# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Lin, Shen' _publ_contact_author_email ShenLin@fjnu.edu.cn _publ_section_title ; Inorganic-Organic Hybrid Compounds Based on Molybdenum Oxide Chains and Tetrazolate-Bridged Polymeric Silver Cations ; loop_ _publ_author_name 'Ming-Xing Yang' 'Lijuan Chen' 'Shen Lin' 'Xiao-Hua Chen' 'Hua Huang' # Attachment '- 1-3.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 768263' #TrackingRef '- 1-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H8 Ag4 Mo3 N10 O10' _chemical_formula_sum 'C12 H8 Ag4 Mo3 N10 O10' _chemical_formula_weight 1171.58 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.541(3) _cell_length_b 12.107(5) _cell_length_c 13.226(5) _cell_angle_alpha 79.300(10) _cell_angle_beta 77.552(12) _cell_angle_gamma 87.280(12) _cell_volume 1158.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3275 _cell_measurement_theta_min 3.1978 _cell_measurement_theta_max 27.3948 _exptl_crystal_description Prism _exptl_crystal_colour white _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 4.954 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3180 _exptl_absorpt_correction_T_max 0.7898 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2002)' _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 'Rigaku Mercury CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7322 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3870 _reflns_number_gt 3438 _reflns_threshold_expression >2sigma(I) _computing_data_collection '(CrystalClear; Rigaku, 2002)' _computing_cell_refinement '(CrystalClear; Rigaku, 2002)' _computing_data_reduction '(CrystalClear; Rigaku, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.4240P] 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 3870 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0669 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.56118(6) 0.15951(4) 0.34060(4) 0.02824(13) Uani 1 1 d . . . Ag2 Ag 0.78764(7) 0.46214(4) 0.39592(4) 0.03038(14) Uani 1 1 d . . . Ag3 Ag 0.86837(6) 0.38682(4) -0.34509(4) 0.02624(13) Uani 1 1 d . . . Ag4 Ag 1.19654(7) 0.32351(4) 0.18742(4) 0.03166(14) Uani 1 1 d . . . Mo1 Mo 0.71108(6) 0.37930(4) 0.13463(3) 0.01292(12) Uani 1 1 d . . . Mo2 Mo 1.02645(6) 0.39310(4) -0.08431(3) 0.01131(12) Uani 1 1 d . . . Mo3 Mo 0.52355(6) 0.38624(4) -0.07158(3) 0.01225(12) Uani 1 1 d . . . O1 O 1.0546(5) 0.2513(3) -0.0682(3) 0.0246(9) Uani 1 1 d . . . O2 O 0.4710(5) 0.2503(3) -0.0147(3) 0.0236(9) Uani 1 1 d . . . O3 O 0.6743(5) 0.4048(3) 0.2626(3) 0.0215(9) Uani 1 1 d . . . O4 O 0.6105(5) 0.3799(3) -0.2013(3) 0.0225(9) Uani 1 1 d . . . O5 O 0.6997(5) 0.2359(3) 0.1495(3) 0.0243(9) Uani 1 1 d . . . O6 O 1.2717(4) 0.4305(3) -0.0803(3) 0.0150(8) Uani 1 1 d . . . O7 O 1.0283(5) 0.4314(3) -0.2181(3) 0.0212(9) Uani 1 1 d . . . O8 O 0.9695(4) 0.4105(3) 0.0833(3) 0.0134(8) Uani 1 1 d . . . O9 O 0.7639(4) 0.3994(3) -0.0389(3) 0.0135(8) Uani 1 1 d . . . O10 O 0.4798(4) 0.4267(3) 0.0932(3) 0.0136(8) Uani 1 1 d . . . N1 N 1.1430(6) -0.2459(4) 0.4299(4) 0.0212(11) Uani 1 1 d . . . N2 N 1.1831(6) -0.2788(4) 0.5255(4) 0.0218(11) Uani 1 1 d . . . N3 N 1.2157(7) -0.1877(4) 0.5619(4) 0.0264(12) Uani 1 1 d . . . N4 N 1.1981(7) -0.0952(4) 0.4894(4) 0.0281(12) Uani 1 1 d . . . N5 N 1.1500(7) 0.1292(4) 0.2101(4) 0.0325(13) Uani 1 1 d . . . N6 N 0.7576(6) -0.3978(4) 0.4919(4) 0.0213(11) Uani 1 1 d . . . N7 N 0.7889(6) -0.4321(4) 0.5906(4) 0.0224(11) Uani 1 1 d . . . N8 N 0.7411(6) -0.3514(4) 0.6461(3) 0.0197(11) Uani 1 1 d . . . N9 N 0.6779(6) -0.2629(4) 0.5859(4) 0.0226(11) Uani 1 1 d . . . N10 N 0.6220(7) -0.0183(4) 0.3178(4) 0.0252(11) Uani 1 1 d . . . C1 C 1.1544(7) -0.1326(5) 0.4098(4) 0.0205(13) Uani 1 1 d . . . C2 C 1.1356(7) -0.0598(5) 0.3091(5) 0.0214(13) Uani 1 1 d . . . C3 C 1.1487(8) 0.0573(5) 0.2997(5) 0.0243(13) Uani 1 1 d . . . H3A H 1.1569 0.0861 0.3590 0.029 Uiso 1 1 calc R . . C4 C 1.1359(11) 0.0862(6) 0.1261(6) 0.050(2) Uani 1 1 d . . . H4A H 1.1425 0.1349 0.0622 0.060 Uiso 1 1 calc R . . C5 C 1.1118(13) -0.0277(6) 0.1294(6) 0.060(3) Uani 1 1 d . . . H5A H 1.0942 -0.0536 0.0704 0.072 Uiso 1 1 calc R . . C6 C 1.1147(10) -0.1009(6) 0.2217(5) 0.0428(19) Uani 1 1 d . . . H6A H 1.1026 -0.1777 0.2253 0.051 Uiso 1 1 calc R . . C7 C 0.6921(7) -0.2919(4) 0.4907(4) 0.0162(12) Uani 1 1 d . . . C8 C 0.6550(7) -0.2123(4) 0.3985(4) 0.0177(12) Uani 1 1 d . . . C9 C 0.6516(8) -0.0972(5) 0.3987(5) 0.0240(13) Uani 1 1 d . . . H9A H 0.6710 -0.0735 0.4584 0.029 Uiso 1 1 calc R . . C10 C 0.5991(8) -0.0539(5) 0.2307(5) 0.0276(14) Uani 1 1 d . . . H10A H 0.5800 -0.0005 0.1737 0.033 Uiso 1 1 calc R . . C11 C 0.6028(8) -0.1659(5) 0.2223(5) 0.0293(15) Uani 1 1 d . . . H11A H 0.5887 -0.1872 0.1605 0.035 Uiso 1 1 calc R . . C12 C 0.6277(8) -0.2460(5) 0.3074(4) 0.0237(13) Uani 1 1 d . . . H12A H 0.6263 -0.3220 0.3042 0.028 Uiso 1 1 calc 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 0.0430(3) 0.0188(3) 0.0220(3) -0.00359(19) -0.0063(2) 0.0059(2) Ag2 0.0524(3) 0.0193(3) 0.0220(3) -0.00346(19) -0.0130(2) -0.0034(2) Ag3 0.0356(3) 0.0218(3) 0.0226(3) -0.00731(19) -0.0064(2) 0.00073(19) Ag4 0.0393(3) 0.0273(3) 0.0286(3) 0.0045(2) -0.0139(2) -0.0085(2) Mo1 0.0124(2) 0.0160(3) 0.0101(2) 0.00101(19) -0.00393(18) -0.00243(18) Mo2 0.0088(2) 0.0146(2) 0.0116(2) -0.00304(18) -0.00366(18) -0.00085(17) Mo3 0.0093(2) 0.0157(3) 0.0136(2) -0.00460(19) -0.00482(19) 0.00001(17) O1 0.026(2) 0.018(2) 0.033(2) -0.0084(18) -0.0098(19) -0.0002(16) O2 0.022(2) 0.022(2) 0.029(2) -0.0035(18) -0.0093(18) -0.0063(16) O3 0.020(2) 0.033(2) 0.013(2) -0.0031(17) -0.0077(16) -0.0054(17) O4 0.0163(19) 0.032(2) 0.020(2) -0.0091(18) -0.0009(17) -0.0019(16) O5 0.027(2) 0.018(2) 0.027(2) 0.0006(17) -0.0051(18) -0.0035(16) O6 0.0119(18) 0.017(2) 0.0167(19) -0.0033(16) -0.0026(15) -0.0026(14) O7 0.0177(19) 0.033(2) 0.015(2) -0.0048(17) -0.0070(16) -0.0037(16) O8 0.0060(16) 0.021(2) 0.0137(19) 0.0001(15) -0.0066(14) -0.0003(14) O9 0.0079(17) 0.021(2) 0.0136(19) -0.0033(16) -0.0054(15) -0.0006(14) O10 0.0114(17) 0.017(2) 0.0133(19) -0.0027(15) -0.0037(15) -0.0036(14) N1 0.027(3) 0.019(3) 0.018(3) 0.000(2) -0.008(2) -0.001(2) N2 0.031(3) 0.019(3) 0.016(3) -0.003(2) -0.007(2) -0.005(2) N3 0.041(3) 0.023(3) 0.019(3) -0.004(2) -0.013(2) 0.000(2) N4 0.044(3) 0.019(3) 0.024(3) 0.001(2) -0.014(2) -0.004(2) N5 0.045(3) 0.019(3) 0.033(3) 0.009(2) -0.017(3) -0.006(2) N6 0.031(3) 0.020(3) 0.017(3) -0.007(2) -0.010(2) 0.005(2) N7 0.033(3) 0.018(3) 0.017(3) -0.003(2) -0.006(2) 0.002(2) N8 0.028(3) 0.013(2) 0.017(2) 0.000(2) -0.005(2) 0.0025(19) N9 0.032(3) 0.017(3) 0.020(3) -0.007(2) -0.007(2) 0.004(2) N10 0.039(3) 0.017(3) 0.019(3) -0.003(2) -0.006(2) 0.003(2) C1 0.024(3) 0.015(3) 0.022(3) -0.001(2) -0.005(3) -0.003(2) C2 0.022(3) 0.018(3) 0.025(3) 0.003(2) -0.011(3) -0.002(2) C3 0.028(3) 0.022(3) 0.026(3) -0.004(3) -0.012(3) 0.000(2) C4 0.083(6) 0.033(4) 0.038(4) 0.016(3) -0.041(4) -0.016(4) C5 0.123(8) 0.035(5) 0.036(4) 0.004(4) -0.050(5) -0.021(5) C6 0.079(5) 0.026(4) 0.031(4) -0.002(3) -0.029(4) -0.006(3) C7 0.015(3) 0.018(3) 0.016(3) -0.005(2) -0.002(2) -0.002(2) C8 0.019(3) 0.015(3) 0.019(3) -0.004(2) -0.005(2) 0.001(2) C9 0.038(3) 0.020(3) 0.018(3) -0.003(2) -0.015(3) 0.005(3) C10 0.041(4) 0.022(3) 0.021(3) 0.000(3) -0.012(3) 0.002(3) C11 0.042(4) 0.025(3) 0.026(3) -0.012(3) -0.012(3) 0.003(3) C12 0.034(3) 0.018(3) 0.022(3) -0.005(2) -0.010(3) 0.004(2) _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 N10 2.241(5) . ? Ag1 N9 2.290(5) 2_656 ? Ag1 N3 2.401(5) 2_756 ? Ag1 O5 2.534(4) . ? Ag2 N6 2.275(5) 1_565 ? Ag2 N2 2.292(5) 2_756 ? Ag2 O3 2.342(4) . ? Ag2 O7 2.600(4) 2_765 ? Ag2 Ag3 3.1252(12) 2_765 ? Ag3 N1 2.223(5) 2_755 ? Ag3 N7 2.300(5) 1_564 ? Ag3 O4 2.401(4) . ? Ag3 O7 2.416(4) . ? Ag3 Ag2 3.1252(12) 2_765 ? Ag4 N5 2.349(5) . ? Ag4 N8 2.434(5) 2_756 ? Ag4 O10 2.491(3) 1_655 ? Ag4 O8 2.498(3) . ? Mo1 O5 1.714(4) . ? Mo1 O3 1.738(4) . ? Mo1 O8 1.951(3) . ? Mo1 O10 1.968(3) . ? Mo1 O9 2.212(4) . ? Mo1 O6 2.282(4) 2_765 ? Mo2 O1 1.699(4) . ? Mo2 O7 1.741(4) . ? Mo2 O6 1.939(3) . ? Mo2 O9 1.943(3) . ? Mo2 O8 2.213(4) . ? Mo2 O8 2.383(4) 2_765 ? Mo3 O2 1.704(4) . ? Mo3 O4 1.715(4) . ? Mo3 O6 1.971(3) 1_455 ? Mo3 O9 1.972(3) . ? Mo3 O10 2.229(4) 2_665 ? Mo3 O10 2.274(4) . ? N1 N2 1.348(6) . ? N1 C1 1.351(7) . ? N2 N3 1.335(6) . ? N3 N4 1.354(7) . ? N4 C1 1.328(7) . ? N5 C3 1.333(7) . ? N5 C4 1.337(9) . ? N6 C7 1.351(7) . ? N6 N7 1.363(6) . ? N7 N8 1.320(6) . ? N8 N9 1.345(6) . ? N9 C7 1.350(7) . ? N9 Ag1 2.290(5) 2_656 ? N10 C9 1.346(7) . ? N10 C10 1.349(8) . ? C1 C2 1.484(8) . ? C2 C6 1.382(9) . ? C2 C3 1.407(8) . ? C3 H3A 0.9300 . ? C4 C5 1.390(10) . ? C4 H4A 0.9300 . ? C5 C6 1.372(9) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.477(7) . ? C8 C9 1.392(8) . ? C8 C12 1.399(8) . ? C9 H9A 0.9300 . ? C10 C11 1.379(8) . ? C10 H10A 0.9300 . ? C11 C12 1.382(8) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? 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 N10 Ag1 N9 138.56(18) . 2_656 ? N10 Ag1 N3 101.07(17) . 2_756 ? N9 Ag1 N3 101.20(17) 2_656 2_756 ? N10 Ag1 O5 92.00(15) . . ? N9 Ag1 O5 114.63(15) 2_656 . ? N3 Ag1 O5 105.85(15) 2_756 . ? N6 Ag2 N2 120.42(17) 1_565 2_756 ? N6 Ag2 O3 141.17(15) 1_565 . ? N2 Ag2 O3 90.85(15) 2_756 . ? N6 Ag2 O7 99.32(15) 1_565 2_765 ? N2 Ag2 O7 128.58(14) 2_756 2_765 ? O3 Ag2 O7 73.25(12) . 2_765 ? N6 Ag2 Ag3 66.71(12) 1_565 2_765 ? N2 Ag2 Ag3 117.08(12) 2_756 2_765 ? O3 Ag2 Ag3 121.61(9) . 2_765 ? O7 Ag2 Ag3 48.88(8) 2_765 2_765 ? N1 Ag3 N7 122.17(17) 2_755 1_564 ? N1 Ag3 O4 109.89(15) 2_755 . ? N7 Ag3 O4 89.34(15) 1_564 . ? N1 Ag3 O7 137.72(15) 2_755 . ? N7 Ag3 O7 97.21(15) 1_564 . ? O4 Ag3 O7 83.03(13) . . ? N1 Ag3 Ag2 121.10(12) 2_755 2_765 ? N7 Ag3 Ag2 71.40(12) 1_564 2_765 ? O4 Ag3 Ag2 128.32(10) . 2_765 ? O7 Ag3 Ag2 54.14(9) . 2_765 ? N5 Ag4 N8 104.57(17) . 2_756 ? N5 Ag4 O10 126.44(16) . 1_655 ? N8 Ag4 O10 89.38(14) 2_756 1_655 ? N5 Ag4 O8 104.41(15) . . ? N8 Ag4 O8 132.31(13) 2_756 . ? O10 Ag4 O8 102.61(11) 1_655 . ? O5 Mo1 O3 104.26(19) . . ? O5 Mo1 O8 103.67(16) . . ? O3 Mo1 O8 102.23(16) . . ? O5 Mo1 O10 101.60(17) . . ? O3 Mo1 O10 102.73(16) . . ? O8 Mo1 O10 138.51(14) . . ? O5 Mo1 O9 92.04(16) . . ? O3 Mo1 O9 163.70(16) . . ? O8 Mo1 O9 73.28(13) . . ? O10 Mo1 O9 73.47(13) . . ? O5 Mo1 O6 168.56(16) . 2_765 ? O3 Mo1 O6 87.07(16) . 2_765 ? O8 Mo1 O6 74.86(13) . 2_765 ? O10 Mo1 O6 73.91(13) . 2_765 ? O9 Mo1 O6 76.64(13) . 2_765 ? O1 Mo2 O7 102.95(19) . . ? O1 Mo2 O6 97.53(16) . . ? O7 Mo2 O6 101.38(16) . . ? O1 Mo2 O9 98.95(16) . . ? O7 Mo2 O9 95.32(16) . . ? O6 Mo2 O9 153.21(16) . . ? O1 Mo2 O8 98.57(16) . . ? O7 Mo2 O8 157.07(16) . . ? O6 Mo2 O8 83.38(13) . . ? O9 Mo2 O8 73.40(13) . . ? O1 Mo2 O8 168.08(16) . 2_765 ? O7 Mo2 O8 85.99(16) . 2_765 ? O6 Mo2 O8 72.70(13) . 2_765 ? O9 Mo2 O8 87.89(13) . 2_765 ? O8 Mo2 O8 73.93(14) . 2_765 ? O2 Mo3 O4 104.05(19) . . ? O2 Mo3 O6 94.54(16) . 1_455 ? O4 Mo3 O6 99.33(16) . 1_455 ? O2 Mo3 O9 101.22(16) . . ? O4 Mo3 O9 93.94(16) . . ? O6 Mo3 O9 156.29(15) 1_455 . ? O2 Mo3 O10 159.08(16) . 2_665 ? O4 Mo3 O10 95.64(16) . 2_665 ? O6 Mo3 O10 75.08(13) 1_455 2_665 ? O9 Mo3 O10 84.18(13) . 2_665 ? O2 Mo3 O10 87.86(16) . . ? O4 Mo3 O10 163.32(15) . . ? O6 Mo3 O10 91.19(13) 1_455 . ? O9 Mo3 O10 72.00(13) . . ? O10 Mo3 O10 74.48(14) 2_665 . ? Mo1 O3 Ag2 149.1(2) . . ? Mo3 O4 Ag3 149.3(2) . . ? Mo1 O5 Ag1 108.02(18) . . ? Mo2 O6 Mo3 151.0(2) . 1_655 ? Mo2 O6 Mo1 104.77(15) . 2_765 ? Mo3 O6 Mo1 103.32(14) 1_655 2_765 ? Mo2 O7 Ag3 138.8(2) . . ? Mo2 O7 Ag2 143.69(19) . 2_765 ? Ag3 O7 Ag2 76.98(11) . 2_765 ? Mo1 O8 Mo2 105.13(15) . . ? Mo1 O8 Mo2 100.79(14) . 2_765 ? Mo2 O8 Mo2 106.07(14) . 2_765 ? Mo1 O8 Ag4 120.81(16) . . ? Mo2 O8 Ag4 116.25(14) . . ? Mo2 O8 Ag4 105.82(13) 2_765 . ? Mo2 O9 Mo3 148.1(2) . . ? Mo2 O9 Mo1 105.43(15) . . ? Mo3 O9 Mo1 104.79(14) . . ? Mo1 O10 Mo3 105.36(15) . 2_665 ? Mo1 O10 Mo3 102.71(14) . . ? Mo3 O10 Mo3 105.52(14) 2_665 . ? Mo1 O10 Ag4 119.54(16) . 1_455 ? Mo3 O10 Ag4 118.45(14) 2_665 1_455 ? Mo3 O10 Ag4 103.21(13) . 1_455 ? N2 N1 C1 105.6(5) . . ? N2 N1 Ag3 113.6(3) . 2_755 ? C1 N1 Ag3 139.4(4) . 2_755 ? N3 N2 N1 108.7(4) . . ? N3 N2 Ag2 126.4(4) . 2_756 ? N1 N2 Ag2 124.7(3) . 2_756 ? N2 N3 N4 108.9(5) . . ? N2 N3 Ag1 129.6(4) . 2_756 ? N4 N3 Ag1 111.0(4) . 2_756 ? C1 N4 N3 105.9(5) . . ? C3 N5 C4 117.3(6) . . ? C3 N5 Ag4 124.3(4) . . ? C4 N5 Ag4 118.2(4) . . ? C7 N6 N7 104.9(4) . . ? C7 N6 Ag2 140.7(4) . 1_545 ? N7 N6 Ag2 113.5(3) . 1_545 ? N8 N7 N6 109.5(4) . . ? N8 N7 Ag3 126.0(3) . 1_546 ? N6 N7 Ag3 123.7(3) . 1_546 ? N7 N8 N9 109.2(4) . . ? N7 N8 Ag4 131.8(3) . 2_756 ? N9 N8 Ag4 117.6(3) . 2_756 ? N8 N9 C7 106.0(4) . . ? N8 N9 Ag1 119.7(3) . 2_656 ? C7 N9 Ag1 122.6(4) . 2_656 ? C9 N10 C10 117.3(5) . . ? C9 N10 Ag1 120.1(4) . . ? C10 N10 Ag1 121.6(4) . . ? N4 C1 N1 110.9(5) . . ? N4 C1 C2 124.1(5) . . ? N1 C1 C2 124.9(5) . . ? C6 C2 C3 117.7(5) . . ? C6 C2 C1 123.6(5) . . ? C3 C2 C1 118.6(5) . . ? N5 C3 C2 123.3(6) . . ? N5 C3 H3A 118.3 . . ? C2 C3 H3A 118.3 . . ? N5 C4 C5 123.4(6) . . ? N5 C4 H4A 118.3 . . ? C5 C4 H4A 118.3 . . ? C6 C5 C4 118.5(7) . . ? C6 C5 H5A 120.8 . . ? C4 C5 H5A 120.8 . . ? C5 C6 C2 119.7(7) . . ? C5 C6 H6A 120.2 . . ? C2 C6 H6A 120.2 . . ? N9 C7 N6 110.4(5) . . ? N9 C7 C8 122.7(5) . . ? N6 C7 C8 126.7(5) . . ? C9 C8 C12 117.0(5) . . ? C9 C8 C7 119.7(5) . . ? C12 C8 C7 123.3(5) . . ? N10 C9 C8 124.0(6) . . ? N10 C9 H9A 118.0 . . ? C8 C9 H9A 118.0 . . ? N10 C10 C11 123.0(6) . . ? N10 C10 H10A 118.5 . . ? C11 C10 H10A 118.5 . . ? C10 C11 C12 118.8(6) . . ? C10 C11 H11A 120.6 . . ? C12 C11 H11A 120.6 . . ? C11 C12 C8 119.8(6) . . ? C11 C12 H12A 120.1 . . ? C8 C12 H12A 120.1 . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.006 _refine_diff_density_min -1.289 _refine_diff_density_rms 0.150 data_2 _database_code_depnum_ccdc_archive 'CCDC 768264' #TrackingRef '- 1-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H8 Ag4 Mo4 N10 O13' _chemical_formula_sum 'C12 H8 Ag4 Mo4 N10 O13' _chemical_formula_weight 1315.52 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.623(3) _cell_length_b 11.188(4) _cell_length_c 12.212(4) _cell_angle_alpha 71.944(7) _cell_angle_beta 88.358(9) _cell_angle_gamma 88.491(7) _cell_volume 1249.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3263 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 24.99 _exptl_crystal_description prism _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 5.091 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6939 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2002)' _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 'Rigaku Mercury CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8005 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4212 _reflns_number_gt 3511 _reflns_threshold_expression >2sigma(I) _computing_data_collection '(CrystalClear; Rigaku, 2002)' _computing_cell_refinement '(CrystalClear; Rigaku, 2002)' _computing_data_reduction '(CrystalClear; Rigaku, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4212 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0619 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Mo1 Mo 0.32888(4) 0.91883(4) 0.18530(4) 0.01145(11) Uani 1 1 d . . . Mo2 Mo 0.30405(4) 1.10992(4) -0.09318(4) 0.01117(11) Uani 1 1 d . . . Mo3 Mo 0.09100(4) 0.85670(4) 0.02765(4) 0.01076(11) Uani 1 1 d . . . Mo4 Mo 0.05640(4) 1.06256(4) -0.25108(4) 0.01162(11) Uani 1 1 d . . . Ag1 Ag 0.81642(4) 0.98886(4) 0.54250(4) 0.02479(12) Uani 1 1 d . . . Ag2 Ag 0.57869(4) 0.99892(4) 0.36030(4) 0.02394(12) Uani 1 1 d . . . Ag3 Ag 0.53573(5) 0.59501(4) 0.34156(4) 0.03163(13) Uani 1 1 d . . . Ag4 Ag 0.84843(5) 0.38672(4) 0.57553(4) 0.03439(14) Uani 1 1 d . . . O2 O 0.2793(3) 0.8955(3) 0.0171(3) 0.0139(7) Uani 1 1 d . . . O3 O 0.0500(3) 0.8668(3) -0.1132(3) 0.0157(8) Uani 1 1 d . . . O4 O 0.3375(4) 0.7623(3) 0.2619(3) 0.0232(9) Uani 1 1 d . . . O5 O 0.4836(3) 1.0668(3) -0.1264(3) 0.0183(8) Uani 1 1 d . . . O6 O 0.1258(3) 0.9308(3) 0.1714(3) 0.0134(7) Uani 1 1 d . . . O7 O 0.2459(3) 1.0406(3) -0.2239(3) 0.0153(8) Uani 1 1 d . . . O8 O 0.0897(4) 0.7013(3) 0.0999(3) 0.0223(8) Uani 1 1 d . . . O9 O 0.0480(4) 1.2177(3) -0.3306(3) 0.0212(8) Uani 1 1 d . . . O10 O 0.2995(4) 1.2655(3) -0.1650(3) 0.0220(8) Uani 1 1 d . . . O11 O 0.3169(3) 1.1083(3) 0.0507(3) 0.0155(8) Uani 1 1 d . . . O12 O 0.3441(3) 0.9938(3) 0.2882(3) 0.0216(8) Uani 1 1 d . . . O13 O 0.0192(4) 0.9867(3) -0.3499(3) 0.0207(8) Uani 1 1 d . . . N1 N 0.7480(4) 0.7965(4) 0.5395(4) 0.0198(10) Uani 1 1 d . . . N2 N 0.6476(4) 0.7998(4) 0.4639(4) 0.0197(10) Uani 1 1 d . . . N3 N 0.6362(5) 0.6864(4) 0.4544(4) 0.0216(10) Uani 1 1 d . . . N4 N 0.7285(5) 0.6079(4) 0.5229(4) 0.0226(10) Uani 1 1 d . . . N5 N 0.9645(4) 0.5156(4) 0.6524(4) 0.0200(10) Uani 1 1 d . . . N6 N 0.6455(5) 0.3768(4) 0.3929(4) 0.0239(11) Uani 1 1 d . . . N7 N 0.7289(5) 0.2954(4) 0.4677(4) 0.0222(10) Uani 1 1 d . . . N8 N 0.7208(5) 0.1827(4) 0.4548(4) 0.0206(10) Uani 1 1 d . . . N9 N 0.6299(4) 0.1894(4) 0.3701(4) 0.0187(10) Uani 1 1 d . . . N10 N 0.4560(5) 0.4905(4) 0.2256(4) 0.0242(11) Uani 1 1 d . . . C1 C 0.7955(5) 0.6784(5) 0.5735(4) 0.0172(12) Uani 1 1 d . . . C2 C 0.9075(5) 0.6276(5) 0.6542(5) 0.0205(12) Uani 1 1 d . . . C3 C 1.0708(5) 0.4675(5) 0.7221(5) 0.0222(12) Uani 1 1 d . . . H3A H 1.1105 0.3912 0.7207 0.027 Uiso 1 1 calc R . . C4 C 1.1240(6) 0.5255(5) 0.7954(5) 0.0312(14) Uani 1 1 d . . . H4A H 1.1990 0.4897 0.8414 0.037 Uiso 1 1 calc R . . C5 C 1.0651(7) 0.6371(6) 0.7999(6) 0.0419(18) Uani 1 1 d . . . H5A H 1.0971 0.6767 0.8508 0.050 Uiso 1 1 calc R . . C6 C 0.9575(7) 0.6890(5) 0.7274(5) 0.0326(15) Uani 1 1 d . . . H6A H 0.9180 0.7658 0.7275 0.039 Uiso 1 1 calc R . . C7 C 0.5868(5) 0.3092(5) 0.3344(5) 0.0186(12) Uani 1 1 d . . . C8 C 0.4917(5) 0.3683(5) 0.2395(5) 0.0210(12) Uani 1 1 d . . . C9 C 0.3709(7) 0.5489(6) 0.1403(5) 0.0392(17) Uani 1 1 d . . . H9A H 0.3482 0.6330 0.1294 0.047 Uiso 1 1 calc R . . C10 C 0.3149(7) 0.4914(6) 0.0673(6) 0.0456(19) Uani 1 1 d . . . H10A H 0.2538 0.5348 0.0102 0.055 Uiso 1 1 calc R . . C11 C 0.3519(8) 0.3681(6) 0.0812(6) 0.053(2) Uani 1 1 d . . . H11A H 0.3177 0.3272 0.0323 0.064 Uiso 1 1 calc R . . C12 C 0.4408(7) 0.3051(5) 0.1693(5) 0.0384(17) Uani 1 1 d . . . H12A H 0.4656 0.2213 0.1806 0.046 Uiso 1 1 calc R . . O1 O 0.0913(3) 1.0848(3) -0.0751(3) 0.0123(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0073(2) 0.0157(2) 0.0110(2) -0.00346(19) -0.00240(17) -0.00026(17) Mo2 0.0067(2) 0.0139(2) 0.0123(2) -0.00305(19) -0.00185(18) -0.00154(17) Mo3 0.0075(2) 0.0119(2) 0.0139(2) -0.00533(19) -0.00097(18) -0.00061(17) Mo4 0.0081(2) 0.0159(2) 0.0114(2) -0.00480(19) -0.00191(17) -0.00055(17) Ag1 0.0280(2) 0.0215(2) 0.0266(3) -0.0094(2) -0.0102(2) 0.00248(18) Ag2 0.0250(2) 0.0196(2) 0.0292(3) -0.0101(2) -0.00852(19) 0.00289(18) Ag3 0.0413(3) 0.0235(3) 0.0353(3) -0.0154(2) -0.0182(2) 0.0027(2) Ag4 0.0424(3) 0.0259(3) 0.0406(3) -0.0170(2) -0.0182(2) -0.0015(2) O2 0.0088(16) 0.0174(19) 0.0162(19) -0.0061(16) 0.0002(15) -0.0002(14) O3 0.0162(18) 0.0180(19) 0.0142(19) -0.0067(16) -0.0023(15) -0.0006(15) O4 0.022(2) 0.022(2) 0.022(2) -0.0027(17) -0.0026(17) 0.0009(16) O5 0.0060(16) 0.029(2) 0.0175(19) -0.0038(16) -0.0040(15) 0.0020(15) O6 0.0082(16) 0.0184(19) 0.0154(18) -0.0075(15) -0.0047(14) 0.0013(14) O7 0.0092(16) 0.0205(19) 0.0171(19) -0.0072(16) -0.0024(15) 0.0022(14) O8 0.0194(19) 0.015(2) 0.029(2) -0.0010(17) 0.0003(17) 0.0049(15) O9 0.0208(19) 0.019(2) 0.020(2) -0.0005(17) -0.0020(17) -0.0023(16) O10 0.0187(19) 0.018(2) 0.026(2) -0.0025(17) -0.0052(17) 0.0023(16) O11 0.0119(17) 0.0172(19) 0.0185(19) -0.0067(16) -0.0044(15) -0.0013(14) O12 0.0180(19) 0.034(2) 0.019(2) -0.0158(18) -0.0011(16) -0.0031(17) O13 0.0197(19) 0.026(2) 0.019(2) -0.0109(17) -0.0028(16) -0.0009(16) N1 0.022(2) 0.016(2) 0.023(3) -0.008(2) -0.004(2) -0.0011(19) N2 0.022(2) 0.018(2) 0.020(3) -0.006(2) -0.002(2) -0.0021(19) N3 0.030(3) 0.017(2) 0.019(2) -0.006(2) -0.004(2) -0.005(2) N4 0.030(3) 0.019(2) 0.018(3) -0.006(2) -0.010(2) 0.008(2) N5 0.026(2) 0.016(2) 0.018(2) -0.005(2) -0.005(2) -0.002(2) N6 0.031(3) 0.020(3) 0.020(3) -0.005(2) -0.008(2) 0.000(2) N7 0.031(3) 0.017(2) 0.022(3) -0.010(2) -0.008(2) 0.001(2) N8 0.028(3) 0.015(2) 0.019(2) -0.005(2) -0.004(2) -0.001(2) N9 0.021(2) 0.016(2) 0.019(2) -0.004(2) -0.008(2) -0.0016(19) N10 0.031(3) 0.017(2) 0.027(3) -0.009(2) -0.015(2) 0.006(2) C1 0.024(3) 0.013(3) 0.014(3) -0.004(2) 0.003(2) -0.003(2) C2 0.025(3) 0.015(3) 0.018(3) -0.001(2) -0.005(2) 0.004(2) C3 0.021(3) 0.017(3) 0.027(3) -0.005(3) -0.007(3) 0.004(2) C4 0.037(3) 0.028(3) 0.030(4) -0.010(3) -0.019(3) 0.006(3) C5 0.062(5) 0.029(4) 0.044(4) -0.023(3) -0.032(4) 0.012(3) C6 0.050(4) 0.015(3) 0.038(4) -0.014(3) -0.021(3) 0.009(3) C7 0.018(3) 0.017(3) 0.021(3) -0.007(2) 0.001(2) 0.000(2) C8 0.024(3) 0.020(3) 0.020(3) -0.006(2) -0.003(2) 0.001(2) C9 0.052(4) 0.028(4) 0.045(4) -0.022(3) -0.029(4) 0.020(3) C10 0.065(5) 0.033(4) 0.046(4) -0.020(3) -0.040(4) 0.017(3) C11 0.084(6) 0.037(4) 0.052(5) -0.029(4) -0.046(4) 0.018(4) C12 0.064(5) 0.017(3) 0.037(4) -0.012(3) -0.032(4) 0.010(3) O1 0.0072(16) 0.0157(18) 0.0154(18) -0.0066(15) -0.0015(14) 0.0005(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O4 1.711(4) . ? Mo1 O12 1.724(3) . ? Mo1 O5 1.915(3) 2_675 ? Mo1 O6 1.964(3) . ? Mo1 O2 2.216(3) . ? Mo1 O11 2.247(3) . ? Mo2 O10 1.689(4) . ? Mo2 O11 1.759(3) . ? Mo2 O5 1.850(3) . ? Mo2 O1 2.070(3) . ? Mo2 O7 2.075(3) . ? Mo2 O2 2.374(3) . ? Mo3 O8 1.688(3) . ? Mo3 O3 1.745(3) . ? Mo3 O2 1.866(3) . ? Mo3 O1 1.990(3) 2_575 ? Mo3 O6 2.198(3) . ? Mo3 O1 2.471(3) . ? Mo4 O9 1.707(3) . ? Mo4 O13 1.726(3) . ? Mo4 O7 1.859(3) . ? Mo4 O6 1.991(3) 2_575 ? Mo4 O1 2.274(3) . ? Mo4 O3 2.313(3) . ? Ag1 N1 2.279(4) . ? Ag1 N8 2.282(4) 1_565 ? Ag1 O13 2.379(3) 1_656 ? Ag1 O12 2.598(3) 2_676 ? Ag1 Ag2 3.2126(10) . ? Ag2 N9 2.240(4) 1_565 ? Ag2 N2 2.286(4) . ? Ag2 O12 2.455(3) . ? Ag2 O7 2.465(3) 2_675 ? Ag3 N3 2.209(4) . ? Ag3 N10 2.258(4) . ? Ag3 N6 2.534(5) . ? Ag4 N7 2.255(4) . ? Ag4 N5 2.279(4) . ? Ag4 N4 2.603(4) . ? O5 Mo1 1.915(3) 2_675 ? O6 Mo4 1.991(3) 2_575 ? O7 Ag2 2.465(3) 2_675 ? O12 Ag1 2.598(3) 2_676 ? O13 Ag1 2.379(3) 1_454 ? N1 C1 1.329(6) . ? N1 N2 1.347(6) . ? N2 N3 1.317(6) . ? N3 N4 1.344(6) . ? N4 C1 1.331(6) . ? N5 C3 1.341(6) . ? N5 C2 1.360(6) . ? N6 C7 1.334(6) . ? N6 N7 1.340(6) . ? N7 N8 1.323(6) . ? N8 N9 1.357(6) . ? N8 Ag1 2.282(4) 1_545 ? N9 C7 1.333(6) . ? N9 Ag2 2.240(4) 1_545 ? N10 C9 1.335(7) . ? N10 C8 1.360(6) . ? C1 C2 1.462(7) . ? C2 C6 1.388(7) . ? C3 C4 1.375(7) . ? C3 H3A 0.9300 . ? C4 C5 1.374(8) . ? C4 H4A 0.9300 . ? C5 C6 1.377(8) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.474(7) . ? C8 C12 1.376(7) . ? C9 C10 1.378(7) . ? C9 H9A 0.9300 . ? C10 C11 1.375(8) . ? C10 H10A 0.9300 . ? C11 C12 1.392(8) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? O1 Mo3 1.990(3) 2_575 ? 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 O4 Mo1 O12 104.10(18) . . ? O4 Mo1 O5 97.09(16) . 2_675 ? O12 Mo1 O5 99.18(15) . 2_675 ? O4 Mo1 O6 96.58(15) . . ? O12 Mo1 O6 98.35(15) . . ? O5 Mo1 O6 154.39(14) 2_675 . ? O4 Mo1 O2 96.97(15) . . ? O12 Mo1 O2 157.97(15) . . ? O5 Mo1 O2 84.33(13) 2_675 . ? O6 Mo1 O2 72.57(12) . . ? O4 Mo1 O11 167.18(14) . . ? O12 Mo1 O11 88.68(15) . . ? O5 Mo1 O11 79.58(13) 2_675 . ? O6 Mo1 O11 82.31(13) . . ? O2 Mo1 O11 70.46(12) . . ? O10 Mo2 O11 102.11(16) . . ? O10 Mo2 O5 101.29(16) . . ? O11 Mo2 O5 101.85(15) . . ? O10 Mo2 O1 97.21(15) . . ? O11 Mo2 O1 91.83(14) . . ? O5 Mo2 O1 154.01(14) . . ? O10 Mo2 O7 99.62(16) . . ? O11 Mo2 O7 155.04(14) . . ? O5 Mo2 O7 85.67(14) . . ? O1 Mo2 O7 73.30(12) . . ? O10 Mo2 O2 172.12(14) . . ? O11 Mo2 O2 75.43(13) . . ? O5 Mo2 O2 86.57(13) . . ? O1 Mo2 O2 75.52(12) . . ? O7 Mo2 O2 81.38(12) . . ? O8 Mo3 O3 104.59(16) . . ? O8 Mo3 O2 103.59(16) . . ? O3 Mo3 O2 103.62(15) . . ? O8 Mo3 O1 102.06(15) . 2_575 ? O3 Mo3 O1 98.16(14) . 2_575 ? O2 Mo3 O1 140.64(13) . 2_575 ? O8 Mo3 O6 99.67(15) . . ? O3 Mo3 O6 155.28(14) . . ? O2 Mo3 O6 74.79(12) . . ? O1 Mo3 O6 71.85(12) 2_575 . ? O8 Mo3 O1 179.05(14) . . ? O3 Mo3 O1 76.19(13) . . ? O2 Mo3 O1 76.69(12) . . ? O1 Mo3 O1 77.24(13) 2_575 . ? O6 Mo3 O1 79.51(11) . . ? O9 Mo4 O13 103.10(17) . . ? O9 Mo4 O7 101.11(16) . . ? O13 Mo4 O7 107.13(15) . . ? O9 Mo4 O6 93.48(15) . 2_575 ? O13 Mo4 O6 103.52(15) . 2_575 ? O7 Mo4 O6 141.81(14) . 2_575 ? O9 Mo4 O1 98.89(14) . . ? O13 Mo4 O1 157.50(14) . . ? O7 Mo4 O1 72.76(12) . . ? O6 Mo4 O1 70.19(12) 2_575 . ? O9 Mo4 O3 168.30(14) . . ? O13 Mo4 O3 86.66(14) . . ? O7 Mo4 O3 81.78(13) . . ? O6 Mo4 O3 77.79(13) 2_575 . ? O1 Mo4 O3 70.97(11) . . ? N1 Ag1 N8 129.35(16) . 1_565 ? N1 Ag1 O13 115.03(14) . 1_656 ? N8 Ag1 O13 115.61(14) 1_565 1_656 ? N1 Ag1 O12 97.87(13) . 2_676 ? N8 Ag1 O12 81.75(14) 1_565 2_676 ? O13 Ag1 O12 91.56(11) 1_656 2_676 ? N1 Ag1 Ag2 65.80(11) . . ? N8 Ag1 Ag2 64.17(11) 1_565 . ? O13 Ag1 Ag2 170.22(9) 1_656 . ? O12 Ag1 Ag2 98.00(8) 2_676 . ? N9 Ag2 N2 132.95(15) 1_565 . ? N9 Ag2 O12 112.12(14) 1_565 . ? N2 Ag2 O12 109.42(14) . . ? N9 Ag2 O7 104.20(14) 1_565 2_675 ? N2 Ag2 O7 80.86(13) . 2_675 ? O12 Ag2 O7 110.09(11) . 2_675 ? N9 Ag2 Ag1 67.24(11) 1_565 . ? N2 Ag2 Ag1 65.96(10) . . ? O12 Ag2 Ag1 158.25(8) . . ? O7 Ag2 Ag1 90.54(8) 2_675 . ? N3 Ag3 N10 173.63(17) . . ? N3 Ag3 N6 104.82(15) . . ? N10 Ag3 N6 69.96(15) . . ? N7 Ag4 N5 168.07(16) . . ? N7 Ag4 N4 101.20(15) . . ? N5 Ag4 N4 69.40(15) . . ? Mo3 O2 Mo1 105.46(14) . . ? Mo3 O2 Mo2 108.65(14) . . ? Mo1 O2 Mo2 96.33(12) . . ? Mo3 O3 Mo4 117.86(16) . . ? Mo2 O5 Mo1 160.9(2) . 2_675 ? Mo1 O6 Mo4 146.26(18) . 2_575 ? Mo1 O6 Mo3 102.75(14) . . ? Mo4 O6 Mo3 108.05(14) 2_575 . ? Mo4 O7 Mo2 111.93(16) . . ? Mo4 O7 Ag2 124.74(16) . 2_675 ? Mo2 O7 Ag2 120.53(14) . 2_675 ? Mo2 O11 Mo1 116.79(16) . . ? Mo1 O12 Ag2 116.22(17) . . ? Mo1 O12 Ag1 133.22(17) . 2_676 ? Ag2 O12 Ag1 103.23(12) . 2_676 ? Mo4 O13 Ag1 131.56(18) . 1_454 ? C1 N1 N2 105.6(4) . . ? C1 N1 Ag1 138.1(3) . . ? N2 N1 Ag1 114.6(3) . . ? N3 N2 N1 108.6(4) . . ? N3 N2 Ag2 136.0(3) . . ? N1 N2 Ag2 113.7(3) . . ? N2 N3 N4 109.4(4) . . ? N2 N3 Ag3 138.7(4) . . ? N4 N3 Ag3 111.0(3) . . ? C1 N4 N3 105.2(4) . . ? C1 N4 Ag4 108.7(3) . . ? N3 N4 Ag4 145.4(3) . . ? C3 N5 C2 118.2(4) . . ? C3 N5 Ag4 118.7(3) . . ? C2 N5 Ag4 120.9(3) . . ? C7 N6 N7 105.0(4) . . ? C7 N6 Ag3 110.4(3) . . ? N7 N6 Ag3 143.8(3) . . ? N8 N7 N6 109.7(4) . . ? N8 N7 Ag4 137.5(3) . . ? N6 N7 Ag4 112.8(3) . . ? N7 N8 N9 108.6(4) . . ? N7 N8 Ag1 135.4(3) . 1_545 ? N9 N8 Ag1 116.0(3) . 1_545 ? C7 N9 N8 104.9(4) . . ? C7 N9 Ag2 141.9(3) . 1_545 ? N8 N9 Ag2 112.0(3) . 1_545 ? C9 N10 C8 118.0(5) . . ? C9 N10 Ag3 119.9(4) . . ? C8 N10 Ag3 122.1(4) . . ? N1 C1 N4 111.2(5) . . ? N1 C1 C2 126.6(5) . . ? N4 C1 C2 122.2(5) . . ? N5 C2 C6 120.6(5) . . ? N5 C2 C1 116.0(4) . . ? C6 C2 C1 123.3(5) . . ? N5 C3 C4 123.1(5) . . ? N5 C3 H3A 118.5 . . ? C4 C3 H3A 118.5 . . ? C5 C4 C3 119.2(5) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? C4 C5 C6 118.4(5) . . ? C4 C5 H5A 120.8 . . ? C6 C5 H5A 120.8 . . ? C5 C6 C2 120.5(5) . . ? C5 C6 H6A 119.8 . . ? C2 C6 H6A 119.8 . . ? N9 C7 N6 111.7(5) . . ? N9 C7 C8 127.1(4) . . ? N6 C7 C8 121.1(5) . . ? N10 C8 C12 121.6(5) . . ? N10 C8 C7 115.6(4) . . ? C12 C8 C7 122.8(5) . . ? N10 C9 C10 123.7(5) . . ? N10 C9 H9A 118.2 . . ? C10 C9 H9A 118.2 . . ? C11 C10 C9 118.1(6) . . ? C11 C10 H10A 121.0 . . ? C9 C10 H10A 121.0 . . ? C10 C11 C12 119.5(6) . . ? C10 C11 H11A 120.3 . . ? C12 C11 H11A 120.3 . . ? C8 C12 C11 119.1(5) . . ? C8 C12 H12A 120.4 . . ? C11 C12 H12A 120.4 . . ? Mo3 O1 Mo2 147.23(16) 2_575 . ? Mo3 O1 Mo4 105.27(13) 2_575 . ? Mo2 O1 Mo4 97.25(12) . . ? Mo3 O1 Mo3 102.76(13) 2_575 . ? Mo2 O1 Mo3 98.78(12) . . ? Mo4 O1 Mo3 94.56(11) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.931 _refine_diff_density_min -1.076 _refine_diff_density_rms 0.148 data_3 _database_code_depnum_ccdc_archive 'CCDC 768265' #TrackingRef '- 1-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H6 Ag4 Mo4 N12 O13' _chemical_formula_sum 'C10 H6 Ag4 Mo4 N12 O13' _chemical_formula_weight 1317.51 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.690(4) _cell_length_b 10.240(5) _cell_length_c 13.130(5) _cell_angle_alpha 102.000(2) _cell_angle_beta 93.610(4) _cell_angle_gamma 110.870(6) _cell_volume 1177.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3041 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.50 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.1500 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1219 _exptl_absorpt_coefficient_mu 5.405 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5846 _exptl_absorpt_correction_T_max 0.7236 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2002)' _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 'Rigaku Mercury CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7846 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4164 _reflns_number_gt 3526 _reflns_threshold_expression >2sigma(I) _computing_data_collection '(CrystalClear; Rigaku, 2002)' _computing_cell_refinement '(CrystalClear; Rigaku, 2002)' _computing_data_reduction '(CrystalClear; Rigaku, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+2.6955P] 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 4164 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.29563(7) 0.26643(8) 0.28797(5) 0.0428(2) Uani 1 1 d . . . Ag2 Ag 0.36389(7) -0.14566(7) 0.76282(5) 0.03575(18) Uani 1 1 d . . . Ag3 Ag 0.92661(7) 0.50974(7) 0.66956(5) 0.03809(19) Uani 1 1 d . . . Ag4 Ag 0.74076(7) 0.60097(7) 0.37188(5) 0.0410(2) Uani 1 1 d . . . Mo1 Mo 0.43414(6) 0.52771(6) 0.11873(4) 0.01142(14) Uani 1 1 d . . . Mo2 Mo 0.21659(6) 0.57438(6) -0.07857(4) 0.01294(14) Uani 1 1 d . . . Mo3 Mo 0.09372(6) 0.29337(6) 0.03947(4) 0.01349(15) Uani 1 1 d . . . Mo4 Mo 0.56227(6) 0.80076(6) -0.01060(4) 0.01324(15) Uani 1 1 d . . . O1 O 0.4285(5) 0.5572(5) -0.0579(3) 0.0139(9) Uani 1 1 d . . . O2 O 0.2460(5) 0.5288(5) 0.0873(3) 0.0141(9) Uani 1 1 d . . . O3 O 0.2989(5) 0.3043(5) 0.0303(3) 0.0157(10) Uani 1 1 d . . . O4 O 0.4388(5) 0.4953(5) 0.2412(3) 0.0222(11) Uani 1 1 d . . . O5 O 0.5480(5) 0.7095(5) 0.1381(3) 0.0173(10) Uani 1 1 d . . . O6 O 0.0636(5) 0.6278(5) -0.0406(4) 0.0227(11) Uani 1 1 d . . . O7 O 0.1290(5) 0.3835(5) -0.1010(3) 0.0177(10) Uani 1 1 d . . . O8 O 0.3638(5) 0.7702(5) 0.0009(3) 0.0163(10) Uani 1 1 d . . . O9 O 0.2264(5) 0.5969(5) -0.2042(4) 0.0224(11) Uani 1 1 d . . . O10 O -0.0060(5) 0.1258(5) -0.0355(4) 0.0278(12) Uani 1 1 d . . . O11 O 0.0939(5) 0.2796(5) 0.1675(4) 0.0258(11) Uani 1 1 d . . . O12 O 0.5686(5) 0.8307(5) -0.1353(4) 0.0232(11) Uani 1 1 d . . . O13 O 0.6652(5) 0.9638(5) 0.0744(4) 0.0263(11) Uani 1 1 d . . . N1 N 0.7711(6) 0.3036(6) 0.6975(4) 0.0174(12) Uani 1 1 d . . . N2 N 0.5594(6) 0.0519(6) 0.7307(4) 0.0218(13) Uani 1 1 d . . . N3 N 0.4738(7) 0.2376(7) 0.4846(5) 0.0332(16) Uani 1 1 d . . . N4 N 0.4893(7) 0.3220(7) 0.4183(5) 0.0341(16) Uani 1 1 d . . . N5 N 0.6209(7) 0.4294(7) 0.4468(5) 0.0281(15) Uani 1 1 d . . . N6 N 0.6923(7) 0.4175(7) 0.5316(5) 0.0280(15) Uani 1 1 d . . . N7 N -0.1014(6) -0.1908(6) 0.3446(4) 0.0210(13) Uani 1 1 d . . . N8 N 0.1056(6) 0.0650(6) 0.3160(4) 0.0213(13) Uani 1 1 d . . . N9 N 0.1911(7) -0.1189(6) 0.5627(5) 0.0251(14) Uani 1 1 d . . . N10 N 0.1755(6) -0.2072(6) 0.6266(4) 0.0220(13) Uani 1 1 d . . . N11 N 0.0482(7) -0.3173(7) 0.5968(5) 0.0247(14) Uani 1 1 d . . . N12 N -0.0222(7) -0.3045(7) 0.5105(5) 0.0288(15) Uani 1 1 d . . . C1 C 0.6344(8) 0.2361(7) 0.6372(5) 0.0189(15) Uani 1 1 d . . . C2 C 0.7975(8) 0.2428(7) 0.7741(5) 0.0215(15) Uani 1 1 d . . . H2A H 0.8892 0.2860 0.8178 0.026 Uiso 1 1 calc R . . C3 C 0.6930(7) 0.1181(7) 0.7905(5) 0.0183(14) Uani 1 1 d . . . H3B H 0.7166 0.0798 0.8443 0.022 Uiso 1 1 calc R . . C4 C 0.5318(8) 0.1130(8) 0.6554(5) 0.0255(16) Uani 1 1 d . . . H4A H 0.4388 0.0704 0.6133 0.031 Uiso 1 1 calc R . . C5 C 0.6002(8) 0.2991(7) 0.5532(5) 0.0213(15) Uani 1 1 d . . . C6 C 0.0322(7) -0.1206(7) 0.4077(5) 0.0171(14) Uani 1 1 d . . . C7 C -0.1300(9) -0.1290(8) 0.2679(5) 0.0254(16) Uani 1 1 d . . . H7B H -0.2218 -0.1714 0.2243 0.031 Uiso 1 1 calc R . . C8 C -0.0250(8) -0.0047(8) 0.2538(6) 0.0227(15) Uani 1 1 d . . . H8A H -0.0464 0.0322 0.1985 0.027 Uiso 1 1 calc R . . C9 C 0.1342(8) 0.0052(7) 0.3923(5) 0.0203(15) Uani 1 1 d . . . H9B H 0.2257 0.0500 0.4362 0.024 Uiso 1 1 calc R . . C10 C 0.0679(7) -0.1824(7) 0.4931(5) 0.0191(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0261(3) 0.0485(4) 0.0453(4) 0.0337(3) -0.0091(3) -0.0056(3) Ag2 0.0251(3) 0.0367(4) 0.0380(4) 0.0226(3) -0.0102(2) -0.0020(3) Ag3 0.0340(4) 0.0299(3) 0.0390(4) 0.0191(3) -0.0036(3) -0.0056(3) Ag4 0.0351(4) 0.0340(4) 0.0403(4) 0.0205(3) -0.0032(3) -0.0077(3) Mo1 0.0092(3) 0.0138(3) 0.0126(3) 0.0044(2) 0.0010(2) 0.0053(2) Mo2 0.0077(3) 0.0171(3) 0.0170(3) 0.0088(2) 0.0016(2) 0.0056(2) Mo3 0.0087(3) 0.0159(3) 0.0186(3) 0.0089(2) 0.0027(2) 0.0051(2) Mo4 0.0101(3) 0.0130(3) 0.0185(3) 0.0068(2) 0.0023(2) 0.0049(2) O1 0.012(2) 0.018(2) 0.017(2) 0.0075(18) 0.0055(17) 0.0089(19) O2 0.012(2) 0.016(2) 0.019(2) 0.0088(18) 0.0056(17) 0.0082(19) O3 0.009(2) 0.016(2) 0.022(2) 0.0067(19) 0.0018(18) 0.0045(18) O4 0.028(3) 0.025(3) 0.016(2) 0.008(2) 0.003(2) 0.011(2) O5 0.015(2) 0.017(2) 0.018(2) 0.0052(19) -0.0036(18) 0.0037(19) O6 0.013(2) 0.023(3) 0.039(3) 0.016(2) 0.007(2) 0.009(2) O7 0.011(2) 0.022(2) 0.018(2) 0.006(2) -0.0040(18) 0.0049(19) O8 0.014(2) 0.012(2) 0.024(2) 0.0076(19) 0.0021(18) 0.0055(19) O9 0.018(2) 0.031(3) 0.020(2) 0.013(2) -0.0001(19) 0.009(2) O10 0.022(3) 0.020(3) 0.037(3) 0.003(2) 0.004(2) 0.006(2) O11 0.024(3) 0.032(3) 0.027(3) 0.014(2) 0.011(2) 0.012(2) O12 0.023(3) 0.028(3) 0.026(3) 0.014(2) 0.005(2) 0.015(2) O13 0.022(3) 0.022(3) 0.031(3) 0.003(2) 0.003(2) 0.004(2) N1 0.012(3) 0.017(3) 0.020(3) 0.000(2) -0.001(2) 0.005(2) N2 0.021(3) 0.024(3) 0.022(3) 0.010(3) 0.004(2) 0.008(3) N3 0.020(3) 0.030(4) 0.035(4) 0.019(3) -0.010(3) -0.011(3) N4 0.031(4) 0.034(4) 0.031(4) 0.015(3) 0.000(3) 0.002(3) N5 0.020(3) 0.034(4) 0.026(3) 0.011(3) -0.001(3) 0.004(3) N6 0.020(3) 0.034(4) 0.026(3) 0.015(3) -0.003(3) 0.003(3) N7 0.018(3) 0.021(3) 0.023(3) 0.008(2) -0.001(2) 0.005(2) N8 0.019(3) 0.024(3) 0.023(3) 0.011(3) 0.005(2) 0.007(3) N9 0.025(3) 0.023(3) 0.024(3) 0.015(3) 0.002(3) 0.002(3) N10 0.020(3) 0.021(3) 0.021(3) 0.007(2) 0.000(2) 0.002(3) N11 0.021(3) 0.026(3) 0.025(3) 0.012(3) -0.002(2) 0.004(3) N12 0.023(3) 0.025(3) 0.030(3) 0.011(3) -0.006(3) -0.003(3) C1 0.021(4) 0.023(4) 0.014(3) 0.005(3) 0.004(3) 0.010(3) C2 0.019(4) 0.022(4) 0.022(4) -0.001(3) -0.002(3) 0.010(3) C3 0.018(3) 0.019(3) 0.021(3) 0.006(3) 0.004(3) 0.009(3) C4 0.022(4) 0.025(4) 0.024(4) 0.007(3) 0.001(3) 0.004(3) C5 0.019(4) 0.019(4) 0.025(4) 0.006(3) 0.000(3) 0.005(3) C6 0.014(3) 0.019(3) 0.013(3) 0.001(3) 0.001(2) 0.002(3) C7 0.030(4) 0.023(4) 0.022(4) 0.005(3) 0.001(3) 0.010(3) C8 0.024(4) 0.026(4) 0.023(4) 0.011(3) 0.003(3) 0.013(3) C9 0.018(3) 0.025(4) 0.012(3) 0.004(3) 0.000(3) 0.002(3) C10 0.013(3) 0.022(4) 0.021(3) 0.005(3) 0.002(3) 0.004(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 N4 2.281(7) . ? Ag1 N8 2.340(6) . ? Ag1 O4 2.486(5) . ? Ag1 O11 2.496(5) . ? Ag1 Ag3 3.6522(16) 2_666 ? Ag2 N10 2.287(6) . ? Ag2 N2 2.363(6) . ? Ag2 O12 2.434(5) 1_546 ? Ag2 O9 2.637(5) 1_546 ? Ag3 N11 2.190(6) 1_665 ? Ag3 N1 2.233(6) . ? Ag3 N6 2.564(6) . ? Ag3 Ag1 3.6522(16) 2_666 ? Ag4 N5 2.194(6) . ? Ag4 N7 2.253(6) 1_665 ? Ag4 N12 2.585(6) 1_665 ? Mo1 O4 1.709(5) . ? Mo1 O5 1.747(4) . ? Mo1 O2 1.848(4) . ? Mo1 O1 1.958(4) 2_665 ? Mo1 O3 2.206(4) . ? Mo1 O1 2.399(4) . ? Mo1 Mo3 3.2576(13) . ? Mo1 Mo4 3.3814(17) 2_665 ? Mo2 O9 1.716(5) . ? Mo2 O7 1.782(5) . ? Mo2 O6 1.817(5) . ? Mo2 O8 2.012(4) . ? Mo2 O1 2.128(4) . ? Mo2 O2 2.341(4) . ? Mo2 Mo4 3.2590(13) . ? Mo2 Mo3 3.4272(14) . ? Mo3 O10 1.686(5) . ? Mo3 O11 1.716(5) . ? Mo3 O6 1.962(5) 2_565 ? Mo3 O3 1.964(4) . ? Mo3 O7 2.221(5) . ? Mo3 O2 2.259(4) . ? Mo4 O13 1.710(5) . ? Mo4 O12 1.728(5) . ? Mo4 O8 1.856(4) . ? Mo4 O3 1.999(4) 2_665 ? Mo4 O1 2.289(4) . ? Mo4 O5 2.325(4) . ? Mo4 Mo1 3.3814(17) 2_665 ? N1 C2 1.344(9) . ? N1 C1 1.359(9) . ? N2 C3 1.333(9) . ? N2 C4 1.335(9) . ? N3 N4 1.328(9) . ? N3 C5 1.335(9) . ? N4 N5 1.321(9) . ? N5 N6 1.324(9) . ? N6 C5 1.323(9) . ? N7 C6 1.353(9) . ? N7 C7 1.360(9) . ? N7 Ag4 2.253(6) 1_445 ? N8 C8 1.327(9) . ? N8 C9 1.339(9) . ? N9 C10 1.321(9) . ? N9 N10 1.333(8) . ? N10 N11 1.308(8) . ? N11 N12 1.340(8) . ? N11 Ag3 2.190(6) 1_445 ? N12 C10 1.321(9) . ? N12 Ag4 2.585(6) 1_445 ? C1 C4 1.378(10) . ? C1 C5 1.464(10) . ? C2 C3 1.386(10) . ? C2 H2A 0.9300 . ? C3 H3B 0.9300 . ? C4 H4A 0.9300 . ? C6 C9 1.380(9) . ? C6 C10 1.476(10) . ? C7 C8 1.374(10) . ? C7 H7B 0.9300 . ? C8 H8A 0.9300 . ? C9 H9B 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ag1 N8 105.2(2) . . ? N4 Ag1 O4 88.0(2) . . ? N8 Ag1 O4 164.38(18) . . ? N4 Ag1 O11 163.4(2) . . ? N8 Ag1 O11 84.45(18) . . ? O4 Ag1 O11 80.81(16) . . ? N4 Ag1 O12 94.2(2) . 2_665 ? N8 Ag1 O12 107.08(18) . 2_665 ? O4 Ag1 O12 79.66(15) . 2_665 ? O11 Ag1 O12 95.81(15) . 2_665 ? N4 Ag1 Ag3 115.54(18) . 2_666 ? N8 Ag1 Ag3 93.08(15) . 2_666 ? O4 Ag1 Ag3 73.39(12) . 2_666 ? O11 Ag1 Ag3 49.43(11) . 2_666 ? O12 Ag1 Ag3 138.40(10) 2_665 2_666 ? N10 Ag2 N2 104.7(2) . . ? N10 Ag2 O12 156.66(19) . 1_546 ? N2 Ag2 O12 82.56(18) . 1_546 ? N10 Ag2 O13 110.93(19) . 2_666 ? N2 Ag2 O13 87.43(18) . 2_666 ? O12 Ag2 O13 91.29(16) 1_546 2_666 ? N10 Ag2 O9 87.32(18) . 1_546 ? N2 Ag2 O9 158.55(18) . 1_546 ? O12 Ag2 O9 79.81(16) 1_546 1_546 ? O13 Ag2 O9 105.02(15) 2_666 1_546 ? N11 Ag3 N1 164.0(2) 1_665 . ? N11 Ag3 N6 93.2(2) 1_665 . ? N1 Ag3 N6 72.8(2) . . ? N11 Ag3 Ag1 79.44(17) 1_665 2_666 ? N1 Ag3 Ag1 101.35(14) . 2_666 ? N6 Ag3 Ag1 67.05(15) . 2_666 ? N5 Ag4 N7 162.8(2) . 1_665 ? N5 Ag4 N12 92.8(2) . 1_665 ? N7 Ag4 N12 72.0(2) 1_665 1_665 ? O4 Mo1 O5 105.1(2) . . ? O4 Mo1 O2 104.9(2) . . ? O5 Mo1 O2 102.0(2) . . ? O4 Mo1 O1 101.4(2) . 2_665 ? O5 Mo1 O1 98.5(2) . 2_665 ? O2 Mo1 O1 140.81(19) . 2_665 ? O4 Mo1 O3 97.1(2) . . ? O5 Mo1 O3 157.47(18) . . ? O2 Mo1 O3 75.77(17) . . ? O1 Mo1 O3 72.60(17) 2_665 . ? O4 Mo1 O1 176.02(19) . . ? O5 Mo1 O1 77.98(17) . . ? O2 Mo1 O1 76.70(16) . . ? O1 Mo1 O1 75.44(18) 2_665 . ? O3 Mo1 O1 79.73(15) . . ? O4 Mo1 Mo3 93.19(16) . . ? O5 Mo1 Mo3 143.67(15) . . ? O2 Mo1 Mo3 42.16(13) . . ? O1 Mo1 Mo3 108.48(13) 2_665 . ? O3 Mo1 Mo3 36.03(11) . . ? O1 Mo1 Mo3 85.60(10) . . ? O4 Mo1 Mo4 90.79(16) . 2_665 ? O5 Mo1 Mo4 139.04(15) . 2_665 ? O2 Mo1 Mo4 110.08(13) . 2_665 ? O1 Mo1 Mo4 40.76(12) 2_665 2_665 ? O3 Mo1 Mo4 34.43(11) . 2_665 ? O1 Mo1 Mo4 85.24(10) . 2_665 ? Mo3 Mo1 Mo4 69.92(3) . 2_665 ? O9 Mo2 O7 102.3(2) . . ? O9 Mo2 O6 103.5(2) . . ? O7 Mo2 O6 100.5(2) . . ? O9 Mo2 O8 98.8(2) . . ? O7 Mo2 O8 153.49(19) . . ? O6 Mo2 O8 89.86(19) . . ? O9 Mo2 O1 95.01(19) . . ? O7 Mo2 O1 89.22(18) . . ? O6 Mo2 O1 156.6(2) . . ? O8 Mo2 O1 73.05(17) . . ? O9 Mo2 O2 167.88(19) . . ? O7 Mo2 O2 75.22(17) . . ? O6 Mo2 O2 88.64(18) . . ? O8 Mo2 O2 80.76(17) . . ? O1 Mo2 O2 73.21(15) . . ? O9 Mo2 Mo4 88.75(16) . . ? O7 Mo2 Mo4 133.37(14) . . ? O6 Mo2 Mo4 120.94(15) . . ? O8 Mo2 Mo4 31.16(12) . . ? O1 Mo2 Mo4 44.39(12) . . ? O2 Mo2 Mo4 84.74(10) . . ? O9 Mo2 Mo3 137.45(17) . . ? O7 Mo2 Mo3 35.15(14) . . ? O6 Mo2 Mo3 90.17(15) . . ? O8 Mo2 Mo3 121.66(13) . . ? O1 Mo2 Mo3 85.65(11) . . ? O2 Mo2 Mo3 40.93(10) . . ? Mo4 Mo2 Mo3 118.51(3) . . ? O10 Mo3 O11 105.8(3) . . ? O10 Mo3 O6 98.8(2) . 2_565 ? O11 Mo3 O6 94.9(2) . 2_565 ? O10 Mo3 O3 101.2(2) . . ? O11 Mo3 O3 96.3(2) . . ? O6 Mo3 O3 153.41(19) 2_565 . ? O10 Mo3 O7 92.0(2) . . ? O11 Mo3 O7 162.1(2) . . ? O6 Mo3 O7 80.38(18) 2_565 . ? O3 Mo3 O7 81.59(17) . . ? O10 Mo3 O2 161.0(2) . . ? O11 Mo3 O2 92.8(2) . . ? O6 Mo3 O2 83.05(17) 2_565 . ? O3 Mo3 O2 72.39(17) . . ? O7 Mo3 O2 69.53(16) . . ? O10 Mo3 Mo1 142.47(17) . . ? O11 Mo3 Mo1 85.67(17) . . ? O6 Mo3 Mo1 116.04(14) 2_565 . ? O3 Mo3 Mo1 41.36(13) . . ? O7 Mo3 Mo1 81.03(11) . . ? O2 Mo3 Mo1 33.31(11) . . ? O10 Mo3 Mo2 119.29(18) . . ? O11 Mo3 Mo2 134.60(17) . . ? O6 Mo3 Mo2 74.40(14) 2_565 . ? O3 Mo3 Mo2 80.58(13) . . ? O7 Mo3 Mo2 27.51(11) . . ? O2 Mo3 Mo2 42.76(11) . . ? Mo1 Mo3 Mo2 62.15(2) . . ? O13 Mo4 O12 105.8(2) . . ? O13 Mo4 O8 105.9(2) . . ? O12 Mo4 O8 100.0(2) . . ? O13 Mo4 O3 105.3(2) . 2_665 ? O12 Mo4 O3 92.6(2) . 2_665 ? O8 Mo4 O3 141.49(18) . 2_665 ? O13 Mo4 O1 155.7(2) . . ? O12 Mo4 O1 98.3(2) . . ? O8 Mo4 O1 72.16(17) . . ? O3 Mo4 O1 70.08(16) 2_665 . ? O13 Mo4 O5 85.4(2) . . ? O12 Mo4 O5 167.4(2) . . ? O8 Mo4 O5 82.09(17) . . ? O3 Mo4 O5 78.50(17) 2_665 . ? O1 Mo4 O5 70.35(15) . . ? O13 Mo4 Mo2 139.73(16) . . ? O12 Mo4 Mo2 91.14(16) . . ? O8 Mo4 Mo2 34.11(13) . . ? O3 Mo4 Mo2 110.27(13) 2_665 . ? O1 Mo4 Mo2 40.59(10) . . ? O5 Mo4 Mo2 83.71(11) . . ? O13 Mo4 Mo1 143.17(17) . 2_665 ? O12 Mo4 Mo1 86.86(16) . 2_665 ? O8 Mo4 Mo1 105.59(13) . 2_665 ? O3 Mo4 Mo1 38.60(12) 2_665 2_665 ? O1 Mo4 Mo1 33.96(10) . 2_665 ? O5 Mo4 Mo1 80.60(11) . 2_665 ? Mo2 Mo4 Mo1 72.27(3) . 2_665 ? Mo1 O1 Mo2 146.8(2) 2_665 . ? Mo1 O1 Mo4 105.28(18) 2_665 . ? Mo2 O1 Mo4 95.03(16) . . ? Mo1 O1 Mo1 104.56(18) 2_665 . ? Mo2 O1 Mo1 99.24(15) . . ? Mo4 O1 Mo1 95.30(15) . . ? Mo1 O2 Mo3 104.53(19) . . ? Mo1 O2 Mo2 110.53(18) . . ? Mo3 O2 Mo2 96.32(16) . . ? Mo3 O3 Mo4 147.6(2) . 2_665 ? Mo3 O3 Mo1 102.61(19) . . ? Mo4 O3 Mo1 106.97(19) 2_665 . ? Mo1 O4 Ag1 126.7(2) . . ? Mo1 O5 Mo4 115.9(2) . . ? Mo2 O6 Mo3 162.2(3) . 2_565 ? Mo2 O7 Mo3 117.3(2) . . ? Mo4 O8 Mo2 114.7(2) . . ? Mo2 O9 Ag2 120.8(2) . 1_564 ? Mo3 O11 Ag1 128.5(2) . . ? Mo4 O12 Ag2 123.5(2) . 1_564 ? Mo4 O12 Ag1 128.3(2) . 2_665 ? Ag2 O12 Ag1 101.49(17) 1_564 2_665 ? Mo4 O13 Ag2 139.7(2) . 2_666 ? C2 N1 C1 115.9(6) . . ? C2 N1 Ag3 125.3(4) . . ? C1 N1 Ag3 118.7(5) . . ? C3 N2 C4 116.4(6) . . ? C3 N2 Ag2 124.2(5) . . ? C4 N2 Ag2 119.0(5) . . ? N4 N3 C5 104.9(6) . . ? N5 N4 N3 108.7(6) . . ? N5 N4 Ag1 132.8(5) . . ? N3 N4 Ag1 118.4(5) . . ? N4 N5 N6 110.0(6) . . ? N4 N5 Ag4 131.8(5) . . ? N6 N5 Ag4 117.9(5) . . ? C5 N6 N5 104.7(6) . . ? C5 N6 Ag3 105.6(5) . . ? N5 N6 Ag3 149.6(5) . . ? C6 N7 C7 116.5(6) . . ? C6 N7 Ag4 119.0(5) . 1_445 ? C7 N7 Ag4 124.5(5) . 1_445 ? C8 N8 C9 116.7(6) . . ? C8 N8 Ag1 124.1(5) . . ? C9 N8 Ag1 118.8(5) . . ? C10 N9 N10 103.9(6) . . ? N11 N10 N9 110.3(6) . . ? N11 N10 Ag2 131.9(5) . . ? N9 N10 Ag2 117.8(4) . . ? N10 N11 N12 108.7(5) . . ? N10 N11 Ag3 132.9(5) . 1_445 ? N12 N11 Ag3 117.9(4) . 1_445 ? C10 N12 N11 104.5(6) . . ? C10 N12 Ag4 106.7(5) . 1_445 ? N11 N12 Ag4 148.5(4) . 1_445 ? N1 C1 C4 120.7(6) . . ? N1 C1 C5 117.8(6) . . ? C4 C1 C5 121.5(6) . . ? N1 C2 C3 122.5(6) . . ? N1 C2 H2A 118.8 . . ? C3 C2 H2A 118.8 . . ? N2 C3 C2 121.4(7) . . ? N2 C3 H3B 119.3 . . ? C2 C3 H3B 119.3 . . ? N2 C4 C1 123.2(7) . . ? N2 C4 H4A 118.4 . . ? C1 C4 H4A 118.4 . . ? N6 C5 N3 111.7(6) . . ? N6 C5 C1 124.9(6) . . ? N3 C5 C1 123.3(6) . . ? N7 C6 C9 121.0(6) . . ? N7 C6 C10 118.6(6) . . ? C9 C6 C10 120.3(6) . . ? N7 C7 C8 120.9(7) . . ? N7 C7 H7B 119.6 . . ? C8 C7 H7B 119.6 . . ? N8 C8 C7 122.7(7) . . ? N8 C8 H8A 118.6 . . ? C7 C8 H8A 118.6 . . ? N8 C9 C6 122.1(6) . . ? N8 C9 H9B 119.0 . . ? C6 C9 H9B 119.0 . . ? N12 C10 N9 112.6(6) . . ? N12 C10 C6 123.7(6) . . ? N9 C10 C6 123.7(6) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 3.036 _refine_diff_density_min -2.736 _refine_diff_density_rms 0.175