# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Jian-Fang Ma' _publ_contact_author_email JIANFANGMA@YAHOO.COM.CN _publ_section_title ; Influence of Sulfonate Anions on the Solid-structures of Silver Complexes Supported by 4,4'-Bipyridine Bridge ; loop_ _publ_author_name 'Jian-Fang Ma' 'Xian-Wu Dong' 'Shun-Li Li' 'Hai-Yan Liu' ; Ying-Ying Liu ; 'Zhong-Min Su' 'Hua Wu' 'Jin Yang' # Attachment 'crystal.cif' data_compd1 _database_code_depnum_ccdc_archive 'CCDC 684623' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H16 Ag N3 O3 S, H2 O' _chemical_formula_sum 'C20 H18 Ag N3 O4 S' _chemical_formula_weight 504.30 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.089(2) _cell_length_b 15.699(3) _cell_length_c 11.355(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.39(3) _cell_angle_gamma 90.00 _cell_volume 1896.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4319 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.4 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 1.207 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.749 _exptl_absorpt_correction_T_max 0.789 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18400 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.42 _reflns_number_total 4319 _reflns_number_gt 3618 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+1.0294P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4319 _refine_ls_number_parameters 274 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0805 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.103 _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 0.15769(2) 0.579266(14) 0.687741(16) 0.04615(9) Uani 1 1 d . . . C1 C 0.4792(2) 0.67729(14) 0.2462(2) 0.0283(5) Uani 1 1 d . . . C2 C 0.4155(3) 0.72317(16) 0.1457(2) 0.0380(6) Uani 1 1 d . . . H2 H 0.4432 0.7231 0.0756 0.046 Uiso 1 1 calc R . . C3 C 0.3077(3) 0.77072(17) 0.1473(2) 0.0447(6) Uani 1 1 d . . . H3 H 0.2634 0.8003 0.0775 0.054 Uiso 1 1 calc R . . C4 C 0.2685(2) 0.77349(16) 0.2499(2) 0.0407(6) Uani 1 1 d . . . H4 H 0.1984 0.8059 0.2502 0.049 Uiso 1 1 calc R . . C5 C 0.3325(2) 0.72782(14) 0.3568(2) 0.0300(5) Uani 1 1 d . . . C6 C 0.4385(2) 0.67674(14) 0.35547(19) 0.0266(4) Uani 1 1 d . . . C7 C 0.4972(2) 0.62977(15) 0.4633(2) 0.0305(5) Uani 1 1 d . . . H7 H 0.5645 0.5943 0.4639 0.037 Uiso 1 1 calc R . . C8 C 0.4570(2) 0.63562(15) 0.5659(2) 0.0331(5) Uani 1 1 d . . . H8 H 0.4966 0.6034 0.6346 0.040 Uiso 1 1 calc R . . C9 C 0.3562(2) 0.68974(14) 0.5700(2) 0.0305(5) Uani 1 1 d . . . C10 C 0.1936(3) 0.51450(18) 0.4518(2) 0.0437(6) Uani 1 1 d . . . H10 H 0.2493 0.4806 0.5093 0.052 Uiso 1 1 calc R . . C11 C 0.2002(3) 0.51364(17) 0.3321(2) 0.0400(6) Uani 1 1 d . . . H11 H 0.2590 0.4793 0.3106 0.048 Uiso 1 1 calc R . . C12 C 0.1195(2) 0.56391(14) 0.2441(2) 0.0269(4) Uani 1 1 d . . . C13 C 0.0317(2) 0.61028(17) 0.2829(2) 0.0372(6) Uani 1 1 d . . . H13 H -0.0270 0.6434 0.2269 0.045 Uiso 1 1 calc R . . C14 C 0.0307(2) 0.60776(18) 0.4043(2) 0.0395(6) Uani 1 1 d . . . H14 H -0.0291 0.6399 0.4279 0.047 Uiso 1 1 calc R . . C15 C 0.1289(2) 0.56720(14) 0.1167(2) 0.0277(5) Uani 1 1 d . . . C16 C 0.0610(3) 0.62294(19) 0.0307(2) 0.0572(9) Uani 1 1 d . . . H16 H 0.0063 0.6610 0.0519 0.069 Uiso 1 1 calc R . . C17 C 0.0726(3) 0.62326(19) -0.0872(2) 0.0579(9) Uani 1 1 d . . . H17 H 0.0239 0.6616 -0.1432 0.069 Uiso 1 1 calc R . . C18 C 0.2136(4) 0.5185(3) -0.0433(3) 0.0751(12) Uani 1 1 d . . . H18 H 0.2676 0.4814 -0.0674 0.090 Uiso 1 1 calc R . . C19 C 0.2066(4) 0.5138(3) 0.0752(3) 0.0738(12) Uani 1 1 d . . . H19 H 0.2552 0.4738 0.1284 0.089 Uiso 1 1 calc R . . C20 C 0.2951(2) 0.73380(15) 0.4660(2) 0.0326(5) Uani 1 1 d . . . H20 H 0.2274 0.7685 0.4672 0.039 Uiso 1 1 calc R . . N1 N 0.11138(19) 0.56143(13) 0.48885(17) 0.0334(4) Uani 1 1 d . . . N2 N 0.1477(2) 0.57299(13) -0.12467(18) 0.0346(5) Uani 1 1 d . . . N4 N 0.3178(2) 0.69345(14) 0.6769(2) 0.0372(5) Uani 1 1 d D . . O1 O 0.63776(19) 0.64429(12) 0.12327(16) 0.0451(4) Uani 1 1 d . . . O2 O 0.71945(17) 0.65860(13) 0.34289(17) 0.0455(4) Uani 1 1 d . . . O3 O 0.6009(2) 0.53330(11) 0.25697(18) 0.0472(5) Uani 1 1 d . . . OW1 O 0.4782(3) 0.38880(15) 0.1266(2) 0.0624(6) Uani 1 1 d D . . S1 S 0.62019(6) 0.62385(4) 0.24270(5) 0.03113(13) Uani 1 1 d . . . H1A H 0.516(3) 0.4345(17) 0.142(3) 0.047 Uiso 1 1 d D . . H1B H 0.450(3) 0.3881(18) 0.053(2) 0.047 Uiso 1 1 d D . . HN1 H 0.277(3) 0.7353(18) 0.682(3) 0.047 Uiso 1 1 d D . . HN2 H 0.374(3) 0.6813(19) 0.743(3) 0.047 Uiso 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 0.05793(16) 0.06620(16) 0.01853(11) -0.00086(8) 0.01767(9) -0.00849(10) C1 0.0326(12) 0.0290(11) 0.0240(11) -0.0003(8) 0.0090(9) -0.0029(9) C2 0.0456(15) 0.0409(13) 0.0276(12) 0.0053(10) 0.0104(11) 0.0005(11) C3 0.0491(16) 0.0483(15) 0.0315(13) 0.0128(11) 0.0031(11) 0.0109(13) C4 0.0359(14) 0.0387(14) 0.0445(14) 0.0094(11) 0.0067(11) 0.0097(11) C5 0.0288(12) 0.0299(11) 0.0307(11) 0.0026(9) 0.0075(9) -0.0038(9) C6 0.0253(11) 0.0303(11) 0.0237(11) 0.0027(8) 0.0061(8) -0.0032(9) C7 0.0265(11) 0.0368(12) 0.0292(12) 0.0054(9) 0.0097(9) 0.0032(9) C8 0.0289(12) 0.0428(13) 0.0279(12) 0.0059(9) 0.0083(9) 0.0011(10) C9 0.0289(12) 0.0329(12) 0.0324(12) -0.0010(9) 0.0130(10) -0.0063(9) C10 0.0542(16) 0.0578(16) 0.0190(12) 0.0086(10) 0.0100(11) 0.0140(13) C11 0.0513(16) 0.0497(14) 0.0219(12) 0.0061(10) 0.0149(11) 0.0201(12) C12 0.0297(11) 0.0320(11) 0.0196(10) -0.0013(8) 0.0079(9) -0.0014(9) C13 0.0382(14) 0.0539(15) 0.0214(11) 0.0029(10) 0.0116(10) 0.0123(11) C14 0.0372(14) 0.0589(16) 0.0262(12) -0.0035(11) 0.0152(11) 0.0073(12) C15 0.0323(12) 0.0328(11) 0.0187(10) -0.0009(8) 0.0083(9) 0.0016(9) C16 0.091(2) 0.0608(18) 0.0254(13) 0.0123(12) 0.0260(14) 0.0483(17) C17 0.096(3) 0.0565(17) 0.0266(13) 0.0147(12) 0.0258(15) 0.0398(17) C18 0.090(3) 0.111(3) 0.0351(16) 0.0188(17) 0.0354(17) 0.069(2) C19 0.093(3) 0.106(3) 0.0294(15) 0.0249(16) 0.0286(16) 0.072(2) C20 0.0291(12) 0.0331(12) 0.0375(13) 0.0020(9) 0.0126(10) 0.0029(9) N1 0.0366(11) 0.0469(11) 0.0189(9) -0.0016(8) 0.0112(8) -0.0084(9) N2 0.0440(12) 0.0443(11) 0.0183(9) 0.0012(8) 0.0135(8) 0.0011(9) N4 0.0399(12) 0.0405(12) 0.0363(12) -0.0021(9) 0.0189(10) -0.0005(10) O1 0.0583(12) 0.0547(11) 0.0293(9) 0.0047(8) 0.0237(9) 0.0064(9) O2 0.0320(9) 0.0658(12) 0.0387(10) -0.0075(9) 0.0101(8) -0.0010(9) O3 0.0645(13) 0.0326(9) 0.0491(11) 0.0034(8) 0.0235(10) 0.0049(9) OW1 0.0771(17) 0.0606(13) 0.0383(12) 0.0026(10) -0.0018(11) -0.0098(12) S1 0.0373(3) 0.0352(3) 0.0235(3) 0.0008(2) 0.0128(2) 0.0014(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 N2 2.166(2) 1_556 ? Ag1 N1 2.188(2) . ? Ag1 N4 2.550(2) . ? C1 C2 1.366(3) . ? C1 C6 1.435(3) . ? C1 S1 1.785(2) . ? C2 C3 1.414(4) . ? C2 H2 0.9300 . ? C3 C4 1.354(4) . ? C3 H3 0.9300 . ? C4 C5 1.416(3) . ? C4 H4 0.9300 . ? C5 C20 1.418(3) . ? C5 C6 1.426(3) . ? C6 C7 1.420(3) . ? C7 C8 1.363(3) . ? C7 H7 0.9300 . ? C8 C9 1.415(3) . ? C8 H8 0.9300 . ? C9 C20 1.371(3) . ? C9 N4 1.397(3) . ? C10 N1 1.329(3) . ? C10 C11 1.382(3) . ? C10 H10 0.9300 . ? C11 C12 1.385(3) . ? C11 H11 0.9300 . ? C12 C13 1.383(3) . ? C12 C15 1.480(3) . ? C13 C14 1.383(3) . ? C13 H13 0.9300 . ? C14 N1 1.329(3) . ? C14 H14 0.9300 . ? C15 C16 1.368(3) . ? C15 C19 1.378(4) . ? C16 C17 1.381(4) . ? C16 H16 0.9300 . ? C17 N2 1.303(3) . ? C17 H17 0.9300 . ? C18 N2 1.319(4) . ? C18 C19 1.371(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? N2 Ag1 2.166(2) 1_554 ? N4 HN1 0.81(3) . ? N4 HN2 0.85(3) . ? O1 S1 1.4592(18) . ? O2 S1 1.448(2) . ? O3 S1 1.4533(19) . ? OW1 H1A 0.82(2) . ? OW1 H1B 0.81(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 161.25(8) 1_556 . ? N2 Ag1 N4 107.98(8) 1_556 . ? N1 Ag1 N4 90.23(8) . . ? C2 C1 C6 120.7(2) . . ? C2 C1 S1 118.61(18) . . ? C6 C1 S1 120.52(17) . . ? C1 C2 C3 120.5(2) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 120.4(2) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 121.1(2) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C20 121.1(2) . . ? C4 C5 C6 119.4(2) . . ? C20 C5 C6 119.5(2) . . ? C7 C6 C5 117.5(2) . . ? C7 C6 C1 124.7(2) . . ? C5 C6 C1 117.9(2) . . ? C8 C7 C6 121.4(2) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C7 C8 C9 121.4(2) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C20 C9 N4 122.0(2) . . ? C20 C9 C8 118.6(2) . . ? N4 C9 C8 119.4(2) . . ? N1 C10 C11 123.3(2) . . ? N1 C10 H10 118.4 . . ? C11 C10 H10 118.4 . . ? C10 C11 C12 120.1(2) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 116.1(2) . . ? C13 C12 C15 122.9(2) . . ? C11 C12 C15 121.0(2) . . ? C12 C13 C14 120.5(2) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? N1 C14 C13 122.8(2) . . ? N1 C14 H14 118.6 . . ? C13 C14 H14 118.6 . . ? C16 C15 C19 114.6(2) . . ? C16 C15 C12 122.9(2) . . ? C19 C15 C12 122.5(2) . . ? C15 C16 C17 120.7(2) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? N2 C17 C16 123.9(2) . . ? N2 C17 H17 118.1 . . ? C16 C17 H17 118.1 . . ? N2 C18 C19 123.3(3) . . ? N2 C18 H18 118.3 . . ? C19 C18 H18 118.3 . . ? C18 C19 C15 121.1(3) . . ? C18 C19 H19 119.4 . . ? C15 C19 H19 119.4 . . ? C9 C20 C5 121.6(2) . . ? C9 C20 H20 119.2 . . ? C5 C20 H20 119.2 . . ? C14 N1 C10 117.2(2) . . ? C14 N1 Ag1 126.11(17) . . ? C10 N1 Ag1 114.54(16) . . ? C17 N2 C18 116.3(2) . . ? C17 N2 Ag1 120.54(17) . 1_554 ? C18 N2 Ag1 123.16(17) . 1_554 ? C9 N4 Ag1 113.56(15) . . ? C9 N4 HN1 114(2) . . ? Ag1 N4 HN1 99(2) . . ? C9 N4 HN2 116(2) . . ? Ag1 N4 HN2 98(2) . . ? HN1 N4 HN2 113(3) . . ? H1A OW1 H1B 105(2) . . ? O2 S1 O3 112.58(12) . . ? O2 S1 O1 112.09(12) . . ? O3 S1 O1 112.41(11) . . ? O2 S1 C1 106.37(11) . . ? O3 S1 C1 107.47(11) . . ? O1 S1 C1 105.37(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 C6 C1 C2 C3 -0.3(4) . . . . ? S1 C1 C2 C3 -176.1(2) . . . . ? C1 C2 C3 C4 2.1(4) . . . . ? C2 C3 C4 C5 -1.2(4) . . . . ? C3 C4 C5 C20 177.1(2) . . . . ? C3 C4 C5 C6 -1.3(4) . . . . ? C4 C5 C6 C7 -177.9(2) . . . . ? C20 C5 C6 C7 3.7(3) . . . . ? C4 C5 C6 C1 2.9(3) . . . . ? C20 C5 C6 C1 -175.5(2) . . . . ? C2 C1 C6 C7 178.7(2) . . . . ? S1 C1 C6 C7 -5.5(3) . . . . ? C2 C1 C6 C5 -2.2(3) . . . . ? S1 C1 C6 C5 173.59(16) . . . . ? C5 C6 C7 C8 -2.4(3) . . . . ? C1 C6 C7 C8 176.7(2) . . . . ? C6 C7 C8 C9 -1.0(4) . . . . ? C7 C8 C9 C20 3.0(4) . . . . ? C7 C8 C9 N4 179.7(2) . . . . ? N1 C10 C11 C12 0.6(5) . . . . ? C10 C11 C12 C13 -2.6(4) . . . . ? C10 C11 C12 C15 177.0(2) . . . . ? C11 C12 C13 C14 2.5(4) . . . . ? C15 C12 C13 C14 -177.1(2) . . . . ? C12 C13 C14 N1 -0.4(4) . . . . ? C13 C12 C15 C16 7.2(4) . . . . ? C11 C12 C15 C16 -172.4(3) . . . . ? C13 C12 C15 C19 -172.4(3) . . . . ? C11 C12 C15 C19 8.0(4) . . . . ? C19 C15 C16 C17 -0.1(5) . . . . ? C12 C15 C16 C17 -179.7(3) . . . . ? C15 C16 C17 N2 -0.9(6) . . . . ? N2 C18 C19 C15 -0.3(7) . . . . ? C16 C15 C19 C18 0.6(6) . . . . ? C12 C15 C19 C18 -179.8(4) . . . . ? N4 C9 C20 C5 -178.2(2) . . . . ? C8 C9 C20 C5 -1.6(3) . . . . ? C4 C5 C20 C9 179.8(2) . . . . ? C6 C5 C20 C9 -1.8(3) . . . . ? C13 C14 N1 C10 -1.7(4) . . . . ? C13 C14 N1 Ag1 160.6(2) . . . . ? C11 C10 N1 C14 1.6(4) . . . . ? C11 C10 N1 Ag1 -162.8(2) . . . . ? N2 Ag1 N1 C14 82.5(3) 1_556 . . . ? N4 Ag1 N1 C14 -83.9(2) . . . . ? N2 Ag1 N1 C10 -114.7(3) 1_556 . . . ? N4 Ag1 N1 C10 78.84(19) . . . . ? C16 C17 N2 C18 1.1(5) . . . . ? C16 C17 N2 Ag1 179.9(3) . . . 1_554 ? C19 C18 N2 C17 -0.6(6) . . . . ? C19 C18 N2 Ag1 -179.3(3) . . . 1_554 ? C20 C9 N4 Ag1 90.2(2) . . . . ? C8 C9 N4 Ag1 -86.4(2) . . . . ? N2 Ag1 N4 C9 165.03(17) 1_556 . . . ? N1 Ag1 N4 C9 -19.53(18) . . . . ? C2 C1 S1 O2 120.1(2) . . . . ? C6 C1 S1 O2 -55.8(2) . . . . ? C2 C1 S1 O3 -119.1(2) . . . . ? C6 C1 S1 O3 65.0(2) . . . . ? C2 C1 S1 O1 0.9(2) . . . . ? C6 C1 S1 O1 -174.90(18) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OW1 H1B O1 0.81(3) 2.03(2) 2.813(3) 165(3) 3_665 OW1 H1A O3 0.82(2) 2.07(2) 2.838(3) 154(3) . N4 HN2 OW1 0.85(3) 2.17(3) 2.985(4) 160(3) 3_666 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.302 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.069 #===end data_compd2 _database_code_depnum_ccdc_archive 'CCDC 684624' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 Ag N2, C10 H7 O3 S, 2(H2 O)' _chemical_formula_sum 'C20 H19 Ag N2 O5 S' _chemical_formula_weight 507.31 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' 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 'F d d 2' _symmetry_space_group_name_Hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' _cell_length_a 21.952(4) _cell_length_b 30.898(7) _cell_length_c 11.369(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7711(4) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4530 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.3 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4096 _exptl_absorpt_coefficient_mu 1.190 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.750 _exptl_absorpt_correction_T_max 0.812 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 13871 _diffrn_reflns_av_R_equivalents 0.0890 _diffrn_reflns_av_sigmaI/netI 0.1038 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.63 _reflns_number_total 4530 _reflns_number_gt 2424 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT software (Bruker, 1999)' _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(3) _refine_ls_number_reflns 4530 _refine_ls_number_parameters 274 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0998 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.0895 _refine_ls_goodness_of_fit_ref 0.862 _refine_ls_restrained_S_all 0.862 _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 0.56571(2) 0.530513(18) 1.10205(5) 0.05178(17) Uani 1 1 d . . . C1 C 0.6957(3) 0.5878(2) 1.0065(6) 0.0489(17) Uani 1 1 d . . . H1 H 0.7228 0.5693 1.0442 0.059 Uiso 1 1 calc R . . C2 C 0.6545(3) 0.6105(2) 1.0696(6) 0.0529(19) Uani 1 1 d . . . H2 H 0.6539 0.6074 1.1510 0.063 Uiso 1 1 calc R . . C3 C 0.6125(3) 0.6386(2) 1.0168(6) 0.0525(18) Uani 1 1 d . . . H3 H 0.5854 0.6543 1.0631 0.063 Uiso 1 1 calc R . . C4 C 0.6115(3) 0.6428(2) 0.8995(6) 0.0503(18) Uani 1 1 d . . . H4 H 0.5829 0.6605 0.8634 0.060 Uiso 1 1 calc R . . C5 C 0.6560(3) 0.61934(19) 0.8299(5) 0.0404(15) Uani 1 1 d . . . C6 C 0.6579(3) 0.6234(2) 0.7054(6) 0.0458(16) Uani 1 1 d . . . H6 H 0.6312 0.6424 0.6685 0.055 Uiso 1 1 calc R . . C7 C 0.6979(3) 0.6002(2) 0.6390(6) 0.0455(18) Uani 1 1 d . . . H7 H 0.6978 0.6027 0.5575 0.055 Uiso 1 1 calc R . . C8 C 0.7401(3) 0.5719(2) 0.6967(6) 0.0407(15) Uani 1 1 d . . . C9 C 0.7404(3) 0.5669(2) 0.8148(6) 0.0475(17) Uani 1 1 d . . . H9 H 0.7674 0.5477 0.8505 0.057 Uiso 1 1 calc R . . C10 C 0.6974(3) 0.5922(2) 0.8855(5) 0.0399(15) Uani 1 1 d . . . C11 C 0.6114(2) 0.50770(19) 0.7316(4) 0.0315(13) Uani 1 1 d . . . H11 H 0.6413 0.4916 0.6934 0.038 Uiso 1 1 calc R . . C12 C 0.6079(2) 0.50697(18) 0.8514(6) 0.0352(12) Uani 1 1 d . . . H12 H 0.6361 0.4902 0.8921 0.042 Uiso 1 1 calc R . . C13 C 0.5705(3) 0.5324(2) 0.6662(8) 0.031(2) Uani 1 1 d . . . C14 C 0.5271(2) 0.55550(18) 0.7316(4) 0.0285(12) Uani 1 1 d . . . H14 H 0.4985 0.5725 0.6931 0.034 Uiso 1 1 calc R . . C15 C 0.5268(2) 0.55311(17) 0.8543(5) 0.0325(12) Uani 1 1 d . . . H15 H 0.4978 0.5690 0.8956 0.039 Uiso 1 1 calc R . . C16 C 0.5706(2) 0.5332(2) 0.5352(7) 0.027(2) Uani 1 1 d . . . C17 C 0.5596(2) 0.57037(18) 0.4731(4) 0.0318(13) Uani 1 1 d . . . H17 H 0.5538 0.5965 0.5122 0.038 Uiso 1 1 calc R . . C18 C 0.5570(2) 0.56862(19) 0.3515(6) 0.0364(12) Uani 1 1 d . . . H18 H 0.5490 0.5938 0.3096 0.044 Uiso 1 1 calc R . . C19 C 0.5781(2) 0.49597(19) 0.3526(5) 0.0352(12) Uani 1 1 d . . . H19 H 0.5849 0.4704 0.3115 0.042 Uiso 1 1 calc R . . C20 C 0.5813(2) 0.4953(2) 0.4746(4) 0.0323(13) Uani 1 1 d . . . H20 H 0.5903 0.4699 0.5146 0.039 Uiso 1 1 calc R . . N1 N 0.56629(19) 0.52904(16) 0.9146(7) 0.0314(18) Uani 1 1 d . . . N2 N 0.5659(2) 0.53158(18) 0.2928(7) 0.0363(19) Uani 1 1 d . . . O1 O 0.8275(3) 0.5715(2) 0.5486(6) 0.113(2) Uani 1 1 d . . . O2 O 0.8178(2) 0.50929(18) 0.6758(5) 0.0742(17) Uani 1 1 d . . . O3 O 0.7487(3) 0.5187(2) 0.5214(5) 0.105(2) Uani 1 1 d . . . OW1 O 0.9592(3) 0.5919(2) 0.6051(7) 0.0935(18) Uani 1 1 d D . . S1 S 0.78971(8) 0.54177(6) 0.60644(19) 0.0594(5) Uani 1 1 d . . . OW2 O 0.5299(3) 0.8140(2) 0.5592(6) 0.099(2) Uani 1 1 d D . . HW1A H 0.924(2) 0.588(3) 0.603(13) 0.148 Uiso 1 1 d D . . HW1B H 0.966(4) 0.6174(19) 0.584(10) 0.148 Uiso 1 1 d D . . HW2A H 0.504(4) 0.803(4) 0.509(7) 0.148 Uiso 1 1 d D . . HW2B H 0.522(5) 0.801(3) 0.623(5) 0.148 Uiso 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 0.0732(3) 0.0651(3) 0.01700(16) 0.0010(3) -0.0010(3) -0.0081(3) C1 0.059(4) 0.049(5) 0.039(4) -0.009(3) -0.001(3) -0.012(4) C2 0.068(5) 0.047(4) 0.043(5) -0.017(4) 0.008(4) -0.018(4) C3 0.057(4) 0.048(5) 0.053(4) -0.020(4) 0.023(4) -0.013(4) C4 0.048(4) 0.036(4) 0.066(5) -0.007(3) 0.003(3) -0.011(3) C5 0.046(3) 0.038(4) 0.037(4) -0.007(3) 0.002(3) -0.016(3) C6 0.049(4) 0.043(4) 0.046(4) 0.007(3) -0.004(3) -0.003(3) C7 0.042(4) 0.047(4) 0.047(4) -0.006(3) -0.002(3) -0.009(3) C8 0.040(3) 0.042(4) 0.041(3) -0.009(3) 0.010(3) -0.003(3) C9 0.045(4) 0.045(4) 0.052(4) 0.004(3) -0.001(3) -0.007(3) C10 0.039(3) 0.038(4) 0.042(4) 0.000(3) -0.003(3) -0.012(3) C11 0.040(3) 0.027(3) 0.027(3) -0.002(2) -0.003(2) -0.001(3) C12 0.039(3) 0.035(3) 0.032(3) 0.004(3) -0.010(3) -0.002(2) C13 0.041(5) 0.026(5) 0.025(5) 0.003(3) -0.002(3) -0.003(3) C14 0.037(3) 0.028(3) 0.021(3) -0.004(2) -0.001(2) 0.003(3) C15 0.040(3) 0.034(3) 0.023(2) 0.003(3) 0.003(3) -0.001(2) C16 0.026(4) 0.036(5) 0.018(5) 0.001(3) 0.000(2) -0.002(3) C17 0.049(4) 0.024(3) 0.022(3) -0.002(2) -0.001(2) 0.003(3) C18 0.048(3) 0.038(3) 0.023(2) 0.009(3) -0.004(3) 0.009(3) C19 0.052(3) 0.033(3) 0.021(2) -0.002(3) 0.004(3) 0.009(3) C20 0.043(3) 0.033(4) 0.020(3) 0.003(2) -0.002(2) 0.000(3) N1 0.034(4) 0.040(4) 0.021(5) 0.002(2) -0.0043(19) -0.006(2) N2 0.049(4) 0.044(4) 0.015(5) 0.003(2) 0.003(2) -0.005(3) O1 0.127(5) 0.092(5) 0.119(6) 0.005(4) 0.080(4) 0.012(4) O2 0.077(4) 0.072(4) 0.074(4) 0.003(3) 0.001(3) 0.042(3) O3 0.121(5) 0.122(6) 0.073(4) -0.041(4) -0.036(4) 0.039(4) OW1 0.112(4) 0.099(5) 0.069(4) -0.009(5) -0.013(5) 0.039(4) S1 0.0654(11) 0.0718(14) 0.0410(9) 0.0054(12) 0.0168(11) 0.0179(10) OW2 0.118(5) 0.092(5) 0.085(5) 0.019(4) 0.033(4) 0.021(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 N1 2.132(8) . ? Ag1 N2 2.169(8) 1_556 ? C1 C2 1.353(9) . ? C1 C10 1.382(8) . ? C1 H1 0.9300 . ? C2 C3 1.401(9) . ? C2 H2 0.9300 . ? C3 C4 1.340(9) . ? C3 H3 0.9300 . ? C4 C5 1.451(8) . ? C4 H4 0.9300 . ? C5 C10 1.390(8) . ? C5 C6 1.421(8) . ? C6 C7 1.362(9) . ? C6 H6 0.9300 . ? C7 C8 1.434(9) . ? C7 H7 0.9300 . ? C8 C9 1.352(9) . ? C8 S1 1.763(6) . ? C9 C10 1.466(8) . ? C9 H9 0.9300 . ? C11 C12 1.364(8) . ? C11 C13 1.393(8) . ? C11 H11 0.9300 . ? C12 N1 1.348(8) . ? C12 H12 0.9300 . ? C13 C14 1.403(8) . ? C13 C16 1.490(6) . ? C14 C15 1.396(8) . ? C14 H14 0.9300 . ? C15 N1 1.332(7) . ? C15 H15 0.9300 . ? C16 C17 1.369(9) . ? C16 C20 1.379(9) . ? C17 C18 1.384(8) . ? C17 H17 0.9300 . ? C18 N2 1.339(8) . ? C18 H18 0.9300 . ? C19 N2 1.321(8) . ? C19 C20 1.389(8) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? N2 Ag1 2.169(8) 1_554 ? O1 S1 1.402(6) . ? O2 S1 1.417(5) . ? O3 S1 1.501(6) . ? OW1 HW1A 0.78(4) . ? OW1 HW1B 0.84(4) . ? OW2 HW2A 0.87(4) . ? OW2 HW2B 0.84(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 Ag1 N2 179.4(2) . 1_556 ? C2 C1 C10 119.7(7) . . ? C2 C1 H1 120.2 . . ? C10 C1 H1 120.2 . . ? C1 C2 C3 122.3(7) . . ? C1 C2 H2 118.8 . . ? C3 C2 H2 118.8 . . ? C4 C3 C2 119.8(6) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 119.0(6) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C10 C5 C6 119.2(6) . . ? C10 C5 C4 119.6(6) . . ? C6 C5 C4 121.3(6) . . ? C7 C6 C5 121.6(6) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C8 118.9(6) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C9 C8 C7 121.9(6) . . ? C9 C8 S1 120.9(5) . . ? C7 C8 S1 117.1(5) . . ? C8 C9 C10 118.7(6) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C1 C10 C5 119.6(6) . . ? C1 C10 C9 120.7(6) . . ? C5 C10 C9 119.6(5) . . ? C12 C11 C13 120.4(6) . . ? C12 C11 H11 119.8 . . ? C13 C11 H11 119.8 . . ? N1 C12 C11 124.2(6) . . ? N1 C12 H12 117.9 . . ? C11 C12 H12 117.9 . . ? C11 C13 C14 115.7(7) . . ? C11 C13 C16 122.8(6) . . ? C14 C13 C16 121.5(6) . . ? C15 C14 C13 120.4(6) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? N1 C15 C14 122.6(6) . . ? N1 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? C17 C16 C20 119.0(7) . . ? C17 C16 C13 122.0(6) . . ? C20 C16 C13 119.0(6) . . ? C16 C17 C18 119.3(6) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? N2 C18 C17 121.7(6) . . ? N2 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? N2 C19 C20 122.4(6) . . ? N2 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C16 C20 C19 118.6(6) . . ? C16 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? C15 N1 C12 116.7(7) . . ? C15 N1 Ag1 119.9(5) . . ? C12 N1 Ag1 123.2(5) . . ? C19 N2 C18 119.0(7) . . ? C19 N2 Ag1 120.2(5) . 1_554 ? C18 N2 Ag1 120.8(5) . 1_554 ? HW1A OW1 HW1B 107(5) . . ? O1 S1 O2 117.8(4) . . ? O1 S1 O3 111.3(5) . . ? O2 S1 O3 106.5(4) . . ? O1 S1 C8 107.0(3) . . ? O2 S1 C8 108.6(3) . . ? O3 S1 C8 104.8(3) . . ? HW2A OW2 HW2B 105(5) . . ? 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 C10 C1 C2 C3 0.3(10) . . . . ? C1 C2 C3 C4 1.5(10) . . . . ? C2 C3 C4 C5 -2.5(9) . . . . ? C3 C4 C5 C10 1.7(8) . . . . ? C3 C4 C5 C6 -178.5(6) . . . . ? C10 C5 C6 C7 2.4(9) . . . . ? C4 C5 C6 C7 -177.4(6) . . . . ? C5 C6 C7 C8 -1.8(10) . . . . ? C6 C7 C8 C9 1.6(10) . . . . ? C6 C7 C8 S1 178.7(5) . . . . ? C7 C8 C9 C10 -1.9(9) . . . . ? S1 C8 C9 C10 -178.8(4) . . . . ? C2 C1 C10 C5 -1.1(9) . . . . ? C2 C1 C10 C9 -178.1(6) . . . . ? C6 C5 C10 C1 -179.7(6) . . . . ? C4 C5 C10 C1 0.1(8) . . . . ? C6 C5 C10 C9 -2.6(8) . . . . ? C4 C5 C10 C9 177.2(5) . . . . ? C8 C9 C10 C1 179.4(6) . . . . ? C8 C9 C10 C5 2.4(9) . . . . ? C13 C11 C12 N1 0.1(9) . . . . ? C12 C11 C13 C14 0.0(8) . . . . ? C12 C11 C13 C16 -177.8(6) . . . . ? C11 C13 C14 C15 0.1(8) . . . . ? C16 C13 C14 C15 178.0(6) . . . . ? C13 C14 C15 N1 -0.5(8) . . . . ? C11 C13 C16 C17 -141.9(6) . . . . ? C14 C13 C16 C17 40.4(10) . . . . ? C11 C13 C16 C20 39.1(10) . . . . ? C14 C13 C16 C20 -138.6(5) . . . . ? C20 C16 C17 C18 2.5(8) . . . . ? C13 C16 C17 C18 -176.5(6) . . . . ? C16 C17 C18 N2 -0.9(8) . . . . ? C17 C16 C20 C19 -2.3(8) . . . . ? C13 C16 C20 C19 176.6(5) . . . . ? N2 C19 C20 C16 0.6(8) . . . . ? C14 C15 N1 C12 0.7(7) . . . . ? C14 C15 N1 Ag1 176.2(4) . . . . ? C11 C12 N1 C15 -0.5(8) . . . . ? C11 C12 N1 Ag1 -175.8(4) . . . . ? C20 C19 N2 C18 1.0(8) . . . . ? C20 C19 N2 Ag1 177.3(4) . . . 1_554 ? C17 C18 N2 C19 -0.9(8) . . . . ? C17 C18 N2 Ag1 -177.1(4) . . . 1_554 ? C9 C8 S1 O1 -118.2(6) . . . . ? C7 C8 S1 O1 64.6(6) . . . . ? C9 C8 S1 O2 10.0(7) . . . . ? C7 C8 S1 O2 -167.2(5) . . . . ? C9 C8 S1 O3 123.4(6) . . . . ? C7 C8 S1 O3 -53.7(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OW2 HW2B O3 0.84(4) 2.02(5) 2.858(9) 177(10) 3_655 OW1 HW1A O1 0.78(4) 2.27(6) 3.027(9) 165(15) . OW1 HW1B OW2 0.84(4) 2.14(5) 2.965(10) 168(11) 14_665 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.659 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.086 #===end data_Compd3 _database_code_depnum_ccdc_archive 'CCDC 684625' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C10 H8 Ag N2), C7 H4 O6 S, 3(H2 O)' _chemical_formula_sum 'C27 H26 Ag2 N4 O9 S' _chemical_formula_weight 798.32 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/m' _symmetry_space_group_name_Hall '-P 2yb ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.3615(2) _cell_length_b 17.614(4) _cell_length_c 11.267(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.06(3) _cell_angle_gamma 90.00 _cell_volume 1388.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used Total _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.333 _exptl_crystal_size_mid 0.313 _exptl_crystal_size_min 0.296 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.909 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 1.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.605 _exptl_absorpt_correction_T_max 0.635 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 3287 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13545 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3287 _reflns_number_gt 2836 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.6621P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0062(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3287 _refine_ls_number_parameters 227 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0661 _refine_ls_wR_factor_gt 0.0636 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.056 _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 0.15175(2) 0.513079(11) -0.081356(14) 0.04461(9) Uani 1 1 d . . . C1 C 0.6568(4) 0.2500 0.2209(3) 0.0356(6) Uani 1 2 d S . . C2 C 0.4607(5) 0.2500 0.2041(3) 0.0448(8) Uani 1 2 d S . . H2 H 0.3745 0.2500 0.1238 0.054 Uiso 1 2 calc SR . . C3 C 0.3947(5) 0.2500 0.3050(4) 0.0505(9) Uani 1 2 d S . . H3 H 0.2638 0.2500 0.2925 0.061 Uiso 1 2 calc SR . . C4 C 0.5201(5) 0.2500 0.4256(4) 0.0437(8) Uani 1 2 d S . . C5 C 0.7191(4) 0.2500 0.4447(3) 0.0359(6) Uani 1 2 d S . . C6 C 0.7835(4) 0.2500 0.3409(3) 0.0326(6) Uani 1 2 d S . . H6 H 0.9142 0.2500 0.3523 0.039 Uiso 1 2 calc SR . . C7 C 0.8585(5) 0.2500 0.5742(3) 0.0431(7) Uani 1 2 d S . . C8 C 0.4250(3) 0.45304(14) 0.1620(2) 0.0450(5) Uani 1 1 d . . . H8A H 0.3821 0.4073 0.1217 0.054 Uiso 1 1 calc R . . C9 C 0.5481(3) 0.45060(12) 0.2819(2) 0.0429(5) Uani 1 1 d . . . H9A H 0.5876 0.4041 0.3202 0.052 Uiso 1 1 calc R . . C10 C 0.6135(3) 0.51733(11) 0.34570(18) 0.0298(4) Uani 1 1 d . . . C11 C 0.5554(4) 0.58383(13) 0.2803(2) 0.0529(7) Uani 1 1 d . . . H11A H 0.5995 0.6303 0.3174 0.063 Uiso 1 1 calc R . . C12 C 0.4316(4) 0.58162(14) 0.1596(2) 0.0543(7) Uani 1 1 d . . . H12A H 0.3940 0.6273 0.1180 0.065 Uiso 1 1 calc R . . C13 C 0.7765(4) 0.45030(13) 0.5465(2) 0.0444(5) Uani 1 1 d . . . H13A H 0.7270 0.4045 0.5090 0.053 Uiso 1 1 calc R . . C14 C 0.8891(4) 0.45091(13) 0.6694(2) 0.0441(5) Uani 1 1 d . . . H14A H 0.9138 0.4052 0.7128 0.053 Uiso 1 1 calc R . . C15 C 0.9246(3) 0.57923(13) 0.6637(2) 0.0449(5) Uani 1 1 d . . . H15A H 0.9740 0.6243 0.7039 0.054 Uiso 1 1 calc R . . C16 C 0.8141(3) 0.58273(12) 0.5399(2) 0.0414(5) Uani 1 1 d . . . H16A H 0.7923 0.6291 0.4985 0.050 Uiso 1 1 calc R . . C17 C 0.7357(3) 0.51691(11) 0.47758(18) 0.0283(4) Uani 1 1 d . . . N1 N 0.9644(3) 0.51467(10) 0.72902(16) 0.0344(4) Uani 1 1 d . . . N2 N 0.3634(3) 0.51748(11) 0.10009(17) 0.0381(4) Uani 1 1 d . . . O1 O 0.5859(4) 0.2500 -0.0190(2) 0.0670(8) Uani 1 2 d S . . O2 O 0.8584(3) 0.31814(13) 0.10363(18) 0.0747(7) Uani 1 1 d . . . O3 O 0.7857(4) 0.2500 0.6627(2) 0.0640(7) Uani 1 2 d S . . O4 O 1.0326(4) 0.2500 0.5878(2) 0.0578(7) Uani 1 2 d S . . O5 O 0.4546(4) 0.2500 0.5239(3) 0.0622(7) Uani 1 2 d SD . . OW1 O 0.2088(4) 0.2500 0.8356(3) 0.0687(8) Uani 1 2 d SD . . OW2 O 0.0803(3) 0.36690(11) 0.9534(2) 0.0630(5) Uani 1 1 d D . . S1 S 0.74595(12) 0.2500 0.09221(7) 0.03840(18) Uani 1 2 d S . . H7A H 0.550(5) 0.2500 0.589(4) 0.058 Uiso 1 2 d SD . . HW1A H 0.184(4) 0.2500 0.7567(10) 0.058 Uiso 1 2 d SD . . HW1B H 0.3304(15) 0.2500 0.859(3) 0.058 Uiso 1 2 d SD . . HW2A H 0.115(4) 0.3289(10) 0.921(2) 0.058 Uiso 1 1 d D . . HW2B H 0.011(3) 0.3468(13) 0.993(2) 0.058 Uiso 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 0.04711(12) 0.05444(13) 0.02037(10) -0.00009(7) -0.00689(7) 0.00349(8) C1 0.0420(16) 0.0233(13) 0.0371(15) 0.000 0.0058(13) 0.000 C2 0.0405(16) 0.0298(15) 0.053(2) 0.000 -0.0019(15) 0.000 C3 0.0370(16) 0.0357(17) 0.076(3) 0.000 0.0126(17) 0.000 C4 0.0499(18) 0.0267(14) 0.060(2) 0.000 0.0244(17) 0.000 C5 0.0433(16) 0.0245(14) 0.0394(16) 0.000 0.0123(13) 0.000 C6 0.0351(14) 0.0259(13) 0.0331(14) 0.000 0.0051(12) 0.000 C7 0.060(2) 0.0342(16) 0.0341(17) 0.000 0.0136(15) 0.000 C8 0.0574(13) 0.0333(11) 0.0287(10) -0.0034(9) -0.0095(10) 0.0009(10) C9 0.0554(13) 0.0268(11) 0.0307(11) -0.0005(9) -0.0097(9) 0.0042(10) C10 0.0331(9) 0.0301(10) 0.0211(9) 0.0018(7) 0.0009(7) 0.0012(8) C11 0.0777(17) 0.0289(11) 0.0314(11) 0.0040(9) -0.0133(11) -0.0065(11) C12 0.0780(17) 0.0349(12) 0.0305(11) 0.0081(10) -0.0116(11) -0.0035(12) C13 0.0638(14) 0.0275(11) 0.0273(10) 0.0003(9) -0.0073(10) -0.0026(10) C14 0.0589(13) 0.0330(12) 0.0278(10) 0.0040(9) -0.0048(9) 0.0001(10) C15 0.0582(14) 0.0356(12) 0.0276(10) -0.0032(9) -0.0063(9) -0.0085(10) C16 0.0562(13) 0.0281(10) 0.0278(10) 0.0020(8) -0.0047(9) -0.0038(10) C17 0.0334(9) 0.0268(10) 0.0198(9) 0.0004(7) 0.0012(7) 0.0010(7) N1 0.0385(9) 0.0375(9) 0.0193(8) 0.0010(7) -0.0025(7) -0.0001(7) N2 0.0438(10) 0.0377(10) 0.0231(8) 0.0037(7) -0.0034(7) 0.0013(8) O1 0.0665(17) 0.082(2) 0.0331(13) 0.000 -0.0124(12) 0.000 O2 0.1097(17) 0.0730(14) 0.0477(11) -0.0221(10) 0.0336(11) -0.0477(13) O3 0.0763(18) 0.082(2) 0.0392(14) 0.000 0.0264(13) 0.000 O4 0.0515(14) 0.083(2) 0.0331(12) 0.000 0.0054(11) 0.000 O5 0.0625(16) 0.0610(17) 0.076(2) 0.000 0.0396(15) 0.000 OW1 0.0566(16) 0.099(2) 0.0429(15) 0.000 0.0048(13) 0.000 OW2 0.0797(14) 0.0441(10) 0.0643(13) 0.0014(9) 0.0209(11) -0.0075(10) S1 0.0509(4) 0.0298(4) 0.0251(3) 0.000 -0.0019(3) 0.000 _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 N2 2.154(2) . ? Ag1 N1 2.154(2) 1_454 ? Ag1 Ag1 3.3323(9) 3_565 ? C1 C6 1.384(4) . ? C1 C2 1.396(4) . ? C1 S1 1.767(3) . ? C2 C3 1.368(5) . ? C2 H2 0.9300 . ? C3 C4 1.386(5) . ? C3 H3 0.9300 . ? C4 O5 1.338(4) . ? C4 C5 1.413(5) . ? C5 C6 1.392(4) . ? C5 C7 1.501(5) . ? C6 H6 0.9300 . ? C7 O4 1.242(4) . ? C7 O3 1.270(4) . ? C8 N2 1.336(3) . ? C8 C9 1.375(3) . ? C8 H8A 0.9300 . ? C9 C10 1.384(3) . ? C9 H9A 0.9300 . ? C10 C11 1.380(3) . ? C10 C17 1.479(3) . ? C11 C12 1.383(3) . ? C11 H11A 0.9300 . ? C12 N2 1.330(3) . ? C12 H12A 0.9300 . ? C13 C14 1.377(3) . ? C13 C17 1.387(3) . ? C13 H13A 0.9300 . ? C14 N1 1.337(3) . ? C14 H14A 0.9300 . ? C15 N1 1.337(3) . ? C15 C16 1.381(3) . ? C15 H15A 0.9300 . ? C16 C17 1.385(3) . ? C16 H16A 0.9300 . ? N1 Ag1 2.1541(19) 1_656 ? O1 S1 1.429(3) . ? O2 S1 1.441(2) . ? O5 H7A 0.84(3) . ? OW1 HW1A 0.851(10) . ? OW1 HW1B 0.852(10) . ? OW2 HW2A 0.842(10) . ? OW2 HW2B 0.846(10) . ? S1 O2 1.441(2) 4_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 N2 Ag1 N1 173.37(7) . 1_454 ? N2 Ag1 Ag1 83.91(5) . 3_565 ? N1 Ag1 Ag1 102.43(5) 1_454 3_565 ? C6 C1 C2 119.2(3) . . ? C6 C1 S1 119.5(2) . . ? C2 C1 S1 121.3(3) . . ? C3 C2 C1 120.4(3) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 121.0(3) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? O5 C4 C3 120.7(3) . . ? O5 C4 C5 119.7(3) . . ? C3 C4 C5 119.6(3) . . ? C6 C5 C4 118.6(3) . . ? C6 C5 C7 120.6(3) . . ? C4 C5 C7 120.8(3) . . ? C1 C6 C5 121.2(3) . . ? C1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? O4 C7 O3 125.0(3) . . ? O4 C7 C5 119.3(3) . . ? O3 C7 C5 115.8(3) . . ? N2 C8 C9 123.6(2) . . ? N2 C8 H8A 118.2 . . ? C9 C8 H8A 118.2 . . ? C8 C9 C10 120.1(2) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 116.30(19) . . ? C11 C10 C17 122.16(18) . . ? C9 C10 C17 121.52(18) . . ? C10 C11 C12 120.1(2) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? N2 C12 C11 123.4(2) . . ? N2 C12 H12A 118.3 . . ? C11 C12 H12A 118.3 . . ? C14 C13 C17 121.0(2) . . ? C14 C13 H13A 119.5 . . ? C17 C13 H13A 119.5 . . ? N1 C14 C13 122.6(2) . . ? N1 C14 H14A 118.7 . . ? C13 C14 H14A 118.7 . . ? N1 C15 C16 123.6(2) . . ? N1 C15 H15A 118.2 . . ? C16 C15 H15A 118.2 . . ? C15 C16 C17 119.8(2) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C16 C17 C13 116.13(19) . . ? C16 C17 C10 122.20(18) . . ? C13 C17 C10 121.66(18) . . ? C15 N1 C14 116.87(19) . . ? C15 N1 Ag1 121.39(14) . 1_656 ? C14 N1 Ag1 121.68(15) . 1_656 ? C12 N2 C8 116.4(2) . . ? C12 N2 Ag1 123.93(15) . . ? C8 N2 Ag1 119.56(15) . . ? C4 O5 H7A 107(3) . . ? HW1A OW1 HW1B 100.4(15) . . ? HW2A OW2 HW2B 102.0(14) . . ? O1 S1 O2 111.91(12) . . ? O1 S1 O2 111.91(12) . 4_565 ? O2 S1 O2 112.8(2) . 4_565 ? O1 S1 C1 107.70(17) . . ? O2 S1 C1 106.03(10) . . ? O2 S1 C1 106.03(10) 4_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.0 . . . . ? S1 C1 C2 C3 180.0 . . . . ? C1 C2 C3 C4 0.0 . . . . ? C2 C3 C4 O5 180.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? O5 C4 C5 C6 180.000(1) . . . . ? C3 C4 C5 C6 0.0 . . . . ? O5 C4 C5 C7 0.0 . . . . ? C3 C4 C5 C7 180.000(1) . . . . ? C2 C1 C6 C5 0.0 . . . . ? S1 C1 C6 C5 180.0 . . . . ? C4 C5 C6 C1 0.0 . . . . ? C7 C5 C6 C1 180.0 . . . . ? C6 C5 C7 O4 0.000(1) . . . . ? C4 C5 C7 O4 180.0 . . . . ? C6 C5 C7 O3 180.000(1) . . . . ? C4 C5 C7 O3 0.000(1) . . . . ? N2 C8 C9 C10 0.8(4) . . . . ? C8 C9 C10 C11 -2.9(4) . . . . ? C8 C9 C10 C17 175.9(2) . . . . ? C9 C10 C11 C12 2.8(4) . . . . ? C17 C10 C11 C12 -176.0(2) . . . . ? C10 C11 C12 N2 -0.5(5) . . . . ? C17 C13 C14 N1 0.1(4) . . . . ? N1 C15 C16 C17 0.9(4) . . . . ? C15 C16 C17 C13 -0.3(4) . . . . ? C15 C16 C17 C10 178.9(2) . . . . ? C14 C13 C17 C16 -0.2(4) . . . . ? C14 C13 C17 C10 -179.4(2) . . . . ? C11 C10 C17 C16 -6.2(4) . . . . ? C9 C10 C17 C16 175.1(2) . . . . ? C11 C10 C17 C13 172.9(2) . . . . ? C9 C10 C17 C13 -5.8(3) . . . . ? C16 C15 N1 C14 -1.0(4) . . . . ? C16 C15 N1 Ag1 176.3(2) . . . 1_656 ? C13 C14 N1 C15 0.4(4) . . . . ? C13 C14 N1 Ag1 -176.8(2) . . . 1_656 ? C11 C12 N2 C8 -1.8(4) . . . . ? C11 C12 N2 Ag1 174.4(2) . . . . ? C9 C8 N2 C12 1.6(4) . . . . ? C9 C8 N2 Ag1 -174.7(2) . . . . ? Ag1 Ag1 N2 C12 -97.8(2) 3_565 . . . ? Ag1 Ag1 N2 C8 78.28(18) 3_565 . . . ? C6 C1 S1 O1 180.0 . . . . ? C2 C1 S1 O1 0.0 . . . . ? C6 C1 S1 O2 -60.06(12) . . . . ? C2 C1 S1 O2 119.94(12) . . . . ? C6 C1 S1 O2 60.06(12) . . . 4_565 ? C2 C1 S1 O2 -119.94(12) . . . 4_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OW2 HW2B O2 0.846(10) 1.991(10) 2.825(3) 169(2) 1_456 OW2 HW2A OW1 0.842(10) 1.932(10) 2.770(3) 173(2) . OW1 HW1A O4 0.851(10) 1.884(14) 2.689(4) 157(3) 1_455 O5 H7A O3 0.84(3) 1.67(4) 2.454(4) 153(4) . OW1 HW1B O1 0.852(10) 1.956(15) 2.752(4) 155(3) 1_556 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.388 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.102 #===end data_compd4 _database_code_depnum_ccdc_archive 'CCDC 684626' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H14 Ag N3 O3 S, H2 O ' _chemical_formula_sum 'C16 H16 Ag N3 O4 S' _chemical_formula_weight 454.25 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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.992(2) _cell_length_b 10.059(1) _cell_length_c 10.216(2) _cell_angle_alpha 103.93(3) _cell_angle_beta 111.48(1) _cell_angle_gamma 103.55(1) _cell_volume 866.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4244 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.4 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 1.310 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.649 _exptl_absorpt_correction_T_max 0.785 _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 SMART APEX CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 6270 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 28.35 _reflns_number_total 4244 _reflns_number_gt 2940 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4244 _refine_ls_number_parameters 242 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _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 -0.12942(3) 0.39222(3) 0.08450(3) 0.05469(12) Uani 1 1 d . . . C1 C 0.1693(3) 0.8519(3) 0.3848(3) 0.0409(7) Uani 1 1 d . . . C2 C 0.0933(3) 0.8688(3) 0.4724(3) 0.0442(7) Uani 1 1 d . . . H2 H -0.0053 0.8717 0.4315 0.053 Uiso 1 1 calc R . . C3 C 0.1641(4) 0.8816(3) 0.6214(4) 0.0457(7) Uani 1 1 d . . . H3 H 0.1136 0.8961 0.6811 0.055 Uiso 1 1 calc R . . C4 C 0.3105(3) 0.8731(3) 0.6840(3) 0.0427(7) Uani 1 1 d . . . C5 C 0.3867(4) 0.8595(4) 0.5943(4) 0.0519(8) Uani 1 1 d . . . H5 H 0.4856 0.8572 0.6345 0.062 Uiso 1 1 calc R . . C6 C 0.3171(4) 0.8495(4) 0.4467(4) 0.0500(8) Uani 1 1 d . . . H6 H 0.3695 0.8411 0.3882 0.060 Uiso 1 1 calc R . . C7 C 0.1149(4) 0.4922(3) 0.4111(3) 0.0511(8) Uani 1 1 d . . . H7 H 0.0778 0.5689 0.4173 0.061 Uiso 1 1 calc R . . C8 C 0.2265(4) 0.4948(3) 0.5399(3) 0.0495(8) Uani 1 1 d . . . H8 H 0.2627 0.5715 0.6307 0.059 Uiso 1 1 calc R . . C9 C 0.2858(3) 0.3825(3) 0.5350(3) 0.0374(7) Uani 1 1 d . . . C10 C 0.2251(3) 0.2711(3) 0.3966(3) 0.0426(7) Uani 1 1 d . . . H10 H 0.2601 0.1930 0.3875 0.051 Uiso 1 1 calc R . . C11 C 0.5284(4) 0.5150(3) 0.7754(4) 0.0616(10) Uani 1 1 d . . . H11 H 0.5285 0.6029 0.7610 0.074 Uiso 1 1 calc R . . C12 C 0.4085(3) 0.3844(3) 0.6727(3) 0.0394(7) Uani 1 1 d . . . C13 C 0.4120(3) 0.2599(3) 0.7057(3) 0.0474(8) Uani 1 1 d . . . H13 H 0.3325 0.1706 0.6429 0.057 Uiso 1 1 calc R . . C14 C 0.5332(4) 0.2680(3) 0.8318(4) 0.0523(9) Uani 1 1 d . . . H14 H 0.5323 0.1825 0.8520 0.063 Uiso 1 1 calc R . . C15 C 0.6464(4) 0.5141(4) 0.8976(4) 0.0646(11) Uani 1 1 d . . . H15 H 0.7264 0.6024 0.9633 0.078 Uiso 1 1 calc R . . C16 C 0.1121(3) 0.2768(3) 0.2719(3) 0.0459(7) Uani 1 1 d . . . H16 H 0.0727 0.2010 0.1797 0.055 Uiso 1 1 calc R . . N1 N 0.3744(4) 0.8734(4) 0.8287(4) 0.0609(8) Uani 1 1 d . . . N2 N 0.0566(3) 0.3859(3) 0.2773(3) 0.0417(6) Uani 1 1 d . . . N3 N 0.6517(3) 0.3915(3) 0.9267(3) 0.0484(7) Uani 1 1 d . . . O1 O 0.0164(3) 0.6665(2) 0.1104(3) 0.0626(7) Uani 1 1 d . . . O2 O 0.1947(4) 0.8930(3) 0.1531(3) 0.0979(11) Uani 1 1 d . . . O3 O -0.0425(4) 0.8835(4) 0.1708(3) 0.1121(14) Uani 1 1 d . . . OW1 O 0.2934(3) 0.0916(4) 0.0433(4) 0.0812(9) Uani 1 1 d D . . S1 S 0.07540(10) 0.82240(9) 0.19061(9) 0.0516(2) Uani 1 1 d . . . HN1 H 0.481(5) 0.891(4) 0.876(4) 0.078(13) Uiso 1 1 d . . . HN2 H 0.352(6) 0.922(5) 0.888(6) 0.10(2) Uiso 1 1 d . . . HW1A H 0.224(5) 0.104(5) -0.016(5) 0.103(18) Uiso 1 1 d D . . HW1B H 0.251(5) 0.015(4) 0.056(5) 0.089(16) Uiso 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 0.04357(16) 0.06512(19) 0.03897(15) 0.02151(12) -0.00368(10) 0.02521(13) C1 0.0387(16) 0.0299(14) 0.0382(15) 0.0105(12) 0.0033(12) 0.0099(12) C2 0.0339(15) 0.0383(16) 0.0467(17) 0.0114(13) 0.0064(13) 0.0131(13) C3 0.0433(17) 0.0432(16) 0.0479(17) 0.0149(14) 0.0186(14) 0.0154(14) C4 0.0394(16) 0.0348(15) 0.0371(15) 0.0091(13) 0.0045(13) 0.0093(12) C5 0.0341(16) 0.064(2) 0.0481(18) 0.0193(16) 0.0066(14) 0.0218(15) C6 0.0418(18) 0.061(2) 0.0425(17) 0.0161(15) 0.0157(14) 0.0192(15) C7 0.0488(18) 0.0383(16) 0.0474(18) 0.0141(14) -0.0010(14) 0.0223(14) C8 0.0494(18) 0.0350(15) 0.0372(16) 0.0076(13) -0.0062(13) 0.0171(14) C9 0.0261(13) 0.0334(14) 0.0397(15) 0.0169(12) 0.0004(11) 0.0083(11) C10 0.0391(16) 0.0412(16) 0.0380(15) 0.0118(13) 0.0056(13) 0.0199(13) C11 0.0472(19) 0.0363(16) 0.061(2) 0.0227(15) -0.0140(16) 0.0041(14) C12 0.0301(14) 0.0390(15) 0.0368(15) 0.0164(13) 0.0012(12) 0.0113(12) C13 0.0369(16) 0.0373(15) 0.0469(17) 0.0201(14) -0.0033(13) 0.0088(12) C14 0.0430(18) 0.0454(17) 0.0540(19) 0.0289(15) 0.0012(15) 0.0133(14) C15 0.049(2) 0.0400(17) 0.058(2) 0.0161(16) -0.0171(16) 0.0049(15) C16 0.0407(17) 0.0503(17) 0.0341(15) 0.0108(14) 0.0046(13) 0.0193(14) N1 0.056(2) 0.072(2) 0.0407(16) 0.0195(16) 0.0088(15) 0.0232(17) N2 0.0339(13) 0.0435(13) 0.0374(13) 0.0206(11) 0.0016(10) 0.0134(11) N3 0.0365(14) 0.0487(15) 0.0392(14) 0.0189(12) -0.0052(11) 0.0131(11) O1 0.0662(16) 0.0473(13) 0.0467(13) 0.0070(11) 0.0088(12) 0.0111(11) O2 0.096(2) 0.097(2) 0.0682(18) 0.0505(17) 0.0171(17) -0.0091(18) O3 0.132(3) 0.137(3) 0.0561(17) 0.0244(18) 0.0033(18) 0.105(3) OW1 0.0530(17) 0.114(3) 0.091(2) 0.072(2) 0.0228(16) 0.0331(17) S1 0.0548(5) 0.0428(4) 0.0388(4) 0.0149(3) 0.0016(4) 0.0177(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 N2 2.184(2) . ? Ag1 N3 2.188(2) 1_454 ? C1 C2 1.375(4) . ? C1 C6 1.386(4) . ? C1 S1 1.768(3) . ? C2 C3 1.381(4) . ? C2 H2 0.9300 . ? C3 C4 1.398(4) . ? C3 H3 0.9300 . ? C4 N1 1.379(4) . ? C4 C5 1.392(5) . ? C5 C6 1.375(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 N2 1.331(4) . ? C7 C8 1.368(4) . ? C7 H7 0.9300 . ? C8 C9 1.391(4) . ? C8 H8 0.9300 . ? C9 C10 1.384(4) . ? C9 C12 1.482(4) . ? C10 C16 1.383(4) . ? C10 H10 0.9300 . ? C11 C15 1.372(4) . ? C11 C12 1.393(4) . ? C11 H11 0.9300 . ? C12 C13 1.377(4) . ? C13 C14 1.376(4) . ? C13 H13 0.9300 . ? C14 N3 1.333(4) . ? C14 H14 0.9300 . ? C15 N3 1.345(4) . ? C15 H15 0.9300 . ? C16 N2 1.340(4) . ? C16 H16 0.9300 . ? N1 HN1 0.94(4) . ? N1 HN2 0.82(5) . ? N3 Ag1 2.188(2) 1_656 ? O1 S1 1.439(2) . ? O2 S1 1.463(3) . ? O3 S1 1.426(3) . ? OW1 HW1A 0.79(3) . ? OW1 HW1B 0.85(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N3 164.95(10) . 1_454 ? C2 C1 C6 119.9(3) . . ? C2 C1 S1 120.4(2) . . ? C6 C1 S1 119.6(3) . . ? C1 C2 C3 119.8(3) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 121.1(3) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? N1 C4 C5 121.3(3) . . ? N1 C4 C3 120.5(3) . . ? C5 C4 C3 118.1(3) . . ? C6 C5 C4 120.6(3) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 120.4(3) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? N2 C7 C8 123.6(3) . . ? N2 C7 H7 118.2 . . ? C8 C7 H7 118.2 . . ? C7 C8 C9 119.9(3) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 116.9(2) . . ? C10 C9 C12 122.3(2) . . ? C8 C9 C12 120.8(3) . . ? C16 C10 C9 119.5(3) . . ? C16 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C15 C11 C12 120.0(3) . . ? C15 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 116.7(2) . . ? C13 C12 C9 122.8(2) . . ? C11 C12 C9 120.5(2) . . ? C14 C13 C12 119.9(3) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? N3 C14 C13 123.7(3) . . ? N3 C14 H14 118.2 . . ? C13 C14 H14 118.2 . . ? N3 C15 C11 123.0(3) . . ? N3 C15 H15 118.5 . . ? C11 C15 H15 118.5 . . ? N2 C16 C10 123.3(3) . . ? N2 C16 H16 118.4 . . ? C10 C16 H16 118.4 . . ? C4 N1 HN1 118(2) . . ? C4 N1 HN2 116(4) . . ? HN1 N1 HN2 109(4) . . ? C7 N2 C16 116.8(2) . . ? C7 N2 Ag1 119.10(19) . . ? C16 N2 Ag1 124.0(2) . . ? C14 N3 C15 116.6(2) . . ? C14 N3 Ag1 122.43(19) . 1_656 ? C15 N3 Ag1 119.0(2) . 1_656 ? HW1A OW1 HW1B 104(3) . . ? O3 S1 O1 113.1(2) . . ? O3 S1 O2 114.1(2) . . ? O1 S1 O2 109.33(19) . . ? O3 S1 C1 106.85(17) . . ? O1 S1 C1 106.92(13) . . ? O2 S1 C1 106.08(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.8(4) . . . . ? S1 C1 C2 C3 175.5(2) . . . . ? C1 C2 C3 C4 -2.0(4) . . . . ? C2 C3 C4 N1 -174.4(3) . . . . ? C2 C3 C4 C5 3.5(4) . . . . ? N1 C4 C5 C6 175.6(3) . . . . ? C3 C4 C5 C6 -2.3(5) . . . . ? C4 C5 C6 C1 -0.4(5) . . . . ? C2 C1 C6 C5 2.0(5) . . . . ? S1 C1 C6 C5 -174.3(3) . . . . ? N2 C7 C8 C9 0.5(6) . . . . ? C7 C8 C9 C10 -0.8(5) . . . . ? C7 C8 C9 C12 179.0(3) . . . . ? C8 C9 C10 C16 0.6(5) . . . . ? C12 C9 C10 C16 -179.2(3) . . . . ? C15 C11 C12 C13 3.4(6) . . . . ? C15 C11 C12 C9 -176.0(4) . . . . ? C10 C9 C12 C13 -39.4(5) . . . . ? C8 C9 C12 C13 140.8(3) . . . . ? C10 C9 C12 C11 140.0(3) . . . . ? C8 C9 C12 C11 -39.8(5) . . . . ? C11 C12 C13 C14 -2.5(5) . . . . ? C9 C12 C13 C14 176.9(3) . . . . ? C12 C13 C14 N3 -0.5(6) . . . . ? C12 C11 C15 N3 -1.4(7) . . . . ? C9 C10 C16 N2 -0.1(5) . . . . ? C8 C7 N2 C16 0.1(5) . . . . ? C8 C7 N2 Ag1 176.9(3) . . . . ? C10 C16 N2 C7 -0.3(5) . . . . ? C10 C16 N2 Ag1 -177.0(2) . . . . ? N3 Ag1 N2 C7 -64.3(4) 1_454 . . . ? N3 Ag1 N2 C16 112.3(4) 1_454 . . . ? C13 C14 N3 C15 2.6(6) . . . . ? C13 C14 N3 Ag1 -161.6(3) . . . 1_656 ? C11 C15 N3 C14 -1.6(6) . . . . ? C11 C15 N3 Ag1 163.2(3) . . . 1_656 ? C2 C1 S1 O3 25.0(3) . . . . ? C6 C1 S1 O3 -158.7(3) . . . . ? C2 C1 S1 O1 -96.3(3) . . . . ? C6 C1 S1 O1 80.0(3) . . . . ? C2 C1 S1 O2 147.1(3) . . . . ? C6 C1 S1 O2 -36.6(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OW1 HW1B O2 0.85(3) 1.87(3) 2.681(4) 160(4) 1_545 OW1 HW1A O3 0.79(3) 1.98(4) 2.770(4) 175(5) 2_565 N1 HN1 OW1 0.94(4) 2.04(4) 2.984(5) 173(3) 2_666 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.476 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.090 #===end data_compd5 _database_code_depnum_ccdc_archive 'CCDC 684627' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H22 Ag N5 O3 S ' _chemical_formula_sum 'C24 H22 Ag N5 O3 S' _chemical_formula_weight 568.40 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' 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 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.241(2) _cell_length_b 11.441(2) _cell_length_c 13.314(3) _cell_angle_alpha 76.90(3) _cell_angle_beta 82.36(3) _cell_angle_gamma 71.57(3) _cell_volume 1157.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5243 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.272 _exptl_crystal_size_mid 0.236 _exptl_crystal_size_min 0.124 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 0.889 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11469 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5243 _reflns_number_gt 3828 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+0.2364P] 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 5243 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1103 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 0.76929(4) 1.07222(2) 0.45611(2) 0.05645(13) Uani 1 1 d . . . C1 C 0.2495(4) 0.2659(3) 0.9164(3) 0.0451(8) Uani 1 1 d . . . C2 C 0.4270(5) 0.2229(4) 0.8905(3) 0.0560(9) Uani 1 1 d . . . H2 H 0.4778 0.1386 0.8873 0.067 Uiso 1 1 calc R . . C3 C 0.5260(5) 0.3029(4) 0.8698(3) 0.0572(10) Uani 1 1 d . . . H3 H 0.6421 0.2722 0.8511 0.069 Uiso 1 1 calc R . . C4 C 0.4574(5) 0.4284(3) 0.8759(3) 0.0472(8) Uani 1 1 d . . . C5 C 0.2829(5) 0.4723(3) 0.9039(3) 0.0479(8) Uani 1 1 d . . . H5 H 0.2338 0.5560 0.9095 0.057 Uiso 1 1 calc R . . C6 C 0.1832(5) 0.3929(3) 0.9230(3) 0.0497(8) Uani 1 1 d . . . H6 H 0.0670 0.4245 0.9411 0.060 Uiso 1 1 calc R . . C7 C 0.6094(5) 0.6934(4) 0.8244(3) 0.0487(8) Uani 1 1 d . . . C8 C 0.7843(5) 0.6491(4) 0.8155(3) 0.0588(10) Uani 1 1 d . . . H8 H 0.8383 0.5630 0.8249 0.071 Uiso 1 1 calc R . . C9 C 0.8806(5) 0.7319(4) 0.7926(3) 0.0602(10) Uani 1 1 d . . . H9 H 0.9995 0.7012 0.7868 0.072 Uiso 1 1 calc R . . C10 C 0.8036(5) 0.8583(3) 0.7784(3) 0.0465(8) Uani 1 1 d . . . C11 C 0.6259(5) 0.9041(4) 0.7864(4) 0.0657(11) Uani 1 1 d . . . H11 H 0.5723 0.9903 0.7759 0.079 Uiso 1 1 calc R . . C12 C 0.5292(5) 0.8217(4) 0.8099(4) 0.0643(11) Uani 1 1 d . . . H12 H 0.4102 0.8521 0.8160 0.077 Uiso 1 1 calc R . . C13 C 0.7073(9) 0.8148(5) 0.5369(4) 0.0877(17) Uani 1 1 d . . . H13 H 0.6877 0.8439 0.5985 0.105 Uiso 1 1 calc R . . C14 C 0.7062(8) 0.6941(4) 0.5412(3) 0.0812(16) Uani 1 1 d . . . H14 H 0.6846 0.6456 0.6048 0.097 Uiso 1 1 calc R . . C15 C 0.7351(4) 0.6447(3) 0.4568(3) 0.0411(7) Uani 1 1 d . . . C16 C 0.7716(8) 0.7220(4) 0.3654(3) 0.0739(14) Uani 1 1 d . . . H16 H 0.7977 0.6924 0.3038 0.089 Uiso 1 1 calc R . . C17 C 0.7689(8) 0.8430(4) 0.3667(4) 0.0766(14) Uani 1 1 d . . . H17 H 0.7926 0.8936 0.3048 0.092 Uiso 1 1 calc R . . C18 C 0.7149(5) 0.3566(3) 0.3750(3) 0.0534(9) Uani 1 1 d . . . H18 H 0.6984 0.3347 0.3148 0.064 Uiso 1 1 calc R . . C19 C 0.7133(5) 0.4779(3) 0.3707(3) 0.0520(9) Uani 1 1 d . . . H19 H 0.6974 0.5354 0.3085 0.062 Uiso 1 1 calc R . . C20 C 0.7353(4) 0.5147(3) 0.4583(3) 0.0420(7) Uani 1 1 d . . . C21 C 0.7589(6) 0.4232(3) 0.5481(3) 0.0576(10) Uani 1 1 d . . . H21 H 0.7726 0.4432 0.6098 0.069 Uiso 1 1 calc R . . C22 C 0.7619(6) 0.3023(3) 0.5458(3) 0.0603(10) Uani 1 1 d . . . H22 H 0.7810 0.2418 0.6063 0.072 Uiso 1 1 calc R . . C23 C -0.0344(6) 0.2344(5) 0.9524(5) 0.0776(14) Uani 1 1 d . . . H23A H -0.0827 0.1662 0.9618 0.116 Uiso 1 1 calc R . . H23B H -0.0831 0.2981 0.8949 0.116 Uiso 1 1 calc R . . H23C H -0.0595 0.2694 1.0138 0.116 Uiso 1 1 calc R . . C24 C 0.2197(7) 0.0554(4) 0.9428(4) 0.0750(13) Uani 1 1 d . . . H24A H 0.1287 0.0174 0.9538 0.112 Uiso 1 1 calc R . . H24B H 0.2904 0.0228 1.0005 0.112 Uiso 1 1 calc R . . H24C H 0.2877 0.0367 0.8808 0.112 Uiso 1 1 calc R . . N5 N 0.5700(4) 0.5031(3) 0.8513(2) 0.0535(7) Uani 1 1 d . . . N4 N 0.4966(4) 0.6172(3) 0.8473(2) 0.0533(7) Uani 1 1 d . . . N1 N 0.1484(4) 0.1888(3) 0.9326(3) 0.0576(8) Uani 1 1 d . . . N2 N 0.7340(4) 0.8910(3) 0.4524(2) 0.0527(7) Uani 1 1 d . . . N3 N 0.7386(4) 0.2690(3) 0.4605(2) 0.0510(7) Uani 1 1 d . . . O1 O 0.9217(4) 0.9965(3) 0.6262(2) 0.0687(8) Uani 1 1 d . . . O2 O 0.8426(5) 1.0720(3) 0.7846(3) 0.0808(10) Uani 1 1 d . . . O3 O 1.0969(4) 0.8996(3) 0.7674(3) 0.0713(9) Uani 1 1 d . . . S1 S 0.92565(12) 0.96604(8) 0.73743(7) 0.0488(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 0.0711(2) 0.02982(15) 0.0767(2) -0.01882(13) -0.00467(15) -0.02068(13) C1 0.048(2) 0.0439(18) 0.0460(18) -0.0094(15) -0.0103(14) -0.0136(15) C2 0.048(2) 0.0397(18) 0.082(3) -0.0198(18) -0.0139(18) -0.0054(16) C3 0.043(2) 0.049(2) 0.081(3) -0.0179(19) -0.0118(18) -0.0092(17) C4 0.048(2) 0.0442(19) 0.0532(19) -0.0140(15) -0.0085(15) -0.0143(16) C5 0.056(2) 0.0341(17) 0.053(2) -0.0131(15) -0.0042(16) -0.0091(15) C6 0.045(2) 0.0456(19) 0.057(2) -0.0154(16) 0.0004(16) -0.0106(16) C7 0.053(2) 0.049(2) 0.0490(19) -0.0128(16) -0.0035(15) -0.0196(17) C8 0.054(2) 0.0382(19) 0.079(3) -0.0014(18) -0.0159(19) -0.0088(17) C9 0.050(2) 0.045(2) 0.080(3) -0.0001(19) -0.0112(19) -0.0119(18) C10 0.047(2) 0.0460(19) 0.0485(18) -0.0127(15) -0.0060(15) -0.0137(16) C11 0.056(2) 0.046(2) 0.099(3) -0.031(2) 0.005(2) -0.0139(18) C12 0.048(2) 0.053(2) 0.100(3) -0.033(2) 0.003(2) -0.0158(18) C13 0.173(6) 0.059(3) 0.055(2) -0.028(2) 0.003(3) -0.061(3) C14 0.164(5) 0.050(2) 0.046(2) -0.0103(19) 0.000(3) -0.058(3) C15 0.0503(19) 0.0284(15) 0.0506(18) -0.0112(14) -0.0078(14) -0.0160(14) C16 0.137(4) 0.048(2) 0.052(2) -0.0129(18) -0.011(2) -0.046(3) C17 0.136(4) 0.046(2) 0.059(2) -0.0039(19) -0.014(3) -0.044(3) C18 0.075(3) 0.0402(18) 0.054(2) -0.0174(16) -0.0127(18) -0.0206(18) C19 0.081(3) 0.0353(17) 0.0444(18) -0.0088(14) -0.0112(17) -0.0202(18) C20 0.054(2) 0.0292(15) 0.0469(17) -0.0103(13) -0.0069(15) -0.0144(14) C21 0.094(3) 0.0352(18) 0.050(2) -0.0097(15) -0.0188(19) -0.022(2) C22 0.098(3) 0.0303(17) 0.055(2) -0.0044(16) -0.013(2) -0.0215(19) C23 0.054(3) 0.061(3) 0.122(4) -0.019(3) -0.001(2) -0.025(2) C24 0.079(3) 0.048(2) 0.104(4) -0.022(2) 0.004(3) -0.027(2) N5 0.0568(19) 0.0488(18) 0.0598(18) -0.0156(15) -0.0104(14) -0.0165(15) N4 0.0555(19) 0.0480(18) 0.0605(18) -0.0161(15) -0.0070(14) -0.0162(15) N1 0.0496(18) 0.0430(17) 0.082(2) -0.0111(16) -0.0061(15) -0.0155(14) N2 0.073(2) 0.0351(15) 0.0601(19) -0.0160(14) -0.0039(15) -0.0249(15) N3 0.068(2) 0.0264(13) 0.0627(18) -0.0129(13) -0.0075(15) -0.0153(14) O1 0.084(2) 0.0680(19) 0.0570(16) -0.0045(14) -0.0026(14) -0.0333(17) O2 0.092(2) 0.0624(19) 0.104(2) -0.0455(18) 0.0247(19) -0.0366(17) O3 0.0586(18) 0.0621(18) 0.095(2) 0.0035(16) -0.0186(15) -0.0276(15) S1 0.0535(5) 0.0405(4) 0.0557(5) -0.0114(4) -0.0045(4) -0.0168(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 N2 2.195(3) . ? Ag1 N3 2.199(3) 1_565 ? Ag1 O1 2.576(3) . ? Ag1 O1 2.586(3) 2_776 ? C1 N1 1.359(5) . ? C1 C6 1.400(5) . ? C1 C2 1.410(5) . ? C2 C3 1.370(5) . ? C2 H2 0.9300 . ? C3 C4 1.384(5) . ? C3 H3 0.9300 . ? C4 C5 1.395(5) . ? C4 N5 1.411(5) . ? C5 C6 1.370(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.367(5) . ? C7 C12 1.385(6) . ? C7 N4 1.426(5) . ? C8 C9 1.379(5) . ? C8 H8 0.9300 . ? C9 C10 1.362(5) . ? C9 H9 0.9300 . ? C10 C11 1.389(6) . ? C10 S1 1.778(4) . ? C11 C12 1.378(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 N2 1.297(5) . ? C13 C14 1.371(6) . ? C13 H13 0.9300 . ? C14 C15 1.330(5) . ? C14 H14 0.9300 . ? C15 C16 1.392(5) . ? C15 C20 1.483(4) . ? C16 C17 1.381(5) . ? C16 H16 0.9300 . ? C17 N2 1.336(6) . ? C17 H17 0.9300 . ? C18 N3 1.325(5) . ? C18 C19 1.372(5) . ? C18 H18 0.9300 . ? C19 C20 1.378(5) . ? C19 H19 0.9300 . ? C20 C21 1.389(5) . ? C21 C22 1.383(5) . ? C21 H21 0.9300 . ? C22 N3 1.331(5) . ? C22 H22 0.9300 . ? C23 N1 1.440(5) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N1 1.433(5) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? N5 N4 1.245(4) . ? N3 Ag1 2.199(3) 1_545 ? O1 S1 1.445(3) . ? O1 Ag1 2.586(3) 2_776 ? O2 S1 1.428(3) . ? O3 S1 1.436(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N3 166.5(1) . 1_565 ? N2 Ag1 O1 95.8(1) . . ? N3 Ag1 O1 91.0(1) 1_565 . ? N2 Ag1 O1 91.1(1) . 2_776 ? N3 Ag1 O1 101.3(1) 1_565 2_776 ? O1 Ag1 O1 83.2(1) . 2_776 ? N1 C1 C6 122.0(3) . . ? N1 C1 C2 121.9(3) . . ? C6 C1 C2 116.1(3) . . ? C3 C2 C1 121.3(4) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C2 C3 C4 121.6(4) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C3 C4 C5 118.1(3) . . ? C3 C4 N5 117.0(3) . . ? C5 C4 N5 124.9(3) . . ? C6 C5 C4 120.3(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C1 122.6(3) . . ? C5 C6 H6 118.7 . . ? C1 C6 H6 118.7 . . ? C8 C7 C12 119.9(4) . . ? C8 C7 N4 125.0(4) . . ? C12 C7 N4 115.1(3) . . ? C7 C8 C9 120.0(4) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.8(4) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 119.5(4) . . ? C9 C10 S1 121.0(3) . . ? C11 C10 S1 119.1(3) . . ? C12 C11 C10 119.8(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C7 119.9(4) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? N2 C13 C14 124.3(4) . . ? N2 C13 H13 117.8 . . ? C14 C13 H13 117.8 . . ? C15 C14 C13 121.7(4) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C14 C15 C16 115.6(3) . . ? C14 C15 C20 123.3(3) . . ? C16 C15 C20 121.1(3) . . ? C17 C16 C15 119.5(4) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? N2 C17 C16 123.3(4) . . ? N2 C17 H17 118.3 . . ? C16 C17 H17 118.3 . . ? N3 C18 C19 123.4(3) . . ? N3 C18 H18 118.3 . . ? C19 C18 H18 118.3 . . ? C18 C19 C20 120.2(3) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C21 116.4(3) . . ? C19 C20 C15 121.9(3) . . ? C21 C20 C15 121.7(3) . . ? C22 C21 C20 119.9(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? N3 C22 C21 122.7(3) . . ? N3 C22 H22 118.7 . . ? C21 C22 H22 118.7 . . ? N1 C23 H23A 109.5 . . ? N1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C24 H24A 109.5 . . ? N1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 N5 C4 113.6(3) . . ? N5 N4 C7 114.2(3) . . ? C1 N1 C24 121.7(3) . . ? C1 N1 C23 121.9(3) . . ? C24 N1 C23 116.0(4) . . ? C13 N2 C17 115.5(3) . . ? C13 N2 Ag1 121.3(3) . . ? C17 N2 Ag1 122.1(3) . . ? C18 N3 C22 117.4(3) . . ? C18 N3 Ag1 120.7(2) . 1_545 ? C22 N3 Ag1 121.5(2) . 1_545 ? S1 O1 Ag1 153.73(19) . . ? S1 O1 Ag1 109.28(17) . 2_776 ? Ag1 O1 Ag1 96.76(10) . 2_776 ? O2 S1 O3 114.4(2) . . ? O2 S1 O1 112.8(2) . . ? O3 S1 O1 110.7(2) . . ? O2 S1 C10 106.95(18) . . ? O3 S1 C10 106.60(17) . . ? O1 S1 C10 104.67(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 177.0(4) . . . . ? C6 C1 C2 C3 -2.1(6) . . . . ? C1 C2 C3 C4 1.7(6) . . . . ? C2 C3 C4 C5 -0.2(6) . . . . ? C2 C3 C4 N5 -178.9(4) . . . . ? C3 C4 C5 C6 -0.9(5) . . . . ? N5 C4 C5 C6 177.8(3) . . . . ? C4 C5 C6 C1 0.4(6) . . . . ? N1 C1 C6 C5 -178.0(4) . . . . ? C2 C1 C6 C5 1.1(5) . . . . ? C12 C7 C8 C9 0.3(6) . . . . ? N4 C7 C8 C9 179.8(4) . . . . ? C7 C8 C9 C10 -0.1(7) . . . . ? C8 C9 C10 C11 -0.5(6) . . . . ? C8 C9 C10 S1 -174.2(3) . . . . ? C9 C10 C11 C12 0.9(7) . . . . ? S1 C10 C11 C12 174.8(4) . . . . ? C10 C11 C12 C7 -0.7(7) . . . . ? C8 C7 C12 C11 0.1(7) . . . . ? N4 C7 C12 C11 -179.4(4) . . . . ? N2 C13 C14 C15 0.8(10) . . . . ? C13 C14 C15 C16 1.9(8) . . . . ? C13 C14 C15 C20 179.9(5) . . . . ? C14 C15 C16 C17 -2.5(7) . . . . ? C20 C15 C16 C17 179.5(4) . . . . ? C15 C16 C17 N2 0.6(8) . . . . ? N3 C18 C19 C20 -0.7(7) . . . . ? C18 C19 C20 C21 0.2(6) . . . . ? C18 C19 C20 C15 179.8(4) . . . . ? C14 C15 C20 C19 159.9(5) . . . . ? C16 C15 C20 C19 -22.3(6) . . . . ? C14 C15 C20 C21 -20.6(6) . . . . ? C16 C15 C20 C21 157.2(4) . . . . ? C19 C20 C21 C22 1.0(6) . . . . ? C15 C20 C21 C22 -178.6(4) . . . . ? C20 C21 C22 N3 -1.8(7) . . . . ? C3 C4 N5 N4 172.5(3) . . . . ? C5 C4 N5 N4 -6.2(5) . . . . ? C4 N5 N4 C7 178.9(3) . . . . ? C8 C7 N4 N5 -5.3(5) . . . . ? C12 C7 N4 N5 174.2(4) . . . . ? C6 C1 N1 C24 -169.5(4) . . . . ? C2 C1 N1 C24 11.5(6) . . . . ? C6 C1 N1 C23 3.1(6) . . . . ? C2 C1 N1 C23 -175.8(4) . . . . ? C14 C13 N2 C17 -2.8(9) . . . . ? C14 C13 N2 Ag1 -171.2(5) . . . . ? C16 C17 N2 C13 2.1(8) . . . . ? C16 C17 N2 Ag1 170.4(4) . . . . ? N3 Ag1 N2 C13 -86.3(7) 1_565 . . . ? O1 Ag1 N2 C13 33.5(4) . . . . ? O1 Ag1 N2 C13 116.8(4) 2_776 . . . ? N3 Ag1 N2 C17 106.0(6) 1_565 . . . ? O1 Ag1 N2 C17 -134.2(4) . . . . ? O1 Ag1 N2 C17 -50.9(4) 2_776 . . . ? C19 C18 N3 C22 0.0(6) . . . . ? C19 C18 N3 Ag1 -172.8(3) . . . 1_545 ? C21 C22 N3 C18 1.2(7) . . . . ? C21 C22 N3 Ag1 173.9(3) . . . 1_545 ? N2 Ag1 O1 S1 -82.2(4) . . . . ? N3 Ag1 O1 S1 86.2(4) 1_565 . . . ? O1 Ag1 O1 S1 -172.5(5) 2_776 . . . ? N2 Ag1 O1 Ag1 90.37(12) . . . 2_776 ? N3 Ag1 O1 Ag1 -101.28(12) 1_565 . . 2_776 ? O1 Ag1 O1 Ag1 0.0 2_776 . . 2_776 ? Ag1 O1 S1 O2 -62.3(5) . . . . ? Ag1 O1 S1 O2 125.54(19) 2_776 . . . ? Ag1 O1 S1 O3 168.1(4) . . . . ? Ag1 O1 S1 O3 -4.1(2) 2_776 . . . ? Ag1 O1 S1 C10 53.6(5) . . . . ? Ag1 O1 S1 C10 -118.57(17) 2_776 . . . ? C9 C10 S1 O2 -147.0(4) . . . . ? C11 C10 S1 O2 39.2(4) . . . . ? C9 C10 S1 O3 -24.2(4) . . . . ? C11 C10 S1 O3 162.0(3) . . . . ? C9 C10 S1 O1 93.1(4) . . . . ? C11 C10 S1 O1 -80.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.948 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.091 #===end data_compd6 _database_code_depnum_ccdc_archive 'CCDC 684628' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C10 H8 Ag N2),4(C6 H4 Cl2 N O 3 S), C4 H6 N2' _chemical_formula_sum 'C17 H13.50 Ag Cl2 N3.50 O3 S' _chemical_formula_weight 525.64 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' 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 'P 21/n ' _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.249(4) _cell_length_b 7.917(6) _cell_length_c 19.309(3) _cell_angle_alpha 90 _cell_angle_beta 90.562(5) _cell_angle_gamma 90 _cell_volume 1872(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4228 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.490 _exptl_crystal_size_mid 0.317 _exptl_crystal_size_min 0.315 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 1.499 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.575 _exptl_absorpt_correction_T_max 0.615 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15037 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4220 _reflns_number_gt 3329 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+5.9640P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0054(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4220 _refine_ls_number_parameters 271 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1416 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.161 _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 0.41827(3) 0.25621(6) 0.039259(19) 0.04958(18) Uani 1 1 d . . . C1 C 0.3602(4) 0.8261(5) 0.1483(2) 0.0280(9) Uani 1 1 d . . . C2 C 0.2914(4) 0.9447(6) 0.1779(2) 0.0336(10) Uani 1 1 d . . . C3 C 0.3037(4) 0.9961(7) 0.2460(2) 0.0407(11) Uani 1 1 d . . . H3 H 0.2554 1.0745 0.2643 0.049 Uiso 1 1 calc R . . C4 C 0.3880(5) 0.9318(7) 0.2876(2) 0.0416(12) Uani 1 1 d . . . C5 C 0.4587(4) 0.8178(6) 0.2561(2) 0.0356(10) Uani 1 1 d . . . C6 C 0.4450(4) 0.7647(6) 0.1892(2) 0.0339(10) Uani 1 1 d . . . H6 H 0.4933 0.6863 0.1709 0.041 Uiso 1 1 calc R . . C7 C 0.5921(4) 0.1362(7) 0.1465(2) 0.0390(11) Uani 1 1 d . . . H7 H 0.6175 0.0771 0.1083 0.047 Uiso 1 1 calc R . . C8 C 0.6494(4) 0.1234(6) 0.2078(2) 0.0355(10) Uani 1 1 d . . . H8 H 0.7120 0.0572 0.2104 0.043 Uiso 1 1 calc R . . C9 C 0.7530(4) 0.0825(6) 0.3473(2) 0.0358(10) Uani 1 1 d . . . H9 H 0.7651 -0.0049 0.3161 0.043 Uiso 1 1 calc R . . C10 C 0.8123(4) 0.0903(6) 0.4084(2) 0.0385(11) Uani 1 1 d . . . H10 H 0.8628 0.0053 0.4176 0.046 Uiso 1 1 calc R . . C11 C 0.7249(4) 0.3299(7) 0.4420(2) 0.0369(11) Uani 1 1 d . . . H11 H 0.7146 0.4153 0.4743 0.044 Uiso 1 1 calc R . . C12 C 0.6603(4) 0.3289(6) 0.3818(2) 0.0367(11) Uani 1 1 d . . . H12 H 0.6072 0.4114 0.3751 0.044 Uiso 1 1 calc R . . C14 C 0.5180(4) 0.3023(7) 0.2585(2) 0.0374(11) Uani 1 1 d . . . H14 H 0.4892 0.3596 0.2962 0.045 Uiso 1 1 calc R . . C15 C 0.4656(4) 0.3094(7) 0.1948(2) 0.0371(10) Uani 1 1 d . . . H15 H 0.4021 0.3730 0.1908 0.045 Uiso 1 1 calc R . . C16 C 0.6135(4) 0.2097(6) 0.2663(2) 0.0289(9) Uani 1 1 d . . . C17 C 0.6757(4) 0.2052(6) 0.3326(2) 0.0291(9) Uani 1 1 d . . . C18 C 0.0440(12) 0.7431(15) 0.9803(7) 0.061(3) Uani 0.50 1 d PD . . C19 C 0.0486(10) 0.5497(15) 0.9763(6) 0.054(3) Uani 0.50 1 d PD . . N1 N 0.5020(3) 0.2290(5) 0.13883(19) 0.0350(9) Uani 1 1 d . . . N2 N 0.8010(3) 0.2121(5) 0.4545(2) 0.0357(9) Uani 1 1 d . . . N3 N 0.4021(6) 0.9836(8) 0.3540(2) 0.0612(14) Uani 1 1 d D . . N6 N 0.0426(8) 0.874(2) 0.9949(6) 0.067(3) Uani 0.50 1 d P . . O1 O 0.2370(3) 0.6930(6) 0.0540(2) 0.0560(10) Uani 1 1 d . . . O2 O 0.4274(3) 0.6192(5) 0.0564(2) 0.0520(10) Uani 1 1 d . . . O3 O 0.3722(4) 0.8958(5) 0.01775(18) 0.0579(11) Uani 1 1 d . . . S1 S 0.34771(10) 0.75248(15) 0.06157(6) 0.0343(3) Uani 1 1 d . . . Cl1 Cl 0.56866(13) 0.7406(2) 0.30441(8) 0.0572(4) Uani 1 1 d . . . Cl2 Cl 0.18810(12) 1.0417(2) 0.13040(7) 0.0535(4) Uani 1 1 d . . . HN3A H 0.451(4) 0.958(8) 0.379(3) 0.049(19) Uiso 1 1 d D . . HN3B H 0.360(5) 1.041(9) 0.379(3) 0.08(3) Uiso 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 0.0476(3) 0.0720(3) 0.0288(2) 0.00678(18) -0.01940(16) -0.0057(2) C1 0.031(2) 0.028(2) 0.026(2) 0.0012(16) 0.0014(16) -0.0024(17) C2 0.032(2) 0.036(2) 0.032(2) 0.0038(18) 0.0034(18) 0.0015(19) C3 0.048(3) 0.041(3) 0.033(2) -0.006(2) 0.007(2) 0.001(2) C4 0.051(3) 0.045(3) 0.030(2) -0.001(2) 0.003(2) -0.012(2) C5 0.035(3) 0.039(2) 0.033(2) 0.0034(19) -0.0079(19) -0.006(2) C6 0.032(2) 0.034(2) 0.035(2) 0.0025(19) -0.0012(18) 0.0018(19) C7 0.045(3) 0.048(3) 0.024(2) -0.0029(19) -0.0053(19) 0.000(2) C8 0.036(3) 0.045(3) 0.025(2) -0.0012(19) -0.0055(18) 0.006(2) C9 0.042(3) 0.037(2) 0.029(2) -0.0062(18) -0.0096(19) 0.005(2) C10 0.037(3) 0.041(3) 0.037(2) -0.002(2) -0.013(2) 0.008(2) C11 0.040(3) 0.045(3) 0.026(2) -0.0087(19) -0.0121(19) 0.005(2) C12 0.042(3) 0.040(3) 0.028(2) -0.0038(19) -0.0124(19) 0.008(2) C14 0.038(3) 0.046(3) 0.028(2) -0.0060(19) -0.0072(19) 0.004(2) C15 0.032(2) 0.044(3) 0.035(2) 0.001(2) -0.0106(19) 0.004(2) C16 0.030(2) 0.033(2) 0.0235(19) 0.0007(16) -0.0053(16) -0.0047(17) C17 0.030(2) 0.035(2) 0.0223(19) 0.0003(16) -0.0074(16) -0.0046(17) C18 0.056(8) 0.074(10) 0.055(7) 0.010(7) -0.012(6) -0.005(7) C19 0.048(6) 0.074(8) 0.039(6) -0.007(5) -0.019(5) -0.003(6) N1 0.040(2) 0.040(2) 0.0251(18) 0.0012(15) -0.0109(15) -0.0040(17) N2 0.039(2) 0.042(2) 0.0262(18) -0.0014(16) -0.0106(16) 0.0007(17) N3 0.078(4) 0.075(4) 0.031(2) -0.013(2) -0.003(3) -0.009(3) N6 0.035(5) 0.110(10) 0.058(7) 0.039(7) -0.012(5) -0.010(6) O1 0.044(2) 0.073(3) 0.051(2) -0.012(2) -0.0101(18) -0.010(2) O2 0.057(2) 0.049(2) 0.050(2) -0.0161(18) -0.0063(18) 0.0136(19) O3 0.087(3) 0.060(2) 0.0276(18) 0.0079(17) 0.0065(18) -0.007(2) S1 0.0383(6) 0.0381(6) 0.0263(5) -0.0026(4) -0.0022(4) 0.0012(5) Cl1 0.0553(8) 0.0646(9) 0.0513(8) 0.0084(7) -0.0243(6) -0.0032(7) Cl2 0.0513(8) 0.0634(9) 0.0459(7) 0.0040(6) -0.0002(6) 0.0258(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 N2 2.181(4) 4_565 ? Ag1 N1 2.181(4) . ? C1 C6 1.387(6) . ? C1 C2 1.389(6) . ? C1 S1 1.778(4) . ? C2 C3 1.382(7) . ? C2 Cl2 1.735(5) . ? C3 C4 1.398(8) . ? C3 H3 0.9300 . ? C4 N3 1.356(7) . ? C4 C5 1.395(7) . ? C5 C6 1.367(7) . ? C5 Cl1 1.742(5) . ? C6 H6 0.9300 . ? C7 N1 1.332(6) . ? C7 C8 1.375(6) . ? C7 H7 0.9300 . ? C8 C16 1.394(6) . ? C8 H8 0.9300 . ? C9 C10 1.381(6) . ? C9 C17 1.385(6) . ? C9 H9 0.9300 . ? C10 N2 1.321(6) . ? C10 H10 0.9300 . ? C11 N2 1.339(6) . ? C11 C12 1.398(6) . ? C11 H11 0.9300 . ? C12 C17 1.379(6) . ? C12 H12 0.9300 . ? C14 C15 1.383(6) . ? C14 C16 1.387(7) . ? C14 H14 0.9300 . ? C15 N1 1.335(6) . ? C15 H15 0.9300 . ? C16 C17 1.484(6) . ? C18 N6 1.074(18) . ? C18 C19 1.534(9) . ? N2 Ag1 2.181(4) 4_666 ? N3 HN3A 0.79(4) . ? N3 HN3B 0.84(4) . ? O1 S1 1.442(4) . ? O2 S1 1.442(4) . ? O3 S1 1.449(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 N2 Ag1 N1 166.7(2) 4_565 . ? C6 C1 C2 117.1(4) . . ? C6 C1 S1 118.6(3) . . ? C2 C1 S1 124.3(3) . . ? C3 C2 C1 122.0(4) . . ? C3 C2 Cl2 116.4(4) . . ? C1 C2 Cl2 121.5(4) . . ? C2 C3 C4 120.9(5) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? N3 C4 C5 122.3(6) . . ? N3 C4 C3 121.4(6) . . ? C5 C4 C3 116.3(4) . . ? C6 C5 C4 122.7(5) . . ? C6 C5 Cl1 119.0(4) . . ? C4 C5 Cl1 118.3(4) . . ? C5 C6 C1 121.0(4) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? N1 C7 C8 123.4(4) . . ? N1 C7 H7 118.3 . . ? C8 C7 H7 118.3 . . ? C7 C8 C16 120.0(4) . . ? C7 C8 H8 120.0 . . ? C16 C8 H8 120.0 . . ? C10 C9 C17 119.8(4) . . ? C10 C9 H9 120.1 . . ? C17 C9 H9 120.1 . . ? N2 C10 C9 123.5(4) . . ? N2 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? N2 C11 C12 122.3(4) . . ? N2 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C17 C12 C11 119.8(4) . . ? C17 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C15 C14 C16 120.1(4) . . ? C15 C14 H14 120.0 . . ? C16 C14 H14 120.0 . . ? N1 C15 C14 123.0(5) . . ? N1 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C14 C16 C8 116.3(4) . . ? C14 C16 C17 122.1(4) . . ? C8 C16 C17 121.6(4) . . ? C12 C17 C9 117.1(4) . . ? C12 C17 C16 120.4(4) . . ? C9 C17 C16 122.5(4) . . ? N6 C18 C19 167.6(15) . . ? C18 C19 C19 114.1(12) . 3_567 ? C7 N1 C15 117.1(4) . . ? C7 N1 Ag1 122.3(3) . . ? C15 N1 Ag1 120.6(3) . . ? C10 N2 C11 117.6(4) . . ? C10 N2 Ag1 121.2(3) . 4_666 ? C11 N2 Ag1 120.5(3) . 4_666 ? C4 N3 HN3A 125(4) . . ? C4 N3 HN3B 129(5) . . ? HN3A N3 HN3B 106(4) . . ? O2 S1 O1 113.0(3) . . ? O2 S1 O3 112.9(3) . . ? O1 S1 O3 113.4(3) . . ? O2 S1 C1 104.7(2) . . ? O1 S1 C1 105.9(2) . . ? O3 S1 C1 106.1(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -2.1(7) . . . . ? S1 C1 C2 C3 179.1(4) . . . . ? C6 C1 C2 Cl2 175.6(3) . . . . ? S1 C1 C2 Cl2 -3.2(6) . . . . ? C1 C2 C3 C4 1.0(8) . . . . ? Cl2 C2 C3 C4 -176.8(4) . . . . ? C2 C3 C4 N3 178.8(5) . . . . ? C2 C3 C4 C5 1.4(7) . . . . ? N3 C4 C5 C6 179.9(5) . . . . ? C3 C4 C5 C6 -2.7(7) . . . . ? N3 C4 C5 Cl1 -0.1(7) . . . . ? C3 C4 C5 Cl1 177.2(4) . . . . ? C4 C5 C6 C1 1.6(7) . . . . ? Cl1 C5 C6 C1 -178.3(4) . . . . ? C2 C1 C6 C5 0.8(7) . . . . ? S1 C1 C6 C5 179.7(4) . . . . ? N1 C7 C8 C16 0.3(8) . . . . ? C17 C9 C10 N2 -1.2(8) . . . . ? N2 C11 C12 C17 -1.2(8) . . . . ? C16 C14 C15 N1 0.6(8) . . . . ? C15 C14 C16 C8 -1.9(7) . . . . ? C15 C14 C16 C17 176.9(4) . . . . ? C7 C8 C16 C14 1.5(7) . . . . ? C7 C8 C16 C17 -177.3(4) . . . . ? C11 C12 C17 C9 2.6(7) . . . . ? C11 C12 C17 C16 -175.5(4) . . . . ? C10 C9 C17 C12 -1.4(7) . . . . ? C10 C9 C17 C16 176.6(5) . . . . ? C14 C16 C17 C12 -19.4(7) . . . . ? C8 C16 C17 C12 159.3(5) . . . . ? C14 C16 C17 C9 162.7(5) . . . . ? C8 C16 C17 C9 -18.6(7) . . . . ? N6 C18 C19 C19 57(8) . . . 3_567 ? C8 C7 N1 C15 -1.6(8) . . . . ? C8 C7 N1 Ag1 176.8(4) . . . . ? C14 C15 N1 C7 1.2(7) . . . . ? C14 C15 N1 Ag1 -177.2(4) . . . . ? N2 Ag1 N1 C7 148.4(6) 4_565 . . . ? N2 Ag1 N1 C15 -33.2(9) 4_565 . . . ? C9 C10 N2 C11 2.6(8) . . . . ? C9 C10 N2 Ag1 -167.8(4) . . . 4_666 ? C12 C11 N2 C10 -1.4(8) . . . . ? C12 C11 N2 Ag1 169.1(4) . . . 4_666 ? C6 C1 S1 O2 7.5(4) . . . . ? C2 C1 S1 O2 -173.7(4) . . . . ? C6 C1 S1 O1 127.2(4) . . . . ? C2 C1 S1 O1 -54.1(5) . . . . ? C6 C1 S1 O3 -112.1(4) . . . . ? C2 C1 S1 O3 66.7(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 HN3B O1 0.84(4) 2.13(4) 2.977(8) 175(7) 2 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.947 _refine_diff_density_min -0.721 _refine_diff_density_rms 0.117 #===end data_compd7 _database_code_depnum_ccdc_archive 'CCDC 684629' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H28 Ag3 N6 O8 S2, 2(H2 O)' _chemical_formula_sum 'C38 H32 Ag3 N6 O10 S2' _chemical_formula_weight 1120.43 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' 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' _symmetry_space_group_name_Hall '-C 2yc ' 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 16.818(5) _cell_length_b 13.215(5) _cell_length_c 16.947(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.991(5) _cell_angle_gamma 90.00 _cell_volume 3752(2) _cell_formula_units_Z 4 _cell_measurement_temperature 292(2) _cell_measurement_reflns_used 4353 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.3 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2220 _exptl_absorpt_coefficient_mu 1.732 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.671 _exptl_absorpt_correction_T_max 0.738 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 292(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11351 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.28 _reflns_number_total 4353 _reflns_number_gt 2500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT software (Bruker, 1999)' _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4353 _refine_ls_number_parameters 273 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0502 _refine_ls_goodness_of_fit_ref 0.8720 _refine_ls_restrained_S_all 0.777 _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 0.0000 0.72964(3) 0.2500 0.05160(10) Uani 1 2 d S . . Ag2 Ag 0.594957(13) 0.60108(2) 0.606600(13) 0.06420(10) Uani 1 1 d . . . C1 C 0.77462(16) 0.5900(2) 0.65693(15) 0.0462(7) Uani 1 1 d . . . H1 H 0.7759 0.6305 0.6122 0.055 Uiso 1 1 calc R . . C2 C 0.84560(15) 0.5702(2) 0.70200(16) 0.0480(7) Uani 1 1 d . . . H2 H 0.8930 0.5990 0.6884 0.058 Uiso 1 1 calc R . . C3 C 0.84573(13) 0.50880(19) 0.76574(15) 0.0416(7) Uani 1 1 d . . . H3 H 0.8934 0.4952 0.7960 0.050 Uiso 1 1 calc R . . C4 C 0.76829(13) 0.3969(2) 0.85122(14) 0.0366(6) Uani 1 1 d . . . C5 C 0.69607(14) 0.35754(19) 0.86532(15) 0.0426(7) Uani 1 1 d . . . H5 H 0.6929 0.3122 0.9069 0.051 Uiso 1 1 calc R . . C6 C 0.62651(14) 0.3840(2) 0.81846(16) 0.0508(8) Uani 1 1 d . . . H6 H 0.5784 0.3542 0.8289 0.061 Uiso 1 1 calc R . . C7 C 0.62697(14) 0.4521(2) 0.75787(15) 0.0438(7) Uani 1 1 d . . . C8 C 0.77377(13) 0.46513(18) 0.78664(14) 0.0340(6) Uani 1 1 d . . . C9 C 0.70325(13) 0.49129(19) 0.73897(14) 0.0355(6) Uani 1 1 d . . . C10 C 0.42065(17) 0.5746(2) 0.54906(16) 0.0536(8) Uani 1 1 d . . . H10 H 0.4256 0.5273 0.5898 0.064 Uiso 1 1 calc R . . C11 C 0.34626(15) 0.5883(2) 0.50913(15) 0.0475(7) Uani 1 1 d . . . H11 H 0.3028 0.5505 0.5226 0.057 Uiso 1 1 calc R . . C12 C 0.33715(13) 0.65889(18) 0.44890(13) 0.0336(6) Uani 1 1 d . . . C13 C 0.40476(14) 0.7097(2) 0.43135(15) 0.0479(7) Uani 1 1 d . . . H13 H 0.4019 0.7568 0.3904 0.057 Uiso 1 1 calc R . . C14 C 0.47676(14) 0.6914(2) 0.47413(15) 0.0496(7) Uani 1 1 d . . . H14 H 0.5214 0.7273 0.4612 0.060 Uiso 1 1 calc R . . C15 C 0.11559(14) 0.6622(2) 0.39002(15) 0.0431(7) Uani 1 1 d . . . H15 H 0.0696 0.6351 0.4083 0.052 Uiso 1 1 calc R . . C16 C 0.18787(14) 0.6405(2) 0.43080(14) 0.0430(7) Uani 1 1 d . . . H16 H 0.1897 0.5987 0.4751 0.052 Uiso 1 1 calc R . . C17 C 0.25770(13) 0.68009(18) 0.40658(13) 0.0318(6) Uani 1 1 d . . . C18 C 0.24932(14) 0.7408(2) 0.34002(15) 0.0437(7) Uani 1 1 d . . . H18 H 0.2941 0.7700 0.3208 0.052 Uiso 1 1 calc R . . C19 C 0.17589(14) 0.7582(2) 0.30246(15) 0.0461(7) Uani 1 1 d . . . H19 H 0.1724 0.7991 0.2577 0.055 Uiso 1 1 calc R . . N1 N 0.70503(12) 0.55366(16) 0.67490(12) 0.0399(5) Uani 1 1 d . . . N2 N 0.48536(12) 0.62511(17) 0.53272(13) 0.0474(6) Uani 1 1 d . . . N3 N 0.10841(11) 0.71979(16) 0.32607(12) 0.0386(5) Uani 1 1 d . . . O1 O 0.87635(11) 0.45471(16) 0.95818(11) 0.0719(6) Uani 1 1 d . . . O2 O 0.91355(10) 0.32875(17) 0.86741(10) 0.0645(6) Uani 1 1 d . . . O3 O 0.82805(11) 0.28524(17) 0.96711(12) 0.0792(7) Uani 1 1 d . . . O4 O 0.56206(9) 0.48403(15) 0.71586(10) 0.0617(6) Uani 1 1 d . . . H4 H 0.5105 0.4655 0.7255 0.074 Uiso 1 1 calc R . . OW1 O 1.00394(14) 0.5798(2) 0.90916(15) 0.0893(8) Uani 1 1 d D . . S1 S 0.85332(4) 0.36324(6) 0.91600(4) 0.04413(18) Uani 1 1 d . . . HW1 H 0.9680(14) 0.5419(19) 0.9284(16) 0.066 Uiso 1 1 d D . . HW2 H 1.0403(13) 0.574(2) 0.9487(11) 0.066 Uiso 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 0.02906(16) 0.0693(2) 0.0537(2) 0.000 -0.01192(13) 0.000 Ag2 0.04949(15) 0.07844(19) 0.05927(16) -0.00363(13) -0.02610(11) 0.01564(12) C1 0.0479(17) 0.0448(18) 0.0453(17) 0.0012(13) 0.0013(13) 0.0016(14) C2 0.0333(15) 0.0524(19) 0.0582(19) -0.0013(15) 0.0043(13) -0.0040(13) C3 0.0272(14) 0.0505(18) 0.0459(17) -0.0039(14) -0.0036(12) 0.0025(12) C4 0.0252(13) 0.0445(17) 0.0392(15) -0.0061(13) -0.0027(11) 0.0070(11) C5 0.0351(15) 0.0445(17) 0.0479(17) 0.0012(13) 0.0008(12) 0.0028(13) C6 0.0284(14) 0.059(2) 0.064(2) 0.0020(16) -0.0009(13) -0.0022(13) C7 0.0263(14) 0.0531(19) 0.0505(18) -0.0051(15) -0.0059(12) 0.0045(12) C8 0.0248(13) 0.0382(16) 0.0381(15) -0.0074(12) -0.0028(10) 0.0046(11) C9 0.0265(13) 0.0374(16) 0.0411(16) -0.0069(13) -0.0050(11) 0.0053(11) C10 0.0551(18) 0.051(2) 0.0518(19) 0.0111(14) -0.0135(14) 0.0037(15) C11 0.0406(15) 0.0492(19) 0.0511(18) 0.0062(14) -0.0053(13) -0.0023(13) C12 0.0315(13) 0.0358(16) 0.0325(14) -0.0035(12) -0.0030(11) 0.0022(11) C13 0.0326(14) 0.066(2) 0.0432(16) 0.0121(14) -0.0068(12) -0.0028(14) C14 0.0304(14) 0.068(2) 0.0488(18) 0.0013(15) -0.0043(12) -0.0020(13) C15 0.0310(14) 0.0534(19) 0.0445(17) 0.0005(14) 0.0008(12) -0.0077(13) C16 0.0395(15) 0.0528(18) 0.0358(15) 0.0134(13) -0.0018(12) -0.0057(13) C17 0.0292(13) 0.0340(15) 0.0316(14) -0.0035(12) -0.0010(10) -0.0024(11) C18 0.0294(14) 0.0490(18) 0.0518(18) 0.0121(14) -0.0011(12) -0.0074(12) C19 0.0352(15) 0.0541(19) 0.0473(17) 0.0155(14) -0.0062(13) -0.0034(13) N1 0.0353(12) 0.0422(14) 0.0408(13) -0.0049(11) -0.0052(10) 0.0076(10) N2 0.0406(13) 0.0508(16) 0.0479(15) -0.0014(12) -0.0131(11) 0.0074(11) N3 0.0302(11) 0.0449(14) 0.0393(13) -0.0008(11) -0.0048(9) -0.0011(10) O1 0.0625(13) 0.0809(17) 0.0668(14) -0.0276(12) -0.0254(11) 0.0118(11) O2 0.0394(11) 0.1056(17) 0.0477(12) -0.0019(11) -0.0013(9) 0.0338(11) O3 0.0498(12) 0.1054(19) 0.0797(16) 0.0481(14) -0.0101(11) 0.0004(12) O4 0.0206(9) 0.0904(16) 0.0716(13) 0.0147(11) -0.0112(9) 0.0013(9) OW1 0.0722(18) 0.114(2) 0.0780(18) 0.0021(15) -0.0128(13) -0.0046(15) S1 0.0299(3) 0.0624(5) 0.0386(4) -0.0007(4) -0.0054(3) 0.0092(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 N3 2.143(2) . ? Ag1 N3 2.143(2) 2 ? Ag2 N2 2.160(2) . ? Ag2 N1 2.188(2) . ? Ag2 O4 2.511(2) . ? C1 N1 1.325(3) . ? C1 C2 1.385(3) . ? C1 H1 0.9300 . ? C2 C3 1.351(3) . ? C2 H2 0.9300 . ? C3 C8 1.413(3) . ? C3 H3 0.9300 . ? C4 C5 1.361(3) . ? C4 C8 1.427(3) . ? C4 S1 1.782(2) . ? C5 C6 1.400(3) . ? C5 H5 0.9300 . ? C6 C7 1.366(4) . ? C6 H6 0.9300 . ? C7 O4 1.320(3) . ? C7 C9 1.445(3) . ? C8 C9 1.418(3) . ? C9 N1 1.366(3) . ? C10 N2 1.326(3) . ? C10 C11 1.381(3) . ? C10 H10 0.9300 . ? C11 C12 1.381(3) . ? C11 H11 0.9300 . ? C12 C13 1.375(3) . ? C12 C17 1.487(3) . ? C13 C14 1.378(3) . ? C13 H13 0.9300 . ? C14 N2 1.323(3) . ? C14 H14 0.9300 . ? C15 N3 1.321(3) . ? C15 C16 1.375(3) . ? C15 H15 0.9300 . ? C16 C17 1.380(3) . ? C16 H16 0.9300 . ? C17 C18 1.382(3) . ? C18 C19 1.359(3) . ? C18 H18 0.9300 . ? C19 N3 1.336(3) . ? C19 H19 0.9300 . ? O1 S1 1.440(2) . ? O2 S1 1.4342(18) . ? O3 S1 1.434(2) . ? O4 H4 0.9300 . ? OW1 HW1 0.869(10) . ? OW1 HW2 0.872(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 N3 Ag1 N3 173.0(1) . 2 ? N2 Ag2 N1 171.50(8) . . ? N2 Ag2 O4 106.64(8) . . ? N1 Ag2 O4 70.37(7) . . ? N1 C1 C2 122.8(3) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 119.7(3) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C8 120.2(2) . . ? C2 C3 H3 119.9 . . ? C8 C3 H3 119.9 . . ? C5 C4 C8 119.6(2) . . ? C5 C4 S1 118.5(2) . . ? C8 C4 S1 121.88(18) . . ? C4 C5 C6 121.3(2) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C7 C6 C5 122.1(2) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? O4 C7 C6 123.9(2) . . ? O4 C7 C9 118.3(2) . . ? C6 C7 C9 117.8(2) . . ? C3 C8 C9 116.7(2) . . ? C3 C8 C4 124.3(2) . . ? C9 C8 C4 119.0(2) . . ? N1 C9 C8 121.7(2) . . ? N1 C9 C7 118.3(2) . . ? C8 C9 C7 120.0(2) . . ? N2 C10 C11 123.8(3) . . ? N2 C10 H10 118.1 . . ? C11 C10 H10 118.1 . . ? C12 C11 C10 119.2(3) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C13 C12 C11 116.7(2) . . ? C13 C12 C17 121.9(2) . . ? C11 C12 C17 121.4(2) . . ? C12 C13 C14 120.4(2) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? N2 C14 C13 123.0(2) . . ? N2 C14 H14 118.5 . . ? C13 C14 H14 118.5 . . ? N3 C15 C16 123.1(2) . . ? N3 C15 H15 118.4 . . ? C16 C15 H15 118.4 . . ? C15 C16 C17 120.6(2) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C18 115.7(2) . . ? C16 C17 C12 122.5(2) . . ? C18 C17 C12 121.8(2) . . ? C19 C18 C17 120.3(2) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? N3 C19 C18 123.9(2) . . ? N3 C19 H19 118.1 . . ? C18 C19 H19 118.1 . . ? C1 N1 C9 118.8(2) . . ? C1 N1 Ag2 119.90(17) . . ? C9 N1 Ag2 121.16(16) . . ? C14 N2 C10 116.9(2) . . ? C14 N2 Ag2 124.39(18) . . ? C10 N2 Ag2 118.66(18) . . ? C15 N3 C19 116.4(2) . . ? C15 N3 Ag1 122.74(16) . . ? C19 N3 Ag1 119.82(16) . . ? C7 O4 Ag2 111.71(16) . . ? C7 O4 H4 124.1 . . ? Ag2 O4 H4 124.1 . . ? HW1 OW1 HW2 97(3) . . ? O2 S1 O3 112.31(13) . . ? O2 S1 O1 112.26(13) . . ? O3 S1 O1 112.61(14) . . ? O2 S1 C4 107.14(11) . . ? O3 S1 C4 106.70(12) . . ? O1 S1 C4 105.25(12) . . ? 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 N1 C1 C2 C3 2.2(4) . . . . ? C1 C2 C3 C8 -0.2(4) . . . . ? C8 C4 C5 C6 -1.1(4) . . . . ? S1 C4 C5 C6 177.6(2) . . . . ? C4 C5 C6 C7 -1.7(4) . . . . ? C5 C6 C7 O4 -175.3(2) . . . . ? C5 C6 C7 C9 4.7(4) . . . . ? C2 C3 C8 C9 -1.6(4) . . . . ? C2 C3 C8 C4 177.9(3) . . . . ? C5 C4 C8 C3 -178.7(2) . . . . ? S1 C4 C8 C3 2.7(3) . . . . ? C5 C4 C8 C9 0.7(4) . . . . ? S1 C4 C8 C9 -177.92(18) . . . . ? C3 C8 C9 N1 1.5(3) . . . . ? C4 C8 C9 N1 -177.9(2) . . . . ? C3 C8 C9 C7 -178.2(2) . . . . ? C4 C8 C9 C7 2.3(3) . . . . ? O4 C7 C9 N1 -4.8(4) . . . . ? C6 C7 C9 N1 175.3(2) . . . . ? O4 C7 C9 C8 175.0(2) . . . . ? C6 C7 C9 C8 -4.9(4) . . . . ? N2 C10 C11 C12 -0.6(4) . . . . ? C10 C11 C12 C13 1.6(4) . . . . ? C10 C11 C12 C17 -177.1(2) . . . . ? C11 C12 C13 C14 -1.6(4) . . . . ? C17 C12 C13 C14 177.1(2) . . . . ? C12 C13 C14 N2 0.5(4) . . . . ? N3 C15 C16 C17 0.9(4) . . . . ? C15 C16 C17 C18 -0.3(4) . . . . ? C15 C16 C17 C12 179.8(2) . . . . ? C13 C12 C17 C16 -170.6(2) . . . . ? C11 C12 C17 C16 8.0(4) . . . . ? C13 C12 C17 C18 9.6(4) . . . . ? C11 C12 C17 C18 -171.8(2) . . . . ? C16 C17 C18 C19 -0.2(4) . . . . ? C12 C17 C18 C19 179.6(2) . . . . ? C17 C18 C19 N3 0.3(4) . . . . ? C2 C1 N1 C9 -2.3(4) . . . . ? C2 C1 N1 Ag2 174.1(2) . . . . ? C8 C9 N1 C1 0.3(4) . . . . ? C7 C9 N1 C1 -179.9(2) . . . . ? C8 C9 N1 Ag2 -175.99(17) . . . . ? C7 C9 N1 Ag2 3.8(3) . . . . ? O4 Ag2 N1 C1 -177.7(2) . . . . ? O4 Ag2 N1 C9 -1.43(17) . . . . ? C13 C14 N2 C10 0.6(4) . . . . ? C13 C14 N2 Ag2 -175.6(2) . . . . ? C11 C10 N2 C14 -0.5(4) . . . . ? C11 C10 N2 Ag2 175.9(2) . . . . ? O4 Ag2 N2 C14 172.1(2) . . . . ? O4 Ag2 N2 C10 -4.1(2) . . . . ? C16 C15 N3 C19 -0.8(4) . . . . ? C16 C15 N3 Ag1 167.49(19) . . . . ? C18 C19 N3 C15 0.2(4) . . . . ? C18 C19 N3 Ag1 -168.5(2) . . . . ? C6 C7 O4 Ag2 -176.8(2) . . . . ? C9 C7 O4 Ag2 3.3(3) . . . . ? N2 Ag2 O4 C7 170.54(17) . . . . ? N1 Ag2 O4 C7 -1.08(16) . . . . ? C5 C4 S1 O2 128.6(2) . . . . ? C8 C4 S1 O2 -52.7(2) . . . . ? C5 C4 S1 O3 8.1(2) . . . . ? C8 C4 S1 O3 -173.2(2) . . . . ? C5 C4 S1 O1 -111.7(2) . . . . ? C8 C4 S1 O1 66.9(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OW1 HW1 O1 0.869(10) 2.024(11) 2.887(3) 172(3) . OW1 HW2 O1 0.872(10) 2.051(10) 2.920(3) 175(3) 5_767 _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.434 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.064 #===end data_Compd8 _database_code_depnum_ccdc_archive 'CCDC 684630' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H11 Ag N2 O6 S, C10 H8 Ag N2, H2 O ' _chemical_formula_sum 'C25 H21 Ag2 N4 O7 S' _chemical_formula_weight 737.26 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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.929(2) _cell_length_b 10.597(2) _cell_length_c 13.095(3) _cell_angle_alpha 79.59(2) _cell_angle_beta 80.74(3) _cell_angle_gamma 67.55(3) _cell_volume 1246.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5636 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.965 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 730 _exptl_absorpt_coefficient_mu 1.711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 0.751 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12302 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.45 _reflns_number_total 5636 _reflns_number_gt 4362 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+1.5127P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5636 _refine_ls_number_parameters 366 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.09649(3) 0.51419(3) 0.59701(2) 0.04480(10) Uani 1 1 d . . . Ag2 Ag 0.07745(3) 0.65504(3) 0.86198(3) 0.05735(12) Uani 1 1 d . . . C1 C 0.5415(3) 0.4536(3) 0.7290(3) 0.0315(7) Uani 1 1 d . . . H1 H 0.5450 0.4894 0.6588 0.038 Uiso 1 1 calc R . . C2 C 0.6645(3) 0.3616(3) 0.7670(3) 0.0278(6) Uani 1 1 d . . . C3 C 0.6659(3) 0.3054(3) 0.8774(3) 0.0287(7) Uani 1 1 d . . . C4 C 0.7936(4) 0.2125(3) 0.9221(3) 0.0381(8) Uani 1 1 d . . . H5 H 0.8820 0.1844 0.8802 0.046 Uiso 1 1 calc R . . C5 C 0.7888(4) 0.1633(4) 1.0267(3) 0.0448(9) Uani 1 1 d . . . H4 H 0.8738 0.1021 1.0548 0.054 Uiso 1 1 calc R . . C6 C 0.6581(4) 0.2041(4) 1.0904(3) 0.0438(9) Uani 1 1 d . . . H3 H 0.6558 0.1705 1.1611 0.053 Uiso 1 1 calc R . . C7 C 0.5321(4) 0.2942(4) 1.0492(3) 0.0382(8) Uani 1 1 d . . . H2 H 0.4447 0.3204 1.0923 0.046 Uiso 1 1 calc R . . C8 C 0.5335(3) 0.3469(3) 0.9434(3) 0.0302(7) Uani 1 1 d . . . C9 C 0.3970(3) 0.4435(3) 0.9024(3) 0.0299(7) Uani 1 1 d . . . C10 C 0.4050(3) 0.4985(3) 0.7930(3) 0.0314(7) Uani 1 1 d . . . C11 C -0.1893(4) 0.7854(4) 1.0207(3) 0.0458(9) Uani 1 1 d . . . H16 H -0.1324 0.7177 1.0684 0.055 Uiso 1 1 calc R . . C12 C -0.2118(4) 0.9047(4) 0.8570(3) 0.0437(9) Uani 1 1 d . . . H12 H -0.1705 0.9226 0.7896 0.052 Uiso 1 1 calc R . . C13 C -0.3568(4) 0.9823(4) 0.8847(3) 0.0410(8) Uani 1 1 d . . . H13 H -0.4108 1.0500 0.8356 0.049 Uiso 1 1 calc R . . C14 C -0.4223(3) 0.9607(3) 0.9839(3) 0.0297(7) Uani 1 1 d . . . C15 C -0.3324(4) 0.8610(4) 1.0537(3) 0.0436(9) Uani 1 1 d . . . H15 H -0.3690 0.8453 1.1228 0.052 Uiso 1 1 calc R . . C16 C 0.2767(3) 0.2023(3) 0.6459(3) 0.0405(9) Uani 1 1 d . . . H037 H 0.1857 0.1999 0.6749 0.049 Uiso 1 1 calc R . . C17 C 0.3942(3) 0.0815(3) 0.6474(3) 0.0384(8) Uani 1 1 d . . . H019 H 0.3818 -0.0004 0.6770 0.046 Uiso 1 1 calc R . . C18 C 0.5327(3) 0.0798(3) 0.6048(2) 0.0253(6) Uani 1 1 d . . . C19 C 0.5423(3) 0.2063(3) 0.5622(3) 0.0375(8) Uani 1 1 d . . . H23 H 0.6320 0.2115 0.5327 0.045 Uiso 1 1 calc R . . C20 C 0.4190(4) 0.3235(3) 0.5639(3) 0.0409(9) Uani 1 1 d . . . H24 H 0.4281 0.4071 0.5352 0.049 Uiso 1 1 calc R . . C21 C 0.7717(4) -0.2967(3) 0.6405(3) 0.0426(9) Uani 1 1 d . . . H21 H 0.7602 -0.3801 0.6660 0.051 Uiso 1 1 calc R . . C22 C 0.6504(3) -0.1784(3) 0.6432(3) 0.0387(8) Uani 1 1 d . . . H20 H 0.5597 -0.1828 0.6709 0.046 Uiso 1 1 calc R . . C23 C 0.6626(3) -0.0517(3) 0.6045(2) 0.0259(6) Uani 1 1 d . . . C24 C 0.8019(3) -0.0542(3) 0.5659(3) 0.0352(8) Uani 1 1 d . . . H18 H 0.8166 0.0277 0.5397 0.042 Uiso 1 1 calc R . . C25 C 0.9184(3) -0.1774(3) 0.5664(3) 0.0379(8) Uani 1 1 d . . . H17 H 1.0106 -0.1762 0.5398 0.046 Uiso 1 1 calc R . . N1 N 0.2817(3) 0.5923(3) 0.7566(2) 0.0384(7) Uani 1 1 d . . . N2 N -0.1290(3) 0.8052(3) 0.9234(3) 0.0393(7) Uani 1 1 d . . . N3 N 0.2861(3) 0.3239(3) 0.6046(2) 0.0351(6) Uani 1 1 d . . . N4 N 0.9059(3) -0.2986(3) 0.6031(2) 0.0332(6) Uani 1 1 d . . . O1 O 0.7806(3) 0.3801(3) 0.5764(2) 0.0511(7) Uani 1 1 d . . . O2 O 0.8689(3) 0.1593(2) 0.6829(2) 0.0477(7) Uani 1 1 d . . . O3 O 0.9323(2) 0.3471(3) 0.7133(2) 0.0466(6) Uani 1 1 d . . . O4 O 0.2859(3) 0.6439(3) 0.6609(2) 0.0557(8) Uani 1 1 d . . . O5 O 0.2794(2) 0.4771(3) 0.9607(2) 0.0433(6) Uani 1 1 d . . . OW1 O -0.0718(4) 0.5033(4) 0.8654(3) 0.0621(9) Uani 1 1 d D . . OW2 O 1.1480(4) -0.0634(4) 0.7024(4) 0.0896(13) Uani 1 1 d D . . S1 S 0.82468(8) 0.30745(8) 0.67748(7) 0.03294(19) Uani 1 1 d . . . HW1 H -0.146(5) 0.517(5) 0.908(4) 0.087(18) Uiso 1 1 d D . . HW2 H -0.073(6) 0.453(5) 0.828(4) 0.08(2) Uiso 1 1 d D . . HW3 H 1.063(5) -0.016(5) 0.693(5) 0.122 Uiso 1 1 d D . . HW4 H 1.161(7) -0.134(5) 0.674(6) 0.122 Uiso 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 0.02944(14) 0.02762(13) 0.05682(19) -0.00498(12) -0.00110(12) 0.01073(10) Ag2 0.02403(15) 0.0555(2) 0.0741(2) -0.01480(16) 0.01055(13) 0.00249(12) C1 0.0291(16) 0.0359(16) 0.0272(17) -0.0053(13) 0.0007(12) -0.0102(13) C2 0.0186(14) 0.0250(14) 0.0344(17) -0.0082(13) 0.0039(11) -0.0027(11) C3 0.0274(15) 0.0263(14) 0.0339(17) -0.0052(13) -0.0006(12) -0.0117(12) C4 0.0310(17) 0.0323(17) 0.049(2) -0.0046(16) -0.0070(15) -0.0090(14) C5 0.044(2) 0.0341(18) 0.056(3) 0.0039(17) -0.0198(18) -0.0119(16) C6 0.055(2) 0.0402(19) 0.038(2) 0.0022(16) -0.0089(17) -0.0212(18) C7 0.045(2) 0.0397(18) 0.0343(19) -0.0046(15) 0.0022(15) -0.0221(16) C8 0.0321(16) 0.0276(15) 0.0336(18) -0.0070(13) 0.0016(13) -0.0144(13) C9 0.0263(15) 0.0277(15) 0.0377(19) -0.0115(13) 0.0053(13) -0.0122(12) C10 0.0244(15) 0.0331(16) 0.0357(18) -0.0098(14) 0.0012(12) -0.0085(13) C11 0.0276(17) 0.0380(19) 0.056(2) 0.0027(17) -0.0032(16) 0.0008(15) C12 0.0280(17) 0.053(2) 0.042(2) -0.0117(17) 0.0050(14) -0.0064(16) C13 0.0304(17) 0.050(2) 0.035(2) -0.0071(16) -0.0022(14) -0.0065(15) C14 0.0222(15) 0.0258(14) 0.0423(19) -0.0140(14) -0.0005(13) -0.0070(12) C15 0.0333(18) 0.043(2) 0.043(2) -0.0001(16) 0.0028(15) -0.0063(15) C16 0.0232(16) 0.0326(17) 0.053(2) -0.0015(16) 0.0073(14) -0.0022(13) C17 0.0249(16) 0.0254(15) 0.051(2) 0.0046(15) 0.0029(14) -0.0007(13) C18 0.0187(13) 0.0194(13) 0.0294(16) -0.0038(12) -0.0023(11) 0.0024(11) C19 0.0226(15) 0.0276(16) 0.056(2) -0.0034(15) -0.0009(14) -0.0042(13) C20 0.0300(17) 0.0226(15) 0.062(3) 0.0004(15) -0.0079(16) -0.0024(13) C21 0.0319(18) 0.0209(15) 0.064(3) 0.0000(16) 0.0017(16) -0.0020(13) C22 0.0250(16) 0.0290(16) 0.054(2) -0.0031(15) 0.0056(14) -0.0060(13) C23 0.0208(14) 0.0189(13) 0.0309(17) -0.0041(12) -0.0037(11) 0.0014(11) C24 0.0262(16) 0.0242(15) 0.047(2) -0.0045(14) 0.0052(14) -0.0040(13) C25 0.0223(15) 0.0312(17) 0.050(2) -0.0073(15) 0.0055(14) -0.0016(13) N1 0.0217(13) 0.0379(15) 0.0446(18) -0.0107(13) -0.0018(12) 0.0030(11) N2 0.0227(13) 0.0341(15) 0.055(2) -0.0141(14) 0.0018(12) -0.0021(11) N3 0.0233(13) 0.0240(13) 0.0453(17) -0.0049(12) -0.0048(11) 0.0060(10) N4 0.0216(13) 0.0208(12) 0.0439(17) -0.0039(11) -0.0014(11) 0.0058(10) O1 0.0410(14) 0.0583(16) 0.0362(15) 0.0009(12) 0.0103(11) -0.0071(12) O2 0.0447(14) 0.0308(12) 0.0611(18) -0.0156(12) 0.0071(12) -0.0072(11) O3 0.0280(12) 0.0541(15) 0.0606(18) -0.0229(13) 0.0109(11) -0.0174(11) O4 0.0412(15) 0.0636(18) 0.0389(16) -0.0019(13) -0.0061(11) 0.0053(13) O5 0.0282(12) 0.0465(14) 0.0454(15) -0.0097(12) 0.0130(10) -0.0076(10) OW1 0.065(2) 0.082(2) 0.056(2) -0.0287(18) 0.0198(16) -0.0464(18) OW2 0.067(2) 0.063(2) 0.133(4) 0.011(2) -0.043(2) -0.0164(19) S1 0.0231(4) 0.0295(4) 0.0394(5) -0.0093(3) 0.0076(3) -0.0042(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 N4 2.160(2) 1_465 ? Ag1 N3 2.170(3) . ? Ag2 N2 2.195(3) . ? Ag2 N1 2.205(3) . ? Ag2 O5 2.512(3) . ? Ag2 OW1 2.560(3) . ? C1 C2 1.342(4) . ? C1 C10 1.432(4) . ? C1 H1 0.9300 . ? C2 C3 1.461(5) . ? C2 S1 1.783(3) . ? C3 C4 1.413(5) . ? C3 C8 1.414(4) . ? C4 C5 1.375(5) . ? C4 H5 0.9300 . ? C5 C6 1.385(6) . ? C5 H4 0.9300 . ? C6 C7 1.374(5) . ? C6 H3 0.9300 . ? C7 C8 1.397(5) . ? C7 H2 0.9300 . ? C8 C9 1.466(5) . ? C9 O5 1.251(4) . ? C9 C10 1.447(5) . ? C10 N1 1.343(4) . ? C11 N2 1.335(5) . ? C11 C15 1.380(5) . ? C11 H16 0.9300 . ? C12 N2 1.334(5) . ? C12 C13 1.385(5) . ? C12 H12 0.9300 . ? C13 C14 1.378(5) . ? C13 H13 0.9300 . ? C14 C15 1.393(5) . ? C14 C14 1.480(6) 2_477 ? C15 H15 0.9300 . ? C16 N3 1.336(4) . ? C16 C17 1.363(4) . ? C16 H037 0.9300 . ? C17 C18 1.393(4) . ? C17 H019 0.9300 . ? C18 C19 1.388(4) . ? C18 C23 1.495(4) . ? C19 C20 1.372(4) . ? C19 H23 0.9300 . ? C20 N3 1.340(4) . ? C20 H24 0.9300 . ? C21 N4 1.337(4) . ? C21 C22 1.368(4) . ? C21 H21 0.9300 . ? C22 C23 1.391(4) . ? C22 H20 0.9300 . ? C23 C24 1.386(4) . ? C24 C25 1.375(4) . ? C24 H18 0.9300 . ? C25 N4 1.332(4) . ? C25 H17 0.9300 . ? N1 O4 1.274(4) . ? N4 Ag1 2.160(2) 1_645 ? O1 S1 1.448(3) . ? O2 S1 1.451(2) . ? O3 S1 1.454(3) . ? OW1 HW1 0.83(4) . ? OW1 HW2 0.79(3) . ? OW2 HW3 0.82(4) . ? OW2 HW4 0.85(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 N4 Ag1 N3 175.36(11) 1_465 . ? N2 Ag2 N1 153.91(12) . . ? N2 Ag2 O5 128.66(10) . . ? N1 Ag2 O5 70.40(10) . . ? N2 Ag2 OW1 85.45(12) . . ? N1 Ag2 OW1 112.15(12) . . ? O5 Ag2 OW1 96.52(11) . . ? C2 C1 C10 122.2(3) . . ? C2 C1 H1 118.9 . . ? C10 C1 H1 118.9 . . ? C1 C2 C3 121.1(3) . . ? C1 C2 S1 117.6(3) . . ? C3 C2 S1 121.3(2) . . ? C4 C3 C8 118.1(3) . . ? C4 C3 C2 123.3(3) . . ? C8 C3 C2 118.6(3) . . ? C5 C4 C3 120.8(3) . . ? C5 C4 H5 119.6 . . ? C3 C4 H5 119.6 . . ? C4 C5 C6 120.5(3) . . ? C4 C5 H4 119.8 . . ? C6 C5 H4 119.8 . . ? C7 C6 C5 120.0(4) . . ? C7 C6 H3 120.0 . . ? C5 C6 H3 120.0 . . ? C6 C7 C8 121.0(3) . . ? C6 C7 H2 119.5 . . ? C8 C7 H2 119.5 . . ? C7 C8 C3 119.6(3) . . ? C7 C8 C9 119.4(3) . . ? C3 C8 C9 121.0(3) . . ? O5 C9 C10 122.1(3) . . ? O5 C9 C8 120.7(3) . . ? C10 C9 C8 117.2(3) . . ? N1 C10 C1 122.9(3) . . ? N1 C10 C9 117.3(3) . . ? C1 C10 C9 119.8(3) . . ? N2 C11 C15 122.8(3) . . ? N2 C11 H16 118.6 . . ? C15 C11 H16 118.6 . . ? N2 C12 C13 122.5(3) . . ? N2 C12 H12 118.8 . . ? C13 C12 H12 118.8 . . ? C14 C13 C12 120.9(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 115.9(3) . . ? C13 C14 C14 122.6(4) . 2_477 ? C15 C14 C14 121.5(4) . 2_477 ? C11 C15 C14 120.4(3) . . ? C11 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? N3 C16 C17 123.1(3) . . ? N3 C16 H037 118.5 . . ? C17 C16 H037 118.5 . . ? C16 C17 C18 120.6(3) . . ? C16 C17 H019 119.7 . . ? C18 C17 H019 119.7 . . ? C19 C18 C17 116.3(3) . . ? C19 C18 C23 122.3(3) . . ? C17 C18 C23 121.4(3) . . ? C20 C19 C18 119.8(3) . . ? C20 C19 H23 120.1 . . ? C18 C19 H23 120.1 . . ? N3 C20 C19 123.5(3) . . ? N3 C20 H24 118.3 . . ? C19 C20 H24 118.3 . . ? N4 C21 C22 123.5(3) . . ? N4 C21 H21 118.3 . . ? C22 C21 H21 118.3 . . ? C21 C22 C23 120.0(3) . . ? C21 C22 H20 120.0 . . ? C23 C22 H20 120.0 . . ? C24 C23 C22 116.3(3) . . ? C24 C23 C18 121.9(3) . . ? C22 C23 C18 121.8(3) . . ? C25 C24 C23 120.1(3) . . ? C25 C24 H18 119.9 . . ? C23 C24 H18 119.9 . . ? N4 C25 C24 123.3(3) . . ? N4 C25 H17 118.3 . . ? C24 C25 H17 118.3 . . ? O4 N1 C10 118.8(3) . . ? O4 N1 Ag2 121.3(2) . . ? C10 N1 Ag2 120.0(2) . . ? C12 N2 C11 117.5(3) . . ? C12 N2 Ag2 119.1(2) . . ? C11 N2 Ag2 122.1(2) . . ? C16 N3 C20 116.8(3) . . ? C16 N3 Ag1 122.7(2) . . ? C20 N3 Ag1 120.5(2) . . ? C25 N4 C21 116.8(3) . . ? C25 N4 Ag1 119.9(2) . 1_645 ? C21 N4 Ag1 123.3(2) . 1_645 ? C9 O5 Ag2 110.2(2) . . ? Ag2 OW1 HW1 117(3) . . ? Ag2 OW1 HW2 135(4) . . ? HW1 OW1 HW2 107(4) . . ? HW3 OW2 HW4 102(4) . . ? O1 S1 O2 112.88(18) . . ? O1 S1 O3 112.80(18) . . ? O2 S1 O3 112.56(16) . . ? O1 S1 C2 105.62(15) . . ? O2 S1 C2 106.32(15) . . ? O3 S1 C2 105.92(15) . . ? 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 C10 C1 C2 C3 -1.9(5) . . . . ? C10 C1 C2 S1 176.6(3) . . . . ? C1 C2 C3 C4 -177.4(3) . . . . ? S1 C2 C3 C4 4.0(4) . . . . ? C1 C2 C3 C8 1.9(5) . . . . ? S1 C2 C3 C8 -176.6(2) . . . . ? C8 C3 C4 C5 0.4(5) . . . . ? C2 C3 C4 C5 179.8(3) . . . . ? C3 C4 C5 C6 -0.1(6) . . . . ? C4 C5 C6 C7 0.2(6) . . . . ? C5 C6 C7 C8 -0.6(6) . . . . ? C6 C7 C8 C3 1.0(5) . . . . ? C6 C7 C8 C9 -179.6(3) . . . . ? C4 C3 C8 C7 -0.9(5) . . . . ? C2 C3 C8 C7 179.8(3) . . . . ? C4 C3 C8 C9 179.8(3) . . . . ? C2 C3 C8 C9 0.4(5) . . . . ? C7 C8 C9 O5 -1.1(5) . . . . ? C3 C8 C9 O5 178.2(3) . . . . ? C7 C8 C9 C10 178.1(3) . . . . ? C3 C8 C9 C10 -2.5(4) . . . . ? C2 C1 C10 N1 178.8(3) . . . . ? C2 C1 C10 C9 -0.3(5) . . . . ? O5 C9 C10 N1 2.6(5) . . . . ? C8 C9 C10 N1 -176.6(3) . . . . ? O5 C9 C10 C1 -178.2(3) . . . . ? C8 C9 C10 C1 2.5(5) . . . . ? N2 C12 C13 C14 0.8(6) . . . . ? C12 C13 C14 C15 2.3(5) . . . . ? C12 C13 C14 C14 -178.7(4) . . . 2_477 ? N2 C11 C15 C14 1.7(6) . . . . ? C13 C14 C15 C11 -3.4(5) . . . . ? C14 C14 C15 C11 177.5(4) 2_477 . . . ? N3 C16 C17 C18 0.0(6) . . . . ? C16 C17 C18 C19 0.1(5) . . . . ? C16 C17 C18 C23 -179.2(3) . . . . ? C17 C18 C19 C20 0.0(5) . . . . ? C23 C18 C19 C20 179.4(3) . . . . ? C18 C19 C20 N3 -0.3(6) . . . . ? N4 C21 C22 C23 0.8(6) . . . . ? C21 C22 C23 C24 -0.9(5) . . . . ? C21 C22 C23 C18 179.3(3) . . . . ? C19 C18 C23 C24 3.1(5) . . . . ? C17 C18 C23 C24 -177.5(3) . . . . ? C19 C18 C23 C22 -177.0(3) . . . . ? C17 C18 C23 C22 2.3(5) . . . . ? C22 C23 C24 C25 0.6(5) . . . . ? C18 C23 C24 C25 -179.6(3) . . . . ? C23 C24 C25 N4 -0.3(6) . . . . ? C1 C10 N1 O4 0.0(5) . . . . ? C9 C10 N1 O4 179.2(3) . . . . ? C1 C10 N1 Ag2 -179.7(2) . . . . ? C9 C10 N1 Ag2 -0.6(4) . . . . ? N2 Ag2 N1 O4 -39.0(4) . . . . ? O5 Ag2 N1 O4 179.7(3) . . . . ? OW1 Ag2 N1 O4 90.5(3) . . . . ? N2 Ag2 N1 C10 140.8(3) . . . . ? O5 Ag2 N1 C10 -0.6(2) . . . . ? OW1 Ag2 N1 C10 -89.7(3) . . . . ? C13 C12 N2 C11 -2.6(6) . . . . ? C13 C12 N2 Ag2 164.3(3) . . . . ? C15 C11 N2 C12 1.4(6) . . . . ? C15 C11 N2 Ag2 -165.1(3) . . . . ? N1 Ag2 N2 C12 38.8(4) . . . . ? O5 Ag2 N2 C12 169.9(2) . . . . ? OW1 Ag2 N2 C12 -95.4(3) . . . . ? N1 Ag2 N2 C11 -154.9(3) . . . . ? O5 Ag2 N2 C11 -23.8(3) . . . . ? OW1 Ag2 N2 C11 70.9(3) . . . . ? C17 C16 N3 C20 -0.3(6) . . . . ? C17 C16 N3 Ag1 177.4(3) . . . . ? C19 C20 N3 C16 0.5(6) . . . . ? C19 C20 N3 Ag1 -177.3(3) . . . . ? C24 C25 N4 C21 0.2(6) . . . . ? C24 C25 N4 Ag1 178.9(3) . . . 1_645 ? C22 C21 N4 C25 -0.5(6) . . . . ? C22 C21 N4 Ag1 -179.1(3) . . . 1_645 ? C10 C9 O5 Ag2 -2.9(4) . . . . ? C8 C9 O5 Ag2 176.3(2) . . . . ? N2 Ag2 O5 C9 -157.6(2) . . . . ? N1 Ag2 O5 C9 1.8(2) . . . . ? OW1 Ag2 O5 C9 113.1(2) . . . . ? C1 C2 S1 O1 -0.7(3) . . . . ? C3 C2 S1 O1 177.9(3) . . . . ? C1 C2 S1 O2 -120.8(3) . . . . ? C3 C2 S1 O2 57.7(3) . . . . ? C1 C2 S1 O3 119.2(3) . . . . ? C3 C2 S1 O3 -62.2(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OW1 HW2 O3 0.79(3) 2.02(4) 2.798(5) 170(6) 1_455 OW1 HW1 O5 0.83(4) 1.99(4) 2.795(4) 163(5) 2_567 OW2 HW4 O4 0.85(4) 2.22(4) 2.986(5) 149(6) 1_645 OW2 HW3 O2 0.82(4) 2.10(4) 2.886(5) 160(6) . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.662 _refine_diff_density_min -0.840 _refine_diff_density_rms 0.090 #===end data_compd9 _database_code_depnum_ccdc_archive 'CCDC 684631' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H16 Ag2 N4, C10 H6 O6 S2, 2(H2 O)' _chemical_formula_sum 'C30 H26 Ag2 N4 O8 S2' _chemical_formula_weight 850.41 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc ' 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 18.944(4) _cell_length_b 11.431(2) _cell_length_c 13.951(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.24(3) _cell_angle_gamma 90.00 _cell_volume 2973(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5636 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.203 _exptl_crystal_size_min 0.156 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.900 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 1.518 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 0.792 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27955 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6742 _reflns_number_gt 3931 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+23.9662P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6742 _refine_ls_number_parameters 430 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1258 _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.2193 _refine_ls_wR_factor_gt 0.1974 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.23925(4) 0.11032(5) 0.87243(7) 0.0548(3) Uani 1 1 d . . . Ag2 Ag 0.25886(4) 0.45180(6) 0.61419(7) 0.0553(3) Uani 1 1 d . . . C1 C 0.1985(5) 0.2011(8) 0.5900(9) 0.054(3) Uani 1 1 d . . . H1 H 0.1568 0.2415 0.5645 0.065 Uiso 1 1 calc R . . C2 C 0.1953(5) 0.0781(7) 0.5925(8) 0.049(2) Uani 1 1 d . . . H2 H 0.1526 0.0388 0.5697 0.059 Uiso 1 1 calc R . . C3 C 0.2569(4) 0.0174(6) 0.6296(7) 0.0347(19) Uani 1 1 d . . . C4 C 0.3197(5) 0.0803(8) 0.6668(8) 0.050(2) Uani 1 1 d . . . H4 H 0.3614 0.0410 0.6943 0.060 Uiso 1 1 calc R . . C5 C 0.3186(5) 0.2006(8) 0.6618(9) 0.057(3) Uani 1 1 d . . . H5 H 0.3606 0.2409 0.6865 0.069 Uiso 1 1 calc R . . C6 C 0.3204(5) 0.7024(8) 0.6208(8) 0.049(2) Uani 1 1 d . . . H6 H 0.3632 0.6621 0.6215 0.059 Uiso 1 1 calc R . . C7 C 0.3214(4) 0.8242(7) 0.6240(8) 0.045(2) Uani 1 1 d . . . H7 H 0.3644 0.8638 0.6246 0.054 Uiso 1 1 calc R . . C8C C 0.2582(4) 0.8884(6) 0.6264(6) 0.0351(18) Uani 1 1 d . . . C9 C 0.1955(5) 0.8185(7) 0.6248(7) 0.045(2) Uani 1 1 d . . . H9 H 0.1520 0.8551 0.6274 0.054 Uiso 1 1 calc R . . C10 C 0.1978(5) 0.7011(7) 0.6195(7) 0.046(2) Uani 1 1 d . . . H10 H 0.1556 0.6588 0.6176 0.055 Uiso 1 1 calc R . . C13 C 0.1812(5) 0.3633(8) 0.8243(8) 0.054(3) Uani 1 1 d . . . H13 H 0.1392 0.3235 0.7993 0.065 Uiso 1 1 calc R . . C14 C 0.1804(5) 0.4823(7) 0.8202(8) 0.049(2) Uani 1 1 d . . . H14 H 0.1388 0.5209 0.7915 0.059 Uiso 1 1 calc R . . C15 C 0.2414(5) 0.5470(8) 0.8585(7) 0.043(2) Uani 1 1 d . . . C16 C 0.3025(5) 0.4811(8) 0.8972(8) 0.050(2) Uani 1 1 d . . . H16 H 0.3451 0.5182 0.9239 0.060 Uiso 1 1 calc R . . C17 C 0.2982(5) 0.3558(8) 0.8951(8) 0.052(3) Uani 1 1 d . . . H17 H 0.3394 0.3129 0.9183 0.063 Uiso 1 1 calc R . . C18 C 0.2414(5) 0.6774(7) 0.8641(7) 0.042(2) Uani 1 1 d . . . C19 C 0.1785(5) 0.7372(7) 0.8651(7) 0.046(2) Uani 1 1 d . . . H19 H 0.1356 0.6968 0.8631 0.055 Uiso 1 1 calc R . . C20 C 0.1797(5) 0.8574(7) 0.8692(8) 0.047(2) Uani 1 1 d . . . H20 H 0.1366 0.8958 0.8706 0.056 Uiso 1 1 calc R . . C21 C 0.3001(5) 0.8616(8) 0.8699(7) 0.047(2) Uani 1 1 d . . . H21 H 0.3426 0.9030 0.8719 0.056 Uiso 1 1 calc R . . C22 C 0.3032(5) 0.7401(7) 0.8657(8) 0.046(2) Uani 1 1 d . . . H22 H 0.3464 0.7022 0.8639 0.055 Uiso 1 1 calc R . . C23 C 0.4913(6) 0.5735(13) 0.8666(10) 0.088(5) Uani 1 1 d D . . H23 H 0.4886 0.6458 0.8355 0.106 Uiso 1 1 calc R . . C24 C 0.4888(5) 0.4652(11) 0.8202(9) 0.066(3) Uani 1 1 d D . . C25 C 0.4886(7) 0.3529(12) 0.8636(8) 0.077(4) Uani 1 1 d D . . H25 H 0.4844 0.2864 0.8247 0.092 Uiso 1 1 calc R . . C26 C 0.4947(6) 0.3415(8) 0.9653(10) 0.112(7) Uani 1 1 d D . . H26 H 0.4948 0.2683 0.9945 0.135 Uiso 1 1 calc R . . C27 C 0.5008(5) 0.4451(6) 1.0215(9) 0.066(4) Uani 1 1 d D . . C28 C 0.0039(5) 0.3375(6) 0.0190(7) 0.040(2) Uani 1 1 d . . . H28 H 0.0037 0.2695 -0.0176 0.048 Uiso 1 1 calc R . . C29 C 0.0092(5) 0.3306(7) 0.1171(7) 0.043(2) Uani 1 1 d . . . H29 H 0.0114 0.2576 0.1469 0.051 Uiso 1 1 calc R . . C30 C 0.0115(4) 0.4333(8) 0.1747(7) 0.041(2) Uani 1 1 d . . . C31 C 0.0062(5) 0.5413(8) 0.1310(7) 0.042(2) Uani 1 1 d . . . H31 H 0.0058 0.6081 0.1689 0.051 Uiso 1 1 calc R . . C32 C 0.0015(4) 0.5524(6) 0.0280(7) 0.0349(19) Uani 1 1 d . . . N1 N 0.2591(4) 0.2646(5) 0.6227(6) 0.0443(19) Uani 1 1 d . . . N2 N 0.2599(4) 0.6422(7) 0.6169(6) 0.0459(18) Uani 1 1 d . . . N3 N 0.2393(4) 0.2999(7) 0.8624(6) 0.052(2) Uani 1 1 d . . . N4 N 0.2392(4) 0.9238(5) 0.8714(6) 0.0405(18) Uani 1 1 d . . . O1 O 0.0015(4) 0.5341(6) 0.3388(6) 0.0616(19) Uani 1 1 d . . . O2 O -0.0407(4) 0.3332(6) 0.3115(5) 0.0532(17) Uani 1 1 d . . . O3 O 0.0857(4) 0.3761(6) 0.3425(6) 0.0596(18) Uani 1 1 d . . . O5 O 0.5074(6) 0.5770(8) 0.6639(7) 0.093(3) Uani 1 1 d . . . O6 O 0.5328(5) 0.3714(10) 0.6750(7) 0.099(3) Uani 1 1 d . . . O4 O 0.4106(4) 0.4397(8) 0.6499(6) 0.072(2) Uani 1 1 d . . . OW1 O 0.1135(4) 0.4471(7) 0.5529(6) 0.0592(18) Uani 1 1 d D . . OW2 O 0.3813(4) 0.1123(7) 0.9471(7) 0.065(2) Uani 1 1 d D . . S1 S 0.01486(12) 0.41723(19) 0.30217(18) 0.0410(5) Uani 1 1 d . . . S2 S 0.48506(13) 0.4624(2) 0.6919(2) 0.0546(6) Uani 1 1 d . . . HW1A H 0.078(5) 0.457(12) 0.577(8) 0.09(5) Uiso 1 1 d D . . HW2A H 0.418(4) 0.100(9) 0.920(7) 0.05(3) Uiso 1 1 d D . . HW2B H 0.393(7) 0.094(12) 1.007(4) 0.09(5) Uiso 1 1 d D . . HW1B H 0.100(7) 0.430(15) 0.495(5) 0.139 Uiso 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 0.0633(5) 0.0252(3) 0.0793(6) -0.0001(3) 0.0215(4) 0.0010(3) Ag2 0.0625(5) 0.0251(3) 0.0819(6) -0.0022(3) 0.0225(4) -0.0009(3) C1 0.031(4) 0.035(5) 0.099(9) 0.006(5) 0.017(5) 0.002(4) C2 0.030(4) 0.028(4) 0.090(8) 0.000(4) 0.011(5) -0.001(4) C3 0.024(4) 0.016(3) 0.065(6) -0.011(3) 0.008(4) 0.002(3) C4 0.025(4) 0.043(5) 0.078(7) -0.001(5) 0.001(4) -0.004(4) C5 0.036(5) 0.039(5) 0.095(9) -0.013(5) 0.011(5) -0.018(4) C6 0.035(5) 0.040(5) 0.074(7) 0.004(5) 0.016(4) 0.010(4) C7 0.033(4) 0.030(4) 0.076(7) 0.003(4) 0.022(4) -0.001(4) C8C 0.033(4) 0.018(3) 0.054(5) 0.001(3) 0.006(4) -0.006(3) C9 0.037(5) 0.030(4) 0.071(7) -0.003(4) 0.021(4) -0.003(4) C10 0.045(5) 0.032(4) 0.062(6) 0.000(4) 0.015(4) -0.011(4) C13 0.050(6) 0.030(4) 0.082(8) 0.008(4) 0.012(5) 0.007(4) C14 0.041(5) 0.024(4) 0.082(7) 0.003(4) 0.008(5) 0.009(4) C15 0.041(5) 0.045(5) 0.045(5) 0.001(4) 0.013(4) -0.007(4) C16 0.033(5) 0.040(5) 0.075(7) 0.001(5) 0.006(4) 0.004(4) C17 0.043(5) 0.027(4) 0.089(8) -0.002(4) 0.016(5) 0.005(4) C18 0.054(5) 0.029(4) 0.046(6) 0.002(4) 0.014(4) 0.013(4) C19 0.046(5) 0.029(4) 0.063(7) -0.006(4) 0.011(4) -0.004(4) C20 0.047(5) 0.027(4) 0.070(7) -0.002(4) 0.019(5) 0.000(4) C21 0.039(5) 0.038(4) 0.064(7) 0.006(4) 0.013(4) -0.001(4) C22 0.036(5) 0.029(4) 0.073(7) 0.002(4) 0.010(4) 0.007(4) C23 0.035(5) 0.153(14) 0.081(9) -0.035(9) 0.023(6) -0.028(7) C24 0.034(5) 0.088(9) 0.077(8) -0.016(7) 0.017(5) -0.003(5) C25 0.066(8) 0.108(11) 0.058(8) 0.012(7) 0.015(6) -0.003(7) C26 0.044(6) 0.027(5) 0.27(2) -0.017(9) 0.046(10) -0.009(5) C27 0.036(5) 0.012(4) 0.152(12) -0.007(5) 0.022(6) -0.006(3) C28 0.049(5) 0.011(3) 0.061(6) 0.000(3) 0.013(4) -0.002(3) C29 0.047(5) 0.028(4) 0.055(6) 0.003(4) 0.014(4) 0.003(4) C30 0.035(4) 0.040(4) 0.051(6) 0.000(4) 0.016(4) -0.001(4) C31 0.038(5) 0.041(5) 0.050(6) -0.003(4) 0.013(4) -0.002(4) C32 0.033(4) 0.012(3) 0.062(6) -0.001(3) 0.016(4) -0.003(3) N1 0.044(4) 0.019(3) 0.073(6) -0.004(3) 0.019(4) 0.000(3) N2 0.042(4) 0.046(4) 0.051(5) 0.003(3) 0.014(4) 0.000(4) N3 0.041(4) 0.053(5) 0.065(6) -0.001(4) 0.019(4) 0.000(4) N4 0.046(4) 0.010(2) 0.067(5) -0.003(3) 0.016(4) -0.004(3) O1 0.080(5) 0.049(4) 0.063(5) -0.013(3) 0.030(4) -0.005(4) O2 0.059(4) 0.043(3) 0.062(5) 0.006(3) 0.022(3) -0.012(3) O3 0.043(4) 0.068(5) 0.065(5) 0.004(4) 0.004(3) 0.009(3) O5 0.121(8) 0.081(6) 0.081(7) -0.010(5) 0.029(6) -0.046(6) O6 0.082(6) 0.133(9) 0.085(7) -0.006(6) 0.024(5) 0.051(6) O4 0.041(4) 0.099(6) 0.074(6) -0.011(5) 0.009(4) -0.013(4) OW1 0.048(4) 0.058(4) 0.071(5) -0.006(4) 0.009(4) 0.001(4) OW2 0.048(4) 0.069(5) 0.078(7) 0.001(5) 0.010(4) 0.010(4) S1 0.0397(11) 0.0354(10) 0.0497(14) 0.0004(9) 0.0126(10) -0.0011(9) S2 0.0429(13) 0.0590(15) 0.0643(17) -0.0048(13) 0.0164(12) -0.0078(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 N4 2.132(6) 1_545 ? Ag1 N3 2.171(8) . ? Ag2 N1 2.143(6) . ? Ag2 N2 2.177(8) . ? C1 N1 1.367(11) . ? C1 C2 1.407(12) . ? C1 H1 0.9300 . ? C2 C3 1.377(12) . ? C2 H2 0.9300 . ? C3 C4 1.408(11) . ? C3 C8C 1.477(9) 1_545 ? C4 C5 1.378(13) . ? C4 H4 0.9300 . ? C5 N1 1.373(12) . ? C5 H5 0.9300 . ? C6 N2 1.330(11) . ? C6 C7 1.394(12) . ? C6 H6 0.9300 . ? C7 C8C 1.409(11) . ? C7 H7 0.9300 . ? C8C C9 1.428(11) . ? C8C C3 1.477(9) 1_565 ? C9 C10 1.346(11) . ? C9 H9 0.9300 . ? C10 N2 1.361(11) . ? C10 H10 0.9300 . ? C13 N3 1.346(12) . ? C13 C14 1.362(11) . ? C13 H13 0.9300 . ? C14 C15 1.396(13) . ? C14 H14 0.9300 . ? C15 C16 1.405(13) . ? C15 C18 1.493(12) . ? C16 C17 1.435(12) . ? C16 H16 0.9300 . ? C17 N3 1.296(12) . ? C17 H17 0.9300 . ? C18 C22 1.369(12) . ? C18 C19 1.376(12) . ? C19 C20 1.375(11) . ? C19 H19 0.9300 . ? C20 N4 1.354(11) . ? C20 H20 0.9300 . ? C21 N4 1.360(11) . ? C21 C22 1.392(11) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.394(9) . ? C23 C27 1.557(18) 3_667 ? C23 H23 0.9300 . ? C24 C25 1.420(17) . ? C24 S2 1.779(13) . ? C25 C26 1.408(9) . ? C25 H25 0.9300 . ? C26 C27 1.413(8) . ? C26 H26 0.9300 . ? C27 C27 1.389(18) 3_667 ? C27 C23 1.557(18) 3_667 ? C28 C29 1.357(13) . ? C28 C32 1.414(10) 3_565 ? C28 H28 0.9300 . ? C29 C30 1.419(12) . ? C29 H29 0.9300 . ? C30 C31 1.373(12) . ? C30 S1 1.778(10) . ? C31 C32 1.430(13) . ? C31 H31 0.9300 . ? C32 C28 1.414(10) 3_565 ? C32 C32 1.425(14) 3_565 ? N4 Ag1 2.132(6) 1_565 ? O1 S1 1.469(7) . ? O2 S1 1.449(6) . ? O3 S1 1.439(7) . ? O5 S2 1.451(9) . ? O6 S2 1.426(9) . ? O4 S2 1.451(7) . ? OW1 HW1A 0.81(5) . ? OW1 HW1B 0.83(5) . ? OW2 HW2A 0.86(5) . ? OW2 HW2B 0.85(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 N4 Ag1 N3 175.9(3) 1_545 . ? N1 Ag2 N2 175.9(3) . . ? N1 C1 C2 124.0(8) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C3 C2 C1 118.4(8) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 119.1(7) . . ? C2 C3 C8C 120.7(7) . 1_545 ? C4 C3 C8C 120.2(7) . 1_545 ? C5 C4 C3 119.1(8) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 123.8(8) . . ? N1 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? N2 C6 C7 121.6(8) . . ? N2 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C6 C7 C8C 120.9(7) . . ? C6 C7 H7 119.5 . . ? C8C C7 H7 119.5 . . ? C7 C8C C9 114.6(7) . . ? C7 C8C C3 122.6(7) . 1_565 ? C9 C8C C3 122.8(7) . 1_565 ? C10 C9 C8C 121.6(8) . . ? C10 C9 H9 119.2 . . ? C8C C9 H9 119.2 . . ? C9 C10 N2 122.0(8) . . ? C9 C10 H10 119.0 . . ? N2 C10 H10 119.0 . . ? N3 C13 C14 123.8(9) . . ? N3 C13 H13 118.1 . . ? C14 C13 H13 118.1 . . ? C13 C14 C15 120.8(9) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C16 115.5(8) . . ? C14 C15 C18 122.8(8) . . ? C16 C15 C18 121.6(8) . . ? C15 C16 C17 119.2(9) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? N3 C17 C16 122.8(9) . . ? N3 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? C22 C18 C19 118.7(8) . . ? C22 C18 C15 121.0(7) . . ? C19 C18 C15 120.3(8) . . ? C20 C19 C18 119.2(8) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? N4 C20 C19 124.7(8) . . ? N4 C20 H20 117.7 . . ? C19 C20 H20 117.7 . . ? N4 C21 C22 124.4(8) . . ? N4 C21 H21 117.8 . . ? C22 C21 H21 117.8 . . ? C18 C22 C21 118.7(8) . . ? C18 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C24 C23 C27 109.4(12) . 3_667 ? C24 C23 H23 125.3 . . ? C27 C23 H23 125.3 3_667 . ? C23 C24 C25 127.5(12) . . ? C23 C24 S2 118.3(11) . . ? C25 C24 S2 114.2(8) . . ? C26 C25 C24 120.5(11) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 117.7(9) . . ? C25 C26 H26 121.1 . . ? C27 C26 H26 121.1 . . ? C27 C27 C26 121.7(12) 3_667 . ? C27 C27 C23 123.2(11) 3_667 3_667 ? C26 C27 C23 115.2(9) . 3_667 ? C29 C28 C32 120.4(8) . 3_565 ? C29 C28 H28 119.8 . . ? C32 C28 H28 119.8 3_565 . ? C28 C29 C30 120.8(8) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C31 C30 C29 120.0(9) . . ? C31 C30 S1 121.6(7) . . ? C29 C30 S1 118.3(7) . . ? C30 C31 C32 120.9(8) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C28 C32 C32 120.1(10) 3_565 3_565 ? C28 C32 C31 122.1(7) 3_565 . ? C32 C32 C31 117.7(9) 3_565 . ? C1 N1 C5 115.6(7) . . ? C1 N1 Ag2 121.2(6) . . ? C5 N1 Ag2 123.2(6) . . ? C6 N2 C10 119.1(8) . . ? C6 N2 Ag2 121.5(6) . . ? C10 N2 Ag2 119.3(6) . . ? C17 N3 C13 117.7(9) . . ? C17 N3 Ag1 118.7(7) . . ? C13 N3 Ag1 123.6(7) . . ? C20 N4 C21 114.3(7) . . ? C20 N4 Ag1 124.1(6) . 1_565 ? C21 N4 Ag1 121.6(5) . 1_565 ? HW1A OW1 HW1B 108(6) . . ? HW2A OW2 HW2B 108(10) . . ? O3 S1 O2 113.0(4) . . ? O3 S1 O1 111.6(5) . . ? O2 S1 O1 113.5(4) . . ? O3 S1 C30 106.9(4) . . ? O2 S1 C30 105.1(4) . . ? O1 S1 C30 106.1(4) . . ? O6 S2 O5 112.9(6) . . ? O6 S2 O4 113.8(6) . . ? O5 S2 O4 111.2(6) . . ? O6 S2 C24 105.5(6) . . ? O5 S2 C24 107.1(6) . . ? O4 S2 C24 105.8(5) . . ? 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 N1 C1 C2 C3 -0.4(17) . . . . ? C1 C2 C3 C4 2.4(15) . . . . ? C1 C2 C3 C8C -174.8(9) . . . 1_545 ? C2 C3 C4 C5 -2.4(15) . . . . ? C8C C3 C4 C5 174.9(10) 1_545 . . . ? C3 C4 C5 N1 0.3(17) . . . . ? N2 C6 C7 C8C 2.1(16) . . . . ? C6 C7 C8C C9 -0.3(14) . . . . ? C6 C7 C8C C3 -179.9(9) . . . 1_565 ? C7 C8C C9 C10 -1.2(14) . . . . ? C3 C8C C9 C10 178.4(9) 1_565 . . . ? C8C C9 C10 N2 1.0(16) . . . . ? N3 C13 C14 C15 -1.5(17) . . . . ? C13 C14 C15 C16 2.1(15) . . . . ? C13 C14 C15 C18 -174.2(10) . . . . ? C14 C15 C16 C17 -0.1(14) . . . . ? C18 C15 C16 C17 176.2(9) . . . . ? C15 C16 C17 N3 -2.8(16) . . . . ? C14 C15 C18 C22 -154.7(10) . . . . ? C16 C15 C18 C22 29.2(14) . . . . ? C14 C15 C18 C19 23.5(14) . . . . ? C16 C15 C18 C19 -152.6(10) . . . . ? C22 C18 C19 C20 -1.0(15) . . . . ? C15 C18 C19 C20 -179.2(9) . . . . ? C18 C19 C20 N4 0.7(16) . . . . ? C19 C18 C22 C21 1.1(15) . . . . ? C15 C18 C22 C21 179.3(9) . . . . ? N4 C21 C22 C18 -0.9(16) . . . . ? C27 C23 C24 C25 3.8(15) 3_667 . . . ? C27 C23 C24 S2 -176.4(6) 3_667 . . . ? C23 C24 C25 C26 -3.2(19) . . . . ? S2 C24 C25 C26 177.0(9) . . . . ? C24 C25 C26 C27 0.2(17) . . . . ? C25 C26 C27 C27 1.4(18) . . . 3_667 ? C25 C26 C27 C23 -179.0(10) . . . 3_667 ? C32 C28 C29 C30 -1.7(13) 3_565 . . . ? C28 C29 C30 C31 1.8(13) . . . . ? C28 C29 C30 S1 177.5(7) . . . . ? C29 C30 C31 C32 -2.6(13) . . . . ? S1 C30 C31 C32 -178.1(6) . . . . ? C30 C31 C32 C28 -179.9(8) . . . 3_565 ? C30 C31 C32 C32 3.2(14) . . . 3_565 ? C2 C1 N1 C5 -1.6(15) . . . . ? C2 C1 N1 Ag2 179.3(8) . . . . ? C4 C5 N1 C1 1.7(16) . . . . ? C4 C5 N1 Ag2 -179.3(9) . . . . ? C7 C6 N2 C10 -2.4(15) . . . . ? C7 C6 N2 Ag2 -179.0(8) . . . . ? C9 C10 N2 C6 0.8(15) . . . . ? C9 C10 N2 Ag2 177.6(8) . . . . ? C16 C17 N3 C13 3.6(16) . . . . ? C16 C17 N3 Ag1 -176.1(8) . . . . ? C14 C13 N3 C17 -1.5(16) . . . . ? C14 C13 N3 Ag1 178.2(8) . . . . ? C19 C20 N4 C21 -0.5(15) . . . . ? C19 C20 N4 Ag1 177.7(8) . . . 1_565 ? C22 C21 N4 C20 0.6(15) . . . . ? C22 C21 N4 Ag1 -177.6(8) . . . 1_565 ? C31 C30 S1 O3 -112.0(8) . . . . ? C29 C30 S1 O3 72.5(8) . . . . ? C31 C30 S1 O2 127.7(8) . . . . ? C29 C30 S1 O2 -47.8(8) . . . . ? C31 C30 S1 O1 7.2(9) . . . . ? C29 C30 S1 O1 -168.4(7) . . . . ? C23 C24 S2 O6 137.8(9) . . . . ? C25 C24 S2 O6 -42.4(10) . . . . ? C23 C24 S2 O5 17.2(10) . . . . ? C25 C24 S2 O5 -162.9(9) . . . . ? C23 C24 S2 O4 -101.4(9) . . . . ? C25 C24 S2 O4 78.4(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OW1 HW1A O1 0.81(5) 2.07(5) 2.872(11) 169(13) 3_566 OW2 HW2A O5 0.86(5) 2.00(5) 2.858(13) 171(10) 2_646 OW2 HW2B O4 0.85(5) 2.00(5) 2.848(13) 174(14) 4_566 OW1 HW1B O3 0.83(5) 2.18(5) 3.000(11) 170(13) . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.260 _refine_diff_density_min -1.395 _refine_diff_density_rms 0.160 #===end data_compd10 _database_code_depnum_ccdc_archive 'CCDC 684632' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C10 H8 Ag N2), C10 H5 O9 S3, 5.5(H2 O) ' _chemical_formula_sum 'C40 H40 Ag3 N6 O14.50 S3' _chemical_formula_weight 1256.57 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' 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 c ' _symmetry_space_group_name_Hall 'C -2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 11.809(2) _cell_length_b 18.114(4) _cell_length_c 20.703(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.88(3) _cell_angle_gamma 90.00 _cell_volume 4405(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9032 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.446 _exptl_crystal_size_mid 0.251 _exptl_crystal_size_min 0.147 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2508 _exptl_absorpt_coefficient_mu 1.539 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.633 _exptl_absorpt_correction_T_max 0.778 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21313 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9032 _reflns_number_gt 8587 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+1.4494P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.415(18) _refine_ls_number_reflns 9032 _refine_ls_number_parameters 629 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0826 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.141 _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 1.11236(3) 0.747566(19) 0.347481(16) 0.03089(9) Uani 1 1 d . . . Ag2 Ag 1.02495(3) 0.76497(2) 0.594301(18) 0.03377(9) Uani 1 1 d . . . Ag3 Ag 0.24831(3) 0.75424(2) 0.132098(17) 0.03514(9) Uani 1 1 d . . . C1 C 0.7262(3) 0.48407(19) 0.39191(17) 0.0234(7) Uani 1 1 d . . . C2 C 0.7935(3) 0.48603(19) 0.33872(16) 0.0209(7) Uani 1 1 d . . . C3 C 0.7455(3) 0.47704(18) 0.27354(16) 0.0204(7) Uani 1 1 d . . . H3 H 0.6677 0.4687 0.2647 0.024 Uiso 1 1 calc R . . C4 C 0.8131(4) 0.48050(17) 0.22353(17) 0.0201(7) Uani 1 1 d . . . C5 C 0.9313(4) 0.4936(2) 0.23563(19) 0.0215(7) Uani 1 1 d . . . H5 H 0.9759 0.4969 0.2013 0.026 Uiso 1 1 calc R . . C6 C 0.9798(3) 0.50124(19) 0.29822(18) 0.0220(7) Uani 1 1 d . . . C7 C 0.9128(3) 0.49749(17) 0.35158(16) 0.0184(6) Uani 1 1 d . . . C8 C 0.9607(3) 0.5027(2) 0.41770(18) 0.0264(8) Uani 1 1 d . . . H8 H 1.0389 0.5088 0.4267 0.032 Uiso 1 1 calc R . . C9 C 0.8954(4) 0.4991(2) 0.46730(17) 0.0273(8) Uani 1 1 d . . . H9 H 0.9285 0.5018 0.5100 0.033 Uiso 1 1 calc R . . C10 C 0.7772(4) 0.4914(2) 0.45424(18) 0.0276(8) Uani 1 1 d . . . H10 H 0.7322 0.4911 0.4886 0.033 Uiso 1 1 calc R . . C11 C 1.3300(5) 0.7433(2) 0.5650(2) 0.0202(10) Uani 1 1 d . . . C12 C 1.2785(5) 0.8061(2) 0.5384(2) 0.0392(12) Uani 1 1 d . . . H12 H 1.2871 0.8506 0.5609 0.047 Uiso 1 1 calc R . . C13 C 1.2146(5) 0.8039(2) 0.4788(2) 0.0386(12) Uani 1 1 d . . . H13 H 1.1815 0.8474 0.4622 0.046 Uiso 1 1 calc R . . C14 C 1.2419(4) 0.6804(2) 0.4704(2) 0.0311(10) Uani 1 1 d . . . H14 H 1.2279 0.6364 0.4479 0.037 Uiso 1 1 calc R . . C15 C 1.3076(4) 0.6786(2) 0.5301(2) 0.0328(10) Uani 1 1 d . . . H15 H 1.3366 0.6339 0.5466 0.039 Uiso 1 1 calc R . . C16 C 1.4024(5) 0.7440(2) 0.6280(3) 0.0234(10) Uani 1 1 d . . . C17 C 1.4208(5) 0.8092(2) 0.6625(2) 0.0369(11) Uani 1 1 d . . . H17 H 1.3895 0.8532 0.6457 0.044 Uiso 1 1 calc R . . C18 C 1.4511(4) 0.6815(2) 0.6570(2) 0.0334(10) Uani 1 1 d . . . H18 H 1.4409 0.6363 0.6359 0.040 Uiso 1 1 calc R . . C19 C 1.4852(5) 0.8086(3) 0.7216(2) 0.0444(14) Uani 1 1 d . . . H19 H 1.4976 0.8534 0.7432 0.053 Uiso 1 1 calc R . . C20 C 1.5137(4) 0.6849(2) 0.7160(2) 0.0319(9) Uani 1 1 d . . . H20 H 1.5458 0.6415 0.7335 0.038 Uiso 1 1 calc R . . C21 C 0.6338(4) 0.6771(2) 0.2276(2) 0.0319(9) Uani 1 1 d . . . H21 H 0.5972 0.6335 0.2140 0.038 Uiso 1 1 calc R . . C22 C 0.6946(4) 0.6788(2) 0.28814(19) 0.0267(8) Uani 1 1 d . . . H22 H 0.6976 0.6373 0.3147 0.032 Uiso 1 1 calc R . . C23 C 0.7514(5) 0.7431(2) 0.3092(2) 0.0231(10) Uani 1 1 d . . . C24 C 0.7428(4) 0.8040(2) 0.26807(19) 0.0258(8) Uani 1 1 d . . . H24 H 0.7786 0.8482 0.2805 0.031 Uiso 1 1 calc R . . C25 C 0.6800(4) 0.7973(2) 0.20843(19) 0.0283(8) Uani 1 1 d . . . H25 H 0.6754 0.8379 0.1809 0.034 Uiso 1 1 calc R . . C26 C 0.8767(4) 0.8164(2) 0.4702(2) 0.0326(9) Uani 1 1 d . . . H26 H 0.8782 0.8608 0.4927 0.039 Uiso 1 1 calc R . . C27 C 0.8215(4) 0.8139(2) 0.4096(2) 0.0295(9) Uani 1 1 d . . . H27 H 0.7884 0.8566 0.3913 0.035 Uiso 1 1 calc R . . C28 C 0.8134(4) 0.7482(2) 0.3743(2) 0.0194(8) Uani 1 1 d . . . C29 C 0.8694(4) 0.6870(2) 0.4049(2) 0.0316(10) Uani 1 1 d . . . H29 H 0.8689 0.6419 0.3835 0.038 Uiso 1 1 calc R . . C30 C 0.9254(4) 0.6939(2) 0.4667(2) 0.0359(10) Uani 1 1 d . . . H30 H 0.9614 0.6527 0.4862 0.043 Uiso 1 1 calc R . . C31 C 0.3280(3) 0.6886(2) 0.26750(18) 0.0258(8) Uani 1 1 d . . . H31 H 0.2817 0.6493 0.2527 0.031 Uiso 1 1 calc R . . C32 C 0.3844(3) 0.6852(2) 0.32923(18) 0.0245(7) Uani 1 1 d . . . H32 H 0.3765 0.6436 0.3548 0.029 Uiso 1 1 calc R . . C33 C 0.4529(5) 0.7434(2) 0.3536(2) 0.0210(10) Uani 1 1 d . . . C34 C 0.4617(4) 0.8039(2) 0.31213(17) 0.0232(7) Uani 1 1 d . . . H34 H 0.5064 0.8443 0.3260 0.028 Uiso 1 1 calc R . . C35 C 0.4034(4) 0.8033(2) 0.25036(18) 0.0253(8) Uani 1 1 d . . . H35 H 0.4106 0.8438 0.2235 0.030 Uiso 1 1 calc R . . C36 C 0.6222(4) 0.6809(3) 0.5077(2) 0.0355(11) Uani 1 1 d . . . H36 H 0.6508 0.6371 0.5263 0.043 Uiso 1 1 calc R . . C37 C 0.5587(4) 0.6777(2) 0.4474(2) 0.0302(10) Uani 1 1 d . . . H37 H 0.5448 0.6327 0.4265 0.036 Uiso 1 1 calc R . . C38 C 0.5163(5) 0.7426(2) 0.4187(3) 0.0221(10) Uani 1 1 d . . . C39 C 0.5369(4) 0.8081(2) 0.4535(2) 0.0300(10) Uani 1 1 d . . . H39 H 0.5085 0.8527 0.4364 0.036 Uiso 1 1 calc R . . C40 C 0.5995(4) 0.8064(3) 0.5135(2) 0.0340(10) Uani 1 1 d . . . H40 H 0.6114 0.8504 0.5364 0.041 Uiso 1 1 calc R . . N1 N 0.6442(5) 0.7442(2) 0.5404(2) 0.0290(11) Uani 1 1 d . . . N2 N 0.3376(4) 0.74711(19) 0.2278(3) 0.0278(11) Uani 1 1 d . . . N3 N 0.9295(5) 0.75755(19) 0.4993(2) 0.0279(10) Uani 1 1 d . . . N4 N 0.6252(4) 0.7352(2) 0.1879(2) 0.0270(9) Uani 1 1 d . . . N5 N 1.1982(5) 0.7424(2) 0.4441(3) 0.0277(10) Uani 1 1 d . . . N6 N 1.5314(4) 0.74798(18) 0.7501(2) 0.0240(10) Uani 1 1 d . . . O1 O 0.6366(3) 0.4587(2) 0.14125(14) 0.0448(8) Uani 1 1 d . . . O2 O 0.8121(3) 0.40123(16) 0.12054(14) 0.0350(7) Uani 1 1 d . . . O3 O 0.7908(4) 0.53212(17) 0.10787(14) 0.0496(10) Uani 1 1 d . . . O4 O 1.1658(3) 0.5244(2) 0.24552(16) 0.0450(8) Uani 1 1 d . . . O5 O 1.1786(3) 0.46028(16) 0.34943(17) 0.0417(8) Uani 1 1 d . . . O6 O 1.1384(3) 0.59121(15) 0.34316(15) 0.0345(7) Uani 1 1 d . . . O7 O 0.5364(3) 0.4777(2) 0.44383(14) 0.0414(8) Uani 1 1 d . . . O8 O 0.5327(2) 0.52895(16) 0.33592(14) 0.0330(6) Uani 1 1 d . . . O9 O 0.5597(3) 0.39750(17) 0.35176(15) 0.0359(7) Uani 1 1 d . . . OW1 O 0.8299(7) 0.9004(4) 0.6309(3) 0.051(2) Uani 0.50 1 d PD . . OW2 O 0.3101(4) 0.5077(3) 0.4616(2) 0.0668(13) Uani 1 1 d D . . OW3 O 1.0480(3) 0.39053(18) 0.09395(18) 0.0451(8) Uani 1 1 d D . . OW5 O 1.0452(5) 0.9166(3) 0.5669(3) 0.096(2) Uani 1 1 d D . . OW6 O 0.3873(4) 0.4940(4) 0.2213(2) 0.0757(15) Uani 1 1 d D . . S1 S 1.12863(8) 0.52085(5) 0.31019(5) 0.0285(2) Uani 1 1 d . . . S2 S 0.75790(9) 0.46700(5) 0.14165(4) 0.02449(18) Uani 1 1 d . . . S3 S 0.57638(8) 0.47077(5) 0.37927(4) 0.02532(19) Uani 1 1 d . . . OW4 O 1.1712(5) 0.5109(4) 0.0608(3) 0.0921(17) Uani 1 1 d D . . H2A H 0.277(8) 0.482(5) 0.424(4) 0.138 Uiso 1 1 d D . . H2B H 0.369(6) 0.482(5) 0.469(5) 0.138 Uiso 1 1 d D . . H3A H 1.080(7) 0.424(5) 0.072(5) 0.138 Uiso 1 1 d D . . H3B H 0.970(5) 0.406(6) 0.075(5) 0.138 Uiso 1 1 d D . . H4A H 1.202(8) 0.499(6) 0.022(3) 0.138 Uiso 1 1 d D . . H4B H 1.238(6) 0.525(6) 0.084(4) 0.138 Uiso 1 1 d D . . H6A H 0.314(4) 0.495(6) 0.226(5) 0.138 Uiso 1 1 d D . . H6B H 0.415(8) 0.515(6) 0.258(3) 0.138 Uiso 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 0.03512(19) 0.03884(17) 0.01606(16) -0.00131(11) -0.01017(13) -0.00247(12) Ag2 0.03620(18) 0.04101(16) 0.02155(15) 0.00120(15) -0.00940(12) -0.00202(16) Ag3 0.03382(19) 0.0525(2) 0.01653(16) 0.00104(13) -0.00999(14) -0.00322(14) C1 0.031(2) 0.0185(15) 0.0203(16) -0.0018(12) -0.0005(15) -0.0008(13) C2 0.0251(17) 0.0141(15) 0.0223(16) -0.0008(11) -0.0027(14) 0.0009(12) C3 0.0266(18) 0.0174(15) 0.0168(15) 0.0008(12) 0.0001(13) -0.0015(13) C4 0.0320(18) 0.0146(13) 0.0124(13) 0.0005(12) -0.0047(13) -0.0007(14) C5 0.0259(17) 0.0196(15) 0.0192(15) -0.0012(12) 0.0031(13) -0.0023(13) C6 0.0219(17) 0.0171(15) 0.0258(17) -0.0051(13) -0.0031(14) -0.0009(12) C7 0.0244(17) 0.0119(14) 0.0185(15) 0.0008(11) 0.0001(13) -0.0019(12) C8 0.032(2) 0.0188(16) 0.0263(18) -0.0039(13) -0.0074(16) -0.0025(13) C9 0.041(2) 0.0243(17) 0.0150(15) -0.0019(13) -0.0047(15) -0.0034(15) C10 0.039(2) 0.0268(17) 0.0167(16) -0.0013(13) 0.0010(16) -0.0056(16) C11 0.026(2) 0.0187(18) 0.015(2) -0.0017(13) -0.0027(18) -0.0021(13) C12 0.058(3) 0.024(2) 0.030(2) -0.0047(17) -0.021(2) 0.0060(19) C13 0.057(3) 0.026(2) 0.028(2) 0.0001(17) -0.021(2) 0.0077(19) C14 0.046(3) 0.0228(19) 0.0212(19) -0.0053(15) -0.0134(18) -0.0008(17) C15 0.048(3) 0.0211(19) 0.026(2) -0.0029(15) -0.0089(19) 0.0029(18) C16 0.026(2) 0.024(2) 0.019(3) 0.0007(15) -0.0023(19) 0.0017(15) C17 0.059(3) 0.0186(19) 0.028(2) 0.0011(16) -0.020(2) 0.0034(18) C18 0.050(3) 0.0184(18) 0.028(2) -0.0075(15) -0.0118(19) 0.0096(17) C19 0.067(3) 0.025(2) 0.034(2) -0.0003(18) -0.030(2) -0.003(2) C20 0.043(2) 0.029(2) 0.0219(19) 0.0005(15) -0.0076(18) 0.0115(17) C21 0.036(2) 0.027(2) 0.030(2) -0.0017(16) -0.0076(17) -0.0016(16) C22 0.040(2) 0.0182(17) 0.0207(17) 0.0029(14) -0.0045(16) -0.0047(15) C23 0.030(3) 0.0197(18) 0.019(2) -0.0007(14) 0.0017(18) 0.0016(15) C24 0.029(2) 0.0222(18) 0.0252(19) 0.0017(14) -0.0036(16) 0.0016(15) C25 0.034(2) 0.031(2) 0.0203(18) 0.0062(15) 0.0044(16) 0.0049(17) C26 0.045(3) 0.0250(19) 0.0265(19) -0.0044(15) -0.0013(18) 0.0034(17) C27 0.040(2) 0.0192(18) 0.0268(19) 0.0049(15) -0.0080(17) 0.0024(15) C28 0.022(2) 0.0219(17) 0.012(2) 0.0006(13) -0.0076(17) -0.0001(13) C29 0.045(3) 0.0206(18) 0.0255(19) -0.0015(14) -0.0165(18) 0.0058(16) C30 0.046(3) 0.024(2) 0.034(2) 0.0024(16) -0.0134(19) 0.0083(17) C31 0.0249(19) 0.0299(19) 0.0219(17) 0.0001(14) -0.0017(15) -0.0068(14) C32 0.0266(19) 0.0254(18) 0.0203(16) 0.0021(13) -0.0036(14) -0.0034(14) C33 0.030(2) 0.0171(17) 0.015(2) 0.0012(13) -0.002(2) 0.0034(14) C34 0.031(2) 0.0205(17) 0.0167(16) 0.0006(13) -0.0018(15) 0.0005(14) C35 0.036(2) 0.0190(17) 0.0197(17) 0.0017(13) -0.0051(16) 0.0017(14) C36 0.046(3) 0.032(2) 0.026(2) 0.0055(17) -0.0075(19) 0.0097(19) C37 0.041(2) 0.0218(19) 0.0249(19) -0.0005(16) -0.0096(18) 0.0051(17) C38 0.026(2) 0.0227(19) 0.016(2) 0.0009(14) -0.0024(18) -0.0013(14) C39 0.045(3) 0.0212(19) 0.022(2) -0.0023(14) -0.0090(18) 0.0036(16) C40 0.044(3) 0.025(2) 0.029(2) -0.0030(16) -0.0118(19) 0.0036(18) N1 0.034(3) 0.039(2) 0.012(2) -0.0003(13) -0.0094(19) 0.0030(14) N2 0.028(3) 0.028(2) 0.025(3) 0.0019(14) -0.005(2) 0.0036(13) N3 0.031(2) 0.0271(17) 0.024(3) 0.0036(14) -0.0053(19) 0.0015(15) N4 0.028(2) 0.0298(19) 0.023(2) 0.0010(14) 0.0003(17) 0.0015(14) N5 0.035(2) 0.0263(18) 0.019(2) -0.0010(13) -0.0123(18) -0.0022(14) N6 0.031(3) 0.0281(19) 0.010(2) 0.0024(11) -0.0119(17) 0.0003(12) O1 0.0351(17) 0.072(2) 0.0248(14) -0.0031(14) -0.0100(13) -0.0014(15) O2 0.0507(19) 0.0287(14) 0.0236(13) -0.0080(11) -0.0051(12) 0.0017(13) O3 0.099(3) 0.0294(15) 0.0183(13) 0.0059(11) -0.0057(15) -0.0145(16) O4 0.0284(16) 0.066(2) 0.0414(18) -0.0059(16) 0.0076(14) -0.0101(15) O5 0.0354(17) 0.0275(14) 0.059(2) 0.0000(14) -0.0101(15) 0.0080(12) O6 0.0326(16) 0.0223(12) 0.0449(17) -0.0018(11) -0.0131(14) -0.0071(10) O7 0.0379(18) 0.063(2) 0.0248(14) -0.0062(14) 0.0085(13) -0.0036(15) O8 0.0307(15) 0.0363(15) 0.0316(14) 0.0045(12) 0.0009(12) 0.0046(12) O9 0.0404(17) 0.0316(15) 0.0357(16) -0.0053(12) 0.0034(13) -0.0073(13) OW1 0.106(7) 0.033(3) 0.015(3) 0.007(2) 0.006(3) 0.005(4) OW2 0.054(3) 0.070(3) 0.072(3) -0.025(2) -0.010(2) 0.024(2) OW3 0.050(2) 0.0379(16) 0.0446(18) 0.0009(15) -0.0106(16) 0.0088(14) OW5 0.119(5) 0.070(3) 0.090(3) 0.017(3) -0.042(3) -0.038(3) OW6 0.051(3) 0.128(4) 0.047(2) -0.016(3) 0.0021(19) 0.028(3) S1 0.0222(5) 0.0265(4) 0.0358(5) -0.0027(4) -0.0023(4) -0.0029(3) S2 0.0370(5) 0.0235(4) 0.0119(3) 0.0007(3) -0.0027(3) -0.0028(4) S3 0.0275(5) 0.0272(4) 0.0216(4) -0.0006(3) 0.0043(3) -0.0019(3) OW4 0.082(4) 0.085(4) 0.108(5) 0.019(3) 0.001(3) -0.002(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 N6 2.141(5) 4_464 ? Ag1 N5 2.150(5) . ? Ag2 N4 2.164(5) 4_565 ? Ag2 N3 2.169(5) . ? Ag3 N2 2.151(5) . ? Ag3 N1 2.153(5) 4_464 ? C1 C10 1.373(5) . ? C1 C2 1.423(5) . ? C1 S3 1.778(4) . ? C2 C3 1.419(5) . ? C2 C7 1.422(5) . ? C3 C4 1.372(5) . ? C3 H3 0.9300 . ? C4 C5 1.412(6) . ? C4 S2 1.770(4) . ? C5 C6 1.369(5) . ? C5 H5 0.9300 . ? C6 C7 1.425(5) . ? C6 S1 1.786(4) . ? C7 C8 1.430(5) . ? C8 C9 1.348(6) . ? C8 H8 0.9300 . ? C9 C10 1.401(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.379(6) . ? C11 C15 1.389(6) . ? C11 C16 1.483(6) . ? C12 C13 1.379(6) . ? C12 H12 0.9300 . ? C13 N5 1.329(6) . ? C13 H13 0.9300 . ? C14 N5 1.328(6) . ? C14 C15 1.390(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C18 1.379(6) . ? C16 C17 1.386(6) . ? C17 C19 1.373(6) . ? C17 H17 0.9300 . ? C18 C20 1.362(6) . ? C18 H18 0.9300 . ? C19 N6 1.337(6) . ? C19 H19 0.9300 . ? C20 N6 1.350(6) . ? C20 H20 0.9300 . ? C21 N4 1.334(6) . ? C21 C22 1.379(5) . ? C21 H21 0.9300 . ? C22 C23 1.391(6) . ? C22 H22 0.9300 . ? C23 C24 1.390(6) . ? C23 C28 1.469(6) . ? C24 C25 1.379(5) . ? C24 H24 0.9300 . ? C25 N4 1.345(6) . ? C25 H25 0.9300 . ? C26 N3 1.346(6) . ? C26 C27 1.353(6) . ? C26 H26 0.9300 . ? C27 C28 1.394(6) . ? C27 H27 0.9300 . ? C28 C29 1.408(6) . ? C29 C30 1.385(6) . ? C29 H29 0.9300 . ? C30 N3 1.334(6) . ? C30 H30 0.9300 . ? C31 N2 1.353(6) . ? C31 C32 1.380(5) . ? C31 H31 0.9300 . ? C32 C33 1.392(6) . ? C32 H32 0.9300 . ? C33 C34 1.402(5) . ? C33 C38 1.475(6) . ? C34 C35 1.389(5) . ? C34 H34 0.9300 . ? C35 N2 1.335(6) . ? C35 H35 0.9300 . ? C36 N1 1.343(7) . ? C36 C37 1.392(6) . ? C36 H36 0.9300 . ? C37 C38 1.386(6) . ? C37 H37 0.9300 . ? C38 C39 1.398(6) . ? C39 C40 1.379(6) . ? C39 H39 0.9300 . ? C40 N1 1.341(6) . ? C40 H40 0.9300 . ? N1 Ag3 2.153(5) 4_565 ? N4 Ag2 2.164(5) 4_464 ? N6 Ag1 2.141(5) 4_565 ? O1 S2 1.439(4) . ? O2 S2 1.441(3) . ? O3 S2 1.445(3) . ? O4 S1 1.453(3) . ? O5 S1 1.454(3) . ? O6 S1 1.445(3) . ? O7 S3 1.468(3) . ? O8 S3 1.445(3) . ? O9 S3 1.450(3) . ? OW2 H2A 0.96(5) . ? OW2 H2B 0.83(5) . ? OW3 H3A 0.87(5) . ? OW3 H3B 1.00(5) . ? OW6 H6A 0.88(5) . ? OW6 H6B 0.88(5) . ? OW4 H4A 0.95(5) . ? OW4 H4B 0.91(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 N6 Ag1 N5 178.3(2) 4_464 . ? N4 Ag2 N3 176.0(1) 4_565 . ? N2 Ag3 N1 174.0(2) . 4_464 ? C10 C1 C2 119.9(4) . . ? C10 C1 S3 119.0(3) . . ? C2 C1 S3 121.1(3) . . ? C3 C2 C7 119.1(3) . . ? C3 C2 C1 122.2(3) . . ? C7 C2 C1 118.7(3) . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 121.0(3) . . ? C3 C4 S2 122.1(3) . . ? C5 C4 S2 117.0(3) . . ? C6 C5 C4 119.6(4) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 121.2(3) . . ? C5 C6 S1 117.5(3) . . ? C7 C6 S1 121.2(3) . . ? C2 C7 C6 118.7(3) . . ? C2 C7 C8 118.4(3) . . ? C6 C7 C8 122.9(3) . . ? C9 C8 C7 121.7(4) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C10 119.7(3) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C1 C10 C9 121.5(4) . . ? C1 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C12 C11 C15 115.9(5) . . ? C12 C11 C16 122.3(4) . . ? C15 C11 C16 121.8(4) . . ? C11 C12 C13 120.8(4) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? N5 C13 C12 123.0(4) . . ? N5 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? N5 C14 C15 122.9(4) . . ? N5 C14 H14 118.6 . . ? C15 C14 H14 118.6 . . ? C14 C15 C11 120.1(4) . . ? C14 C15 H15 119.9 . . ? C11 C15 H15 119.9 . . ? C18 C16 C17 116.0(5) . . ? C18 C16 C11 123.5(4) . . ? C17 C16 C11 120.4(4) . . ? C19 C17 C16 119.8(4) . . ? C19 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C20 C18 C16 121.1(4) . . ? C20 C18 H18 119.4 . . ? C16 C18 H18 119.4 . . ? N6 C19 C17 124.4(4) . . ? N6 C19 H19 117.8 . . ? C17 C19 H19 117.8 . . ? N6 C20 C18 123.3(4) . . ? N6 C20 H20 118.4 . . ? C18 C20 H20 118.4 . . ? N4 C21 C22 122.8(4) . . ? N4 C21 H21 118.6 . . ? C22 C21 H21 118.6 . . ? C21 C22 C23 119.6(4) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C24 C23 C22 117.9(4) . . ? C24 C23 C28 120.7(3) . . ? C22 C23 C28 121.3(3) . . ? C25 C24 C23 118.6(4) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? N4 C25 C24 123.7(4) . . ? N4 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? N3 C26 C27 123.1(4) . . ? N3 C26 H26 118.5 . . ? C27 C26 H26 118.5 . . ? C26 C27 C28 121.0(4) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C27 C28 C29 115.6(4) . . ? C27 C28 C23 122.4(3) . . ? C29 C28 C23 122.0(3) . . ? C30 C29 C28 120.2(4) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? N3 C30 C29 122.3(4) . . ? N3 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? N2 C31 C32 122.3(4) . . ? N2 C31 H31 118.8 . . ? C32 C31 H31 118.8 . . ? C31 C32 C33 120.6(4) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C32 C33 C34 116.6(4) . . ? C32 C33 C38 123.0(4) . . ? C34 C33 C38 120.4(4) . . ? C35 C34 C33 119.7(4) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? N2 C35 C34 123.0(4) . . ? N2 C35 H35 118.5 . . ? C34 C35 H35 118.5 . . ? N1 C36 C37 123.1(4) . . ? N1 C36 H36 118.5 . . ? C37 C36 H36 118.5 . . ? C38 C37 C36 119.1(4) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C37 C38 C39 117.7(5) . . ? C37 C38 C33 121.8(4) . . ? C39 C38 C33 120.5(4) . . ? C40 C39 C38 119.6(4) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? N1 C40 C39 123.0(4) . . ? N1 C40 H40 118.5 . . ? C39 C40 H40 118.5 . . ? C40 N1 C36 117.5(5) . . ? C40 N1 Ag3 121.3(3) . 4_565 ? C36 N1 Ag3 121.3(3) . 4_565 ? C35 N2 C31 117.8(4) . . ? C35 N2 Ag3 119.3(3) . . ? C31 N2 Ag3 122.9(3) . . ? C30 N3 C26 117.8(5) . . ? C30 N3 Ag2 120.1(4) . . ? C26 N3 Ag2 122.1(3) . . ? C21 N4 C25 117.4(4) . . ? C21 N4 Ag2 123.5(3) . 4_464 ? C25 N4 Ag2 119.1(3) . 4_464 ? C14 N5 C13 117.2(5) . . ? C14 N5 Ag1 123.0(3) . . ? C13 N5 Ag1 119.7(3) . . ? C19 N6 C20 115.4(5) . . ? C19 N6 Ag1 120.5(3) . 4_565 ? C20 N6 Ag1 123.8(3) . 4_565 ? H2A OW2 H2B 98(4) . . ? H3A OW3 H3B 92(4) . . ? H6A OW6 H6B 100(5) . . ? O6 S1 O4 112.3(2) . . ? O6 S1 O5 113.17(18) . . ? O4 S1 O5 113.9(2) . . ? O6 S1 C6 105.73(17) . . ? O4 S1 C6 105.50(19) . . ? O5 S1 C6 105.36(18) . . ? O1 S2 O2 112.6(2) . . ? O1 S2 O3 113.5(2) . . ? O2 S2 O3 112.2(2) . . ? O1 S2 C4 106.76(19) . . ? O2 S2 C4 105.87(17) . . ? O3 S2 C4 105.07(17) . . ? O8 S3 O9 113.47(18) . . ? O8 S3 O7 112.1(2) . . ? O9 S3 O7 113.1(2) . . ? O8 S3 C1 106.21(17) . . ? O9 S3 C1 105.94(18) . . ? O7 S3 C1 105.24(18) . . ? H4A OW4 H4B 96(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 C10 C1 C2 C3 178.5(3) . . . . ? S3 C1 C2 C3 -0.5(5) . . . . ? C10 C1 C2 C7 -1.6(5) . . . . ? S3 C1 C2 C7 179.4(3) . . . . ? C7 C2 C3 C4 -1.0(5) . . . . ? C1 C2 C3 C4 178.9(3) . . . . ? C2 C3 C4 C5 -0.5(5) . . . . ? C2 C3 C4 S2 178.1(3) . . . . ? C3 C4 C5 C6 1.5(5) . . . . ? S2 C4 C5 C6 -177.2(3) . . . . ? C4 C5 C6 C7 -1.0(5) . . . . ? C4 C5 C6 S1 -177.9(3) . . . . ? C3 C2 C7 C6 1.4(5) . . . . ? C1 C2 C7 C6 -178.5(3) . . . . ? C3 C2 C7 C8 -176.9(3) . . . . ? C1 C2 C7 C8 3.2(5) . . . . ? C5 C6 C7 C2 -0.4(5) . . . . ? S1 C6 C7 C2 176.3(3) . . . . ? C5 C6 C7 C8 177.8(3) . . . . ? S1 C6 C7 C8 -5.4(5) . . . . ? C2 C7 C8 C9 -1.8(5) . . . . ? C6 C7 C8 C9 179.9(3) . . . . ? C7 C8 C9 C10 -1.1(5) . . . . ? C2 C1 C10 C9 -1.4(6) . . . . ? S3 C1 C10 C9 177.6(3) . . . . ? C8 C9 C10 C1 2.8(6) . . . . ? C15 C11 C12 C13 -3.6(9) . . . . ? C16 C11 C12 C13 177.9(5) . . . . ? C11 C12 C13 N5 0.4(10) . . . . ? N5 C14 C15 C11 0.1(8) . . . . ? C12 C11 C15 C14 3.3(8) . . . . ? C16 C11 C15 C14 -178.2(4) . . . . ? C12 C11 C16 C18 177.3(6) . . . . ? C15 C11 C16 C18 -1.1(7) . . . . ? C12 C11 C16 C17 0.1(7) . . . . ? C15 C11 C16 C17 -178.3(6) . . . . ? C18 C16 C17 C19 0.7(9) . . . . ? C11 C16 C17 C19 178.1(5) . . . . ? C17 C16 C18 C20 -0.4(9) . . . . ? C11 C16 C18 C20 -177.7(5) . . . . ? C16 C17 C19 N6 -1.5(10) . . . . ? C16 C18 C20 N6 0.8(9) . . . . ? N4 C21 C22 C23 -1.0(7) . . . . ? C21 C22 C23 C24 0.9(7) . . . . ? C21 C22 C23 C28 177.6(4) . . . . ? C22 C23 C24 C25 -0.9(7) . . . . ? C28 C23 C24 C25 -177.6(4) . . . . ? C23 C24 C25 N4 0.8(7) . . . . ? N3 C26 C27 C28 2.0(8) . . . . ? C26 C27 C28 C29 -2.2(7) . . . . ? C26 C27 C28 C23 178.2(5) . . . . ? C24 C23 C28 C27 29.6(7) . . . . ? C22 C23 C28 C27 -147.0(5) . . . . ? C24 C23 C28 C29 -149.9(5) . . . . ? C22 C23 C28 C29 33.6(7) . . . . ? C27 C28 C29 C30 1.5(7) . . . . ? C23 C28 C29 C30 -178.9(5) . . . . ? C28 C29 C30 N3 -0.5(8) . . . . ? N2 C31 C32 C33 1.1(7) . . . . ? C31 C32 C33 C34 -0.7(6) . . . . ? C31 C32 C33 C38 -179.2(5) . . . . ? C32 C33 C34 C35 0.0(6) . . . . ? C38 C33 C34 C35 178.6(4) . . . . ? C33 C34 C35 N2 0.3(7) . . . . ? N1 C36 C37 C38 0.5(8) . . . . ? C36 C37 C38 C39 -2.1(8) . . . . ? C36 C37 C38 C33 177.1(5) . . . . ? C32 C33 C38 C37 32.0(8) . . . . ? C34 C33 C38 C37 -146.5(5) . . . . ? C32 C33 C38 C39 -148.8(5) . . . . ? C34 C33 C38 C39 32.7(8) . . . . ? C37 C38 C39 C40 1.3(8) . . . . ? C33 C38 C39 C40 -177.9(5) . . . . ? C38 C39 C40 N1 1.1(8) . . . . ? C39 C40 N1 C36 -2.6(9) . . . . ? C39 C40 N1 Ag3 176.9(4) . . . 4_565 ? C37 C36 N1 C40 1.8(9) . . . . ? C37 C36 N1 Ag3 -177.7(4) . . . 4_565 ? C34 C35 N2 C31 0.0(7) . . . . ? C34 C35 N2 Ag3 178.4(3) . . . . ? C32 C31 N2 C35 -0.7(7) . . . . ? C32 C31 N2 Ag3 -179.0(3) . . . . ? C29 C30 N3 C26 0.1(8) . . . . ? C29 C30 N3 Ag2 -177.4(4) . . . . ? C27 C26 N3 C30 -0.8(8) . . . . ? C27 C26 N3 Ag2 176.6(4) . . . . ? C22 C21 N4 C25 0.9(7) . . . . ? C22 C21 N4 Ag2 -177.6(4) . . . 4_464 ? C24 C25 N4 C21 -0.8(7) . . . . ? C24 C25 N4 Ag2 177.7(4) . . . 4_464 ? C15 C14 N5 C13 -3.4(9) . . . . ? C15 C14 N5 Ag1 173.1(4) . . . . ? C12 C13 N5 C14 3.2(9) . . . . ? C12 C13 N5 Ag1 -173.4(5) . . . . ? C17 C19 N6 C20 1.8(9) . . . . ? C17 C19 N6 Ag1 -172.3(5) . . . 4_565 ? C18 C20 N6 C19 -1.5(9) . . . . ? C18 C20 N6 Ag1 172.4(4) . . . 4_565 ? C5 C6 S1 O6 119.2(3) . . . . ? C7 C6 S1 O6 -57.6(3) . . . . ? C5 C6 S1 O4 0.1(3) . . . . ? C7 C6 S1 O4 -176.7(3) . . . . ? C5 C6 S1 O5 -120.7(3) . . . . ? C7 C6 S1 O5 62.5(3) . . . . ? C3 C4 S2 O1 4.3(3) . . . . ? C5 C4 S2 O1 -177.1(3) . . . . ? C3 C4 S2 O2 -115.9(3) . . . . ? C5 C4 S2 O2 62.7(3) . . . . ? C3 C4 S2 O3 125.1(3) . . . . ? C5 C4 S2 O3 -56.2(3) . . . . ? C10 C1 S3 O8 124.2(3) . . . . ? C2 C1 S3 O8 -56.8(3) . . . . ? C10 C1 S3 O9 -114.8(3) . . . . ? C2 C1 S3 O9 64.2(3) . . . . ? C10 C1 S3 O7 5.2(4) . . . . ? C2 C1 S3 O7 -175.8(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OW2 H2A O5 0.96(5) 1.87(5) 2.794(5) 160(9) 1_455 OW2 H2B O7 0.83(5) 2.10(9) 2.788(6) 140(11) . OW3 H3B O2 1.00(5) 2.18(8) 2.901(5) 128(7) . OW3 H3A OW4 0.87(5) 1.93(6) 2.747(7) 156(10) . OW4 H4A OW2 0.95(5) 1.87(7) 2.777(9) 158(9) 2_664 OW6 H6A O4 0.88(5) 1.91(6) 2.768(6) 163(10) 1_455 OW6 H6B O8 0.88(5) 2.03(6) 2.853(6) 154(10) . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.263 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.129 #===end