Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Muthu, Sabestian' ; Department of Chemistry National University of Singapore Singapore 173543 ; 'Vittal, Jagadese J.' ; Department of Chemistry National University of Singapore SINGAPORE 117543 ; 'Yip, H.K. John' ; Department of Chemistry National University of Singapore SINGAPORE 117543 ; _publ_contact_author_name 'Dr John Yip' _publ_contact_author_address ; Department of Chemistry The National University of Singapore 10 Kent Ridge Crescent Singapore SINGAPORE ; _publ_contact_author_phone '(65) 6874 6256' _publ_contact_author_fax '(65) 6779 1691' _publ_contact_author_email chmyiphk@nus.edu.sg _publ_requested_journal 'J Chem Soc Dalton Trans.' _publ_contact_letter ; Please consider this CIF submission for publication in 'J Chem Soc Dalton Trans.' ; _publ_section_title ; Coordination Networks of Silver(I) and N,N'-bis(3-pyridinecarboxamide)-n- hexane structure and anion exchange. ; data_compoundL _database_code_CSD 189551 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 N4 O2' _chemical_formula_weight 326.40 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' 'O' 'O' 0.0106 0.0060 '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' 'H' 'H' 0.0000 0.0000 '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 5.2078(8) _cell_length_b 5.0943(8) _cell_length_c 30.930(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.829(3) _cell_angle_gamma 90.00 _cell_volume 817.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1032 _cell_measurement_theta_min 2.643 _cell_measurement_theta_max 28.534 _exptl_crystal_description 'Long Rod' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 348 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.476415 _exptl_absorpt_correction_T_max 0.776315 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6158 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 30.04 _reflns_number_total 2256 _reflns_number_gt 1405 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0542P)^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_number_reflns 2256 _refine_ls_number_parameters 117 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0954 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1273 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.915 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.2301(2) 0.3174(2) 0.10227(4) 0.0451(4) Uani 1 1 d . . . N1 N 0.8454(3) 0.4965(3) 0.19177(5) 0.0463(4) Uani 1 1 d . . . N2 N 0.1176(3) 0.7422(3) 0.09505(5) 0.0347(4) Uani 1 1 d . . . H2 H 0.154(3) 0.903(3) 0.1020(6) 0.042(5) Uiso 1 1 d . . . C1 C -0.4252(3) 0.8784(3) 0.00777(5) 0.0340(4) Uani 1 1 d . . . H1A H -0.3351 0.8078 -0.0163 0.041 Uiso 1 1 calc R . . H1B H -0.5469 0.7446 0.0161 0.041 Uiso 1 1 calc R . . C2 C -0.2298(3) 0.9315(3) 0.04607(5) 0.0344(4) Uani 1 1 d . . . H2A H -0.1112 1.0696 0.0382 0.041 Uiso 1 1 calc R . . H2B H -0.3199 0.9948 0.0706 0.041 Uiso 1 1 calc R . . C3 C -0.0775(3) 0.6889(3) 0.05960(5) 0.0358(4) Uani 1 1 d . . . H3A H -0.1953 0.5535 0.0687 0.043 Uiso 1 1 calc R . . H3B H 0.0062 0.6210 0.0347 0.043 Uiso 1 1 calc R . . C4 C 0.2578(3) 0.5483(3) 0.11404(5) 0.0320(4) Uani 1 1 d . . . C5 C 0.6636(3) 0.4592(3) 0.15924(6) 0.0383(4) Uani 1 1 d . . . H5 H 0.6807 0.3138 0.1410 0.046 Uiso 1 1 calc R . . C6 C 0.4504(3) 0.6217(3) 0.15062(5) 0.0314(4) Uani 1 1 d . . . C7 C 0.4278(3) 0.8371(3) 0.17706(6) 0.0374(4) Uani 1 1 d . . . H7 H 0.279(3) 0.945(3) 0.1727(6) 0.042(5) Uiso 1 1 d . . . C8 C 0.6143(3) 0.8783(4) 0.21096(6) 0.0434(5) Uani 1 1 d . . . H8 H 0.6031 1.0229 0.2296 0.052 Uiso 1 1 calc R . . C9 C 0.8152(3) 0.7053(4) 0.21690(6) 0.0455(5) Uani 1 1 d . . . H9 H 0.9398 0.7354 0.2402 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0538(8) 0.0275(6) 0.0499(8) -0.0044(6) -0.0201(6) 0.0008(5) N1 0.0397(9) 0.0470(9) 0.0488(10) 0.0041(8) -0.0164(7) -0.0011(7) N2 0.0374(8) 0.0251(7) 0.0383(9) -0.0007(6) -0.0157(6) -0.0013(6) C1 0.0322(8) 0.0307(8) 0.0370(10) -0.0011(7) -0.0104(7) -0.0001(6) C2 0.0349(9) 0.0293(8) 0.0369(10) -0.0008(7) -0.0096(7) -0.0003(6) C3 0.0362(9) 0.0321(8) 0.0363(10) -0.0020(7) -0.0134(7) -0.0002(7) C4 0.0321(8) 0.0290(8) 0.0334(9) 0.0009(7) -0.0062(7) -0.0016(6) C5 0.0371(9) 0.0358(9) 0.0399(10) 0.0019(8) -0.0089(8) -0.0007(7) C6 0.0339(8) 0.0278(8) 0.0309(9) 0.0031(7) -0.0064(7) -0.0050(6) C7 0.0368(10) 0.0347(9) 0.0391(10) 0.0014(8) -0.0069(8) -0.0019(7) C8 0.0509(11) 0.0397(10) 0.0376(11) -0.0059(8) -0.0081(8) -0.0075(8) C9 0.0429(10) 0.0485(11) 0.0416(11) 0.0042(9) -0.0176(8) -0.0134(8) _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 O1 C4 1.2362(18) . ? N1 C9 1.335(2) . ? N1 C5 1.336(2) . ? N2 C4 1.3349(19) . ? N2 C3 1.456(2) . ? C1 C1 1.520(3) 3_475 ? C1 C2 1.520(2) . ? C2 C3 1.508(2) . ? C4 C6 1.495(2) . ? C5 C6 1.393(2) . ? C6 C7 1.380(2) . ? C7 C8 1.384(2) . ? C8 C9 1.369(3) . ? 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 C9 N1 C5 116.18(15) . . ? C4 N2 C3 120.97(13) . . ? C1 C1 C2 113.18(16) 3_475 . ? C3 C2 C1 111.88(13) . . ? N2 C3 C2 111.94(13) . . ? O1 C4 N2 121.91(14) . . ? O1 C4 C6 121.03(14) . . ? N2 C4 C6 117.06(14) . . ? N1 C5 C6 124.24(16) . . ? C7 C6 C5 117.77(15) . . ? C7 C6 C4 124.23(14) . . ? C5 C6 C4 117.99(15) . . ? C6 C7 C8 118.70(16) . . ? C9 C8 C7 118.95(17) . . ? N1 C9 C8 124.15(16) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.207 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.058 #======== data_[Ag2L3(OH)][ClO4].2.5H2O _database_code_CSD 189552 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [Ag2L3(OH)][ClO4].2.5H2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H72 Ag2 Cl N12 O13.50' _chemical_formula_weight 1356.43 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P3(2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 15.1300(2) _cell_length_b 15.1300(2) _cell_length_c 22.1343(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4388.08(13) _cell_formula_units_Z 3 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6842 _cell_measurement_theta_min 1.55 _cell_measurement_theta_max 29.29 _exptl_crystal_description 'Needle, cut' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2097 _exptl_absorpt_coefficient_mu 0.789 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 1996)' _exptl_absorpt_correction_T_min 0.7281 _exptl_absorpt_correction_T_max 0.8789 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27380 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12302 _reflns_number_gt 9835 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0638P)^2^+6.0246P] 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 0.12(3) _refine_ls_number_reflns 12302 _refine_ls_number_parameters 748 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1462 _refine_ls_wR_factor_gt 0.1359 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.62300(4) 0.64491(4) 0.29385(3) 0.06269(17) Uani 1 1 d . . . Ag2 Ag 0.99608(4) 0.30159(4) 1.04428(3) 0.05960(15) Uani 1 1 d . . . O1 O 0.8759(5) 0.4439(4) 0.4450(3) 0.0728(16) Uani 1 1 d . . . O2 O 0.7640(4) 0.5423(4) 0.9174(3) 0.0683(14) Uani 1 1 d . . . O3 O 0.2035(4) 0.4208(6) 0.4765(3) 0.102(2) Uani 1 1 d . . . O4 O 0.4727(4) 0.5415(6) 0.9289(3) 0.099(2) Uani 1 1 d . . . O5 O 0.8791(5) 1.1261(5) 0.4049(3) 0.0909(19) Uani 1 1 d . . . O6 O 0.8071(5) -0.1344(4) 0.8786(3) 0.0810(17) Uani 1 1 d . . . O7 O 0.5713(7) 0.6114(5) 0.1847(3) 0.118(3) Uani 1 1 d . . . H7A H 0.6225 0.6279 0.1635 0.177 Uiso 1 1 calc R . . N1 N 0.7063(4) 0.5561(4) 0.3108(2) 0.0407(11) Uani 1 1 d . . . N2 N 0.8480(4) 0.5684(4) 0.4789(2) 0.0460(12) Uani 1 1 d . . . H2A H 0.8205 0.6058 0.4712 0.055 Uiso 1 1 calc R . . N3 N 0.8305(5) 0.4577(5) 0.8693(3) 0.0552(15) Uani 1 1 d . . . H3B H 0.8716 0.4332 0.8717 0.066 Uiso 1 1 calc R . . N4 N 0.9374(4) 0.4147(3) 1.0386(2) 0.0400(11) Uani 1 1 d . . . N5 N 0.4568(4) 0.5779(4) 0.3242(3) 0.0560(15) Uani 1 1 d . . . N6 N 0.3659(4) 0.4905(5) 0.5076(3) 0.0669(18) Uani 1 1 d . . . H6A H 0.4300 0.5238 0.4973 0.080 Uiso 1 1 calc R . . N7 N 0.3232(5) 0.4868(7) 0.8830(3) 0.082(2) Uani 1 1 d . . . H7B H 0.2579 0.4625 0.8872 0.098 Uiso 1 1 calc R . . N8 N 0.7340(4) 0.8155(4) 0.2930(3) 0.0512(13) Uani 1 1 d . . . N9 N 0.7754(5) 0.9823(5) 0.4561(3) 0.0610(16) Uani 1 1 d . . . H9A H 0.7367 0.9164 0.4540 0.073 Uiso 1 1 calc R . . N10 N 1.1687(5) 0.3697(4) 1.0486(3) 0.0597(15) Uani 1 1 d . . . N11 N 0.8961(4) 0.1326(4) 1.0214(3) 0.0477(12) Uani 1 1 d . . . N12 N 0.8919(5) 0.0267(4) 0.8434(3) 0.0570(15) Uani 1 1 d . . . H12C H 0.9164 0.0911 0.8514 0.068 Uiso 1 1 calc R . . C1 C 0.7260(5) 0.5101(5) 0.2651(3) 0.0505(16) Uani 1 1 d . . . H1A H 0.7001 0.5110 0.2266 0.061 Uiso 1 1 calc R . . C2 C 0.7812(6) 0.4625(6) 0.2712(3) 0.0550(18) Uani 1 1 d . . . H2B H 0.7939 0.4324 0.2377 0.066 Uiso 1 1 calc R . . C3 C 0.8190(5) 0.4588(5) 0.3283(3) 0.0509(16) Uani 1 1 d . . . H3C H 0.8566 0.4253 0.3339 0.061 Uiso 1 1 calc R . . C4 C 0.8000(5) 0.5054(5) 0.3763(3) 0.0394(12) Uani 1 1 d . . . C5 C 0.7430(4) 0.5532(4) 0.3659(3) 0.0402(13) Uani 1 1 d . . . H5A H 0.7295 0.5845 0.3985 0.048 Uiso 1 1 calc R . . C6 C 0.8446(5) 0.5038(5) 0.4377(3) 0.0461(15) Uani 1 1 d . . . C7 C 0.8978(5) 0.5781(5) 0.5380(3) 0.0510(15) Uani 1 1 d . . . H7C H 0.9462 0.6504 0.5458 0.061 Uiso 1 1 calc R . . H7D H 0.9367 0.5423 0.5361 0.061 Uiso 1 1 calc R . . C8 C 0.8243(5) 0.5362(5) 0.5893(3) 0.0436(13) Uani 1 1 d . . . H8A H 0.7734 0.4649 0.5810 0.052 Uiso 1 1 calc R . . H8B H 0.7886 0.5750 0.5934 0.052 Uiso 1 1 calc R . . C9 C 0.8804(5) 0.5426(5) 0.6485(3) 0.0422(14) Uani 1 1 d . . . H9B H 0.9161 0.5038 0.6439 0.051 Uiso 1 1 calc R . . H9C H 0.9319 0.6140 0.6562 0.051 Uiso 1 1 calc R . . C10 C 0.8088(5) 0.5012(5) 0.7027(3) 0.0439(14) Uani 1 1 d . . . H10A H 0.7567 0.4303 0.6944 0.053 Uiso 1 1 calc R . . H10B H 0.7740 0.5407 0.7073 0.053 Uiso 1 1 calc R . . C11 C 0.8619(5) 0.5048(5) 0.7621(3) 0.0471(15) Uani 1 1 d . . . H11A H 0.9010 0.4696 0.7573 0.057 Uiso 1 1 calc R . . H11B H 0.9094 0.5759 0.7731 0.057 Uiso 1 1 calc R . . C12 C 0.7833(5) 0.4541(6) 0.8114(3) 0.0584(18) Uani 1 1 d . . . H12A H 0.7431 0.4884 0.8151 0.070 Uiso 1 1 calc R . . H12B H 0.7366 0.3827 0.8004 0.070 Uiso 1 1 calc R . . C13 C 0.8137(5) 0.4963(5) 0.9179(3) 0.0448(14) Uani 1 1 d . . . C14 C 0.9124(5) 0.4484(5) 1.0876(3) 0.0465(14) Uani 1 1 d . . . H14A H 0.9314 0.4356 1.1257 0.056 Uiso 1 1 calc R . . C15 C 0.8612(6) 0.5001(6) 1.0854(3) 0.0597(19) Uani 1 1 d . . . H15A H 0.8473 0.5243 1.1212 0.072 Uiso 1 1 calc R . . C16 C 0.8289(5) 0.5175(5) 1.0301(3) 0.0527(16) Uani 1 1 d . . . H16A H 0.7919 0.5522 1.0279 0.063 Uiso 1 1 calc R . . C17 C 0.8531(5) 0.4821(5) 0.9779(3) 0.0460(15) Uani 1 1 d . . . C18 C 0.9079(4) 0.4324(4) 0.9848(3) 0.0404(13) Uani 1 1 d . . . H18A H 0.9258 0.4096 0.9498 0.048 Uiso 1 1 calc R . . C19 C 0.3823(7) 0.5511(6) 0.2831(4) 0.069(2) Uani 1 1 d . . . H19A H 0.4000 0.5672 0.2423 0.082 Uiso 1 1 calc R . . C20 C 0.2788(7) 0.4996(7) 0.2995(5) 0.078(3) Uani 1 1 d . . . H20A H 0.2278 0.4825 0.2701 0.094 Uiso 1 1 calc R . . C21 C 0.2535(6) 0.4752(6) 0.3582(5) 0.070(2) Uani 1 1 d . . . H21A H 0.1845 0.4402 0.3697 0.084 Uiso 1 1 calc R . . C22 C 0.3292(5) 0.5015(5) 0.4017(4) 0.062(2) Uani 1 1 d . . . C23 C 0.4304(5) 0.5538(5) 0.3816(4) 0.062(2) Uani 1 1 d . . . H23A H 0.4826 0.5729 0.4104 0.074 Uiso 1 1 calc R . . C24 C 0.2984(6) 0.4703(6) 0.4663(4) 0.0584(19) Uani 1 1 d . . . C25 C 0.3408(6) 0.4610(5) 0.5696(4) 0.070(2) Uani 1 1 d . . . H25A H 0.3699 0.4183 0.5811 0.083 Uiso 1 1 calc R . . H25B H 0.2665 0.4192 0.5732 0.083 Uiso 1 1 calc R . . C26 C 0.3775(5) 0.5476(5) 0.6133(4) 0.062(2) Uani 1 1 d . . . H26A H 0.3534 0.5938 0.6000 0.074 Uiso 1 1 calc R . . H26B H 0.4523 0.5860 0.6127 0.074 Uiso 1 1 calc R . . C27 C 0.3414(5) 0.5137(6) 0.6787(4) 0.069(3) Uani 1 1 d . . . H27A H 0.2666 0.4769 0.6792 0.083 Uiso 1 1 calc R . . H27B H 0.3634 0.4655 0.6911 0.083 Uiso 1 1 calc R . . C28 C 0.3792(6) 0.5981(6) 0.7247(4) 0.080(2) Uani 1 1 d . . . H28A H 0.3663 0.6509 0.7085 0.096 Uiso 1 1 calc R . . H28B H 0.4535 0.6284 0.7274 0.096 Uiso 1 1 calc R . . C29 C 0.3360(7) 0.5745(7) 0.7913(5) 0.082(3) Uani 1 1 d . . . H29A H 0.3605 0.6387 0.8134 0.098 Uiso 1 1 calc R . . H29B H 0.2613 0.5395 0.7902 0.098 Uiso 1 1 calc R . . C30 C 0.3675(8) 0.5124(11) 0.8217(5) 0.105(4) Uani 1 1 d . . . H30A H 0.4422 0.5486 0.8245 0.126 Uiso 1 1 calc R . . H30B H 0.3456 0.4495 0.7987 0.126 Uiso 1 1 calc R . . C31 C 0.3774(6) 0.4990(6) 0.9304(4) 0.064(2) Uani 1 1 d . . . C32 C 0.7779(5) 0.8694(6) 0.2433(4) 0.0583(17) Uani 1 1 d . . . H32A H 0.7680 0.8341 0.2067 0.070 Uiso 1 1 calc R . . C33 C 0.8369(6) 0.9739(6) 0.2428(4) 0.067(2) Uani 1 1 d . . . H33A H 0.8679 1.0086 0.2069 0.080 Uiso 1 1 calc R . . C34 C 0.8501(6) 1.0268(6) 0.2951(4) 0.068(2) Uani 1 1 d . . . H34A H 0.8874 1.0985 0.2946 0.082 Uiso 1 1 calc R . . C35 C 0.8091(5) 0.9758(5) 0.3493(4) 0.0529(17) Uani 1 1 d . . . C36 C 0.7503(5) 0.8682(5) 0.3447(3) 0.0522(16) Uani 1 1 d . . . H36A H 0.7205 0.8310 0.3802 0.063 Uiso 1 1 calc R . . C37 C 0.8253(6) 1.0335(6) 0.4060(4) 0.062(2) Uani 1 1 d . . . C38 C 0.7832(7) 1.0324(6) 0.5136(4) 0.072(2) Uani 1 1 d . . . H38A H 0.7151 1.0181 0.5262 0.086 Uiso 1 1 calc R . . H38B H 0.8261 1.1064 0.5086 0.086 Uiso 1 1 calc R . . C39 C 0.8277(5) 0.9970(5) 0.5620(3) 0.0520(16) Uani 1 1 d . . . H39A H 0.7870 0.9225 0.5653 0.062 Uiso 1 1 calc R . . H39B H 0.8972 1.0148 0.5505 0.062 Uiso 1 1 calc R . . C40 C 0.8305(5) 1.0435(5) 0.6223(3) 0.0491(16) Uani 1 1 d . . . H40A H 0.7615 1.0285 0.6328 0.059 Uiso 1 1 calc R . . H40B H 0.8738 1.1178 0.6193 0.059 Uiso 1 1 calc R . . C41 C 0.8704(5) 1.0049(5) 0.6718(3) 0.0489(16) Uani 1 1 d . . . H41A H 0.9413 1.0248 0.6626 0.059 Uiso 1 1 calc R . . H41B H 0.8306 0.9302 0.6723 0.059 Uiso 1 1 calc R . . C42 C 0.8663(5) 1.0445(5) 0.7345(3) 0.0487(15) Uani 1 1 d . . . H42A H 0.9101 1.1189 0.7356 0.058 Uiso 1 1 calc R . . H42B H 0.7962 1.0282 0.7434 0.058 Uiso 1 1 calc R . . C43 C 0.9017(5) 0.9963(5) 0.7821(3) 0.0571(17) Uani 1 1 d . . . H43A H 0.8611 0.9218 0.7787 0.069 Uiso 1 1 calc R . . H43B H 0.9732 1.0167 0.7746 0.069 Uiso 1 1 calc R . . C44 C 1.2188(5) 0.4035(5) 0.9957(4) 0.0559(19) Uani 1 1 d . . . H44A H 1.1800 0.3868 0.9601 0.067 Uiso 1 1 calc R . . C45 C 1.3250(5) 0.4618(5) 0.9908(4) 0.0551(18) Uani 1 1 d . . . C46 C 1.3819(6) 0.4854(6) 1.0432(5) 0.070(2) Uani 1 1 d . . . H46A H 1.4535 0.5248 1.0418 0.085 Uiso 1 1 calc R . . C47 C 1.3323(7) 0.4506(6) 1.0972(5) 0.076(3) Uani 1 1 d . . . H47A H 1.3693 0.4646 1.1335 0.091 Uiso 1 1 calc R . . C48 C 1.2290(6) 0.3957(5) 1.0975(4) 0.0628(19) Uani 1 1 d . . . H48A H 1.1968 0.3738 1.1353 0.075 Uiso 1 1 calc R . . C49 C 0.8474(5) 0.0629(6) 1.0647(3) 0.0523(16) Uani 1 1 d . . . H49A H 0.8483 0.0851 1.1045 0.063 Uiso 1 1 calc R . . C50 C 0.7952(6) -0.0426(6) 1.0525(4) 0.061(2) Uani 1 1 d . . . H50A H 0.7613 -0.0901 1.0836 0.073 Uiso 1 1 calc R . . C51 C 0.7945(5) -0.0742(5) 0.9953(3) 0.0545(18) Uani 1 1 d . . . H51A H 0.7598 -0.1444 0.9864 0.065 Uiso 1 1 calc R . . C52 C 0.8455(4) -0.0029(5) 0.9491(3) 0.0452(15) Uani 1 1 d . . . C53 C 0.8947(4) 0.0988(5) 0.9650(3) 0.0414(14) Uani 1 1 d . . . H53A H 0.9294 0.1475 0.9346 0.050 Uiso 1 1 calc R . . C54 C 0.8463(5) -0.0420(5) 0.8874(3) 0.0487(15) Uani 1 1 d . . . Cl1 Cl 0.66659(12) 0.68523(11) 0.51282(7) 0.0400(3) Uani 1 1 d . . . O8 O 0.5909(3) 0.5791(3) 0.4982(2) 0.0551(12) Uani 1 1 d . . . O9 O 0.6399(5) 0.7558(4) 0.4838(4) 0.100(2) Uani 1 1 d . . . O10 O 0.7684(3) 0.7066(4) 0.4940(2) 0.0608(13) Uani 1 1 d . . . O11 O 0.6720(4) 0.6974(5) 0.5804(2) 0.0775(17) Uani 1 1 d . . . O1S O 0.9343(7) 0.2567(7) 1.1608(3) 0.109(2) Uani 1 1 d . . . O2S O 0.6646(7) 0.6493(6) 0.9932(7) 0.170(5) Uani 1 1 d D . . H2SA H 0.6765 0.6018 0.9774 0.050 Uiso 1 1 d RD . . H2SB H 0.6369 0.6606 0.9602 0.050 Uiso 1 1 d RD . . O3S O 0.7125(8) 0.6086(10) 0.1294(6) 0.086(4) Uani 0.50 1 d PD . . H3SA H 0.6697 0.6170 0.1043 0.050 Uiso 0.50 1 d PRD . . H3SB H 0.7710 0.6579 0.1125 0.050 Uiso 0.50 1 d PRD . . 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 0.0663(4) 0.0572(3) 0.0725(4) -0.0025(3) -0.0092(3) 0.0369(3) Ag2 0.0656(3) 0.0634(3) 0.0609(3) -0.0005(3) -0.0058(3) 0.0405(3) O1 0.095(4) 0.085(4) 0.074(4) -0.017(3) -0.025(3) 0.071(3) O2 0.078(3) 0.077(4) 0.073(4) 0.004(3) -0.005(3) 0.056(3) O3 0.050(3) 0.132(6) 0.114(6) 0.009(4) 0.001(3) 0.037(4) O4 0.048(3) 0.125(6) 0.111(5) -0.005(4) -0.018(3) 0.035(3) O5 0.075(4) 0.062(4) 0.115(5) -0.013(3) 0.015(4) 0.018(3) O6 0.110(5) 0.039(3) 0.081(4) 0.001(3) -0.006(3) 0.027(3) O7 0.168(7) 0.098(5) 0.069(4) 0.020(4) -0.033(5) 0.052(5) N1 0.043(3) 0.038(2) 0.043(3) 0.001(2) -0.001(2) 0.021(2) N2 0.051(3) 0.058(3) 0.038(3) -0.001(2) -0.002(2) 0.034(3) N3 0.059(4) 0.070(4) 0.051(4) 0.008(3) 0.000(3) 0.044(3) N4 0.047(3) 0.032(2) 0.038(3) -0.001(2) 0.001(2) 0.017(2) N5 0.049(3) 0.046(3) 0.083(5) -0.007(3) -0.015(3) 0.031(3) N6 0.033(3) 0.051(3) 0.103(6) 0.010(3) -0.006(3) 0.011(3) N7 0.049(4) 0.132(7) 0.065(5) -0.015(4) -0.001(3) 0.045(4) N8 0.043(3) 0.055(3) 0.062(4) -0.001(3) -0.007(3) 0.030(3) N9 0.072(4) 0.054(4) 0.059(4) -0.014(3) -0.009(3) 0.032(3) N10 0.073(4) 0.045(3) 0.069(4) -0.009(3) -0.015(3) 0.036(3) N11 0.043(3) 0.055(3) 0.048(3) 0.011(2) -0.001(2) 0.027(3) N12 0.062(4) 0.041(3) 0.071(4) 0.000(3) 0.008(3) 0.028(3) C1 0.060(4) 0.050(4) 0.034(3) 0.004(3) 0.006(3) 0.021(3) C2 0.076(5) 0.061(4) 0.041(4) -0.007(3) 0.008(3) 0.045(4) C3 0.050(4) 0.051(4) 0.058(4) -0.001(3) 0.009(3) 0.030(3) C4 0.038(3) 0.035(3) 0.045(3) -0.003(2) 0.003(2) 0.019(2) C5 0.038(3) 0.036(3) 0.046(3) 0.000(2) 0.008(2) 0.018(2) C6 0.043(3) 0.046(3) 0.055(4) 0.002(3) -0.003(3) 0.027(3) C7 0.051(4) 0.060(4) 0.048(4) 0.003(3) -0.004(3) 0.033(3) C8 0.040(3) 0.054(4) 0.041(3) 0.002(3) -0.007(2) 0.027(3) C9 0.040(3) 0.040(3) 0.049(4) -0.001(3) -0.010(3) 0.022(3) C10 0.038(3) 0.042(3) 0.050(4) 0.010(3) -0.006(3) 0.019(3) C11 0.047(3) 0.050(4) 0.047(4) 0.005(3) -0.010(3) 0.026(3) C12 0.046(4) 0.070(5) 0.050(4) 0.012(3) -0.009(3) 0.022(3) C13 0.040(3) 0.038(3) 0.056(4) 0.004(3) -0.004(3) 0.020(3) C14 0.046(3) 0.040(3) 0.044(4) 0.000(3) -0.006(3) 0.015(3) C15 0.075(5) 0.054(4) 0.046(4) -0.014(3) 0.006(3) 0.028(4) C16 0.058(4) 0.045(4) 0.063(5) 0.002(3) 0.002(3) 0.031(3) C17 0.042(3) 0.033(3) 0.054(4) 0.009(3) 0.000(3) 0.012(3) C18 0.040(3) 0.033(3) 0.043(3) 0.001(2) 0.005(2) 0.014(2) C19 0.082(6) 0.055(4) 0.074(6) -0.009(4) -0.015(4) 0.038(4) C20 0.056(5) 0.077(6) 0.111(8) -0.013(5) -0.029(5) 0.041(5) C21 0.057(5) 0.063(5) 0.097(7) -0.007(4) -0.002(4) 0.034(4) C22 0.042(4) 0.048(4) 0.099(6) -0.017(4) -0.021(4) 0.027(3) C23 0.055(4) 0.055(4) 0.092(6) -0.011(4) -0.018(4) 0.040(4) C24 0.049(4) 0.053(4) 0.074(5) 0.005(4) 0.004(4) 0.025(3) C25 0.059(4) 0.045(4) 0.092(6) 0.021(4) 0.010(4) 0.017(3) C26 0.041(4) 0.043(4) 0.097(6) 0.019(4) 0.011(4) 0.018(3) C27 0.034(4) 0.054(5) 0.119(7) 0.039(5) 0.021(4) 0.023(3) C28 0.054(5) 0.070(5) 0.097(7) 0.018(5) 0.020(4) 0.016(4) C29 0.061(5) 0.059(5) 0.119(8) -0.002(5) 0.025(5) 0.026(4) C30 0.072(6) 0.169(12) 0.094(8) 0.006(7) 0.006(5) 0.076(7) C31 0.059(5) 0.065(5) 0.075(5) -0.020(4) -0.026(4) 0.036(4) C32 0.050(4) 0.069(5) 0.061(5) -0.003(4) -0.006(3) 0.033(4) C33 0.057(5) 0.070(5) 0.061(5) 0.015(4) -0.002(4) 0.023(4) C34 0.054(4) 0.059(5) 0.092(7) 0.012(4) -0.005(4) 0.029(4) C35 0.043(4) 0.051(4) 0.072(5) 0.005(3) 0.003(3) 0.029(3) C36 0.047(4) 0.057(4) 0.065(5) 0.002(3) -0.002(3) 0.034(3) C37 0.044(4) 0.048(4) 0.091(6) -0.004(4) -0.008(4) 0.019(3) C38 0.091(6) 0.062(5) 0.072(5) -0.018(4) -0.017(4) 0.046(5) C39 0.050(4) 0.039(3) 0.066(5) -0.009(3) 0.001(3) 0.021(3) C40 0.043(3) 0.034(3) 0.063(5) -0.004(3) 0.008(3) 0.014(3) C41 0.041(3) 0.036(3) 0.069(5) -0.010(3) 0.008(3) 0.018(3) C42 0.042(3) 0.044(3) 0.060(4) 0.001(3) 0.013(3) 0.021(3) C43 0.055(4) 0.050(4) 0.071(5) -0.002(3) 0.012(3) 0.029(3) C44 0.063(4) 0.046(4) 0.069(5) -0.021(3) -0.033(4) 0.036(3) C45 0.050(4) 0.048(4) 0.078(5) -0.016(3) -0.018(4) 0.033(3) C46 0.055(4) 0.047(4) 0.105(7) -0.013(4) -0.032(5) 0.022(4) C47 0.093(6) 0.061(5) 0.080(6) -0.007(4) -0.044(5) 0.042(5) C48 0.075(5) 0.049(4) 0.070(5) -0.008(3) -0.029(4) 0.036(4) C49 0.045(3) 0.069(5) 0.050(4) 0.015(3) 0.005(3) 0.034(3) C50 0.059(4) 0.057(4) 0.065(5) 0.027(4) 0.011(4) 0.029(4) C51 0.048(4) 0.046(4) 0.069(5) 0.020(3) -0.004(3) 0.023(3) C52 0.030(3) 0.039(3) 0.066(4) 0.018(3) -0.004(3) 0.016(2) C53 0.034(3) 0.044(3) 0.048(4) 0.015(3) 0.005(2) 0.021(3) C54 0.042(3) 0.042(3) 0.064(4) 0.008(3) -0.002(3) 0.022(3) Cl1 0.0323(6) 0.0350(7) 0.0512(10) 0.0000(6) 0.0027(6) 0.0157(5) O8 0.041(2) 0.037(2) 0.071(3) -0.004(2) -0.007(2) 0.0072(19) O9 0.087(4) 0.068(4) 0.159(7) 0.013(4) -0.036(4) 0.050(3) O10 0.042(2) 0.061(3) 0.081(4) -0.011(2) 0.006(2) 0.027(2) O11 0.072(3) 0.105(4) 0.042(3) -0.026(3) 0.007(2) 0.033(3) O1S 0.145(6) 0.169(7) 0.063(4) 0.010(4) -0.002(4) 0.115(6) O2S 0.089(5) 0.111(7) 0.319(17) 0.049(8) -0.018(7) 0.057(5) O3S 0.054(6) 0.102(9) 0.082(8) -0.001(7) 0.016(5) 0.024(6) _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 N8 2.268(6) . ? Ag1 N1 2.288(5) . ? Ag1 N5 2.292(6) . ? Ag1 O7 2.511(7) . ? Ag2 N10 2.281(6) . ? Ag2 N11 2.284(6) . ? Ag2 N4 2.291(5) . ? O1 C6 1.224(8) . ? O2 C13 1.255(8) . ? O3 C24 1.265(9) . ? O4 C31 1.252(10) . ? O5 C37 1.218(9) . ? O6 C54 1.230(8) . ? N1 C1 1.342(8) . ? N1 C5 1.350(8) . ? N2 C6 1.320(9) . ? N2 C7 1.481(8) . ? N3 C13 1.308(9) . ? N3 C12 1.456(9) . ? N4 C14 1.333(8) . ? N4 C18 1.346(8) . ? N5 C23 1.328(10) . ? N5 C19 1.343(10) . ? N6 C24 1.287(10) . ? N6 C25 1.436(11) . ? N7 C31 1.288(10) . ? N7 C30 1.476(12) . ? N8 C32 1.332(9) . ? N8 C36 1.345(9) . ? N9 C37 1.348(10) . ? N9 C38 1.456(10) . ? N10 C48 1.343(9) . ? N10 C44 1.347(10) . ? N11 C49 1.341(8) . ? N11 C53 1.345(8) . ? N12 C54 1.338(9) . ? N12 C43 1.462(9) 1_545 ? C1 C2 1.354(10) . ? C2 C3 1.399(10) . ? C3 C4 1.383(9) . ? C4 C5 1.394(8) . ? C4 C6 1.524(9) . ? C7 C8 1.489(9) . ? C8 C9 1.539(8) . ? C9 C10 1.525(9) . ? C10 C11 1.527(8) . ? C11 C12 1.512(10) . ? C13 C17 1.514(9) . ? C14 C15 1.350(10) . ? C15 C16 1.391(10) . ? C16 C17 1.397(10) . ? C17 C18 1.379(9) . ? C19 C20 1.405(12) . ? C20 C21 1.352(13) . ? C21 C22 1.395(11) . ? C22 C23 1.399(11) . ? C22 C24 1.504(12) . ? C25 C26 1.494(12) . ? C26 C27 1.542(12) . ? C27 C28 1.505(13) . ? C28 C29 1.579(13) . ? C29 C30 1.418(14) . ? C31 C45 1.511(12) 1_455 ? C32 C33 1.374(11) . ? C33 C34 1.364(12) . ? C34 C35 1.392(11) . ? C35 C36 1.416(10) . ? C35 C37 1.478(11) . ? C38 C39 1.499(11) . ? C39 C40 1.499(10) . ? C40 C41 1.502(10) . ? C41 C42 1.526(9) . ? C42 C43 1.524(10) . ? C43 N12 1.462(9) 1_565 ? C44 C45 1.397(10) . ? C45 C46 1.381(11) . ? C45 C31 1.511(12) 1_655 ? C46 C47 1.370(14) . ? C47 C48 1.354(12) . ? C49 C50 1.408(11) . ? C50 C51 1.352(11) . ? C51 C52 1.405(9) . ? C52 C53 1.380(9) . ? C52 C54 1.490(10) . ? Cl1 O9 1.465(5) . ? Cl1 O10 1.467(5) . ? Cl1 O8 1.468(4) . ? Cl1 O11 1.505(5) . ? 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 N8 Ag1 N1 110.96(17) . . ? N8 Ag1 N5 122.00(19) . . ? N1 Ag1 N5 119.84(18) . . ? N8 Ag1 O7 101.6(2) . . ? N1 Ag1 O7 104.2(2) . . ? N5 Ag1 O7 91.8(3) . . ? N10 Ag2 N11 118.88(18) . . ? N10 Ag2 N4 116.65(18) . . ? N11 Ag2 N4 122.48(17) . . ? C1 N1 C5 117.6(5) . . ? C1 N1 Ag1 120.8(4) . . ? C5 N1 Ag1 121.5(4) . . ? C6 N2 C7 120.9(5) . . ? C13 N3 C12 122.6(6) . . ? C14 N4 C18 117.3(5) . . ? C14 N4 Ag2 122.1(4) . . ? C18 N4 Ag2 119.2(4) . . ? C23 N5 C19 118.3(7) . . ? C23 N5 Ag1 121.0(5) . . ? C19 N5 Ag1 120.3(6) . . ? C24 N6 C25 123.4(7) . . ? C31 N7 C30 122.6(8) . . ? C32 N8 C36 116.9(6) . . ? C32 N8 Ag1 124.2(5) . . ? C36 N8 Ag1 118.6(5) . . ? C37 N9 C38 123.0(7) . . ? C48 N10 C44 114.7(7) . . ? C48 N10 Ag2 128.5(6) . . ? C44 N10 Ag2 115.8(4) . . ? C49 N11 C53 117.9(6) . . ? C49 N11 Ag2 121.2(5) . . ? C53 N11 Ag2 120.4(4) . . ? C54 N12 C43 121.7(6) . 1_545 ? N1 C1 C2 123.7(6) . . ? C1 C2 C3 119.0(6) . . ? C4 C3 C2 118.6(6) . . ? C3 C4 C5 118.6(6) . . ? C3 C4 C6 118.0(6) . . ? C5 C4 C6 123.4(5) . . ? N1 C5 C4 122.4(5) . . ? O1 C6 N2 124.8(7) . . ? O1 C6 C4 118.0(6) . . ? N2 C6 C4 117.2(5) . . ? N2 C7 C8 113.3(5) . . ? C7 C8 C9 110.5(5) . . ? C10 C9 C8 112.8(5) . . ? C9 C10 C11 114.2(5) . . ? C12 C11 C10 109.8(5) . . ? N3 C12 C11 111.7(6) . . ? O2 C13 N3 123.0(6) . . ? O2 C13 C17 118.3(6) . . ? N3 C13 C17 118.7(6) . . ? N4 C14 C15 123.2(6) . . ? C14 C15 C16 120.0(6) . . ? C15 C16 C17 118.1(6) . . ? C18 C17 C16 117.6(6) . . ? C18 C17 C13 124.1(6) . . ? C16 C17 C13 118.3(6) . . ? N4 C18 C17 123.8(6) . . ? N5 C19 C20 121.9(9) . . ? C21 C20 C19 118.9(8) . . ? C20 C21 C22 120.5(8) . . ? C21 C22 C23 116.9(9) . . ? C21 C22 C24 119.1(7) . . ? C23 C22 C24 124.0(7) . . ? N5 C23 C22 123.6(7) . . ? O3 C24 N6 123.1(8) . . ? O3 C24 C22 115.8(7) . . ? N6 C24 C22 121.0(7) . . ? N6 C25 C26 115.0(6) . . ? C25 C26 C27 113.6(6) . . ? C28 C27 C26 115.5(6) . . ? C27 C28 C29 120.0(7) . . ? C30 C29 C28 110.7(8) . . ? C29 C30 N7 110.5(9) . . ? O4 C31 N7 122.5(9) . . ? O4 C31 C45 118.1(7) . 1_455 ? N7 C31 C45 119.4(7) . 1_455 ? N8 C32 C33 123.3(7) . . ? C34 C33 C32 119.3(8) . . ? C33 C34 C35 120.8(8) . . ? C34 C35 C36 115.2(7) . . ? C34 C35 C37 120.5(7) . . ? C36 C35 C37 124.3(7) . . ? N8 C36 C35 124.5(7) . . ? O5 C37 N9 122.5(8) . . ? O5 C37 C35 118.7(8) . . ? N9 C37 C35 118.7(6) . . ? N9 C38 C39 111.9(6) . . ? C40 C39 C38 112.3(6) . . ? C39 C40 C41 112.9(5) . . ? C40 C41 C42 114.1(5) . . ? C43 C42 C41 110.4(5) . . ? N12 C43 C42 112.0(5) 1_565 . ? N10 C44 C45 124.0(7) . . ? C46 C45 C44 117.9(8) . . ? C46 C45 C31 120.2(7) . 1_655 ? C44 C45 C31 121.9(7) . 1_655 ? C47 C46 C45 118.9(8) . . ? C48 C47 C46 118.9(8) . . ? N10 C48 C47 125.6(9) . . ? N11 C49 C50 122.0(7) . . ? C51 C50 C49 118.8(7) . . ? C50 C51 C52 120.4(7) . . ? C53 C52 C51 117.0(7) . . ? C53 C52 C54 124.7(6) . . ? C51 C52 C54 118.2(6) . . ? N11 C53 C52 123.9(6) . . ? O6 C54 N12 122.4(7) . . ? O6 C54 C52 120.0(6) . . ? N12 C54 C52 117.6(6) . . ? O9 Cl1 O10 110.9(4) . . ? O9 Cl1 O8 110.6(3) . . ? O10 Cl1 O8 109.7(3) . . ? O9 Cl1 O11 111.4(4) . . ? O10 Cl1 O11 105.6(3) . . ? O8 Cl1 O11 108.5(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.393 _refine_diff_density_min -0.998 _refine_diff_density_rms 0.085 #======== data_compoundAgLClO4 _database_code_CSD 189553 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 Ag Cl N4 O6' _chemical_formula_weight 533.72 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 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 26.502(2) _cell_length_b 5.1431(4) _cell_length_c 44.366(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.348(2) _cell_angle_gamma 90.00 _cell_volume 6029.7(8) _cell_formula_units_Z 12 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6749 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 29.8 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3240 _exptl_absorpt_coefficient_mu 1.181 _exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.6759 _exptl_absorpt_correction_T_max 0.9115 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16461 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5285 _reflns_number_gt 4579 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, 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^)+(0.0507P)^2^+40.6497P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5285 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.1134 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 0.5000 0.5000 0.0000 0.04170(17) Uani 1 2 d S . . Ag2 Ag 1.003771(14) -0.08147(8) 0.332400(9) 0.04395(15) Uani 1 1 d . . . C1 C 0.55618(18) 0.9702(9) -0.02636(10) 0.0357(11) Uani 1 1 d . . . H1 H 0.5358 0.9294 -0.0440 0.043 Uiso 1 1 calc R . . C2 C 0.58763(17) 1.1826(10) -0.02669(10) 0.0361(11) Uani 1 1 d . . . H2 H 0.5888 1.2843 -0.0442 0.043 Uiso 1 1 calc R . . C3 C 0.61738(16) 1.2436(9) -0.00088(10) 0.0310(10) Uani 1 1 d . . . H3 H 0.6385 1.3905 -0.0004 0.037 Uiso 1 1 calc R . . C4 C 0.61594(16) 1.0865(8) 0.02451(10) 0.0280(9) Uani 1 1 d . . . C5 C 0.58335(16) 0.8769(9) 0.02316(10) 0.0302(10) Uani 1 1 d . . . H5 H 0.5819 0.7706 0.0403 0.036 Uiso 1 1 calc R . . C6 C 0.64837(16) 1.1575(8) 0.05274(9) 0.0268(9) Uani 1 1 d . . . C7 C 0.69197(19) 1.0124(9) 0.10010(10) 0.0373(11) Uani 1 1 d . . . H7A H 0.6752 1.1464 0.1115 0.045 Uiso 1 1 calc R . . H7B H 0.7253 1.0789 0.0957 0.045 Uiso 1 1 calc R . . C8 C 0.69880(17) 0.7712(9) 0.11927(10) 0.0327(10) Uani 1 1 d . . . H8A H 0.7122 0.6306 0.1073 0.039 Uiso 1 1 calc R . . H8B H 0.6659 0.7158 0.1258 0.039 Uiso 1 1 calc R . . C9 C 0.73522(17) 0.8234(9) 0.14707(10) 0.0333(10) Uani 1 1 d . . . H9A H 0.7682 0.8727 0.1403 0.040 Uiso 1 1 calc R . . H9B H 0.7225 0.9711 0.1582 0.040 Uiso 1 1 calc R . . C10 C 0.74235(18) 0.5921(9) 0.16851(10) 0.0356(11) Uani 1 1 d . . . H10A H 0.7556 0.4449 0.1575 0.043 Uiso 1 1 calc R . . H10B H 0.7093 0.5411 0.1751 0.043 Uiso 1 1 calc R . . C11 C 0.77829(18) 0.6488(9) 0.19635(10) 0.0356(11) Uani 1 1 d . . . H11A H 0.8114 0.6993 0.1898 0.043 Uiso 1 1 calc R . . H11B H 0.7651 0.7953 0.2075 0.043 Uiso 1 1 calc R . . C12 C 0.78465(17) 0.4173(9) 0.21706(10) 0.0325(10) Uani 1 1 d . . . H12A H 0.7516 0.3699 0.2240 0.039 Uiso 1 1 calc R . . H12B H 0.7969 0.2695 0.2057 0.039 Uiso 1 1 calc R . . C13 C 0.84051(16) 0.2714(8) 0.26002(10) 0.0271(9) Uani 1 1 d . . . C14 C 0.93388(17) 0.4052(9) 0.33979(10) 0.0333(10) Uani 1 1 d . . . H14 H 0.9541 0.4266 0.3580 0.040 Uiso 1 1 calc R . . C15 C 0.89626(18) 0.5830(9) 0.33258(10) 0.0347(10) Uani 1 1 d . . . H15 H 0.8912 0.7240 0.3455 0.042 Uiso 1 1 calc R . . C16 C 0.86575(17) 0.5524(9) 0.30602(10) 0.0317(10) Uani 1 1 d . . . H16 H 0.8402 0.6741 0.3005 0.038 Uiso 1 1 calc R . . C17 C 0.87347(16) 0.3394(8) 0.28776(9) 0.0270(9) Uani 1 1 d . . . C18 C 0.91273(16) 0.1701(9) 0.29658(10) 0.0294(10) Uani 1 1 d . . . H18 H 0.9183 0.0266 0.2841 0.035 Uiso 1 1 calc R . . C19 C 1.06675(18) -0.5523(9) 0.31495(10) 0.0359(11) Uani 1 1 d . . . H19 H 1.0471 -0.5246 0.2967 0.043 Uiso 1 1 calc R . . C20 C 1.10066(18) -0.7563(10) 0.31665(10) 0.0384(11) Uani 1 1 d . . . H20 H 1.1042 -0.8643 0.2998 0.046 Uiso 1 1 calc R . . C21 C 1.12894(17) -0.7983(9) 0.34320(10) 0.0334(10) Uani 1 1 d . . . H21 H 1.1521 -0.9369 0.3449 0.040 Uiso 1 1 calc R . . C22 C 1.12352(16) -0.6361(8) 0.36774(9) 0.0268(9) Uani 1 1 d . . . C23 C 1.08902(16) -0.4337(9) 0.36447(10) 0.0306(10) Uani 1 1 d . . . H23 H 1.0853 -0.3223 0.3809 0.037 Uiso 1 1 calc R . . C24 C 1.15516(16) -0.6952(8) 0.39664(9) 0.0270(9) Uani 1 1 d . . . C25 C 1.20397(17) -0.5425(8) 0.44160(9) 0.0306(10) Uani 1 1 d . . . H25A H 1.2375 -0.5935 0.4357 0.037 Uiso 1 1 calc R . . H25B H 1.1905 -0.6872 0.4529 0.037 Uiso 1 1 calc R . . C26 C 1.20951(17) -0.3081(9) 0.46184(10) 0.0330(10) Uani 1 1 d . . . H26A H 1.1763 -0.2578 0.4682 0.040 Uiso 1 1 calc R . . H26B H 1.2229 -0.1623 0.4507 0.040 Uiso 1 1 calc R . . C27 C 1.24513(18) -0.3662(8) 0.48966(10) 0.0322(10) Uani 1 1 d . . . H27A H 1.2307 -0.5070 0.5011 0.039 Uiso 1 1 calc R . . H27B H 1.2775 -0.4277 0.4830 0.039 Uiso 1 1 calc R . . N1 N 0.55340(14) 0.8190(7) -0.00194(8) 0.0334(9) Uani 1 1 d . . . N2 N 0.66193(14) 0.9631(7) 0.07161(8) 0.0332(9) Uani 1 1 d . . . H2A H 0.6528 0.8049 0.0669 0.040 Uiso 1 1 calc R . . N3 N 0.82001(14) 0.4665(7) 0.24337(8) 0.0305(8) Uani 1 1 d . . . H3A H 0.8279 0.6260 0.2483 0.037 Uiso 1 1 calc R . . N4 N 0.94308(14) 0.2010(7) 0.32193(8) 0.0330(9) Uani 1 1 d . . . N5 N 1.06054(14) -0.3914(7) 0.33829(9) 0.0349(9) Uani 1 1 d . . . N6 N 1.17043(14) -0.4965(7) 0.41423(8) 0.0300(8) Uani 1 1 d . . . H6A H 1.1606 -0.3393 0.4095 0.036 Uiso 1 1 calc R . . O1 O 0.66194(12) 1.3829(6) 0.05720(7) 0.0362(8) Uani 1 1 d . . . O2 O 0.83221(13) 0.0414(6) 0.25313(8) 0.0401(8) Uani 1 1 d . . . O3 O 1.16706(13) -0.9220(6) 0.40260(7) 0.0420(9) Uani 1 1 d . . . Cl1 Cl 0.51910(8) 0.4935(4) 0.08956(3) 0.0703(5) Uani 1 1 d . . . O4 O 0.5242(4) 0.784(2) 0.0874(3) 0.098(3) Uiso 0.50 1 d P A 1 O5 O 0.5453(5) 0.393(2) 0.1131(3) 0.094(3) Uiso 0.50 1 d P A 1 O6 O 0.4642(5) 0.458(3) 0.0885(3) 0.117(4) Uiso 0.50 1 d P A 1 O7 O 0.5322(3) 0.3936(15) 0.06017(17) 0.0424(18) Uiso 0.50 1 d P A 1 O4A O 0.5103(8) 0.221(5) 0.0996(5) 0.199(8) Uiso 0.50 1 d P A 2 O5A O 0.5709(5) 0.530(2) 0.1036(3) 0.099(3) Uiso 0.50 1 d P A 2 O6A O 0.4818(5) 0.576(3) 0.1071(3) 0.109(4) Uiso 0.50 1 d P A 2 O7A O 0.5143(4) 0.491(2) 0.0605(2) 0.072(3) Uiso 0.50 1 d P A 2 Cl2 Cl 0.5000 0.3169(3) 0.2500 0.0365(4) Uani 1 2 d S . . O8 O 0.46951(19) 0.4758(10) 0.23050(10) 0.0785(14) Uani 1 1 d . . . O9 O 0.53074(16) 0.1570(8) 0.23245(10) 0.0642(11) 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 0.0387(3) 0.0363(3) 0.0478(3) 0.0004(2) -0.0121(2) -0.0141(2) Ag2 0.0404(2) 0.0433(2) 0.0458(2) 0.00372(17) -0.01302(18) 0.01419(17) C1 0.037(3) 0.040(3) 0.028(2) -0.003(2) -0.011(2) 0.000(2) C2 0.041(3) 0.042(3) 0.023(2) 0.007(2) -0.004(2) 0.001(2) C3 0.031(2) 0.030(2) 0.031(2) 0.0024(19) -0.0033(19) -0.0039(19) C4 0.027(2) 0.028(2) 0.028(2) 0.0017(18) -0.0056(18) 0.0027(18) C5 0.032(2) 0.030(2) 0.027(2) 0.0010(18) -0.0075(19) -0.0048(19) C6 0.027(2) 0.029(2) 0.024(2) -0.0025(18) -0.0019(18) -0.0043(18) C7 0.048(3) 0.032(2) 0.030(2) 0.003(2) -0.015(2) -0.010(2) C8 0.039(2) 0.029(2) 0.028(2) 0.0003(19) -0.011(2) -0.004(2) C9 0.038(2) 0.030(2) 0.030(2) 0.0030(19) -0.010(2) -0.003(2) C10 0.043(3) 0.028(2) 0.034(2) 0.0013(19) -0.013(2) -0.004(2) C11 0.044(3) 0.027(2) 0.034(3) 0.0028(19) -0.014(2) -0.001(2) C12 0.035(2) 0.029(2) 0.031(2) 0.0007(19) -0.012(2) -0.0012(19) C13 0.026(2) 0.024(2) 0.030(2) 0.0039(18) -0.0009(18) 0.0031(17) C14 0.038(2) 0.037(3) 0.024(2) 0.004(2) -0.004(2) -0.002(2) C15 0.044(3) 0.031(2) 0.029(2) -0.003(2) 0.001(2) 0.000(2) C16 0.034(2) 0.027(2) 0.033(2) 0.0026(19) -0.003(2) 0.0023(19) C17 0.029(2) 0.024(2) 0.028(2) 0.0059(18) -0.0007(18) 0.0003(17) C18 0.031(2) 0.029(2) 0.028(2) 0.0025(18) -0.0010(19) 0.0009(18) C19 0.039(3) 0.040(3) 0.027(2) 0.003(2) -0.009(2) -0.002(2) C20 0.044(3) 0.042(3) 0.028(2) -0.008(2) -0.009(2) 0.000(2) C21 0.033(2) 0.030(2) 0.035(3) -0.006(2) -0.009(2) 0.0045(19) C22 0.027(2) 0.026(2) 0.026(2) 0.0018(17) -0.0079(18) -0.0004(17) C23 0.033(2) 0.031(2) 0.026(2) 0.0000(19) -0.0094(19) 0.0025(19) C24 0.032(2) 0.025(2) 0.022(2) -0.0014(18) -0.0054(18) 0.0038(18) C25 0.037(2) 0.031(2) 0.021(2) -0.0008(18) -0.0131(19) 0.0072(19) C26 0.039(2) 0.030(2) 0.029(2) -0.0033(19) -0.009(2) 0.005(2) C27 0.039(2) 0.028(2) 0.027(2) -0.0033(19) -0.012(2) 0.0054(19) N1 0.0299(19) 0.034(2) 0.035(2) -0.0005(17) -0.0086(17) -0.0059(17) N2 0.045(2) 0.0242(19) 0.028(2) 0.0012(16) -0.0160(17) -0.0086(16) N3 0.038(2) 0.0219(19) 0.030(2) 0.0013(15) -0.0094(17) -0.0009(16) N4 0.033(2) 0.034(2) 0.030(2) 0.0046(17) -0.0088(17) 0.0032(17) N5 0.035(2) 0.034(2) 0.033(2) 0.0033(17) -0.0122(17) 0.0056(17) N6 0.040(2) 0.0233(18) 0.0239(18) 0.0000(15) -0.0147(16) 0.0062(16) O1 0.0443(18) 0.0268(17) 0.0355(18) 0.0004(14) -0.0105(15) -0.0091(14) O2 0.051(2) 0.0217(17) 0.045(2) 0.0008(14) -0.0165(16) 0.0008(14) O3 0.057(2) 0.0274(18) 0.0380(19) -0.0021(14) -0.0211(16) 0.0078(15) Cl1 0.0978(13) 0.0819(12) 0.0305(7) -0.0018(7) -0.0007(8) -0.0159(10) Cl2 0.0461(9) 0.0397(9) 0.0231(7) 0.000 -0.0019(7) 0.000 O8 0.088(3) 0.086(3) 0.059(3) 0.023(3) -0.011(3) 0.025(3) O9 0.067(3) 0.060(3) 0.069(3) -0.014(2) 0.029(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.173(4) . ? Ag1 N1 2.173(4) 5_665 ? Ag2 N4 2.191(4) . ? Ag2 N5 2.194(4) . ? C1 N1 1.340(6) . ? C1 C2 1.375(7) . ? C2 C3 1.376(6) . ? C3 C4 1.389(6) . ? C4 C5 1.380(6) . ? C4 C6 1.509(6) . ? C5 N1 1.351(5) . ? C6 O1 1.225(5) . ? C6 N2 1.336(5) . ? C7 N2 1.464(5) . ? C7 C8 1.507(6) . ? C8 C9 1.531(6) . ? C9 C10 1.526(6) . ? C10 C11 1.529(6) . ? C11 C12 1.505(6) . ? C12 N3 1.462(5) . ? C13 O2 1.237(5) . ? C13 N3 1.336(5) . ? C13 C17 1.496(6) . ? C14 N4 1.349(6) . ? C14 C15 1.373(6) . ? C15 C16 1.387(6) . ? C16 C17 1.387(6) . ? C17 C18 1.390(6) . ? C18 N4 1.342(5) . ? C19 N5 1.345(6) . ? C19 C20 1.380(7) . ? C20 C21 1.365(6) . ? C21 C22 1.387(6) . ? C22 C23 1.386(6) . ? C22 C24 1.509(5) . ? C23 N5 1.354(5) . ? C24 O3 1.232(5) . ? C24 N6 1.330(5) . ? C25 N6 1.469(5) . ? C25 C26 1.504(6) . ? C26 C27 1.526(6) . ? C27 C27 1.517(8) 7_746 ? Cl1 O7A 1.287(10) . ? Cl1 O5 1.315(12) . ? Cl1 O6A 1.369(14) . ? Cl1 O6 1.465(14) . ? Cl1 O7 1.467(8) . ? Cl1 O5A 1.477(12) . ? Cl1 O4A 1.50(2) . ? Cl1 O4 1.502(12) . ? Cl2 O8 1.401(4) 2_655 ? Cl2 O8 1.401(4) . ? Cl2 O9 1.429(4) . ? Cl2 O9 1.429(4) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 180.0(3) . 5_665 ? N4 Ag2 N5 173.15(14) . . ? N1 C1 C2 122.7(4) . . ? C1 C2 C3 118.8(4) . . ? C2 C3 C4 119.5(4) . . ? C5 C4 C3 118.3(4) . . ? C5 C4 C6 122.7(4) . . ? C3 C4 C6 118.9(4) . . ? N1 C5 C4 122.3(4) . . ? O1 C6 N2 123.0(4) . . ? O1 C6 C4 120.3(4) . . ? N2 C6 C4 116.6(4) . . ? N2 C7 C8 112.3(4) . . ? C7 C8 C9 110.6(4) . . ? C10 C9 C8 114.0(4) . . ? C9 C10 C11 113.3(4) . . ? C12 C11 C10 112.1(4) . . ? N3 C12 C11 112.7(4) . . ? O2 C13 N3 121.6(4) . . ? O2 C13 C17 120.6(4) . . ? N3 C13 C17 117.8(4) . . ? N4 C14 C15 122.8(4) . . ? C14 C15 C16 119.3(4) . . ? C15 C16 C17 118.9(4) . . ? C16 C17 C18 118.1(4) . . ? C16 C17 C13 124.2(4) . . ? C18 C17 C13 117.6(4) . . ? N4 C18 C17 123.4(4) . . ? N5 C19 C20 122.9(4) . . ? C21 C20 C19 118.7(4) . . ? C20 C21 C22 120.0(4) . . ? C23 C22 C21 118.4(4) . . ? C23 C22 C24 124.1(4) . . ? C21 C22 C24 117.5(4) . . ? N5 C23 C22 122.1(4) . . ? O3 C24 N6 122.7(4) . . ? O3 C24 C22 119.3(4) . . ? N6 C24 C22 117.9(4) . . ? N6 C25 C26 113.0(3) . . ? C25 C26 C27 110.6(4) . . ? C27 C27 C26 113.7(4) 7_746 . ? C1 N1 C5 118.3(4) . . ? C1 N1 Ag1 123.1(3) . . ? C5 N1 Ag1 118.5(3) . . ? C6 N2 C7 120.9(4) . . ? C13 N3 C12 121.4(4) . . ? C18 N4 C14 117.5(4) . . ? C18 N4 Ag2 118.9(3) . . ? C14 N4 Ag2 123.7(3) . . ? C19 N5 C23 117.9(4) . . ? C19 N5 Ag2 118.6(3) . . ? C23 N5 Ag2 123.5(3) . . ? C24 N6 C25 120.0(4) . . ? O7A Cl1 O5 143.1(7) . . ? O7A Cl1 O6A 123.5(7) . . ? O5 Cl1 O6A 91.6(8) . . ? O7A Cl1 O6 86.8(7) . . ? O5 Cl1 O6 116.1(8) . . ? O6A Cl1 O6 45.5(7) . . ? O7A Cl1 O7 28.0(5) . . ? O5 Cl1 O7 115.1(6) . . ? O6A Cl1 O7 147.3(7) . . ? O6 Cl1 O7 103.2(7) . . ? O7A Cl1 O5A 116.3(7) . . ? O5 Cl1 O5A 45.3(6) . . ? O6A Cl1 O5A 114.1(8) . . ? O6 Cl1 O5A 156.9(8) . . ? O7 Cl1 O5A 98.4(6) . . ? O7A Cl1 O4A 106.5(10) . . ? O5 Cl1 O4A 58.7(8) . . ? O6A Cl1 O4A 89.1(10) . . ? O6 Cl1 O4A 73.5(9) . . ? O7 Cl1 O4A 89.4(9) . . ? O5A Cl1 O4A 98.9(9) . . ? O7A Cl1 O4 87.0(6) . . ? O5 Cl1 O4 113.3(7) . . ? O6A Cl1 O4 78.5(7) . . ? O6 Cl1 O4 102.4(7) . . ? O7 Cl1 O4 105.2(5) . . ? O5A Cl1 O4 79.4(6) . . ? O4A Cl1 O4 165.4(9) . . ? O8 Cl2 O8 108.6(5) 2_655 . ? O8 Cl2 O9 110.2(3) 2_655 . ? O8 Cl2 O9 109.0(3) . . ? O8 Cl2 O9 109.0(3) 2_655 2_655 ? O8 Cl2 O9 110.2(3) . 2_655 ? O9 Cl2 O9 109.8(4) . 2_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.133 _refine_diff_density_min -0.850 _refine_diff_density_rms 0.113 #======== data_compound AgLNO3 _database_code_CSD 189554 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 Ag N5 O5' _chemical_formula_weight 496.28 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.0952(1) _cell_length_b 6.9931(2) _cell_length_c 13.6355(4) _cell_angle_alpha 93.510(2) _cell_angle_beta 98.761(2) _cell_angle_gamma 95.219(2) _cell_volume 476.80(2) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'thin plate' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 252 _exptl_absorpt_coefficient_mu 1.099 _exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.7760 _exptl_absorpt_correction_T_max 0.9562 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3178 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 26.37 _reflns_number_total 1861 _reflns_number_gt 1683 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, 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^)+(0.0363P)^2^+0.7733P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1861 _refine_ls_number_parameters 144 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0897 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.0000 0.5000 0.5000 0.04628(19) Uani 1 2 d S . . C1 C 0.5041(7) 0.3546(6) 0.6154(3) 0.0326(8) Uani 1 1 d . . . H1 H 0.4412 0.2450 0.5733 0.039 Uiso 1 1 calc R . . C2 C 0.7389(8) 0.3533(6) 0.6796(3) 0.0324(8) Uani 1 1 d . . . H2 H 0.8321 0.2449 0.6817 0.039 Uiso 1 1 calc R . . C3 C 0.8338(7) 0.5177(5) 0.7415(2) 0.0281(8) Uani 1 1 d . . . H3 H 0.9947 0.5222 0.7846 0.034 Uiso 1 1 calc R . . C4 C 0.6875(6) 0.6748(5) 0.7386(2) 0.0233(7) Uani 1 1 d . . . C5 C 0.4525(7) 0.6644(5) 0.6719(2) 0.0281(8) Uani 1 1 d . . . H5 H 0.3541 0.7702 0.6695 0.034 Uiso 1 1 calc R . . C6 C 0.7979(6) 0.8510(5) 0.8059(2) 0.0230(7) Uani 1 1 d . . . O1 O 1.0414(5) 0.8842(4) 0.83278(19) 0.0349(6) Uani 1 1 d . . . N1 N 0.3607(6) 0.5068(5) 0.6103(2) 0.0310(7) Uani 1 1 d . . . C7 C 0.7208(6) 1.1344(5) 0.9048(2) 0.0259(7) Uani 1 1 d . . . H7A H 0.8619 1.2090 0.8792 0.031 Uiso 1 1 calc R . . H7B H 0.7958 1.0937 0.9690 0.031 Uiso 1 1 calc R . . C8 C 0.5021(6) 1.2605(5) 0.9186(3) 0.0260(7) Uani 1 1 d . . . H8A H 0.3605 1.1865 0.9442 0.031 Uiso 1 1 calc R . . H8B H 0.4275 1.3025 0.8546 0.031 Uiso 1 1 calc R . . C9 C 0.6072(6) 1.4359(5) 0.9902(3) 0.0266(7) Uani 1 1 d . . . H9A H 0.6889 1.3928 1.0529 0.032 Uiso 1 1 calc R . . H9B H 0.7448 1.5112 0.9630 0.032 Uiso 1 1 calc R . . N2 N 0.6256(5) 0.9641(4) 0.8366(2) 0.0257(6) Uani 1 1 d . . . H2A H 0.4573 0.9369 0.8163 0.031 Uiso 1 1 calc R . . N3 N 0.0000 1.0000 0.5000 0.0635(19) Uani 1 2 d SD . . O2 O 0.1067(19) 0.8656(10) 0.5181(6) 0.071(2) Uani 0.50 1 d PD . . O3 O 0.087(2) 1.0893(16) 0.4255(8) 0.083(2) Uiso 0.40 1 d PD . . O4 O -0.194(2) 1.0579(19) 0.5177(10) 0.083(2) Uiso 0.40 1 d PD . . O3A O -0.053(12) 1.117(6) 0.560(2) 0.15(2) Uiso 0.10 1 d PD . . O4A O -0.045(13) 1.037(7) 0.4106(15) 0.15(2) Uiso 0.10 1 d PD . . 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 0.0272(2) 0.0724(4) 0.0317(2) -0.0130(2) -0.00793(16) -0.0020(2) C1 0.0347(19) 0.032(2) 0.0285(18) -0.0057(15) 0.0057(14) -0.0045(16) C2 0.038(2) 0.029(2) 0.0305(18) -0.0018(15) 0.0056(15) 0.0061(16) C3 0.0239(17) 0.035(2) 0.0241(16) 0.0014(14) -0.0001(13) 0.0038(15) C4 0.0201(15) 0.0270(18) 0.0215(15) -0.0023(13) 0.0032(12) -0.0017(13) C5 0.0220(16) 0.034(2) 0.0271(17) -0.0059(14) 0.0019(13) 0.0024(14) C6 0.0209(16) 0.0251(18) 0.0220(15) 0.0005(13) 0.0013(12) 0.0013(13) O1 0.0170(12) 0.0406(15) 0.0427(15) -0.0126(12) -0.0024(10) 0.0026(10) N1 0.0253(15) 0.0387(18) 0.0258(14) -0.0068(13) 0.0013(11) -0.0025(13) C7 0.0219(16) 0.0237(18) 0.0291(17) -0.0041(14) -0.0015(13) 0.0000(13) C8 0.0208(16) 0.0249(18) 0.0302(17) -0.0046(14) 0.0017(13) -0.0002(13) C9 0.0206(16) 0.0265(19) 0.0299(17) -0.0059(14) 0.0002(13) -0.0003(13) N2 0.0167(13) 0.0271(16) 0.0304(15) -0.0061(12) -0.0004(11) -0.0014(11) N3 0.036(3) 0.050(4) 0.098(5) -0.036(4) 0.011(3) -0.003(3) O2 0.101(6) 0.035(4) 0.072(5) 0.003(4) -0.018(5) 0.041(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 2.185(3) 2_566 ? Ag1 N1 2.185(3) . ? Ag1 O2 2.554(8) . ? Ag1 O2 2.554(8) 2_566 ? C1 N1 1.344(5) . ? C1 C2 1.372(5) . ? C2 C3 1.387(5) . ? C3 C4 1.382(5) . ? C4 C5 1.382(5) . ? C4 C6 1.502(4) . ? C5 N1 1.346(4) . ? C6 O1 1.235(4) . ? C6 N2 1.330(4) . ? C7 N2 1.463(4) . ? C7 C8 1.509(5) . ? C8 C9 1.523(4) . ? C9 C9 1.519(7) 2_687 ? N3 O2 1.149(6) 2_576 ? N3 O2 1.149(6) . ? N3 O4 1.155(10) . ? N3 O4 1.155(10) 2_576 ? N3 O3A 1.200(15) . ? N3 O3A 1.200(15) 2_576 ? N3 O4A 1.253(15) . ? N3 O4A 1.253(15) 2_576 ? N3 O3 1.334(9) 2_576 ? N3 O3 1.334(9) . ? O2 O4 0.882(12) 2_576 ? O2 O3A 1.07(3) 2_576 ? O2 O4A 1.25(3) 2_576 ? O2 O3 1.386(14) 2_576 ? O3 O4A 0.73(7) . ? O3 O2 1.386(14) 2_576 ? O3 O4 1.424(16) 2_576 ? O3 O3A 1.47(4) 2_576 ? O4 O2 0.882(12) 2_576 ? O4 O3A 0.90(6) . ? O4 O3 1.424(16) 2_576 ? O4 O4A 1.66(4) 2_576 ? O4 O4A 1.75(4) . ? O3A O2 1.07(3) 2_576 ? O3A O4A 1.29(3) 2_576 ? O3A O3 1.47(4) 2_576 ? O4A O2 1.25(3) 2_576 ? O4A O3A 1.29(3) 2_576 ? O4A O4 1.66(4) 2_576 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 180.000(1) 2_566 . ? N1 Ag1 O2 96.51(19) 2_566 . ? N1 Ag1 O2 83.49(19) . . ? N1 Ag1 O2 83.49(19) 2_566 2_566 ? N1 Ag1 O2 96.51(19) . 2_566 ? O2 Ag1 O2 180.000(1) . 2_566 ? N1 C1 C2 123.1(3) . . ? C1 C2 C3 118.3(3) . . ? C4 C3 C2 119.5(3) . . ? C5 C4 C3 118.6(3) . . ? C5 C4 C6 123.4(3) . . ? C3 C4 C6 118.0(3) . . ? N1 C5 C4 122.4(3) . . ? O1 C6 N2 122.3(3) . . ? O1 C6 C4 119.9(3) . . ? N2 C6 C4 117.9(3) . . ? C1 N1 C5 118.0(3) . . ? C1 N1 Ag1 120.3(2) . . ? C5 N1 Ag1 121.6(2) . . ? N2 C7 C8 112.5(3) . . ? C7 C8 C9 111.2(3) . . ? C9 C9 C8 113.5(3) 2_687 . ? C6 N2 C7 120.4(3) . . ? O2 N3 O2 180.0(9) 2_576 . ? O2 N3 O4 45.0(6) 2_576 . ? O2 N3 O4 135.0(6) . . ? O2 N3 O4 135.0(6) 2_576 2_576 ? O2 N3 O4 45.0(6) . 2_576 ? O4 N3 O4 180.0(13) . 2_576 ? O2 N3 O3A 54.3(16) 2_576 . ? O2 N3 O3A 125.7(16) . . ? O4 N3 O3A 45(3) . . ? O4 N3 O3A 135(3) 2_576 . ? O2 N3 O3A 125.7(16) 2_576 2_576 ? O2 N3 O3A 54.3(16) . 2_576 ? O4 N3 O3A 135(3) . 2_576 ? O4 N3 O3A 45(3) 2_576 2_576 ? O3A N3 O3A 180.00(4) . 2_576 ? O2 N3 O4A 62.4(15) 2_576 . ? O2 N3 O4A 117.6(15) . . ? O4 N3 O4A 93(2) . . ? O4 N3 O4A 87(2) 2_576 . ? O3A N3 O4A 116.4(13) . . ? O3A N3 O4A 63.6(13) 2_576 . ? O2 N3 O4A 117.6(15) 2_576 2_576 ? O2 N3 O4A 62.4(15) . 2_576 ? O4 N3 O4A 87(2) . 2_576 ? O4 N3 O4A 93(2) 2_576 2_576 ? O3A N3 O4A 63.6(13) . 2_576 ? O3A N3 O4A 116.4(13) 2_576 2_576 ? O4A N3 O4A 180.00(4) . 2_576 ? O2 N3 O3 112.7(6) 2_576 2_576 ? O2 N3 O3 67.3(6) . 2_576 ? O4 N3 O3 69.4(7) . 2_576 ? O4 N3 O3 110.6(7) 2_576 2_576 ? O3A N3 O3 71(2) . 2_576 ? O3A N3 O3 109(2) 2_576 2_576 ? O4A N3 O3 147(3) . 2_576 ? O4A N3 O3 33(3) 2_576 2_576 ? O2 N3 O3 67.3(6) 2_576 . ? O2 N3 O3 112.7(6) . . ? O4 N3 O3 110.6(7) . . ? O4 N3 O3 69.4(7) 2_576 . ? O3A N3 O3 109(2) . . ? O3A N3 O3 71(2) 2_576 . ? O4A N3 O3 33(3) . . ? O4A N3 O3 147(3) 2_576 . ? O3 N3 O3 180.000(5) 2_576 . ? O4 O2 O3A 54(3) 2_576 2_576 ? O4 O2 N3 67.8(8) 2_576 . ? O3A O2 N3 65.2(10) 2_576 . ? O4 O2 O4A 109(3) 2_576 2_576 ? O3A O2 O4A 127.7(16) 2_576 2_576 ? N3 O2 O4A 62.9(9) . 2_576 ? O4 O2 O3 127.9(12) 2_576 2_576 ? O3A O2 O3 114(3) 2_576 2_576 ? N3 O2 O3 62.7(6) . 2_576 ? O4A O2 O3 32(3) 2_576 2_576 ? O4 O2 Ag1 130.1(12) 2_576 . ? O3A O2 Ag1 94(2) 2_576 . ? N3 O2 Ag1 138.3(6) . . ? O4A O2 Ag1 121(3) 2_576 . ? O3 O2 Ag1 98.5(7) 2_576 . ? O4A O3 N3 67.6(16) . . ? O4A O3 O2 64(3) . 2_576 ? N3 O3 O2 50.0(4) . 2_576 ? O4A O3 O4 95(2) . 2_576 ? N3 O3 O4 49.4(5) . 2_576 ? O2 O3 O4 98.5(7) 2_576 2_576 ? O4A O3 O3A 62(3) . 2_576 ? N3 O3 O3A 50.4(12) . 2_576 ? O2 O3 O3A 94.1(18) 2_576 2_576 ? O4 O3 O3A 36(2) 2_576 2_576 ? O2 O4 O3A 74(3) 2_576 . ? O2 O4 N3 67.1(8) 2_576 . ? O3A O4 N3 70.2(17) . . ? O2 O4 O3 125.9(13) 2_576 2_576 ? O3A O4 O3 75(2) . 2_576 ? N3 O4 O3 61.2(6) . 2_576 ? O2 O4 O4A 104(2) 2_576 2_576 ? O3A O4 O4A 51(2) . 2_576 ? N3 O4 O4A 49.0(14) . 2_576 ? O3 O4 O4A 26(2) 2_576 2_576 ? O2 O4 O4A 42.3(19) 2_576 . ? O3A O4 O4A 99(3) . . ? N3 O4 O4A 45.7(12) . . ? O3 O4 O4A 102.5(11) 2_576 . ? O4A O4 O4A 94.6(7) 2_576 . ? O4 O3A O2 52(2) . 2_576 ? O4 O3A N3 64.9(16) . . ? O2 O3A N3 60.5(11) 2_576 . ? O4 O3A O4A 97(3) . 2_576 ? O2 O3A O4A 120(2) 2_576 2_576 ? N3 O3A O4A 60.2(11) . 2_576 ? O4 O3A O3 69(3) . 2_576 ? O2 O3A O3 108(3) 2_576 2_576 ? N3 O3A O3 58.9(15) . 2_576 ? O4A O3A O3 30(3) 2_576 2_576 ? O3 O4A O2 85(4) . 2_576 ? O3 O4A N3 80(3) . . ? O2 O4A N3 54.7(10) 2_576 . ? O3 O4A O3A 89(4) . 2_576 ? O2 O4A O3A 110.7(18) 2_576 2_576 ? N3 O4A O3A 56.2(10) . 2_576 ? O3 O4A O4 59(2) . 2_576 ? O2 O4A O4 93.1(16) 2_576 2_576 ? N3 O4A O4 44.1(10) . 2_576 ? O3A O4A O4 33(2) 2_576 2_576 ? O3 O4A O4 104(3) . . ? O2 O4A O4 28.4(12) 2_576 . ? N3 O4A O4 41.3(12) . . ? O3A O4A O4 90(2) 2_576 . ? O4 O4A O4 85.4(7) 2_576 . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.560 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.081 #======== data_compound AgLCF3SO3 _database_code_CSD 189555 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H22 Ag F3 N4 O5 S' _chemical_formula_weight 583.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.12890(10) _cell_length_b 10.0509(2) _cell_length_c 13.0946(2) _cell_angle_alpha 108.6080(10) _cell_angle_beta 107.6770(10) _cell_angle_gamma 93.5970(10) _cell_volume 1067.82(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4940 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'Rectangular Shape, Cut' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 1.109 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 1996)' _exptl_absorpt_correction_T_min 0.8747 _exptl_absorpt_correction_T_max 0.9944 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6625 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4649 _reflns_number_gt 4230 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0304P)^2^+1.2063P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4649 _refine_ls_number_parameters 298 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.134 _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 0.52842(3) 0.24976(2) 0.499932(18) 0.02909(8) Uani 1 1 d . . . O1 O 0.4481(2) -0.09673(19) 0.84051(17) 0.0265(4) Uani 1 1 d . . . O2 O 0.5669(2) 0.5948(2) 0.15781(18) 0.0289(4) Uani 1 1 d . . . N1 N 0.5966(3) 0.1344(2) 0.61636(19) 0.0241(5) Uani 1 1 d . . . N2 N 0.3731(3) 0.1171(2) 0.85566(19) 0.0212(4) Uani 1 1 d . . . H2A H 0.3862 0.1970 0.8443 0.025 Uiso 1 1 calc R . . N3 N 0.4301(3) 0.3601(2) 0.38403(19) 0.0230(5) Uani 1 1 d . . . N4 N 0.6389(3) 0.3797(2) 0.1404(2) 0.0227(5) Uani 1 1 d . . . H4A H 0.6269 0.3007 0.1533 0.027 Uiso 1 1 calc R . . C1 C 0.7273(3) 0.0760(3) 0.6249(2) 0.0271(6) Uani 1 1 d . . . H1 H 0.7872 0.0873 0.5802 0.032 Uiso 1 1 calc R . . C2 C 0.7761(3) 0.0009(3) 0.6967(3) 0.0280(6) Uani 1 1 d . . . H2 H 0.8685 -0.0370 0.7016 0.034 Uiso 1 1 calc R . . C3 C 0.6879(3) -0.0182(3) 0.7613(2) 0.0240(5) Uani 1 1 d . . . H3 H 0.7183 -0.0709 0.8096 0.029 Uiso 1 1 calc R . . C4 C 0.5528(3) 0.0417(3) 0.7541(2) 0.0191(5) Uani 1 1 d . . . C5 C 0.5111(3) 0.1174(3) 0.6809(2) 0.0206(5) Uani 1 1 d . . . H5 H 0.4205 0.1583 0.6760 0.025 Uiso 1 1 calc R . . C6 C 0.4524(3) 0.0153(3) 0.8207(2) 0.0186(5) Uani 1 1 d . . . C7 C 0.2642(3) 0.0949(3) 0.9130(2) 0.0247(6) Uani 1 1 d . . . H7A H 0.3229 0.0932 0.9888 0.030 Uiso 1 1 calc R . . H7B H 0.1950 0.0024 0.8682 0.030 Uiso 1 1 calc R . . C8 C 0.1669(3) 0.2121(3) 0.9266(2) 0.0241(5) Uani 1 1 d . . . H8A H 0.1051 0.2114 0.8507 0.029 Uiso 1 1 calc R . . H8B H 0.2362 0.3049 0.9689 0.029 Uiso 1 1 calc R . . C9 C 0.0574(3) 0.1914(3) 0.9909(2) 0.0237(5) Uani 1 1 d . . . H9A H -0.0049 0.0952 0.9517 0.028 Uiso 1 1 calc R . . H9B H 0.1205 0.1989 1.0685 0.028 Uiso 1 1 calc R . . C10 C 0.2917(3) 0.4059(3) 0.3708(2) 0.0279(6) Uani 1 1 d . . . H10 H 0.2311 0.3874 0.4129 0.034 Uiso 1 1 calc R . . C11 C 0.2361(3) 0.4785(3) 0.2979(3) 0.0295(6) Uani 1 1 d . . . H11 H 0.1398 0.5096 0.2914 0.035 Uiso 1 1 calc R . . C12 C 0.3230(3) 0.5053(3) 0.2346(2) 0.0253(6) Uani 1 1 d . . . H12 H 0.2881 0.5565 0.1857 0.030 Uiso 1 1 calc R . . C13 C 0.4638(3) 0.4548(3) 0.2445(2) 0.0181(5) Uani 1 1 d . . . C14 C 0.5137(3) 0.3844(3) 0.3209(2) 0.0197(5) Uani 1 1 d . . . H14 H 0.6097 0.3524 0.3289 0.024 Uiso 1 1 calc R . . C15 C 0.5615(3) 0.4829(3) 0.1773(2) 0.0193(5) Uani 1 1 d . . . C16 C 0.7434(3) 0.3980(3) 0.0789(3) 0.0267(6) Uani 1 1 d . . . H16A H 0.8138 0.4902 0.1215 0.032 Uiso 1 1 calc R . . H16B H 0.6817 0.3985 0.0034 0.032 Uiso 1 1 calc R . . C17 C 0.8392(3) 0.2796(3) 0.0640(2) 0.0232(5) Uani 1 1 d . . . H17A H 0.7689 0.1873 0.0216 0.028 Uiso 1 1 calc R . . H17B H 0.9014 0.2793 0.1394 0.028 Uiso 1 1 calc R . . C18 C 0.9474(3) 0.2995(3) -0.0007(2) 0.0238(5) Uani 1 1 d . . . H18A H 1.0098 0.3958 0.0380 0.029 Uiso 1 1 calc R . . H18B H 0.8839 0.2917 -0.0783 0.029 Uiso 1 1 calc R . . C19 C 1.0768(3) 0.2851(3) 0.5603(2) 0.0286(6) Uani 1 1 d D . . F1 F 1.2034(2) 0.2325(3) 0.54669(19) 0.0531(6) Uani 1 1 d D . . F2 F 1.1127(3) 0.4253(2) 0.5922(2) 0.0593(6) Uani 1 1 d D . . F3 F 1.0533(2) 0.2578(2) 0.64737(16) 0.0466(5) Uani 1 1 d D . . S1 S 0.90788(8) 0.21021(8) 0.42833(6) 0.02699(15) Uani 1 1 d . . . O3 O 0.7886(3) 0.2801(3) 0.4627(2) 0.0471(6) Uani 1 1 d . . . O4 O 0.8854(3) 0.0605(3) 0.4065(2) 0.0547(7) Uani 1 1 d . . . O5 O 0.9558(3) 0.2527(3) 0.34708(19) 0.0431(6) 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 0.03979(14) 0.02763(12) 0.02881(12) 0.01635(9) 0.01720(9) 0.00704(9) O1 0.0345(11) 0.0189(9) 0.0365(11) 0.0163(8) 0.0187(9) 0.0097(8) O2 0.0382(11) 0.0221(10) 0.0402(11) 0.0199(9) 0.0218(9) 0.0119(8) N1 0.0308(12) 0.0217(11) 0.0252(11) 0.0111(9) 0.0143(10) 0.0039(9) N2 0.0243(11) 0.0195(10) 0.0296(12) 0.0148(9) 0.0155(10) 0.0080(8) N3 0.0262(11) 0.0233(11) 0.0230(11) 0.0096(9) 0.0123(9) 0.0025(9) N4 0.0287(12) 0.0203(11) 0.0336(12) 0.0174(9) 0.0212(10) 0.0105(9) C1 0.0246(14) 0.0282(14) 0.0322(15) 0.0088(12) 0.0174(12) 0.0027(11) C2 0.0189(13) 0.0323(15) 0.0344(15) 0.0107(12) 0.0120(11) 0.0070(11) C3 0.0227(13) 0.0231(13) 0.0269(14) 0.0106(11) 0.0071(11) 0.0071(10) C4 0.0214(12) 0.0150(11) 0.0228(12) 0.0069(10) 0.0100(10) 0.0030(9) C5 0.0238(13) 0.0202(12) 0.0223(12) 0.0089(10) 0.0120(10) 0.0067(10) C6 0.0179(12) 0.0209(12) 0.0185(12) 0.0081(10) 0.0072(10) 0.0037(9) C7 0.0284(14) 0.0276(14) 0.0323(14) 0.0184(12) 0.0205(12) 0.0118(11) C8 0.0269(13) 0.0254(13) 0.0309(14) 0.0172(11) 0.0164(11) 0.0091(11) C9 0.0284(14) 0.0253(13) 0.0283(14) 0.0157(11) 0.0174(11) 0.0097(11) C10 0.0222(13) 0.0342(15) 0.0306(14) 0.0099(12) 0.0161(12) 0.0007(11) C11 0.0189(13) 0.0369(16) 0.0348(16) 0.0120(13) 0.0118(12) 0.0092(11) C12 0.0229(13) 0.0276(14) 0.0284(14) 0.0114(11) 0.0101(11) 0.0098(11) C13 0.0198(12) 0.0155(11) 0.0203(12) 0.0061(9) 0.0090(10) 0.0030(9) C14 0.0203(12) 0.0195(12) 0.0246(13) 0.0101(10) 0.0121(10) 0.0064(9) C15 0.0209(12) 0.0186(12) 0.0207(12) 0.0084(10) 0.0086(10) 0.0042(9) C16 0.0320(15) 0.0275(14) 0.0387(16) 0.0211(12) 0.0256(13) 0.0128(11) C17 0.0278(13) 0.0228(13) 0.0287(13) 0.0149(11) 0.0158(11) 0.0095(10) C18 0.0270(14) 0.0243(13) 0.0307(14) 0.0153(11) 0.0178(12) 0.0088(10) C19 0.0269(14) 0.0323(15) 0.0282(15) 0.0115(12) 0.0112(12) 0.0029(11) F1 0.0244(10) 0.0875(17) 0.0543(13) 0.0310(12) 0.0143(9) 0.0227(10) F2 0.0669(15) 0.0381(12) 0.0576(14) 0.0141(10) 0.0067(12) -0.0078(10) F3 0.0431(11) 0.0682(14) 0.0317(10) 0.0256(10) 0.0106(9) 0.0009(10) S1 0.0211(3) 0.0358(4) 0.0292(4) 0.0166(3) 0.0102(3) 0.0058(3) O3 0.0272(12) 0.0815(19) 0.0495(14) 0.0344(14) 0.0215(11) 0.0257(12) O4 0.0654(18) 0.0354(13) 0.0492(15) 0.0145(12) 0.0033(13) -0.0047(12) O5 0.0362(12) 0.0680(16) 0.0353(12) 0.0272(12) 0.0178(10) 0.0065(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.168(2) . ? Ag1 N3 2.170(2) . ? Ag1 O3 2.584(2) . ? O1 C6 1.234(3) . ? O2 C15 1.231(3) . ? N1 C5 1.352(3) . ? N1 C1 1.353(4) . ? N2 C6 1.332(3) . ? N2 C7 1.461(3) . ? N3 C14 1.347(3) . ? N3 C10 1.352(4) . ? N4 C15 1.336(3) . ? N4 C16 1.460(3) . ? C1 C2 1.375(4) . ? C2 C3 1.377(4) . ? C3 C4 1.397(4) . ? C4 C5 1.387(3) . ? C4 C6 1.509(3) . ? C7 C8 1.517(4) . ? C8 C9 1.532(3) . ? C9 C18 1.526(4) 1_456 ? C10 C11 1.378(4) . ? C11 C12 1.380(4) . ? C12 C13 1.396(4) . ? C13 C14 1.387(3) . ? C13 C15 1.502(3) . ? C16 C17 1.519(4) . ? C17 C18 1.525(3) . ? C18 C9 1.526(4) 1_654 ? C19 F2 1.324(3) . ? C19 F3 1.327(3) . ? C19 F1 1.337(3) . ? C19 S1 1.827(3) . ? S1 O4 1.428(3) . ? S1 O5 1.433(2) . ? S1 O3 1.440(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N3 172.61(8) . . ? N1 Ag1 O3 98.16(8) . . ? N3 Ag1 O3 89.18(8) . . ? C5 N1 C1 118.3(2) . . ? C5 N1 Ag1 121.87(18) . . ? C1 N1 Ag1 119.79(18) . . ? C6 N2 C7 120.2(2) . . ? C14 N3 C10 117.9(2) . . ? C14 N3 Ag1 117.25(17) . . ? C10 N3 Ag1 124.82(18) . . ? C15 N4 C16 120.8(2) . . ? N1 C1 C2 122.5(3) . . ? C1 C2 C3 119.2(3) . . ? C2 C3 C4 119.2(3) . . ? C5 C4 C3 118.7(2) . . ? C5 C4 C6 122.0(2) . . ? C3 C4 C6 119.2(2) . . ? N1 C5 C4 122.1(2) . . ? O1 C6 N2 123.7(2) . . ? O1 C6 C4 119.4(2) . . ? N2 C6 C4 117.0(2) . . ? N2 C7 C8 111.2(2) . . ? C7 C8 C9 111.0(2) . . ? C18 C9 C8 113.5(2) 1_456 . ? N3 C10 C11 122.6(2) . . ? C10 C11 C12 119.5(3) . . ? C11 C12 C13 118.7(3) . . ? C14 C13 C12 118.7(2) . . ? C14 C13 C15 121.2(2) . . ? C12 C13 C15 120.0(2) . . ? N3 C14 C13 122.6(2) . . ? O2 C15 N4 123.3(2) . . ? O2 C15 C13 120.6(2) . . ? N4 C15 C13 116.0(2) . . ? N4 C16 C17 111.4(2) . . ? C16 C17 C18 111.0(2) . . ? C17 C18 C9 113.4(2) . 1_654 ? F2 C19 F3 107.2(2) . . ? F2 C19 F1 106.7(3) . . ? F3 C19 F1 107.3(2) . . ? F2 C19 S1 111.6(2) . . ? F3 C19 S1 112.5(2) . . ? F1 C19 S1 111.2(2) . . ? O4 S1 O5 115.50(17) . . ? O4 S1 O3 114.18(18) . . ? O5 S1 O3 115.23(15) . . ? O4 S1 C19 104.39(15) . . ? O5 S1 C19 103.61(14) . . ? O3 S1 C19 101.49(15) . . ? S1 O3 Ag1 146.27(17) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.502 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.083