# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_globa _journal_name_full CrystEngComm #TrackingRef '- p1-2-r1.cif' _journal_coden_Cambridge 1350 _audit_update_record ; 2010-01-10 # Formatted by publCIF ; #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Rongbin Huang Department of Chemistry Xiamen University Xiamen, 361005 P. R. China ; _publ_contact_author_phone 86-592-2185191 _publ_contact_author_fax 86-592-2183047 _publ_contact_author_email rbhuang@xmu.edu.cn _publ_requested_coeditor_name ? _publ_contact_letter ; ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) # 3. TITLE AND AUTHOR LIST _publ_section_title ; Self-assembly, thermal stability and photoluminescence of two mixed-ligand silver(I) networks via 2D-2D and 2D-3D parallel interpenetration of (4,4) nets ; loop_ _publ_author_name _publ_author_address 'Di Sun' ; Department of chemistry, Xiamen University, Xiamen 361005, People's Republic of China ; 'Na Zhang' ; Department of chemistry, Xiamen University, Xiamen 361005, People's Republic of China ; 'Qin-Juan Xu' ; Department of chemistry, Xiamen University, Xiamen 361005, People's Republic of China ; 'Rong-Bin Huang' ; Department of chemistry, Xiamen University, Xiamen 361005, People's Republic of China ; 'Lan-Sun Zheng' ; State key Laboratory for Physical Chemistry of Solid Surfaces, Xiamen University, Xiamen 361005, People's Republic of China ; _publ_section_exptl_refinement ; All H atoms were placed geometrically with C---H = 0.93 (aromatic) or 0.96 \%A (CH~3~), N---H distances of 0.86\%A and refined using a riding atom model with their isotropic displacement factors, U~iso~ fixed at 1.2 time the U~eq~ of the parent C and N atom. ; _publ_contact_author_name 'Rongbin Huang' data_p1 _database_code_depnum_ccdc_archive 'CCDC 769616' #TrackingRef '- p1-2-r1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C8 H11 Ag N3 O2), H O' _chemical_formula_sum 'C16 H23 Ag2 N6 O5' _chemical_formula_weight 595.14 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' Ag Ag -0.8971 1.1015 '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' _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 12.502(3) _cell_length_b 20.211(4) _cell_length_c 9.1833(18) _cell_angle_alpha 90.00 _cell_angle_beta 112.49(3) _cell_angle_gamma 90.00 _cell_volume 2143.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4895 _cell_measurement_theta_min 6.27 _cell_measurement_theta_max 54.95 _exptl_crystal_description ? _exptl_crystal_colour ? _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 1.844 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 1.865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7672 _exptl_absorpt_correction_T_max 0.8354 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7739 _diffrn_reflns_av_R_equivalents 0.0862 _diffrn_reflns_av_sigmaI/netI 0.0727 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1884 _reflns_number_gt 1175 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1884 _refine_ls_number_parameters 135 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1417 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.21586(5) 0.7500 0.0711(4) Uani 1 2 d S . . Ag2 Ag 0.0000 0.12200(5) 0.2500 0.0723(4) Uani 1 2 d S . . C1 C 0.2561(7) 0.1392(4) 0.4838(9) 0.0534(18) Uani 1 1 d . . . C2 C 0.4222(7) 0.1016(4) 0.4600(11) 0.071(2) Uani 1 1 d . . . C3 C 0.3555(8) 0.0636(4) 0.3350(10) 0.077(3) Uani 1 1 d . . . H3A H 0.3906 0.0365 0.2843 0.093 Uiso 1 1 calc R . . C4 C 0.2375(7) 0.0652(4) 0.2844(9) 0.059(2) Uani 1 1 d . . . C5 C 0.1605(8) 0.0246(5) 0.1469(10) 0.082(3) Uani 1 1 d . . . H5A H 0.1109 -0.0027 0.1795 0.124 Uiso 1 1 calc R . . H5B H 0.2073 -0.0028 0.1096 0.124 Uiso 1 1 calc R . . H5C H 0.1142 0.0536 0.0638 0.124 Uiso 1 1 calc R . . C6 C 0.5515(8) 0.1032(5) 0.5167(14) 0.107(4) Uani 1 1 d . . . H6A H 0.5843 0.1029 0.6299 0.161 Uiso 1 1 calc R . . H6B H 0.5752 0.1426 0.4789 0.161 Uiso 1 1 calc R . . H6C H 0.5780 0.0650 0.4778 0.161 Uiso 1 1 calc R . . C7 C 0.7012(7) 0.2743(4) 0.4666(10) 0.067(2) Uani 1 1 d . . . H7A H 0.6542 0.2608 0.3598 0.080 Uiso 1 1 calc R . . H7B H 0.7340 0.3172 0.4605 0.080 Uiso 1 1 calc R . . C8 C 0.6218(7) 0.2825(4) 0.5568(9) 0.052(2) Uani 1 1 d . . . N1 N 0.2066(5) 0.1749(3) 0.5618(7) 0.0664(18) Uani 1 1 d . . . H1A H 0.1325 0.1751 0.5320 0.080 Uiso 1 1 calc R . . H1B H 0.2486 0.1978 0.6422 0.080 Uiso 1 1 calc R . . N2 N 0.3737(5) 0.1406(3) 0.5373(7) 0.0555(16) Uani 1 1 d . . . N3 N 0.1866(5) 0.1038(3) 0.3575(6) 0.0532(15) Uani 1 1 d . . . O1 O 0.6456(4) 0.2493(3) 0.6809(6) 0.0638(14) Uani 1 1 d . . . O1W O 0.0000 0.0916(5) 0.7500 0.113(4) Uani 1 2 d S . . H1WA H -0.0122 0.1162 0.6702 0.135 Uiso 0.50 1 d PR . . O2 O 0.5389(5) 0.3209(3) 0.5023(6) 0.0713(16) 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 0.0491(6) 0.1086(9) 0.0693(6) 0.000 0.0378(4) 0.000 Ag2 0.0498(6) 0.0937(8) 0.0631(6) 0.000 0.0102(4) 0.000 C1 0.048(5) 0.061(5) 0.053(4) 0.002(4) 0.022(4) 0.004(4) C2 0.057(5) 0.070(6) 0.098(6) -0.021(5) 0.043(5) 0.000(4) C3 0.079(6) 0.080(6) 0.084(6) -0.031(5) 0.045(5) -0.006(5) C4 0.064(5) 0.056(5) 0.062(5) -0.003(4) 0.028(4) -0.002(4) C5 0.085(7) 0.086(7) 0.075(5) -0.029(5) 0.030(5) -0.008(5) C6 0.056(6) 0.123(9) 0.147(10) -0.049(8) 0.044(6) 0.002(6) C7 0.052(5) 0.094(7) 0.068(5) 0.017(4) 0.038(4) 0.015(4) C8 0.048(5) 0.064(5) 0.051(4) 0.003(4) 0.025(4) -0.004(4) N1 0.044(4) 0.089(5) 0.069(4) -0.018(4) 0.026(3) -0.001(4) N2 0.044(4) 0.063(4) 0.067(4) -0.009(3) 0.030(3) -0.003(3) N3 0.051(4) 0.060(4) 0.049(3) -0.005(3) 0.020(3) -0.007(3) O1 0.049(3) 0.089(4) 0.066(3) 0.023(3) 0.035(3) 0.012(3) O1W 0.175(11) 0.085(7) 0.080(6) 0.000 0.052(6) 0.000 O2 0.057(3) 0.101(4) 0.067(3) 0.024(3) 0.036(3) 0.029(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 O1 2.248(5) . y Ag1 O1 2.248(5) 2_656 ? Ag1 N2 2.503(6) . ? Ag1 N2 2.503(6) 2_656 y Ag1 Ag2 3.2770(16) 7_556 y Ag2 N3 2.189(6) 2 y Ag2 N3 2.189(6) . ? Ag2 O2 2.755(5) 7_556 ? Ag2 O2 2.755(5) 8_455 y Ag2 Ag1 3.2770(16) 7_556 ? C1 N1 1.324(9) . ? C1 N3 1.358(9) . ? C1 N2 1.361(9) . ? C2 N2 1.349(9) . ? C2 C3 1.368(11) . ? C2 C6 1.498(12) . ? C3 C4 1.368(11) . ? C3 H3A 0.9300 . ? C4 N3 1.337(9) . ? C4 C5 1.504(10) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C7 1.503(14) 7_656 ? C7 C8 1.525(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O2 1.237(9) . ? C8 O1 1.256(8) . ? N1 H1A 0.8600 . ? N1 H1B 0.8600 . ? O1W H1WA 0.8499 . ? O2 Ag2 2.755(5) 7_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 O1 Ag1 O1 145.0(3) . 2_656 y O1 Ag1 N2 107.4(2) . . y O1 Ag1 N2 93.78(19) 2_656 . y O1 Ag1 N2 93.78(19) . 2_656 y O1 Ag1 N2 107.4(2) 2_656 2_656 y N2 Ag1 N2 105.1(3) . 2_656 y O1 Ag1 Ag2 72.52(15) . 7_556 y O1 Ag1 Ag2 72.52(15) 2_656 7_556 y N2 Ag1 Ag2 127.44(14) . 7_556 y N2 Ag1 Ag2 127.44(14) 2_656 7_556 y N3 Ag2 N3 160.6(3) 2 . y N3 Ag2 O2 87.05(19) 2 7_556 y N3 Ag2 O2 101.1(2) . 7_556 y N3 Ag2 O2 101.1(2) 2 8_455 y N3 Ag2 O2 87.05(19) . 8_455 y O2 Ag2 O2 130.5(3) 7_556 8_455 y N3 Ag2 Ag1 99.70(16) 2 7_556 y N3 Ag2 Ag1 99.70(16) . 7_556 y O2 Ag2 Ag1 65.23(13) 7_556 7_556 y O2 Ag2 Ag1 65.23(13) 8_455 7_556 y N1 C1 N3 118.1(7) . . ? N1 C1 N2 117.2(7) . . ? N3 C1 N2 124.7(7) . . ? N2 C2 C3 121.2(8) . . ? N2 C2 C6 116.6(8) . . ? C3 C2 C6 122.3(8) . . ? C2 C3 C4 120.2(8) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? N3 C4 C3 120.1(7) . . ? N3 C4 C5 117.7(7) . . ? C3 C4 C5 122.2(7) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C7 C7 C8 116.4(8) 7_656 . ? C7 C7 H7A 108.2 7_656 . ? C8 C7 H7A 108.2 . . ? C7 C7 H7B 108.2 7_656 . ? C8 C7 H7B 108.2 . . ? H7A C7 H7B 107.3 . . ? O2 C8 O1 125.0(7) . . ? O2 C8 C7 117.8(6) . . ? O1 C8 C7 117.2(7) . . ? C1 N1 H1A 120.0 . . ? C1 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? C2 N2 C1 116.1(7) . . ? C2 N2 Ag1 119.3(5) . . ? C1 N2 Ag1 124.4(5) . . ? C4 N3 C1 117.7(7) . . ? C4 N3 Ag2 120.1(5) . . ? C1 N3 Ag2 121.3(5) . . ? C8 O1 Ag1 118.7(5) . . ? C8 O2 Ag2 108.3(4) . 7_556 ? 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 N1 H1A O2 0.86 2.05 2.897(9) 170.9 7_556 O1W H1WA O2 0.85 1.96 2.806(8) 175.4 7_556 N1 H1B O1 0.86 1.96 2.814(8) 175.3 2_656 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.899 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.106 data_p2 _database_code_depnum_ccdc_archive 'CCDC 769617' #TrackingRef '- p1-2-r1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H22 Ag2 N6 O4, 2(H2 O)' _chemical_formula_sum 'C20 H26 Ag2 N6 O6' _chemical_formula_weight 662.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.699(2) _cell_length_b 11.427(2) _cell_length_c 18.680(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.18(3) _cell_angle_gamma 90.00 _cell_volume 2372.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9146 _cell_measurement_theta_min 6.06 _cell_measurement_theta_max 54.89 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.854 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 1.699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7275 _exptl_absorpt_correction_T_max 0.8485 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13894 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4610 _reflns_number_gt 3403 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+0.0699P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4610 _refine_ls_number_parameters 312 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0858 _refine_ls_wR_factor_gt 0.0778 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.23521(2) 0.22753(3) 0.488162(18) 0.03816(11) Uani 1 1 d . . . Ag2 Ag 0.73159(3) 0.45595(3) 0.497784(17) 0.03735(11) Uani 1 1 d . . . C1 C -0.0268(3) 0.2920(4) 0.4870(2) 0.0274(9) Uani 1 1 d . . . C2 C -0.2048(3) 0.2230(4) 0.4049(2) 0.0316(10) Uani 1 1 d . . . C3 C -0.1448(4) 0.1315(4) 0.3855(2) 0.0404(11) Uani 1 1 d . . . H3A H -0.1864 0.0738 0.3524 0.049 Uiso 1 1 calc R . . C4 C -0.0200(3) 0.1269(4) 0.4164(2) 0.0359(10) Uani 1 1 d . . . C5 C 0.0533(4) 0.0309(5) 0.3960(3) 0.0553(14) Uani 1 1 d . . . H5A H 0.0979 -0.0103 0.4408 0.083 Uiso 1 1 calc R . . H5B H 0.1081 0.0647 0.3728 0.083 Uiso 1 1 calc R . . H5C H 0.0005 -0.0225 0.3615 0.083 Uiso 1 1 calc R . . C6 C -0.3380(3) 0.2407(4) 0.3686(2) 0.0415(11) Uani 1 1 d . . . H6A H -0.3793 0.2233 0.4044 0.062 Uiso 1 1 calc R . . H6B H -0.3664 0.1895 0.3260 0.062 Uiso 1 1 calc R . . H6C H -0.3532 0.3204 0.3523 0.062 Uiso 1 1 calc R . . C7 C 0.4987(3) 0.3066(4) 0.5028(2) 0.0279(9) Uani 1 1 d . . . C8 C 0.4909(3) 0.1374(4) 0.5684(2) 0.0327(10) Uani 1 1 d . . . C9 C 0.6128(3) 0.1469(4) 0.6048(2) 0.0372(11) Uani 1 1 d . . . H9A H 0.6533 0.0896 0.6386 0.045 Uiso 1 1 calc R . . C10 C 0.6734(3) 0.2425(4) 0.5902(2) 0.0317(10) Uani 1 1 d . . . C11 C 0.8041(4) 0.2630(5) 0.6330(2) 0.0458(12) Uani 1 1 d . . . H11A H 0.8516 0.2521 0.5998 0.069 Uiso 1 1 calc R . . H11B H 0.8295 0.2086 0.6740 0.069 Uiso 1 1 calc R . . H11C H 0.8144 0.3415 0.6523 0.069 Uiso 1 1 calc R . . C12 C 0.4201(4) 0.0354(4) 0.5821(3) 0.0461(12) Uani 1 1 d . . . H12A H 0.3732 0.0026 0.5347 0.069 Uiso 1 1 calc R . . H12B H 0.3675 0.0611 0.6094 0.069 Uiso 1 1 calc R . . H12C H 0.4741 -0.0229 0.6109 0.069 Uiso 1 1 calc R . . C13 C 1.0084(3) 0.6489(4) 0.70642(19) 0.0277(9) Uani 1 1 d . . . C14 C 1.1153(3) 0.5919(4) 0.7087(2) 0.0318(9) Uani 1 1 d . . . H14A H 1.1142 0.5286 0.6773 0.038 Uiso 1 1 calc R . . C15 C 1.2239(3) 0.6317(4) 0.7589(2) 0.0346(10) Uani 1 1 d . . . H15A H 1.2954 0.5945 0.7605 0.041 Uiso 1 1 calc R . . C16 C 1.2265(3) 0.7254(4) 0.8062(2) 0.0338(10) Uani 1 1 d . . . H16A H 1.2994 0.7507 0.8393 0.041 Uiso 1 1 calc R . . C17 C 1.1196(3) 0.7825(4) 0.80420(19) 0.0282(9) Uani 1 1 d . . . C18 C 1.0115(3) 0.7432(4) 0.75399(19) 0.0282(9) Uani 1 1 d . . . H18A H 0.9401 0.7807 0.7523 0.034 Uiso 1 1 calc R . . C19 C 0.8908(3) 0.6117(4) 0.6483(2) 0.0304(9) Uani 1 1 d . . . C20 C 1.1227(3) 0.8841(4) 0.8572(2) 0.0291(9) Uani 1 1 d . . . N1 N 0.0397(3) 0.2081(3) 0.46600(18) 0.0298(8) Uani 1 1 d . . . N2 N 0.0285(3) 0.3661(3) 0.54144(18) 0.0346(8) Uani 1 1 d . . . H2A H -0.0123 0.4184 0.5560 0.042 Uiso 1 1 calc R . . H2B H 0.1051 0.3619 0.5622 0.042 Uiso 1 1 calc R . . N3 N -0.1480(3) 0.3026(3) 0.45622(17) 0.0303(8) Uani 1 1 d . . . N4 N 0.4325(3) 0.2193(3) 0.51873(18) 0.0312(8) Uani 1 1 d . . . N5 N 0.4422(3) 0.3841(3) 0.44972(18) 0.0365(9) Uani 1 1 d . . . H5D H 0.3663 0.3773 0.4270 0.044 Uiso 1 1 calc R . . H5E H 0.4819 0.4406 0.4383 0.044 Uiso 1 1 calc R . . N6 N 0.6183(2) 0.3215(3) 0.53758(17) 0.0293(8) Uani 1 1 d . . . O1 O 0.8963(2) 0.5380(3) 0.60092(15) 0.0407(8) Uani 1 1 d . . . O1W O 0.6877(3) 0.5167(4) 0.7423(2) 0.0848(14) Uani 1 1 d . . . H1WA H 0.7200 0.5586 0.7164 0.102 Uiso 1 1 d R . . H1WB H 0.6199 0.4931 0.7137 0.102 Uiso 1 1 d R . . O2 O 0.7959(2) 0.6593(3) 0.65114(17) 0.0480(9) Uani 1 1 d . . . O2W O 0.8473(5) 0.3543(6) 0.8290(3) 0.156(3) Uani 1 1 d . . . H2WB H 0.7993 0.4050 0.8025 0.187 Uiso 1 1 d R . . H2WA H 0.8062 0.2963 0.8356 0.187 Uiso 1 1 d R . . O3 O 1.2222(2) 0.9023(3) 0.90829(15) 0.0372(7) Uani 1 1 d . . . O4 O 1.0306(2) 0.9422(3) 0.85094(16) 0.0507(9) 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 0.02295(16) 0.0426(3) 0.0485(2) 0.00163(16) 0.01046(13) 0.00048(14) Ag2 0.03096(17) 0.0373(2) 0.04074(19) 0.00701(14) 0.00677(13) -0.00287(14) C1 0.0238(18) 0.032(3) 0.0270(18) 0.0051(17) 0.0081(15) 0.0009(17) C2 0.0293(19) 0.036(3) 0.0302(19) -0.0015(19) 0.0102(16) -0.0080(19) C3 0.038(2) 0.041(3) 0.042(2) -0.016(2) 0.0120(19) -0.011(2) C4 0.035(2) 0.033(3) 0.040(2) -0.007(2) 0.0122(18) -0.0034(19) C5 0.047(3) 0.045(4) 0.074(3) -0.020(3) 0.018(2) 0.004(2) C6 0.029(2) 0.049(3) 0.042(2) -0.011(2) 0.0052(18) -0.009(2) C7 0.0238(18) 0.032(3) 0.0285(19) 0.0021(18) 0.0092(16) 0.0024(17) C8 0.034(2) 0.032(3) 0.035(2) 0.0028(19) 0.0148(17) -0.0004(19) C9 0.034(2) 0.041(3) 0.036(2) 0.013(2) 0.0087(18) 0.011(2) C10 0.029(2) 0.034(3) 0.032(2) 0.0066(18) 0.0108(17) 0.0033(18) C11 0.030(2) 0.056(4) 0.045(2) 0.020(2) 0.0029(19) 0.000(2) C12 0.044(2) 0.034(3) 0.059(3) 0.008(2) 0.014(2) -0.006(2) C13 0.0277(19) 0.033(3) 0.0209(17) -0.0019(16) 0.0048(15) -0.0008(17) C14 0.035(2) 0.026(3) 0.032(2) -0.0047(18) 0.0073(17) 0.0039(18) C15 0.027(2) 0.040(3) 0.035(2) 0.000(2) 0.0061(17) 0.0076(19) C16 0.0244(19) 0.043(3) 0.0284(19) -0.0016(19) 0.0009(16) -0.0011(18) C17 0.0236(18) 0.038(3) 0.0210(17) -0.0020(17) 0.0036(14) 0.0007(17) C18 0.0239(18) 0.030(3) 0.0282(19) 0.0009(18) 0.0051(15) 0.0017(17) C19 0.030(2) 0.032(3) 0.0256(19) -0.0026(18) 0.0038(16) -0.0049(18) C20 0.0243(19) 0.035(3) 0.0244(18) -0.0042(17) 0.0022(16) -0.0030(17) N1 0.0237(15) 0.030(2) 0.0356(17) -0.0006(15) 0.0089(14) 0.0010(15) N2 0.0245(16) 0.041(3) 0.0364(18) -0.0105(17) 0.0069(14) 0.0001(16) N3 0.0243(15) 0.035(2) 0.0315(17) -0.0049(15) 0.0080(13) -0.0022(15) N4 0.0270(16) 0.036(2) 0.0324(17) -0.0004(16) 0.0109(14) 0.0000(15) N5 0.0244(16) 0.041(3) 0.0390(19) 0.0090(17) 0.0024(14) -0.0032(16) N6 0.0226(15) 0.038(2) 0.0260(16) 0.0064(15) 0.0061(13) 0.0023(15) O1 0.0355(15) 0.045(2) 0.0374(16) -0.0157(14) 0.0049(12) -0.0042(14) O1W 0.069(2) 0.110(4) 0.057(2) 0.007(2) -0.0058(19) -0.041(3) O2 0.0225(14) 0.060(3) 0.0535(19) -0.0200(17) 0.0005(13) 0.0033(15) O2W 0.135(5) 0.110(6) 0.167(6) 0.045(4) -0.032(4) -0.053(4) O3 0.0264(14) 0.042(2) 0.0374(15) -0.0149(14) 0.0013(12) -0.0004(13) O4 0.0333(16) 0.059(3) 0.0476(18) -0.0199(17) -0.0055(13) 0.0151(16) _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 2.201(3) . y Ag1 N1 2.205(3) . y Ag2 N6 2.299(3) . y Ag2 O3 2.306(3) 4_575 y Ag2 O1 2.447(3) . y Ag2 N3 2.518(3) 1_655 y C1 N2 1.327(5) . ? C1 N3 1.359(4) . ? C1 N1 1.367(5) . ? C2 N3 1.338(5) . ? C2 C3 1.370(6) . ? C2 C6 1.507(5) . ? C3 C4 1.394(6) . ? C3 H3A 0.9300 . ? C4 N1 1.343(5) . ? C4 C5 1.512(6) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 N5 1.340(5) . ? C7 N4 1.351(5) . ? C7 N6 1.358(4) . ? C8 N4 1.344(5) . ? C8 C9 1.379(5) . ? C8 C12 1.498(6) . ? C9 C10 1.375(6) . ? C9 H9A 0.9300 . ? C10 N6 1.342(5) . ? C10 C11 1.507(5) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.390(6) . ? C13 C14 1.399(5) . ? C13 C19 1.523(5) . ? C14 C15 1.399(5) . ? C14 H14A 0.9300 . ? C15 C16 1.382(6) . ? C15 H15A 0.9300 . ? C16 C17 1.401(5) . ? C16 H16A 0.9300 . ? C17 C18 1.393(5) . ? C17 C20 1.519(6) . ? C18 H18A 0.9300 . ? C19 O1 1.238(5) . ? C19 O2 1.252(5) . ? C20 O4 1.240(5) . ? C20 O3 1.271(4) . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? N3 Ag2 2.518(3) 1_455 ? N5 H5D 0.8600 . ? N5 H5E 0.8600 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WB 0.8500 . ? O2W H2WA 0.8500 . ? O3 Ag2 2.306(3) 4_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ag1 N1 170.86(14) . . y N6 Ag2 O3 143.33(10) . 4_575 y N6 Ag2 O1 113.16(10) . . y O3 Ag2 O1 98.60(11) 4_575 . y N6 Ag2 N3 93.96(12) . 1_655 y O3 Ag2 N3 99.80(11) 4_575 1_655 y O1 Ag2 N3 97.50(10) . 1_655 y N2 C1 N3 117.5(4) . . ? N2 C1 N1 118.9(3) . . ? N3 C1 N1 123.6(4) . . ? N3 C2 C3 121.9(4) . . ? N3 C2 C6 116.4(4) . . ? C3 C2 C6 121.8(4) . . ? C2 C3 C4 118.4(4) . . ? C2 C3 H3A 120.8 . . ? C4 C3 H3A 120.8 . . ? N1 C4 C3 120.8(4) . . ? N1 C4 C5 117.5(4) . . ? C3 C4 C5 121.7(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N5 C7 N4 117.9(3) . . ? N5 C7 N6 117.9(4) . . ? N4 C7 N6 124.3(4) . . ? N4 C8 C9 120.7(4) . . ? N4 C8 C12 118.1(4) . . ? C9 C8 C12 121.2(4) . . ? C10 C9 C8 118.8(4) . . ? C10 C9 H9A 120.6 . . ? C8 C9 H9A 120.6 . . ? N6 C10 C9 121.3(4) . . ? N6 C10 C11 117.4(4) . . ? C9 C10 C11 121.3(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 119.8(4) . . ? C18 C13 C19 120.6(3) . . ? C14 C13 C19 119.5(4) . . ? C13 C14 C15 119.1(4) . . ? C13 C14 H14A 120.5 . . ? C15 C14 H14A 120.5 . . ? C16 C15 C14 120.9(4) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C15 C16 C17 120.2(4) . . ? C15 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C18 C17 C16 118.9(4) . . ? C18 C17 C20 121.2(3) . . ? C16 C17 C20 119.9(3) . . ? C13 C18 C17 121.1(3) . . ? C13 C18 H18A 119.4 . . ? C17 C18 H18A 119.4 . . ? O1 C19 O2 124.8(4) . . ? O1 C19 C13 117.6(3) . . ? O2 C19 C13 117.6(4) . . ? O4 C20 O3 123.3(4) . . ? O4 C20 C17 120.3(3) . . ? O3 C20 C17 116.4(3) . . ? C4 N1 C1 117.6(3) . . ? C4 N1 Ag1 119.0(2) . . ? C1 N1 Ag1 121.7(3) . . ? C1 N2 H2A 120.0 . . ? C1 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C2 N3 C1 117.5(4) . . ? C2 N3 Ag2 119.6(2) . 1_455 ? C1 N3 Ag2 122.8(3) . 1_455 ? C8 N4 C7 117.6(3) . . ? C8 N4 Ag1 118.4(2) . . ? C7 N4 Ag1 122.5(3) . . ? C7 N5 H5D 120.0 . . ? C7 N5 H5E 120.0 . . ? H5D N5 H5E 120.0 . . ? C10 N6 C7 117.0(4) . . ? C10 N6 Ag2 119.5(2) . . ? C7 N6 Ag2 122.8(3) . . ? C19 O1 Ag2 128.3(3) . . ? H1WA O1W H1WB 108.4 . . ? H2WB O2W H2WA 108.4 . . ? C20 O3 Ag2 119.0(2) . 4_676 ? 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 O2 0.85 2.07 2.916(5) 178.8 . O1W H1WB O4 0.85 1.89 2.740(5) 179.1 2_646 O2W H2WB O1W 0.85 1.92 2.768(7) 178.5 . O2W H2WA O2 0.85 2.03 2.881(6) 178.4 2_646 N2 H2A O1 0.86 2.07 2.925(4) 174.8 1_455 N2 H2B O3 0.86 1.98 2.802(4) 160.8 2_646 N5 H5D O2 0.86 2.04 2.878(4) 163.0 3_666 N5 H5E O4 0.86 2.32 3.099(4) 151.5 4_575 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.559 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.095