# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Huang, Rongbin' _publ_contact_author_email rbhuang@xmu.edu.cn _publ_section_title ; pH-Dependent Ag(I) coordination architectures constructed from 4-cyanopyridine and phthalic acid: from discrete structure to 2D sheet ; loop_ _publ_author_name 'Di Sun' 'Zhan-Hua Wei' 'Cheng-Feng Yang' 'Dan-Feng Wang' 'Na Zhang' ; Rongbin Huang ; 'Lansun Zheng' # Attachment '- p1-4.cif' data_p1 _database_code_depnum_ccdc_archive 'CCDC 783312' #TrackingRef '- p1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H13 Ag N4 O4' _chemical_formula_sum 'C20 H13 Ag N4 O4' _chemical_formula_weight 481.21 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' 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 TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6399(13) _cell_length_b 9.959(2) _cell_length_c 14.116(3) _cell_angle_alpha 79.80(3) _cell_angle_beta 87.28(3) _cell_angle_gamma 84.30(3) _cell_volume 913.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8278 _cell_measurement_theta_min 6.17 _cell_measurement_theta_max 55.00 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 1.140 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8754 _exptl_absorpt_correction_T_max 0.9044 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 7858 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3574 _reflns_number_gt 3335 _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^)+(0.0314P)^2^+0.3004P] 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 3574 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.17742(2) 0.393034(16) 0.494146(10) 0.03236(7) Uani 1 1 d . . . C1 C -0.3138(3) 0.3840(2) 0.70771(15) 0.0277(4) Uani 1 1 d . . . H1A H -0.2979 0.2888 0.7051 0.033 Uiso 1 1 calc R . . C2 C -0.3406(3) 0.4227(2) 0.79674(14) 0.0261(4) Uani 1 1 d . . . H2A H -0.3458 0.3563 0.8539 0.031 Uiso 1 1 calc R . . C3 C -0.3596(3) 0.5618(2) 0.80032(13) 0.0223(4) Uani 1 1 d . . . C4 C -0.3582(3) 0.65561(19) 0.71492(14) 0.0236(4) Uani 1 1 d . . . H4B H -0.3739 0.7513 0.7156 0.028 Uiso 1 1 calc R . . C5 C -0.3336(3) 0.6071(2) 0.62892(14) 0.0240(4) Uani 1 1 d . . . H5A H -0.3340 0.6713 0.5705 0.029 Uiso 1 1 calc R . . C6 C -0.3741(3) 0.6091(2) 0.89149(15) 0.0299(4) Uani 1 1 d . . . C7 C -0.1555(3) 0.45470(19) 0.27056(14) 0.0223(4) Uani 1 1 d . . . H7A H -0.1635 0.5459 0.2827 0.027 Uiso 1 1 calc R . . C8 C -0.1404(3) 0.4343(2) 0.17637(14) 0.0241(4) Uani 1 1 d . . . H8A H -0.1386 0.5095 0.1246 0.029 Uiso 1 1 calc R . . C9 C -0.1278(3) 0.3003(2) 0.15916(13) 0.0242(4) Uani 1 1 d . . . C10 C -0.1336(3) 0.19267(19) 0.23652(14) 0.0247(4) Uani 1 1 d . . . H10A H -0.1273 0.1006 0.2263 0.030 Uiso 1 1 calc R . . C11 C -0.1487(3) 0.22278(19) 0.32887(14) 0.0237(4) Uani 1 1 d . . . H11A H -0.1514 0.1495 0.3819 0.028 Uiso 1 1 calc R . . C12 C -0.1086(3) 0.2719(2) 0.06201(15) 0.0347(5) Uani 1 1 d . . . C13 C 0.1744(3) 0.19804(18) 0.60864(13) 0.0204(4) Uani 1 1 d . . . C14 C 0.3042(3) 0.14596(17) 0.69632(13) 0.0207(4) Uani 1 1 d . . . C15 C 0.2222(3) 0.16469(19) 0.78607(14) 0.0270(4) Uani 1 1 d . . . H15A H 0.0918 0.2124 0.7904 0.032 Uiso 1 1 calc R . . C16 C 0.3282(4) 0.1146(2) 0.86935(15) 0.0392(6) Uani 1 1 d . . . H16A H 0.2719 0.1298 0.9301 0.047 Uiso 1 1 calc R . . C17 C 0.5166(4) 0.0424(3) 0.86352(15) 0.0429(6) Uani 1 1 d . . . H17A H 0.5889 0.0071 0.9204 0.051 Uiso 1 1 calc R . . C18 C 0.5992(3) 0.0216(2) 0.77517(15) 0.0310(5) Uani 1 1 d . . . H18A H 0.7277 -0.0287 0.7716 0.037 Uiso 1 1 calc R . . C19 C 0.4950(3) 0.07424(17) 0.69082(13) 0.0203(4) Uani 1 1 d . . . C20 C 0.5991(3) 0.06243(18) 0.59604(13) 0.0193(4) Uani 1 1 d . . . N1 N -0.3090(2) 0.47306(17) 0.62450(11) 0.0243(3) Uani 1 1 d . . . N2 N -0.3822(3) 0.6466(2) 0.96372(15) 0.0462(5) Uani 1 1 d . . . N3 N -0.1595(2) 0.35137(16) 0.34623(11) 0.0202(3) Uani 1 1 d . . . N4 N -0.0907(4) 0.2490(3) -0.01452(15) 0.0543(6) Uani 1 1 d . . . O1 O 0.1163(2) 0.32296(13) 0.59492(10) 0.0293(3) Uani 1 1 d . . . O2 O 0.1261(2) 0.11085(14) 0.56198(10) 0.0275(3) Uani 1 1 d . . . O3 O 0.5775(2) 0.15159(13) 0.52544(9) 0.0256(3) Uani 1 1 d . . . O4 O 0.7203(2) -0.05147(13) 0.59947(9) 0.0238(3) Uani 1 1 d . . . H4A H 0.7790 -0.0562 0.5452 0.029 Uiso 1 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 0.03882(12) 0.04270(11) 0.01786(10) -0.01150(7) -0.00326(6) -0.00271(7) C1 0.0324(11) 0.0221(9) 0.0289(11) -0.0040(8) -0.0026(8) -0.0041(8) C2 0.0316(11) 0.0249(9) 0.0205(9) 0.0020(8) -0.0031(8) -0.0057(8) C3 0.0167(9) 0.0304(10) 0.0209(9) -0.0063(8) -0.0001(7) -0.0045(7) C4 0.0207(10) 0.0214(9) 0.0281(10) -0.0037(8) -0.0004(7) -0.0006(7) C5 0.0210(10) 0.0279(9) 0.0205(9) 0.0014(8) -0.0010(7) 0.0005(7) C6 0.0272(11) 0.0365(11) 0.0274(11) -0.0079(9) -0.0005(8) -0.0063(9) C7 0.0212(10) 0.0208(9) 0.0253(10) -0.0036(8) -0.0043(7) -0.0022(7) C8 0.0229(10) 0.0271(9) 0.0203(9) 0.0022(8) -0.0021(7) -0.0038(8) C9 0.0189(9) 0.0354(10) 0.0198(9) -0.0088(8) -0.0009(7) -0.0020(8) C10 0.0238(10) 0.0226(9) 0.0286(10) -0.0077(8) 0.0015(8) -0.0019(7) C11 0.0252(10) 0.0211(9) 0.0231(9) -0.0005(8) 0.0021(7) -0.0011(7) C12 0.0297(12) 0.0503(13) 0.0251(11) -0.0124(10) -0.0010(8) 0.0019(10) C13 0.0205(9) 0.0239(9) 0.0168(8) -0.0054(7) 0.0019(7) -0.0007(7) C14 0.0303(10) 0.0144(8) 0.0173(9) -0.0025(7) -0.0012(7) -0.0026(7) C15 0.0361(11) 0.0235(9) 0.0203(9) -0.0048(8) 0.0016(8) 0.0035(8) C16 0.0574(15) 0.0415(12) 0.0155(10) -0.0057(9) 0.0018(9) 0.0100(11) C17 0.0608(16) 0.0471(13) 0.0159(10) -0.0017(9) -0.0106(10) 0.0167(12) C18 0.0379(12) 0.0308(10) 0.0223(10) -0.0040(8) -0.0069(8) 0.0090(9) C19 0.0284(10) 0.0155(8) 0.0170(9) -0.0024(7) -0.0018(7) -0.0028(7) C20 0.0196(9) 0.0191(8) 0.0197(9) -0.0031(7) -0.0036(7) -0.0038(7) N1 0.0243(9) 0.0294(8) 0.0195(8) -0.0051(7) -0.0022(6) -0.0011(7) N2 0.0521(13) 0.0615(13) 0.0303(10) -0.0211(10) 0.0020(9) -0.0091(10) N3 0.0190(8) 0.0244(8) 0.0171(7) -0.0040(6) -0.0017(6) -0.0007(6) N4 0.0482(14) 0.0877(18) 0.0292(11) -0.0252(11) -0.0050(9) 0.0112(12) O1 0.0390(9) 0.0219(7) 0.0262(7) -0.0049(6) -0.0101(6) 0.0062(6) O2 0.0302(8) 0.0316(7) 0.0241(7) -0.0121(6) 0.0007(6) -0.0075(6) O3 0.0286(7) 0.0254(7) 0.0189(7) 0.0037(6) 0.0017(5) 0.0014(5) O4 0.0304(8) 0.0216(6) 0.0178(6) -0.0028(5) 0.0010(5) 0.0031(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 N3 2.1954(16) . y Ag1 N1 2.2390(17) . y Ag1 O1 2.4404(16) . y Ag1 Ag1 3.3581(10) 2_566 y C1 N1 1.342(3) . ? C1 C2 1.377(3) . ? C1 H1A 0.9500 . ? C2 C3 1.387(3) . ? C2 H2A 0.9500 . ? C3 C4 1.389(3) . ? C3 C6 1.443(3) . ? C4 C5 1.381(3) . ? C4 H4B 0.9500 . ? C5 N1 1.341(3) . ? C5 H5A 0.9500 . ? C6 N2 1.144(3) . ? C7 N3 1.347(2) . ? C7 C8 1.378(3) . ? C7 H7A 0.9500 . ? C8 C9 1.391(3) . ? C8 H8A 0.9500 . ? C9 C10 1.390(3) . ? C9 C12 1.446(3) . ? C10 C11 1.386(3) . ? C10 H10A 0.9500 . ? C11 N3 1.340(3) . ? C11 H11A 0.9500 . ? C12 N4 1.141(3) . ? C13 O1 1.249(2) . ? C13 O2 1.252(2) . ? C13 C14 1.526(2) . ? C14 C15 1.391(3) . ? C14 C19 1.397(3) . ? C15 C16 1.389(3) . ? C15 H15A 0.9500 . ? C16 C17 1.386(3) . ? C16 H16A 0.9500 . ? C17 C18 1.379(3) . ? C17 H17A 0.9500 . ? C18 C19 1.398(3) . ? C18 H18A 0.9500 . ? C19 C20 1.494(3) . ? C20 O3 1.215(2) . ? C20 O4 1.319(2) . ? O4 H4A 0.8500 . ? 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 N3 Ag1 N1 158.21(6) . . y N3 Ag1 O1 118.66(6) . . y N1 Ag1 O1 83.09(6) . . y N3 Ag1 Ag1 106.18(5) . 2_566 ? N1 Ag1 Ag1 83.42(5) . 2_566 ? O1 Ag1 Ag1 58.49(4) . 2_566 ? N1 C1 C2 123.67(18) . . ? N1 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? C1 C2 C3 117.93(17) . . ? C1 C2 H2A 121.0 . . ? C3 C2 H2A 121.0 . . ? C2 C3 C4 119.25(18) . . ? C2 C3 C6 120.72(18) . . ? C4 C3 C6 119.99(18) . . ? C5 C4 C3 118.68(18) . . ? C5 C4 H4B 120.7 . . ? C3 C4 H4B 120.7 . . ? N1 C5 C4 122.70(17) . . ? N1 C5 H5A 118.6 . . ? C4 C5 H5A 118.6 . . ? N2 C6 C3 178.9(2) . . ? N3 C7 C8 123.07(18) . . ? N3 C7 H7A 118.5 . . ? C8 C7 H7A 118.5 . . ? C7 C8 C9 118.15(17) . . ? C7 C8 H8A 120.9 . . ? C9 C8 H8A 120.9 . . ? C10 C9 C8 119.44(18) . . ? C10 C9 C12 119.69(19) . . ? C8 C9 C12 120.87(19) . . ? C11 C10 C9 118.47(18) . . ? C11 C10 H10A 120.8 . . ? C9 C10 H10A 120.8 . . ? N3 C11 C10 122.54(17) . . ? N3 C11 H11A 118.7 . . ? C10 C11 H11A 118.7 . . ? N4 C12 C9 179.0(2) . . ? O1 C13 O2 126.75(18) . . ? O1 C13 C14 115.85(16) . . ? O2 C13 C14 117.22(16) . . ? C15 C14 C19 119.08(17) . . ? C15 C14 C13 117.79(17) . . ? C19 C14 C13 123.03(17) . . ? C16 C15 C14 120.89(19) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C15 C16 C17 119.8(2) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C18 C17 C16 120.1(2) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C17 C18 C19 120.5(2) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C14 C19 C18 119.72(18) . . ? C14 C19 C20 121.39(16) . . ? C18 C19 C20 118.69(17) . . ? O3 C20 O4 124.78(17) . . ? O3 C20 C19 122.62(16) . . ? O4 C20 C19 112.55(15) . . ? C5 N1 C1 117.73(17) . . ? C5 N1 Ag1 122.64(13) . . ? C1 N1 Ag1 117.38(13) . . ? C11 N3 C7 118.33(17) . . ? C11 N3 Ag1 121.02(13) . . ? C7 N3 Ag1 120.64(13) . . ? C13 O1 Ag1 115.96(13) . . ? C20 O4 H4A 111.3 . . ? 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 O4 H4A O2 0.85 1.76 2.5925(19) 164.1 2_656 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.664 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.086 #==================================================================== data_p2 _database_code_depnum_ccdc_archive 'CCDC 783313' #TrackingRef 'p1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H36 Ag4 N8 O16 ' _chemical_formula_sum 'C56 H36 Ag4 N8 O16' _chemical_formula_weight 1508.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8033(16) _cell_length_b 12.222(2) _cell_length_c 14.569(3) _cell_angle_alpha 108.39(3) _cell_angle_beta 99.67(3) _cell_angle_gamma 95.65(3) _cell_volume 1282.6(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7489 _cell_measurement_theta_min 6.03 _cell_measurement_theta_max 55.05 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.953 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 1.589 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8573 _exptl_absorpt_correction_T_max 0.8834 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 9684 _diffrn_reflns_av_R_equivalents 0.0784 _diffrn_reflns_av_sigmaI/netI 0.0995 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4436 _reflns_number_gt 3085 _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^)+(0.1675P)^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 SHELXL _refine_ls_extinction_coef 0.008(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4436 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1087 _refine_ls_R_factor_gt 0.0885 _refine_ls_wR_factor_ref 0.2584 _refine_ls_wR_factor_gt 0.2239 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.67587(9) 0.58075(6) 0.44692(5) 0.0445(4) Uani 1 1 d . . . Ag2 Ag 0.81350(9) 0.43836(6) 0.55599(5) 0.0458(4) Uani 1 1 d . . . C1 C 0.8113(12) 0.7274(8) 0.3125(7) 0.041(2) Uani 1 1 d . . . H1A H 0.8048 0.7913 0.3687 0.049 Uiso 1 1 calc R . . C2 C 0.8722(12) 0.7508(8) 0.2366(7) 0.041(2) Uani 1 1 d . . . H2A H 0.9054 0.8292 0.2403 0.050 Uiso 1 1 calc R . . C3 C 0.8845(11) 0.6586(8) 0.1545(6) 0.038(2) Uani 1 1 d . . . C4 C 0.8318(12) 0.5450(8) 0.1512(6) 0.041(2) Uani 1 1 d . . . H4A H 0.8370 0.4800 0.0955 0.049 Uiso 1 1 calc R . . C5 C 0.7728(12) 0.5293(8) 0.2294(7) 0.040(2) Uani 1 1 d . . . H5A H 0.7379 0.4516 0.2269 0.047 Uiso 1 1 calc R . . C6 C 0.9467(13) 0.6800(9) 0.0741(7) 0.048(2) Uani 1 1 d . . . C7 C 0.6871(11) 0.2715(8) 0.6819(7) 0.040(2) Uani 1 1 d . . . H7A H 0.6916 0.2094 0.6238 0.047 Uiso 1 1 calc R . . C8 C 0.6242(12) 0.2444(8) 0.7558(7) 0.043(2) Uani 1 1 d . . . H8A H 0.5891 0.1653 0.7496 0.052 Uiso 1 1 calc R . . C9 C 0.6126(11) 0.3346(8) 0.8398(7) 0.040(2) Uani 1 1 d . . . C10 C 0.6679(12) 0.4497(8) 0.8473(7) 0.043(2) Uani 1 1 d . . . H10A H 0.6621 0.5128 0.9043 0.051 Uiso 1 1 calc R . . C11 C 0.7305(12) 0.4698(8) 0.7711(7) 0.042(2) Uani 1 1 d . . . H11A H 0.7670 0.5483 0.7760 0.051 Uiso 1 1 calc R . . C12 C 0.5471(12) 0.3109(8) 0.9193(8) 0.048(2) Uani 1 1 d . . . C13 C 0.6627(11) 0.8787(7) 0.5723(7) 0.039(2) Uani 1 1 d . . . C14 C 0.6816(11) 0.8790(7) 0.6759(6) 0.038(2) Uani 1 1 d . . . C15 C 0.7908(12) 0.9737(7) 0.7522(7) 0.044(2) Uani 1 1 d . . . H15A H 0.8420 1.0382 0.7373 0.053 Uiso 1 1 calc R . . C16 C 0.8246(13) 0.9740(8) 0.8483(7) 0.050(2) Uani 1 1 d . . . H16A H 0.8973 1.0390 0.8994 0.060 Uiso 1 1 calc R . . C17 C 0.7519(13) 0.8787(9) 0.8707(7) 0.051(2) Uani 1 1 d . . . H17A H 0.7724 0.8785 0.9368 0.062 Uiso 1 1 calc R . . C18 C 0.6496(12) 0.7851(8) 0.7944(6) 0.041(2) Uani 1 1 d . . . H18A H 0.6055 0.7185 0.8090 0.049 Uiso 1 1 calc R . . C19 C 0.6078(11) 0.7832(7) 0.6974(6) 0.0360(19) Uani 1 1 d . . . C20 C 0.4866(11) 0.6785(7) 0.6231(6) 0.035(2) Uani 1 1 d . . . C21 C 1.2016(11) 0.9223(7) 0.6120(6) 0.041(2) Uani 1 1 d . . . C22 C 1.2041(11) 0.8975(7) 0.7081(6) 0.037(2) Uani 1 1 d . . . C23 C 1.3041(12) 0.9861(7) 0.7906(6) 0.044(2) Uani 1 1 d . . . H23A H 1.3592 1.0542 0.7822 0.052 Uiso 1 1 calc R . . C24 C 1.3266(12) 0.9788(8) 0.8847(7) 0.047(2) Uani 1 1 d . . . H24A H 1.3965 1.0411 0.9395 0.056 Uiso 1 1 calc R . . C25 C 1.2468(12) 0.8805(8) 0.8986(7) 0.045(2) Uani 1 1 d . . . H25A H 1.2576 0.8751 0.9629 0.054 Uiso 1 1 calc R . . C26 C 1.1507(12) 0.7903(7) 0.8161(7) 0.042(2) Uani 1 1 d . . . H26A H 1.1007 0.7213 0.8251 0.051 Uiso 1 1 calc R . . C27 C 1.1236(11) 0.7951(7) 0.7209(6) 0.0369(19) Uani 1 1 d . . . C28 C 1.0129(11) 0.6870(7) 0.6422(6) 0.0361(19) Uani 1 1 d . . . N1 N 0.7605(10) 0.6189(6) 0.3116(5) 0.0395(17) Uani 1 1 d . . . N2 N 1.0028(12) 0.6948(9) 0.0100(7) 0.061(2) Uani 1 1 d . . . N3 N 0.7428(10) 0.3813(7) 0.6877(5) 0.0390(17) Uani 1 1 d . . . N4 N 0.4929(13) 0.2954(9) 0.9828(7) 0.062(2) Uani 1 1 d . . . O1 O 0.6214(8) 0.7923(5) 0.4990(4) 0.0412(14) Uani 1 1 d . . . O2 O 0.6974(9) 0.9858(5) 0.5687(4) 0.0513(17) Uani 1 1 d . . . H2B H 0.6960 0.9818 0.5099 0.077 Uiso 1 1 calc R . . O3 O 0.5319(8) 0.5811(5) 0.6161(5) 0.0478(16) Uani 1 1 d . . . O4 O 0.3487(8) 0.6959(5) 0.5767(4) 0.0437(15) Uani 1 1 d . . . O5 O 0.9458(7) 0.6913(5) 0.5580(4) 0.0418(14) Uani 1 1 d . . . O6 O 0.9926(8) 0.5971(5) 0.6639(4) 0.0468(16) Uani 1 1 d . . . O7 O 1.0857(9) 0.8598(6) 0.5313(4) 0.0520(18) Uani 1 1 d . . . H7B H 1.0362 0.8006 0.5397 0.078 Uiso 1 1 calc R . . O8 O 1.3017(9) 1.0044(5) 0.6111(4) 0.0504(17) 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 0.0541(6) 0.0299(5) 0.0389(5) 0.0088(3) -0.0025(4) -0.0118(3) Ag2 0.0553(6) 0.0310(5) 0.0375(5) 0.0070(3) -0.0071(4) -0.0105(3) C1 0.043(5) 0.037(5) 0.039(5) 0.015(4) 0.002(4) -0.005(4) C2 0.037(5) 0.037(5) 0.041(5) 0.011(4) -0.006(4) -0.003(4) C3 0.034(4) 0.045(5) 0.033(4) 0.014(4) 0.000(4) -0.001(4) C4 0.043(5) 0.037(5) 0.034(5) 0.007(4) -0.001(4) 0.000(4) C5 0.040(5) 0.026(5) 0.042(5) 0.007(4) -0.008(4) -0.004(4) C6 0.043(5) 0.043(6) 0.045(6) 0.001(5) 0.003(4) 0.000(4) C7 0.035(4) 0.039(5) 0.041(5) 0.017(4) -0.003(4) -0.005(4) C8 0.044(5) 0.028(5) 0.048(5) 0.010(4) -0.002(4) -0.010(4) C9 0.029(4) 0.047(6) 0.043(5) 0.023(5) -0.008(4) -0.003(4) C10 0.042(5) 0.041(5) 0.036(5) 0.008(4) -0.005(4) 0.004(4) C11 0.048(5) 0.031(5) 0.043(5) 0.012(4) 0.000(4) 0.000(4) C12 0.042(5) 0.041(6) 0.052(6) 0.009(5) 0.005(5) -0.002(4) C13 0.039(5) 0.020(4) 0.054(6) 0.010(4) 0.011(4) -0.005(4) C14 0.045(5) 0.021(4) 0.040(5) 0.004(4) 0.004(4) 0.001(4) C15 0.042(5) 0.025(5) 0.053(6) 0.003(4) 0.004(4) -0.009(4) C16 0.050(6) 0.036(6) 0.044(6) -0.005(4) -0.004(5) -0.005(4) C17 0.055(6) 0.039(6) 0.044(5) 0.001(4) -0.002(4) -0.004(4) C18 0.045(5) 0.036(5) 0.034(5) 0.007(4) 0.005(4) -0.004(4) C19 0.033(4) 0.031(5) 0.035(4) 0.007(4) 0.001(4) -0.008(4) C20 0.035(5) 0.025(5) 0.039(5) 0.002(4) 0.011(4) -0.004(4) C21 0.044(5) 0.028(5) 0.046(5) 0.010(4) 0.006(4) -0.007(4) C22 0.043(5) 0.026(4) 0.038(5) 0.009(4) 0.006(4) -0.006(4) C23 0.053(5) 0.025(5) 0.047(5) 0.011(4) 0.006(4) -0.005(4) C24 0.048(5) 0.035(5) 0.045(5) 0.004(4) 0.004(4) -0.010(4) C25 0.044(5) 0.043(5) 0.036(5) 0.005(4) 0.001(4) -0.008(4) C26 0.043(5) 0.024(5) 0.046(5) 0.005(4) -0.004(4) -0.007(4) C27 0.039(5) 0.029(5) 0.042(5) 0.015(4) 0.005(4) 0.000(4) C28 0.036(4) 0.025(5) 0.039(5) 0.003(4) 0.008(4) -0.003(3) N1 0.046(4) 0.038(4) 0.033(4) 0.013(3) 0.003(3) 0.005(3) N2 0.059(6) 0.073(7) 0.049(5) 0.021(5) 0.013(5) -0.001(5) N3 0.041(4) 0.039(5) 0.034(4) 0.016(3) -0.002(3) -0.003(3) N4 0.058(6) 0.079(7) 0.053(6) 0.032(5) 0.009(5) 0.006(5) O1 0.048(3) 0.029(3) 0.038(3) 0.006(3) -0.001(3) -0.002(3) O2 0.075(5) 0.030(3) 0.043(4) 0.008(3) 0.012(3) -0.004(3) O3 0.048(4) 0.030(4) 0.055(4) 0.011(3) -0.007(3) -0.002(3) O4 0.044(4) 0.023(3) 0.049(4) 0.004(3) -0.007(3) -0.003(3) O5 0.042(3) 0.032(3) 0.042(3) 0.011(3) -0.004(3) -0.012(3) O6 0.054(4) 0.025(3) 0.053(4) 0.016(3) -0.007(3) -0.008(3) O7 0.063(4) 0.040(4) 0.041(4) 0.017(3) -0.013(3) -0.020(3) O8 0.065(4) 0.037(4) 0.047(4) 0.017(3) 0.014(3) -0.011(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 O3 2.260(6) 2_666 y Ag1 N1 2.345(7) . y Ag1 O5 2.408(6) . y Ag1 O1 2.555(6) . y Ag1 Ag2 2.8719(13) . y Ag2 O4 2.191(6) 2_666 y Ag2 O6 2.234(6) . y Ag2 N3 2.366(7) . y C1 N1 1.341(11) . ? C1 C2 1.372(13) . ? C1 H1A 0.9500 . ? C2 C3 1.385(13) . ? C2 H2A 0.9500 . ? C3 C4 1.392(12) . ? C3 C6 1.427(13) . ? C4 C5 1.358(12) . ? C4 H4A 0.9500 . ? C5 N1 1.368(12) . ? C5 H5A 0.9500 . ? C6 N2 1.151(13) . ? C7 N3 1.342(11) . ? C7 C8 1.370(13) . ? C7 H7A 0.9500 . ? C8 C9 1.387(13) . ? C8 H8A 0.9500 . ? C9 C10 1.395(13) . ? C9 C12 1.438(13) . ? C10 C11 1.364(13) . ? C10 H10A 0.9500 . ? C11 N3 1.374(12) . ? C11 H11A 0.9500 . ? C12 N4 1.140(13) . ? C13 O1 1.210(10) . ? C13 O2 1.331(10) . ? C13 C14 1.490(12) . ? C14 C19 1.401(11) . ? C14 C15 1.406(12) . ? C15 C16 1.381(12) . ? C15 H15A 0.9500 . ? C16 C17 1.398(13) . ? C16 H16A 0.9500 . ? C17 C18 1.379(13) . ? C17 H17A 0.9500 . ? C18 C19 1.388(12) . ? C18 H18A 0.9500 . ? C19 C20 1.499(11) . ? C20 O4 1.245(10) . ? C20 O3 1.253(10) . ? C21 O8 1.214(9) . ? C21 O7 1.313(10) . ? C21 C22 1.520(12) . ? C22 C23 1.386(12) . ? C22 C27 1.425(11) . ? C23 C24 1.385(12) . ? C23 H23A 0.9500 . ? C24 C25 1.387(13) . ? C24 H24A 0.9500 . ? C25 C26 1.387(12) . ? C25 H25A 0.9500 . ? C26 C27 1.387(12) . ? C26 H26A 0.9500 . ? C27 C28 1.514(12) . ? C28 O6 1.239(10) . ? C28 O5 1.269(10) . ? O2 H2B 0.8400 . ? O3 Ag1 2.260(6) 2_666 ? O4 Ag2 2.191(6) 2_666 ? O7 H7B 0.8400 . ? 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 O3 Ag1 N1 106.5(2) 2_666 . y O3 Ag1 O5 151.5(2) 2_666 . y N1 Ag1 O5 92.4(2) . . y O3 Ag1 O1 126.4(2) 2_666 . y N1 Ag1 O1 84.7(2) . . y O5 Ag1 O1 75.40(19) . . y O3 Ag1 Ag2 78.81(16) 2_666 . ? N1 Ag1 Ag2 129.77(19) . . ? O5 Ag1 Ag2 72.69(14) . . ? O1 Ag1 Ag2 132.95(13) . . ? O4 Ag2 O6 165.5(2) 2_666 . y O4 Ag2 N3 103.9(2) 2_666 . y O6 Ag2 N3 90.4(2) . . y O4 Ag2 Ag1 79.27(16) 2_666 . ? O6 Ag2 Ag1 89.02(15) . . ? N3 Ag2 Ag1 135.59(19) . . ? N1 C1 C2 123.5(9) . . ? N1 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C1 C2 C3 119.1(8) . . ? C1 C2 H2A 120.5 . . ? C3 C2 H2A 120.5 . . ? C2 C3 C4 118.8(8) . . ? C2 C3 C6 120.5(8) . . ? C4 C3 C6 120.8(8) . . ? C5 C4 C3 118.5(8) . . ? C5 C4 H4A 120.8 . . ? C3 C4 H4A 120.8 . . ? C4 C5 N1 123.9(8) . . ? C4 C5 H5A 118.1 . . ? N1 C5 H5A 118.1 . . ? N2 C6 C3 177.0(11) . . ? N3 C7 C8 123.2(9) . . ? N3 C7 H7A 118.4 . . ? C8 C7 H7A 118.4 . . ? C7 C8 C9 118.9(8) . . ? C7 C8 H8A 120.6 . . ? C9 C8 H8A 120.6 . . ? C8 C9 C10 119.1(8) . . ? C8 C9 C12 121.1(8) . . ? C10 C9 C12 119.8(9) . . ? C11 C10 C9 118.7(9) . . ? C11 C10 H10A 120.6 . . ? C9 C10 H10A 120.6 . . ? C10 C11 N3 122.7(8) . . ? C10 C11 H11A 118.7 . . ? N3 C11 H11A 118.7 . . ? N4 C12 C9 177.8(11) . . ? O1 C13 O2 122.8(8) . . ? O1 C13 C14 125.1(7) . . ? O2 C13 C14 112.1(7) . . ? C19 C14 C15 119.7(8) . . ? C19 C14 C13 121.7(7) . . ? C15 C14 C13 118.3(8) . . ? C16 C15 C14 120.8(8) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C15 C16 C17 120.1(9) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C18 C17 C16 118.3(9) . . ? C18 C17 H17A 120.8 . . ? C16 C17 H17A 120.8 . . ? C17 C18 C19 123.3(9) . . ? C17 C18 H18A 118.4 . . ? C19 C18 H18A 118.4 . . ? C18 C19 C14 117.8(8) . . ? C18 C19 C20 117.6(8) . . ? C14 C19 C20 124.6(8) . . ? O4 C20 O3 126.3(8) . . ? O4 C20 C19 117.4(8) . . ? O3 C20 C19 116.3(8) . . ? O8 C21 O7 119.6(8) . . ? O8 C21 C22 119.6(8) . . ? O7 C21 C22 120.6(7) . . ? C23 C22 C27 118.5(8) . . ? C23 C22 C21 113.5(7) . . ? C27 C22 C21 127.9(8) . . ? C24 C23 C22 122.3(8) . . ? C24 C23 H23A 118.8 . . ? C22 C23 H23A 118.8 . . ? C23 C24 C25 119.8(9) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C24 C25 C26 118.1(9) . . ? C24 C25 H25A 120.9 . . ? C26 C25 H25A 120.9 . . ? C25 C26 C27 123.6(8) . . ? C25 C26 H26A 118.2 . . ? C27 C26 H26A 118.2 . . ? C26 C27 C22 117.5(8) . . ? C26 C27 C28 114.6(7) . . ? C22 C27 C28 127.8(8) . . ? O6 C28 O5 122.9(8) . . ? O6 C28 C27 117.3(8) . . ? O5 C28 C27 119.8(7) . . ? C1 N1 C5 116.3(7) . . ? C1 N1 Ag1 122.7(6) . . ? C5 N1 Ag1 120.7(6) . . ? C7 N3 C11 117.4(7) . . ? C7 N3 Ag2 125.4(6) . . ? C11 N3 Ag2 116.3(6) . . ? C13 O1 Ag1 137.4(6) . . ? C13 O2 H2B 109.5 . . ? C20 O3 Ag1 119.0(5) . 2_666 ? C20 O4 Ag2 122.3(5) . 2_666 ? C28 O5 Ag1 128.1(5) . . ? C28 O6 Ag2 119.3(6) . . ? C21 O7 H7B 109.5 . . ? 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 O7 H7B O5 0.84 1.57 2.406(8) 178.7 . O2 H2B O8 0.84 1.83 2.661(8) 171.9 2_776 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 3.207 _refine_diff_density_min -1.983 _refine_diff_density_rms 0.237 #================================================================= data_p3 _database_code_depnum_ccdc_archive 'CCDC 783314' #TrackingRef 'p1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H18 Ag4 N4 O9 ' _chemical_formula_sum 'C28 H18 Ag4 N4 O9' _chemical_formula_weight 985.94 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 Cc 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' _cell_length_a 33.834(7) _cell_length_b 6.0198(12) _cell_length_c 14.566(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.49(3) _cell_angle_gamma 90.00 _cell_volume 2796.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9205 _cell_measurement_theta_min 6.41 _cell_measurement_theta_max 54.95 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 2.824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7654 _exptl_absorpt_correction_T_max 0.8056 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 11489 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4847 _reflns_number_gt 4770 _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^)+(0.0200P)^2^+1.9566P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.738(19) _refine_ls_number_reflns 4847 _refine_ls_number_parameters 407 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0179 _refine_ls_R_factor_gt 0.0173 _refine_ls_wR_factor_ref 0.0424 _refine_ls_wR_factor_gt 0.0408 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 -0.088500(8) 0.78145(5) -0.392302(19) 0.02632(7) Uani 1 1 d . . . Ag2 Ag -0.053804(9) 0.68912(5) -0.17600(2) 0.03151(8) Uani 1 1 d . . . Ag3 Ag -0.019667(8) 0.25903(5) -0.062897(19) 0.02118(7) Uani 1 1 d . . . Ag4 Ag -0.054272(11) 0.35654(4) -0.46496(2) 0.02952(7) Uani 1 1 d . . . C1 C -0.17518(11) 0.5770(5) -0.4283(3) 0.0193(7) Uani 1 1 d . . . H1A H -0.1625 0.4554 -0.4494 0.023 Uiso 1 1 calc R . . C2 C -0.21676(11) 0.5590(6) -0.4341(3) 0.0227(8) Uani 1 1 d . . . H2A H -0.2325 0.4291 -0.4598 0.027 Uiso 1 1 calc R . . C3 C -0.23468(11) 0.7353(6) -0.4016(3) 0.0219(8) Uani 1 1 d . . . C4 C -0.21120(11) 0.9263(6) -0.3652(3) 0.0217(7) Uani 1 1 d . . . H4A H -0.2231 1.0493 -0.3430 0.026 Uiso 1 1 calc R . . C5 C -0.16997(11) 0.9299(6) -0.3629(3) 0.0197(7) Uani 1 1 d . . . H5A H -0.1536 1.0585 -0.3381 0.024 Uiso 1 1 calc R . . C6 C -0.27751(14) 0.7207(7) -0.4030(4) 0.0322(10) Uani 1 1 d . . . C7 C 0.02104(10) 0.1165(5) -0.3965(3) 0.0175(7) Uani 1 1 d . . . C8 C 0.05639(10) -0.0449(5) -0.3519(2) 0.0162(7) Uani 1 1 d . . . C9 C 0.09688(10) -0.0009(6) -0.3533(3) 0.0203(7) Uani 1 1 d . . . H9A H 0.1023 0.1323 -0.3820 0.024 Uiso 1 1 calc R . . C10 C 0.12911(11) -0.1511(6) -0.3128(3) 0.0240(8) Uani 1 1 d . . . H10A H 0.1565 -0.1190 -0.3133 0.029 Uiso 1 1 calc R . . C11 C 0.12173(11) -0.3473(6) -0.2715(3) 0.0232(8) Uani 1 1 d . . . H11A H 0.1438 -0.4512 -0.2458 0.028 Uiso 1 1 calc R . . C12 C 0.08191(11) -0.3922(6) -0.2678(3) 0.0197(7) Uani 1 1 d . . . H12A H 0.0770 -0.5251 -0.2381 0.024 Uiso 1 1 calc R . . C13 C 0.04922(11) -0.2413(5) -0.3077(3) 0.0152(7) Uani 1 1 d . . . C14 C 0.00646(11) -0.2876(5) -0.3022(3) 0.0146(7) Uani 1 1 d . . . C15 C 0.06009(11) 0.1045(6) -0.1014(3) 0.0191(7) Uani 1 1 d . . . H15A H 0.0425 -0.0191 -0.1277 0.023 Uiso 1 1 calc R . . C16 C 0.10155(11) 0.0977(6) -0.0988(3) 0.0212(7) Uani 1 1 d . . . H16A H 0.1122 -0.0264 -0.1235 0.025 Uiso 1 1 calc R . . C17 C 0.12685(12) 0.2789(6) -0.0589(3) 0.0198(8) Uani 1 1 d . . . C18 C 0.11036(11) 0.4593(6) -0.0255(3) 0.0231(8) Uani 1 1 d . . . H18A H 0.1273 0.5845 0.0017 0.028 Uiso 1 1 calc R . . C19 C 0.06830(11) 0.4537(6) -0.0324(3) 0.0212(8) Uani 1 1 d . . . H19A H 0.0566 0.5786 -0.0109 0.025 Uiso 1 1 calc R . . C20 C 0.17058(13) 0.2821(6) -0.0548(3) 0.0278(9) Uani 1 1 d . . . C21 C -0.12741(10) 0.8862(5) -0.0834(3) 0.0161(7) Uani 1 1 d . . . C22 C -0.16398(10) 1.0479(5) -0.1168(3) 0.0153(7) Uani 1 1 d . . . C23 C -0.20369(11) 0.9940(6) -0.1153(3) 0.0194(7) Uani 1 1 d . . . H23A H -0.2082 0.8542 -0.0901 0.023 Uiso 1 1 calc R . . C24 C -0.23692(11) 1.1418(6) -0.1501(3) 0.0233(8) Uani 1 1 d . . . H24A H -0.2640 1.1032 -0.1489 0.028 Uiso 1 1 calc R . . C25 C -0.23031(11) 1.3463(6) -0.1866(3) 0.0231(8) Uani 1 1 d . . . H25A H -0.2529 1.4477 -0.2106 0.028 Uiso 1 1 calc R . . C26 C -0.19062(11) 1.4035(6) -0.1882(3) 0.0183(7) Uani 1 1 d . . . H26A H -0.1863 1.5440 -0.2129 0.022 Uiso 1 1 calc R . . C27 C -0.15743(11) 1.2559(5) -0.1538(3) 0.0141(7) Uani 1 1 d . . . C28 C -0.11439(10) 1.3198(5) -0.1524(3) 0.0148(7) Uani 1 1 d . . . N1 N -0.15205(10) 0.7599(5) -0.3940(3) 0.0181(7) Uani 1 1 d . . . N2 N -0.31092(13) 0.7030(7) -0.4030(4) 0.0507(12) Uani 1 1 d . . . N3 N 0.04393(11) 0.2775(5) -0.0684(3) 0.0186(7) Uani 1 1 d . . . N4 N 0.20444(12) 0.2866(6) -0.0532(4) 0.0448(11) Uani 1 1 d . . . O1 O -0.10900(8) 0.8523(4) -0.1429(2) 0.0260(6) Uani 1 1 d . . . O1W O -0.05214(8) 1.0858(4) -0.2529(2) 0.0268(6) Uani 1 1 d . . . H1WA H -0.0681 1.1845 -0.2423 0.032 Uiso 1 1 d R . . H1WB H -0.0282 1.1345 -0.2505 0.032 Uiso 1 1 d R . . O2 O -0.11896(9) 0.8038(4) 0.0004(2) 0.0290(7) Uani 1 1 d . . . O3 O -0.10992(8) 1.3881(4) -0.23003(19) 0.0204(5) Uani 1 1 d . . . O4 O -0.08530(8) 1.3036(4) -0.0707(2) 0.0195(6) Uani 1 1 d . . . O5 O 0.00506(8) 0.2095(4) -0.3398(2) 0.0244(6) Uani 1 1 d . . . O6 O 0.00937(9) 0.1496(4) -0.4865(2) 0.0273(6) Uani 1 1 d . . . O7 O 0.00381(8) -0.3341(4) -0.22096(18) 0.0176(5) Uani 1 1 d . . . O8 O -0.02363(8) -0.2697(4) -0.3823(2) 0.0162(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01316(14) 0.03642(16) 0.03066(18) -0.00194(13) 0.00903(13) -0.00073(11) Ag2 0.02582(16) 0.02873(15) 0.0506(2) 0.01486(15) 0.02681(15) 0.00644(12) Ag3 0.01288(13) 0.02656(13) 0.02526(16) 0.00159(12) 0.00788(12) 0.00060(10) Ag4 0.02428(13) 0.02083(12) 0.03132(17) 0.00187(12) -0.00687(12) -0.00185(12) C1 0.0200(18) 0.0171(15) 0.0210(19) -0.0015(14) 0.0071(15) 0.0015(13) C2 0.0194(18) 0.0220(17) 0.025(2) 0.0007(14) 0.0058(16) -0.0038(13) C3 0.0093(19) 0.0329(19) 0.021(2) 0.0108(15) 0.0022(17) 0.0026(13) C4 0.0230(19) 0.0272(17) 0.0172(19) 0.0019(14) 0.0097(16) 0.0057(14) C5 0.0201(18) 0.0206(16) 0.0182(19) -0.0005(14) 0.0062(15) -0.0004(13) C6 0.018(2) 0.037(2) 0.042(3) 0.0140(19) 0.009(2) 0.0067(16) C7 0.0170(17) 0.0137(15) 0.023(2) 0.0010(14) 0.0087(16) -0.0039(13) C8 0.0167(17) 0.0197(16) 0.0119(17) -0.0048(13) 0.0041(14) -0.0039(13) C9 0.0168(17) 0.0270(18) 0.0186(19) -0.0012(14) 0.0076(15) -0.0053(14) C10 0.0119(17) 0.040(2) 0.021(2) -0.0007(16) 0.0060(15) -0.0038(14) C11 0.0134(17) 0.0317(19) 0.022(2) 0.0007(16) 0.0034(15) 0.0057(14) C12 0.0176(18) 0.0213(16) 0.0184(19) 0.0018(14) 0.0036(15) 0.0023(13) C13 0.0133(18) 0.0169(16) 0.015(2) -0.0018(12) 0.0039(16) -0.0001(11) C14 0.0145(17) 0.0092(13) 0.022(2) -0.0035(13) 0.0089(15) -0.0002(12) C15 0.0203(18) 0.0211(16) 0.0164(18) -0.0014(13) 0.0066(15) -0.0041(13) C16 0.0227(19) 0.0234(17) 0.0190(19) 0.0021(14) 0.0087(16) 0.0019(14) C17 0.0153(19) 0.0251(17) 0.020(2) 0.0086(14) 0.0076(17) 0.0022(13) C18 0.0199(19) 0.0214(16) 0.024(2) 0.0007(15) 0.0019(16) -0.0035(14) C19 0.0200(19) 0.0223(17) 0.019(2) -0.0010(14) 0.0039(16) -0.0001(13) C20 0.023(2) 0.0278(18) 0.033(3) 0.0109(16) 0.009(2) 0.0032(15) C21 0.0144(16) 0.0118(14) 0.0208(19) 0.0000(13) 0.0042(14) -0.0039(11) C22 0.0132(16) 0.0186(15) 0.0143(18) -0.0015(13) 0.0049(14) -0.0007(12) C23 0.0183(18) 0.0226(16) 0.0180(18) 0.0028(14) 0.0072(15) -0.0052(13) C24 0.0115(17) 0.0346(19) 0.024(2) -0.0011(16) 0.0066(16) -0.0029(14) C25 0.0176(18) 0.0288(18) 0.021(2) 0.0023(15) 0.0040(16) 0.0067(14) C26 0.0175(18) 0.0188(16) 0.0178(18) -0.0002(13) 0.0048(15) 0.0002(13) C27 0.0148(18) 0.0181(16) 0.0089(18) -0.0018(12) 0.0033(15) -0.0014(12) C28 0.0151(17) 0.0121(14) 0.0184(18) 0.0004(13) 0.0073(15) 0.0003(13) N1 0.0137(16) 0.0251(15) 0.0137(17) -0.0012(12) 0.0021(14) -0.0013(11) N2 0.026(2) 0.054(2) 0.077(4) 0.027(2) 0.023(2) 0.0120(18) N3 0.0188(17) 0.0191(15) 0.0207(19) 0.0008(12) 0.0105(15) -0.0008(11) N4 0.020(2) 0.045(2) 0.071(3) 0.021(2) 0.018(2) 0.0039(15) O1 0.0274(15) 0.0265(13) 0.0286(16) 0.0020(11) 0.0154(13) 0.0101(11) O1W 0.0239(13) 0.0254(12) 0.0373(16) -0.0039(11) 0.0186(12) 0.0001(11) O2 0.0293(16) 0.0278(14) 0.0289(17) 0.0097(12) 0.0084(14) 0.0064(11) O3 0.0233(13) 0.0202(11) 0.0204(14) 0.0028(10) 0.0111(11) 0.0008(9) O4 0.0127(14) 0.0260(12) 0.0183(15) -0.0004(12) 0.0033(12) -0.0007(10) O5 0.0257(14) 0.0215(12) 0.0302(15) -0.0030(11) 0.0149(13) 0.0021(10) O6 0.0251(14) 0.0258(14) 0.0302(17) 0.0081(12) 0.0082(13) 0.0056(11) O7 0.0172(12) 0.0223(12) 0.0152(13) 0.0029(10) 0.0078(11) 0.0005(9) O8 0.0098(12) 0.0224(12) 0.0164(14) 0.0017(9) 0.0043(11) -0.0003(9) _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 2.146(3) . y Ag1 O8 2.173(3) 1_565 y Ag1 Ag2 3.0242(10) . y Ag1 Ag4 3.1340(6) . y Ag2 O7 2.258(2) 1_565 y Ag2 O1 2.299(3) . y Ag2 O3 2.552(2) 1_545 y Ag2 Ag3 3.0792(7) . y Ag2 Ag4 3.0914(8) 2_565 y Ag3 N3 2.183(3) . y Ag3 O4 2.202(3) 1_545 y Ag3 Ag4 3.1426(6) 2_565 y Ag4 O2 2.289(3) 2_564 y Ag4 O5 2.386(3) . y Ag4 O4 2.565(3) 2_574 y Ag4 O6 2.596(3) . y Ag4 O8 2.599(3) 1_565 y Ag4 Ag2 3.0914(8) 2_564 y Ag4 Ag3 3.1426(6) 2_564 y C1 N1 1.346(4) . ? C1 C2 1.385(5) . ? C1 H1A 0.9500 . ? C2 C3 1.382(5) . ? C2 H2A 0.9500 . ? C3 C4 1.397(5) . ? C3 C6 1.445(5) . ? C4 C5 1.384(5) . ? C4 H4A 0.9500 . ? C5 N1 1.343(5) . ? C5 H5A 0.9500 . ? C6 N2 1.135(6) . ? C7 O6 1.253(5) . ? C7 O5 1.258(4) . ? C7 C8 1.509(5) . ? C8 C9 1.402(4) . ? C8 C13 1.406(5) . ? C9 C10 1.387(5) . ? C9 H9A 0.9500 . ? C10 C11 1.385(5) . ? C10 H10A 0.9500 . ? C11 C12 1.393(5) . ? C11 H11A 0.9500 . ? C12 C13 1.399(5) . ? C12 H12A 0.9500 . ? C13 C14 1.501(5) . ? C14 O7 1.248(4) . ? C14 O8 1.271(5) . ? C15 N3 1.338(5) . ? C15 C16 1.391(5) . ? C15 H15A 0.9500 . ? C16 C17 1.389(5) . ? C16 H16A 0.9500 . ? C17 C18 1.382(5) . ? C17 C20 1.461(5) . ? C18 C19 1.393(5) . ? C18 H18A 0.9500 . ? C19 N3 1.339(5) . ? C19 H19A 0.9500 . ? C20 N4 1.138(6) . ? C21 O1 1.240(4) . ? C21 O2 1.259(4) . ? C21 C22 1.521(4) . ? C22 C23 1.389(4) . ? C22 C27 1.409(5) . ? C23 C24 1.390(5) . ? C23 H23A 0.9500 . ? C24 C25 1.388(5) . ? C24 H24A 0.9500 . ? C25 C26 1.394(5) . ? C25 H25A 0.9500 . ? C26 C27 1.388(5) . ? C26 H26A 0.9500 . ? C27 C28 1.500(5) . ? C28 O3 1.258(4) . ? C28 O4 1.270(5) . ? O1W H1WA 0.8499 . ? O1W H1WB 0.8501 . ? O2 Ag4 2.289(3) 2_565 ? O3 Ag2 2.552(2) 1_565 ? O4 Ag3 2.202(3) 1_565 ? O4 Ag4 2.565(3) 2_575 ? O7 Ag2 2.258(2) 1_545 ? O8 Ag1 2.173(3) 1_545 ? O8 Ag4 2.599(3) 1_545 ? 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 O8 168.00(10) . 1_565 y O7 Ag2 O1 158.03(9) 1_565 . y O7 Ag2 O3 119.47(8) 1_565 1_545 y O1 Ag2 O3 78.18(9) . 1_545 y N3 Ag3 O4 168.98(10) . 1_545 y O2 Ag4 O5 120.73(10) 2_564 . y O2 Ag4 O4 91.95(10) 2_564 2_574 y O5 Ag4 O4 145.68(8) . 2_574 y O2 Ag4 O6 122.80(9) 2_564 . y O5 Ag4 O6 52.70(9) . . y O4 Ag4 O6 119.98(9) 2_574 . y O2 Ag4 O8 132.19(10) 2_564 1_565 y O5 Ag4 O8 82.15(9) . 1_565 y O4 Ag4 O8 66.91(7) 2_574 1_565 y O6 Ag4 O8 104.64(9) . 1_565 y N1 C1 C2 122.6(3) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 118.1(3) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? C2 C3 C4 120.2(3) . . ? C2 C3 C6 120.0(3) . . ? C4 C3 C6 119.7(3) . . ? C5 C4 C3 117.6(3) . . ? C5 C4 H4A 121.2 . . ? C3 C4 H4A 121.2 . . ? N1 C5 C4 123.0(3) . . ? N1 C5 H5A 118.5 . . ? C4 C5 H5A 118.5 . . ? N2 C6 C3 178.0(5) . . ? O6 C7 O5 124.1(3) . . ? O6 C7 C8 118.7(3) . . ? O5 C7 C8 117.2(3) . . ? C9 C8 C13 119.0(3) . . ? C9 C8 C7 120.7(3) . . ? C13 C8 C7 120.4(3) . . ? C10 C9 C8 120.3(3) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C11 C10 C9 120.7(3) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C10 C11 C12 120.0(3) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C13 119.9(3) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C12 C13 C8 120.2(3) . . ? C12 C13 C14 120.0(3) . . ? C8 C13 C14 119.8(3) . . ? O7 C14 O8 126.9(3) . . ? O7 C14 C13 117.8(3) . . ? O8 C14 C13 115.3(3) . . ? N3 C15 C16 122.8(3) . . ? N3 C15 H15A 118.6 . . ? C16 C15 H15A 118.6 . . ? C17 C16 C15 117.6(3) . . ? C17 C16 H16A 121.2 . . ? C15 C16 H16A 121.2 . . ? C18 C17 C16 120.0(3) . . ? C18 C17 C20 119.9(3) . . ? C16 C17 C20 120.1(3) . . ? C17 C18 C19 118.6(3) . . ? C17 C18 H18A 120.7 . . ? C19 C18 H18A 120.7 . . ? N3 C19 C18 121.9(3) . . ? N3 C19 H19A 119.1 . . ? C18 C19 H19A 119.1 . . ? N4 C20 C17 178.8(5) . . ? O1 C21 O2 127.4(3) . . ? O1 C21 C22 115.3(3) . . ? O2 C21 C22 117.3(3) . . ? C23 C22 C27 119.3(3) . . ? C23 C22 C21 122.2(3) . . ? C27 C22 C21 118.4(3) . . ? C22 C23 C24 120.9(3) . . ? C22 C23 H23A 119.6 . . ? C24 C23 H23A 119.6 . . ? C25 C24 C23 119.6(3) . . ? C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C24 C25 C26 120.3(3) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C27 C26 C25 120.2(3) . . ? C27 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C26 C27 C22 119.7(3) . . ? C26 C27 C28 120.3(3) . . ? C22 C27 C28 119.9(3) . . ? O3 C28 O4 125.4(3) . . ? O3 C28 C27 118.6(3) . . ? O4 C28 C27 116.0(3) . . ? C5 N1 C1 118.5(3) . . ? C5 N1 Ag1 120.9(2) . . ? C1 N1 Ag1 120.7(2) . . ? C15 N3 C19 119.1(3) . . ? C15 N3 Ag3 120.0(2) . . ? C19 N3 Ag3 120.8(2) . . ? C21 O1 Ag2 148.1(2) . . ? H1WA O1W H1WB 113.8 . . ? C21 O2 Ag4 105.7(2) . 2_565 ? C28 O3 Ag2 104.8(2) . 1_565 ? C28 O4 Ag3 120.7(2) . 1_565 ? C28 O4 Ag4 122.4(2) . 2_575 ? Ag3 O4 Ag4 82.10(8) 1_565 2_575 ? C7 O5 Ag4 95.8(2) . . ? C7 O6 Ag4 86.2(2) . . ? C14 O7 Ag2 127.1(2) . 1_545 ? C14 O8 Ag1 123.7(2) . 1_545 ? C14 O8 Ag4 115.14(19) . 1_545 ? Ag1 O8 Ag4 81.58(8) 1_545 1_545 ? 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 O3 0.85 1.93 2.771(3) 172.7 . O1W H1WB O5 0.85 2.04 2.746(3) 140.6 1_565 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.452 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.070 #================================================================= data_p4 _database_code_depnum_ccdc_archive 'CCDC 783315' #TrackingRef 'p1-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H16 Ag2 N4 O6, 3(H2 O) ' _chemical_formula_sum 'C20 H22 Ag2 N4 O9' _chemical_formula_weight 678.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.906(2) _cell_length_b 11.060(2) _cell_length_c 11.520(2) _cell_angle_alpha 69.44(3) _cell_angle_beta 70.84(3) _cell_angle_gamma 87.16(3) _cell_volume 1113.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9142 _cell_measurement_theta_min 6.10 _cell_measurement_theta_max 54.92 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.023 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 1.821 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8389 _exptl_absorpt_correction_T_max 0.8680 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 8700 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3896 _reflns_number_gt 3349 _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^)+(0.0628P)^2^+0.7710P] 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 3896 _refine_ls_number_parameters 316 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.004 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 0.44994(4) 0.64015(3) 0.42821(3) 0.02459(14) Uani 1 1 d . . . Ag2 Ag 0.51122(4) 0.16168(3) -0.10790(3) 0.02969(14) Uani 1 1 d . . . C1 C 0.3210(5) 0.3066(4) 0.0696(4) 0.0225(9) Uani 1 1 d . . . H1A H 0.2467 0.2802 0.0465 0.027 Uiso 1 1 calc R . . C2 C 0.2881(5) 0.3811(4) 0.1482(4) 0.0205(9) Uani 1 1 d . . . H2A H 0.1927 0.4044 0.1781 0.025 Uiso 1 1 calc R . . C3 C 0.3941(5) 0.4220(4) 0.1837(4) 0.0178(9) Uani 1 1 d . . . C4 C 0.5308(5) 0.3843(4) 0.1371(4) 0.0176(9) Uani 1 1 d . . . H4A H 0.6067 0.4098 0.1590 0.021 Uiso 1 1 calc R . . C5 C 0.5566(5) 0.3094(4) 0.0587(4) 0.0203(9) Uani 1 1 d . . . H5A H 0.6514 0.2852 0.0279 0.024 Uiso 1 1 calc R . . C6 C 0.3626(5) 0.5029(4) 0.2696(4) 0.0181(9) Uani 1 1 d U . . C7 C 0.6739(5) 0.0097(4) -0.2909(4) 0.0275(10) Uani 1 1 d . . . H7A H 0.7566 0.0383 -0.2804 0.033 Uiso 1 1 calc R . . C8 C 0.6897(5) -0.0697(4) -0.3623(4) 0.0244(10) Uani 1 1 d . . . H8A H 0.7818 -0.0953 -0.4001 0.029 Uiso 1 1 calc R . . C9 C 0.5706(5) -0.1122(4) -0.3792(4) 0.0208(9) Uani 1 1 d . . . C10 C 0.4393(5) -0.0706(4) -0.3240(4) 0.0228(9) Uani 1 1 d . . . H10A H 0.3554 -0.0967 -0.3345 0.027 Uiso 1 1 calc R . . C11 C 0.4315(5) 0.0098(4) -0.2531(4) 0.0246(10) Uani 1 1 d . . . H11A H 0.3406 0.0380 -0.2163 0.030 Uiso 1 1 calc R . . C12 C 0.5796(5) -0.2012(4) -0.4555(4) 0.0207(9) Uani 1 1 d . . . C13 C 0.0819(4) 0.7398(4) 0.5358(4) 0.0197(9) Uani 1 1 d . . . C14 C 0.0775(4) 0.7529(4) 0.6641(4) 0.0183(9) Uani 1 1 d . . . C15 C 0.0524(5) 0.8739(4) 0.6779(4) 0.0223(9) Uani 1 1 d . . . H15A H 0.0345 0.9436 0.6091 0.027 Uiso 1 1 calc R . . C16 C 0.0532(5) 0.8934(4) 0.7894(4) 0.0261(10) Uani 1 1 d . . . H16A H 0.0370 0.9763 0.7966 0.031 Uiso 1 1 calc R . . C17 C 0.0774(5) 0.7927(4) 0.8906(4) 0.0269(10) Uani 1 1 d . . . H17A H 0.0774 0.8057 0.9678 0.032 Uiso 1 1 calc R . . C18 C 0.1018(5) 0.6717(4) 0.8788(4) 0.0228(9) Uani 1 1 d . . . H18A H 0.1184 0.6024 0.9486 0.027 Uiso 1 1 calc R . . C19 C 0.1023(4) 0.6507(4) 0.7660(4) 0.0181(8) Uani 1 1 d . . . C20 C 0.1178(5) 0.5138(4) 0.7678(4) 0.0228(9) Uani 1 1 d . . . N1 N 0.4550(4) 0.2693(3) 0.0238(3) 0.0194(8) Uani 1 1 d . . . N2 N 0.5434(4) 0.0493(3) -0.2338(3) 0.0210(8) Uani 1 1 d . . . N3 N 0.2296(4) 0.5338(4) 0.3124(4) 0.0283(9) Uani 1 1 d . . . H3A H 0.2080 0.5800 0.3637 0.034 Uiso 1 1 calc R . . H3B H 0.1625 0.5081 0.2897 0.034 Uiso 1 1 calc R . . N4 N 0.7086(4) -0.2287(4) -0.5172(4) 0.0295(9) Uani 1 1 d . . . H4B H 0.7179 -0.2790 -0.5637 0.035 Uiso 1 1 calc R . . H4C H 0.7850 -0.1968 -0.5119 0.035 Uiso 1 1 calc R . . O1W O -0.0124(3) 0.2164(3) 0.7552(3) 0.0272(7) Uani 1 1 d . . . H1WA H -0.0108 0.2940 0.7529 0.033 Uiso 1 1 d R . . H1WB H 0.0036 0.2041 0.6832 0.033 Uiso 1 1 d R . . O1 O 0.4639(4) 0.5397(3) 0.3018(4) 0.0378(8) Uani 1 1 d U . . O2W O 0.7527(4) 0.0629(3) -0.0510(3) 0.0394(8) Uani 1 1 d . . . H2WB H 0.7486 -0.0118 0.0063 0.047 Uiso 1 1 d R . . H2WA H 0.8346 0.1038 -0.0926 0.047 Uiso 1 1 d R . . O2 O 0.4670(4) -0.2474(3) -0.4625(4) 0.0401(9) Uani 1 1 d . . . O3W O 0.2170(4) 0.1945(3) 0.8590(3) 0.0365(8) Uani 1 1 d . . . H3WA H 0.2341 0.2761 0.8313 0.044 Uiso 1 1 d R . . H3WB H 0.1369 0.1802 0.8522 0.044 Uiso 1 1 d R . . O3 O 0.0136(3) 0.4588(3) 0.7613(3) 0.0294(7) Uani 1 1 d . . . O4 O 0.2275(4) 0.4604(3) 0.7865(4) 0.0344(8) Uani 1 1 d . . . O5 O 0.1713(4) 0.6697(3) 0.4928(3) 0.0320(8) Uani 1 1 d . . . O6 O -0.0034(3) 0.8031(3) 0.4806(3) 0.0272(7) 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 0.0349(2) 0.0248(2) 0.0263(2) -0.01742(15) -0.01705(16) 0.00475(15) Ag2 0.0364(3) 0.0330(2) 0.0293(2) -0.02455(17) -0.00832(17) 0.00037(16) C1 0.024(2) 0.026(2) 0.020(2) -0.0100(17) -0.0093(18) -0.0026(18) C2 0.022(2) 0.023(2) 0.021(2) -0.0108(16) -0.0097(17) 0.0020(17) C3 0.023(2) 0.016(2) 0.015(2) -0.0046(15) -0.0080(17) 0.0024(16) C4 0.019(2) 0.020(2) 0.016(2) -0.0065(16) -0.0088(17) 0.0016(16) C5 0.024(2) 0.022(2) 0.017(2) -0.0075(16) -0.0092(18) 0.0064(17) C6 0.025(2) 0.019(2) 0.013(2) -0.0064(15) -0.0086(17) 0.0002(16) C7 0.041(3) 0.025(2) 0.020(2) -0.0117(18) -0.008(2) -0.002(2) C8 0.022(2) 0.033(2) 0.022(2) -0.0131(18) -0.0082(18) 0.0030(18) C9 0.024(2) 0.021(2) 0.015(2) -0.0020(16) -0.0090(17) 0.0023(17) C10 0.024(2) 0.022(2) 0.024(2) -0.0065(17) -0.0127(18) 0.0028(18) C11 0.027(3) 0.028(2) 0.023(2) -0.0155(18) -0.0075(19) 0.0107(18) C12 0.023(2) 0.022(2) 0.017(2) -0.0049(16) -0.0083(18) 0.0011(17) C13 0.017(2) 0.023(2) 0.021(2) -0.0106(17) -0.0053(17) -0.0019(17) C14 0.017(2) 0.022(2) 0.019(2) -0.0109(16) -0.0049(16) -0.0016(16) C15 0.019(2) 0.025(2) 0.023(2) -0.0104(17) -0.0053(17) 0.0019(17) C16 0.024(2) 0.025(2) 0.037(3) -0.0213(19) -0.008(2) 0.0010(18) C17 0.023(2) 0.040(3) 0.026(2) -0.021(2) -0.0075(19) -0.0004(19) C18 0.021(2) 0.032(2) 0.018(2) -0.0092(17) -0.0091(17) -0.0003(18) C19 0.014(2) 0.021(2) 0.023(2) -0.0101(16) -0.0079(16) 0.0024(16) C20 0.023(2) 0.026(2) 0.024(2) -0.0111(17) -0.0104(18) 0.0031(18) N1 0.029(2) 0.0171(17) 0.0158(18) -0.0093(13) -0.0080(15) 0.0010(14) N2 0.032(2) 0.0175(18) 0.0155(18) -0.0085(14) -0.0083(16) 0.0025(15) N3 0.023(2) 0.042(2) 0.042(2) -0.0341(19) -0.0197(18) 0.0118(17) N4 0.027(2) 0.039(2) 0.037(2) -0.0294(18) -0.0117(18) 0.0019(17) O1W 0.040(2) 0.0212(15) 0.0254(17) -0.0118(12) -0.0131(14) 0.0034(13) O1 0.040(2) 0.042(2) 0.040(2) -0.0223(16) -0.0161(17) 0.0033(16) O2W 0.030(2) 0.056(2) 0.0318(19) -0.0140(16) -0.0101(15) -0.0025(16) O2 0.052(2) 0.038(2) 0.039(2) -0.0200(16) -0.0192(18) 0.0016(17) O3W 0.038(2) 0.0348(18) 0.047(2) -0.0190(15) -0.0232(17) 0.0143(15) O3 0.0261(18) 0.0259(16) 0.048(2) -0.0185(14) -0.0218(15) 0.0062(13) O4 0.0234(18) 0.0303(17) 0.060(2) -0.0212(16) -0.0233(17) 0.0096(14) O5 0.0320(19) 0.046(2) 0.0318(18) -0.0276(16) -0.0153(15) 0.0139(15) O6 0.0283(18) 0.0372(17) 0.0233(16) -0.0147(13) -0.0140(14) 0.0076(14) _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 2.089(4) . y Ag1 O2 2.103(4) 1_566 y Ag1 Ag1 3.2406(12) 2_666 y Ag2 N1 2.163(3) . y Ag2 N2 2.162(4) . y C1 N1 1.360(6) . ? C1 C2 1.381(6) . ? C1 H1A 0.9500 . ? C2 C3 1.391(6) . ? C2 H2A 0.9500 . ? C3 C4 1.385(7) . ? C3 C6 1.506(6) . ? C4 C5 1.386(6) . ? C4 H4A 0.9500 . ? C5 N1 1.344(6) . ? C5 H5A 0.9500 . ? C6 O1 1.304(5) . ? C6 N3 1.321(6) . ? C7 N2 1.373(6) . ? C7 C8 1.372(6) . ? C7 H7A 0.9500 . ? C8 C9 1.386(6) . ? C8 H8A 0.9500 . ? C9 C10 1.383(7) . ? C9 C12 1.516(6) . ? C10 C11 1.387(6) . ? C10 H10A 0.9500 . ? C11 N2 1.321(6) . ? C11 H11A 0.9500 . ? C12 O2 1.287(6) . ? C12 N4 1.322(6) . ? C13 O5 1.243(5) . ? C13 O6 1.260(5) . ? C13 C14 1.522(6) . ? C14 C19 1.394(6) . ? C14 C15 1.403(6) . ? C15 C16 1.378(6) . ? C15 H15A 0.9500 . ? C16 C17 1.379(7) . ? C16 H16A 0.9500 . ? C17 C18 1.393(6) . ? C17 H17A 0.9500 . ? C18 C19 1.397(6) . ? C18 H18A 0.9500 . ? C19 C20 1.508(6) . ? C20 O3 1.259(5) . ? C20 O4 1.256(6) . ? N3 H3A 0.8800 . ? N3 H3B 0.8800 . ? N4 H4B 0.8800 . ? N4 H4C 0.8800 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8501 . ? O2W H2WB 0.8500 . ? O2W H2WA 0.8500 . ? O2 Ag1 2.103(3) 1_544 ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? 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 O2 171.48(15) . 1_566 y O1 Ag1 Ag1 76.00(10) . 2_666 ? O2 Ag1 Ag1 104.60(10) 1_566 2_666 ? N1 Ag2 N2 173.94(14) . . y N1 C1 C2 123.0(4) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C1 C2 C3 120.2(4) . . ? C1 C2 H2A 119.9 . . ? C3 C2 H2A 119.9 . . ? C2 C3 C4 117.0(4) . . ? C2 C3 C6 121.9(4) . . ? C4 C3 C6 121.1(4) . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? N1 C5 C4 123.6(4) . . ? N1 C5 H5A 118.2 . . ? C4 C5 H5A 118.2 . . ? O1 C6 N3 121.2(4) . . ? O1 C6 C3 120.7(4) . . ? N3 C6 C3 118.1(4) . . ? N2 C7 C8 122.6(4) . . ? N2 C7 H7A 118.7 . . ? C8 C7 H7A 118.7 . . ? C7 C8 C9 119.6(4) . . ? C7 C8 H8A 120.2 . . ? C9 C8 H8A 120.2 . . ? C10 C9 C8 118.0(4) . . ? C10 C9 C12 119.4(4) . . ? C8 C9 C12 122.6(4) . . ? C9 C10 C11 119.1(4) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? N2 C11 C10 123.8(4) . . ? N2 C11 H11A 118.1 . . ? C10 C11 H11A 118.1 . . ? O2 C12 N4 120.5(4) . . ? O2 C12 C9 122.0(4) . . ? N4 C12 C9 117.5(4) . . ? O5 C13 O6 125.5(4) . . ? O5 C13 C14 117.2(4) . . ? O6 C13 C14 117.3(4) . . ? C19 C14 C15 119.1(4) . . ? C19 C14 C13 122.5(4) . . ? C15 C14 C13 118.3(4) . . ? C16 C15 C14 121.1(4) . . ? C16 C15 H15A 119.4 . . ? C14 C15 H15A 119.4 . . ? C15 C16 C17 120.0(4) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C16 C17 C18 119.6(4) . . ? C16 C17 H17A 120.2 . . ? C18 C17 H17A 120.2 . . ? C17 C18 C19 121.0(4) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C14 C19 C18 119.1(4) . . ? C14 C19 C20 124.0(4) . . ? C18 C19 C20 116.7(4) . . ? O3 C20 O4 125.2(4) . . ? O3 C20 C19 116.9(4) . . ? O4 C20 C19 117.7(4) . . ? C5 N1 C1 116.3(4) . . ? C5 N1 Ag2 120.1(3) . . ? C1 N1 Ag2 123.5(3) . . ? C11 N2 C7 116.9(4) . . ? C11 N2 Ag2 119.3(3) . . ? C7 N2 Ag2 123.7(3) . . ? C6 N3 H3A 120.0 . . ? C6 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C12 N4 H4B 120.0 . . ? C12 N4 H4C 120.0 . . ? H4B N4 H4C 120.0 . . ? H1WA O1W H1WB 118.0 . . ? C6 O1 Ag1 129.2(3) . . ? H2WB O2W H2WA 117.3 . . ? C12 O2 Ag1 129.6(3) . 1_544 ? H3WA O3W H3WB 107.6 . . ? 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 N3 H3A O5 0.88 1.99 2.869(5) 173.1 . N4 H4C O6 0.88 2.07 2.884(5) 153.4 1_644 O1W H1WA O3 0.85 1.89 2.734(4) 171.1 . O1W H1WB O6 0.85 1.92 2.754(4) 167.5 2_566 O2W H2WB O3W 0.85 2.16 3.003(5) 168.8 2_656 O2W H2WA O1W 0.85 1.96 2.757(5) 156.4 1_654 O3W H3WB O1W 0.85 2.07 2.859(5) 153.1 . O3W H3WA O4 0.85 1.92 2.757(4) 167.2 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.992 _refine_diff_density_min -1.249 _refine_diff_density_rms 0.133