# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Jin Jin' 'Hongwei Hou et al.' _publ_contact_author_name 'Jin Jin' _publ_contact_author_email jinjin8405@163.com data_a _database_code_depnum_ccdc_archive 'CCDC 819876' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H42 Ag3 Cl2 N18 O15' _chemical_formula_weight 1469.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'P 21/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 11.978(2) _cell_length_b 14.054(3) _cell_length_c 18.062(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.83(3) _cell_angle_gamma 90.00 _cell_volume 2877.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1466 _exptl_absorpt_coefficient_mu 1.183 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 29147 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5287 _reflns_number_gt 4783 _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^)+(0.1337P)^2^+5.9721P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5287 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1005 _refine_ls_R_factor_gt 0.0923 _refine_ls_wR_factor_ref 0.2680 _refine_ls_wR_factor_gt 0.2581 _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_restrained_S_all 1.178 _refine_ls_shift/su_max 3.742 _refine_ls_shift/su_mean 0.069 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 0.32780(7) 0.49480(5) 0.46861(4) 0.0869(3) Uani 1 1 d . . . Ag2 Ag -0.15034(11) 0.7500 0.39891(7) 0.1370(7) Uani 1 2 d S . . N1 N 0.3547(6) 0.4893(5) 0.5904(4) 0.0718(17) Uani 1 1 d . . . N2 N 0.3613(6) 0.5239(4) 0.7075(3) 0.0653(15) Uani 1 1 d . . . N3 N 0.4098(8) 0.4369(6) 0.7125(4) 0.095(2) Uani 1 1 d . . . N4 N 0.3127(7) 0.4883(4) 0.3482(4) 0.0745(18) Uani 1 1 d . . . N5 N 0.2937(5) 0.5241(4) 0.2290(3) 0.0578(14) Uani 1 1 d . . . N6 N 0.3378(7) 0.4350(4) 0.2397(4) 0.0802(19) Uani 1 1 d . . . N7 N -0.1505(10) 0.7500 0.5168(7) 0.108(4) Uani 1 2 d S . . N8 N -0.0943(8) 0.7500 0.6427(6) 0.080(3) Uani 1 2 d S . . N9 N -0.2162(10) 0.7500 0.6163(9) 0.101(4) Uani 1 2 d S . . N10 N -0.1735(11) 0.7500 0.2757(7) 0.124(5) Uani 1 2 d S . . N11 N -0.1527(8) 0.7500 0.1619(6) 0.087(3) Uani 1 2 d S . . N12 N -0.2694(12) 0.7500 0.1466(9) 0.191(11) Uani 1 2 d S . . Cl1 Cl 0.0164(13) 0.5232(12) 0.4776(7) 0.188(5) Uani 0.50 1 d P . . Cl2 Cl 0.4118(3) 0.7500 0.4847(2) 0.0873(9) Uani 1 2 d S . . O1 O 0.5563(4) 0.4236(4) 0.0097(4) 0.093(2) Uani 1 1 d . . . O2 O 0.7223(5) 0.5039(3) 0.0401(4) 0.0779(17) Uani 1 1 d . . . O3 O 1.0946(4) 0.3292(3) 0.0778(3) 0.0645(12) Uani 1 1 d . . . O4 O 0.326(2) 0.7500 0.514(2) 0.293(15) Uani 1 2 d S . . O5 O 0.364(3) 0.7500 0.4061(10) 0.274(14) Uani 1 2 d S . . O6 O 0.4770(9) 0.6661(8) 0.5046(7) 0.169(4) Uani 1 1 d . . . O7 O 0.3210(11) 0.3418(5) 0.0638(5) 0.165(4) Uani 1 1 d . . . O8 O 0.0933(19) 0.552(6) 0.414(3) 0.92(10) Uani 0.50 1 d P . . H8 H 0.0961 0.5060 0.3871 1.387 Uiso 0.50 1 calc PR . . O9 O 0.074(2) 0.599(3) 0.505(3) 0.34(3) Uani 0.50 1 d P . . O10 O -0.0767(17) 0.547(3) 0.4326(19) 0.238(18) Uani 0.50 1 d P . . C1 C 1.0435(8) 0.2500 0.0733(5) 0.0497(19) Uani 1 2 d S . . C2 C 0.9133(6) 0.2500 0.0611(4) 0.0381(16) Uani 1 2 d S . . C3 C 0.8522(5) 0.3345(4) 0.0538(3) 0.0402(12) Uani 1 1 d . . . H3 H 0.8931 0.3917 0.0588 0.048 Uiso 1 1 calc R . . C4 C 0.7316(5) 0.3365(4) 0.0392(3) 0.0410(12) Uani 1 1 d . . . C5 C 0.6718(7) 0.2500 0.0320(5) 0.0432(18) Uani 1 2 d S . . H5 H 0.5907 0.2500 0.0223 0.052 Uiso 1 2 calc SR . . C6 C 0.6678(5) 0.4289(4) 0.0295(4) 0.0521(15) Uani 1 1 d . . . C7 C 0.4038(9) 0.7500 0.1839(7) 0.078(3) Uani 1 2 d S . . H7A H 0.4347 0.7020 0.2229 0.117 Uiso 0.50 1 calc PR . . H7B H 0.4333 0.8112 0.2049 0.117 Uiso 0.50 1 calc PR . . H7C H 0.4280 0.7368 0.1391 0.117 Uiso 0.50 1 calc PR . . C8 C 0.2720(7) 0.7500 0.1599(5) 0.0491(19) Uani 1 2 d S . . C9 C 0.2087(5) 0.6644(4) 0.1480(3) 0.0477(13) Uani 1 1 d . . . C10 C 0.2730(8) 0.5716(5) 0.1532(4) 0.0679(19) Uani 1 1 d . . . H10A H 0.2274 0.5298 0.1117 0.082 Uiso 1 1 calc R . . H10B H 0.3482 0.5831 0.1453 0.082 Uiso 1 1 calc R . . C11 C 0.0866(6) 0.6640(4) 0.1290(3) 0.0505(14) Uani 1 1 d . . . C12 C 0.0221(9) 0.5681(7) 0.1170(5) 0.093(3) Uani 1 1 d . . . H12A H -0.0408 0.5708 0.1390 0.140 Uiso 1 1 calc R . . H12B H 0.0765 0.5188 0.1424 0.140 Uiso 1 1 calc R . . H12C H -0.0097 0.5545 0.0621 0.140 Uiso 1 1 calc R . . C13 C 0.0265(7) 0.7500 0.1211(5) 0.052(2) Uani 1 2 d S . . C14 C -0.1095(9) 0.7500 0.0966(7) 0.091(4) Uani 1 2 d S . . H14A H -0.1396 0.8058 0.0648 0.109 Uiso 0.50 1 calc PR . . H14B H -0.1396 0.6942 0.0648 0.109 Uiso 0.50 1 calc PR . . C15 C -0.1026(12) 0.7500 0.2358(8) 0.121(6) Uani 1 2 d S . . C16 C -0.2774(14) 0.7500 0.2206(11) 0.188(13) Uani 1 2 d S . . C17 C 0.2794(7) 0.5546(6) 0.2942(4) 0.071(2) Uani 1 1 d . . . H17 H 0.2502 0.6141 0.3011 0.085 Uiso 1 1 calc R . . C18 C 0.3468(9) 0.4163(6) 0.3124(5) 0.083(2) Uani 1 1 d . . . H18 H 0.3743 0.3586 0.3366 0.100 Uiso 1 1 calc R . . C19 C 0.3288(8) 0.5537(6) 0.6341(4) 0.074(2) Uani 1 1 d . . . H19 H 0.2928 0.6118 0.6164 0.089 Uiso 1 1 calc R . . C20 C 0.4038(8) 0.4203(7) 0.6395(5) 0.086(2) Uani 1 1 d . . . H20 H 0.4317 0.3646 0.6240 0.103 Uiso 1 1 calc R . . C21 C -0.0611(13) 0.7500 0.5805(8) 0.120(6) Uani 1 2 d S . . C22 C -0.2406(13) 0.7500 0.5411(9) 0.092(4) Uani 1 2 d S . . C23 C -0.0298(13) 0.7500 0.7281(8) 0.116(5) Uani 1 2 d S . . H23A H -0.0513 0.6941 0.7519 0.139 Uiso 0.50 1 calc PR . . H23B H -0.0513 0.8059 0.7519 0.139 Uiso 0.50 1 calc PR . . C24 C 0.1058(10) 0.7500 0.7424(6) 0.078(4) Uani 1 2 d S . . C25 C 0.1012(10) 0.5704(8) 0.7412(6) 0.108(3) Uani 1 1 d . . . H25A H 0.1404 0.5233 0.7200 0.161 Uiso 1 1 calc R . . H25B H 0.0216 0.5781 0.7070 0.161 Uiso 1 1 calc R . . H25C H 0.1005 0.5504 0.7919 0.161 Uiso 1 1 calc R . . C26 C 0.1652(7) 0.6632(7) 0.7485(4) 0.075(2) Uani 1 1 d . . . C27 C 0.2853(7) 0.6646(6) 0.7626(4) 0.0659(18) Uani 1 1 d . . . C28 C 0.3456(10) 0.7500 0.7667(5) 0.067(3) Uani 1 2 d S . . C29 C 0.3557(8) 0.5725(6) 0.7790(4) 0.081(2) Uani 1 1 d . . . H29A H 0.4354 0.5864 0.8125 0.097 Uiso 1 1 calc R . . H29B H 0.3206 0.5297 0.8074 0.097 Uiso 1 1 calc R . . C30 C 0.4767(10) 0.7500 0.7735(8) 0.085(3) Uani 1 2 d S . . H30A H 0.5236 0.7373 0.8266 0.128 Uiso 0.50 1 calc PR . . H30B H 0.4976 0.8110 0.7580 0.128 Uiso 0.50 1 calc PR . . H30C H 0.4908 0.7017 0.7400 0.128 Uiso 0.50 1 calc PR . . 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 0.1173(7) 0.0899(6) 0.0529(4) 0.0116(3) 0.0265(4) 0.0116(4) Ag2 0.0936(8) 0.246(2) 0.0726(7) 0.000 0.0286(6) 0.000 N1 0.080(4) 0.078(4) 0.053(4) 0.008(3) 0.015(3) 0.009(3) N2 0.078(4) 0.067(4) 0.044(3) 0.010(3) 0.009(3) 0.000(3) N3 0.129(6) 0.079(5) 0.068(4) 0.019(4) 0.017(4) 0.026(4) N4 0.101(5) 0.069(4) 0.055(4) 0.015(3) 0.028(4) 0.019(3) N5 0.077(4) 0.047(3) 0.051(3) 0.004(2) 0.023(3) 0.015(3) N6 0.124(6) 0.052(3) 0.075(4) 0.012(3) 0.046(4) 0.025(3) N7 0.070(6) 0.188(14) 0.071(7) 0.000 0.028(6) 0.000 N8 0.064(5) 0.110(8) 0.074(6) 0.000 0.034(5) 0.000 N9 0.081(7) 0.107(9) 0.134(11) 0.000 0.061(7) 0.000 N10 0.074(7) 0.227(17) 0.083(8) 0.000 0.042(7) 0.000 N11 0.052(5) 0.149(10) 0.062(6) 0.000 0.022(4) 0.000 N12 0.072(8) 0.42(3) 0.086(9) 0.000 0.035(7) 0.000 Cl1 0.149(9) 0.235(16) 0.143(11) -0.046(10) -0.005(8) -0.030(9) Cl2 0.0760(18) 0.084(2) 0.101(2) 0.000 0.0273(17) 0.000 O1 0.048(3) 0.051(3) 0.178(7) -0.011(3) 0.034(3) 0.007(2) O2 0.057(3) 0.041(3) 0.129(5) -0.002(2) 0.020(3) 0.003(2) O3 0.046(2) 0.050(2) 0.097(4) -0.007(2) 0.022(2) -0.0093(19) O4 0.28(3) 0.28(3) 0.42(4) 0.000 0.26(3) 0.000 O5 0.42(4) 0.24(2) 0.098(11) 0.000 -0.010(17) 0.000 O6 0.160(8) 0.105(7) 0.229(13) 0.029(6) 0.047(8) 0.018(6) O7 0.253(11) 0.078(5) 0.109(6) 0.005(4) -0.017(6) 0.004(6) O8 0.087(14) 2.0(2) 0.54(6) -1.00(11) -0.10(2) 0.26(5) O9 0.117(18) 0.32(4) 0.48(6) -0.26(5) -0.03(2) 0.04(2) O10 0.081(12) 0.35(4) 0.26(3) -0.19(3) 0.029(16) -0.053(19) C1 0.049(5) 0.058(5) 0.041(4) 0.000 0.013(4) 0.000 C2 0.037(4) 0.043(4) 0.035(4) 0.000 0.011(3) 0.000 C3 0.041(3) 0.042(3) 0.041(3) -0.004(2) 0.017(2) -0.003(2) C4 0.045(3) 0.037(3) 0.044(3) -0.003(2) 0.018(2) -0.001(2) C5 0.033(4) 0.051(5) 0.049(5) 0.000 0.019(3) 0.000 C6 0.049(3) 0.044(3) 0.068(4) -0.008(3) 0.025(3) 0.003(3) C7 0.050(5) 0.104(9) 0.072(7) 0.000 0.008(5) 0.000 C8 0.041(4) 0.067(5) 0.035(4) 0.000 0.006(3) 0.000 C9 0.055(3) 0.049(3) 0.032(3) 0.001(2) 0.006(2) 0.003(3) C10 0.100(5) 0.058(4) 0.047(4) 0.007(3) 0.026(4) 0.023(4) C11 0.064(4) 0.057(4) 0.032(3) -0.003(2) 0.017(3) -0.016(3) C12 0.112(7) 0.090(6) 0.071(5) 0.004(4) 0.022(5) -0.050(5) C13 0.045(4) 0.081(6) 0.031(4) 0.000 0.013(3) 0.000 C14 0.039(5) 0.165(13) 0.069(7) 0.000 0.017(5) 0.000 C15 0.072(8) 0.22(2) 0.056(7) 0.000 0.005(6) 0.000 C16 0.070(9) 0.41(4) 0.089(12) 0.000 0.034(9) 0.000 C17 0.096(5) 0.062(4) 0.055(4) 0.009(3) 0.025(4) 0.021(4) C18 0.118(7) 0.066(5) 0.076(5) 0.024(4) 0.046(5) 0.031(5) C19 0.093(5) 0.078(5) 0.049(4) 0.013(4) 0.018(4) 0.009(4) C20 0.105(6) 0.085(6) 0.059(5) 0.012(4) 0.014(4) 0.022(5) C21 0.083(9) 0.22(2) 0.065(8) 0.000 0.035(7) 0.000 C22 0.088(9) 0.102(10) 0.085(9) 0.000 0.025(7) 0.000 C23 0.099(10) 0.184(17) 0.078(9) 0.000 0.047(8) 0.000 C24 0.063(6) 0.140(12) 0.042(5) 0.000 0.032(5) 0.000 C25 0.126(8) 0.126(9) 0.082(6) -0.001(6) 0.049(6) -0.045(7) C26 0.081(5) 0.103(6) 0.047(4) 0.002(4) 0.028(4) -0.019(5) C27 0.081(5) 0.084(5) 0.033(3) 0.003(3) 0.019(3) -0.005(4) C28 0.077(7) 0.082(7) 0.037(5) 0.000 0.011(5) 0.000 C29 0.109(6) 0.082(5) 0.049(4) 0.014(4) 0.021(4) 0.002(5) C30 0.063(6) 0.088(8) 0.095(9) 0.000 0.012(6) 0.000 _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 2.120(7) . ? Ag1 N4 2.126(7) . ? Ag2 N7 2.129(11) . ? Ag2 N10 2.153(12) . ? N1 C19 1.303(11) . ? N1 C20 1.316(10) . ? N2 C19 1.323(9) . ? N2 N3 1.343(10) . ? N2 C29 1.482(10) . ? N3 C20 1.317(11) . ? N4 C17 1.314(9) . ? N4 C18 1.334(10) . ? N5 C17 1.316(9) . ? N5 N6 1.349(8) . ? N5 C10 1.470(8) . ? N6 C18 1.308(10) . ? N7 C21 1.294(18) . ? N7 C22 1.291(18) . ? N8 C21 1.308(16) . ? N8 N9 1.382(15) . ? N8 C23 1.485(17) . ? N9 C22 1.295(19) . ? N10 C15 1.279(18) . ? N10 C16 1.32(2) . ? N11 C15 1.274(16) . ? N11 N12 1.335(16) . ? N11 C14 1.432(14) . ? N12 C16 1.37(2) . ? Cl1 O10 1.19(3) . ? Cl1 Cl1 1.20(2) 3_566 ? Cl1 O9 1.29(4) . ? Cl1 O8 1.74(7) . ? Cl1 O10 1.83(4) 3_566 ? Cl1 O9 2.11(6) 3_566 ? Cl2 O4 1.306(19) . ? Cl2 O5 1.348(17) . ? Cl2 O6 1.396(10) 4_575 ? Cl2 O6 1.396(10) . ? O1 C6 1.268(8) . ? O2 C6 1.221(8) . ? O3 C1 1.261(6) . ? O9 Cl1 2.11(5) 3_566 ? O10 Cl1 1.83(4) 3_566 ? C1 O3 1.261(6) 4_565 ? C1 C2 1.502(11) . ? C2 C3 1.380(7) 4_565 ? C2 C3 1.380(7) . ? C3 C4 1.382(7) . ? C4 C5 1.396(6) . ? C4 C6 1.488(8) . ? C5 C4 1.396(6) 4_565 ? C7 C8 1.497(13) . ? C8 C9 1.402(7) . ? C8 C9 1.402(7) 4_575 ? C9 C11 1.390(9) . ? C9 C10 1.503(9) . ? C11 C13 1.391(8) . ? C11 C12 1.534(10) . ? C13 C11 1.391(8) 4_575 ? C13 C14 1.545(13) . ? C23 C24 1.560(18) . ? C24 C26 1.398(11) 4_575 ? C24 C26 1.398(10) . ? C25 C26 1.497(13) . ? C26 C27 1.378(11) . ? C27 C28 1.390(10) . ? C27 C29 1.521(12) . ? C28 C27 1.390(9) 4_575 ? C28 C30 1.535(16) . ? 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 N4 174.2(2) . . ? N7 Ag2 N10 173.0(4) . . ? C19 N1 C20 104.2(7) . . ? C19 N1 Ag1 128.1(5) . . ? C20 N1 Ag1 127.7(6) . . ? C19 N2 N3 109.7(7) . . ? C19 N2 C29 130.2(7) . . ? N3 N2 C29 120.1(6) . . ? C20 N3 N2 102.2(6) . . ? C17 N4 C18 104.2(7) . . ? C17 N4 Ag1 129.4(5) . . ? C18 N4 Ag1 126.2(5) . . ? C17 N5 N6 109.4(6) . . ? C17 N5 C10 130.9(6) . . ? N6 N5 C10 119.7(5) . . ? C18 N6 N5 103.4(6) . . ? C21 N7 C22 103.9(12) . . ? C21 N7 Ag2 128.4(9) . . ? C22 N7 Ag2 127.6(10) . . ? C21 N8 N9 106.5(11) . . ? C21 N8 C23 133.7(11) . . ? N9 N8 C23 119.7(10) . . ? C22 N9 N8 102.6(11) . . ? C15 N10 C16 102.2(13) . . ? C15 N10 Ag2 134.1(10) . . ? C16 N10 Ag2 123.7(10) . . ? C15 N11 N12 108.9(12) . . ? C15 N11 C14 133.6(11) . . ? N12 N11 C14 117.5(10) . . ? N11 N12 C16 101.4(13) . . ? O10 Cl1 Cl1 100(2) . 3_566 ? O10 Cl1 O9 108(2) . . ? Cl1 Cl1 O9 116(3) 3_566 . ? O10 Cl1 O8 94(2) . . ? Cl1 Cl1 O8 159(3) 3_566 . ? O9 Cl1 O8 74(3) . . ? O10 Cl1 O10 139.8(17) . 3_566 ? Cl1 Cl1 O10 39.9(12) 3_566 3_566 ? O9 Cl1 O10 95(3) . 3_566 ? O8 Cl1 O10 125(2) . 3_566 ? O10 Cl1 O9 85(2) . 3_566 ? Cl1 Cl1 O9 33.2(16) 3_566 3_566 ? O9 Cl1 O9 149.3(19) . 3_566 ? O8 Cl1 O9 134(2) . 3_566 ? O10 Cl1 O9 60.5(12) 3_566 3_566 ? O4 Cl2 O5 108(2) . . ? O4 Cl2 O6 110.1(9) . 4_575 ? O5 Cl2 O6 106.4(9) . 4_575 ? O4 Cl2 O6 110.1(9) . . ? O5 Cl2 O6 106.4(9) . . ? O6 Cl2 O6 115.3(10) 4_575 . ? Cl1 O9 Cl1 30.7(19) . 3_566 ? Cl1 O10 Cl1 40.2(17) . 3_566 ? O3 C1 O3 124.0(8) . 4_565 ? O3 C1 C2 118.0(4) . . ? O3 C1 C2 118.0(4) 4_565 . ? C3 C2 C3 118.9(7) 4_565 . ? C3 C2 C1 120.5(3) 4_565 . ? C3 C2 C1 120.5(3) . . ? C4 C3 C2 121.7(5) . . ? C3 C4 C5 118.2(5) . . ? C3 C4 C6 120.4(5) . . ? C5 C4 C6 121.4(5) . . ? C4 C5 C4 121.2(7) . 4_565 ? O2 C6 O1 123.8(6) . . ? O2 C6 C4 120.4(5) . . ? O1 C6 C4 115.8(5) . . ? C9 C8 C9 118.3(7) . 4_575 ? C9 C8 C7 120.8(4) . . ? C9 C8 C7 120.8(4) 4_575 . ? C8 C9 C11 121.0(6) . . ? C8 C9 C10 119.6(6) . . ? C11 C9 C10 119.3(6) . . ? N5 C10 C9 112.3(5) . . ? C13 C11 C9 119.4(6) . . ? C13 C11 C12 121.9(7) . . ? C9 C11 C12 118.7(7) . . ? C11 C13 C11 120.8(8) 4_575 . ? C11 C13 C14 119.5(4) 4_575 . ? C11 C13 C14 119.5(4) . . ? N11 C14 C13 113.1(9) . . ? N10 C15 N11 114.6(13) . . ? N10 C16 N12 112.9(14) . . ? N5 C17 N4 109.7(7) . . ? N6 C18 N4 113.3(7) . . ? N1 C19 N2 109.6(7) . . ? N3 C20 N1 114.3(8) . . ? N7 C21 N8 111.7(12) . . ? N9 C22 N7 115.3(13) . . ? N8 C23 C24 109.7(10) . . ? C26 C24 C26 121.4(10) 4_575 . ? C26 C24 C23 119.3(5) 4_575 . ? C26 C24 C23 119.3(5) . . ? C27 C26 C24 118.5(8) . . ? C27 C26 C25 120.2(9) . . ? C24 C26 C25 121.3(8) . . ? C28 C27 C26 121.0(8) . . ? C28 C27 C29 118.6(7) . . ? C26 C27 C29 120.3(8) . . ? C27 C28 C27 119.3(11) . 4_575 ? C27 C28 C30 120.3(5) . . ? C27 C28 C30 120.3(5) 4_575 . ? N2 C29 C27 113.6(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.235 _refine_diff_density_min -1.180 _refine_diff_density_rms 0.107 data_p3 _database_code_depnum_ccdc_archive 'CCDC 806617' #TrackingRef '- CIF data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H84 Ag6 N42 O28' _chemical_formula_weight 2633.03 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 ? _symmetry_space_group_name_H-M P6/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z' '-y, x-y, z' '-x, -y, z' '-x+y, -x, z' 'y, -x+y, z' '-x, -y, -z' '-x+y, -x, -z' 'y, -x+y, -z' 'x, y, -z' 'x-y, x, -z' '-y, x-y, -z' _cell_length_a 26.362(4) _cell_length_b 26.362(4) _cell_length_c 17.809(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10718(3) _cell_formula_units_Z 3 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3948 _exptl_absorpt_coefficient_mu 0.873 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8518 _exptl_absorpt_correction_T_max 0.8730 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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 61090 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0173 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6225 _reflns_number_gt 5298 _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^)+(0.1965P)^2^+15.9609P] 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 6225 _refine_ls_number_parameters 364 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1077 _refine_ls_R_factor_gt 0.0991 _refine_ls_wR_factor_ref 0.3036 _refine_ls_wR_factor_gt 0.2942 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.594 _refine_ls_shift/su_mean 0.019 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 0.353094(7) -0.042500(7) 0.0000 0.08026(6) Uani 1 2 d S . . Ag2 Ag 0.588413(8) 0.215305(8) 0.0000 0.08949(7) Uani 1 2 d S . . Ag3 Ag 0.336441(11) 0.205075(8) 0.0000 0.11311(8) Uani 1 2 d S . . N1 N 0.35631(6) -0.04557(5) 0.11895(9) 0.0915(6) Uani 1 1 d . . . N2 N 0.36665(8) -0.02725(6) 0.23870(9) 0.1114(7) Uani 1 1 d . . . N3 N 0.35290(8) -0.08482(6) 0.23337(10) 0.1125(7) Uani 1 1 d . . . N4 N 0.59456(6) 0.21991(6) 0.12131(9) 0.0974(6) Uani 1 1 d . . . N5 N 0.57859(6) 0.21275(6) 0.23910(9) 0.1028(6) Uani 1 1 d . . . N6 N 0.63701(8) 0.23733(11) 0.23063(14) 0.1618(10) Uani 1 1 d . . . N7 N 0.32867(7) 0.20159(6) 0.11978(9) 0.1080(6) Uani 1 1 d . . . N8 N 0.33522(7) 0.18868(6) 0.23944(10) 0.1095(6) Uani 1 1 d . . . N9 N 0.29664(8) 0.20817(8) 0.23463(12) 0.1414(7) Uani 1 1 d . . . N10 N 0.48546(9) 0.27802(10) 0.0000 0.1151(10) Uani 1 2 d S . . N11 N 0.49517(8) 0.06749(6) 0.03586(9) 0.1062(11) Uani 0.50 1 d PD . . N12 N 0.15610(4) 0.07091(4) 0.0000 0.0577(5) Uani 1 2 d SD . . C1 C 0.36910(8) -0.00569(6) 0.17169(10) 0.0977(7) Uani 1 1 d . . . H1 H 0.3788 0.0336 0.1622 0.117 Uiso 1 1 calc R . . C2 C 0.34761(8) -0.09425(6) 0.16070(12) 0.0979(7) Uani 1 1 d . . . H2 H 0.3387 -0.1306 0.1386 0.117 Uiso 1 1 calc R . . C3 C 0.37802(14) -0.00026(8) 0.31596(14) 0.1645(15) Uani 1 1 d . . . H3A H 0.4059 -0.0084 0.3432 0.197 Uiso 1 1 calc R . . H3B H 0.3410 -0.0176 0.3448 0.197 Uiso 1 1 calc R . . C4 C 0.40335(11) 0.06576(7) 0.30893(9) 0.1237(9) Uani 1 1 d . . . C5 C 0.36458(11) 0.08832(8) 0.30834(10) 0.1168(10) Uani 1 1 d . . . C6 C 0.29765(12) 0.04974(11) 0.30583(15) 0.1611(13) Uani 1 1 d . . . H6A H 0.2870 0.0154 0.2742 0.242 Uiso 1 1 calc R . . H6B H 0.2806 0.0723 0.2849 0.242 Uiso 1 1 calc R . . H6C H 0.2827 0.0369 0.3568 0.242 Uiso 1 1 calc R . . C7 C 0.38796(9) 0.14944(7) 0.31032(10) 0.1001(7) Uani 1 1 d . . . C8 C 0.44921(8) 0.18709(7) 0.30960(10) 0.0933(7) Uani 1 1 d . . . C9 C 0.47579(10) 0.25277(7) 0.30741(12) 0.1116(8) Uani 1 1 d . . . H9A H 0.4923 0.2692 0.3567 0.167 Uiso 1 1 calc R . . H9B H 0.4455 0.2624 0.2945 0.167 Uiso 1 1 calc R . . H9C H 0.5069 0.2693 0.2695 0.167 Uiso 1 1 calc R . . C10 C 0.48518(8) 0.16215(7) 0.31098(10) 0.0974(6) Uani 1 1 d . . . C11 C 0.46437(9) 0.10356(7) 0.31041(11) 0.1085(8) Uani 1 1 d . . . C12 C 0.50311(11) 0.07622(9) 0.31113(14) 0.1747(10) Uani 1 1 d . . . H12A H 0.5356 0.0971 0.2758 0.262 Uiso 1 1 calc R . . H12B H 0.4801 0.0350 0.2962 0.262 Uiso 1 1 calc R . . H12C H 0.5187 0.0788 0.3618 0.262 Uiso 1 1 calc R . . C13 C 0.54907(9) 0.20093(10) 0.31457(11) 0.1264(8) Uani 1 1 d . . . H13A H 0.5658 0.1829 0.3477 0.152 Uiso 1 1 calc R . . H13B H 0.5577 0.2387 0.3374 0.152 Uiso 1 1 calc R . . C14 C 0.64459(10) 0.23917(14) 0.15792(15) 0.1564(14) Uani 1 1 d . . . H14 H 0.6815 0.2526 0.1343 0.188 Uiso 1 1 calc R . . C15 C 0.55406(8) 0.20159(8) 0.17282(11) 0.0998(7) Uani 1 1 d . . . H15 H 0.5131 0.1830 0.1636 0.120 Uiso 1 1 calc R . . C16 C 0.35057(9) 0.17744(9) 0.31496(12) 0.1196(9) Uani 1 1 d . . . H16A H 0.3143 0.1514 0.3430 0.144 Uiso 1 1 calc R . . H16B H 0.3719 0.2149 0.3428 0.144 Uiso 1 1 calc R . . C17 C 0.35336(8) 0.18451(7) 0.17309(11) 0.0997(7) Uani 1 1 d . . . H17 H 0.3803 0.1713 0.1635 0.120 Uiso 1 1 calc R . . C18 C 0.29454(9) 0.21648(9) 0.16348(15) 0.1288(8) Uani 1 1 d . . . H18 H 0.2715 0.2315 0.1428 0.155 Uiso 1 1 calc R . . O1 O 0.46320(14) 0.25069(15) 0.05057(17) 0.3164(19) Uani 1 1 d . . . O2 O 0.49722(8) 0.33077(10) 0.0000 0.1532(10) Uani 1 2 d S . . O3 O 0.50157(8) 0.03001(6) 0.0000 0.306(3) Uani 1 2 d SDU . . O4 O 0.50394(10) 0.07057(11) 0.10416(7) 0.1517(18) Uani 0.50 1 d PD . . H4 H 0.5004 0.0389 0.1196 0.228 Uiso 0.50 1 calc PR . . O5 O 0.49503(10) 0.10785(6) 0.0000 0.241(3) Uani 1 2 d SD . . O6 O 0.42188(7) 0.12998(6) 0.09378(14) 0.1375(7) Uani 1 1 d . . . O7 O 0.5000 0.0000 0.14661(18) 0.1730(15) Uani 1 2 d S . . O8 O 0.16280(8) 0.02798(6) 0.0000 0.817(12) Uani 1 2 d SD . . O9 O 0.17537(9) 0.09215(10) 0.07335(10) 0.853(5) Uani 1 1 d D . . O10 O 0.10976(6) 0.07091(9) 0.0000 0.820(14) Uani 1 2 d SD . . O11 O 0.5365(3) 0.2883(2) 0.0000 0.325(4) Uani 1 2 d S . . 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 0.08321(8) 0.06652(7) 0.07770(10) 0.000 0.000 0.02742(6) Ag2 0.08581(8) 0.08179(8) 0.09294(12) 0.000 0.000 0.03596(6) Ag3 0.15528(13) 0.09263(8) 0.10614(14) 0.000 0.000 0.07302(7) N1 0.1073(8) 0.0664(6) 0.0871(9) -0.0070(6) 0.0048(7) 0.0332(5) N2 0.1750(13) 0.0600(5) 0.0754(8) 0.0006(6) 0.0135(8) 0.0410(6) N3 0.1682(11) 0.0610(5) 0.0942(10) 0.0139(6) 0.0015(9) 0.0468(6) N4 0.0912(6) 0.1021(7) 0.1003(10) -0.0079(7) -0.0255(6) 0.0494(5) N5 0.1202(8) 0.1091(7) 0.0875(9) -0.0124(7) -0.0315(7) 0.0635(5) N6 0.1211(10) 0.1960(17) 0.1453(14) -0.0150(13) -0.0646(9) 0.0620(10) N7 0.1318(8) 0.0970(6) 0.1087(10) -0.0081(7) 0.0089(8) 0.0673(5) N8 0.1243(7) 0.1030(6) 0.1163(10) -0.0286(7) 0.0048(8) 0.0682(5) N9 0.1960(10) 0.1705(9) 0.1109(13) -0.0219(9) 0.0031(10) 0.1315(6) N10 0.0886(10) 0.1105(13) 0.144(2) 0.000 0.000 0.0479(8) N11 0.1084(11) 0.1063(11) 0.133(2) 0.0285(12) 0.0101(12) 0.0757(7) N12 0.0474(5) 0.0383(4) 0.0850(10) 0.000 0.000 0.0196(3) C1 0.1503(12) 0.0700(6) 0.0717(9) 0.0068(7) 0.0130(9) 0.0542(6) C2 0.1245(11) 0.0606(6) 0.0946(12) 0.0034(7) 0.0041(10) 0.0359(6) C3 0.293(3) 0.0714(9) 0.0910(13) 0.0187(9) 0.0481(15) 0.0624(12) C4 0.2409(17) 0.0858(7) 0.0486(7) 0.0046(6) 0.0131(10) 0.0850(8) C5 0.1531(16) 0.0771(9) 0.0625(9) -0.0081(8) 0.0164(10) 0.0142(10) C6 0.1644(18) 0.1184(15) 0.1211(15) -0.0183(12) 0.0583(13) 0.0111(14) C7 0.1216(11) 0.0870(8) 0.0772(10) -0.0082(8) 0.0124(9) 0.0413(7) C8 0.1385(11) 0.0837(7) 0.0599(8) -0.0043(7) -0.0016(8) 0.0572(6) C9 0.1654(13) 0.0775(7) 0.0947(12) -0.0073(8) -0.0138(11) 0.0630(7) C10 0.1397(10) 0.0851(7) 0.0788(9) -0.0055(7) -0.0258(8) 0.0647(5) C11 0.1808(13) 0.0806(7) 0.0708(10) 0.0022(7) -0.0027(10) 0.0704(7) C12 0.3369(16) 0.1709(9) 0.1041(14) -0.0343(10) -0.0658(13) 0.1928(7) C13 0.1673(11) 0.1562(11) 0.0864(11) -0.0396(9) -0.0550(9) 0.1038(8) C14 0.1098(14) 0.206(2) 0.1040(15) -0.0030(16) -0.0296(11) 0.0413(14) C15 0.0973(9) 0.0949(9) 0.0895(11) -0.0130(9) -0.0142(9) 0.0348(7) C16 0.1193(10) 0.1372(11) 0.1077(13) -0.0134(10) 0.0168(10) 0.0682(8) C17 0.1034(8) 0.0975(8) 0.1024(12) -0.0114(8) 0.0094(9) 0.0534(6) C18 0.1736(10) 0.1473(9) 0.1163(16) -0.0173(10) -0.0083(11) 0.1182(6) O1 0.316(2) 0.206(3) 0.300(2) 0.025(2) 0.2043(15) 0.035(2) O2 0.1407(9) 0.1864(11) 0.186(2) 0.000 0.000 0.1216(6) O3 0.1024(11) 0.1466(13) 0.696(9) 0.000 0.000 0.0821(8) O4 0.0868(14) 0.251(3) 0.0784(15) 0.0278(19) 0.0067(12) 0.0553(16) O5 0.253(3) 0.265(3) 0.202(4) 0.000 0.000 0.127(2) O6 0.1449(9) 0.1341(8) 0.1386(14) -0.0285(8) -0.0074(9) 0.0734(6) O7 0.1464(18) 0.186(2) 0.156(2) 0.000 0.000 0.0595(15) O8 0.302(6) 1.18(2) 0.168(5) 0.000 0.000 -0.229(10) O9 0.285(3) 0.355(3) 1.971(16) 0.591(5) 0.496(5) 0.199(2) O10 1.41(3) 0.162(4) 0.161(4) 0.000 0.000 -0.154(8) O11 0.350(5) 0.256(4) 0.409(8) 0.000 0.000 0.182(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 2.1233(16) 10 ? Ag1 N1 2.1233(16) . ? Ag2 N4 2.1654(17) . ? Ag2 N4 2.1654(17) 10 ? Ag3 N7 2.1405(17) 10 ? Ag3 N7 2.1405(17) . ? N1 C1 1.322(2) . ? N1 C2 1.399(2) . ? N2 C1 1.309(2) . ? N2 N3 1.376(2) . ? N2 C3 1.508(3) . ? N3 C2 1.312(3) . ? N4 C14 1.324(3) . ? N4 C15 1.303(2) . ? N5 C15 1.307(3) . ? N5 N6 1.348(2) . ? N5 C13 1.505(3) . ? N6 C14 1.308(4) . ? N7 C17 1.349(3) . ? N7 C18 1.387(3) . ? N8 C17 1.300(3) . ? N8 N9 1.352(3) . ? N8 C16 1.476(3) . ? N9 C18 1.292(3) . ? N10 O1 1.119(3) 10 ? N10 O1 1.119(3) . ? N10 O2 1.264(4) . ? N10 O11 1.232(7) . ? N11 O4 1.233(2) . ? N11 O5 1.243(3) . ? N11 N11 1.277(3) 10 ? N11 O3 1.257(3) . ? N12 O10 1.222(2) . ? N12 O8 1.229(2) . ? N12 O9 1.4120(18) . ? N12 O9 1.4120(18) 10 ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 C4 1.526(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C11 1.407(3) . ? C4 C5 1.416(4) . ? C5 C7 1.409(3) . ? C5 C6 1.535(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.410(3) . ? C7 C16 1.501(4) . ? C8 C10 1.398(3) . ? C8 C9 1.509(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.356(2) . ? C10 C13 1.471(3) . ? C11 C12 1.516(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? O3 N11 1.257(3) 10 ? O3 O3 1.543(3) 7_655 ? O4 H4 0.8400 . ? O5 N11 1.243(3) 10 ? O9 O10 2.011(2) . ? O10 O9 2.011(2) 10 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 172.25(10) 10 . ? N4 Ag2 N4 172.27(6) . 10 ? N7 Ag3 N7 170.48(9) 10 . ? C1 N1 C2 102.22(15) . . ? C1 N1 Ag1 132.67(12) . . ? C2 N1 Ag1 125.01(12) . . ? C1 N2 N3 110.14(15) . . ? C1 N2 C3 132.18(16) . . ? N3 N2 C3 117.63(16) . . ? C2 N3 N2 102.80(15) . . ? C14 N4 C15 105.66(18) . . ? C14 N4 Ag2 123.02(15) . . ? C15 N4 Ag2 131.07(13) . . ? C15 N5 N6 108.96(18) . . ? C15 N5 C13 127.84(16) . . ? N6 N5 C13 123.20(17) . . ? C14 N6 N5 104.2(2) . . ? C17 N7 C18 100.90(18) . . ? C17 N7 Ag3 131.58(16) . . ? C18 N7 Ag3 127.52(16) . . ? C17 N8 N9 110.67(19) . . ? C17 N8 C16 131.4(2) . . ? N9 N8 C16 117.87(18) . . ? C18 N9 N8 103.3(2) . . ? O1 N10 O1 107.2(3) 10 . ? O1 N10 O2 118.0(3) 10 . ? O1 N10 O2 118.0(3) . . ? O1 N10 O11 107.8(3) 10 . ? O1 N10 O11 107.8(3) . . ? O2 N10 O11 96.7(3) . . ? O4 N11 O5 122.1(2) . . ? O4 N11 N11 170.52(15) . 10 ? O5 N11 N11 59.07(9) . 10 ? O4 N11 O3 117.3(2) . . ? O5 N11 O3 118.11(15) . . ? N11 N11 O3 59.46(9) 10 . ? O10 N12 O8 127.14(14) . . ? O10 N12 O9 99.29(13) . . ? O8 N12 O9 100.16(14) . . ? O10 N12 O9 99.29(13) . 10 ? O8 N12 O9 100.16(14) . 10 ? O9 N12 O9 135.40(16) . 10 ? N2 C1 N1 111.40(16) . . ? N2 C1 H1 124.3 . . ? N1 C1 H1 124.3 . . ? N3 C2 N1 113.40(16) . . ? N3 C2 H2 123.3 . . ? N1 C2 H2 123.3 . . ? N2 C3 C4 109.49(17) . . ? N2 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? N2 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? C11 C4 C5 120.83(17) . . ? C11 C4 C3 120.0(3) . . ? C5 C4 C3 118.9(2) . . ? C7 C5 C4 119.0(2) . . ? C7 C5 C6 117.4(3) . . ? C4 C5 C6 123.6(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 C8 119.8(2) . . ? C5 C7 C16 123.01(19) . . ? C8 C7 C16 117.17(16) . . ? C10 C8 C7 118.39(16) . . ? C10 C8 C9 120.32(17) . . ? C7 C8 C9 121.3(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C8 123.52(17) . . ? C11 C10 C13 117.5(2) . . ? C8 C10 C13 118.94(17) . . ? C10 C11 C4 118.4(2) . . ? C10 C11 C12 123.81(18) . . ? C4 C11 C12 117.84(17) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 N5 113.51(15) . . ? C10 C13 H13A 108.9 . . ? N5 C13 H13A 108.9 . . ? C10 C13 H13B 108.9 . . ? N5 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? N4 C14 N6 111.6(2) . . ? N4 C14 H14 124.2 . . ? N6 C14 H14 124.2 . . ? N5 C15 N4 109.32(17) . . ? N5 C15 H15 125.3 . . ? N4 C15 H15 125.3 . . ? N8 C16 C7 111.21(18) . . ? N8 C16 H16A 109.4 . . ? C7 C16 H16A 109.4 . . ? N8 C16 H16B 109.4 . . ? C7 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N8 C17 N7 110.6(2) . . ? N8 C17 H17 124.7 . . ? N7 C17 H17 124.7 . . ? N9 C18 N7 114.4(2) . . ? N9 C18 H18 122.8 . . ? N7 C18 H18 122.8 . . ? N11 O3 N11 61.08(19) 10 . ? N11 O3 O3 147.89(9) 10 7_655 ? N11 O3 O3 147.89(9) . 7_655 ? N11 O4 H4 109.5 . . ? N11 O5 N11 61.85(19) . 10 ? O10 O9 N12 36.84(9) . . ? N12 O10 O9 43.87(8) . . ? N12 O10 O9 43.87(8) . 10 ? O9 O10 O9 81.04(13) . 10 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag1 N1 C1 133.7(4) 10 . . . ? N1 Ag1 N1 C2 -42.1(5) 10 . . . ? C1 N2 N3 C2 -0.3(2) . . . . ? C3 N2 N3 C2 -178.1(2) . . . . ? N4 Ag2 N4 C14 -24.7(9) 10 . . . ? N4 Ag2 N4 C15 161.9(6) 10 . . . ? C15 N5 N6 C14 -0.6(3) . . . . ? C13 N5 N6 C14 179.1(3) . . . . ? N7 Ag3 N7 C17 132.8(5) 10 . . . ? N7 Ag3 N7 C18 -46.2(6) 10 . . . ? C17 N8 N9 C18 -1.64(17) . . . . ? C16 N8 N9 C18 176.94(14) . . . . ? N3 N2 C1 N1 1.6(3) . . . . ? C3 N2 C1 N1 179.0(3) . . . . ? C2 N1 C1 N2 -2.1(2) . . . . ? Ag1 N1 C1 N2 -178.56(14) . . . . ? N2 N3 C2 N1 -1.1(2) . . . . ? C1 N1 C2 N3 2.0(2) . . . . ? Ag1 N1 C2 N3 178.82(14) . . . . ? C1 N2 C3 C4 -7.7(4) . . . . ? N3 N2 C3 C4 169.5(2) . . . . ? N2 C3 C4 C11 -95.0(3) . . . . ? N2 C3 C4 C5 91.1(3) . . . . ? C11 C4 C5 C7 -0.9(3) . . . . ? C3 C4 C5 C7 172.99(17) . . . . ? C11 C4 C5 C6 179.27(18) . . . . ? C3 C4 C5 C6 -6.9(3) . . . . ? C4 C5 C7 C8 2.7(3) . . . . ? C6 C5 C7 C8 -177.44(18) . . . . ? C4 C5 C7 C16 -175.88(17) . . . . ? C6 C5 C7 C16 4.0(3) . . . . ? C5 C7 C8 C10 -3.4(3) . . . . ? C16 C7 C8 C10 175.29(17) . . . . ? C5 C7 C8 C9 176.63(17) . . . . ? C16 C7 C8 C9 -4.7(3) . . . . ? C7 C8 C10 C11 2.3(3) . . . . ? C9 C8 C10 C11 -177.68(18) . . . . ? C7 C8 C10 C13 -176.59(17) . . . . ? C9 C8 C10 C13 3.4(3) . . . . ? C8 C10 C11 C4 -0.5(3) . . . . ? C13 C10 C11 C4 178.41(16) . . . . ? C8 C10 C11 C12 179.38(19) . . . . ? C13 C10 C11 C12 -1.7(3) . . . . ? C5 C4 C11 C10 -0.2(3) . . . . ? C3 C4 C11 C10 -174.03(18) . . . . ? C5 C4 C11 C12 179.87(18) . . . . ? C3 C4 C11 C12 6.1(3) . . . . ? C11 C10 C13 N5 84.2(2) . . . . ? C8 C10 C13 N5 -96.9(2) . . . . ? C15 N5 C13 C10 12.9(3) . . . . ? N6 N5 C13 C10 -166.7(2) . . . . ? C15 N4 C14 N6 -4.6(4) . . . . ? Ag2 N4 C14 N6 -179.5(2) . . . . ? N5 N6 C14 N4 3.2(4) . . . . ? N6 N5 C15 N4 -2.3(3) . . . . ? C13 N5 C15 N4 178.1(2) . . . . ? C14 N4 C15 N5 4.1(3) . . . . ? Ag2 N4 C15 N5 178.39(14) . . . . ? C17 N8 C16 C7 -8.5(2) . . . . ? N9 N8 C16 C7 173.24(13) . . . . ? C5 C7 C16 N8 -90.2(2) . . . . ? C8 C7 C16 N8 91.20(19) . . . . ? N9 N8 C17 N7 0.75(17) . . . . ? C16 N8 C17 N7 -177.58(14) . . . . ? C18 N7 C17 N8 0.43(16) . . . . ? Ag3 N7 C17 N8 -178.79(10) . . . . ? N8 N9 C18 N7 2.00(19) . . . . ? C17 N7 C18 N9 -1.57(18) . . . . ? Ag3 N7 C18 N9 177.69(11) . . . . ? O4 N11 O3 N11 -169.82(13) . . . 10 ? O5 N11 O3 N11 -7.4(2) . . . 10 ? O4 N11 O3 O3 30.1(5) . . . 7_655 ? O5 N11 O3 O3 -167.5(3) . . . 7_655 ? N11 N11 O3 O3 -160.1(4) 10 . . 7_655 ? O4 N11 O5 N11 168.96(18) . . . 10 ? O3 N11 O5 N11 7.4(2) . . . 10 ? O8 N12 O9 O10 -130.61(14) . . . . ? O9 N12 O9 O10 113.5(4) 10 . . . ? O8 N12 O10 O9 110.37(10) . . . . ? O9 N12 O10 O9 -139.3(2) 10 . . . ? O8 N12 O10 O9 -110.37(10) . . . 10 ? O9 N12 O10 O9 139.3(2) . . . 10 ? N12 O9 O10 O9 -27.24(14) . . . 10 ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 2.196 _refine_diff_density_min -1.346 _refine_diff_density_rms 0.123 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.007 -0.006 -0.139 3755.6 77.3 _platon_squeeze_details ; ;