# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Jiang-Gao Mao' 'Chun-Li Hu' 'Fang Kong' 'Chuan-Fu Sun' 'Bing-Ping Yang' _publ_contact_author_name 'Jiang-Gao Mao' _publ_contact_author_email MJG@MS.FJIRSM.AC.CN _publ_section_title ; Syntheses and crystal structures of four new silver(I) iodates with d0-transition metal cations ; # Attachment 'SCF-Dalton-CIF.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 746273' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ag2 I6 O18 Ti' _chemical_formula_sum 'Ag2 I6 O18 Ti ' _chemical_formula_weight 1313.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 10.9332(7) _cell_length_b 10.9332(7) _cell_length_c 11.2807(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1167.78(16) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1074 _cell_measurement_theta_min 2.8085 _cell_measurement_theta_max 27.4449 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1734.0 _exptl_absorpt_coefficient_mu 14.989 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.407 _exptl_absorpt_correction_T_min 0.247 _exptl_absorpt_process_details CrystalClear _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 Mercury2 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2980 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 27.47 _reflns_number_total 603 _reflns_number_gt 574 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0348P)^2^+11.7966P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00082(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 603 _refine_ls_number_parameters 43 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0558 _refine_ls_wR_factor_gt 0.0545 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.6667 0.3333 0.01150(8) 0.0334(2) Uani 1 3 d S . . Ti1 Ti 0.0000 0.0000 0.0000 0.0132(4) Uani 1 6 d S . . I1 I 0.32605(3) 0.05749(3) -0.10719(2) 0.01158(15) Uani 1 1 d . . . O1 O 0.1655(4) 0.0791(4) -0.1022(3) 0.0191(7) Uani 1 1 d . . . O2 O 0.4007(3) 0.1595(4) 0.0269(3) 0.0177(7) Uani 1 1 d . . . O3 O 0.4093(3) 0.1902(3) -0.2215(3) 0.0163(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0271(3) 0.0271(3) 0.0461(5) 0.000 0.000 0.01357(14) Ti1 0.0135(6) 0.0135(6) 0.0128(9) 0.000 0.000 0.0067(3) I1 0.01330(19) 0.01060(19) 0.0107(2) 0.00099(8) 0.00158(9) 0.00586(12) O1 0.0188(16) 0.0243(17) 0.0187(16) 0.0046(13) 0.0031(13) 0.0142(14) O2 0.0222(17) 0.0195(16) 0.0128(15) -0.0034(12) -0.0011(12) 0.0114(14) O3 0.0184(16) 0.0133(15) 0.0166(15) 0.0061(12) 0.0051(12) 0.0074(13) _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 O2 2.563(3) 2_655 ? Ag1 O2 2.563(3) . ? Ag1 O2 2.563(3) 3_665 ? Ti1 O1 1.946(3) 12 ? Ti1 O1 1.946(3) 3 ? Ti1 O1 1.946(3) 10 ? Ti1 O1 1.946(3) 11 ? Ti1 O1 1.946(3) 2 ? Ti1 O1 1.946(3) . ? I1 O3 1.810(3) . ? I1 O2 1.813(3) . ? I1 O1 1.886(3) . ? I1 O3 2.381(3) 18_544 ? O3 I1 2.381(3) 17_554 ? 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 O2 Ag1 O2 119.545(17) 2_655 . ? O2 Ag1 O2 119.545(17) 2_655 3_665 ? O2 Ag1 O2 119.545(17) . 3_665 ? O1 Ti1 O1 180.0(2) 12 3 ? O1 Ti1 O1 88.49(14) 12 10 ? O1 Ti1 O1 91.51(14) 3 10 ? O1 Ti1 O1 88.49(14) 12 11 ? O1 Ti1 O1 91.51(14) 3 11 ? O1 Ti1 O1 88.49(14) 10 11 ? O1 Ti1 O1 91.51(14) 12 2 ? O1 Ti1 O1 88.49(14) 3 2 ? O1 Ti1 O1 91.51(14) 10 2 ? O1 Ti1 O1 180.00(15) 11 2 ? O1 Ti1 O1 91.51(14) 12 . ? O1 Ti1 O1 88.49(14) 3 . ? O1 Ti1 O1 180.0(4) 10 . ? O1 Ti1 O1 91.51(14) 11 . ? O1 Ti1 O1 88.49(14) 2 . ? O3 I1 O2 102.13(15) . . ? O3 I1 O1 92.72(14) . . ? O2 I1 O1 93.39(15) . . ? O3 I1 O3 80.30(16) . 18_544 ? O2 I1 O3 80.60(13) . 18_544 ? O1 I1 O3 169.53(13) . 18_544 ? I1 O1 Ti1 132.77(18) . . ? I1 O2 Ag1 113.24(14) . . ? I1 O3 I1 122.15(16) . 17_554 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.503 _refine_diff_density_min -1.907 _refine_diff_density_rms 0.209 #===end data_2 _database_code_depnum_ccdc_archive 'CCDC 746274' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ag2 I3 O11 V ' _chemical_formula_sum 'Ag2 I3 O11 V ' _chemical_formula_weight 823.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 35.245(4) _cell_length_b 7.7757(9) _cell_length_c 7.1720(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1965.5(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4272 _cell_measurement_theta_min 2.3114 _cell_measurement_theta_max 27.4758 _exptl_crystal_description acerose _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912.0 _exptl_absorpt_coefficient_mu 14.355 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.423 _exptl_absorpt_correction_T_min 0.262 _exptl_absorpt_process_details CrystalClear _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 Mercury2 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12285 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2248 _reflns_number_gt 1919 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0418P)^2^+6.0881P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00017(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2248 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 0.261520(19) 0.71710(9) 0.05360(10) 0.03176(18) Uani 1 1 d . . . Ag2 Ag 0.08343(2) 0.72492(9) 0.55294(9) 0.03278(18) Uani 1 1 d . . . V1 V 0.08046(3) 0.22222(14) 0.45151(16) 0.0118(2) Uani 1 1 d . . . I1 I 0.148390(13) 0.46679(5) 0.31287(6) 0.01288(13) Uani 1 1 d . . . I2 I 0.184714(13) 0.55307(6) -0.17771(7) 0.01512(13) Uani 1 1 d . . . I3 I 0.007622(13) 0.51652(5) 0.74825(6) 0.01161(13) Uani 1 1 d . . . O1 O 0.11959(14) 0.3801(6) 0.5179(7) 0.0181(11) Uani 1 1 d . . . O2 O 0.12126(16) 0.6649(6) 0.2980(7) 0.0232(12) Uani 1 1 d . . . O3 O 0.18668(15) 0.5388(7) 0.4542(7) 0.0209(12) Uani 1 1 d . . . O4 O 0.18692(16) 0.5827(7) 0.0747(7) 0.0240(12) Uani 1 1 d . . . O5 O 0.23359(14) 0.6053(7) -0.2207(8) 0.0225(12) Uani 1 1 d . . . O6 O 0.18960(15) 0.3229(7) -0.1813(8) 0.0231(12) Uani 1 1 d . . . O7 O 0.03124(15) 0.7225(6) 0.7789(8) 0.0207(11) Uani 1 1 d . . . O8 O 0.03010(15) 0.4022(7) 0.9455(6) 0.0188(11) Uani 1 1 d . . . O9 O 0.03692(15) 0.4447(6) 0.5561(7) 0.0180(11) Uani 1 1 d . . . O10 O 0.10553(15) 0.0530(6) 0.4165(7) 0.0198(11) Uani 1 1 d . . . O11 O 0.07378(14) 0.1925(6) 0.7348(7) 0.0140(10) 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 0.0268(3) 0.0449(4) 0.0237(3) -0.0103(3) -0.0015(3) 0.0052(3) Ag2 0.0288(4) 0.0424(4) 0.0272(4) -0.0109(3) 0.0080(3) -0.0091(3) V1 0.0118(5) 0.0123(5) 0.0112(5) 0.0006(4) -0.0010(5) -0.0006(4) I1 0.0138(2) 0.0115(2) 0.0134(2) -0.00053(16) 0.00004(18) -0.00133(15) I2 0.0158(2) 0.0143(2) 0.0152(2) 0.00131(17) 0.00084(18) 0.00073(16) I3 0.0137(3) 0.0109(2) 0.0102(2) 0.00067(15) 0.00016(18) 0.00236(15) O1 0.019(3) 0.022(3) 0.013(2) 0.000(2) 0.000(2) -0.005(2) O2 0.026(3) 0.016(3) 0.027(3) 0.002(2) 0.010(2) 0.007(2) O3 0.019(3) 0.026(3) 0.018(3) -0.003(2) -0.002(2) -0.011(2) O4 0.025(3) 0.028(3) 0.018(3) 0.001(2) 0.001(2) -0.007(2) O5 0.010(3) 0.033(3) 0.024(3) 0.005(2) 0.003(2) -0.004(2) O6 0.021(3) 0.020(3) 0.028(3) -0.002(2) -0.003(2) -0.004(2) O7 0.020(3) 0.012(2) 0.031(3) 0.000(2) -0.001(2) -0.004(2) O8 0.021(3) 0.023(3) 0.012(2) 0.003(2) 0.002(2) 0.009(2) O9 0.022(3) 0.017(3) 0.015(2) 0.0008(19) -0.001(2) 0.004(2) O10 0.019(3) 0.017(3) 0.023(3) 0.002(2) 0.003(2) 0.003(2) O11 0.012(2) 0.015(2) 0.015(2) -0.0005(19) -0.0019(19) 0.0021(18) _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 O5 2.344(5) 8_576 ? Ag1 O5 2.365(6) . ? Ag1 O6 2.546(5) 7_665 ? Ag1 O6 2.584(6) 2_565 ? Ag1 I2 3.4215(9) . ? Ag1 I2 3.4231(9) 2_565 ? Ag1 Ag1 3.6223(4) 8_575 ? Ag1 Ag1 3.6223(4) 8_576 ? Ag2 O2 2.310(5) . ? Ag2 O2 2.367(6) 8_576 ? Ag2 O7 2.452(5) . ? Ag2 O7 2.723(5) 8_575 ? Ag2 O9 2.727(5) . ? Ag2 I3 3.4246(8) . ? Ag2 Ag2 3.6072(4) 8_575 ? Ag2 Ag2 3.6072(4) 8_576 ? V1 O10 1.604(5) . ? V1 O11 1.706(5) 8_565 ? V1 O1 1.907(5) . ? V1 O8 2.022(5) 8_565 ? V1 O11 2.058(5) . ? V1 O9 2.431(5) . ? V1 I1 3.2152(12) . ? I1 O3 1.778(5) . ? I1 O2 1.816(5) . ? I1 O1 1.909(5) . ? I1 O4 2.361(5) . ? I2 O5 1.796(5) . ? I2 O6 1.798(5) . ? I2 O4 1.827(5) . ? I2 Ag1 3.4231(9) 2_564 ? I3 O9 1.810(5) . ? I3 O7 1.819(5) . ? I3 O8 1.849(5) . ? O2 Ag2 2.367(6) 8_575 ? O5 Ag1 2.344(5) 8_575 ? O6 Ag1 2.546(5) 7_655 ? O6 Ag1 2.584(6) 2_564 ? O7 Ag2 2.723(5) 8_576 ? O8 V1 2.022(5) 8_566 ? O11 V1 1.706(5) 8_566 ? 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 O5 Ag1 O5 128.0(2) 8_576 . ? O5 Ag1 O6 123.42(18) 8_576 7_665 ? O5 Ag1 O6 81.37(17) . 7_665 ? O5 Ag1 O6 80.96(17) 8_576 2_565 ? O5 Ag1 O6 147.68(18) . 2_565 ? O6 Ag1 O6 94.27(18) 7_665 2_565 ? O5 Ag1 I2 102.83(13) 8_576 . ? O5 Ag1 I2 29.60(12) . . ? O6 Ag1 I2 109.57(13) 7_665 . ? O6 Ag1 I2 147.06(12) 2_565 . ? O5 Ag1 I2 101.84(14) 8_576 2_565 ? O5 Ag1 I2 118.23(14) . 2_565 ? O6 Ag1 I2 101.31(12) 7_665 2_565 ? O6 Ag1 I2 31.02(11) 2_565 2_565 ? I2 Ag1 I2 118.83(2) . 2_565 ? O5 Ag1 Ag1 126.90(14) 8_576 8_575 ? O5 Ag1 Ag1 39.52(13) . 8_575 ? O6 Ag1 Ag1 45.52(13) 7_665 8_575 ? O6 Ag1 Ag1 138.18(12) 2_565 8_575 ? I2 Ag1 Ag1 64.701(14) . 8_575 ? I2 Ag1 Ag1 130.09(2) 2_565 8_575 ? O5 Ag1 Ag1 39.94(13) 8_576 8_576 ? O5 Ag1 Ag1 151.08(12) . 8_576 ? O6 Ag1 Ag1 127.55(13) 7_665 8_576 ? O6 Ag1 Ag1 44.66(12) 2_565 8_576 ? I2 Ag1 Ag1 122.185(17) . 8_576 ? I2 Ag1 Ag1 61.926(19) 2_565 8_576 ? Ag1 Ag1 Ag1 163.76(5) 8_575 8_576 ? O2 Ag2 O2 109.6(2) . 8_576 ? O2 Ag2 O7 162.66(18) . . ? O2 Ag2 O7 86.24(18) 8_576 . ? O2 Ag2 O7 81.32(18) . 8_575 ? O2 Ag2 O7 149.58(16) 8_576 8_575 ? O7 Ag2 O7 88.36(16) . 8_575 ? O2 Ag2 O9 101.08(17) . . ? O2 Ag2 O9 128.44(16) 8_576 . ? O7 Ag2 O9 62.44(16) . . ? O7 Ag2 O9 73.73(15) 8_575 . ? O2 Ag2 I3 132.72(14) . . ? O2 Ag2 I3 107.88(13) 8_576 . ? O7 Ag2 I3 30.75(11) . . ? O7 Ag2 I3 80.74(11) 8_575 . ? O9 Ag2 I3 31.72(11) . . ? O2 Ag2 Ag2 40.11(14) . 8_575 ? O2 Ag2 Ag2 134.36(13) 8_576 8_575 ? O7 Ag2 Ag2 131.15(13) . 8_575 ? O7 Ag2 Ag2 42.79(11) 8_575 8_575 ? O9 Ag2 Ag2 95.44(10) . 8_575 ? I3 Ag2 Ag2 117.246(17) . 8_575 ? O2 Ag2 Ag2 143.95(14) . 8_576 ? O2 Ag2 Ag2 38.97(13) 8_576 8_576 ? O7 Ag2 Ag2 48.97(13) . 8_576 ? O7 Ag2 Ag2 134.54(11) 8_575 8_576 ? O9 Ag2 Ag2 94.47(11) . 8_576 ? I3 Ag2 Ag2 69.178(17) . 8_576 ? Ag2 Ag2 Ag2 167.58(5) 8_575 8_576 ? O10 V1 O11 104.6(2) . 8_565 ? O10 V1 O1 99.7(3) . . ? O11 V1 O1 94.4(2) 8_565 . ? O10 V1 O8 95.0(3) . 8_565 ? O11 V1 O8 92.6(2) 8_565 8_565 ? O1 V1 O8 161.5(2) . 8_565 ? O10 V1 O11 97.2(2) . . ? O11 V1 O11 158.0(2) 8_565 . ? O1 V1 O11 84.8(2) . . ? O8 V1 O11 82.35(19) 8_565 . ? O10 V1 O9 168.3(2) . . ? O11 V1 O9 85.3(2) 8_565 . ? O1 V1 O9 85.5(2) . . ? O8 V1 O9 78.0(2) 8_565 . ? O11 V1 O9 72.73(17) . . ? O10 V1 I1 91.52(19) . . ? O11 V1 I1 65.86(16) 8_565 . ? O1 V1 I1 32.62(15) . . ? O8 V1 I1 158.45(15) 8_565 . ? O11 V1 I1 117.18(14) . . ? O9 V1 I1 98.31(13) . . ? O3 I1 O2 99.5(3) . . ? O3 I1 O1 94.4(2) . . ? O2 I1 O1 93.7(2) . . ? O3 I1 O4 81.7(2) . . ? O2 I1 O4 86.4(2) . . ? O1 I1 O4 176.0(2) . . ? O3 I1 V1 125.12(17) . . ? O2 I1 V1 97.34(18) . . ? O1 I1 V1 32.56(15) . . ? O4 I1 V1 151.39(13) . . ? O5 I2 O6 97.5(3) . . ? O5 I2 O4 95.8(2) . . ? O6 I2 O4 97.8(3) . . ? O5 I2 Ag1 40.56(18) . . ? O6 I2 Ag1 107.59(17) . . ? O4 I2 Ag1 55.86(17) . . ? O5 I2 Ag1 60.75(19) . 2_564 ? O6 I2 Ag1 47.79(18) . 2_564 ? O4 I2 Ag1 127.71(18) . 2_564 ? Ag1 I2 Ag1 93.654(18) . 2_564 ? O9 I3 O7 95.9(2) . . ? O9 I3 O8 100.9(2) . . ? O7 I3 O8 97.8(2) . . ? O9 I3 Ag2 52.37(16) . . ? O7 I3 Ag2 43.58(17) . . ? O8 I3 Ag2 101.90(16) . . ? V1 O1 I1 114.8(2) . . ? I1 O2 Ag2 115.4(2) . . ? I1 O2 Ag2 130.3(3) . 8_575 ? Ag2 O2 Ag2 100.9(2) . 8_575 ? I2 O4 I1 130.1(3) . . ? I2 O5 Ag1 130.9(3) . 8_575 ? I2 O5 Ag1 109.8(2) . . ? Ag1 O5 Ag1 100.5(2) 8_575 . ? I2 O6 Ag1 112.1(2) . 7_655 ? I2 O6 Ag1 101.2(2) . 2_564 ? Ag1 O6 Ag1 89.82(18) 7_655 2_564 ? I3 O7 Ag2 105.7(2) . . ? I3 O7 Ag2 121.9(2) . 8_576 ? Ag2 O7 Ag2 88.23(16) . 8_576 ? I3 O8 V1 128.5(3) . 8_566 ? I3 O9 V1 144.5(3) . . ? I3 O9 Ag2 95.9(2) . . ? V1 O9 Ag2 100.75(19) . . ? V1 O11 V1 147.1(3) 8_566 . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.171 _refine_diff_density_min -1.480 _refine_diff_density_rms 0.288 #===end data_3 _database_code_depnum_ccdc_archive 'CCDC 746275' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ag2 I4 O16 V2 ' _chemical_formula_sum 'Ag2 I4 O16 V2' _chemical_formula_weight 1081.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n ' _symmetry_space_group_name_Hall '-P 2ab 2ac ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 17.5991(10) _cell_length_b 10.7094(5) _cell_length_c 14.2861(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2692.6(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6110 _cell_measurement_theta_min 2.2260 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1200 _exptl_crystal_size_mid 0.1100 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3840.0 _exptl_absorpt_coefficient_mu 13.477 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.216 _exptl_absorpt_correction_T_max 0.260 _exptl_absorpt_process_details CrystalClear _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 'Mercury2 ' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18718 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3101 _reflns_number_gt 2868 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0610P)^2^+39.5025P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3101 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1131 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.149 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.36953(4) 0.24720(7) 0.01270(5) 0.02490(19) Uani 1 1 d . . . Ag2 Ag 0.36502(4) 0.24079(7) 0.24187(5) 0.02595(19) Uani 1 1 d . . . V1 V 0.39499(7) -0.23628(13) 0.26526(9) 0.0112(3) Uani 1 1 d . . . V2 V 0.38873(8) -0.23747(13) 0.50939(8) 0.0118(3) Uani 1 1 d . . . I1 I 0.28296(3) 0.48602(5) 0.12415(3) 0.01399(15) Uani 1 1 d . . . I2 I 0.48748(3) -0.00363(5) 0.12370(3) 0.01164(16) Uani 1 1 d . . . I3 I 0.29346(3) 0.51762(5) 0.37687(3) 0.01177(15) Uani 1 1 d . . . I4 I 0.51806(3) -0.04032(5) 0.62447(3) 0.01286(16) Uani 1 1 d . . . O1 O 0.3804(3) 0.4311(6) 0.1229(4) 0.0190(12) Uani 1 1 d . . . O2 O 0.2534(3) 0.3930(6) 0.2253(4) 0.0183(12) Uani 1 1 d . . . O3 O 0.2498(3) 0.3899(6) 0.0274(4) 0.0173(12) Uani 1 1 d . . . O4 O 0.3966(3) 0.0716(6) 0.1226(4) 0.0204(13) Uani 1 1 d . . . O5 O 0.4769(3) -0.1161(6) 0.0278(3) 0.0152(11) Uani 1 1 d . . . O6 O 0.4728(3) -0.1120(6) 0.2241(3) 0.0159(11) Uani 1 1 d . . . O7 O 0.3343(3) 0.6085(6) 0.2787(4) 0.0169(11) Uani 1 1 d . . . O8 O 0.3271(3) 0.6189(6) 0.4717(4) 0.0203(12) Uani 1 1 d . . . O9 O 0.3659(3) 0.3985(6) 0.3796(4) 0.0190(13) Uani 1 1 d . . . O10 O 0.4858(3) -0.1345(6) 0.7220(4) 0.0186(12) Uani 1 1 d . . . O11 O 0.6126(4) -0.1036(7) 0.6207(4) 0.0246(14) Uani 1 1 d . . . O12 O 0.4806(3) -0.1288(6) 0.5229(4) 0.0181(12) Uani 1 1 d . . . O13 O 0.3321(3) -0.1263(6) 0.4760(4) 0.0176(12) Uani 1 1 d . . . O14 O 0.3706(3) -0.2420(6) 0.6245(3) 0.0138(12) Uani 1 1 d . . . O15 O 0.4337(3) -0.2495(5) 0.3737(3) 0.0123(12) Uani 1 1 d . . . O16 O 0.3260(3) -0.1404(6) 0.2791(4) 0.0208(12) 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 0.0356(4) 0.0182(4) 0.0209(3) -0.0021(2) 0.0017(3) -0.0009(3) Ag2 0.0345(4) 0.0212(4) 0.0221(3) -0.0016(3) -0.0041(3) 0.0069(3) V1 0.0153(6) 0.0111(6) 0.0072(5) -0.0001(4) 0.0020(5) 0.0011(5) V2 0.0150(6) 0.0109(7) 0.0095(5) -0.0001(4) -0.0017(4) 0.0002(5) I1 0.0166(3) 0.0135(3) 0.0118(3) 0.00003(17) -0.00044(17) 0.00082(19) I2 0.0141(3) 0.0120(3) 0.0088(2) 0.00024(16) -0.00003(15) -0.00144(18) I3 0.0121(3) 0.0121(3) 0.0111(3) -0.00010(16) 0.00044(15) -0.00088(18) I4 0.0173(3) 0.0129(3) 0.0084(2) 0.00039(16) -0.00060(15) -0.00328(19) O1 0.016(3) 0.021(3) 0.021(3) -0.004(2) 0.004(2) 0.000(3) O2 0.022(3) 0.017(3) 0.016(3) 0.005(2) 0.005(2) -0.003(2) O3 0.021(3) 0.017(3) 0.014(2) -0.003(2) -0.003(2) -0.002(2) O4 0.018(3) 0.026(4) 0.017(3) -0.002(2) -0.002(2) 0.002(3) O5 0.022(3) 0.014(3) 0.009(2) -0.002(2) -0.001(2) -0.005(2) O6 0.025(3) 0.015(3) 0.007(2) 0.003(2) -0.002(2) -0.008(2) O7 0.022(3) 0.018(3) 0.010(2) 0.003(2) 0.002(2) -0.007(2) O8 0.023(3) 0.024(3) 0.014(3) -0.004(2) -0.001(2) -0.007(3) O9 0.021(3) 0.016(3) 0.020(3) 0.002(2) 0.002(2) 0.006(2) O10 0.029(3) 0.016(3) 0.011(2) 0.003(2) 0.000(2) -0.007(2) O11 0.026(3) 0.028(4) 0.020(3) -0.001(2) 0.000(2) -0.002(3) O12 0.025(3) 0.021(3) 0.009(2) 0.001(2) 0.000(2) -0.007(2) O13 0.020(3) 0.022(3) 0.011(2) 0.003(2) 0.001(2) 0.006(2) O14 0.017(3) 0.015(3) 0.010(3) 0.001(2) 0.0008(18) 0.000(2) O15 0.011(3) 0.016(3) 0.010(2) -0.001(2) -0.0018(17) 0.002(2) O16 0.026(3) 0.016(3) 0.021(3) -0.003(2) 0.002(2) 0.008(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 O9 2.460(6) 7_565 ? Ag1 O4 2.496(6) . ? Ag1 O11 2.507(6) 3_655 ? Ag1 O1 2.528(6) . ? Ag1 O3 2.570(6) 2 ? Ag1 Ag2 3.2756(11) . ? Ag2 O11 2.483(6) 5_656 ? Ag2 O2 2.541(6) 2 ? Ag2 O4 2.548(6) . ? Ag2 O2 2.563(6) . ? Ag2 O9 2.593(6) . ? V1 O16 1.603(6) . ? V1 O15 1.698(5) . ? V1 O7 1.986(6) 1_545 ? V1 O6 1.998(6) . ? V1 O14 2.069(5) 7 ? V1 O10 2.203(6) 7 ? V2 O13 1.625(6) . ? V2 O14 1.676(5) . ? V2 O8 1.958(6) 1_545 ? V2 O12 2.002(6) . ? V2 O15 2.098(5) . ? V2 O5 2.222(6) 7_556 ? I1 O1 1.812(6) . ? I1 O3 1.820(5) . ? I1 O2 1.830(5) . ? I2 O4 1.792(6) . ? I2 O5 1.833(5) . ? I2 O6 1.863(5) . ? I3 O9 1.805(6) . ? I3 O8 1.833(6) . ? I3 O7 1.852(5) . ? I4 O11 1.798(7) . ? I4 O10 1.811(6) . ? I4 O12 1.854(5) . ? O2 Ag2 2.541(6) 2 ? O3 Ag1 2.570(6) 2 ? O5 V2 2.222(6) 7 ? O7 V1 1.986(6) 1_565 ? O8 V2 1.958(6) 1_565 ? O9 Ag1 2.460(6) 7_566 ? O10 V1 2.203(6) 7_556 ? O11 Ag2 2.483(6) 5_656 ? O11 Ag1 2.507(6) 3_645 ? O14 V1 2.069(5) 7_556 ? 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 O9 Ag1 O4 90.8(2) 7_565 . ? O9 Ag1 O11 79.6(2) 7_565 3_655 ? O4 Ag1 O11 159.2(2) . 3_655 ? O9 Ag1 O1 167.68(19) 7_565 . ? O4 Ag1 O1 100.40(19) . . ? O11 Ag1 O1 88.1(2) 3_655 . ? O9 Ag1 O3 71.33(18) 7_565 2 ? O4 Ag1 O3 70.98(19) . 2 ? O11 Ag1 O3 121.9(2) 3_655 2 ? O1 Ag1 O3 117.11(19) . 2 ? O9 Ag1 Ag2 139.34(14) 7_565 . ? O4 Ag1 Ag2 50.19(13) . . ? O11 Ag1 Ag2 140.92(15) 3_655 . ? O1 Ag1 Ag2 52.83(13) . . ? O3 Ag1 Ag2 83.50(12) 2 . ? O11 Ag2 O2 82.5(2) 5_656 2 ? O11 Ag2 O4 94.2(2) 5_656 . ? O2 Ag2 O4 73.48(19) 2 . ? O11 Ag2 O2 124.8(2) 5_656 . ? O2 Ag2 O2 73.8(2) 2 . ? O4 Ag2 O2 123.87(19) . . ? O11 Ag2 O9 77.6(2) 5_656 . ? O2 Ag2 O9 116.30(19) 2 . ? O4 Ag2 O9 165.70(19) . . ? O2 Ag2 O9 70.18(18) . . ? O11 Ag2 Ag1 143.00(15) 5_656 . ? O2 Ag2 Ag1 86.47(13) 2 . ? O4 Ag2 Ag1 48.81(14) . . ? O2 Ag2 Ag1 85.00(12) . . ? O9 Ag2 Ag1 138.13(13) . . ? O16 V1 O15 104.2(3) . . ? O16 V1 O7 96.7(3) . 1_545 ? O15 V1 O7 93.3(3) . 1_545 ? O16 V1 O6 97.4(3) . . ? O15 V1 O6 92.8(2) . . ? O7 V1 O6 162.7(2) 1_545 . ? O16 V1 O14 92.0(3) . 7 ? O15 V1 O14 163.8(3) . 7 ? O7 V1 O14 83.5(2) 1_545 7 ? O6 V1 O14 86.1(2) . 7 ? O16 V1 O10 170.8(3) . 7 ? O15 V1 O10 85.0(2) . 7 ? O7 V1 O10 83.8(2) 1_545 7 ? O6 V1 O10 80.7(2) . 7 ? O14 V1 O10 78.9(2) 7 7 ? O13 V2 O14 101.1(3) . . ? O13 V2 O8 98.9(3) . 1_545 ? O14 V2 O8 98.2(3) . 1_545 ? O13 V2 O12 95.6(3) . . ? O14 V2 O12 94.4(3) . . ? O8 V2 O12 158.6(3) 1_545 . ? O13 V2 O15 90.3(2) . . ? O14 V2 O15 167.7(3) . . ? O8 V2 O15 84.6(2) 1_545 . ? O12 V2 O15 79.6(2) . . ? O13 V2 O5 168.7(2) . 7_556 ? O14 V2 O5 89.8(2) . 7_556 ? O8 V2 O5 82.2(2) 1_545 7_556 ? O12 V2 O5 80.5(2) . 7_556 ? O15 V2 O5 78.6(2) . 7_556 ? O1 I1 O3 96.5(3) . . ? O1 I1 O2 95.7(3) . . ? O3 I1 O2 101.6(3) . . ? O4 I2 O5 101.4(3) . . ? O4 I2 O6 99.4(3) . . ? O5 I2 O6 98.7(3) . . ? O9 I3 O8 100.1(3) . . ? O9 I3 O7 96.5(3) . . ? O8 I3 O7 97.1(3) . . ? O11 I4 O10 95.9(3) . . ? O11 I4 O12 96.5(3) . . ? O10 I4 O12 101.9(3) . . ? I1 O1 Ag1 100.8(3) . . ? I1 O2 Ag2 127.8(3) . 2 ? I1 O2 Ag2 101.6(2) . . ? Ag2 O2 Ag2 105.2(2) 2 . ? I1 O3 Ag1 130.3(3) . 2 ? I2 O4 Ag1 121.0(3) . . ? I2 O4 Ag2 120.6(3) . . ? Ag1 O4 Ag2 81.0(2) . . ? I2 O5 V2 128.5(3) . 7 ? I2 O6 V1 137.5(3) . . ? I3 O7 V1 136.2(3) . 1_565 ? I3 O8 V2 147.9(3) . 1_565 ? I3 O9 Ag1 118.9(3) . 7_566 ? I3 O9 Ag2 116.1(3) . . ? Ag1 O9 Ag2 100.0(2) 7_566 . ? I4 O10 V1 142.5(3) . 7_556 ? I4 O11 Ag2 110.2(3) . 5_656 ? I4 O11 Ag1 112.3(3) . 3_645 ? Ag2 O11 Ag1 101.8(3) 5_656 3_645 ? I4 O12 V2 131.3(3) . . ? V2 O14 V1 156.5(4) . 7_556 ? V1 O15 V2 133.4(3) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 4.495 _refine_diff_density_min -2.168 _refine_diff_density_rms 0.330 #===end data_4 _database_code_depnum_ccdc_archive 'CCDC 746276' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ag2 I4 Mo O14' _chemical_formula_sum 'Ag2 I4 Mo O14 ' _chemical_formula_weight 1043.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.6289(14) _cell_length_b 5.7026(5) _cell_length_c 17.521(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.782(6) _cell_angle_gamma 90.00 _cell_volume 1243.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1613 _cell_measurement_theta_min 2.3591 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Prism _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 14.120 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.244 _exptl_absorpt_correction_T_min 0.143 _exptl_absorpt_process_details CrystalClear _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 'Mercury2 ' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4406 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1424 _reflns_number_gt 1291 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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^)+(0.0519P)^2^+1.1606P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00044(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1424 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 0.32315(5) 0.99638(10) 0.03896(3) 0.03037(19) Uani 1 1 d . . . Mo1 Mo 0.5000 0.06592(13) 0.2500 0.01268(18) Uani 1 2 d S . . I1 I 0.54132(3) 0.39623(7) 0.08855(2) 0.01363(15) Uani 1 1 d . . . I2 I 0.28699(3) 0.49076(6) 0.17464(2) 0.01354(15) Uani 1 1 d . . . O1 O 0.6612(3) 0.2468(8) 0.0710(2) 0.0185(9) Uani 1 1 d . . . O2 O 0.4866(4) 0.1367(7) 0.1396(2) 0.0170(9) Uani 1 1 d . . . O3 O 0.4515(4) 0.3008(8) 0.0008(2) 0.0198(9) Uani 1 1 d . . . O4 O 0.3730(4) 0.5914(9) 0.1089(3) 0.0231(10) Uani 1 1 d . . . O5 O 0.3881(4) 0.3606(8) 0.2518(2) 0.0187(9) Uani 1 1 d . . . O6 O 0.2321(4) 0.2293(9) 0.1258(3) 0.0251(10) Uani 1 1 d . . . O7 O 0.6087(4) -0.1181(8) 0.2569(3) 0.0227(10) 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 0.0388(4) 0.0301(3) 0.0249(3) -0.0099(2) 0.0130(3) -0.0120(2) Mo1 0.0180(4) 0.0102(3) 0.0103(3) 0.000 0.0039(3) 0.000 I1 0.0150(2) 0.0168(2) 0.0094(2) 0.00063(13) 0.00284(15) 0.00122(13) I2 0.0152(2) 0.0145(2) 0.0113(2) -0.00037(13) 0.00324(16) 0.00147(13) O1 0.014(2) 0.020(2) 0.021(2) -0.0008(18) 0.0040(17) 0.0060(17) O2 0.027(2) 0.014(2) 0.009(2) 0.0009(16) 0.0029(17) -0.0073(18) O3 0.024(2) 0.023(2) 0.0107(19) 0.0021(17) -0.0006(17) -0.0025(19) O4 0.026(3) 0.027(3) 0.018(2) 0.0055(19) 0.010(2) 0.007(2) O5 0.026(2) 0.018(2) 0.011(2) -0.0008(16) 0.0007(18) 0.0068(18) O6 0.022(2) 0.024(2) 0.028(2) -0.011(2) 0.0007(19) -0.0027(19) O7 0.035(3) 0.017(2) 0.017(2) 0.0039(17) 0.008(2) 0.008(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 O1 2.408(4) 5_665 ? Ag1 O6 2.448(5) 1_565 ? Ag1 O3 2.541(5) 1_565 ? Ag1 O2 2.603(4) 1_565 ? Ag1 O1 2.629(4) 3_455 ? Ag1 O4 2.640(5) . ? Ag1 Ag1 3.5095(11) 7_565 ? Ag1 Ag1 3.5759(13) 7_575 ? Mo1 O7 1.716(5) 2_655 ? Mo1 O7 1.716(5) . ? Mo1 O2 1.954(4) 2_655 ? Mo1 O2 1.954(4) . ? Mo1 O5 2.200(4) 2_655 ? Mo1 O5 2.200(4) . ? I1 O1 1.809(4) . ? I1 O3 1.832(4) . ? I1 O2 1.918(4) . ? I1 O3 2.343(4) 5_665 ? I1 O4 2.478(4) . ? I2 O6 1.799(5) . ? I2 O4 1.806(4) . ? I2 O5 1.850(4) . ? O1 Ag1 2.408(4) 5_665 ? O1 Ag1 2.629(4) 3_545 ? O2 Ag1 2.603(4) 1_545 ? O3 I1 2.343(4) 5_665 ? O3 Ag1 2.541(5) 1_545 ? O6 Ag1 2.448(5) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ag1 O6 156.97(15) 5_665 1_565 ? O1 Ag1 O3 92.30(15) 5_665 1_565 ? O6 Ag1 O3 100.42(15) 1_565 1_565 ? O1 Ag1 O2 123.74(14) 5_665 1_565 ? O6 Ag1 O2 79.29(14) 1_565 1_565 ? O3 Ag1 O2 60.04(13) 1_565 1_565 ? O1 Ag1 O1 91.80(13) 5_665 3_455 ? O6 Ag1 O1 72.35(15) 1_565 3_455 ? O3 Ag1 O1 168.54(15) 1_565 3_455 ? O2 Ag1 O1 125.30(13) 1_565 3_455 ? O1 Ag1 O4 79.74(14) 5_665 . ? O6 Ag1 O4 106.64(15) 1_565 . ? O3 Ag1 O4 127.39(15) 1_565 . ? O2 Ag1 O4 81.66(14) 1_565 . ? O1 Ag1 O4 63.93(14) 3_455 . ? O1 Ag1 Ag1 48.49(10) 5_665 7_565 ? O6 Ag1 Ag1 113.85(11) 1_565 7_565 ? O3 Ag1 Ag1 139.62(10) 1_565 7_565 ? O2 Ag1 Ag1 144.50(10) 1_565 7_565 ? O1 Ag1 Ag1 43.31(9) 3_455 7_565 ? O4 Ag1 Ag1 63.16(11) . 7_565 ? O1 Ag1 Ag1 105.53(11) 5_665 7_575 ? O6 Ag1 Ag1 62.08(12) 1_565 7_575 ? O3 Ag1 Ag1 70.01(11) 1_565 7_575 ? O2 Ag1 Ag1 108.00(10) 1_565 7_575 ? O1 Ag1 Ag1 98.57(10) 3_455 7_575 ? O4 Ag1 Ag1 162.16(10) . 7_575 ? Ag1 Ag1 Ag1 107.19(3) 7_565 7_575 ? O7 Mo1 O7 104.6(3) 2_655 . ? O7 Mo1 O2 97.47(19) 2_655 2_655 ? O7 Mo1 O2 97.04(19) . 2_655 ? O7 Mo1 O2 97.04(19) 2_655 . ? O7 Mo1 O2 97.47(19) . . ? O2 Mo1 O2 156.2(2) 2_655 . ? O7 Mo1 O5 167.1(2) 2_655 2_655 ? O7 Mo1 O5 87.7(2) . 2_655 ? O2 Mo1 O5 84.76(17) 2_655 2_655 ? O2 Mo1 O5 77.04(16) . 2_655 ? O7 Mo1 O5 87.7(2) 2_655 . ? O7 Mo1 O5 167.1(2) . . ? O2 Mo1 O5 77.04(16) 2_655 . ? O2 Mo1 O5 84.76(17) . . ? O5 Mo1 O5 80.3(2) 2_655 . ? O1 I1 O3 97.69(19) . . ? O1 I1 O2 95.4(2) . . ? O3 I1 O2 86.66(19) . . ? O1 I1 O3 96.03(18) . 5_665 ? O3 I1 O3 75.4(2) . 5_665 ? O2 I1 O3 159.80(18) . 5_665 ? O1 I1 O4 177.84(18) . . ? O3 I1 O4 80.23(18) . . ? O2 I1 O4 83.90(17) . . ? O3 I1 O4 84.05(15) 5_665 . ? O6 I2 O4 100.6(2) . . ? O6 I2 O5 100.2(2) . . ? O4 I2 O5 100.3(2) . . ? I1 O1 Ag1 126.3(2) . 5_665 ? I1 O1 Ag1 119.0(2) . 3_545 ? Ag1 O1 Ag1 88.20(13) 5_665 3_545 ? I1 O2 Mo1 130.1(2) . . ? I1 O2 Ag1 103.17(17) . 1_545 ? Mo1 O2 Ag1 122.17(18) . 1_545 ? I1 O3 I1 104.6(2) . 5_665 ? I1 O3 Ag1 108.29(18) . 1_545 ? I1 O3 Ag1 141.1(2) 5_665 1_545 ? I2 O4 I1 124.9(2) . . ? I2 O4 Ag1 116.9(2) . . ? I1 O4 Ag1 117.97(17) . . ? I2 O5 Mo1 131.4(2) . . ? I2 O6 Ag1 124.2(2) . 1_545 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.982 _refine_diff_density_min -1.926 _refine_diff_density_rms 0.323