# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_email JIANFANGMA@YAHOO.COM.CN _publ_section_title ; Syntheses, Structures, and Photoluminescence of a Series of Silver(I) Sulfonates with Pyrazine Derivatives ; loop_ _publ_author_name 'Jian-Fang Ma.' 'Hai-Yan Liu.' 'Ying-Ying Liu.' 'Hua Wu.' 'Jin Yang.' # Attachment 'crystals.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 724281' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H14 Ag N3 O4 S' _chemical_formula_sum 'C11 H14 Ag N3 O4 S' _chemical_formula_weight 392.18 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 7.038(3) _cell_length_b 13.778(5) _cell_length_c 13.841(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.026(19) _cell_angle_gamma 90.00 _cell_volume 1332.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3036 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.348 _exptl_crystal_size_mid 0.282 _exptl_crystal_size_min 0.143 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.956 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 1.686 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.585 _exptl_absorpt_correction_T_max 0.782 _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 R-AXIS RAPID' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12669 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3036 _reflns_number_gt 2671 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO (Rigaku, 1998)' _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1990)' _computing_publication_material SHELXL97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.6645P] 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 3036 _refine_ls_number_parameters 197 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0811 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.167 _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 0.15813(3) 0.264533(18) 0.718859(14) 0.03866(10) Uani 1 1 d . . . C1 C 0.3483(3) 0.34152(17) 0.36650(16) 0.0225(5) Uani 1 1 d . . . C2 C 0.2984(4) 0.25287(18) 0.32290(19) 0.0269(5) Uani 1 1 d . . . H2 H 0.2695 0.2483 0.2557 0.032 Uiso 1 1 calc R . . C3 C 0.2924(4) 0.17120(18) 0.38093(18) 0.0287(5) Uani 1 1 d . . . H3 H 0.2575 0.1119 0.3520 0.034 Uiso 1 1 calc R . . C4 C 0.3372(3) 0.17603(18) 0.48101(18) 0.0261(5) Uani 1 1 d . . . C5 C 0.3931(3) 0.26522(17) 0.52379(17) 0.0236(5) Uani 1 1 d . . . C6 C 0.3958(3) 0.34850(18) 0.46634(16) 0.0240(5) Uani 1 1 d . . . H6 H 0.4293 0.4082 0.4949 0.029 Uiso 1 1 calc R . . C7 C 0.3267(4) 0.0867(2) 0.5425(2) 0.0375(6) Uani 1 1 d . . . H7A H 0.3621 0.1029 0.6097 0.056 Uiso 0.50 1 calc PRD . . H7B H 0.4128 0.0384 0.5232 0.056 Uiso 0.50 1 calc PR . . H7C H 0.1984 0.0617 0.5338 0.056 Uiso 0.50 1 calc PR . . H7D H 0.2868 0.0325 0.5014 0.056 Uiso 0.50 1 calc PR . . H7E H 0.2360 0.0970 0.5880 0.056 Uiso 0.50 1 calc PR . . H7F H 0.4505 0.0736 0.5773 0.056 Uiso 0.50 1 calc PR . . C8 C -0.0698(4) 0.3395(2) 0.5181(2) 0.0354(6) Uani 1 1 d . . . H8 H -0.0249 0.3986 0.5442 0.042 Uiso 1 1 calc R . . C9 C -0.1413(4) 0.3352(2) 0.4208(2) 0.0358(6) Uani 1 1 d . . . H9 H -0.1441 0.3915 0.3836 0.043 Uiso 1 1 calc R . . C10 C -0.2021(4) 0.1752(2) 0.43699(18) 0.0312(5) Uani 1 1 d . . . H10 H -0.2487 0.1163 0.4113 0.037 Uiso 1 1 calc R . . C11 C -0.1307(4) 0.1802(2) 0.53410(18) 0.0318(6) Uani 1 1 d . . . H11 H -0.1299 0.1242 0.5717 0.038 Uiso 1 1 calc R . . N1 N 0.4375(3) 0.27221(18) 0.62575(16) 0.0302(5) Uani 1 1 d D . . H2A H 0.507(4) 0.2254(14) 0.647(3) 0.049(11) Uiso 1 1 d D . . H2B H 0.498(4) 0.3240(16) 0.640(2) 0.034(8) Uiso 1 1 d D . . N2 N -0.0627(3) 0.26190(16) 0.57613(16) 0.0309(5) Uani 1 1 d . . . N3 N -0.2065(3) 0.25286(15) 0.37869(16) 0.0286(5) Uani 1 1 d . . . O1 O 0.1805(3) 0.43893(16) 0.22214(14) 0.0393(5) Uani 1 1 d . . . O2 O 0.3639(3) 0.52992(14) 0.35170(14) 0.0426(5) Uani 1 1 d . . . O3 O 0.5239(3) 0.43234(15) 0.24012(14) 0.0380(4) Uani 1 1 d . . . O1W O 0.1413(3) 0.44920(18) 0.7263(2) 0.0504(6) Uani 1 1 d D . . H1A H 0.238(4) 0.484(3) 0.738(3) 0.066(13) Uiso 1 1 d D . . H1B H 0.044(5) 0.484(3) 0.744(3) 0.093(16) Uiso 1 1 d D . . S1 S 0.35489(9) 0.44459(5) 0.29032(4) 0.02581(14) 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 0.04555(15) 0.04844(16) 0.01997(12) -0.00043(8) -0.00415(9) -0.00555(9) C1 0.0213(10) 0.0271(12) 0.0189(10) 0.0011(9) 0.0019(8) -0.0006(9) C2 0.0283(12) 0.0325(13) 0.0192(11) -0.0041(9) -0.0005(10) -0.0027(9) C3 0.0310(12) 0.0259(12) 0.0287(12) -0.0069(10) 0.0017(10) -0.0024(10) C4 0.0250(11) 0.0260(12) 0.0273(12) 0.0013(10) 0.0031(9) 0.0010(9) C5 0.0215(11) 0.0311(12) 0.0181(11) -0.0003(9) 0.0016(9) -0.0004(9) C6 0.0252(11) 0.0264(11) 0.0199(11) -0.0038(9) 0.0013(9) -0.0038(9) C7 0.0454(16) 0.0281(13) 0.0379(14) 0.0071(12) 0.0013(12) 0.0011(11) C8 0.0413(15) 0.0310(13) 0.0318(14) 0.0014(11) -0.0032(11) -0.0032(11) C9 0.0425(15) 0.0328(14) 0.0305(13) 0.0089(11) -0.0016(11) 0.0001(11) C10 0.0363(13) 0.0311(13) 0.0254(12) 0.0016(10) 0.0000(10) -0.0045(11) C11 0.0362(13) 0.0341(14) 0.0246(12) 0.0065(10) 0.0016(10) -0.0037(11) N1 0.0346(12) 0.0354(12) 0.0196(10) 0.0007(9) -0.0008(9) -0.0032(10) N2 0.0305(11) 0.0391(12) 0.0220(11) 0.0021(9) -0.0009(9) -0.0010(9) N3 0.0301(11) 0.0352(12) 0.0198(10) 0.0044(8) 0.0005(8) 0.0022(8) O1 0.0384(11) 0.0421(11) 0.0338(10) 0.0059(8) -0.0101(9) 0.0021(8) O2 0.0696(14) 0.0276(10) 0.0302(10) -0.0039(8) 0.0044(10) -0.0034(9) O3 0.0392(11) 0.0439(11) 0.0330(10) 0.0033(9) 0.0122(8) -0.0058(9) O1W 0.0415(13) 0.0359(12) 0.0735(17) -0.0063(11) 0.0058(12) -0.0025(10) S1 0.0311(3) 0.0262(3) 0.0194(3) 0.0007(2) -0.0002(2) -0.0017(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 N3 2.312(2) 4_666 ? Ag1 N2 2.360(2) . ? Ag1 N1 2.481(3) . ? Ag1 O1W 2.550(3) . ? C1 C6 1.385(3) . ? C1 C2 1.388(3) . ? C1 S1 1.773(2) . ? C2 C3 1.386(4) . ? C2 H2 0.9300 . ? C3 C4 1.384(3) . ? C3 H3 0.9300 . ? C4 C5 1.399(3) . ? C4 C7 1.503(4) . ? C5 C6 1.397(3) . ? C5 N1 1.411(3) . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C7 H7D 0.9600 . ? C7 H7E 0.9600 . ? C7 H7F 0.9600 . ? C8 N2 1.334(3) . ? C8 C9 1.380(4) . ? C8 H8 0.9300 . ? C9 N3 1.332(4) . ? C9 H9 0.9300 . ? C10 N3 1.338(3) . ? C10 C11 1.378(4) . ? C10 H10 0.9300 . ? C11 N2 1.329(4) . ? C11 H11 0.9300 . ? N1 H2A 0.84(2) . ? N1 H2B 0.84(2) . ? N3 Ag1 2.312(2) 4_565 ? O1 S1 1.4559(19) . ? O2 S1 1.447(2) . ? O3 S1 1.459(2) . ? O1W H1A 0.83(3) . ? O1W H1B 0.89(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 N3 Ag1 N2 162.13(8) 4_666 . ? N3 Ag1 N1 103.97(8) 4_666 . ? N2 Ag1 N1 92.78(8) . . ? N3 Ag1 O1W 94.62(8) 4_666 . ? N2 Ag1 O1W 91.15(8) . . ? N1 Ag1 O1W 91.28(8) . . ? C6 C1 C2 120.8(2) . . ? C6 C1 S1 121.15(19) . . ? C2 C1 S1 118.02(18) . . ? C3 C2 C1 119.1(2) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C4 C3 C2 121.4(2) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 118.9(2) . . ? C3 C4 C7 120.4(2) . . ? C5 C4 C7 120.7(2) . . ? C6 C5 C4 120.2(2) . . ? C6 C5 N1 119.8(2) . . ? C4 C5 N1 120.0(2) . . ? C1 C6 C5 119.5(2) . . ? C1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C7 H7D 109.5 . . ? H7A C7 H7D 141.1 . . ? H7B C7 H7D 56.3 . . ? H7C C7 H7D 56.3 . . ? C4 C7 H7E 109.5 . . ? H7A C7 H7E 56.3 . . ? H7B C7 H7E 141.1 . . ? H7C C7 H7E 56.3 . . ? H7D C7 H7E 109.5 . . ? C4 C7 H7F 109.5 . . ? H7A C7 H7F 56.3 . . ? H7B C7 H7F 56.3 . . ? H7C C7 H7F 141.1 . . ? H7D C7 H7F 109.5 . . ? H7E C7 H7F 109.5 . . ? N2 C8 C9 122.4(3) . . ? N2 C8 H8 118.8 . . ? C9 C8 H8 118.8 . . ? N3 C9 C8 121.9(3) . . ? N3 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? N3 C10 C11 121.8(3) . . ? N3 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? N2 C11 C10 122.5(2) . . ? N2 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? C5 N1 Ag1 115.11(16) . . ? C5 N1 H2A 110(2) . . ? Ag1 N1 H2A 105(2) . . ? C5 N1 H2B 109(2) . . ? Ag1 N1 H2B 109(2) . . ? H2A N1 H2B 108(3) . . ? C11 N2 C8 115.5(2) . . ? C11 N2 Ag1 122.98(18) . . ? C8 N2 Ag1 117.63(18) . . ? C9 N3 C10 115.8(2) . . ? C9 N3 Ag1 125.94(18) . 4_565 ? C10 N3 Ag1 118.08(18) . 4_565 ? Ag1 O1W H1A 123(3) . . ? Ag1 O1W H1B 126(3) . . ? H1A O1W H1B 106(4) . . ? O2 S1 O1 113.39(13) . . ? O2 S1 O3 113.19(13) . . ? O1 S1 O3 110.90(12) . . ? O2 S1 C1 107.70(12) . . ? O1 S1 C1 105.15(12) . . ? O3 S1 C1 105.82(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 C6 C1 C2 C3 1.5(4) . . . . ? S1 C1 C2 C3 179.97(19) . . . . ? C1 C2 C3 C4 -0.8(4) . . . . ? C2 C3 C4 C5 -1.2(4) . . . . ? C2 C3 C4 C7 179.1(2) . . . . ? C3 C4 C5 C6 2.6(4) . . . . ? C7 C4 C5 C6 -177.7(2) . . . . ? C3 C4 C5 N1 179.3(2) . . . . ? C7 C4 C5 N1 -1.0(4) . . . . ? C2 C1 C6 C5 -0.1(4) . . . . ? S1 C1 C6 C5 -178.56(18) . . . . ? C4 C5 C6 C1 -2.0(4) . . . . ? N1 C5 C6 C1 -178.7(2) . . . . ? N2 C8 C9 N3 -0.5(5) . . . . ? N3 C10 C11 N2 0.4(4) . . . . ? C6 C5 N1 Ag1 103.7(2) . . . . ? C4 C5 N1 Ag1 -73.0(3) . . . . ? N3 Ag1 N1 C5 169.00(17) 4_666 . . . ? N2 Ag1 N1 C5 -4.72(19) . . . . ? O1W Ag1 N1 C5 -95.93(19) . . . . ? C10 C11 N2 C8 0.6(4) . . . . ? C10 C11 N2 Ag1 -156.6(2) . . . . ? C9 C8 N2 C11 -0.5(4) . . . . ? C9 C8 N2 Ag1 158.0(2) . . . . ? N3 Ag1 N2 C11 -66.5(4) 4_666 . . . ? N1 Ag1 N2 C11 93.3(2) . . . . ? O1W Ag1 N2 C11 -175.4(2) . . . . ? N3 Ag1 N2 C8 136.8(3) 4_666 . . . ? N1 Ag1 N2 C8 -63.5(2) . . . . ? O1W Ag1 N2 C8 27.9(2) . . . . ? C8 C9 N3 C10 1.4(4) . . . . ? C8 C9 N3 Ag1 177.2(2) . . . 4_565 ? C11 C10 N3 C9 -1.4(4) . . . . ? C11 C10 N3 Ag1 -177.5(2) . . . 4_565 ? C6 C1 S1 O2 -15.1(2) . . . . ? C2 C1 S1 O2 166.4(2) . . . . ? C6 C1 S1 O1 -136.3(2) . . . . ? C2 C1 S1 O1 45.2(2) . . . . ? C6 C1 S1 O3 106.3(2) . . . . ? C2 C1 S1 O3 -72.2(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 N1 H2B O2 0.84(2) 2.23(2) 3.062(3) 169(3) 3_666 O1W H1B O1 0.89(3) 2.01(3) 2.900(3) 177(5) 3_566 O1W H1A O3 0.83(3) 2.03(3) 2.858(3) 177(4) 3_666 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.703 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.085 #=====================================end data_2 _database_code_depnum_ccdc_archive 'CCDC 724282' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H16 Ag N3 O3 S' _chemical_formula_sum 'C13 H16 Ag N3 O3 S' _chemical_formula_weight 402.22 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 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 11.717(3) _cell_length_b 14.333(5) _cell_length_c 17.265(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2899.5(14) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2834 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 1.547 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.79 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25991 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3313 _reflns_number_gt 2834 _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^)+(0.0335P)^2^+2.8360P] 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 3313 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.053768(16) 0.463700(14) 0.121721(12) 0.03628(8) Uani 1 1 d . . . S1 S 0.48061(5) 0.19558(4) 0.07630(3) 0.02608(13) Uani 1 1 d . . . O1 O 0.60450(15) 0.19666(13) 0.07423(12) 0.0387(4) Uani 1 1 d . . . O3 O 0.43797(16) 0.15517(13) 0.14812(11) 0.0388(4) Uani 1 1 d . . . N1 N 0.18799(18) 0.45879(15) 0.02514(13) 0.0278(4) Uani 1 1 d . . . H1N H 0.180(2) 0.5176(19) 0.0067(15) 0.023(6) Uiso 1 1 d . . . H2N H 0.163(2) 0.418(2) -0.0051(16) 0.029(7) Uiso 1 1 d . . . N3 N -0.31023(18) 0.44989(14) 0.27101(12) 0.0296(4) Uani 1 1 d . . . O2 O 0.42940(18) 0.15260(13) 0.00855(11) 0.0401(4) Uani 1 1 d . . . C4 C 0.3749(2) 0.50264(16) 0.07762(14) 0.0282(5) Uani 1 1 d . . . C9 C -0.2607(2) 0.37061(16) 0.24868(13) 0.0256(4) Uani 1 1 d . . . N2 N -0.12179(18) 0.45133(14) 0.17398(12) 0.0297(4) Uani 1 1 d . . . C1 C 0.43858(19) 0.31462(16) 0.07627(13) 0.0246(4) Uani 1 1 d . . . C11 C -0.2668(2) 0.52938(17) 0.24360(15) 0.0342(5) Uani 1 1 d . . . H11 H -0.3016 0.5855 0.2566 0.041 Uiso 1 1 calc R . . C5 C 0.30032(19) 0.43426(15) 0.04942(13) 0.0233(4) Uani 1 1 d . . . C10 C -0.1726(2) 0.53062(17) 0.19704(16) 0.0357(6) Uani 1 1 d . . . H10 H -0.1429 0.5876 0.1809 0.043 Uiso 1 1 calc R . . C6 C 0.33268(19) 0.34060(15) 0.04764(13) 0.0246(4) Uani 1 1 d . . . H6 H 0.2835 0.2959 0.0274 0.030 Uiso 1 1 calc R . . C8 C -0.1670(2) 0.37076(16) 0.19832(13) 0.0252(4) Uani 1 1 d . . . C7 C 0.3432(2) 0.60382(18) 0.07631(18) 0.0424(7) Uani 1 1 d . . . H7A H 0.2680 0.6107 0.0551 0.064 Uiso 1 1 calc R . . H7B H 0.3968 0.6375 0.0449 0.064 Uiso 1 1 calc R . . H7C H 0.3445 0.6281 0.1281 0.064 Uiso 1 1 calc R . . C3 C 0.4798(2) 0.47386(18) 0.10589(18) 0.0379(6) Uani 1 1 d . . . H3 H 0.5302 0.5183 0.1251 0.045 Uiso 1 1 calc R . . C13 C -0.3079(2) 0.28144(17) 0.27981(17) 0.0378(6) Uani 1 1 d . . . H13A H -0.3714 0.2947 0.3132 0.057 Uiso 1 1 calc R . . H13B H -0.2499 0.2494 0.3086 0.057 Uiso 1 1 calc R . . H13C H -0.3329 0.2429 0.2376 0.057 Uiso 1 1 calc R . . C2 C 0.5121(2) 0.38075(19) 0.10638(16) 0.0344(5) Uani 1 1 d . . . H2 H 0.5823 0.3630 0.1267 0.041 Uiso 1 1 calc R . . C12 C -0.1172(2) 0.28115(17) 0.16962(17) 0.0379(6) Uani 1 1 d . . . H12A H -0.0541 0.2943 0.1359 0.057 Uiso 1 1 calc R . . H12B H -0.1744 0.2469 0.1417 0.057 Uiso 1 1 calc R . . H12C H -0.0912 0.2447 0.2128 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02601(11) 0.03740(13) 0.04543(13) 0.00415(8) 0.00312(8) 0.00092(8) S1 0.0274(3) 0.0200(3) 0.0309(3) 0.0027(2) 0.0038(2) 0.0044(2) O1 0.0266(9) 0.0335(10) 0.0560(12) 0.0028(8) 0.0068(8) 0.0082(7) O3 0.0441(11) 0.0329(10) 0.0396(10) 0.0119(8) 0.0097(9) 0.0045(8) N1 0.0259(10) 0.0229(10) 0.0347(11) -0.0019(9) -0.0038(9) 0.0035(8) N3 0.0311(11) 0.0260(10) 0.0315(10) -0.0008(8) 0.0049(9) -0.0009(8) O2 0.0546(12) 0.0259(9) 0.0399(10) -0.0061(7) -0.0049(9) 0.0028(8) C4 0.0268(12) 0.0212(11) 0.0366(13) -0.0042(9) 0.0030(10) 0.0001(9) C9 0.0261(11) 0.0241(11) 0.0265(10) 0.0018(9) -0.0019(9) -0.0029(9) N2 0.0303(10) 0.0273(10) 0.0314(10) 0.0001(8) 0.0055(8) -0.0018(8) C1 0.0271(11) 0.0215(10) 0.0252(11) -0.0005(8) 0.0024(9) 0.0026(9) C11 0.0403(14) 0.0223(11) 0.0400(13) 0.0001(10) 0.0065(11) 0.0013(10) C5 0.0217(10) 0.0230(10) 0.0251(10) 0.0000(8) 0.0016(8) 0.0013(8) C10 0.0446(15) 0.0226(11) 0.0400(14) 0.0017(10) 0.0104(12) -0.0042(11) C6 0.0240(11) 0.0204(10) 0.0295(11) -0.0032(8) -0.0004(9) -0.0009(9) C8 0.0277(11) 0.0240(11) 0.0240(10) -0.0015(8) -0.0032(9) -0.0001(9) C7 0.0387(14) 0.0220(12) 0.0665(19) -0.0078(12) 0.0058(14) -0.0014(11) C3 0.0304(13) 0.0296(13) 0.0536(16) -0.0119(11) -0.0076(12) -0.0052(10) C13 0.0402(15) 0.0262(12) 0.0469(15) 0.0058(11) 0.0100(12) -0.0035(11) C2 0.0265(12) 0.0331(13) 0.0437(14) -0.0053(10) -0.0084(11) 0.0028(10) C12 0.0417(15) 0.0268(12) 0.0451(15) -0.0024(11) 0.0104(12) 0.0036(11) _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 2.253(2) . ? Ag1 N1 2.293(2) . ? Ag1 N3 2.451(2) 6_656 ? Ag1 O3 2.784(2) 7_665 ? S1 O2 1.4517(19) . ? S1 O1 1.4521(19) . ? S1 O3 1.4570(19) . ? S1 C1 1.776(2) . ? N1 C5 1.425(3) . ? N1 H1N 0.91(3) . ? N1 H2N 0.83(3) . ? N3 C9 1.333(3) . ? N3 C11 1.335(3) . ? N3 Ag1 2.451(2) 6_556 ? C4 C3 1.386(4) . ? C4 C5 1.400(3) . ? C4 C7 1.497(3) . ? C9 C8 1.400(3) . ? C9 C13 1.493(3) . ? N2 C8 1.338(3) . ? N2 C10 1.343(3) . ? C1 C2 1.382(3) . ? C1 C6 1.387(3) . ? C11 C10 1.366(4) . ? C11 H11 0.9300 . ? C5 C6 1.395(3) . ? C10 H10 0.9300 . ? C6 H6 0.9300 . ? C8 C12 1.495(3) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C3 C2 1.387(4) . ? C3 H3 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C2 H2 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? 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 156.19(8) . . ? N2 Ag1 N3 106.54(7) . 6_656 ? N1 Ag1 N3 95.80(8) . 6_656 ? N3 Ag1 O3 86.18(7) 6_656 7_665 ? N1 Ag1 O3 97.21(8) . 7_665 ? N2 Ag1 O3 92.51(8) . 7_665 ? O2 S1 O1 113.45(12) . . ? O2 S1 O3 112.04(12) . . ? O1 S1 O3 111.59(12) . . ? O2 S1 C1 107.03(11) . . ? O1 S1 C1 105.49(11) . . ? O3 S1 C1 106.68(11) . . ? C5 N1 Ag1 115.28(15) . . ? C5 N1 H1N 115.1(17) . . ? Ag1 N1 H1N 99.2(17) . . ? C5 N1 H2N 109.6(19) . . ? Ag1 N1 H2N 103.9(19) . . ? H1N N1 H2N 113(3) . . ? C9 N3 C11 117.3(2) . . ? C9 N3 Ag1 124.79(16) . 6_556 ? C11 N3 Ag1 116.55(16) . 6_556 ? C3 C4 C5 117.9(2) . . ? C3 C4 C7 120.9(2) . . ? C5 C4 C7 121.2(2) . . ? N3 C9 C8 121.3(2) . . ? N3 C9 C13 117.7(2) . . ? C8 C9 C13 121.0(2) . . ? C8 N2 C10 117.5(2) . . ? C8 N2 Ag1 123.72(16) . . ? C10 N2 Ag1 117.16(16) . . ? C2 C1 C6 120.5(2) . . ? C2 C1 S1 119.08(18) . . ? C6 C1 S1 120.42(17) . . ? N3 C11 C10 121.9(2) . . ? N3 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C6 C5 C4 120.8(2) . . ? C6 C5 N1 118.8(2) . . ? C4 C5 N1 120.4(2) . . ? N2 C10 C11 121.4(2) . . ? N2 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C1 C6 C5 119.6(2) . . ? C1 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? N2 C8 C9 120.4(2) . . ? N2 C8 C12 118.8(2) . . ? C9 C8 C12 120.7(2) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C3 C2 122.0(2) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C1 C2 C3 119.2(2) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? 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 N2 Ag1 N1 C5 -149.69(17) . . . . ? N3 Ag1 N1 C5 10.14(17) 6_656 . . . ? C11 N3 C9 C8 -0.2(3) . . . . ? Ag1 N3 C9 C8 -166.45(16) 6_556 . . . ? C11 N3 C9 C13 179.3(2) . . . . ? Ag1 N3 C9 C13 13.0(3) 6_556 . . . ? N1 Ag1 N2 C8 84.1(3) . . . . ? N3 Ag1 N2 C8 -74.9(2) 6_656 . . . ? N1 Ag1 N2 C10 -110.8(2) . . . . ? N3 Ag1 N2 C10 90.2(2) 6_656 . . . ? O2 S1 C1 C2 -148.1(2) . . . . ? O1 S1 C1 C2 -27.0(2) . . . . ? O3 S1 C1 C2 91.8(2) . . . . ? O2 S1 C1 C6 33.0(2) . . . . ? O1 S1 C1 C6 154.13(19) . . . . ? O3 S1 C1 C6 -87.1(2) . . . . ? C9 N3 C11 C10 -2.6(4) . . . . ? Ag1 N3 C11 C10 164.8(2) 6_556 . . . ? C3 C4 C5 C6 -2.1(4) . . . . ? C7 C4 C5 C6 177.1(2) . . . . ? C3 C4 C5 N1 175.2(2) . . . . ? C7 C4 C5 N1 -5.7(4) . . . . ? Ag1 N1 C5 C6 91.9(2) . . . . ? Ag1 N1 C5 C4 -85.4(2) . . . . ? C8 N2 C10 C11 0.0(4) . . . . ? Ag1 N2 C10 C11 -166.0(2) . . . . ? N3 C11 C10 N2 2.8(4) . . . . ? C2 C1 C6 C5 -0.1(3) . . . . ? S1 C1 C6 C5 178.82(17) . . . . ? C4 C5 C6 C1 1.9(3) . . . . ? N1 C5 C6 C1 -175.4(2) . . . . ? C10 N2 C8 C9 -2.8(3) . . . . ? Ag1 N2 C8 C9 162.28(16) . . . . ? C10 N2 C8 C12 176.1(2) . . . . ? Ag1 N2 C8 C12 -18.9(3) . . . . ? N3 C9 C8 N2 2.9(3) . . . . ? C13 C9 C8 N2 -176.5(2) . . . . ? N3 C9 C8 C12 -175.9(2) . . . . ? C13 C9 C8 C12 4.6(3) . . . . ? C5 C4 C3 C2 0.4(4) . . . . ? C7 C4 C3 C2 -178.8(3) . . . . ? C6 C1 C2 C3 -1.6(4) . . . . ? S1 C1 C2 C3 179.5(2) . . . . ? C4 C3 C2 C1 1.4(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 N1 H2N O1 0.83(3) 2.15(3) 2.977(3) 174(3) 3_455 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.700 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.102 #===========end data_3 _database_code_depnum_ccdc_archive 'CCDC 724283' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H16 Ag N3 O3 S, H2 O' _chemical_formula_sum 'C13 H18 Ag N3 O4 S' _chemical_formula_weight 420.23 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 26.532(5) _cell_length_b 8.8959(18) _cell_length_c 14.081(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.46(3) _cell_angle_gamma 90.00 _cell_volume 3152.3(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3208 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 1.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.82 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14181 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3619 _reflns_number_gt 3208 _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^)+(0.0400P)^2^+3.5636P] 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 3619 _refine_ls_number_parameters 213 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 0.132257(7) 0.67096(2) 0.072723(15) 0.03512(8) Uani 1 1 d . . . C8 C 0.04434(8) 0.4192(2) 0.02765(17) 0.0277(4) Uani 1 1 d . . . H8 H 0.0749 0.3603 0.0468 0.033 Uiso 1 1 calc R . . C9 C 0.00477(9) 0.6509(2) -0.00348(17) 0.0272(4) Uani 1 1 d . . . C10 C 0.23298(9) 0.6071(2) 0.00362(16) 0.0268(4) Uani 1 1 d . . . C11 C 0.22201(9) 0.8596(3) 0.02200(17) 0.0295(4) Uani 1 1 d . . . H11 H 0.2029 0.9385 0.0371 0.035 Uiso 1 1 calc R . . C14 C 0.21551(10) 0.4479(3) 0.00888(19) 0.0370(5) Uani 1 1 d . . . H14A H 0.1839 0.4470 0.0280 0.055 Uiso 1 1 calc R . . H14B H 0.2431 0.3935 0.0575 0.055 Uiso 1 1 calc R . . H14C H 0.2084 0.4012 -0.0555 0.055 Uiso 1 1 calc R . . C15 C 0.00890(11) 0.8183(3) -0.0065(3) 0.0444(6) Uani 1 1 d . . . H15A H 0.0457 0.8469 0.0125 0.067 Uiso 1 1 calc R . . H15B H -0.0072 0.8621 0.0391 0.067 Uiso 1 1 calc R . . H15C H -0.0091 0.8533 -0.0732 0.067 Uiso 1 1 calc R . . N1 N 0.17036(8) 1.5635(2) 0.24108(16) 0.0309(4) Uani 1 1 d . . . HN1 H 0.1656(11) 1.641(3) 0.274(2) 0.026(6) Uiso 1 1 d . . . HN2 H 0.2027(12) 1.547(3) 0.246(2) 0.034(7) Uiso 1 1 d . . . N2 N 0.20478(7) 0.7188(2) 0.02598(14) 0.0279(4) Uani 1 1 d . . . N3 N 0.04944(7) 0.5689(2) 0.02447(14) 0.0271(4) Uani 1 1 d . . . OW1 O 0.11417(16) 1.8568(3) 0.4774(2) 0.0921(11) Uani 1 1 d D . . H1A H 0.126(2) 1.891(6) 0.433(3) 0.138 Uiso 1 1 d D . . H2A H 0.123(2) 1.928(4) 0.520(3) 0.138 Uiso 1 1 d D . . C1 C 0.14063(9) 1.1611(2) 0.25979(16) 0.0255(4) Uani 1 1 d . . . C2 C 0.09428(10) 1.1680(3) 0.28583(19) 0.0335(5) Uani 1 1 d . . . H2 H 0.0771 1.0806 0.2948 0.040 Uiso 1 1 calc R . . C3 C 0.07443(10) 1.3075(3) 0.29810(19) 0.0341(5) Uani 1 1 d . . . H3 H 0.0436 1.3125 0.3161 0.041 Uiso 1 1 calc R . . C4 C 0.09854(9) 1.4402(3) 0.28466(16) 0.0291(4) Uani 1 1 d . . . C5 C 0.14562(8) 1.4314(2) 0.25918(15) 0.0253(4) Uani 1 1 d . . . C6 C 0.16637(9) 1.2917(2) 0.24711(16) 0.0248(4) Uani 1 1 d . . . H6 H 0.1976 1.2859 0.2305 0.030 Uiso 1 1 calc R . . C7 C 0.07550(11) 1.5911(3) 0.2965(2) 0.0397(6) Uani 1 1 d . . . H7A H 0.0437 1.5770 0.3140 0.059 Uiso 1 1 calc R . . H7B H 0.0673 1.6456 0.2347 0.059 Uiso 1 1 calc R . . H7C H 0.1009 1.6468 0.3485 0.059 Uiso 1 1 calc R . . O1 O 0.13008(7) 0.93468(18) 0.14046(13) 0.0392(4) Uani 1 1 d . . . O2 O 0.21884(7) 1.0064(2) 0.23777(16) 0.0444(4) Uani 1 1 d . . . O3 O 0.16160(9) 0.8855(2) 0.31819(14) 0.0431(4) Uani 1 1 d . . . S1 S 0.16517(2) 0.98331(6) 0.23842(4) 0.02653(12) 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 0.02542(10) 0.03277(11) 0.04994(13) 0.00000(7) 0.01585(8) -0.00645(7) C8 0.0232(10) 0.0228(10) 0.0365(11) -0.0015(8) 0.0084(9) 0.0015(8) C9 0.0286(11) 0.0188(9) 0.0348(11) -0.0021(8) 0.0110(9) -0.0015(8) C10 0.0267(10) 0.0271(10) 0.0256(10) -0.0008(8) 0.0068(8) -0.0010(8) C11 0.0271(11) 0.0287(11) 0.0346(11) -0.0012(9) 0.0124(9) 0.0032(9) C14 0.0390(13) 0.0310(12) 0.0404(13) -0.0012(10) 0.0119(11) -0.0083(10) C15 0.0392(14) 0.0207(11) 0.0721(19) -0.0017(11) 0.0159(13) -0.0030(10) N1 0.0294(10) 0.0213(9) 0.0430(11) -0.0009(8) 0.0126(9) -0.0001(8) N2 0.0234(9) 0.0304(9) 0.0317(9) 0.0002(7) 0.0114(7) -0.0010(7) N3 0.0232(8) 0.0239(8) 0.0342(10) -0.0032(7) 0.0090(7) -0.0041(7) OW1 0.142(3) 0.0783(18) 0.085(2) -0.0391(15) 0.077(2) -0.0647(19) C1 0.0278(10) 0.0229(10) 0.0258(10) -0.0028(8) 0.0086(8) -0.0005(8) C2 0.0313(12) 0.0312(12) 0.0417(13) -0.0028(9) 0.0167(10) -0.0081(9) C3 0.0281(11) 0.0380(12) 0.0407(13) -0.0040(10) 0.0174(10) -0.0014(9) C4 0.0267(10) 0.0305(11) 0.0293(10) -0.0040(9) 0.0078(9) 0.0036(9) C5 0.0267(10) 0.0238(10) 0.0233(9) -0.0009(8) 0.0050(8) -0.0003(8) C6 0.0241(10) 0.0227(9) 0.0279(10) -0.0003(8) 0.0089(8) -0.0013(8) C7 0.0373(13) 0.0354(13) 0.0481(14) -0.0064(11) 0.0162(11) 0.0069(11) O1 0.0460(10) 0.0289(8) 0.0374(9) -0.0090(7) 0.0058(8) -0.0010(7) O2 0.0331(9) 0.0341(9) 0.0697(13) -0.0076(8) 0.0216(9) -0.0001(7) O3 0.0625(12) 0.0273(8) 0.0438(10) 0.0057(7) 0.0228(9) 0.0033(8) S1 0.0296(3) 0.0195(2) 0.0309(3) -0.00212(19) 0.0102(2) -0.0016(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 2.2625(18) . ? Ag1 N3 2.2736(18) . ? Ag1 N1 2.457(2) 1_545 ? Ag1 O1 2.5400(17) . ? C8 N3 1.340(3) . ? C8 C9 1.386(3) 5_565 ? C8 H8 0.9300 . ? C9 N3 1.341(3) . ? C9 C8 1.386(3) 5_565 ? C9 C15 1.494(3) . ? C10 N2 1.340(3) . ? C10 C11 1.384(3) 7_565 ? C10 C14 1.500(3) . ? C11 N2 1.341(3) . ? C11 C10 1.384(3) 7_565 ? C11 H11 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? N1 C5 1.408(3) . ? N1 Ag1 2.457(2) 1_565 ? N1 HN1 0.86(3) . ? N1 HN2 0.85(3) . ? OW1 H1A 0.84(5) . ? OW1 H2A 0.85(4) . ? C1 C6 1.388(3) . ? C1 C2 1.391(3) . ? C1 S1 1.772(2) . ? C2 C3 1.380(3) . ? C2 H2 0.9300 . ? C3 C4 1.384(3) . ? C3 H3 0.9300 . ? C4 C5 1.407(3) . ? C4 C7 1.506(3) . ? C5 C6 1.391(3) . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? O1 S1 1.4639(18) . ? O2 S1 1.4417(18) . ? O3 S1 1.4474(18) . ? 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 144.96(7) . . ? N2 Ag1 N1 103.06(7) . 1_545 ? N3 Ag1 N1 101.31(7) . 1_545 ? N2 Ag1 O1 93.33(7) . . ? N3 Ag1 O1 110.27(6) . . ? N1 Ag1 O1 92.78(6) 1_545 . ? N3 C8 C9 122.4(2) . 5_565 ? N3 C8 H8 118.8 . . ? C9 C8 H8 118.8 5_565 . ? N3 C9 C8 120.12(19) . 5_565 ? N3 C9 C15 119.0(2) . . ? C8 C9 C15 120.9(2) 5_565 . ? N2 C10 C11 119.6(2) . 7_565 ? N2 C10 C14 119.0(2) . . ? C11 C10 C14 121.4(2) 7_565 . ? N2 C11 C10 123.0(2) . 7_565 ? N2 C11 H11 118.5 . . ? C10 C11 H11 118.5 7_565 . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C5 N1 Ag1 115.24(14) . 1_565 ? C5 N1 HN1 114.6(17) . . ? Ag1 N1 HN1 96.8(17) 1_565 . ? C5 N1 HN2 110.8(19) . . ? Ag1 N1 HN2 104.1(19) 1_565 . ? HN1 N1 HN2 114(3) . . ? C10 N2 C11 117.38(19) . . ? C10 N2 Ag1 121.23(15) . . ? C11 N2 Ag1 121.37(15) . . ? C8 N3 C9 117.48(18) . . ? C8 N3 Ag1 119.01(15) . . ? C9 N3 Ag1 123.45(14) . . ? H1A OW1 H2A 100(5) . . ? C6 C1 C2 120.58(19) . . ? C6 C1 S1 120.22(17) . . ? C2 C1 S1 119.16(16) . . ? C3 C2 C1 118.5(2) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 122.6(2) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C3 C4 C5 118.2(2) . . ? C3 C4 C7 121.6(2) . . ? C5 C4 C7 120.2(2) . . ? C6 C5 C4 119.92(19) . . ? C6 C5 N1 119.9(2) . . ? C4 C5 N1 120.14(19) . . ? C1 C6 C5 120.1(2) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? S1 O1 Ag1 122.92(10) . . ? O2 S1 O3 113.47(12) . . ? O2 S1 O1 111.77(12) . . ? O3 S1 O1 112.04(11) . . ? O2 S1 C1 106.89(10) . . ? O3 S1 C1 106.67(10) . . ? O1 S1 C1 105.40(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C10 N2 C11 0.2(4) 7_565 . . . ? C14 C10 N2 C11 179.0(2) . . . . ? C11 C10 N2 Ag1 -178.21(16) 7_565 . . . ? C14 C10 N2 Ag1 0.6(3) . . . . ? C10 C11 N2 C10 -0.2(4) 7_565 . . . ? C10 C11 N2 Ag1 178.20(16) 7_565 . . . ? N3 Ag1 N2 C10 -61.8(2) . . . . ? N1 Ag1 N2 C10 71.18(17) 1_545 . . . ? O1 Ag1 N2 C10 164.81(17) . . . . ? N3 Ag1 N2 C11 119.93(18) . . . . ? N1 Ag1 N2 C11 -107.12(18) 1_545 . . . ? O1 Ag1 N2 C11 -13.49(18) . . . . ? C9 C8 N3 C9 -0.1(4) 5_565 . . . ? C9 C8 N3 Ag1 177.23(17) 5_565 . . . ? C8 C9 N3 C8 0.1(4) 5_565 . . . ? C15 C9 N3 C8 179.2(2) . . . . ? C8 C9 N3 Ag1 -177.11(16) 5_565 . . . ? C15 C9 N3 Ag1 2.0(3) . . . . ? N2 Ag1 N3 C8 78.9(2) . . . . ? N1 Ag1 N3 C8 -54.43(17) 1_545 . . . ? O1 Ag1 N3 C8 -151.70(16) . . . . ? N2 Ag1 N3 C9 -103.92(19) . . . . ? N1 Ag1 N3 C9 122.73(18) 1_545 . . . ? O1 Ag1 N3 C9 25.45(19) . . . . ? C6 C1 C2 C3 0.4(4) . . . . ? S1 C1 C2 C3 -177.30(19) . . . . ? C1 C2 C3 C4 0.6(4) . . . . ? C2 C3 C4 C5 -1.1(4) . . . . ? C2 C3 C4 C7 178.8(2) . . . . ? C3 C4 C5 C6 0.7(3) . . . . ? C7 C4 C5 C6 -179.2(2) . . . . ? C3 C4 C5 N1 177.6(2) . . . . ? C7 C4 C5 N1 -2.3(3) . . . . ? Ag1 N1 C5 C6 95.5(2) 1_565 . . . ? Ag1 N1 C5 C4 -81.4(2) 1_565 . . . ? C2 C1 C6 C5 -0.8(3) . . . . ? S1 C1 C6 C5 176.88(16) . . . . ? C4 C5 C6 C1 0.2(3) . . . . ? N1 C5 C6 C1 -176.7(2) . . . . ? N2 Ag1 O1 S1 -79.08(13) . . . . ? N3 Ag1 O1 S1 127.32(12) . . . . ? N1 Ag1 O1 S1 24.18(13) 1_545 . . . ? Ag1 O1 S1 O2 74.21(14) . . . . ? Ag1 O1 S1 O3 -54.41(15) . . . . ? Ag1 O1 S1 C1 -170.04(11) . . . . ? C6 C1 S1 O2 16.3(2) . . . . ? C2 C1 S1 O2 -166.05(19) . . . . ? C6 C1 S1 O3 137.94(19) . . . . ? C2 C1 S1 O3 -44.4(2) . . . . ? C6 C1 S1 O1 -102.80(19) . . . . ? C2 C1 S1 O1 74.9(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 N1 HN2 O2 0.85(3) 2.05(3) 2.904(3) 179(3) 4 OW1 H2A O1 0.85(4) 2.05(4) 2.876(3) 163(5) 6_586 OW1 H1A O3 0.84(5) 2.12(5) 2.909(3) 158(5) 1_565 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.720 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.093 #==============================================end data_4 _database_code_depnum_ccdc_archive 'CCDC 724284' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H18 Ag N3 O3 S' _chemical_formula_sum 'C14 H18 Ag N3 O3 S' _chemical_formula_weight 416.24 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 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 12.257(3) _cell_length_b 15.403(3) _cell_length_c 8.7304(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1648.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2987 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 1.364 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15432 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3689 _reflns_number_gt 2987 _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. H atoms bonded to N atom were located in a difference map and refined with distance restraints of N---H = 0.85+-0.01 \%A. ISOR has been applied to restrain the anisotropic U~ij~-values of the atoms (O3, O2' and O1) to behave more isotropically. ; _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^)+(0.0361P)^2^+1.2868P] 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 0.09(5) _refine_ls_number_reflns 3689 _refine_ls_number_parameters 235 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1012 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.056 _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 0.70784(3) 0.88187(2) 0.22668(7) 0.05669(13) Uani 1 1 d . . . C1 C 0.7273(4) 1.0387(3) 0.9832(5) 0.0400(11) Uani 1 1 d . . . C2 C 0.6778(4) 1.0282(3) 0.8395(6) 0.0386(10) Uani 1 1 d . . . H2 H 0.6050 1.0116 0.8344 0.046 Uiso 1 1 calc R . . C3 C 0.7345(4) 1.0420(3) 0.7064(6) 0.0440(11) Uani 1 1 d . A . C4 C 0.8435(5) 1.0677(4) 0.7141(8) 0.0600(13) Uani 1 1 d . . . H4 H 0.8827 1.0782 0.6248 0.072 Uiso 1 1 calc R . . C5 C 0.8923(5) 1.0773(4) 0.8543(7) 0.0595(15) Uani 1 1 d . . . H5 H 0.9655 1.0929 0.8584 0.071 Uiso 1 1 calc R . . C6 C 0.8364(5) 1.0646(4) 0.9893(6) 0.0498(12) Uani 1 1 d . . . C7 C 0.8924(6) 1.0745(5) 1.1433(8) 0.080(2) Uani 1 1 d . . . H7A H 0.8413 1.0621 1.2237 0.120 Uiso 1 1 calc R . . H7B H 0.9186 1.1329 1.1541 0.120 Uiso 1 1 calc R . . H7C H 0.9526 1.0349 1.1494 0.120 Uiso 1 1 calc R . . C8 C 0.4883(5) 0.7949(4) 0.3475(8) 0.0550(15) Uani 1 1 d . . . H8 H 0.5121 0.8213 0.4373 0.066 Uiso 1 1 calc R A . C9 C 0.3943(5) 0.7458(4) 0.3502(7) 0.0485(13) Uani 1 1 d . A . C10 C 0.3289(6) 0.7358(5) 0.4962(7) 0.0697(17) Uani 1 1 d . . . H10A H 0.2667 0.6994 0.4770 0.105 Uiso 1 1 calc R A . H10B H 0.3047 0.7918 0.5303 0.105 Uiso 1 1 calc R . . H10C H 0.3737 0.7097 0.5737 0.105 Uiso 1 1 calc R . . C11 C 0.4182(5) 0.7156(4) 0.0924(7) 0.0480(13) Uani 1 1 d . A . C12 C 0.3795(6) 0.6720(5) -0.0465(7) 0.0674(17) Uani 1 1 d . . . H12A H 0.3151 0.6391 -0.0232 0.101 Uiso 1 1 calc R . . H12B H 0.4353 0.6338 -0.0840 0.101 Uiso 1 1 calc R . . H12C H 0.3627 0.7146 -0.1232 0.101 Uiso 1 1 calc R . . C13 C 0.5722(7) 0.7852(5) -0.0539(8) 0.080(2) Uani 1 1 d . A . H13A H 0.6328 0.8227 -0.0323 0.120 Uiso 1 1 calc R . . H13B H 0.5252 0.8124 -0.1275 0.120 Uiso 1 1 calc R . . H13C H 0.5986 0.7312 -0.0945 0.120 Uiso 1 1 calc R . . C14 C 0.5100(6) 0.7684(4) 0.0905(7) 0.0509(14) Uani 1 1 d . . . N1 N 0.6691(4) 1.0189(3) 1.1172(5) 0.0493(11) Uani 1 1 d D . . N2 N 0.5459(3) 0.8055(3) 0.2199(8) 0.0560(10) Uani 1 1 d . A . N3 N 0.3600(3) 0.7051(2) 0.2245(7) 0.0481(8) Uani 1 1 d . . . S1 S 0.67330(14) 1.02402(11) 0.52555(15) 0.0545(4) Uani 1 1 d . . . O1 O 0.706(3) 0.9452(13) 0.475(2) 0.084(5) Uani 0.48(4) 1 d PU A 1 O2 O 0.5540(11) 1.029(2) 0.5519(15) 0.082(7) Uani 0.48(4) 1 d P A 1 O3 O 0.7066(19) 1.1007(19) 0.430(3) 0.066(5) Uani 0.48(4) 1 d PU A 1 O1' O 0.7572(15) 0.9637(9) 0.4520(15) 0.059(4) Uani 0.52(4) 1 d P A 2 O2' O 0.5749(16) 0.9768(17) 0.5550(14) 0.080(5) Uani 0.52(4) 1 d PU A 2 O3' O 0.666(2) 1.1001(15) 0.444(3) 0.070(5) Uani 0.52(4) 1 d P A 2 H1N H 0.686(3) 1.051(3) 1.193(4) 0.037(13) Uiso 1 1 d D . . H2N H 0.6000(10) 1.018(4) 1.114(7) 0.048(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 0.0616(2) 0.0601(2) 0.0484(2) -0.0084(3) -0.0005(3) -0.00026(18) C1 0.057(3) 0.041(3) 0.022(2) 0.002(2) -0.001(2) 0.001(2) C2 0.048(2) 0.039(2) 0.029(2) -0.001(2) -0.004(2) 0.003(2) C3 0.058(3) 0.047(2) 0.028(3) -0.004(2) 0.005(2) -0.0005(19) C4 0.072(3) 0.068(3) 0.040(3) 0.007(3) 0.007(4) -0.014(3) C5 0.061(3) 0.067(4) 0.051(3) -0.005(3) 0.004(3) -0.021(3) C6 0.060(3) 0.054(3) 0.036(3) -0.003(2) -0.006(2) -0.011(3) C7 0.075(4) 0.110(6) 0.056(4) -0.005(4) -0.023(3) -0.026(4) C8 0.062(4) 0.052(3) 0.050(3) -0.011(3) -0.006(3) 0.002(3) C9 0.056(3) 0.044(3) 0.046(3) 0.004(3) 0.002(3) 0.013(3) C10 0.092(4) 0.067(4) 0.050(4) 0.002(3) 0.011(3) -0.003(4) C11 0.058(3) 0.042(3) 0.044(3) -0.003(2) 0.001(2) 0.002(3) C12 0.084(4) 0.073(4) 0.046(3) -0.006(3) 0.005(3) -0.021(3) C13 0.099(5) 0.087(5) 0.054(4) -0.012(4) 0.025(4) -0.028(4) C14 0.055(3) 0.049(3) 0.049(3) -0.006(3) 0.002(3) -0.001(3) N1 0.060(3) 0.065(3) 0.0229(19) -0.001(2) 0.0007(19) -0.002(2) N2 0.056(2) 0.057(2) 0.055(2) -0.009(3) 0.013(3) -0.0023(18) N3 0.055(2) 0.0430(18) 0.046(2) 0.003(3) 0.000(3) 0.0033(15) S1 0.0725(9) 0.0657(9) 0.0254(6) -0.0070(7) -0.0009(7) 0.0067(8) O1 0.111(10) 0.075(7) 0.065(7) -0.017(6) -0.010(7) 0.018(7) O2 0.068(7) 0.136(19) 0.042(6) -0.014(8) -0.008(4) -0.003(8) O3 0.076(9) 0.082(8) 0.041(6) 0.002(5) 0.004(7) -0.003(8) O1' 0.065(8) 0.063(7) 0.048(5) -0.021(5) -0.007(5) 0.015(6) O2' 0.081(7) 0.112(10) 0.047(5) -0.005(6) -0.014(5) -0.028(7) O3' 0.089(13) 0.068(7) 0.051(7) 0.013(5) -0.002(9) 0.023(9) _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 2.296(4) 4_565 ? Ag1 N2 2.308(4) . ? Ag1 N1 2.366(5) 1_554 ? Ag1 O1 2.375(16) . ? Ag1 O1' 2.413(12) . ? C1 C6 1.396(8) . ? C1 C2 1.403(7) . ? C1 N1 1.403(6) . ? C2 C3 1.370(7) . ? C2 H2 0.9300 . ? C3 C4 1.395(7) . ? C3 S1 1.769(5) . ? C4 C5 1.370(9) . ? C4 H4 0.9300 . ? C5 C6 1.377(8) . ? C5 H5 0.9300 . ? C6 C7 1.517(8) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N2 1.329(9) . ? C8 C9 1.379(9) . ? C8 H8 0.9300 . ? C9 N3 1.332(8) . ? C9 C10 1.514(8) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N3 1.366(8) . ? C11 C14 1.389(10) . ? C11 C12 1.465(8) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.495(9) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N2 1.340(9) . ? N1 Ag1 2.366(5) 1_556 ? N1 H1N 0.85(4) . ? N1 H2N 0.847(10) . ? N3 Ag1 2.296(4) 4_465 ? S1 O1 1.353(16) . ? S1 O3' 1.37(2) . ? S1 O2' 1.432(13) . ? S1 O2 1.483(14) . ? S1 O3 1.50(3) . ? S1 O1' 1.527(13) . ? 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 N2 113.66(13) 4_565 . ? N3 Ag1 N1 132.86(17) 4_565 1_554 ? N2 Ag1 N1 105.75(18) . 1_554 ? N3 Ag1 O1 104.8(6) 4_565 . ? N2 Ag1 O1 102.9(8) . . ? N1 Ag1 O1 90.0(4) 1_554 . ? N3 Ag1 O1' 96.2(3) 4_565 . ? N2 Ag1 O1' 120.2(5) . . ? N1 Ag1 O1' 85.1(3) 1_554 . ? O1 Ag1 O1' 17.2(5) . . ? C6 C1 C2 118.7(5) . . ? C6 C1 N1 121.2(5) . . ? C2 C1 N1 120.0(5) . . ? C3 C2 C1 121.4(5) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C4 119.2(5) . . ? C2 C3 S1 121.2(4) . . ? C4 C3 S1 119.6(4) . . ? C5 C4 C3 119.5(6) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 122.1(5) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 119.0(5) . . ? C5 C6 C7 121.3(6) . . ? C1 C6 C7 119.7(5) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C9 121.7(6) . . ? N2 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? N3 C9 C8 120.5(5) . . ? N3 C9 C10 118.6(5) . . ? C8 C9 C10 120.9(6) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C14 120.2(5) . . ? N3 C11 C12 118.4(5) . . ? C14 C11 C12 121.4(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 C11 120.4(5) . . ? N2 C14 C13 118.0(6) . . ? C11 C14 C13 121.6(5) . . ? C1 N1 Ag1 115.3(4) . 1_556 ? C1 N1 H1N 113(3) . . ? Ag1 N1 H1N 99(3) 1_556 . ? C1 N1 H2N 119(4) . . ? Ag1 N1 H2N 101(4) 1_556 . ? H1N N1 H2N 107(5) . . ? C8 N2 C14 118.7(4) . . ? C8 N2 Ag1 119.9(5) . . ? C14 N2 Ag1 121.4(4) . . ? C9 N3 C11 118.4(4) . . ? C9 N3 Ag1 121.6(4) . 4_465 ? C11 N3 Ag1 120.0(4) . 4_465 ? O1 S1 O3' 127.8(12) . . ? O1 S1 O2' 81.5(9) . . ? O3' S1 O2' 118.4(10) . . ? O1 S1 O2 113.0(9) . . ? O3' S1 O2 88.5(10) . . ? O1 S1 O3 116.3(12) . . ? O2' S1 O3 136.8(10) . . ? O2 S1 O3 108.2(11) . . ? O3' S1 O1' 110.0(9) . . ? O2' S1 O1' 109.5(8) . . ? O2 S1 O1' 139.7(9) . . ? O3 S1 O1' 93.6(9) . . ? O1 S1 C3 107.9(8) . . ? O3' S1 C3 110.8(11) . . ? O2' S1 C3 106.0(5) . . ? O2 S1 C3 105.7(5) . . ? O3 S1 C3 104.8(10) . . ? O1' S1 C3 100.7(5) . . ? S1 O1 Ag1 132.1(10) . . ? S1 O1' Ag1 119.5(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.7(7) . . . . ? N1 C1 C2 C3 -176.0(5) . . . . ? C1 C2 C3 C4 -0.6(7) . . . . ? C1 C2 C3 S1 177.2(4) . . . . ? C2 C3 C4 C5 1.1(8) . . . . ? S1 C3 C4 C5 -176.7(5) . . . . ? C3 C4 C5 C6 -1.7(10) . . . . ? C4 C5 C6 C1 1.8(9) . . . . ? C4 C5 C6 C7 179.3(6) . . . . ? C2 C1 C6 C5 -1.2(8) . . . . ? N1 C1 C6 C5 175.4(6) . . . . ? C2 C1 C6 C7 -178.7(6) . . . . ? N1 C1 C6 C7 -2.1(8) . . . . ? N2 C8 C9 N3 2.0(8) . . . . ? N2 C8 C9 C10 -178.9(6) . . . . ? N3 C11 C14 N2 3.8(9) . . . . ? C12 C11 C14 N2 -178.0(6) . . . . ? N3 C11 C14 C13 -176.7(6) . . . . ? C12 C11 C14 C13 1.6(10) . . . . ? C6 C1 N1 Ag1 -76.9(6) . . . 1_556 ? C2 C1 N1 Ag1 99.7(5) . . . 1_556 ? C9 C8 N2 C14 1.1(9) . . . . ? C9 C8 N2 Ag1 -176.4(4) . . . . ? C11 C14 N2 C8 -3.9(9) . . . . ? C13 C14 N2 C8 176.5(6) . . . . ? C11 C14 N2 Ag1 173.5(5) . . . . ? C13 C14 N2 Ag1 -6.0(8) . . . . ? N3 Ag1 N2 C8 102.1(5) 4_565 . . . ? N1 Ag1 N2 C8 -104.3(5) 1_554 . . . ? O1 Ag1 N2 C8 -10.6(6) . . . . ? O1' Ag1 N2 C8 -10.9(6) . . . . ? N3 Ag1 N2 C14 -75.3(5) 4_565 . . . ? N1 Ag1 N2 C14 78.3(4) 1_554 . . . ? O1 Ag1 N2 C14 172.0(6) . . . . ? O1' Ag1 N2 C14 171.7(5) . . . . ? C8 C9 N3 C11 -2.2(8) . . . . ? C10 C9 N3 C11 178.8(5) . . . . ? C8 C9 N3 Ag1 177.4(4) . . . 4_465 ? C10 C9 N3 Ag1 -1.6(7) . . . 4_465 ? C14 C11 N3 C9 -0.7(8) . . . . ? C12 C11 N3 C9 -179.0(5) . . . . ? C14 C11 N3 Ag1 179.7(4) . . . 4_465 ? C12 C11 N3 Ag1 1.4(7) . . . 4_465 ? C2 C3 S1 O1 -99.2(15) . . . . ? C4 C3 S1 O1 78.6(15) . . . . ? C2 C3 S1 O3' 116.5(12) . . . . ? C4 C3 S1 O3' -65.8(12) . . . . ? C2 C3 S1 O2' -13.2(13) . . . . ? C4 C3 S1 O2' 164.6(13) . . . . ? C2 C3 S1 O2 22.0(15) . . . . ? C4 C3 S1 O2 -160.2(15) . . . . ? C2 C3 S1 O3 136.2(11) . . . . ? C4 C3 S1 O3 -46.0(11) . . . . ? C2 C3 S1 O1' -127.2(9) . . . . ? C4 C3 S1 O1' 50.6(9) . . . . ? O3' S1 O1 Ag1 -25(3) . . . . ? O2' S1 O1 Ag1 95(2) . . . . ? O2 S1 O1 Ag1 83(2) . . . . ? O3 S1 O1 Ag1 -43(3) . . . . ? O1' S1 O1 Ag1 -82(3) . . . . ? C3 S1 O1 Ag1 -160.9(19) . . . . ? N3 Ag1 O1 S1 146(2) 4_565 . . . ? N2 Ag1 O1 S1 -95(3) . . . . ? N1 Ag1 O1 S1 11(3) 1_554 . . . ? O1' Ag1 O1 S1 84(3) . . . . ? O1 S1 O1' Ag1 56.1(19) . . . . ? O3' S1 O1' Ag1 -78.7(12) . . . . ? O2' S1 O1' Ag1 53.0(10) . . . . ? O2 S1 O1' Ag1 34.0(14) . . . . ? O3 S1 O1' Ag1 -89.8(12) . . . . ? C3 S1 O1' Ag1 164.4(8) . . . . ? N3 Ag1 O1' S1 -169.8(11) 4_565 . . . ? N2 Ag1 O1' S1 -47.8(12) . . . . ? N1 Ag1 O1' S1 57.5(11) 1_554 . . . ? O1 Ag1 O1' S1 -48.7(17) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H2N O2 0.847(10) 2.09(3) 2.889(15) 157(5) 2_675 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.730 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.077 #=========end data_5 _database_code_depnum_ccdc_archive 'CCDC 724285' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H20 Ag N3 O3 S' _chemical_formula_sum 'C15 H20 Ag N3 O3 S' _chemical_formula_weight 430.27 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 12.073(2) _cell_length_b 8.6984(17) _cell_length_c 16.254(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.42(3) _cell_angle_gamma 90.00 _cell_volume 1683.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3249 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 1.338 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.83 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15979 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3863 _reflns_number_gt 3249 _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^)+(0.0426P)^2^+1.0795P] 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 3863 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0830 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 0.782424(18) 0.52974(3) 0.135117(14) 0.03570(9) Uani 1 1 d . . . C5 C 0.8295(2) 1.1397(3) 0.28409(15) 0.0265(5) Uani 1 1 d . . . H5 H 0.8997 1.1328 0.2679 0.032 Uiso 1 1 calc R . . C6 C 0.7819(2) 1.2835(3) 0.29267(15) 0.0262(5) Uani 1 1 d . . . C7 C 0.6213(3) 1.4474(4) 0.3241(3) 0.0585(10) Uani 1 1 d . . . H7A H 0.6704 1.5275 0.3112 0.088 Uiso 1 1 calc R . . H7B H 0.6060 1.4616 0.3797 0.088 Uiso 1 1 calc R . . H7C H 0.5522 1.4512 0.2853 0.088 Uiso 1 1 calc R . . C8 C 0.6289(3) 0.7752(4) 0.0132(2) 0.0485(8) Uani 1 1 d . . . H18A H 0.6957 0.7600 0.0534 0.073 Uiso 1 1 calc R . . H18B H 0.5860 0.8582 0.0309 0.073 Uiso 1 1 calc R . . H18C H 0.6492 0.7995 -0.0400 0.073 Uiso 1 1 calc R . . C11 C 0.5884(3) 0.2487(4) 0.1016(2) 0.0470(8) Uani 1 1 d . . . H16A H 0.6588 0.2782 0.1343 0.070 Uiso 1 1 calc R . . H16B H 0.5999 0.1628 0.0669 0.070 Uiso 1 1 calc R . . H16C H 0.5366 0.2206 0.1379 0.070 Uiso 1 1 calc R . . C1 C 0.7733(2) 1.0073(3) 0.29944(17) 0.0279(5) Uani 1 1 d . . . C2 C 0.6697(3) 1.0154(3) 0.3252(2) 0.0416(7) Uani 1 1 d . . . H2 H 0.6321 0.9264 0.3365 0.050 Uiso 1 1 calc R . . C3 C 0.6232(3) 1.1586(4) 0.3337(2) 0.0439(7) Uani 1 1 d . . . H3 H 0.5535 1.1644 0.3508 0.053 Uiso 1 1 calc R . . C4 C 0.6766(3) 1.2937(3) 0.31793(18) 0.0352(6) Uani 1 1 d . . . C13 C 0.9721(2) 0.6394(3) 0.02651(16) 0.0298(5) Uani 1 1 d . . . C14 C 0.9458(2) 0.3766(3) 0.02363(17) 0.0317(6) Uani 1 1 d . . . C15 C 0.8864(3) 0.2407(4) 0.0508(2) 0.0508(8) Uani 1 1 d . . . H12A H 0.8328 0.2740 0.0847 0.076 Uiso 1 1 calc R . . H12B H 0.9399 0.1730 0.0827 0.076 Uiso 1 1 calc R . . H12C H 0.8482 0.1873 0.0028 0.076 Uiso 1 1 calc R . . C12 C 0.9404(3) 0.7943(3) 0.05472(19) 0.0374(6) Uani 1 1 d . . . H13A H 0.8826 0.7834 0.0884 0.056 Uiso 1 1 calc R . . H13B H 0.9132 0.8567 0.0070 0.056 Uiso 1 1 calc R . . H13C H 1.0050 0.8422 0.0869 0.056 Uiso 1 1 calc R . . C9 C 0.5602(2) 0.6318(3) 0.00586(17) 0.0316(6) Uani 1 1 d . . . C10 C 0.5418(2) 0.3805(3) 0.04807(17) 0.0310(6) Uani 1 1 d . . . N2 N 0.9185(2) 0.5160(3) 0.04966(15) 0.0321(5) Uani 1 1 d . . . N3 N 0.6011(2) 0.5112(3) 0.05330(15) 0.0312(5) Uani 1 1 d . . . O1 O 0.7542(2) 0.7680(2) 0.20754(13) 0.0467(6) Uani 1 1 d . . . O2 O 0.8210(2) 0.7311(2) 0.35386(13) 0.0439(5) Uani 1 1 d . . . O3 O 0.9415(2) 0.8470(3) 0.26739(17) 0.0510(6) Uani 1 1 d . . . S1 S 0.82835(6) 0.82426(7) 0.28143(4) 0.02986(15) Uani 1 1 d . . . N1 N 0.8361(2) 1.4173(3) 0.27068(16) 0.0312(5) Uani 1 1 d . . . HN1 H 0.825(3) 1.495(4) 0.303(2) 0.028(8) Uiso 1 1 d . . . HN2 H 0.904(3) 1.403(4) 0.2673(19) 0.034(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03713(13) 0.03320(13) 0.03737(13) -0.00143(9) 0.00787(9) 0.00083(9) C5 0.0305(13) 0.0229(12) 0.0260(12) 0.0000(10) 0.0040(10) 0.0002(9) C6 0.0323(13) 0.0207(11) 0.0253(12) -0.0008(10) 0.0034(10) -0.0008(10) C7 0.057(2) 0.0338(17) 0.091(3) -0.0098(19) 0.031(2) 0.0093(15) C8 0.0489(19) 0.0408(17) 0.0496(18) 0.0112(16) -0.0104(15) -0.0168(14) C11 0.0457(18) 0.0397(17) 0.0495(18) 0.0136(15) -0.0100(14) -0.0066(14) C1 0.0383(14) 0.0190(11) 0.0270(12) -0.0017(10) 0.0073(10) 0.0001(10) C2 0.0509(18) 0.0268(14) 0.0529(19) -0.0015(14) 0.0259(15) -0.0085(12) C3 0.0469(18) 0.0378(16) 0.0546(19) -0.0056(15) 0.0311(15) -0.0013(13) C4 0.0427(16) 0.0270(13) 0.0384(15) -0.0033(12) 0.0143(12) 0.0021(11) C13 0.0323(14) 0.0298(13) 0.0264(12) 0.0005(11) 0.0016(10) 0.0010(10) C14 0.0334(14) 0.0313(13) 0.0305(13) -0.0021(12) 0.0055(11) -0.0006(11) C15 0.060(2) 0.0369(16) 0.063(2) -0.0025(17) 0.0317(18) -0.0068(15) C12 0.0421(16) 0.0317(14) 0.0401(15) -0.0050(13) 0.0116(13) 0.0008(12) C9 0.0327(14) 0.0319(14) 0.0304(13) -0.0003(12) 0.0057(11) -0.0057(11) C10 0.0320(14) 0.0334(14) 0.0274(12) 0.0017(12) 0.0040(10) -0.0040(11) N2 0.0327(12) 0.0336(12) 0.0302(11) 0.0004(10) 0.0060(9) 0.0000(9) N3 0.0304(12) 0.0335(12) 0.0291(11) 0.0019(10) 0.0029(9) -0.0038(9) O1 0.0673(15) 0.0320(11) 0.0362(11) -0.0122(10) -0.0051(10) 0.0085(10) O2 0.0669(15) 0.0269(10) 0.0378(11) 0.0056(9) 0.0079(10) 0.0004(10) O3 0.0440(13) 0.0345(11) 0.0786(17) -0.0026(12) 0.0225(12) 0.0044(9) S1 0.0403(4) 0.0183(3) 0.0307(3) -0.0020(3) 0.0048(3) 0.0003(2) N1 0.0355(14) 0.0189(10) 0.0388(13) 0.0008(10) 0.0053(10) -0.0001(9) _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 2.321(2) . ? Ag1 N3 2.373(2) . ? Ag1 N1 2.401(2) 1_545 ? Ag1 O1 2.435(2) . ? C5 C1 1.380(3) . ? C5 C6 1.393(3) . ? C5 H5 0.9300 . ? C6 C4 1.402(4) . ? C6 N1 1.410(3) . ? C7 C4 1.505(4) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.492(4) . ? C8 H18A 0.9600 . ? C8 H18B 0.9600 . ? C8 H18C 0.9600 . ? C11 C10 1.492(4) . ? C11 H16A 0.9600 . ? C11 H16B 0.9600 . ? C11 H16C 0.9600 . ? C1 C2 1.385(4) . ? C1 S1 1.768(3) . ? C2 C3 1.383(4) . ? C2 H2 0.9300 . ? C3 C4 1.384(4) . ? C3 H3 0.9300 . ? C13 N2 1.339(4) . ? C13 C14 1.389(4) 3_765 ? C13 C12 1.493(4) . ? C14 N2 1.343(4) . ? C14 C13 1.389(4) 3_765 ? C14 C15 1.487(4) . ? C15 H12A 0.9600 . ? C15 H12B 0.9600 . ? C15 H12C 0.9600 . ? C12 H13A 0.9600 . ? C12 H13B 0.9600 . ? C12 H13C 0.9600 . ? C9 N3 1.347(4) . ? C9 C10 1.394(4) 3_665 ? C10 N3 1.339(4) . ? C10 C9 1.394(4) 3_665 ? O1 S1 1.460(2) . ? O2 S1 1.444(2) . ? O3 S1 1.435(2) . ? N1 Ag1 2.401(2) 1_565 ? N1 HN1 0.88(3) . ? N1 HN2 0.84(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 109.83(8) . . ? N2 Ag1 N1 114.65(9) . 1_545 ? N3 Ag1 N1 124.91(9) . 1_545 ? N2 Ag1 O1 120.13(8) . . ? N3 Ag1 O1 98.02(8) . . ? N1 Ag1 O1 86.62(8) 1_545 . ? C1 C5 C6 120.6(3) . . ? C1 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C4 119.7(2) . . ? C5 C6 N1 120.0(2) . . ? C4 C6 N1 120.2(2) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 H18A 109.5 . . ? C9 C8 H18B 109.5 . . ? H18A C8 H18B 109.5 . . ? C9 C8 H18C 109.5 . . ? H18A C8 H18C 109.5 . . ? H18B C8 H18C 109.5 . . ? C10 C11 H16A 109.5 . . ? C10 C11 H16B 109.5 . . ? H16A C11 H16B 109.5 . . ? C10 C11 H16C 109.5 . . ? H16A C11 H16C 109.5 . . ? H16B C11 H16C 109.5 . . ? C5 C1 C2 120.5(2) . . ? C5 C1 S1 120.8(2) . . ? C2 C1 S1 118.6(2) . . ? C3 C2 C1 118.5(3) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 122.5(3) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C3 C4 C6 118.2(3) . . ? C3 C4 C7 121.1(3) . . ? C6 C4 C7 120.6(3) . . ? N2 C13 C14 120.6(3) . 3_765 ? N2 C13 C12 118.5(3) . . ? C14 C13 C12 120.9(3) 3_765 . ? N2 C14 C13 120.7(3) . 3_765 ? N2 C14 C15 118.0(3) . . ? C13 C14 C15 121.3(3) 3_765 . ? C14 C15 H12A 109.5 . . ? C14 C15 H12B 109.5 . . ? H12A C15 H12B 109.5 . . ? C14 C15 H12C 109.5 . . ? H12A C15 H12C 109.5 . . ? H12B C15 H12C 109.5 . . ? C13 C12 H13A 109.5 . . ? C13 C12 H13B 109.5 . . ? H13A C12 H13B 109.5 . . ? C13 C12 H13C 109.5 . . ? H13A C12 H13C 109.5 . . ? H13B C12 H13C 109.5 . . ? N3 C9 C10 120.2(3) . 3_665 ? N3 C9 C8 117.3(2) . . ? C10 C9 C8 122.5(3) 3_665 . ? N3 C10 C9 120.9(3) . 3_665 ? N3 C10 C11 117.9(2) . . ? C9 C10 C11 121.2(3) 3_665 . ? C13 N2 C14 118.7(2) . . ? C13 N2 Ag1 123.29(19) . . ? C14 N2 Ag1 117.99(19) . . ? C10 N3 C9 118.9(2) . . ? C10 N3 Ag1 121.88(18) . . ? C9 N3 Ag1 119.07(18) . . ? S1 O1 Ag1 124.58(13) . . ? O3 S1 O2 113.23(15) . . ? O3 S1 O1 112.77(15) . . ? O2 S1 O1 111.79(14) . . ? O3 S1 C1 107.17(13) . . ? O2 S1 C1 107.19(13) . . ? O1 S1 C1 103.99(13) . . ? C6 N1 Ag1 120.16(17) . 1_565 ? C6 N1 HN1 111(2) . . ? Ag1 N1 HN1 101(2) 1_565 . ? C6 N1 HN2 113(2) . . ? Ag1 N1 HN2 97(2) 1_565 . ? HN1 N1 HN2 114(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C5 C6 C4 0.6(4) . . . . ? C1 C5 C6 N1 -175.1(2) . . . . ? C6 C5 C1 C2 -1.3(4) . . . . ? C6 C5 C1 S1 175.4(2) . . . . ? C5 C1 C2 C3 1.1(5) . . . . ? S1 C1 C2 C3 -175.6(3) . . . . ? C1 C2 C3 C4 -0.3(5) . . . . ? C2 C3 C4 C6 -0.3(5) . . . . ? C2 C3 C4 C7 177.2(4) . . . . ? C5 C6 C4 C3 0.1(4) . . . . ? N1 C6 C4 C3 175.9(3) . . . . ? C5 C6 C4 C7 -177.4(3) . . . . ? N1 C6 C4 C7 -1.6(4) . . . . ? C14 C13 N2 C14 0.1(4) 3_765 . . . ? C12 C13 N2 C14 179.2(2) . . . . ? C14 C13 N2 Ag1 178.88(19) 3_765 . . . ? C12 C13 N2 Ag1 -2.0(3) . . . . ? C13 C14 N2 C13 -0.1(4) 3_765 . . . ? C15 C14 N2 C13 179.2(3) . . . . ? C13 C14 N2 Ag1 -178.9(2) 3_765 . . . ? C15 C14 N2 Ag1 0.4(3) . . . . ? N3 Ag1 N2 C13 101.4(2) . . . . ? N1 Ag1 N2 C13 -112.1(2) 1_545 . . . ? O1 Ag1 N2 C13 -11.0(2) . . . . ? N3 Ag1 N2 C14 -79.9(2) . . . . ? N1 Ag1 N2 C14 66.7(2) 1_545 . . . ? O1 Ag1 N2 C14 167.72(18) . . . . ? C9 C10 N3 C9 0.5(4) 3_665 . . . ? C11 C10 N3 C9 -179.7(3) . . . . ? C9 C10 N3 Ag1 -174.4(2) 3_665 . . . ? C11 C10 N3 Ag1 5.4(4) . . . . ? C10 C9 N3 C10 -0.5(4) 3_665 . . . ? C8 C9 N3 C10 -179.8(3) . . . . ? C10 C9 N3 Ag1 174.6(2) 3_665 . . . ? C8 C9 N3 Ag1 -4.7(4) . . . . ? N2 Ag1 N3 C10 101.8(2) . . . . ? N1 Ag1 N3 C10 -40.6(2) 1_545 . . . ? O1 Ag1 N3 C10 -132.1(2) . . . . ? N2 Ag1 N3 C9 -73.1(2) . . . . ? N1 Ag1 N3 C9 144.46(19) 1_545 . . . ? O1 Ag1 N3 C9 53.0(2) . . . . ? N2 Ag1 O1 S1 -75.84(18) . . . . ? N3 Ag1 O1 S1 165.62(17) . . . . ? N1 Ag1 O1 S1 40.83(17) 1_545 . . . ? Ag1 O1 S1 O3 58.96(19) . . . . ? Ag1 O1 S1 O2 -70.0(2) . . . . ? Ag1 O1 S1 C1 174.72(15) . . . . ? C5 C1 S1 O3 11.4(3) . . . . ? C2 C1 S1 O3 -171.9(3) . . . . ? C5 C1 S1 O2 133.3(2) . . . . ? C2 C1 S1 O2 -50.1(3) . . . . ? C5 C1 S1 O1 -108.2(2) . . . . ? C2 C1 S1 O1 68.5(3) . . . . ? C5 C6 N1 Ag1 95.9(3) . . . 1_565 ? C4 C6 N1 Ag1 -79.9(3) . . . 1_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 N1 HN1 O2 0.88(3) 2.22(3) 3.065(3) 162(3) 1_565 N1 HN2 O3 0.84(3) 2.09(3) 2.917(4) 167(3) 2_755 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.926 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.093 #========end data_6 _database_code_depnum_ccdc_archive 'CCDC 724286' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H14 Ag N3 O3 S' _chemical_formula_sum 'C12 H14 Ag N3 O3 S' _chemical_formula_weight 388.19 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 23.209(5) _cell_length_b 7.8185(16) _cell_length_c 15.131(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.82(3) _cell_angle_gamma 90.00 _cell_volume 2742.3(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2615 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.880 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 1.632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.651 _exptl_absorpt_correction_T_max 0.678 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12911 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3138 _reflns_number_gt 2615 _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^)+(0.0411P)^2^+10.9635P] 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 3138 _refine_ls_number_parameters 189 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0997 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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 0.145662(14) 0.21790(4) 0.67128(2) 0.04563(13) Uani 1 1 d . . . O2 O 0.20298(13) -0.2420(4) 0.6734(2) 0.0478(7) Uani 1 1 d . . . N3 N 0.20936(14) 0.2380(4) 0.5644(2) 0.0349(7) Uani 1 1 d . . . N2 N 0.05248(13) 0.2004(4) 0.7094(2) 0.0366(7) Uani 1 1 d . . . O3 O 0.10169(15) -0.3090(6) 0.6537(2) 0.0700(11) Uani 1 1 d . . . O1 O 0.16491(17) -0.4938(4) 0.7412(3) 0.0678(10) Uani 1 1 d . . . C9 C 0.02593(15) 0.0551(5) 0.7295(3) 0.0375(8) Uani 1 1 d . . . H9 H 0.0427 -0.0487 0.7154 0.045 Uiso 1 1 calc R . . C10 C 0.02588(16) 0.3458(5) 0.7298(3) 0.0386(8) Uani 1 1 d . . . H10 H 0.0429 0.4497 0.7164 0.046 Uiso 1 1 calc R . . C11 C 0.21488(19) 0.3779(5) 0.5161(3) 0.0444(10) Uani 1 1 d . . . H11 H 0.1907 0.4703 0.5253 0.053 Uiso 1 1 calc R . . C12 C 0.2447(2) 0.1091(5) 0.5474(3) 0.0477(10) Uani 1 1 d . . . H12 H 0.2420 0.0077 0.5791 0.057 Uiso 1 1 calc R . . C7 C 0.0292(2) -0.2865(8) 0.9850(4) 0.0654(15) Uani 1 1 d . . . H7A H 0.0193 -0.2126 1.0326 0.098 Uiso 1 1 calc R . . H7B H 0.0442 -0.3923 1.0089 0.098 Uiso 1 1 calc R . . H7C H -0.0045 -0.3090 0.9476 0.098 Uiso 1 1 calc R . . S1 S 0.15273(4) -0.31887(13) 0.71058(7) 0.0403(2) Uani 1 1 d . . . C1 C 0.13636(16) -0.2061(5) 0.8080(3) 0.0335(8) Uani 1 1 d . . . C2 C 0.09598(18) -0.2821(5) 0.8594(3) 0.0381(8) Uani 1 1 d . . . H2 H 0.0830 -0.3914 0.8445 0.046 Uiso 1 1 calc R . . N1 N 0.19697(15) 0.0435(5) 0.7791(3) 0.0416(8) Uani 1 1 d . . . H1N H 0.217(2) -0.039(7) 0.743(3) 0.066(16) Uiso 1 1 d . . . H2N H 0.220(3) 0.108(8) 0.797(4) 0.11(3) Uiso 1 1 d D . . C6 C 0.15758(15) -0.0432(5) 0.8311(2) 0.0335(8) Uani 1 1 d . . . C8 C 0.1567(3) 0.2176(6) 0.9295(3) 0.0576(12) Uani 1 1 d . . . H8A H 0.1850 0.2537 0.8893 0.086 Uiso 1 1 calc RD . . H8B H 0.1734 0.2174 0.9888 0.086 Uiso 1 1 calc R . . H8C H 0.1245 0.2950 0.9258 0.086 Uiso 1 1 calc R . . C3 C 0.07394(18) -0.2022(6) 0.9323(3) 0.0424(9) Uani 1 1 d . . . C5 C 0.13627(18) 0.0396(5) 0.9052(3) 0.0394(9) Uani 1 1 d . . . C4 C 0.09533(18) -0.0405(6) 0.9538(3) 0.0458(10) Uani 1 1 d . . . H4 H 0.0815 0.0157 1.0026 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03736(19) 0.0467(2) 0.0549(2) 0.00568(14) 0.02375(14) 0.00312(13) O2 0.0423(16) 0.0392(16) 0.0637(19) 0.0005(13) 0.0226(15) 0.0018(12) N3 0.0308(15) 0.0321(16) 0.0430(17) 0.0024(13) 0.0135(13) 0.0023(12) N2 0.0278(15) 0.0453(19) 0.0374(17) -0.0005(14) 0.0083(13) 0.0002(14) O3 0.0458(19) 0.114(3) 0.0494(19) -0.020(2) -0.0036(15) 0.0022(19) O1 0.094(3) 0.0274(15) 0.085(3) -0.0059(16) 0.031(2) -0.0016(17) C9 0.0294(18) 0.037(2) 0.047(2) -0.0018(17) 0.0036(16) 0.0032(15) C10 0.0327(19) 0.041(2) 0.042(2) 0.0034(17) 0.0068(16) -0.0034(16) C11 0.048(2) 0.037(2) 0.050(2) 0.0074(18) 0.0215(19) 0.0148(18) C12 0.059(3) 0.0316(19) 0.055(2) 0.0094(18) 0.027(2) 0.0083(19) C7 0.062(3) 0.083(4) 0.053(3) 0.002(3) 0.017(2) -0.026(3) S1 0.0354(5) 0.0379(5) 0.0483(6) -0.0074(4) 0.0097(4) 0.0007(4) C1 0.0299(17) 0.0298(18) 0.0408(19) 0.0010(15) 0.0026(15) 0.0007(14) C2 0.039(2) 0.0324(19) 0.043(2) -0.0002(16) 0.0011(17) -0.0070(16) N1 0.0361(18) 0.0361(18) 0.053(2) 0.0020(16) 0.0086(16) -0.0073(15) C6 0.0307(17) 0.0277(17) 0.042(2) 0.0035(15) 0.0010(15) -0.0012(14) C8 0.077(3) 0.040(2) 0.057(3) -0.012(2) 0.010(3) -0.013(2) C3 0.040(2) 0.052(2) 0.036(2) 0.0053(18) 0.0031(16) -0.0095(19) C5 0.045(2) 0.0317(19) 0.041(2) -0.0007(16) -0.0010(17) -0.0018(17) C4 0.047(2) 0.051(2) 0.040(2) -0.0061(18) 0.0055(18) -0.001(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 N3 2.250(3) . ? Ag1 N2 2.270(3) . ? Ag1 N1 2.397(4) . ? Ag1 O1 2.521(3) 1_565 ? O2 S1 1.450(3) . ? N3 C11 1.325(5) . ? N3 C12 1.333(5) . ? N2 C9 1.334(5) . ? N2 C10 1.337(5) . ? O3 S1 1.431(4) . ? O1 S1 1.467(3) . ? O1 Ag1 2.521(3) 1_545 ? C9 C9 1.382(7) 2_556 ? C9 H9 0.9300 . ? C10 C10 1.374(7) 2_556 ? C10 H10 0.9300 . ? C11 C12 1.379(6) 7_556 ? C11 H11 0.9300 . ? C12 C11 1.379(6) 7_556 ? C12 H12 0.9300 . ? C7 C3 1.493(6) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? S1 C1 1.775(4) . ? C1 C2 1.381(5) . ? C1 C6 1.403(5) . ? C2 C3 1.387(6) . ? C2 H2 0.9300 . ? N1 C6 1.409(5) . ? N1 H1N 0.98(6) . ? N1 H2N 0.77(7) . ? C6 C5 1.405(5) . ? C8 C5 1.510(6) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C3 C4 1.391(6) . ? C5 C4 1.380(6) . ? C4 H4 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ag1 N2 148.75(12) . . ? N3 Ag1 N1 101.94(12) . . ? N2 Ag1 N1 103.92(12) . . ? N3 Ag1 O1 97.46(12) . 1_565 ? N2 Ag1 O1 95.67(12) . 1_565 ? N1 Ag1 O1 98.71(14) . 1_565 ? C11 N3 C12 116.1(3) . . ? C11 N3 Ag1 122.6(3) . . ? C12 N3 Ag1 121.2(3) . . ? C9 N2 C10 116.6(3) . . ? C9 N2 Ag1 124.4(3) . . ? C10 N2 Ag1 117.6(3) . . ? S1 O1 Ag1 132.4(2) . 1_545 ? N2 C9 C9 121.7(2) . 2_556 ? N2 C9 H9 119.2 . . ? C9 C9 H9 119.2 2_556 . ? N2 C10 C10 121.8(2) . 2_556 ? N2 C10 H10 119.1 . . ? C10 C10 H10 119.1 2_556 . ? N3 C11 C12 122.2(4) . 7_556 ? N3 C11 H11 118.9 . . ? C12 C11 H11 118.9 7_556 . ? N3 C12 C11 121.7(4) . 7_556 ? N3 C12 H12 119.2 . . ? C11 C12 H12 119.2 7_556 . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 S1 O2 113.7(2) . . ? O3 S1 O1 112.4(3) . . ? O2 S1 O1 111.3(2) . . ? O3 S1 C1 105.5(2) . . ? O2 S1 C1 109.00(19) . . ? O1 S1 C1 104.30(19) . . ? C2 C1 C6 119.4(4) . . ? C2 C1 S1 115.6(3) . . ? C6 C1 S1 124.8(3) . . ? C1 C2 C3 122.7(4) . . ? C1 C2 H2 118.6 . . ? C3 C2 H2 118.6 . . ? C6 N1 Ag1 109.8(2) . . ? C6 N1 H1N 110(3) . . ? Ag1 N1 H1N 103(3) . . ? C6 N1 H2N 125(4) . . ? Ag1 N1 H2N 100(6) . . ? H1N N1 H2N 107(4) . . ? C1 C6 C5 118.9(3) . . ? C1 C6 N1 121.8(4) . . ? C5 C6 N1 119.1(4) . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C2 C3 C4 117.0(4) . . ? C2 C3 C7 121.3(4) . . ? C4 C3 C7 121.8(4) . . ? C4 C5 C6 119.6(4) . . ? C4 C5 C8 120.3(4) . . ? C6 C5 C8 120.0(4) . . ? C5 C4 C3 122.4(4) . . ? C5 C4 H4 118.8 . . ? C3 C4 H4 118.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 N3 C11 69.7(4) . . . . ? N1 Ag1 N3 C11 -145.0(3) . . . . ? O1 Ag1 N3 C11 -44.4(4) 1_565 . . . ? N2 Ag1 N3 C12 -111.6(4) . . . . ? N1 Ag1 N3 C12 33.7(4) . . . . ? O1 Ag1 N3 C12 134.3(3) 1_565 . . . ? N3 Ag1 N2 C9 99.0(4) . . . . ? N1 Ag1 N2 C9 -46.0(3) . . . . ? O1 Ag1 N2 C9 -146.5(3) 1_565 . . . ? N3 Ag1 N2 C10 -94.7(3) . . . . ? N1 Ag1 N2 C10 120.3(3) . . . . ? O1 Ag1 N2 C10 19.9(3) 1_565 . . . ? C10 N2 C9 C9 -1.0(7) . . . 2_556 ? Ag1 N2 C9 C9 165.5(4) . . . 2_556 ? C9 N2 C10 C10 0.6(7) . . . 2_556 ? Ag1 N2 C10 C10 -166.9(4) . . . 2_556 ? C12 N3 C11 C12 -0.9(7) . . . 7_556 ? Ag1 N3 C11 C12 177.9(4) . . . 7_556 ? C11 N3 C12 C11 0.9(7) . . . 7_556 ? Ag1 N3 C12 C11 -177.9(3) . . . 7_556 ? Ag1 O1 S1 O3 31.1(3) 1_545 . . . ? Ag1 O1 S1 O2 -97.7(3) 1_545 . . . ? Ag1 O1 S1 C1 144.9(2) 1_545 . . . ? O3 S1 C1 C2 68.5(4) . . . . ? O2 S1 C1 C2 -169.0(3) . . . . ? O1 S1 C1 C2 -50.1(4) . . . . ? O3 S1 C1 C6 -106.0(4) . . . . ? O2 S1 C1 C6 16.5(4) . . . . ? O1 S1 C1 C6 135.4(3) . . . . ? C6 C1 C2 C3 1.8(6) . . . . ? S1 C1 C2 C3 -172.9(3) . . . . ? N3 Ag1 N1 C6 -154.7(3) . . . . ? N2 Ag1 N1 C6 7.6(3) . . . . ? O1 Ag1 N1 C6 105.7(3) 1_565 . . . ? C2 C1 C6 C5 -1.2(5) . . . . ? S1 C1 C6 C5 173.1(3) . . . . ? C2 C1 C6 N1 -177.3(4) . . . . ? S1 C1 C6 N1 -3.0(5) . . . . ? Ag1 N1 C6 C1 90.8(4) . . . . ? Ag1 N1 C6 C5 -85.3(4) . . . . ? C1 C2 C3 C4 -1.5(6) . . . . ? C1 C2 C3 C7 178.5(4) . . . . ? C1 C6 C5 C4 0.2(6) . . . . ? N1 C6 C5 C4 176.5(4) . . . . ? C1 C6 C5 C8 -177.7(4) . . . . ? N1 C6 C5 C8 -1.5(6) . . . . ? C6 C5 C4 C3 0.1(6) . . . . ? C8 C5 C4 C3 178.0(4) . . . . ? C2 C3 C4 C5 0.5(6) . . . . ? C7 C3 C4 C5 -179.4(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 N1 H2N O2 0.77(7) 2.18(8) 2.925(5) 166(2) 4_556 N1 H1N O2 0.98(6) 1.92(6) 2.754(5) 141(5) . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.464 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.116 #========end data_7 _database_code_depnum_ccdc_archive 'CCDC 724287' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H18 Ag N3 O3 S' _chemical_formula_sum 'C14 H18 Ag N3 O3 S' _chemical_formula_weight 416.24 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 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 14.092(3) _cell_length_b 11.078(2) _cell_length_c 10.092(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1575.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3409 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 1.427 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_T_max 0.77 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14747 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3596 _reflns_number_gt 3409 _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. H atoms bonded to N atom were located in a difference map and refined with distance restraints of N---H = 0.86+-0.02 \%A. H8A atom bonded to C8 atom and H2N atom bonded to N1 atom were refined with distance restraint of H8A---H2N = 2.02+-0.01 \%A. ; _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^)+(0.0392P)^2^+0.1055P] 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 -0.01(2) _refine_ls_number_reflns 3596 _refine_ls_number_parameters 207 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0240 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0588 _refine_ls_wR_factor_gt 0.0581 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.053 _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 0.457980(10) 0.191397(18) 0.12649(3) 0.04791(7) Uani 1 1 d . . . S1 S 0.43798(4) 0.12140(6) 0.46507(6) 0.03927(13) Uani 1 1 d . . . O3 O 0.44901(13) 0.2294(2) 0.3838(2) 0.0506(5) Uani 1 1 d . . . O2 O 0.42718(14) 0.1480(2) 0.60456(17) 0.0555(5) Uani 1 1 d . . . N2 N 0.61227(13) 0.21850(17) 0.1078(2) 0.0339(4) Uani 1 1 d . . . C3 C 0.23380(18) -0.0321(2) 0.2375(2) 0.0381(5) Uani 1 1 d . . . C12 C 0.65532(15) 0.2604(2) -0.0005(2) 0.0311(4) Uani 1 1 d . . . C11 C 0.75483(15) 0.2761(2) -0.0025(2) 0.0301(4) Uani 1 1 d . . . O1 O 0.51234(15) 0.0339(2) 0.43779(18) 0.0589(6) Uani 1 1 d . . . C2 C 0.32267(17) 0.0037(2) 0.2846(2) 0.0339(5) Uani 1 1 d . . . C8 C 0.2219(2) -0.0884(3) 0.1020(2) 0.0562(7) Uani 1 1 d . . . H8A H 0.2826 -0.0935 0.0591 0.084 Uiso 1 1 calc RD . . H8B H 0.1800 -0.0396 0.0496 0.084 Uiso 1 1 calc R . . H8C H 0.1957 -0.1679 0.1113 0.084 Uiso 1 1 calc R . . N1 N 0.40384(17) -0.0047(2) 0.2043(2) 0.0417(5) Uani 1 1 d D . . H1N H 0.4542(13) -0.015(2) 0.252(2) 0.028(7) Uiso 1 1 d D . . H2N H 0.4070(10) -0.050(3) 0.141(3) 0.068(10) Uiso 1 1 d D . . C5 C 0.16057(17) 0.0323(2) 0.4449(2) 0.0386(5) Uani 1 1 d . . . C1 C 0.32958(16) 0.0562(2) 0.4109(2) 0.0325(4) Uani 1 1 d . . . C4 C 0.15461(19) -0.0155(2) 0.3185(2) 0.0421(5) Uani 1 1 d . . . H4 H 0.0953 -0.0376 0.2862 0.050 Uiso 1 1 calc R . . C6 C 0.24957(16) 0.0680(2) 0.4896(2) 0.0354(5) Uani 1 1 d . . . H6 H 0.2555 0.1004 0.5741 0.043 Uiso 1 1 calc R . . C13 C 0.5951(2) 0.2921(3) -0.1175(3) 0.0460(6) Uani 1 1 d . . . H13A H 0.5298 0.2753 -0.0976 0.069 Uiso 1 1 calc R . . H13B H 0.6146 0.2450 -0.1926 0.069 Uiso 1 1 calc R . . H13C H 0.6023 0.3764 -0.1373 0.069 Uiso 1 1 calc R . . C9 C 0.66575(18) 0.1889(2) 0.2124(3) 0.0386(5) Uani 1 1 d . . . H9 H 0.6368 0.1584 0.2881 0.046 Uiso 1 1 calc R . . C14 C 0.80485(19) 0.3288(2) -0.1204(3) 0.0426(6) Uani 1 1 d . . . H14A H 0.8718 0.3320 -0.1033 0.064 Uiso 1 1 calc R . . H14B H 0.7815 0.4089 -0.1366 0.064 Uiso 1 1 calc R . . H14C H 0.7932 0.2792 -0.1968 0.064 Uiso 1 1 calc R . . C7 C 0.0747(2) 0.0443(3) 0.5323(3) 0.0542(7) Uani 1 1 d . . . H7A H 0.0197 0.0155 0.4859 0.081 Uiso 1 1 calc R . . H7B H 0.0658 0.1276 0.5556 0.081 Uiso 1 1 calc R . . H7C H 0.0837 -0.0025 0.6114 0.081 Uiso 1 1 calc R . . C10 C 0.76280(18) 0.2029(2) 0.2102(2) 0.0373(5) Uani 1 1 d . . . H10 H 0.7983 0.1815 0.2842 0.045 Uiso 1 1 calc R . . N3 N 0.80685(12) 0.24702(17) 0.1028(2) 0.0341(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01793(8) 0.07142(14) 0.05438(11) 0.01752(11) 0.00244(9) 0.00047(7) S1 0.0276(2) 0.0618(4) 0.0284(2) 0.0006(3) -0.0033(2) 0.0097(2) O3 0.0408(11) 0.0622(12) 0.0488(11) 0.0054(9) -0.0113(8) -0.0125(8) O2 0.0451(10) 0.0911(14) 0.0301(10) -0.0078(9) -0.0061(8) 0.0167(10) N2 0.0219(8) 0.0411(10) 0.0387(12) 0.0020(8) 0.0000(8) -0.0020(6) C3 0.0500(14) 0.0316(11) 0.0326(10) 0.0027(8) 0.0007(10) -0.0065(10) C12 0.0242(10) 0.0342(11) 0.0349(11) -0.0048(8) -0.0019(8) -0.0020(8) C11 0.0242(10) 0.0311(10) 0.0350(11) -0.0062(8) 0.0043(8) -0.0038(8) O1 0.0389(10) 0.0968(16) 0.0410(10) 0.0017(10) -0.0011(8) 0.0318(11) C2 0.0420(12) 0.0301(11) 0.0295(10) 0.0041(8) 0.0070(8) 0.0057(9) C8 0.082(2) 0.0492(15) 0.0376(15) -0.0056(11) 0.0014(13) -0.0194(14) N1 0.0454(12) 0.0466(12) 0.0329(10) -0.0034(8) 0.0113(9) 0.0094(9) C5 0.0380(12) 0.0334(11) 0.0443(12) 0.0029(9) 0.0084(10) 0.0022(9) C1 0.0321(11) 0.0358(11) 0.0295(10) 0.0028(8) 0.0028(8) 0.0092(9) C4 0.0386(12) 0.0403(13) 0.0473(13) 0.0042(10) -0.0020(10) -0.0093(10) C6 0.0377(12) 0.0365(11) 0.0321(10) 0.0004(8) 0.0044(9) 0.0051(9) C13 0.0318(12) 0.0621(17) 0.0443(13) 0.0084(11) -0.0066(11) -0.0014(11) C9 0.0279(12) 0.0523(15) 0.0354(11) 0.0057(10) 0.0042(9) -0.0029(9) C14 0.0360(13) 0.0512(15) 0.0408(12) -0.0032(10) 0.0114(10) -0.0112(10) C7 0.0406(14) 0.0590(17) 0.0629(16) -0.0007(14) 0.0167(13) -0.0029(12) C10 0.0273(11) 0.0501(14) 0.0346(11) 0.0002(9) -0.0053(9) -0.0009(9) N3 0.0211(8) 0.0415(10) 0.0397(12) -0.0092(8) -0.0003(7) -0.0023(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 2.2029(19) . ? Ag1 N3 2.2491(18) 4_455 ? Ag1 N1 2.433(2) . ? Ag1 O3 2.634(2) . ? S1 O2 1.4464(18) . ? S1 O1 1.454(2) . ? S1 O3 1.459(2) . ? S1 C1 1.776(2) . ? N2 C12 1.334(3) . ? N2 C9 1.338(3) . ? C3 C4 1.396(4) . ? C3 C2 1.397(3) . ? C3 C8 1.512(3) . ? C12 C11 1.413(3) . ? C12 C13 1.496(3) . ? C11 N3 1.330(3) . ? C11 C14 1.502(3) . ? C2 C1 1.404(3) . ? C2 N1 1.405(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? N1 H1N 0.866(16) . ? N1 H2N 0.815(18) . ? C5 C4 1.384(4) . ? C5 C6 1.390(3) . ? C5 C7 1.504(4) . ? C1 C6 1.385(3) . ? C4 H4 0.9300 . ? C6 H6 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C9 C10 1.377(3) . ? C9 H9 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C10 N3 1.342(3) . ? C10 H10 0.9300 . ? N3 Ag1 2.2491(18) 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 N3 152.14(7) . 4_455 ? N2 Ag1 N1 117.31(7) . . ? N3 Ag1 N1 90.54(7) 4_455 . ? N1 Ag1 O3 79.00(7) . . ? N2 Ag1 O3 96.31(7) . . ? N3 Ag1 O3 90.66(7) 4_455 . ? O2 S1 O1 113.34(11) . . ? O2 S1 O3 113.01(15) . . ? O1 S1 O3 111.34(13) . . ? O2 S1 C1 106.99(12) . . ? O1 S1 C1 106.88(13) . . ? O3 S1 C1 104.60(10) . . ? C12 N2 C9 118.4(2) . . ? C12 N2 Ag1 124.51(15) . . ? C9 N2 Ag1 117.08(16) . . ? C4 C3 C2 118.7(2) . . ? C4 C3 C8 119.7(2) . . ? C2 C3 C8 121.6(2) . . ? N2 C12 C11 120.39(19) . . ? N2 C12 C13 118.1(2) . . ? C11 C12 C13 121.5(2) . . ? N3 C11 C12 120.39(19) . . ? N3 C11 C14 117.9(2) . . ? C12 C11 C14 121.7(2) . . ? C3 C2 C1 119.2(2) . . ? C3 C2 N1 121.0(2) . . ? C1 C2 N1 119.6(2) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C2 N1 Ag1 112.46(16) . . ? C2 N1 H1N 110.6(17) . . ? Ag1 N1 H1N 92.2(18) . . ? C2 N1 H2N 122.7(15) . . ? Ag1 N1 H2N 106(3) . . ? H1N N1 H2N 109(2) . . ? C4 C5 C6 117.6(2) . . ? C4 C5 C7 121.7(3) . . ? C6 C5 C7 120.7(2) . . ? C6 C1 C2 120.2(2) . . ? C6 C1 S1 119.03(17) . . ? C2 C1 S1 120.51(16) . . ? C5 C4 C3 122.8(2) . . ? C5 C4 H4 118.6 . . ? C3 C4 H4 118.6 . . ? C1 C6 C5 121.5(2) . . ? C1 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C9 C10 121.3(2) . . ? N2 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C10 C9 120.9(2) . . ? N3 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C11 N3 C10 118.60(18) . . ? C11 N3 Ag1 122.24(15) . 4 ? C10 N3 Ag1 117.55(16) . 4 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ag1 N2 C12 -46.9(3) 4_455 . . . ? N1 Ag1 N2 C12 128.73(18) . . . . ? N3 Ag1 N2 C9 134.05(19) 4_455 . . . ? N1 Ag1 N2 C9 -50.30(19) . . . . ? C9 N2 C12 C11 -1.7(3) . . . . ? Ag1 N2 C12 C11 179.27(16) . . . . ? C9 N2 C12 C13 179.4(2) . . . . ? Ag1 N2 C12 C13 0.4(3) . . . . ? N2 C12 C11 N3 1.3(3) . . . . ? C13 C12 C11 N3 -179.9(2) . . . . ? N2 C12 C11 C14 -176.9(2) . . . . ? C13 C12 C11 C14 1.9(3) . . . . ? C4 C3 C2 C1 -0.7(3) . . . . ? C8 C3 C2 C1 179.6(2) . . . . ? C4 C3 C2 N1 -176.4(2) . . . . ? C8 C3 C2 N1 3.9(4) . . . . ? C3 C2 N1 Ag1 106.7(2) . . . . ? C1 C2 N1 Ag1 -69.0(2) . . . . ? N2 Ag1 N1 C2 144.50(16) . . . . ? N3 Ag1 N1 C2 -37.53(17) 4_455 . . . ? C3 C2 C1 C6 2.5(3) . . . . ? N1 C2 C1 C6 178.3(2) . . . . ? C3 C2 C1 S1 -171.39(17) . . . . ? N1 C2 C1 S1 4.4(3) . . . . ? O2 S1 C1 C6 15.8(2) . . . . ? O1 S1 C1 C6 137.50(18) . . . . ? O3 S1 C1 C6 -104.34(19) . . . . ? O2 S1 C1 C2 -170.28(19) . . . . ? O1 S1 C1 C2 -48.6(2) . . . . ? O3 S1 C1 C2 69.6(2) . . . . ? C6 C5 C4 C3 1.8(4) . . . . ? C7 C5 C4 C3 -177.3(2) . . . . ? C2 C3 C4 C5 -1.5(4) . . . . ? C8 C3 C4 C5 178.2(2) . . . . ? C2 C1 C6 C5 -2.2(3) . . . . ? S1 C1 C6 C5 171.77(18) . . . . ? C4 C5 C6 C1 0.0(3) . . . . ? C7 C5 C6 C1 179.2(2) . . . . ? C12 N2 C9 C10 1.0(4) . . . . ? Ag1 N2 C9 C10 -179.87(19) . . . . ? N2 C9 C10 N3 0.1(4) . . . . ? C12 C11 N3 C10 -0.1(3) . . . . ? C14 C11 N3 C10 178.2(2) . . . . ? C12 C11 N3 Ag1 -165.23(16) . . . 4 ? C14 C11 N3 Ag1 13.0(3) . . . 4 ? C9 C10 N3 C11 -0.6(4) . . . . ? C9 C10 N3 Ag1 165.24(19) . . . 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 N1 H2N O1 0.815(18) 2.35(3) 2.955(3) 132(3) 2_654 N1 H2N O2 0.815(18) 2.603(19) 3.034(3) 114.5(11) 2_654 N1 H1N O1 0.866(16) 2.11(2) 2.842(3) 141(2) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.303 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.083 #========end data_8 _database_code_depnum_ccdc_archive 'CCDC 724288' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H18 Ag N3 O3 S' _chemical_formula_sum 'C14 H18 Ag N3 O3 S' _chemical_formula_weight 416.24 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 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 14.223(3) _cell_length_b 8.5662(17) _cell_length_c 12.881(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1569.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3576 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 1.433 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.78 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14546 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3576 _reflns_number_gt 3260 _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. H7A atom bonded to C7 atom and HN1 atom bonded to N1 atom were refined with distance restraint of H7A---HN1 = 2.02+-0.01 \%A. ; _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^)+(0.0371P)^2^+0.3486P] 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 0.00(2) _refine_ls_number_reflns 3576 _refine_ls_number_parameters 207 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0653 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.064 _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 0.483223(12) -0.16307(3) 0.70033(3) 0.04224(8) Uani 1 1 d . . . S1 S 0.56666(5) -0.08664(9) 1.00273(6) 0.03452(16) Uani 1 1 d . . . O2 O 0.49226(16) 0.0286(3) 1.0179(2) 0.0442(5) Uani 1 1 d . . . N2 N 0.33039(13) -0.2338(3) 0.7025(3) 0.0309(4) Uani 1 1 d . . . O1 O 0.61433(19) -0.1240(4) 1.0984(2) 0.0589(7) Uani 1 1 d . . . N3 N 0.13689(16) -0.2635(3) 0.6835(2) 0.0362(6) Uani 1 1 d . . . O3 O 0.53337(18) -0.2211(3) 0.9450(2) 0.0534(6) Uani 1 1 d . . . N1 N 0.52656(18) 0.0776(4) 0.7985(2) 0.0373(6) Uani 1 1 d . . . HN2 H 0.493(4) 0.062(7) 0.853(5) 0.074(16) Uiso 1 1 d . . . HN1 H 0.500(3) 0.170(6) 0.770(3) 0.065(15) Uiso 1 1 d D . . C2 C 0.6208(2) 0.0813(3) 0.8302(2) 0.0319(6) Uani 1 1 d . . . C9 C 0.2728(2) -0.1762(4) 0.7742(3) 0.0363(7) Uani 1 1 d . . . C6 C 0.7446(2) 0.0037(4) 0.9483(3) 0.0352(6) Uani 1 1 d . . . H6 H 0.7625 -0.0447 1.0098 0.042 Uiso 1 1 calc R . . C4 C 0.7828(2) 0.1438(4) 0.7955(3) 0.0428(8) Uani 1 1 d . . . H4 H 0.8276 0.1895 0.7525 0.051 Uiso 1 1 calc R . . C11 C 0.1949(2) -0.3225(4) 0.6136(3) 0.0380(7) Uani 1 1 d . . . H11 H 0.1696 -0.3740 0.5564 0.046 Uiso 1 1 calc R . . C5 C 0.8129(2) 0.0705(4) 0.8851(3) 0.0394(7) Uani 1 1 d . . . C12 C 0.2925(2) -0.3107(4) 0.6220(2) 0.0329(6) Uani 1 1 d . . . C10 C 0.1760(2) -0.1917(4) 0.7640(3) 0.0375(7) Uani 1 1 d . . . H10 H 0.1372 -0.1504 0.8152 0.045 Uiso 1 1 calc R . . C1 C 0.65059(19) 0.0076(3) 0.9215(2) 0.0294(6) Uani 1 1 d . . . C3 C 0.6894(3) 0.1523(4) 0.7668(3) 0.0414(8) Uani 1 1 d . . . C14 C 0.3571(3) -0.3810(5) 0.5434(3) 0.0538(9) Uani 1 1 d . . . H14A H 0.4211 -0.3606 0.5628 0.081 Uiso 1 1 calc R . . H14B H 0.3448 -0.3358 0.4765 0.081 Uiso 1 1 calc R . . H14C H 0.3469 -0.4917 0.5403 0.081 Uiso 1 1 calc R . . C13 C 0.3137(3) -0.0982(6) 0.8667(3) 0.0608(11) Uani 1 1 d . . . H13A H 0.3810 -0.0974 0.8610 0.091 Uiso 1 1 calc R . . H13B H 0.2956 -0.1539 0.9282 0.091 Uiso 1 1 calc R . . H13C H 0.2910 0.0072 0.8706 0.091 Uiso 1 1 calc R . . C8 C 0.9155(2) 0.0625(5) 0.9145(4) 0.0608(11) Uani 1 1 d . . . H8A H 0.9220 0.0074 0.9789 0.091 Uiso 1 1 calc R . . H8B H 0.9399 0.1664 0.9220 0.091 Uiso 1 1 calc R . . H8C H 0.9497 0.0088 0.8611 0.091 Uiso 1 1 calc R . . C7 C 0.6611(3) 0.2365(6) 0.6693(3) 0.0652(12) Uani 1 1 d . . . H7A H 0.5941 0.2313 0.6612 0.098 Uiso 1 1 calc RD . . H7B H 0.6909 0.1883 0.6106 0.098 Uiso 1 1 calc R . . H7C H 0.6803 0.3437 0.6737 0.098 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01606(10) 0.06193(15) 0.04874(13) -0.00315(16) 0.00025(13) -0.00199(8) S1 0.0285(3) 0.0436(4) 0.0315(3) 0.0040(3) 0.0051(3) -0.0014(3) O2 0.0344(11) 0.0573(15) 0.0410(13) -0.0037(11) 0.0079(9) 0.0050(10) N2 0.0192(8) 0.0376(11) 0.0358(11) 0.0042(15) 0.0022(13) -0.0023(8) O1 0.0458(15) 0.089(2) 0.0423(14) 0.0244(14) 0.0008(11) 0.0001(13) N3 0.0195(10) 0.0523(14) 0.0369(17) 0.0040(12) 0.0001(10) -0.0041(9) O3 0.0485(14) 0.0493(13) 0.0624(16) -0.0094(13) 0.0180(12) -0.0160(12) N1 0.0301(13) 0.0481(16) 0.0336(14) 0.0026(12) -0.0038(11) -0.0024(11) C2 0.0283(14) 0.0353(14) 0.0321(14) -0.0038(12) -0.0032(10) -0.0039(11) C9 0.0224(14) 0.051(2) 0.0352(16) -0.0037(14) 0.0002(11) -0.0052(12) C6 0.0296(15) 0.0360(14) 0.0400(15) 0.0033(12) -0.0031(11) -0.0019(11) C4 0.0354(17) 0.0474(19) 0.0456(19) -0.0008(15) 0.0090(14) -0.0134(13) C11 0.0248(15) 0.0545(19) 0.0349(16) -0.0014(14) -0.0003(11) -0.0076(12) C5 0.0265(14) 0.0393(17) 0.0524(19) -0.0031(14) 0.0013(13) -0.0040(12) C12 0.0246(14) 0.0408(16) 0.0332(15) 0.0008(12) 0.0025(11) -0.0016(12) C10 0.0201(14) 0.0525(19) 0.0399(18) -0.0030(14) 0.0072(12) 0.0002(12) C1 0.0276(14) 0.0320(13) 0.0286(14) 0.0011(11) 0.0029(10) -0.0043(11) C3 0.0464(19) 0.0452(19) 0.0326(17) 0.0017(14) -0.0012(13) -0.0146(14) C14 0.0311(17) 0.069(2) 0.061(2) -0.0246(19) 0.0092(15) -0.0071(17) C13 0.0368(18) 0.095(3) 0.051(2) -0.029(2) 0.0071(16) -0.012(2) C8 0.0300(17) 0.064(2) 0.089(3) 0.013(2) -0.0029(18) -0.0030(16) C7 0.062(3) 0.089(3) 0.044(2) 0.026(2) -0.0103(16) -0.029(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 2.2567(19) . ? Ag1 N3 2.284(2) 4_545 ? Ag1 N1 2.496(3) . ? Ag1 O2 2.640(3) 2_654 ? S1 O1 1.443(3) . ? S1 O3 1.450(3) . ? S1 O2 1.460(2) . ? S1 C1 1.781(3) . ? N2 C9 1.329(4) . ? N2 C12 1.342(4) . ? N3 C11 1.322(4) . ? N3 C10 1.327(4) . ? N3 Ag1 2.284(2) 4_445 ? N1 C2 1.402(4) . ? N1 HN2 0.86(6) . ? N1 HN1 0.95(5) . ? C2 C1 1.400(4) . ? C2 C3 1.410(4) . ? C9 C10 1.389(4) . ? C9 C13 1.485(5) . ? C6 C1 1.381(4) . ? C6 C5 1.391(4) . ? C6 H6 0.9300 . ? C4 C3 1.381(5) . ? C4 C5 1.381(5) . ? C4 H4 0.9300 . ? C11 C12 1.396(4) . ? C11 H11 0.9300 . ? C5 C8 1.509(4) . ? C12 C14 1.494(4) . ? C10 H10 0.9300 . ? C3 C7 1.503(5) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? 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 148.08(9) . 4_545 ? N2 Ag1 N1 116.96(9) . . ? N3 Ag1 N1 92.24(9) 4_545 . ? N1 Ag1 O2 93.34(9) . 2_654 ? N2 Ag1 O2 104.82(8) . 2_654 ? N3 Ag1 O2 84.77(8) 4_545 2_654 ? O1 S1 O3 114.53(19) . . ? O1 S1 O2 112.12(17) . . ? O3 S1 O2 111.63(16) . . ? O1 S1 C1 106.71(15) . . ? O3 S1 C1 106.12(14) . . ? O2 S1 C1 104.94(14) . . ? C9 N2 C12 118.1(2) . . ? C9 N2 Ag1 120.2(2) . . ? C12 N2 Ag1 120.6(2) . . ? C11 N3 C10 116.6(2) . . ? C11 N3 Ag1 123.8(2) . 4_445 ? C10 N3 Ag1 117.02(19) . 4_445 ? C2 N1 Ag1 113.7(2) . . ? C2 N1 HN2 108(4) . . ? Ag1 N1 HN2 98(4) . . ? C2 N1 HN1 119(3) . . ? Ag1 N1 HN1 113(3) . . ? HN2 N1 HN1 103(4) . . ? C1 C2 N1 121.6(3) . . ? C1 C2 C3 118.2(3) . . ? N1 C2 C3 120.2(3) . . ? N2 C9 C10 120.6(3) . . ? N2 C9 C13 118.8(3) . . ? C10 C9 C13 120.5(3) . . ? C1 C6 C5 121.3(3) . . ? C1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C3 C4 C5 123.0(3) . . ? C3 C4 H4 118.5 . . ? C5 C4 H4 118.5 . . ? N3 C11 C12 122.7(3) . . ? N3 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C4 C5 C6 117.4(3) . . ? C4 C5 C8 122.0(3) . . ? C6 C5 C8 120.6(3) . . ? N2 C12 C11 119.7(3) . . ? N2 C12 C14 118.4(3) . . ? C11 C12 C14 122.0(3) . . ? N3 C10 C9 122.2(3) . . ? N3 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C6 C1 C2 120.9(3) . . ? C6 C1 S1 119.4(2) . . ? C2 C1 S1 119.7(2) . . ? C4 C3 C2 119.2(3) . . ? C4 C3 C7 120.4(3) . . ? C2 C3 C7 120.4(3) . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? 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 N3 Ag1 N2 C9 136.4(2) 4_545 . . . ? N1 Ag1 N2 C9 -17.7(3) . . . . ? N3 Ag1 N2 C12 -55.7(4) 4_545 . . . ? N1 Ag1 N2 C12 150.2(2) . . . . ? N2 Ag1 N1 C2 155.3(2) . . . . ? N3 Ag1 N1 C2 -11.4(2) 4_545 . . . ? Ag1 N1 C2 C1 -83.9(3) . . . . ? Ag1 N1 C2 C3 92.3(3) . . . . ? C12 N2 C9 C10 -1.9(5) . . . . ? Ag1 N2 C9 C10 166.3(2) . . . . ? C12 N2 C9 C13 176.8(3) . . . . ? Ag1 N2 C9 C13 -15.1(5) . . . . ? C10 N3 C11 C12 -0.3(5) . . . . ? Ag1 N3 C11 C12 -161.6(2) 4_445 . . . ? C3 C4 C5 C6 -0.3(5) . . . . ? C3 C4 C5 C8 179.8(3) . . . . ? C1 C6 C5 C4 1.3(5) . . . . ? C1 C6 C5 C8 -178.8(3) . . . . ? C9 N2 C12 C11 2.6(4) . . . . ? Ag1 N2 C12 C11 -165.6(2) . . . . ? C9 N2 C12 C14 -177.7(3) . . . . ? Ag1 N2 C12 C14 14.2(4) . . . . ? N3 C11 C12 N2 -1.6(5) . . . . ? N3 C11 C12 C14 178.7(3) . . . . ? C11 N3 C10 C9 1.1(5) . . . . ? Ag1 N3 C10 C9 163.6(3) 4_445 . . . ? N2 C9 C10 N3 0.0(5) . . . . ? C13 C9 C10 N3 -178.6(4) . . . . ? C5 C6 C1 C2 -0.9(5) . . . . ? C5 C6 C1 S1 177.5(3) . . . . ? N1 C2 C1 C6 175.8(3) . . . . ? C3 C2 C1 C6 -0.4(4) . . . . ? N1 C2 C1 S1 -2.6(4) . . . . ? C3 C2 C1 S1 -178.8(2) . . . . ? O1 S1 C1 C6 12.4(3) . . . . ? O3 S1 C1 C6 -110.1(3) . . . . ? O2 S1 C1 C6 131.5(3) . . . . ? O1 S1 C1 C2 -169.2(2) . . . . ? O3 S1 C1 C2 68.3(3) . . . . ? O2 S1 C1 C2 -50.0(3) . . . . ? C5 C4 C3 C2 -1.0(5) . . . . ? C5 C4 C3 C7 178.8(4) . . . . ? C1 C2 C3 C4 1.3(5) . . . . ? N1 C2 C3 C4 -174.9(3) . . . . ? C1 C2 C3 C7 -178.5(3) . . . . ? N1 C2 C3 C7 5.3(5) . . . . ? 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 N1 HN2 O2 0.86(6) 2.15(7) 2.899(4) 146(5) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.831 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.068 #======end data_9 _database_code_depnum_ccdc_archive 'CCDC 724289' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H16 Ag N3 O3 S' _chemical_formula_sum 'C13 H16 Ag N3 O3 S' _chemical_formula_weight 402.22 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 'P n a 21' _symmetry_space_group_name_hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 14.2740(2) _cell_length_b 8.2430(2) _cell_length_c 12.6120(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.000(5) _cell_angle_gamma 90.00 _cell_volume 1483.94(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3321 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 27.4 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.800 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.512 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.548 _exptl_absorpt_correction_T_max 0.650 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _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 scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13395 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0131 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 27.36 _reflns_number_total 3321 _reflns_number_gt 3160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO(Rigaku, 1998)' _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. H atoms bonded to N atom were located in a difference map and refined with distance restraints of N---H = 0.85+-0.02 \%A. H8A atom bonded to C8 atom and H1N atom bonded to N1 atom were refined with distance restraint of H8A---H1N = 2.02+-0.01 \%A. ; _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^)+(0.0388P)^2^+0.2098P] 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 -0.01(2) _refine_ls_number_reflns 3321 _refine_ls_number_parameters 198 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0240 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 0.493057(10) 0.31070(2) 0.67460(3) 0.04803(7) Uani 1 1 d . . . C1 C 0.36865(15) 0.5184(3) 0.88796(16) 0.0292(4) Uani 1 1 d . . . C2 C 0.27610(16) 0.5151(3) 0.91981(19) 0.0347(5) Uani 1 1 d . . . H2 H 0.2602 0.4605 0.9818 0.042 Uiso 1 1 calc R . . C3 C 0.20611(18) 0.5914(3) 0.8616(2) 0.0395(5) Uani 1 1 d . . . C4 C 0.23388(19) 0.6770(3) 0.7717(2) 0.0419(6) Uani 1 1 d . . . H4 H 0.1885 0.7313 0.7324 0.050 Uiso 1 1 calc R . . C5 C 0.3267(2) 0.6847(3) 0.73833(19) 0.0383(5) Uani 1 1 d . . . C6 C 0.39519(16) 0.6007(2) 0.79488(16) 0.0309(4) Uani 1 1 d . . . C7 C 0.10455(19) 0.5789(4) 0.8956(3) 0.0576(7) Uani 1 1 d . . . H7A H 0.0659 0.6382 0.8469 0.086 Uiso 1 1 calc R . . H7B H 0.0976 0.6234 0.9655 0.086 Uiso 1 1 calc R . . H7C H 0.0858 0.4670 0.8961 0.086 Uiso 1 1 calc R . . C8 C 0.3528(3) 0.7793(4) 0.6405(2) 0.0677(10) Uani 1 1 d . . . H8A H 0.4192 0.7725 0.6295 0.102 Uiso 1 1 calc RD . . H8B H 0.3351 0.8908 0.6495 0.102 Uiso 1 1 calc R . . H8C H 0.3208 0.7349 0.5802 0.102 Uiso 1 1 calc R . . C9 C 0.28571(17) 0.3361(3) 0.5955(2) 0.0356(5) Uani 1 1 d . . . H9 H 0.3150 0.3924 0.5409 0.043 Uiso 1 1 calc R . . C10 C 0.29362(19) 0.1870(3) 0.7462(2) 0.0452(6) Uani 1 1 d . . . H10 H 0.3281 0.1369 0.7995 0.054 Uiso 1 1 calc R . . C11 C 0.19747(19) 0.1795(3) 0.7491(2) 0.0459(6) Uani 1 1 d . . . H11 H 0.1683 0.1242 0.8043 0.055 Uiso 1 1 calc R . . C12 C 0.18841(16) 0.3305(3) 0.59733(18) 0.0321(5) Uani 1 1 d . . . C13 C 0.1317(2) 0.4145(4) 0.5143(3) 0.0554(7) Uani 1 1 d . . . H13A H 0.0663 0.3986 0.5285 0.083 Uiso 1 1 calc R . . H13B H 0.1468 0.3705 0.4459 0.083 Uiso 1 1 calc R . . H13C H 0.1456 0.5284 0.5152 0.083 Uiso 1 1 calc R . . N1 N 0.48679(15) 0.5887(3) 0.75732(17) 0.0382(4) Uani 1 1 d D . . H1N H 0.5136(12) 0.646(5) 0.714(3) 0.099(18) Uiso 1 1 d D . . H2N H 0.5237(19) 0.586(4) 0.811(2) 0.041(8) Uiso 1 1 d D . . N2 N 0.33859(12) 0.2648(2) 0.6682(2) 0.0378(4) Uani 1 1 d . . . N3 N 0.14475(11) 0.2501(2) 0.67414(19) 0.0350(3) Uani 1 1 d . . . O1 O 0.40715(15) 0.3511(3) 1.05594(13) 0.0489(5) Uani 1 1 d . . . O2 O 0.48081(15) 0.2734(3) 0.89177(18) 0.0500(5) Uani 1 1 d . . . O3 O 0.52943(15) 0.5191(3) 0.98172(16) 0.0526(5) Uani 1 1 d . . . S2 S 0.45293(4) 0.40617(6) 0.96054(4) 0.03274(12) 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 0.01775(8) 0.06489(13) 0.06144(12) -0.01468(12) -0.00050(12) 0.00455(6) C1 0.0310(10) 0.0291(10) 0.0275(9) -0.0005(8) -0.0023(8) 0.0003(8) C2 0.0343(11) 0.0326(11) 0.0373(10) 0.0039(8) 0.0059(9) -0.0001(9) C3 0.0308(11) 0.0354(12) 0.0522(14) -0.0032(10) 0.0005(10) 0.0031(9) C4 0.0411(14) 0.0413(14) 0.0435(14) -0.0007(10) -0.0074(11) 0.0157(10) C5 0.0493(15) 0.0349(13) 0.0306(11) 0.0013(9) 0.0022(10) 0.0115(10) C6 0.0367(11) 0.0294(10) 0.0265(9) -0.0030(8) 0.0010(9) 0.0001(8) C7 0.0308(12) 0.0575(17) 0.085(2) 0.0024(16) 0.0064(14) 0.0071(11) C8 0.079(2) 0.082(2) 0.0419(14) 0.0263(14) 0.0150(15) 0.0423(19) C9 0.0233(10) 0.0443(13) 0.0392(12) -0.0002(10) 0.0005(9) -0.0058(9) C10 0.0284(12) 0.0629(18) 0.0444(13) 0.0089(12) -0.0118(11) -0.0037(10) C11 0.0286(12) 0.0656(18) 0.0436(13) 0.0115(12) -0.0045(11) -0.0131(11) C12 0.0233(10) 0.0348(12) 0.0384(12) -0.0028(9) -0.0015(9) -0.0020(8) C13 0.0396(13) 0.0615(18) 0.0650(16) 0.0195(14) -0.0117(13) 0.0011(12) N1 0.0354(10) 0.0449(12) 0.0342(10) 0.0054(9) 0.0060(9) -0.0015(8) N2 0.0211(7) 0.0460(10) 0.0463(11) -0.0069(11) 0.0017(11) -0.0028(7) N3 0.0195(7) 0.0438(9) 0.0419(9) -0.0020(12) -0.0023(11) -0.0057(6) O1 0.0510(11) 0.0612(11) 0.0345(9) 0.0161(8) -0.0046(8) -0.0053(9) O2 0.0567(12) 0.0486(11) 0.0448(10) -0.0012(9) -0.0070(9) 0.0207(9) O3 0.0427(10) 0.0610(12) 0.0540(12) 0.0109(9) -0.0184(9) -0.0155(9) S2 0.0313(3) 0.0382(3) 0.0287(2) 0.0048(2) -0.0068(2) -0.0006(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 N3 2.2224(15) 4 ? Ag1 N2 2.2386(17) . ? Ag1 N1 2.520(2) . ? Ag1 O2 2.760(3) . ? Ag1 O3 2.827(2) 2_664 ? C1 C2 1.381(3) . ? C1 C6 1.408(3) . ? C1 S2 1.772(2) . ? C2 C3 1.390(4) . ? C2 H2 0.9300 . ? C3 C4 1.393(4) . ? C3 C7 1.515(4) . ? C4 C5 1.391(4) . ? C4 H4 0.9300 . ? C5 C6 1.395(3) . ? C5 C8 1.507(4) . ? C6 N1 1.394(3) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N2 1.325(3) . ? C9 C12 1.390(3) . ? C9 H9 0.9300 . ? C10 N2 1.339(4) . ? C10 C11 1.374(4) . ? C10 H10 0.9300 . ? C11 N3 1.342(3) . ? C11 H11 0.9300 . ? C12 N3 1.329(3) . ? C12 C13 1.493(3) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? N1 H1N 0.82(4) . ? N1 H2N 0.860(18) . ? N3 Ag1 2.2224(15) 4_455 ? O1 S2 1.4423(18) . ? O2 S2 1.452(2) . ? O3 S2 1.459(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ag1 N2 157.13(8) 4 . ? N3 Ag1 N1 103.93(7) 4 . ? N2 Ag1 N1 97.69(7) . . ? O2 Ag1 N1 71.83(8) . . ? N1 Ag1 O3 84.33(9) . 2_664 ? N3 Ag1 O3 102.76(9) 4 2_664 ? N2 Ag1 O3 86.59(9) . 2_664 ? O2 Ag1 O3 154.38(9) . 2_664 ? C2 C1 C6 120.6(2) . . ? C2 C1 S2 119.27(17) . . ? C6 C1 S2 119.97(17) . . ? C1 C2 C3 121.7(2) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C2 C3 C4 117.0(2) . . ? C2 C3 C7 120.5(2) . . ? C4 C3 C7 122.5(2) . . ? C5 C4 C3 122.7(2) . . ? C5 C4 H4 118.7 . . ? C3 C4 H4 118.7 . . ? C4 C5 C6 119.4(2) . . ? C4 C5 C8 120.5(3) . . ? C6 C5 C8 120.1(3) . . ? N1 C6 C5 121.3(2) . . ? N1 C6 C1 120.1(2) . . ? C5 C6 C1 118.5(2) . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 C12 122.9(2) . . ? N2 C9 H9 118.5 . . ? C12 C9 H9 118.5 . . ? N2 C10 C11 121.3(2) . . ? N2 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? N3 C11 C10 121.4(2) . . ? N3 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? N3 C12 C9 119.8(2) . . ? N3 C12 C13 119.2(2) . . ? C9 C12 C13 121.0(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C6 N1 Ag1 103.78(15) . . ? C6 N1 H1N 128.6(16) . . ? Ag1 N1 H1N 104(4) . . ? C6 N1 H2N 108(2) . . ? Ag1 N1 H2N 106(2) . . ? H1N N1 H2N 105(3) . . ? C9 N2 C10 116.6(2) . . ? C9 N2 Ag1 120.74(17) . . ? C10 N2 Ag1 121.78(18) . . ? C12 N3 C11 117.86(19) . . ? C12 N3 Ag1 124.84(16) . 4_455 ? C11 N3 Ag1 116.54(16) . 4_455 ? O1 S2 O2 112.66(13) . . ? O1 S2 O3 112.77(12) . . ? O2 S2 O3 112.64(14) . . ? O1 S2 C1 106.70(11) . . ? O2 S2 C1 105.72(10) . . ? O3 S2 C1 105.64(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) . . . . ? S2 C1 C2 C3 -175.38(19) . . . . ? C1 C2 C3 C4 -2.5(4) . . . . ? C1 C2 C3 C7 177.0(2) . . . . ? C2 C3 C4 C5 1.5(4) . . . . ? C7 C3 C4 C5 -178.0(3) . . . . ? C3 C4 C5 C6 1.6(4) . . . . ? C3 C4 C5 C8 -179.9(3) . . . . ? C4 C5 C6 N1 172.2(2) . . . . ? C8 C5 C6 N1 -6.4(4) . . . . ? C4 C5 C6 C1 -3.7(3) . . . . ? C8 C5 C6 C1 177.8(2) . . . . ? C2 C1 C6 N1 -173.1(2) . . . . ? S2 C1 C6 N1 2.6(3) . . . . ? C2 C1 C6 C5 2.8(3) . . . . ? S2 C1 C6 C5 178.51(18) . . . . ? N2 C10 C11 N3 -0.2(4) . . . . ? N2 C9 C12 N3 -0.4(4) . . . . ? N2 C9 C12 C13 179.3(2) . . . . ? C5 C6 N1 Ag1 -99.8(2) . . . . ? C1 C6 N1 Ag1 76.0(2) . . . . ? N3 Ag1 N1 C6 -157.86(15) 4 . . . ? N2 Ag1 N1 C6 14.62(16) . . . . ? C12 C9 N2 C10 -0.9(4) . . . . ? C12 C9 N2 Ag1 -170.44(18) . . . . ? C11 C10 N2 C9 1.2(4) . . . . ? C11 C10 N2 Ag1 170.6(2) . . . . ? N3 Ag1 N2 C9 -123.1(3) 4 . . . ? N1 Ag1 N2 C9 76.01(19) . . . . ? N3 Ag1 N2 C10 67.9(4) 4 . . . ? N1 Ag1 N2 C10 -93.0(2) . . . . ? C9 C12 N3 C11 1.4(4) . . . . ? C13 C12 N3 C11 -178.3(3) . . . . ? C9 C12 N3 Ag1 -168.20(17) . . . 4_455 ? C13 C12 N3 Ag1 12.1(3) . . . 4_455 ? C10 C11 N3 C12 -1.2(4) . . . . ? C10 C11 N3 Ag1 169.3(2) . . . 4_455 ? C2 C1 S2 O1 -10.0(2) . . . . ? C6 C1 S2 O1 174.20(17) . . . . ? C2 C1 S2 O2 110.1(2) . . . . ? C6 C1 S2 O2 -65.6(2) . . . . ? C2 C1 S2 O3 -130.3(2) . . . . ? C6 C1 S2 O3 53.97(19) . . . . ? 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 N1 H2N O3 0.860(18) 2.22(2) 2.951(3) 143(3) . N1 H1N O1 0.82(4) 2.30(4) 2.998(3) 144(5) 2_664 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.288 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.073 #============end data_10 _database_code_depnum_ccdc_archive 'CCDC 724290' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H18 Ag N3 O3 S, H2 O' _chemical_formula_sum 'C14 H20 Ag N3 O4 S' _chemical_formula_weight 434.26 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 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 24.041(5) _cell_length_b 10.974(2) _cell_length_c 15.315(3) _cell_angle_alpha 90.00 _cell_angle_beta 122.99(3) _cell_angle_gamma 90.00 _cell_volume 3388.9(12) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2917 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 1.335 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 0.77 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 scans' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14678 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3853 _reflns_number_gt 2917 _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. H atoms bonded to O atom of water molecule were located in a difference Fourier map and refined with distance restraints of O---H = 0.86+-0.01 \%A, with U~iso~ = 1.5U~eq~(N). H atoms bonded to N atom were located in a difference map and refined with distance restraint of N---H = 0.86+-0.01 \%A. H7A atom bonded to C7 atom and HN1 atom bonded to N1 atom were refined with distance restraint of H7A---HN1 = 2.02+-0.01 \%A. ; _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^)+(0.0708P)^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 3853 _refine_ls_number_parameters 222 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.038 _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 0.668403(13) 0.12018(3) 0.11936(3) 0.05968(14) Uani 1 1 d . . . S1 S 0.73066(4) -0.20598(8) 0.14340(7) 0.0486(2) Uani 1 1 d . . . O2 O 0.72367(14) -0.3196(3) 0.0904(2) 0.0605(7) Uani 1 1 d . . . O1 O 0.70863(16) -0.1015(2) 0.0755(2) 0.0618(7) Uani 1 1 d . . . O3 O 0.79671(13) -0.1902(3) 0.2360(2) 0.0682(8) Uani 1 1 d . . . N2 N 0.55935(13) 0.0581(3) 0.0362(2) 0.0472(7) Uani 1 1 d . . . N3 N 0.71841(13) 0.2026(3) 0.0456(2) 0.0447(6) Uani 1 1 d . . . N1 N 0.71123(17) -0.0125(3) 0.2638(3) 0.0544(8) Uani 1 1 d D . . HN1 H 0.7203(13) 0.041(3) 0.310(3) 0.079(15) Uiso 1 1 d D . . HN2 H 0.7507(10) -0.035(4) 0.285(3) 0.079(15) Uiso 1 1 d D . . C10 C 0.76751(17) 0.1428(3) 0.0473(3) 0.0456(7) Uani 1 1 d . . . H10 H 0.7806 0.0674 0.0801 0.055 Uiso 1 1 calc R . . C5 C 0.59235(18) -0.3269(4) 0.1942(3) 0.0525(8) Uani 1 1 d . . . C6 C 0.63791(17) -0.3177(3) 0.1659(3) 0.0451(7) Uani 1 1 d . . . H6 H 0.6425 -0.3822 0.1309 0.054 Uiso 1 1 calc R . . C4 C 0.58584(19) -0.2263(4) 0.2431(3) 0.0543(9) Uani 1 1 d . . . H4 H 0.5541 -0.2291 0.2599 0.065 Uiso 1 1 calc R . . C1 C 0.67669(16) -0.2151(3) 0.1885(2) 0.0396(7) Uani 1 1 d . . . C9 C 0.54656(16) -0.0509(3) -0.0080(3) 0.0487(8) Uani 1 1 d . . . H9 H 0.5789 -0.0883 -0.0143 0.058 Uiso 1 1 calc R . . C3 C 0.6241(2) -0.1224(3) 0.2680(3) 0.0510(8) Uani 1 1 d . . . C7 C 0.6144(3) -0.0159(4) 0.3206(4) 0.0756(13) Uani 1 1 d . . . H7A H 0.6449 0.0479 0.3314 0.113 Uiso 1 1 calc RD . . H7B H 0.6225 -0.0415 0.3864 0.113 Uiso 1 1 calc R . . H7C H 0.5698 0.0136 0.2773 0.113 Uiso 1 1 calc R . . C2 C 0.67156(17) -0.1173(3) 0.2424(3) 0.0418(7) Uani 1 1 d . . . C8 C 0.5517(2) -0.4394(4) 0.1715(4) 0.0804(14) Uani 1 1 d . . . H8A H 0.5232 -0.4295 0.1968 0.121 Uiso 1 1 calc R . . H8B H 0.5805 -0.5078 0.2054 0.121 Uiso 1 1 calc R . . H8C H 0.5253 -0.4531 0.0977 0.121 Uiso 1 1 calc R . . C11 C 0.51282(17) 0.1116(3) 0.0451(3) 0.0478(8) Uani 1 1 d . . . C13 C 0.70054(16) 0.3111(3) -0.0022(3) 0.0456(7) Uani 1 1 d . . . C14 C 0.6450(2) 0.3774(4) -0.0068(4) 0.0600(10) Uani 1 1 d . . . H14A H 0.6292 0.3308 0.0286 0.090 Uiso 1 1 calc R . . H14B H 0.6095 0.3886 -0.0782 0.090 Uiso 1 1 calc R . . H14C H 0.6603 0.4554 0.0262 0.090 Uiso 1 1 calc R . . C12 C 0.5252(2) 0.2347(4) 0.0933(4) 0.0718(12) Uani 1 1 d . . . H12A H 0.5687 0.2618 0.1142 0.108 Uiso 1 1 calc R . . H12B H 0.5221 0.2307 0.1532 0.108 Uiso 1 1 calc R . . H12C H 0.4927 0.2909 0.0437 0.108 Uiso 1 1 calc R . . OW1 O 0.6240(2) -0.3286(6) -0.1305(4) 0.1244(16) Uani 1 1 d D . . H2A H 0.647(4) -0.291(8) -0.072(4) 0.187 Uiso 1 1 d D . . H1A H 0.646(4) -0.323(10) -0.161(6) 0.187 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 0.05052(19) 0.0538(2) 0.0701(2) 0.01571(14) 0.02987(17) -0.00825(12) S1 0.0534(5) 0.0423(5) 0.0528(5) 0.0115(4) 0.0306(4) 0.0093(4) O2 0.0813(18) 0.0481(16) 0.0624(17) 0.0094(13) 0.0459(15) 0.0188(13) O1 0.0810(19) 0.0474(16) 0.074(2) 0.0226(13) 0.0528(17) 0.0143(13) O3 0.0489(14) 0.078(2) 0.0694(19) 0.0048(16) 0.0271(14) 0.0002(14) N2 0.0377(13) 0.0449(17) 0.0469(17) 0.0100(13) 0.0153(12) -0.0034(12) N3 0.0461(14) 0.0382(15) 0.0417(16) 0.0037(12) 0.0186(13) -0.0085(11) N1 0.0624(19) 0.0343(17) 0.0491(19) -0.0038(14) 0.0191(16) -0.0062(14) C10 0.0496(18) 0.0330(17) 0.0459(19) 0.0069(14) 0.0207(15) -0.0033(13) C5 0.056(2) 0.043(2) 0.052(2) 0.0087(16) 0.0247(18) -0.0025(16) C6 0.0522(18) 0.0331(17) 0.0435(19) -0.0002(14) 0.0218(15) 0.0006(14) C4 0.0530(19) 0.060(2) 0.055(2) 0.0118(18) 0.0328(18) 0.0066(17) C1 0.0472(16) 0.0313(16) 0.0352(17) 0.0052(12) 0.0191(14) 0.0036(12) C9 0.0418(16) 0.051(2) 0.049(2) 0.0102(16) 0.0223(15) 0.0026(15) C3 0.063(2) 0.045(2) 0.0384(19) 0.0057(15) 0.0236(17) 0.0145(16) C7 0.102(3) 0.067(3) 0.064(3) 0.002(2) 0.049(3) 0.028(3) C2 0.0502(17) 0.0305(16) 0.0328(17) 0.0047(12) 0.0149(14) 0.0042(13) C8 0.075(3) 0.061(3) 0.100(4) 0.009(3) 0.044(3) -0.018(2) C11 0.0436(17) 0.0431(19) 0.0396(19) 0.0085(14) 0.0117(15) -0.0007(14) C13 0.0483(17) 0.0380(18) 0.0433(19) -0.0003(14) 0.0203(15) -0.0059(14) C14 0.061(2) 0.050(2) 0.070(3) 0.0073(18) 0.036(2) 0.0046(17) C12 0.066(2) 0.051(2) 0.073(3) -0.006(2) 0.022(2) -0.0017(19) OW1 0.097(3) 0.163(5) 0.094(3) -0.002(3) 0.040(3) -0.031(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 2.240(3) . ? Ag1 N2 2.307(3) . ? Ag1 N1 2.365(3) . ? Ag1 O1 2.831(3) . ? Ag1 O3 2.814(3) 4_655 ? S1 O1 1.441(3) . ? S1 O2 1.447(3) . ? S1 O3 1.453(3) . ? S1 C1 1.774(3) . ? N2 C9 1.325(5) . ? N2 C11 1.334(5) . ? N3 C10 1.338(5) . ? N3 C13 1.341(4) . ? N1 C2 1.413(4) . ? N1 HN1 0.85(4) . ? N1 HN2 0.86(4) . ? C10 C13 1.378(5) 7_655 ? C10 H10 0.9300 . ? C5 C6 1.383(5) . ? C5 C4 1.389(6) . ? C5 C8 1.493(6) . ? C6 C1 1.381(4) . ? C6 H6 0.9300 . ? C4 C3 1.382(5) . ? C4 H4 0.9300 . ? C1 C2 1.400(4) . ? C9 C11 1.386(5) 5_655 ? C9 H9 0.9300 . ? C3 C2 1.395(5) . ? C3 C7 1.507(5) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C11 C9 1.386(5) 5_655 ? C11 C12 1.490(5) . ? C13 C10 1.378(5) 7_655 ? C13 C14 1.489(5) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? OW1 H2A 0.86(7) . ? OW1 H1A 0.88(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 N2 126.97(10) . . ? N3 Ag1 N1 129.82(11) . . ? N2 Ag1 N1 96.86(11) . . ? N1 Ag1 O1 70.2(1) . . ? O1 Ag1 O3 146.0(1) . 4_655 ? N1 Ag1 O3 85.9(1) . 4_655 ? N3 Ag1 O3 95.0(1) . 4_655 ? N2 Ag1 O3 114.5(1) . 4_655 ? O1 S1 O2 113.34(17) . . ? O1 S1 O3 112.71(19) . . ? O2 S1 O3 112.43(18) . . ? O1 S1 C1 105.46(15) . . ? O2 S1 C1 106.48(16) . . ? O3 S1 C1 105.63(16) . . ? C9 N2 C11 118.4(3) . . ? C9 N2 Ag1 115.2(2) . . ? C11 N2 Ag1 125.3(2) . . ? C10 N3 C13 117.6(3) . . ? C10 N3 Ag1 120.2(2) . . ? C13 N3 Ag1 122.2(2) . . ? C2 N1 Ag1 112.9(2) . . ? C2 N1 HN1 125.9(19) . . ? Ag1 N1 HN1 98(4) . . ? C2 N1 HN2 109(3) . . ? Ag1 N1 HN2 111(3) . . ? HN1 N1 HN2 98(4) . . ? N3 C10 C13 122.5(3) . 7_655 ? N3 C10 H10 118.8 . . ? C13 C10 H10 118.8 7_655 . ? C6 C5 C4 116.8(3) . . ? C6 C5 C8 121.1(4) . . ? C4 C5 C8 122.1(4) . . ? C1 C6 C5 121.5(3) . . ? C1 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C3 C4 C5 123.4(3) . . ? C3 C4 H4 118.3 . . ? C5 C4 H4 118.3 . . ? C6 C1 C2 120.6(3) . . ? C6 C1 S1 119.1(2) . . ? C2 C1 S1 120.3(2) . . ? N2 C9 C11 123.0(3) . 5_655 ? N2 C9 H9 118.5 . . ? C11 C9 H9 118.5 5_655 . ? C4 C3 C2 118.6(3) . . ? C4 C3 C7 120.9(4) . . ? C2 C3 C7 120.4(4) . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C2 C1 118.9(3) . . ? C3 C2 N1 121.3(3) . . ? C1 C2 N1 119.7(3) . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C11 C9 118.7(3) . 5_655 ? N2 C11 C12 119.8(3) . . ? C9 C11 C12 121.5(4) 5_655 . ? N3 C13 C10 119.9(3) . 7_655 ? N3 C13 C14 118.2(3) . . ? C10 C13 C14 121.9(3) 7_655 . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? H2A OW1 H1A 108(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ag1 N2 C9 81.2(3) . . . . ? N1 Ag1 N2 C9 -72.7(3) . . . . ? N3 Ag1 N2 C11 -111.3(3) . . . . ? N1 Ag1 N2 C11 94.9(3) . . . . ? N2 Ag1 N3 C10 -114.7(3) . . . . ? N1 Ag1 N3 C10 30.6(3) . . . . ? N2 Ag1 N3 C13 64.6(3) . . . . ? N1 Ag1 N3 C13 -150.1(2) . . . . ? N3 Ag1 N1 C2 -128.6(2) . . . . ? N2 Ag1 N1 C2 24.1(3) . . . . ? C13 N3 C10 C13 0.0(6) . . . 7_655 ? Ag1 N3 C10 C13 179.4(3) . . . 7_655 ? C4 C5 C6 C1 2.2(5) . . . . ? C8 C5 C6 C1 -178.6(4) . . . . ? C6 C5 C4 C3 -2.9(6) . . . . ? C8 C5 C4 C3 178.0(4) . . . . ? C5 C6 C1 C2 0.9(5) . . . . ? C5 C6 C1 S1 -176.4(3) . . . . ? O1 S1 C1 C6 118.8(3) . . . . ? O2 S1 C1 C6 -1.9(3) . . . . ? O3 S1 C1 C6 -121.6(3) . . . . ? O1 S1 C1 C2 -58.5(3) . . . . ? O2 S1 C1 C2 -179.2(3) . . . . ? O3 S1 C1 C2 61.1(3) . . . . ? C11 N2 C9 C11 -0.1(6) . . . 5_655 ? Ag1 N2 C9 C11 168.4(3) . . . 5_655 ? C5 C4 C3 C2 0.4(6) . . . . ? C5 C4 C3 C7 179.7(4) . . . . ? C4 C3 C2 C1 2.8(5) . . . . ? C7 C3 C2 C1 -176.5(3) . . . . ? C4 C3 C2 N1 178.6(3) . . . . ? C7 C3 C2 N1 -0.6(5) . . . . ? C6 C1 C2 C3 -3.4(5) . . . . ? S1 C1 C2 C3 173.9(3) . . . . ? C6 C1 C2 N1 -179.4(3) . . . . ? S1 C1 C2 N1 -2.1(4) . . . . ? Ag1 N1 C2 C3 -95.8(3) . . . . ? Ag1 N1 C2 C1 80.0(3) . . . . ? C9 N2 C11 C9 0.1(5) . . . 5_655 ? Ag1 N2 C11 C9 -167.1(2) . . . 5_655 ? C9 N2 C11 C12 -179.4(3) . . . . ? Ag1 N2 C11 C12 13.5(5) . . . . ? C10 N3 C13 C10 0.0(5) . . . 7_655 ? Ag1 N3 C13 C10 -179.4(2) . . . 7_655 ? C10 N3 C13 C14 178.7(3) . . . . ? Ag1 N3 C13 C14 -0.7(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 N1 HN1 O2 0.85(4) 2.06(4) 2.848(4) 153.5(13) 4_655 OW1 H2A O2 0.86(7) 2.16(6) 2.893(6) 142(9) . N1 HN2 O3 0.86(4) 2.37(4) 3.026(5) 134(4) . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.035 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.095 #=================================end