#------------------------------------------------------------------------------ #$Date: 2025-01-16 01:17:42 +0200 (Thu, 16 Jan 2025) $ #$Revision: 297336 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/36/1573697.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_1573697 _journal_paper_doi 10.1039/D4SC06620K _chemical_formula_moiety 'O7 S Te Ti' _chemical_formula_sum 'O7 S Te Ti' _chemical_formula_weight 319.56 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_primary dual _audit_creation_date 2023-08-21 _audit_creation_method ; Olex2 1.5 (compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429) ; _audit_update_record ; 2024-06-24 deposited with the CCDC. 2025-01-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 105.062(6) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 4.9516(3) _cell_length_b 7.6029(4) _cell_length_c 7.1865(4) _cell_measurement_reflns_used 2040 _cell_measurement_temperature 300(2) _cell_measurement_theta_max 28.9730 _cell_measurement_theta_min 2.9350 _cell_volume 261.25(3) _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 300(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.842 _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_unetI/netI 0.0460 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.842 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 2750 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.789 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.282 _diffrn_reflns_theta_min 2.935 _exptl_absorpt_coefficient_mu 7.487 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.69894 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 4.062 _exptl_crystal_description block _exptl_crystal_F_000 292 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.831 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.164 _refine_ls_abs_structure_details ; Flack x determined using 446 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_extinction_coef 0.0093(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 92 _refine_ls_number_reflns 1127 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.069 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0232 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0080P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.0453 _reflns_Friedel_coverage 0.750 _reflns_Friedel_fraction_full 0.995 _reflns_Friedel_fraction_max 0.727 _reflns_number_gt 1082 _reflns_number_total 1127 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc06620k2.cif _cod_data_source_block titeso2 _cod_database_code 1573697 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.467 _shelx_estimated_absorpt_t_min 0.420 _olex2_refinement_description ; ; _shelx_res_file ; TITL titeso2_a.res in P2(1) titeso2.res created by SHELXL-2018/3 at 12:45:00 on 21-Aug-2023 REM Old TITL TiTeSO2 in P2(1) REM SHELXT solution in P2(1): R1 0.026, Rweak 0.009, Alpha 0.010 REM 1.606 for 5 systematic absences, Orientation as input REM Flack x = 0.011 ( 0.029 ) from 437 Parsons' quotients REM Formula found by SHELXT: O7 S Ti Te CELL 0.71073 4.9516 7.6029 7.1865 90 105.062 90 ZERR 2 0.0003 0.0004 0.0004 0 0.006 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC O S Te Ti UNIT 14 2 2 2 L.S. 4 PLAN 3 SIZE 0.12 0.12 0.14 TEMP 27(2) CONF list 4 MORE -1 fmap 2 acta REM REM REM WGHT 0.008000 EXTI 0.009251 FVAR 0.62667 TE1 3 0.078104 0.580520 0.409879 11.00000 0.00946 0.01080 = 0.01015 -0.00123 0.00190 0.00053 TI1 4 0.749198 0.643589 0.753224 11.00000 0.00819 0.00901 = 0.00823 0.00003 0.00395 -0.00098 S1 2 0.622555 0.258530 0.943462 11.00000 0.00880 0.01217 = 0.00830 0.00338 0.00368 0.00029 O1 1 0.831258 0.849537 0.641024 11.00000 0.02962 0.01099 = 0.01784 0.00494 0.01146 -0.00001 O2 1 0.879295 0.497770 0.584909 11.00000 0.00959 0.01818 = 0.01503 -0.00508 0.00801 -0.00131 O3 1 0.388002 0.625825 0.613712 11.00000 0.01269 0.01462 = 0.01046 -0.00166 0.00213 -0.00099 O4 1 0.728937 0.437139 0.925646 11.00000 0.02039 0.01229 = 0.01915 0.00436 0.00490 -0.00533 O5 1 0.519291 0.176090 0.755039 11.00000 0.01363 0.02954 = 0.00924 -0.01007 -0.00149 -0.00097 O6 1 0.855577 0.153008 1.058248 11.00000 0.00896 0.01419 = 0.01551 0.00371 0.00004 0.00268 O7 1 0.394010 0.274812 1.039720 11.00000 0.01495 0.01015 = 0.01698 0.00430 0.00760 0.00290 HKLF 4 REM titeso2_a.res in P2(1) REM wR2 = 0.0453, GooF = S = 1.070, Restrained GooF = 1.069 for all data REM R1 = 0.0232 for 1082 Fo > 4sig(Fo) and 0.0244 for all 1127 data REM 92 parameters refined using 1 restraints END WGHT 0.0080 0.0000 REM Highest difference peak 0.831, deepest hole -0.634, 1-sigma level 0.164 Q1 1 0.8408 0.5755 0.6394 11.00000 0.05 0.83 Q2 1 -0.0111 0.6370 0.5194 11.00000 0.05 0.72 Q3 1 0.9646 0.5010 0.4875 11.00000 0.05 0.66 ; _shelx_res_checksum 71274 _shelx_hkl_file ; 0 -9 0 2.76 4.14 0 -9 -1 474.30 41.16 0 -9 1 380.64 38.53 0 -9 -2 600.70 46.73 0 -9 -3 167.27 23.56 0 -8 0 65.73 14.54 0 -8 -1 787.41 52.58 0 -8 -2 139.78 21.09 0 -8 -3 7.69 5.78 0 -8 -3 2.36 3.55 0 -8 -4 635.59 47.54 0 -8 -4 635.46 60.99 0 -7 0 2.11 2.25 0 -7 -1 661.20 44.55 0 -7 2 680.73 35.43 0 -7 -2 740.12 56.71 0 -7 -2 713.41 46.19 0 -7 -3 434.25 46.19 0 -7 -3 511.75 38.91 0 -7 3 515.35 29.20 0 -7 -4 493.16 39.59 0 -7 -4 497.14 51.10 0 -7 -5 309.15 31.99 0 -7 -6 68.92 16.18 0 -6 -1 374.27 34.80 0 -6 -1 322.28 28.05 0 -6 2 818.93 31.04 0 -6 -2 896.23 49.28 0 -6 2 822.64 38.21 0 -6 -3 60.06 11.91 0 -6 -3 57.10 7.33 0 -6 -3 76.31 17.71 0 -6 3 48.78 7.85 0 -6 4 565.93 31.81 0 -6 -4 629.45 42.84 0 -6 -4 574.04 32.66 0 -6 -4 575.87 53.79 0 -6 -5 387.27 35.32 0 -6 -5 422.38 30.79 0 -6 -6 345.70 45.32 0 -6 -6 355.48 35.32 0 -5 0 1.87 1.98 0 -5 0 -1.30 1.95 0 -5 -1 1309.87 59.43 0 -5 -1 1494.18 73.51 0 -5 1 1314.43 52.04 0 -5 -1 1376.81 61.70 0 -5 -2 997.35 51.48 0 -5 -2 1051.65 50.49 0 -5 2 1011.62 42.78 0 -5 -2 1067.25 37.97 0 -5 -2 1040.66 64.40 0 -5 3 1681.90 63.86 0 -5 -3 1729.24 75.19 0 -5 -3 1624.51 90.84 0 -5 -4 466.96 35.09 0 -5 4 460.39 28.48 0 -5 5 480.02 32.08 0 -5 -5 486.63 49.88 0 -5 -5 453.96 36.80 0 -5 -6 256.19 28.32 0 -5 -6 196.06 32.64 0 -5 -7 319.63 42.80 0 -5 -8 378.18 38.49 0 -4 0 1679.18 72.81 0 -4 1 2190.06 74.29 0 -4 -1 2240.64 82.09 0 -4 -1 2217.82 83.01 0 -4 -1 2125.77 92.95 0 -4 2 1090.09 42.04 0 -4 -2 1010.52 48.89 0 -4 -2 1098.43 48.08 0 -4 -3 54.27 10.09 0 -4 -3 57.99 9.39 0 -4 -3 42.53 12.11 0 -4 3 61.37 8.54 0 -4 -4 757.25 44.80 0 -4 4 773.05 40.30 0 -4 -4 845.23 42.28 0 -4 -4 712.81 55.97 0 -4 -5 1046.44 56.87 0 -4 -5 905.34 67.35 0 -4 5 994.20 51.05 0 -4 -6 405.90 44.85 0 -4 -6 469.50 38.44 0 -4 -7 274.90 37.97 0 -4 -8 280.15 38.40 0 -3 0 1.55 1.22 0 -3 0 4.68 2.79 0 -3 1 204.72 12.30 0 -3 -1 183.45 14.63 0 -3 -1 180.28 14.81 0 -3 -1 177.25 18.66 0 -3 -2 1423.62 55.30 0 -3 -2 1368.32 67.37 0 -3 -2 1395.13 56.72 0 -3 2 1382.64 51.48 0 -3 -3 1887.17 70.59 0 -3 -3 1825.74 73.60 0 -3 3 1892.75 69.68 0 -3 -4 1106.08 65.05 0 -3 -4 982.76 50.96 0 -3 -5 126.98 22.07 0 -3 -5 130.24 17.35 0 -3 -6 9.98 7.08 0 -3 -7 318.46 38.91 0 -3 -8 402.66 44.30 0 -3 -9 581.13 53.61 0 -2 0 5059.52 161.67 0 -2 0 5206.85 152.61 0 -2 -1 4098.99 126.53 0 -2 -1 3882.43 133.79 0 -2 1 4021.78 121.86 0 -2 -1 4122.23 125.54 0 -2 -2 130.35 10.88 0 -2 -2 133.17 11.83 0 -2 -3 84.81 13.29 0 -2 -3 69.12 9.62 0 -2 -4 744.28 46.87 0 -2 -4 615.11 36.69 0 -2 -5 1544.12 79.94 0 -2 -6 1700.89 89.02 0 -2 -7 498.47 45.68 0 -2 -8 61.75 16.30 0 -1 0 1.24 0.88 0 -1 -1 61.37 7.04 0 -1 -1 59.95 5.19 0 -1 -1 49.05 5.04 0 -1 -2 1773.68 62.31 0 -1 3 1912.74 61.55 0 -1 -3 1919.54 74.65 0 -1 -3 1808.61 60.47 0 -1 -4 920.53 36.17 0 -1 4 887.09 36.51 0 -1 -4 932.79 49.09 0 -1 -5 53.45 11.60 0 -1 -5 43.66 6.59 0 -1 5 47.36 7.15 0 -1 6 21.35 5.17 0 -1 -6 27.70 5.66 0 -1 -6 18.86 7.96 0 -1 -7 109.36 19.27 0 -1 -8 444.93 41.50 0 0 1 798.39 27.90 0 0 -2 682.13 28.97 0 0 2 694.26 29.00 0 0 -3 831.02 37.52 0 0 -4 216.70 18.48 0 0 4 193.23 15.73 0 0 -4 215.41 16.09 0 0 -5 1616.98 64.00 0 0 5 1543.81 63.93 0 0 -5 1727.40 72.14 0 0 -6 2745.26 113.39 0 0 -6 3071.12 104.82 0 0 6 2834.26 103.72 0 0 -7 30.82 9.96 0 0 -7 26.82 6.70 0 0 8 2.16 3.26 0 0 -8 2.27 2.41 0 0 9 268.51 28.70 0 1 0 3.58 0.99 0 1 1 38.73 5.49 0 1 2 1754.87 65.41 0 1 2 1794.18 61.26 0 1 -3 1961.89 66.20 0 1 3 1956.81 74.94 0 1 3 1961.54 71.39 0 1 -4 869.49 38.82 0 1 4 835.14 44.35 0 1 4 969.32 46.76 0 1 4 930.34 44.22 0 1 -5 49.47 8.47 0 1 5 41.27 8.95 0 1 6 18.01 6.41 0 1 6 18.79 7.06 0 1 -6 16.84 6.12 0 1 -6 24.93 6.99 0 1 -7 99.36 14.41 0 1 -7 92.70 14.72 0 1 7 82.27 14.46 0 1 8 518.05 39.49 0 1 9 561.28 42.89 0 2 0 5317.31 153.60 0 2 0 4922.94 160.30 0 2 -1 3868.97 120.53 0 2 -1 3920.78 119.03 0 2 1 3989.00 129.14 0 2 2 106.98 10.05 0 2 2 96.71 12.34 0 2 2 110.78 10.52 0 2 3 78.74 10.20 0 2 3 70.74 5.06 0 2 3 76.31 11.92 0 2 3 67.08 8.93 0 2 -4 628.11 26.82 0 2 4 684.06 38.03 0 2 4 648.29 40.60 0 2 4 635.55 35.43 0 2 5 1486.18 65.91 0 2 -5 1363.62 53.41 0 2 5 1582.52 73.12 0 2 -6 1552.87 62.42 0 2 6 1653.67 74.23 0 2 -7 525.40 38.80 0 2 -7 543.48 31.22 0 2 7 514.63 38.30 0 2 8 28.44 9.04 0 2 9 55.79 13.17 0 3 0 1.66 1.31 0 3 0 1.08 1.98 0 3 1 170.98 12.95 0 3 -1 172.43 14.61 0 3 -1 211.89 13.29 0 3 2 1572.51 67.35 0 3 2 1547.00 59.01 0 3 -2 1339.29 52.60 0 3 2 1475.45 57.81 0 3 3 1909.50 75.53 0 3 3 2085.08 86.50 0 3 -3 1948.38 60.40 0 3 -3 1992.24 63.41 0 3 3 1911.86 74.67 0 3 3 1900.98 62.00 0 3 4 1078.11 59.84 0 3 4 1097.29 52.96 0 3 4 1099.90 52.04 0 3 -4 1035.94 35.41 0 3 5 144.36 17.46 0 3 -5 123.46 7.91 0 3 6 1.89 2.86 0 3 7 324.98 30.35 0 3 8 419.86 36.48 0 3 -8 477.72 39.70 0 4 0 1672.68 69.01 0 4 0 1561.23 58.45 0 4 1 2267.11 91.85 0 4 1 2183.61 68.79 0 4 -1 2335.97 70.23 0 4 1 2326.86 80.36 0 4 -1 2394.95 86.28 0 4 -1 2240.25 78.23 0 4 -2 1074.23 46.40 0 4 3 57.25 12.52 0 4 -3 82.75 8.84 0 4 3 60.35 10.20 0 4 3 76.05 11.65 0 4 -4 702.44 25.34 0 4 4 772.69 26.61 0 4 4 749.58 42.98 0 4 -4 753.92 26.77 0 4 5 1019.01 54.94 0 4 6 437.58 35.22 0 4 7 296.59 29.87 0 4 -8 225.24 28.62 0 4 8 230.09 27.15 0 5 0 -1.69 1.80 0 5 0 0.95 1.42 0 5 1 1321.51 65.24 0 5 1 1260.35 53.50 0 5 -1 1251.05 51.81 0 5 -1 1214.16 57.95 0 5 -2 1077.75 41.67 0 5 2 1049.93 49.75 0 5 -2 1077.04 49.65 0 5 -3 1637.35 62.72 0 5 4 445.73 33.70 0 5 -4 488.44 19.33 0 5 -4 476.11 21.18 0 5 5 488.08 37.04 0 5 6 223.53 25.38 0 5 7 248.06 28.48 0 5 8 408.55 37.83 0 6 0 1005.95 46.67 0 6 0 993.10 56.58 0 6 1 343.91 24.53 0 6 -1 292.43 26.62 0 6 -1 315.67 22.97 0 6 -2 858.31 33.29 0 6 -2 854.49 46.29 0 6 2 905.65 31.34 0 6 2 905.93 46.51 0 6 -3 49.72 8.57 0 6 3 66.33 11.92 0 6 -3 55.72 8.23 0 6 -4 569.66 34.87 0 6 -4 568.22 26.88 0 6 -5 400.40 31.94 0 6 6 332.40 33.11 0 6 -6 391.67 34.89 0 6 7 121.77 19.92 0 6 -7 112.55 19.81 0 7 0 1.37 2.07 0 7 1 724.70 40.46 0 7 -1 632.71 37.31 0 7 2 695.14 41.21 0 7 -2 649.35 41.85 0 7 -3 523.11 26.05 0 7 3 541.40 24.71 0 7 -3 568.51 34.66 0 7 3 536.98 37.22 0 7 -4 429.66 27.31 0 7 4 416.02 34.75 0 7 5 277.01 29.79 0 7 -5 297.37 26.10 0 8 0 81.80 12.97 0 8 -1 857.14 47.03 0 8 1 890.88 48.83 0 8 2 155.35 19.44 0 8 3 14.07 6.05 0 8 4 613.79 43.92 0 9 0 1.84 1.96 0 9 1 384.52 31.58 0 9 2 549.88 40.21 0 9 3 127.23 18.86 1 -9 -4 96.39 17.40 1 -9 -3 490.83 39.74 1 -9 -2 128.06 24.16 1 -9 -2 110.84 18.34 1 -9 -1 555.19 43.63 -1 -9 1 588.27 49.00 1 -9 0 201.48 25.81 -1 -9 0 234.63 30.12 -1 -9 -1 2.94 3.12 1 -8 -5 80.43 16.07 1 -8 -4 430.52 51.64 1 -8 -4 479.88 38.06 1 -8 -3 606.35 42.82 1 -8 -3 666.16 59.93 1 -8 -2 16.43 6.56 1 -8 -2 3.42 5.13 1 -8 -1 294.11 29.13 1 -8 -1 299.91 33.70 -1 -8 1 323.58 33.96 1 -8 0 785.62 50.69 -1 -8 0 792.40 55.27 -1 -8 -1 164.91 23.42 -1 -8 -2 615.27 46.96 -1 -8 -3 132.54 21.24 1 -7 -6 472.60 40.55 1 -7 -5 19.35 11.53 1 -7 -5 33.67 10.16 1 -7 -4 449.62 35.04 1 -7 -4 332.82 43.93 1 -7 -3 695.97 43.52 1 -7 -3 590.95 55.63 1 -7 -2 369.19 29.88 1 -7 -2 320.35 37.34 1 -7 -1 827.25 48.11 1 -7 -1 818.24 57.82 1 -7 0 376.64 34.06 -1 -7 0 397.52 35.34 -1 -7 -1 6.92 4.90 -1 -7 -2 730.92 49.43 -1 -7 -3 448.37 38.13 -1 -7 -4 292.11 31.79 -1 -7 -5 406.19 38.78 1 -6 -6 177.32 22.91 1 -6 -6 151.62 30.19 1 -6 -5 816.10 69.50 1 -6 -5 837.83 51.18 -1 -6 4 238.52 20.95 -1 -6 4 257.25 15.82 1 -6 -4 201.97 31.67 1 -6 -4 246.93 24.08 -1 -6 3 798.07 35.70 1 -6 -3 853.64 46.51 1 -6 -3 778.65 60.99 -1 -6 3 819.45 33.51 -1 -6 2 8.21 2.07 1 -6 -2 6.27 1.69 1 -6 -2 3.03 2.79 1 -6 -2 8.86 7.03 1 -6 -1 895.79 46.78 1 -6 -1 753.59 53.64 -1 -6 0 434.77 34.57 1 -6 0 452.91 36.14 -1 -6 -1 1006.95 57.16 1 -6 1 1008.58 36.23 1 -6 1 1136.45 55.27 -1 -6 -2 171.51 21.26 -1 -6 -3 677.72 34.23 -1 -6 -3 872.74 51.64 -1 -6 -4 155.26 16.43 -1 -6 -4 127.50 20.03 -1 -6 -5 449.36 34.19 -1 -6 -5 501.12 42.39 1 -5 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23.60 6.94 -4 -3 1 396.95 29.56 4 -3 -1 392.06 34.42 -4 -3 0 829.90 47.43 4 -3 0 873.47 52.19 4 -3 1 921.16 50.58 -4 -3 -1 820.98 49.50 -4 -3 -2 510.75 39.07 4 -3 2 531.22 34.80 -4 -3 -3 68.61 14.55 -4 -3 -3 55.41 13.56 -4 -3 -4 34.84 11.42 -4 -3 -4 17.20 8.09 -4 -2 7 827.86 59.43 4 -2 -7 700.45 59.26 -4 -2 6 194.35 26.16 -4 -2 6 163.11 13.91 4 -2 -5 10.93 7.13 -4 -2 5 28.39 9.08 -4 -2 5 14.97 3.76 4 -2 -4 64.18 11.91 -4 -2 4 38.95 10.11 4 -2 -4 66.25 14.92 -4 -2 3 1133.17 59.25 -4 -2 3 1127.99 51.57 4 -2 -3 1085.93 40.08 4 -2 -2 1948.21 89.78 -4 -2 2 1915.63 76.32 4 -2 -1 1713.62 79.03 -4 -2 1 1580.97 66.92 4 -2 0 1.84 3.40 4 -2 0 1.68 1.19 -4 -2 0 1.41 2.11 4 -2 1 121.21 16.30 4 -2 1 94.77 10.48 -4 -2 -1 125.88 16.36 4 -2 2 509.80 33.25 -4 -2 -2 438.56 34.42 -4 -2 -3 712.69 48.19 -4 -2 -3 678.50 51.30 -4 -2 -4 850.22 60.18 4 -1 -8 3.64 5.49 -4 -1 7 15.80 8.93 -4 -1 7 48.46 8.99 -4 -1 6 380.10 37.05 -4 -1 6 371.40 24.82 4 -1 -5 1366.72 66.56 -4 -1 5 1545.14 79.08 -4 -1 5 1607.31 61.97 4 -1 -4 520.30 40.82 -4 -1 4 509.98 38.17 -4 -1 4 509.35 28.97 4 -1 -3 13.22 2.81 4 -1 -3 6.45 5.13 -4 -1 3 12.75 4.02 4 -1 -3 12.48 4.02 -4 -1 3 13.29 5.73 -4 -1 2 78.39 9.55 4 -1 -2 75.21 14.28 -4 -1 2 71.26 13.20 4 -1 -2 81.04 11.02 4 -1 -2 73.08 8.84 4 -1 -1 157.78 19.53 -4 -1 1 183.54 15.40 4 -1 0 666.84 30.48 -4 -1 0 665.40 35.74 4 -1 1 1510.07 59.44 -4 -1 -1 1471.31 65.48 4 -1 2 271.48 21.63 -4 -1 -2 235.47 23.81 -4 -1 -2 276.78 30.69 -4 -1 -3 2.83 5.22 -4 -1 -4 115.61 21.22 4 0 -8 1706.71 94.21 -4 0 8 1342.56 67.28 -4 0 7 381.15 39.79 -4 0 7 385.40 29.52 4 0 -7 352.11 37.45 4 0 -6 55.86 14.30 -4 0 6 91.02 12.18 -4 0 6 94.01 18.01 -4 0 6 69.44 11.40 4 0 -5 12.01 6.77 -4 0 5 19.20 7.67 -4 0 5 15.89 5.30 -4 0 4 -2.07 0.02 -4 0 4 1.30 2.38 -4 0 3 332.06 29.96 4 0 -3 460.68 35.25 -4 0 3 411.30 19.20 4 0 -3 397.47 19.90 -4 0 3 400.53 27.54 4 0 -3 394.95 24.14 4 0 -2 3480.42 131.26 -4 0 2 3493.25 105.99 4 0 -2 3354.89 112.84 -4 0 2 3340.12 128.54 4 0 -2 3292.60 114.73 -4 0 1 439.29 22.64 4 0 -1 426.65 27.11 4 0 -1 410.42 26.77 -4 0 0 270.47 19.62 4 0 0 240.70 22.05 4 0 1 93.92 14.81 4 0 1 110.71 13.06 4 0 2 6.68 4.74 -4 0 -2 8.02 5.69 -4 0 -3 1318.71 77.39 4 0 3 1339.18 74.77 -4 0 -4 1263.88 76.43 4 0 4 1155.87 71.68 -4 1 9 38.91 10.93 -4 1 8 4.18 3.85 4 1 -7 39.00 11.51 -4 1 7 30.30 8.83 4 1 -6 326.19 32.89 -4 1 6 327.22 27.54 4 1 -5 1529.08 78.90 -4 1 5 1574.94 56.29 -4 1 5 1597.11 70.00 -4 1 4 456.77 16.90 -4 1 4 455.67 16.45 -4 1 3 14.00 5.26 4 1 -3 28.53 5.49 4 1 -2 87.64 10.86 4 1 -2 90.21 10.16 -4 1 2 81.19 13.28 4 1 -1 183.14 16.23 4 1 -1 180.75 17.35 4 1 0 718.36 38.67 4 1 0 626.98 39.22 4 1 1 1507.51 64.09 4 1 1 1452.63 70.83 4 1 2 264.55 28.01 4 1 3 2.61 3.93 4 1 4 126.45 21.96 -4 2 8 715.71 49.25 4 2 -8 700.71 54.26 -4 2 7 681.40 54.35 -4 2 7 686.39 46.20 4 2 -7 634.36 48.56 4 2 -6 144.27 21.63 -4 2 6 162.52 24.61 -4 2 6 187.86 21.83 4 2 -5 22.23 8.20 -4 2 5 17.11 2.81 -4 2 5 16.64 7.60 -4 2 5 14.36 5.75 -4 2 4 58.00 12.39 4 2 -4 60.13 12.79 -4 2 4 69.14 12.59 -4 2 3 1047.34 58.29 -4 2 3 1160.65 58.33 4 2 -2 2036.77 80.12 -4 2 2 2117.72 90.21 4 2 -2 2096.61 72.02 4 2 -1 1427.86 64.76 4 2 -1 1490.27 58.09 4 2 0 -1.69 2.54 -4 2 0 2.38 4.40 4 2 0 2.52 1.89 4 2 1 96.25 15.76 -4 2 -2 491.14 43.30 -4 2 -2 483.34 40.93 4 2 2 382.12 35.18 -4 2 -3 744.97 57.39 -4 2 -3 786.88 56.27 4 2 3 726.00 53.23 -4 2 -4 999.84 70.31 -4 2 -4 989.19 66.78 4 2 4 997.98 67.01 4 3 -8 2.74 4.11 4 3 -7 15.26 7.69 -4 3 7 49.97 14.10 -4 3 7 38.84 10.99 4 3 -6 687.11 47.57 -4 3 6 579.39 47.43 -4 3 6 607.69 43.65 4 3 -5 590.64 42.40 -4 3 5 575.96 43.43 -4 3 5 524.41 39.13 -4 3 4 1210.07 62.63 -4 3 4 1120.78 62.04 -4 3 3 169.85 20.61 -4 3 3 125.30 18.03 -4 3 2 26.66 8.48 4 3 -2 24.16 4.13 4 3 -2 29.87 7.44 4 3 -1 367.06 29.24 -4 3 1 324.12 30.93 4 3 -1 395.65 22.70 -4 3 1 393.54 34.87 -4 3 0 844.38 55.63 4 3 0 875.47 42.51 4 3 0 769.32 47.75 4 3 1 858.94 53.21 -4 3 -2 533.20 47.05 4 3 2 565.08 44.12 4 3 3 43.34 12.75 -4 3 -3 66.81 17.09 -4 3 -3 46.51 12.75 4 3 4 13.01 8.48 -4 3 -4 21.58 10.83 -4 3 -4 17.98 8.45 4 4 -8 252.30 29.83 4 4 -7 395.32 36.39 -4 4 7 401.48 40.42 -4 4 7 350.34 35.92 4 4 -6 280.87 29.36 -4 4 6 270.85 30.57 -4 4 6 263.56 29.24 -4 4 5 2.25 2.40 -4 4 5 6.85 5.42 -4 4 4 463.70 36.93 -4 4 4 396.98 33.74 -4 4 3 496.81 36.42 -4 4 3 473.66 38.17 -4 4 2 648.23 46.04 -4 4 2 649.44 45.75 -4 4 1 544.73 43.16 4 4 -1 581.37 39.63 -4 4 1 607.49 45.05 -4 4 0 442.95 40.49 4 4 0 495.15 37.77 -4 4 -1 50.89 13.22 4 4 1 70.79 14.30 4 4 2 370.09 36.35 -4 4 -3 414.26 44.21 -4 4 -3 460.15 40.21 4 4 3 486.94 44.58 -4 4 -4 582.86 48.01 4 5 -7 148.49 21.51 -4 5 7 191.90 26.82 4 5 -6 294.61 29.83 -4 5 6 252.98 29.06 -4 5 6 266.29 30.71 -4 5 5 681.07 49.03 -4 5 5 678.53 46.84 -4 5 4 311.47 29.04 -4 5 4 334.64 32.57 -4 5 3 574.99 44.22 -4 5 2 26.19 9.17 -4 5 1 180.32 24.57 -4 5 0 700.31 52.49 4 5 0 643.17 46.19 -4 5 -1 596.66 50.35 4 5 1 605.49 46.85 -4 5 -2 272.65 34.33 4 5 2 239.18 29.96 4 6 -6 303.46 31.34 -4 6 6 322.33 31.97 -4 6 5 16.66 7.69 -4 6 4 498.18 36.98 -4 6 3 318.32 32.24 -4 6 2 595.35 46.67 -4 6 2 550.10 46.02 -4 6 1 203.50 27.18 -4 6 1 177.83 25.33 -4 6 0 366.14 38.26 -4 6 -1 92.32 20.05 4 6 1 116.57 20.45 -4 7 3 604.06 46.80 -4 7 2 16.45 7.73 -4 7 1 416.83 40.66 -4 7 0 442.20 44.15 -4 8 2 34.77 11.15 -4 8 1 561.79 49.77 -5 -6 4 11.06 7.21 -5 -6 3 259.14 30.68 5 -6 -3 244.17 36.46 -5 -6 2 374.41 36.80 5 -6 -2 409.07 45.47 -5 -6 1 342.26 34.96 -5 -5 5 204.87 26.17 -5 -5 5 209.50 25.76 -5 -5 4 418.36 37.49 5 -5 -4 457.99 50.40 -5 -5 3 316.06 31.78 5 -5 -3 348.47 42.53 -5 -5 2 233.27 26.91 5 -5 -2 271.12 36.04 -5 -5 1 30.23 9.91 5 -5 -1 17.04 8.90 -5 -5 0 223.98 26.89 -5 -5 -1 434.88 38.80 -5 -4 6 299.49 33.13 -5 -4 5 445.02 39.13 -5 -4 4 6.18 4.38 -5 -4 4 2.36 3.55 -5 -4 3 220.86 24.30 -5 -4 2 467.94 35.85 -5 -4 1 447.53 35.47 -5 -4 0 233.40 25.90 -5 -4 -1 438.21 37.54 -5 -4 -2 53.28 13.31 -5 -3 6 99.54 18.86 -5 -3 5 356.87 35.25 -5 -3 4 599.24 38.95 -5 -3 4 612.35 44.93 5 -3 -4 576.86 50.91 -5 -3 3 858.54 48.10 5 -3 -3 903.97 63.44 5 -3 -2 20.55 8.86 -5 -3 2 24.41 7.17 5 -3 -1 35.49 11.29 -5 -3 1 41.14 9.53 -5 -3 0 374.03 31.34 5 -3 0 466.01 39.11 -5 -3 -1 418.27 34.59 -5 -3 -2 727.08 49.93 -5 -3 -3 347.48 35.27 -5 -2 6 821.65 58.02 5 -2 -5 32.41 11.98 -5 -2 5 34.19 10.50 -5 -2 4 53.52 13.01 5 -2 -4 39.58 12.61 -5 -2 4 44.12 8.74 -5 -2 3 93.38 12.47 5 -2 -3 109.20 19.72 5 -2 -2 665.45 50.33 -5 -2 2 715.05 38.06 5 -2 -2 647.93 34.68 5 -2 -1 1109.36 65.52 -5 -2 1 1107.09 53.16 5 -2 0 783.21 50.91 -5 -2 0 746.95 43.72 5 -2 1 35.85 10.11 -5 -2 -1 49.39 10.90 -5 -2 -2 82.65 15.29 -5 -1 6 43.61 13.17 -5 -1 5 338.60 23.38 -5 -1 5 332.35 25.71 -5 -1 5 395.14 36.82 5 -1 -5 301.69 35.13 5 -1 -4 1497.07 82.14 -5 -1 4 1365.96 75.21 -5 -1 4 1447.31 56.65 5 -1 -3 355.96 34.93 -5 -1 3 286.40 19.20 -5 -1 2 78.95 10.09 5 -1 -2 95.74 17.31 5 -1 -2 101.24 12.14 5 -1 -1 52.98 10.05 -5 -1 1 76.94 10.72 5 -1 -1 88.79 16.36 5 -1 0 80.38 13.73 5 -1 0 84.86 15.11 -5 -1 0 63.95 10.93 5 -1 1 869.31 51.55 5 -1 1 833.65 53.01 5 -1 2 977.36 62.00 5 -1 3 223.67 29.20 -5 0 6 463.81 42.40 -5 0 6 459.47 33.31 5 0 -6 380.28 39.86 -5 0 5 18.61 8.03 -5 0 5 28.16 7.71 5 0 -4 10.65 6.34 -5 0 4 12.30 6.41 -5 0 4 1.66 3.94 -5 0 3 35.92 3.89 -5 0 3 30.93 10.48 5 0 -2 288.52 29.99 5 0 -2 314.89 22.88 5 0 -1 1669.49 72.04 5 0 0 236.23 23.81 5 0 1 19.65 7.37 5 0 2 116.78 19.92 5 0 3 2.90 3.08 -5 1 7 2.04 3.76 5 1 -6 11.89 7.75 -5 1 6 23.47 7.80 5 1 -5 349.50 36.51 -5 1 5 410.69 32.75 5 1 -4 1339.27 75.10 -5 1 4 1467.97 70.38 5 1 -3 338.80 32.93 -5 1 3 296.83 28.34 5 1 -2 109.72 13.69 5 1 -1 63.73 11.38 5 1 0 36.04 9.51 5 1 1 909.34 55.70 5 1 2 906.22 59.16 -5 2 8 272.02 29.65 -5 2 7 673.96 47.16 5 2 -6 705.82 54.26 -5 2 6 838.38 58.87 -5 2 6 826.84 51.54 5 2 -5 39.86 12.05 -5 2 5 31.79 10.21 -5 2 5 46.28 11.29 -5 2 4 54.06 13.15 -5 2 4 54.74 12.20 -5 2 3 84.52 15.33 5 2 -2 724.56 41.56 5 2 -1 1149.62 58.53 5 2 0 727.26 46.78 5 2 1 40.22 11.02 5 2 2 106.64 19.53 -5 3 7 25.80 9.53 -5 3 6 91.92 18.28 5 3 -6 103.27 19.20 -5 3 6 93.76 17.42 -5 3 5 359.77 35.65 5 3 -5 424.20 38.49 -5 3 5 370.50 34.91 -5 3 4 574.72 44.39 -5 3 4 594.27 44.91 -5 3 3 894.68 57.16 5 3 -2 27.31 7.94 5 3 -1 29.45 8.65 5 3 0 383.92 33.60 5 3 1 420.76 37.85 5 3 2 734.48 54.85 -5 4 5 376.34 36.48 -5 4 5 461.29 40.53 -5 4 4 2.45 4.50 -5 4 4 10.77 7.01 -5 4 3 243.33 29.13 -5 4 2 533.45 44.60 5 4 -1 411.48 34.78 5 4 0 248.64 28.03 -5 4 0 238.44 32.44 -5 4 -1 440.88 45.61 5 4 1 389.78 37.86 -5 5 5 248.98 29.04 -5 5 3 397.31 39.56 -5 5 2 287.82 33.36 -5 5 1 12.95 7.71 5 5 -1 18.45 7.76 -5 5 0 235.99 32.93 5 5 0 256.15 29.43 -5 6 2 407.07 42.21 6 -3 -2 371.76 41.21 6 -3 -1 106.96 20.84 6 -2 -2 154.66 24.79 6 -2 -1 400.60 39.58 6 -2 0 622.67 49.00 6 -2 1 427.33 38.44 6 -1 -3 1021.18 68.29 6 -1 -2 243.61 30.53 6 -1 -1 2.72 2.90 6 -1 0 63.19 14.83 6 -1 1 85.85 16.68 6 0 -3 52.92 14.07 6 0 -2 5.51 5.08 6 0 -1 304.57 32.35 6 0 0 917.10 57.91 6 0 0 790.94 50.92 6 0 1 213.44 26.55 -6 1 5 50.33 12.72 6 1 -2 219.60 28.23 6 1 0 48.46 11.55 6 1 1 69.08 15.02 -6 2 6 468.89 41.16 -6 2 5 528.41 43.92 6 2 0 518.77 41.16 -6 3 4 232.66 29.56 6 3 0 2.47 4.56 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 92595 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.07810(9) 0.58052(7) 0.40988(7) 0.01026(18) Uani 1 1 d . . . . . Ti1 Ti 0.7492(3) 0.64359(19) 0.7532(2) 0.0081(3) Uani 1 1 d . . . . . S1 S 0.6226(4) 0.2585(3) 0.9435(3) 0.0095(4) Uani 1 1 d . . . . . O1 O 0.8313(12) 0.8495(7) 0.6410(9) 0.0185(13) Uani 1 1 d . . . . . O2 O 0.8793(10) 0.4978(8) 0.5849(8) 0.0134(12) Uani 1 1 d . . . . . O3 O 0.3880(10) 0.6258(6) 0.6137(8) 0.0128(15) Uani 1 1 d . . . . . O4 O 0.7289(11) 0.4371(7) 0.9256(9) 0.0173(13) Uani 1 1 d . . . . . O5 O 0.5193(10) 0.1761(8) 0.7550(8) 0.0183(13) Uani 1 1 d . . . . . O6 O 0.8556(10) 0.1530(8) 1.0582(8) 0.0135(12) Uani 1 1 d . . . . . O7 O 0.3940(10) 0.2748(8) 1.0397(8) 0.0134(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 Te1 0.0095(3) 0.0108(3) 0.0101(3) -0.0012(3) 0.00190(17) 0.0005(3) Ti1 0.0082(7) 0.0090(7) 0.0082(7) 0.0000(5) 0.0040(6) -0.0010(5) S1 0.0088(10) 0.0122(11) 0.0083(10) 0.0034(8) 0.0037(8) 0.0003(8) O1 0.030(4) 0.011(3) 0.018(3) 0.005(2) 0.011(3) 0.000(2) O2 0.010(3) 0.018(3) 0.015(3) -0.005(2) 0.008(2) -0.001(2) O3 0.013(3) 0.015(4) 0.010(3) -0.002(2) 0.002(2) -0.0010(19) O4 0.020(3) 0.012(3) 0.019(3) 0.004(3) 0.005(3) -0.005(3) O5 0.014(3) 0.030(3) 0.009(3) -0.010(3) -0.001(2) -0.001(3) O6 0.009(2) 0.014(3) 0.016(3) 0.004(2) 0.000(2) 0.003(2) O7 0.015(3) 0.010(3) 0.017(3) 0.004(3) 0.008(2) 0.003(2) 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' S S 0.1246 0.1234 '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' Ti Ti 0.2776 0.4457 '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 O1 Te1 O2 90.6(2) 2_646 1_455 ? O3 Te1 O1 97.9(2) . 2_646 ? O3 Te1 O2 90.2(2) . 1_455 ? O1 Ti1 O2 93.9(3) . . ? O1 Ti1 O4 167.2(3) . . ? O1 Ti1 O6 88.8(2) . 2_757 ? O1 Ti1 O7 93.5(2) . 2_657 ? O2 Ti1 O4 90.9(2) . . ? O2 Ti1 O6 91.0(2) . 2_757 ? O2 Ti1 O7 172.4(2) . 2_657 ? O3 Ti1 O1 96.8(3) . . ? O3 Ti1 O2 93.1(2) . . ? O3 Ti1 O4 94.7(2) . . ? O3 Ti1 O6 172.8(2) . 2_757 ? O3 Ti1 O7 87.7(2) . 2_657 ? O4 Ti1 O6 79.3(2) . 2_757 ? O4 Ti1 O7 81.5(2) . 2_657 ? O7 Ti1 O6 87.4(2) 2_657 2_757 ? O4 S1 O7 107.3(4) . . ? O5 S1 O4 111.2(4) . . ? O5 S1 O6 108.7(3) . . ? O5 S1 O7 110.1(3) . . ? O6 S1 O4 107.8(3) . . ? O6 S1 O7 111.6(3) . . ? Ti1 O1 Te1 165.5(4) . 2_656 ? Ti1 O2 Te1 123.9(3) . 1_655 ? Ti1 O3 Te1 160.6(3) . . ? S1 O4 Ti1 147.7(4) . . ? S1 O6 Ti1 148.9(4) . 2_747 ? S1 O7 Ti1 138.2(4) . 2_647 ? 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 O1 1.872(6) 2_646 ? Te1 O2 1.895(5) 1_455 ? Te1 O3 1.858(5) . ? Ti1 O1 1.854(6) . ? Ti1 O2 1.874(5) . ? Ti1 O3 1.814(5) . ? Ti1 O4 2.018(6) . ? Ti1 O6 2.072(6) 2_757 ? Ti1 O7 2.064(6) 2_657 ? S1 O4 1.474(6) . ? S1 O5 1.459(6) . ? S1 O6 1.470(5) . ? S1 O7 1.477(5) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Te1 O3 Ti1 51.7(9) 2_646 . . . ? O1 Ti1 O2 Te1 9.4(3) . . . 1_655 ? O1 Ti1 O3 Te1 78.0(9) . . . . ? O2 Te1 O3 Ti1 142.3(9) 1_455 . . . ? O2 Ti1 O1 Te1 -153.0(14) . . . 2_656 ? O2 Ti1 O3 Te1 -16.3(9) . . . . ? O3 Ti1 O1 Te1 113.4(14) . . . 2_656 ? O3 Ti1 O2 Te1 106.5(3) . . . 1_655 ? O4 Ti1 O1 Te1 -41(2) . . . 2_656 ? O4 Ti1 O2 Te1 -158.7(3) . . . 1_655 ? O4 Ti1 O3 Te1 -107.6(9) . . . . ? O4 S1 O6 Ti1 16.8(7) . . . 2_747 ? O4 S1 O7 Ti1 -139.4(5) . . . 2_647 ? O5 S1 O4 Ti1 15.0(8) . . . . ? O5 S1 O6 Ti1 137.5(6) . . . 2_747 ? O5 S1 O7 Ti1 99.3(6) . . . 2_647 ? O6 Ti1 O1 Te1 -62.0(14) 2_757 . . 2_656 ? O6 Ti1 O2 Te1 -79.4(3) 2_757 . . 1_655 ? O6 S1 O4 Ti1 134.1(6) . . . . ? O6 S1 O7 Ti1 -21.5(6) . . . 2_647 ? O7 Ti1 O1 Te1 25.3(14) 2_657 . . 2_656 ? O7 Ti1 O3 Te1 171.2(9) 2_657 . . . ? O7 S1 O4 Ti1 -105.6(7) . . . . ? O7 S1 O6 Ti1 -100.8(6) . . . 2_747 ?