# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2262 data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Chen, Xiao-Ming School of Chemistry and Chemical Engineering Zhongshan University Guangzhou, 510275 P. R. China ; _publ_contact_author_phone '86-20-84113986' _publ_contact_author_fax '86 20 84112245' _publ_contact_author_email cescxm@zsu.edu.cn _publ_requested_joiurnal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir, Please consider this CIF submission as supplementary data for a paper submitted to J. Chem. Soc., Dalton Trans. Xiao-Ming Chen ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Syntheses and crystal structures of five two-dimensional networks constructed from staircase-like silver(I) thiocyanate chains and bridging polyamines ; loop_ _publ_author_name _publ_author_address 'Ren, Chun-Xia' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Zhu, Hai-Liang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Yang,Guang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Chen, Xiao-Ming' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; #============================================================ data_complex_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H8 Ag2 N4 S2' _chemical_formula_weight 392.00 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' '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 6.025(4) _cell_length_b 6.232(3) _cell_length_c 7.292(5) _cell_angle_alpha 65.91(4) _cell_angle_beta 77.87(5) _cell_angle_gamma 84.49(5) _cell_volume 244.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 186 _exptl_absorpt_coefficient_mu 4.384 _exptl_absorpt_correction_type semi-emprical _exptl_absorpt_correction_T_min 0.549 _exptl_absorpt_correction_T_max 0.728 _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 'R3m' _diffrn_measurement_method '\w-scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 1442 _diffrn_reflns_av_R_equivalents 0.0135 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 30.00 _reflns_number_total 1434 _reflns_number_gt 1151 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL Version 5 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.119(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1434 _refine_ls_number_parameters 56 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.1103 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.06041(6) 0.18807(8) 0.10334(6) 0.0520(2) Uani 1 d . . . S1 S -0.13171(19) 0.3079(2) -0.23986(16) 0.0350(3) Uani 1 d . . . N1 N -0.5886(7) 0.2810(7) -0.0406(7) 0.0385(8) Uani 1 d . . . N2 N -0.2479(7) 0.1965(6) 0.3350(5) 0.0347(7) Uani 1 d . . . H2C H -0.3335 0.3267 0.2731 0.080 Uiso 1 d R . . H2D H -0.2092 0.2237 0.4391 0.080 Uiso 1 d R . . C1 C -0.3996(7) 0.2898(7) -0.1220(6) 0.0292(7) Uani 1 d . . . C2 C -0.3861(7) -0.0170(7) 0.4373(6) 0.0312(8) Uani 1 d . . . H2B H -0.4147 -0.0670 0.3362 0.080 Uiso 1 d R . . H2A H -0.3018 -0.1399 0.5259 0.080 Uiso 1 d 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 0.0237(2) 0.0658(4) 0.0522(3) -0.0146(2) 0.00518(16) -0.00332(17) S1 0.0238(5) 0.0389(6) 0.0365(5) -0.0115(4) 0.0017(4) -0.0050(4) N1 0.0228(17) 0.0363(19) 0.055(2) -0.0188(16) -0.0010(15) -0.0048(14) N2 0.0302(19) 0.0323(17) 0.0367(16) -0.0118(14) 0.0021(14) -0.0049(14) C1 0.0264(19) 0.0285(18) 0.0325(16) -0.0113(14) -0.0059(14) -0.0019(14) C2 0.0232(18) 0.034(2) 0.0336(17) -0.0130(15) 0.0024(15) -0.0045(15) _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 2.172(4) 1_655 ? Ag1 N2 2.245(4) . ? Ag1 S1 2.772(2) . ? Ag1 S1 2.8533(19) 2 ? S1 C1 1.652(4) . ? S1 Ag1 2.8533(19) 2 ? N1 C1 1.163(6) . ? N1 Ag1 2.172(4) 1_455 ? N2 C2 1.470(5) . ? C2 C2 1.529(8) 2_456 ? 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 150.09(15) 1_655 . ? N1 Ag1 S1 100.24(13) 1_655 . ? N2 Ag1 S1 100.64(12) . . ? N1 Ag1 S1 95.76(11) 1_655 2 ? N2 Ag1 S1 99.63(10) . 2 ? S1 Ag1 S1 104.12(3) . 2 ? C1 S1 Ag1 96.85(15) . . ? C1 S1 Ag1 94.93(14) . 2 ? Ag1 S1 Ag1 75.88(3) . 2 ? C1 N1 Ag1 166.7(3) . 1_455 ? C2 N2 Ag1 116.7(2) . . ? N1 C1 S1 178.9(4) . . ? N2 C2 C2 113.5(4) . 2_456 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.011 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.194 #===========================================END data_complex_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H10 Ag2 N4 S2' _chemical_formula_weight 406.03 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 5.8590(10) _cell_length_b 6.440(2) _cell_length_c 14.316(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.520(10) _cell_angle_gamma 90.00 _cell_volume 538.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 3.984 _exptl_absorpt_correction_type semi-emprical _exptl_absorpt_correction_T_min 0.472 _exptl_absorpt_correction_T_max 0.586 _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 'Siemens R3m' _diffrn_measurement_method '\w-scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 1704 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 30.00 _reflns_number_total 1566 _reflns_number_gt 1244 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL Version 5 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0971P)^2^+0.4286P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.378(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1566 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1463 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.41009(8) 0.20721(9) 0.03839(3) 0.0646(3) Uani 1 d . . . S1 S 0.3562(2) -0.1626(2) 0.12239(8) 0.0479(3) Uani 1 d . . . C1 C 0.1044(8) -0.2139(7) 0.0705(3) 0.0439(9) Uani 1 d . . . N1 N -0.0720(8) -0.2521(9) 0.0336(3) 0.0550(11) Uani 1 d . . . N2 N 0.6719(7) 0.3711(7) 0.1311(3) 0.0501(9) Uani 1 d . . . H2C H 0.5986 0.4588 0.1674 0.080 Uiso 1 d R . . H2D H 0.7561 0.4492 0.0945 0.080 Uiso 1 d R . . C2 C 0.8288(10) 0.2475(8) 0.1917(3) 0.0479(10) Uani 1 d . . . H2A H 0.7216 0.1682 0.2357 0.080 Uiso 1 d R . . H2B H 0.8704 0.1167 0.1613 0.080 Uiso 1 d R . . C3 C 1.0000 0.3720(12) 0.2500 0.0508(14) Uani 1 d S . . H3 H 1.0840 0.4828 0.2149 0.080 Uiso 1 d 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 0.0427(3) 0.0826(5) 0.0664(4) 0.0076(2) -0.0094(2) -0.00900(18) S1 0.0372(6) 0.0552(7) 0.0504(6) 0.0046(5) -0.0020(4) 0.0000(4) C1 0.036(2) 0.046(2) 0.051(2) 0.0054(18) 0.0082(18) 0.0031(16) N1 0.040(2) 0.058(2) 0.066(3) 0.0119(18) 0.000(2) 0.0004(17) N2 0.046(2) 0.051(2) 0.051(2) 0.0042(17) -0.0068(17) 0.0006(18) C2 0.048(3) 0.049(2) 0.045(2) 0.0013(17) -0.0043(19) 0.0011(19) C3 0.050(4) 0.046(3) 0.054(3) 0.000 -0.011(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.179(5) 3 ? Ag1 N2 2.215(4) . ? Ag1 S1 2.6979(15) . ? Ag1 S1 2.7843(15) 3_655 ? Ag1 Ag1 3.1021(14) 3_655 ? S1 C1 1.632(5) . ? S1 Ag1 2.7843(15) 3_655 ? C1 N1 1.150(7) . ? N1 Ag1 2.179(5) 3 ? N2 C2 1.452(6) . ? C2 C3 1.488(6) . ? C3 C2 1.488(6) 2_755 ? 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 141.35(19) 3 . ? N1 Ag1 S1 101.18(14) 3 . ? N2 Ag1 S1 104.68(11) . . ? N1 Ag1 S1 96.36(13) 3 3_655 ? N2 Ag1 S1 100.47(12) . 3_655 ? S1 Ag1 S1 111.10(4) . 3_655 ? N1 Ag1 Ag1 105.55(15) 3 3_655 ? N2 Ag1 Ag1 112.55(12) . 3_655 ? S1 Ag1 Ag1 56.87(4) . 3_655 ? S1 Ag1 Ag1 54.23(3) 3_655 3_655 ? C1 S1 Ag1 96.26(16) . . ? C1 S1 Ag1 95.08(17) . 3_655 ? Ag1 S1 Ag1 68.90(4) . 3_655 ? N1 C1 S1 179.2(5) . . ? C1 N1 Ag1 160.0(5) . 3 ? C2 N2 Ag1 118.3(3) . . ? N2 C2 C3 114.0(4) . . ? C2 C3 C2 114.8(6) . 2_755 ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 1.025 _refine_diff_density_min -1.242 _refine_diff_density_rms 0.177 #===========================================END data_complex_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H12 Ag2 N4 S2' _chemical_formula_weight 420.06 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' '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 5.994(3) _cell_length_b 7.145(5) _cell_length_c 7.622(5) _cell_angle_alpha 73.63(5) _cell_angle_beta 69.97(4) _cell_angle_gamma 82.16(5) _cell_volume 294.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 202 _exptl_absorpt_coefficient_mu 3.653 _exptl_absorpt_correction_type semi-emprical _exptl_absorpt_correction_T_min 0.394 _exptl_absorpt_correction_T_max 0.540 _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 'R3m' _diffrn_measurement_method '\w-scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 1432 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.99 _reflns_number_total 1423 _reflns_number_gt 1093 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL Version 5 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.1107P)^2^+0.2924P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1423 _refine_ls_number_parameters 64 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1600 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.03102(10) 0.16674(12) 0.09897(9) 0.0554(3) Uani 1 d . . . S1 S -0.0944(3) 0.2238(3) -0.2233(3) 0.0361(4) Uani 1 d . . . N1 N -0.5906(11) 0.2564(10) -0.0640(10) 0.0417(14) Uani 1 d . . . N2 N -0.2309(12) 0.3140(9) 0.3194(9) 0.0389(13) Uani 1 d . . . C1 C -0.3884(12) 0.2421(9) -0.1258(9) 0.0281(12) Uani 1 d . . . C2 C -0.4873(14) 0.2803(11) 0.3731(11) 0.0381(15) Uani 1 d . . . H2A H -0.5448 0.3532 0.2693 0.080 Uiso 1 d R . . H2B H -0.5741 0.3272 0.4852 0.080 Uiso 1 d R . . C3 C -0.5294(12) 0.0659(10) 0.4128(9) 0.0315(13) Uani 1 d . . . H3A H -0.4396 0.0208 0.3002 0.080 Uiso 1 d R . . H3B H -0.6945 0.0544 0.4328 0.080 Uiso 1 d R . . H2C H -0.2103 0.4271 0.2774 0.050 Uiso 1 d R . . H2D H -0.1652 0.2769 0.4244 0.050 Uiso 1 d 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 0.0304(4) 0.0742(6) 0.0553(5) -0.0207(4) -0.0033(3) -0.0003(3) S1 0.0252(8) 0.0415(10) 0.0364(8) -0.0060(7) -0.0054(6) -0.0048(7) N1 0.030(3) 0.043(4) 0.049(4) -0.006(3) -0.012(3) -0.005(3) N2 0.044(3) 0.030(3) 0.037(3) -0.006(2) -0.004(3) -0.010(3) C1 0.031(3) 0.021(3) 0.031(3) -0.002(2) -0.013(2) -0.002(2) C2 0.040(4) 0.030(4) 0.040(4) -0.009(3) -0.008(3) 0.002(3) C3 0.032(3) 0.031(3) 0.029(3) -0.005(3) -0.008(3) -0.004(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 2.262(7) 1_655 ? Ag1 N2 2.266(7) . ? Ag1 S1 2.701(3) 2 ? Ag1 S1 2.717(2) . ? Ag1 Ag1 3.278(2) 2 ? S1 C1 1.664(7) . ? S1 Ag1 2.701(3) 2 ? N1 C1 1.141(9) . ? N1 Ag1 2.262(7) 1_455 ? N2 C2 1.483(10) . ? C2 C3 1.515(10) . ? C3 C3 1.517(12) 2_456 ? 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 124.2(2) 1_655 . ? N1 Ag1 S1 101.43(18) 1_655 2 ? N2 Ag1 S1 115.34(17) . 2 ? N1 Ag1 S1 94.73(17) 1_655 . ? N2 Ag1 S1 112.54(18) . . ? S1 Ag1 S1 105.54(5) 2 . ? N1 Ag1 Ag1 103.40(18) 1_655 2 ? N2 Ag1 Ag1 132.09(16) . 2 ? S1 Ag1 Ag1 52.99(6) 2 2 ? S1 Ag1 Ag1 52.55(5) . 2 ? C1 S1 Ag1 98.7(2) . 2 ? C1 S1 Ag1 99.3(2) . . ? Ag1 S1 Ag1 74.46(5) 2 . ? C1 N1 Ag1 159.1(6) . 1_455 ? C2 N2 Ag1 118.1(5) . . ? N1 C1 S1 178.1(6) . . ? N2 C2 C3 111.3(6) . . ? C2 C3 C3 115.3(7) . 2_456 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.048 _refine_diff_density_min -1.755 _refine_diff_density_rms 0.230 #===========================================END data_complex_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H14 Ag2 N4 S2' _chemical_formula_weight 434.08 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' '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 5.9910(10) _cell_length_b 6.875(2) _cell_length_c 16.187(4) _cell_angle_alpha 85.56(5) _cell_angle_beta 82.65(4) _cell_angle_gamma 80.71(4) _cell_volume 651.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 420 _exptl_absorpt_coefficient_mu 3.301 _exptl_absorpt_correction_type semi-emprical _exptl_absorpt_correction_T_min 0.403 _exptl_absorpt_correction_T_max 0.631 _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 'R3m' _diffrn_measurement_method '\w-scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 3494 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 29.00 _reflns_number_total 3475 _reflns_number_gt 2342 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL Version 5 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+0.6032P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.049(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3475 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1105 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.36438(8) 0.21832(8) 0.97525(3) 0.0581(2) Uani 1 d . . . Ag2 Ag 1.55734(8) 0.69889(9) 0.54593(3) 0.0666(2) Uani 1 d . . . S1 S 0.3851(2) -0.1090(2) 0.88435(8) 0.0436(3) Uani 1 d . . . C1 C 0.1440(9) -0.1783(8) 0.9286(3) 0.0386(11) Uiso 1 d . . . N1 N -0.0213(9) -0.2316(7) 0.9597(3) 0.0506(11) Uiso 1 d . . . S2 S 2.3505(2) 0.6913(2) 0.40944(9) 0.0460(3) Uani 1 d . . . C2 C 2.0829(9) 0.7300(8) 0.4498(3) 0.0413(11) Uani 1 d . . . N2 N 1.8937(8) 0.7566(8) 0.4787(3) 0.0561(13) Uani 1 d . . . N3 N 0.6294(8) 0.3718(7) 0.8986(3) 0.0449(10) Uani 1 d . . . H3A H 0.7333 0.3900 0.9316 0.080 Uiso 1 d R . . H3D H 0.5628 0.4918 0.8807 0.080 Uiso 1 d R . . N4 N 1.3419(8) 0.8895(7) 0.6427(3) 0.0502(11) Uani 1 d . . . H4A H 1.3183 1.0139 0.6202 0.080 Uiso 1 d R . . H4D H 1.4240 0.8903 0.6855 0.080 Uiso 1 d R . . C3 C 0.7495(11) 0.2681(9) 0.8259(4) 0.0536(15) Uani 1 d . . . H3B H 0.6470 0.2761 0.7843 0.080 Uiso 1 d R . . H3C H 0.7905 0.1313 0.8426 0.080 Uiso 1 d R . . C4 C 0.9619(10) 0.3487(9) 0.7869(4) 0.0542(15) Uani 1 d . . . H4B H 1.0355 0.2672 0.7428 0.080 Uiso 1 d R . . H4C H 1.0643 0.3387 0.8286 0.080 Uiso 1 d R . . C5 C 0.9250(9) 0.5598(8) 0.7530(3) 0.0406(11) Uani 1 d . . . H5A H 0.8633 0.6448 0.7974 0.080 Uiso 1 d R . . H5B H 0.8167 0.5739 0.7132 0.080 Uiso 1 d R . . C6 C 1.1460(9) 0.6223(8) 0.7102(3) 0.0424(12) Uani 1 d . . . H6A H 1.2036 0.5399 0.6646 0.080 Uiso 1 d R . . H6B H 1.2560 0.6009 0.7495 0.080 Uiso 1 d R . . C7 C 1.1200(9) 0.8354(8) 0.6781(4) 0.0468(13) Uani 1 d . . . H7A H 1.0195 0.8558 0.6355 0.080 Uiso 1 d R . . H7B H 1.0539 0.9185 0.7226 0.080 Uiso 1 d 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 0.0458(3) 0.0721(4) 0.0584(3) -0.0104(2) 0.0103(2) -0.0246(2) Ag2 0.0368(3) 0.0934(5) 0.0657(3) -0.0041(3) 0.0081(2) -0.0091(2) S1 0.0363(7) 0.0502(8) 0.0440(7) -0.0061(6) 0.0032(5) -0.0100(6) S2 0.0306(6) 0.0575(9) 0.0481(7) 0.0027(6) 0.0015(5) -0.0096(6) C2 0.038(3) 0.037(3) 0.049(3) 0.006(2) -0.008(2) -0.010(2) N2 0.034(3) 0.058(3) 0.073(3) 0.008(3) 0.002(2) -0.011(2) N3 0.045(3) 0.041(3) 0.046(2) 0.0014(19) 0.005(2) -0.011(2) N4 0.048(3) 0.041(3) 0.061(3) 0.005(2) 0.001(2) -0.014(2) C3 0.061(4) 0.043(3) 0.052(3) -0.005(2) 0.019(3) -0.013(3) C4 0.047(3) 0.041(3) 0.066(4) 0.004(3) 0.017(3) -0.005(2) C5 0.035(3) 0.040(3) 0.046(3) -0.005(2) 0.003(2) -0.007(2) C6 0.039(3) 0.037(3) 0.050(3) -0.002(2) 0.004(2) -0.007(2) C7 0.042(3) 0.045(3) 0.052(3) 0.000(2) 0.003(2) -0.011(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 2.178(5) 2_557 ? Ag1 N3 2.238(4) . ? Ag1 S1 2.7604(16) . ? Ag1 S1 2.8681(16) 2_657 ? Ag1 Ag1 3.2680(14) 2_657 ? Ag2 N2 2.244(5) . ? Ag2 N4 2.257(5) . ? Ag2 S2 2.6756(16) 1_455 ? Ag2 S2 2.7103(18) 2_966 ? S1 C1 1.653(5) . ? S1 Ag1 2.8681(16) 2_657 ? C1 N1 1.153(7) . ? N1 Ag1 2.178(5) 2_557 ? S2 C2 1.640(6) . ? S2 Ag2 2.6756(16) 1_655 ? S2 Ag2 2.7103(18) 2_966 ? C2 N2 1.161(7) . ? N3 C3 1.469(7) . ? N4 C7 1.471(7) . ? C3 C4 1.514(8) . ? C4 C5 1.504(8) . ? C5 C6 1.524(7) . ? C6 C7 1.507(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 N1 Ag1 N3 149.13(18) 2_557 . ? N1 Ag1 S1 100.08(14) 2_557 . ? N3 Ag1 S1 100.53(12) . . ? N1 Ag1 S1 98.55(13) 2_557 2_657 ? N3 Ag1 S1 96.15(13) . 2_657 ? S1 Ag1 S1 109.04(4) . 2_657 ? N1 Ag1 Ag1 106.16(13) 2_557 2_657 ? N3 Ag1 Ag1 104.38(12) . 2_657 ? S1 Ag1 Ag1 56.06(4) . 2_657 ? S1 Ag1 Ag1 52.98(3) 2_657 2_657 ? N2 Ag2 N4 125.25(19) . . ? N2 Ag2 S2 96.41(14) . 1_455 ? N4 Ag2 S2 112.35(14) . 1_455 ? N2 Ag2 S2 101.55(14) . 2_966 ? N4 Ag2 S2 116.00(12) . 2_966 ? S2 Ag2 S2 101.31(4) 1_455 2_966 ? C1 S1 Ag1 97.13(19) . . ? C1 S1 Ag1 96.41(18) . 2_657 ? Ag1 S1 Ag1 70.96(4) . 2_657 ? N1 C1 S1 178.2(5) . . ? C1 N1 Ag1 159.2(5) . 2_557 ? C2 S2 Ag2 100.4(2) . 1_655 ? C2 S2 Ag2 98.18(19) . 2_966 ? Ag2 S2 Ag2 78.69(4) 1_655 2_966 ? N2 C2 S2 179.6(5) . . ? C2 N2 Ag2 160.6(5) . . ? C3 N3 Ag1 115.4(3) . . ? C7 N4 Ag2 118.3(4) . . ? N3 C3 C4 114.3(5) . . ? C5 C4 C3 115.5(5) . . ? C4 C5 C6 111.4(4) . . ? C7 C6 C5 113.5(4) . . ? N4 C7 C6 110.7(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.750 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.133 #===========================================END data_complex_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H22 Ag3 N7 S3' _chemical_formula_weight 672.15 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' '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 8.8570(10) _cell_length_b 9.860(4) _cell_length_c 12.630(5) _cell_angle_alpha 70.21(6) _cell_angle_beta 76.11(5) _cell_angle_gamma 82.01(5) _cell_volume 1005.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 3.213 _exptl_absorpt_correction_type semi-emprical _exptl_absorpt_correction_T_min 0.409 _exptl_absorpt_correction_T_max 0.802 _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 'R3m' _diffrn_measurement_method '/w-scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 4864 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 28.00 _reflns_number_total 4850 _reflns_number_gt 3381 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL Version 5 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0854P)^2^+1.8662P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0009(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4850 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1596 _refine_ls_wR_factor_gt 0.1439 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.08458(6) 0.88505(6) 0.95627(6) 0.0533(2) Uani 1 d . . . Ag2 Ag 0.21312(8) 1.14832(7) 0.45349(6) 0.0623(2) Uani 1 d . . . Ag3 Ag 0.29089(9) 1.37800(8) 0.56613(6) 0.0695(2) Uani 1 d . . . S1 S 0.4617(2) 1.29815(18) 0.37940(15) 0.0459(4) Uani 1 d . . . S2 S 0.0375(2) 1.21471(19) 0.64059(15) 0.0460(4) Uani 1 d . . . S3 S -0.17467(19) 0.95179(18) 0.91275(15) 0.0423(4) Uani 1 d . . . N1 N 0.0447(8) 0.1647(6) 1.3372(5) 0.0521(15) Uani 1 d . . . H1C H 0.1416 0.1510 1.3511 0.080 Uiso 1 d R . . H1D H -0.0191 0.0914 1.3665 0.080 Uiso 1 d R . . N2 N 0.1570(6) 0.6786(6) 1.1055(5) 0.0388(12) Uani 1 d . . . H2C H 0.1105 0.7631 1.1129 0.080 Uiso 1 d R . . N3 N 0.3266(6) 0.8171(6) 0.8632(4) 0.0362(11) Uani 1 d . . . H3C H 0.2371 0.8389 0.8374 0.080 Uiso 1 d R . . N4 N 0.4540(7) 1.3281(6) 0.6887(5) 0.0488(14) Uani 1 d . . . H4C H 0.3524 1.3463 0.6855 0.080 Uiso 1 d R . . H4D H 0.5164 1.4016 0.6666 0.080 Uiso 1 d R . . N5 N 0.6844(7) 1.0817(6) 0.4653(6) 0.0545(15) Uani 1 d . . . N6 N -0.1818(7) 1.4146(6) 0.5346(6) 0.0549(16) Uani 1 d . . . N7 N -0.2998(8) 0.6867(8) 1.0547(7) 0.0623(17) Uani 1 d . . . C1 C -0.0098(8) 0.3069(8) 1.2667(7) 0.0491(17) Uani 1 d . . . H1A H -0.1006 0.3420 1.3114 0.080 Uiso 1 d R . . H1B H -0.0390 0.2968 1.2014 0.080 Uiso 1 d R . . C2 C 0.1136(8) 0.4167(7) 1.2245(6) 0.0446(15) Uani 1 d . . . H2A H 0.2109 0.3745 1.1930 0.080 Uiso 1 d R . . H2B H 0.1277 0.4424 1.2881 0.080 Uiso 1 d R . . C3 C 0.0669(8) 0.5525(7) 1.1333(6) 0.0450(15) Uani 1 d . . . H3A H 0.0762 0.5291 1.0641 0.080 Uiso 1 d R . . H3B H -0.0411 0.5783 1.1586 0.080 Uiso 1 d R . . C4 C 0.3247(8) 0.6609(7) 1.0654(6) 0.0460(16) Uani 1 d . . . H4A H 0.3620 0.5684 1.1106 0.080 Uiso 1 d R . . H4B H 0.3746 0.7337 1.0769 0.080 Uiso 1 d R . . C5 C 0.3703(8) 0.6724(7) 0.9385(7) 0.0480(17) Uani 1 d . . . H5A H 0.4807 0.6530 0.9177 0.080 Uiso 1 d R . . H5B H 0.3194 0.6004 0.9266 0.080 Uiso 1 d R . . C6 C 0.4462(7) 0.9216(7) 0.8351(6) 0.0376(13) Uani 1 d . . . H6A H 0.5414 0.8892 0.7930 0.080 Uiso 1 d R . . H6B H 0.4663 0.9270 0.9050 0.080 Uiso 1 d R . . C7 C 0.3932(7) 1.0709(7) 0.7634(5) 0.0384(13) Uani 1 d . . . H7A H 0.3001 1.1047 0.8068 0.080 Uiso 1 d R . . H7B H 0.3692 1.0646 0.6951 0.080 Uiso 1 d R . . C8 C 0.5169(8) 1.1780(7) 0.7302(6) 0.0416(14) Uani 1 d . . . H8A H 0.5609 1.1653 0.7957 0.080 Uiso 1 d R . . H8B H 0.5988 1.1590 0.6707 0.080 Uiso 1 d R . . C9 C 0.5917(7) 1.1690(7) 0.4324(6) 0.0379(13) Uani 1 d . . . C10 C -0.0914(7) 1.3337(7) 0.5769(6) 0.0407(14) Uani 1 d . . . C11 C -0.2474(7) 0.7945(8) 0.9985(6) 0.0408(14) Uani 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 0.0309(3) 0.0414(3) 0.0724(4) 0.0006(3) -0.0130(2) 0.0031(2) Ag2 0.0574(4) 0.0530(4) 0.0695(4) -0.0069(3) -0.0262(3) 0.0097(3) Ag3 0.0707(4) 0.0630(4) 0.0644(4) -0.0055(3) -0.0298(3) 0.0192(3) S1 0.0455(9) 0.0354(8) 0.0470(9) -0.0035(7) -0.0090(7) 0.0039(7) S2 0.0436(9) 0.0389(9) 0.0429(9) -0.0008(7) -0.0088(7) 0.0071(7) S3 0.0361(8) 0.0402(9) 0.0514(10) -0.0106(7) -0.0180(7) 0.0001(7) N1 0.055(4) 0.039(3) 0.057(4) -0.001(3) -0.017(3) -0.013(3) N2 0.038(3) 0.031(3) 0.040(3) -0.005(2) -0.006(2) 0.001(2) N3 0.033(3) 0.034(3) 0.039(3) -0.008(2) -0.008(2) -0.004(2) N4 0.051(3) 0.035(3) 0.058(4) -0.001(3) -0.020(3) -0.011(3) N5 0.049(3) 0.037(3) 0.070(4) -0.009(3) -0.014(3) 0.005(3) N6 0.049(3) 0.034(3) 0.073(4) -0.004(3) -0.019(3) 0.005(3) N7 0.053(4) 0.056(4) 0.074(5) -0.013(4) -0.010(3) -0.014(3) C1 0.043(4) 0.048(4) 0.054(4) -0.004(3) -0.020(3) -0.009(3) C2 0.048(4) 0.035(3) 0.052(4) -0.007(3) -0.021(3) -0.004(3) C3 0.037(3) 0.046(4) 0.045(4) 0.002(3) -0.016(3) -0.007(3) C4 0.037(3) 0.035(3) 0.057(4) 0.004(3) -0.020(3) -0.003(3) C5 0.040(3) 0.028(3) 0.066(5) -0.011(3) -0.003(3) 0.005(3) C6 0.032(3) 0.035(3) 0.042(3) -0.006(3) -0.009(3) -0.002(2) C7 0.036(3) 0.040(3) 0.037(3) -0.007(3) -0.011(3) -0.003(3) C8 0.038(3) 0.041(3) 0.046(4) -0.010(3) -0.014(3) -0.004(3) C9 0.035(3) 0.032(3) 0.044(3) -0.012(3) -0.002(3) -0.002(3) C10 0.035(3) 0.031(3) 0.046(4) -0.004(3) -0.002(3) 0.001(3) C11 0.034(3) 0.046(4) 0.048(4) -0.019(3) -0.012(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.313(5) . ? Ag1 N2 2.393(5) . ? Ag1 S3 2.4389(17) . ? Ag1 Ag1 2.9257(14) 2_577 ? Ag1 S3 2.9588(19) 2_577 ? Ag2 N1 2.287(6) 1_564 ? Ag2 N5 2.307(6) 2_676 ? Ag2 S1 2.623(2) . ? Ag2 S2 2.726(2) . ? Ag2 Ag3 3.2731(14) . ? Ag3 N6 2.239(6) 2_586 ? Ag3 N4 2.255(6) . ? Ag3 S2 2.735(2) . ? Ag3 S1 2.772(2) . ? S1 C9 1.668(7) . ? S2 C10 1.660(7) . ? S3 C11 1.673(7) . ? S3 Ag1 2.9588(19) 2_577 ? N1 C1 1.472(9) . ? N1 Ag2 2.287(6) 1_546 ? N2 C4 1.457(8) . ? N2 C3 1.468(8) . ? N3 C6 1.479(8) . ? N3 C5 1.481(8) . ? N4 C8 1.470(8) . ? N5 C9 1.146(9) . ? N5 Ag2 2.307(6) 2_676 ? N6 C10 1.141(9) . ? N6 Ag3 2.239(6) 2_586 ? N7 C11 1.148(9) . ? C1 C2 1.519(9) . ? C2 C3 1.523(9) . ? C4 C5 1.524(10) . ? C6 C7 1.522(9) . ? C7 C8 1.514(9) . ? 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 79.30(18) . . ? N3 Ag1 S3 136.30(14) . . ? N2 Ag1 S3 126.41(14) . . ? N3 Ag1 Ag1 142.60(13) . 2_577 ? N2 Ag1 Ag1 112.58(14) . 2_577 ? S3 Ag1 Ag1 66.22(5) . 2_577 ? N3 Ag1 S3 100.93(13) . 2_577 ? N2 Ag1 S3 83.71(14) . 2_577 ? S3 Ag1 S3 115.19(5) . 2_577 ? Ag1 Ag1 S3 48.97(4) 2_577 2_577 ? N1 Ag2 N5 115.1(2) 1_564 2_676 ? N1 Ag2 S1 121.73(16) 1_564 . ? N5 Ag2 S1 101.93(17) 2_676 . ? N1 Ag2 S2 105.90(17) 1_564 . ? N5 Ag2 S2 102.45(18) 2_676 . ? S1 Ag2 S2 108.04(6) . . ? N1 Ag2 Ag3 131.96(16) 1_564 . ? N5 Ag2 Ag3 111.85(18) 2_676 . ? S1 Ag2 Ag3 54.75(5) . . ? S2 Ag2 Ag3 53.30(5) . . ? N6 Ag3 N4 132.5(2) 2_586 . ? N6 Ag3 S2 98.74(17) 2_586 . ? N4 Ag3 S2 115.67(15) . . ? N6 Ag3 S1 96.90(19) 2_586 . ? N4 Ag3 S1 104.99(17) . . ? S2 Ag3 S1 103.66(6) . . ? N6 Ag3 Ag2 101.95(18) 2_586 . ? N4 Ag3 Ag2 124.59(15) . . ? S2 Ag3 Ag2 53.05(5) . . ? S1 Ag3 Ag2 50.61(4) . . ? C9 S1 Ag2 99.3(2) . . ? C9 S1 Ag3 105.0(2) . . ? Ag2 S1 Ag3 74.64(5) . . ? C10 S2 Ag2 98.9(2) . . ? C10 S2 Ag3 100.1(2) . . ? Ag2 S2 Ag3 73.64(5) . . ? C11 S3 Ag1 94.5(2) . . ? C11 S3 Ag1 112.1(2) . 2_577 ? Ag1 S3 Ag1 64.81(5) . 2_577 ? C1 N1 Ag2 120.2(4) . 1_546 ? C4 N2 C3 116.9(5) . . ? C4 N2 Ag1 102.4(4) . . ? C3 N2 Ag1 114.5(4) . . ? C6 N3 C5 112.6(5) . . ? C6 N3 Ag1 114.0(4) . . ? C5 N3 Ag1 105.9(4) . . ? C8 N4 Ag3 117.6(4) . . ? C9 N5 Ag2 156.9(6) . 2_676 ? C10 N6 Ag3 160.3(6) . 2_586 ? N1 C1 C2 112.5(6) . . ? C1 C2 C3 111.2(5) . . ? N2 C3 C2 116.2(5) . . ? N2 C4 C5 112.8(5) . . ? N3 C5 C4 112.1(5) . . ? N3 C6 C7 111.0(5) . . ? C8 C7 C6 111.7(5) . . ? N4 C8 C7 112.0(5) . . ? N5 C9 S1 177.7(6) . . ? N6 C10 S2 178.9(6) . . ? N7 C11 S3 177.8(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.112 _refine_diff_density_min -0.805 _refine_diff_density_rms 0.160 #_eof #End of Crystallographic Information File