Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author 'Chen, Xiao-Ming' _publ_contact_author_address ; 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 'JCS Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as a supplmentary data for a manuscript submitted to JCS Dalton Trans. Xiao-Ming Chen Nov. 12, 2000 ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Syntheses and structures of three two-dimensional silver(I)- hexamethylenetetramine co-ordination polymers with new topologic motifs ; loop_ _publ_author_name _publ_author_address 'Zheng, Shao-Liang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Tong, Ming-Liang' ; 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 ; 'Fang, Yue' ; 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_complex1 _database_code_CSD 159017 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H23 Ag N4 O4' _chemical_formula_weight 431.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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(1)/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 12.219(3) _cell_length_b 10.842(3) _cell_length_c 13.006(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.140(10) _cell_angle_gamma 90.00 _cell_volume 1718.5(7) _cell_formula_units_Z 4 _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 0.46 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.32 _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.200 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.6083 _exptl_absorpt_correction_T_max 0.7001 _exptl_absorpt_process_details '\y-scans (North et al., 1968)' _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_reflns_number 4331 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 28.00 _reflns_number_total 4146 _reflns_number_gt 3541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V. 5.0 (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^)+(0.0431P)^2^+1.2975P] 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 0.0187(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4146 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.001205(17) 0.068701(18) 0.105462(16) 0.04072(10) Uani 1 d . . . O2 O -0.1086(2) 0.1953(2) 0.00176(18) 0.0585(6) Uani 1 d . . . N1 N 0.10032(18) 0.22604(19) 0.20797(16) 0.0339(4) Uani 1 d . . . O1 O -0.16677(18) 0.03714(19) -0.09624(18) 0.0500(5) Uani 1 d . . . N3 N 0.2374(2) 0.2529(2) 0.35235(18) 0.0430(5) Uani 1 d . . . C8 C -0.2579(2) 0.2282(3) -0.1187(2) 0.0449(6) Uani 1 d . . . H8A H -0.2826 0.2983 -0.0816 0.080 Uiso 1 d R . . C4 C 0.1682(2) 0.1644(3) 0.2920(2) 0.0436(6) Uani 1 d . . . H4A H 0.2146 0.1044 0.2627 0.080 Uiso 1 d R . . H4B H 0.1218 0.1220 0.3369 0.080 Uiso 1 d R . . C7 C -0.1718(2) 0.1461(3) -0.0675(2) 0.0408(6) Uani 1 d . . . C9 C -0.3025(2) 0.2064(2) -0.2122(2) 0.0419(6) Uani 1 d . . . H9A H -0.2769 0.1350 -0.2470 0.080 Uiso 1 d R . . C3 C 0.1756(2) 0.2894(3) 0.1419(2) 0.0404(6) Uani 1 d . . . H3A H 0.1334 0.3306 0.0869 0.080 Uiso 1 d R . . H3B H 0.2212 0.2293 0.1117 0.080 Uiso 1 d R . . C10 C -0.3868(2) 0.2813(3) -0.2697(2) 0.0452(7) Uani 1 d . . . C11 C -0.4164(3) 0.2539(4) -0.3711(3) 0.0686(10) Uani 1 d . . . H11A H -0.3818 0.1869 -0.4046 0.080 Uiso 1 d R . . C1 C 0.3085(2) 0.3158(3) 0.2830(2) 0.0486(7) Uani 1 d . . . H1A H 0.3564 0.2570 0.2542 0.080 Uiso 1 d R . . H1B H 0.3529 0.3750 0.3218 0.080 Uiso 1 d R . . C15 C -0.4387(3) 0.3794(3) -0.2255(3) 0.0581(9) Uani 1 d . . . H15A H -0.4220 0.3994 -0.1541 0.080 Uiso 1 d R . . C13 C -0.5465(3) 0.4194(4) -0.3823(4) 0.0837(15) Uani 1 d . . . H13A H -0.6037 0.4654 -0.4194 0.080 Uiso 1 d R . . C12 C -0.4960(4) 0.3236(5) -0.4274(4) 0.0899(15) Uani 1 d . . . H12A H -0.5162 0.3050 -0.4984 0.080 Uiso 1 d R . . C14 C -0.5177(3) 0.4476(3) -0.2823(4) 0.0744(13) Uani 1 d . . . H14A H -0.5492 0.5182 -0.2512 0.080 Uiso 1 d R . . N2 N 0.09910(18) 0.41242(18) 0.31416(16) 0.0323(4) Uani 1 d . . . C6 C 0.1742(2) 0.4708(2) 0.2445(2) 0.0400(6) Uani 1 d . . . H6A H 0.2187 0.5305 0.2827 0.080 Uiso 1 d R . . H6B H 0.1319 0.5133 0.1904 0.080 Uiso 1 d R . . C5 C 0.0318(2) 0.3198(2) 0.25421(19) 0.0344(5) Uani 1 d . . . H5A H -0.0170 0.2800 0.2984 0.080 Uiso 1 d R . . H5B H -0.0119 0.3614 0.2005 0.080 Uiso 1 d R . . C2 C 0.1661(2) 0.3453(3) 0.3952(2) 0.0411(6) Uani 1 d . . . H2A H 0.2109 0.4040 0.4343 0.080 Uiso 1 d R . . H2B H 0.1192 0.3058 0.4414 0.080 Uiso 1 d R . . N4 N 0.24512(19) 0.3801(2) 0.19920(18) 0.0431(5) Uani 1 d . . . O1W O -0.0980(4) 0.4467(3) 0.0310(3) 0.1193(15) Uani 1 d . . . H1WA H -0.0985 0.3598 0.0145 0.120 Uiso 1 d R . . H1WB H -0.1801 0.4743 0.0220 0.120 Uiso 1 d R . . O2W O -0.3318(4) 0.5422(4) 0.0105(3) 0.1247(15) Uani 1 d . . . H2WA H -0.3049 0.6264 0.0488 0.120 Uiso 1 d R . . H2WB H -0.3219 0.5721 -0.0599 0.120 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 0.04152(14) 0.02924(12) 0.05031(15) 0.00254(8) -0.00412(8) -0.00233(8) O2 0.0679(14) 0.0439(12) 0.0601(13) 0.0000(10) -0.0194(11) 0.0133(11) N1 0.0386(11) 0.0278(10) 0.0345(10) -0.0049(8) -0.0025(8) 0.0013(8) O1 0.0470(11) 0.0339(10) 0.0682(14) 0.0031(9) -0.0021(10) 0.0079(9) N3 0.0500(13) 0.0389(12) 0.0381(12) -0.0046(10) -0.0103(10) 0.0099(10) C8 0.0428(15) 0.0395(15) 0.0522(16) 0.0020(12) 0.0016(12) 0.0112(12) C4 0.0538(16) 0.0291(12) 0.0461(15) -0.0009(11) -0.0079(12) 0.0071(12) C7 0.0398(14) 0.0389(14) 0.0439(14) 0.0094(11) 0.0055(11) 0.0066(11) C9 0.0354(13) 0.0318(12) 0.0581(17) 0.0063(12) 0.0011(12) 0.0020(11) C3 0.0483(15) 0.0420(14) 0.0311(12) -0.0058(11) 0.0047(11) -0.0014(12) C10 0.0341(13) 0.0390(14) 0.0616(18) 0.0133(13) -0.0015(12) -0.0025(11) C11 0.068(2) 0.082(3) 0.055(2) 0.0163(18) -0.0025(17) 0.015(2) C1 0.0348(13) 0.0525(17) 0.0577(17) -0.0139(14) -0.0025(12) 0.0038(12) C15 0.0419(16) 0.0368(15) 0.093(3) 0.0027(16) -0.0155(16) 0.0024(13) C13 0.049(2) 0.078(3) 0.121(4) 0.058(3) -0.016(2) 0.0004(19) C12 0.085(3) 0.116(4) 0.066(2) 0.039(3) -0.018(2) 0.002(3) C14 0.0444(18) 0.0433(18) 0.133(4) 0.016(2) -0.014(2) 0.0034(14) N2 0.0381(11) 0.0282(10) 0.0301(10) -0.0027(8) -0.0011(8) 0.0006(8) C6 0.0475(15) 0.0294(12) 0.0431(14) -0.0022(11) 0.0027(12) -0.0060(11) C5 0.0340(12) 0.0311(12) 0.0376(13) -0.0037(10) -0.0009(10) -0.0004(10) C2 0.0528(16) 0.0387(14) 0.0307(12) -0.0044(10) -0.0053(11) 0.0079(12) N4 0.0425(12) 0.0439(13) 0.0438(12) -0.0071(10) 0.0096(10) -0.0077(10) O1W 0.172(4) 0.066(2) 0.111(3) -0.0213(18) -0.055(3) 0.044(2) O2W 0.170(4) 0.103(3) 0.101(3) -0.012(2) 0.012(3) -0.021(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 O2 2.289(2) . ? Ag1 O1 2.336(2) 3 ? Ag1 N2 2.377(2) 2_545 ? Ag1 N1 2.433(2) . ? Ag1 Ag1 3.1199(7) 3 ? O2 C7 1.262(4) . ? O2 O1W 2.754(4) . ? N1 C5 1.473(3) . ? N1 C3 1.473(3) . ? N1 C4 1.483(3) . ? O1 C7 1.242(4) . ? O1 Ag1 2.336(2) 3 ? N3 C1 1.464(4) . ? N3 C2 1.465(4) . ? N3 C4 1.468(4) . ? C8 C9 1.318(4) . ? C8 C7 1.498(4) . ? C9 C10 1.472(4) . ? C3 N4 1.468(4) . ? C10 C11 1.376(5) . ? C10 C15 1.384(5) . ? C11 C12 1.397(5) . ? C1 N4 1.467(4) . ? C15 C14 1.387(5) . ? C13 C14 1.357(7) . ? C13 C12 1.362(7) . ? N2 C6 1.478(3) . ? N2 C2 1.478(3) . ? N2 C5 1.483(3) . ? N2 Ag1 2.377(2) 2 ? C6 N4 1.462(4) . ? O1W O2W 3.032(7) . ? O2W N3 3.072(5) 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 O2 Ag1 O1 137.47(9) . 3 ? O2 Ag1 N2 112.80(8) . 2_545 ? O1 Ag1 N2 98.53(8) 3 2_545 ? O2 Ag1 N1 98.62(8) . . ? O1 Ag1 N1 88.50(8) 3 . ? N2 Ag1 N1 120.71(7) 2_545 . ? O2 Ag1 Ag1 78.48(6) . 3 ? O1 Ag1 Ag1 70.95(6) 3 3 ? N2 Ag1 Ag1 94.24(5) 2_545 3 ? N1 Ag1 Ag1 142.11(5) . 3 ? C7 O2 Ag1 118.04(18) . . ? C7 O2 O1W 122.46(19) . . ? Ag1 O2 O1W 119.50(12) . . ? C5 N1 C3 108.3(2) . . ? C5 N1 C4 108.3(2) . . ? C3 N1 C4 107.5(2) . . ? C5 N1 Ag1 115.62(15) . . ? C3 N1 Ag1 108.29(15) . . ? C4 N1 Ag1 108.54(15) . . ? C7 O1 Ag1 123.00(19) . 3 ? C1 N3 C2 108.1(2) . . ? C1 N3 C4 108.6(2) . . ? C2 N3 C4 108.4(2) . . ? C9 C8 C7 122.3(3) . . ? N3 C4 N1 111.7(2) . . ? O1 C7 O2 125.1(3) . . ? O1 C7 C8 118.7(3) . . ? O2 C7 C8 116.1(3) . . ? C8 C9 C10 126.6(3) . . ? N4 C3 N1 112.3(2) . . ? C11 C10 C15 117.9(3) . . ? C11 C10 C9 119.5(3) . . ? C15 C10 C9 122.5(3) . . ? C10 C11 C12 120.7(4) . . ? N3 C1 N4 112.0(2) . . ? C10 C15 C14 120.7(4) . . ? C14 C13 C12 119.3(4) . . ? C13 C12 C11 120.5(5) . . ? C13 C14 C15 120.9(4) . . ? C6 N2 C2 108.2(2) . . ? C6 N2 C5 108.24(19) . . ? C2 N2 C5 107.4(2) . . ? C6 N2 Ag1 109.09(15) . 2 ? C2 N2 Ag1 108.26(15) . 2 ? C5 N2 Ag1 115.45(15) . 2 ? N4 C6 N2 111.8(2) . . ? N1 C5 N2 111.8(2) . . ? N3 C2 N2 112.3(2) . . ? C6 N4 C1 108.4(2) . . ? C6 N4 C3 108.5(2) . . ? C1 N4 C3 108.3(2) . . ? O2 O1W O2W 106.94(18) . . ? O1W O2W N3 83.73(14) . 2 ? O1W O2W N4 77.95(15) . 3_565 ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.471 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.068 #==================================END data_complex_2 _database_code_CSD 159018 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H22 Ag2 N4 O6' _chemical_formula_weight 630.16 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' '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.066(17) _cell_length_b 10.856(7) _cell_length_c 18.750(8) _cell_angle_alpha 90.00 _cell_angle_beta 120.81(1) _cell_angle_gamma 90.00 _cell_volume 4207(4) _cell_formula_units_Z 8 _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 0.48 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.990 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 1.909 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.4611 _exptl_absorpt_correction_T_max 0.7014 _exptl_absorpt_process_details '\y-scans (North et al., 1968)' _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 5216 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.01 _reflns_number_total 5097 _reflns_number_gt 3392 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V. 5.0 (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^)+(0.0674P)^2^+5.9135P] 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 0.00096(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5097 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1328 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.32382(2) 0.03280(4) 0.56123(2) 0.04799(17) Uani 1 d . . . Ag2 Ag 0.28366(2) 0.02861(4) 0.69087(2) 0.04345(16) Uani 1 d . . . O11 O 0.3649(2) 0.2186(4) 0.6286(2) 0.0540(11) Uani 1 d . . . O12 O 0.3907(2) 0.1001(4) 0.7375(3) 0.0556(11) Uani 1 d . . . O13 O 0.4564(2) 0.1813(5) 0.8819(3) 0.0657(13) Uani 1 d . . . H13 H 0.4229 0.1447 0.8336 0.120 Uiso 1 d R . . C11 C 0.3902(2) 0.2041(6) 0.7040(3) 0.0423(13) Uani 1 d . . . C12 C 0.4216(2) 0.3099(5) 0.7622(3) 0.0375(11) Uani 1 d . . . C13 C 0.4525(3) 0.2940(6) 0.8486(3) 0.0430(13) Uani 1 d . . . C14 C 0.4806(3) 0.3947(7) 0.9007(4) 0.0595(17) Uani 1 d . . . H14A H 0.5017 0.3840 0.9597 0.080 Uiso 1 d R . . C15 C 0.4776(3) 0.5097(7) 0.8687(5) 0.064(2) Uani 1 d . . . H15A H 0.4979 0.5786 0.9051 0.080 Uiso 1 d R . . C16 C 0.4451(4) 0.5268(6) 0.7830(5) 0.0652(19) Uani 1 d . . . H16A H 0.4414 0.6077 0.7602 0.080 Uiso 1 d R . . C17 C 0.4178(3) 0.4279(6) 0.7307(4) 0.0513(15) Uani 1 d . . . H17A H 0.3963 0.4393 0.6716 0.080 Uiso 1 d R . . O21 O 0.2041(2) -0.0776(5) 0.5811(3) 0.0673(13) Uani 1 d . . . O22 O 0.2325(2) -0.0788(4) 0.4856(3) 0.0577(11) Uani 1 d . . . O23 O 0.1764(2) -0.2195(4) 0.3609(2) 0.0551(11) Uani 1 d . . . H23 H 0.2019 -0.1573 0.4095 0.120 Uiso 1 d R . . C21 C 0.1977(3) -0.1136(5) 0.5147(4) 0.0456(13) Uani 1 d . . . C22 C 0.1473(2) -0.2083(5) 0.4651(3) 0.0346(11) Uani 1 d . . . C23 C 0.1392(2) -0.2568(5) 0.3918(3) 0.0388(12) Uani 1 d . . . C24 C 0.0932(3) -0.3486(6) 0.3498(3) 0.0457(14) Uani 1 d . . . H24A H 0.0885 -0.3837 0.3000 0.080 Uiso 1 d R . . C25 C 0.0543(3) -0.3882(6) 0.3795(4) 0.0480(14) Uani 1 d . . . H25A H 0.0231 -0.4522 0.3508 0.080 Uiso 1 d R . . C26 C 0.0599(3) -0.3382(6) 0.4497(4) 0.0481(14) Uani 1 d . . . H26A H 0.0317 -0.3644 0.4689 0.080 Uiso 1 d R . . C27 C 0.1061(3) -0.2502(5) 0.4925(3) 0.0436(13) Uani 1 d . . . H27A H 0.1102 -0.2157 0.5421 0.080 Uiso 1 d R . . N1 N 0.32723(19) 0.1190(4) 0.4442(2) 0.0335(9) Uani 1 d . . . N2 N 0.3101(2) 0.0994(4) 0.3042(2) 0.0340(9) Uani 1 d . . . N3 N 0.2819(2) 0.2920(4) 0.3463(2) 0.0351(9) Uani 1 d . . . N4 N 0.39579(19) 0.2348(4) 0.4065(2) 0.0360(10) Uani 1 d . . . C31 C 0.3089(3) 0.0363(5) 0.3736(3) 0.0358(11) Uani 1 d . . . H31A H 0.2662 0.0048 0.3540 0.080 Uiso 1 d R . . H31B H 0.3383 -0.0322 0.3917 0.080 Uiso 1 d R . . C32 C 0.2817(2) 0.2243(5) 0.4147(3) 0.0354(11) Uani 1 d . . . H32A H 0.2931 0.2796 0.4601 0.080 Uiso 1 d R . . H32B H 0.2387 0.1942 0.3955 0.080 Uiso 1 d R . . C33 C 0.3933(2) 0.1691(5) 0.4734(3) 0.0373(12) Uani 1 d . . . H33A H 0.4237 0.1022 0.4923 0.080 Uiso 1 d R . . H33B H 0.4057 0.2241 0.5192 0.080 Uiso 1 d R . . C34 C 0.3765(2) 0.1501(5) 0.3375(3) 0.0390(12) Uani 1 d . . . H34A H 0.3782 0.1923 0.2937 0.080 Uiso 1 d R . . H34B H 0.4068 0.0831 0.3556 0.080 Uiso 1 d R . . C35 C 0.3494(3) 0.3363(5) 0.3780(3) 0.0404(12) Uani 1 d . . . H35A H 0.3613 0.3924 0.4232 0.080 Uiso 1 d R . . H35B H 0.3508 0.3802 0.3345 0.080 Uiso 1 d R . . C36 C 0.2649(2) 0.2043(5) 0.2778(3) 0.0369(11) Uani 1 d . . . H36A H 0.2219 0.1740 0.2573 0.080 Uiso 1 d R . . H36B H 0.2654 0.2467 0.2332 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 0.0652(3) 0.0447(3) 0.0331(2) -0.00545(19) 0.0245(2) -0.0165(2) Ag2 0.0496(3) 0.0386(3) 0.0348(2) 0.00739(18) 0.01636(19) 0.00047(19) O11 0.061(3) 0.060(3) 0.0323(19) -0.015(2) 0.0183(19) -0.012(2) O12 0.056(2) 0.035(2) 0.066(3) -0.009(2) 0.024(2) -0.0120(19) O13 0.078(3) 0.062(3) 0.045(2) 0.014(2) 0.023(2) -0.001(2) C11 0.036(3) 0.044(3) 0.048(3) -0.012(3) 0.023(2) -0.008(2) C12 0.038(3) 0.035(3) 0.040(3) -0.004(2) 0.020(2) -0.004(2) C13 0.041(3) 0.049(3) 0.032(3) 0.000(2) 0.014(2) 0.003(3) C14 0.059(4) 0.069(5) 0.041(3) -0.017(3) 0.019(3) -0.001(3) C15 0.056(4) 0.052(4) 0.076(5) -0.036(4) 0.027(4) -0.010(3) C16 0.074(5) 0.037(3) 0.080(5) -0.007(4) 0.035(4) -0.001(3) C17 0.055(4) 0.047(3) 0.048(3) 0.001(3) 0.024(3) -0.007(3) O21 0.068(3) 0.069(3) 0.061(3) -0.034(3) 0.031(2) -0.009(2) O22 0.056(3) 0.055(3) 0.051(2) -0.007(2) 0.020(2) -0.018(2) O23 0.061(3) 0.064(3) 0.049(2) -0.006(2) 0.035(2) -0.009(2) C21 0.043(3) 0.038(3) 0.047(3) -0.007(3) 0.017(3) -0.002(2) C22 0.032(3) 0.031(3) 0.035(2) -0.002(2) 0.013(2) 0.002(2) C23 0.042(3) 0.039(3) 0.029(2) 0.002(2) 0.013(2) 0.002(2) C24 0.053(3) 0.045(3) 0.032(3) -0.007(2) 0.017(2) -0.003(3) C25 0.043(3) 0.040(3) 0.049(3) 0.002(3) 0.015(3) -0.007(3) C26 0.046(3) 0.047(3) 0.049(3) 0.005(3) 0.023(3) -0.005(3) C27 0.045(3) 0.046(3) 0.039(3) -0.002(3) 0.021(2) 0.007(3) N1 0.037(2) 0.035(2) 0.0280(19) 0.0000(17) 0.0161(17) -0.0012(18) N2 0.042(2) 0.029(2) 0.030(2) 0.0014(18) 0.0185(18) 0.0036(19) N3 0.039(2) 0.034(2) 0.030(2) -0.0003(18) 0.0159(18) 0.0034(18) N4 0.037(2) 0.039(2) 0.029(2) -0.0006(18) 0.0145(18) -0.0032(19) C31 0.044(3) 0.030(3) 0.031(2) 0.001(2) 0.017(2) -0.003(2) C32 0.037(3) 0.036(3) 0.040(3) -0.001(2) 0.024(2) 0.001(2) C33 0.037(3) 0.043(3) 0.026(2) 0.002(2) 0.012(2) -0.002(2) C34 0.045(3) 0.041(3) 0.038(3) -0.003(2) 0.027(2) -0.001(2) C35 0.046(3) 0.035(3) 0.040(3) -0.003(2) 0.022(2) -0.005(2) C36 0.043(3) 0.036(3) 0.025(2) 0.003(2) 0.013(2) 0.007(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 O22 2.262(4) . ? Ag1 O11 2.316(4) . ? Ag1 N1 2.426(4) . ? Ag1 Ag2 3.0417(13) . ? Ag2 O21 2.279(4) . ? Ag2 N2 2.338(4) 6_556 ? Ag2 N3 2.376(4) 7_556 ? Ag2 O12 2.387(4) . ? O11 C11 1.230(6) . ? O12 C11 1.288(7) . ? O12 O13 2.495(6) . ? O13 C13 1.356(7) . ? C11 C12 1.495(7) . ? C12 C17 1.394(8) . ? C12 C13 1.404(7) . ? C13 C14 1.389(8) . ? C14 C15 1.372(10) . ? C15 C16 1.393(10) . ? C16 C17 1.374(9) . ? O21 C21 1.235(7) . ? O22 C21 1.272(7) . ? O22 O23 2.527(6) . ? O23 C23 1.355(6) . ? C21 C22 1.495(7) . ? C22 C23 1.390(7) . ? C22 C27 1.404(7) . ? C23 C24 1.394(8) . ? C24 C25 1.380(8) . ? C25 C26 1.364(8) . ? C26 C27 1.371(8) . ? N1 C31 1.468(6) . ? N1 C32 1.481(6) . ? N1 C33 1.494(6) . ? N2 C36 1.474(6) . ? N2 C31 1.483(6) . ? N2 C34 1.492(7) . ? N2 Ag2 2.338(4) 6 ? N3 C36 1.479(6) . ? N3 C32 1.481(6) . ? N3 C35 1.493(7) . ? N3 Ag2 2.376(4) 7_556 ? N4 C34 1.456(6) . ? N4 C35 1.461(7) . ? N4 C33 1.470(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 O22 Ag1 O11 144.57(16) . . ? O22 Ag1 N1 96.39(15) . . ? O11 Ag1 N1 87.42(14) . . ? O22 Ag1 Ag2 83.63(13) . . ? O11 Ag1 Ag2 78.37(11) . . ? N1 Ag1 Ag2 154.25(10) . . ? O21 Ag2 N2 103.42(18) . 6_556 ? O21 Ag2 N3 91.44(17) . 7_556 ? N2 Ag2 N3 125.77(14) 6_556 7_556 ? O21 Ag2 O12 138.12(16) . . ? N2 Ag2 O12 96.91(15) 6_556 . ? N3 Ag2 O12 105.76(15) 7_556 . ? O21 Ag2 Ag1 75.47(13) . . ? N2 Ag2 Ag1 133.26(11) 6_556 . ? N3 Ag2 Ag1 100.88(10) 7_556 . ? O12 Ag2 Ag1 64.05(11) . . ? C11 O11 Ag1 109.7(4) . . ? C11 O12 Ag2 111.5(3) . . ? C11 O12 O13 93.6(3) . . ? Ag2 O12 O13 118.5(2) . . ? C13 O13 O12 87.8(3) . . ? O11 C11 O12 123.2(5) . . ? O11 C11 C12 120.5(5) . . ? O12 C11 C12 116.3(5) . . ? C17 C12 C13 118.9(5) . . ? C17 C12 C11 119.9(5) . . ? C13 C12 C11 121.2(5) . . ? O13 C13 C14 119.5(5) . . ? O13 C13 C12 120.9(5) . . ? C14 C13 C12 119.6(6) . . ? C15 C14 C13 120.7(6) . . ? C14 C15 C16 119.9(6) . . ? C17 C16 C15 120.0(6) . . ? C16 C17 C12 120.8(6) . . ? C21 O21 Ag2 133.2(4) . . ? C21 O22 Ag1 122.2(4) . . ? C21 O22 O23 93.5(3) . . ? Ag1 O22 O23 142.3(2) . . ? C23 O23 O22 86.7(3) . . ? O21 C21 O22 124.6(6) . . ? O21 C21 C22 119.2(6) . . ? O22 C21 C22 116.1(5) . . ? C23 C22 C27 118.1(5) . . ? C23 C22 C21 122.2(5) . . ? C27 C22 C21 119.7(5) . . ? O23 C23 C22 121.5(5) . . ? O23 C23 C24 118.7(5) . . ? C22 C23 C24 119.8(5) . . ? C25 C24 C23 120.1(5) . . ? C26 C25 C24 120.8(5) . . ? C25 C26 C27 119.5(6) . . ? C26 C27 C22 121.6(5) . . ? C31 N1 C32 108.2(4) . . ? C31 N1 C33 108.9(4) . . ? C32 N1 C33 107.6(4) . . ? C31 N1 Ag1 116.5(3) . . ? C32 N1 Ag1 105.9(3) . . ? C33 N1 Ag1 109.4(3) . . ? C36 N2 C31 108.0(4) . . ? C36 N2 C34 107.7(4) . . ? C31 N2 C34 107.5(4) . . ? C36 N2 Ag2 110.1(3) . 6 ? C31 N2 Ag2 113.8(3) . 6 ? C34 N2 Ag2 109.5(3) . 6 ? C36 N3 C32 108.0(4) . . ? C36 N3 C35 108.3(4) . . ? C32 N3 C35 107.5(4) . . ? C36 N3 Ag2 115.2(3) . 7_556 ? C32 N3 Ag2 111.4(3) . 7_556 ? C35 N3 Ag2 106.1(3) . 7_556 ? C34 N4 C35 108.3(4) . . ? C34 N4 C33 108.5(4) . . ? C35 N4 C33 108.7(4) . . ? N1 C31 N2 112.1(4) . . ? N1 C32 N3 112.1(4) . . ? N4 C33 N1 111.4(4) . . ? N4 C34 N2 113.0(4) . . ? N4 C35 N3 112.0(4) . . ? N2 C36 N3 112.2(4) . . ? _diffrn_measured_fraction_theta_max 0.476 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.476 _refine_diff_density_max 0.792 _refine_diff_density_min -0.913 _refine_diff_density_rms 0.117 #==================================END data_complex3 _database_code_CSD 159019 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H28 Ag2 N8 O6 S' _chemical_formula_weight 712.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca 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' '-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 17.059(10) _cell_length_b 11.247(5) _cell_length_c 24.520(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4704(4) _cell_formula_units_Z 8 _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 'yellow' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.40 _exptl_crystal_density_diffrn 2.011 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 1.809 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.4530 _exptl_absorpt_correction_T_max 0.5314 _exptl_absorpt_process_details '\y-scans (North et al., 1968)' _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 5483 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0727 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.71 _reflns_number_total 5246 _reflns_number_gt 3264 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V. 5.0 (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^)+(0.0602P)^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 0.00085(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5246 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1050 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1303 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.16478(3) 0.15356(4) 0.42122(2) 0.03074(15) Uani 1 d . . . Ag2 Ag -0.10868(4) 0.30784(6) 0.27257(2) 0.04435(19) Uani 1 d . . . S1 S 0.10572(10) 0.02169(16) 0.74186(7) 0.0333(4) Uani 1 d . . . O1 O 0.1381(4) 0.0677(6) 0.5257(2) 0.0697(19) Uani 1 d . . . O2 O 0.1929(3) 0.2433(6) 0.5106(2) 0.0589(16) Uani 1 d . . . O3 O 0.2111(3) 0.3918(5) 0.5869(2) 0.0507(14) Uani 1 d . . . H3 H 0.2372 0.3392 0.5598 0.080 Uiso 1 d . . . O4 O 0.1402(3) 0.0485(5) 0.79400(19) 0.0545(15) Uani 1 d . . . O5 O 0.0214(3) 0.0308(6) 0.7434(3) 0.076(2) Uani 1 d . . . O6 O 0.1306(5) -0.0894(5) 0.7195(2) 0.076(2) Uani 1 d . . . C1 C 0.1642(5) 0.1633(8) 0.5418(3) 0.048(2) Uani 1 d . . . C2 C 0.1645(4) 0.1930(6) 0.6019(2) 0.0301(15) Uani 1 d . . . C3 C 0.1865(4) 0.3047(6) 0.6209(3) 0.0337(16) Uani 1 d . . . C4 C 0.1819(4) 0.3303(6) 0.6770(3) 0.0378(17) Uani 1 d . . . H4A H 0.1971 0.4075 0.6900 0.080 Uiso 1 d R . . C5 C 0.1569(4) 0.2464(6) 0.7130(3) 0.0332(16) Uani 1 d . . . H5A H 0.1518 0.2665 0.7509 0.080 Uiso 1 d R . . C6 C 0.1382(4) 0.1322(6) 0.6952(2) 0.0261(14) Uani 1 d . . . C7 C 0.1413(4) 0.1070(6) 0.6399(3) 0.0309(15) Uani 1 d . . . H7A H 0.1276 0.0289 0.6274 0.080 Uiso 1 d R . . C8 C -0.0159(4) 0.2034(6) 0.4532(2) 0.0293(15) Uani 1 d . . . H8A H 0.0061 0.2052 0.4893 0.080 Uiso 1 d R . . H8B H -0.0268 0.1221 0.4442 0.080 Uiso 1 d R . . C9 C 0.0076(4) 0.2487(6) 0.3589(2) 0.0280(14) Uani 1 d . . . H9A H -0.0032 0.1678 0.3488 0.080 Uiso 1 d R . . H9B H 0.0446 0.2804 0.3332 0.080 Uiso 1 d R . . C10 C 0.0570(4) 0.3781(6) 0.4288(3) 0.0329(16) Uani 1 d . . . H10A H 0.0939 0.4115 0.4036 0.080 Uiso 1 d R . . H10B H 0.0798 0.3813 0.4646 0.080 Uiso 1 d R . . C11 C -0.0701(4) 0.3957(6) 0.4668(3) 0.0339(16) Uani 1 d . . . H11A H -0.1177 0.4414 0.4668 0.080 Uiso 1 d R . . H11B H -0.0484 0.3987 0.5028 0.080 Uiso 1 d R . . C12 C -0.0487(4) 0.4439(6) 0.3736(3) 0.0317(15) Uani 1 d . . . H12A H -0.0128 0.4787 0.3481 0.080 Uiso 1 d R . . H12B H -0.0960 0.4900 0.3731 0.080 Uiso 1 d R . . C13 C -0.1220(4) 0.2689(6) 0.3979(3) 0.0325(16) Uani 1 d . . . H13A H -0.1339 0.1882 0.3881 0.080 Uiso 1 d R . . H13B H -0.1700 0.3134 0.3976 0.080 Uiso 1 d R . . C14 C 0.2283(4) -0.1098(5) 0.4046(2) 0.0253(14) Uani 1 d . . . H14A H 0.2398 -0.1030 0.4428 0.080 Uiso 1 d R . . H14B H 0.2708 -0.0746 0.3847 0.080 Uiso 1 d R . . C15 C 0.2091(3) -0.2419(5) 0.3300(2) 0.0234(13) Uani 1 d . . . H15A H 0.2068 -0.3232 0.3181 0.080 Uiso 1 d R . . H15B H 0.2521 -0.2041 0.3116 0.080 Uiso 1 d R . . C16 C 0.1550(4) -0.2882(6) 0.4179(3) 0.0317(15) Uani 1 d . . . H16A H 0.1639 -0.2845 0.4565 0.080 Uiso 1 d R . . H16B H 0.1500 -0.3704 0.4080 0.080 Uiso 1 d R . . C17 C 0.0689(4) -0.2352(6) 0.3463(3) 0.0340(16) Uani 1 d . . . H17A H 0.0207 -0.1960 0.3371 0.080 Uiso 1 d R . . H17B H 0.0643 -0.3172 0.3360 0.080 Uiso 1 d R . . C18 C 0.1425(4) -0.0546(6) 0.3317(2) 0.0293(15) Uani 1 d . . . H18A H 0.1857 -0.0191 0.3126 0.080 Uiso 1 d R . . H18B H 0.0958 -0.0121 0.3219 0.080 Uiso 1 d R . . C19 C 0.0891(4) -0.1029(6) 0.4206(3) 0.0347(16) Uani 1 d . . . H19A H 0.0413 -0.0619 0.4120 0.080 Uiso 1 d R . . H19B H 0.0971 -0.0976 0.4592 0.080 Uiso 1 d R . . N1 N 0.0426(3) 0.2516(5) 0.4138(2) 0.0255(12) Uani 1 d . . . N2 N -0.0145(3) 0.4498(5) 0.4281(2) 0.0299(12) Uani 1 d . . . N3 N -0.0667(3) 0.3199(5) 0.3563(2) 0.0265(12) Uani 1 d . . . N4 N -0.0887(3) 0.2706(5) 0.4530(2) 0.0288(13) Uani 1 d . . . N5 N 0.1559(3) -0.0437(4) 0.3917(2) 0.0232(11) Uani 1 d . . . N6 N 0.2228(3) -0.2370(4) 0.38933(19) 0.0232(11) Uani 1 d . . . N7 N 0.0820(3) -0.2276(5) 0.4052(2) 0.0302(13) Uani 1 d . . . N8 N 0.1348(3) -0.1798(4) 0.31494(19) 0.0252(12) 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 0.0294(3) 0.0297(3) 0.0331(3) -0.0024(2) 0.0017(2) -0.0005(2) Ag2 0.0570(4) 0.0528(4) 0.0232(3) -0.0006(3) -0.0148(3) 0.0074(3) S1 0.0373(10) 0.0352(10) 0.0274(8) 0.0020(7) 0.0002(7) -0.0001(8) O1 0.097(5) 0.084(5) 0.029(3) -0.021(3) -0.008(3) 0.009(4) O2 0.052(3) 0.094(5) 0.031(3) 0.014(3) 0.010(3) 0.008(3) O3 0.050(3) 0.049(3) 0.054(3) 0.020(3) 0.017(3) 0.006(3) O4 0.067(4) 0.072(4) 0.025(3) 0.016(3) -0.012(3) -0.015(3) O5 0.038(4) 0.125(6) 0.066(4) 0.034(4) 0.007(3) -0.001(4) O6 0.136(6) 0.030(3) 0.061(4) 0.000(3) 0.043(4) 0.006(4) C1 0.040(4) 0.075(6) 0.029(4) 0.005(4) 0.003(3) 0.020(4) C2 0.025(3) 0.043(4) 0.022(3) -0.001(3) -0.001(3) 0.006(3) C3 0.030(4) 0.044(4) 0.027(3) 0.008(3) 0.000(3) 0.007(3) C4 0.045(4) 0.033(4) 0.036(4) -0.005(3) -0.008(3) 0.002(3) C5 0.040(4) 0.033(4) 0.027(3) 0.003(3) -0.007(3) 0.004(3) C6 0.026(3) 0.033(4) 0.019(3) 0.000(3) -0.003(3) 0.007(3) C7 0.026(3) 0.037(4) 0.029(3) 0.000(3) -0.006(3) 0.003(3) C8 0.034(4) 0.033(4) 0.021(3) 0.004(3) -0.001(3) -0.001(3) C9 0.026(3) 0.035(4) 0.023(3) -0.006(3) 0.007(3) 0.004(3) C10 0.035(4) 0.031(4) 0.032(4) 0.000(3) 0.004(3) -0.011(3) C11 0.033(4) 0.040(4) 0.028(3) -0.005(3) 0.001(3) 0.004(3) C12 0.030(4) 0.028(4) 0.037(4) 0.003(3) 0.001(3) 0.003(3) C13 0.024(3) 0.037(4) 0.036(4) -0.005(3) -0.006(3) 0.002(3) C14 0.024(3) 0.027(3) 0.025(3) -0.007(3) -0.004(2) 0.004(3) C15 0.024(3) 0.023(3) 0.022(3) -0.002(3) 0.000(3) 0.005(3) C16 0.045(4) 0.023(3) 0.027(3) 0.004(3) 0.003(3) -0.002(3) C17 0.020(3) 0.035(4) 0.047(4) -0.005(3) -0.006(3) 0.000(3) C18 0.035(4) 0.025(4) 0.028(3) 0.003(3) -0.007(3) 0.000(3) C19 0.032(4) 0.036(4) 0.037(4) -0.001(3) 0.010(3) -0.001(3) N1 0.022(3) 0.031(3) 0.024(3) 0.001(2) 0.001(2) 0.005(2) N2 0.032(3) 0.030(3) 0.028(3) -0.005(2) -0.006(2) 0.006(2) N3 0.023(3) 0.032(3) 0.025(3) -0.001(2) -0.004(2) 0.004(2) N4 0.027(3) 0.036(3) 0.024(3) -0.002(2) 0.005(2) 0.001(2) N5 0.021(3) 0.024(3) 0.024(3) 0.001(2) -0.004(2) 0.003(2) N6 0.025(3) 0.025(3) 0.019(2) 0.003(2) 0.000(2) 0.004(2) N7 0.026(3) 0.036(4) 0.029(3) 0.000(2) 0.002(2) -0.004(2) N8 0.030(3) 0.027(3) 0.019(2) -0.003(2) -0.005(2) 0.003(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 N5 2.339(5) . ? Ag1 N1 2.365(5) . ? Ag1 N6 2.409(5) 8_665 ? Ag1 O2 2.461(6) . ? Ag2 N3 2.178(5) . ? Ag2 N8 2.196(5) 3 ? Ag2 O6 2.493(6) 5_556 ? S1 O6 1.429(6) . ? S1 O4 1.439(5) . ? S1 O5 1.442(6) . ? S1 C6 1.778(6) . ? O1 C1 1.228(10) . ? O2 C1 1.278(9) . ? O2 O3 2.527(8) . ? O3 C3 1.352(8) . ? O6 Ag2 2.493(6) 5_556 ? C1 C2 1.512(9) . ? C2 C3 1.391(9) . ? C2 C7 1.400(9) . ? C3 C4 1.408(9) . ? C4 C5 1.361(9) . ? C5 C6 1.394(9) . ? C6 C7 1.387(8) . ? C8 N4 1.454(8) . ? C8 N1 1.491(8) . ? C9 N1 1.473(7) . ? C9 N3 1.501(8) . ? C10 N2 1.461(8) . ? C10 N1 1.491(8) . ? C11 N2 1.473(8) . ? C11 N4 1.482(9) . ? C12 N2 1.458(8) . ? C12 N3 1.491(8) . ? C13 N4 1.465(8) . ? C13 N3 1.503(8) . ? C14 N5 1.475(7) . ? C14 N6 1.482(8) . ? C15 N6 1.476(7) . ? C15 N8 1.493(7) . ? C16 N7 1.454(8) . ? C16 N6 1.470(8) . ? C17 N7 1.465(8) . ? C17 N8 1.497(8) . ? C18 N8 1.473(8) . ? C18 N5 1.494(7) . ? C19 N7 1.457(9) . ? C19 N5 1.499(8) . ? N6 Ag1 2.409(5) 8_655 ? N8 Ag2 2.196(5) 3_545 ? 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 N5 Ag1 N1 111.17(18) . . ? N5 Ag1 N6 115.81(17) . 8_665 ? N1 Ag1 N6 116.00(18) . 8_665 ? N5 Ag1 O2 132.67(19) . . ? N1 Ag1 O2 92.84(18) . . ? N6 Ag1 O2 85.67(17) 8_665 . ? N3 Ag2 N8 169.62(19) . 3 ? N3 Ag2 O6 92.1(2) . 5_556 ? N8 Ag2 O6 96.19(19) 3 5_556 ? O6 S1 O4 113.7(4) . . ? O6 S1 O5 111.6(5) . . ? O4 S1 O5 111.7(4) . . ? O6 S1 C6 105.8(3) . . ? O4 S1 C6 107.3(3) . . ? O5 S1 C6 106.1(3) . . ? C1 O2 Ag1 99.7(5) . . ? C1 O2 O3 94.0(5) . . ? Ag1 O2 O3 162.7(3) . . ? C3 O3 O2 86.5(4) . . ? S1 O6 Ag2 141.9(4) . 5_556 ? O1 C1 O2 124.3(7) . . ? O1 C1 C2 120.5(7) . . ? O2 C1 C2 115.2(8) . . ? C3 C2 C7 118.5(6) . . ? C3 C2 C1 121.8(6) . . ? C7 C2 C1 119.6(7) . . ? O3 C3 C2 122.1(6) . . ? O3 C3 C4 118.1(7) . . ? C2 C3 C4 119.8(6) . . ? C5 C4 C3 120.6(7) . . ? C4 C5 C6 120.5(6) . . ? C7 C6 C5 119.1(6) . . ? C7 C6 S1 119.9(5) . . ? C5 C6 S1 120.9(5) . . ? C6 C7 C2 121.4(7) . . ? N4 C8 N1 112.3(5) . . ? N1 C9 N3 111.6(5) . . ? N2 C10 N1 112.7(5) . . ? N2 C11 N4 112.5(5) . . ? N2 C12 N3 112.7(5) . . ? N4 C13 N3 112.2(5) . . ? N5 C14 N6 112.3(5) . . ? N6 C15 N8 111.2(5) . . ? N7 C16 N6 112.9(5) . . ? N7 C17 N8 111.6(5) . . ? N8 C18 N5 111.5(5) . . ? N7 C19 N5 111.6(5) . . ? C9 N1 C10 108.3(5) . . ? C9 N1 C8 108.3(5) . . ? C10 N1 C8 107.2(5) . . ? C9 N1 Ag1 114.7(4) . . ? C10 N1 Ag1 106.3(4) . . ? C8 N1 Ag1 111.7(4) . . ? C12 N2 C10 108.6(5) . . ? C12 N2 C11 108.2(5) . . ? C10 N2 C11 107.6(5) . . ? C12 N3 C9 108.2(5) . . ? C12 N3 C13 107.0(5) . . ? C9 N3 C13 107.3(5) . . ? C12 N3 Ag2 113.3(4) . . ? C9 N3 Ag2 106.5(3) . . ? C13 N3 Ag2 114.2(4) . . ? C8 N4 C13 109.1(5) . . ? C8 N4 C11 108.0(5) . . ? C13 N4 C11 107.8(5) . . ? C14 N5 C18 107.4(5) . . ? C14 N5 C19 108.1(5) . . ? C18 N5 C19 108.2(5) . . ? C14 N5 Ag1 110.9(3) . . ? C18 N5 Ag1 113.1(4) . . ? C19 N5 Ag1 108.9(4) . . ? C16 N6 C15 109.3(5) . . ? C16 N6 C14 107.9(5) . . ? C15 N6 C14 107.2(5) . . ? C16 N6 Ag1 105.8(4) . 8_655 ? C15 N6 Ag1 115.3(3) . 8_655 ? C14 N6 Ag1 111.2(3) . 8_655 ? C16 N7 C19 109.0(5) . . ? C16 N7 C17 108.3(5) . . ? C19 N7 C17 108.8(5) . . ? C18 N8 C15 107.6(5) . . ? C18 N8 C17 108.8(5) . . ? C15 N8 C17 108.4(5) . . ? C18 N8 Ag2 110.5(4) . 3_545 ? C15 N8 Ag2 112.6(3) . 3_545 ? C17 N8 Ag2 108.9(4) . 3_545 ? _diffrn_measured_fraction_theta_max 0.783 _diffrn_reflns_theta_full 28.71 _diffrn_measured_fraction_theta_full 0.783 _refine_diff_density_max 0.929 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.137 #_eof #End of Crystallographic Information File