# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Mak, Thomas' _publ_contact_author_email tcwmak@cuhk.edu.hk _publ_section_title ; Supramolecular Frameworks Constructed from Angular-shaped Sulfonyldipyrazine and Various Silver(I) Salts ; loop_ _publ_author_name C.-Q.Wan T.Mak ######################################################## data_compound5 _database_code_depnum_ccdc_archive 'CCDC 728103' #TrackingRef 'cqw6rev.CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H6 Ag F3 N4 O4 S' _chemical_formula_weight 443.12 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' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 12.8437(14) _cell_length_b 8.3562(9) _cell_length_c 25.590(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.944(2) _cell_angle_gamma 90.00 _cell_volume 2746.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prims _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 1.682 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.844166 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18510 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.27 _reflns_number_total 6787 _reflns_number_gt 3792 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.The DFIX command is used to the F-C bonds' lengthes at 1.32 angstrom for separate triflates because of their abnormal thermal vibration. ; _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^)+(0.0937P)^2^+1.3450P] 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 6787 _refine_ls_number_parameters 453 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1157 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1883 _refine_ls_wR_factor_gt 0.1542 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.066 _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 0.0000 -0.5000 0.5000 0.0524(2) Uani 1 2 d S . . Ag3 Ag -0.5000 -0.10548(9) 0.7500 0.0524(2) Uani 1 2 d S . . Ag2 Ag 0.00760(5) -0.84005(8) 0.51703(3) 0.0675(2) Uani 1 1 d . . . N1 N -0.1543(4) -0.4929(6) 0.45555(19) 0.0375(11) Uani 1 1 d . . . N2 N -0.3388(4) -0.4447(7) 0.39795(19) 0.0394(12) Uani 1 1 d . . . C4 C -0.2430(5) -0.4540(8) 0.4779(2) 0.0435(15) Uani 1 1 d . . . H4A H -0.2437 -0.4405 0.5140 0.052 Uiso 1 1 calc R . . C3 C -0.3353(5) -0.4326(8) 0.4494(2) 0.0449(16) Uani 1 1 d . . . H3A H -0.3961 -0.4091 0.4671 0.054 Uiso 1 1 calc R . . C2 C -0.2483(4) -0.4801(7) 0.3761(2) 0.0322(12) Uani 1 1 d . . . C1 C -0.1580(5) -0.5095(7) 0.4041(2) 0.0335(12) Uani 1 1 d . . . H1A H -0.0987 -0.5416 0.3866 0.040 Uiso 1 1 calc R . . S1 S -0.24866(12) -0.48000(18) 0.30630(5) 0.0357(3) Uani 1 1 d . . . O1 O -0.1511(4) -0.5431(6) 0.29044(17) 0.0538(12) Uani 1 1 d . . . O2 O -0.3440(4) -0.5481(5) 0.28717(17) 0.0486(11) Uani 1 1 d . . . N3 N -0.3479(4) -0.0397(6) 0.26947(19) 0.0385(12) Uani 1 1 d . . . N4 N -0.1623(4) -0.1957(7) 0.2941(2) 0.0475(14) Uani 1 1 d . . . C5 C -0.2530(4) -0.2712(7) 0.2921(2) 0.0305(12) Uani 1 1 d . . . C6 C -0.3459(5) -0.1974(7) 0.2801(2) 0.0356(13) Uani 1 1 d . . . H6A H -0.4073 -0.2564 0.2793 0.043 Uiso 1 1 calc R . . C7 C -0.2569(6) 0.0359(9) 0.2713(3) 0.0517(17) Uani 1 1 d . . . H7A H -0.2555 0.1448 0.2639 0.062 Uiso 1 1 calc R . . C8 C -0.1659(6) -0.0388(9) 0.2835(3) 0.0582(19) Uani 1 1 d . . . H8A H -0.1046 0.0204 0.2845 0.070 Uiso 1 1 calc R . . N5 N -0.0922(4) -0.7544(6) 0.5840(2) 0.0400(12) Uani 1 1 d . . . N6 N -0.2089(4) -0.6596(6) 0.6691(2) 0.0394(12) Uani 1 1 d . . . C9 C -0.0480(5) -0.7267(8) 0.6304(3) 0.0455(16) Uani 1 1 d . . . H9A H 0.0233 -0.7413 0.6351 0.055 Uiso 1 1 calc R . . C10 C -0.1090(5) -0.6752(8) 0.6727(3) 0.0485(17) Uani 1 1 d . . . H10A H -0.0759 -0.6516 0.7044 0.058 Uiso 1 1 calc R . . C11 C -0.2515(4) -0.6918(7) 0.6230(2) 0.0331(12) Uani 1 1 d . . . C12 C -0.1959(4) -0.7375(7) 0.5799(2) 0.0360(13) Uani 1 1 d . . . H12A H -0.2301 -0.7566 0.5482 0.043 Uiso 1 1 calc R . . S2 S -0.38917(11) -0.67266(18) 0.61872(6) 0.0360(4) Uani 1 1 d . . . O3 O -0.4326(3) -0.7417(5) 0.66459(19) 0.0495(12) Uani 1 1 d . . . O4 O -0.4216(3) -0.7264(6) 0.56772(19) 0.0559(13) Uani 1 1 d . . . N7 N -0.3941(5) -0.3795(7) 0.5801(2) 0.0535(16) Uani 1 1 d . . . N8 N -0.4500(4) -0.2359(6) 0.6738(2) 0.0400(12) Uani 1 1 d . . . C13 C -0.4084(4) -0.4594(7) 0.6235(2) 0.0331(12) Uani 1 1 d . . . C14 C -0.4345(4) -0.3915(7) 0.6701(2) 0.0354(13) Uani 1 1 d . . . H14A H -0.4414 -0.4558 0.6995 0.042 Uiso 1 1 calc R . . C15 C -0.4372(6) -0.1522(8) 0.6304(3) 0.0558(19) Uani 1 1 d . . . H15A H -0.4479 -0.0422 0.6311 0.067 Uiso 1 1 calc R . . C16 C -0.4085(7) -0.2233(10) 0.5846(3) 0.069(2) Uani 1 1 d . . . H16A H -0.3987 -0.1591 0.5554 0.083 Uiso 1 1 calc R . . C17 C -0.0951(6) -0.2478(9) 0.5904(3) 0.0540(18) Uani 1 1 d . . . C18 C -0.1245(6) -0.1977(9) 0.6463(3) 0.060(2) Uani 1 1 d D . . O5 O -0.1066(9) -0.1388(10) 0.5568(3) 0.080(3) Uani 0.70 1 d P . . O5' O -0.0204(18) -0.157(2) 0.5742(8) 0.074(6) Uani 0.30 1 d P . . O6 O -0.0886(5) -0.3856(7) 0.5825(2) 0.0717(16) Uani 1 1 d . . . F11 F -0.1774(8) -0.0634(7) 0.6476(3) 0.163(4) Uani 1 1 d D . . F12 F -0.1856(6) -0.2939(7) 0.6700(2) 0.115(2) Uani 1 1 d D . . F13 F -0.0482(6) -0.1743(16) 0.6749(3) 0.262(9) Uani 1 1 d D . . C19 C 0.1999(7) -1.0040(12) 0.5581(3) 0.072(2) Uani 1 1 d . . . C20 C 0.3056(7) -1.0485(11) 0.5735(3) 0.070(2) Uani 1 1 d D . . O7 O 0.1558(9) -1.1294(13) 0.5345(5) 0.090(3) Uani 0.70 1 d P . . O7' O 0.1667(19) -1.008(5) 0.5111(9) 0.122(12) Uani 0.30 1 d P . . O8 O 0.1640(5) -0.8797(8) 0.5751(3) 0.090(2) Uani 1 1 d . . . F21 F 0.3627(14) -1.108(3) 0.5394(7) 0.142(9) Uani 0.50 1 d PD . . F21' F 0.3773(14) -0.985(2) 0.5367(8) 0.122(7) Uani 0.50 1 d P . . F22 F 0.3078(12) -1.1625(16) 0.6118(5) 0.130(6) Uani 0.60 1 d PD . . F22' F 0.329(2) -1.1916(19) 0.5650(18) 0.170(17) Uani 0.40 1 d P . . F23 F 0.3555(6) -0.9457(10) 0.6021(3) 0.144(3) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0458(4) 0.0707(5) 0.0401(4) 0.0022(4) -0.0159(3) 0.0083(4) Ag3 0.0577(5) 0.0403(4) 0.0594(5) 0.000 0.0059(4) 0.000 Ag2 0.0632(4) 0.0696(4) 0.0703(5) -0.0063(3) 0.0180(3) 0.0057(3) N1 0.040(3) 0.045(3) 0.028(2) 0.001(2) -0.006(2) 0.001(2) N2 0.034(3) 0.050(3) 0.034(3) 0.003(2) -0.002(2) 0.004(2) C4 0.050(4) 0.052(4) 0.029(3) 0.002(3) 0.001(3) 0.007(3) C3 0.038(3) 0.060(4) 0.037(4) -0.002(3) 0.011(3) -0.001(3) C2 0.036(3) 0.032(3) 0.029(3) -0.001(2) -0.006(2) -0.002(2) C1 0.032(3) 0.038(3) 0.030(3) 0.001(2) -0.002(2) 0.003(2) S1 0.0427(8) 0.0382(8) 0.0258(7) -0.0024(6) -0.0056(6) 0.0066(6) O1 0.060(3) 0.066(3) 0.036(2) -0.003(2) 0.003(2) 0.029(3) O2 0.064(3) 0.041(2) 0.041(3) 0.000(2) -0.019(2) -0.008(2) N3 0.048(3) 0.033(3) 0.034(3) 0.000(2) 0.002(2) 0.000(2) N4 0.042(3) 0.053(3) 0.047(3) 0.002(3) -0.012(3) -0.007(3) C5 0.031(3) 0.040(3) 0.021(3) -0.001(2) -0.003(2) 0.002(2) C6 0.037(3) 0.037(3) 0.032(3) 0.000(3) 0.002(2) -0.003(3) C7 0.057(5) 0.042(4) 0.056(4) 0.005(3) 0.003(3) -0.009(3) C8 0.051(4) 0.057(4) 0.066(5) 0.006(4) -0.004(4) -0.021(4) N5 0.031(3) 0.041(3) 0.048(3) 0.001(3) 0.005(2) 0.003(2) N6 0.040(3) 0.045(3) 0.033(3) 0.000(2) 0.000(2) -0.003(2) C9 0.036(3) 0.050(4) 0.051(4) 0.009(3) -0.009(3) -0.002(3) C10 0.044(4) 0.058(4) 0.043(4) 0.008(3) -0.011(3) -0.007(3) C11 0.033(3) 0.032(3) 0.035(3) 0.000(2) -0.002(2) 0.000(2) C12 0.034(3) 0.035(3) 0.039(3) 0.005(3) -0.004(2) 0.006(2) S2 0.0286(7) 0.0361(8) 0.0434(9) -0.0071(7) 0.0010(6) 0.0015(6) O3 0.042(3) 0.038(2) 0.069(3) 0.004(2) 0.016(2) -0.003(2) O4 0.037(3) 0.073(3) 0.057(3) -0.030(3) -0.012(2) 0.004(2) N7 0.078(4) 0.050(3) 0.034(3) 0.011(3) 0.012(3) 0.017(3) N8 0.040(3) 0.037(3) 0.043(3) -0.005(2) 0.003(2) 0.004(2) C13 0.030(3) 0.038(3) 0.032(3) -0.001(3) 0.000(2) 0.001(2) C14 0.034(3) 0.038(3) 0.033(3) 0.006(3) 0.001(2) -0.002(3) C15 0.065(5) 0.040(4) 0.063(5) 0.013(4) 0.013(4) 0.010(3) C16 0.103(7) 0.052(5) 0.052(5) 0.023(4) 0.010(4) 0.022(5) C17 0.069(5) 0.042(4) 0.051(4) -0.005(4) 0.004(4) -0.005(4) C18 0.074(5) 0.049(4) 0.058(5) -0.015(4) 0.008(4) -0.016(4) O5 0.117(9) 0.064(5) 0.059(5) 0.024(4) 0.020(6) 0.018(5) O5' 0.074(14) 0.077(14) 0.070(14) -0.008(10) 0.016(11) -0.025(11) O6 0.105(5) 0.059(3) 0.052(3) -0.008(3) 0.005(3) 0.014(3) F11 0.291(11) 0.067(4) 0.134(6) 0.001(4) 0.116(7) 0.036(5) F12 0.163(6) 0.094(4) 0.091(4) -0.008(3) 0.068(4) -0.031(4) F13 0.112(6) 0.56(3) 0.110(6) -0.170(10) -0.004(5) -0.084(9) C19 0.071(6) 0.092(7) 0.055(5) -0.019(5) 0.004(4) 0.014(5) C20 0.069(6) 0.068(5) 0.071(6) -0.027(5) -0.009(5) -0.002(4) O7 0.095(8) 0.086(7) 0.089(8) -0.006(6) -0.036(6) 0.003(6) O7' 0.071(16) 0.23(4) 0.061(15) -0.04(2) -0.023(12) 0.06(2) O8 0.071(4) 0.080(4) 0.118(6) -0.001(4) 0.012(4) 0.017(3) F21 0.112(17) 0.19(2) 0.120(18) -0.06(2) 0.007(12) 0.07(2) F21' 0.078(9) 0.156(15) 0.132(15) 0.071(15) 0.044(9) 0.016(12) F22 0.120(11) 0.133(12) 0.135(11) 0.061(9) -0.044(9) 0.015(8) F22' 0.121(18) 0.030(8) 0.36(5) 0.037(16) 0.02(3) 0.004(8) F23 0.104(5) 0.145(6) 0.183(8) -0.049(6) -0.053(5) 0.016(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.269(5) 3_546 ? Ag1 N1 2.269(5) . ? Ag1 O6 2.596(5) . ? Ag1 O6 2.596(5) 3_546 ? Ag1 Ag2 2.8762(7) 3_546 ? Ag1 Ag2 2.8762(7) . ? Ag3 N8 2.334(5) . ? Ag3 N8 2.334(5) 2_456 ? Ag3 N3 2.346(5) 4_556 ? Ag3 N3 2.346(5) 3_456 ? Ag2 N5 2.273(5) . ? Ag2 O5 2.302(9) 3_546 ? Ag2 O5' 2.34(2) 3_546 ? Ag2 O7 2.474(11) 3_536 ? Ag2 O7' 2.49(2) . ? Ag2 O8 2.500(7) . ? Ag2 Ag2 2.8174(13) 3_536 ? N1 C1 1.323(7) . ? N1 C4 1.324(8) . ? N2 C3 1.320(8) . ? N2 C2 1.331(7) . ? C4 C3 1.394(9) . ? C4 H4A 0.9300 . ? C3 H3A 0.9300 . ? C2 C1 1.375(8) . ? C2 S1 1.787(6) . ? C1 H1A 0.9300 . ? S1 O1 1.425(5) . ? S1 O2 1.429(5) . ? S1 C5 1.783(6) . ? N3 C7 1.329(8) . ? N3 C6 1.346(7) . ? N3 Ag3 2.346(5) 3_456 ? N4 C5 1.325(8) . ? N4 C8 1.340(9) . ? C5 C6 1.374(8) . ? C6 H6A 0.9300 . ? C7 C8 1.357(10) . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? N5 C9 1.328(8) . ? N5 C12 1.342(7) . ? N6 C10 1.292(8) . ? N6 C11 1.318(8) . ? C9 C10 1.414(10) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.378(8) . ? C11 S2 1.777(6) . ? C12 H12A 0.9300 . ? S2 O3 1.430(5) . ? S2 O4 1.435(5) . ? S2 C13 1.804(6) . ? N7 C13 1.310(8) . ? N7 C16 1.323(10) . ? N8 C14 1.319(8) . ? N8 C15 1.324(9) . ? C13 C14 1.367(8) . ? C14 H14A 0.9300 . ? C15 C16 1.370(11) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C17 O6 1.173(9) . ? C17 O5 1.260(11) . ? C17 O5' 1.297(19) . ? C17 C18 1.543(10) . ? C18 F13 1.229(10) . ? C18 F12 1.283(8) . ? C18 F11 1.312(9) . ? O5 O5' 1.20(2) . ? O5 Ag2 2.302(9) 3_546 ? O5' Ag2 2.34(2) 3_546 ? C19 O8 1.219(10) . ? C19 O7' 1.27(2) . ? C19 O7 1.331(13) . ? C19 C20 1.455(12) . ? C20 F21 1.250(13) . ? C20 F22' 1.25(2) . ? C20 F23 1.292(9) . ? C20 F22 1.369(12) . ? C20 F21' 1.429(17) . ? O7 O7' 1.18(4) . ? O7 Ag2 2.474(11) 3_536 ? F21 F21' 1.05(2) . ? F21 F22' 1.06(2) . ? F21' F23 1.73(2) . ? F22 F22' 1.26(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 180.0(2) 3_546 . ? N1 Ag1 O6 89.60(19) 3_546 . ? N1 Ag1 O6 90.40(19) . . ? N1 Ag1 O6 90.40(19) 3_546 3_546 ? N1 Ag1 O6 89.60(19) . 3_546 ? O6 Ag1 O6 180.00(14) . 3_546 ? N1 Ag1 Ag2 97.41(13) 3_546 3_546 ? N1 Ag1 Ag2 82.59(13) . 3_546 ? O6 Ag1 Ag2 75.24(13) . 3_546 ? O6 Ag1 Ag2 104.76(13) 3_546 3_546 ? N1 Ag1 Ag2 82.59(13) 3_546 . ? N1 Ag1 Ag2 97.41(13) . . ? O6 Ag1 Ag2 104.76(13) . . ? O6 Ag1 Ag2 75.24(13) 3_546 . ? Ag2 Ag1 Ag2 180.0 3_546 . ? N8 Ag3 N8 124.3(3) . 2_456 ? N8 Ag3 N3 100.32(17) . 4_556 ? N8 Ag3 N3 107.67(18) 2_456 4_556 ? N8 Ag3 N3 107.67(18) . 3_456 ? N8 Ag3 N3 100.32(17) 2_456 3_456 ? N3 Ag3 N3 117.7(2) 4_556 3_456 ? N5 Ag2 O5 165.8(2) . 3_546 ? N5 Ag2 O5' 143.5(6) . 3_546 ? O5 Ag2 O5' 29.9(5) 3_546 3_546 ? N5 Ag2 O7 87.2(3) . 3_536 ? O5 Ag2 O7 91.7(4) 3_546 3_536 ? O5' Ag2 O7 62.6(6) 3_546 3_536 ? N5 Ag2 O7' 134.3(6) . . ? O5 Ag2 O7' 56.0(7) 3_546 . ? O5' Ag2 O7' 82.1(8) 3_546 . ? O7 Ag2 O7' 126.9(7) 3_536 . ? N5 Ag2 O8 93.0(2) . . ? O5 Ag2 O8 91.6(3) 3_546 . ? O5' Ag2 O8 121.4(6) 3_546 . ? O7 Ag2 O8 165.8(3) 3_536 . ? O7' Ag2 O8 46.2(6) . . ? N5 Ag2 Ag2 119.67(14) . 3_536 ? O5 Ag2 Ag2 73.1(2) 3_546 3_536 ? O5' Ag2 Ag2 71.8(5) 3_546 3_536 ? O7 Ag2 Ag2 71.5(3) 3_536 3_536 ? O7' Ag2 Ag2 59.8(9) . 3_536 ? O8 Ag2 Ag2 96.26(16) . 3_536 ? N5 Ag2 Ag1 77.59(13) . . ? O5 Ag2 Ag1 88.2(2) 3_546 . ? O5' Ag2 Ag1 82.1(5) 3_546 . ? O7 Ag2 Ag1 89.7(3) 3_536 . ? O7' Ag2 Ag1 125.1(10) . . ? O8 Ag2 Ag1 104.22(16) . . ? Ag2 Ag2 Ag1 152.68(4) 3_536 . ? C1 N1 C4 116.0(5) . . ? C1 N1 Ag1 120.9(4) . . ? C4 N1 Ag1 122.7(4) . . ? C3 N2 C2 114.8(5) . . ? N1 C4 C3 122.4(6) . . ? N1 C4 H4A 118.8 . . ? C3 C4 H4A 118.8 . . ? N2 C3 C4 121.8(6) . . ? N2 C3 H3A 119.1 . . ? C4 C3 H3A 119.1 . . ? N2 C2 C1 123.8(5) . . ? N2 C2 S1 115.5(4) . . ? C1 C2 S1 120.6(4) . . ? N1 C1 C2 121.0(5) . . ? N1 C1 H1A 119.5 . . ? C2 C1 H1A 119.5 . . ? O1 S1 O2 120.5(3) . . ? O1 S1 C5 109.2(3) . . ? O2 S1 C5 107.3(3) . . ? O1 S1 C2 107.3(3) . . ? O2 S1 C2 109.3(3) . . ? C5 S1 C2 101.7(2) . . ? C7 N3 C6 116.4(6) . . ? C7 N3 Ag3 119.4(4) . 3_456 ? C6 N3 Ag3 124.2(4) . 3_456 ? C5 N4 C8 115.5(6) . . ? N4 C5 C6 123.7(6) . . ? N4 C5 S1 115.7(4) . . ? C6 C5 S1 120.6(4) . . ? N3 C6 C5 119.9(5) . . ? N3 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? N3 C7 C8 122.9(7) . . ? N3 C7 H7A 118.5 . . ? C8 C7 H7A 118.5 . . ? N4 C8 C7 121.6(7) . . ? N4 C8 H8A 119.2 . . ? C7 C8 H8A 119.2 . . ? C9 N5 C12 117.4(5) . . ? C9 N5 Ag2 119.4(4) . . ? C12 N5 Ag2 123.1(4) . . ? C10 N6 C11 116.2(6) . . ? N5 C9 C10 120.2(6) . . ? N5 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? N6 C10 C9 122.5(6) . . ? N6 C10 H10A 118.7 . . ? C9 C10 H10A 118.7 . . ? N6 C11 C12 124.0(5) . . ? N6 C11 S2 115.8(4) . . ? C12 C11 S2 120.2(5) . . ? N5 C12 C11 119.6(6) . . ? N5 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? O3 S2 O4 120.6(3) . . ? O3 S2 C11 108.3(3) . . ? O4 S2 C11 107.6(3) . . ? O3 S2 C13 106.7(3) . . ? O4 S2 C13 109.4(3) . . ? C11 S2 C13 102.8(3) . . ? C13 N7 C16 114.1(6) . . ? C14 N8 C15 116.1(6) . . ? C14 N8 Ag3 124.3(4) . . ? C15 N8 Ag3 119.6(4) . . ? N7 C13 C14 124.6(6) . . ? N7 C13 S2 115.1(4) . . ? C14 C13 S2 120.3(5) . . ? N8 C14 C13 120.7(6) . . ? N8 C14 H14A 119.6 . . ? C13 C14 H14A 119.6 . . ? N8 C15 C16 121.8(6) . . ? N8 C15 H15A 119.1 . . ? C16 C15 H15A 119.1 . . ? N7 C16 C15 122.8(7) . . ? N7 C16 H16A 118.6 . . ? C15 C16 H16A 118.6 . . ? O6 C17 O5 126.8(8) . . ? O6 C17 O5' 117.6(12) . . ? O5 C17 O5' 55.8(11) . . ? O6 C17 C18 116.5(7) . . ? O5 C17 C18 114.1(7) . . ? O5' C17 C18 109.4(11) . . ? F13 C18 F12 107.8(9) . . ? F13 C18 F11 104.9(8) . . ? F12 C18 F11 101.8(7) . . ? F13 C18 C17 113.0(7) . . ? F12 C18 C17 115.4(6) . . ? F11 C18 C17 112.9(7) . . ? O5' O5 C17 63.7(11) . . ? O5' O5 Ag2 76.9(11) . 3_546 ? C17 O5 Ag2 116.4(7) . 3_546 ? O5 O5' C17 60.5(11) . . ? O5 O5' Ag2 73.2(12) . 3_546 ? C17 O5' Ag2 112.2(13) . 3_546 ? C17 O6 Ag1 122.4(5) . . ? O8 C19 O7' 103.8(17) . . ? O8 C19 O7 132.2(10) . . ? O7' C19 O7 54.1(18) . . ? O8 C19 C20 118.6(9) . . ? O7' C19 C20 123.0(12) . . ? O7 C19 C20 108.0(9) . . ? F21 C20 F22' 49.9(14) . . ? F21 C20 F23 111.6(12) . . ? F22' C20 F23 127.8(19) . . ? F21 C20 F22 102.7(11) . . ? F22' C20 F22 57.2(17) . . ? F23 C20 F22 93.0(9) . . ? F21 C20 F21' 45.3(11) . . ? F22' C20 F21' 94.6(16) . . ? F23 C20 F21' 78.9(11) . . ? F22 C20 F21' 136.5(12) . . ? F21 C20 C19 117.9(11) . . ? F22' C20 C19 115.2(16) . . ? F23 C20 C19 115.7(8) . . ? F22 C20 C19 112.3(10) . . ? F21' C20 C19 109.7(10) . . ? O7' O7 C19 60.3(14) . . ? O7' O7 Ag2 85.7(15) . 3_536 ? C19 O7 Ag2 132.3(8) . 3_536 ? O7 O7' C19 65.6(17) . . ? O7 O7' Ag2 110.4(18) . . ? C19 O7' Ag2 100.9(14) . . ? C19 O8 Ag2 101.9(6) . . ? F21' F21 F22' 140(3) . . ? F21' F21 C20 76.4(14) . . ? F22' F21 C20 65.2(16) . . ? F21 F21' C20 58.2(10) . . ? F21 F21' F23 95.2(15) . . ? C20 F21' F23 47.1(7) . . ? F22' F22 C20 56.8(10) . . ? F21 F22' C20 64.9(12) . . ? F21 F22' F22 124(3) . . ? C20 F22' F22 66.0(18) . . ? C20 F23 F21' 54.1(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 N1 Ag1 Ag2 N5 96.00(19) 3_546 . . . ? N1 Ag1 Ag2 N5 -84.00(19) . . . . ? O6 Ag1 Ag2 N5 8.4(2) . . . . ? O6 Ag1 Ag2 N5 -171.6(2) 3_546 . . . ? Ag2 Ag1 Ag2 N5 -60(2) 3_546 . . . ? N1 Ag1 Ag2 O5 -85.1(3) 3_546 . . 3_546 ? N1 Ag1 Ag2 O5 94.9(3) . . . 3_546 ? O6 Ag1 Ag2 O5 -172.7(3) . . . 3_546 ? O6 Ag1 Ag2 O5 7.3(3) 3_546 . . 3_546 ? Ag2 Ag1 Ag2 O5 119(2) 3_546 . . 3_546 ? N1 Ag1 Ag2 O5' -114.4(6) 3_546 . . 3_546 ? N1 Ag1 Ag2 O5' 65.6(6) . . . 3_546 ? O6 Ag1 Ag2 O5' 157.9(6) . . . 3_546 ? O6 Ag1 Ag2 O5' -22.1(6) 3_546 . . 3_546 ? Ag2 Ag1 Ag2 O5' 90(3) 3_546 . . 3_546 ? N1 Ag1 Ag2 O7 -176.8(3) 3_546 . . 3_536 ? N1 Ag1 Ag2 O7 3.2(3) . . . 3_536 ? O6 Ag1 Ag2 O7 95.5(3) . . . 3_536 ? O6 Ag1 Ag2 O7 -84.5(3) 3_546 . . 3_536 ? Ag2 Ag1 Ag2 O7 27(2) 3_546 . . 3_536 ? N1 Ag1 Ag2 O7' -40.0(6) 3_546 . . . ? N1 Ag1 Ag2 O7' 140.0(6) . . . . ? O6 Ag1 Ag2 O7' -127.6(6) . . . . ? O6 Ag1 Ag2 O7' 52.4(6) 3_546 . . . ? Ag2 Ag1 Ag2 O7' 164(5) 3_546 . . . ? N1 Ag1 Ag2 O8 6.1(2) 3_546 . . . ? N1 Ag1 Ag2 O8 -173.9(2) . . . . ? O6 Ag1 Ag2 O8 -81.5(2) . . . . ? O6 Ag1 Ag2 O8 98.5(2) 3_546 . . . ? Ag2 Ag1 Ag2 O8 -150(2) 3_546 . . . ? N1 Ag1 Ag2 Ag2 -131.29(15) 3_546 . . 3_536 ? N1 Ag1 Ag2 Ag2 48.71(15) . . . 3_536 ? O6 Ag1 Ag2 Ag2 141.08(17) . . . 3_536 ? O6 Ag1 Ag2 Ag2 -38.92(17) 3_546 . . 3_536 ? Ag2 Ag1 Ag2 Ag2 73(100) 3_546 . . 3_536 ? N1 Ag1 N1 C1 -99(74) 3_546 . . . ? O6 Ag1 N1 C1 166.3(5) . . . . ? O6 Ag1 N1 C1 -13.7(5) 3_546 . . . ? Ag2 Ag1 N1 C1 91.2(4) 3_546 . . . ? Ag2 Ag1 N1 C1 -88.8(4) . . . . ? N1 Ag1 N1 C4 89(75) 3_546 . . . ? O6 Ag1 N1 C4 -5.7(5) . . . . ? O6 Ag1 N1 C4 174.3(5) 3_546 . . . ? Ag2 Ag1 N1 C4 -80.7(5) 3_546 . . . ? Ag2 Ag1 N1 C4 99.3(5) . . . . ? C1 N1 C4 C3 0.4(9) . . . . ? Ag1 N1 C4 C3 172.7(5) . . . . ? C2 N2 C3 C4 0.6(9) . . . . ? N1 C4 C3 N2 -2.3(11) . . . . ? C3 N2 C2 C1 2.9(9) . . . . ? C3 N2 C2 S1 -174.8(5) . . . . ? C4 N1 C1 C2 3.0(8) . . . . ? Ag1 N1 C1 C2 -169.5(4) . . . . ? N2 C2 C1 N1 -4.9(9) . . . . ? S1 C2 C1 N1 172.6(4) . . . . ? N2 C2 S1 O1 -171.4(5) . . . . ? C1 C2 S1 O1 10.8(6) . . . . ? N2 C2 S1 O2 -39.2(5) . . . . ? C1 C2 S1 O2 143.0(5) . . . . ? N2 C2 S1 C5 74.0(5) . . . . ? C1 C2 S1 C5 -103.8(5) . . . . ? C8 N4 C5 C6 0.0(9) . . . . ? C8 N4 C5 S1 -180.0(5) . . . . ? O1 S1 C5 N4 -30.6(5) . . . . ? O2 S1 C5 N4 -162.7(5) . . . . ? C2 S1 C5 N4 82.6(5) . . . . ? O1 S1 C5 C6 149.4(5) . . . . ? O2 S1 C5 C6 17.3(5) . . . . ? C2 S1 C5 C6 -97.4(5) . . . . ? C7 N3 C6 C5 0.2(8) . . . . ? Ag3 N3 C6 C5 -178.6(4) 3_456 . . . ? N4 C5 C6 N3 0.0(9) . . . . ? S1 C5 C6 N3 -180.0(4) . . . . ? C6 N3 C7 C8 -0.5(10) . . . . ? Ag3 N3 C7 C8 178.4(6) 3_456 . . . ? C5 N4 C8 C7 -0.3(10) . . . . ? N3 C7 C8 N4 0.6(12) . . . . ? O5 Ag2 N5 C9 -100.1(14) 3_546 . . . ? O5' Ag2 N5 C9 -153.1(9) 3_546 . . . ? O7 Ag2 N5 C9 174.2(6) 3_536 . . . ? O7' Ag2 N5 C9 31.9(14) . . . . ? O8 Ag2 N5 C9 8.4(5) . . . . ? Ag2 Ag2 N5 C9 107.3(5) 3_536 . . . ? Ag1 Ag2 N5 C9 -95.5(5) . . . . ? O5 Ag2 N5 C12 83.4(14) 3_546 . . . ? O5' Ag2 N5 C12 30.3(10) 3_546 . . . ? O7 Ag2 N5 C12 -2.4(5) 3_536 . . . ? O7' Ag2 N5 C12 -144.6(14) . . . . ? O8 Ag2 N5 C12 -168.1(5) . . . . ? Ag2 Ag2 N5 C12 -69.2(5) 3_536 . . . ? Ag1 Ag2 N5 C12 87.9(5) . . . . ? C12 N5 C9 C10 -2.5(9) . . . . ? Ag2 N5 C9 C10 -179.3(5) . . . . ? C11 N6 C10 C9 -1.2(9) . . . . ? N5 C9 C10 N6 3.1(10) . . . . ? C10 N6 C11 C12 -0.9(9) . . . . ? C10 N6 C11 S2 179.2(4) . . . . ? C9 N5 C12 C11 0.5(9) . . . . ? Ag2 N5 C12 C11 177.1(4) . . . . ? N6 C11 C12 N5 1.3(9) . . . . ? S2 C11 C12 N5 -178.8(4) . . . . ? N6 C11 S2 O3 -42.9(5) . . . . ? C12 C11 S2 O3 137.2(5) . . . . ? N6 C11 S2 O4 -174.7(5) . . . . ? C12 C11 S2 O4 5.3(6) . . . . ? N6 C11 S2 C13 69.8(5) . . . . ? C12 C11 S2 C13 -110.1(5) . . . . ? N8 Ag3 N8 C14 -8.4(4) 2_456 . . . ? N3 Ag3 N8 C14 111.5(5) 4_556 . . . ? N3 Ag3 N8 C14 -124.8(5) 3_456 . . . ? N8 Ag3 N8 C15 170.5(6) 2_456 . . . ? N3 Ag3 N8 C15 -69.6(5) 4_556 . . . ? N3 Ag3 N8 C15 54.0(6) 3_456 . . . ? C16 N7 C13 C14 -0.9(10) . . . . ? C16 N7 C13 S2 -179.9(6) . . . . ? O3 S2 C13 N7 -165.9(5) . . . . ? O4 S2 C13 N7 -33.9(6) . . . . ? C11 S2 C13 N7 80.3(5) . . . . ? O3 S2 C13 C14 15.1(6) . . . . ? O4 S2 C13 C14 147.1(5) . . . . ? C11 S2 C13 C14 -98.8(5) . . . . ? C15 N8 C14 C13 -1.0(9) . . . . ? Ag3 N8 C14 C13 177.9(4) . . . . ? N7 C13 C14 N8 1.9(10) . . . . ? S2 C13 C14 N8 -179.2(4) . . . . ? C14 N8 C15 C16 -0.6(11) . . . . ? Ag3 N8 C15 C16 -179.6(7) . . . . ? C13 N7 C16 C15 -0.8(13) . . . . ? N8 C15 C16 N7 1.6(14) . . . . ? O6 C17 C18 F13 91.8(11) . . . . ? O5 C17 C18 F13 -104.9(12) . . . . ? O5' C17 C18 F13 -44.6(17) . . . . ? O6 C17 C18 F12 -32.8(11) . . . . ? O5 C17 C18 F12 130.5(10) . . . . ? O5' C17 C18 F12 -169.2(14) . . . . ? O6 C17 C18 F11 -149.3(8) . . . . ? O5 C17 C18 F11 14.0(12) . . . . ? O5' C17 C18 F11 74.3(16) . . . . ? O6 C17 O5 O5' -101.0(15) . . . . ? C18 C17 O5 O5' 97.8(13) . . . . ? O6 C17 O5 Ag2 -42.7(14) . . . 3_546 ? O5' C17 O5 Ag2 58.2(12) . . . 3_546 ? C18 C17 O5 Ag2 156.0(6) . . . 3_546 ? Ag2 O5 O5' C17 -128.6(8) 3_546 . . . ? C17 O5 O5' Ag2 128.6(8) . . . 3_546 ? O6 C17 O5' O5 117.6(12) . . . . ? C18 C17 O5' O5 -106.5(10) . . . . ? O6 C17 O5' Ag2 63.7(18) . . . 3_546 ? O5 C17 O5' Ag2 -53.9(11) . . . 3_546 ? C18 C17 O5' Ag2 -160.4(8) . . . 3_546 ? O5 C17 O6 Ag1 33.7(13) . . . . ? O5' C17 O6 Ag1 -32.6(16) . . . . ? C18 C17 O6 Ag1 -165.4(5) . . . . ? N1 Ag1 O6 C17 90.5(7) 3_546 . . . ? N1 Ag1 O6 C17 -89.5(7) . . . . ? O6 Ag1 O6 C17 129(100) 3_546 . . . ? Ag2 Ag1 O6 C17 -7.3(6) 3_546 . . . ? Ag2 Ag1 O6 C17 172.7(6) . . . . ? O8 C19 C20 F21 -139.5(15) . . . . ? O7' C19 C20 F21 -7(3) . . . . ? O7 C19 C20 F21 51.6(17) . . . . ? O8 C19 C20 F22' 164(2) . . . . ? O7' C19 C20 F22' -63(3) . . . . ? O7 C19 C20 F22' -5(2) . . . . ? O8 C19 C20 F23 -3.7(14) . . . . ? O7' C19 C20 F23 129(3) . . . . ? O7 C19 C20 F23 -172.6(10) . . . . ? O8 C19 C20 F22 101.4(12) . . . . ? O7' C19 C20 F22 -126(3) . . . . ? O7 C19 C20 F22 -67.5(12) . . . . ? O8 C19 C20 F21' -90.5(14) . . . . ? O7' C19 C20 F21' 42(3) . . . . ? O7 C19 C20 F21' 100.6(14) . . . . ? O8 C19 O7 O7' 75.0(19) . . . . ? C20 C19 O7 O7' -118.2(15) . . . . ? O8 C19 O7 Ag2 25(2) . . . 3_536 ? O7' C19 O7 Ag2 -50.4(15) . . . 3_536 ? C20 C19 O7 Ag2 -168.5(8) . . . 3_536 ? Ag2 O7 O7' C19 145.2(9) 3_536 . . . ? C19 O7 O7' Ag2 -93.0(14) . . . . ? Ag2 O7 O7' Ag2 52.1(12) 3_536 . . . ? O8 C19 O7' O7 -132.6(13) . . . . ? C20 C19 O7' O7 89(2) . . . . ? O8 C19 O7' Ag2 -25(2) . . . . ? O7 C19 O7' Ag2 107.6(19) . . . . ? C20 C19 O7' Ag2 -163.3(8) . . . . ? N5 Ag2 O7' O7 50(3) . . . . ? O5 Ag2 O7' O7 -142(2) 3_546 . . . ? O5' Ag2 O7' O7 -126.6(19) 3_546 . . . ? O7 Ag2 O7' O7 -79.8(17) 3_536 . . . ? O8 Ag2 O7' O7 83.9(16) . . . . ? Ag2 Ag2 O7' O7 -53.1(18) 3_536 . . . ? Ag1 Ag2 O7' O7 159.0(15) . . . . ? N5 Ag2 O7' C19 -17(3) . . . . ? O5 Ag2 O7' C19 150(3) 3_546 . . . ? O5' Ag2 O7' C19 166(2) 3_546 . . . ? O7 Ag2 O7' C19 -147.6(18) 3_536 . . . ? O8 Ag2 O7' C19 16.1(14) . . . . ? Ag2 Ag2 O7' C19 -121(3) 3_536 . . . ? Ag1 Ag2 O7' C19 91(2) . . . . ? O7' C19 O8 Ag2 25.0(19) . . . . ? O7 C19 O8 Ag2 -28.8(14) . . . . ? C20 C19 O8 Ag2 165.5(7) . . . . ? N5 Ag2 O8 C19 139.8(6) . . . . ? O5 Ag2 O8 C19 -53.6(6) 3_546 . . . ? O5' Ag2 O8 C19 -52.9(8) 3_546 . . . ? O7 Ag2 O8 C19 49.7(15) 3_536 . . . ? O7' Ag2 O8 C19 -16.8(15) . . . . ? Ag2 Ag2 O8 C19 19.6(6) 3_536 . . . ? Ag1 Ag2 O8 C19 -142.2(6) . . . . ? F22' C20 F21 F21' -169(3) . . . . ? F23 C20 F21 F21' -47(2) . . . . ? F22 C20 F21 F21' -145.3(18) . . . . ? C19 C20 F21 F21' 90.7(19) . . . . ? F23 C20 F21 F22' 122(3) . . . . ? F22 C20 F21 F22' 24(3) . . . . ? F21' C20 F21 F22' 169(3) . . . . ? C19 C20 F21 F22' -101(2) . . . . ? F22' F21 F21' C20 -16(4) . . . . ? F22' F21 F21' F23 15(5) . . . . ? C20 F21 F21' F23 30.6(11) . . . . ? F22' C20 F21' F21 9(2) . . . . ? F23 C20 F21' F21 136(2) . . . . ? F22 C20 F21' F21 54(3) . . . . ? C19 C20 F21' F21 -110.2(18) . . . . ? F21 C20 F21' F23 -136(2) . . . . ? F22' C20 F21' F23 -128(2) . . . . ? F22 C20 F21' F23 -82.5(15) . . . . ? C19 C20 F21' F23 113.5(9) . . . . ? F21 C20 F22 F22' -21(2) . . . . ? F23 C20 F22 F22' -134.2(18) . . . . ? F21' C20 F22 F22' -57(3) . . . . ? C19 C20 F22 F22' 106.4(18) . . . . ? F21' F21 F22' C20 17(4) . . . . ? F21' F21 F22' F22 -14(6) . . . . ? C20 F21 F22' F22 -31(2) . . . . ? F23 C20 F22' F21 -87(3) . . . . ? F22 C20 F22' F21 -152(3) . . . . ? F21' C20 F22' F21 -8(2) . . . . ? C19 C20 F22' F21 106.3(18) . . . . ? F21 C20 F22' F22 152(3) . . . . ? F23 C20 F22' F22 65.0(18) . . . . ? F21' C20 F22' F22 144.5(17) . . . . ? C19 C20 F22' F22 -101.3(19) . . . . ? C20 F22 F22' F21 30(3) . . . . ? F21 C20 F23 F21' 32.0(13) . . . . ? F22' C20 F23 F21' 87(2) . . . . ? F22 C20 F23 F21' 136.9(11) . . . . ? C19 C20 F23 F21' -106.6(11) . . . . ? F21 F21' F23 C20 -36.2(16) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.642 _refine_diff_density_min -1.512 _refine_diff_density_rms 0.145 ####################END########################### ######################################################### data_compound3 _database_code_depnum_ccdc_archive 'CCDC 728104' #TrackingRef 'cqw6rev.CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H6 Ag3 N7 O8 S' _chemical_formula_weight 683.87 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 Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 9.7425(9) _cell_length_b 20.2668(19) _cell_length_c 8.0361(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1586.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.863 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 3.858 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.721724 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10255 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.30 _reflns_number_total 2018 _reflns_number_gt 1536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0724P)^2^+6.8743P] 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 2018 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1440 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.114 _refine_ls_shift/su_mean 0.001 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 0.81837(7) 0.7500 0.14743(9) 0.0523(3) Uani 1 2 d S . . Ag2 Ag 1.11887(7) 0.55917(4) -0.57513(7) 0.0696(3) Uani 1 1 d . . . S1 S 0.74891(18) 0.7500 -0.2896(2) 0.0301(4) Uani 1 2 d S . . O1 O 0.6416(6) 0.7500 -0.1716(8) 0.0437(14) Uani 1 2 d S . . O2 O 0.7194(6) 0.7500 -0.4630(8) 0.0448(14) Uani 1 2 d S . . N1 N 1.0137(5) 0.6020(2) -0.3507(6) 0.0366(10) Uani 1 1 d . . . N2 N 0.8873(5) 0.6697(2) -0.0887(6) 0.0332(10) Uani 1 1 d . . . C1 C 1.0408(6) 0.5888(3) -0.1946(8) 0.0396(13) Uani 1 1 d . . . H1A H 1.1038 0.5556 -0.1710 0.048 Uiso 1 1 calc R . . C2 C 0.9798(6) 0.6222(3) -0.0622(7) 0.0374(12) Uani 1 1 d . . . H2A H 1.0037 0.6111 0.0463 0.045 Uiso 1 1 calc R . . C3 C 0.8592(5) 0.6825(3) -0.2490(6) 0.0273(10) Uani 1 1 d . . . C4 C 0.9199(6) 0.6493(3) -0.3802(7) 0.0316(11) Uani 1 1 d . . . H4A H 0.8958 0.6597 -0.4890 0.038 Uiso 1 1 calc R . . N5 N 1.2740(8) 0.5359(4) -0.8730(9) 0.0636(17) Uani 1 1 d . . . O3 O 1.3304(8) 0.5713(4) -0.7757(9) 0.089(2) Uani 1 1 d . . . O4 O 1.1653(7) 0.5140(3) -0.8346(8) 0.0810(19) Uani 1 1 d . . . N6 N 1.0945(16) 0.7500 0.2933(13) 0.024(2) Uani 0.50 2 d SP . . N6' N 1.0228(17) 0.7500 0.264(2) 0.086(12) Uani 0.50 2 d SP . . O5 O 1.0610(11) 0.6978(3) 0.2806(8) 0.090(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0259(3) 0.0917(6) 0.0392(4) 0.000 0.0015(3) 0.000 Ag2 0.0688(4) 0.0975(6) 0.0426(3) -0.0180(3) 0.0116(3) 0.0172(3) S1 0.0236(8) 0.0355(9) 0.0313(9) 0.000 -0.0068(7) 0.000 O1 0.027(3) 0.053(4) 0.052(4) 0.000 0.003(2) 0.000 O2 0.046(3) 0.051(4) 0.037(3) 0.000 -0.023(3) 0.000 N1 0.042(3) 0.035(2) 0.032(2) -0.005(2) 0.003(2) 0.000(2) N2 0.035(2) 0.036(2) 0.028(2) 0.0014(18) 0.0015(18) 0.0036(19) C1 0.045(3) 0.031(3) 0.043(3) -0.002(2) -0.005(3) 0.005(2) C2 0.043(3) 0.041(3) 0.029(3) 0.003(2) -0.003(2) 0.004(2) C3 0.023(2) 0.032(2) 0.027(2) -0.002(2) -0.0029(18) -0.0058(19) C4 0.036(3) 0.031(3) 0.028(2) -0.001(2) 0.000(2) -0.001(2) N5 0.058(4) 0.077(5) 0.056(4) 0.010(4) 0.005(3) 0.014(4) O3 0.090(5) 0.111(5) 0.068(4) 0.002(4) -0.008(4) -0.045(4) O4 0.083(4) 0.083(4) 0.077(4) -0.014(3) 0.014(3) -0.029(4) N6 0.029(8) 0.034(8) 0.009(5) 0.000 0.000(5) 0.000 N6' 0.000(6) 0.23(4) 0.027(8) 0.000 -0.008(6) 0.000 O5 0.160(8) 0.063(4) 0.046(3) 0.006(3) 0.018(4) 0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N6' 2.199(18) . ? Ag1 N6 2.232(16) 6_556 ? Ag1 N2 2.588(5) . ? Ag1 N2 2.588(5) 7_575 ? Ag2 N1 2.249(5) . ? Ag2 O4 2.322(7) . ? S1 O1 1.411(6) . ? S1 O2 1.423(6) . ? S1 C3 1.770(5) 7_575 ? S1 C3 1.770(5) . ? N1 C1 1.310(8) . ? N1 C4 1.345(7) . ? N2 C2 1.336(8) . ? N2 C3 1.342(7) . ? C1 C2 1.394(8) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.383(7) . ? C4 H4A 0.9300 . ? N5 O4 1.189(9) . ? N5 O3 1.195(10) . ? N6 N6' 0.739(16) . ? N6 O5 1.111(10) . ? N6 O5 1.111(10) 7_575 ? N6 Ag1 2.232(16) 6_656 ? N6' O5 1.130(9) . ? N6' O5 1.130(9) 7_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6' Ag1 N6 142.6(5) . 6_556 ? N6' Ag1 N2 94.4(4) . . ? N6 Ag1 N2 114.2(2) 6_556 . ? N6' Ag1 N2 94.4(4) . 7_575 ? N6 Ag1 N2 114.2(2) 6_556 7_575 ? N2 Ag1 N2 77.9(2) . 7_575 ? N1 Ag2 O4 164.0(2) . . ? O1 S1 O2 120.5(4) . . ? O1 S1 C3 109.0(2) . 7_575 ? O2 S1 C3 107.6(2) . 7_575 ? O1 S1 C3 109.0(2) . . ? O2 S1 C3 107.6(2) . . ? C3 S1 C3 101.3(3) 7_575 . ? C1 N1 C4 116.8(5) . . ? C1 N1 Ag2 126.7(4) . . ? C4 N1 Ag2 116.3(4) . . ? C2 N2 C3 115.4(5) . . ? C2 N2 Ag1 120.8(4) . . ? C3 N2 Ag1 122.0(4) . . ? N1 C1 C2 123.1(5) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? N2 C2 C1 121.0(5) . . ? N2 C2 H2A 119.5 . . ? C1 C2 H2A 119.5 . . ? N2 C3 C4 123.4(5) . . ? N2 C3 S1 116.7(4) . . ? C4 C3 S1 119.7(4) . . ? N1 C4 C3 120.2(5) . . ? N1 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? O4 N5 O3 117.6(8) . . ? N5 O4 Ag2 105.0(5) . . ? N6' N6 O5 72.1(11) . . ? N6' N6 O5 72.1(11) . 7_575 ? O5 N6 O5 144(2) . 7_575 ? N6' N6 Ag1 173.4(17) . 6_656 ? O5 N6 Ag1 107.8(11) . 6_656 ? O5 N6 Ag1 107.8(11) 7_575 6_656 ? N6 N6' O5 69.4(12) . . ? N6 N6' O5 69.4(12) . 7_575 ? O5 N6' O5 139(2) . 7_575 ? N6 N6' Ag1 174(2) . . ? O5 N6' Ag1 110.5(12) . . ? O5 N6' Ag1 110.5(12) 7_575 . ? N6 O5 N6' 38.5(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 O4 Ag2 N1 C1 138.8(8) . . . . ? O4 Ag2 N1 C4 -46.0(10) . . . . ? N6' Ag1 N2 C2 33.2(5) . . . . ? N6 Ag1 N2 C2 -121.9(5) 6_556 . . . ? N2 Ag1 N2 C2 126.8(4) 7_575 . . . ? N6' Ag1 N2 C3 -130.7(5) . . . . ? N6 Ag1 N2 C3 74.1(4) 6_556 . . . ? N2 Ag1 N2 C3 -37.2(4) 7_575 . . . ? C4 N1 C1 C2 -1.4(9) . . . . ? Ag2 N1 C1 C2 173.7(5) . . . . ? C3 N2 C2 C1 -0.1(8) . . . . ? Ag1 N2 C2 C1 -165.1(4) . . . . ? N1 C1 C2 N2 0.8(10) . . . . ? C2 N2 C3 C4 0.2(8) . . . . ? Ag1 N2 C3 C4 164.9(4) . . . . ? C2 N2 C3 S1 -174.6(4) . . . . ? Ag1 N2 C3 S1 -9.8(5) . . . . ? O1 S1 C3 N2 -40.7(5) . . . . ? O2 S1 C3 N2 -173.1(4) . . . . ? C3 S1 C3 N2 74.1(5) 7_575 . . . ? O1 S1 C3 C4 144.3(4) . . . . ? O2 S1 C3 C4 12.0(5) . . . . ? C3 S1 C3 C4 -100.8(4) 7_575 . . . ? C1 N1 C4 C3 1.4(8) . . . . ? Ag2 N1 C4 C3 -174.2(4) . . . . ? N2 C3 C4 N1 -0.8(8) . . . . ? S1 C3 C4 N1 173.8(4) . . . . ? O3 N5 O4 Ag2 1.9(9) . . . . ? N1 Ag2 O4 N5 145.9(7) . . . . ? O5 N6 N6' O5 -179.0(13) 7_575 . . . ? Ag1 N6 N6' O5 90.5(7) 6_656 . . . ? O5 N6 N6' O5 179.0(13) . . . 7_575 ? Ag1 N6 N6' O5 -90.5(7) 6_656 . . 7_575 ? O5 N6 N6' Ag1 -90.5(7) . . . . ? O5 N6 N6' Ag1 90.5(7) 7_575 . . . ? Ag1 N6 N6' Ag1 0.00(3) 6_656 . . . ? N6 Ag1 N6' N6 180.000(6) 6_556 . . . ? N2 Ag1 N6' N6 39.07(11) . . . . ? N2 Ag1 N6' N6 -39.07(11) 7_575 . . . ? N6 Ag1 N6' O5 91.8(12) 6_556 . . . ? N2 Ag1 N6' O5 -49.1(12) . . . . ? N2 Ag1 N6' O5 -127.2(12) 7_575 . . . ? N6 Ag1 N6' O5 -91.8(12) 6_556 . . 7_575 ? N2 Ag1 N6' O5 127.2(12) . . . 7_575 ? N2 Ag1 N6' O5 49.1(12) 7_575 . . 7_575 ? O5 N6 O5 N6' 2(2) 7_575 . . . ? Ag1 N6 O5 N6' -173.1(18) 6_656 . . . ? O5 N6' O5 N6 -1.4(19) 7_575 . . . ? Ag1 N6' O5 N6 173(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.752 _refine_diff_density_min -0.951 _refine_diff_density_rms 0.157 ################################################### data_compound1 _database_code_depnum_ccdc_archive 'CCDC 728105' #TrackingRef 'cqw6rev.CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H6 Ag Cl N4 O6 S' _chemical_formula_weight 429.55 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.8459(8) _cell_length_b 11.2785(12) _cell_length_c 14.4645(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1280.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 1.981 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.884088 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8900 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 28.29 _reflns_number_total 3188 _reflns_number_gt 2833 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruler SMART' _computing_cell_refinement 'Bruler SMART' _computing_data_reduction 'Bruler SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruler SHELXTL' _computing_publication_material 'Bruler 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. The DFIX command is used to the Cl-O bonds' lengthes at 1.44 angstrom in perchlorate because of their abnormal thermal vibration. The 'SADI' command is used to refine the normal tetrahedral geometry of the perchlorate. ; _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^)+(0.0504P)^2^+0.4798P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 3188 _refine_ls_number_parameters 190 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0927 _refine_ls_wR_factor_gt 0.0887 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.092 _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 0.67310(5) 0.44820(4) 0.83684(2) 0.03981(12) Uani 1 1 d . . . S1 S 0.53258(14) 0.35040(9) 0.43612(7) 0.0297(2) Uani 1 1 d . . . O1 O 0.4304(5) 0.2635(3) 0.4812(3) 0.0474(9) Uani 1 1 d . . . O2 O 0.6468(5) 0.3181(3) 0.3624(2) 0.0436(8) Uani 1 1 d . . . N1 N 0.7188(5) 0.4570(4) 0.6803(2) 0.0336(8) Uani 1 1 d . . . N2 N 0.7719(4) 0.5004(3) 0.4929(3) 0.0293(7) Uani 1 1 d . . . N3 N 0.1317(5) 0.5576(4) 0.3710(3) 0.0405(9) Uani 1 1 d . . . N4 N 0.4828(4) 0.5465(3) 0.3437(3) 0.0328(7) Uani 1 1 d . . . C1 C 0.6270(5) 0.4025(4) 0.6155(3) 0.0285(9) Uani 1 1 d . . . H1A H 0.5430 0.3488 0.6328 0.034 Uiso 1 1 calc R . . C2 C 0.6549(5) 0.4248(3) 0.5230(3) 0.0246(7) Uani 1 1 d . . . C3 C 0.8618(6) 0.5552(5) 0.5572(3) 0.0374(10) Uani 1 1 d . . . H3A H 0.9454 0.6089 0.5393 0.045 Uiso 1 1 calc R . . C4 C 0.8349(6) 0.5348(4) 0.6505(3) 0.0377(9) Uani 1 1 d . . . H4A H 0.8994 0.5764 0.6936 0.045 Uiso 1 1 calc R . . C5 C 0.3991(5) 0.4657(4) 0.3930(3) 0.0290(8) Uani 1 1 d . . . C6 C 0.2259(6) 0.4689(4) 0.4071(4) 0.0372(10) Uani 1 1 d . . . H6A H 0.1735 0.4097 0.4416 0.045 Uiso 1 1 calc R . . C7 C 0.2161(6) 0.6394(5) 0.3216(4) 0.0420(11) Uani 1 1 d . . . H7A H 0.1556 0.7021 0.2957 0.050 Uiso 1 1 calc R . . C8 C 0.3896(6) 0.6334(4) 0.3082(4) 0.0397(11) Uani 1 1 d . . . H8A H 0.4429 0.6918 0.2732 0.048 Uiso 1 1 calc R . . Cl1 Cl 0.67475(16) 0.14605(11) 0.85765(10) 0.0514(3) Uani 1 1 d D . . O3 O 0.5846(11) 0.1666(6) 0.7727(3) 0.142(3) Uani 1 1 d D . . O4 O 0.8113(7) 0.2262(5) 0.8775(8) 0.204(6) Uani 1 1 d D . . O5 O 0.5451(7) 0.1622(6) 0.9273(4) 0.108(2) Uani 1 1 d D . . O6 O 0.7332(6) 0.0260(2) 0.8650(4) 0.0815(16) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03704(17) 0.0588(2) 0.02356(16) -0.00532(16) 0.00262(14) -0.01007(17) S1 0.0364(5) 0.0261(4) 0.0264(5) 0.0003(4) -0.0048(4) -0.0035(4) O1 0.056(2) 0.0383(17) 0.048(2) 0.0070(17) -0.0082(18) -0.0189(16) O2 0.056(2) 0.0408(17) 0.0336(17) -0.0114(14) -0.0038(15) 0.0116(15) N1 0.0333(17) 0.0456(19) 0.0220(17) 0.0017(17) -0.0009(13) -0.0044(16) N2 0.0291(16) 0.0335(16) 0.0253(17) 0.0028(14) 0.0014(14) -0.0041(13) N3 0.0296(17) 0.048(2) 0.044(2) 0.000(2) -0.0011(16) 0.0003(17) N4 0.0275(15) 0.0380(17) 0.0329(18) 0.008(2) 0.0012(15) -0.0015(14) C1 0.027(2) 0.033(2) 0.025(2) 0.0037(16) 0.0014(16) -0.0008(15) C2 0.0252(18) 0.0246(17) 0.0241(18) -0.0019(14) -0.0017(15) 0.0013(15) C3 0.037(2) 0.045(2) 0.030(2) 0.005(2) -0.0060(17) -0.010(2) C4 0.038(2) 0.047(2) 0.029(2) -0.0054(18) -0.004(2) -0.006(2) C5 0.0307(18) 0.033(2) 0.0233(19) -0.0008(18) -0.0026(16) -0.0032(17) C6 0.035(2) 0.039(3) 0.038(2) -0.001(2) 0.0040(18) -0.0078(18) C7 0.036(2) 0.043(2) 0.047(3) 0.006(2) -0.003(2) 0.0058(19) C8 0.036(2) 0.038(2) 0.045(3) 0.014(2) 0.003(2) -0.0053(19) Cl1 0.0384(5) 0.0387(5) 0.0771(9) 0.0055(6) 0.0045(7) 0.0036(5) O3 0.224(9) 0.134(5) 0.068(4) 0.004(4) 0.000(5) 0.104(6) O4 0.078(4) 0.064(4) 0.47(2) 0.048(7) -0.018(8) -0.008(3) O5 0.111(5) 0.119(5) 0.093(4) -0.005(4) 0.032(4) 0.018(4) O6 0.081(3) 0.039(2) 0.125(5) 0.002(3) -0.003(3) 0.006(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 N1 2.295(3) . ? Ag1 N2 2.370(4) 2_665 ? Ag1 N3 2.443(4) 2_565 ? S1 O1 1.424(3) . ? S1 O2 1.440(4) . ? S1 C5 1.782(5) . ? S1 C2 1.790(4) . ? N1 C1 1.333(6) . ? N1 C4 1.336(6) . ? N2 C3 1.321(6) . ? N2 C2 1.327(5) . ? N2 Ag1 2.370(4) 2_664 ? N3 C7 1.342(7) . ? N3 C6 1.349(7) . ? N3 Ag1 2.443(4) 2_564 ? N4 C8 1.326(6) . ? N4 C5 1.330(5) . ? C1 C2 1.378(6) . ? C1 H1A 0.9300 . ? C3 C4 1.385(6) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 C6 1.375(6) . ? C6 H6A 0.9300 . ? C7 C8 1.377(7) . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? Cl1 O4 1.431(2) . ? Cl1 O6 1.4337(19) . ? Cl1 O3 1.436(2) . ? Cl1 O5 1.443(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 N1 Ag1 N2 154.26(13) . 2_665 ? N1 Ag1 N3 110.71(14) . 2_565 ? N2 Ag1 N3 89.55(13) 2_665 2_565 ? O1 S1 O2 121.0(2) . . ? O1 S1 C5 109.3(2) . . ? O2 S1 C5 106.9(2) . . ? O1 S1 C2 107.6(2) . . ? O2 S1 C2 107.8(2) . . ? C5 S1 C2 102.61(19) . . ? C1 N1 C4 116.4(4) . . ? C1 N1 Ag1 126.2(3) . . ? C4 N1 Ag1 116.9(3) . . ? C3 N2 C2 116.0(4) . . ? C3 N2 Ag1 117.3(3) . 2_664 ? C2 N2 Ag1 126.6(3) . 2_664 ? C7 N3 C6 116.5(4) . . ? C7 N3 Ag1 113.2(3) . 2_564 ? C6 N3 Ag1 126.5(3) . 2_564 ? C8 N4 C5 116.2(4) . . ? N1 C1 C2 120.9(4) . . ? N1 C1 H1A 119.6 . . ? C2 C1 H1A 119.6 . . ? N2 C2 C1 123.1(4) . . ? N2 C2 S1 116.2(3) . . ? C1 C2 S1 120.7(3) . . ? N2 C3 C4 121.8(4) . . ? N2 C3 H3A 119.1 . . ? C4 C3 H3A 119.1 . . ? N1 C4 C3 121.8(4) . . ? N1 C4 H4A 119.1 . . ? C3 C4 H4A 119.1 . . ? N4 C5 C6 123.3(4) . . ? N4 C5 S1 113.4(3) . . ? C6 C5 S1 123.2(4) . . ? N3 C6 C5 120.3(5) . . ? N3 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 . . ? N3 C7 C8 121.9(5) . . ? N3 C7 H7A 119.0 . . ? C8 C7 H7A 119.0 . . ? N4 C8 C7 121.8(5) . . ? N4 C8 H8A 119.1 . . ? C7 C8 H8A 119.1 . . ? O4 Cl1 O6 110.0(4) . . ? O4 Cl1 O3 116.0(5) . . ? O6 Cl1 O3 111.9(3) . . ? O4 Cl1 O5 107.9(5) . . ? O6 Cl1 O5 107.0(4) . . ? O3 Cl1 O5 103.3(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 C1 -176.3(3) 2_665 . . . ? N3 Ag1 N1 C1 -36.4(4) 2_565 . . . ? N2 Ag1 N1 C4 -4.9(5) 2_665 . . . ? N3 Ag1 N1 C4 135.0(3) 2_565 . . . ? C4 N1 C1 C2 1.3(6) . . . . ? Ag1 N1 C1 C2 172.7(3) . . . . ? C3 N2 C2 C1 -0.4(6) . . . . ? Ag1 N2 C2 C1 -177.8(3) 2_664 . . . ? C3 N2 C2 S1 179.9(3) . . . . ? Ag1 N2 C2 S1 2.6(5) 2_664 . . . ? N1 C1 C2 N2 -0.2(6) . . . . ? N1 C1 C2 S1 179.4(3) . . . . ? O1 S1 C2 N2 172.9(3) . . . . ? O2 S1 C2 N2 40.9(4) . . . . ? C5 S1 C2 N2 -71.8(3) . . . . ? O1 S1 C2 C1 -6.7(4) . . . . ? O2 S1 C2 C1 -138.8(3) . . . . ? C5 S1 C2 C1 108.6(4) . . . . ? C2 N2 C3 C4 -0.1(7) . . . . ? Ag1 N2 C3 C4 177.5(4) 2_664 . . . ? C1 N1 C4 C3 -1.8(7) . . . . ? Ag1 N1 C4 C3 -174.1(4) . . . . ? N2 C3 C4 N1 1.3(8) . . . . ? C8 N4 C5 C6 0.5(7) . . . . ? C8 N4 C5 S1 178.7(4) . . . . ? O1 S1 C5 N4 -175.2(3) . . . . ? O2 S1 C5 N4 -42.5(4) . . . . ? C2 S1 C5 N4 70.7(3) . . . . ? O1 S1 C5 C6 2.9(5) . . . . ? O2 S1 C5 C6 135.6(4) . . . . ? C2 S1 C5 C6 -111.1(4) . . . . ? C7 N3 C6 C5 0.3(7) . . . . ? Ag1 N3 C6 C5 156.7(4) 2_564 . . . ? N4 C5 C6 N3 -0.7(8) . . . . ? S1 C5 C6 N3 -178.6(3) . . . . ? C6 N3 C7 C8 0.2(8) . . . . ? Ag1 N3 C7 C8 -159.3(4) 2_564 . . . ? C5 N4 C8 C7 0.0(7) . . . . ? N3 C7 C8 N4 -0.3(9) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.912 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.109 ###################################### data_compound4 _database_code_depnum_ccdc_archive 'CCDC 728106' #TrackingRef 'cqw6rev.CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H6 Ag F3 N4 O5 S2' _chemical_formula_weight 479.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' F F 0.0171 0.0103 '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 Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 12.178(5) _cell_length_b 8.010(3) _cell_length_c 14.622(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1426.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.774 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.419549 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9129 _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_av_sigmaI/netI 0.0820 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 28.38 _reflns_number_total 3321 _reflns_number_gt 2027 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0769P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(6) _refine_ls_number_reflns 3321 _refine_ls_number_parameters 217 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1655 _refine_ls_wR_factor_gt 0.1341 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.43148(6) 0.06437(9) 0.31881(5) 0.0565(3) Uani 1 1 d . . . S1 S 0.6896(2) 0.0581(3) 0.42348(16) 0.0424(5) Uani 1 1 d . . . O1 O 0.6557(7) 0.1622(8) 0.3500(5) 0.0604(19) Uani 1 1 d . . . O2 O 0.7943(6) 0.0831(9) 0.4653(6) 0.062(2) Uani 1 1 d . . . N1 N 0.5356(7) 0.0382(10) 0.6647(6) 0.0478(19) Uani 1 1 d . . . N2 N 0.4825(6) 0.0761(9) 0.4782(6) 0.0413(17) Uani 1 1 d . . . N3 N 0.7673(7) -0.4073(9) 0.3485(6) 0.050(2) Uani 1 1 d . . . N4 N 0.5855(6) -0.1944(9) 0.3486(5) 0.0449(19) Uani 1 1 d . . . C1 C 0.6135(9) 0.0456(12) 0.5984(7) 0.045(2) Uani 1 1 d . . . H1A H 0.6871 0.0402 0.6151 0.054 Uiso 1 1 calc R . . C2 C 0.5876(8) 0.0603(10) 0.5100(7) 0.043(2) Uani 1 1 d . . . C3 C 0.4059(8) 0.0685(11) 0.5457(7) 0.046(2) Uani 1 1 d . . . H3A H 0.3321 0.0778 0.5303 0.055 Uiso 1 1 calc R . . C4 C 0.4336(9) 0.0478(13) 0.6348(8) 0.052(2) Uani 1 1 d . . . H4A H 0.3772 0.0400 0.6775 0.063 Uiso 1 1 calc R . . C5 C 0.6821(7) -0.1472(11) 0.3839(6) 0.0365(18) Uani 1 1 d . . . C6 C 0.7724(8) -0.2541(11) 0.3865(6) 0.044(2) Uani 1 1 d . . . H6A H 0.8370 -0.2194 0.4147 0.053 Uiso 1 1 calc R . . C7 C 0.6718(8) -0.4539(10) 0.3133(10) 0.052(2) Uani 1 1 d . . . H7A H 0.6651 -0.5603 0.2884 0.062 Uiso 1 1 calc R . . C8 C 0.5815(7) -0.3476(11) 0.3125(8) 0.045(2) Uani 1 1 d . . . H8A H 0.5163 -0.3843 0.2862 0.054 Uiso 1 1 calc R . . C9 C 0.4598(10) 0.4551(13) 0.0811(8) 0.054(3) Uani 1 1 d . . . F1 F 0.5421(7) 0.5510(9) 0.1129(6) 0.082(2) Uani 1 1 d . . . F2 F 0.4165(9) 0.5320(11) 0.0141(6) 0.104(3) Uani 1 1 d . . . F3 F 0.5069(7) 0.3148(8) 0.0501(5) 0.080(2) Uani 1 1 d . . . S2 S 0.3640(2) 0.4070(3) 0.1732(2) 0.0496(6) Uani 1 1 d . . . O3 O 0.4314(6) 0.3327(10) 0.2429(5) 0.0587(19) Uani 1 1 d . . . O4 O 0.3242(7) 0.5729(9) 0.1980(7) 0.070(2) Uani 1 1 d . . . O5 O 0.2860(6) 0.3010(10) 0.1307(7) 0.080(3) 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 0.0657(5) 0.0609(5) 0.0428(4) 0.0089(4) -0.0050(5) -0.0161(4) S1 0.0514(13) 0.0308(10) 0.0450(11) -0.0007(9) 0.0028(11) -0.0057(9) O1 0.084(5) 0.035(3) 0.062(4) 0.019(3) 0.013(4) 0.010(3) O2 0.055(4) 0.063(5) 0.067(5) -0.019(4) 0.000(4) -0.023(4) N1 0.056(5) 0.049(5) 0.039(4) -0.010(3) 0.002(4) -0.003(4) N2 0.044(4) 0.033(4) 0.047(4) -0.003(3) -0.006(4) 0.003(3) N3 0.050(5) 0.035(4) 0.065(5) -0.002(3) -0.002(4) 0.006(3) N4 0.050(5) 0.040(4) 0.044(4) -0.011(3) -0.009(3) -0.003(3) C1 0.046(5) 0.035(5) 0.054(6) -0.010(4) -0.006(5) 0.008(4) C2 0.049(5) 0.023(4) 0.057(6) -0.002(4) 0.000(4) 0.003(4) C3 0.044(5) 0.040(5) 0.054(6) -0.002(4) 0.001(4) 0.005(4) C4 0.051(6) 0.052(6) 0.054(6) -0.008(5) 0.006(5) -0.002(5) C5 0.034(5) 0.041(5) 0.034(4) 0.011(4) 0.001(3) -0.001(4) C6 0.040(5) 0.036(5) 0.055(5) -0.003(4) 0.000(4) 0.006(4) C7 0.073(6) 0.027(4) 0.056(5) 0.002(5) -0.024(7) 0.000(4) C8 0.046(5) 0.043(4) 0.046(5) -0.014(5) -0.006(5) -0.008(4) C9 0.079(8) 0.042(6) 0.042(6) -0.010(4) 0.009(5) 0.004(5) F1 0.097(5) 0.078(6) 0.072(5) -0.018(4) 0.027(4) -0.040(4) F2 0.182(10) 0.079(6) 0.050(4) 0.009(4) -0.021(5) 0.014(5) F3 0.110(6) 0.048(4) 0.081(4) -0.014(3) 0.042(4) 0.003(4) S2 0.0506(14) 0.0365(12) 0.0617(15) -0.0072(11) -0.0032(13) -0.0034(11) O3 0.067(5) 0.057(5) 0.052(4) 0.012(3) -0.005(3) -0.011(4) O4 0.078(5) 0.045(5) 0.088(6) -0.025(4) -0.003(5) 0.007(4) O5 0.043(4) 0.063(5) 0.136(8) -0.038(5) -0.019(5) -0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.402(8) 3_445 ? Ag1 N2 2.413(8) . ? Ag1 O3 2.419(7) . ? Ag1 N1 2.432(9) 2_654 ? S1 O1 1.421(7) . ? S1 O2 1.428(8) . ? S1 C5 1.746(10) . ? S1 C2 1.772(11) . ? N1 C4 1.319(14) . ? N1 C1 1.358(14) . ? N1 Ag1 2.432(9) 2_655 ? N2 C3 1.360(14) . ? N2 C2 1.368(12) . ? N3 C7 1.325(13) . ? N3 C6 1.348(12) . ? N3 Ag1 2.402(8) 3_545 ? N4 C8 1.336(11) . ? N4 C5 1.339(11) . ? C1 C2 1.337(14) . ? C1 H1A 0.9300 . ? C3 C4 1.355(16) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 C6 1.395(13) . ? C6 H6A 0.9300 . ? C7 C8 1.391(13) . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? C9 F2 1.273(14) . ? C9 F3 1.341(12) . ? C9 F1 1.346(14) . ? C9 S2 1.822(11) . ? S2 O5 1.418(7) . ? S2 O3 1.437(8) . ? S2 O4 1.460(7) . ? 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 93.4(3) 3_445 . ? N3 Ag1 O3 123.2(3) 3_445 . ? N2 Ag1 O3 114.1(2) . . ? N3 Ag1 N1 97.4(3) 3_445 2_654 ? N2 Ag1 N1 149.9(3) . 2_654 ? O3 Ag1 N1 82.8(3) . 2_654 ? O1 S1 O2 120.0(5) . . ? O1 S1 C5 106.7(4) . . ? O2 S1 C5 108.7(4) . . ? O1 S1 C2 109.3(4) . . ? O2 S1 C2 108.6(5) . . ? C5 S1 C2 102.1(4) . . ? C4 N1 C1 114.8(9) . . ? C4 N1 Ag1 118.8(7) . 2_655 ? C1 N1 Ag1 124.1(7) . 2_655 ? C3 N2 C2 113.0(9) . . ? C3 N2 Ag1 121.5(6) . . ? C2 N2 Ag1 124.4(6) . . ? C7 N3 C6 117.2(8) . . ? C7 N3 Ag1 120.8(7) . 3_545 ? C6 N3 Ag1 120.8(6) . 3_545 ? C8 N4 C5 116.4(7) . . ? C2 C1 N1 122.0(10) . . ? C2 C1 H1A 119.0 . . ? N1 C1 H1A 119.0 . . ? C1 C2 N2 123.9(10) . . ? C1 C2 S1 121.6(8) . . ? N2 C2 S1 114.5(7) . . ? C4 C3 N2 122.2(10) . . ? C4 C3 H3A 118.9 . . ? N2 C3 H3A 118.9 . . ? N1 C4 C3 124.0(10) . . ? N1 C4 H4A 118.0 . . ? C3 C4 H4A 118.0 . . ? N4 C5 C6 122.0(8) . . ? N4 C5 S1 116.1(6) . . ? C6 C5 S1 121.9(7) . . ? N3 C6 C5 120.7(9) . . ? N3 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? N3 C7 C8 121.6(8) . . ? N3 C7 H7A 119.2 . . ? C8 C7 H7A 119.2 . . ? N4 C8 C7 122.0(8) . . ? N4 C8 H8A 119.0 . . ? C7 C8 H8A 119.0 . . ? F2 C9 F3 108.8(10) . . ? F2 C9 F1 107.3(10) . . ? F3 C9 F1 106.1(10) . . ? F2 C9 S2 113.9(10) . . ? F3 C9 S2 110.3(7) . . ? F1 C9 S2 110.1(8) . . ? O5 S2 O3 116.4(5) . . ? O5 S2 O4 115.6(5) . . ? O3 S2 O4 112.9(5) . . ? O5 S2 C9 103.4(6) . . ? O3 S2 C9 104.2(5) . . ? O4 S2 C9 101.8(5) . . ? S2 O3 Ag1 133.9(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 C3 -27.1(6) 3_445 . . . ? O3 Ag1 N2 C3 101.8(6) . . . . ? N1 Ag1 N2 C3 -138.2(7) 2_654 . . . ? N3 Ag1 N2 C2 140.5(7) 3_445 . . . ? O3 Ag1 N2 C2 -90.6(7) . . . . ? N1 Ag1 N2 C2 29.4(10) 2_654 . . . ? C4 N1 C1 C2 -0.4(14) . . . . ? Ag1 N1 C1 C2 162.2(7) 2_655 . . . ? N1 C1 C2 N2 2.8(14) . . . . ? N1 C1 C2 S1 -176.4(7) . . . . ? C3 N2 C2 C1 -2.5(12) . . . . ? Ag1 N2 C2 C1 -171.1(7) . . . . ? C3 N2 C2 S1 176.7(6) . . . . ? Ag1 N2 C2 S1 8.2(9) . . . . ? O1 S1 C2 C1 -147.6(8) . . . . ? O2 S1 C2 C1 -15.0(9) . . . . ? C5 S1 C2 C1 99.7(8) . . . . ? O1 S1 C2 N2 33.1(8) . . . . ? O2 S1 C2 N2 165.7(6) . . . . ? C5 S1 C2 N2 -79.6(7) . . . . ? C2 N2 C3 C4 0.2(12) . . . . ? Ag1 N2 C3 C4 169.1(7) . . . . ? C1 N1 C4 C3 -1.9(15) . . . . ? Ag1 N1 C4 C3 -165.5(7) 2_655 . . . ? N2 C3 C4 N1 2.0(15) . . . . ? C8 N4 C5 C6 -2.5(12) . . . . ? C8 N4 C5 S1 175.6(8) . . . . ? O1 S1 C5 N4 -53.9(7) . . . . ? O2 S1 C5 N4 175.3(7) . . . . ? C2 S1 C5 N4 60.7(7) . . . . ? O1 S1 C5 C6 124.3(7) . . . . ? O2 S1 C5 C6 -6.5(9) . . . . ? C2 S1 C5 C6 -121.1(8) . . . . ? C7 N3 C6 C5 -3.3(14) . . . . ? Ag1 N3 C6 C5 164.6(6) 3_545 . . . ? N4 C5 C6 N3 3.7(13) . . . . ? S1 C5 C6 N3 -174.4(7) . . . . ? C6 N3 C7 C8 2.1(17) . . . . ? Ag1 N3 C7 C8 -165.8(9) 3_545 . . . ? C5 N4 C8 C7 1.3(15) . . . . ? N3 C7 C8 N4 -1.1(19) . . . . ? F2 C9 S2 O5 61.8(9) . . . . ? F3 C9 S2 O5 -60.9(10) . . . . ? F1 C9 S2 O5 -177.6(8) . . . . ? F2 C9 S2 O3 -176.0(8) . . . . ? F3 C9 S2 O3 61.3(10) . . . . ? F1 C9 S2 O3 -55.4(8) . . . . ? F2 C9 S2 O4 -58.4(9) . . . . ? F3 C9 S2 O4 178.9(9) . . . . ? F1 C9 S2 O4 62.2(9) . . . . ? O5 S2 O3 Ag1 -7.5(9) . . . . ? O4 S2 O3 Ag1 129.8(6) . . . . ? C9 S2 O3 Ag1 -120.6(6) . . . . ? N3 Ag1 O3 S2 -32.2(7) 3_445 . . . ? N2 Ag1 O3 S2 -144.0(6) . . . . ? N1 Ag1 O3 S2 61.9(6) 2_654 . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.491 _refine_diff_density_min -1.244 _refine_diff_density_rms 0.169 ############################################################ data_compound2 _database_code_depnum_ccdc_archive 'CCDC 728107' #TrackingRef 'cqw6rev.CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H6 Ag N5 O5 S' _chemical_formula_weight 392.11 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 orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.7095(12) _cell_length_b 10.9140(17) _cell_length_c 14.571(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1226.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 1.843 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.862543 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8451 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.29 _reflns_number_total 3018 _reflns_number_gt 2518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.7214P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.11(4) _refine_ls_number_reflns 3018 _refine_ls_number_parameters 181 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.027 _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 0.69450(5) 0.40877(4) 0.84211(3) 0.04159(12) Uani 1 1 d U . . S1 S 0.52324(17) 0.35928(11) 0.43543(8) 0.0342(3) Uani 1 1 d . . . O1 O 0.4149(6) 0.2692(3) 0.4769(3) 0.0537(10) Uani 1 1 d . . . O2 O 0.6420(5) 0.3270(3) 0.3641(2) 0.0492(10) Uani 1 1 d . . . N1 N 0.7158(6) 0.4527(4) 0.6807(3) 0.0421(10) Uani 1 1 d . . . N2 N 0.7659(5) 0.5100(4) 0.4961(3) 0.0351(9) Uani 1 1 d . . . N3 N 0.1181(6) 0.5712(4) 0.3639(3) 0.0473(11) Uani 1 1 d . . . N4 N 0.4762(5) 0.5637(4) 0.3445(3) 0.0377(9) Uani 1 1 d . . . C1 C 0.6162(7) 0.4032(5) 0.6158(3) 0.0368(10) Uani 1 1 d . . . H1A H 0.5276 0.3495 0.6319 0.044 Uiso 1 1 calc R . . C2 C 0.6444(6) 0.4316(4) 0.5240(3) 0.0301(10) Uani 1 1 d . . . C3 C 0.8611(7) 0.5603(5) 0.5621(4) 0.0425(12) Uani 1 1 d . . . H3A H 0.9456 0.6176 0.5468 0.051 Uiso 1 1 calc R . . C4 C 0.8369(7) 0.5291(5) 0.6533(4) 0.0432(12) Uani 1 1 d . . . H4A H 0.9096 0.5638 0.6972 0.052 Uiso 1 1 calc R . . C5 C 0.3893(6) 0.4789(4) 0.3918(3) 0.0309(10) Uani 1 1 d . . . C6 C 0.2110(7) 0.4818(5) 0.4020(4) 0.0406(12) Uani 1 1 d . . . H6A H 0.1556 0.4210 0.4358 0.049 Uiso 1 1 calc R . . C7 C 0.2040(8) 0.6548(5) 0.3173(4) 0.0483(13) Uani 1 1 d . . . H7A H 0.1423 0.7185 0.2902 0.058 Uiso 1 1 calc R . . C8 C 0.3807(7) 0.6518(5) 0.3070(4) 0.0450(13) Uani 1 1 d . . . H8A H 0.4350 0.7129 0.2730 0.054 Uiso 1 1 calc R . . N5 N 0.7066(7) 0.1286(5) 0.8626(4) 0.0590(13) Uani 1 1 d U . . O3 O 0.7468(12) 0.1862(5) 0.7954(5) 0.128(3) Uani 1 1 d U . . O4 O 0.6364(14) 0.1858(6) 0.9232(5) 0.149(4) Uani 1 1 d . . . O5 O 0.7347(7) 0.0188(4) 0.8702(4) 0.0851(17) 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 0.03637(18) 0.0566(2) 0.03179(18) -0.00592(18) 0.00226(17) -0.00677(18) S1 0.0441(7) 0.0277(5) 0.0309(6) -0.0001(5) -0.0047(5) -0.0051(5) O1 0.065(3) 0.0374(19) 0.059(3) 0.0098(18) -0.007(2) -0.0179(19) O2 0.063(3) 0.046(2) 0.038(2) -0.0145(16) -0.0032(17) 0.0109(18) N1 0.049(3) 0.054(2) 0.0237(19) -0.0002(16) -0.0019(18) -0.002(2) N2 0.038(2) 0.039(2) 0.029(2) 0.0029(17) -0.0018(16) -0.0031(17) N3 0.036(2) 0.056(3) 0.050(3) 0.007(2) -0.004(2) -0.008(2) N4 0.034(2) 0.043(2) 0.036(2) 0.010(2) 0.005(2) -0.0054(16) C1 0.041(3) 0.040(2) 0.030(2) 0.000(2) 0.0039(19) -0.002(2) C2 0.031(2) 0.030(2) 0.029(2) -0.0005(18) -0.0028(17) 0.0006(17) C3 0.041(3) 0.049(3) 0.038(3) 0.002(2) -0.004(2) -0.006(2) C4 0.045(3) 0.054(3) 0.031(2) 0.002(2) -0.009(2) -0.007(2) C5 0.032(3) 0.034(2) 0.027(2) -0.0009(19) -0.0012(19) -0.005(2) C6 0.037(3) 0.042(3) 0.043(3) 0.005(2) 0.000(3) -0.010(3) C7 0.040(3) 0.055(3) 0.050(3) 0.012(2) -0.007(3) 0.008(3) C8 0.041(3) 0.047(3) 0.048(3) 0.016(2) -0.002(2) 0.002(2) N5 0.049(3) 0.047(3) 0.081(4) -0.005(3) -0.001(3) 0.001(2) O3 0.197(9) 0.073(4) 0.115(5) 0.016(3) 0.063(5) -0.005(5) O4 0.257(12) 0.085(4) 0.106(5) -0.011(4) 0.039(6) 0.062(6) O5 0.066(3) 0.046(2) 0.144(5) 0.001(3) 0.001(3) 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 N1 2.406(4) . ? Ag1 N2 2.433(4) 2_665 ? Ag1 N3 2.441(5) 2_565 ? Ag1 O3 2.555(6) . ? Ag1 N4 2.557(4) 2_665 ? S1 O1 1.425(4) . ? S1 O2 1.430(4) . ? S1 C2 1.778(5) . ? S1 C5 1.782(5) . ? N1 C4 1.314(7) . ? N1 C1 1.333(7) . ? N2 C3 1.329(6) . ? N2 C2 1.332(6) . ? N2 Ag1 2.433(4) 2_664 ? N3 C7 1.317(7) . ? N3 C6 1.331(7) . ? N3 Ag1 2.441(5) 2_564 ? N4 C8 1.328(7) . ? N4 C5 1.335(6) . ? N4 Ag1 2.557(4) 2_664 ? C1 C2 1.390(6) . ? C1 H1A 0.9300 . ? C3 C4 1.384(8) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 C6 1.383(7) . ? C6 H6A 0.9300 . ? C7 C8 1.371(8) . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? N5 O3 1.204(7) . ? N5 O4 1.209(8) . ? N5 O5 1.224(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 145.16(15) . 2_665 ? N1 Ag1 N3 100.18(16) . 2_565 ? N2 Ag1 N3 88.35(15) 2_665 2_565 ? N1 Ag1 O3 85.31(19) . . ? N2 Ag1 O3 124.9(2) 2_665 . ? N3 Ag1 O3 106.0(2) 2_565 . ? N1 Ag1 N4 85.52(15) . 2_665 ? N2 Ag1 N4 79.63(14) 2_665 2_665 ? N3 Ag1 N4 165.51(13) 2_565 2_665 ? O3 Ag1 N4 87.6(2) . 2_665 ? O1 S1 O2 120.9(2) . . ? O1 S1 C2 107.8(2) . . ? O2 S1 C2 107.5(2) . . ? O1 S1 C5 108.5(3) . . ? O2 S1 C5 107.0(2) . . ? C2 S1 C5 103.8(2) . . ? C4 N1 C1 116.8(4) . . ? C4 N1 Ag1 118.1(3) . . ? C1 N1 Ag1 125.0(3) . . ? C3 N2 C2 115.7(4) . . ? C3 N2 Ag1 116.6(3) . 2_664 ? C2 N2 Ag1 127.1(3) . 2_664 ? C7 N3 C6 116.9(5) . . ? C7 N3 Ag1 111.5(4) . 2_564 ? C6 N3 Ag1 130.6(3) . 2_564 ? C8 N4 C5 115.9(4) . . ? C8 N4 Ag1 117.3(3) . 2_664 ? C5 N4 Ag1 125.9(3) . 2_664 ? N1 C1 C2 120.2(5) . . ? N1 C1 H1A 119.9 . . ? C2 C1 H1A 119.9 . . ? N2 C2 C1 123.1(4) . . ? N2 C2 S1 115.7(3) . . ? C1 C2 S1 121.1(4) . . ? N2 C3 C4 121.2(5) . . ? N2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 . . ? N1 C4 C3 122.9(5) . . ? N1 C4 H4A 118.6 . . ? C3 C4 H4A 118.6 . . ? N4 C5 C6 122.6(5) . . ? N4 C5 S1 113.7(4) . . ? C6 C5 S1 123.7(4) . . ? N3 C6 C5 120.4(5) . . ? N3 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? N3 C7 C8 122.6(5) . . ? N3 C7 H7A 118.7 . . ? C8 C7 H7A 118.7 . . ? N4 C8 C7 121.5(5) . . ? N4 C8 H8A 119.2 . . ? C7 C8 H8A 119.2 . . ? O3 N5 O4 116.2(6) . . ? O3 N5 O5 122.6(6) . . ? O4 N5 O5 121.2(7) . . ? N5 O3 Ag1 103.8(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 N1 C4 31.9(5) 2_665 . . . ? N3 Ag1 N1 C4 133.8(4) 2_565 . . . ? O3 Ag1 N1 C4 -120.7(5) . . . . ? N4 Ag1 N1 C4 -32.7(4) 2_665 . . . ? N2 Ag1 N1 C1 -149.8(4) 2_665 . . . ? N3 Ag1 N1 C1 -47.8(4) 2_565 . . . ? O3 Ag1 N1 C1 57.6(5) . . . . ? N4 Ag1 N1 C1 145.6(4) 2_665 . . . ? C4 N1 C1 C2 0.9(7) . . . . ? Ag1 N1 C1 C2 -177.4(4) . . . . ? C3 N2 C2 C1 0.2(7) . . . . ? Ag1 N2 C2 C1 -170.7(4) 2_664 . . . ? C3 N2 C2 S1 -177.4(4) . . . . ? Ag1 N2 C2 S1 11.7(5) 2_664 . . . ? N1 C1 C2 N2 -1.7(8) . . . . ? N1 C1 C2 S1 175.8(4) . . . . ? O1 S1 C2 N2 173.4(4) . . . . ? O2 S1 C2 N2 41.5(4) . . . . ? C5 S1 C2 N2 -71.7(4) . . . . ? O1 S1 C2 C1 -4.3(5) . . . . ? O2 S1 C2 C1 -136.2(4) . . . . ? C5 S1 C2 C1 110.6(4) . . . . ? C2 N2 C3 C4 1.9(7) . . . . ? Ag1 N2 C3 C4 173.8(4) 2_664 . . . ? C1 N1 C4 C3 1.2(8) . . . . ? Ag1 N1 C4 C3 179.7(4) . . . . ? N2 C3 C4 N1 -2.7(8) . . . . ? C8 N4 C5 C6 -0.2(7) . . . . ? Ag1 N4 C5 C6 169.0(4) 2_664 . . . ? C8 N4 C5 S1 177.0(4) . . . . ? Ag1 N4 C5 S1 -13.8(5) 2_664 . . . ? O1 S1 C5 N4 -174.6(3) . . . . ? O2 S1 C5 N4 -42.6(4) . . . . ? C2 S1 C5 N4 70.9(4) . . . . ? O1 S1 C5 C6 2.5(5) . . . . ? O2 S1 C5 C6 134.5(5) . . . . ? C2 S1 C5 C6 -111.9(5) . . . . ? C7 N3 C6 C5 -0.2(8) . . . . ? Ag1 N3 C6 C5 167.8(4) 2_564 . . . ? N4 C5 C6 N3 0.1(8) . . . . ? S1 C5 C6 N3 -176.8(4) . . . . ? C6 N3 C7 C8 0.4(9) . . . . ? Ag1 N3 C7 C8 -169.9(5) 2_564 . . . ? C5 N4 C8 C7 0.3(8) . . . . ? Ag1 N4 C8 C7 -169.8(5) 2_664 . . . ? N3 C7 C8 N4 -0.4(10) . . . . ? O4 N5 O3 Ag1 9.1(9) . . . . ? O5 N5 O3 Ag1 -170.6(5) . . . . ? N1 Ag1 O3 N5 -165.3(6) . . . . ? N2 Ag1 O3 N5 33.4(7) 2_665 . . . ? N3 Ag1 O3 N5 -66.0(6) 2_565 . . . ? N4 Ag1 O3 N5 109.0(6) 2_665 . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.128 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.095 # Attachment 'cqw6rev.CIF.CIF' data_Ligand _database_code_depnum_ccdc_archive 'CCDC 779356' #TrackingRef 'cqw6rev.CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H6 N4 O2 S' _chemical_formula_weight 222.23 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 5.7845(10) _cell_length_b 7.2446(13) _cell_length_c 22.243(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.951(4) _cell_angle_gamma 90.00 _cell_volume 930.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 0.331 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.830658 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details sadabs _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6253 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.33 _reflns_number_total 2325 _reflns_number_gt 1773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+0.1280P] 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 2325 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1100 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 S1 S 0.25240(8) 0.26182(6) 0.11799(2) 0.04370(17) Uani 1 1 d . . . O1 O 0.4669(3) 0.1679(2) 0.11093(6) 0.0601(4) Uani 1 1 d . . . O2 O 0.0397(3) 0.1827(2) 0.09505(6) 0.0598(4) Uani 1 1 d . . . N1 N 0.5119(3) 0.7194(2) 0.04588(8) 0.0538(4) Uani 1 1 d . . . N2 N 0.0826(3) 0.5752(2) 0.07411(7) 0.0458(4) Uani 1 1 d . . . N3 N -0.0049(3) 0.3366(3) 0.28030(8) 0.0633(5) Uani 1 1 d . . . N4 N 0.4225(3) 0.3301(3) 0.22777(7) 0.0513(4) Uani 1 1 d . . . C1 C 0.4936(3) 0.5550(3) 0.07357(9) 0.0467(5) Uani 1 1 d . . . H1A H 0.6263 0.4878 0.0843 0.056 Uiso 1 1 calc R . . C2 C 0.2800(3) 0.4861(2) 0.08601(7) 0.0377(4) Uani 1 1 d . . . C3 C 0.1029(3) 0.7367(3) 0.04657(9) 0.0488(5) Uani 1 1 d . . . H3A H -0.0297 0.8051 0.0368 0.059 Uiso 1 1 calc R . . C4 C 0.3148(4) 0.8057(3) 0.03217(9) 0.0501(5) Uani 1 1 d . . . H4A H 0.3194 0.9178 0.0119 0.060 Uiso 1 1 calc R . . C5 C 0.2233(3) 0.3053(2) 0.19612(8) 0.0392(4) Uani 1 1 d . . . C6 C 0.0115(4) 0.3082(3) 0.22110(9) 0.0500(5) Uani 1 1 d . . . H6A H -0.1221 0.2904 0.1967 0.060 Uiso 1 1 calc R . . C7 C 0.1932(4) 0.3614(3) 0.31201(9) 0.0566(5) Uani 1 1 d . . . H7A H 0.1890 0.3831 0.3532 0.068 Uiso 1 1 calc R . . C8 C 0.4041(4) 0.3564(3) 0.28646(9) 0.0560(5) Uani 1 1 d . . . H8A H 0.5380 0.3719 0.3109 0.067 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 S1 0.0514(3) 0.0434(3) 0.0363(2) -0.00087(18) 0.00099(19) -0.0006(2) O1 0.0745(11) 0.0570(8) 0.0495(8) 0.0007(7) 0.0108(7) 0.0226(8) O2 0.0718(10) 0.0580(9) 0.0486(8) -0.0004(7) -0.0074(7) -0.0214(8) N1 0.0432(9) 0.0559(10) 0.0628(11) 0.0019(8) 0.0076(8) -0.0082(8) N2 0.0353(8) 0.0526(9) 0.0497(9) 0.0047(7) 0.0047(7) 0.0005(7) N3 0.0496(11) 0.0885(14) 0.0526(10) -0.0021(10) 0.0114(8) 0.0031(10) N4 0.0415(9) 0.0696(11) 0.0427(9) -0.0062(8) 0.0016(7) -0.0041(8) C1 0.0361(10) 0.0546(11) 0.0493(10) -0.0043(9) 0.0019(8) 0.0010(9) C2 0.0388(9) 0.0435(9) 0.0307(8) -0.0030(7) 0.0017(6) -0.0007(7) C3 0.0433(11) 0.0505(11) 0.0527(11) 0.0049(9) 0.0020(8) 0.0041(9) C4 0.0535(12) 0.0459(10) 0.0513(11) 0.0033(9) 0.0056(9) -0.0035(9) C5 0.0407(10) 0.0407(8) 0.0361(9) 0.0021(7) 0.0018(7) -0.0010(8) C6 0.0402(10) 0.0624(12) 0.0471(10) 0.0000(9) 0.0007(8) -0.0004(9) C7 0.0595(13) 0.0712(14) 0.0396(10) -0.0060(9) 0.0066(9) 0.0043(11) C8 0.0519(12) 0.0738(14) 0.0417(10) -0.0097(10) -0.0028(9) -0.0043(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 S1 O2 1.4279(15) . ? S1 O1 1.4312(15) . ? S1 C5 1.7824(18) . ? S1 C2 1.7843(18) . ? N1 C4 1.322(3) . ? N1 C1 1.347(3) . ? N2 C2 1.327(2) . ? N2 C3 1.329(2) . ? N3 C7 1.327(3) . ? N3 C6 1.341(3) . ? N4 C8 1.329(2) . ? N4 C5 1.331(2) . ? C1 C2 1.374(3) . ? C1 H1A 0.9300 . ? C3 C4 1.376(3) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 C6 1.371(3) . ? C6 H6A 0.9300 . ? C7 C8 1.373(3) . ? C7 H7A 0.9300 . ? C8 H8A 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 O2 S1 O1 120.40(10) . . ? O2 S1 C5 107.24(9) . . ? O1 S1 C5 108.47(8) . . ? O2 S1 C2 108.44(8) . . ? O1 S1 C2 107.07(9) . . ? C5 S1 C2 104.05(8) . . ? C4 N1 C1 115.87(17) . . ? C2 N2 C3 115.11(16) . . ? C7 N3 C6 116.09(18) . . ? C8 N4 C5 115.36(17) . . ? N1 C1 C2 120.39(18) . . ? N1 C1 H1A 119.8 . . ? C2 C1 H1A 119.8 . . ? N2 C2 C1 123.85(17) . . ? N2 C2 S1 115.38(13) . . ? C1 C2 S1 120.74(14) . . ? N2 C3 C4 121.89(18) . . ? N2 C3 H3A 119.1 . . ? C4 C3 H3A 119.1 . . ? N1 C4 C3 122.83(19) . . ? N1 C4 H4A 118.6 . . ? C3 C4 H4A 118.6 . . ? N4 C5 C6 123.40(17) . . ? N4 C5 S1 114.64(14) . . ? C6 C5 S1 121.94(14) . . ? N3 C6 C5 120.69(18) . . ? N3 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? N3 C7 C8 122.57(19) . . ? N3 C7 H7A 118.7 . . ? C8 C7 H7A 118.7 . . ? N4 C8 C7 121.88(18) . . ? N4 C8 H8A 119.1 . . ? C7 C8 H8A 119.1 . . ? 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 C4 N1 C1 C2 0.0(3) . . . . ? C3 N2 C2 C1 2.5(3) . . . . ? C3 N2 C2 S1 -175.63(13) . . . . ? N1 C1 C2 N2 -2.3(3) . . . . ? N1 C1 C2 S1 175.71(14) . . . . ? O2 S1 C2 N2 31.72(16) . . . . ? O1 S1 C2 N2 163.05(13) . . . . ? C5 S1 C2 N2 -82.21(14) . . . . ? O2 S1 C2 C1 -146.47(15) . . . . ? O1 S1 C2 C1 -15.13(17) . . . . ? C5 S1 C2 C1 99.61(16) . . . . ? C2 N2 C3 C4 -0.5(3) . . . . ? C1 N1 C4 C3 1.9(3) . . . . ? N2 C3 C4 N1 -1.7(3) . . . . ? C8 N4 C5 C6 0.8(3) . . . . ? C8 N4 C5 S1 -177.83(16) . . . . ? O2 S1 C5 N4 162.14(14) . . . . ? O1 S1 C5 N4 30.66(17) . . . . ? C2 S1 C5 N4 -83.08(15) . . . . ? O2 S1 C5 C6 -16.5(2) . . . . ? O1 S1 C5 C6 -147.95(17) . . . . ? C2 S1 C5 C6 98.31(18) . . . . ? C7 N3 C6 C5 0.2(3) . . . . ? N4 C5 C6 N3 -0.2(3) . . . . ? S1 C5 C6 N3 178.29(17) . . . . ? C6 N3 C7 C8 -0.8(3) . . . . ? C5 N4 C8 C7 -1.3(3) . . . . ? N3 C7 C8 N4 1.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.327 _refine_diff_density_min -0.200 _refine_diff_density_rms 0.054