# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Jiang-Gao Mao' 'Chun-Li Hu' 'Ting Hu' 'Fang Kong' 'Yong Zhou' _publ_contact_author_name 'Jiang-Gao Mao' _publ_contact_author_email MJG@MS.FJIRSM.AC.CN _publ_section_title ; Explorations of new second-order NLO materials in the AgI-MoVI/WVI-TeIV-O Systems ; # Attachment 'Ag2Mo3Te3O16.CIF' data_Ag2Mo3Te3O16 _database_code_depnum_ccdc_archive 'CCDC 720733' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ag2 Mo3 O16 Te3' _chemical_formula_weight 1142.36 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' 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M I2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 7.398(6) _cell_length_b 11.296(8) _cell_length_c 8.245(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.730(11) _cell_angle_gamma 90.00 _cell_volume 682.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 495 _cell_measurement_theta_min 3.0755 _cell_measurement_theta_max 27.4379 _exptl_crystal_description Brick _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 11.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5000 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 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_% <1.0% _diffrn_reflns_number 2212 _diffrn_reflns_av_R_equivalents 0.1022 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 27.45 _reflns_number_total 1042 _reflns_number_gt 1032 _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^)+(0.0821P)^2^+7.7208P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0080(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.58(9) _refine_ls_number_reflns 1042 _refine_ls_number_parameters 113 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1294 _refine_ls_wR_factor_gt 0.1290 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.134 _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 1.0000 0.39924(18) 1.5000 0.0203(6) Uani 1 2 d S . . Ag2 Ag 1.0000 0.4743(2) 1.0000 0.0380(9) Uani 1 2 d S . . Mo1 Mo 1.24300(17) 0.16115(13) 0.77342(16) 0.0086(4) Uani 1 1 d . . . Mo2 Mo 1.0000 -0.00065(18) 1.0000 0.0075(5) Uani 1 2 d S . . Te1 Te 1.5000 0.40818(11) 1.0000 0.0083(4) Uani 1 2 d S . . Te2 Te 1.22436(12) 0.24353(10) 1.22228(12) 0.0097(3) Uani 1 1 d . . . O1 O 1.6004(14) 0.2992(11) 1.1619(15) 0.020(3) Uani 1 1 d . . . O2 O 1.2650(13) 0.3846(10) 1.1045(12) 0.010(2) Uani 1 1 d . . . O3 O 0.9854(12) 0.2896(10) 1.2264(15) 0.016(2) Uani 1 1 d . . . O4 O 1.1901(12) 0.1518(10) 1.0268(11) 0.0089(18) Uani 1 1 d . . . O5 O 1.4169(15) 0.0602(13) 0.8093(19) 0.031(3) Uani 1 1 d . . . O6 O 1.2174(14) 0.1724(12) 0.5670(14) 0.022(3) Uani 1 1 d . . . O7 O 1.0401(13) 0.0495(10) 0.7837(13) 0.011(2) Uani 1 1 d . . . O8 O 1.1792(15) -0.0962(12) 1.0532(14) 0.019(3) 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 0.0208(8) 0.0169(13) 0.0242(12) 0.000 0.0061(8) 0.000 Ag2 0.0201(13) 0.0205(19) 0.069(2) 0.000 -0.0091(12) 0.000 Mo1 0.0096(5) 0.0043(7) 0.0119(6) -0.0017(7) 0.0017(4) -0.0014(5) Mo2 0.0073(11) 0.0020(10) 0.0129(13) 0.000 0.0003(8) 0.000 Te1 0.0090(6) 0.0029(7) 0.0131(9) 0.000 0.0023(5) 0.000 Te2 0.0119(4) 0.0062(5) 0.0111(5) -0.0018(5) 0.0022(3) -0.0011(5) O1 0.019(5) 0.009(6) 0.032(7) 0.009(6) 0.002(5) -0.002(4) O2 0.014(4) 0.007(5) 0.011(5) 0.001(4) 0.005(4) -0.001(4) O3 0.011(4) 0.008(6) 0.032(6) 0.000(5) 0.010(4) 0.002(4) O4 0.015(4) 0.003(5) 0.008(4) -0.001(5) 0.000(3) -0.004(4) O5 0.020(5) 0.017(7) 0.054(9) -0.004(7) 0.001(6) 0.005(5) O6 0.027(5) 0.018(7) 0.020(6) -0.002(5) 0.004(4) -0.011(5) O7 0.018(4) 0.012(6) 0.006(5) 0.006(4) 0.006(4) -0.001(4) O8 0.024(5) 0.016(6) 0.020(6) -0.012(5) 0.010(5) 0.000(5) _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 2.428(16) 4_757 ? Ag1 O5 2.428(16) 3_455 ? Ag1 O8 2.472(11) 3_455 ? Ag1 O8 2.472(11) 4_757 ? Ag1 O3 2.563(12) . ? Ag1 O3 2.563(12) 2_758 ? Ag2 O2 2.271(10) 2_757 ? Ag2 O2 2.271(10) . ? Mo1 O6 1.692(12) . ? Mo1 O5 1.715(13) . ? Mo1 O7 1.971(11) . ? Mo1 O1 1.973(12) 2_857 ? Mo1 O4 2.179(9) . ? Mo1 O3 2.227(10) 2_757 ? Mo2 O8 1.720(13) 2_757 ? Mo2 O8 1.720(13) . ? Mo2 O7 1.932(10) 2_757 ? Mo2 O7 1.932(10) . ? Mo2 O4 2.215(10) . ? Mo2 O4 2.215(10) 2_757 ? Te1 O1 1.893(12) 2_857 ? Te1 O1 1.893(12) . ? Te1 O2 2.059(9) . ? Te1 O2 2.059(9) 2_857 ? Te2 O3 1.848(9) . ? Te2 O4 1.904(10) . ? Te2 O2 1.910(11) . ? O1 Mo1 1.973(12) 2_857 ? O3 Mo1 2.227(10) 2_757 ? O5 Ag1 2.428(16) 3_544 ? O8 Ag1 2.472(11) 3_544 ? 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 83.0(7) 4_757 3_455 ? O5 Ag1 O8 92.0(4) 4_757 3_455 ? O5 Ag1 O8 86.2(4) 3_455 3_455 ? O5 Ag1 O8 86.2(4) 4_757 4_757 ? O5 Ag1 O8 92.0(4) 3_455 4_757 ? O8 Ag1 O8 177.6(6) 3_455 4_757 ? O5 Ag1 O3 155.3(4) 4_757 . ? O5 Ag1 O3 79.3(4) 3_455 . ? O8 Ag1 O3 103.8(3) 3_455 . ? O8 Ag1 O3 77.4(4) 4_757 . ? O5 Ag1 O3 79.3(4) 4_757 2_758 ? O5 Ag1 O3 155.3(4) 3_455 2_758 ? O8 Ag1 O3 77.4(4) 3_455 2_758 ? O8 Ag1 O3 103.8(3) 4_757 2_758 ? O3 Ag1 O3 122.2(5) . 2_758 ? O2 Ag2 O2 127.0(6) 2_757 . ? O6 Mo1 O5 101.8(7) . . ? O6 Mo1 O7 96.2(5) . . ? O5 Mo1 O7 97.2(6) . . ? O6 Mo1 O1 101.2(5) . 2_857 ? O5 Mo1 O1 94.5(5) . 2_857 ? O7 Mo1 O1 156.5(4) . 2_857 ? O6 Mo1 O4 163.3(4) . . ? O5 Mo1 O4 91.7(6) . . ? O7 Mo1 O4 72.0(4) . . ? O1 Mo1 O4 87.4(4) 2_857 . ? O6 Mo1 O3 88.2(5) . 2_757 ? O5 Mo1 O3 170.0(6) . 2_757 ? O7 Mo1 O3 80.5(4) . 2_757 ? O1 Mo1 O3 84.4(4) 2_857 2_757 ? O4 Mo1 O3 78.3(4) . 2_757 ? O8 Mo2 O8 102.2(9) 2_757 . ? O8 Mo2 O7 102.2(5) 2_757 2_757 ? O8 Mo2 O7 99.1(5) . 2_757 ? O8 Mo2 O7 99.1(5) 2_757 . ? O8 Mo2 O7 102.2(5) . . ? O7 Mo2 O7 145.9(7) 2_757 . ? O8 Mo2 O4 166.0(5) 2_757 . ? O8 Mo2 O4 90.3(5) . . ? O7 Mo2 O4 81.6(4) 2_757 . ? O7 Mo2 O4 71.9(4) . . ? O8 Mo2 O4 90.3(5) 2_757 2_757 ? O8 Mo2 O4 166.0(5) . 2_757 ? O7 Mo2 O4 71.9(4) 2_757 2_757 ? O7 Mo2 O4 81.6(4) . 2_757 ? O4 Mo2 O4 78.0(5) . 2_757 ? O1 Te1 O1 98.9(8) 2_857 . ? O1 Te1 O2 86.4(5) 2_857 . ? O1 Te1 O2 83.9(4) . . ? O1 Te1 O2 83.9(4) 2_857 2_857 ? O1 Te1 O2 86.4(5) . 2_857 ? O2 Te1 O2 165.1(6) . 2_857 ? O3 Te2 O4 98.6(5) . . ? O3 Te2 O2 89.5(5) . . ? O4 Te2 O2 92.1(4) . . ? Te1 O1 Mo1 149.9(7) . 2_857 ? Te2 O2 Te1 121.3(5) . . ? Te2 O2 Ag2 112.2(4) . . ? Te1 O2 Ag2 121.2(5) . . ? Te2 O3 Mo1 123.0(6) . 2_757 ? Te2 O3 Ag1 103.0(5) . . ? Mo1 O3 Ag1 104.9(4) 2_757 . ? Te2 O4 Mo1 139.8(5) . . ? Te2 O4 Mo2 121.2(4) . . ? Mo1 O4 Mo2 97.8(4) . . ? Mo1 O5 Ag1 136.7(7) . 3_544 ? Mo2 O7 Mo1 116.1(6) . . ? Mo2 O8 Ag1 133.9(7) . 3_544 ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 3.284 _refine_diff_density_min -3.238 _refine_diff_density_rms 0.696 # Attachment 'Ag2MoTe4O12.CIF' data_Ag2MoTe4O12 _database_code_depnum_ccdc_archive 'CCDC 720734' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ag2 Mo O12 Te4' _chemical_formula_weight 1014.08 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' 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M c2/c 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 17.598(4) _cell_length_b 5.8063(7) _cell_length_c 11.3908(16) _cell_angle_alpha 90.00 _cell_angle_beta 104.276(10) _cell_angle_gamma 90.00 _cell_volume 1128.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1769 _cell_measurement_theta_min 2.6335 _cell_measurement_theta_max 27.4680 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0400 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.972 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 14.735 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4531 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Saturn70 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0% _diffrn_reflns_number 4127 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.46 _reflns_number_total 1268 _reflns_number_gt 1123 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0539P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1268 _refine_ls_number_parameters 87 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0926 _refine_ls_wR_factor_gt 0.0611 _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 Te1 Te 0.15520(3) 0.17226(9) 0.43070(4) 0.01032(18) Uani 1 1 d . . . Te2 Te 0.09323(3) -0.27801(8) 0.59416(4) 0.01003(18) Uani 1 1 d . . . Ag1 Ag 0.28638(4) 0.21968(11) 0.22833(6) 0.0198(2) Uani 1 1 d . . . Mo1 Mo 0.0000 0.15851(14) 0.7500 0.0091(2) Uani 1 2 d S . . O4 O 0.0108(3) -0.1284(9) 0.6334(5) 0.0138(11) Uani 1 1 d . . . O1 O 0.1083(3) -0.0973(8) 0.3351(4) 0.0125(11) Uani 1 1 d . . . O2 O 0.2544(3) 0.0693(10) 0.4259(5) 0.0157(11) Uani 1 1 d . . . O6 O 0.0219(3) 0.3431(9) 0.6447(5) 0.0203(13) Uani 1 1 d . . . O3 O 0.1564(3) -0.0096(9) 0.5833(5) 0.0166(11) Uani 1 1 d . . . O5 O 0.1535(3) -0.3442(9) 0.7504(5) 0.0135(11) 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 Te1 0.0111(3) 0.0092(3) 0.0107(3) -0.00133(17) 0.0027(2) -0.00090(15) Te2 0.0114(3) 0.0104(3) 0.0079(3) -0.00152(17) 0.0016(2) 0.00046(17) Ag1 0.0162(3) 0.0155(3) 0.0296(4) 0.0065(3) 0.0093(3) 0.0018(2) Mo1 0.0100(4) 0.0056(4) 0.0103(5) 0.000 -0.0004(3) 0.000 O4 0.011(2) 0.015(2) 0.016(3) -0.005(2) 0.005(2) 0.001(2) O1 0.012(2) 0.010(2) 0.014(3) -0.002(2) -0.001(2) -0.0005(19) O2 0.010(2) 0.021(3) 0.017(3) -0.001(2) 0.004(2) 0.002(2) O6 0.018(3) 0.016(3) 0.022(3) 0.006(2) -0.003(2) -0.006(2) O3 0.022(3) 0.016(3) 0.012(2) 0.001(2) 0.005(2) -0.006(2) O5 0.017(3) 0.013(2) 0.010(3) -0.001(2) 0.002(2) 0.002(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 Te1 O2 1.859(5) . ? Te1 O1 1.968(5) . ? Te1 O3 2.029(5) . ? Te1 O5 2.278(5) 6 ? Te1 O2 2.483(5) 7_556 ? Te2 O4 1.838(5) . ? Te2 O5 1.873(5) . ? Te2 O3 1.935(5) . ? Ag1 O1 2.397(5) 4 ? Ag1 O5 2.409(5) 7_546 ? Ag1 O5 2.519(5) 6 ? Ag1 Ag1 3.2593(7) 4_545 ? Ag1 Ag1 3.2593(7) 4 ? Mo1 O6 1.722(6) . ? Mo1 O6 1.722(6) 2_556 ? Mo1 O1 1.946(5) 6_556 ? Mo1 O1 1.946(5) 5_556 ? Mo1 O4 2.168(5) . ? Mo1 O4 2.168(5) 2_556 ? O1 Mo1 1.946(5) 5_556 ? O1 Ag1 2.397(5) 4_545 ? O2 Te1 2.483(5) 7_556 ? O5 Te1 2.278(5) 6_556 ? O5 Ag1 2.409(5) 7_546 ? O5 Ag1 2.519(5) 6_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 O2 Te1 O1 89.8(2) . . ? O2 Te1 O3 92.7(2) . . ? O1 Te1 O3 88.5(2) . . ? O2 Te1 O5 85.3(2) . 6 ? O1 Te1 O5 86.52(19) . 6 ? O3 Te1 O5 174.6(2) . 6 ? O2 Te1 O2 76.1(2) . 7_556 ? O1 Te1 O2 163.24(18) . 7_556 ? O3 Te1 O2 83.21(19) . 7_556 ? O5 Te1 O2 101.07(18) 6 7_556 ? O4 Te2 O5 99.3(2) . . ? O4 Te2 O3 97.8(2) . . ? O5 Te2 O3 91.5(2) . . ? O1 Ag1 O5 94.50(17) 4 7_546 ? O1 Ag1 O5 135.12(16) 4 6 ? O5 Ag1 O5 130.19(18) 7_546 6 ? O1 Ag1 Ag1 143.34(12) 4 4_545 ? O5 Ag1 Ag1 50.05(13) 7_546 4_545 ? O5 Ag1 Ag1 80.30(12) 6 4_545 ? O1 Ag1 Ag1 90.72(12) 4 4 ? O5 Ag1 Ag1 165.91(13) 7_546 4 ? O5 Ag1 Ag1 47.17(12) 6 4 ? Ag1 Ag1 Ag1 125.93(4) 4_545 4 ? O6 Mo1 O6 103.0(4) . 2_556 ? O6 Mo1 O1 95.8(2) . 6_556 ? O6 Mo1 O1 97.3(2) 2_556 6_556 ? O6 Mo1 O1 97.3(2) . 5_556 ? O6 Mo1 O1 95.8(2) 2_556 5_556 ? O1 Mo1 O1 159.0(3) 6_556 5_556 ? O6 Mo1 O4 89.0(2) . . ? O6 Mo1 O4 166.8(3) 2_556 . ? O1 Mo1 O4 86.68(19) 6_556 . ? O1 Mo1 O4 77.1(2) 5_556 . ? O6 Mo1 O4 166.8(3) . 2_556 ? O6 Mo1 O4 89.0(2) 2_556 2_556 ? O1 Mo1 O4 77.1(2) 6_556 2_556 ? O1 Mo1 O4 86.68(19) 5_556 2_556 ? O4 Mo1 O4 79.6(3) . 2_556 ? Te2 O4 Mo1 134.9(3) . . ? Mo1 O1 Te1 130.3(3) 5_556 . ? Mo1 O1 Ag1 120.3(2) 5_556 4_545 ? Te1 O1 Ag1 105.6(2) . 4_545 ? Te1 O2 Te1 103.9(2) . 7_556 ? Te2 O3 Te1 126.1(2) . . ? Te2 O5 Te1 130.2(3) . 6_556 ? Te2 O5 Ag1 114.4(2) . 7_546 ? Te1 O5 Ag1 113.5(2) 6_556 7_546 ? Te2 O5 Ag1 99.7(2) . 6_556 ? Te1 O5 Ag1 99.08(18) 6_556 6_556 ? Ag1 O5 Ag1 82.78(16) 7_546 6_556 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.327 _refine_diff_density_min -1.270 _refine_diff_density_rms 0.320 # Attachment 'Ag6W3Te4O20.CIF' data_Ag6W3Te4O20 _database_code_depnum_ccdc_archive 'CCDC 720735' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ag6 O20 Te4 W3' _chemical_formula_weight 2029.17 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 29.792(9) _cell_length_b 6.7016(19) _cell_length_c 9.534(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.745(6) _cell_angle_gamma 90.00 _cell_volume 1902.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2768 _cell_measurement_theta_min 2.1370 _cell_measurement_theta_max 27.4642 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.0400 _exptl_crystal_size_min 0.0300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 7.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3488 _exptl_absorpt_coefficient_mu 30.201 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6139 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Saturn70 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7107 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2157 _reflns_number_gt 2031 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0200P)^2^+6.7080P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2157 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0194 _refine_ls_R_factor_gt 0.0174 _refine_ls_wR_factor_ref 0.0395 _refine_ls_wR_factor_gt 0.0388 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.002 _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 W1 W 0.0000 0.06644(4) 0.2500 0.00945(7) Uani 1 2 d S . . W2 W 0.165061(6) 0.18745(3) -0.15378(2) 0.00897(6) Uani 1 1 d . . . Te2 Te 0.079822(10) 0.13932(4) -0.46169(3) 0.00922(8) Uani 1 1 d . . . Te1 Te 0.229736(10) 0.13100(4) 0.14640(3) 0.00873(8) Uani 1 1 d . . . Ag1 Ag -0.031757(17) -0.39228(7) 0.09792(5) 0.03341(13) Uani 1 1 d . . . Ag2 Ag 0.106985(15) 0.35258(6) 0.20544(5) 0.02283(10) Uani 1 1 d . . . Ag3 Ag 0.18424(2) 0.66708(8) -0.00644(6) 0.03879(14) Uani 1 1 d . . . O1 O 0.22781(11) 0.0862(5) -0.0515(3) 0.0102(7) Uani 1 1 d . . . O6 O 0.02960(11) 0.1922(5) -0.3511(4) 0.0118(7) Uani 1 1 d . . . O3 O 0.29098(11) 0.0565(5) 0.1640(3) 0.0120(7) Uani 1 1 d . . . O4 O 0.04682(11) 0.0047(5) -0.6111(3) 0.0144(7) Uani 1 1 d . . . O5 O 0.08389(12) 0.3840(5) -0.5473(4) 0.0167(8) Uani 1 1 d . . . O2 O 0.20793(11) -0.1320(5) 0.1781(3) 0.0127(7) Uani 1 1 d . . . O7 O 0.14710(12) -0.0647(5) -0.1614(4) 0.0175(8) Uani 1 1 d . . . O10 O 0.03235(13) 0.2294(6) 0.1519(4) 0.0215(8) Uani 1 1 d . . . O9 O 0.14979(12) 0.2593(6) 0.0168(4) 0.0202(8) Uani 1 1 d . . . O8 O 0.12525(12) 0.3099(5) -0.2672(4) 0.0178(8) 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 W1 0.01040(13) 0.00986(13) 0.00806(14) 0.000 -0.00008(10) 0.000 W2 0.00837(10) 0.00936(10) 0.00914(11) -0.00075(7) -0.00042(7) 0.00009(6) Te2 0.00859(15) 0.00923(15) 0.00982(16) 0.00052(12) -0.00025(11) 0.00024(11) Te1 0.00993(15) 0.00843(15) 0.00783(15) 0.00014(11) 0.00028(11) -0.00006(11) Ag1 0.0426(3) 0.0240(2) 0.0332(3) -0.0015(2) -0.0058(2) -0.0188(2) Ag2 0.0277(2) 0.0192(2) 0.0221(2) -0.00280(17) 0.00932(18) -0.00394(16) Ag3 0.0605(4) 0.0274(3) 0.0283(3) -0.0161(2) -0.0015(2) 0.0136(2) O1 0.0103(16) 0.0129(16) 0.0073(16) 0.0000(13) -0.0011(13) 0.0000(12) O6 0.0099(16) 0.0135(17) 0.0121(18) 0.0002(14) 0.0025(13) 0.0003(12) O3 0.0118(17) 0.0119(17) 0.0121(17) 0.0004(14) -0.0020(13) 0.0036(12) O4 0.0150(17) 0.0169(18) 0.0110(18) -0.0039(15) -0.0029(14) -0.0005(14) O5 0.0201(19) 0.0092(16) 0.021(2) 0.0064(15) 0.0037(15) 0.0007(14) O2 0.0190(18) 0.0092(16) 0.0098(17) 0.0000(14) -0.0009(13) -0.0048(13) O7 0.0170(19) 0.0123(18) 0.023(2) -0.0023(15) 0.0004(15) -0.0031(13) O10 0.025(2) 0.023(2) 0.0158(19) 0.0043(16) -0.0021(16) -0.0069(16) O9 0.023(2) 0.024(2) 0.0136(19) -0.0020(16) 0.0038(15) 0.0017(16) O8 0.0144(18) 0.0176(19) 0.021(2) -0.0012(15) -0.0055(15) 0.0018(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 W1 O10 1.747(4) . ? W1 O10 1.747(4) 2 ? W1 O4 1.938(3) 2_554 ? W1 O4 1.938(3) 1_556 ? W1 O6 2.183(3) 5 ? W1 O6 2.183(3) 6_556 ? W2 O9 1.769(4) . ? W2 O7 1.773(3) . ? W2 O8 1.781(3) . ? W2 O2 2.112(3) 6 ? W2 O3 2.162(3) 7 ? W2 O1 2.190(3) . ? Te2 O5 1.837(3) . ? Te2 O6 1.890(3) . ? Te2 O4 1.930(3) . ? Te1 O3 1.894(3) . ? Te1 O2 1.906(3) . ? Te1 O1 1.910(3) . ? Te1 O1 2.466(3) 7 ? Ag1 O5 2.202(3) 2_544 ? Ag1 O6 2.307(3) 6_556 ? Ag1 Ag1 3.0604(12) 5_545 ? Ag2 O9 2.322(4) . ? Ag2 O8 2.339(4) 6_566 ? Ag2 O10 2.412(4) . ? Ag2 O5 2.484(4) 1_556 ? Ag2 O7 2.583(3) 6_556 ? Ag3 O3 2.262(3) 7 ? Ag3 O2 2.309(3) 1_565 ? Ag3 O7 2.557(4) 1_565 ? O1 Te1 2.466(3) 7 ? O6 W1 2.183(3) 5 ? O6 Ag1 2.307(3) 6 ? O3 W2 2.162(3) 7 ? O3 Ag3 2.262(3) 7 ? O4 W1 1.938(3) 1_554 ? O5 Ag1 2.202(3) 2_564 ? O5 Ag2 2.484(4) 1_554 ? O2 W2 2.112(3) 6_556 ? O2 Ag3 2.309(3) 1_545 ? O7 Ag3 2.557(4) 1_545 ? O7 Ag2 2.583(3) 6 ? O8 Ag2 2.339(4) 6_565 ? 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 O10 W1 O10 102.6(3) . 2 ? O10 W1 O4 99.50(16) . 2_554 ? O10 W1 O4 95.85(16) 2 2_554 ? O10 W1 O4 95.85(16) . 1_556 ? O10 W1 O4 99.50(16) 2 1_556 ? O4 W1 O4 155.3(2) 2_554 1_556 ? O10 W1 O6 165.93(16) . 5 ? O10 W1 O6 91.32(15) 2 5 ? O4 W1 O6 80.80(13) 2_554 5 ? O4 W1 O6 79.67(13) 1_556 5 ? O10 W1 O6 91.32(15) . 6_556 ? O10 W1 O6 165.93(16) 2 6_556 ? O4 W1 O6 79.67(13) 2_554 6_556 ? O4 W1 O6 80.80(13) 1_556 6_556 ? O6 W1 O6 74.84(17) 5 6_556 ? O9 W2 O7 102.19(17) . . ? O9 W2 O8 104.35(17) . . ? O7 W2 O8 102.70(16) . . ? O9 W2 O2 157.49(15) . 6 ? O7 W2 O2 89.43(15) . 6 ? O8 W2 O2 91.56(15) . 6 ? O9 W2 O3 89.93(15) . 7 ? O7 W2 O3 159.49(14) . 7 ? O8 W2 O3 90.00(14) . 7 ? O2 W2 O3 74.00(13) 6 7 ? O9 W2 O1 85.12(15) . . ? O7 W2 O1 88.58(14) . . ? O8 W2 O1 163.13(15) . . ? O2 W2 O1 75.86(12) 6 . ? O3 W2 O1 75.88(12) 7 . ? O5 Te2 O6 98.31(15) . . ? O5 Te2 O4 97.36(16) . . ? O6 Te2 O4 96.04(14) . . ? O3 Te1 O2 94.26(14) . . ? O3 Te1 O1 92.64(14) . . ? O2 Te1 O1 90.64(14) . . ? O3 Te1 O1 74.44(13) . 7 ? O2 Te1 O1 161.85(13) . 7 ? O1 Te1 O1 76.04(13) . 7 ? O5 Ag1 O6 172.38(12) 2_544 6_556 ? O5 Ag1 Ag1 89.44(9) 2_544 5_545 ? O6 Ag1 Ag1 84.38(9) 6_556 5_545 ? O9 Ag2 O8 102.43(13) . 6_566 ? O9 Ag2 O10 105.57(13) . . ? O8 Ag2 O10 124.36(13) 6_566 . ? O9 Ag2 O5 158.77(12) . 1_556 ? O8 Ag2 O5 83.26(12) 6_566 1_556 ? O10 Ag2 O5 87.11(12) . 1_556 ? O9 Ag2 O7 85.57(12) . 6_556 ? O8 Ag2 O7 124.40(12) 6_566 6_556 ? O10 Ag2 O7 104.96(12) . 6_556 ? O5 Ag2 O7 74.59(11) 1_556 6_556 ? O3 Ag3 O2 142.59(12) 7 1_565 ? O3 Ag3 O7 103.08(12) 7 1_565 ? O2 Ag3 O7 98.46(11) 1_565 1_565 ? Te1 O1 W2 113.00(15) . . ? Te1 O1 Te1 103.96(13) . 7 ? W2 O1 Te1 92.22(11) . 7 ? Te2 O6 W1 115.77(15) . 5 ? Te2 O6 Ag1 128.85(17) . 6 ? W1 O6 Ag1 103.09(13) 5 6 ? Te1 O3 W2 111.72(15) . 7 ? Te1 O3 Ag3 116.65(15) . 7 ? W2 O3 Ag3 106.58(14) 7 7 ? Te2 O4 W1 138.08(19) . 1_554 ? Te2 O5 Ag1 130.50(18) . 2_564 ? Te2 O5 Ag2 111.72(16) . 1_554 ? Ag1 O5 Ag2 93.66(12) 2_564 1_554 ? Te1 O2 W2 120.00(17) . 6_556 ? Te1 O2 Ag3 121.07(16) . 1_545 ? W2 O2 Ag3 107.32(14) 6_556 1_545 ? W2 O7 Ag3 121.44(17) . 1_545 ? W2 O7 Ag2 150.05(19) . 6 ? Ag3 O7 Ag2 86.82(11) 1_545 6 ? W1 O10 Ag2 128.37(18) . . ? W2 O9 Ag2 161.5(2) . . ? W2 O8 Ag2 131.43(18) . 6_565 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.351 _refine_diff_density_min -1.442 _refine_diff_density_rms 0.214