# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name _publ_author_address 'Zheng, Shao-Liang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Tong, Ming-Liang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Zhu, Hai-Liang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Chen, Xiao-Ming' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof Xiao-Ming Chen' _publ_contact_author_address ; School of Chemistry and Chemical Engineerin Zhongshan University Xingang Xilu 135 Guangzhou 510275 CHINA ; _publ_contact_author_phone '86-20-84113986' _publ_contact_author_fax '86 20 84112245' _publ_contact_author_email 'cescxm@zsu.edu.cn' _publ_requested_joiurnal 'New J. Chem.' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as a supplmentary data for a manuscript submitted to New J. Chem. Xiao-Ming Chen ; #================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Four two-dimensional highly undulated silver(I)- hexamethylenetetramine co-ordination networks containing micropores ; #============================================================ data_complex_1 _database_code_CSD 170950 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H27 Ag2 Cl2 N9 O8' _chemical_formula_weight 736.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.112(10) _cell_length_b 10.860(5) _cell_length_c 23.781(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4678(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.34 _exptl_crystal_density_diffrn 2.090 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 1.965 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.4785 _exptl_absorpt_correction_T_max 0.5547 _exptl_absorpt_process_details '\y-scans (North et al., 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 5486 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.01 _reflns_number_total 5103 _reflns_number_gt 3180 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V. 5.0 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+9.8900P] 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 0.00003(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5103 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0946 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1289 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.16536(2) 0.00076(4) 0.09029(2) 0.03320(15) Uani 1 d . . . Ag2 Ag 1.01753(3) 0.49348(4) 0.18441(2) 0.03866(16) Uani 1 d . . . N1 N 0.9345(3) 0.8722(5) 0.1335(3) 0.0376(13) Uani 1 d . . . N2 N 1.0126(3) 0.7114(4) 0.1744(2) 0.0286(11) Uani 1 d . . . N3 N 0.9930(3) 0.9064(4) 0.2255(2) 0.0275(11) Uani 1 d . . . N4 N 1.0683(3) 0.9041(4) 0.1395(2) 0.0268(11) Uani 1 d . . . N5 N 1.1489(2) 0.2178(4) 0.0769(2) 0.0236(10) Uani 1 d . . . N6 N 1.2181(2) 0.4133(4) 0.0740(2) 0.0249(11) Uani 1 d . . . N7 N 1.1102(3) 0.3816(4) 0.0126(2) 0.0312(12) Uani 1 d . . . N8 N 1.0928(2) 0.4063(4) 0.1145(2) 0.0235(10) Uani 1 d . . . C1 C 0.9456(3) 0.7394(6) 0.1398(3) 0.0329(15) Uani 1 d . . . H1A H 0.9513 0.7038 0.1031 0.080 Uiso 1 d R . . H1B H 0.9028 0.7033 0.1570 0.080 Uiso 1 d R . . C2 C 0.9996(3) 0.9241(5) 0.1053(3) 0.0313(14) Uani 1 d . . . H2A H 0.9922 1.0107 0.0997 0.080 Uiso 1 d R . . H2B H 1.0052 0.8861 0.0691 0.080 Uiso 1 d R . . C3 C 0.9257(3) 0.9262(6) 0.1890(3) 0.0372(16) Uani 1 d . . . H3A H 0.8836 0.8897 0.2070 0.080 Uiso 1 d R . . H3B H 0.9164 1.0128 0.1850 0.080 Uiso 1 d R . . C4 C 1.0040(3) 0.7716(5) 0.2300(3) 0.0301(14) Uani 1 d . . . H4A H 1.0472 0.7557 0.2523 0.080 Uiso 1 d R . . H4B H 0.9624 0.7361 0.2490 0.080 Uiso 1 d R . . C5 C 1.0766(3) 0.7678(5) 0.1458(3) 0.0243(12) Uani 1 d . . . H5A H 1.0823 0.7313 0.1093 0.080 Uiso 1 d R . . H5B H 1.1206 0.7510 0.1669 0.080 Uiso 1 d R . . C6 C 1.0585(3) 0.9584(6) 0.1957(3) 0.0294(14) Uani 1 d . . . H6A H 1.1021 0.9441 0.2178 0.080 Uiso 1 d R . . H6B H 1.0523 1.0458 0.1919 0.080 Uiso 1 d R . . C7 C 1.1003(3) 0.2704(5) 0.1205(3) 0.0269(13) Uani 1 d . . . H7A H 1.1204 0.2524 0.1569 0.080 Uiso 1 d R . . H7B H 1.0524 0.2328 0.1181 0.080 Uiso 1 d R . . C8 C 1.0626(3) 0.4314(5) 0.0573(3) 0.0295(13) Uani 1 d . . . H8A H 1.0145 0.3949 0.0542 0.080 Uiso 1 d R . . H8B H 1.0573 0.5187 0.0525 0.080 Uiso 1 d R . . C9 C 1.1834(3) 0.4386(6) 0.0184(3) 0.0323(14) Uani 1 d . . . H9A H 1.2149 0.4072 -0.0107 0.080 Uiso 1 d R . . H9B H 1.1789 0.5260 0.0132 0.080 Uiso 1 d R . . C10 C 1.1682(3) 0.4613(5) 0.1181(3) 0.0261(13) Uani 1 d . . . H10A H 1.1645 0.5492 0.1149 0.080 Uiso 1 d R . . H10B H 1.1890 0.4426 0.1543 0.080 Uiso 1 d R . . C11 C 1.1181(4) 0.2481(6) 0.0206(3) 0.0317(14) Uani 1 d . . . H11A H 1.0708 0.2093 0.0163 0.080 Uiso 1 d R . . H11B H 1.1504 0.2158 -0.0078 0.080 Uiso 1 d R . . C12 C 1.2227(3) 0.2777(5) 0.0808(3) 0.0277(13) Uani 1 d . . . H12A H 1.2546 0.2440 0.0524 0.080 Uiso 1 d R . . H12B H 1.2440 0.2598 0.1168 0.080 Uiso 1 d R . . C13 C 0.8371(4) 0.4365(7) 0.1432(4) 0.053(2) Uani 1 d . . . C14 C 0.7585(5) 0.4320(9) 0.1326(4) 0.067(2) Uani 1 d . . . N9 N 0.8976(4) 0.4411(7) 0.1539(4) 0.078(2) Uani 1 d . . . H14A H 0.7418 0.4430 0.1708 0.080 Uiso 1 d . . . H14B H 0.7368 0.3536 0.1242 0.080 Uiso 1 d . . . H14C H 0.7522 0.4612 0.0951 0.080 Uiso 1 d . . . Cl1 Cl 1.11930(8) -0.18291(15) -0.03499(7) 0.0363(4) Uani 1 d . . . O1 O 1.0727(3) -0.1911(5) -0.0824(3) 0.0715(18) Uani 1 d . . . O2 O 1.1908(3) -0.2265(7) -0.0488(3) 0.101(3) Uani 1 d . . . O3 O 1.0920(5) -0.2636(6) 0.0075(3) 0.101(3) Uani 1 d . . . O4 O 1.1222(4) -0.0610(5) -0.0131(2) 0.0667(17) Uani 1 d . . . Cl2 Cl 0.75090(9) 0.17642(16) 0.25773(7) 0.0404(4) Uani 1 d . . . O5 O 0.8208(3) 0.1204(6) 0.2499(3) 0.086(2) Uani 1 d . . . O6 O 0.7148(4) 0.1074(6) 0.3016(3) 0.091(2) Uani 1 d . . . O7 O 0.7098(5) 0.1711(8) 0.2092(3) 0.136(4) Uani 1 d . . . O8 O 0.7600(3) 0.3018(5) 0.2755(2) 0.0629(16) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0270(2) 0.0269(2) 0.0457(3) 0.0007(2) 0.0028(2) 0.0011(2) Ag2 0.0431(3) 0.0297(3) 0.0432(3) 0.0037(2) 0.0163(2) 0.0043(2) N1 0.021(3) 0.036(3) 0.055(4) 0.007(3) 0.002(3) 0.007(2) N2 0.025(3) 0.022(2) 0.038(3) -0.001(2) 0.001(2) -0.001(2) N3 0.027(3) 0.022(2) 0.034(3) -0.004(2) 0.008(2) 0.000(2) N4 0.023(2) 0.020(2) 0.037(3) -0.001(2) 0.003(2) 0.000(2) N5 0.022(2) 0.017(2) 0.032(3) -0.003(2) 0.001(2) -0.0006(18) N6 0.018(2) 0.021(2) 0.036(3) -0.002(2) 0.007(2) 0.0004(19) N7 0.036(3) 0.028(3) 0.030(3) 0.003(2) -0.001(2) 0.001(2) N8 0.019(2) 0.019(2) 0.032(3) 0.002(2) 0.001(2) -0.0006(19) C1 0.029(3) 0.030(3) 0.040(4) -0.003(3) -0.002(3) -0.003(3) C2 0.028(3) 0.028(3) 0.037(3) 0.005(3) 0.002(3) 0.004(3) C3 0.031(3) 0.030(3) 0.051(4) -0.002(3) 0.012(3) 0.004(3) C4 0.035(3) 0.022(3) 0.034(3) 0.001(2) 0.005(3) -0.002(3) C5 0.023(3) 0.019(3) 0.031(3) 0.003(2) 0.003(3) 0.006(2) C6 0.028(3) 0.026(3) 0.034(3) -0.001(3) 0.006(3) -0.004(2) C7 0.022(3) 0.022(3) 0.037(4) 0.003(3) 0.002(3) -0.002(2) C8 0.022(3) 0.026(3) 0.040(4) -0.002(3) -0.005(3) 0.006(2) C9 0.035(3) 0.028(3) 0.034(3) 0.008(3) 0.004(3) 0.001(3) C10 0.025(3) 0.023(3) 0.029(3) -0.001(2) 0.003(3) -0.002(2) C11 0.033(3) 0.034(3) 0.029(3) -0.011(3) -0.005(3) 0.000(3) C12 0.020(3) 0.021(3) 0.043(4) 0.002(3) 0.004(3) 0.003(2) C13 0.042(4) 0.051(5) 0.065(5) -0.017(4) 0.012(4) -0.014(4) C14 0.049(5) 0.092(7) 0.061(5) -0.016(5) -0.002(4) -0.010(5) N9 0.044(4) 0.064(5) 0.125(7) -0.025(5) -0.001(5) -0.009(4) Cl1 0.0319(8) 0.0410(9) 0.0360(8) -0.0023(7) -0.0065(7) 0.0029(7) O1 0.079(4) 0.050(3) 0.086(4) -0.014(3) -0.051(4) 0.012(3) O2 0.036(3) 0.135(6) 0.131(6) -0.070(5) 0.002(4) 0.006(4) O3 0.171(8) 0.061(4) 0.070(5) 0.015(3) 0.026(5) -0.002(5) O4 0.096(5) 0.045(3) 0.059(3) -0.015(3) -0.019(3) 0.003(3) Cl2 0.0345(8) 0.0447(9) 0.0419(9) -0.0121(8) -0.0048(8) 0.0042(8) O5 0.046(3) 0.085(5) 0.128(6) -0.035(4) 0.019(4) 0.010(3) O6 0.109(5) 0.059(4) 0.105(6) -0.001(4) 0.051(5) 0.003(4) O7 0.178(8) 0.108(6) 0.121(6) -0.035(5) -0.115(6) 0.040(6) O8 0.082(4) 0.036(3) 0.071(4) -0.009(3) 0.008(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N6 2.347(5) 8_855 ? Ag1 N4 2.359(5) 1_545 ? Ag1 N5 2.397(4) . ? Ag2 N3 2.349(5) 3_745 ? Ag2 N8 2.350(5) . ? Ag2 N9 2.360(7) . ? Ag2 N2 2.380(5) . ? N1 C3 1.452(8) . ? N1 C1 1.463(8) . ? N1 C2 1.470(8) . ? N2 C5 1.478(7) . ? N2 C4 1.483(7) . ? N2 C1 1.499(8) . ? N3 C4 1.482(7) . ? N3 C6 1.493(7) . ? N3 C3 1.512(8) . ? N3 Ag2 2.349(5) 3_755 ? N4 C6 1.472(7) . ? N4 C5 1.495(7) . ? N4 C2 1.503(7) . ? N4 Ag1 2.359(5) 1_565 ? N5 C7 1.474(7) . ? N5 C11 1.488(8) . ? N5 C12 1.489(7) . ? N6 C10 1.480(7) . ? N6 C12 1.485(7) . ? N6 C9 1.488(8) . ? N6 Ag1 2.347(5) 8_865 ? N7 C11 1.470(8) . ? N7 C9 1.471(8) . ? N7 C8 1.471(7) . ? N8 C7 1.490(7) . ? N8 C8 1.492(7) . ? N8 C10 1.493(7) . ? C13 N9 1.125(10) . ? C13 C14 1.448(11) . ? Cl1 O1 1.411(5) . ? Cl1 O2 1.418(6) . ? Cl1 O4 1.424(5) . ? Cl1 O3 1.426(7) . ? Cl2 O7 1.374(6) . ? Cl2 O5 1.418(6) . ? Cl2 O8 1.436(5) . ? Cl2 O6 1.442(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ag1 N4 124.90(17) 8_855 1_545 ? N6 Ag1 N5 119.19(16) 8_855 . ? N4 Ag1 N5 114.27(16) 1_545 . ? N3 Ag2 N8 122.02(16) 3_745 . ? N3 Ag2 N9 96.3(3) 3_745 . ? N8 Ag2 N9 102.7(2) . . ? N3 Ag2 N2 119.21(17) 3_745 . ? N8 Ag2 N2 110.58(16) . . ? N9 Ag2 N2 100.1(2) . . ? C3 N1 C1 108.7(5) . . ? C3 N1 C2 110.4(5) . . ? C1 N1 C2 108.3(5) . . ? C5 N2 C4 108.1(4) . . ? C5 N2 C1 107.3(5) . . ? C4 N2 C1 108.4(5) . . ? C5 N2 Ag2 115.4(3) . . ? C4 N2 Ag2 110.7(3) . . ? C1 N2 Ag2 106.7(3) . . ? C4 N3 C6 107.4(5) . . ? C4 N3 C3 106.9(5) . . ? C6 N3 C3 108.3(5) . . ? C4 N3 Ag2 110.1(4) . 3_755 ? C6 N3 Ag2 110.2(3) . 3_755 ? C3 N3 Ag2 113.7(3) . 3_755 ? C6 N4 C5 108.6(5) . . ? C6 N4 C2 109.5(5) . . ? C5 N4 C2 106.3(4) . . ? C6 N4 Ag1 111.3(3) . 1_565 ? C5 N4 Ag1 114.5(3) . 1_565 ? C2 N4 Ag1 106.5(3) . 1_565 ? C7 N5 C11 108.9(4) . . ? C7 N5 C12 108.9(4) . . ? C11 N5 C12 107.2(5) . . ? C7 N5 Ag1 111.2(3) . . ? C11 N5 Ag1 112.5(3) . . ? C12 N5 Ag1 108.0(3) . . ? C10 N6 C12 107.8(5) . . ? C10 N6 C9 107.9(4) . . ? C12 N6 C9 107.7(5) . . ? C10 N6 Ag1 106.8(3) . 8_865 ? C12 N6 Ag1 109.4(3) . 8_865 ? C9 N6 Ag1 116.9(3) . 8_865 ? C11 N7 C9 108.4(5) . . ? C11 N7 C8 109.1(5) . . ? C9 N7 C8 107.7(5) . . ? C7 N8 C8 107.6(5) . . ? C7 N8 C10 107.9(4) . . ? C8 N8 C10 108.4(4) . . ? C7 N8 Ag2 112.6(4) . . ? C8 N8 Ag2 111.1(3) . . ? C10 N8 Ag2 109.2(3) . . ? N1 C1 N2 111.6(5) . . ? N1 C2 N4 111.2(5) . . ? N1 C3 N3 112.1(5) . . ? N3 C4 N2 112.7(5) . . ? N2 C5 N4 112.1(4) . . ? N4 C6 N3 112.1(5) . . ? N5 C7 N8 111.8(5) . . ? N7 C8 N8 112.2(4) . . ? N7 C9 N6 112.8(5) . . ? N6 C10 N8 112.1(5) . . ? N7 C11 N5 111.8(5) . . ? N6 C12 N5 112.1(4) . . ? N9 C13 C14 176.9(10) . . ? C13 N9 Ag2 167.5(7) . . ? O1 Cl1 O2 109.8(4) . . ? O1 Cl1 O4 111.8(3) . . ? O2 Cl1 O4 111.2(4) . . ? O1 Cl1 O3 108.7(4) . . ? O2 Cl1 O3 106.1(5) . . ? O4 Cl1 O3 109.0(4) . . ? O7 Cl2 O5 110.8(5) . . ? O7 Cl2 O8 110.4(4) . . ? O5 Cl2 O8 110.1(4) . . ? O7 Cl2 O6 109.9(6) . . ? O5 Cl2 O6 106.1(4) . . ? O8 Cl2 O6 109.4(4) . . ? _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.901 _refine_diff_density_max 0.914 _refine_diff_density_min -1.062 _refine_diff_density_rms 0.134 #=======================================END data_complex_2 _database_code_CSD 170951 #data_ag _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H15 Ag N4 O4' _chemical_formula_weight 351.12 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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.488(3) _cell_length_b 10.395(3) _cell_length_c 19.527(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2331.9(12) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 2.000 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 1.743 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.5280 _exptl_absorpt_correction_T_max 0.6797 _exptl_absorpt_process_details '\y-scans (North et al., 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 2826 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2675 _reflns_number_gt 1972 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V. 5.0 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1033P)^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 2675 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1540 _refine_ls_wR_factor_gt 0.1384 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.59658(3) 0.21944(4) 0.31298(2) 0.03008(19) Uani 1 d . . . O1 O 0.4247(4) 0.2540(4) 0.3896(2) 0.0380(10) Uani 1 d . . . O2 O 0.5301(4) 0.4313(4) 0.3909(2) 0.0448(11) Uani 1 d . . . O3 O 0.2245(4) 0.6125(4) 0.4475(2) 0.0436(10) Uani 1 d . . . H3 H 0.1749 0.6471 0.4097 0.080 Uiso 1 d R . . O4 O 0.2627(4) 0.5153(4) 0.3487(2) 0.0428(11) Uani 1 d . . . N1 N 0.7866(4) 0.2977(4) 0.3265(2) 0.0216(9) Uani 1 d . . . N2 N 0.9871(4) 0.2949(4) 0.2833(2) 0.0264(9) Uani 1 d . . . N3 N 0.9035(3) 0.4924(4) 0.3308(2) 0.0236(9) Uani 1 d . . . N4 N 0.9502(4) 0.3145(4) 0.4059(2) 0.0302(10) Uani 1 d . . . C1 C 0.4430(5) 0.3692(5) 0.4080(3) 0.0288(11) Uani 1 d . . . C2 C 0.3516(5) 0.4374(6) 0.4512(3) 0.0331(12) Uani 1 d . . . H2A H 0.3899 0.4863 0.4863 0.080 Uiso 1 d R . . H2B H 0.3032 0.3745 0.4731 0.080 Uiso 1 d R . . C3 C 0.2759(4) 0.5254(5) 0.4097(3) 0.0288(11) Uani 1 d . . . C4 C 0.8674(5) 0.2447(5) 0.2749(3) 0.0253(11) Uani 1 d . . . H4A H 0.8393 0.2660 0.2300 0.080 Uiso 1 d R . . H4B H 0.8688 0.1526 0.2787 0.080 Uiso 1 d R . . C5 C 0.8326(5) 0.2633(5) 0.3958(3) 0.0282(11) Uani 1 d . . . H5A H 0.8341 0.1714 0.4005 0.080 Uiso 1 d R . . H5B H 0.7816 0.2973 0.4303 0.080 Uiso 1 d R . . C6 C 0.7859(4) 0.4376(5) 0.3210(3) 0.0249(10) Uani 1 d . . . H6A H 0.7341 0.4726 0.3548 0.080 Uiso 1 d R . . H6B H 0.7572 0.4616 0.2766 0.080 Uiso 1 d R . . C7 C 1.0269(5) 0.2608(5) 0.3539(3) 0.0307(12) Uani 1 d . . . H7A H 1.1044 0.2927 0.3610 0.080 Uiso 1 d R . . H7B H 1.0288 0.1688 0.3585 0.080 Uiso 1 d R . . C8 C 0.9816(4) 0.4375(5) 0.2783(3) 0.0259(11) Uani 1 d . . . H8A H 0.9542 0.4615 0.2337 0.080 Uiso 1 d R . . H8B H 1.0584 0.4723 0.2841 0.080 Uiso 1 d R . . C9 C 0.9459(5) 0.4547(5) 0.3998(3) 0.0302(12) Uani 1 d . . . H9A H 0.8956 0.4898 0.4343 0.080 Uiso 1 d R . . H9B H 1.0227 0.4888 0.4068 0.080 Uiso 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0213(3) 0.0208(3) 0.0481(3) 0.00038(17) -0.00312(17) 0.00061(15) O1 0.041(2) 0.028(2) 0.045(3) -0.0038(18) 0.010(2) -0.0038(17) O2 0.031(2) 0.041(2) 0.062(3) -0.004(2) 0.010(2) -0.0060(19) O3 0.055(3) 0.038(2) 0.038(2) -0.0115(19) -0.004(2) 0.014(2) O4 0.043(2) 0.053(3) 0.032(2) -0.0090(19) -0.0036(19) 0.013(2) N1 0.0211(19) 0.0150(18) 0.029(2) -0.0017(15) 0.0032(17) -0.0036(16) N2 0.019(2) 0.024(2) 0.037(2) 0.0019(19) 0.0017(18) -0.0005(16) N3 0.019(2) 0.019(2) 0.032(2) 0.0007(17) -0.0005(17) -0.0009(16) N4 0.038(3) 0.021(2) 0.031(2) 0.0037(18) -0.007(2) 0.0000(19) C1 0.027(2) 0.028(3) 0.031(3) 0.002(2) 0.000(2) 0.005(2) C2 0.034(3) 0.037(3) 0.028(3) -0.001(2) 0.004(2) 0.002(2) C3 0.024(2) 0.027(3) 0.036(3) -0.004(2) 0.002(2) -0.005(2) C4 0.024(2) 0.024(2) 0.028(3) -0.003(2) 0.001(2) -0.001(2) C5 0.038(3) 0.019(2) 0.028(3) 0.003(2) 0.001(2) -0.007(2) C6 0.017(2) 0.023(2) 0.035(3) 0.001(2) 0.002(2) 0.0005(19) C7 0.024(2) 0.024(2) 0.044(3) 0.004(2) -0.006(2) 0.005(2) C8 0.023(2) 0.019(2) 0.036(3) 0.001(2) 0.006(2) -0.0043(19) C9 0.034(3) 0.023(3) 0.033(3) -0.002(2) -0.004(2) -0.005(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 2.345(4) . ? Ag1 N3 2.386(4) 8_755 ? Ag1 N2 2.394(5) 6_556 ? Ag1 O1 2.503(4) . ? O1 C1 1.268(7) . ? O2 C1 1.237(7) . ? O3 C3 1.308(6) . ? O4 C3 1.206(7) . ? N1 C6 1.458(6) . ? N1 C4 1.478(7) . ? N1 C5 1.495(7) . ? N2 C4 1.480(6) . ? N2 C8 1.487(6) . ? N2 C7 1.496(8) . ? N2 Ag1 2.394(5) 6_656 ? N3 C8 1.476(7) . ? N3 C6 1.478(6) . ? N3 C9 1.485(7) . ? N3 Ag1 2.386(4) 8_765 ? N4 C7 1.456(7) . ? N4 C9 1.463(7) . ? N4 C5 1.466(7) . ? C1 C2 1.522(8) . ? C2 C3 1.500(8) . ? 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 109.09(13) . 8_755 ? N1 Ag1 N2 117.66(15) . 6_556 ? N3 Ag1 N2 116.01(15) 8_755 6_556 ? N1 Ag1 O1 128.11(15) . . ? N3 Ag1 O1 93.13(14) 8_755 . ? N2 Ag1 O1 90.44(16) 6_556 . ? C1 O1 Ag1 100.0(3) . . ? C6 N1 C4 108.9(4) . . ? C6 N1 C5 107.9(4) . . ? C4 N1 C5 107.9(4) . . ? C6 N1 Ag1 109.4(3) . . ? C4 N1 Ag1 112.2(3) . . ? C5 N1 Ag1 110.4(3) . . ? C4 N2 C8 107.8(4) . . ? C4 N2 C7 107.6(4) . . ? C8 N2 C7 108.0(4) . . ? C4 N2 Ag1 106.6(3) . 6_656 ? C8 N2 Ag1 107.3(3) . 6_656 ? C7 N2 Ag1 119.1(3) . 6_656 ? C8 N3 C6 108.5(4) . . ? C8 N3 C9 109.1(4) . . ? C6 N3 C9 108.4(4) . . ? C8 N3 Ag1 106.3(3) . 8_765 ? C6 N3 Ag1 111.2(3) . 8_765 ? C9 N3 Ag1 113.2(3) . 8_765 ? C7 N4 C9 110.2(4) . . ? C7 N4 C5 108.9(4) . . ? C9 N4 C5 108.6(4) . . ? O2 C1 O1 123.4(5) . . ? O2 C1 C2 117.7(5) . . ? O1 C1 C2 118.9(5) . . ? C3 C2 C1 112.6(5) . . ? O4 C3 O3 124.1(5) . . ? O4 C3 C2 123.6(5) . . ? O3 C3 C2 112.2(5) . . ? N1 C4 N2 112.1(4) . . ? N4 C5 N1 111.2(4) . . ? N1 C6 N3 111.7(4) . . ? N4 C7 N2 111.6(4) . . ? N3 C8 N2 111.4(4) . . ? N4 C9 N3 110.4(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O1 1.00 1.64 2.526(6) 144.8 8_665 _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.883 _refine_diff_density_max 1.974 _refine_diff_density_min -1.237 _refine_diff_density_rms 0.185 #=======================================END data_complex_3 _database_code_CSD 170952 #data_ag1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H19 Ag N4 O3' _chemical_formula_weight 387.19 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 Pca2(1) 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 11.717(4) _cell_length_b 11.741(6) _cell_length_c 10.478(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1441.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 1.414 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.5880 _exptl_absorpt_correction_T_max 0.7848 _exptl_absorpt_process_details '\y-scans (North et al., 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 1908 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1745 _reflns_number_gt 1480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V. 5.0 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1067P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(16) _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 -0.06(9) _refine_ls_number_reflns 1745 _refine_ls_number_parameters 188 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1404 _refine_ls_wR_factor_gt 0.1319 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 1.312 _refine_ls_shift/su_mean 0.007 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.10365(3) 0.10073(4) -0.00004(10) 0.04034(12) Uani 1 d . . . O1 O -0.0617(7) 0.2339(6) 0.0359(8) 0.087(2) Uani 1 d . . . O2 O 0.0659(7) 0.2480(8) 0.1876(11) 0.108(3) Uani 1 d . . . N1 N 0.0975(4) 0.1277(5) -0.2251(5) 0.0368(13) Uani 1 d . . . N3 N 0.0525(6) 0.2558(5) -0.3964(5) 0.0423(13) Uani 1 d . . . N2 N 0.2090(4) 0.1210(4) -0.4207(5) 0.0320(11) Uani 1 d . . . N4 N 0.0103(4) 0.0547(5) -0.4224(4) 0.0343(11) Uani 1 d . . . C1 C 0.2089(6) 0.1063(5) -0.2810(5) 0.0329(13) Uani 1 d . . . H1A H 0.2327 0.0303 -0.2605 0.080 Uiso 1 d R . . H1B H 0.2631 0.1581 -0.2442 0.080 Uiso 1 d R . . C2 C 0.0575(7) 0.2390(6) -0.2597(7) 0.0450(17) Uani 1 d . . . H2A H 0.1076 0.2949 -0.2232 0.080 Uiso 1 d R . . H2B H -0.0171 0.2503 -0.2239 0.080 Uiso 1 d R . . C3 C 0.0176(5) 0.0423(6) -0.2806(5) 0.0354(13) Uani 1 d . . . H3A H -0.0568 0.0530 -0.2441 0.080 Uiso 1 d R . . H3B H 0.0428 -0.0333 -0.2599 0.080 Uiso 1 d R . . C4 C 0.1265(5) 0.0373(5) -0.4733(5) 0.0343(15) Uani 1 d . . . H4A H 0.1513 -0.0385 -0.4529 0.080 Uiso 1 d R . . H4B H 0.1245 0.0441 -0.5646 0.080 Uiso 1 d R . . C5 C -0.0248(5) 0.1706(6) -0.4508(7) 0.0445(16) Uani 1 d . . . H5A H -0.0261 0.1803 -0.5418 0.080 Uiso 1 d R . . H5B H -0.1008 0.1830 -0.4195 0.080 Uiso 1 d R . . C6 C 0.1646(5) 0.2361(5) -0.4491(7) 0.0386(14) Uani 1 d . . . H6A H 0.2164 0.2916 -0.4147 0.080 Uiso 1 d R . . H6B H 0.1615 0.2468 -0.5398 0.080 Uiso 1 d R . . C7 C -0.0268(7) 0.2746(6) 0.1357(10) 0.057(2) Uani 1 d . . . C8 C -0.1022(6) 0.3581(7) 0.2053(8) 0.0460(18) Uani 1 d . . . C9 C -0.0628(8) 0.4083(7) 0.3203(10) 0.057(2) Uani 1 d . . . H9A H 0.0124 0.3931 0.3523 0.080 Uiso 1 d R . . C10 C -0.1380(10) 0.4815(8) 0.3853(12) 0.075(3) Uani 1 d . . . H10A H -0.1144 0.5143 0.4650 0.080 Uiso 1 d R . . C11 C -0.2420(11) 0.5054(7) 0.3389(11) 0.074(3) Uani 1 d . . . H11A H -0.2909 0.5565 0.3849 0.080 Uiso 1 d R . . C12 C -0.2773(8) 0.4582(8) 0.2282(10) 0.071(3) Uani 1 d . . . H12A H -0.3514 0.4774 0.1955 0.080 Uiso 1 d R . . C13 C -0.2089(5) 0.3853(4) 0.1616(5) 0.056(2) Uani 1 d . . . H13A H -0.2363 0.3510 0.0843 0.080 Uiso 1 d R . . O1W O -0.2300(5) 0.1713(4) -0.1379(5) 0.076(2) Uani 1 d R . . H1WA H -0.1704 0.1938 -0.0762 0.120 Uiso 1 d R . . H1WB H -0.1934 0.1332 -0.2111 0.120 Uiso 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0349(2) 0.0601(3) 0.02604(19) -0.0022(3) 0.0010(3) -0.00308(16) O1 0.102(4) 0.076(4) 0.084(6) -0.019(4) 0.018(4) 0.023(4) O2 0.070(4) 0.113(5) 0.140(8) -0.018(6) 0.010(5) 0.045(4) N1 0.047(3) 0.044(3) 0.019(2) 0.005(2) -0.002(2) 0.003(2) N3 0.053(3) 0.040(3) 0.034(3) 0.001(2) -0.003(2) 0.006(2) N2 0.029(2) 0.051(3) 0.0159(19) -0.0009(19) -0.0003(18) -0.0049(19) N4 0.038(2) 0.045(3) 0.020(2) -0.002(2) 0.0002(19) -0.002(2) C1 0.041(3) 0.042(3) 0.016(2) 0.000(2) 0.000(2) -0.002(2) C2 0.054(4) 0.043(3) 0.039(3) -0.014(3) -0.001(3) 0.007(3) C3 0.034(3) 0.048(3) 0.024(3) 0.000(2) 0.008(2) -0.003(3) C4 0.031(2) 0.042(3) 0.030(4) -0.007(2) 0.002(2) -0.002(2) C5 0.029(3) 0.067(4) 0.038(3) 0.010(3) -0.005(2) -0.004(3) C6 0.042(3) 0.042(3) 0.032(2) 0.004(3) 0.002(3) -0.003(3) C7 0.053(4) 0.043(4) 0.075(5) 0.005(4) 0.018(4) 0.004(3) C8 0.054(4) 0.042(3) 0.042(4) 0.006(3) 0.006(3) 0.001(3) C9 0.052(4) 0.064(5) 0.056(5) 0.012(4) 0.005(4) 0.001(4) C10 0.104(7) 0.056(5) 0.064(6) -0.005(4) 0.007(6) -0.016(5) C11 0.096(7) 0.047(4) 0.079(6) -0.004(5) 0.018(6) 0.015(5) C12 0.063(5) 0.072(5) 0.078(7) 0.004(5) -0.002(5) 0.028(4) C13 0.063(5) 0.058(4) 0.048(4) 0.000(3) 0.000(4) 0.017(3) O1W 0.069(4) 0.075(4) 0.085(5) 0.014(4) 0.017(3) 0.026(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.359(5) 4 ? Ag1 N1 2.381(6) . ? Ag1 N4 2.402(5) 2 ? Ag1 O1 2.519(7) . ? O1 C7 1.220(12) . ? O2 C7 1.254(12) . ? N1 C2 1.435(9) . ? N1 C1 1.453(8) . ? N1 C3 1.490(8) . ? N3 C6 1.444(9) . ? N3 C2 1.447(9) . ? N3 C5 1.465(9) . ? N2 C1 1.473(7) . ? N2 C6 1.479(8) . ? N2 C4 1.484(7) . ? N2 Ag1 2.359(5) 4_554 ? N4 C5 1.452(9) . ? N4 C4 1.477(7) . ? N4 C3 1.495(7) . ? N4 Ag1 2.402(5) 2_554 ? C7 C8 1.508(11) . ? C8 C13 1.369(9) . ? C8 C9 1.419(13) . ? C9 C10 1.407(14) . ? C10 C11 1.341(17) . ? C11 C12 1.350(15) . ? C12 C13 1.365(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 111.36(18) 4 . ? N2 Ag1 N4 118.29(18) 4 2 ? N1 Ag1 N4 114.80(18) . 2 ? N2 Ag1 O1 126.9(2) 4 . ? N1 Ag1 O1 92.4(2) . . ? N4 Ag1 O1 89.6(2) 2 . ? C7 O1 Ag1 96.5(6) . . ? C2 N1 C1 110.4(5) . . ? C2 N1 C3 108.0(5) . . ? C1 N1 C3 106.9(5) . . ? C2 N1 Ag1 112.4(4) . . ? C1 N1 Ag1 110.4(4) . . ? C3 N1 Ag1 108.5(4) . . ? C6 N3 C2 108.7(6) . . ? C6 N3 C5 107.7(5) . . ? C2 N3 C5 108.5(6) . . ? C1 N2 C6 107.8(5) . . ? C1 N2 C4 106.9(5) . . ? C6 N2 C4 107.5(5) . . ? C1 N2 Ag1 109.8(4) . 4_554 ? C6 N2 Ag1 110.4(3) . 4_554 ? C4 N2 Ag1 114.1(4) . 4_554 ? C5 N4 C4 108.4(5) . . ? C5 N4 C3 108.1(5) . . ? C4 N4 C3 107.0(5) . . ? C5 N4 Ag1 119.0(4) . 2_554 ? C4 N4 Ag1 106.6(4) . 2_554 ? C3 N4 Ag1 107.1(4) . 2_554 ? N1 C1 N2 112.4(5) . . ? N1 C2 N3 112.8(6) . . ? N1 C3 N4 111.0(5) . . ? N4 C4 N2 112.0(5) . . ? N4 C5 N3 112.7(5) . . ? N3 C6 N2 112.9(5) . . ? O1 C7 O2 124.4(9) . . ? O1 C7 C8 118.2(8) . . ? O2 C7 C8 117.3(9) . . ? C13 C8 C9 119.0(7) . . ? C13 C8 C7 121.7(7) . . ? C9 C8 C7 119.4(7) . . ? C10 C9 C8 117.5(9) . . ? C11 C10 C9 121.4(11) . . ? C10 C11 C12 120.3(10) . . ? C11 C12 C13 121.1(8) . . ? C12 C13 C8 120.8(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O1 0.99 1.80 2.783(10) 179.7 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.045 _refine_diff_density_min -1.525 _refine_diff_density_rms 0.151 #=======================================END data_complex_4 _database_code_CSD 170953 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H19 Ag N4 O4' _chemical_formula_weight 403.19 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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.620(6) _cell_length_b 10.807(5) _cell_length_c 23.145(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2906(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description polyhedral _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.28 _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 1.412 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.603 _exptl_absorpt_correction_T_max 0.781 _exptl_absorpt_process_details '\y-scans (North et al., 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 2556 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0836 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2556 _reflns_number_gt 1487 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2556 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1362 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 3.191 _refine_ls_shift/su_mean 0.016 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.11325(5) 0.16367(6) 0.20759(3) 0.0402(3) Uani 1 d . . . N1 N 0.1008(5) 0.3764(5) 0.1922(3) 0.0282(16) Uani 1 d . . . N2 N 0.2053(5) 0.5731(6) 0.1910(3) 0.0299(17) Uani 1 d . . . N3 N 0.0560(6) 0.5327(6) 0.1201(3) 0.0387(18) Uani 1 d . . . N4 N 0.0036(5) 0.5679(6) 0.2203(3) 0.0295(17) Uani 1 d . . . O1W O -0.2559(6) 0.3077(6) 0.1703(3) 0.064(2) Uani 1 d . . . H1WA H -0.2248 0.2449 0.1560 0.050 Uiso 1 d R . . C1 C 0.0152(6) 0.4330(6) 0.2306(4) 0.030(2) Uani 1 d . . . H1A H 0.0355 0.4187 0.2703 0.080 Uiso 1 d R . . H1B H -0.0578 0.3942 0.2236 0.080 Uiso 1 d R . . C2 C 0.0651(7) 0.4017(8) 0.1320(4) 0.037(2) Uani 1 d . . . H2A H -0.0092 0.3651 0.1259 0.080 Uiso 1 d R . . H2B H 0.1185 0.3640 0.1057 0.080 Uiso 1 d R . . C3 C 0.2119(6) 0.4375(6) 0.2019(4) 0.0306(19) Uani 1 d . . . H3A H 0.2671 0.4042 0.1753 0.080 Uiso 1 d R . . H3B H 0.2395 0.4224 0.2403 0.080 Uiso 1 d R . . C4 C 0.1674(7) 0.5900(8) 0.1306(4) 0.042(2) Uani 1 d . . . H4A H 0.1607 0.6767 0.1222 0.080 Uiso 1 d R . . H4B H 0.2245 0.5551 0.1054 0.080 Uiso 1 d R . . C5 C -0.0290(6) 0.5863(7) 0.1599(4) 0.037(2) Uani 1 d . . . H5A H -0.0328 0.6736 0.1526 0.080 Uiso 1 d R . . H5B H -0.1036 0.5512 0.1528 0.080 Uiso 1 d R . . C6 C 0.1173(6) 0.6238(7) 0.2301(4) 0.034(2) Uani 1 d . . . H6A H 0.1399 0.6098 0.2695 0.080 Uiso 1 d R . . H6B H 0.1110 0.7114 0.2241 0.080 Uiso 1 d R . . C7 C -0.0417(9) 0.0583(9) 0.1128(4) 0.048(3) Uani 1 d . . . C8 C -0.1018(7) -0.0239(8) 0.0724(3) 0.0338(19) Uani 1 d . . . C9 C -0.0495(9) -0.1296(8) 0.0523(4) 0.048(3) Uani 1 d . . . C10 C -0.1095(13) -0.2152(10) 0.0183(5) 0.078(4) Uani 1 d . . . H10A H -0.0711 -0.2883 0.0048 0.080 Uiso 1 d R . . C11 C -0.2195(15) -0.1895(12) 0.0043(5) 0.094(5) Uani 1 d . . . H11A H -0.2615 -0.2492 -0.0180 0.080 Uiso 1 d R . . C12 C -0.2726(9) -0.0829(12) 0.0214(5) 0.075(4) Uani 1 d . . . H12A H -0.3493 -0.0653 0.0083 0.080 Uiso 1 d R . . C13 C -0.2150(9) -0.0036(10) 0.0567(4) 0.056(3) Uani 1 d . . . H13A H -0.2534 0.0680 0.0718 0.080 Uiso 1 d R . . O1 O 0.0584(6) 0.0305(8) 0.1267(3) 0.079(2) Uani 1 d . . . O2 O -0.0914(7) 0.1488(7) 0.1333(3) 0.079(2) Uani 1 d . . . O3 O 0.0611(6) -0.1570(7) 0.0657(3) 0.079(2) Uani 1 d . . . H3 H 0.0890 -0.1005 0.0924 0.050 Uiso 1 d R . . H1WB H -0.3004 0.3842 0.1691 0.050 Uiso 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0257(3) 0.0273(3) 0.0676(5) -0.0023(4) 0.0044(4) 0.0011(3) N1 0.023(3) 0.023(3) 0.039(4) -0.002(3) -0.001(3) -0.002(3) N2 0.022(3) 0.027(3) 0.041(5) 0.002(3) -0.002(3) 0.000(3) N3 0.033(4) 0.048(4) 0.036(5) 0.003(4) -0.009(4) -0.010(3) N4 0.017(3) 0.029(3) 0.043(5) -0.004(3) -0.001(3) -0.001(3) O1W 0.065(4) 0.060(5) 0.067(5) -0.005(4) 0.000(4) 0.019(4) C1 0.020(4) 0.021(4) 0.049(6) 0.003(4) 0.009(4) -0.002(3) C2 0.038(5) 0.042(5) 0.032(5) -0.007(4) -0.007(4) -0.006(4) C3 0.022(4) 0.026(4) 0.044(5) 0.006(4) -0.003(4) 0.003(3) C4 0.032(5) 0.044(5) 0.050(6) 0.010(5) 0.000(5) 0.002(4) C5 0.018(4) 0.030(5) 0.062(7) 0.010(4) -0.006(4) 0.003(4) C6 0.024(4) 0.028(4) 0.051(6) -0.009(4) 0.009(4) -0.002(4) C7 0.064(7) 0.039(5) 0.041(6) -0.001(5) -0.001(5) -0.008(5) C8 0.033(5) 0.039(5) 0.029(5) 0.004(4) 0.003(4) -0.004(4) C9 0.052(6) 0.042(6) 0.050(7) 0.011(5) 0.008(5) 0.001(5) C10 0.138(13) 0.046(6) 0.049(7) -0.011(5) -0.001(8) 0.005(8) C11 0.153(15) 0.074(9) 0.054(8) 0.012(7) -0.053(10) -0.052(9) C12 0.042(7) 0.118(11) 0.065(8) 0.026(8) -0.029(6) -0.030(7) C13 0.056(7) 0.068(7) 0.044(7) 0.011(6) -0.001(5) 0.000(6) O1 0.044(4) 0.111(7) 0.081(6) 0.005(5) -0.027(4) -0.014(4) O2 0.109(6) 0.061(5) 0.068(5) -0.024(4) -0.006(5) 0.002(5) O3 0.068(5) 0.080(5) 0.089(6) -0.006(5) 0.003(4) 0.035(5) _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 2.331(6) . ? Ag1 N2 2.356(6) 8_655 ? Ag1 N4 2.388(6) 3_545 ? Ag1 O1 2.447(8) . ? N1 C3 1.467(9) . ? N1 C1 1.468(9) . ? N1 C2 1.480(10) . ? N2 C6 1.471(9) . ? N2 C4 1.478(10) . ? N2 C3 1.488(8) . ? N2 Ag1 2.356(6) 8_665 ? N3 C2 1.446(10) . ? N3 C4 1.455(10) . ? N3 C5 1.469(10) . ? N4 C5 1.463(10) . ? N4 C6 1.470(9) . ? N4 C1 1.483(8) . ? N4 Ag1 2.388(6) 3 ? C7 O2 1.231(11) . ? C7 O1 1.243(11) . ? C7 C8 1.466(12) . ? C8 C9 1.375(12) . ? C8 C13 1.383(12) . ? C9 O3 1.354(11) . ? C9 C10 1.401(15) . ? C10 C11 1.347(17) . ? C11 C12 1.366(17) . ? C12 C13 1.360(14) . ? 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 N2 116.1(2) . 8_655 ? N1 Ag1 N4 119.9(2) . 3_545 ? N2 Ag1 N4 116.3(2) 8_655 3_545 ? N1 Ag1 O1 116.6(2) . . ? N2 Ag1 O1 82.2(2) 8_655 . ? N4 Ag1 O1 97.6(2) 3_545 . ? C3 N1 C1 108.5(6) . . ? C3 N1 C2 107.9(6) . . ? C1 N1 C2 107.7(6) . . ? C3 N1 Ag1 111.5(4) . . ? C1 N1 Ag1 111.1(4) . . ? C2 N1 Ag1 110.1(4) . . ? C6 N2 C4 109.2(6) . . ? C6 N2 C3 107.4(6) . . ? C4 N2 C3 107.3(6) . . ? C6 N2 Ag1 111.6(5) . 8_665 ? C4 N2 Ag1 111.7(5) . 8_665 ? C3 N2 Ag1 109.6(4) . 8_665 ? C2 N3 C4 108.7(6) . . ? C2 N3 C5 108.4(7) . . ? C4 N3 C5 109.0(6) . . ? C5 N4 C6 108.9(6) . . ? C5 N4 C1 108.1(6) . . ? C6 N4 C1 107.3(6) . . ? C5 N4 Ag1 117.5(4) . 3 ? C6 N4 Ag1 103.0(4) . 3 ? C1 N4 Ag1 111.4(5) . 3 ? N1 C1 N4 111.9(6) . . ? N3 C2 N1 112.3(6) . . ? N1 C3 N2 111.9(6) . . ? N3 C4 N2 111.7(7) . . ? N4 C5 N3 111.7(6) . . ? N4 C6 N2 112.2(6) . . ? O2 C7 O1 122.1(10) . . ? O2 C7 C8 120.2(10) . . ? O1 C7 C8 117.6(9) . . ? C9 C8 C13 117.6(9) . . ? C9 C8 C7 120.5(9) . . ? C13 C8 C7 121.7(9) . . ? O3 C9 C8 121.5(9) . . ? O3 C9 C10 117.2(10) . . ? C8 C9 C10 121.2(10) . . ? C11 C10 C9 118.1(11) . . ? C10 C11 C12 122.2(11) . . ? C13 C12 C11 118.9(11) . . ? C12 C13 C8 121.8(10) . . ? C7 O1 Ag1 107.4(7) . . ? _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.880 _refine_diff_density_max 0.719 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.117 #_eof #End of Crystallographic Information File