Electronic Supplementary Material for CrystEngComm This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Dr Kumar Biradha' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Kharagpur 721302 INDIA ; _publ_contact_author_email KBIRADHA@CHEM.IITKGP.ERNET.IN _publ_section_title ; Coordination Polymers of Ag(I) with di-Schiff base and diaminoalkanes: double helix, ladder, CdSO4 and zigzag-chain networks ; loop_ _publ_author_name 'Kumar Biradha' 'Madhushree Sarkar' data_2b _database_code_depnum_ccdc_archive 'CCDC 238916' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H18 N4' _chemical_formula_weight 266.34 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' _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 13.361(3) _cell_length_b 11.510(2) _cell_length_c 9.3370(19) _cell_angle_alpha 90.00 _cell_angle_beta 102.89(3) _cell_angle_gamma 90.00 _cell_volume 1399.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 14 _exptl_crystal_description Flakes _exptl_crystal_colour Pale-yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4-MACH3 _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1242 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 24.95 _reflns_number_total 1183 _reflns_number_gt 785 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction CAD4 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0731P)^2^+0.8572P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0044(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1183 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0900 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1664 _refine_ls_wR_factor_gt 0.1393 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 N1 N 0.30369(18) 0.02900(18) 0.2323(3) 0.0728(8) Uani 1 1 d . . . N2 N 0.43499(15) 0.37356(15) 0.0611(2) 0.0513(6) Uani 1 1 d . . . C1 C 0.36366(16) 0.20496(18) 0.1402(2) 0.0425(6) Uani 1 1 d . . . C2 C 0.30478(18) 0.2682(2) 0.2163(2) 0.0497(7) Uani 1 1 d . . . H2 H 0.3042 0.3489 0.2110 0.060 Uiso 1 1 calc R . . C3 C 0.24746(19) 0.2126(2) 0.2993(3) 0.0555(7) Uani 1 1 d . . . H3 H 0.2082 0.2548 0.3517 0.067 Uiso 1 1 calc R . . C4 C 0.2488(2) 0.0927(2) 0.3044(3) 0.0627(8) Uani 1 1 d . . . H4 H 0.2094 0.0552 0.3608 0.075 Uiso 1 1 calc R . . C5 C 0.3590(2) 0.0856(2) 0.1522(3) 0.0586(8) Uani 1 1 d . . . H5 H 0.3973 0.0414 0.1005 0.070 Uiso 1 1 calc R . . C6 C 0.42898(17) 0.26351(18) 0.0513(2) 0.0436(6) Uani 1 1 d . . . C7 C 0.4825(2) 0.1884(2) -0.0397(3) 0.0578(7) Uani 1 1 d . . . H7A H 0.5214 0.2365 -0.0915 0.087 Uiso 1 1 calc R . . H7B H 0.4324 0.1451 -0.1091 0.087 Uiso 1 1 calc R . . H7C H 0.5278 0.1357 0.0231 0.087 Uiso 1 1 calc R . . C8 C 0.4997(2) 0.4370(2) -0.0184(3) 0.0584(7) Uani 1 1 d . . . H8A H 0.4740 0.4265 -0.1233 0.070 Uiso 1 1 calc . . . H8B H 0.5691 0.4067 0.0076 0.070 Uiso 1 1 calc . . . 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 N1 0.0860(17) 0.0377(12) 0.110(2) 0.0127(12) 0.0556(15) -0.0033(11) N2 0.0604(12) 0.0365(11) 0.0651(13) 0.0051(9) 0.0315(10) -0.0042(9) C1 0.0449(12) 0.0320(11) 0.0543(13) 0.0026(9) 0.0190(10) -0.0024(9) C2 0.0615(15) 0.0327(12) 0.0623(15) 0.0033(10) 0.0292(12) 0.0020(10) C3 0.0578(15) 0.0506(15) 0.0666(16) 0.0067(12) 0.0317(13) 0.0045(12) C4 0.0621(16) 0.0577(16) 0.0783(18) 0.0145(13) 0.0369(14) -0.0050(13) C5 0.0719(17) 0.0307(12) 0.0851(18) 0.0005(11) 0.0429(15) 0.0013(11) C6 0.0489(12) 0.0354(12) 0.0506(13) -0.0002(9) 0.0203(10) -0.0017(10) C7 0.0638(16) 0.0491(14) 0.0697(17) -0.0053(12) 0.0344(14) -0.0022(12) C8 0.0678(15) 0.0452(14) 0.0721(16) 0.0035(12) 0.0370(13) -0.0085(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 N1 C4 1.323(3) . ? N1 C5 1.333(3) . ? N2 C6 1.271(3) . ? N2 C8 1.455(3) . ? C1 C2 1.380(3) . ? C1 C5 1.381(3) . ? C1 C6 1.492(3) . ? C2 C3 1.364(3) . ? C3 C4 1.381(4) . ? C6 C7 1.500(3) . ? C8 C8 1.491(5) 5_665 ? 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 C4 N1 C5 117.0(2) . . ? C6 N2 C8 119.90(19) . . ? C2 C1 C5 116.2(2) . . ? C2 C1 C6 121.30(19) . . ? C5 C1 C6 122.51(19) . . ? C3 C2 C1 120.1(2) . . ? C2 C3 C4 118.9(2) . . ? N1 C4 C3 122.8(2) . . ? N1 C5 C1 125.0(2) . . ? N2 C6 C1 116.46(19) . . ? N2 C6 C7 125.7(2) . . ? C1 C6 C7 117.80(19) . . ? N2 C8 C8 110.1(2) . 5_665 ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 24.95 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.179 _refine_diff_density_min -0.162 _refine_diff_density_rms 0.040 #=====END data_3 _database_code_depnum_ccdc_archive 'CCDC 238917' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H18 Ag N5 O3' _chemical_formula_weight 436.22 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 Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 14.947(3) _cell_length_b 11.761(2) _cell_length_c 10.047(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1766.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 14 _exptl_crystal_description prisms _exptl_crystal_colour white _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.167 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4-MACH3 _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4633 _diffrn_reflns_av_R_equivalents 0.4170 _diffrn_reflns_av_sigmaI/netI 0.2552 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3007 _reflns_number_gt 1645 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction CAD4 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0474P)^2^+2.4890P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0003(11) _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 0.0(3) _refine_ls_number_reflns 3007 _refine_ls_number_parameters 238 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1462 _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.1860 _refine_ls_wR_factor_gt 0.1437 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.019 _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 0.67638(5) 0.77756(12) 0.2608(2) 0.0648(4) Uani 0.912(4) 1 d P . 1 Ag2 Ag 0.6755(5) 0.6833(11) 0.262(2) 0.055(4) Uani 0.088(4) 1 d P . 2 N1 N 0.5490(7) 0.8635(10) 0.1601(11) 0.067(3) Uani 1 1 d . . . N2 N 0.5499(6) 0.6749(11) 0.3585(11) 0.072(3) Uani 1 1 d . . . C1 C 0.4683(8) 0.8276(15) 0.2341(15) 0.082(4) Uani 1 1 d . . . H1A H 0.4628 0.8736 0.3138 0.098 Uiso 1 1 calc . . . H1B H 0.4160 0.8415 0.1794 0.098 Uiso 1 1 calc . . . C2 C 0.4703(7) 0.7082(12) 0.272(3) 0.083(4) Uani 1 1 d . . . H2A H 0.4714 0.6625 0.1914 0.099 Uiso 1 1 calc . . . H2B H 0.4156 0.6904 0.3192 0.099 Uiso 1 1 calc . . . N11 N 0.7464(7) 0.9169(11) -0.1288(11) 0.071(3) Uani 1 1 d . . . C11 C 0.7758(10) 1.0226(13) -0.1305(17) 0.084(4) Uani 1 1 d . . . H11 H 0.8282 1.0367 -0.1777 0.100 Uiso 1 1 calc R . . C12 C 0.7361(11) 1.1133(16) -0.0687(16) 0.091(4) Uani 1 1 d . . . H12 H 0.7580 1.1869 -0.0784 0.109 Uiso 1 1 calc R . . C13 C 0.6621(11) 1.0903(13) 0.0086(16) 0.085(4) Uani 1 1 d . . . H13 H 0.6337 1.1472 0.0571 0.102 Uiso 1 1 calc R . . C14 C 0.6323(9) 0.9816(11) 0.0109(13) 0.065(3) Uani 1 1 d . . . C15 C 0.6736(7) 0.8923(13) -0.0548(12) 0.067(3) Uani 1 1 d . . . H15 H 0.6520 0.8184 -0.0482 0.080 Uiso 1 1 calc R . . C16 C 0.5461(9) 0.9493(13) 0.0934(12) 0.071(3) Uani 1 1 d . . . C17 C 0.4680(12) 1.0262(17) 0.077(2) 0.119(6) Uani 1 1 d . . . H17A H 0.4209 1.0029 0.1358 0.179 Uiso 1 1 calc R . . H17B H 0.4472 1.0225 -0.0135 0.179 Uiso 1 1 calc R . . H17C H 0.4854 1.1027 0.0974 0.179 Uiso 1 1 calc R . . N21 N 0.7473(9) 0.6369(9) 0.6540(12) 0.077(3) Uani 1 1 d . . . C21 C 0.7692(9) 0.5328(12) 0.6656(12) 0.065(3) Uani 1 1 d . . . H21 H 0.8167 0.5184 0.7230 0.078 Uiso 1 1 calc R . . C22 C 0.7344(11) 0.4428(14) 0.6082(17) 0.088(4) Uani 1 1 d . . . H22 H 0.7593 0.3711 0.6202 0.106 Uiso 1 1 calc R . . C23 C 0.6574(12) 0.4588(14) 0.5268(17) 0.090(5) Uani 1 1 d . . . H23 H 0.6299 0.3984 0.4832 0.107 Uiso 1 1 calc R . . C24 C 0.6261(8) 0.5670(13) 0.5161(13) 0.071(3) Uani 1 1 d . . . C25 C 0.6723(7) 0.6561(10) 0.5788(12) 0.056(3) Uani 1 1 d . . . H25 H 0.6514 0.7301 0.5691 0.068 Uiso 1 1 calc R . . C26 C 0.5470(9) 0.5949(12) 0.4357(14) 0.071(4) Uani 1 1 d . . . C27 C 0.4672(11) 0.5134(16) 0.4517(19) 0.115(6) Uani 1 1 d . . . H27A H 0.4178 0.5404 0.3996 0.172 Uiso 1 1 calc R . . H27B H 0.4500 0.5100 0.5437 0.172 Uiso 1 1 calc R . . H27C H 0.4841 0.4388 0.4219 0.172 Uiso 1 1 calc R . . O102 O 0.489(3) 0.278(3) -0.772(5) 0.37(3) Uani 1 1 d . . . O101 O 0.5428(17) 0.214(2) -0.614(4) 0.266(17) Uani 1 1 d . . . N100 N 0.5479(12) 0.2623(15) -0.717(3) 0.118(8) Uani 1 1 d . . . O100 O 0.615(2) 0.2852(16) -0.752(4) 0.247(15) 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 0.0468(4) 0.0784(9) 0.0692(6) -0.0043(7) -0.0008(9) -0.0005(5) Ag2 0.038(4) 0.099(10) 0.028(4) -0.006(11) 0.007(5) -0.007(4) N1 0.050(5) 0.087(8) 0.063(6) 0.008(5) 0.005(5) 0.013(5) N2 0.043(5) 0.121(9) 0.051(5) -0.002(6) 0.006(4) -0.003(6) C1 0.047(6) 0.122(10) 0.076(12) 0.002(9) -0.001(7) 0.003(7) C2 0.037(5) 0.118(11) 0.094(10) 0.027(13) 0.003(10) -0.012(6) N11 0.051(6) 0.105(9) 0.059(7) -0.001(6) 0.009(5) 0.010(6) C11 0.055(8) 0.083(10) 0.113(12) 0.014(8) 0.002(8) -0.010(7) C12 0.077(10) 0.107(12) 0.090(10) 0.008(8) 0.001(9) 0.013(10) C13 0.080(10) 0.086(10) 0.089(10) -0.013(8) -0.003(8) 0.015(8) C14 0.071(8) 0.079(8) 0.045(6) 0.002(6) -0.015(6) 0.024(7) C15 0.046(6) 0.098(9) 0.057(7) -0.012(6) -0.002(6) 0.018(6) C16 0.066(7) 0.101(10) 0.046(7) -0.006(7) 0.000(6) 0.019(8) C17 0.082(11) 0.149(17) 0.127(15) 0.038(12) 0.005(11) 0.029(12) N21 0.088(8) 0.063(7) 0.081(7) -0.008(5) 0.002(7) -0.006(6) C21 0.066(8) 0.088(10) 0.040(6) -0.009(6) -0.004(6) -0.017(7) C22 0.080(10) 0.083(9) 0.101(12) 0.008(8) 0.023(10) 0.011(8) C23 0.091(11) 0.088(10) 0.090(12) -0.001(8) 0.002(9) -0.017(9) C24 0.045(6) 0.112(11) 0.056(8) 0.000(7) 0.010(5) -0.012(7) C25 0.047(6) 0.061(6) 0.062(7) -0.006(5) 0.005(6) 0.008(5) C26 0.063(8) 0.086(10) 0.063(8) 0.015(7) 0.009(7) -0.006(7) C27 0.091(11) 0.132(14) 0.122(14) 0.030(11) -0.022(11) -0.068(11) O102 0.30(4) 0.43(4) 0.38(5) -0.07(3) -0.27(4) 0.15(3) O101 0.141(18) 0.28(3) 0.38(4) 0.18(3) 0.05(2) 0.017(18) N100 0.091(10) 0.122(11) 0.14(2) 0.002(12) -0.038(16) -0.011(9) O100 0.30(3) 0.190(15) 0.26(3) 0.01(2) 0.20(3) -0.045(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 N21 2.278(12) 4_654 ? Ag1 N11 2.291(12) 4_655 ? Ag1 N1 2.381(11) . ? Ag1 N2 2.449(11) . ? Ag2 N21 1.68(2) 4_654 ? Ag2 N2 2.114(15) . ? Ag2 C21 2.18(2) 4_654 ? N1 C16 1.212(16) . ? N1 C1 1.479(17) . ? N2 C26 1.220(16) . ? N2 C2 1.53(2) . ? C1 C2 1.455(19) . ? N11 C11 1.319(17) . ? N11 C15 1.349(16) . ? N11 Ag1 2.291(12) 4_654 ? C11 C12 1.37(2) . ? C12 C13 1.38(2) . ? C13 C14 1.354(19) . ? C14 C15 1.385(17) . ? C14 C16 1.58(2) . ? C16 C17 1.486(19) . ? N21 C21 1.272(16) . ? N21 C25 1.371(16) . ? N21 Ag2 1.68(2) 4_655 ? N21 Ag1 2.278(12) 4_655 ? C21 C22 1.31(2) . ? C21 Ag2 2.18(2) 4_655 ? C22 C23 1.42(2) . ? C23 C24 1.36(2) . ? C24 C25 1.404(17) . ? C24 C26 1.470(19) . ? C26 C27 1.538(18) . ? O102 N100 1.06(3) . ? O101 N100 1.18(3) . ? N100 O100 1.09(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 N21 Ag1 N11 119.7(4) 4_654 4_655 ? N21 Ag1 N1 120.6(5) 4_654 . ? N11 Ag1 N1 107.8(4) 4_655 . ? N21 Ag1 N2 102.5(4) 4_654 . ? N11 Ag1 N2 123.2(4) 4_655 . ? N1 Ag1 N2 76.3(4) . . ? N21 Ag2 N2 153.2(10) 4_654 . ? N21 Ag2 C21 35.5(6) 4_654 4_654 ? N2 Ag2 C21 120.2(8) . 4_654 ? C16 N1 C1 119.0(12) . . ? C16 N1 Ag1 128.1(10) . . ? C1 N1 Ag1 108.5(8) . . ? C26 N2 C2 122.2(12) . . ? C26 N2 Ag2 111.0(11) . . ? C2 N2 Ag2 114.7(13) . . ? C26 N2 Ag1 131.5(10) . . ? C2 N2 Ag1 104.2(9) . . ? Ag2 N2 Ag1 26.9(4) . . ? C2 C1 N1 112.9(12) . . ? C1 C2 N2 114.4(12) . . ? C11 N11 C15 118.6(12) . . ? C11 N11 Ag1 120.0(9) . 4_654 ? C15 N11 Ag1 121.3(10) . 4_654 ? N11 C11 C12 125.7(14) . . ? C11 C12 C13 116.8(16) . . ? C14 C13 C12 117.3(14) . . ? C13 C14 C15 124.1(14) . . ? C13 C14 C16 120.3(12) . . ? C15 C14 C16 115.6(12) . . ? N11 C15 C14 117.3(14) . . ? N1 C16 C17 126.7(14) . . ? N1 C16 C14 117.4(11) . . ? C17 C16 C14 115.9(12) . . ? C21 N21 C25 114.8(11) . . ? C21 N21 Ag2 94.4(11) . 4_655 ? C25 N21 Ag2 150.1(11) . 4_655 ? C21 N21 Ag1 121.8(10) . 4_655 ? C25 N21 Ag1 123.3(8) . 4_655 ? Ag2 N21 Ag1 27.6(5) 4_655 4_655 ? N21 C21 C22 129.4(14) . . ? N21 C21 Ag2 50.0(8) . 4_655 ? C22 C21 Ag2 179.0(12) . 4_655 ? C21 C22 C23 117.7(15) . . ? C24 C23 C22 116.5(15) . . ? C23 C24 C25 119.6(13) . . ? C23 C24 C26 122.0(14) . . ? C25 C24 C26 118.4(13) . . ? N21 C25 C24 121.8(11) . . ? N2 C26 C24 119.5(13) . . ? N2 C26 C27 125.1(14) . . ? C24 C26 C27 115.3(12) . . ? O102 N100 O100 123(5) . . ? O102 N100 O101 119(4) . . ? O100 N100 O101 118(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.413 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.106 #=====END data_4 _database_code_depnum_ccdc_archive 'CCDC 238918' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H8 Ag N3 O3' _chemical_formula_weight 229.98 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' 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 10.418(2) _cell_length_b 10.521(2) _cell_length_c 6.2870(13) _cell_angle_alpha 90.00 _cell_angle_beta 115.16(3) _cell_angle_gamma 90.00 _cell_volume 623.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description needles _exptl_crystal_colour white _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 3.171 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4-MACH3 _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1122 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 24.94 _reflns_number_total 549 _reflns_number_gt 488 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction MACH3 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1000P)^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 549 _refine_ls_number_parameters 48 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1559 _refine_ls_wR_factor_gt 0.1462 _refine_ls_goodness_of_fit_ref 1.320 _refine_ls_restrained_S_all 1.320 _refine_ls_shift/su_max 0.003 _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 0.0000 0.5000 0.0303(5) Uani 1 2 d S . . N1 N 0.3127(4) 0.1098(4) 0.3816(7) 0.0363(10) Uani 1 1 d . . . H1 H 0.3076 0.1692 0.2643 0.07(2) Uiso 1 1 d R . . H2 H 0.2265 0.0543 0.3347 0.059(17) Uiso 1 1 d R . . C1 C 0.3165(4) 0.2106(4) 0.5464(7) 0.0290(10) Uani 1 1 d . . . H1A H 0.3971 0.2654 0.5759 0.032(15) Uiso 1 1 d R . . H1B H 0.3294 0.1725 0.6947 0.038(13) Uiso 1 1 d R . . O101 O 0.1105(6) 0.1636(8) 0.8595(8) 0.108(3) Uani 1 1 d . . . O102 O 0.0000 -0.0072(8) 0.7500 0.087(6) Uani 1 2 d S . . N100 N 0.0000 0.1081(7) 0.7500 0.0427(15) Uani 1 2 d S . . 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 0.0263(7) 0.0353(7) 0.0255(7) -0.00425(13) 0.0073(5) 0.00963(14) N1 0.030(2) 0.039(2) 0.033(2) -0.0068(16) 0.0070(16) 0.0099(17) C1 0.024(2) 0.038(2) 0.0181(17) 0.0011(16) 0.0017(15) 0.0081(18) O101 0.077(4) 0.172(7) 0.044(2) 0.028(4) -0.003(3) -0.071(4) O102 0.110(18) 0.071(11) 0.102(15) 0.000 0.065(14) 0.000 N100 0.037(3) 0.056(4) 0.033(3) 0.000 0.013(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.112(4) 5_656 ? Ag1 N1 2.112(4) . ? Ag1 Ag1 3.1435(6) 2_655 ? Ag1 Ag1 3.1435(6) 2_656 ? N1 C1 1.472(5) . ? C1 C1 1.503(8) 7_556 ? O101 N100 1.211(6) . ? O102 N100 1.214(8) . ? N100 O101 1.211(6) 2_556 ? 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 5_656 . ? N1 Ag1 Ag1 87.68(11) 5_656 2_655 ? N1 Ag1 Ag1 92.32(11) . 2_655 ? N1 Ag1 Ag1 92.32(11) 5_656 2_656 ? N1 Ag1 Ag1 87.68(11) . 2_656 ? Ag1 Ag1 Ag1 180.0 2_655 2_656 ? C1 N1 Ag1 113.7(3) . . ? N1 C1 C1 112.3(4) . 7_556 ? O101 N100 O101 122.3(11) . 2_556 ? O101 N100 O102 118.8(5) . . ? O101 N100 O102 118.8(5) 2_556 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.94 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.716 _refine_diff_density_min -2.486 _refine_diff_density_rms 0.269 #=======END data_5 _database_code_depnum_ccdc_archive 'CCDC 238919' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H11 Ag N3 O3.50' _chemical_formula_weight 253.02 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 8.1010(16) _cell_length_b 8.3910(17) _cell_length_c 11.034(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.88(3) _cell_angle_gamma 90.00 _cell_volume 717.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6 _cell_measurement_theta_max 15 _exptl_crystal_description Needles _exptl_crystal_colour White _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 2.772 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4-MACH3 _diffrn_measurement_method /w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1296 _diffrn_reflns_av_R_equivalents 0.0777 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 24.97 _reflns_number_total 1206 _reflns_number_gt 835 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction MACH3 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0896P)^2^+0.1337P] 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 1206 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1630 _refine_ls_wR_factor_gt 0.1338 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.085 _refine_ls_shift/su_mean 0.005 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 -1.0000 0.958(5) -0.2500 0.235(19) Uani 1 2 d S . . Ag1 Ag -1.0000 0.30398(14) -0.2500 0.0408(4) Uani 1 2 d S . . Ag2 Ag -1.0000 0.66638(15) -0.2500 0.0474(5) Uani 1 2 d S . . N100 N -0.3679(15) 0.3353(13) -0.0578(9) 0.049(3) Uani 1 1 d . . . O101 O -0.2138(13) 0.3684(13) -0.0452(12) 0.076(3) Uani 1 1 d . . . O102 O -0.4758(18) 0.434(2) -0.1136(18) 0.139(6) Uani 1 1 d . . . O103 O -0.4169(17) 0.2151(13) -0.0172(11) 0.076(3) Uani 1 1 d . . . N1 N -1.1818(14) 0.3012(11) -0.4319(8) 0.046(2) Uani 1 1 d . . . H11N H -1.1733 0.4012 -0.4754 0.050 Uiso 1 1 d . . . H12N H -1.2631 0.3173 -0.3954 0.050 Uiso 1 1 d . . . N2 N -1.2496(14) 0.3194(11) -0.7192(10) 0.047(2) Uani 1 1 d . . . H21N H -1.2912 0.3179 -0.7925 0.050 Uiso 1 1 d . . . H22N H -1.2390 0.4208 -0.6738 0.050 Uiso 1 1 d . . . C1 C -1.1577(15) 0.1690(12) -0.5176(11) 0.039(3) Uani 1 1 d . . . H1A H -1.1722 0.0676 -0.4797 0.046 Uiso 1 1 calc . . . H1B H -1.0405 0.1732 -0.5232 0.046 Uiso 1 1 calc . . . C2 C -1.2810(16) 0.1762(14) -0.6497(11) 0.043(3) Uani 1 1 d . . . H2 H -1.3998 0.1787 -0.6446 0.052 Uiso 1 1 calc R . . C3 C -1.2563(16) 0.0297(14) -0.7222(10) 0.046(3) Uani 1 1 d . . . H3A H -1.3339 0.0339 -0.8064 0.069 Uiso 1 1 calc R . . H3B H -1.2798 -0.0639 -0.6799 0.069 Uiso 1 1 calc R . . H3C H -1.1396 0.0262 -0.7262 0.069 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 0.19(3) 0.25(4) 0.31(6) 0.000 0.14(4) 0.000 Ag1 0.0534(9) 0.0362(7) 0.0262(6) 0.000 0.0012(5) 0.000 Ag2 0.0619(10) 0.0392(8) 0.0481(8) 0.000 0.0273(7) 0.000 N100 0.062(7) 0.051(6) 0.032(5) 0.008(4) 0.010(5) -0.012(6) O101 0.049(6) 0.063(6) 0.119(10) -0.008(6) 0.030(6) 0.000(5) O102 0.079(9) 0.148(14) 0.175(16) 0.066(13) 0.015(10) 0.020(10) O103 0.108(9) 0.067(7) 0.066(7) 0.006(5) 0.045(6) -0.017(6) N1 0.066(7) 0.047(6) 0.020(4) -0.001(4) 0.005(4) 0.008(5) N2 0.057(6) 0.040(6) 0.044(6) -0.003(4) 0.015(5) -0.002(5) C1 0.047(7) 0.033(6) 0.035(6) -0.003(5) 0.010(5) -0.007(5) C2 0.045(7) 0.053(7) 0.037(6) 0.002(5) 0.019(5) -0.018(6) C3 0.052(7) 0.061(8) 0.032(5) -0.010(5) 0.022(5) -0.015(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 O1 Ag2 2.45(4) . ? Ag1 N1 2.117(9) 2_354 ? Ag1 N1 2.117(9) . ? Ag1 Ag2 3.041(2) . ? Ag2 N2 2.149(11) 4_566 ? Ag2 N2 2.149(11) 3_364 ? N100 O103 1.216(13) . ? N100 O102 1.230(16) . ? N100 O101 1.247(14) . ? N1 C1 1.506(14) . ? N2 C2 1.487(14) . ? N2 Ag2 2.149(11) 3_364 ? C1 C2 1.511(17) . ? C2 C3 1.511(16) . ? 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 178.7(5) 2_354 . ? N1 Ag1 Ag2 90.6(3) 2_354 . ? N1 Ag1 Ag2 90.6(3) . . ? N2 Ag2 N2 173.6(5) 4_566 3_364 ? N2 Ag2 O1 86.8(2) 4_566 . ? N2 Ag2 O1 86.8(2) 3_364 . ? N2 Ag2 Ag1 93.2(2) 4_566 . ? N2 Ag2 Ag1 93.2(2) 3_364 . ? O1 Ag2 Ag1 180.000(2) . . ? O103 N100 O102 118.7(14) . . ? O103 N100 O101 124.6(13) . . ? O102 N100 O101 116.7(12) . . ? C1 N1 Ag1 114.9(7) . . ? C2 N2 Ag2 115.9(8) . 3_364 ? N1 C1 C2 113.9(9) . . ? N2 C2 C1 111.5(9) . . ? N2 C2 C3 108.4(10) . . ? C1 C2 C3 109.0(10) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.982 _refine_diff_density_min -1.234 _refine_diff_density_rms 0.212 #===========END data_6 _database_code_depnum_ccdc_archive 'CCDC 238920' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H10 Ag N3 O3' _chemical_formula_weight 244.01 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 Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 9.4230(19) _cell_length_b 10.410(2) _cell_length_c 7.6430(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 749.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 16 _exptl_crystal_description Needles _exptl_crystal_colour white _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 2.645 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4-MACH3 _diffrn_measurement_method /w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1287 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 684 _reflns_number_gt 462 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction CAD4 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0500P)^2^+2.9154P] 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 684 _refine_ls_number_parameters 52 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 0.759 _refine_ls_restrained_S_all 0.759 _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 0.5000 0.0000 0.5000 0.0532(3) Uani 1 2 d S . . O2 O 0.4388(5) 0.1451(3) 0.9162(6) 0.0845(11) Uani 1 1 d . . . N3 N 0.3955(7) 0.2500 0.8650(7) 0.0585(14) Uani 1 2 d S . . N4 N 0.3495(4) 0.0145(3) 0.2951(5) 0.0519(9) Uani 1 1 d . . . H4A H 0.2924 -0.0617 0.3012 0.062 Uiso 1 1 d R . . H4B H 0.4026 0.0145 0.1879 0.062 Uiso 1 1 d R . . C5 C 0.3445(6) 0.2500 0.3196(8) 0.0422(12) Uani 1 2 d S . . H5A H 0.3894 0.2500 0.4323 0.051 Uiso 1 2 d SR . . H5B H 0.4157 0.2500 0.2298 0.051 Uiso 1 2 d SR . . C6 C 0.2577(4) 0.1287(4) 0.2988(6) 0.0498(10) Uani 1 1 d . . . H6A H 0.2034 0.1337 0.1927 0.060 Uiso 1 1 d R . . H6B H 0.1945 0.1222 0.3970 0.060 Uiso 1 1 d R . . O1 O 0.2887(10) 0.2500 0.7746(12) 0.135(3) Uani 1 2 d S . . 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 0.0478(4) 0.0394(3) 0.0725(4) 0.01301(18) 0.0002(2) 0.00016(18) O2 0.095(3) 0.058(2) 0.101(3) 0.003(2) 0.001(3) 0.021(2) N3 0.073(4) 0.045(3) 0.058(3) 0.000 0.000(3) 0.000 N4 0.061(2) 0.0318(16) 0.063(2) -0.0030(14) 0.0008(18) -0.0068(15) C5 0.042(3) 0.030(2) 0.055(3) 0.000 -0.004(3) 0.000 C6 0.046(2) 0.039(2) 0.064(2) 0.0018(18) -0.008(2) -0.0050(17) O1 0.160(6) 0.058(3) 0.186(8) 0.000 -0.087(7) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.118(4) 5_656 ? Ag1 N4 2.118(4) . ? O2 N3 1.229(4) . ? N3 O1 1.222(9) . ? N3 O2 1.229(4) 7_565 ? N4 C6 1.471(5) . ? C5 C6 1.513(5) . ? C5 C6 1.513(5) 7_565 ? 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 N4 180.0 5_656 . ? O1 N3 O2 117.0(3) . 7_565 ? O1 N3 O2 117.0(3) . . ? O2 N3 O2 125.3(7) 7_565 . ? C6 N4 Ag1 115.9(3) . . ? C6 C5 C6 113.1(4) . 7_565 ? N4 C6 C5 111.0(3) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.444 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.095 #=======END