(10) C1 0.071(2) 0.0496(16) 0.0591(18) 0.0256(14) 0.0136(15) 0.0112(14) C2 0.0445(14) 0.0482(14) 0.0383(13) 0.0133(11) 0.0119(11) 0.0140(11) C3 0.0474(15) 0.0531(16) 0.0478(15) 0.0149(13) 0.0129(12) 0.0087(12) C4 0.0459(15) 0.0633(19) 0.0518(17) 0.0077(15) 0.0082(13) 0.0132(14) C5 0.0603(18) 0.077(2) 0.0470(16) 0.0137(16) 0.0061(14) 0.0344(17) C6 0.0692(19) 0.0569(17) 0.0444(15) 0.0181(13) 0.0163(14) 0.0296(15) C7 0.0494(14) 0.0449(14) 0.0385(13) 0.0112(11) 0.0154(11) 0.0176(11) C8 0.0549(16) 0.0469(15) 0.0481(15) 0.0190(12) 0.0198(13) 0.0132(12) C9 0.079(2) 0.0579(19) 0.072(2) 0.0312(17) -0.0060(17) 0.0248(17) C10 0.089(3) 0.0470(17) 0.080(2) 0.0263(17) -0.0108(19) 0.0240(17) C11 0.080(2) 0.0456(16) 0.067(2) 0.0168(15) 0.0221(17) 0.0311(15) C12 0.0617(18) 0.0571(17) 0.0621(18) 0.0245(15) 0.0275(15) 0.0306(14) C13 0.0517(16) 0.0544(16) 0.0623(18) 0.0275(14) 0.0176(14) 0.0186(13) C14 0.0490(15) 0.0550(16) 0.0528(16) 0.0305(14) 0.0158(12) 0.0141(12) C15 0.066(2) 0.072(2) 0.0572(18) 0.0338(17) 0.0096(15) 0.0158(16) C16 0.066(2) 0.095(3) 0.067(2) 0.053(2) 0.0062(17) 0.0190(19) C17 0.065(2) 0.100(3) 0.083(2) 0.065(2) 0.0227(18) 0.038(2) C18 0.068(2) 0.071(2) 0.069(2) 0.0442(17) 0.0251(16) 0.0346(16) C19 0.0495(15) 0.0588(16) 0.0522(15) 0.0344(14) 0.0159(12) 0.0189(13) C20 0.076(2) 0.0501(16) 0.0612(18) 0.0262(15) 0.0156(16) 0.0255(15) Cl 0.0776(12) 0.0962(16) 0.0856(15) 0.0610(14) 0.0151(10) 0.0271(11) O3 0.201(5) 0.180(4) 0.133(3) 0.091(3) 0.045(3) 0.109(4) O4 0.079(4) 0.114(5) 0.109(5) 0.044(4) 0.002(4) 0.030(4) O5 0.078(4) 0.137(6) 0.145(6) 0.100(5) 0.009(4) 0.033(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 Ag S1 2.7299(7) 2_666 ? Ag S1 2.7299(7) . ? Ag S3 2.7917(8) . ? Ag S3 2.7917(8) 2_666 ? Ag S2 2.8596(8) 2_666 ? Ag S2 2.8596(8) . ? S1 C9 1.823(3) . ? S1 C8 1.834(3) . ? S2 C11 1.808(4) . ? S2 C10 1.823(3) . ? S3 C12 1.807(3) . ? S3 C13 1.814(3) . ? O1 C2 1.363(3) . ? O1 C1 1.420(4) . ? O2 C19 1.368(3) . ? O2 C20 1.420(4) . ? C1 C20 1.491(5) . ? C2 C3 1.391(4) . ? C2 C7 1.394(4) . ? C3 C4 1.380(4) . ? C4 C5 1.371(5) . ? C5 C6 1.390(5) . ? C6 C7 1.391(4) . ? C7 C8 1.500(4) . ? C9 C10 1.473(5) . ? C11 C12 1.513(4) . ? C13 C14 1.507(4) . ? C14 C15 1.381(4) . ? C14 C19 1.392(4) . ? C15 C16 1.389(5) . ? C16 C17 1.367(5) . ? C17 C18 1.381(5) . ? C18 C19 1.394(4) . ? Cl Cl 1.131(4) 2_565 ? Cl O3 1.284(5) 2_565 ? Cl O4 1.394(7) . ? Cl O5 1.405(6) . ? Cl O3 1.453(6) . ? O3 Cl 1.284(5) 2_565 ? 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 Ag S1 180.0 2_666 . ? S1 Ag S3 90.15(2) 2_666 . ? S1 Ag S3 89.85(2) . . ? S1 Ag S3 89.85(2) 2_666 2_666 ? S1 Ag S3 90.15(2) . 2_666 ? S3 Ag S3 180.0 . 2_666 ? S1 Ag S2 76.00(2) 2_666 2_666 ? S1 Ag S2 104.00(2) . 2_666 ? S3 Ag S2 103.65(2) . 2_666 ? S3 Ag S2 76.35(2) 2_666 2_666 ? S1 Ag S2 104.00(2) 2_666 . ? S1 Ag S2 76.00(2) . . ? S3 Ag S2 76.35(2) . . ? S3 Ag S2 103.65(2) 2_666 . ? S2 Ag S2 180.0 2_666 . ? C9 S1 C8 97.90(15) . . ? C9 S1 Ag 97.08(12) . . ? C8 S1 Ag 108.65(10) . . ? C11 S2 C10 100.03(19) . . ? C11 S2 Ag 102.10(10) . . ? C10 S2 Ag 102.08(10) . . ? C12 S3 C13 99.44(14) . . ? C12 S3 Ag 99.28(10) . . ? C13 S3 Ag 110.99(11) . . ? C2 O1 C1 117.6(2) . . ? C19 O2 C20 118.0(2) . . ? O1 C1 C20 108.4(3) . . ? O1 C2 C3 124.5(3) . . ? O1 C2 C7 114.9(2) . . ? C3 C2 C7 120.6(3) . . ? C4 C3 C2 119.6(3) . . ? C5 C4 C3 120.5(3) . . ? C4 C5 C6 120.3(3) . . ? C5 C6 C7 120.2(3) . . ? C6 C7 C2 118.8(3) . . ? C6 C7 C8 122.2(3) . . ? C2 C7 C8 119.0(3) . . ? C7 C8 S1 112.05(19) . . ? C10 C9 S1 113.6(3) . . ? C9 C10 S2 116.0(3) . . ? C12 C11 S2 116.3(2) . . ? C11 C12 S3 111.5(2) . . ? C14 C13 S3 108.6(2) . . ? C15 C14 C19 118.3(3) . . ? C15 C14 C13 120.6(3) . . ? C19 C14 C13 121.0(3) . . ? C14 C15 C16 122.0(3) . . ? C17 C16 C15 118.6(3) . . ? C16 C17 C18 121.1(3) . . ? C17 C18 C19 119.8(3) . . ? O2 C19 C14 115.7(3) . . ? O2 C19 C18 124.2(3) . . ? C14 C19 C18 120.1(3) . . ? O2 C20 C1 108.1(3) . . ? Cl Cl O3 73.7(3) 2_565 2_565 ? Cl Cl O4 123.6(4) 2_565 . ? O3 Cl O4 105.1(4) 2_565 . ? Cl Cl O5 126.7(4) 2_565 . ? O3 Cl O5 106.5(4) 2_565 . ? O4 Cl O5 108.0(4) . . ? Cl Cl O3 58.0(3) 2_565 . ? O3 Cl O3 131.7(3) 2_565 . ? O4 Cl O3 101.6(4) . . ? O5 Cl O3 102.4(4) . . ? Cl O3 Cl 48.3(3) 2_565 . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.643 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.060 data_2a _database_code_depnum_ccdc_archive 'CCDC 271049' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H27 Ag Cl N O7 S2' _chemical_formula_weight 624.89 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6319(10) _cell_length_b 21.039(2) _cell_length_c 11.8585(11) _cell_angle_alpha 90.00 _cell_angle_beta 107.158(2) _cell_angle_gamma 90.00 _cell_volume 2534.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6159 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 28.36 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 1.108 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16246 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.36 _reflns_number_total 6159 _reflns_number_gt 4961 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0497P)^2^+2.4655P] 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 6159 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1123 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.08430(3) 0.938368(12) 0.47202(2) 0.05129(10) Uani 1 1 d . . . S1 S 0.16998(8) 1.01458(4) 0.34902(7) 0.04617(18) Uani 1 1 d . . . S2 S -0.12196(8) 0.87602(4) 0.43854(8) 0.05006(19) Uani 1 1 d . . . O1 O 0.3591(2) 0.88117(11) 0.4771(2) 0.0510(5) Uani 1 1 d . . . O2 O -0.0313(2) 0.91314(11) 0.2181(2) 0.0509(5) Uani 1 1 d . . . O3 O 0.1935(2) 0.81956(12) 0.6021(2) 0.0530(6) Uani 1 1 d . . . N1 N 0.1950(3) 0.97170(15) 0.6620(3) 0.0632(8) Uani 1 1 d . . . C1 C 0.3815(4) 0.82018(18) 0.5347(3) 0.0541(8) Uani 1 1 d . . . H1A H 0.4736 0.8101 0.5576 0.065 Uiso 1 1 calc R . . H1B H 0.3346 0.7877 0.4820 0.065 Uiso 1 1 calc R . . C2 C 0.3999(3) 0.88706(15) 0.3784(3) 0.0429(6) Uani 1 1 d . . . C3 C 0.4463(3) 0.83609(17) 0.3265(3) 0.0534(8) Uani 1 1 d . . . H3 H 0.4545 0.7947 0.3620 0.064 Uiso 1 1 calc R . . C4 C 0.4803(4) 0.8453(2) 0.2240(3) 0.0606(9) Uani 1 1 d . . . H4 H 0.5112 0.8102 0.1879 0.073 Uiso 1 1 calc R . . C5 C 0.4701(4) 0.9042(2) 0.1738(3) 0.0625(10) Uani 1 1 d . . . H5 H 0.4912 0.9102 0.1012 0.075 Uiso 1 1 calc R . . C6 C 0.4296(4) 0.95508(19) 0.2275(3) 0.0569(8) Uani 1 1 d . . . H6 H 0.4266 0.9966 0.1932 0.068 Uiso 1 1 calc R . . C7 C 0.3928(3) 0.94793(15) 0.3303(3) 0.0444(7) Uani 1 1 d . . . C8 C 0.3481(3) 1.00428(16) 0.3845(3) 0.0516(7) Uani 1 1 d . . . H8A H 0.3844 1.0418 0.3600 0.062 Uiso 1 1 calc R . . H8B H 0.3840 1.0012 0.4687 0.062 Uiso 1 1 calc R . . C9 C 0.1097(4) 0.9948(2) 0.1941(3) 0.0571(8) Uani 1 1 d . . . H9A H 0.0341 1.0207 0.1581 0.069 Uiso 1 1 calc R . . H9B H 0.1764 1.0052 0.1574 0.069 Uiso 1 1 calc R . . C10 C 0.0723(4) 0.9260(2) 0.1700(3) 0.0592(9) Uani 1 1 d . . . H10A H 0.0445 0.9181 0.0866 0.071 Uiso 1 1 calc R . . H10B H 0.1463 0.8991 0.2059 0.071 Uiso 1 1 calc R . . C11 C -0.0546(4) 0.84796(17) 0.2334(3) 0.0576(9) Uani 1 1 d . . . H11A H 0.0234 0.8282 0.2833 0.069 Uiso 1 1 calc R . . H11B H -0.0795 0.8265 0.1586 0.069 Uiso 1 1 calc R . . C12 C -0.1635(4) 0.84455(18) 0.2892(3) 0.0583(9) Uani 1 1 d . . . H12A H -0.1897 0.8009 0.2906 0.070 Uiso 1 1 calc R . . H12B H -0.2379 0.8676 0.2407 0.070 Uiso 1 1 calc R . . C13 C -0.0738(4) 0.80239(17) 0.5218(3) 0.0559(8) Uani 1 1 d . . . H13A H -0.1509 0.7772 0.5157 0.067 Uiso 1 1 calc R . . H13B H -0.0170 0.7785 0.4881 0.067 Uiso 1 1 calc R . . C14 C -0.0045(3) 0.81508(14) 0.6490(3) 0.0478(7) Uani 1 1 d . . . C15 C -0.0739(4) 0.82071(16) 0.7309(4) 0.0578(9) Uani 1 1 d . . . H15 H -0.1682 0.8183 0.7048 0.069 Uiso 1 1 calc R . . C16 C -0.0096(5) 0.82970(18) 0.8498(4) 0.0654(10) Uani 1 1 d . . . H16 H -0.0591 0.8349 0.9050 0.078 Uiso 1 1 calc R . . C17 C 0.1240(5) 0.83112(18) 0.8875(3) 0.0631(10) Uani 1 1 d . . . H17 H 0.1688 0.8350 0.9703 0.076 Uiso 1 1 calc R . . C18 C 0.1968(4) 0.82701(17) 0.8079(3) 0.0550(8) Uani 1 1 d . . . H18 H 0.2912 0.8286 0.8353 0.066 Uiso 1 1 calc R . . C19 C 0.1325(3) 0.82063(15) 0.6892(3) 0.0472(7) Uani 1 1 d . . . C20 C 0.3339(3) 0.82362(19) 0.6409(3) 0.0549(8) Uani 1 1 d . . . H20A H 0.3701 0.7892 0.6937 0.066 Uiso 1 1 calc R . . H20B H 0.3611 0.8629 0.6820 0.066 Uiso 1 1 calc R . . C21 C 0.2340(3) 0.97985(16) 0.7596(3) 0.0514(8) Uani 1 1 d . . . C22 C 0.2832(4) 0.9888(2) 0.8863(3) 0.0627(9) Uani 1 1 d . . . H22A H 0.2348 0.9622 0.9245 0.075 Uiso 1 1 calc R . . H22B H 0.2726 1.0325 0.9051 0.075 Uiso 1 1 calc R . . H22C H 0.3748 0.9777 0.9132 0.075 Uiso 1 1 calc R . . Cl Cl 0.36825(8) 1.15292(5) 0.09065(8) 0.0560(2) Uani 1 1 d . . . O4 O 0.3639(4) 1.1848(3) 0.1908(4) 0.141(2) Uani 1 1 d . . . O5 O 0.2506(4) 1.1222(3) 0.0335(5) 0.148(2) Uani 1 1 d . . . O6 O 0.4702(4) 1.1097(3) 0.1069(4) 0.1309(17) Uani 1 1 d . . . O7 O 0.3867(10) 1.1967(3) 0.0129(7) 0.240(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.05959(17) 0.05124(16) 0.03965(14) -0.00328(10) 0.00939(10) -0.00510(11) S1 0.0524(4) 0.0413(4) 0.0443(4) -0.0005(3) 0.0135(3) 0.0060(3) S2 0.0506(4) 0.0449(4) 0.0523(4) -0.0025(3) 0.0114(3) 0.0027(3) O1 0.0634(14) 0.0510(13) 0.0438(12) 0.0076(10) 0.0236(11) 0.0096(11) O2 0.0477(12) 0.0519(13) 0.0494(12) -0.0103(10) 0.0084(10) 0.0031(10) O3 0.0544(13) 0.0650(15) 0.0444(12) 0.0049(10) 0.0218(10) 0.0049(11) N1 0.079(2) 0.0546(18) 0.0459(17) -0.0067(13) 0.0033(15) 0.0059(16) C1 0.058(2) 0.0553(19) 0.0528(19) 0.0122(15) 0.0224(16) 0.0180(16) C2 0.0392(15) 0.0507(17) 0.0394(15) -0.0007(12) 0.0124(12) -0.0014(13) C3 0.0565(19) 0.0511(18) 0.058(2) 0.0013(15) 0.0248(16) 0.0026(15) C4 0.060(2) 0.070(2) 0.062(2) -0.0061(18) 0.0335(18) 0.0025(18) C5 0.061(2) 0.080(3) 0.056(2) 0.0064(19) 0.0322(18) 0.0029(19) C6 0.0531(19) 0.063(2) 0.060(2) 0.0114(17) 0.0236(16) -0.0019(16) C7 0.0381(15) 0.0503(17) 0.0434(16) 0.0006(13) 0.0100(12) -0.0032(13) C8 0.0492(18) 0.0463(17) 0.0555(19) -0.0043(14) 0.0098(14) -0.0078(14) C9 0.0549(19) 0.075(2) 0.0384(16) 0.0089(16) 0.0094(14) 0.0064(17) C10 0.054(2) 0.081(3) 0.0393(17) -0.0141(16) 0.0094(14) 0.0070(18) C11 0.064(2) 0.053(2) 0.0473(18) -0.0140(15) 0.0032(15) 0.0044(16) C12 0.055(2) 0.0526(19) 0.056(2) -0.0078(16) -0.0011(16) -0.0039(16) C13 0.063(2) 0.0401(16) 0.064(2) -0.0009(15) 0.0174(17) -0.0047(15) C14 0.0586(19) 0.0329(14) 0.0561(19) 0.0057(13) 0.0233(15) 0.0006(13) C15 0.064(2) 0.0434(17) 0.076(2) 0.0146(16) 0.0366(19) 0.0048(16) C16 0.090(3) 0.053(2) 0.069(2) 0.0126(18) 0.048(2) 0.009(2) C17 0.093(3) 0.056(2) 0.0471(19) 0.0105(16) 0.0312(19) 0.009(2) C18 0.064(2) 0.0554(19) 0.0476(18) 0.0098(15) 0.0200(16) 0.0063(16) C19 0.0579(19) 0.0405(15) 0.0487(17) 0.0092(13) 0.0243(14) 0.0066(14) C20 0.0532(19) 0.068(2) 0.0449(17) 0.0159(16) 0.0166(14) 0.0171(16) C21 0.0555(19) 0.0445(17) 0.0478(18) -0.0002(14) 0.0053(14) 0.0059(14) C22 0.066(2) 0.070(2) 0.0426(18) -0.0037(16) 0.0008(16) 0.0009(19) Cl 0.0486(4) 0.0660(5) 0.0505(4) -0.0109(4) 0.0104(3) 0.0057(4) O4 0.082(2) 0.243(6) 0.098(3) -0.095(3) 0.027(2) 0.001(3) O5 0.075(2) 0.201(5) 0.153(4) -0.100(4) 0.007(3) -0.016(3) O6 0.102(3) 0.162(4) 0.110(3) -0.028(3) 0.001(2) 0.065(3) O7 0.471(14) 0.099(4) 0.220(7) 0.016(4) 0.208(9) -0.026(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N1 2.321(3) . ? Ag S2 2.4847(9) . ? Ag S1 2.5124(9) . ? Ag Ag 3.3288(6) 3_576 ? S1 C9 1.806(4) . ? S1 C8 1.827(3) . ? S2 C12 1.819(4) . ? S2 C13 1.827(4) . ? O1 C2 1.368(4) . ? O1 C1 1.440(4) . ? O2 C10 1.407(4) . ? O2 C11 1.415(4) . ? O3 C19 1.373(4) . ? O3 C20 1.429(4) . ? N1 C21 1.122(4) . ? C1 C20 1.491(5) . ? C2 C7 1.395(4) . ? C2 C3 1.397(5) . ? C3 C4 1.379(5) . ? C4 C5 1.366(6) . ? C5 C6 1.377(6) . ? C6 C7 1.394(5) . ? C7 C8 1.492(5) . ? C9 C10 1.508(6) . ? C11 C12 1.495(5) . ? C13 C14 1.495(5) . ? C14 C15 1.387(5) . ? C14 C19 1.397(5) . ? C15 C16 1.386(6) . ? C16 C17 1.358(6) . ? C17 C18 1.388(5) . ? C18 C19 1.377(5) . ? C21 C22 1.450(5) . ? Cl O7 1.358(6) . ? Cl O4 1.376(3) . ? Cl O6 1.384(4) . ? Cl O5 1.394(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag S2 119.05(9) . . ? N1 Ag S1 101.76(9) . . ? S2 Ag S1 134.28(3) . . ? N1 Ag Ag 73.73(8) . 3_576 ? S2 Ag Ag 86.64(2) . 3_576 ? S1 Ag Ag 85.83(2) . 3_576 ? C9 S1 C8 103.87(17) . . ? C9 S1 Ag 111.29(13) . . ? C8 S1 Ag 108.60(12) . . ? C12 S2 C13 99.59(17) . . ? C12 S2 Ag 107.29(13) . . ? C13 S2 Ag 105.55(12) . . ? C2 O1 C1 115.9(2) . . ? C10 O2 C11 115.1(3) . . ? C19 O3 C20 116.0(3) . . ? C21 N1 Ag 167.2(3) . . ? O1 C1 C20 107.9(3) . . ? O1 C2 C7 116.1(3) . . ? O1 C2 C3 123.4(3) . . ? C7 C2 C3 120.5(3) . . ? C4 C3 C2 119.9(3) . . ? C5 C4 C3 120.3(4) . . ? C4 C5 C6 119.9(3) . . ? C5 C6 C7 121.8(4) . . ? C6 C7 C2 117.5(3) . . ? C6 C7 C8 119.9(3) . . ? C2 C7 C8 122.6(3) . . ? C7 C8 S1 115.8(2) . . ? C10 C9 S1 114.1(3) . . ? O2 C10 C9 107.6(3) . . ? O2 C11 C12 106.9(3) . . ? C11 C12 S2 114.6(2) . . ? C14 C13 S2 111.7(2) . . ? C15 C14 C19 118.0(3) . . ? C15 C14 C13 121.1(3) . . ? C19 C14 C13 120.9(3) . . ? C16 C15 C14 121.3(4) . . ? C17 C16 C15 119.5(3) . . ? C16 C17 C18 120.9(4) . . ? C19 C18 C17 119.5(4) . . ? O3 C19 C18 124.6(3) . . ? O3 C19 C14 114.7(3) . . ? C18 C19 C14 120.7(3) . . ? O3 C20 C1 107.9(3) . . ? N1 C21 C22 178.6(4) . . ? O7 Cl O4 107.6(4) . . ? O7 Cl O6 106.0(5) . . ? O4 Cl O6 115.1(3) . . ? O7 Cl O5 105.8(5) . . ? O4 Cl O5 113.1(3) . . ? O6 Cl O5 108.5(3) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.876 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.075 data_2b _database_code_depnum_ccdc_archive 'CCDC 271050' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H56 Ag4 Cl4 O24 S4' _chemical_formula_weight 1646.39 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.310(2) _cell_length_b 12.6134(12) _cell_length_c 18.2148(18) _cell_angle_alpha 90.00 _cell_angle_beta 92.659(2) _cell_angle_gamma 90.00 _cell_volume 5579.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 13691 _cell_measurement_theta_min 0.84 _cell_measurement_theta_max 28.58 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.960 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3280 _exptl_absorpt_coefficient_mu 1.805 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36083 _diffrn_reflns_av_R_equivalents 0.1117 _diffrn_reflns_av_sigmaI/netI 0.1028 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 0.84 _diffrn_reflns_theta_max 28.58 _reflns_number_total 13691 _reflns_number_gt 6437 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1008P)^2^+4.6212P] 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 13691 _refine_ls_number_parameters 722 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1573 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.2212 _refine_ls_wR_factor_gt 0.1725 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 0.11972(4) 0.79695(6) 0.12649(5) 0.0917(3) Uani 1 1 d . . . Ag2 Ag 0.34223(3) 0.28834(5) 0.08111(4) 0.0586(2) Uani 1 1 d . . . Ag3 Ag 0.24492(3) 0.56435(6) 0.12943(4) 0.0673(2) Uani 1 1 d . . . Ag4 Ag 0.25404(3) 1.01531(8) 0.13967(4) 0.0795(3) Uani 1 1 d . . . Cl1 Cl 0.23838(10) 0.78766(17) 0.00658(13) 0.0606(6) Uani 1 1 d . . . Cl2 Cl 0.36289(11) 0.9556(2) 0.26676(14) 0.0753(7) Uani 1 1 d . . . Cl3 Cl 0.01368(10) 1.2466(2) 0.24222(13) 0.0654(6) Uani 1 1 d . . . Cl4 Cl 0.22870(9) 0.30250(17) 0.20642(11) 0.0544(5) Uani 1 1 d . . . S1 S 0.15213(8) 0.62044(16) 0.16820(11) 0.0465(5) Uani 1 1 d . A . S2 S 0.15956(8) 0.96911(17) 0.16470(11) 0.0475(5) Uani 1 1 d . . . S3 S 0.30213(8) 0.46469(16) 0.04408(11) 0.0476(5) Uani 1 1 d . . . S4 S 0.31964(7) 0.09334(16) 0.05481(11) 0.0460(5) Uani 1 1 d . . . O1 O 0.0434(2) 0.6938(4) 0.0615(3) 0.0475(13) Uani 1 1 d . . . O2 O 0.1923(7) 0.7954(11) 0.2770(6) 0.062(5) Uani 0.66(4) 1 d P A 1 O2' O 0.1529(19) 0.807(2) 0.2782(14) 0.080(13) Uani 0.34(4) 1 d P A 2 O3 O 0.0614(2) 0.9225(4) 0.0316(3) 0.0466(12) Uani 1 1 d . . . O4 O 0.4391(2) 0.4115(4) 0.0509(3) 0.0564(14) Uani 1 1 d . . . O5 O 0.2766(2) 0.2621(4) -0.0493(3) 0.0538(14) Uani 1 1 d . . . O6 O 0.4453(2) 0.1821(5) 0.0149(3) 0.0570(15) Uani 1 1 d . . . O7 O 0.3971(3) 0.2434(7) 0.1894(4) 0.095(2) Uani 1 1 d . . . O8 O 0.2876(3) 0.6669(7) 0.2242(4) 0.094(2) Uani 1 1 d . . . O9 O 0.2796(6) 0.7952(10) -0.0404(7) 0.190(6) Uani 1 1 d . . . O10 O 0.1996(4) 0.8651(8) -0.0044(6) 0.149(4) Uani 1 1 d . . . O11 O 0.2161(6) 0.6878(8) -0.0026(6) 0.168(5) Uani 1 1 d . . . O12 O 0.2614(4) 0.7924(8) 0.0795(5) 0.133(4) Uani 1 1 d . . . O13 O 0.4131(4) 0.9481(16) 0.2458(8) 0.251(10) Uani 1 1 d . . . O14 O 0.3295(4) 0.8944(10) 0.2128(6) 0.155(4) Uani 1 1 d . . . O15 O 0.3594(8) 0.9278(13) 0.3336(7) 0.254(9) Uani 1 1 d . . . O16 O 0.3502(12) 1.0524(12) 0.2609(11) 0.331(14) Uani 1 1 d . . . O17 O 0.0531(4) 1.2021(8) 0.2884(5) 0.135(4) Uani 1 1 d . . . O18 O -0.0183(4) 1.1677(11) 0.2068(8) 0.178(6) Uani 1 1 d . . . O19 O 0.0402(5) 1.2946(10) 0.1871(7) 0.174(6) Uani 1 1 d . . . O20 O -0.0227(4) 1.3135(8) 0.2792(6) 0.127(3) Uani 1 1 d . . . O21 O 0.2575(6) 0.3871(8) 0.2321(6) 0.187(6) Uani 1 1 d . . . O22 O 0.2124(6) 0.3188(10) 0.1351(5) 0.188(6) Uani 1 1 d . . . O23 O 0.2619(8) 0.2240(12) 0.2076(10) 0.243(9) Uani 1 1 d . . . O24 O 0.1913(7) 0.2769(18) 0.2479(10) 0.295(12) Uani 1 1 d . . . C1 C 0.0051(3) 0.7677(6) 0.0301(5) 0.0461(18) Uani 1 1 d . . . H1A H -0.0134 0.8025 0.0689 0.055 Uiso 1 1 calc R . . H1B H -0.0222 0.7300 0.0005 0.055 Uiso 1 1 calc R . . C2 C 0.0585(3) 0.6080(6) 0.0208(4) 0.0438(17) Uani 1 1 d . . . C3 C 0.0459(3) 0.5956(6) -0.0535(4) 0.0473(18) Uani 1 1 d . . . H3 H 0.0257 0.6501 -0.0799 0.057 Uiso 1 1 calc R . . C4 C 0.0619(3) 0.5057(7) -0.0899(5) 0.054(2) Uani 1 1 d . . . H4 H 0.0521 0.4966 -0.1412 0.065 Uiso 1 1 calc R . . C5 C 0.0919(3) 0.4298(7) -0.0527(5) 0.060(2) Uani 1 1 d . . . H5 H 0.1046 0.3688 -0.0784 0.071 Uiso 1 1 calc R . . C6 C 0.1040(3) 0.4401(7) 0.0215(6) 0.061(2) Uani 1 1 d . . . H6 H 0.1243 0.3850 0.0471 0.073 Uiso 1 1 calc R . . C7 C 0.0873(3) 0.5287(6) 0.0603(4) 0.0450(18) Uani 1 1 d . . . C8 C 0.0949(3) 0.5317(6) 0.1414(5) 0.054(2) Uani 1 1 d . . . H8A H 0.1025 0.4616 0.1598 0.064 Uiso 1 1 calc R . . H8B H 0.0617 0.5564 0.1624 0.064 Uiso 1 1 calc R . . C9 C 0.1511(4) 0.6197(8) 0.2677(4) 0.063(2) Uani 1 1 d . . . H9A H 0.1201 0.5779 0.2826 0.076 Uiso 0.66(4) 1 calc PR A 1 H9B H 0.1845 0.5865 0.2878 0.076 Uiso 0.66(4) 1 calc PR A 1 H9C H 0.1133 0.6126 0.2817 0.076 Uiso 0.34(4) 1 d PR A 2 H9D H 0.1711 0.5580 0.2861 0.076 Uiso 0.34(4) 1 d PR A 2 C10 C 0.1467(10) 0.732(2) 0.2991(10) 0.060(7) Uani 0.66(4) 1 d P A 1 H10A H 0.1124 0.7646 0.2814 0.072 Uiso 0.66(4) 1 calc PR A 1 H10B H 0.1468 0.7291 0.3524 0.072 Uiso 0.66(4) 1 calc PR A 1 C10' C 0.174(2) 0.711(4) 0.302(2) 0.071(14) Uani 0.34(4) 1 d P A 2 H10C H 0.1690 0.7052 0.3544 0.085 Uiso 0.34(4) 1 calc PR A 2 H10D H 0.2133 0.7109 0.2949 0.085 Uiso 0.34(4) 1 calc PR A 2 C11 C 0.1860(5) 0.9006(9) 0.3037(5) 0.081(3) Uani 1 1 d . . . H11A H 0.2222 0.9331 0.3067 0.097 Uiso 0.66(4) 1 calc PR A 1 H11B H 0.1738 0.8956 0.3535 0.097 Uiso 0.66(4) 1 calc PR A 1 H11C H 0.2231 0.9011 0.2862 0.097 Uiso 0.34(4) 1 d PR A 2 H11D H 0.1866 0.9104 0.3566 0.097 Uiso 0.34(4) 1 d PR A 2 C12 C 0.1478(4) 0.9756(8) 0.2625(5) 0.067(3) Uani 1 1 d . A . H12A H 0.1540 1.0466 0.2799 0.081 Uiso 1 1 calc R . . H12B H 0.1103 0.9570 0.2708 0.081 Uiso 1 1 calc R . . C13 C 0.1121(3) 1.0687(6) 0.1265(5) 0.056(2) Uani 1 1 d . . . H13A H 0.0751 1.0506 0.1379 0.067 Uiso 1 1 calc R . . H13B H 0.1207 1.1365 0.1480 0.067 Uiso 1 1 calc R . . C14 C 0.1165(3) 1.0748(6) 0.0445(5) 0.0472(19) Uani 1 1 d . . . C15 C 0.1472(3) 1.1556(6) 0.0122(6) 0.061(2) Uani 1 1 d . . . H15 H 0.1674 1.2050 0.0431 0.073 Uiso 1 1 calc R . . C16 C 0.1485(4) 1.1648(7) -0.0623(6) 0.062(2) Uani 1 1 d . . . H16 H 0.1702 1.2198 -0.0829 0.074 Uiso 1 1 calc R . . C17 C 0.1202(4) 1.0990(7) -0.1069(5) 0.063(2) Uani 1 1 d . . . H17 H 0.1204 1.1085 -0.1592 0.076 Uiso 1 1 calc R . . C18 C 0.0896(3) 1.0148(6) -0.0770(5) 0.052(2) Uani 1 1 d . . . H18 H 0.0696 0.9666 -0.1090 0.063 Uiso 1 1 calc R . . C19 C 0.0888(3) 1.0023(6) -0.0024(4) 0.0436(17) Uani 1 1 d . . . C20 C 0.0314(3) 0.8503(6) -0.0166(4) 0.0443(17) Uani 1 1 d . . . H20A H 0.0560 0.8171 -0.0494 0.053 Uiso 1 1 calc R . . H20B H 0.0037 0.8878 -0.0454 0.053 Uiso 1 1 calc R . . C21 C 0.4865(3) 0.3430(7) 0.0614(5) 0.065(2) Uani 1 1 d . . . H21A H 0.4856 0.3072 0.1078 0.077 Uiso 1 1 calc R . . H21B H 0.5198 0.3838 0.0606 0.077 Uiso 1 1 calc R . . C22 C 0.4396(3) 0.5035(6) 0.0911(4) 0.0481(19) Uani 1 1 d . . . C23 C 0.4792(4) 0.5280(7) 0.1456(5) 0.058(2) Uani 1 1 d . . . H23 H 0.5089 0.4799 0.1575 0.069 Uiso 1 1 calc R . . C24 C 0.4751(4) 0.6222(8) 0.1820(5) 0.067(2) Uani 1 1 d . . . H24 H 0.5020 0.6390 0.2205 0.080 Uiso 1 1 calc R . . C25 C 0.4347(4) 0.6921(8) 0.1658(6) 0.071(3) Uani 1 1 d . . . H25 H 0.4334 0.7585 0.1914 0.085 Uiso 1 1 calc R . . C26 C 0.3952(4) 0.6671(7) 0.1118(5) 0.061(2) Uani 1 1 d . . . H26 H 0.3652 0.7153 0.1019 0.073 Uiso 1 1 calc R . . C27 C 0.3976(3) 0.5743(6) 0.0714(4) 0.0492(19) Uani 1 1 d . . . C28 C 0.3571(3) 0.5492(6) 0.0103(5) 0.0509(19) Uani 1 1 d . . . H28A H 0.3752 0.5133 -0.0282 0.061 Uiso 1 1 calc R . . H28B H 0.3415 0.6137 -0.0094 0.061 Uiso 1 1 calc R . . C29 C 0.2603(4) 0.4435(7) -0.0387(5) 0.066(3) Uani 1 1 d . . . H29A H 0.2238 0.4243 -0.0257 0.079 Uiso 1 1 calc R . . H29B H 0.2578 0.5088 -0.0657 0.079 Uiso 1 1 calc R . . C30 C 0.2822(4) 0.3589(7) -0.0874(4) 0.063(2) Uani 1 1 d . . . H30A H 0.2615 0.3570 -0.1336 0.076 Uiso 1 1 calc R . . H30B H 0.3201 0.3721 -0.0966 0.076 Uiso 1 1 calc R . . C31 C 0.3011(4) 0.1729(7) -0.0844(4) 0.055(2) Uani 1 1 d . . . H31A H 0.3401 0.1830 -0.0873 0.066 Uiso 1 1 calc R . . H31B H 0.2853 0.1633 -0.1332 0.066 Uiso 1 1 calc R . . C32 C 0.2893(3) 0.0800(7) -0.0373(4) 0.055(2) Uani 1 1 d . . . H32A H 0.3034 0.0171 -0.0594 0.066 Uiso 1 1 calc R . . H32B H 0.2502 0.0720 -0.0348 0.066 Uiso 1 1 calc R . . C33 C 0.3812(3) 0.0109(6) 0.0565(5) 0.053(2) Uani 1 1 d . . . H33A H 0.4054 0.0338 0.0966 0.064 Uiso 1 1 calc R . . H33B H 0.3707 -0.0608 0.0664 0.064 Uiso 1 1 calc R . . C34 C 0.4123(3) 0.0120(7) -0.0119(4) 0.052(2) Uani 1 1 d . . . C35 C 0.4101(4) -0.0766(7) -0.0583(5) 0.062(2) Uani 1 1 d . . . H35 H 0.3871 -0.1353 -0.0462 0.075 Uiso 1 1 calc R . . C36 C 0.4400(4) -0.0825(9) -0.1205(6) 0.073(3) Uani 1 1 d . . . H36 H 0.4380 -0.1441 -0.1514 0.088 Uiso 1 1 calc R . . C37 C 0.4728(4) 0.0016(10) -0.1373(5) 0.075(3) Uani 1 1 d . . . H37 H 0.4943 -0.0017 -0.1801 0.090 Uiso 1 1 calc R . . C38 C 0.4753(4) 0.0898(8) -0.0941(5) 0.062(2) Uani 1 1 d . . . H38 H 0.4984 0.1479 -0.1071 0.074 Uiso 1 1 calc R . . C39 C 0.4449(3) 0.0972(6) -0.0316(4) 0.0454(18) Uani 1 1 d . . . C40 C 0.4842(4) 0.2638(7) -0.0006(5) 0.061(2) Uani 1 1 d . . . H40A H 0.4733 0.2986 -0.0459 0.073 Uiso 1 1 calc R . . H40B H 0.5199 0.2332 -0.0059 0.073 Uiso 1 1 calc R . . C41 C 0.4027(6) 0.3130(10) 0.2454(7) 0.113(5) Uani 1 1 d . . . H41A H 0.4261 0.2831 0.2840 0.135 Uiso 1 1 calc R . . H41B H 0.3672 0.3279 0.2640 0.135 Uiso 1 1 calc R . . H41C H 0.4187 0.3775 0.2283 0.135 Uiso 1 1 calc R . . C42 C 0.3182(7) 0.6270(17) 0.2827(8) 0.158(7) Uani 1 1 d . . . H42A H 0.3312 0.6842 0.3137 0.190 Uiso 1 1 calc R . . H42B H 0.3491 0.5887 0.2652 0.190 Uiso 1 1 calc R . . H42C H 0.2959 0.5801 0.3103 0.190 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 0.1171(7) 0.0460(4) 0.1060(7) 0.0044(4) -0.0590(6) -0.0070(4) Ag2 0.0633(4) 0.0506(4) 0.0605(4) 0.0047(3) -0.0116(3) 0.0020(3) Ag3 0.0580(4) 0.0722(5) 0.0725(5) -0.0032(4) 0.0134(3) 0.0081(4) Ag4 0.0469(4) 0.1124(7) 0.0805(5) 0.0229(5) 0.0165(3) -0.0078(4) Cl1 0.0694(14) 0.0457(11) 0.0678(14) 0.0031(10) 0.0136(11) 0.0103(11) Cl2 0.0783(17) 0.0840(18) 0.0644(15) 0.0019(13) 0.0124(12) 0.0179(15) Cl3 0.0587(13) 0.0796(15) 0.0574(13) 0.0120(12) -0.0029(11) -0.0084(12) Cl4 0.0576(12) 0.0536(12) 0.0517(12) -0.0008(9) -0.0004(9) 0.0009(10) S1 0.0429(10) 0.0485(11) 0.0481(11) 0.0072(9) 0.0026(8) -0.0003(9) S2 0.0407(10) 0.0561(12) 0.0456(11) -0.0080(9) 0.0023(8) -0.0050(9) S3 0.0418(10) 0.0490(11) 0.0521(11) 0.0043(9) 0.0016(8) 0.0031(9) S4 0.0377(9) 0.0508(11) 0.0500(11) 0.0011(9) 0.0057(8) -0.0005(9) O1 0.044(3) 0.040(3) 0.058(3) -0.004(2) -0.005(2) 0.000(2) O2 0.038(9) 0.096(10) 0.052(6) 0.005(6) 0.000(5) -0.004(6) O2' 0.09(3) 0.073(17) 0.075(15) 0.006(12) -0.031(14) -0.014(16) O3 0.045(3) 0.048(3) 0.047(3) -0.005(2) 0.007(2) -0.007(2) O4 0.043(3) 0.054(3) 0.072(4) -0.002(3) 0.000(3) 0.005(3) O5 0.063(4) 0.045(3) 0.053(3) 0.001(3) 0.005(3) 0.001(3) O6 0.056(3) 0.061(4) 0.055(3) 0.007(3) 0.017(3) 0.006(3) O7 0.107(6) 0.112(6) 0.065(5) -0.001(4) -0.013(4) -0.003(5) O8 0.083(5) 0.108(6) 0.090(5) -0.004(4) -0.016(4) -0.006(5) O9 0.198(12) 0.206(13) 0.178(12) 0.039(9) 0.130(11) 0.019(10) O10 0.162(9) 0.140(8) 0.142(8) -0.008(7) -0.037(7) 0.100(8) O11 0.262(15) 0.105(7) 0.134(9) 0.017(6) -0.026(9) -0.075(9) O12 0.135(8) 0.150(9) 0.110(7) -0.019(6) -0.030(6) 0.036(7) O13 0.067(6) 0.44(3) 0.243(16) -0.169(17) -0.001(8) -0.009(10) O14 0.143(9) 0.181(11) 0.133(8) 0.003(8) -0.062(7) -0.032(8) O15 0.42(3) 0.264(18) 0.081(8) 0.008(9) 0.047(11) -0.104(18) O16 0.58(4) 0.135(12) 0.29(2) -0.021(13) 0.06(2) 0.135(19) O17 0.151(9) 0.142(9) 0.109(7) 0.013(6) -0.048(6) 0.048(7) O18 0.099(7) 0.208(12) 0.227(13) -0.123(11) -0.009(8) -0.040(8) O19 0.142(9) 0.207(12) 0.177(11) 0.120(9) 0.070(8) 0.042(8) O20 0.112(7) 0.141(8) 0.127(8) -0.034(6) -0.006(6) 0.040(6) O21 0.312(16) 0.117(8) 0.120(8) 0.025(6) -0.109(9) -0.100(10) O22 0.288(16) 0.169(10) 0.097(7) 0.035(7) -0.090(9) -0.107(11) O23 0.274(19) 0.180(13) 0.268(19) -0.074(13) -0.067(15) 0.110(14) O24 0.176(13) 0.50(3) 0.217(17) -0.043(18) 0.128(13) -0.093(18) C1 0.027(3) 0.041(4) 0.070(5) -0.007(4) 0.004(3) 0.004(3) C2 0.031(3) 0.037(4) 0.063(5) -0.004(4) 0.001(3) 0.001(3) C3 0.043(4) 0.041(4) 0.058(5) 0.008(4) 0.001(4) 0.000(4) C4 0.050(5) 0.056(5) 0.057(5) -0.010(4) 0.010(4) -0.012(4) C5 0.050(5) 0.061(6) 0.069(6) -0.018(5) 0.016(4) 0.000(4) C6 0.038(4) 0.042(5) 0.104(8) 0.000(5) 0.000(4) 0.001(4) C7 0.036(4) 0.033(4) 0.065(5) 0.000(3) -0.005(3) -0.007(3) C8 0.049(4) 0.042(4) 0.070(6) 0.010(4) 0.001(4) -0.005(4) C9 0.059(5) 0.083(7) 0.047(5) 0.013(5) 0.002(4) 0.006(5) C10 0.043(11) 0.10(2) 0.038(8) -0.016(10) 0.017(8) -0.007(11) C10' 0.07(3) 0.10(3) 0.050(17) -0.003(18) 0.01(2) 0.03(3) C11 0.109(8) 0.090(8) 0.044(5) -0.019(5) 0.000(5) -0.012(7) C12 0.068(6) 0.082(7) 0.053(5) -0.017(5) 0.016(4) -0.014(5) C13 0.042(4) 0.049(5) 0.075(6) -0.020(4) -0.012(4) 0.002(4) C14 0.034(4) 0.038(4) 0.069(5) -0.002(4) -0.001(3) 0.008(3) C15 0.043(4) 0.036(4) 0.102(8) -0.007(5) -0.011(5) 0.004(4) C16 0.053(5) 0.042(5) 0.091(7) 0.009(5) 0.007(5) 0.002(4) C17 0.064(5) 0.048(5) 0.078(6) 0.009(5) 0.016(5) 0.014(5) C18 0.051(4) 0.041(4) 0.066(6) -0.003(4) 0.009(4) 0.009(4) C19 0.040(4) 0.033(4) 0.059(5) -0.006(3) 0.012(3) 0.000(3) C20 0.034(4) 0.043(4) 0.055(5) -0.003(3) -0.008(3) 0.001(3) C21 0.047(5) 0.060(5) 0.088(7) 0.015(5) 0.013(5) 0.009(4) C22 0.042(4) 0.046(5) 0.056(5) 0.012(4) 0.007(4) -0.001(4) C23 0.055(5) 0.062(5) 0.055(5) 0.005(4) -0.001(4) -0.002(4) C24 0.071(6) 0.073(7) 0.054(5) 0.004(5) -0.001(4) -0.022(6) C25 0.071(6) 0.058(6) 0.086(7) -0.011(5) 0.029(6) -0.014(5) C26 0.046(5) 0.056(5) 0.082(6) 0.002(5) 0.025(5) 0.000(4) C27 0.042(4) 0.049(5) 0.059(5) 0.004(4) 0.016(4) -0.004(4) C28 0.041(4) 0.049(5) 0.063(5) 0.013(4) 0.004(4) 0.003(4) C29 0.067(6) 0.059(5) 0.069(6) 0.016(5) -0.026(5) 0.006(5) C30 0.086(6) 0.060(5) 0.043(5) 0.016(4) -0.013(4) 0.002(5) C31 0.058(5) 0.063(5) 0.042(4) 0.000(4) -0.003(4) 0.004(4) C32 0.048(5) 0.055(5) 0.062(5) -0.013(4) -0.010(4) 0.006(4) C33 0.052(5) 0.042(4) 0.066(5) 0.007(4) 0.016(4) 0.002(4) C34 0.042(4) 0.059(5) 0.054(5) 0.005(4) 0.002(4) 0.012(4) C35 0.060(5) 0.053(5) 0.074(6) 0.005(4) -0.003(5) 0.006(4) C36 0.065(6) 0.083(7) 0.071(6) -0.018(5) 0.007(5) 0.015(6) C37 0.061(6) 0.115(9) 0.050(5) -0.002(6) 0.011(4) 0.018(6) C38 0.061(5) 0.069(6) 0.056(5) 0.008(5) 0.011(4) 0.008(5) C39 0.034(4) 0.053(5) 0.050(4) 0.011(4) 0.008(3) 0.008(4) C40 0.048(5) 0.052(5) 0.085(7) 0.006(5) 0.029(5) 0.004(4) C41 0.152(13) 0.106(10) 0.081(8) -0.011(7) 0.008(8) -0.020(9) C42 0.128(12) 0.23(2) 0.117(12) -0.016(13) -0.040(10) 0.009(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 2.465(2) . ? Ag1 S1 2.470(2) . ? Ag1 O1 2.516(5) . ? Ag2 O7 2.398(7) . ? Ag2 S3 2.508(2) . ? Ag2 S4 2.561(2) . ? Ag3 O8 2.358(8) . ? Ag3 S3 2.476(2) . ? Ag3 S1 2.497(2) . ? Ag4 S2 2.433(2) . ? Ag4 S4 2.476(2) 1_565 ? Cl1 O9 1.352(10) . ? Cl1 O10 1.366(8) . ? Cl1 O11 1.378(10) . ? Cl1 O12 1.418(9) . ? Cl2 O16 1.262(14) . ? Cl2 O15 1.273(12) . ? Cl2 O13 1.298(11) . ? Cl2 O14 1.465(10) . ? Cl3 O19 1.360(9) . ? Cl3 O17 1.367(8) . ? Cl3 O18 1.402(9) . ? Cl3 O20 1.417(9) . ? Cl4 O24 1.251(13) . ? Cl4 O23 1.278(14) . ? Cl4 O21 1.349(9) . ? Cl4 O22 1.355(9) . ? S1 C9 1.813(8) . ? S1 C8 1.835(8) . ? S2 C12 1.818(8) . ? S2 C13 1.821(8) . ? S3 C29 1.799(8) . ? S3 C28 1.837(8) . ? S4 C32 1.809(8) . ? S4 C33 1.821(8) . ? S4 Ag4 2.476(2) 1_545 ? O1 C2 1.373(9) . ? O1 C1 1.419(8) . ? O2 C11 1.424(16) . ? O2 C10 1.44(3) . ? O2' C10' 1.38(7) . ? O2' C11 1.49(3) . ? O3 C19 1.371(9) . ? O3 C20 1.439(8) . ? O4 C22 1.372(10) . ? O4 C21 1.446(9) . ? O5 C30 1.415(10) . ? O5 C31 1.436(10) . ? O6 C39 1.366(9) . ? O6 C40 1.436(10) . ? O7 C41 1.348(13) . ? O8 C42 1.368(16) . ? C1 C20 1.507(11) . ? C2 C3 1.382(10) . ? C2 C7 1.400(10) . ? C3 C4 1.380(11) . ? C4 C5 1.364(12) . ? C5 C6 1.375(13) . ? C6 C7 1.393(11) . ? C7 C8 1.481(11) . ? C9 C10' 1.41(5) . ? C9 C10 1.54(3) . ? C11 C12 1.502(14) . ? C13 C14 1.505(11) . ? C14 C19 1.402(10) . ? C14 C15 1.408(12) . ? C15 C16 1.364(13) . ? C16 C17 1.330(12) . ? C17 C18 1.420(12) . ? C18 C19 1.367(11) . ? C21 C40 1.507(13) . ? C22 C23 1.384(11) . ? C22 C27 1.391(11) . ? C23 C24 1.367(13) . ? C24 C25 1.341(13) . ? C25 C26 1.380(14) . ? C26 C27 1.385(12) . ? C27 C28 1.485(11) . ? C29 C30 1.501(13) . ? C31 C32 1.489(11) . ? C33 C34 1.489(11) . ? C34 C39 1.392(11) . ? C34 C35 1.401(12) . ? C35 C36 1.376(13) . ? C36 C37 1.369(14) . ? C37 C38 1.363(14) . ? C38 C39 1.387(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Ag1 S1 126.28(7) . . ? S2 Ag1 O1 149.29(13) . . ? S1 Ag1 O1 84.05(12) . . ? O7 Ag2 S3 128.7(2) . . ? O7 Ag2 S4 91.9(2) . . ? S3 Ag2 S4 136.40(7) . . ? O8 Ag3 S3 119.8(2) . . ? O8 Ag3 S1 90.6(2) . . ? S3 Ag3 S1 149.59(7) . . ? S2 Ag4 S4 148.56(7) . 1_565 ? O9 Cl1 O10 112.6(8) . . ? O9 Cl1 O11 106.6(8) . . ? O10 Cl1 O11 111.8(8) . . ? O9 Cl1 O12 108.6(9) . . ? O10 Cl1 O12 110.3(6) . . ? O11 Cl1 O12 106.7(6) . . ? O16 Cl2 O15 108.7(12) . . ? O16 Cl2 O13 106.0(15) . . ? O15 Cl2 O13 111.5(12) . . ? O16 Cl2 O14 109.1(13) . . ? O15 Cl2 O14 115.9(9) . . ? O13 Cl2 O14 105.2(8) . . ? O19 Cl3 O17 107.1(7) . . ? O19 Cl3 O18 104.4(9) . . ? O17 Cl3 O18 110.5(8) . . ? O19 Cl3 O20 114.4(7) . . ? O17 Cl3 O20 112.8(6) . . ? O18 Cl3 O20 107.3(6) . . ? O24 Cl4 O23 105.5(14) . . ? O24 Cl4 O21 112.0(11) . . ? O23 Cl4 O21 106.9(10) . . ? O24 Cl4 O22 115.5(11) . . ? O23 Cl4 O22 106.8(11) . . ? O21 Cl4 O22 109.7(6) . . ? C9 S1 C8 102.5(4) . . ? C9 S1 Ag1 107.0(3) . . ? C8 S1 Ag1 103.9(3) . . ? C9 S1 Ag3 109.6(3) . . ? C8 S1 Ag3 115.9(3) . . ? Ag1 S1 Ag3 116.61(8) . . ? C12 S2 C13 102.6(4) . . ? C12 S2 Ag4 111.4(3) . . ? C13 S2 Ag4 110.5(3) . . ? C12 S2 Ag1 103.8(3) . . ? C13 S2 Ag1 105.4(3) . . ? Ag4 S2 Ag1 121.34(9) . . ? C29 S3 C28 101.4(4) . . ? C29 S3 Ag3 106.8(3) . . ? C28 S3 Ag3 110.7(3) . . ? C29 S3 Ag2 106.9(3) . . ? C28 S3 Ag2 109.0(3) . . ? Ag3 S3 Ag2 120.26(8) . . ? C32 S4 C33 105.2(4) . . ? C32 S4 Ag4 107.2(3) . 1_545 ? C33 S4 Ag4 108.4(3) . 1_545 ? C32 S4 Ag2 109.7(3) . . ? C33 S4 Ag2 112.1(3) . . ? Ag4 S4 Ag2 113.82(8) 1_545 . ? C2 O1 C1 119.1(6) . . ? C2 O1 Ag1 116.9(4) . . ? C1 O1 Ag1 107.8(4) . . ? C11 O2 C10 108.9(16) . . ? C10' O2' C11 114(4) . . ? C19 O3 C20 115.6(6) . . ? C22 O4 C21 116.5(6) . . ? C30 O5 C31 114.0(6) . . ? C39 O6 C40 115.2(6) . . ? C41 O7 Ag2 120.1(8) . . ? C42 O8 Ag3 125.0(10) . . ? O1 C1 C20 113.2(6) . . ? O1 C2 C3 124.4(7) . . ? O1 C2 C7 115.2(7) . . ? C3 C2 C7 120.4(7) . . ? C4 C3 C2 120.6(7) . . ? C5 C4 C3 119.6(8) . . ? C4 C5 C6 120.5(8) . . ? C5 C6 C7 121.3(8) . . ? C6 C7 C2 117.6(8) . . ? C6 C7 C8 120.0(7) . . ? C2 C7 C8 122.1(7) . . ? C7 C8 S1 109.8(5) . . ? C10' C9 C10 27.7(15) . . ? C10' C9 S1 114.5(19) . . ? C10 C9 S1 111.9(10) . . ? O2 C10 C9 109.8(16) . . ? O2' C10' C9 116(4) . . ? O2 C11 O2' 38.9(14) . . ? O2 C11 C12 119.3(9) . . ? O2' C11 C12 91.7(15) . . ? C11 C12 S2 109.9(6) . . ? C14 C13 S2 110.0(5) . . ? C19 C14 C15 117.8(8) . . ? C19 C14 C13 121.2(7) . . ? C15 C14 C13 121.0(7) . . ? C16 C15 C14 120.9(8) . . ? C17 C16 C15 121.3(9) . . ? C16 C17 C18 119.8(9) . . ? C19 C18 C17 120.0(8) . . ? C18 C19 O3 124.2(7) . . ? C18 C19 C14 120.1(7) . . ? O3 C19 C14 115.6(7) . . ? O3 C20 C1 108.0(6) . . ? O4 C21 C40 107.2(7) . . ? O4 C22 C23 124.1(7) . . ? O4 C22 C27 114.6(7) . . ? C23 C22 C27 121.3(8) . . ? C24 C23 C22 118.6(9) . . ? C25 C24 C23 122.2(9) . . ? C24 C25 C26 119.0(9) . . ? C25 C26 C27 121.8(9) . . ? C26 C27 C22 117.0(8) . . ? C26 C27 C28 122.3(8) . . ? C22 C27 C28 120.7(7) . . ? C27 C28 S3 109.9(5) . . ? C30 C29 S3 113.5(6) . . ? O5 C30 C29 106.2(7) . . ? O5 C31 C32 105.4(6) . . ? C31 C32 S4 112.3(6) . . ? C34 C33 S4 115.4(6) . . ? C39 C34 C35 117.8(8) . . ? C39 C34 C33 122.8(8) . . ? C35 C34 C33 119.4(8) . . ? C36 C35 C34 122.2(9) . . ? C37 C36 C35 118.5(9) . . ? C38 C37 C36 120.9(9) . . ? C37 C38 C39 121.1(9) . . ? O6 C39 C38 125.0(7) . . ? O6 C39 C34 115.6(7) . . ? C38 C39 C34 119.4(8) . . ? O6 C40 C21 109.3(7) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 28.58 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.605 _refine_diff_density_min -2.358 _refine_diff_density_rms 0.128 data_3 _database_code_depnum_ccdc_archive 'CCDC 271051' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H106 Ag4 Cl4 N6 O24 S8' _chemical_formula_weight 2413.51 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5691(8) _cell_length_b 13.3821(10) _cell_length_c 16.2842(12) _cell_angle_alpha 85.7870(10) _cell_angle_beta 75.2830(10) _cell_angle_gamma 82.8980(10) _cell_volume 2417.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9269 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.31 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1228 _exptl_absorpt_coefficient_mu 1.156 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29151 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 28.32 _reflns_number_total 11330 _reflns_number_gt 8071 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0645P)^2^+0.8548P] 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 11330 _refine_ls_number_parameters 605 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1282 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.85750(3) 0.87504(3) 0.38415(2) 0.02558(10) Uani 1 1 d . . . Ag2 Ag 0.46859(3) 0.87501(3) 0.33892(2) 0.02374(10) Uani 1 1 d . . . Cl2 Cl 1.14439(10) 1.08633(9) 0.29790(7) 0.0271(2) Uani 1 1 d . . . Cl1 Cl 0.77908(10) 1.08945(8) 0.50416(7) 0.0272(2) Uani 1 1 d . . . S1 S 1.02399(10) 0.72887(8) 0.33836(7) 0.0230(2) Uani 1 1 d . . . S2 S 0.59987(9) 0.75697(8) 0.41157(7) 0.0201(2) Uani 1 1 d . . . S3 S 0.39493(9) 0.80788(9) 0.21915(7) 0.0234(2) Uani 1 1 d . . . S4 S 0.75511(9) 0.93199(8) 0.26606(7) 0.0212(2) Uani 1 1 d . . . O1 O 0.9182(3) 0.4748(2) 0.3787(2) 0.0259(7) Uani 1 1 d . . . O2 O 0.6675(3) 0.4988(2) 0.3791(2) 0.0284(7) Uani 1 1 d . . . O3 O 0.6339(3) 0.8268(3) 0.0122(2) 0.0336(8) Uani 1 1 d . . . O5 O 0.8324(3) 1.1360(2) 0.5688(2) 0.0315(8) Uani 1 1 d . . . O4 O 0.8151(3) 0.9249(3) 0.0480(2) 0.0300(7) Uani 1 1 d . . . O9 O 1.0676(2) 1.1227(2) 0.23140(17) 0.0182(6) Uani 1 1 d . . . O10 O 1.0601(3) 1.1297(2) 0.38200(19) 0.0280(7) Uani 1 1 d . . . O8 O 0.7374(3) 1.1898(2) 0.45702(19) 0.0226(6) Uani 1 1 d . . . O11 O 1.1527(3) 0.9739(2) 0.3003(2) 0.0305(7) Uani 1 1 d . . . O12 O 1.2547(3) 1.1375(2) 0.27096(19) 0.0244(7) Uani 1 1 d . . . O7 O 0.6696(3) 1.0393(2) 0.5433(2) 0.0300(7) Uani 1 1 d . . . O6 O 0.8747(3) 1.0348(2) 0.4376(2) 0.0287(7) Uani 1 1 d . . . N1 N 0.8087(3) 0.7712(3) 0.5104(2) 0.0231(8) Uani 1 1 d . . . H1 H 0.8487 0.7936 0.5471 0.028 Uiso 1 1 calc R . . N2 N 0.4898(3) 1.0196(3) 0.2456(2) 0.0220(8) Uani 1 1 d . . . H2 H 0.4150 1.0575 0.2569 0.026 Uiso 1 1 calc R . . C1 C 0.8400(4) 0.3966(3) 0.4001(3) 0.0249(9) Uani 1 1 d . . . H1A H 0.8005 0.3970 0.4617 0.030 Uiso 1 1 calc R . . H1B H 0.8882 0.3304 0.3884 0.030 Uiso 1 1 calc R . . C2 C 1.0064(4) 0.4665(3) 0.3035(3) 0.0208(9) Uani 1 1 d . . . C3 C 1.0771(4) 0.3767(3) 0.2810(3) 0.0269(10) Uani 1 1 d . . . H3A H 1.0631 0.3174 0.3162 0.032 Uiso 1 1 calc R . . C4 C 1.1680(4) 0.3737(4) 0.2074(3) 0.0305(11) Uani 1 1 d . . . H4A H 1.2162 0.3120 0.1918 0.037 Uiso 1 1 calc R . . C5 C 1.1896(4) 0.4593(4) 0.1563(3) 0.0313(11) Uani 1 1 d . . . H5B H 1.2522 0.4568 0.1056 0.038 Uiso 1 1 calc R . . C6 C 1.1189(4) 0.5499(4) 0.1796(3) 0.0277(10) Uani 1 1 d . . . H6A H 1.1341 0.6090 0.1443 0.033 Uiso 1 1 calc R . . C7 C 1.0271(4) 0.5552(3) 0.2531(3) 0.0220(9) Uani 1 1 d . . . C8 C 0.9532(4) 0.6545(3) 0.2791(3) 0.0225(9) Uani 1 1 d . . . H8B H 0.8731 0.6410 0.3147 0.027 Uiso 1 1 calc R . . H8C H 0.9412 0.6941 0.2276 0.027 Uiso 1 1 calc R . . C9 C 0.9963(4) 0.6659(3) 0.4422(3) 0.0271(10) Uani 1 1 d . . . H9B H 1.0303 0.5944 0.4357 0.032 Uiso 1 1 calc R . . H9C H 1.0403 0.6967 0.4769 0.032 Uiso 1 1 calc R . . C10 C 0.8644(4) 0.6689(3) 0.4911(3) 0.0262(10) Uani 1 1 d . . . H10B H 0.8194 0.6382 0.4570 0.031 Uiso 1 1 calc R . . H10C H 0.8588 0.6280 0.5448 0.031 Uiso 1 1 calc R . . C11 C 0.6810(4) 0.7754(4) 0.5582(3) 0.0289(10) Uani 1 1 d . . . H11B H 0.6692 0.8143 0.6096 0.035 Uiso 1 1 calc R . . H11C H 0.6613 0.7061 0.5769 0.035 Uiso 1 1 calc R . . C12 C 0.5954(4) 0.8235(4) 0.5061(3) 0.0246(10) Uani 1 1 d . . . H12B H 0.6144 0.8932 0.4886 0.030 Uiso 1 1 calc R . . H12C H 0.5124 0.8277 0.5427 0.030 Uiso 1 1 calc R . . C13 C 0.5123(4) 0.6543(3) 0.4612(3) 0.0221(9) Uani 1 1 d . . . H13A H 0.5593 0.6085 0.4944 0.027 Uiso 1 1 calc R . . H13B H 0.4377 0.6824 0.5011 0.027 Uiso 1 1 calc R . . C14 C 0.4800(4) 0.5949(3) 0.3965(3) 0.0200(9) Uani 1 1 d . . . C15 C 0.3692(4) 0.6161(4) 0.3769(3) 0.0255(10) Uani 1 1 d . . . H15A H 0.3152 0.6712 0.4021 0.031 Uiso 1 1 calc R . . C16 C 0.3357(4) 0.5584(4) 0.3211(3) 0.0291(10) Uani 1 1 d . . . H16A H 0.2592 0.5733 0.3089 0.035 Uiso 1 1 calc R . . C17 C 0.4147(4) 0.4793(4) 0.2837(3) 0.0300(10) Uani 1 1 d . . . H17A H 0.3919 0.4393 0.2459 0.036 Uiso 1 1 calc R . . C18 C 0.5270(4) 0.4574(4) 0.3005(3) 0.0291(10) Uani 1 1 d . . . H18A H 0.5811 0.4033 0.2738 0.035 Uiso 1 1 calc R . . C19 C 0.5601(4) 0.5152(3) 0.3567(3) 0.0216(9) Uani 1 1 d . . . C20 C 0.7449(4) 0.4098(3) 0.3504(3) 0.0229(9) Uani 1 1 d . . . H20A H 0.7824 0.4171 0.2887 0.028 Uiso 1 1 calc R . . H20B H 0.6987 0.3506 0.3606 0.028 Uiso 1 1 calc R . . C21 C 0.7390(4) 0.8433(4) -0.0540(3) 0.0287(10) Uani 1 1 d . . . H21A H 0.7176 0.8557 -0.1093 0.034 Uiso 1 1 calc R . . H21B H 0.7989 0.7831 -0.0580 0.034 Uiso 1 1 calc R . . C22 C 0.5638(4) 0.7558(3) 0.0015(3) 0.0233(9) Uani 1 1 d . . . C23 C 0.5442(4) 0.7371(4) -0.0767(3) 0.0273(10) Uani 1 1 d . . . H23A H 0.5842 0.7715 -0.1271 0.033 Uiso 1 1 calc R . . C24 C 0.4663(4) 0.6685(4) -0.0806(3) 0.0315(11) Uani 1 1 d . . . H24A H 0.4505 0.6576 -0.1336 0.038 Uiso 1 1 calc R . . C25 C 0.4110(4) 0.6153(4) -0.0081(3) 0.0340(11) Uani 1 1 d . . . H25A H 0.3591 0.5668 -0.0114 0.041 Uiso 1 1 calc R . . C26 C 0.4321(4) 0.6333(4) 0.0692(3) 0.0290(10) Uani 1 1 d . . . H26A H 0.3938 0.5967 0.1188 0.035 Uiso 1 1 calc R . . C27 C 0.5079(4) 0.7036(3) 0.0759(3) 0.0227(9) Uani 1 1 d . . . C28 C 0.5232(4) 0.7257(3) 0.1616(3) 0.0246(9) Uani 1 1 d . . . H28A H 0.5976 0.7585 0.1541 0.030 Uiso 1 1 calc R . . H28B H 0.5316 0.6617 0.1952 0.030 Uiso 1 1 calc R . . C29 C 0.4096(4) 0.9221(3) 0.1526(3) 0.0238(9) Uani 1 1 d . . . H29A H 0.4233 0.9041 0.0928 0.029 Uiso 1 1 calc R . . H29B H 0.3323 0.9658 0.1673 0.029 Uiso 1 1 calc R . . C30 C 0.5103(4) 0.9832(3) 0.1591(3) 0.0245(9) Uani 1 1 d . . . H30A H 0.5883 0.9406 0.1445 0.029 Uiso 1 1 calc R . . H30B H 0.5142 1.0415 0.1178 0.029 Uiso 1 1 calc R . . C31 C 0.5769(4) 1.0883(3) 0.2525(3) 0.0251(10) Uani 1 1 d . . . H31A H 0.5324 1.1517 0.2769 0.030 Uiso 1 1 calc R . . H31B H 0.6254 1.1051 0.1949 0.030 Uiso 1 1 calc R . . C32 C 0.6602(4) 1.0447(3) 0.3069(3) 0.0247(9) Uani 1 1 d . . . H32A H 0.6116 1.0286 0.3647 0.030 Uiso 1 1 calc R . . H32B H 0.7121 1.0965 0.3117 0.030 Uiso 1 1 calc R . . C33 C 0.8709(4) 0.9909(3) 0.1862(3) 0.0243(9) Uani 1 1 d . . . H33A H 0.8321 1.0410 0.1510 0.029 Uiso 1 1 calc R . . H33B H 0.9179 1.0271 0.2151 0.029 Uiso 1 1 calc R . . C34 C 0.9551(4) 0.9146(3) 0.1293(3) 0.0224(9) Uani 1 1 d . . . C35 C 1.0654(4) 0.8751(4) 0.1455(3) 0.0282(10) Uani 1 1 d . . . H35A H 1.0842 0.8906 0.1963 0.034 Uiso 1 1 calc R . . C36 C 1.1473(4) 0.8134(4) 0.0881(3) 0.0346(12) Uani 1 1 d . . . H36A H 1.2222 0.7871 0.0993 0.042 Uiso 1 1 calc R . . C37 C 1.1195(4) 0.7906(4) 0.0148(3) 0.0364(12) Uani 1 1 d . . . H37A H 1.1765 0.7495 -0.0250 0.044 Uiso 1 1 calc R . . C38 C 1.0100(4) 0.8263(4) -0.0020(3) 0.0318(11) Uani 1 1 d . . . H38A H 0.9915 0.8097 -0.0526 0.038 Uiso 1 1 calc R . . C39 C 0.9273(4) 0.8870(3) 0.0565(3) 0.0236(9) Uani 1 1 d . . . C40 C 0.7901(4) 0.9317(4) -0.0338(3) 0.0311(11) Uani 1 1 d . . . H40A H 0.8655 0.9408 -0.0774 0.037 Uiso 1 1 calc R . . H40B H 0.7330 0.9925 -0.0372 0.037 Uiso 1 1 calc R . . N3 N 0.797(3) 0.4299(15) 0.1260(16) 0.090(8) Uani 0.54(6) 1 d PD A 1 C44 C 0.875(3) 0.6017(13) 0.0584(17) 0.064(6) Uani 0.54(6) 1 d PD A 1 H44A H 0.9538 0.6109 0.0676 0.077 Uiso 0.54(6) 1 calc PR A 1 H44B H 0.8154 0.6556 0.0851 0.077 Uiso 0.54(6) 1 calc PR A 1 H44C H 0.8807 0.6040 -0.0027 0.077 Uiso 0.54(6) 1 calc PR A 1 N3' N 0.843(5) 0.4167(9) 0.110(2) 0.092(11) Uani 0.46(6) 1 d PD A 2 C44' C 0.841(4) 0.6140(7) 0.090(4) 0.084(10) Uani 0.46(6) 1 d PD A 2 H44D H 0.7967 0.6434 0.1441 0.101 Uiso 0.46(6) 1 calc PR A 2 H44E H 0.8043 0.6426 0.0447 0.101 Uiso 0.46(6) 1 calc PR A 2 H44F H 0.9249 0.6293 0.0773 0.101 Uiso 0.46(6) 1 calc PR A 2 C43 C 0.8382(8) 0.4997(6) 0.0977(5) 0.069(2) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02949(19) 0.01959(17) 0.02708(19) -0.00125(14) -0.00909(14) 0.00409(13) Ag2 0.02402(18) 0.02898(19) 0.01782(17) 0.00130(13) -0.00539(13) -0.00226(14) Cl2 0.0259(6) 0.0308(6) 0.0247(5) -0.0059(5) -0.0058(4) -0.0018(4) Cl1 0.0292(6) 0.0234(6) 0.0276(6) -0.0040(4) -0.0037(5) -0.0028(4) S1 0.0216(5) 0.0179(5) 0.0307(6) -0.0032(4) -0.0093(4) 0.0007(4) S2 0.0197(5) 0.0217(5) 0.0189(5) -0.0026(4) -0.0051(4) -0.0010(4) S3 0.0199(5) 0.0311(6) 0.0184(5) -0.0027(4) -0.0038(4) -0.0011(4) S4 0.0204(5) 0.0236(5) 0.0206(5) -0.0008(4) -0.0070(4) -0.0020(4) O1 0.0227(16) 0.0255(17) 0.0283(17) -0.0025(13) -0.0034(13) -0.0036(13) O2 0.0265(17) 0.0251(17) 0.0367(19) -0.0109(14) -0.0156(14) 0.0066(13) O3 0.0314(18) 0.044(2) 0.0234(17) -0.0107(15) 0.0048(14) -0.0167(16) O5 0.042(2) 0.0291(18) 0.0269(17) -0.0087(14) -0.0069(15) -0.0148(15) O4 0.0193(16) 0.048(2) 0.0255(17) -0.0058(15) -0.0096(13) -0.0014(14) O9 0.0152(14) 0.0261(16) 0.0180(14) -0.0001(12) -0.0122(11) -0.0038(12) O10 0.0243(16) 0.0336(18) 0.0228(16) -0.0145(14) 0.0055(13) -0.0070(14) O8 0.0271(16) 0.0112(14) 0.0277(16) 0.0053(12) -0.0076(13) 0.0033(12) O11 0.041(2) 0.0205(17) 0.0294(18) -0.0089(14) -0.0053(15) -0.0033(14) O12 0.0174(15) 0.0289(17) 0.0261(16) -0.0031(13) -0.0035(12) -0.0018(13) O7 0.0234(16) 0.0299(18) 0.0328(18) -0.0103(15) 0.0052(14) -0.0082(14) O6 0.0201(16) 0.0293(18) 0.0330(18) -0.0138(14) 0.0039(13) -0.0032(13) N1 0.026(2) 0.024(2) 0.0231(19) -0.0047(15) -0.0118(16) -0.0036(15) N2 0.0181(18) 0.0234(19) 0.0231(19) -0.0023(15) -0.0063(15) 0.0063(14) C1 0.021(2) 0.025(2) 0.027(2) 0.0059(19) -0.0046(18) -0.0023(18) C2 0.017(2) 0.021(2) 0.023(2) -0.0035(17) -0.0038(17) -0.0022(17) C3 0.027(2) 0.020(2) 0.033(3) -0.0027(19) -0.006(2) -0.0023(18) C4 0.032(3) 0.025(2) 0.033(3) -0.011(2) -0.005(2) 0.001(2) C5 0.029(3) 0.034(3) 0.026(2) -0.010(2) 0.005(2) -0.006(2) C6 0.029(2) 0.027(2) 0.030(2) 0.001(2) -0.009(2) -0.0085(19) C7 0.022(2) 0.023(2) 0.023(2) -0.0042(18) -0.0104(18) -0.0006(17) C8 0.024(2) 0.020(2) 0.026(2) -0.0021(18) -0.0124(18) 0.0019(17) C9 0.031(2) 0.023(2) 0.031(3) 0.0011(19) -0.018(2) -0.0003(19) C10 0.031(2) 0.024(2) 0.025(2) -0.0009(19) -0.0119(19) 0.0000(19) C11 0.034(3) 0.033(3) 0.021(2) -0.009(2) -0.009(2) -0.003(2) C12 0.022(2) 0.029(2) 0.025(2) -0.0104(19) -0.0069(18) 0.0005(18) C13 0.027(2) 0.020(2) 0.017(2) 0.0001(17) -0.0012(17) -0.0041(17) C14 0.022(2) 0.021(2) 0.017(2) 0.0026(17) -0.0038(17) -0.0051(17) C15 0.022(2) 0.029(2) 0.023(2) -0.0004(19) -0.0015(18) -0.0020(18) C16 0.021(2) 0.036(3) 0.033(3) 0.001(2) -0.012(2) -0.0032(19) C17 0.034(3) 0.033(3) 0.027(2) -0.005(2) -0.012(2) -0.008(2) C18 0.028(2) 0.027(2) 0.031(3) -0.006(2) -0.007(2) -0.001(2) C19 0.021(2) 0.021(2) 0.023(2) -0.0016(17) -0.0079(17) 0.0005(17) C20 0.021(2) 0.020(2) 0.027(2) -0.0015(18) -0.0069(18) 0.0009(17) C21 0.025(2) 0.039(3) 0.020(2) -0.002(2) -0.0020(18) -0.008(2) C22 0.021(2) 0.024(2) 0.026(2) -0.0091(18) -0.0046(18) -0.0021(17) C23 0.028(2) 0.031(3) 0.020(2) -0.0053(19) -0.0011(18) 0.0013(19) C24 0.029(2) 0.039(3) 0.029(3) -0.017(2) -0.011(2) 0.003(2) C25 0.030(3) 0.037(3) 0.036(3) -0.012(2) -0.007(2) -0.006(2) C26 0.028(2) 0.027(2) 0.031(3) -0.001(2) -0.004(2) -0.0046(19) C27 0.021(2) 0.023(2) 0.023(2) -0.0046(18) -0.0056(17) 0.0022(17) C28 0.023(2) 0.025(2) 0.025(2) 0.0016(19) -0.0067(18) -0.0010(18) C29 0.025(2) 0.029(2) 0.017(2) -0.0031(18) -0.0081(17) 0.0086(18) C30 0.025(2) 0.027(2) 0.018(2) 0.0011(18) -0.0031(18) 0.0021(18) C31 0.025(2) 0.020(2) 0.029(2) -0.0010(18) -0.0074(19) 0.0035(18) C32 0.025(2) 0.024(2) 0.025(2) -0.0062(19) -0.0063(18) -0.0001(18) C33 0.023(2) 0.024(2) 0.027(2) -0.0010(19) -0.0040(18) -0.0092(18) C34 0.021(2) 0.022(2) 0.024(2) 0.0010(18) -0.0038(18) -0.0079(17) C35 0.026(2) 0.028(2) 0.035(3) 0.002(2) -0.013(2) -0.0096(19) C36 0.024(2) 0.029(3) 0.053(3) 0.005(2) -0.015(2) -0.003(2) C37 0.026(3) 0.034(3) 0.043(3) -0.013(2) 0.004(2) -0.001(2) C38 0.029(3) 0.038(3) 0.029(3) -0.008(2) -0.005(2) -0.010(2) C39 0.020(2) 0.026(2) 0.025(2) -0.0009(18) -0.0049(18) -0.0019(18) C40 0.034(3) 0.037(3) 0.025(2) 0.006(2) -0.013(2) -0.006(2) N3 0.077(14) 0.16(2) 0.034(9) 0.009(9) -0.005(9) -0.050(10) C44 0.067(14) 0.073(12) 0.061(12) -0.018(9) -0.026(10) -0.003(9) N3' 0.15(3) 0.064(12) 0.059(13) -0.008(9) 0.002(16) -0.068(13) C44' 0.08(2) 0.076(15) 0.10(2) 0.009(13) -0.048(18) 0.019(12) C43 0.069(5) 0.104(8) 0.041(4) -0.010(4) -0.015(4) -0.026(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.379(4) . ? Ag1 O6 2.415(3) . ? Ag1 S4 2.5300(11) . ? Ag1 S1 2.5778(11) . ? Ag2 N2 2.369(4) . ? Ag2 O7 2.421(3) 2_676 ? Ag2 S2 2.4993(11) . ? Ag2 S3 2.5745(11) . ? Cl2 O12 1.476(3) . ? Cl2 O11 1.494(3) . ? Cl2 O10 1.569(3) . ? Cl2 O9 1.582(3) . ? Cl1 O7 1.483(3) . ? Cl1 O6 1.497(3) . ? Cl1 O5 1.549(3) . ? Cl1 O8 1.582(3) . ? S1 C9 1.804(5) . ? S1 C8 1.827(4) . ? S2 C12 1.820(4) . ? S2 C13 1.826(4) . ? S3 C29 1.807(5) . ? S3 C28 1.825(4) . ? S4 C32 1.814(4) . ? S4 C33 1.826(4) . ? O1 C2 1.382(5) . ? O1 C1 1.435(5) . ? O2 C19 1.370(5) . ? O2 C20 1.430(5) . ? O3 C22 1.370(5) . ? O3 C21 1.434(5) . ? O4 C39 1.370(5) . ? O4 C40 1.427(5) . ? O7 Ag2 2.421(3) 2_676 ? N1 C10 1.460(6) . ? N1 C11 1.481(6) . ? N2 C31 1.474(6) . ? N2 C30 1.477(5) . ? C1 C20 1.511(6) . ? C2 C3 1.384(6) . ? C2 C7 1.403(6) . ? C3 C4 1.379(6) . ? C4 C5 1.375(7) . ? C5 C6 1.395(7) . ? C6 C7 1.384(6) . ? C7 C8 1.514(6) . ? C9 C10 1.528(6) . ? C11 C12 1.517(6) . ? C13 C14 1.509(6) . ? C14 C15 1.390(6) . ? C14 C19 1.403(6) . ? C15 C16 1.388(6) . ? C16 C17 1.379(7) . ? C17 C18 1.387(6) . ? C18 C19 1.392(6) . ? C21 C40 1.478(7) . ? C22 C23 1.394(6) . ? C22 C27 1.401(6) . ? C23 C24 1.379(7) . ? C24 C25 1.384(7) . ? C25 C26 1.384(7) . ? C26 C27 1.391(6) . ? C27 C28 1.506(6) . ? C29 C30 1.533(6) . ? C31 C32 1.507(6) . ? C33 C34 1.512(6) . ? C34 C39 1.389(6) . ? C34 C35 1.401(6) . ? C35 C36 1.387(7) . ? C36 C37 1.377(7) . ? C37 C38 1.384(7) . ? C38 C39 1.394(6) . ? N3 C43 1.114(7) . ? C44 C43 1.528(6) . ? N3' C43 1.111(7) . ? C44' C43 1.530(6) . ? 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 N1 Ag1 O6 102.72(12) . . ? N1 Ag1 S4 134.57(9) . . ? O6 Ag1 S4 101.19(8) . . ? N1 Ag1 S1 82.53(9) . . ? O6 Ag1 S1 128.08(8) . . ? S4 Ag1 S1 111.14(4) . . ? N2 Ag2 O7 95.53(12) . 2_676 ? N2 Ag2 S2 137.06(9) . . ? O7 Ag2 S2 102.47(9) 2_676 . ? N2 Ag2 S3 82.32(9) . . ? O7 Ag2 S3 121.61(8) 2_676 . ? S2 Ag2 S3 118.25(4) . . ? O12 Cl2 O11 120.00(19) . . ? O12 Cl2 O10 111.15(18) . . ? O11 Cl2 O10 111.29(19) . . ? O12 Cl2 O9 106.03(17) . . ? O11 Cl2 O9 104.81(18) . . ? O10 Cl2 O9 101.50(17) . . ? O7 Cl1 O6 117.64(19) . . ? O7 Cl1 O5 114.15(19) . . ? O6 Cl1 O5 111.94(19) . . ? O7 Cl1 O8 106.89(18) . . ? O6 Cl1 O8 104.80(18) . . ? O5 Cl1 O8 99.01(18) . . ? C9 S1 C8 103.0(2) . . ? C9 S1 Ag1 94.17(15) . . ? C8 S1 Ag1 101.34(14) . . ? C12 S2 C13 99.3(2) . . ? C12 S2 Ag2 102.57(15) . . ? C13 S2 Ag2 106.85(15) . . ? C29 S3 C28 100.9(2) . . ? C29 S3 Ag2 95.17(15) . . ? C28 S3 Ag2 104.64(14) . . ? C32 S4 C33 99.0(2) . . ? C32 S4 Ag1 102.70(14) . . ? C33 S4 Ag1 103.48(15) . . ? C2 O1 C1 116.7(3) . . ? C19 O2 C20 117.5(3) . . ? C22 O3 C21 118.4(3) . . ? C39 O4 C40 119.8(4) . . ? Cl1 O7 Ag2 114.91(17) . 2_676 ? Cl1 O6 Ag1 124.36(17) . . ? C10 N1 C11 113.3(4) . . ? C10 N1 Ag1 108.2(3) . . ? C11 N1 Ag1 117.9(3) . . ? C31 N2 C30 113.1(3) . . ? C31 N2 Ag2 118.3(2) . . ? C30 N2 Ag2 106.1(3) . . ? O1 C1 C20 111.8(3) . . ? O1 C2 C3 122.1(4) . . ? O1 C2 C7 116.9(4) . . ? C3 C2 C7 120.9(4) . . ? C4 C3 C2 119.8(4) . . ? C5 C4 C3 120.6(4) . . ? C4 C5 C6 119.6(4) . . ? C7 C6 C5 121.2(4) . . ? C6 C7 C2 118.0(4) . . ? C6 C7 C8 120.8(4) . . ? C2 C7 C8 121.2(4) . . ? C7 C8 S1 112.6(3) . . ? C10 C9 S1 115.7(3) . . ? N1 C10 C9 112.6(4) . . ? N1 C11 C12 112.8(4) . . ? C11 C12 S2 114.7(3) . . ? C14 C13 S2 112.0(3) . . ? C15 C14 C19 118.6(4) . . ? C15 C14 C13 120.8(4) . . ? C19 C14 C13 120.6(4) . . ? C16 C15 C14 121.3(4) . . ? C17 C16 C15 119.2(4) . . ? C16 C17 C18 120.9(4) . . ? C17 C18 C19 119.7(4) . . ? O2 C19 C18 124.5(4) . . ? O2 C19 C14 115.3(4) . . ? C18 C19 C14 120.2(4) . . ? O2 C20 C1 106.7(4) . . ? O3 C21 C40 108.5(4) . . ? O3 C22 C23 123.7(4) . . ? O3 C22 C27 115.4(4) . . ? C23 C22 C27 120.8(4) . . ? C24 C23 C22 119.6(4) . . ? C23 C24 C25 120.6(4) . . ? C24 C25 C26 119.4(5) . . ? C25 C26 C27 121.6(4) . . ? C26 C27 C22 117.9(4) . . ? C26 C27 C28 120.2(4) . . ? C22 C27 C28 121.8(4) . . ? C27 C28 S3 111.1(3) . . ? C30 C29 S3 115.7(3) . . ? N2 C30 C29 111.1(4) . . ? N2 C31 C32 113.4(4) . . ? C31 C32 S4 113.9(3) . . ? C34 C33 S4 112.1(3) . . ? C39 C34 C35 118.7(4) . . ? C39 C34 C33 120.2(4) . . ? C35 C34 C33 121.1(4) . . ? C36 C35 C34 120.6(4) . . ? C37 C36 C35 119.6(4) . . ? C36 C37 C38 121.2(5) . . ? C37 C38 C39 118.9(4) . . ? O4 C39 C34 114.7(4) . . ? O4 C39 C38 124.3(4) . . ? C34 C39 C38 121.0(4) . . ? O4 C40 C21 114.5(4) . . ? N3' C43 N3 28(2) . . ? N3' C43 C44 159(2) . . ? N3 C43 C44 171.5(19) . . ? N3' C43 C44' 172(3) . . ? N3 C43 C44' 152.8(19) . . ? C44 C43 C44' 22.1(17) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.865 _refine_diff_density_min -1.294 _refine_diff_density_rms 0.162