# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Luo, Fang' _publ_contact_author_email luof746@nenu.edu.cn _publ_section_title ; Design Synthesis and Photocatalytic Activity of a Novel Lilac-like Silver-Vanadate Hybrid Solid Based on Dicyclic Rings of [V4O12]4- with Argentophilic {Ag7}7+ Cluster ; _publ_author_name 'Fang Luo' # Attachment '- h.cif' data_h _database_code_depnum_ccdc_archive 'CCDC 759774' #TrackingRef '- h.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H56 Ag7 N16 O24 V8,C10 H14 Ag N4, 2(H2 O)' _chemical_formula_sum 'C50 H74 Ag8 N20 O26 V8' _chemical_formula_weight 2641.78 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' 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' V V 0.3005 0.5294 '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' H H 0.0000 0.0000 '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 12.107(5) _cell_length_b 12.154(5) _cell_length_c 15.078(5) _cell_angle_alpha 83.821(5) _cell_angle_beta 68.816(5) _cell_angle_gamma 68.176(5) _cell_volume 1919.6(13) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6762 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1282 _exptl_absorpt_coefficient_mu 2.997 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.442 _exptl_absorpt_correction_T_max 0.533 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 9721 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6762 _reflns_number_gt 5839 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. During the refinement, the command 'isor' was used to restrain the non-H atoms with ADP and NPD problems. These atoms are as follows: c4 n2 These refinement led to the restraint number of 12. all the non-H atoms are refined anisotropically. ; _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^)+(0.0436P)^2^+16.1941P] 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 0.00026(5) _refine_ls_number_reflns 6685 _refine_ls_number_parameters 508 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1320 _refine_ls_wR_factor_gt 0.1279 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.100 _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 1.0000 0.0000 0.0000 0.0432(2) Uani 1 2 d S . . Ag2 Ag 1.04194(6) -0.26284(6) -0.01235(4) 0.04122(18) Uani 1 1 d . . . Ag3 Ag 0.75908(7) 0.61516(7) 0.37187(6) 0.0575(2) Uani 1 1 d . . . Ag4 Ag 0.5000 0.5000 0.5000 0.0691(4) Uani 1 2 d S . . Ag5 Ag 0.90576(6) -0.40042(7) 0.13291(5) 0.0510(2) Uani 1 1 d . . . C22 C 1.1636(9) -0.6139(9) 0.1021(7) 0.054(2) Uani 1 1 d . . . H22A H 1.1325 -0.6691 0.0922 0.065 Uiso 1 1 calc R . . C21 C 1.1782(8) -0.4512(8) 0.1257(6) 0.0410(19) Uani 1 1 d . . . H21A H 1.1603 -0.3712 0.1352 0.049 Uiso 1 1 calc R . . C11 C 1.0292(9) 0.5757(8) 0.3716(7) 0.049(2) Uani 1 1 d . . . H11A H 1.0070 0.6562 0.3825 0.059 Uiso 1 1 calc R . . C23 C 1.2802(8) -0.6386(8) 0.1042(7) 0.046(2) Uani 1 1 d . . . H23A H 1.3432 -0.7134 0.0965 0.056 Uiso 1 1 calc R . . C24 C 1.3979(8) -0.5195(8) 0.1311(6) 0.0399(19) Uani 1 1 d . . . H24A H 1.4222 -0.5718 0.1796 0.048 Uiso 1 1 calc R . . H24B H 1.3728 -0.4385 0.1526 0.048 Uiso 1 1 calc R . . C13 C 1.2420(12) 0.2698(11) 0.3218(9) 0.078(3) Uani 1 1 d . . . H13A H 1.2235 0.2185 0.2885 0.094 Uiso 1 1 calc R . . H13B H 1.3215 0.2781 0.2818 0.094 Uiso 1 1 calc R . . C15 C 1.3520(13) 0.0871(11) 0.3920(9) 0.088(4) Uani 1 1 d . . . H15A H 1.3348 0.0416 0.3529 0.106 Uiso 1 1 calc R . . H15B H 1.4376 0.0867 0.3605 0.106 Uiso 1 1 calc R . . C14 C 1.2511(14) 0.2203(12) 0.4096(9) 0.086(4) Uani 1 1 d . . . H14A H 1.1687 0.2204 0.4518 0.103 Uiso 1 1 calc R . . H14B H 1.2773 0.2680 0.4396 0.103 Uiso 1 1 calc R . . C8 C 0.9342(11) 0.1628(9) 0.5427(9) 0.067(3) Uani 1 1 d . . . H8A H 0.9663 0.1497 0.5948 0.080 Uiso 1 1 calc R . . H8B H 0.9914 0.1893 0.4891 0.080 Uiso 1 1 calc R . . C4 C 0.3370(14) 1.0370(13) 0.4873(11) 0.102(5) Uani 1 1 d U . . H4A H 0.2482 1.0500 0.5223 0.122 Uiso 1 1 calc R . . H4B H 0.3664 1.0755 0.5225 0.122 Uiso 1 1 calc R . . C25 C 1.5114(7) -0.5455(7) 0.0388(6) 0.0373(18) Uani 1 1 d . . . H25A H 1.5314 -0.6240 0.0146 0.045 Uiso 1 1 calc R . . H25B H 1.5843 -0.5460 0.0519 0.045 Uiso 1 1 calc R . . C1 C 0.5195(10) 0.8414(11) 0.4094(10) 0.089(5) Uani 1 1 d . . . H1A H 0.5517 0.8654 0.3477 0.107 Uiso 1 1 calc R . . N1 N 0.5729(7) 0.7384(6) 0.4420(5) 0.0439(17) Uani 1 1 d . . . C3 C 0.3939(10) 0.8468(9) 0.5528(9) 0.073(4) Uani 1 1 d . . . H3A H 0.3248 0.8696 0.6093 0.087 Uiso 1 1 calc R . . N5 N 0.8093(8) 0.2552(7) 0.5712(6) 0.053(2) Uani 1 1 d . . . C19 C 0.4527(9) -0.0346(8) 0.1351(7) 0.052(2) Uani 1 1 d . . . H19A H 0.4776 0.0235 0.1544 0.062 Uiso 1 1 calc R . . H19B H 0.3706 -0.0301 0.1811 0.062 Uiso 1 1 calc R . . C7 C 0.7219(12) 0.2836(11) 0.6606(8) 0.075(3) Uani 1 1 d . . . H7A H 0.7326 0.2498 0.7167 0.089 Uiso 1 1 calc R . . C18 C 0.5275(8) -0.2567(7) 0.1324(6) 0.0412(19) Uani 1 1 d . . . H18A H 0.4560 -0.2649 0.1284 0.049 Uiso 1 1 calc R . . C20 C 0.4406(8) -0.0042(7) 0.0381(7) 0.045(2) Uani 1 1 d . . . H20A H 0.4186 -0.0642 0.0181 0.054 Uiso 1 1 calc R . . H20B H 0.3714 0.0710 0.0436 0.054 Uiso 1 1 calc R . . C16 C 0.6637(8) -0.1824(8) 0.1368(7) 0.047(2) Uani 1 1 d . . . H16A H 0.7004 -0.1273 0.1367 0.057 Uiso 1 1 calc R . . C17 C 0.6336(8) -0.3439(8) 0.1358(7) 0.047(2) Uani 1 1 d . . . H17A H 0.6463 -0.4243 0.1368 0.057 Uiso 1 1 calc R . . C9 C 0.9338(11) 0.0481(8) 0.5155(8) 0.062(3) Uani 1 1 d . . . H9A H 0.9009 0.0611 0.4638 0.074 Uiso 1 1 calc R . . H9B H 0.8776 0.0209 0.5693 0.074 Uiso 1 1 calc R . . C10 C 1.0226(9) 0.4100(9) 0.3406(7) 0.055(2) Uani 1 1 d . . . H10A H 0.9945 0.3530 0.3295 0.066 Uiso 1 1 calc R . . C12 C 1.1400(11) 0.4903(9) 0.3681(8) 0.065(3) Uani 1 1 d . . . H12A H 1.2058 0.4999 0.3806 0.077 Uiso 1 1 calc R . . C6 C 0.6167(11) 0.3703(11) 0.6527(7) 0.065(3) Uani 1 1 d . . . H6A H 0.5416 0.4058 0.7027 0.078 Uiso 1 1 calc R . . C5 C 0.7549(9) 0.3262(8) 0.5129(6) 0.047(2) Uani 1 1 d . . . H5A H 0.7943 0.3258 0.4473 0.057 Uiso 1 1 calc R . . N3 N 0.9541(7) 0.5234(6) 0.3561(5) 0.0456(17) Uani 1 1 d . . . N7 N 1.0963(7) -0.4920(7) 0.1173(5) 0.0445(17) Uani 1 1 d . . . N8 N 1.2900(6) -0.5357(6) 0.1194(5) 0.0365(15) Uani 1 1 d . . . N4 N 1.1380(8) 0.3878(7) 0.3429(7) 0.065(2) Uani 1 1 d . . . N2 N 0.4128(8) 0.9073(8) 0.4762(8) 0.078(3) Uani 1 1 d U . . N10 N 0.5463(6) -0.1539(6) 0.1361(5) 0.0376(15) Uani 1 1 d . . . C2 C 0.4945(10) 0.7443(9) 0.5344(7) 0.055(2) Uani 1 1 d . . . H2A H 0.5086 0.6858 0.5784 0.066 Uiso 1 1 calc R . . N9 N 0.7212(6) -0.2982(6) 0.1376(5) 0.0394(16) Uani 1 1 d . . . N6 N 0.6392(8) 0.3967(7) 0.5597(5) 0.0491(18) Uani 1 1 d . . . O1 O 0.5462(5) 0.1911(5) 0.1522(5) 0.0482(15) Uani 1 1 d . . . O2 O 0.6688(5) 0.2883(5) 0.2287(4) 0.0412(13) Uani 1 1 d . . . O3 O 0.8928(6) 0.2337(5) 0.2812(4) 0.0418(14) Uani 1 1 d . . . O4 O 0.9600(7) -0.0266(5) 0.2653(5) 0.0550(17) Uani 1 1 d . . . O5 O 0.7262(5) 0.0295(5) 0.2235(4) 0.0433(14) Uani 1 1 d . . . O6 O 0.7917(5) 0.1569(5) 0.0551(4) 0.0456(14) Uani 1 1 d . . . O7 O 1.0610(7) 0.1049(6) 0.1116(4) 0.0630(19) Uani 1 1 d . . . O8 O 0.8323(6) -0.1854(5) 0.2988(5) 0.0550(17) Uani 1 1 d . . . O9 O 0.9519(5) -0.1481(5) 0.1170(4) 0.0441(14) Uani 1 1 d . . . O10 O 0.8560(6) 0.3905(5) 0.1334(4) 0.0407(13) Uani 1 1 d . . . O11 O 1.1354(6) 0.0725(7) 0.2624(5) 0.066(2) Uani 1 1 d . . . O12 O 0.7039(5) 0.4585(5) 0.3155(4) 0.0433(14) Uani 1 1 d . . . V1 V 0.77998(12) 0.34627(10) 0.23867(9) 0.0288(3) Uani 1 1 d . . . V2 V 0.68183(11) 0.16727(11) 0.16249(9) 0.0289(3) Uani 1 1 d . . . V3 V 0.86944(12) -0.08621(10) 0.22603(9) 0.0285(3) Uani 1 1 d . . . V4 V 1.01702(13) 0.09523(12) 0.22781(10) 0.0373(3) Uani 1 1 d . . . O1W O 0.7589(6) 0.1985(6) 0.8760(5) 0.0549(17) Uani 1 1 d . . . H1W H 0.8290 0.1543 0.8373 0.066 Uiso 1 1 d R . . H2W H 0.7612 0.1840 0.9319 0.066 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 0.0458(5) 0.0278(4) 0.0389(5) 0.0023(4) -0.0048(4) -0.0046(4) Ag2 0.0530(4) 0.0360(3) 0.0294(3) -0.0056(2) -0.0050(3) -0.0174(3) Ag3 0.0434(4) 0.0432(4) 0.0738(5) -0.0119(4) -0.0189(4) 0.0000(3) Ag4 0.0770(8) 0.0705(8) 0.0854(9) 0.0257(7) -0.0584(7) -0.0315(7) Ag5 0.0328(3) 0.0659(5) 0.0569(4) 0.0269(4) -0.0222(3) -0.0212(3) C22 0.047(5) 0.066(7) 0.058(6) 0.003(5) -0.015(5) -0.034(5) C21 0.033(4) 0.039(5) 0.042(5) 0.009(4) -0.006(4) -0.012(4) C11 0.053(5) 0.030(5) 0.060(6) -0.008(4) -0.018(5) -0.008(4) C23 0.042(5) 0.033(5) 0.062(6) -0.001(4) -0.014(4) -0.014(4) C24 0.038(4) 0.049(5) 0.039(4) 0.006(4) -0.016(4) -0.021(4) C13 0.070(8) 0.070(8) 0.071(8) -0.008(6) -0.013(6) -0.008(6) C15 0.091(9) 0.076(8) 0.064(7) -0.013(6) -0.038(7) 0.021(7) C14 0.104(10) 0.087(9) 0.077(8) 0.018(7) -0.042(8) -0.039(8) C8 0.069(7) 0.050(6) 0.091(8) 0.003(6) -0.051(6) -0.010(5) C4 0.077(7) 0.092(8) 0.113(8) 0.010(7) -0.019(6) -0.022(6) C25 0.029(4) 0.036(4) 0.052(5) 0.005(4) -0.021(4) -0.013(3) C1 0.049(6) 0.077(8) 0.090(9) 0.041(7) 0.000(6) 0.000(6) N1 0.042(4) 0.021(3) 0.059(5) 0.004(3) -0.017(4) -0.002(3) C3 0.055(6) 0.050(6) 0.091(9) -0.032(6) 0.012(6) -0.021(5) N5 0.067(5) 0.054(5) 0.053(5) 0.010(4) -0.038(4) -0.024(4) C19 0.048(5) 0.040(5) 0.068(6) -0.006(4) -0.023(5) -0.012(4) C7 0.099(9) 0.094(9) 0.047(6) 0.024(6) -0.045(6) -0.039(8) C18 0.045(5) 0.036(5) 0.052(5) 0.013(4) -0.024(4) -0.021(4) C20 0.037(4) 0.029(4) 0.075(6) 0.004(4) -0.032(4) -0.007(4) C16 0.046(5) 0.041(5) 0.067(6) 0.001(4) -0.030(5) -0.020(4) C17 0.046(5) 0.039(5) 0.070(6) 0.023(4) -0.031(5) -0.024(4) C9 0.093(8) 0.039(5) 0.075(7) 0.015(5) -0.053(7) -0.027(5) C10 0.038(5) 0.045(5) 0.072(7) -0.004(5) -0.015(5) -0.008(4) C12 0.067(7) 0.052(6) 0.085(8) -0.002(6) -0.039(6) -0.020(5) C6 0.063(7) 0.089(8) 0.040(5) 0.013(5) -0.019(5) -0.026(6) C5 0.063(6) 0.046(5) 0.039(5) 0.006(4) -0.029(4) -0.017(5) N3 0.045(4) 0.035(4) 0.051(4) 0.001(3) -0.014(3) -0.010(3) N7 0.036(4) 0.060(5) 0.041(4) 0.010(3) -0.012(3) -0.024(4) N8 0.031(3) 0.038(4) 0.040(4) 0.002(3) -0.012(3) -0.012(3) N4 0.043(5) 0.032(4) 0.109(8) -0.004(4) -0.026(5) 0.000(3) N2 0.039(4) 0.048(5) 0.116(7) 0.008(5) -0.002(4) -0.007(4) N10 0.039(4) 0.041(4) 0.040(4) 0.003(3) -0.018(3) -0.018(3) C2 0.062(6) 0.046(6) 0.054(6) -0.002(4) -0.017(5) -0.019(5) N9 0.035(4) 0.039(4) 0.051(4) 0.012(3) -0.023(3) -0.016(3) N6 0.058(5) 0.057(5) 0.040(4) 0.013(4) -0.027(4) -0.023(4) O1 0.034(3) 0.044(3) 0.076(4) 0.008(3) -0.030(3) -0.016(3) O2 0.040(3) 0.038(3) 0.042(3) -0.010(3) -0.006(3) -0.016(3) O3 0.050(3) 0.030(3) 0.037(3) -0.006(2) -0.018(3) 0.000(3) O4 0.078(5) 0.037(3) 0.071(4) 0.001(3) -0.052(4) -0.018(3) O5 0.029(3) 0.038(3) 0.049(3) 0.003(3) -0.010(3) 0.001(2) O6 0.041(3) 0.046(3) 0.038(3) -0.005(3) -0.005(3) -0.008(3) O7 0.067(4) 0.057(4) 0.035(3) -0.015(3) -0.013(3) 0.009(3) O8 0.059(4) 0.030(3) 0.055(4) 0.012(3) -0.005(3) -0.010(3) O9 0.043(3) 0.039(3) 0.037(3) -0.012(3) -0.008(3) -0.003(3) O10 0.053(4) 0.025(3) 0.036(3) -0.002(2) -0.005(3) -0.015(3) O11 0.039(4) 0.090(5) 0.072(5) -0.002(4) -0.032(3) -0.014(4) O12 0.048(3) 0.030(3) 0.038(3) -0.016(2) -0.008(3) -0.001(3) V1 0.0364(7) 0.0212(6) 0.0262(6) -0.0023(5) -0.0092(5) -0.0083(5) V2 0.0249(6) 0.0255(6) 0.0358(7) -0.0007(5) -0.0123(5) -0.0063(5) V3 0.0313(7) 0.0208(6) 0.0273(6) 0.0006(5) -0.0086(5) -0.0041(5) V4 0.0340(7) 0.0341(7) 0.0420(8) -0.0064(6) -0.0216(6) 0.0000(6) O1W 0.045(4) 0.056(4) 0.052(4) -0.005(3) -0.026(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 O6 2.437(6) 2_755 ? Ag1 O6 2.437(6) . ? Ag1 O9 2.459(6) . ? Ag1 O9 2.459(6) 2_755 ? Ag1 Ag2 3.0580(14) 2_755 ? Ag2 O10 2.195(5) 2_755 ? Ag2 O9 2.204(5) . ? Ag2 O7 2.536(7) 2_755 ? Ag3 N1 2.133(7) . ? Ag3 N3 2.138(7) . ? Ag3 O12 2.549(6) . ? Ag4 N6 2.123(7) . ? Ag4 N6 2.123(7) 2_666 ? Ag5 N7 2.091(7) . ? Ag5 N9 2.094(7) . ? C22 C23 1.341(13) . ? C22 N7 1.398(13) . ? C21 N7 1.309(11) . ? C21 N8 1.338(10) . ? C11 C12 1.343(14) . ? C11 N3 1.378(12) . ? C23 N8 1.350(11) . ? C24 N8 1.464(10) . ? C24 C25 1.522(11) . ? C13 C14 1.418(16) . ? C13 N4 1.487(13) . ? C15 C4 1.474(18) 1_645 ? C15 C14 1.604(17) . ? C8 N5 1.450(13) . ? C8 C9 1.498(14) . ? C4 C15 1.474(18) 1_465 ? C4 N2 1.491(16) . ? C25 C25 1.548(15) 2_845 ? C1 N1 1.312(12) . ? C1 N2 1.338(14) . ? N1 C2 1.365(12) . ? C3 N2 1.296(15) . ? C3 C2 1.347(14) . ? N5 C5 1.335(11) . ? N5 C7 1.362(14) . ? C19 N10 1.474(11) . ? C19 C20 1.516(13) . ? C7 C6 1.353(16) . ? C18 C17 1.341(12) . ? C18 N10 1.361(10) . ? C20 C20 1.513(18) 2_655 ? C16 N9 1.319(11) . ? C16 N10 1.336(11) . ? C17 N9 1.377(10) . ? C9 C9 1.53(2) 2_756 ? C10 N3 1.312(11) . ? C10 N4 1.334(12) . ? C12 N4 1.351(13) . ? C6 N6 1.355(12) . ? C5 N6 1.311(12) . ? O1 V2 1.620(5) . ? O2 V1 1.791(6) . ? O2 V2 1.793(5) . ? O3 V1 1.789(6) . ? O3 V4 1.810(5) . ? O4 V3 1.797(6) . ? O4 V4 1.812(7) . ? O5 V3 1.791(5) . ? O5 V2 1.815(6) . ? O6 V2 1.664(6) . ? O7 V4 1.642(6) . ? O7 Ag2 2.536(7) 2_755 ? O8 V3 1.619(6) . ? O9 V3 1.669(5) . ? O10 V1 1.669(5) . ? O10 Ag2 2.195(5) 2_755 ? O11 V4 1.618(6) . ? O12 V1 1.639(5) . ? 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 O6 Ag1 O6 180.0(2) 2_755 . ? O6 Ag1 O9 82.30(19) 2_755 . ? O6 Ag1 O9 97.70(19) . . ? O6 Ag1 O9 97.70(19) 2_755 2_755 ? O6 Ag1 O9 82.30(19) . 2_755 ? O9 Ag1 O9 180.0(3) . 2_755 ? O6 Ag1 Ag2 124.05(15) 2_755 2_755 ? O6 Ag1 Ag2 55.95(15) . 2_755 ? O9 Ag1 Ag2 134.49(13) . 2_755 ? O9 Ag1 Ag2 45.51(13) 2_755 2_755 ? O10 Ag2 O9 174.0(2) 2_755 . ? O10 Ag2 O7 91.6(2) 2_755 2_755 ? O9 Ag2 O7 94.3(2) . 2_755 ? N1 Ag3 N3 153.0(3) . . ? N1 Ag3 O12 99.9(2) . . ? N3 Ag3 O12 102.4(2) . . ? N6 Ag4 N6 180.000(1) . 2_666 ? N7 Ag5 N9 174.3(3) . . ? C23 C22 N7 109.2(8) . . ? N7 C21 N8 113.6(8) . . ? C12 C11 N3 108.3(8) . . ? C22 C23 N8 107.9(8) . . ? N8 C24 C25 111.8(7) . . ? C14 C13 N4 107.8(10) . . ? C4 C15 C14 105.6(10) 1_645 . ? C13 C14 C15 110.0(11) . . ? N5 C8 C9 112.9(9) . . ? C15 C4 N2 108.7(12) 1_465 . ? C24 C25 C25 113.2(8) . 2_845 ? N1 C1 N2 111.3(10) . . ? C1 N1 C2 103.4(8) . . ? C1 N1 Ag3 125.4(7) . . ? C2 N1 Ag3 129.9(6) . . ? N2 C3 C2 106.2(10) . . ? C5 N5 C7 106.2(9) . . ? C5 N5 C8 126.1(9) . . ? C7 N5 C8 127.7(9) . . ? N10 C19 C20 112.6(7) . . ? C6 C7 N5 107.2(9) . . ? C17 C18 N10 105.6(7) . . ? C20 C20 C19 114.1(9) 2_655 . ? N9 C16 N10 111.6(7) . . ? C18 C17 N9 110.8(8) . . ? C8 C9 C9 112.3(11) . 2_756 ? N3 C10 N4 110.6(9) . . ? C11 C12 N4 107.1(9) . . ? C7 C6 N6 108.6(10) . . ? N6 C5 N5 111.6(8) . . ? C10 N3 C11 106.2(8) . . ? C10 N3 Ag3 129.6(7) . . ? C11 N3 Ag3 123.9(6) . . ? C21 N7 C22 103.5(7) . . ? C21 N7 Ag5 128.8(6) . . ? C22 N7 Ag5 127.5(6) . . ? C21 N8 C23 105.8(7) . . ? C21 N8 C24 126.7(7) . . ? C23 N8 C24 127.5(7) . . ? C10 N4 C12 107.5(8) . . ? C10 N4 C13 124.4(9) . . ? C12 N4 C13 128.1(10) . . ? C3 N2 C1 108.6(9) . . ? C3 N2 C4 116.2(11) . . ? C1 N2 C4 133.0(11) . . ? C16 N10 C18 107.7(7) . . ? C16 N10 C19 127.9(7) . . ? C18 N10 C19 124.3(7) . . ? C3 C2 N1 110.4(10) . . ? C16 N9 C17 104.3(7) . . ? C16 N9 Ag5 131.0(6) . . ? C17 N9 Ag5 124.6(6) . . ? C5 N6 C6 106.4(8) . . ? C5 N6 Ag4 126.4(6) . . ? C6 N6 Ag4 125.7(7) . . ? V1 O2 V2 134.4(3) . . ? V1 O3 V4 132.2(3) . . ? V3 O4 V4 133.9(4) . . ? V3 O5 V2 137.6(3) . . ? V2 O6 Ag1 125.4(3) . . ? V4 O7 Ag2 129.2(3) . 2_755 ? V3 O9 Ag2 166.3(4) . . ? V3 O9 Ag1 111.1(3) . . ? Ag2 O9 Ag1 81.77(19) . . ? V1 O10 Ag2 118.7(3) . 2_755 ? V1 O12 Ag3 136.1(3) . . ? O12 V1 O10 109.7(3) . . ? O12 V1 O3 108.7(3) . . ? O10 V1 O3 109.4(3) . . ? O12 V1 O2 109.1(3) . . ? O10 V1 O2 110.7(3) . . ? O3 V1 O2 109.3(3) . . ? O1 V2 O6 109.7(3) . . ? O1 V2 O2 109.3(3) . . ? O6 V2 O2 109.1(3) . . ? O1 V2 O5 108.8(3) . . ? O6 V2 O5 109.5(3) . . ? O2 V2 O5 110.4(3) . . ? O8 V3 O9 109.0(3) . . ? O8 V3 O5 108.6(3) . . ? O9 V3 O5 108.5(3) . . ? O8 V3 O4 109.7(3) . . ? O9 V3 O4 111.0(3) . . ? O5 V3 O4 110.0(3) . . ? O11 V4 O7 110.3(4) . . ? O11 V4 O3 108.9(3) . . ? O7 V4 O3 108.5(3) . . ? O11 V4 O4 108.7(4) . . ? O7 V4 O4 110.1(3) . . ? O3 V4 O4 110.3(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.244 _refine_diff_density_min -1.203 _refine_diff_density_rms 0.135