#------------------------------------------------------------------------------ #$Date: 2014-07-11 23:16:09 +0100 (Fri, 11 Jul 2014) $ #$Revision: 120081 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/89/4308948.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4308948 loop_ _publ_author_name 'Tyler A. Sullens' 'Thomas E. Albrecht-Schmitt' _publ_section_title ; Structure and Properties of the Thorium Vanadyl Tellurate, Th(VO2)2(TeO6)(H2O)2 ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 2282 _journal_page_last 2286 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety Th(VO2)2(TeO6)(H2O)2 _chemical_formula_sum 'H4 O12 Te Th V2' _chemical_formula_weight 657.55 _chemical_name_common 'thorium vanadyl telurate' _chemical_name_systematic ; ? ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_formula_units_Z 8 _cell_length_a 12.6921(7) _cell_length_b 11.5593(7) _cell_length_c 13.0950(8) _cell_measurement_reflns_used 2382 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 28.29 _cell_measurement_theta_min 2.85 _cell_volume 1921.2(2) _computing_cell_refinement 'SMART, SAINT' _computing_data_collection SMART _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXP-97 (Sheldrick, 1997)' _computing_publication_material 'SHELCIF-97 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 193(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method '0.3 wide w/ exposures' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 18312 _diffrn_reflns_theta_full 28.29 _diffrn_reflns_theta_max 28.29 _diffrn_reflns_theta_min 2.85 _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_number na _exptl_absorpt_coefficient_mu 20.383 _exptl_absorpt_correction_T_max 0.442 _exptl_absorpt_correction_T_min 0.278 _exptl_absorpt_correction_type 'analytical and multiscan' _exptl_absorpt_process_details SADABS _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 4.519 _exptl_crystal_density_meas nm _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'rectangular plate' _exptl_crystal_F_000 2272 _exptl_crystal_size_max 0.110 _exptl_crystal_size_mid 0.054 _exptl_crystal_size_min 0.040 _refine_diff_density_max 3.480 _refine_diff_density_min -1.013 _refine_diff_density_rms 0.246 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 145 _refine_ls_number_reflns 2382 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.084 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0250 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+20.2217P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.0622 _reflns_number_gt 2254 _reflns_number_total 2385 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic048256jsi20050125_020111.cif _[local]_cod_data_source_block face _cod_database_code 4308948 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' 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 Th1 Th 0.156268(15) 0.065122(17) 0.175256(15) 0.00954(7) Uani 1 1 d . . . Te1 Te -0.07545(3) 0.22523(3) 0.25827(3) 0.00934(9) Uani 1 1 d . . . V1 V 0.07358(7) 0.42168(8) 0.20293(8) 0.00947(19) Uani 1 1 d . . . V2 V 0.06217(8) -0.18383(9) -0.00118(8) 0.0151(2) Uani 1 1 d . . . O1 O 0.0589(4) 0.4391(4) 0.0804(4) 0.0243(10) Uani 1 1 d . . . O2 O 0.2011(4) 0.4446(4) 0.2274(4) 0.0188(9) Uani 1 1 d . . . O3 O 0.0266(3) 0.5690(3) 0.2583(3) 0.0106(8) Uani 1 1 d . . . O4 O -0.0731(3) 0.3901(3) 0.2609(3) 0.0104(7) Uani 1 1 d . . . O5 O 0.0693(3) 0.2557(3) 0.2183(3) 0.0110(8) Uani 1 1 d . . . O6 O 0.1467(4) -0.0897(4) 0.0472(4) 0.0213(10) Uani 1 1 d . . . O7 O -0.0505(4) -0.1207(4) -0.0315(4) 0.0246(10) Uani 1 1 d . . . O8 O 0.1206(3) -0.2326(4) -0.1162(3) 0.0139(8) Uani 1 1 d . . . O9 O 0.0342(3) -0.2868(3) 0.0984(3) 0.0142(8) Uani 1 1 d . . . O10 O -0.2123(3) 0.1950(3) 0.2929(3) 0.0128(8) Uani 1 1 d . . . O11 O 0.2723(4) 0.0941(4) 0.0170(4) 0.0269(11) Uani 1 1 d . . . O12 O 0.1694(4) 0.0951(4) 0.3717(3) 0.0203(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 Th1 0.00800(11) 0.00710(11) 0.01351(11) -0.00009(7) 0.00003(7) -0.00033(7) Te1 0.00935(16) 0.00700(17) 0.01165(17) -0.00003(12) 0.00057(13) -0.00009(12) V1 0.0071(4) 0.0046(4) 0.0167(5) -0.0018(3) 0.0015(3) 0.0001(3) V2 0.0186(5) 0.0148(5) 0.0120(5) 0.0001(4) -0.0005(4) -0.0003(4) O1 0.036(3) 0.020(2) 0.016(2) 0.0003(18) 0.003(2) 0.000(2) O2 0.014(2) 0.0061(19) 0.036(3) 0.0003(17) 0.0025(19) 0.0005(16) O3 0.0103(19) 0.0070(18) 0.0144(19) -0.0024(14) 0.0006(15) -0.0006(14) O4 0.0109(18) 0.0060(18) 0.0141(19) 0.0012(15) 0.0014(15) 0.0002(14) O5 0.0070(17) 0.0071(18) 0.019(2) 0.0007(15) 0.0020(15) -0.0008(14) O6 0.031(3) 0.017(2) 0.016(2) -0.0019(18) 0.0035(19) -0.0063(19) O7 0.026(3) 0.032(3) 0.015(2) 0.003(2) -0.0006(18) 0.011(2) O8 0.015(2) 0.016(2) 0.0106(19) -0.0011(15) -0.0034(16) 0.0012(16) O9 0.022(2) 0.0099(18) 0.0110(18) 0.0018(15) -0.0037(16) -0.0019(16) O10 0.0095(18) 0.0106(19) 0.018(2) -0.0008(16) 0.0035(16) -0.0018(15) O11 0.030(3) 0.030(3) 0.021(2) -0.002(2) 0.003(2) -0.010(2) O12 0.022(2) 0.025(2) 0.014(2) 0.0020(18) 0.0004(17) 0.0018(19) 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' H H 0.0000 0.0000 '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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Th1 O2 77.13(15) 6_656 8_655 ? O10 Th1 O7 112.10(16) 6_656 5 ? O2 Th1 O7 143.70(17) 8_655 5 ? O10 Th1 O4 143.31(14) 6_656 3_545 ? O2 Th1 O4 75.19(14) 8_655 3_545 ? O7 Th1 O4 104.47(16) 5 3_545 ? O10 Th1 O6 129.84(15) 6_656 . ? O2 Th1 O6 78.89(16) 8_655 . ? O7 Th1 O6 68.40(17) 5 . ? O4 Th1 O6 66.82(14) 3_545 . ? O10 Th1 O3 127.44(14) 6_656 3_545 ? O2 Th1 O3 128.37(14) 8_655 3_545 ? O7 Th1 O3 75.32(15) 5 3_545 ? O4 Th1 O3 59.19(12) 3_545 3_545 ? O6 Th1 O3 101.91(14) . 3_545 ? O10 Th1 O5 72.84(13) 6_656 . ? O2 Th1 O5 140.98(15) 8_655 . ? O7 Th1 O5 72.38(15) 5 . ? O4 Th1 O5 117.35(13) 3_545 . ? O6 Th1 O5 139.99(15) . . ? O3 Th1 O5 59.82(12) 3_545 . ? O10 Th1 O11 69.04(16) 6_656 . ? O2 Th1 O11 82.64(17) 8_655 . ? O7 Th1 O11 69.66(17) 5 . ? O4 Th1 O11 129.50(14) 3_545 . ? O6 Th1 O11 64.66(15) . . ? O3 Th1 O11 144.98(15) 3_545 . ? O5 Th1 O11 108.48(15) . . ? O10 Th1 O12 71.63(15) 6_656 . ? O2 Th1 O12 75.27(16) 8_655 . ? O7 Th1 O12 140.90(15) 5 . ? O4 Th1 O12 78.36(14) 3_545 . ? O6 Th1 O12 140.84(16) . . ? O3 Th1 O12 73.16(14) 3_545 . ? O5 Th1 O12 72.04(14) . . ? O11 Th1 O12 138.18(15) . . ? O10 Th1 Te1 101.61(10) 6_656 . ? O2 Th1 Te1 145.56(12) 8_655 . ? O7 Th1 Te1 69.29(11) 5 . ? O4 Th1 Te1 88.26(9) 3_545 . ? O6 Th1 Te1 122.30(12) . . ? O3 Th1 Te1 29.51(8) 3_545 . ? O5 Th1 Te1 30.43(9) . . ? O11 Th1 Te1 129.71(12) . . ? O12 Th1 Te1 71.86(10) . . ? O10 Te1 O4 101.61(17) . . ? O10 Te1 O3 98.90(17) . 3_545 ? O4 Te1 O3 159.49(17) . 3_545 ? O10 Te1 O5 178.60(19) . . ? O4 Te1 O5 78.98(17) . . ? O3 Te1 O5 80.51(17) 3_545 . ? O10 Te1 O8 88.04(19) . 5 ? O4 Te1 O8 88.73(17) . 5 ? O3 Te1 O8 91.61(17) 3_545 5 ? O5 Te1 O8 90.71(18) . 5 ? O10 Te1 O9 90.20(19) . 3 ? O4 Te1 O9 92.84(17) . 3 ? O3 Te1 O9 87.44(17) 3_545 3 ? O5 Te1 O9 91.04(18) . 3 ? O8 Te1 O9 177.84(18) 5 3 ? O10 Te1 V1 142.37(13) . . ? O3 Te1 V1 118.29(12) 3_545 . ? O8 Te1 V1 85.55(13) 5 . ? O9 Te1 V1 96.61(13) 3 . ? O10 Te1 Th1 138.07(13) . . ? O4 Te1 Th1 120.08(12) . . ? O8 Te1 Th1 88.54(12) 5 . ? O9 Te1 Th1 91.95(13) 3 . ? V1 Te1 Th1 78.82(2) . . ? O1 V1 O2 106.3(3) . . ? O1 V1 O5 102.8(2) . . ? O2 V1 O5 99.47(19) . . ? O1 V1 O3 103.0(2) . . ? O2 V1 O3 94.97(19) . . ? O5 V1 O3 145.41(18) . . ? O1 V1 O4 106.5(2) . . ? O2 V1 O4 147.1(2) . . ? O5 V1 O4 76.02(16) . . ? O3 V1 O4 74.84(17) . . ? O1 V1 Te1 104.82(18) . . ? O2 V1 Te1 132.40(16) . . ? O5 V1 Te1 38.36(11) . . ? O3 V1 Te1 111.97(12) . . ? O4 V1 Te1 38.00(11) . . ? O7 V2 O6 111.2(3) . . ? O7 V2 O8 107.4(2) . . ? O6 V2 O8 105.3(2) . . ? O7 V2 O9 107.1(2) . . ? O6 V2 O9 106.6(2) . . ? O8 V2 O9 119.2(2) . . ? V1 O2 Th1 140.6(3) . 8_665 ? Te1 O3 V1 133.0(2) 3 . ? Te1 O3 Th1 111.02(17) 3 3 ? V1 O3 Th1 113.70(17) . 3 ? Te1 O4 V1 100.70(18) . . ? Te1 O4 Th1 146.3(2) . 3 ? V1 O4 Th1 112.01(17) . 3 ? V1 O5 Te1 103.60(18) . . ? V1 O5 Th1 146.22(19) . . ? Te1 O5 Th1 108.34(17) . . ? V2 O6 Th1 140.7(3) . . ? V2 O7 Th1 142.2(3) . 5 ? V2 O8 Te1 132.5(2) . 5 ? V2 O9 Te1 126.6(2) . 3_545 ? Te1 O10 Th1 149.9(2) . 6_556 ? 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 Th1 O10 2.282(4) 6_656 ? Th1 O2 2.384(4) 8_655 ? Th1 O7 2.400(5) 5 ? Th1 O4 2.430(4) 3_545 ? Th1 O6 2.455(5) . ? Th1 O3 2.479(4) 3_545 ? Th1 O5 2.528(4) . ? Th1 O11 2.564(5) . ? Th1 O12 2.601(5) . ? Th1 Te1 3.6409(4) . ? Te1 O10 1.829(4) . ? Te1 O4 1.907(4) . ? Te1 O3 1.921(4) 3_545 ? Te1 O5 1.943(4) . ? Te1 O8 1.948(4) 5 ? Te1 O9 1.953(4) 3 ? Te1 V1 3.0430(10) . ? V1 O1 1.628(5) . ? V1 O2 1.671(5) . ? V1 O5 1.929(4) . ? V1 O3 1.945(4) . ? V1 O4 2.044(4) . ? V2 O7 1.654(5) . ? V2 O6 1.654(5) . ? V2 O8 1.771(4) . ? V2 O9 1.801(4) . ? O2 Th1 2.384(4) 8_665 ? O3 Te1 1.921(4) 3 ? O3 Th1 2.479(4) 3 ? O4 Th1 2.430(4) 3 ? O7 Th1 2.400(5) 5 ? O8 Te1 1.948(4) 5 ? O9 Te1 1.953(4) 3_545 ? O10 Th1 2.282(4) 6_556 ? _journal_paper_doi 10.1021/ic048256j