data_e:\crystal\yy-18\yy-93\60 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 Ag N2 O2, N O3' _chemical_formula_sum 'C20 H18 Ag N3 O5' _chemical_formula_weight 488.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 Pbcn _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 14.6380(9) _cell_length_b 7.6050(5) _cell_length_c 17.2027(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1915.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4031 _cell_measurement_theta_min 3.0177 _cell_measurement_theta_max 27.4835 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.4000 _exptl_crystal_size_mid 0.4000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.091 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.8156 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Corp., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13677 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0129 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2191 _reflns_number_gt 2038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _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^)+(0.0391P)^2^+0.9556P] 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 2191 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0947 _refine_ls_goodness_of_fit_ref 1.214 _refine_ls_restrained_S_all 1.214 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.002 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 0.09955(4) 0.7500 0.06242(14) Uani 1 2 d S . . C8 C 0.68136(19) 0.2072(3) 0.85035(16) 0.0552(6) Uani 1 1 d . . . C4 C 0.8054(2) 0.1157(3) 0.76561(17) 0.0559(6) Uani 1 1 d . . . C9 C 0.71092(17) 0.1332(3) 0.77908(16) 0.0482(5) Uani 1 1 d . . . C1 C 0.67529(19) 0.0186(3) 0.65687(15) 0.0551(6) Uani 1 1 d . . . C2 C 0.76893(19) -0.0011(4) 0.64033(17) 0.0629(7) Uani 1 1 d . . . H2 H 0.7876 -0.0465 0.5914 0.075 Uiso 1 1 calc R . . C3 C 0.8316(2) 0.0439(4) 0.69322(19) 0.0662(8) Uani 1 1 d . . . H3 H 0.8946 0.0275 0.6820 0.079 Uiso 1 1 calc R . . C7 C 0.7444(2) 0.2594(4) 0.90460(17) 0.0666(7) Uani 1 1 d . . . H7 H 0.7243 0.3090 0.9523 0.080 Uiso 1 1 calc R . . C10 C 0.6052(2) -0.0311(5) 0.59795(19) 0.0777(9) Uani 1 1 d . . . H10A H 0.6352 -0.0867 0.5534 0.116 Uiso 1 1 calc R . . H10B H 0.5727 0.0745 0.5806 0.116 Uiso 1 1 calc R . . H10C H 0.5616 -0.1136 0.6212 0.116 Uiso 1 1 calc R . . C6 C 0.8379(2) 0.2402(4) 0.8904(2) 0.0753(9) Uani 1 1 d . . . H6 H 0.8808 0.2768 0.9286 0.090 Uiso 1 1 calc R . . C5 C 0.8680(2) 0.1705(5) 0.8229(2) 0.0740(9) Uani 1 1 d . . . H5 H 0.9318 0.1582 0.8140 0.089 Uiso 1 1 calc R . . N2 N 1.0000 0.0000 0.5000 0.0628(9) Uani 1 2 d S . . O4 O 0.9329(4) 0.1181(7) 0.4963(3) 0.096(2) Uani 0.50 1 d P . . O2 O 1.0522(5) -0.0025(13) 0.4586(4) 0.117(2) Uani 0.50 1 d P . . O3 O 0.9806(5) -0.1089(10) 0.5523(5) 0.108(3) Uani 0.50 1 d P . . N1 N 0.64680(15) 0.0829(3) 0.72442(14) 0.0485(5) Uani 1 1 d . . . O1 O 0.59068(16) 0.2236(4) 0.86083(15) 0.0813(8) Uani 1 1 d . . . H1 H 0.587(2) 0.282(4) 0.8909(18) 0.057(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.04025(18) 0.0679(2) 0.0791(2) 0.000 0.01116(12) 0.000 C8 0.0546(14) 0.0470(13) 0.0642(15) -0.0039(11) 0.0076(12) -0.0003(11) C4 0.0442(14) 0.0503(14) 0.0733(17) 0.0138(12) 0.0063(12) 0.0006(11) C9 0.0434(13) 0.0425(11) 0.0587(13) 0.0053(11) 0.0072(11) 0.0020(9) C1 0.0606(15) 0.0454(13) 0.0595(14) 0.0002(11) 0.0146(12) 0.0031(11) C2 0.0619(16) 0.0591(15) 0.0677(17) 0.0031(13) 0.0268(13) 0.0071(13) C3 0.0466(14) 0.0655(17) 0.086(2) 0.0104(15) 0.0237(14) 0.0077(13) C7 0.082(2) 0.0535(15) 0.0639(16) -0.0022(13) -0.0034(15) -0.0041(14) C10 0.084(2) 0.081(2) 0.0683(18) -0.0163(17) 0.0056(16) 0.0024(18) C6 0.072(2) 0.0672(18) 0.087(2) 0.0089(16) -0.0215(17) -0.0048(15) C5 0.0491(15) 0.0726(19) 0.100(2) 0.0154(18) -0.0072(15) 0.0014(14) N2 0.074(3) 0.067(2) 0.0475(17) -0.0021(16) -0.0078(18) 0.0062(17) O4 0.127(5) 0.108(4) 0.054(2) 0.016(3) 0.013(3) 0.066(3) O2 0.074(4) 0.186(8) 0.090(4) -0.013(5) 0.045(4) 0.004(5) O3 0.078(4) 0.125(6) 0.121(5) 0.069(4) -0.001(4) 0.017(3) N1 0.0431(11) 0.0437(10) 0.0586(11) -0.0010(9) 0.0119(9) 0.0013(8) O1 0.0576(12) 0.1015(18) 0.0849(16) -0.0420(15) 0.0215(11) -0.0022(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 Ag1 N1 2.197(2) 4_656 ? Ag1 N1 2.197(2) . ? Ag1 O1 2.508(3) . ? Ag1 O1 2.508(3) 4_656 ? C8 O1 1.345(3) . ? C8 C7 1.371(4) . ? C8 C9 1.417(4) . ? C4 C9 1.409(4) . ? C4 C5 1.409(4) . ? C4 C3 1.413(4) . ? C9 N1 1.383(4) . ? C1 N1 1.328(3) . ? C1 C2 1.408(4) . ? C1 C10 1.491(4) . ? C2 C3 1.337(4) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C7 C6 1.399(5) . ? C7 H7 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C6 C5 1.350(5) . ? C6 H6 0.9500 . ? C5 H5 0.9500 . ? N2 O2 1.045(5) 5_756 ? N2 O2 1.045(5) . ? N2 O3 1.255(6) . ? N2 O3 1.255(6) 5_756 ? N2 O4 1.332(5) 5_756 ? N2 O4 1.332(5) . ? O4 O2 1.194(10) 5_756 ? O4 O3 1.517(9) 5_756 ? O2 O3 0.992(9) 5_756 ? O2 O4 1.194(10) 5_756 ? O3 O2 0.992(9) 5_756 ? O3 O4 1.517(9) 5_756 ? O1 H1 0.69(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 173.38(10) 4_656 . ? N1 Ag1 O1 112.78(8) 4_656 . ? N1 Ag1 O1 69.90(8) . . ? N1 Ag1 O1 69.90(8) 4_656 4_656 ? N1 Ag1 O1 112.78(8) . 4_656 ? O1 Ag1 O1 135.78(13) . 4_656 ? O1 C8 C7 123.1(3) . . ? O1 C8 C9 117.0(3) . . ? C7 C8 C9 119.9(3) . . ? C9 C4 C5 119.7(3) . . ? C9 C4 C3 116.6(3) . . ? C5 C4 C3 123.7(3) . . ? N1 C9 C4 121.9(3) . . ? N1 C9 C8 119.4(2) . . ? C4 C9 C8 118.7(3) . . ? N1 C1 C2 121.4(3) . . ? N1 C1 C10 118.2(2) . . ? C2 C1 C10 120.4(3) . . ? C3 C2 C1 120.2(3) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 120.8(3) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C8 C7 C6 120.6(3) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C6 C7 120.7(3) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C5 C4 120.3(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? O2 N2 O2 180.0(6) 5_756 . ? O2 N2 O3 50.1(5) 5_756 . ? O2 N2 O3 129.9(5) . . ? O2 N2 O3 129.9(5) 5_756 5_756 ? O2 N2 O3 50.1(5) . 5_756 ? O3 N2 O3 180.000(2) . 5_756 ? O2 N2 O4 121.2(6) 5_756 5_756 ? O2 N2 O4 58.8(6) . 5_756 ? O3 N2 O4 71.7(4) . 5_756 ? O3 N2 O4 108.3(4) 5_756 5_756 ? O2 N2 O4 58.8(6) 5_756 . ? O2 N2 O4 121.2(6) . . ? O3 N2 O4 108.3(4) . . ? O3 N2 O4 71.7(4) 5_756 . ? O4 N2 O4 180.000(2) 5_756 . ? O2 O4 N2 48.5(3) 5_756 . ? O2 O4 O3 99.9(4) 5_756 5_756 ? N2 O4 O3 51.8(3) . 5_756 ? O3 O2 N2 76.0(6) 5_756 . ? O3 O2 O4 147.1(9) 5_756 5_756 ? N2 O2 O4 72.7(6) . 5_756 ? O2 O3 N2 53.9(5) 5_756 . ? O2 O3 O4 109.9(7) 5_756 5_756 ? N2 O3 O4 56.5(3) . 5_756 ? C1 N1 C9 118.9(2) . . ? C1 N1 Ag1 120.24(19) . . ? C9 N1 Ag1 120.78(17) . . ? C8 O1 Ag1 112.67(18) . . ? C8 O1 H1 104(3) . . ? Ag1 O1 H1 141(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.450 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.049