#------------------------------------------------------------------------------ #$Date: 2008-04-03 13:11:48 +0300 (Thu, 03 Apr 2008) $ #$Revision: 326 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2206023.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2206023 loop_ _publ_author_name 'H\"oss, Patrick' 'Starkulla, Gundula' 'Schleid, Thomas' _publ_section_title ; Lutetium(III) oxotellurate(IV), Lu~2~Te~4~O~11~ ; _journal_issue 6 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first i113 _journal_page_last i115 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac 'Lu2 Te4 O11' _chemical_formula_moiety 'Lu2 O11 Te4' _chemical_formula_sum 'Lu2 O11 Te4' _chemical_formula_weight 1036.34 _chemical_name_common 'lutetium oxotellurate' _chemical_name_systematic 'lutetium(III) oxotellurate(IV)' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 106.202(7) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 12.2953(8) _cell_length_b 5.0596(3) _cell_length_c 15.9134(9) _cell_measurement_reflns_used 3912 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.485 _cell_measurement_theta_min 1.018 _cell_volume 950.64(10) _computing_cell_refinement 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_data_reduction ; SCALEPACK and DENZO (Otwinowski & Minor, 1997) ; _computing_molecular_graphics 'DIAMOND (Brandenburg, 2005)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0963 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 10819 _diffrn_reflns_theta_full 27.57 _diffrn_reflns_theta_max 27.57 _diffrn_reflns_theta_min 2.67 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 32.735 _exptl_absorpt_correction_T_max 0.5394 _exptl_absorpt_correction_T_min 0.3202 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(X-SHAPE; Stoe & Cie, 1998)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 7.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_description spheroid _exptl_crystal_F_000 1752 _exptl_crystal_size_max 0.040 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.019 _exptl_crystal_size_rad 0.018 _refine_diff_density_max 1.859 _refine_diff_density_min -1.382 _refine_ls_extinction_coef 0.00360(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_matrix_type full _refine_ls_number_parameters 79 _refine_ls_number_reflns 1108 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.001 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0336 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0272P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.0739 _reflns_number_gt 791 _reflns_number_total 1108 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file mg6036.cif 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' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Lu Lu -0.4720 5.8584 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Lu 0.11947(4) 0.25158(8) 0.03650(3) 0.01016(19) Uani d . 1 Lu Te1 0.12680(5) 0.27753(16) 0.37376(4) 0.0092(2) Uani d . 1 Te Te2 0.12238(6) 0.72315(17) 0.19938(5) 0.0103(2) Uani d . 1 Te O1 0.2506(6) 0.0593(13) 0.3708(5) 0.0132(16) Uani d . 1 O O2 0.2058(6) 0.5491(13) 0.4468(5) 0.0136(16) Uani d . 1 O O3 0.0700(6) 0.1034(13) 0.4563(5) 0.0155(16) Uani d . 1 O O4 0.4759(6) 0.0809(13) 0.4059(5) 0.0134(16) Uani d . 1 O O5 0.3522(6) 0.5610(13) 0.3336(5) 0.0146(16) Uani d . 1 O O6 0.0000 0.863(2) 0.2500 0.020(2) Uani d S 1 O loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Lu 0.0104(3) 0.0107(3) 0.0096(3) 0.0002(2) 0.00312(18) 0.0003(2) Te1 0.0089(4) 0.0103(4) 0.0086(4) 0.0000(3) 0.0026(3) -0.0008(3) Te2 0.0108(4) 0.0112(4) 0.0089(4) -0.0003(2) 0.0027(3) 0.0020(3) O1 0.013(4) 0.013(4) 0.015(4) -0.001(3) 0.006(3) 0.005(3) O2 0.014(4) 0.015(4) 0.015(4) -0.001(3) 0.008(3) -0.001(3) O3 0.021(4) 0.014(4) 0.010(4) 0.002(3) 0.002(3) 0.002(3) O4 0.012(4) 0.011(4) 0.014(4) -0.001(3) -0.002(3) -0.001(3) O5 0.026(4) 0.011(3) 0.010(4) 0.006(3) 0.010(3) 0.005(3) O6 0.018(6) 0.025(6) 0.021(7) 0.000 0.013(5) 0.000 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Lu O3 6 2.189(7) y Lu O5 4_545 2.218(7) y Lu O2 6_565 2.243(7) y Lu O2 4_545 2.327(7) y Lu O4 4 2.365(7) y Lu O1 4 2.416(7) y Lu O4 8_455 2.471(7) y Lu O3 2 2.480(7) y Lu Te2 . 3.5157(10) ? Lu Te1 6_565 3.5386(9) ? Lu Lu 7 3.7058(9) ? Lu Lu 5_565 3.7942(9) ? Te1 O3 . 1.871(7) y Te1 O2 . 1.885(7) y Te1 O1 . 1.892(7) y Te1 O4 3_455 2.567(7) y Te1 Lu 6_566 3.5385(9) ? Te2 O5 4 1.841(7) y Te2 O4 4 1.912(7) y Te2 O6 . 2.023(4) y Te2 O1 4 2.312(7) y O1 Te2 4_545 2.312(7) ? O1 Lu 4_545 2.416(7) ? O2 Lu 6_566 2.243(7) ? O2 Lu 4 2.327(7) ? O3 Lu 6_556 2.189(7) ? O3 Lu 2 2.480(7) ? O4 Te2 4_545 1.912(7) ? O4 Lu 4_545 2.365(7) ? O4 Lu 8_556 2.471(7) ? O5 Te2 4_545 1.841(7) ? O5 Lu 4 2.218(7) ? O6 Te2 2 2.023(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 Lu O5 6 4_545 97.6(3) ? O3 Lu O2 6 6_565 95.8(3) ? O5 Lu O2 4_545 6_565 144.0(3) ? O3 Lu O2 6 4_545 78.6(3) ? O5 Lu O2 4_545 4_545 78.6(2) ? O2 Lu O2 6_565 4_545 71.6(3) ? O3 Lu O4 6 4 135.8(2) ? O5 Lu O4 4_545 4 84.9(2) ? O2 Lu O4 6_565 4 107.7(2) ? O2 Lu O4 4_545 4 143.9(2) ? O3 Lu O1 6 4 156.0(3) ? O5 Lu O1 4_545 4 78.8(2) ? O2 Lu O1 6_565 4 75.5(2) ? O2 Lu O1 4_545 4 77.4(2) ? O4 Lu O1 4 4 67.9(2) ? O3 Lu O4 6 8_455 76.9(2) ? O5 Lu O4 4_545 8_455 145.3(2) ? O2 Lu O4 6_565 8_455 70.4(2) ? O2 Lu O4 4_545 8_455 131.8(2) ? O4 Lu O4 4 8_455 76.7(3) ? O1 Lu O4 4 8_455 119.2(2) ? O3 Lu O3 6 2 70.5(3) ? O5 Lu O3 4_545 2 74.4(2) ? O2 Lu O3 6_565 2 141.6(2) ? O2 Lu O3 4_545 2 135.3(2) ? O4 Lu O3 4 2 67.7(2) ? O1 Lu O3 4 2 129.5(2) ? O4 Lu O3 8_455 2 71.5(2) ? O3 Lu Te2 6 . 158.54(19) ? O5 Lu Te2 4_545 . 69.00(17) ? O2 Lu Te2 6_565 . 104.77(17) ? O2 Lu Te2 4_545 . 113.29(17) ? O4 Lu Te2 4 . 30.70(16) ? O1 Lu Te2 4 . 40.84(16) ? O4 Lu Te2 8_455 . 104.19(16) ? O3 Lu Te2 2 . 89.28(16) ? O3 Lu Te1 6 6_565 100.68(19) ? O5 Lu Te1 4_545 6_565 160.92(17) ? O2 Lu Te1 6_565 6_565 28.11(17) ? O2 Lu Te1 4_545 6_565 99.73(17) ? O4 Lu Te1 4 6_565 85.76(17) ? O1 Lu Te1 4 6_565 82.28(17) ? O4 Lu Te1 8_455 6_565 46.49(16) ? O3 Lu Te1 2 6_565 116.97(17) ? Te2 Lu Te1 . 6_565 94.907(18) ? O3 Lu Lu 6 7 86.44(19) ? O5 Lu Lu 4_545 7 111.43(19) ? O2 Lu Lu 6_565 7 36.58(17) ? O2 Lu Lu 4_545 7 35.06(16) ? O4 Lu Lu 4 7 133.73(16) ? O1 Lu Lu 4 7 73.23(16) ? O4 Lu Lu 8_455 7 102.45(17) ? O3 Lu Lu 2 7 156.94(16) ? Te2 Lu Lu . 7 113.74(2) ? Te1 Lu Lu 6_565 7 64.681(15) ? O3 Lu Lu 6 5_565 107.42(19) ? O5 Lu Lu 4_545 5_565 118.71(18) ? O2 Lu Lu 6_565 5_565 88.33(17) ? O2 Lu Lu 4_545 5_565 159.70(16) ? O4 Lu Lu 4 5_565 39.33(17) ? O1 Lu Lu 4 5_565 94.79(16) ? O4 Lu Lu 8_455 5_565 37.33(16) ? O3 Lu Lu 2 5_565 63.74(16) ? Te2 Lu Lu . 5_565 67.902(17) ? Te1 Lu Lu 6_565 5_565 60.361(17) ? Lu Lu Lu 7 5_565 124.84(2) ? O3 Te1 O2 . . 98.1(3) ? O3 Te1 O1 . . 101.7(3) ? O2 Te1 O1 . . 99.2(3) ? O3 Te1 Lu . 6_566 73.3(2) ? O1 Te1 Lu . 6_566 126.6(2) ? O5 Te2 O4 4 4 102.5(3) ? O5 Te2 O6 4 . 89.6(3) ? O4 Te2 O6 4 . 97.0(2) ? O5 Te2 O1 4 4 90.2(3) ? O4 Te2 O1 4 4 77.8(3) ? O6 Te2 O1 . 4 174.65(18) ? O5 Te2 Lu 4 . 112.8(2) ? O6 Te2 Lu . . 132.52(18) ? Te1 O1 Te2 . 4_545 117.3(3) ? Te1 O1 Lu . 4_545 139.5(4) ? Te2 O1 Lu 4_545 4_545 96.1(2) ? Te1 O2 Lu . 6_566 117.8(3) ? Te1 O2 Lu . 4 133.8(3) ? Lu O2 Lu 6_566 4 108.4(3) ? Te1 O3 Lu . 6_556 134.3(4) ? Te1 O3 Lu . 2 115.4(3) ? Lu O3 Lu 6_556 2 109.5(3) ? Te2 O4 Lu 4_545 4_545 110.1(3) ? Te2 O4 Lu 4_545 8_556 137.4(3) ? Lu O4 Lu 4_545 8_556 103.3(3) ? Te2 O5 Lu 4_545 4 132.4(4) ? Te2 O6 Te2 2 . 138.9(5) y