Supplementary Material for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' 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 ; 'Chen, Xiao-Ming' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Ng, Seik-Weng' ; Institute of Postgraduate Studies and Research University of Malaya 50603 Kuala Lumpur Malaysia ; #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof Xiao-Ming Chen' _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_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 July 31, 2001 ; #================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Self-assembly of new three-dimensional molecular architectures constructed from silver(I)-hexamethylenetetramine layers with supramolecular interactions ; #============================================================ data_complex_1 _database_code_CSD 169729 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H18 Ag N5 O3 S' _chemical_formula_weight 420.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pmn2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y, z+1/2' '-x, y, z' _cell_length_a 6.562(5) _cell_length_b 13.342(8) _cell_length_c 8.555(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00(5) _cell_angle_gamma 90.00 _cell_volume 749.0(8) _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 needl _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.863 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 1.505 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.6445 _exptl_absorpt_correction_T_max 0.7734 _exptl_absorpt_process_details '\y-scans (North et al., 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _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 2251 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 28.99 _reflns_number_total 1148 _reflns_number_gt 1085 _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^)+(0.0429P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(4) _refine_ls_number_reflns 1148 _refine_ls_number_parameters 115 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0645 _refine_ls_wR_factor_gt 0.0635 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 1.0000 0.88876(3) 1.00018(6) 0.02763(11) Uani 1 d S . . S1 S 1.0000 0.76900(9) 0.67374(16) 0.0323(3) Uani 1 d S . . O1 O 1.0000 0.8417(3) 0.5467(5) 0.0332(9) Uani 1 d S . . O2 O 0.8138(9) 0.7773(3) 0.7673(5) 0.0673(14) Uani 1 d . . . N1 N 1.0000 0.3633(4) 0.3816(8) 0.0464(15) Uani 1 d S . . H1A H 0.8712 0.3448 0.3599 0.080 Uiso 1 d R . . N2 N 0.8115(5) 1.1273(2) 0.6387(4) 0.0214(6) Uani 1 d . . . N3 N 1.0000 1.2281(3) 0.8300(6) 0.0251(9) Uani 1 d S . . N4 N 1.0000 1.0445(3) 0.8522(5) 0.0230(8) Uani 1 d S . . C1 C 1.0000 0.6485(4) 0.5879(7) 0.0312(11) Uani 1 d S . . C2 C 0.8181(7) 0.6021(3) 0.5495(6) 0.0412(11) Uani 1 d . . . H2A H 0.6916 0.6352 0.5719 0.080 Uiso 1 d R . . C3 C 0.8166(7) 0.5087(3) 0.4782(7) 0.0453(13) Uani 1 d . . . H3A H 0.6891 0.4774 0.4529 0.080 Uiso 1 d R . . C4 C 1.0000 0.4595(4) 0.4446(7) 0.0340(12) Uani 1 d S . . C5 C 0.8176(6) 1.2230(3) 0.7304(5) 0.0268(7) Uani 1 d . . . H5A H 0.6979 1.2276 0.7945 0.080 Uiso 1 d R . . H5B H 0.8173 1.2789 0.6597 0.080 Uiso 1 d R . . C6 C 1.0000 1.1426(4) 0.9384(7) 0.0276(10) Uani 1 d S . . H6A H 0.8816 1.1462 1.0041 0.080 Uiso 1 d R . . C7 C 0.8153(5) 1.0431(2) 0.7517(4) 0.0240(7) Uani 1 d . . . H7A H 0.8106 0.9809 0.6955 0.080 Uiso 1 d R . . H7B H 0.6963 1.0466 0.8168 0.080 Uiso 1 d R . . C8 C 1.0000 1.1211(4) 0.5420(6) 0.0238(11) Uani 1 d S . . H8A H 1.0000 1.1743 0.4664 0.080 Uiso 1 d SR . . H8B H 1.0000 1.0586 0.4864 0.080 Uiso 1 d SR . . 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 0.02587(16) 0.03359(18) 0.02343(16) 0.0014(2) 0.000 0.000 S1 0.0521(8) 0.0216(5) 0.0233(6) -0.0036(5) 0.000 0.000 O1 0.044(2) 0.0245(17) 0.031(2) 0.0024(14) 0.000 0.000 O2 0.100(4) 0.0351(17) 0.067(3) -0.0074(18) 0.056(3) -0.004(2) N1 0.063(4) 0.026(2) 0.051(4) -0.010(2) 0.000 0.000 N2 0.0211(12) 0.0220(12) 0.0210(13) -0.0009(10) -0.0020(11) -0.0001(10) N3 0.026(2) 0.0234(19) 0.026(2) -0.0039(17) 0.000 0.000 N4 0.025(2) 0.0228(18) 0.0212(19) 0.0008(16) 0.000 0.000 C1 0.039(3) 0.023(2) 0.031(3) -0.003(2) 0.000 0.000 C2 0.0290(18) 0.040(2) 0.055(3) -0.0152(18) -0.0030(17) 0.0076(15) C3 0.0326(17) 0.045(2) 0.059(4) -0.017(2) -0.001(2) -0.0061(16) C4 0.044(3) 0.026(2) 0.033(3) -0.005(2) 0.000 0.000 C5 0.0288(18) 0.0241(16) 0.0274(18) -0.0005(14) 0.0012(15) 0.0051(14) C6 0.028(2) 0.032(2) 0.023(2) -0.004(2) 0.000 0.000 C7 0.0212(14) 0.0217(14) 0.0291(17) 0.0012(13) 0.0013(13) -0.0049(13) C8 0.020(2) 0.033(2) 0.018(2) -0.0014(16) 0.000 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 N2 2.373(4) 3_575 ? Ag1 N2 2.373(4) 2_675 ? Ag1 N4 2.433(4) . ? S1 O1 1.457(4) . ? S1 O2 1.465(5) 4_755 ? S1 O2 1.465(5) . ? S1 C1 1.768(6) . ? N1 C4 1.391(7) . ? N1 O2 2.953(6) 2_664 ? N2 C7 1.482(4) . ? N2 C8 1.490(4) . ? N2 C5 1.499(5) . ? N2 Ag1 2.373(4) 2_674 ? N3 C6 1.470(7) . ? N3 C5 1.471(5) . ? N3 C5 1.471(5) 4_755 ? N4 C7 1.486(4) . ? N4 C7 1.486(4) 4_755 ? N4 C6 1.503(7) . ? C1 C2 1.384(5) . ? C1 C2 1.384(5) 4_755 ? C2 C3 1.388(6) . ? C3 C4 1.401(5) . ? C4 C3 1.401(5) 4_755 ? C8 N2 1.490(4) 4_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 N2 Ag1 N2 118.99(16) 3_575 2_675 ? N2 Ag1 N4 109.70(8) 3_575 . ? N2 Ag1 N4 109.70(8) 2_675 . ? O1 S1 O2 110.9(2) . 4_755 ? O1 S1 O2 110.9(2) . . ? O2 S1 O2 113.0(4) 4_755 . ? O1 S1 C1 107.2(3) . . ? O2 S1 C1 107.22(18) 4_755 . ? O2 S1 C1 107.22(18) . . ? C4 N1 O2 135.58(13) . 2_664 ? C7 N2 C8 107.8(3) . . ? C7 N2 C5 107.7(3) . . ? C8 N2 C5 108.4(3) . . ? C7 N2 Ag1 105.8(2) . 2_674 ? C8 N2 Ag1 115.6(2) . 2_674 ? C5 N2 Ag1 111.2(2) . 2_674 ? C6 N3 C5 109.2(3) . . ? C6 N3 C5 109.2(3) . 4_755 ? C5 N3 C5 108.9(4) . 4_755 ? C7 N4 C7 109.3(4) . 4_755 ? C7 N4 C6 107.1(3) . . ? C7 N4 C6 107.1(3) 4_755 . ? C7 N4 Ag1 106.9(2) . . ? C7 N4 Ag1 106.9(2) 4_755 . ? C6 N4 Ag1 119.3(3) . . ? C2 C1 C2 119.2(5) . 4_755 ? C2 C1 S1 120.4(3) . . ? C2 C1 S1 120.4(3) 4_755 . ? C1 C2 C3 120.8(4) . . ? C2 C3 C4 120.3(4) . . ? N1 C4 C3 120.8(3) . 4_755 ? N1 C4 C3 120.8(3) . . ? C3 C4 C3 118.5(5) 4_755 . ? N3 C5 N2 111.4(3) . . ? N3 C6 N4 111.5(4) . . ? N2 C7 N4 112.4(3) . . ? N2 C8 N2 112.2(4) 4_755 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.472 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.084 #=======================================END data_complex_2 _database_code_CSD 169730 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H26 Ag N4 O5 S' _chemical_formula_weight 530.37 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 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 30.323(18) _cell_length_b 10.923(10) _cell_length_c 6.349(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2103(3) _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 'pale yellow' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.32 _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 1.097 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.6439 _exptl_absorpt_correction_T_max 0.7203 _exptl_absorpt_process_details '\y-scans (North et al., 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _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 2095 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2018 _reflns_number_gt 1538 _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^)+(0.0574P)^2^+10.5412P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.13(13) _refine_ls_number_reflns 2018 _refine_ls_number_parameters 188 _refine_ls_number_restraints 112 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1316 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.006 _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 0.24269(2) 0.09387(6) 0.5060(6) 0.0326(2) Uani 1 d . . . S1 S 0.35115(7) 0.2714(2) 0.5091(9) 0.0316(5) Uani 1 d D . . O1 O 0.3216(3) 0.1867(11) 0.625(2) 0.036(3) Uani 0.67 d PD A 1 O2 O 0.3487(3) 0.2561(11) 0.2820(13) 0.024(2) Uani 0.67 d PD A 1 O3 O 0.3415(5) 0.3972(9) 0.576(3) 0.077(7) Uani 0.67 d PD A 1 O1' O 0.3323(7) 0.1826(18) 0.361(4) 0.036(3) Uani 0.33 d PD A 2 O2' O 0.3470(6) 0.3956(12) 0.427(4) 0.024(2) Uani 0.33 d PD A 2 O3' O 0.3266(6) 0.259(2) 0.710(3) 0.077(7) Uani 0.33 d PD A 2 O1W O 0.1662(3) -0.0319(7) 0.504(3) 0.052(2) Uani 1 d . . . H1W1 H 0.1645 -0.0850 0.6233 0.050 Uiso 1 d . . . H1W2 H 0.1653 -0.0847 0.3764 0.050 Uiso 1 d . . . O2W O 0.3385(2) 0.0497(7) 1.010(3) 0.051(2) Uani 1 d . . . H2W1 H 0.3376 0.0995 0.9018 0.050 Uiso 1 d . . . H2W2 H 0.3451 0.0947 1.1148 0.050 Uiso 1 d . . . C1 C 0.43614(17) 0.1825(6) 0.4447(11) 0.046(5) Uani 1 d G . . H1 H 0.4264 0.1615 0.3106 0.055 Uiso 1 calc R . . C2 C 0.40710(15) 0.2347(6) 0.5883(12) 0.045(3) Uani 1 d GD . . C3 C 0.4217(2) 0.2661(7) 0.7887(12) 0.051(4) Uani 1 d G . . H3 H 0.4023 0.3010 0.8848 0.061 Uiso 1 calc R . . C4 C 0.4653(2) 0.2452(7) 0.8455(11) 0.050(4) Uani 1 d G . . H4 H 0.4751 0.2661 0.9796 0.060 Uiso 1 calc R . . C5 C 0.49435(16) 0.1929(5) 0.7019(11) 0.044(3) Uani 1 d G . . C6 C 0.47976(15) 0.1616(4) 0.5015(11) 0.040(3) Uani 1 d G . . C7 C 0.5088(2) 0.1093(7) 0.3579(13) 0.046(3) Uani 1 d G . . H7 H 0.4990 0.0884 0.2238 0.055 Uiso 1 calc R . . C8 C 0.55242(19) 0.0884(7) 0.4147(17) 0.083(8) Uani 1 d G . . H8 H 0.5718 0.0535 0.3186 0.100 Uiso 1 calc R . . C9 C 0.56701(16) 0.1198(8) 0.6151(18) 0.056(5) Uani 1 d G . . H9 H 0.5962 0.1058 0.6531 0.068 Uiso 1 calc R . . C10 C 0.53798(18) 0.1720(7) 0.7587(15) 0.059(4) Uani 1 d G . . H10 H 0.5477 0.1930 0.8928 0.071 Uiso 1 calc R . . N1 N 0.2155(4) 0.2030(12) 0.205(2) 0.0249(8) Uani 1 d D . . N2 N 0.22130(19) 0.3993(6) 0.010(3) 0.0249(8) Uani 1 d D . . N3 N 0.2172(4) 0.2036(12) -0.186(2) 0.0249(8) Uani 1 d D . . N4 N 0.1523(2) 0.2804(5) 0.004(2) 0.0249(8) Uani 1 d D . . C11 C 0.2363(6) 0.3270(14) 0.196(3) 0.0277(8) Uani 1 d D . . H11A H 0.2681 0.3179 0.1906 0.033 Uiso 1 calc R . . H11B H 0.2290 0.3715 0.3237 0.033 Uiso 1 calc R . . C12 C 0.2309(3) 0.1386(7) 0.010(2) 0.0277(8) Uani 1 d D . . H12A H 0.2628 0.1322 0.0133 0.033 Uiso 1 calc R . . H12B H 0.2189 0.0563 0.0085 0.033 Uiso 1 calc R . . C13 C 0.1664(4) 0.2186(15) 0.202(2) 0.0277(8) Uani 1 d D . . H13A H 0.1524 0.1391 0.2116 0.033 Uiso 1 calc R . . H13B H 0.1573 0.2670 0.3220 0.033 Uiso 1 calc R . . C14 C 0.1720(2) 0.4046(7) 0.003(5) 0.0277(8) Uani 1 d D . . H14A H 0.1613 0.4503 0.1231 0.033 Uiso 1 calc R . . H14B H 0.1628 0.4474 -0.1239 0.033 Uiso 1 calc R . . C15 C 0.1680(4) 0.2089(14) -0.180(2) 0.0277(8) Uani 1 d D . . H15A H 0.1572 0.2462 -0.3084 0.033 Uiso 1 calc R . . H15B H 0.1563 0.1264 -0.1721 0.033 Uiso 1 calc R . . C16 C 0.2340(6) 0.3314(13) -0.184(2) 0.0277(8) Uani 1 d D . . H16A H 0.2225 0.3744 -0.3063 0.033 Uiso 1 calc R . . H16B H 0.2659 0.3301 -0.1957 0.033 Uiso 1 calc R . . C1A C 0.5345(9) 0.454(3) 0.386(5) 0.095(5) Uiso 0.50 d PG B -1 H1A H 0.5525 0.4264 0.4950 0.114 Uiso 0.50 calc PR B -1 C2A C 0.4905(9) 0.482(3) 0.426(4) 0.095(5) Uiso 0.50 d PG B -1 H2A H 0.4791 0.4724 0.5606 0.114 Uiso 0.50 calc PR B -1 C3A C 0.4636(7) 0.523(3) 0.263(5) 0.095(5) Uiso 0.50 d PG B -1 H3A H 0.4342 0.5415 0.2895 0.114 Uiso 0.50 calc PR B -1 C4A C 0.4807(9) 0.537(3) 0.061(4) 0.095(5) Uiso 0.50 d PG B -1 H4A H 0.4627 0.5645 -0.0472 0.114 Uiso 0.50 calc PR B -1 C5A C 0.5247(10) 0.509(3) 0.022(5) 0.095(5) Uiso 0.50 d PG B -1 H5A H 0.5361 0.5185 -0.1128 0.114 Uiso 0.50 calc PR B -1 C6A C 0.5516(7) 0.468(3) 0.185(6) 0.095(5) Uiso 0.50 d PG B -1 H6A H 0.5810 0.4495 0.1583 0.114 Uiso 0.50 calc PR B -1 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 0.0432(4) 0.0248(4) 0.0299(4) -0.0010(11) 0.0012(11) 0.0063(3) S1 0.0252(11) 0.0319(12) 0.0377(13) 0.007(3) 0.000(3) 0.0071(9) O1 0.021(6) 0.026(4) 0.061(7) -0.001(8) -0.006(6) 0.012(4) O2 0.009(4) 0.039(7) 0.025(5) -0.011(6) -0.006(4) 0.011(4) O3 0.072(10) 0.032(7) 0.13(2) -0.010(10) -0.013(11) 0.008(7) O1' 0.021(6) 0.026(4) 0.061(7) -0.001(8) -0.006(6) 0.012(4) O2' 0.009(4) 0.039(7) 0.025(5) -0.011(6) -0.006(4) 0.011(4) O3' 0.072(10) 0.032(7) 0.13(2) -0.010(10) -0.013(11) 0.008(7) O1W 0.059(5) 0.046(4) 0.053(5) 0.020(10) 0.015(11) -0.009(4) O2W 0.052(4) 0.055(4) 0.045(5) -0.006(12) -0.012(13) 0.003(4) C1 0.038(6) 0.029(6) 0.070(14) -0.002(6) -0.012(6) 0.012(5) C2 0.052(8) 0.032(6) 0.051(8) 0.012(6) -0.010(7) 0.002(6) C3 0.053(8) 0.052(8) 0.048(9) -0.010(8) 0.000(7) 0.011(7) C4 0.046(8) 0.059(9) 0.045(8) -0.010(8) -0.022(7) 0.005(7) C5 0.031(6) 0.042(7) 0.060(10) 0.013(8) -0.010(7) 0.009(6) C6 0.029(5) 0.038(6) 0.055(8) -0.034(11) -0.001(12) 0.005(4) C7 0.025(6) 0.064(9) 0.049(8) -0.003(8) 0.009(6) 0.000(6) C8 0.051(10) 0.065(11) 0.13(2) -0.010(12) 0.001(11) 0.027(9) C9 0.044(8) 0.073(11) 0.052(10) -0.002(9) 0.001(8) 0.023(9) C10 0.057(9) 0.053(9) 0.067(11) 0.011(9) -0.022(9) 0.006(7) N1 0.0261(17) 0.0241(17) 0.0244(19) -0.002(5) 0.001(5) 0.0020(14) N2 0.0261(17) 0.0241(17) 0.0244(19) -0.002(5) 0.001(5) 0.0020(14) N3 0.0261(17) 0.0241(17) 0.0244(19) -0.002(5) 0.001(5) 0.0020(14) N4 0.0261(17) 0.0241(17) 0.0244(19) -0.002(5) 0.001(5) 0.0020(14) C11 0.0332(19) 0.0241(17) 0.0258(19) 0.001(6) -0.009(5) 0.0001(15) C12 0.0332(19) 0.0241(17) 0.0258(19) 0.001(6) -0.009(5) 0.0001(15) C13 0.0332(19) 0.0241(17) 0.0258(19) 0.001(6) -0.009(5) 0.0001(15) C14 0.0332(19) 0.0241(17) 0.0258(19) 0.001(6) -0.009(5) 0.0001(15) C15 0.0332(19) 0.0241(17) 0.0258(19) 0.001(6) -0.009(5) 0.0001(15) C16 0.0332(19) 0.0241(17) 0.0258(19) 0.001(6) -0.009(5) 0.0001(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 N2 2.389(7) 4_545 ? Ag1 N1 2.400(14) . ? Ag1 N3 2.421(14) 1_556 ? S1 O2 1.453(8) . ? S1 O2' 1.458(9) . ? S1 O1' 1.466(9) . ? S1 O3 1.466(8) . ? S1 O1 1.483(8) . ? S1 O3' 1.485(9) . ? S1 C2 1.814(5) . ? O1 O2W 2.91(2) . ? O3' O2W 3.00(3) . ? O1W O2' 2.83(3) 4_545 ? O1W O3 2.84(3) 4_544 ? O1W O2 2.946(16) 4_545 ? O1W O3' 2.95(3) 4_544 ? O1W S1 3.843(19) 4_544 ? O1W S1 3.895(17) 4_545 ? O2W O1' 2.67(2) 1_556 ? O2W O2 2.856(17) 1_556 ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C5 C10 1.3900 . ? C6 C7 1.3900 . ? C7 C8 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? N1 C11 1.494(7) . ? N1 C12 1.495(7) . ? N1 C13 1.498(7) . ? N2 C16 1.488(7) . ? N2 C11 1.494(7) . ? N2 C14 1.496(7) . ? N2 Ag1 2.389(7) 4_554 ? N3 C16 1.485(7) . ? N3 C12 1.492(7) . ? N3 C15 1.493(7) . ? N3 Ag1 2.421(14) 1_554 ? N4 C14 1.482(7) . ? N4 C15 1.484(7) . ? N4 C13 1.487(7) . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C2A C3A 1.3900 . ? C3A C4A 1.3900 . ? C4A C5A 1.3900 . ? C5A C6A 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 127.3(4) 4_545 . ? N2 Ag1 N3 125.3(4) 4_545 1_556 ? N1 Ag1 N3 106.79(19) . 1_556 ? O2 S1 O2' 75.4(9) . . ? O2 S1 O1' 43.1(10) . . ? O2' S1 O1' 110.7(9) . . ? O2 S1 O3 112.6(8) . . ? O2 S1 O1 112.9(7) . . ? O3 S1 O1 108.8(7) . . ? O2' S1 O3' 110.4(9) . . ? O1' S1 O3' 107.2(9) . . ? O2 S1 C2 107.3(5) . . ? O2' S1 C2 112.6(8) . . ? O1' S1 C2 113.4(8) . . ? O3 S1 C2 108.3(7) . . ? O1 S1 C2 106.8(5) . . ? O3' S1 C2 102.1(8) . . ? S1 O1 O2W 129.1(6) . . ? S1 O3' O2W 123.7(12) . . ? O2' O1W O3 145.3(4) 4_545 4_544 ? O3 O1W O2 110.3(4) 4_544 4_545 ? O2' O1W O3' 113.2(5) 4_545 4_544 ? O3 O1W O3' 35.9(4) 4_544 4_544 ? O2 O1W O3' 77.4(5) 4_545 4_544 ? O1' O2W O2 22.0(5) 1_556 1_556 ? O1' O2W O1 114.2(5) 1_556 . ? O2 O2W O1 97.0(4) 1_556 . ? O1' O2W O3' 96.1(6) 1_556 . ? O2 O2W O3' 78.1(5) 1_556 . ? C2 C1 C6 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 S1 119.8(4) . . ? C1 C2 S1 120.1(4) . . ? C4 C3 C2 120.0 . . ? C3 C4 C5 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 C10 120.0 . . ? C4 C5 C10 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 C1 120.0 . . ? C5 C6 C1 120.0 . . ? C8 C7 C6 120.0 . . ? C7 C8 C9 120.0 . . ? C10 C9 C8 120.0 . . ? C9 C10 C5 120.0 . . ? C11 N1 C12 105.4(12) . . ? C11 N1 C13 108.4(12) . . ? C12 N1 C13 110.7(11) . . ? C11 N1 Ag1 109.5(9) . . ? C12 N1 Ag1 108.5(8) . . ? C13 N1 Ag1 114.1(9) . . ? C16 N2 C11 108.3(6) . . ? C16 N2 C14 104.7(15) . . ? C11 N2 C14 110.4(14) . . ? C16 N2 Ag1 108.5(8) . 4_554 ? C11 N2 Ag1 109.8(8) . 4_554 ? C14 N2 Ag1 114.9(4) . 4_554 ? C16 N3 C12 110.3(11) . . ? C16 N3 C15 107.8(12) . . ? C12 N3 C15 105.9(10) . . ? C16 N3 Ag1 111.2(10) . 1_554 ? C12 N3 Ag1 110.5(9) . 1_554 ? C15 N3 Ag1 111.0(8) . 1_554 ? C14 N4 C15 110.3(14) . . ? C14 N4 C13 107.7(14) . . ? C15 N4 C13 109.3(6) . . ? N1 C11 N2 112.3(11) . . ? N3 C12 N1 112.2(6) . . ? N4 C13 N1 110.5(11) . . ? N4 C14 N2 111.6(6) . . ? N4 C15 N3 111.3(10) . . ? N3 C16 N2 112.7(12) . . ? C2A C1A C6A 120.0 . . ? C1A C2A C3A 120.0 . . ? C2A C3A C4A 120.0 . . ? C5A C4A C3A 120.0 . . ? C6A C5A C4A 120.0 . . ? C5A C6A C1A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.801 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.127 #=======================================END data_complex_3 _database_code_CSD 169731 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H44 Ag4 N12 O11' _chemical_formula_weight 1084.17 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' '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 Pnnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 10.588(4) _cell_length_b 23.728(12) _cell_length_c 6.3740(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1601.4(10) _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 colorless _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 2.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 2.487 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.3077 _exptl_absorpt_correction_T_max 0.5867 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _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 1999 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.00 _reflns_number_total 1906 _reflns_number_gt 1509 _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^)+(0.0860P)^2^+4.3002P] 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 0.0005(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1906 _refine_ls_number_parameters 143 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1424 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.065 _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 0.69823(5) 0.21042(3) 0.0000 0.0267(2) Uani 1 d S . . Ag2 Ag 0.61721(9) 0.45706(4) 0.0000 0.0565(3) Uani 1 d S . . O1 O 1.2748(7) 0.0958(3) 0.0000 0.079(4) Uani 1 d S . . O2 O 1.1071(7) 0.1489(3) 0.0000 0.086(4) Uani 1 d S . . O3 O 0.8305(5) 0.12805(19) 0.1730(8) 0.0446(12) Uani 1 d . . . N1 N 0.5674(4) 0.20130(18) -0.3062(7) 0.0223(9) Uani 1 d . . . N2 N 0.4481(7) 0.1298(3) -0.5000 0.0283(15) Uani 1 d S . . N3 N 0.3742(6) 0.2271(3) -0.5000 0.0228(13) Uani 1 d S . . C1 C 1.1583(8) 0.1031(3) 0.0000 0.0274(17) Uani 1 d S . . C2 C 0.8653(7) 0.1077(3) 0.0000 0.0249(16) Uani 1 d S . . C3 C 1.1304(7) -0.0032(3) 0.0000 0.0248(16) Uani 1 d S . . H3A H 1.2209 -0.0058 0.0000 0.080 Uiso 1 d SR . . C4 C 1.0731(7) 0.0507(3) 0.0000 0.0231(15) Uani 1 d S . . C5 C 0.9420(7) 0.0539(3) 0.0000 0.0224(15) Uani 1 d S . . C6 C 0.5233(5) 0.1409(2) -0.3120(9) 0.0278(12) Uani 1 d . . . H6A H 0.4734 0.1331 -0.1897 0.080 Uiso 1 d R . . H6B H 0.5954 0.1164 -0.3097 0.080 Uiso 1 d R . . C7 C 0.3380(7) 0.1661(3) -0.5000 0.0264(17) Uani 1 d S . . H7A H 0.2877 0.1582 -0.3782 0.080 Uiso 1 d R . . C8 C 0.4536(5) 0.2381(2) -0.3111(8) 0.0239(11) Uani 1 d . . . H8A H 0.4797 0.2768 -0.3116 0.080 Uiso 1 d R . . H8B H 0.4041 0.2317 -0.1871 0.080 Uiso 1 d R . . C9 C 0.6417(7) 0.2120(4) -0.5000 0.0253(16) Uani 1 d S . . H9A H 0.7149 0.1881 -0.5000 0.080 Uiso 1 d SR . . H9B H 0.6700 0.2504 -0.5000 0.080 Uiso 1 d SR . . N4 N 0.5237(8) 0.3773(3) 0.0000 0.046(2) Uani 1 d S . . H4A H 0.4394 0.3824 0.0000 0.150 Uiso 1 d SR . . H4B H 0.5465 0.3579 -0.1153 0.150 Uiso 1 d R . . N5 N 0.7184(11) 0.5334(4) 0.0000 0.059(3) Uani 1 d S . . H5A H 0.7673 0.5352 0.1153 0.150 Uiso 1 d R . . H5B H 0.6637 0.5625 0.0000 0.150 Uiso 1 d SR . . O1W O 0.958(4) 0.493(2) 0.0000 0.199(19) Uani 0.50 d SPU . . H1WA H 0.9736 0.4722 -0.1044 0.150 Uiso 0.50 d PR . . O2W O 0.9352(18) 0.4853(7) -0.316(5) 0.188(12) Uani 0.50 d PU . . H2WA H 0.9675 0.4779 -0.5000 0.150 Uiso 1 d SR . . H2WB H 0.9781 0.5154 -0.3065 0.150 Uiso 0.50 d PR . . 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 0.0217(3) 0.0314(4) 0.0271(3) 0.000 0.000 0.0000(2) Ag2 0.0645(6) 0.0552(6) 0.0499(5) 0.000 0.000 -0.0160(4) O1 0.027(3) 0.035(4) 0.174(11) 0.000 0.000 -0.007(3) O2 0.042(4) 0.015(3) 0.202(13) 0.000 0.000 -0.001(3) O3 0.058(3) 0.040(2) 0.037(3) -0.006(2) 0.007(2) 0.018(2) N1 0.022(2) 0.027(2) 0.018(2) 0.0007(18) -0.0010(18) 0.0033(17) N2 0.038(4) 0.021(3) 0.026(3) 0.000 0.000 0.002(3) N3 0.022(3) 0.027(3) 0.020(3) 0.000 0.000 0.004(3) C1 0.029(4) 0.020(4) 0.033(4) 0.000 0.000 -0.002(3) C2 0.020(3) 0.015(3) 0.039(5) 0.000 0.000 -0.003(3) C3 0.021(3) 0.016(3) 0.037(4) 0.000 0.000 -0.004(3) C4 0.024(4) 0.020(4) 0.025(4) 0.000 0.000 0.004(3) C5 0.028(4) 0.018(3) 0.021(4) 0.000 0.000 0.008(3) C6 0.030(3) 0.028(3) 0.025(3) 0.003(2) 0.000(2) 0.002(2) C7 0.020(3) 0.037(4) 0.022(4) 0.000 0.000 -0.004(3) C8 0.024(2) 0.028(3) 0.019(3) -0.004(2) -0.002(2) 0.004(2) C9 0.019(3) 0.033(4) 0.024(4) 0.000 0.000 0.004(3) N4 0.045(5) 0.055(5) 0.039(4) 0.000 0.000 -0.009(4) N5 0.075(7) 0.060(6) 0.042(5) 0.000 0.000 -0.011(5) O1W 0.20(2) 0.19(2) 0.20(2) 0.000 0.000 0.011(10) O2W 0.110(13) 0.082(11) 0.37(3) -0.025(18) -0.018(19) 0.005(10) _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 2.381(6) 7_666 ? Ag1 N1 2.403(4) . ? Ag1 N1 2.403(4) 6 ? Ag2 N5 2.104(10) . ? Ag2 N4 2.135(8) . ? Ag2 Ag2 3.211(2) 5_665 ? O1 C1 1.246(11) . ? O2 C1 1.214(11) . ? O3 C2 1.259(6) . ? N1 C9 1.486(6) . ? N1 C8 1.488(6) . ? N1 C6 1.507(7) . ? N2 C7 1.449(10) . ? N2 C6 1.463(7) . ? N2 C6 1.463(7) 6_554 ? N3 C8 1.492(6) . ? N3 C8 1.492(6) 6_554 ? N3 C7 1.498(10) . ? N3 Ag1 2.381(6) 7_565 ? C1 C4 1.538(11) . ? C2 O3 1.259(6) 6 ? C2 C5 1.512(10) . ? C3 C4 1.416(10) . ? C3 C5 1.425(10) 5_755 ? C4 C5 1.391(11) . ? C5 C3 1.425(10) 5_755 ? C9 N1 1.486(6) 6_554 ? N4 O3 2.923(8) 7_565 ? N4 O3 2.923(8) 4_455 ? N5 O3 3.107(9) 3_655 ? N5 O3 3.107(9) 8_765 ? N5 O2W 3.26(3) 6 ? O1W O1W 0.95(9) 5_765 ? O2W O2W 1.54(4) 2_765 ? O2W O2W 2.81(6) 5_764 ? 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 N1 120.47(12) 7_666 . ? N3 Ag1 N1 120.47(12) 7_666 6 ? N1 Ag1 N1 108.6(2) . 6 ? N5 Ag2 N4 177.0(4) . . ? N5 Ag2 Ag2 81.2(3) . 5_665 ? N4 Ag2 Ag2 101.7(2) . 5_665 ? C9 N1 C8 108.2(5) . . ? C9 N1 C6 107.8(5) . . ? C8 N1 C6 107.8(4) . . ? C9 N1 Ag1 110.8(3) . . ? C8 N1 Ag1 115.5(3) . . ? C6 N1 Ag1 106.5(3) . . ? C7 N2 C6 109.3(4) . . ? C7 N2 C6 109.3(4) . 6_554 ? C6 N2 C6 110.0(6) . 6_554 ? C8 N3 C8 107.7(6) . 6_554 ? C8 N3 C7 108.2(4) . . ? C8 N3 C7 108.2(4) 6_554 . ? C8 N3 Ag1 109.4(3) . 7_565 ? C8 N3 Ag1 109.4(3) 6_554 7_565 ? C7 N3 Ag1 113.7(4) . 7_565 ? O2 C1 O1 124.6(8) . . ? O2 C1 C4 117.6(8) . . ? O1 C1 C4 117.9(7) . . ? O3 C2 O3 122.3(7) 6 . ? O3 C2 C5 118.7(4) 6 . ? O3 C2 C5 118.7(4) . . ? C4 C3 C5 122.1(7) . 5_755 ? C5 C4 C3 118.6(7) . . ? C5 C4 C1 122.8(7) . . ? C3 C4 C1 118.7(7) . . ? C4 C5 C3 119.3(7) . 5_755 ? C4 C5 C2 125.6(7) . . ? C3 C5 C2 115.0(7) 5_755 . ? N2 C6 N1 111.1(4) . . ? N2 C7 N3 111.6(6) . . ? N1 C8 N3 111.8(4) . . ? N1 C9 N1 112.4(6) 6_554 . ? Ag2 N4 O3 111.3(3) . 7_565 ? Ag2 N4 O3 111.3(3) . 4_455 ? O3 N4 O3 91.0(3) 7_565 4_455 ? Ag2 N5 O3 122.5(3) . 3_655 ? Ag2 N5 O3 122.5(3) . 8_765 ? O3 N5 O3 84.2(3) 3_655 8_765 ? Ag2 N5 O2W 93.3(4) . 6 ? O3 N5 O2W 87.5(5) 3_655 6 ? O3 N5 O2W 141.7(5) 8_765 6 ? O2W O2W O2W 56.7(9) 2_765 5_764 ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 1.437 _refine_diff_density_min -1.055 _refine_diff_density_rms 0.184 #_eof #End of Crystallographic Information File