# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Geng-Geng Luo' _publ_contact_author_email ggluo@hqu.edu.cn loop_ _publ_author_name 'Geng-Geng Luo' 'Dong-Liang Wu' 'Ji-Huai Wu' 'Jiu-Xu Xia' 'Li Liu' 'Jing-Cao Dai' data_837533 _database_code_depnum_ccdc_archive 'CCDC 837533' #TrackingRef '- 837533-837534.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H24 Ag N2 O6' _chemical_formula_weight 436.23 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.134(2) _cell_length_b 16.751(3) _cell_length_c 9.859(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.73(3) _cell_angle_gamma 90.00 _cell_volume 1760.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 1.177 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8432 _exptl_absorpt_correction_T_max 0.9015 _exptl_absorpt_process_details ABSCOR _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11422 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3052 _reflns_number_gt 2613 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.9261P] 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 3052 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0941 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.004 _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 0.07534(2) 0.240163(17) 0.93479(3) 0.03303(13) Uani 1 1 d . . . C1 C 0.2964(3) 0.00227(17) 0.1763(3) 0.0236(7) Uani 1 1 d . . . C2 C 0.3452(3) 0.0166(2) 0.0496(3) 0.0298(7) Uani 1 1 d . . . H2A H 0.2905 -0.0127 -0.0323 0.036 Uiso 1 1 calc R . . H2B H 0.3364 0.0742 0.0263 0.036 Uiso 1 1 calc R . . C3 C 0.4792(3) -0.0071(2) 0.0651(3) 0.0313(7) Uani 1 1 d . . . H3A H 0.5349 0.0232 0.1449 0.038 Uiso 1 1 calc R . . H3B H 0.4893 -0.0645 0.0895 0.038 Uiso 1 1 calc R . . C4 C 0.8988(3) 0.1804(2) 0.5836(3) 0.0298(7) Uani 1 1 d . . . H4A H 0.9324 0.1329 0.5564 0.036 Uiso 1 1 calc R . . C5 C 0.8088(3) 0.17313(19) 0.6527(3) 0.0287(7) Uani 1 1 d . . . H5A H 0.7811 0.1217 0.6713 0.034 Uiso 1 1 calc R . . C6 C 0.7576(3) 0.24135(19) 0.6959(4) 0.0261(7) Uani 1 1 d . . . C7 C 0.8044(3) 0.31464(19) 0.6665(4) 0.0319(8) Uani 1 1 d . . . H7A H 0.7739 0.3630 0.6946 0.038 Uiso 1 1 calc R . . C8 C 0.8944(3) 0.3164(2) 0.5972(4) 0.0333(8) Uani 1 1 d . . . H8A H 0.9254 0.3670 0.5795 0.040 Uiso 1 1 calc R . . C9 C 0.6528(3) 0.2366(2) 0.7619(4) 0.0303(8) Uani 1 1 d . . . H9A H 0.6549 0.2840 0.8226 0.036 Uiso 1 1 calc R . . H9B H 0.6631 0.1885 0.8224 0.036 Uiso 1 1 calc R . . C10 C 0.5258(3) 0.2330(2) 0.6465(4) 0.0280(7) Uani 1 1 d . . . H10A H 0.5196 0.2787 0.5811 0.034 Uiso 1 1 calc R . . H10B H 0.5219 0.1833 0.5909 0.034 Uiso 1 1 calc R . . C11 C 0.4170(3) 0.23506(18) 0.7060(3) 0.0236(7) Uani 1 1 d . . . C12 C 0.3885(3) 0.30465(18) 0.7710(3) 0.0262(7) Uani 1 1 d . . . H12A H 0.4373 0.3516 0.7747 0.031 Uiso 1 1 calc R . . C13 C 0.2901(3) 0.30445(18) 0.8289(3) 0.0267(7) Uani 1 1 d . . . H13A H 0.2720 0.3523 0.8710 0.032 Uiso 1 1 calc R . . C14 C 0.2440(3) 0.17392(18) 0.7658(3) 0.0258(7) Uani 1 1 d . . . H14A H 0.1933 0.1280 0.7632 0.031 Uiso 1 1 calc R . . C15 C 0.3407(3) 0.16950(17) 0.7050(3) 0.0239(7) Uani 1 1 d . . . H15A H 0.3553 0.1211 0.6619 0.029 Uiso 1 1 calc R . . N1 N 0.9421(3) 0.25055(14) 0.5522(3) 0.0249(6) Uani 1 1 d . . . N2 N 0.2182(3) 0.24031(14) 0.8289(3) 0.0236(6) Uani 1 1 d . . . O1 O 0.1797(2) 0.01046(14) 0.1579(2) 0.0322(5) Uani 1 1 d . . . O1W O 0.0468(2) 0.08164(14) 0.9042(2) 0.0349(6) Uani 1 1 d . . . H1WA H -0.0215 0.0619 0.8836 0.042 Uiso 1 1 d R . . H1WB H 0.0848 0.0600 0.9761 0.042 Uiso 1 1 d R . . O2 O 0.3728(2) -0.01521(14) 0.2940(2) 0.0320(5) Uani 1 1 d . . . O2W O 0.1654(2) -0.00583(15) 0.6287(3) 0.0433(6) Uani 1 1 d . . . H2WA H 0.2320 -0.0214 0.6240 0.052 Uiso 1 1 d R . . H2WB H 0.1327 0.0148 0.5539 0.052 Uiso 1 1 d R . . O3W O 0.0663(2) 0.06799(15) 0.3657(3) 0.0420(6) Uani 1 1 d . . . H3WA H 0.0924 0.0494 0.3048 0.050 Uiso 1 1 d R . . H3WB H -0.0010 0.0474 0.3510 0.050 Uiso 1 1 d R . . O4W O 0.6111(2) 0.04484(16) 0.4229(2) 0.0423(6) Uani 1 1 d . . . H4WA H 0.6199 0.0283 0.5013 0.051 Uiso 1 1 d R . . H4WB H 0.5538 0.0140 0.4015 0.051 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 0.01949(18) 0.0570(2) 0.02773(19) 0.00122(10) 0.01492(12) 0.00261(10) C1 0.0225(17) 0.0239(15) 0.0262(16) -0.0014(12) 0.0098(13) -0.0060(12) C2 0.0239(18) 0.0470(19) 0.0204(15) 0.0008(14) 0.0096(13) 0.0018(14) C3 0.0237(18) 0.051(2) 0.0204(16) 0.0050(14) 0.0086(13) 0.0043(14) C4 0.0246(18) 0.0355(18) 0.0317(17) -0.0043(14) 0.0118(14) 0.0023(13) C5 0.0271(18) 0.0326(17) 0.0292(16) 0.0007(13) 0.0124(14) -0.0036(13) C6 0.0163(18) 0.0443(19) 0.0178(16) 0.0019(12) 0.0051(13) -0.0026(12) C7 0.032(2) 0.0280(16) 0.0419(19) -0.0023(14) 0.0210(16) -0.0028(14) C8 0.0306(19) 0.0348(18) 0.0398(19) -0.0025(15) 0.0185(16) -0.0084(14) C9 0.0214(19) 0.0474(19) 0.0243(17) 0.0001(14) 0.0103(14) -0.0015(14) C10 0.0199(18) 0.0435(18) 0.0227(16) -0.0005(13) 0.0096(14) -0.0024(13) C11 0.0173(17) 0.0342(16) 0.0194(16) 0.0032(12) 0.0057(13) 0.0018(12) C12 0.0216(17) 0.0296(16) 0.0300(16) 0.0006(13) 0.0112(14) -0.0001(12) C13 0.0231(17) 0.0299(16) 0.0290(16) -0.0013(13) 0.0107(13) 0.0052(13) C14 0.0209(17) 0.0278(16) 0.0300(16) 0.0021(13) 0.0095(13) -0.0024(12) C15 0.0208(17) 0.0273(15) 0.0257(15) 0.0009(12) 0.0100(13) 0.0014(12) N1 0.0185(15) 0.0342(15) 0.0246(15) -0.0046(10) 0.0104(12) -0.0042(10) N2 0.0183(15) 0.0314(14) 0.0229(14) 0.0023(10) 0.0090(11) 0.0039(10) O1 0.0193(13) 0.0484(14) 0.0324(12) 0.0039(10) 0.0128(10) -0.0033(10) O1W 0.0238(13) 0.0433(13) 0.0392(13) 0.0085(10) 0.0114(10) -0.0008(10) O2 0.0259(13) 0.0510(14) 0.0204(11) 0.0063(10) 0.0088(10) -0.0056(10) O2W 0.0349(15) 0.0582(16) 0.0430(14) -0.0033(12) 0.0212(12) -0.0076(12) O3W 0.0326(15) 0.0544(15) 0.0451(15) -0.0026(12) 0.0211(12) -0.0074(11) O4W 0.0291(14) 0.0718(18) 0.0270(12) 0.0043(11) 0.0097(10) -0.0101(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.133(3) 4_466 ? Ag1 N2 2.139(3) . ? Ag1 O1W 2.681(2) . ? C1 O2 1.260(4) . ? C1 O1 1.268(4) . ? C1 C2 1.517(4) . ? C2 C3 1.508(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C3 1.503(6) 3_655 ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N1 1.341(4) . ? C4 C5 1.369(5) . ? C4 H4A 0.9500 . ? C5 C6 1.397(5) . ? C5 H5A 0.9500 . ? C6 C7 1.396(4) . ? C6 C9 1.493(5) . ? C7 C8 1.366(5) . ? C7 H7A 0.9500 . ? C8 N1 1.354(4) . ? C8 H8A 0.9500 . ? C9 C10 1.540(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.491(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C15 1.386(4) . ? C11 C12 1.409(4) . ? C12 C13 1.373(5) . ? C12 H12A 0.9500 . ? C13 N2 1.340(4) . ? C13 H13A 0.9500 . ? C14 N2 1.345(4) . ? C14 C15 1.377(5) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? N1 Ag1 2.133(3) 4_665 ? O1W H1WA 0.8000 . ? O1W H1WB 0.8000 . ? O2W H2WA 0.8000 . ? O2W H2WB 0.8000 . ? O3W H3WA 0.8000 . ? O3W H3WB 0.8001 . ? O4W H4WA 0.8000 . ? O4W H4WB 0.8000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 174.48(9) 4_466 . ? N1 Ag1 O1W 93.15(8) 4_466 . ? N2 Ag1 O1W 91.54(8) . . ? O2 C1 O1 123.3(3) . . ? O2 C1 C2 119.2(3) . . ? O1 C1 C2 117.4(3) . . ? C3 C2 C1 116.9(3) . . ? C3 C2 H2A 108.1 . . ? C1 C2 H2A 108.1 . . ? C3 C2 H2B 108.1 . . ? C1 C2 H2B 108.1 . . ? H2A C2 H2B 107.3 . . ? C3 C3 C2 114.3(3) 3_655 . ? C3 C3 H3A 108.7 3_655 . ? C2 C3 H3A 108.7 . . ? C3 C3 H3B 108.7 3_655 . ? C2 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? N1 C4 C5 123.8(3) . . ? N1 C4 H4A 118.1 . . ? C5 C4 H4A 118.1 . . ? C4 C5 C6 120.0(3) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C5 C6 C7 116.5(3) . . ? C5 C6 C9 121.9(3) . . ? C7 C6 C9 121.5(3) . . ? C8 C7 C6 119.6(3) . . ? C8 C7 H7A 120.2 . . ? C6 C7 H7A 120.2 . . ? N1 C8 C7 124.0(3) . . ? N1 C8 H8A 118.0 . . ? C7 C8 H8A 118.0 . . ? C6 C9 C10 110.3(3) . . ? C6 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? C6 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 112.7(3) . . ? C11 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? C11 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C15 C11 C12 116.2(3) . . ? C15 C11 C10 122.9(3) . . ? C12 C11 C10 120.8(3) . . ? C13 C12 C11 119.8(3) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? N2 C13 C12 123.4(3) . . ? N2 C13 H13A 118.3 . . ? C12 C13 H13A 118.3 . . ? N2 C14 C15 122.9(3) . . ? N2 C14 H14A 118.5 . . ? C15 C14 H14A 118.5 . . ? C14 C15 C11 120.5(3) . . ? C14 C15 H15A 119.7 . . ? C11 C15 H15A 119.7 . . ? C4 N1 C8 115.9(3) . . ? C4 N1 Ag1 122.8(2) . 4_665 ? C8 N1 Ag1 121.2(2) . 4_665 ? C13 N2 C14 117.1(3) . . ? C13 N2 Ag1 121.9(2) . . ? C14 N2 Ag1 120.8(2) . . ? Ag1 O1W H1WA 120.7 . . ? Ag1 O1W H1WB 109.4 . . ? H1WA O1W H1WB 105.0 . . ? H2WA O2W H2WB 105.7 . . ? H3WA O3W H3WB 102.7 . . ? H4WA O4W H4WB 84.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O1 0.80 2.08 2.868(3) 168.6 3_556 O1W H1WB O1 0.80 1.98 2.781(3) 177.8 1_556 O2W H2WA O4W 0.80 1.97 2.758(4) 167.9 3_656 O2W H2WB O3W 0.80 2.00 2.797(4) 174.9 . O3W H3WA O1 0.80 2.07 2.864(3) 172.7 . O3W H3WB O2W 0.80 2.02 2.798(3) 163.6 3_556 O4W H4WA O2 0.80 2.01 2.790(3) 165.2 3_656 O4W H4WB O2 0.80 2.05 2.779(3) 151.9 . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.477 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.127 data_837534 _database_code_depnum_ccdc_archive 'CCDC 837534' #TrackingRef '- 837533-837534.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H56 Ag2 N4 O14' _chemical_formula_weight 936.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.9962(18) _cell_length_b 25.246(5) _cell_length_c 35.100(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7972(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3856 _exptl_absorpt_coefficient_mu 1.049 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8585 _exptl_absorpt_correction_T_max 0.9208 _exptl_absorpt_process_details ABSCOR _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29708 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6771 _reflns_number_gt 4308 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1162P)^2^+8.3246P] 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 6771 _refine_ls_number_parameters 475 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.2159 _refine_ls_wR_factor_gt 0.1878 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.038 _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 0.23392(6) 0.60430(3) 0.737245(18) 0.0456(2) Uani 1 1 d . . . Ag2 Ag 0.5000 1.0000 0.5000 0.0488(3) Uani 1 2 d S . . Ag3 Ag 0.4893(4) 0.50095(16) 0.49110(6) 0.0537(7) Uani 0.50 1 d P . . C1 C 0.4462(9) 0.7045(3) 0.61586(19) 0.0422(19) Uani 1 1 d . . . C2 C 0.4666(10) 0.7551(4) 0.5923(2) 0.057(2) Uani 1 1 d . . . H2A H 0.5501 0.7497 0.5744 0.068 Uiso 1 1 calc R . . H2B H 0.3757 0.7611 0.5770 0.068 Uiso 1 1 calc R . . C3 C 0.4953(10) 0.8012(4) 0.6144(2) 0.070(3) Uani 1 1 d . . . H3A H 0.4148 0.8046 0.6335 0.084 Uiso 1 1 calc R . . H3B H 0.4884 0.8323 0.5973 0.084 Uiso 1 1 calc R . . C4 C 0.6445(11) 0.8043(4) 0.6356(3) 0.067(3) Uani 1 1 d U . . H4A H 0.6456 0.7751 0.6544 0.080 Uiso 1 1 calc R . . H4B H 0.7234 0.7964 0.6167 0.080 Uiso 1 1 calc R . . C5 C 0.6887(11) 0.8528(4) 0.6557(3) 0.066(3) Uani 1 1 d . . . H5A H 0.7812 0.8457 0.6701 0.079 Uiso 1 1 calc R . . H5B H 0.6104 0.8620 0.6744 0.079 Uiso 1 1 calc R . . C6 C 0.7142(9) 0.8998(3) 0.6296(2) 0.045(2) Uani 1 1 d . . . C21 C 0.3220(9) 0.5897(4) 0.5383(2) 0.054(2) Uani 1 1 d . . . H21A H 0.3742 0.5787 0.5605 0.065 Uiso 1 1 calc R . . C22 C 0.2270(8) 0.6307(3) 0.5418(2) 0.0407(18) Uani 1 1 d . . . H22A H 0.2118 0.6463 0.5661 0.049 Uiso 1 1 calc R . . C23 C 0.1518(7) 0.6503(3) 0.51070(19) 0.040(2) Uani 1 1 d . . . C24 C 0.1815(9) 0.6243(4) 0.4763(2) 0.053(2) Uani 1 1 d . . . H24A H 0.1342 0.6360 0.4536 0.064 Uiso 1 1 calc R . . C25 C 0.2739(10) 0.5841(5) 0.4750(3) 0.068(3) Uani 1 1 d . . . H25A H 0.2908 0.5681 0.4509 0.081 Uiso 1 1 calc R . . C26 C 0.0540(7) 0.6999(3) 0.5130(2) 0.0355(16) Uani 1 1 d . . . H26A H -0.0206 0.6990 0.4923 0.043 Uiso 1 1 calc R . . H26B H 0.0000 0.7001 0.5376 0.043 Uiso 1 1 calc R . . C27 C 0.1451(7) 0.7496(3) 0.50965(19) 0.0382(18) Uani 1 1 d . . . H27A H 0.1946 0.7501 0.4845 0.046 Uiso 1 1 calc R . . H27B H 0.2236 0.7492 0.5294 0.046 Uiso 1 1 calc R . . C28 C 0.0528(7) 0.7998(3) 0.5141(2) 0.0409(19) Uani 1 1 d . . . H28A H -0.0249 0.8007 0.4941 0.049 Uiso 1 1 calc R . . H28B H 0.0027 0.7994 0.5392 0.049 Uiso 1 1 calc R . . C29 C 0.2983(9) 0.9162(3) 0.5389(2) 0.0458(19) Uani 1 1 d . . . H29A H 0.3361 0.9323 0.5614 0.055 Uiso 1 1 calc R . . C30 C 0.2043(8) 0.8740(3) 0.5425(2) 0.0426(19) Uani 1 1 d . . . H30A H 0.1778 0.8619 0.5672 0.051 Uiso 1 1 calc R . . C31 C 0.1473(7) 0.8487(3) 0.51101(19) 0.0361(18) Uani 1 1 d . . . C32 C 0.1869(8) 0.8703(3) 0.4763(2) 0.0394(18) Uani 1 1 d . . . H32A H 0.1470 0.8555 0.4536 0.047 Uiso 1 1 calc R . . C33 C 0.2828(8) 0.9129(3) 0.4737(2) 0.0407(18) Uani 1 1 d . . . H33A H 0.3092 0.9263 0.4493 0.049 Uiso 1 1 calc R . . C41 C 0.4515(8) 0.5183(3) 0.7125(2) 0.0427(19) Uani 1 1 d . . . H41A H 0.4247 0.5312 0.6881 0.051 Uiso 1 1 calc R . . C42 C 0.5488(8) 0.4759(4) 0.7146(2) 0.0454(19) Uani 1 1 d . . . H42A H 0.5871 0.4606 0.6919 0.054 Uiso 1 1 calc R . . C43 C 0.5903(7) 0.4557(3) 0.7500(2) 0.0398(19) Uani 1 1 d . . . C44 C 0.5299(8) 0.4811(3) 0.7819(2) 0.0417(18) Uani 1 1 d . . . H44A H 0.5547 0.4691 0.8068 0.050 Uiso 1 1 calc R . . C45 C 0.4359(8) 0.5230(3) 0.7775(2) 0.0418(19) Uani 1 1 d . . . H45A H 0.3984 0.5395 0.7998 0.050 Uiso 1 1 calc R . . C46 C 0.6885(8) 0.4094(3) 0.7537(2) 0.0412(19) Uani 1 1 d . . . H46A H 0.7396 0.4107 0.7787 0.049 Uiso 1 1 calc R . . H46B H 0.7653 0.4106 0.7335 0.049 Uiso 1 1 calc R . . C47 C 0.5992(7) 0.3564(3) 0.75043(19) 0.0331(17) Uani 1 1 d . . . H47A H 0.5219 0.3555 0.7705 0.040 Uiso 1 1 calc R . . H47B H 0.5485 0.3552 0.7254 0.040 Uiso 1 1 calc R . . C48 C 0.6983(8) 0.3079(3) 0.7544(2) 0.0357(17) Uani 1 1 d . . . H48A H 0.7759 0.3084 0.7345 0.043 Uiso 1 1 calc R . . H48B H 0.7481 0.3084 0.7796 0.043 Uiso 1 1 calc R . . C49 C 0.4580(8) 0.1985(3) 0.7126(2) 0.0426(19) Uani 1 1 d . . . H49A H 0.4195 0.1895 0.6882 0.051 Uiso 1 1 calc R . . C50 C 0.5479(8) 0.2417(3) 0.71563(19) 0.0377(17) Uani 1 1 d . . . H50A H 0.5720 0.2612 0.6933 0.045 Uiso 1 1 calc R . . C51 C 0.6061(7) 0.2584(3) 0.75070(19) 0.0334(17) Uani 1 1 d . . . C52 C 0.5695(7) 0.2263(3) 0.78146(19) 0.0407(19) Uani 1 1 d . . . H52A H 0.6076 0.2343 0.8060 0.049 Uiso 1 1 calc R . . C53 C 0.4766(7) 0.1820(4) 0.7766(2) 0.045(2) Uani 1 1 d . . . H53A H 0.4523 0.1613 0.7983 0.054 Uiso 1 1 calc R . . N1 N 0.3925(6) 0.5424(3) 0.74348(16) 0.0390(15) Uani 1 1 d . . . N2 N 0.4212(6) 0.1678(3) 0.74295(15) 0.0355(14) Uani 1 1 d . . . N3 N 0.3482(7) 0.5633(3) 0.5060(2) 0.0545(19) Uani 1 1 d . . . N4 N 0.3393(6) 0.9357(3) 0.50502(16) 0.0415(16) Uani 1 1 d . . . O1W O 0.2341(5) 0.6014(2) 0.66153(14) 0.0452(13) Uani 1 1 d . . . H1WA H 0.2656 0.6284 0.6528 0.054 Uiso 1 1 d R . . H1WB H 0.1502 0.5977 0.6544 0.054 Uiso 1 1 d R . . O1 O 0.5608(6) 0.6761(3) 0.61847(18) 0.0696(18) Uani 1 1 d . . . O2 O 0.3227(5) 0.6942(2) 0.62969(13) 0.0425(13) Uani 1 1 d . . . O2W O -0.0538(6) 0.5955(3) 0.63489(16) 0.0652(17) Uani 1 1 d . . . H2WA H -0.0334 0.5725 0.6201 0.078 Uiso 1 1 d R . . H2WB H -0.1426 0.5937 0.6349 0.078 Uiso 1 1 d R . . O3 O 0.8445(6) 0.9125(2) 0.62231(15) 0.0531(15) Uani 1 1 d . . . O3W O 0.5091(5) 1.0137(2) 0.58350(14) 0.0524(15) Uani 1 1 d . . . H3WA H 0.5455 0.9876 0.5925 0.063 Uiso 1 1 d R . . H3WB H 0.4238 1.0164 0.5774 0.063 Uiso 1 1 d R . . O4 O 0.5992(5) 0.9242(3) 0.61750(16) 0.0587(16) Uani 1 1 d . . . O4W O 0.2787(5) 0.5113(2) 0.61660(15) 0.0518(15) Uani 1 1 d . . . H4WA H 0.2578 0.5410 0.6107 0.062 Uiso 1 1 d R . . H4WB H 0.2477 0.4847 0.6262 0.062 Uiso 1 1 d R . . O5W O 0.9382(6) 1.0056(3) 0.59217(16) 0.0657(18) Uani 1 1 d . . . H5WA H 1.0230 1.0085 0.5987 0.079 Uiso 1 1 d R . . H5WB H 0.9067 0.9783 0.6005 0.079 Uiso 1 1 d R . . O6W O 0.6359(7) 0.5815(3) 0.64676(19) 0.086(2) Uani 1 1 d . . . H6WA H 0.6147 0.5594 0.6313 0.103 Uiso 1 1 d R . . H6WB H 0.6138 0.6099 0.6384 0.103 Uiso 1 1 d R . . O7W O 0.0753(6) 0.7555(3) 0.61506(18) 0.075(2) Uani 1 1 d . . . H7WA H -0.0090 0.7488 0.6097 0.091 Uiso 1 1 d R . . H7WB H 0.1486 0.7387 0.6195 0.091 Uiso 1 1 d R . . O8W O 0.3162(6) 0.9139(3) 0.64363(15) 0.0634(18) Uani 1 1 d . . . H8WA H 0.2628 0.8886 0.6422 0.076 Uiso 1 1 d R . . H8WB H 0.3942 0.9069 0.6339 0.076 Uiso 1 1 d R . . O9W O -0.1440(6) 0.6851(3) 0.60062(17) 0.0694(18) Uani 1 1 d . . . H9WA H -0.2315 0.6852 0.6047 0.083 Uiso 1 1 d R . . H9WB H -0.0771 0.6664 0.6074 0.083 Uiso 1 1 d R . . O10W O 1.0761(6) 0.8518(2) 0.65139(15) 0.0595(16) Uani 1 1 d . . . H10A H 1.0758 0.8238 0.6407 0.071 Uiso 1 1 d R . . H10B H 1.0097 0.8694 0.6430 0.071 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 0.0370(3) 0.0356(4) 0.0641(4) 0.0032(3) -0.0023(3) 0.0044(2) Ag2 0.0389(5) 0.0366(6) 0.0710(6) 0.0006(4) 0.0030(4) -0.0041(4) Ag3 0.0378(11) 0.0358(9) 0.088(2) 0.0045(18) 0.0066(16) 0.0033(7) C1 0.054(5) 0.036(5) 0.037(4) -0.001(3) -0.005(4) 0.001(4) C2 0.060(5) 0.035(6) 0.074(6) 0.010(4) -0.013(4) -0.011(4) C3 0.085(7) 0.054(8) 0.071(6) 0.020(5) -0.022(5) -0.010(5) C4 0.091(6) 0.035(6) 0.074(5) 0.014(4) -0.029(5) -0.011(4) C5 0.075(6) 0.057(8) 0.064(5) 0.019(5) -0.017(5) -0.027(5) C6 0.053(5) 0.038(6) 0.043(4) -0.009(4) -0.005(4) -0.008(4) C21 0.053(5) 0.054(7) 0.056(5) 0.009(4) 0.005(4) 0.002(4) C22 0.048(4) 0.036(5) 0.038(4) 0.001(3) 0.005(3) 0.006(4) C23 0.024(3) 0.053(6) 0.042(4) 0.007(4) 0.001(3) -0.014(3) C24 0.052(5) 0.059(7) 0.049(5) -0.013(4) -0.003(4) 0.007(4) C25 0.058(6) 0.081(9) 0.064(6) -0.024(6) 0.014(5) -0.005(5) C26 0.033(4) 0.025(5) 0.049(4) 0.005(3) -0.003(3) 0.001(3) C27 0.024(3) 0.052(6) 0.039(4) 0.004(3) -0.003(3) -0.001(3) C28 0.024(3) 0.051(6) 0.048(4) 0.007(4) 0.002(3) -0.001(3) C29 0.060(5) 0.031(5) 0.046(4) -0.005(4) 0.003(4) 0.002(4) C30 0.043(4) 0.041(6) 0.043(4) 0.006(4) 0.004(3) -0.003(4) C31 0.021(3) 0.045(6) 0.043(4) -0.001(3) 0.002(3) 0.011(3) C32 0.035(4) 0.040(5) 0.044(4) -0.003(4) 0.001(3) -0.008(3) C33 0.040(4) 0.040(5) 0.043(4) 0.003(4) -0.001(3) 0.001(3) C41 0.041(4) 0.042(6) 0.045(4) 0.009(4) -0.006(3) 0.005(4) C42 0.044(4) 0.047(6) 0.045(4) -0.001(4) 0.006(3) 0.002(4) C43 0.026(3) 0.046(6) 0.047(4) -0.002(4) 0.000(3) -0.012(3) C44 0.047(4) 0.034(5) 0.045(4) -0.001(3) -0.010(3) 0.006(4) C45 0.041(4) 0.046(6) 0.038(4) -0.004(4) -0.004(3) 0.001(4) C46 0.024(3) 0.044(6) 0.056(4) -0.002(4) -0.002(3) 0.004(3) C47 0.027(3) 0.031(5) 0.041(4) -0.002(3) -0.005(3) -0.005(3) C48 0.032(3) 0.024(5) 0.051(4) -0.006(3) -0.009(3) 0.007(3) C49 0.043(4) 0.045(6) 0.039(4) -0.007(4) -0.008(3) 0.000(4) C50 0.050(4) 0.030(5) 0.033(4) 0.002(3) -0.002(3) -0.007(3) C51 0.026(3) 0.031(5) 0.044(4) 0.000(3) 0.000(3) 0.004(3) C52 0.035(4) 0.051(6) 0.036(4) 0.004(4) -0.005(3) -0.008(4) C53 0.035(4) 0.061(7) 0.040(4) 0.013(4) 0.004(3) -0.002(4) N1 0.034(3) 0.035(4) 0.048(4) -0.003(3) -0.001(3) -0.007(3) N2 0.038(3) 0.030(4) 0.039(3) 0.004(3) 0.004(3) -0.003(3) N3 0.035(3) 0.043(5) 0.086(5) -0.001(4) 0.018(4) -0.005(3) N4 0.035(3) 0.043(5) 0.046(4) -0.007(3) 0.002(3) 0.010(3) O1W 0.043(3) 0.040(4) 0.053(3) -0.001(3) -0.005(2) -0.001(2) O1 0.044(3) 0.049(5) 0.115(5) 0.013(4) 0.014(3) 0.005(3) O2 0.040(3) 0.048(4) 0.040(3) 0.000(2) 0.007(2) 0.001(2) O2W 0.044(3) 0.063(5) 0.089(4) -0.019(3) -0.008(3) 0.009(3) O3 0.049(3) 0.047(4) 0.063(3) 0.012(3) -0.002(3) -0.007(3) O3W 0.043(3) 0.058(5) 0.057(3) 0.003(3) 0.004(2) -0.004(3) O4 0.040(3) 0.056(5) 0.081(4) 0.016(3) -0.001(3) -0.004(3) O4W 0.048(3) 0.042(4) 0.065(4) 0.005(3) -0.001(3) 0.000(3) O5W 0.055(3) 0.063(5) 0.079(4) 0.031(3) -0.018(3) -0.025(3) O6W 0.078(5) 0.063(6) 0.117(5) 0.029(4) 0.033(4) 0.010(4) O7W 0.053(4) 0.069(6) 0.104(5) -0.009(4) -0.019(3) 0.011(3) O8W 0.038(3) 0.085(6) 0.068(4) 0.010(3) 0.002(3) -0.004(3) O9W 0.054(3) 0.058(5) 0.096(4) -0.002(4) 0.005(3) 0.002(3) O10W 0.061(4) 0.037(4) 0.081(4) 0.003(3) -0.005(3) 0.005(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 N1 2.127(7) . ? Ag1 N2 2.134(6) 8_665 ? Ag1 O1W 2.659(5) . ? Ag2 N4 2.180(7) . ? Ag2 N4 2.180(7) 5_676 ? Ag3 Ag3 0.656(3) 5_666 ? Ag3 N3 2.089(8) . ? Ag3 N3 2.186(8) 5_666 ? C1 O2 1.239(9) . ? C1 O1 1.259(9) . ? C1 C2 1.533(11) . ? C2 C3 1.422(13) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.536(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.469(13) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.518(12) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O3 1.242(9) . ? C6 O4 1.277(9) . ? C21 N3 1.335(11) . ? C21 C22 1.349(12) . ? C21 H21A 0.9500 . ? C22 C23 1.376(10) . ? C22 H22A 0.9500 . ? C23 C24 1.399(10) . ? C23 C26 1.533(10) . ? C24 C25 1.313(14) . ? C24 H24A 0.9500 . ? C25 N3 1.382(12) . ? C25 H25A 0.9500 . ? C26 C27 1.503(10) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.524(11) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C31 1.503(11) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 N4 1.340(9) . ? C29 C30 1.365(12) . ? C29 H29A 0.9500 . ? C30 C31 1.376(10) . ? C30 H30A 0.9500 . ? C31 C32 1.381(10) . ? C32 C33 1.382(11) . ? C32 H32A 0.9500 . ? C33 N4 1.341(9) . ? C33 H33A 0.9500 . ? C41 N1 1.353(9) . ? C41 C42 1.384(11) . ? C41 H41A 0.9500 . ? C42 C43 1.394(10) . ? C42 H42A 0.9500 . ? C43 C44 1.403(10) . ? C43 C46 1.471(11) . ? C44 C45 1.361(11) . ? C44 H44A 0.9500 . ? C45 N1 1.349(9) . ? C45 H45A 0.9500 . ? C46 C47 1.565(11) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.521(10) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C51 1.506(10) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 N2 1.361(9) . ? C49 C50 1.362(11) . ? C49 H49A 0.9500 . ? C50 C51 1.402(9) . ? C50 H50A 0.9500 . ? C51 C52 1.390(10) . ? C52 C53 1.406(11) . ? C52 H52A 0.9500 . ? C53 N2 1.331(9) . ? C53 H53A 0.9500 . ? N2 Ag1 2.134(6) 8_655 ? N3 Ag3 2.186(8) 5_666 ? O1W H1WA 0.8000 . ? O1W H1WB 0.8000 . ? O2W H2WA 0.8000 . ? O2W H2WB 0.8000 . ? O3W H3WA 0.8000 . ? O3W H3WB 0.8000 . ? O4W H4WA 0.8001 . ? O4W H4WB 0.7999 . ? O5W H5WA 0.8000 . ? O5W H5WB 0.8000 . ? O6W H6WA 0.7999 . ? O6W H6WB 0.8000 . ? O7W H7WA 0.8000 . ? O7W H7WB 0.7999 . ? O8W H8WA 0.8001 . ? O8W H8WB 0.7999 . ? O9W H9WA 0.8000 . ? O9W H9WB 0.7999 . ? O10W H10A 0.8000 . ? O10W H10B 0.8000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 168.6(2) . 8_665 ? N1 Ag1 O1W 94.72(19) . . ? N2 Ag1 O1W 96.59(18) 8_665 . ? N4 Ag2 N4 180.0(3) . 5_676 ? Ag3 Ag3 N3 89.7(7) 5_666 . ? Ag3 Ag3 N3 72.9(7) 5_666 5_666 ? N3 Ag3 N3 162.55(11) . 5_666 ? O2 C1 O1 125.9(8) . . ? O2 C1 C2 119.5(7) . . ? O1 C1 C2 114.5(7) . . ? C3 C2 C1 114.3(7) . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2B 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C2 C3 C4 117.6(9) . . ? C2 C3 H3A 107.9 . . ? C4 C3 H3A 107.9 . . ? C2 C3 H3B 107.9 . . ? C4 C3 H3B 107.9 . . ? H3A C3 H3B 107.2 . . ? C5 C4 C3 120.8(9) . . ? C5 C4 H4A 107.1 . . ? C3 C4 H4A 107.1 . . ? C5 C4 H4B 107.1 . . ? C3 C4 H4B 107.1 . . ? H4A C4 H4B 106.8 . . ? C4 C5 C6 113.6(7) . . ? C4 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? C4 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? O3 C6 O4 124.9(8) . . ? O3 C6 C5 118.0(8) . . ? O4 C6 C5 117.1(7) . . ? N3 C21 C22 124.9(8) . . ? N3 C21 H21A 117.5 . . ? C22 C21 H21A 117.5 . . ? C21 C22 C23 121.0(7) . . ? C21 C22 H22A 119.5 . . ? C23 C22 H22A 119.5 . . ? C22 C23 C24 115.0(8) . . ? C22 C23 C26 122.3(7) . . ? C24 C23 C26 122.5(7) . . ? C25 C24 C23 120.9(8) . . ? C25 C24 H24A 119.5 . . ? C23 C24 H24A 119.5 . . ? C24 C25 N3 124.9(8) . . ? C24 C25 H25A 117.6 . . ? N3 C25 H25A 117.6 . . ? C27 C26 C23 111.4(6) . . ? C27 C26 H26A 109.4 . . ? C23 C26 H26A 109.4 . . ? C27 C26 H26B 109.4 . . ? C23 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C28 112.9(6) . . ? C26 C27 H27A 109.0 . . ? C28 C27 H27A 109.0 . . ? C26 C27 H27B 109.0 . . ? C28 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C31 C28 C27 111.6(6) . . ? C31 C28 H28A 109.3 . . ? C27 C28 H28A 109.3 . . ? C31 C28 H28B 109.3 . . ? C27 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? N4 C29 C30 122.7(7) . . ? N4 C29 H29A 118.6 . . ? C30 C29 H29A 118.6 . . ? C29 C30 C31 121.2(7) . . ? C29 C30 H30A 119.4 . . ? C31 C30 H30A 119.4 . . ? C30 C31 C32 115.4(7) . . ? C30 C31 C28 122.3(7) . . ? C32 C31 C28 122.3(7) . . ? C31 C32 C33 121.8(7) . . ? C31 C32 H32A 119.1 . . ? C33 C32 H32A 119.1 . . ? N4 C33 C32 121.1(7) . . ? N4 C33 H33A 119.4 . . ? C32 C33 H33A 119.4 . . ? N1 C41 C42 123.7(7) . . ? N1 C41 H41A 118.2 . . ? C42 C41 H41A 118.2 . . ? C41 C42 C43 119.9(7) . . ? C41 C42 H42A 120.1 . . ? C43 C42 H42A 120.1 . . ? C42 C43 C44 116.2(8) . . ? C42 C43 C46 122.1(7) . . ? C44 C43 C46 121.7(7) . . ? C45 C44 C43 120.3(7) . . ? C45 C44 H44A 119.9 . . ? C43 C44 H44A 119.9 . . ? N1 C45 C44 124.3(7) . . ? N1 C45 H45A 117.9 . . ? C44 C45 H45A 117.9 . . ? C43 C46 C47 111.4(6) . . ? C43 C46 H46A 109.4 . . ? C47 C46 H46A 109.4 . . ? C43 C46 H46B 109.4 . . ? C47 C46 H46B 109.4 . . ? H46A C46 H46B 108.0 . . ? C48 C47 C46 112.4(6) . . ? C48 C47 H47A 109.1 . . ? C46 C47 H47A 109.1 . . ? C48 C47 H47B 109.1 . . ? C46 C47 H47B 109.1 . . ? H47A C47 H47B 107.9 . . ? C51 C48 C47 109.7(6) . . ? C51 C48 H48A 109.7 . . ? C47 C48 H48A 109.7 . . ? C51 C48 H48B 109.7 . . ? C47 C48 H48B 109.7 . . ? H48A C48 H48B 108.2 . . ? N2 C49 C50 122.7(6) . . ? N2 C49 H49A 118.7 . . ? C50 C49 H49A 118.7 . . ? C49 C50 C51 122.1(7) . . ? C49 C50 H50A 119.0 . . ? C51 C50 H50A 119.0 . . ? C52 C51 C50 114.7(7) . . ? C52 C51 C48 123.2(6) . . ? C50 C51 C48 122.1(6) . . ? C51 C52 C53 120.7(6) . . ? C51 C52 H52A 119.7 . . ? C53 C52 H52A 119.7 . . ? N2 C53 C52 123.1(7) . . ? N2 C53 H53A 118.5 . . ? C52 C53 H53A 118.5 . . ? C45 N1 C41 115.7(7) . . ? C45 N1 Ag1 123.5(5) . . ? C41 N1 Ag1 120.7(5) . . ? C53 N2 C49 116.7(7) . . ? C53 N2 Ag1 122.1(5) . 8_655 ? C49 N2 Ag1 121.0(5) . 8_655 ? C21 N3 C25 113.2(8) . . ? C21 N3 Ag3 134.1(6) . . ? C25 N3 Ag3 112.5(6) . . ? C21 N3 Ag3 116.6(6) . 5_666 ? C25 N3 Ag3 130.0(6) . 5_666 ? Ag3 N3 Ag3 17.45(11) . 5_666 ? C29 N4 C33 117.7(7) . . ? C29 N4 Ag2 121.9(5) . . ? C33 N4 Ag2 120.3(5) . . ? Ag1 O1W H1WA 111.2 . . ? Ag1 O1W H1WB 108.3 . . ? H1WA O1W H1WB 108.3 . . ? H2WA O2W H2WB 100.9 . . ? H3WA O3W H3WB 124.7 . . ? H4WA O4W H4WB 144.2 . . ? H5WA O5W H5WB 108.3 . . ? H6WA O6W H6WB 108.4 . . ? H7WA O7W H7WB 135.6 . . ? H8WA O8W H8WB 109.0 . . ? H9WA O9W H9WB 133.5 . . ? H10A O10W H10B 108.4 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O2 0.80 1.92 2.716(8) 174.5 . O1W H1WB O2W 0.80 1.96 2.757(7) 174.6 . O2W H2WA O3W 0.80 1.98 2.772(8) 173.0 8_655 O2W H2WB O6W 0.80 2.06 2.845(8) 167.0 1_455 O3W H3WA O4 0.80 1.89 2.680(8) 170.2 . O3W H3WB O4W 0.80 2.29 2.838(7) 126.6 8_665 O4W H4WA O1W 0.80 2.36 2.797(8) 115.6 . O4W H4WB O8W 0.80 1.98 2.770(9) 171.8 8_655 O5W H5WA O4W 0.80 1.89 2.691(7) 175.7 8_765 O5W H5WB O3 0.80 1.91 2.711(8) 175.9 . O6W H6WA O5W 0.80 1.99 2.790(11) 179.1 8_755 O6W H6WB O1 0.80 1.87 2.674(9) 179.4 . O7W H7WA O9W 0.80 2.04 2.705(9) 140.2 . O7W H7WB O2 0.80 1.96 2.759(8) 177.2 . O8W H8WA O10W 0.80 1.95 2.683(8) 152.7 1_455 O8W H8WB O4 0.80 1.98 2.718(7) 153.1 . O9W H9WA O1 0.80 1.94 2.738(8) 171.9 1_455 O9W H9WB O2W 0.80 2.05 2.687(9) 137.1 . O10W H10A O7W 0.80 1.94 2.744(9) 179.7 1_655 O10W H10B O3 0.80 1.98 2.781(8) 179.7 . _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.137 _refine_diff_density_min -1.019 _refine_diff_density_rms 0.119