Electronic Supplementary Material for crystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm # PROCESSING SUMMARY #========================================================================== _journal_coden_Cambridge 1350 _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _publ_contact_author_name 'Ji-Wen Cai' _publ_contact_author_address ; School of Pharmaceutical Sciences Sun Yat-Sen University Guangzhou 510080 People's Republic of China ; _publ_contact_author_email puscjw@mail.sysu.edu.cn _publ_contact_author_fax '86 20 84114215' _publ_contact_author_phone '86 20 84114215' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_section_title ; Silver isonicotinamide Frameworks Extended by arenedisulfonate via Coordination Bonds, Hydrogen bonds and Ag-Ag Interactions ; loop_ _publ_author_name 'Jiwen Cai.' 'Cai-Hong Chen.' 'Zhao-Xun Lian.' data_1 _database_code_depnum_ccdc_archive 'CCDC 626403' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H30 Ag2 N8 O10 S2, 2(O)' _chemical_formula_sum 'C34 H34 Ag2 N8 O12 S2' _chemical_formula_weight 1026.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.622(4) _cell_length_b 10.286(5) _cell_length_c 24.546(13) _cell_angle_alpha 95.575(9) _cell_angle_beta 91.129(10) _cell_angle_gamma 95.722(10) _cell_volume 1904.9(17) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.212 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.565 _exptl_absorpt_correction_T_max 0.785 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11399 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.07 _reflns_number_total 8078 _reflns_number_gt 6290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT-PLUS (Bruker, 2003)' _computing_data_reduction SAINT-PLUS _computing_structure_solution 'SHELXTL (Bruker, 2005)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+2.9796P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0036(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8078 _refine_ls_number_parameters 524 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1388 _refine_ls_wR_factor_gt 0.1267 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.78090(5) 0.44000(3) 0.471547(13) 0.05968(14) Uani 1 1 d . . . Ag2 Ag 0.27614(5) 0.43835(3) 0.979544(13) 0.05864(14) Uani 1 1 d . . . S1 S 0.66749(13) 0.73958(8) 0.55534(3) 0.0389(2) Uani 1 1 d . . . S2 S 0.18331(13) 0.74201(8) 1.05155(3) 0.0389(2) Uani 1 1 d . . . O1 O 0.6515(5) 0.6545(3) 0.50480(12) 0.0610(8) Uani 1 1 d . . . O2 O 0.5976(4) 0.6763(3) 0.60130(13) 0.0596(8) Uani 1 1 d . . . O3 O 0.8449(4) 0.8034(3) 0.56590(12) 0.0498(7) Uani 1 1 d . . . O4 O 0.1781(5) 0.6620(3) 0.99947(12) 0.0699(10) Uani 1 1 d . . . O5 O 0.1178(4) 0.6709(3) 1.09586(13) 0.0602(8) Uani 1 1 d . . . O6 O 0.3553(4) 0.8130(3) 1.06441(15) 0.0612(8) Uani 1 1 d . . . O7 O 0.7128(5) 0.1449(3) 0.71884(11) 0.0594(8) Uani 1 1 d . . . O8 O 0.8588(4) 0.7332(3) 0.22067(13) 0.0603(8) Uani 1 1 d . . . O9 O 0.6627(4) 0.5161(3) 0.72606(12) 0.0610(8) Uani 1 1 d . . . O10 O 0.1483(4) 0.1393(3) 1.22482(12) 0.0597(8) Uani 1 1 d . . . N1 N 0.7878(4) 0.3284(3) 0.54030(13) 0.0429(7) Uani 1 1 d . . . N2 N 0.8275(5) 0.5022(3) 0.39132(13) 0.0468(7) Uani 1 1 d . . . N3 N 0.3445(4) 0.4845(3) 0.89835(12) 0.0438(7) Uani 1 1 d . . . N4 N 0.2650(4) 0.3262(3) 1.04882(13) 0.0419(7) Uani 1 1 d . . . N5 N 0.8202(5) -0.0247(3) 0.67038(14) 0.0570(9) Uani 1 1 d . . . H5A H 0.8199 -0.0700 0.6980 0.068 Uiso 1 1 calc R . . H5B H 0.8560 -0.0564 0.6393 0.068 Uiso 1 1 calc R . . N6 N 1.0673(5) 0.5973(3) 0.20775(13) 0.0524(8) Uani 1 1 d . . . H6A H 1.0932 0.6241 0.1765 0.063 Uiso 1 1 calc R . . H6B H 1.1232 0.5373 0.2202 0.063 Uiso 1 1 calc R . . N7 N 0.4764(4) 0.6670(3) 0.71557(13) 0.0491(8) Uani 1 1 d . . . H7A H 0.5192 0.6842 0.6846 0.059 Uiso 1 1 calc R . . H7B H 0.3913 0.7082 0.7287 0.059 Uiso 1 1 calc R . . N8 N 0.2592(5) -0.0305(3) 1.17735(14) 0.0605(10) Uani 1 1 d . . . H8A H 0.2511 -0.0775 1.2045 0.073 Uiso 1 1 calc R . . H8B H 0.3004 -0.0612 1.1469 0.073 Uiso 1 1 calc R . . C1 C 0.7042(6) 0.3619(4) 0.58618(16) 0.0488(9) Uani 1 1 d . . . H1 H 0.6502 0.4394 0.5888 0.059 Uiso 1 1 calc R . . C2 C 0.6948(6) 0.2866(4) 0.62958(16) 0.0467(9) Uani 1 1 d . . . H2 H 0.6367 0.3137 0.6610 0.056 Uiso 1 1 calc R . . C3 C 0.7725(5) 0.1703(3) 0.62619(14) 0.0368(7) Uani 1 1 d . . . C4 C 0.8569(5) 0.1344(4) 0.57880(15) 0.0409(8) Uani 1 1 d . . . H4 H 0.9085 0.0559 0.5748 0.049 Uiso 1 1 calc R . . C5 C 0.8641(5) 0.2164(4) 0.53727(15) 0.0421(8) Uani 1 1 d . . . H5 H 0.9246 0.1927 0.5059 0.050 Uiso 1 1 calc R . . C6 C 0.9217(6) 0.4357(4) 0.35492(17) 0.0507(9) Uani 1 1 d . . . H6 H 0.9635 0.3585 0.3641 0.061 Uiso 1 1 calc R . . C7 C 0.9594(5) 0.4773(4) 0.30421(17) 0.0473(9) Uani 1 1 d . . . H7 H 1.0233 0.4276 0.2796 0.057 Uiso 1 1 calc R . . C8 C 0.9012(5) 0.5937(4) 0.29032(15) 0.0396(8) Uani 1 1 d . . . C9 C 0.8019(6) 0.6603(4) 0.32749(16) 0.0486(9) Uani 1 1 d . . . H9 H 0.7584 0.7377 0.3193 0.058 Uiso 1 1 calc R . . C10 C 0.7673(6) 0.6119(4) 0.37673(16) 0.0526(10) Uani 1 1 d . . . H10 H 0.6985 0.6577 0.4012 0.063 Uiso 1 1 calc R . . C11 C 0.4355(5) 0.4028(4) 0.86680(16) 0.0445(8) Uani 1 1 d . . . H11 H 0.4581 0.3236 0.8794 0.053 Uiso 1 1 calc R . . C12 C 0.4966(5) 0.4310(4) 0.81669(16) 0.0442(8) Uani 1 1 d . . . H12 H 0.5604 0.3722 0.7962 0.053 Uiso 1 1 calc R . . C13 C 0.4627(4) 0.5480(3) 0.79677(14) 0.0359(7) Uani 1 1 d . . . C14 C 0.3647(5) 0.6303(4) 0.82830(14) 0.0409(8) Uani 1 1 d . . . H14 H 0.3366 0.7085 0.8159 0.049 Uiso 1 1 calc R . . C15 C 0.3086(5) 0.5955(4) 0.87854(15) 0.0453(9) Uani 1 1 d . . . H15 H 0.2429 0.6520 0.8995 0.054 Uiso 1 1 calc R . . C16 C 0.3482(5) 0.2174(4) 1.04852(15) 0.0417(8) Uani 1 1 d . . . H16 H 0.4199 0.1966 1.0194 0.050 Uiso 1 1 calc R . . C17 C 0.3319(5) 0.1353(4) 1.08949(15) 0.0415(8) Uani 1 1 d . . . H17 H 0.3892 0.0593 1.0876 0.050 Uiso 1 1 calc R . . C18 C 0.2289(5) 0.1673(3) 1.13360(14) 0.0375(7) Uani 1 1 d . . . C19 C 0.1438(6) 0.2798(4) 1.13421(16) 0.0457(9) Uani 1 1 d . . . H19 H 0.0731 0.3037 1.1632 0.055 Uiso 1 1 calc R . . C20 C 0.1651(6) 0.3560(4) 1.09131(16) 0.0466(9) Uani 1 1 d . . . H20 H 0.1074 0.4316 1.0920 0.056 Uiso 1 1 calc R . . C21 C 0.7656(5) 0.0939(4) 0.67558(15) 0.0432(8) Uani 1 1 d . . . C22 C 0.9421(5) 0.6480(4) 0.23647(15) 0.0417(8) Uani 1 1 d . . . C23 C 0.5414(5) 0.5774(4) 0.74307(14) 0.0401(8) Uani 1 1 d . . . C24 C 0.2084(5) 0.0892(4) 1.18244(15) 0.0430(8) Uani 1 1 d . . . C25 C 0.6788(5) 0.9263(4) 0.46062(15) 0.0397(8) Uani 1 1 d . . . H25 H 0.7507 0.8588 0.4625 0.048 Uiso 1 1 calc R . . C26 C 0.5549(4) 0.9474(3) 0.50160(13) 0.0328(7) Uani 1 1 d . . . C27 C 0.5319(4) 0.8691(3) 0.54645(14) 0.0347(7) Uani 1 1 d . . . C28 C 0.4108(5) 0.8941(4) 0.58533(15) 0.0410(8) Uani 1 1 d . . . H28 H 0.3985 0.8425 0.6144 0.049 Uiso 1 1 calc R . . C29 C 0.3044(5) 0.9973(4) 0.58179(16) 0.0452(9) Uani 1 1 d . . . H29 H 0.2223 1.0136 0.6085 0.054 Uiso 1 1 calc R . . C30 C 0.1880(5) 0.9391(4) 0.96058(15) 0.0400(8) Uani 1 1 d . . . H30 H 0.2641 0.8741 0.9614 0.048 Uiso 1 1 calc R . . C31 C 0.0580(4) 0.9495(3) 1.00090(13) 0.0313(7) Uani 1 1 d . . . C32 C 0.0372(4) 0.8654(3) 1.04381(13) 0.0332(7) Uani 1 1 d . . . C33 C -0.0897(5) 0.8791(3) 1.08187(14) 0.0392(8) Uani 1 1 d . . . H33 H -0.1006 0.8232 1.1094 0.047 Uiso 1 1 calc R . . C34 C -0.2038(5) 0.9777(4) 1.07936(16) 0.0458(9) Uani 1 1 d . . . H34 H -0.2907 0.9863 1.1052 0.055 Uiso 1 1 calc R . . OW1 O -0.2082(6) 0.1603(4) 1.2548(2) 0.1111(17) Uani 1 1 d . . . OW2 O 0.6353(7) 0.9161(5) 0.2472(4) 0.207(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 0.0881(3) 0.0533(2) 0.04053(19) 0.01939(14) 0.00400(16) 0.00699(18) Ag2 0.0869(3) 0.0513(2) 0.04181(19) 0.02135(14) 0.00428(16) 0.01036(17) S1 0.0541(5) 0.0324(4) 0.0338(4) 0.0095(3) 0.0058(4) 0.0156(4) S2 0.0552(5) 0.0333(4) 0.0327(4) 0.0112(3) 0.0033(4) 0.0186(4) O1 0.099(2) 0.0398(15) 0.0462(16) -0.0031(12) -0.0054(16) 0.0231(16) O2 0.081(2) 0.0490(16) 0.0588(18) 0.0313(14) 0.0216(15) 0.0267(15) O3 0.0491(16) 0.0511(16) 0.0531(16) 0.0100(13) 0.0023(13) 0.0197(13) O4 0.122(3) 0.0524(18) 0.0413(15) 0.0002(13) -0.0025(17) 0.0435(19) O5 0.086(2) 0.0498(16) 0.0555(17) 0.0303(14) 0.0204(15) 0.0316(15) O6 0.0493(17) 0.0532(17) 0.087(2) 0.0241(16) -0.0066(16) 0.0178(14) O7 0.093(2) 0.0551(17) 0.0343(14) 0.0120(12) 0.0042(14) 0.0213(16) O8 0.0600(18) 0.070(2) 0.0583(18) 0.0298(15) 0.0039(14) 0.0220(15) O9 0.0636(18) 0.076(2) 0.0525(17) 0.0185(15) 0.0197(14) 0.0371(16) O10 0.085(2) 0.0605(18) 0.0404(15) 0.0202(13) 0.0099(14) 0.0221(16) N1 0.0518(18) 0.0365(16) 0.0428(16) 0.0143(13) 0.0015(14) 0.0062(13) N2 0.057(2) 0.0510(19) 0.0329(15) 0.0088(14) 0.0030(14) 0.0054(15) N3 0.0547(19) 0.0448(17) 0.0337(15) 0.0105(13) 0.0012(13) 0.0081(14) N4 0.0543(18) 0.0344(15) 0.0389(15) 0.0128(12) -0.0013(13) 0.0059(13) N5 0.091(3) 0.0475(19) 0.0369(17) 0.0122(14) -0.0050(17) 0.0239(19) N6 0.061(2) 0.061(2) 0.0398(17) 0.0178(15) 0.0089(15) 0.0150(17) N7 0.0513(19) 0.057(2) 0.0445(17) 0.0198(15) 0.0108(14) 0.0183(16) N8 0.098(3) 0.047(2) 0.0411(18) 0.0179(15) -0.0043(18) 0.0210(19) C1 0.070(3) 0.039(2) 0.042(2) 0.0102(16) 0.0083(18) 0.0193(18) C2 0.062(2) 0.042(2) 0.0385(19) 0.0070(16) 0.0076(17) 0.0152(18) C3 0.0410(18) 0.0364(18) 0.0334(16) 0.0053(14) -0.0040(14) 0.0059(14) C4 0.0433(19) 0.0409(19) 0.0412(18) 0.0092(15) -0.0007(15) 0.0129(15) C5 0.045(2) 0.045(2) 0.0369(18) 0.0032(15) 0.0051(15) 0.0070(16) C6 0.056(2) 0.051(2) 0.048(2) 0.0183(18) 0.0061(18) 0.0102(19) C7 0.048(2) 0.050(2) 0.046(2) 0.0118(17) 0.0094(17) 0.0096(17) C8 0.0356(18) 0.045(2) 0.0379(18) 0.0073(15) -0.0022(14) -0.0004(15) C9 0.060(2) 0.048(2) 0.0400(19) 0.0084(17) 0.0023(17) 0.0129(18) C10 0.071(3) 0.052(2) 0.0364(19) 0.0053(17) 0.0069(18) 0.014(2) C11 0.052(2) 0.0396(19) 0.045(2) 0.0155(16) -0.0016(16) 0.0090(16) C12 0.044(2) 0.041(2) 0.050(2) 0.0074(16) 0.0051(16) 0.0140(16) C13 0.0342(17) 0.0387(18) 0.0357(17) 0.0053(14) -0.0009(13) 0.0062(14) C14 0.050(2) 0.0400(19) 0.0351(17) 0.0091(15) 0.0001(15) 0.0126(16) C15 0.055(2) 0.047(2) 0.0370(18) 0.0076(16) 0.0055(16) 0.0165(18) C16 0.048(2) 0.0395(19) 0.0397(18) 0.0078(15) 0.0026(15) 0.0092(16) C17 0.045(2) 0.0368(18) 0.0446(19) 0.0093(15) -0.0022(16) 0.0105(15) C18 0.0430(19) 0.0339(17) 0.0358(17) 0.0081(14) -0.0065(14) 0.0026(14) C19 0.061(2) 0.0394(19) 0.0391(19) 0.0072(15) 0.0053(17) 0.0145(17) C20 0.066(2) 0.0351(19) 0.043(2) 0.0096(15) 0.0039(18) 0.0163(17) C21 0.055(2) 0.043(2) 0.0337(17) 0.0095(15) -0.0037(15) 0.0080(17) C22 0.0424(19) 0.043(2) 0.0396(18) 0.0089(15) -0.0025(15) -0.0003(16) C23 0.0401(19) 0.046(2) 0.0355(17) 0.0038(15) 0.0022(14) 0.0086(15) C24 0.052(2) 0.042(2) 0.0362(18) 0.0101(15) -0.0078(16) 0.0055(16) C25 0.044(2) 0.0398(19) 0.0385(18) 0.0081(15) 0.0057(15) 0.0172(15) C26 0.0366(17) 0.0293(16) 0.0333(16) 0.0050(13) 0.0002(13) 0.0059(13) C27 0.0394(18) 0.0304(16) 0.0352(16) 0.0055(13) -0.0006(13) 0.0065(13) C28 0.048(2) 0.0417(19) 0.0369(17) 0.0132(15) 0.0044(15) 0.0105(16) C29 0.047(2) 0.054(2) 0.0401(19) 0.0113(17) 0.0124(16) 0.0201(17) C30 0.0435(19) 0.0419(19) 0.0388(18) 0.0112(15) 0.0046(15) 0.0178(15) C31 0.0355(17) 0.0308(16) 0.0296(15) 0.0084(12) -0.0007(12) 0.0077(13) C32 0.0380(17) 0.0302(16) 0.0327(16) 0.0084(13) -0.0014(13) 0.0062(13) C33 0.047(2) 0.0373(18) 0.0365(17) 0.0151(14) 0.0015(15) 0.0083(15) C34 0.046(2) 0.054(2) 0.0430(19) 0.0188(17) 0.0132(16) 0.0189(17) OW1 0.089(3) 0.077(3) 0.179(5) 0.027(3) 0.034(3) 0.043(2) OW2 0.095(4) 0.077(3) 0.460(13) 0.038(5) 0.087(6) 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 N1 2.134(3) . ? Ag1 N2 2.154(3) . ? Ag1 O1 2.573(3) . ? Ag2 N4 2.144(3) . ? Ag2 N3 2.155(3) . ? Ag2 O4 2.496(3) . ? S1 O2 1.441(3) . ? S1 O1 1.443(3) . ? S1 O3 1.450(3) . ? S1 C27 1.793(3) . ? S2 O5 1.439(3) . ? S2 O6 1.449(3) . ? S2 O4 1.449(3) . ? S2 C32 1.791(3) . ? O7 C21 1.231(5) . ? O8 C22 1.220(5) . ? O9 C23 1.228(4) . ? O10 C24 1.233(5) . ? N1 C5 1.337(5) . ? N1 C1 1.338(5) . ? N2 C6 1.336(5) . ? N2 C10 1.337(5) . ? N3 C15 1.334(5) . ? N3 C11 1.340(5) . ? N4 C20 1.334(5) . ? N4 C16 1.339(5) . ? N5 C21 1.323(5) . ? N5 H5A 0.8600 . ? N5 H5B 0.8600 . ? N6 C22 1.317(5) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? N7 C23 1.323(5) . ? N7 H7A 0.8600 . ? N7 H7B 0.8600 . ? N8 C24 1.321(5) . ? N8 H8A 0.8600 . ? N8 H8B 0.8600 . ? C1 C2 1.376(5) . ? C1 H1 0.9300 . ? C2 C3 1.383(5) . ? C2 H2 0.9300 . ? C3 C4 1.377(5) . ? C3 C21 1.507(5) . ? C4 C5 1.383(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.381(5) . ? C6 H6 0.9300 . ? C7 C8 1.388(5) . ? C7 H7 0.9300 . ? C8 C9 1.373(5) . ? C8 C22 1.510(5) . ? C9 C10 1.372(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.371(5) . ? C11 H11 0.9300 . ? C12 C13 1.387(5) . ? C12 H12 0.9300 . ? C13 C14 1.377(5) . ? C13 C23 1.503(5) . ? C14 C15 1.381(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.375(5) . ? C16 H16 0.9300 . ? C17 C18 1.383(5) . ? C17 H17 0.9300 . ? C18 C19 1.381(5) . ? C18 C24 1.509(5) . ? C19 C20 1.375(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C25 C29 1.364(5) 2_676 ? C25 C26 1.410(5) . ? C25 H25 0.9300 . ? C26 C27 1.429(5) . ? C26 C26 1.439(6) 2_676 ? C27 C28 1.365(5) . ? C28 C29 1.407(5) . ? C28 H28 0.9300 . ? C29 C25 1.364(5) 2_676 ? C29 H29 0.9300 . ? C30 C34 1.361(5) 2_577 ? C30 C31 1.418(5) . ? C30 H30 0.9300 . ? C31 C32 1.428(4) . ? C31 C31 1.433(6) 2_577 ? C32 C33 1.366(5) . ? C33 C34 1.405(5) . ? C33 H33 0.9300 . ? C34 C30 1.361(5) 2_577 ? C34 H34 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 N1 Ag1 N2 160.61(13) . . ? N1 Ag1 O1 106.61(12) . . ? N2 Ag1 O1 92.43(12) . . ? N4 Ag2 N3 156.55(12) . . ? N4 Ag2 O4 113.40(12) . . ? N3 Ag2 O4 89.66(12) . . ? O2 S1 O1 113.0(2) . . ? O2 S1 O3 112.95(19) . . ? O1 S1 O3 112.5(2) . . ? O2 S1 C27 105.70(17) . . ? O1 S1 C27 106.34(17) . . ? O3 S1 C27 105.62(16) . . ? O5 S2 O6 112.3(2) . . ? O5 S2 O4 113.4(2) . . ? O6 S2 O4 112.3(2) . . ? O5 S2 C32 106.29(17) . . ? O6 S2 C32 105.43(17) . . ? O4 S2 C32 106.33(17) . . ? S1 O1 Ag1 133.80(18) . . ? S2 O4 Ag2 128.16(17) . . ? C5 N1 C1 117.7(3) . . ? C5 N1 Ag1 120.8(3) . . ? C1 N1 Ag1 121.3(2) . . ? C6 N2 C10 117.4(3) . . ? C6 N2 Ag1 121.7(3) . . ? C10 N2 Ag1 120.8(3) . . ? C15 N3 C11 117.5(3) . . ? C15 N3 Ag2 122.8(3) . . ? C11 N3 Ag2 119.6(2) . . ? C20 N4 C16 118.0(3) . . ? C20 N4 Ag2 121.5(2) . . ? C16 N4 Ag2 120.4(3) . . ? C21 N5 H5A 120.0 . . ? C21 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? C22 N6 H6A 120.0 . . ? C22 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C23 N7 H7A 120.0 . . ? C23 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? C24 N8 H8A 120.0 . . ? C24 N8 H8B 120.0 . . ? H8A N8 H8B 120.0 . . ? N1 C1 C2 122.7(3) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 119.5(4) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 118.0(3) . . ? C4 C3 C21 124.2(3) . . ? C2 C3 C21 117.7(3) . . ? C3 C4 C5 119.2(3) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 122.8(3) . . ? N1 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? N2 C6 C7 122.5(4) . . ? N2 C6 H6 118.7 . . ? C7 C6 H6 118.7 . . ? C6 C7 C8 119.5(4) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 117.7(3) . . ? C9 C8 C22 119.6(3) . . ? C7 C8 C22 122.7(3) . . ? C10 C9 C8 119.6(4) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? N2 C10 C9 123.3(4) . . ? N2 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? N3 C11 C12 122.8(3) . . ? N3 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C11 C12 C13 119.5(3) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 117.8(3) . . ? C14 C13 C23 124.9(3) . . ? C12 C13 C23 117.3(3) . . ? C13 C14 C15 119.3(3) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? N3 C15 C14 123.0(4) . . ? N3 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? N4 C16 C17 122.7(4) . . ? N4 C16 H16 118.6 . . ? C17 C16 H16 118.6 . . ? C16 C17 C18 118.9(3) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C19 C18 C17 118.5(3) . . ? C19 C18 C24 117.5(3) . . ? C17 C18 C24 123.9(3) . . ? C20 C19 C18 119.0(4) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? N4 C20 C19 122.8(3) . . ? N4 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? O7 C21 N5 123.2(3) . . ? O7 C21 C3 119.0(3) . . ? N5 C21 C3 117.9(3) . . ? O8 C22 N6 122.7(4) . . ? O8 C22 C8 120.4(4) . . ? N6 C22 C8 117.0(3) . . ? O9 C23 N7 122.4(4) . . ? O9 C23 C13 118.6(3) . . ? N7 C23 C13 119.0(3) . . ? O10 C24 N8 123.4(4) . . ? O10 C24 C18 119.3(3) . . ? N8 C24 C18 117.3(3) . . ? C29 C25 C26 121.4(3) 2_676 . ? C29 C25 H25 119.3 2_676 . ? C26 C25 H25 119.3 . . ? C25 C26 C27 123.3(3) . . ? C25 C26 C26 118.8(4) . 2_676 ? C27 C26 C26 117.9(4) . 2_676 ? C28 C27 C26 121.1(3) . . ? C28 C27 S1 117.6(3) . . ? C26 C27 S1 121.3(3) . . ? C27 C28 C29 120.5(3) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C25 C29 C28 120.3(3) 2_676 . ? C25 C29 H29 119.8 2_676 . ? C28 C29 H29 119.8 . . ? C34 C30 C31 121.5(3) 2_577 . ? C34 C30 H30 119.2 2_577 . ? C31 C30 H30 119.2 . . ? C30 C31 C32 123.5(3) . . ? C30 C31 C31 118.6(4) . 2_577 ? C32 C31 C31 117.9(4) . 2_577 ? C33 C32 C31 121.6(3) . . ? C33 C32 S2 117.3(2) . . ? C31 C32 S2 121.1(2) . . ? C32 C33 C34 120.0(3) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C30 C34 C33 120.4(3) 2_577 . ? C30 C34 H34 119.8 2_577 . ? C33 C34 H34 119.8 . . ? 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 N5 H5A O10 0.86 2.10 2.947(4) 166.2 2_657 N5 H5B O3 0.86 2.19 2.991(5) 154.7 1_545 N6 H6A O5 0.86 2.09 2.941(5) 170.6 1_654 N6 H6B O9 0.86 2.22 2.991(4) 148.9 2_766 N7 H7A O2 0.86 2.14 2.978(5) 165.3 . N7 H7B OW1 0.86 2.06 2.897(5) 165.0 2_567 N8 H8A O7 0.86 2.09 2.922(4) 162.3 2_657 _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.07 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.953 _refine_diff_density_min -1.105 _refine_diff_density_rms 0.094 # Attachment 'Compound_2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 626404' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 Ag N4 O2, 0.5(C10 H6 O6 S2), 2(H2 O)' _chemical_formula_sum 'C17 H19 Ag N4 O7 S' _chemical_formula_weight 531.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.281(4) _cell_length_b 10.145(5) _cell_length_c 12.334(7) _cell_angle_alpha 78.948(9) _cell_angle_beta 80.966(10) _cell_angle_gamma 82.189(9) _cell_volume 998.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 1.163 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.578 _exptl_absorpt_correction_T_max 0.792 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 6556 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.10 _reflns_number_total 4223 _reflns_number_gt 3644 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT-PLUS (Bruker, 2003)' _computing_data_reduction SAINT-PLUS _computing_structure_solution 'SHELXTL (Bruker, 2005)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.6184P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0545(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4223 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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 0.32532(3) 0.41575(2) 0.536428(17) 0.05027(11) Uani 1 1 d . . . S1 S 0.61551(7) 0.24271(6) 0.34200(5) 0.03357(14) Uani 1 1 d . . . O1 O 0.7188(3) -0.07557(19) 0.92242(19) 0.0632(6) Uani 1 1 d . . . O2 O -0.1261(3) 0.8954(2) 0.17439(18) 0.0642(6) Uani 1 1 d . . . O3 O 0.4783(2) 0.1668(2) 0.38537(18) 0.0536(5) Uani 1 1 d . . . O4 O 0.6075(3) 0.36208(18) 0.39083(19) 0.0551(5) Uani 1 1 d . . . O5 O 0.6415(3) 0.2729(2) 0.22125(16) 0.0576(5) Uani 1 1 d . . . OW1 O 0.6432(4) -0.3260(2) 0.8939(2) 0.0766(7) Uani 1 1 d . . . H1A H 0.7043 -0.2639 0.8881 0.18(3) Uiso 1 1 d R . . H1B H 0.5614 -0.3105 0.8580 0.099(15) Uiso 1 1 d R . . OW2 O 0.7801(4) 0.4362(3) 0.0250(3) 0.1191(14) Uani 1 1 d . . . H2A H 0.7375 0.4038 0.0906 0.15(2) Uiso 1 1 d R . . H2B H 0.7156 0.4922 -0.0123 0.098(15) Uiso 1 1 d R . . N1 N 0.4276(3) 0.2936(2) 0.67610(17) 0.0405(5) Uani 1 1 d . . . N2 N 0.1862(3) 0.5311(2) 0.41114(17) 0.0395(5) Uani 1 1 d . . . N3 N 0.7171(3) 0.0941(2) 1.0130(2) 0.0548(6) Uani 1 1 d . . . H3A H 0.7696 0.0434 1.0632 0.066 Uiso 1 1 calc R . . H3B H 0.6885 0.1780 1.0165 0.066 Uiso 1 1 calc R . . N4 N -0.0704(4) 0.7405(3) 0.0631(2) 0.0628(7) Uani 1 1 d . . . H4A H -0.1183 0.7917 0.0108 0.075 Uiso 1 1 calc R . . H4B H -0.0257 0.6609 0.0546 0.075 Uiso 1 1 calc R . . C1 C 0.4730(4) 0.3474(3) 0.7559(2) 0.0446(6) Uani 1 1 d . . . H1 H 0.4494 0.4400 0.7539 0.054 Uiso 1 1 calc R . . C2 C 0.5527(3) 0.2726(2) 0.8406(2) 0.0424(6) Uani 1 1 d . . . H2 H 0.5819 0.3140 0.8946 0.051 Uiso 1 1 calc R . . C3 C 0.5890(3) 0.1346(2) 0.84459(19) 0.0355(5) Uani 1 1 d . . . C4 C 0.5401(3) 0.0785(3) 0.7636(2) 0.0431(6) Uani 1 1 d . . . H4 H 0.5613 -0.0140 0.7643 0.052 Uiso 1 1 calc R . . C5 C 0.4599(3) 0.1602(3) 0.6818(2) 0.0449(6) Uani 1 1 d . . . H5 H 0.4266 0.1207 0.6280 0.054 Uiso 1 1 calc R . . C6 C 0.6807(3) 0.0433(3) 0.9309(2) 0.0394(5) Uani 1 1 d . . . C7 C 0.1559(4) 0.4805(3) 0.3252(2) 0.0468(6) Uani 1 1 d . . . H7 H 0.1915 0.3902 0.3219 0.056 Uiso 1 1 calc R . . C8 C 0.0743(4) 0.5559(3) 0.2414(2) 0.0459(6) Uani 1 1 d . . . H8 H 0.0553 0.5169 0.1829 0.055 Uiso 1 1 calc R . . C9 C 0.0207(3) 0.6900(2) 0.2447(2) 0.0361(5) Uani 1 1 d . . . C10 C 0.0507(4) 0.7416(3) 0.3339(2) 0.0463(6) Uani 1 1 d . . . H10 H 0.0149 0.8313 0.3398 0.056 Uiso 1 1 calc R . . C11 C 0.1331(4) 0.6609(3) 0.4138(2) 0.0483(6) Uani 1 1 d . . . H11 H 0.1534 0.6980 0.4730 0.058 Uiso 1 1 calc R . . C12 C -0.0656(3) 0.7840(3) 0.1562(2) 0.0412(6) Uani 1 1 d . . . C13 C 0.7943(3) 0.1422(2) 0.38554(19) 0.0308(4) Uani 1 1 d . . . C14 C 0.7803(3) 0.0467(2) 0.47924(19) 0.0313(5) Uani 1 1 d . . . H14 H 0.6769 0.0235 0.5126 0.038 Uiso 1 1 calc R . . C15 C 0.9222(3) -0.0178(2) 0.52634(19) 0.0301(4) Uani 1 1 d . . . C16 C 0.9494(3) 0.1745(2) 0.3306(2) 0.0379(5) Uani 1 1 d . . . H16 H 0.9576 0.2370 0.2647 0.045 Uiso 1 1 calc R . . C17 C 1.0876(3) 0.1143(2) 0.3740(2) 0.0375(5) Uani 1 1 d . . . H17 H 1.1899 0.1368 0.3378 0.045 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 0.05549(16) 0.04935(15) 0.04300(14) 0.00520(9) -0.02132(10) 0.00293(9) S1 0.0319(3) 0.0301(3) 0.0377(3) 0.0008(2) -0.0128(2) 0.0000(2) O1 0.0851(16) 0.0362(10) 0.0743(15) -0.0035(10) -0.0496(13) 0.0086(10) O2 0.0835(16) 0.0520(12) 0.0545(12) -0.0110(10) -0.0293(11) 0.0273(11) O3 0.0338(9) 0.0517(11) 0.0709(13) 0.0106(10) -0.0170(9) -0.0085(8) O4 0.0569(12) 0.0349(9) 0.0772(14) -0.0134(9) -0.0286(10) 0.0101(8) O5 0.0518(11) 0.0756(14) 0.0389(10) 0.0058(9) -0.0163(9) 0.0052(10) OW1 0.0949(19) 0.0544(13) 0.0902(18) -0.0126(12) -0.0528(16) 0.0039(13) OW2 0.119(3) 0.099(2) 0.088(2) 0.0279(18) 0.0360(19) 0.047(2) N1 0.0450(12) 0.0384(11) 0.0349(11) -0.0004(9) -0.0099(9) 0.0036(9) N2 0.0454(12) 0.0378(11) 0.0352(11) -0.0020(8) -0.0153(9) 0.0009(9) N3 0.0718(17) 0.0475(13) 0.0459(13) -0.0081(10) -0.0280(12) 0.0135(12) N4 0.0875(19) 0.0509(14) 0.0551(15) -0.0121(12) -0.0435(14) 0.0173(13) C1 0.0592(16) 0.0307(12) 0.0405(13) -0.0001(10) -0.0108(12) 0.0030(11) C2 0.0570(16) 0.0359(13) 0.0344(12) -0.0046(10) -0.0124(11) -0.0007(11) C3 0.0354(12) 0.0338(12) 0.0337(12) -0.0003(9) -0.0053(9) 0.0013(9) C4 0.0518(15) 0.0333(12) 0.0449(14) -0.0062(11) -0.0166(12) 0.0039(11) C5 0.0529(15) 0.0427(14) 0.0406(13) -0.0087(11) -0.0158(12) 0.0027(11) C6 0.0376(13) 0.0368(13) 0.0408(13) 0.0023(10) -0.0107(10) 0.0000(10) C7 0.0634(17) 0.0315(12) 0.0462(15) -0.0040(11) -0.0192(13) 0.0020(11) C8 0.0633(17) 0.0355(13) 0.0435(14) -0.0079(11) -0.0233(12) -0.0020(12) C9 0.0332(12) 0.0384(12) 0.0364(12) -0.0031(10) -0.0104(9) -0.0008(9) C10 0.0572(16) 0.0383(13) 0.0458(15) -0.0142(11) -0.0196(12) 0.0109(12) C11 0.0610(17) 0.0460(15) 0.0428(14) -0.0151(12) -0.0230(13) 0.0062(12) C12 0.0360(13) 0.0430(14) 0.0441(14) -0.0037(11) -0.0140(10) 0.0019(10) C13 0.0292(11) 0.0259(10) 0.0377(12) -0.0044(9) -0.0105(9) 0.0002(8) C14 0.0281(11) 0.0272(10) 0.0378(12) -0.0023(9) -0.0073(9) -0.0018(8) C15 0.0305(11) 0.0243(10) 0.0346(11) -0.0032(8) -0.0058(9) -0.0010(8) C16 0.0386(13) 0.0339(12) 0.0368(12) 0.0053(10) -0.0067(10) -0.0029(10) C17 0.0317(12) 0.0348(12) 0.0413(13) 0.0027(10) -0.0026(10) -0.0033(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 N1 2.139(2) . ? Ag1 N2 2.141(2) . ? Ag1 O4 2.774(3) . ? S1 O3 1.435(2) . ? S1 O4 1.442(2) . ? S1 O5 1.449(2) . ? S1 C13 1.775(2) . ? O1 C6 1.225(3) . ? O2 C12 1.219(3) . ? OW1 H1A 0.8460 . ? OW1 H1B 0.8478 . ? OW2 H2A 0.8526 . ? OW2 H2B 0.8460 . ? N1 C5 1.334(3) . ? N1 C1 1.336(3) . ? N2 C7 1.333(3) . ? N2 C11 1.336(3) . ? N3 C6 1.310(4) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? N4 C12 1.314(4) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? C1 C2 1.371(4) . ? C1 H1 0.9300 . ? C2 C3 1.384(3) . ? C2 H2 0.9300 . ? C3 C4 1.375(4) . ? C3 C6 1.501(3) . ? C4 C5 1.374(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C8 1.374(4) . ? C7 H7 0.9300 . ? C8 C9 1.378(4) . ? C8 H8 0.9300 . ? C9 C10 1.375(4) . ? C9 C12 1.507(3) . ? C10 C11 1.363(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 C14 1.359(3) . ? C13 C16 1.405(3) . ? C14 C15 1.416(3) . ? C14 H14 0.9300 . ? C15 C15 1.409(4) 2_756 ? C15 C17 1.416(3) 2_756 ? C16 C17 1.358(3) . ? C16 H16 0.9300 . ? C17 C15 1.416(3) 2_756 ? C17 H17 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 N1 Ag1 N2 170.97(8) . . ? N1 Ag1 O4 92.47(8) . . ? N2 Ag1 O4 95.62(8) . . ? O3 S1 O4 112.55(14) . . ? O3 S1 O5 112.95(13) . . ? O4 S1 O5 112.00(13) . . ? O3 S1 C13 107.41(11) . . ? O4 S1 C13 103.92(11) . . ? O5 S1 C13 107.35(12) . . ? S1 O4 Ag1 115.89(12) . . ? H1A OW1 H1B 118.4 . . ? H2A OW2 H2B 114.5 . . ? C5 N1 C1 117.4(2) . . ? C5 N1 Ag1 120.34(17) . . ? C1 N1 Ag1 122.05(17) . . ? C7 N2 C11 117.2(2) . . ? C7 N2 Ag1 122.51(17) . . ? C11 N2 Ag1 120.19(16) . . ? C6 N3 H3A 120.0 . . ? C6 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C12 N4 H4A 120.0 . . ? C12 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? N1 C1 C2 123.2(2) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 119.1(2) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 117.9(2) . . ? C4 C3 C6 118.3(2) . . ? C2 C3 C6 123.8(2) . . ? C5 C4 C3 119.5(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 122.8(2) . . ? N1 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? O1 C6 N3 122.3(2) . . ? O1 C6 C3 119.1(2) . . ? N3 C6 C3 118.6(2) . . ? N2 C7 C8 122.8(2) . . ? N2 C7 H7 118.6 . . ? C8 C7 H7 118.6 . . ? C7 C8 C9 119.5(2) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 117.6(2) . . ? C10 C9 C12 118.0(2) . . ? C8 C9 C12 124.4(2) . . ? C11 C10 C9 119.7(2) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? N2 C11 C10 123.2(2) . . ? N2 C11 H11 118.4 . . ? C10 C11 H11 118.4 . . ? O2 C12 N4 123.8(2) . . ? O2 C12 C9 118.6(2) . . ? N4 C12 C9 117.6(2) . . ? C14 C13 C16 120.9(2) . . ? C14 C13 S1 119.60(18) . . ? C16 C13 S1 119.00(17) . . ? C13 C14 C15 120.4(2) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C15 C15 C14 118.9(3) 2_756 . ? C15 C15 C17 119.0(2) 2_756 2_756 ? C14 C15 C17 122.1(2) . 2_756 ? C17 C16 C13 119.9(2) . . ? C17 C16 H16 120.1 . . ? C13 C16 H16 120.1 . . ? C16 C17 C15 120.9(2) . 2_756 ? C16 C17 H17 119.6 . . ? C15 C17 H17 119.6 2_756 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OW1 H1B O5 0.85 2.03 2.878(3) 177.4 2_656 OW1 H1A O1 0.85 2.06 2.796(4) 145.4 . OW2 H2B OW1 0.85 2.05 2.838(4) 155.1 1_564 OW2 H2A O5 0.85 2.01 2.833(4) 160.9 . N3 H3A O2 0.86 2.03 2.876(3) 169.2 1_646 N4 H4A O1 0.86 2.06 2.892(3) 164.0 1_464 N4 H4B OW2 0.86 2.30 2.989(4) 137.7 2_665 _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.351 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.065 # Attachment 'Compound_3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 626405' #========================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 Ag N4 O2, 0.5(C12 H8 O6 S2), 2(H2 O)' _chemical_formula_sum 'C18 H20 Ag N4 O7 S' _chemical_formula_weight 544.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.601(5) _cell_length_b 10.292(6) _cell_length_c 11.721(7) _cell_angle_alpha 78.733(10) _cell_angle_beta 87.057(10) _cell_angle_gamma 65.700(9) _cell_volume 1034.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 550 _exptl_absorpt_coefficient_mu 1.124 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.589 _exptl_absorpt_correction_T_max 0.799 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 6123 _diffrn_reflns_av_R_equivalents 0.0130 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 27.10 _reflns_number_total 4341 _reflns_number_gt 3681 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT-PLUS (Bruker, 2003)' _computing_data_reduction SAINT-PLUS _computing_structure_solution 'SHELXTL (Bruker, 2005)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.5974P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4341 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0805 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.52249(3) 0.47549(2) 0.725717(17) 0.05406(10) Uani 1 1 d . . . S1 S 0.03793(6) 0.62548(6) 0.73626(5) 0.03543(14) Uani 1 1 d . . . O1 O 0.4274(2) 0.9440(2) 1.12370(18) 0.0581(5) Uani 1 1 d . . . O2 O 0.6598(2) -0.0094(2) 0.33414(17) 0.0496(5) Uani 1 1 d . . . O3 O 0.0354(3) 0.4974(2) 0.81100(17) 0.0567(5) Uani 1 1 d . . . O4 O -0.0855(2) 0.6915(2) 0.64965(17) 0.0541(5) Uani 1 1 d . . . O5 O 0.1843(2) 0.6016(3) 0.6871(2) 0.0683(6) Uani 1 1 d . . . OW1 O 0.8449(3) 0.3854(2) 0.7047(2) 0.0639(6) Uani 1 1 d . . . H1A H 0.8905 0.4224 0.7398 0.109(16) Uiso 1 1 d R . . H1B H 0.9033 0.3230 0.6661 0.099(15) Uiso 1 1 d R . . OW2 O 0.9631(3) -0.1798(3) 0.4212(2) 0.0697(6) Uani 1 1 d . . . H2A H 0.9708 -0.2324 0.4887 0.125(19) Uiso 1 1 d R . . H2B H 0.8705 -0.1310 0.3957 0.115(17) Uiso 1 1 d R . . N1 N 0.5230(2) 0.5972(2) 0.85524(17) 0.0386(4) Uani 1 1 d . . . N2 N 0.5259(2) 0.3437(2) 0.60310(18) 0.0412(5) Uani 1 1 d . . . N3 N 0.6709(3) 0.7941(2) 1.1724(2) 0.0492(5) Uani 1 1 d . . . H3A H 0.6762 0.8414 1.2237 0.059 Uiso 1 1 calc R . . H3B H 0.7492 0.7185 1.1607 0.059 Uiso 1 1 calc R . . N4 N 0.4068(2) 0.1105(2) 0.30046(18) 0.0424(5) Uani 1 1 d . . . H4A H 0.4070 0.0592 0.2506 0.051 Uiso 1 1 calc R . . H4B H 0.3226 0.1777 0.3159 0.051 Uiso 1 1 calc R . . C1 C 0.4009(3) 0.7095(3) 0.8813(2) 0.0477(6) Uani 1 1 d . . . H1 H 0.3083 0.7361 0.8425 0.057 Uiso 1 1 calc R . . C2 C 0.4055(3) 0.7878(3) 0.9627(2) 0.0475(6) Uani 1 1 d . . . H2 H 0.3178 0.8657 0.9774 0.057 Uiso 1 1 calc R . . C3 C 0.5408(3) 0.7501(2) 1.0224(2) 0.0350(5) Uani 1 1 d . . . C4 C 0.6664(3) 0.6353(3) 0.9957(2) 0.0497(7) Uani 1 1 d . . . H4 H 0.7601 0.6067 1.0336 0.060 Uiso 1 1 calc R . . C5 C 0.6534(3) 0.5628(3) 0.9128(2) 0.0504(7) Uani 1 1 d . . . H5 H 0.7403 0.4856 0.8959 0.060 Uiso 1 1 calc R . . C6 C 0.5427(3) 0.8376(3) 1.1116(2) 0.0389(5) Uani 1 1 d . . . C7 C 0.3981(3) 0.3641(3) 0.5490(2) 0.0486(6) Uani 1 1 d . . . H7 H 0.3064 0.4351 0.5669 0.058 Uiso 1 1 calc R . . C8 C 0.3949(3) 0.2853(3) 0.4679(2) 0.0465(6) Uani 1 1 d . . . H8 H 0.3026 0.3036 0.4322 0.056 Uiso 1 1 calc R . . C9 C 0.5289(3) 0.1790(2) 0.43945(19) 0.0330(5) Uani 1 1 d . . . C10 C 0.6612(3) 0.1594(3) 0.4944(3) 0.0545(7) Uani 1 1 d . . . H10 H 0.7546 0.0904 0.4769 0.065 Uiso 1 1 calc R . . C11 C 0.6558(3) 0.2415(3) 0.5749(3) 0.0586(8) Uani 1 1 d . . . H11 H 0.7466 0.2254 0.6117 0.070 Uiso 1 1 calc R . . C12 C 0.5357(3) 0.0859(2) 0.3532(2) 0.0360(5) Uani 1 1 d . . . C13 C 0.0077(2) 0.7542(2) 0.8247(2) 0.0322(4) Uani 1 1 d . . . C14 C -0.0048(4) 0.8910(3) 0.7739(2) 0.0507(7) Uani 1 1 d . . . H14 H -0.0098 0.9185 0.6932 0.061 Uiso 1 1 calc R . . C15 C -0.0099(4) 0.9873(3) 0.8426(2) 0.0521(7) Uani 1 1 d . . . H15 H -0.0190 1.0797 0.8073 0.063 Uiso 1 1 calc R . . C16 C -0.0017(2) 0.9495(2) 0.96347(19) 0.0321(5) Uani 1 1 d . . . C17 C 0.0047(3) 0.8137(3) 1.0119(2) 0.0404(5) Uani 1 1 d . . . H17 H 0.0060 0.7868 1.0925 0.048 Uiso 1 1 calc R . . C18 C 0.0092(3) 0.7166(3) 0.9439(2) 0.0402(5) Uani 1 1 d . . . H18 H 0.0132 0.6258 0.9787 0.048 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 0.08149(18) 0.05244(14) 0.04228(13) -0.02514(10) -0.00324(10) -0.03367(12) S1 0.0341(3) 0.0341(3) 0.0397(3) -0.0194(2) -0.0027(2) -0.0096(2) O1 0.0498(11) 0.0576(12) 0.0652(13) -0.0437(10) -0.0039(9) -0.0057(9) O2 0.0447(10) 0.0472(10) 0.0543(11) -0.0305(9) -0.0037(8) -0.0066(8) O3 0.0876(14) 0.0379(9) 0.0509(11) -0.0146(8) -0.0110(10) -0.0277(10) O4 0.0533(11) 0.0557(11) 0.0494(11) -0.0244(9) -0.0164(9) -0.0100(9) O5 0.0472(11) 0.0815(15) 0.0926(17) -0.0595(13) 0.0246(11) -0.0262(11) OW1 0.0633(13) 0.0700(14) 0.0757(15) -0.0349(12) 0.0043(11) -0.0353(11) OW2 0.0552(13) 0.0775(15) 0.0540(13) -0.0050(12) 0.0018(10) -0.0083(11) N1 0.0483(11) 0.0401(10) 0.0358(10) -0.0173(8) -0.0009(9) -0.0217(9) N2 0.0498(12) 0.0446(11) 0.0392(11) -0.0214(9) -0.0002(9) -0.0232(10) N3 0.0486(12) 0.0502(12) 0.0512(13) -0.0319(10) -0.0069(10) -0.0118(10) N4 0.0429(11) 0.0452(11) 0.0440(11) -0.0278(9) -0.0018(9) -0.0140(9) C1 0.0385(13) 0.0585(16) 0.0553(16) -0.0280(13) -0.0016(11) -0.0212(12) C2 0.0349(12) 0.0530(15) 0.0591(16) -0.0320(13) 0.0035(11) -0.0134(11) C3 0.0402(12) 0.0368(11) 0.0333(11) -0.0163(9) 0.0030(9) -0.0172(10) C4 0.0419(13) 0.0524(15) 0.0510(15) -0.0301(13) -0.0094(11) -0.0054(11) C5 0.0462(14) 0.0499(15) 0.0519(15) -0.0301(13) -0.0057(12) -0.0067(12) C6 0.0448(13) 0.0409(12) 0.0377(12) -0.0205(10) 0.0033(10) -0.0187(11) C7 0.0416(13) 0.0540(15) 0.0559(16) -0.0360(13) 0.0016(12) -0.0138(12) C8 0.0386(13) 0.0537(15) 0.0505(15) -0.0308(12) -0.0043(11) -0.0123(11) C9 0.0389(11) 0.0334(11) 0.0305(11) -0.0119(9) 0.0018(9) -0.0162(9) C10 0.0389(13) 0.0592(16) 0.0697(19) -0.0385(15) -0.0014(13) -0.0126(12) C11 0.0435(14) 0.0661(18) 0.075(2) -0.0407(16) -0.0091(14) -0.0180(13) C12 0.0442(13) 0.0346(11) 0.0318(11) -0.0129(9) 0.0020(9) -0.0157(10) C13 0.0295(10) 0.0306(10) 0.0390(12) -0.0174(9) -0.0026(9) -0.0096(8) C14 0.084(2) 0.0387(13) 0.0309(12) -0.0078(10) -0.0101(12) -0.0248(13) C15 0.090(2) 0.0318(12) 0.0362(13) -0.0059(10) -0.0093(13) -0.0258(13) C16 0.0323(11) 0.0297(10) 0.0349(11) -0.0128(9) -0.0021(9) -0.0100(9) C17 0.0592(15) 0.0411(12) 0.0296(11) -0.0133(10) 0.0065(10) -0.0269(11) C18 0.0567(14) 0.0350(12) 0.0370(12) -0.0117(10) 0.0048(11) -0.0250(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 N1 2.150(2) . ? Ag1 N2 2.151(2) . ? Ag1 OW1 2.855(3) . ? Ag1 O5 2.981(3) . ? S1 O5 1.433(2) . ? S1 O3 1.442(2) . ? S1 O4 1.4447(19) . ? S1 C13 1.762(2) . ? O1 C6 1.222(3) . ? O2 C12 1.236(3) . ? OW1 H1A 0.8503 . ? OW1 H1B 0.8497 . ? OW2 H2A 0.8545 . ? OW2 H2B 0.8565 . ? N1 C5 1.333(3) . ? N1 C1 1.338(3) . ? N2 C7 1.329(3) . ? N2 C11 1.336(4) . ? N3 C6 1.317(3) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? N4 C12 1.318(3) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? C1 C2 1.377(4) . ? C1 H1 0.9300 . ? C2 C3 1.378(3) . ? C2 H2 0.9300 . ? C3 C4 1.371(3) . ? C3 C6 1.512(3) . ? C4 C5 1.376(3) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C8 1.374(3) . ? C7 H7 0.9300 . ? C8 C9 1.380(3) . ? C8 H8 0.9300 . ? C9 C10 1.375(3) . ? C9 C12 1.505(3) . ? C10 C11 1.371(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 C18 1.374(3) . ? C13 C14 1.375(3) . ? C14 C15 1.379(3) . ? C14 H14 0.9300 . ? C15 C16 1.392(3) . ? C15 H15 0.9300 . ? C16 C17 1.379(3) . ? C16 C16 1.482(4) 2_577 ? C17 C18 1.381(3) . ? C17 H17 0.9300 . ? C18 H18 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 N1 Ag1 N2 177.01(8) . . ? N1 Ag1 OW1 90.20(7) . . ? N2 Ag1 OW1 89.36(7) . . ? N1 Ag1 O5 96.50(7) . . ? N2 Ag1 O5 84.57(7) . . ? OW1 Ag1 O5 166.14(7) . . ? O5 S1 O3 112.92(14) . . ? O5 S1 O4 112.74(15) . . ? O3 S1 O4 112.42(13) . . ? O5 S1 C13 104.89(11) . . ? O3 S1 C13 106.99(12) . . ? O4 S1 C13 106.17(11) . . ? S1 O5 Ag1 147.50(16) . . ? Ag1 OW1 H1A 119.2 . . ? Ag1 OW1 H1B 126.5 . . ? H1A OW1 H1B 114.3 . . ? H2A OW2 H2B 113.2 . . ? C5 N1 C1 116.5(2) . . ? C5 N1 Ag1 118.97(16) . . ? C1 N1 Ag1 124.52(16) . . ? C7 N2 C11 117.0(2) . . ? C7 N2 Ag1 121.01(17) . . ? C11 N2 Ag1 121.96(17) . . ? C6 N3 H3A 120.0 . . ? C6 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C12 N4 H4A 120.0 . . ? C12 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? N1 C1 C2 123.2(2) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 119.7(2) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 117.3(2) . . ? C4 C3 C6 124.0(2) . . ? C2 C3 C6 118.6(2) . . ? C3 C4 C5 119.8(2) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 123.5(2) . . ? N1 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? O1 C6 N3 123.4(2) . . ? O1 C6 C3 119.2(2) . . ? N3 C6 C3 117.5(2) . . ? N2 C7 C8 123.2(2) . . ? N2 C7 H7 118.4 . . ? C8 C7 H7 118.4 . . ? C7 C8 C9 119.8(2) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 116.9(2) . . ? C10 C9 C12 119.7(2) . . ? C8 C9 C12 123.4(2) . . ? C11 C10 C9 120.2(2) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? N2 C11 C10 123.0(2) . . ? N2 C11 H11 118.5 . . ? C10 C11 H11 118.5 . . ? O2 C12 N4 122.5(2) . . ? O2 C12 C9 119.6(2) . . ? N4 C12 C9 117.8(2) . . ? C18 C13 C14 119.6(2) . . ? C18 C13 S1 121.02(18) . . ? C14 C13 S1 119.21(19) . . ? C13 C14 C15 119.9(2) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 121.6(2) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C17 C16 C15 117.1(2) . . ? C17 C16 C16 121.7(3) . 2_577 ? C15 C16 C16 121.2(3) . 2_577 ? C16 C17 C18 121.7(2) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C13 C18 C17 120.0(2) . . ? C13 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OW1 H1A O3 0.85 2.12 2.959(3) 170.6 1_655 OW1 H1B OW2 0.85 1.94 2.790(3) 179.7 2_756 OW2 H2A O4 0.85 2.03 2.852(3) 160.6 1_645 OW2 H2B O2 0.86 1.97 2.829(3) 176.9 . N3 H3A O2 0.86 2.15 2.999(3) 170.3 1_566 N3 H3B O3 0.86 2.31 3.140(3) 163.0 2_667 N4 H4A O1 0.86 2.03 2.887(3) 173.3 1_544 N4 H4B O4 0.86 2.18 3.020(3) 165.4 2_566 _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 0.311 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.095 # Attachment 'Compound_4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 626406' #============================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 Ag2 N8 O4, 2(C24 H20 Ag N4 O9 S2)' _chemical_formula_sum 'C72 H64 Ag4 N16 O22 S4' _chemical_formula_weight 2065.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4640(19) _cell_length_b 12.346(3) _cell_length_c 18.082(4) _cell_angle_alpha 100.51(3) _cell_angle_beta 103.36(3) _cell_angle_gamma 102.01(3) _cell_volume 1950.7(7) _cell_formula_units_Z 1 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 1.182 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.573 _exptl_absorpt_correction_T_max 0.789 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 8420 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.97 _reflns_number_total 7654 _reflns_number_gt 5331 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT-PLUS (Bruker, 2003)' _computing_data_reduction SAINT-PLUS _computing_structure_solution 'SHELXTL (Bruker, 2005)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1056P)^2^+0.0814P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7654 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1495 _refine_ls_wR_factor_gt 0.1326 _refine_ls_goodness_of_fit_ref 1.056 _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 0.59527(4) 0.07945(3) 0.44828(2) 0.05125(14) Uani 1 1 d . . . Ag2 Ag 0.02838(4) 0.71385(3) 0.89894(2) 0.05680(15) Uani 1 1 d . . . S1 S 0.69749(13) 0.13361(9) 0.68625(6) 0.0434(3) Uani 1 1 d . . . S2 S 0.17492(13) 0.81965(9) 0.75109(6) 0.0432(3) Uani 1 1 d . . . N1 N 0.4718(4) 0.2104(3) 0.4458(2) 0.0398(8) Uani 1 1 d . . . N2 N 0.7414(4) -0.0365(3) 0.4508(2) 0.0413(8) Uani 1 1 d . . . N3 N 0.0999(4) 0.4470(3) 0.3879(2) 0.0457(9) Uani 1 1 d . . . H3A H 0.0469 0.4958 0.3880 0.055 Uiso 1 1 calc R . . H3B H 0.0789 0.3910 0.3477 0.055 Uiso 1 1 calc R . . N4 N 1.0939(4) -0.2858(3) 0.5103(2) 0.0489(10) Uani 1 1 d . . . H4A H 1.1459 -0.3353 0.5100 0.059 Uiso 1 1 calc R . . H4B H 1.1071 -0.2356 0.5528 0.059 Uiso 1 1 calc R . . N5 N 0.1099(4) 0.5605(3) 0.8899(2) 0.0493(10) Uani 1 1 d . . . N6 N -0.1059(4) 0.8353(3) 0.9109(2) 0.0453(9) Uani 1 1 d . . . N7 N 0.1422(4) 0.1529(3) 0.8158(2) 0.0510(10) Uani 1 1 d . . . H7A H 0.1639 0.0882 0.8112 0.061 Uiso 1 1 calc R . . H7B H 0.0630 0.1596 0.7842 0.061 Uiso 1 1 calc R . . N8 N -0.4808(4) 1.0746(3) 0.9071(3) 0.0550(11) Uani 1 1 d . . . H8A H -0.5272 1.1270 0.9130 0.066 Uiso 1 1 calc R . . H8B H -0.5284 1.0080 0.8774 0.066 Uiso 1 1 calc R . . O1 O 0.2502(4) 0.5360(3) 0.50911(19) 0.0561(9) Uani 1 1 d . . . O2 O 0.9700(4) -0.3571(3) 0.38287(18) 0.0571(9) Uani 1 1 d . . . O3 O 0.3455(3) 0.2397(3) 0.91863(18) 0.0453(7) Uani 1 1 d . . . O4 O -0.2657(5) 1.1894(3) 0.9859(2) 0.0825(14) Uani 1 1 d . . . O5 O 0.6276(4) 0.5713(3) 0.85216(19) 0.0587(10) Uani 1 1 d . . . O6 O 0.6617(5) 0.1311(3) 0.60417(19) 0.0706(11) Uani 1 1 d . . . O7 O 0.8514(4) 0.1358(3) 0.7200(3) 0.0787(13) Uani 1 1 d . . . O8 O 0.5921(4) 0.0446(3) 0.7032(2) 0.0635(10) Uani 1 1 d . . . O9 O 0.1717(4) 0.8353(3) 0.67412(19) 0.0621(10) Uani 1 1 d . . . O10 O 0.2172(4) 0.9260(3) 0.81067(19) 0.0589(9) Uani 1 1 d . . . O11 O 0.0348(3) 0.7446(3) 0.7528(2) 0.0558(9) Uani 1 1 d . . . C1 C 0.3830(5) 0.2179(4) 0.3794(3) 0.0458(11) Uani 1 1 d . . . H1 H 0.3793 0.1696 0.3326 0.055 Uiso 1 1 calc R . . C2 C 0.2957(5) 0.2952(4) 0.3774(3) 0.0439(10) Uani 1 1 d . . . H2 H 0.2325 0.2969 0.3300 0.053 Uiso 1 1 calc R . . C3 C 0.3029(4) 0.3696(3) 0.4460(2) 0.0334(8) Uani 1 1 d . . . C4 C 0.3974(5) 0.3632(4) 0.5145(3) 0.0437(10) Uani 1 1 d . . . H4 H 0.4058 0.4124 0.5618 0.052 Uiso 1 1 calc R . . C5 C 0.4795(5) 0.2834(4) 0.5127(3) 0.0443(11) Uani 1 1 d . . . H5 H 0.5426 0.2796 0.5594 0.053 Uiso 1 1 calc R . . C6 C 0.2140(5) 0.4583(3) 0.4499(3) 0.0388(9) Uani 1 1 d . . . C7 C 0.8217(4) -0.0501(3) 0.5181(2) 0.0358(9) Uani 1 1 d . . . H7 H 0.8200 -0.0054 0.5650 0.043 Uiso 1 1 calc R . . C8 C 0.9078(4) -0.1286(3) 0.5203(2) 0.0344(8) Uani 1 1 d . . . H8 H 0.9639 -0.1354 0.5680 0.041 Uiso 1 1 calc R . . C9 C 0.9087(4) -0.1968(3) 0.4503(2) 0.0345(9) Uani 1 1 d . . . C10 C 0.8251(6) -0.1813(4) 0.3810(3) 0.0497(12) Uani 1 1 d . . . H10 H 0.8239 -0.2251 0.3331 0.060 Uiso 1 1 calc R . . C11 C 0.7436(6) -0.1007(4) 0.3835(3) 0.0510(12) Uani 1 1 d . . . H11 H 0.6885 -0.0908 0.3366 0.061 Uiso 1 1 calc R . . C12 C 0.9941(5) -0.2871(4) 0.4457(3) 0.0406(10) Uani 1 1 d . . . C13 C 0.1741(7) 0.5284(4) 0.9531(3) 0.0662(16) Uani 1 1 d . . . H13 H 0.1933 0.5767 1.0022 0.079 Uiso 1 1 calc R . . C14 C 0.2130(6) 0.4268(4) 0.9484(3) 0.0577(14) Uani 1 1 d . . . H14 H 0.2576 0.4075 0.9939 0.069 Uiso 1 1 calc R . . C15 C 0.1862(4) 0.3537(3) 0.8768(2) 0.0344(9) Uani 1 1 d . . . C16 C 0.1213(5) 0.3877(4) 0.8109(3) 0.0454(11) Uani 1 1 d . . . H16 H 0.1005 0.3410 0.7610 0.054 Uiso 1 1 calc R . . C17 C 0.0883(5) 0.4925(4) 0.8208(3) 0.0460(11) Uani 1 1 d . . . H17 H 0.0487 0.5162 0.7764 0.055 Uiso 1 1 calc R . . C18 C 0.2306(5) 0.2422(3) 0.8713(2) 0.0368(9) Uani 1 1 d . . . C19 C -0.1304(5) 0.8729(4) 0.9792(3) 0.0442(10) Uani 1 1 d . . . H19 H -0.0948 0.8417 1.0207 0.053 Uiso 1 1 calc R . . C20 C -0.2061(5) 0.9557(4) 0.9919(3) 0.0423(10) Uani 1 1 d . . . H20 H -0.2199 0.9803 1.0409 0.051 Uiso 1 1 calc R . . C21 C -0.2613(4) 1.0017(3) 0.9302(2) 0.0371(9) Uani 1 1 d . . . C22 C -0.2372(6) 0.9613(4) 0.8589(3) 0.0529(13) Uani 1 1 d . . . H22 H -0.2742 0.9891 0.8159 0.063 Uiso 1 1 calc R . . C23 C -0.1594(6) 0.8808(4) 0.8518(3) 0.0529(12) Uani 1 1 d . . . H23 H -0.1424 0.8560 0.8037 0.063 Uiso 1 1 calc R . . C24 C -0.3361(5) 1.0962(4) 0.9435(2) 0.0411(10) Uani 1 1 d . . . C25 C 0.6713(5) 0.2652(3) 0.7335(2) 0.0366(9) Uani 1 1 d . . . C26 C 0.7317(5) 0.3650(4) 0.7150(3) 0.0447(10) Uani 1 1 d . . . H26 H 0.7844 0.3640 0.6774 0.054 Uiso 1 1 calc R . . C27 C 0.7127(5) 0.4677(4) 0.7534(3) 0.0469(11) Uani 1 1 d . . . H27 H 0.7536 0.5357 0.7419 0.056 Uiso 1 1 calc R . . C28 C 0.6351(5) 0.4684(4) 0.8073(3) 0.0446(11) Uani 1 1 d . . . C29 C 0.5761(6) 0.3706(4) 0.8264(3) 0.0568(13) Uani 1 1 d . . . H29 H 0.5253 0.3726 0.8647 0.068 Uiso 1 1 calc R . . C30 C 0.5927(6) 0.2679(4) 0.7882(3) 0.0540(12) Uani 1 1 d . . . H30 H 0.5500 0.2004 0.7998 0.065 Uiso 1 1 calc R . . C31 C 0.3144(4) 0.7465(3) 0.7777(2) 0.0358(9) Uani 1 1 d . . . C32 C 0.3401(5) 0.6656(4) 0.7219(3) 0.0468(11) Uani 1 1 d . . . H32 H 0.2894 0.6528 0.6692 0.056 Uiso 1 1 calc R . . C33 C 0.4426(6) 0.6034(4) 0.7454(3) 0.0534(13) Uani 1 1 d . . . H33 H 0.4595 0.5481 0.7085 0.064 Uiso 1 1 calc R . . C34 C 0.5179(5) 0.6242(3) 0.8226(3) 0.0407(10) Uani 1 1 d . . . C35 C 0.4915(5) 0.7033(4) 0.8789(2) 0.0411(10) Uani 1 1 d . . . H35 H 0.5424 0.7156 0.9315 0.049 Uiso 1 1 calc R . . C36 C 0.3880(5) 0.7639(4) 0.8559(2) 0.0408(10) Uani 1 1 d . . . H36 H 0.3681 0.8165 0.8934 0.049 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 0.0503(2) 0.0404(2) 0.0695(3) 0.01011(17) 0.00748(17) 0.03894(17) Ag2 0.0595(3) 0.0387(2) 0.0764(3) 0.00862(18) 0.00704(19) 0.04001(18) S1 0.0514(6) 0.0339(5) 0.0466(6) 0.0057(4) 0.0003(5) 0.0331(5) S2 0.0513(6) 0.0349(5) 0.0425(6) 0.0010(4) -0.0016(5) 0.0329(5) N1 0.0392(19) 0.0281(17) 0.057(2) 0.0091(15) 0.0081(16) 0.0264(15) N2 0.0428(19) 0.0383(19) 0.052(2) 0.0090(16) 0.0096(16) 0.0348(16) N3 0.052(2) 0.0347(18) 0.058(2) 0.0116(16) 0.0076(17) 0.0347(17) N4 0.062(2) 0.047(2) 0.051(2) 0.0112(17) 0.0122(18) 0.0461(19) N5 0.060(2) 0.0306(19) 0.061(2) 0.0066(17) 0.0051(19) 0.0358(18) N6 0.045(2) 0.0328(18) 0.064(2) 0.0114(17) 0.0090(17) 0.0291(16) N7 0.056(2) 0.0352(19) 0.059(2) 0.0067(17) -0.0037(18) 0.0321(18) N8 0.044(2) 0.041(2) 0.083(3) 0.009(2) 0.007(2) 0.0324(18) O1 0.064(2) 0.0410(18) 0.063(2) -0.0004(15) 0.0039(16) 0.0410(16) O2 0.083(2) 0.051(2) 0.0481(18) 0.0055(15) 0.0117(16) 0.0550(19) O3 0.0457(17) 0.0409(17) 0.0543(17) 0.0116(14) 0.0052(14) 0.0318(14) O4 0.074(3) 0.056(2) 0.091(3) -0.021(2) -0.019(2) 0.042(2) O5 0.062(2) 0.0521(19) 0.0570(19) -0.0065(15) -0.0072(16) 0.0480(17) O6 0.118(3) 0.062(2) 0.0479(19) 0.0103(17) 0.020(2) 0.066(2) O7 0.053(2) 0.062(2) 0.106(3) -0.006(2) -0.013(2) 0.0439(19) O8 0.077(2) 0.0338(17) 0.080(2) 0.0115(16) 0.0149(19) 0.0262(17) O9 0.083(3) 0.065(2) 0.0501(19) 0.0184(17) 0.0078(17) 0.053(2) O10 0.071(2) 0.0357(17) 0.062(2) -0.0064(14) -0.0059(16) 0.0395(16) O11 0.0398(17) 0.058(2) 0.067(2) 0.0013(17) 0.0049(15) 0.0322(16) C1 0.052(3) 0.038(2) 0.057(3) 0.013(2) 0.012(2) 0.035(2) C2 0.058(3) 0.038(2) 0.048(2) 0.0141(19) 0.012(2) 0.035(2) C3 0.035(2) 0.0232(18) 0.051(2) 0.0139(16) 0.0137(18) 0.0202(16) C4 0.045(2) 0.031(2) 0.052(2) 0.0024(18) 0.0024(19) 0.0218(19) C5 0.047(2) 0.035(2) 0.051(2) 0.0080(19) -0.0015(19) 0.0289(19) C6 0.042(2) 0.028(2) 0.054(2) 0.0106(18) 0.0136(19) 0.0247(18) C7 0.035(2) 0.031(2) 0.049(2) 0.0087(17) 0.0130(17) 0.0239(17) C8 0.036(2) 0.0279(19) 0.043(2) 0.0070(16) 0.0092(17) 0.0194(16) C9 0.037(2) 0.0301(19) 0.048(2) 0.0127(17) 0.0159(18) 0.0261(17) C10 0.065(3) 0.051(3) 0.042(2) 0.007(2) 0.010(2) 0.045(2) C11 0.061(3) 0.056(3) 0.045(2) 0.012(2) 0.007(2) 0.047(2) C12 0.046(2) 0.036(2) 0.052(2) 0.0146(19) 0.0163(19) 0.0324(19) C13 0.099(4) 0.046(3) 0.053(3) 0.001(2) 0.000(3) 0.052(3) C14 0.079(4) 0.047(3) 0.048(3) 0.005(2) -0.001(2) 0.043(3) C15 0.036(2) 0.029(2) 0.047(2) 0.0123(17) 0.0097(17) 0.0237(17) C16 0.060(3) 0.039(2) 0.046(2) 0.0111(19) 0.010(2) 0.037(2) C17 0.052(3) 0.037(2) 0.053(3) 0.014(2) 0.005(2) 0.030(2) C18 0.044(2) 0.036(2) 0.043(2) 0.0138(18) 0.0141(18) 0.0314(19) C19 0.048(2) 0.043(2) 0.058(3) 0.025(2) 0.020(2) 0.030(2) C20 0.042(2) 0.041(2) 0.056(3) 0.019(2) 0.017(2) 0.0268(19) C21 0.032(2) 0.036(2) 0.050(2) 0.0110(18) 0.0091(17) 0.0249(17) C22 0.071(3) 0.058(3) 0.040(2) 0.011(2) 0.010(2) 0.048(3) C23 0.069(3) 0.055(3) 0.045(2) 0.008(2) 0.012(2) 0.048(3) C24 0.047(2) 0.036(2) 0.043(2) 0.0036(18) 0.0069(19) 0.0263(19) C25 0.040(2) 0.032(2) 0.041(2) 0.0082(17) 0.0054(17) 0.0238(18) C26 0.050(3) 0.039(2) 0.052(3) 0.011(2) 0.017(2) 0.025(2) C27 0.056(3) 0.036(2) 0.061(3) 0.020(2) 0.019(2) 0.028(2) C28 0.041(2) 0.039(2) 0.054(3) 0.0016(19) 0.0025(19) 0.0309(19) C29 0.063(3) 0.054(3) 0.063(3) 0.007(2) 0.032(3) 0.027(2) C30 0.072(3) 0.041(3) 0.058(3) 0.013(2) 0.028(3) 0.022(2) C31 0.039(2) 0.0265(19) 0.044(2) 0.0056(16) 0.0057(17) 0.0217(17) C32 0.052(3) 0.055(3) 0.040(2) 0.006(2) 0.0068(19) 0.040(2) C33 0.063(3) 0.056(3) 0.048(3) -0.001(2) 0.010(2) 0.047(3) C34 0.040(2) 0.033(2) 0.052(2) 0.0059(18) 0.0057(19) 0.0260(18) C35 0.046(2) 0.038(2) 0.038(2) 0.0044(17) 0.0004(18) 0.0264(19) C36 0.045(2) 0.035(2) 0.043(2) 0.0004(17) 0.0067(18) 0.0271(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.184(3) . ? Ag1 N2 2.187(3) . ? Ag1 O6 2.666(3) . ? Ag2 N6 2.171(3) . ? Ag2 N5 2.182(3) . ? Ag2 O4 2.573(4) 2_577 ? Ag2 O11 2.749(4) . ? S1 O7 1.436(3) . ? S1 O6 1.437(4) . ? S1 O8 1.451(4) . ? S1 C25 1.786(4) . ? S2 O9 1.434(4) . ? S2 O10 1.453(3) . ? S2 O11 1.462(4) . ? S2 C31 1.775(4) . ? N1 C1 1.328(6) . ? N1 C5 1.347(5) . ? N2 C11 1.333(6) . ? N2 C7 1.337(5) . ? N3 C6 1.327(5) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? N4 C12 1.317(5) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? N5 C17 1.317(6) . ? N5 C13 1.333(6) . ? N6 C19 1.329(6) . ? N6 C23 1.341(6) . ? N7 C18 1.322(5) . ? N7 H7A 0.8600 . ? N7 H7B 0.8600 . ? N8 C24 1.322(6) . ? N8 H8A 0.8600 . ? N8 H8B 0.8600 . ? O1 C6 1.227(5) . ? O2 C12 1.237(5) . ? O3 C18 1.228(5) . ? O4 C24 1.216(6) . ? O4 Ag2 2.573(4) 2_577 ? O5 C34 1.394(5) . ? O5 C28 1.402(5) . ? C1 C2 1.387(5) . ? C1 H1 0.9300 . ? C2 C3 1.381(6) . ? C2 H2 0.9300 . ? C3 C4 1.377(6) . ? C3 C6 1.514(5) . ? C4 C5 1.376(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C8 1.390(5) . ? C7 H7 0.9300 . ? C8 C9 1.390(5) . ? C8 H8 0.9300 . ? C9 C10 1.387(6) . ? C9 C12 1.508(5) . ? C10 C11 1.380(6) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 C14 1.372(6) . ? C13 H13 0.9300 . ? C14 C15 1.372(6) . ? C14 H14 0.9300 . ? C15 C16 1.389(5) . ? C15 C18 1.514(5) . ? C16 C17 1.383(6) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C19 C20 1.381(6) . ? C19 H19 0.9300 . ? C20 C21 1.386(6) . ? C20 H20 0.9300 . ? C21 C22 1.383(6) . ? C21 C24 1.497(5) . ? C22 C23 1.360(6) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C25 C30 1.368(6) . ? C25 C26 1.379(6) . ? C26 C27 1.398(6) . ? C26 H26 0.9300 . ? C27 C28 1.349(7) . ? C27 H27 0.9300 . ? C28 C29 1.359(7) . ? C29 C30 1.386(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.379(6) . ? C31 C32 1.387(5) . ? C32 C33 1.396(6) . ? C32 H32 0.9300 . ? C33 C34 1.362(6) . ? C33 H33 0.9300 . ? C34 C35 1.382(6) . ? C35 C36 1.387(5) . ? C35 H35 0.9300 . ? C36 H36 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 N1 Ag1 N2 173.38(14) . . ? N1 Ag1 O6 89.46(12) . . ? N2 Ag1 O6 90.89(12) . . ? N6 Ag2 N5 164.50(16) . . ? N6 Ag2 O4 101.52(13) . 2_577 ? N5 Ag2 O4 87.02(13) . 2_577 ? N6 Ag2 O11 90.64(12) . . ? N5 Ag2 O11 96.74(13) . . ? O4 Ag2 O11 118.11(14) 2_577 . ? O7 S1 O6 113.8(3) . . ? O7 S1 O8 112.5(2) . . ? O6 S1 O8 112.0(3) . . ? O7 S1 C25 106.4(2) . . ? O6 S1 C25 105.67(19) . . ? O8 S1 C25 105.7(2) . . ? O9 S2 O10 113.6(2) . . ? O9 S2 O11 112.4(2) . . ? O10 S2 O11 111.3(2) . . ? O9 S2 C31 107.4(2) . . ? O10 S2 C31 106.56(19) . . ? O11 S2 C31 104.9(2) . . ? C1 N1 C5 118.1(3) . . ? C1 N1 Ag1 121.4(3) . . ? C5 N1 Ag1 120.4(3) . . ? C11 N2 C7 118.9(3) . . ? C11 N2 Ag1 119.2(3) . . ? C7 N2 Ag1 121.9(3) . . ? C6 N3 H3A 120.0 . . ? C6 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C12 N4 H4A 120.0 . . ? C12 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C17 N5 C13 117.7(4) . . ? C17 N5 Ag2 120.3(3) . . ? C13 N5 Ag2 121.9(3) . . ? C19 N6 C23 117.2(4) . . ? C19 N6 Ag2 120.6(3) . . ? C23 N6 Ag2 122.0(3) . . ? C18 N7 H7A 120.0 . . ? C18 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? C24 N8 H8A 120.0 . . ? C24 N8 H8B 120.0 . . ? H8A N8 H8B 120.0 . . ? C24 O4 Ag2 141.3(3) . 2_577 ? C34 O5 C28 119.7(3) . . ? S1 O6 Ag1 167.7(2) . . ? S2 O11 Ag2 114.36(17) . . ? N1 C1 C2 122.2(4) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.7(4) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 117.9(4) . . ? C4 C3 C6 118.4(4) . . ? C2 C3 C6 123.7(4) . . ? C5 C4 C3 119.6(4) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 122.5(4) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? O1 C6 N3 123.5(4) . . ? O1 C6 C3 119.1(4) . . ? N3 C6 C3 117.4(4) . . ? N2 C7 C8 122.3(4) . . ? N2 C7 H7 118.9 . . ? C8 C7 H7 118.9 . . ? C7 C8 C9 119.0(4) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C10 C9 C8 117.9(3) . . ? C10 C9 C12 118.5(4) . . ? C8 C9 C12 123.6(4) . . ? C11 C10 C9 119.7(4) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? N2 C11 C10 122.2(4) . . ? N2 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? O2 C12 N4 123.0(4) . . ? O2 C12 C9 119.9(4) . . ? N4 C12 C9 117.1(4) . . ? N5 C13 C14 122.4(5) . . ? N5 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C15 C14 C13 120.2(4) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 117.4(4) . . ? C14 C15 C18 120.4(4) . . ? C16 C15 C18 122.2(4) . . ? C17 C16 C15 118.6(4) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? N5 C17 C16 123.5(4) . . ? N5 C17 H17 118.2 . . ? C16 C17 H17 118.2 . . ? O3 C18 N7 123.9(4) . . ? O3 C18 C15 118.4(4) . . ? N7 C18 C15 117.6(3) . . ? N6 C19 C20 123.3(4) . . ? N6 C19 H19 118.3 . . ? C20 C19 H19 118.3 . . ? C19 C20 C21 118.8(4) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? C22 C21 C20 117.7(4) . . ? C22 C21 C24 122.4(4) . . ? C20 C21 C24 119.8(4) . . ? C23 C22 C21 119.7(4) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? N6 C23 C22 123.2(4) . . ? N6 C23 H23 118.4 . . ? C22 C23 H23 118.4 . . ? O4 C24 N8 121.5(4) . . ? O4 C24 C21 121.0(4) . . ? N8 C24 C21 117.4(4) . . ? C30 C25 C26 119.8(4) . . ? C30 C25 S1 120.5(3) . . ? C26 C25 S1 119.7(3) . . ? C25 C26 C27 119.1(4) . . ? C25 C26 H26 120.5 . . ? C27 C26 H26 120.5 . . ? C28 C27 C26 120.1(4) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 121.2(4) . . ? C27 C28 O5 120.9(4) . . ? C29 C28 O5 117.4(4) . . ? C28 C29 C30 119.3(5) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C25 C30 C29 120.5(5) . . ? C25 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C36 C31 C32 120.1(4) . . ? C36 C31 S2 118.9(3) . . ? C32 C31 S2 120.8(3) . . ? C31 C32 C33 119.5(4) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C34 C33 C32 119.7(4) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 121.4(4) . . ? C33 C34 O5 124.6(4) . . ? C35 C34 O5 114.0(4) . . ? C34 C35 C36 119.0(4) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? C31 C36 C35 120.3(4) . . ? C31 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A O2 0.86 2.10 2.938(4) 164.1 1_465 N3 H3B O11 0.86 2.12 2.958(5) 164.0 2_566 N4 H4A O1 0.86 2.04 2.894(4) 174.3 1_645 N4 H4B O9 0.86 2.10 2.911(5) 156.8 1_645 N7 H7A O10 0.86 2.16 3.020(5) 174.7 1_545 N7 H7B O7 0.86 2.00 2.836(5) 163.5 1_455 N8 H8A O3 0.86 2.02 2.881(5) 174.3 1_465 N8 H8B O10 0.86 2.34 2.987(5) 132.3 1_455 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.659 _refine_diff_density_min -2.205 _refine_diff_density_rms 0.153