#------------------------------------------------------------------------------ #$Date: 2025-02-03 01:06:49 +0200 (Mon, 03 Feb 2025) $ #$Revision: 297569 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573839.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_1573839 loop_ _publ_author_name 'Gaidimas, Madeleine A.' 'Smoljan, Courtney S.' 'Ye, Zi-Ming' 'Stern, Charlotte L.' 'Malliakas, Christos D.' 'Kirlikovali, Kent O.' 'Farha, Omar K.' _publ_section_title ; Thorium metal--organic framework crystallization for efficient recovery from rare earth element mixtures ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC07652D _journal_year 2025 _chemical_formula_moiety 'C27 H9 O18 Th2' _chemical_formula_sum 'C27 H9 O18 Th2' _chemical_formula_weight 1085.42 _chemical_name_systematic NU-2500 _space_group_crystal_system cubic _space_group_IT_number 227 _space_group_name_Hall '-F 4vw 2vw 3' _space_group_name_H-M_alt 'F d -3 m :2' _atom_sites_solution_hydrogens geom _audit_creation_date 2024-07-29 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-08-16 deposited with the CCDC. 2025-01-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.66820(8) _cell_length_b 13.66820(8) _cell_length_c 13.66820(8) _cell_measurement_reflns_used 15574 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 73.1620 _cell_measurement_theta_min 5.5670 _cell_volume 2553.49(3) _computing_cell_refinement 'SAINT V8.34A (Bruker, 2017)' _computing_data_collection 'APEX2 V2017.3 (Bruker, 2017)' _computing_data_reduction 'Bruker SAINT' _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_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 8 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -120.00 -33.00 0.50 0.12 -- -47.48 -53.00 86.00 174 2 \w 34.00 120.00 0.50 0.12 -- 47.48 53.00-128.00 172 3 \w 34.00 120.00 0.50 0.12 -- 47.48 53.00-128.00 172 4 \w -56.00 -30.00 0.50 0.49 -- -103.00 53.00-128.00 52 5 \w -174.00 -89.00 0.50 0.49 -- -103.00 -53.00 86.00 170 6 \w -174.00 -89.00 0.50 0.49 -- -103.00 -53.00 86.00 170 7 \w 90.00 176.00 0.50 0.49 -- 103.75 53.00-128.00 172 8 \w 31.00 66.00 0.50 0.49 -- 103.75 -53.00 86.00 70 9 \w -42.00 -14.00 0.50 0.12 -- 6.00 127.00 -3.39 56 10 \w -18.00 27.00 0.50 0.12 -- 14.00 98.00 106.03 90 11 \w -1.00 28.00 0.50 0.12 -- 30.00 97.00 139.83 58 12 \w 8.00 34.00 0.50 0.12 -- 38.00 93.00 -77.12 52 13 \w 13.00 42.00 0.50 0.12 -- 42.00 91.00 51.58 58 14 \w 13.00 42.00 0.50 0.12 -- 42.00 91.00 142.41 58 15 \w -120.00 -25.00 0.50 0.12 -- -47.48 -77.00-150.00 190 16 \w -56.00 25.00 0.50 0.12 -- -47.48 53.00-128.00 162 17 \w -120.00 -25.00 0.50 0.12 -- -47.48 -77.00 90.00 190 18 \w -120.00 -25.00 0.50 0.12 -- -47.48 -77.00-150.00 190 19 \w -121.00 -35.00 0.50 0.12 -- -47.48 -37.00 -90.00 172 20 \w -120.00 -32.00 0.50 0.12 -- -47.48 -57.00 30.00 176 21 \w -24.00 61.00 0.50 0.12 -- 47.48 -53.00 86.00 170 22 \w -24.00 61.00 0.50 0.12 -- 47.48 -53.00 86.00 170 23 \w 19.00 93.00 0.50 0.12 -- 47.48-125.00 -90.00 148 24 \w 33.00 126.00 0.50 0.12 -- 54.00 74.00 174.92 186 25 \w 33.00 126.00 0.50 0.12 -- 54.00 74.00 174.92 186 26 \w 37.00 131.00 0.50 0.12 -- 58.00 74.00 -0.45 188 27 \w 36.00 131.00 0.50 0.12 -- 58.00 75.00-151.91 190 28 \w 37.00 131.00 0.50 0.12 -- 58.00 74.00 -0.45 188 29 \w 40.00 66.00 0.50 0.12 -- 62.00 76.00 72.88 52 30 \w 109.00 135.00 0.50 0.12 -- 62.00 76.00 72.88 52 31 \w 41.00 67.00 0.50 0.12 -- 62.00 73.00 -81.19 52 32 \w -77.00 -48.00 0.50 0.12 -- -66.00 -65.00 20.73 58 33 \w -135.00-106.00 0.50 0.12 -- -66.00 -65.00 20.73 58 34 \w -72.00 -46.00 0.50 0.12 -- -66.00 -69.00-124.98 52 35 \w -76.00 -49.00 0.50 0.12 -- -66.00 -61.00 -4.70 54 36 \w 46.00 76.00 0.50 0.12 -- 66.00 76.00-130.05 60 37 \w 45.00 71.00 0.50 0.12 -- 66.00 77.00 118.83 52 38 \w 44.00 70.00 0.50 0.12 -- 66.00 76.00 96.46 52 39 \w 101.00 126.00 0.50 0.12 -- 66.00 77.00 118.83 50 40 \w 44.00 72.00 0.50 0.12 -- 66.00 77.00 -60.94 56 41 \w -83.00 -53.00 0.50 0.12 -- -70.00 -63.00-150.72 60 42 \w -78.00 -53.00 0.50 0.12 -- -70.00 -63.00 12.68 50 43 \w -90.00 -54.00 0.50 0.12 -- -70.00 -60.00 123.06 72 44 \w -75.00 -49.00 0.50 0.12 -- -70.00 -75.00 131.48 52 45 \w -74.00 -49.00 0.50 0.12 -- -70.00 -73.00 -40.85 50 46 \w -78.00 -53.00 0.50 0.12 -- -70.00 -61.00 -41.81 50 47 \w -77.00 -52.00 0.50 0.12 -- -70.00 -65.00 -25.20 50 48 \w -79.00 -53.00 0.50 0.12 -- -70.00 -65.00 -65.01 52 49 \w -122.00 -96.00 0.50 0.12 -- -70.00 -73.00 -40.85 52 50 \w -83.00 -57.00 0.50 0.12 -- -74.00 -64.00-178.33 52 51 \w -79.00 -53.00 0.50 0.12 -- -74.00 -74.00 90.33 52 52 \w -78.00 -52.00 0.50 0.12 -- -74.00 -74.00 13.38 52 53 \w -83.00 -57.00 0.50 0.49 -- -78.00 -73.00-178.49 52 54 \w -88.00 -62.00 0.50 0.49 -- -78.00 -60.00-164.77 52 55 \w -102.00 -60.00 0.50 0.49 -- -78.00 -64.00 56.23 84 56 \w -88.00 -62.00 0.50 0.49 -- -78.00 -62.00 114.49 52 57 \w -87.00 -61.00 0.50 0.49 -- -78.00 -61.00 147.21 52 58 \w -148.00-123.00 0.50 0.49 -- -78.00 -60.00-164.77 50 59 \w -99.00 -72.00 0.50 0.49 -- -78.00 -59.00-108.11 54 60 \w -87.00 -61.00 0.50 0.49 -- -78.00 -63.00 -97.99 52 61 \w -91.00 -65.00 0.50 0.49 -- -82.00 -62.00 -29.57 52 62 \w -87.00 -62.00 0.50 0.49 -- -82.00 -70.00 118.62 50 63 \w -93.00 -66.00 0.50 0.49 -- -82.00 -60.00 -6.71 54 64 \w -93.00 -65.00 0.50 0.49 -- -82.00 -62.00 -60.94 56 65 \w -102.00 -65.00 0.50 0.49 -- -86.00 -72.00 42.26 74 66 \w -93.00 -66.00 0.50 0.49 -- -86.00 -71.00 84.41 54 67 \w -96.00 -69.00 0.50 0.49 -- -90.00 -73.00 -61.97 54 68 \w -102.00 -73.00 0.50 0.49 -- -90.00 -63.00 153.27 58 69 \w -151.00-126.00 0.50 0.49 -- -90.00 -63.00 153.27 50 70 \w -104.00 -76.00 0.50 0.49 -- -90.00 -60.00 -90.20 56 71 \w -96.00 -70.00 0.50 0.49 -- -90.00 -71.00 31.40 52 72 \w -96.00 -69.00 0.50 0.49 -- -90.00 -74.00 6.81 54 73 \w -111.00 -68.00 0.50 0.49 -- -90.00 -75.00 113.73 86 74 \w -105.00 -78.00 0.50 0.49 -- -90.00 -56.00 -43.36 54 75 \w -166.00 -78.00 0.50 0.49 -- -94.00 -60.00 51.41 176 76 \w -114.00 -73.00 0.50 0.49 -- -94.00 -72.00-118.37 82 77 \w -162.00-125.00 0.50 0.49 -- -94.00 -72.00-118.37 74 78 \w -98.00 -72.00 0.50 0.49 -- -94.00 -75.00 -94.93 52 79 \w -163.00-119.00 0.50 0.49 -- -94.00 -74.00 124.97 88 80 \w -98.00 -72.00 0.50 0.49 -- -94.00 -74.00 124.97 52 81 \w -105.00 -76.00 0.50 0.49 -- -98.00 -76.00 -20.04 58 82 \w -169.00-143.00 0.50 0.49 -- -98.00 -76.00 -20.04 52 83 \w -125.00 -77.00 0.50 0.49 -- -98.00 -76.00 36.03 96 84 \w -170.00 -75.00 0.50 0.49 -- -98.00 -77.00 1.98 190 85 \w -109.00 -80.00 0.50 0.49 -- -98.00 -64.00-166.48 58 86 \w -130.00 -76.00 0.50 0.49 -- -98.00 -77.00-126.33 108 87 \w -166.00-134.00 0.50 0.49 -- -98.00 -77.00-126.33 64 88 \w -128.00 -79.00 0.50 0.49 -- -103.00 -79.00 28.71 98 89 \w -173.00-100.00 0.50 0.49 -- -103.00 -77.00 -30.00 146 90 \w -173.00-108.00 0.50 0.49 -- -103.00 -80.00 -87.10 130 91 \w -111.00 -85.00 0.50 0.49 -- -103.00 -66.00 -80.66 52 92 \w -111.00 -84.00 0.50 0.49 -- -103.00 -69.00 -35.13 54 93 \w -153.00 -84.00 0.50 0.49 -- -103.00 -68.00-172.15 138 94 \w -153.00 -84.00 0.50 0.49 -- -103.00 -68.00 -65.97 138 95 \w -146.00 -86.00 0.50 0.49 -- -103.00 -63.00 145.01 120 96 \w -170.00 -86.00 0.50 0.49 -- -103.00 -61.00-154.32 168 97 \w -112.00 -33.00 0.50 0.49 -- -103.00 125.00-150.00 158 98 \w -166.00 -82.00 0.50 0.49 -- -103.00 -77.00 90.00 168 99 \w -126.00 -92.00 0.50 0.49 -- -103.00 145.00 -86.02 68 100 \w -104.00 -79.00 0.50 0.49 -- -103.00 -80.00 -87.10 50 101 \w 72.00 105.00 0.50 0.49 -- 103.75 -94.00 90.00 66 102 \w 34.00 92.00 0.50 0.49 -- 103.75-125.00-120.00 116 103 \w 42.00 106.00 0.50 0.49 -- 103.75 -94.00 150.00 128 104 \w 64.00 94.00 0.50 0.49 -- 103.75 -94.00-180.00 60 105 \w 83.00 171.00 0.50 0.49 -- 103.75 77.00 90.00 176 106 \w 87.00 150.00 0.50 0.49 -- 103.75 61.00 -30.00 126 107 \w 32.00 106.00 0.50 0.49 -- 103.75 -94.00 -60.00 148 108 \w 48.00 98.00 0.50 0.49 -- 103.75 -77.00 0.00 100 109 \w 56.00 112.00 0.50 0.49 -- 103.75-125.00 120.00 112 110 \w 83.00 109.00 0.50 0.49 -- 103.75 77.00 150.00 52 111 \w 32.00 57.00 0.50 0.49 -- 103.75 -94.00-180.00 50 112 \w 41.00 88.00 0.50 0.49 -- 103.75 -94.00-120.00 94 113 \w 93.00 131.00 0.50 0.49 -- 103.75 61.00 120.00 76 114 \w 133.00 160.00 0.50 0.49 -- 103.75 61.00 -60.00 54 115 \w 88.00 130.00 0.50 0.49 -- 103.75 61.00 -60.00 84 116 \w 32.00 74.00 0.50 0.49 -- 103.75 -61.00 30.00 84 117 \w 56.00 100.00 0.50 0.49 -- 103.75 -94.00 0.00 88 118 \w 44.00 87.00 0.50 0.49 -- 103.75 -77.00-120.00 86 119 \w 31.00 75.00 0.50 0.49 -- 103.75 -61.00 -60.00 88 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type duoCu _diffrn_measurement_method '\w and \f scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0902614000 _diffrn_orient_matrix_UB_12 0.0025010000 _diffrn_orient_matrix_UB_13 0.0674913000 _diffrn_orient_matrix_UB_21 -0.0225234000 _diffrn_orient_matrix_UB_22 -0.1072862000 _diffrn_orient_matrix_UB_23 -0.0261297000 _diffrn_orient_matrix_UB_31 0.0637346000 _diffrn_orient_matrix_UB_32 -0.0343846000 _diffrn_orient_matrix_UB_33 0.0863592000 _diffrn_radiation_monochromator 'Quazar optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_unetI/netI 0.0054 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 23360 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.538 _diffrn_reflns_theta_min 5.606 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 38.207 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.69043 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.101a (Rigaku Oxford Diffraction, 2023) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.823 _exptl_crystal_density_meas 2.823 _exptl_crystal_description irregular _exptl_crystal_F_000 1980 _exptl_crystal_size_max 0.185 _exptl_crystal_size_mid 0.101 _exptl_crystal_size_min 0.021 _refine_diff_density_max 0.965 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.171 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 17 _refine_ls_number_reflns 155 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.221 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0394 _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^)+(0.0611P)^2^+56.5051P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0965 _refine_ls_wR_factor_ref 0.0971 _reflns_Friedel_coverage 0.000 _reflns_number_gt 152 _reflns_number_total 155 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc07652d2.cif _cod_data_source_block mg2-27-7_2_auto _cod_original_cell_volume 2553.49(4) _cod_original_sg_symbol_H-M 'F d -3 m' _cod_database_code 1573839 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula ThCOH _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 0.501 _shelx_estimated_absorpt_t_min 0.053 _olex2_refinement_description ; 1. Restrained distances O2-C2 1.2 with sigma of 0.02 O1-C2 1.2 with sigma of 0.02 O2-C2 \\sim C2-O1 with sigma of 0.02 2. Uiso/Uaniso restraints and constraints Uanis(C2) = Uanis(C1) Uanis(O1) = Uanis(O2) 3. Others Sof(O1)=0.375*(1-FVAR(2)) Sof(O2)=0.375*FVAR(2) Fixed Sof: C1(0.375) H1(0.1875) C2(0.1875) 4.a Aromatic/amide H refined with riding coordinates: C1(H1) ; _shelx_res_file ; TITL mg2-27-7_2_auto.res created by SHELXL-2018/3 at 15:19:54 on 26-Jul-2024 CELL 1.54184 13.6682 13.6682 13.6682 90 90 90 ZERR 4 0.00008 0.00008 0.00008 0 0 0 LATT 4 SYMM 0.75-X,0.25-Y,0.5+Z SYMM 0.25-X,0.5+Y,0.75-Z SYMM 0.5+X,0.75-Y,0.25-Z SYMM +Z,+X,+Y SYMM 0.5+Z,0.75-X,0.25-Y SYMM 0.75-Z,0.25-X,0.5+Y SYMM 0.25-Z,0.5+X,0.75-Y SYMM +Y,+Z,+X SYMM 0.25-Y,0.5+Z,0.75-X SYMM 0.5+Y,0.75-Z,0.25-X SYMM 0.75-Y,0.25-Z,0.5+X SYMM 0.75+Y,0.25+X,0.5-Z SYMM -Y,-X,-Z SYMM 0.25+Y,0.5-X,0.75+Z SYMM 0.5-Y,0.75+X,0.25+Z SYMM 0.75+X,0.25+Z,0.5-Y SYMM 0.5-X,0.75+Z,0.25+Y SYMM -X,-Z,-Y SYMM 0.25+X,0.5-Z,0.75+Y SYMM 0.75+Z,0.25+Y,0.5-X SYMM 0.25+Z,0.5-Y,0.75+X SYMM 0.5-Z,0.75+Y,0.25+X SYMM -Z,-Y,-X SFAC C H O Th UNIT 108 36 72 8 EQIV $1 0.75-X,0.75-Y,+Z EQIV $2 0.75-X,+Z,0.75-Y EQIV $3 1-Y,1-Z,1-X EQIV $4 0.75-X,-0.5+Z,1.25-Y EQIV $5 1-Z,1-X,1-Y EQIV $6 +X,+Z,+Y DFIX 1.2 O2 C2 SADI O2 C2 C2 O1 EADP C2 C1 EADP O1 O2 DFIX 1.2 O1 C2 L.S. 25 0 0 PLAN 5 SIZE 0.021 0.101 0.185 TEMP -173 CONF BIND O1 C2 FREE O2 O2_$1 FREE O2 O2_$2 FREE C2 C2_$3 FREE C2 C2_$4 FREE C2 C2_$5 FREE C2 C2_$6 list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.061100 56.505100 FVAR 0.17377 0.44069 TH1 4 0.625000 0.625000 0.625000 10.04167 0.04579 0.04579 = 0.04579 0.00000 0.00000 0.00000 PART 2 O1 3 0.505700 0.505700 0.637172 -20.37500 0.21852 0.21852 = 0.09195 -0.02581 -0.02581 -0.14865 PART 1 O2 3 0.418174 0.418174 0.552546 20.37500 0.21852 0.21852 = 0.09195 -0.02581 -0.02581 -0.14865 PART 0 C1 1 0.321694 0.500000 0.678306 10.37500 0.11409 0.11253 = 0.11409 -0.04524 0.03205 -0.04524 PART 2 AFIX 43 H1 2 0.370841 0.500000 0.629159 10.18750 -1.20000 AFIX 0 PART 1 C2 1 0.404839 0.500000 0.595161 10.18750 0.11409 0.11253 = 0.11409 -0.04524 0.03205 -0.04524 HKLF 4 REM REM wR2 = 0.0971, GooF = S = 1.175, Restrained GooF = 1.221 for all data REM R1 = 0.0394 for 152 Fo > 4sig(Fo) and 0.0399 for all 155 data REM 17 parameters refined using 1 restraints END WGHT 0.0611 55.9630 REM Highest difference peak 0.965, deepest hole -0.562, 1-sigma level 0.171 Q1 1 0.4011 0.4011 0.5288 10.50000 0.05 0.96 Q2 1 0.6250 0.6250 0.7004 10.25000 0.05 0.91 Q3 1 0.4026 0.4026 0.7204 10.50000 0.05 0.38 Q4 1 0.3750 0.3750 0.8750 10.04167 0.05 0.34 Q5 1 0.3360 0.5988 0.6512 10.50000 0.05 0.27 ; _shelx_res_checksum 7478 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.325 _oxdiff_exptl_absorpt_empirical_full_min 0.814 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+3/4, -y+1/4, z+1/2' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, -y+3/4, -z+1/4' 'z, x, y' 'z+1/2, -x+3/4, -y+1/4' '-z+3/4, -x+1/4, y+1/2' '-z+1/4, x+1/2, -y+3/4' 'y, z, x' '-y+1/4, z+1/2, -x+3/4' 'y+1/2, -z+3/4, -x+1/4' '-y+3/4, -z+1/4, x+1/2' 'y+3/4, x+1/4, -z+1/2' '-y, -x, -z' 'y+1/4, -x+1/2, z+3/4' '-y+1/2, x+3/4, z+1/4' 'x+3/4, z+1/4, -y+1/2' '-x+1/2, z+3/4, y+1/4' '-x, -z, -y' 'x+1/4, -z+1/2, y+3/4' 'z+3/4, y+1/4, -x+1/2' 'z+1/4, -y+1/2, x+3/4' '-z+1/2, y+3/4, x+1/4' '-z, -y, -x' 'x, y+1/2, z+1/2' '-x+3/4, -y+3/4, z+1' '-x+1/4, y+1, -z+5/4' 'x+1/2, -y+5/4, -z+3/4' 'z, x+1/2, y+1/2' 'z+1/2, -x+5/4, -y+3/4' '-z+3/4, -x+3/4, y+1' '-z+1/4, x+1, -y+5/4' 'y, z+1/2, x+1/2' '-y+1/4, z+1, -x+5/4' 'y+1/2, -z+5/4, -x+3/4' '-y+3/4, -z+3/4, x+1' 'y+3/4, x+3/4, -z+1' '-y, -x+1/2, -z+1/2' 'y+1/4, -x+1, z+5/4' '-y+1/2, x+5/4, z+3/4' 'x+3/4, z+3/4, -y+1' '-x+1/2, z+5/4, y+3/4' '-x, -z+1/2, -y+1/2' 'x+1/4, -z+1, y+5/4' 'z+3/4, y+3/4, -x+1' 'z+1/4, -y+1, x+5/4' '-z+1/2, y+5/4, x+3/4' '-z, -y+1/2, -x+1/2' 'x+1/2, y, z+1/2' '-x+5/4, -y+1/4, z+1' '-x+3/4, y+1/2, -z+5/4' 'x+1, -y+3/4, -z+3/4' 'z+1/2, x, y+1/2' 'z+1, -x+3/4, -y+3/4' '-z+5/4, -x+1/4, y+1' '-z+3/4, x+1/2, -y+5/4' 'y+1/2, z, x+1/2' '-y+3/4, z+1/2, -x+5/4' 'y+1, -z+3/4, -x+3/4' '-y+5/4, -z+1/4, x+1' 'y+5/4, x+1/4, -z+1' '-y+1/2, -x, -z+1/2' 'y+3/4, -x+1/2, z+5/4' '-y+1, x+3/4, z+3/4' 'x+5/4, z+1/4, -y+1' '-x+1, z+3/4, y+3/4' '-x+1/2, -z, -y+1/2' 'x+3/4, -z+1/2, y+5/4' 'z+5/4, y+1/4, -x+1' 'z+3/4, -y+1/2, x+5/4' '-z+1, y+3/4, x+3/4' '-z+1/2, -y, -x+1/2' 'x+1/2, y+1/2, z' '-x+5/4, -y+3/4, z+1/2' '-x+3/4, y+1, -z+3/4' 'x+1, -y+5/4, -z+1/4' 'z+1/2, x+1/2, y' 'z+1, -x+5/4, -y+1/4' '-z+5/4, -x+3/4, y+1/2' '-z+3/4, x+1, -y+3/4' 'y+1/2, z+1/2, x' '-y+3/4, z+1, -x+3/4' 'y+1, -z+5/4, -x+1/4' '-y+5/4, -z+3/4, x+1/2' 'y+5/4, x+3/4, -z+1/2' '-y+1/2, -x+1/2, -z' 'y+3/4, -x+1, z+3/4' '-y+1, x+5/4, z+1/4' 'x+5/4, z+3/4, -y+1/2' '-x+1, z+5/4, y+1/4' '-x+1/2, -z+1/2, -y' 'x+3/4, -z+1, y+3/4' 'z+5/4, y+3/4, -x+1/2' 'z+3/4, -y+1, x+3/4' '-z+1, y+5/4, x+1/4' '-z+1/2, -y+1/2, -x' '-x, -y, -z' 'x-3/4, y-1/4, -z-1/2' 'x-1/4, -y-1/2, z-3/4' '-x-1/2, y-3/4, z-1/4' '-z, -x, -y' '-z-1/2, x-3/4, y-1/4' 'z-3/4, x-1/4, -y-1/2' 'z-1/4, -x-1/2, y-3/4' '-y, -z, -x' 'y-1/4, -z-1/2, x-3/4' '-y-1/2, z-3/4, x-1/4' 'y-3/4, z-1/4, -x-1/2' '-y-3/4, -x-1/4, z-1/2' 'y, x, z' '-y-1/4, x-1/2, -z-3/4' 'y-1/2, -x-3/4, -z-1/4' '-x-3/4, -z-1/4, y-1/2' 'x-1/2, -z-3/4, -y-1/4' 'x, z, y' '-x-1/4, z-1/2, -y-3/4' '-z-3/4, -y-1/4, x-1/2' '-z-1/4, y-1/2, -x-3/4' 'z-1/2, -y-3/4, -x-1/4' 'z, y, x' '-x, -y+1/2, -z+1/2' 'x-3/4, y+1/4, -z' 'x-1/4, -y, z-1/4' '-x-1/2, y-1/4, z+1/4' '-z, -x+1/2, -y+1/2' '-z-1/2, x-1/4, y+1/4' 'z-3/4, x+1/4, -y' 'z-1/4, -x, y-1/4' '-y, -z+1/2, -x+1/2' 'y-1/4, -z, x-1/4' '-y-1/2, z-1/4, x+1/4' 'y-3/4, z+1/4, -x' '-y-3/4, -x+1/4, z' 'y, x+1/2, z+1/2' '-y-1/4, x, -z-1/4' 'y-1/2, -x-1/4, -z+1/4' '-x-3/4, -z+1/4, y' 'x-1/2, -z-1/4, -y+1/4' 'x, z+1/2, y+1/2' '-x-1/4, z, -y-1/4' '-z-3/4, -y+1/4, x' '-z-1/4, y, -x-1/4' 'z-1/2, -y-1/4, -x+1/4' 'z, y+1/2, x+1/2' '-x+1/2, -y, -z+1/2' 'x-1/4, y-1/4, -z' 'x+1/4, -y-1/2, z-1/4' '-x, y-3/4, z+1/4' '-z+1/2, -x, -y+1/2' '-z, x-3/4, y+1/4' 'z-1/4, x-1/4, -y' 'z+1/4, -x-1/2, y-1/4' '-y+1/2, -z, -x+1/2' 'y+1/4, -z-1/2, x-1/4' '-y, z-3/4, x+1/4' 'y-1/4, z-1/4, -x' '-y-1/4, -x-1/4, z' 'y+1/2, x, z+1/2' '-y+1/4, x-1/2, -z-1/4' 'y, -x-3/4, -z+1/4' '-x-1/4, -z-1/4, y' 'x, -z-3/4, -y+1/4' 'x+1/2, z, y+1/2' '-x+1/4, z-1/2, -y-1/4' '-z-1/4, -y-1/4, x' '-z+1/4, y-1/2, -x-1/4' 'z, -y-3/4, -x+1/4' 'z+1/2, y, x+1/2' '-x+1/2, -y+1/2, -z' 'x-1/4, y+1/4, -z-1/2' 'x+1/4, -y, z-3/4' '-x, y-1/4, z-1/4' '-z+1/2, -x+1/2, -y' '-z, x-1/4, y-1/4' 'z-1/4, x+1/4, -y-1/2' 'z+1/4, -x, y-3/4' '-y+1/2, -z+1/2, -x' 'y+1/4, -z, x-3/4' '-y, z-1/4, x-1/4' 'y-1/4, z+1/4, -x-1/2' '-y-1/4, -x+1/4, z-1/2' 'y+1/2, x+1/2, z' '-y+1/4, x, -z-3/4' 'y, -x-1/4, -z-1/4' '-x-1/4, -z+1/4, y-1/2' 'x, -z-1/4, -y-1/4' 'x+1/2, z+1/2, y' '-x+1/4, z, -y-3/4' '-z-1/4, -y+1/4, x-1/2' '-z+1/4, y, -x-3/4' 'z, -y-1/4, -x-1/4' 'z+1/2, y+1/2, x' 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 Th1 Th 0.625000 0.625000 0.625000 0.0458(5) Uani 1 24 d S T P . . O1 O 0.5057(18) 0.5057(18) 0.637(2) 0.176(19) Uani 0.42(3) 2 d S T P A 2 O2 O 0.418(2) 0.418(2) 0.553(3) 0.176(19) Uani 0.33(3) 2 d DS T P . 1 C1 C 0.3217(12) 0.500000 0.6783(12) 0.114(7) Uani 0.75 2 d S T P . . H1 H 0.370841 0.500000 0.629159 0.136 Uiso 0.375 2 calc R U P B 2 C2 C 0.405(2) 0.500000 0.595(2) 0.114(7) Uani 0.375 2 d DS T P . 1 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 0.0458(5) 0.0458(5) 0.0458(5) 0.000 0.000 0.000 O1 0.22(3) 0.22(3) 0.092(17) -0.026(8) -0.026(8) -0.15(4) O2 0.22(3) 0.22(3) 0.092(17) -0.026(8) -0.026(8) -0.15(4) C1 0.114(9) 0.113(15) 0.114(9) -0.045(9) 0.032(12) -0.045(9) C2 0.114(9) 0.113(15) 0.114(9) -0.045(9) 0.032(12) -0.045(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -4.1491 12.3296 '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 Th1 O1 119.83(6) . 34_645 ? O1 Th1 O1 90.30(11) 5 55_564 ? O1 Th1 O1 119.83(7) 50_564 9 ? O1 Th1 O1 53.2(13) . 83_456 ? O1 Th1 O1 119.83(6) 50_564 32_645 ? O1 Th1 O1 119.83(7) . 55_564 ? O1 Th1 O1 66.7(12) 78_456 83_456 ? O1 Th1 O1 66.7(12) . 5 ? O1 Th1 O1 90.30(12) 9 83_456 ? O1 Th1 O1 53.2(13) 32_645 83_456 ? O1 Th1 O1 66.7(12) 50_564 55_564 ? O1 Th1 O1 171.7(16) 55_564 32_645 ? O1 Th1 O1 53.2(13) 9 76_456 ? O1 Th1 O1 90.30(11) 34_645 83_456 ? O1 Th1 O1 90.30(12) 78_456 55_564 ? O1 Th1 O1 53.2(13) 9 55_564 ? O1 Th1 O1 66.7(12) 60_564 55_564 ? O1 Th1 O1 66.7(12) . 9 ? O1 Th1 O1 171.7(16) 60_564 83_456 ? O1 Th1 O1 119.83(7) 50_564 5 ? O1 Th1 O1 119.83(6) 34_645 76_456 ? O1 Th1 O1 66.7(12) 78_456 76_456 ? O1 Th1 O1 53.2(13) 50_564 78_456 ? O1 Th1 O1 119.83(6) 60_564 32_645 ? O1 Th1 O1 90.30(12) . 76_456 ? O1 Th1 O1 90.30(11) 50_564 76_456 ? O1 Th1 O1 119.83(7) 60_564 76_456 ? O1 Th1 O1 119.83(6) 32_645 76_456 ? O1 Th1 O1 119.83(7) 5 83_456 ? O1 Th1 O1 119.83(7) 5 76_456 ? O1 Th1 O1 119.83(6) 55_564 83_456 ? O1 Th1 O1 53.2(13) 55_564 76_456 ? O1 Th1 O1 66.7(12) 76_456 83_456 ? O1 Th1 O1 119.83(6) 50_564 83_456 ? O1 Th1 O1 90.30(11) 78_456 32_645 ? O1 Th1 O1 119.83(7) 34_645 5 ? O1 Th1 O1 171.7(16) 78_456 5 ? O1 Th1 O1 53.2(13) . 32_645 ? O1 Th1 O1 171.7(16) 34_645 9 ? O1 Th1 O1 66.7(12) 34_645 32_645 ? O1 Th1 O1 53.2(13) 34_645 78_456 ? O1 Th1 O1 119.83(6) 27_645 83_456 ? O1 Th1 O1 119.83(7) 9 32_645 ? O1 Th1 O1 119.83(6) 34_645 55_564 ? O1 Th1 O1 90.30(11) 5 32_645 ? O1 Th1 O1 119.83(6) 78_456 9 ? O1 Th1 O1 66.7(12) 9 5 ? O1 Th1 O1 119.83(6) . 78_456 ? C2 O2 Th1 127(2) . 97_666 ? C2 O2 Th1 127(2) 105_666 97_666 ? C2 O2 C2 92(3) 105_666 . ? C1 C1 C1 120.003(5) 156_556 150_665 ? C1 C1 H1 120.0 150_665 . ? C1 C1 H1 120.0 156_556 . ? C1 C1 C2 119.999(3) 156_556 . ? C1 C1 C2 119.999(4) 150_665 . ? O2 C2 O2 130(7) . 101_666 ? O2 C2 C1 115(3) 101_666 . ? O2 C2 C1 115(3) . . ? 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 O1 2.31(4) . ? Th1 O1 2.31(4) 50_564 ? Th1 O1 2.31(4) 83_456 ? Th1 O1 2.31(4) 5 ? Th1 O1 2.31(4) 55_564 ? Th1 O1 2.31(4) 9 ? Th1 O1 2.31(4) 32_645 ? Th1 O1 2.31(4) 27_645 ? Th1 O1 2.31(4) 34_645 ? Th1 O1 2.31(4) 60_564 ? Th1 O1 2.31(4) 76_456 ? Th1 O1 2.31(4) 78_456 ? O2 C2 1.274(18) 105_666 ? O2 C2 1.274(18) . ? C1 C1 1.39(2) 150_665 ? C1 C1 1.39(2) 156_556 ? C1 H1 0.9500 . ? C1 C2 1.61(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 Th1 O2 C2 O2 -70(4) 97_666 . . 101_666 ? Th1 O2 C2 C1 110(4) 97_666 . . . ? C1 C1 C2 O2 158.9(12) 156_556 . . 101_666 ? C1 C1 C2 O2 158.9(12) 150_665 . . . ? C1 C1 C2 O2 -21.1(12) 150_665 . . 101_666 ? C1 C1 C2 O2 -21.1(12) 156_556 . . . ? C2 O2 C2 O2 72(3) 105_666 . . 101_666 ? C2 O2 C2 C1 -108(3) 105_666 . . . ?