Electronic Supplementary Material for CrystEngComm This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Jhy-Der Chen' _publ_contact_author_address ; Department of Chemistry Chung-Yuan Christian University Chung Li TAIWAN ; _publ_contact_author_email JDCHEN@CYCU.EDU.TW _publ_section_title ; Adjusting the Frameworks of Polymeric Silver(I) Complexes with 2-Aminopyrimidyl Ligands by Changing the Counterions ; loop_ _publ_author_name 'Jhy-Der Chen.' 'Zhi-Kai Chan.' 'Huan-Ching Chen.' 'Kuan-Lun Chu.' ; Maw-Cherng Suen ; 'Yueh-Hua Wang.' 'Chun-Wei Yeh.' # Attachment 'agll.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 281177' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H10 Ag2 N6 O4 S' _chemical_formula_weight 502.02 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 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 13.689(3) _cell_length_b 8.3977(14) _cell_length_c 11.3004(14) _cell_angle_alpha 90.00 _cell_angle_beta 107.446(13) _cell_angle_gamma 90.00 _cell_volume 1239.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.21 _cell_measurement_theta_max 17.13 _exptl_crystal_description niddle _exptl_crystal_colour colorless _exptl_crystal_size_max 1.0 _exptl_crystal_size_mid 0.7 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 3.356 _exptl_absorpt_correction_type \y-scan _exptl_absorpt_correction_T_min 0.3481 _exptl_absorpt_correction_T_max 0.4586 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1420 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1090 _reflns_number_gt 1029 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+6.6321P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00150(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1090 _refine_ls_number_parameters 117 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0238 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0553 _refine_ls_wR_factor_gt 0.0540 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag -0.24247(2) -0.19063(4) -0.30070(2) 0.02881(15) Uani 1 1 d . . . S S 0.0000 -0.14277(14) -0.2500 0.0191(3) Uani 1 2 d S . . O1 O -0.07955(19) -0.2438(4) -0.3327(3) 0.0344(6) Uani 1 1 d . . . O2 O -0.0462(2) -0.0411(3) -0.1759(3) 0.0370(7) Uani 1 1 d . . . N1 N -0.3054(2) -0.1372(3) -0.1418(3) 0.0202(6) Uani 1 1 d . . . N2 N -0.1926(2) 0.0712(4) -0.0653(3) 0.0205(6) Uani 1 1 d . . . N3 N -0.3079(2) 0.0024(3) 0.0408(3) 0.0205(6) Uani 1 1 d . . . C1 C -0.3841(3) -0.2269(4) -0.1320(3) 0.0246(7) Uani 1 1 d . . . C2 C -0.4284(3) -0.2053(4) -0.0385(4) 0.0275(8) Uani 1 1 d . . . C3 C -0.3858(3) -0.0886(4) 0.0475(3) 0.0243(7) Uani 1 1 d . . . C4 C -0.2707(2) -0.0236(4) -0.0548(3) 0.0178(6) Uani 1 1 d . . . H1 H -0.403(3) -0.313(5) -0.187(4) 0.029(11) Uiso 1 1 d . . . H2 H -0.480(3) -0.268(5) -0.032(4) 0.036(12) Uiso 1 1 d . . . H3 H -0.409(3) -0.069(4) 0.117(4) 0.019(9) Uiso 1 1 d . . . H21 H -0.152(3) 0.029(5) -0.094(4) 0.023(11) Uiso 1 1 d . . . H22 H -0.163(3) 0.115(6) -0.003(4) 0.033(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.0292(2) 0.0344(2) 0.0249(2) -0.00077(11) 0.01121(13) 0.00074(11) S 0.0163(5) 0.0213(6) 0.0203(6) 0.000 0.0066(4) 0.000 O1 0.0260(14) 0.0344(15) 0.0353(16) -0.0042(13) -0.0024(12) -0.0071(12) O2 0.0442(16) 0.0350(15) 0.0414(16) -0.0023(13) 0.0276(13) 0.0059(13) N1 0.0201(13) 0.0191(14) 0.0215(14) 0.0000(12) 0.0065(11) -0.0006(11) N2 0.0207(14) 0.0216(15) 0.0212(16) -0.0026(12) 0.0090(13) -0.0013(12) N3 0.0240(14) 0.0193(14) 0.0191(14) -0.0001(12) 0.0078(11) 0.0018(12) C1 0.0242(17) 0.0207(17) 0.0270(19) -0.0018(15) 0.0047(15) -0.0019(14) C2 0.0234(17) 0.0272(19) 0.034(2) 0.0038(16) 0.0111(16) -0.0051(15) C3 0.0254(17) 0.0258(19) 0.0241(18) 0.0039(15) 0.0113(14) 0.0039(15) C4 0.0194(15) 0.0151(15) 0.0170(16) 0.0039(13) 0.0029(12) 0.0034(12) _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 Ag N1 2.257(3) . ? Ag N3 2.356(3) 6 ? Ag O1 2.406(3) . ? Ag N2 2.506(3) 4_444 ? S O2 1.465(3) . ? S O2 1.465(3) 2_554 ? S O1 1.473(3) 2_554 ? S O1 1.473(3) . ? N1 C1 1.346(4) . ? N1 C4 1.350(4) . ? N2 C4 1.365(4) . ? N2 Ag 2.506(3) 4_454 ? N2 H21 0.80(4) . ? N2 H22 0.79(5) . ? N3 C3 1.333(5) . ? N3 C4 1.344(4) . ? N3 Ag 2.356(3) 6_556 ? C1 C2 1.380(5) . ? C1 H1 0.94(4) . ? C2 C3 1.380(5) . ? C2 H2 0.90(4) . ? C3 H3 0.95(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag N3 108.83(10) . 6 ? N1 Ag O1 138.46(10) . . ? N3 Ag O1 99.71(10) 6 . ? N1 Ag N2 119.26(10) . 4_444 ? N3 Ag N2 95.22(10) 6 4_444 ? O1 Ag N2 86.43(9) . 4_444 ? O2 S O2 108.7(2) . 2_554 ? O2 S O1 109.70(16) . 2_554 ? O2 S O1 109.54(16) 2_554 2_554 ? O2 S O1 109.55(16) . . ? O2 S O1 109.69(16) 2_554 . ? O1 S O1 109.6(2) 2_554 . ? S O1 Ag 109.89(16) . . ? C1 N1 C4 116.9(3) . . ? C1 N1 Ag 117.4(2) . . ? C4 N1 Ag 125.8(2) . . ? C4 N2 Ag 111.9(2) . 4_454 ? C4 N2 H21 115(3) . . ? Ag N2 H21 106(3) 4_454 . ? C4 N2 H22 114(3) . . ? Ag N2 H22 100(3) 4_454 . ? H21 N2 H22 109(4) . . ? C3 N3 C4 117.1(3) . . ? C3 N3 Ag 118.0(2) . 6_556 ? C4 N3 Ag 124.8(2) . 6_556 ? N1 C1 C2 122.4(3) . . ? N1 C1 H1 116(3) . . ? C2 C1 H1 121(3) . . ? C1 C2 C3 116.3(3) . . ? C1 C2 H2 121(3) . . ? C3 C2 H2 122(3) . . ? N3 C3 C2 122.9(3) . . ? N3 C3 H3 115(2) . . ? C2 C3 H3 122(2) . . ? N3 C4 N1 124.3(3) . . ? N3 C4 N2 118.0(3) . . ? N1 C4 N2 117.6(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.507 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.094 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 281178' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H7.50 Ag Cl N4.50 O4' _chemical_formula_weight 349.98 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 9.9740(18) _cell_length_b 11.6687(14) _cell_length_c 9.2700(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1078.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 7.74 _cell_measurement_theta_max 12.49 _exptl_crystal_description PLATE _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 2.124 _exptl_absorpt_correction_type \y-scan _exptl_absorpt_correction_T_min 0.7945 _exptl_absorpt_correction_T_max 0.9841 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1524 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1389 _reflns_number_gt 1372 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.8489P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'difmap and geom' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0081(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(6) _refine_ls_number_reflns 1389 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0259 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0525 _refine_ls_wR_factor_gt 0.0524 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.82573(4) 0.74094(3) 0.94092(5) 0.04807(16) Uani 1 1 d . . . N1 N 0.8355(5) 0.9206(3) 0.8644(5) 0.0348(9) Uani 1 1 d . . . N2 N 0.8227(5) 0.9890(4) 1.0961(5) 0.0415(11) Uani 1 1 d . . . N3 N 0.7933(4) 1.1189(3) 0.9120(5) 0.0361(10) Uani 1 1 d . . . N4 N 0.9704(5) 0.5986(4) 0.8451(5) 0.0379(10) Uani 1 1 d . . . N5 N 1.0000 0.5000 1.0571(8) 0.0415(15) Uani 1 2 d S . . C1 C 0.8183(5) 1.0102(4) 0.9547(6) 0.0302(10) Uani 1 1 d . . . C2 C 0.7957(5) 1.1383(5) 0.7702(6) 0.0434(14) Uani 1 1 d . . . H2A H 0.7818 1.2127 0.7375 0.052 Uiso 1 1 calc R . . C3 C 0.8177(6) 1.0536(5) 0.6705(6) 0.0488(14) Uani 1 1 d . . . H3A H 0.8211 1.0690 0.5721 0.059 Uiso 1 1 calc R . . C4 C 0.8344(6) 0.9451(5) 0.7235(6) 0.0440(13) Uani 1 1 d . . . H4A H 0.8456 0.8854 0.6583 0.053 Uiso 1 1 calc R . . C5 C 1.0000 0.5000 0.9124(8) 0.0325(16) Uani 1 2 d S . . C6 C 0.9738(7) 0.5966(5) 0.7012(6) 0.0477(15) Uani 1 1 d . . . H6A H 0.9575 0.6643 0.6513 0.057 Uiso 1 1 calc R . . C7 C 1.0000 0.5000 0.6246(9) 0.054(2) Uani 1 2 d S . . H7A H 1.0000 0.5000 0.5243 0.065 Uiso 1 2 calc SR . . Cl Cl 0.53655(13) 0.73138(13) 0.68281(13) 0.0419(3) Uani 1 1 d . . . O1 O 0.4473(6) 0.6748(6) 0.5929(7) 0.127(3) Uani 1 1 d . . . O2 O 0.5400(7) 0.8489(5) 0.6503(7) 0.113(2) Uani 1 1 d . . . O3 O 0.4924(5) 0.7227(4) 0.8272(4) 0.0698(13) Uani 1 1 d . . . O4 O 0.6692(4) 0.6830(4) 0.6740(5) 0.0668(13) Uani 1 1 d . . . H2NA H 0.8513 0.9242 1.1279 0.06(2) Uiso 1 1 d R . . H2NB H 0.8145 1.0505 1.1537 0.07(2) Uiso 1 1 d R . . H5NA H 1.0037 0.5650 1.1103 0.029(14) Uiso 1 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 Ag 0.0676(3) 0.02395(19) 0.0526(2) -0.0015(2) -0.0043(2) -0.0006(2) N1 0.034(2) 0.0273(19) 0.043(2) 0.0007(18) 0.002(2) 0.002(2) N2 0.053(3) 0.030(2) 0.041(2) 0.001(2) -0.010(3) 0.008(3) N3 0.035(2) 0.0259(19) 0.048(3) 0.0070(19) 0.003(2) -0.0004(17) N4 0.045(2) 0.032(2) 0.037(2) 0.001(2) 0.008(2) 0.006(2) N5 0.049(4) 0.045(4) 0.031(3) 0.000 0.000 0.008(3) C1 0.024(2) 0.027(2) 0.040(3) -0.001(2) -0.001(3) 0.001(2) C2 0.037(3) 0.035(3) 0.059(3) 0.016(3) 0.008(3) 0.003(2) C3 0.049(3) 0.059(3) 0.038(3) 0.012(3) 0.006(3) 0.000(3) C4 0.045(3) 0.045(3) 0.042(3) -0.005(3) 0.009(3) 0.004(3) C5 0.025(3) 0.036(4) 0.036(4) 0.000 0.000 0.001(3) C6 0.064(4) 0.038(3) 0.041(3) 0.007(3) 0.006(3) 0.006(3) C7 0.082(7) 0.046(5) 0.033(4) 0.000 0.000 0.011(5) Cl 0.0421(6) 0.0502(8) 0.0335(6) 0.0027(6) -0.0001(5) 0.0046(7) O1 0.086(4) 0.178(6) 0.118(5) -0.091(5) -0.045(4) 0.013(4) O2 0.118(5) 0.080(4) 0.142(5) 0.072(4) 0.000(5) 0.008(4) O3 0.072(3) 0.089(4) 0.049(2) 0.010(3) 0.024(2) 0.008(3) O4 0.048(2) 0.089(3) 0.064(3) -0.006(3) 0.012(2) 0.015(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 Ag N1 2.216(4) . ? Ag N3 2.302(4) 3_647 ? Ag N4 2.372(4) . ? N1 C4 1.337(7) . ? N1 C1 1.350(6) . ? N2 C1 1.335(7) . ? N2 H2NA 0.8609 . ? N2 H2NB 0.8975 . ? N3 C2 1.334(7) . ? N3 C1 1.351(6) . ? N3 Ag 2.302(4) 3_657 ? N4 C6 1.334(7) . ? N4 C5 1.342(5) . ? N5 C5 1.341(11) . ? N5 H5NA 0.9053 . ? C2 C3 1.371(8) . ? C2 H2A 0.9300 . ? C3 C4 1.368(7) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 N4 1.342(5) 2_765 ? C6 C7 1.358(7) . ? C6 H6A 0.9300 . ? C7 C6 1.358(7) 2_765 ? C7 H7A 0.9300 . ? Cl O1 1.387(5) . ? Cl O2 1.404(5) . ? Cl O3 1.413(4) . ? Cl O4 1.440(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag N3 142.94(15) . 3_647 ? N1 Ag N4 121.06(16) . . ? N3 Ag N4 95.87(14) 3_647 . ? C4 N1 C1 116.0(4) . . ? C4 N1 Ag 121.0(4) . . ? C1 N1 Ag 121.9(3) . . ? C1 N2 H2NA 120.7 . . ? C1 N2 H2NB 115.6 . . ? H2NA N2 H2NB 122.0 . . ? C2 N3 C1 116.4(5) . . ? C2 N3 Ag 119.2(4) . 3_657 ? C1 N3 Ag 120.1(3) . 3_657 ? C6 N4 C5 116.4(5) . . ? C6 N4 Ag 113.7(4) . . ? C5 N4 Ag 124.1(4) . . ? C5 N5 H5NA 123.0 . . ? N2 C1 N1 117.4(4) . . ? N2 C1 N3 117.9(5) . . ? N1 C1 N3 124.6(5) . . ? N3 C2 C3 123.0(5) . . ? N3 C2 H2A 118.5 . . ? C3 C2 H2A 118.5 . . ? C4 C3 C2 116.3(5) . . ? C4 C3 H3A 121.8 . . ? C2 C3 H3A 121.8 . . ? N1 C4 C3 123.4(5) . . ? N1 C4 H4A 118.3 . . ? C3 C4 H4A 118.3 . . ? N5 C5 N4 117.7(3) . 2_765 ? N5 C5 N4 117.7(3) . . ? N4 C5 N4 124.6(7) 2_765 . ? N4 C6 C7 122.8(6) . . ? N4 C6 H6A 118.6 . . ? C7 C6 H6A 118.6 . . ? C6 C7 C6 116.9(8) 2_765 . ? C6 C7 H7A 121.5 2_765 . ? C6 C7 H7A 121.5 . . ? O1 Cl O2 110.6(5) . . ? O1 Cl O3 109.6(4) . . ? O2 Cl O3 106.3(4) . . ? O1 Cl O4 111.6(3) . . ? O2 Cl O4 110.4(4) . . ? O3 Cl O4 108.2(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.468 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.075 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 281179' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H9 Ag N3 O4' _chemical_formula_weight 295.03 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' 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 Ibam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1, -z+1/2' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x, -y, z+1/2' '-x, y, z+1/2' _cell_length_a 25.249(2) _cell_length_b 6.2859(9) _cell_length_c 12.6954(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2014.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.16 _cell_measurement_theta_max 12.28 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.994 _exptl_absorpt_correction_type \y-scan _exptl_absorpt_correction_T_min 0.6476 _exptl_absorpt_correction_T_max 0.9307 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1255 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0081 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 24.98 _reflns_number_total 932 _reflns_number_gt 845 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+11.2470P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0045(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 932 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0603 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.252038(15) 0.0000 0.2500 0.0404(2) Uani 1 2 d S . . O1 O 0.3344(2) 0.0854(9) 0.2001(4) 0.0465(12) Uani 0.50 1 d P . . O2 O 0.3704(2) -0.0979(10) 0.3302(4) 0.0527(14) Uani 0.50 1 d P . . N1 N 0.21286(10) 0.0704(4) 0.09428(19) 0.0291(6) Uani 1 1 d . . . N2 N 0.29084(15) 0.0730(6) 0.0000 0.0311(8) Uani 1 2 d S . . C1 C 0.15995(13) 0.0774(5) 0.0916(3) 0.0359(7) Uani 1 1 d . . . C2 C 0.13175(19) 0.0846(9) 0.0000 0.0401(11) Uani 1 2 d S . . C3 C 0.23822(17) 0.0723(7) 0.0000 0.0265(9) Uani 1 2 d S . . C4 C 0.37353(18) 0.0000 0.2500 0.0375(11) Uani 1 2 d S . . C5 C 0.4266(3) 0.0321(18) 0.1933(8) 0.073(3) Uani 0.50 1 d P . . O3 O 0.4677(2) 0.1838(9) 0.0744(5) 0.0585(14) Uani 0.50 1 d P . . O4 O 0.0000 0.0000 0.4299(7) 0.061(2) Uani 0.50 2 d SP . . O5 O -0.0165(6) 0.016(4) 0.2855(9) 0.080(6) Uani 0.25 1 d P . . H1 H 0.1430(13) 0.084(6) 0.158(3) 0.036(9) Uiso 1 1 d . . . H2 H 0.099(2) 0.098(10) 0.0000 0.056(17) Uiso 1 2 d S . . H2N H 0.3080(13) 0.080(6) 0.059(3) 0.036(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.0465(3) 0.0482(3) 0.0264(2) 0.00451(16) 0.000 0.000 O1 0.037(3) 0.070(4) 0.033(3) 0.007(3) -0.003(2) 0.000(3) O2 0.045(3) 0.069(4) 0.044(3) 0.020(3) 0.009(3) 0.007(3) N1 0.0344(13) 0.0300(12) 0.0229(13) 0.0004(11) 0.0012(10) 0.0011(10) N2 0.0320(19) 0.037(2) 0.0237(19) 0.000 0.000 0.0008(17) C1 0.0358(16) 0.0395(17) 0.0324(18) 0.0018(15) 0.0070(14) 0.0005(14) C2 0.026(2) 0.051(3) 0.044(3) 0.000 0.000 0.000(2) C3 0.037(2) 0.0198(19) 0.023(2) 0.000 0.000 0.0022(17) C4 0.033(2) 0.046(3) 0.034(3) -0.003(2) 0.000 0.000 C5 0.035(4) 0.118(8) 0.064(6) 0.028(6) 0.013(4) -0.006(5) O3 0.059(3) 0.060(3) 0.057(3) 0.006(3) 0.006(3) -0.001(3) O4 0.060(5) 0.070(5) 0.053(5) 0.000 0.000 -0.005(4) O5 0.120(17) 0.061(9) 0.061(8) 0.011(11) 0.004(6) 0.009(14) _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 Ag O1 2.239(5) 8_445 ? Ag O1 2.239(5) . ? Ag N1 2.254(2) . ? Ag N1 2.254(2) 8_445 ? Ag Ag 3.1446(5) 13_545 ? Ag Ag 3.1446(5) 13 ? O1 O2 0.989(6) 8_445 ? O1 C4 1.291(6) . ? O1 O1 1.662(10) 8_445 ? O2 O1 0.989(6) 8_445 ? O2 C4 1.192(5) . ? O2 C5 1.510(10) 8_445 ? N1 C1 1.337(4) . ? N1 C3 1.357(3) . ? N2 C3 1.329(6) . ? N2 H2N 0.87(4) . ? C1 C2 1.365(4) . ? C1 H1 0.95(4) . ? C2 C1 1.365(4) 10 ? C2 H2 0.83(6) . ? C3 N1 1.358(3) 10 ? C4 O2 1.192(5) 8_445 ? C4 O1 1.291(6) 8_445 ? C4 C5 1.535(8) 8_445 ? C4 C5 1.535(8) . ? C5 C5 1.494(19) 8_445 ? C5 O2 1.510(10) 8_445 ? O4 O4 1.780(18) 9_556 ? O5 O5 0.86(3) 2 ? O5 O5 0.92(3) 8_445 ? O5 O5 1.23(3) 7_445 ? 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 O1 Ag O1 43.6(3) 8_445 . ? O1 Ag N1 134.65(14) 8_445 . ? O1 Ag N1 96.43(14) . . ? O1 Ag N1 96.43(14) 8_445 8_445 ? O1 Ag N1 134.65(14) . 8_445 ? N1 Ag N1 127.95(12) . 8_445 ? O1 Ag Ag 77.92(15) 8_445 13_545 ? O1 Ag Ag 105.67(15) . 13_545 ? N1 Ag Ag 100.48(6) . 13_545 ? N1 Ag Ag 77.84(6) 8_445 13_545 ? O1 Ag Ag 105.67(15) 8_445 13 ? O1 Ag Ag 77.92(15) . 13 ? N1 Ag Ag 77.84(6) . 13 ? N1 Ag Ag 100.48(6) 8_445 13 ? Ag Ag Ag 176.25(3) 13_545 13 ? O2 O1 C4 61.4(4) 8_445 . ? O2 O1 O1 110.3(5) 8_445 8_445 ? C4 O1 O1 49.9(3) . 8_445 ? O2 O1 Ag 169.0(6) 8_445 . ? C4 O1 Ag 118.2(4) . . ? O1 O1 Ag 68.22(13) 8_445 . ? O1 O2 C4 71.9(5) 8_445 . ? O1 O2 C5 140.0(7) 8_445 8_445 ? C4 O2 C5 68.1(5) . 8_445 ? C1 N1 C3 116.7(3) . . ? C1 N1 Ag 117.8(2) . . ? C3 N1 Ag 124.6(2) . . ? C3 N2 H2N 120(2) . . ? N1 C1 C2 123.0(3) . . ? N1 C1 H1 115(2) . . ? C2 C1 H1 122(2) . . ? C1 C2 C1 116.9(4) . 10 ? C1 C2 H2 121.5(2) . . ? C1 C2 H2 121.5(2) 10 . ? N2 C3 N1 118.14(19) . 10 ? N2 C3 N1 118.14(19) . . ? N1 C3 N1 123.7(4) 10 . ? O2 C4 O2 172.3(7) 8_445 . ? O2 C4 O1 46.7(3) 8_445 . ? O2 C4 O1 125.6(6) . . ? O2 C4 O1 125.6(6) 8_445 8_445 ? O2 C4 O1 46.7(3) . 8_445 ? O1 C4 O1 80.1(6) . 8_445 ? O2 C4 C5 121.8(6) 8_445 8_445 ? O2 C4 C5 65.8(5) . 8_445 ? O1 C4 C5 162.4(5) . 8_445 ? O1 C4 C5 112.6(4) 8_445 8_445 ? O2 C4 C5 65.8(5) 8_445 . ? O2 C4 C5 121.8(6) . . ? O1 C4 C5 112.6(4) . . ? O1 C4 C5 162.4(5) 8_445 . ? C5 C4 C5 58.3(7) 8_445 . ? C5 C5 O2 105.3(5) 8_445 8_445 ? C5 C5 C4 60.9(4) 8_445 . ? O2 C5 C4 46.1(3) 8_445 . ? O5 O5 O5 87.2(15) 2 8_445 ? O5 O5 O5 48.6(18) 2 7_445 ? O5 O5 O5 44.2(13) 8_445 7_445 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.447 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.088 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 281180' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H9 Ag N4 O3' _chemical_formula_weight 293.04 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 7.9107(10) _cell_length_b 19.287(2) _cell_length_c 12.2767(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.902(8) _cell_angle_gamma 90.00 _cell_volume 1866.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.85 _cell_measurement_theta_max 12.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.086 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 2.148 _exptl_absorpt_correction_type \y-scan _exptl_absorpt_correction_T_min 0.8896 _exptl_absorpt_correction_T_max 0.9920 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4290 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3272 _reflns_number_gt 2799 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+3.5078P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3272 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0718 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.29901(5) 0.419956(15) 0.50449(3) 0.04869(11) Uani 1 1 d . . . Ag2 Ag 0.70922(5) 0.159454(17) 0.68635(3) 0.05542(12) Uani 1 1 d . . . O1 O 0.8599(5) 0.2584(2) 1.0093(3) 0.0735(10) Uani 1 1 d . . . O2 O 0.7942(6) 0.33460(17) 0.8873(3) 0.0802(12) Uani 1 1 d . . . O3 O 0.7012(5) 0.23114(16) 0.8642(3) 0.0657(9) Uani 1 1 d . . . O4 O 0.4896(6) 0.5286(2) 0.2360(3) 0.0896(13) Uani 1 1 d . . . O5 O 0.3671(6) 0.4393(2) 0.2941(4) 0.1038(16) Uani 1 1 d . . . O6 O 0.4121(5) 0.5276(2) 0.3956(3) 0.0781(11) Uani 1 1 d . . . N1 N 0.1402(4) 0.47861(15) 0.6207(2) 0.0345(7) Uani 1 1 d . . . N2 N 0.2571(5) 0.58404(16) 0.5790(3) 0.0489(9) Uani 1 1 d . . . H2NA H 0.2861 0.5634 0.5189 0.051(13) Uiso 1 1 d R . . H2NB H 0.2535 0.6294 0.5864 0.046(12) Uiso 1 1 d R . . N3 N 0.1308(4) 0.57611(15) 0.7407(2) 0.0345(7) Uani 1 1 d . . . N4 N 0.3580(4) 0.30445(15) 0.5053(2) 0.0357(7) Uani 1 1 d . . . N5 N 0.5288(5) 0.31205(17) 0.6664(3) 0.0515(9) Uani 1 1 d . . . H5NA H 0.5161 0.3568 0.6587 0.067(16) Uiso 1 1 d R . . H5NB H 0.5936 0.2915 0.7231 0.049(12) Uiso 1 1 d R . . N6 N 0.4980(4) 0.20469(15) 0.5845(2) 0.0345(7) Uani 1 1 d . . . N7 N 0.7897(5) 0.27480(16) 0.9204(3) 0.0428(8) Uani 1 1 d . . . N8 N 0.4219(5) 0.49816(18) 0.3057(3) 0.0444(8) Uani 1 1 d . . . C1 C 0.1749(5) 0.54548(18) 0.6476(3) 0.0326(8) Uani 1 1 d . . . C2 C 0.0325(5) 0.53961(19) 0.8035(3) 0.0375(8) Uani 1 1 d . . . C3 C -0.0254(7) 0.5760(2) 0.9015(4) 0.0557(12) Uani 1 1 d . . . H3A H -0.0955 0.5475 0.9328 0.060(15) Uiso 1 1 d R . . H3B H -0.0829 0.6182 0.8798 0.072 Uiso 1 1 d R . . H3C H 0.0703 0.5871 0.9518 0.072 Uiso 1 1 d R . . C4 C -0.0148(5) 0.4723(2) 0.7771(3) 0.0412(9) Uani 1 1 d . . . H4A H -0.0864 0.4477 0.8194 0.049 Uiso 1 1 calc R . . C5 C 0.0470(5) 0.44246(19) 0.6866(3) 0.0372(8) Uani 1 1 d . . . C6 C 0.0113(6) 0.3681(2) 0.6579(4) 0.0515(11) Uani 1 1 d . . . H6C H -0.0643 0.3500 0.7064 0.074(17) Uiso 1 1 d R . . H6B H -0.0413 0.3611 0.5918 0.09(2) Uiso 1 1 d R . . H6A H 0.1178 0.3431 0.6579 0.086(19) Uiso 1 1 d R . . C7 C 0.4618(5) 0.27363(18) 0.5837(3) 0.0344(8) Uani 1 1 d . . . C8 C 0.2819(5) 0.26387(19) 0.4261(3) 0.0390(9) Uani 1 1 d . . . C9 C 0.1696(7) 0.2983(2) 0.3388(4) 0.0597(13) Uani 1 1 d . . . H9A H 0.0931 0.3309 0.3794 0.14(3) Uiso 1 1 d R . . H9B H 0.0992 0.2634 0.2962 0.10(2) Uiso 1 1 d R . . H9C H 0.2360 0.3245 0.2913 0.116 Uiso 1 1 d R . . C10 C 0.3104(6) 0.19344(19) 0.4259(3) 0.0421(9) Uani 1 1 d . . . H10A H 0.2547 0.1655 0.3725 0.050 Uiso 1 1 calc R . . C11 C 0.4215(5) 0.16509(18) 0.5051(3) 0.0349(8) Uani 1 1 d . . . C12 C 0.4641(6) 0.08934(19) 0.5057(4) 0.0471(10) Uani 1 1 d . . . H12A H 0.4439 0.0683 0.5825 0.077(17) Uiso 1 1 d R . . H12B H 0.4005 0.0614 0.4585 0.064(15) Uiso 1 1 d R . . H12C H 0.5815 0.0839 0.4933 0.077 Uiso 1 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 0.0696(2) 0.02783(16) 0.04876(19) -0.00387(13) 0.00588(16) 0.00916(14) Ag2 0.0718(2) 0.03966(18) 0.0521(2) 0.00466(14) -0.01072(17) 0.01926(16) O1 0.086(3) 0.073(2) 0.058(2) 0.0089(18) -0.0122(19) 0.016(2) O2 0.116(3) 0.0412(19) 0.081(3) 0.0201(17) -0.002(2) -0.019(2) O3 0.091(3) 0.0377(16) 0.067(2) -0.0172(15) -0.0035(19) -0.0006(17) O4 0.109(3) 0.107(3) 0.056(2) 0.026(2) 0.025(2) -0.002(3) O5 0.113(4) 0.043(2) 0.147(4) 0.003(2) -0.039(3) -0.022(2) O6 0.077(3) 0.110(3) 0.0477(19) -0.026(2) 0.0124(17) 0.008(2) N1 0.0420(18) 0.0247(15) 0.0364(16) -0.0023(12) 0.0007(14) 0.0018(13) N2 0.072(3) 0.0240(16) 0.054(2) -0.0046(15) 0.0224(19) 0.0013(16) N3 0.0405(17) 0.0259(15) 0.0361(16) -0.0026(12) -0.0019(13) 0.0015(13) N4 0.0460(18) 0.0220(14) 0.0392(16) -0.0005(12) 0.0038(14) 0.0060(13) N5 0.079(3) 0.0296(18) 0.0421(19) -0.0042(15) -0.0145(18) 0.0082(18) N6 0.0445(18) 0.0254(15) 0.0337(15) 0.0020(12) 0.0049(14) 0.0066(13) N7 0.055(2) 0.0320(17) 0.0430(19) 0.0001(15) 0.0107(16) 0.0038(16) N8 0.056(2) 0.0373(18) 0.0386(18) 0.0014(15) -0.0013(16) -0.0004(16) C1 0.035(2) 0.0244(17) 0.0380(19) 0.0000(14) 0.0001(16) 0.0033(15) C2 0.043(2) 0.0343(19) 0.0342(19) -0.0032(16) -0.0025(17) 0.0012(17) C3 0.074(3) 0.049(3) 0.046(2) -0.008(2) 0.017(2) -0.006(2) C4 0.047(2) 0.038(2) 0.039(2) -0.0003(16) 0.0075(18) -0.0090(18) C5 0.040(2) 0.0283(18) 0.041(2) -0.0022(16) -0.0055(17) -0.0021(16) C6 0.068(3) 0.030(2) 0.056(3) -0.0062(18) 0.003(2) -0.011(2) C7 0.044(2) 0.0276(18) 0.0322(18) 0.0004(14) 0.0047(16) 0.0028(16) C8 0.046(2) 0.0307(19) 0.040(2) 0.0011(16) 0.0000(17) -0.0007(17) C9 0.072(3) 0.040(2) 0.062(3) 0.007(2) -0.023(3) -0.003(2) C10 0.057(3) 0.0288(19) 0.039(2) -0.0002(16) -0.0029(18) -0.0035(18) C11 0.046(2) 0.0226(17) 0.0369(19) 0.0014(14) 0.0106(17) 0.0017(16) C12 0.068(3) 0.0228(19) 0.051(2) -0.0041(17) 0.007(2) 0.0055(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.276(3) . ? Ag1 N1 2.280(3) . ? Ag1 O5 2.709(6) . ? Ag1 O6 2.666(4) . ? Ag2 N6 2.182(3) . ? Ag2 N3 2.189(3) 2_646 ? Ag2 O3 2.590(3) . ? O1 N7 1.223(5) . ? O2 N7 1.225(5) . ? O3 N7 1.262(5) . ? O4 N8 1.200(5) . ? O5 N8 1.219(5) . ? O6 N8 1.249(5) . ? N1 C5 1.337(5) . ? N1 C1 1.354(5) . ? N2 C1 1.334(5) . ? N2 H2NA 0.8854 . ? N2 H2NB 0.8805 . ? N3 C2 1.341(5) . ? N3 C1 1.358(5) . ? N3 Ag2 2.190(3) 2_656 ? N4 C7 1.349(5) . ? N4 C8 1.349(5) . ? N5 C7 1.331(5) . ? N5 H5NA 0.8723 . ? N5 H5NB 0.9178 . ? N6 C11 1.341(5) . ? N6 C7 1.360(5) . ? C2 C4 1.383(5) . ? C2 C3 1.497(5) . ? C3 H3A 0.8903 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.377(6) . ? C4 H4A 0.9300 . ? C5 C6 1.498(5) . ? C6 H6C 0.9455 . ? C6 H6B 0.8900 . ? C6 H6A 0.9701 . ? C8 C10 1.377(5) . ? C8 C9 1.489(6) . ? C9 H9A 1.0300 . ? C9 H9B 0.9936 . ? C9 H9C 0.9600 . ? C10 C11 1.368(5) . ? C10 H10A 0.9300 . ? C11 C12 1.499(5) . ? C12 H12A 1.0513 . ? C12 H12B 0.9098 . ? C12 H12C 0.9599 . ? 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 N4 Ag1 N1 127.35(11) . . ? N1 Ag1 O5 133.88(12) . . ? N1 Ag1 O6 98.85(11) . . ? N4 Ag1 O5 94.67(12) . . ? N4 Ag1 O6 133.40(11) . . ? O5 Ag1 O6 46.51(10) . . ? N6 Ag2 N3 156.30(11) . 2_646 ? N6 Ag2 O3 101.36(11) . . ? N3 Ag2 O3 95.85(11) 2_646 . ? N7 O3 Ag2 139.9(3) . . ? C5 N1 C1 117.4(3) . . ? C5 N1 Ag1 118.8(2) . . ? C1 N1 Ag1 121.0(3) . . ? C1 N2 H2NA 116.8 . . ? C1 N2 H2NB 117.8 . . ? H2NA N2 H2NB 123.1 . . ? C2 N3 C1 117.3(3) . . ? C2 N3 Ag2 119.6(2) . 2_656 ? C1 N3 Ag2 118.9(2) . 2_656 ? C7 N4 C8 117.7(3) . . ? C7 N4 Ag1 123.1(2) . . ? C8 N4 Ag1 119.1(2) . . ? C7 N5 H5NA 115.6 . . ? C7 N5 H5NB 119.9 . . ? H5NA N5 H5NB 124.1 . . ? C11 N6 C7 118.0(3) . . ? C11 N6 Ag2 117.7(2) . . ? C7 N6 Ag2 123.1(3) . . ? O1 N7 O2 121.1(4) . . ? O1 N7 O3 120.3(4) . . ? O2 N7 O3 118.5(4) . . ? O4 N8 O5 123.2(5) . . ? O4 N8 O6 118.2(4) . . ? O5 N8 O6 118.6(5) . . ? N2 C1 N1 118.5(3) . . ? N2 C1 N3 117.6(3) . . ? N1 C1 N3 124.0(3) . . ? N3 C2 C4 121.1(4) . . ? N3 C2 C3 116.7(3) . . ? C4 C2 C3 122.2(4) . . ? C2 C3 H3A 107.7 . . ? C2 C3 H3B 110.2 . . ? H3A C3 H3B 110.2 . . ? C2 C3 H3C 110.1 . . ? H3A C3 H3C 110.2 . . ? H3B C3 H3C 108.5 . . ? C5 C4 C2 118.3(4) . . ? C5 C4 H4A 120.9 . . ? C2 C4 H4A 120.9 . . ? N1 C5 C4 121.5(3) . . ? N1 C5 C6 117.4(4) . . ? C4 C5 C6 121.1(4) . . ? C5 C6 H6C 108.7 . . ? C5 C6 H6B 115.0 . . ? H6C C6 H6B 104.3 . . ? C5 C6 H6A 109.2 . . ? H6C C6 H6A 114.4 . . ? H6B C6 H6A 105.3 . . ? N5 C7 N4 118.6(3) . . ? N5 C7 N6 117.9(3) . . ? N4 C7 N6 123.5(3) . . ? N4 C8 C10 120.7(4) . . ? N4 C8 C9 117.5(3) . . ? C10 C8 C9 121.8(4) . . ? C8 C9 H9A 105.3 . . ? C8 C9 H9B 110.5 . . ? H9A C9 H9B 110.0 . . ? C8 C9 H9C 110.3 . . ? H9A C9 H9C 110.3 . . ? H9B C9 H9C 110.3 . . ? C11 C10 C8 119.2(4) . . ? C11 C10 H10A 120.4 . . ? C8 C10 H10A 120.4 . . ? N6 C11 C10 120.8(3) . . ? N6 C11 C12 117.7(3) . . ? C10 C11 C12 121.5(4) . . ? C11 C12 H12A 109.2 . . ? C11 C12 H12B 117.5 . . ? H12A C12 H12B 103.0 . . ? C11 C12 H12C 109.1 . . ? H12A C12 H12C 108.8 . . ? H12B C12 H12C 108.8 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.412 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.089 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 281181' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H11 Ag Cl N3 O5' _chemical_formula_weight 348.50 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.6708(6) _cell_length_b 14.3064(17) _cell_length_c 11.1349(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.022(6) _cell_angle_gamma 90.00 _cell_volume 1195.16(19) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.07 _cell_measurement_theta_max 12.47 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.937 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 1.919 _exptl_absorpt_correction_type \y-scan _exptl_absorpt_correction_T_min 0.7353 _exptl_absorpt_correction_T_max 0.9897 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2815 _diffrn_reflns_av_R_equivalents 0.0148 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2091 _reflns_number_gt 1839 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+3.9005P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0080(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2091 _refine_ls_number_parameters 179 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0852 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.05732(6) 0.78002(3) 0.13041(3) 0.06127(19) Uani 1 1 d . . . N1 N 0.2521(5) 0.8380(2) 0.2830(3) 0.0410(8) Uani 1 1 d . . . N2 N 0.2053(6) 0.7189(3) 0.4112(4) 0.0600(11) Uani 1 1 d . . . H2A H 0.0995 0.7204 0.3710 0.073(18) Uiso 1 1 d R . . H2B H 0.2272 0.6870 0.4782 0.050(14) Uiso 1 1 d R . . N3 N 0.4603(5) 0.8065(3) 0.4697(3) 0.0411(8) Uani 1 1 d . . . C1 C 0.3067(6) 0.7895(3) 0.3882(4) 0.0397(9) Uani 1 1 d . . . C2 C 0.5611(6) 0.8779(3) 0.4462(4) 0.0451(10) Uani 1 1 d . . . C3 C 0.7368(7) 0.8929(4) 0.5322(5) 0.0692(15) Uani 1 1 d . . . H3A H 0.7206 0.8914 0.6154 0.104 Uiso 1 1 calc R . . H3B H 0.7844 0.9526 0.5160 0.104 Uiso 1 1 calc R . . H3C H 0.8181 0.8444 0.5205 0.104 Uiso 1 1 calc R . . C4 C 0.5059(6) 0.9335(3) 0.3448(4) 0.0512(11) Uani 1 1 d . . . H4A H 0.5723 0.9854 0.3318 0.061 Uiso 1 1 calc R . . C5 C 0.3512(6) 0.9113(3) 0.2628(4) 0.0471(10) Uani 1 1 d . . . C6 C 0.2869(9) 0.9663(4) 0.1484(5) 0.0755(17) Uani 1 1 d . . . H6A H 0.1591 0.9691 0.1314 0.113 Uiso 1 1 calc R . . H6B H 0.3255 0.9366 0.0811 0.113 Uiso 1 1 calc R . . H6C H 0.3347 1.0284 0.1591 0.113 Uiso 1 1 calc R . . Cl Cl 0.69504(18) 0.64977(10) 0.26805(15) 0.0680(4) Uani 1 1 d D . . O1 O 0.5838(8) 0.7247(4) 0.2220(6) 0.1142(18) Uani 1 1 d . A . O2 O 0.8674(6) 0.6487(6) 0.2447(10) 0.082(3) Uani 0.50 1 d PD A 1 O3 O 0.760(4) 0.642(2) 0.3948(5) 0.279(17) Uani 0.50 1 d PD A 1 O4 O 0.6151(15) 0.5624(4) 0.240(2) 0.152(8) Uani 0.50 1 d PD A 1 O2' O 0.704(3) 0.6128(11) 0.1532(6) 0.189(9) Uani 0.50 1 d PD A 2 O3' O 0.810(2) 0.7064(16) 0.352(2) 0.263(15) Uani 0.50 1 d PD A 2 O4' O 0.588(2) 0.6024(13) 0.3357(16) 0.156(7) Uani 0.50 1 d PD A 2 O5 O -0.2151(6) 0.8879(3) 0.1421(4) 0.0757(11) Uani 1 1 d . B 2 H5O1 H -0.2222 0.9522 0.1619 0.16(4) Uiso 1 1 d R . . H5O2 H -0.2787 0.8406 0.1749 0.14(4) Uiso 1 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 Ag 0.0633(3) 0.0641(3) 0.0451(2) -0.00541(18) -0.01476(17) -0.00491(19) N1 0.0399(19) 0.0417(19) 0.0364(18) -0.0015(15) -0.0032(15) 0.0042(16) N2 0.052(3) 0.065(3) 0.055(2) 0.016(2) -0.007(2) -0.016(2) N3 0.0379(19) 0.046(2) 0.0354(18) -0.0031(15) -0.0014(15) 0.0020(16) C1 0.039(2) 0.039(2) 0.038(2) -0.0031(18) 0.0022(17) 0.0003(18) C2 0.037(2) 0.048(3) 0.047(2) -0.009(2) 0.0005(19) 0.0007(19) C3 0.047(3) 0.073(4) 0.077(4) -0.010(3) -0.009(3) -0.009(3) C4 0.051(3) 0.045(3) 0.055(3) -0.003(2) 0.007(2) -0.008(2) C5 0.056(3) 0.041(2) 0.042(2) 0.0010(19) 0.007(2) 0.004(2) C6 0.088(4) 0.068(4) 0.061(3) 0.021(3) -0.005(3) -0.005(3) Cl 0.0543(7) 0.0582(8) 0.0942(11) 0.0100(7) 0.0217(7) 0.0060(6) O1 0.119(4) 0.086(4) 0.133(5) 0.000(3) 0.015(4) 0.035(3) O2 0.039(4) 0.063(5) 0.144(9) -0.005(5) 0.022(5) -0.003(4) O3 0.27(3) 0.38(4) 0.146(16) 0.17(2) -0.046(17) -0.05(3) O4 0.062(6) 0.049(6) 0.32(2) 0.037(10) -0.016(10) -0.003(5) O2' 0.29(2) 0.158(14) 0.158(13) 0.036(11) 0.144(16) 0.122(16) O3' 0.084(10) 0.23(2) 0.43(4) -0.13(2) -0.062(18) -0.031(13) O4' 0.141(14) 0.154(14) 0.183(17) 0.034(12) 0.060(12) -0.059(12) O5 0.078(3) 0.069(3) 0.083(3) -0.016(2) 0.022(2) 0.008(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 Ag N3 2.175(3) 4_575 ? Ag N1 2.179(3) . ? Ag O5 2.623(4) . ? N1 C5 1.341(6) . ? N1 C1 1.351(5) . ? N2 C1 1.332(6) . ? N2 H2A 0.8413 . ? N2 H2B 0.8613 . ? N3 C2 1.339(6) . ? N3 C1 1.352(5) . ? N3 Ag 2.175(3) 4_676 ? C2 C4 1.373(6) . ? C2 C3 1.497(6) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.375(6) . ? C4 H4A 0.9300 . ? C5 C6 1.490(6) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? Cl O4' 1.3992(10) . ? Cl O1 1.399(5) . ? Cl O4 1.3995(11) . ? Cl O3 1.3997(10) . ? Cl O3' 1.3998(11) . ? Cl O2 1.3999(10) . ? Cl O2' 1.4002(10) . ? O5 H5O1 0.9500 . ? O5 H5O2 0.9500 . ? 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 Ag N1 156.81(14) 4_575 . ? C5 N1 C1 117.6(4) . . ? C5 N1 Ag 119.2(3) . . ? C1 N1 Ag 121.2(3) . . ? C1 N2 H2A 114.6 . . ? C1 N2 H2B 123.5 . . ? H2A N2 H2B 117.8 . . ? C2 N3 C1 117.6(4) . . ? C2 N3 Ag 118.8(3) . 4_676 ? C1 N3 Ag 123.4(3) . 4_676 ? N2 C1 N1 117.9(4) . . ? N2 C1 N3 118.0(4) . . ? N1 C1 N3 124.0(4) . . ? N3 C2 C4 120.7(4) . . ? N3 C2 C3 117.6(4) . . ? C4 C2 C3 121.7(5) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C5 119.3(4) . . ? C2 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? N1 C5 C4 120.6(4) . . ? N1 C5 C6 117.2(4) . . ? C4 C5 C6 122.2(5) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O4' Cl O1 100.7(9) . . ? O4' Cl O4 53.9(9) . . ? O1 Cl O4 113.4(5) . . ? O4' Cl O3 63.1(12) . . ? O1 Cl O3 119.3(13) . . ? O4 Cl O3 102.1(13) . . ? O4' Cl O3' 106.4(15) . . ? O1 Cl O3' 93.0(10) . . ? O4 Cl O3' 148.6(14) . . ? O3 Cl O3' 47.9(14) . . ? O4' Cl O2 141.1(9) . . ? O1 Cl O2 117.9(5) . . ? O4 Cl O2 109.5(8) . . ? O3 Cl O2 91.9(14) . . ? O3' Cl O2 68.9(10) . . ? O4' Cl O2' 117.2(11) . . ? O1 Cl O2' 95.7(6) . . ? O4 Cl O2' 63.8(10) . . ? O3 Cl O2' 144.8(15) . . ? O3' Cl O2' 132.9(14) . . ? O2 Cl O2' 66.1(8) . . ? H5O1 O5 H5O2 122.7 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.633 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.084 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 281182' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H26 Ag4 N6 O12 S2' _chemical_formula_weight 941.99 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 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 10.727(2) _cell_length_b 17.216(2) _cell_length_c 13.462(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.64(2) _cell_angle_gamma 90.00 _cell_volume 2485.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 4.97 _cell_measurement_theta_max 12.52 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 3.343 _exptl_absorpt_correction_type \y-scan _exptl_absorpt_correction_T_min 0.7157 _exptl_absorpt_correction_T_max 0.9966 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5420 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4327 _reflns_number_gt 3318 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+49.8382P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4327 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1291 _refine_ls_wR_factor_gt 0.1203 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.19416(8) -0.10051(5) 1.30540(10) 0.0581(3) Uani 1 1 d . . . Ag2 Ag 0.85497(7) 0.03937(4) 1.13075(7) 0.0381(2) Uani 1 1 d . . . Ag3 Ag 0.94575(8) 0.12648(5) 0.92611(7) 0.0429(2) Uani 1 1 d . . . Ag4 Ag 0.41350(8) 0.28875(5) 0.87634(8) 0.0441(2) Uani 1 1 d . . . S1 S 0.8692(2) -0.09923(14) 1.30212(19) 0.0277(5) Uani 1 1 d . . . S2 S 1.1646(2) 0.05654(13) 1.09123(19) 0.0255(5) Uani 1 1 d . . . O1 O 0.9781(6) -0.1307(4) 1.2481(6) 0.0368(17) Uani 1 1 d . . . O2 O 0.7813(7) -0.0624(4) 1.2299(6) 0.0440(19) Uani 1 1 d . . . O3 O 0.9121(7) -0.0429(4) 1.3770(6) 0.0425(19) Uani 1 1 d . . . O4 O 0.8054(7) -0.1640(4) 1.3499(6) 0.0413(19) Uani 1 1 d . . . O5 O 1.1354(7) 0.0203(4) 1.3511(6) 0.0383(18) Uani 1 1 d . . . O6 O 1.2095(7) -0.0228(4) 1.1138(7) 0.046(2) Uani 1 1 d . . . O7 O 1.1089(7) 0.0578(4) 0.9909(5) 0.0395(18) Uani 1 1 d . . . O8 O 1.2667(6) 0.1128(4) 1.0963(6) 0.0405(19) Uani 1 1 d . . . O9 O 1.0693(6) 0.0787(4) 1.1634(5) 0.0328(16) Uani 1 1 d . . . O10 O 0.3617(7) 0.1480(4) 0.9082(6) 0.0410(18) Uani 1 1 d . . . O11 O 0.3037(7) 0.3850(5) 0.9742(6) 0.0435(19) Uani 1 1 d . . . O12 O 0.2504(7) 0.2909(4) 0.7625(6) 0.0406(18) Uani 1 1 d . . . N1 N 1.2794(7) -0.2157(4) 1.3286(6) 0.0251(17) Uani 1 1 d . . . N2 N 1.0854(7) -0.2754(5) 1.3199(6) 0.0303(19) Uani 1 1 d . . . H2A H 1.0440 -0.2335 1.3154 0.036 Uiso 1 1 d R . . H2B H 1.0358 -0.3192 1.3109 0.036 Uiso 1 1 d R . . N3 N 1.2586(7) -0.3531(4) 1.3508(5) 0.0225(17) Uani 1 1 d . . . N4 N 0.8190(7) 0.2308(4) 0.9237(6) 0.0265(18) Uani 1 1 d . . . N5 N 0.6379(7) 0.1601(4) 0.9045(6) 0.0275(18) Uani 1 1 d . . . H5A H 0.6820 0.1231 0.9375 0.033 Uiso 1 1 d R . . H5B H 0.5619 0.1655 0.9218 0.033 Uiso 1 1 d R . . N6 N 0.6207(7) 0.2938(4) 0.9025(6) 0.0285(18) Uani 1 1 d . . . C1 C 1.4014(9) -0.2208(6) 1.3408(7) 0.030(2) Uani 1 1 d . . . C2 C 1.4774(9) -0.1476(6) 1.3371(8) 0.037(2) Uani 1 1 d . . . H2C H 1.4298 -0.1077 1.3036 0.055 Uiso 1 1 calc R . . H2D H 1.5523 -0.1573 1.3018 0.055 Uiso 1 1 calc R . . H2E H 1.4986 -0.1310 1.4035 0.055 Uiso 1 1 calc R . . C3 C 1.4573(9) -0.2931(6) 1.3574(7) 0.030(2) Uani 1 1 d . . . H3C H 1.5436 -0.2974 1.3640 0.036 Uiso 1 1 calc R . . C4 C 1.3835(9) -0.3578(6) 1.3639(8) 0.030(2) Uani 1 1 d . . . C5 C 1.4361(10) -0.4374(6) 1.3832(10) 0.044(3) Uani 1 1 d . . . H5D H 1.4135 -0.4711 1.3288 0.066 Uiso 1 1 calc R . . H5E H 1.4032 -0.4577 1.4434 0.066 Uiso 1 1 calc R . . H5F H 1.5254 -0.4342 1.3897 0.066 Uiso 1 1 calc R . . C6 C 1.2090(9) -0.2814(5) 1.3333(7) 0.025(2) Uani 1 1 d . . . C7 C 0.8750(10) 0.3005(6) 0.9319(8) 0.035(2) Uani 1 1 d . . . C8 C 1.0155(10) 0.3011(7) 0.9431(10) 0.050(3) Uani 1 1 d . . . H8B H 1.0410 0.2676 0.9969 0.076 Uiso 1 1 calc R . . H8C H 1.0436 0.3530 0.9567 0.076 Uiso 1 1 calc R . . H8D H 1.0511 0.2830 0.8827 0.076 Uiso 1 1 calc R . . C9 C 0.8058(10) 0.3679(6) 0.9272(8) 0.036(2) Uani 1 1 d . . . H9A H 0.8441 0.4159 0.9360 0.044 Uiso 1 1 calc R . . C10 C 0.6798(10) 0.3630(6) 0.9095(8) 0.033(2) Uani 1 1 d . . . C11 C 0.6033(12) 0.4351(6) 0.9003(10) 0.052(3) Uani 1 1 d . . . H11B H 0.5340 0.4261 0.8551 0.078 Uiso 1 1 calc R . . H11C H 0.6537 0.4765 0.8755 0.078 Uiso 1 1 calc R . . H11D H 0.5731 0.4491 0.9643 0.078 Uiso 1 1 calc R . . C12 C 0.6941(8) 0.2295(5) 0.9105(7) 0.0212(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0351(5) 0.0253(4) 0.1138(9) -0.0062(5) 0.0032(5) 0.0022(4) Ag2 0.0299(4) 0.0253(4) 0.0596(6) -0.0035(4) 0.0070(4) 0.0012(3) Ag3 0.0310(4) 0.0369(5) 0.0609(6) 0.0037(4) 0.0035(4) 0.0076(4) Ag4 0.0295(4) 0.0357(5) 0.0670(6) -0.0013(4) -0.0014(4) 0.0046(3) S1 0.0241(12) 0.0222(11) 0.0371(14) 0.0003(10) 0.0072(10) 0.0005(9) S2 0.0168(11) 0.0189(11) 0.0409(15) -0.0031(10) 0.0036(10) 0.0017(9) O1 0.029(4) 0.037(4) 0.045(4) -0.009(3) 0.007(3) 0.004(3) O2 0.032(4) 0.043(4) 0.057(5) 0.013(4) -0.001(4) 0.004(3) O3 0.042(4) 0.038(4) 0.049(5) -0.014(4) 0.009(4) -0.009(3) O4 0.049(5) 0.030(4) 0.046(5) 0.008(3) 0.011(4) -0.014(3) O5 0.042(4) 0.029(4) 0.045(5) -0.005(3) 0.008(4) 0.001(3) O6 0.043(4) 0.024(4) 0.073(6) -0.001(4) 0.009(4) 0.012(3) O7 0.033(4) 0.047(5) 0.038(4) -0.005(4) -0.002(3) 0.008(3) O8 0.029(4) 0.037(4) 0.056(5) -0.013(4) 0.014(3) -0.016(3) O9 0.025(4) 0.032(4) 0.041(4) -0.005(3) 0.010(3) 0.000(3) O10 0.035(4) 0.043(4) 0.045(5) 0.009(4) -0.005(3) -0.013(3) O11 0.031(4) 0.049(5) 0.050(5) -0.010(4) 0.002(3) 0.002(3) O12 0.040(4) 0.040(4) 0.041(5) 0.005(4) -0.003(3) 0.002(3) N1 0.020(4) 0.022(4) 0.034(5) -0.002(3) 0.005(3) 0.001(3) N2 0.023(4) 0.025(4) 0.043(5) -0.002(4) -0.004(4) -0.002(3) N3 0.017(4) 0.031(4) 0.020(4) 0.002(3) 0.004(3) 0.000(3) N4 0.017(4) 0.026(4) 0.038(5) 0.006(4) 0.010(3) -0.002(3) N5 0.025(4) 0.017(4) 0.041(5) 0.004(4) 0.004(4) 0.003(3) N6 0.022(4) 0.022(4) 0.041(5) 0.000(4) 0.009(4) 0.001(3) C1 0.032(6) 0.030(5) 0.028(5) -0.002(4) 0.004(4) -0.007(4) C2 0.029(5) 0.038(6) 0.042(7) 0.001(5) -0.002(5) -0.012(5) C3 0.017(5) 0.040(6) 0.033(6) 0.003(5) 0.003(4) 0.003(4) C4 0.026(5) 0.027(5) 0.038(6) -0.002(4) 0.004(4) 0.005(4) C5 0.027(6) 0.035(6) 0.070(8) 0.004(6) 0.006(5) 0.005(5) C6 0.025(5) 0.026(5) 0.025(5) -0.001(4) 0.008(4) 0.001(4) C7 0.038(6) 0.035(6) 0.033(6) 0.001(5) 0.008(5) -0.007(5) C8 0.032(6) 0.045(7) 0.074(9) 0.006(6) 0.000(6) -0.010(5) C9 0.035(6) 0.023(5) 0.052(7) -0.004(5) 0.002(5) -0.012(4) C10 0.037(6) 0.022(5) 0.042(6) 0.000(4) 0.014(5) 0.004(4) C11 0.056(8) 0.025(5) 0.077(9) 0.004(6) 0.032(7) 0.002(5) C12 0.023(5) 0.022(5) 0.018(5) -0.001(4) 0.000(4) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.202(7) . ? Ag1 O5 2.264(7) . ? Ag1 O1 2.476(7) . ? Ag2 N3 2.233(7) 2_757 ? Ag2 O2 2.353(8) . ? Ag2 O7 2.381(7) 3_757 ? Ag2 O9 2.425(7) . ? Ag2 Ag3 3.3077(14) . ? Ag3 N4 2.252(8) . ? Ag3 O7 2.265(7) . ? Ag3 O6 2.489(8) 3_757 ? Ag3 O1 2.506(7) 3_757 ? Ag4 N6 2.242(8) . ? Ag4 O12 2.293(7) . ? Ag4 O11 2.441(7) . ? Ag4 O10 2.525(7) . ? S1 O3 1.463(8) . ? S1 O4 1.466(7) . ? S1 O2 1.478(8) . ? S1 O1 1.496(7) . ? S2 O7 1.462(8) . ? S2 O8 1.462(7) . ? S2 O6 1.478(7) . ? S2 O9 1.480(7) . ? O1 Ag3 2.506(7) 3_757 ? O6 Ag3 2.489(8) 3_757 ? O7 Ag2 2.381(7) 3_757 ? N1 C1 1.317(12) . ? N1 C6 1.364(12) . ? N2 C6 1.337(12) . ? N2 H2A 0.8484 . ? N2 H2B 0.9288 . ? N3 C4 1.349(12) . ? N3 C6 1.362(12) . ? N3 Ag2 2.233(7) 2_747 ? N4 C7 1.344(13) . ? N4 C12 1.347(12) . ? N5 C12 1.340(11) . ? N5 H5A 0.9027 . ? N5 H5B 0.8593 . ? N6 C10 1.351(13) . ? N6 C12 1.360(12) . ? C1 C3 1.398(14) . ? C1 C2 1.502(13) . ? C2 H2C 0.9600 . ? C2 H2D 0.9600 . ? C2 H2E 0.9600 . ? C3 C4 1.370(14) . ? C3 H3C 0.9300 . ? C4 C5 1.502(14) . ? C5 H5D 0.9600 . ? C5 H5E 0.9600 . ? C5 H5F 0.9600 . ? C7 C9 1.378(15) . ? C7 C8 1.510(15) . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C8 H8D 0.9600 . ? C9 C10 1.368(15) . ? C9 H9A 0.9300 . ? C10 C11 1.492(14) . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C11 H11D 0.9600 . ? 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 O5 155.0(3) . . ? N1 Ag1 O1 103.7(3) . . ? O5 Ag1 O1 90.7(2) . . ? N3 Ag2 O2 111.2(3) 2_757 . ? N3 Ag2 O7 139.4(3) 2_757 3_757 ? O2 Ag2 O7 86.0(3) . 3_757 ? N3 Ag2 O9 105.4(2) 2_757 . ? O2 Ag2 O9 115.9(2) . . ? O7 Ag2 O9 98.6(2) 3_757 . ? N3 Ag2 Ag3 83.77(19) 2_757 . ? O2 Ag2 Ag3 157.2(2) . . ? O7 Ag2 Ag3 71.84(19) 3_757 . ? O9 Ag2 Ag3 73.98(17) . . ? N4 Ag3 O7 151.7(3) . . ? N4 Ag3 O6 99.7(3) . 3_757 ? O7 Ag3 O6 102.4(3) . 3_757 ? N4 Ag3 O1 100.1(3) . 3_757 ? O7 Ag3 O1 96.1(2) . 3_757 ? O6 Ag3 O1 93.0(3) 3_757 3_757 ? N4 Ag3 Ag2 100.5(2) . . ? O7 Ag3 Ag2 71.68(19) . . ? O6 Ag3 Ag2 69.1(2) 3_757 . ? O1 Ag3 Ag2 154.69(17) 3_757 . ? N6 Ag4 O12 147.0(3) . . ? N6 Ag4 O11 112.3(3) . . ? O12 Ag4 O11 88.8(3) . . ? N6 Ag4 O10 103.5(3) . . ? O12 Ag4 O10 87.8(3) . . ? O11 Ag4 O10 116.6(3) . . ? O3 S1 O4 110.1(5) . . ? O3 S1 O2 110.6(5) . . ? O4 S1 O2 108.6(5) . . ? O3 S1 O1 109.9(4) . . ? O4 S1 O1 108.6(4) . . ? O2 S1 O1 109.1(5) . . ? O7 S2 O8 108.6(5) . . ? O7 S2 O6 109.1(5) . . ? O8 S2 O6 111.3(5) . . ? O7 S2 O9 109.3(4) . . ? O8 S2 O9 109.2(4) . . ? O6 S2 O9 109.3(4) . . ? S1 O1 Ag1 120.6(4) . . ? S1 O1 Ag3 136.5(4) . 3_757 ? Ag1 O1 Ag3 87.6(2) . 3_757 ? S1 O2 Ag2 118.3(4) . . ? S2 O6 Ag3 114.0(4) . 3_757 ? S2 O7 Ag3 130.9(4) . . ? S2 O7 Ag2 123.7(4) . 3_757 ? Ag3 O7 Ag2 104.0(3) . 3_757 ? S2 O9 Ag2 118.6(4) . . ? C1 N1 C6 119.3(8) . . ? C1 N1 Ag1 119.0(6) . . ? C6 N1 Ag1 121.7(6) . . ? C6 N2 H2A 126.2 . . ? C6 N2 H2B 121.1 . . ? H2A N2 H2B 112.6 . . ? C4 N3 C6 117.2(8) . . ? C4 N3 Ag2 118.6(6) . 2_747 ? C6 N3 Ag2 124.0(6) . 2_747 ? C7 N4 C12 117.8(8) . . ? C7 N4 Ag3 116.2(6) . . ? C12 N4 Ag3 125.9(6) . . ? C12 N5 H5A 111.8 . . ? C12 N5 H5B 108.4 . . ? H5A N5 H5B 115.5 . . ? C10 N6 C12 116.3(8) . . ? C10 N6 Ag4 120.4(6) . . ? C12 N6 Ag4 123.3(6) . . ? N1 C1 C3 119.9(9) . . ? N1 C1 C2 118.6(9) . . ? C3 C1 C2 121.5(9) . . ? C1 C2 H2C 109.5 . . ? C1 C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? C1 C2 H2E 109.5 . . ? H2C C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? C4 C3 C1 119.2(9) . . ? C4 C3 H3C 120.4 . . ? C1 C3 H3C 120.4 . . ? N3 C4 C3 121.2(9) . . ? N3 C4 C5 116.3(9) . . ? C3 C4 C5 122.5(9) . . ? C4 C5 H5D 109.5 . . ? C4 C5 H5E 109.5 . . ? H5D C5 H5E 109.5 . . ? C4 C5 H5F 109.5 . . ? H5D C5 H5F 109.5 . . ? H5E C5 H5F 109.5 . . ? N2 C6 N3 118.3(8) . . ? N2 C6 N1 118.6(8) . . ? N3 C6 N1 123.1(8) . . ? N4 C7 C9 120.6(9) . . ? N4 C7 C8 117.2(9) . . ? C9 C7 C8 122.2(10) . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C8 H8D 109.5 . . ? H8B C8 H8D 109.5 . . ? H8C C8 H8D 109.5 . . ? C10 C9 C7 118.9(9) . . ? C10 C9 H9A 120.5 . . ? C7 C9 H9A 120.5 . . ? N6 C10 C9 121.7(9) . . ? N6 C10 C11 118.2(9) . . ? C9 C10 C11 120.1(10) . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C11 H11D 109.5 . . ? H11B C11 H11D 109.5 . . ? H11C C11 H11D 109.5 . . ? N5 C12 N4 117.8(8) . . ? N5 C12 N6 117.6(8) . . ? N4 C12 N6 124.6(8) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.375 _refine_diff_density_min -1.483 _refine_diff_density_rms 0.203 #===END