#------------------------------------------------------------------------------
#$Date: 2024-11-21 05:05:15 +0200 (Thu, 21 Nov 2024) $
#$Revision: 296043 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/26/2312693.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_2312693
loop_
_publ_author_name
'Steiner, Sebastian'
'Djordjevic, Kristina'
'Bockmair, Valentin'
'Hollenwäger, Dirk'
'Kornath, Andreas J.'
_publ_section_title
;
Protonated oxalyl chloride and the ClCO+ cation.
;
_journal_coeditor_code YD3050
_journal_issue 12
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229624010714
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac '(C Cl O) [Sb3 F16]'
_chemical_formula_moiety 'C Cl O +, F16 Sb3 -'
_chemical_formula_sum 'C Cl F16 O Sb3'
_chemical_formula_weight 732.71
_chemical_name_systematic
;
Carbonyl chloride hexadecafluoridotriarsenate(V)
;
_space_group_crystal_system trigonal
_space_group_IT_number 144
_space_group_name_Hall 'P 31'
_space_group_name_H-M_alt 'P 31'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 3
_cell_length_a 8.0824(3)
_cell_length_b 8.0824(3)
_cell_length_c 18.3341(8)
_cell_measurement_reflns_used 2010
_cell_measurement_temperature 102(2)
_cell_measurement_theta_max 31.5220
_cell_measurement_theta_min 2.8900
_cell_volume 1037.22(7)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 102(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device 'CCD camera on \k-goniostat'
_diffrn_measurement_device_type 'Rigaku Xcalibur Sapphire3'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0436
_diffrn_reflns_av_unetI/netI 0.0668
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 6310
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 32.009
_diffrn_reflns_theta_min 2.222
_diffrn_source_current 40
_diffrn_source_voltage 50
_exptl_absorpt_coefficient_mu 6.191
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.88215
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2020)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 3.519
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 984
_exptl_crystal_size_max 0.190
_exptl_crystal_size_mid 0.136
_exptl_crystal_size_min 0.106
_refine_diff_density_max 1.356
_refine_diff_density_min -1.093
_refine_ls_abs_structure_details
;
Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.032
_refine_ls_hydrogen_treatment undef
_refine_ls_matrix_type full
_refine_ls_number_parameters 199
_refine_ls_number_reflns 3334
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.032
_refine_ls_R_factor_all 0.0462
_refine_ls_R_factor_gt 0.0384
_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^)+(0.0262P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0717
_refine_ls_wR_factor_ref 0.0767
_reflns_number_gt 3029
_reflns_number_total 3334
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yd3050.cif
_cod_data_source_block 5
_cod_original_cell_volume 1037.22(9)
_cod_database_code 2312693
_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_min 0.386
_shelx_estimated_absorpt_t_max 0.560
_shelx_hkl_file
;
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10 -7 -1 2991.17 619.053 2
10 -6 -13 1966.22 630.836 2
10 -6 -12 377.436 324.044 2
10 -6 -11 5753.58 956.378 2
10 -6 -10 948.886 540.958 2
10 -6 -9 9325.40 1154.24 2
10 -6 -8 5135.39 874.785 2
10 -6 -7 8330.82 1067.64 2
10 -6 -6 3410.93 738.191 2
10 -6 -5 3299.75 691.201 2
10 -6 -4 22.4607 307.901 2
10 -6 -3 7329.90 967.837 2
10 -6 -2 3283.46 676.075 2
10 -6 -1 8101.49 997.002 2
10 -6 0 6853.21 918.846 2
10 -6 1 653.571 349.539 2
10 -5 -13 559.127 381.605 2
-5 -5 -13-19.7408 451.017 1
10 -5 -12 2910.10 723.508 2
-5 -5 -12 2665.73 694.326 1
10 -5 -11 4253.76 822.414 2
-5 -5 -11 5564.26 996.061 1
10 -5 -10 3887.10 786.155 2
-5 -5 -10 3805.82 839.505 1
10 -5 -9 1742.54 558.378 2
-5 -5 -9 769.432 529.149 1
10 -5 -8 2066.54 597.313 2
-5 -5 -8 736.717 406.672 1
10 -5 -7 4369.08 803.878 2
-5 -5 -7 5871.03 973.957 1
-5 -5 -6 2189.85 624.273 1
10 -5 -6 3275.53 706.125 2
10 -5 -5 16474.7 1486.68 2
-5 -5 -5 17425.9 1549.30 1
10 -5 -4 2132.77 610.538 2
-5 -5 -4 2791.76 673.041 1
10 -5 -3 7788.68 1028.07 2
-5 -5 -3 7167.39 994.561 1
10 -5 -2 5087.35 835.155 2
-5 -5 -2 6052.68 915.915 1
10 -5 -1 6807.45 939.687 2
-5 -5 -1 5936.14 881.632 1
10 -5 0 264.646 264.445 2
-5 -5 0-187.870 471.418 1
10 -5 1 17510.5 1439.67 2
-5 -5 1 15940.5 1391.75 1
-5 -5 2 6411.91 888.458 1
10 -5 2 6447.97 893.698 2
-5 -5 3 7228.89 966.436 1
10 -5 3 7170.22 915.331 2
10 -5 4 15364.7 1316.30 2
-5 -5 4 14675.1 1304.45 1
-5 -5 5 2511.91 588.315 1
-5 -5 6 3610.12 700.382 1
-5 -5 7 1853.59 494.979 1
-5 -5 8 3972.97 730.297 1
-4 -6 -13 4053.29 945.115 1
10 -4 -12 1964.00 658.399 2
-4 -6 -12 1863.25 655.192 1
10 -4 -11 1261.51 522.265 2
-4 -6 -11 784.521 497.641 1
10 -4 -10 576.516 405.204 2
-4 -6 -10 816.957 495.805 1
10 -4 -9 952.081 504.590 2
-4 -6 -9 1105.09 621.443 1
10 -4 -8 2774.08 719.740 2
-4 -6 -8 3575.11 799.583 1
10 -4 -7 1262.90 548.255 2
-4 -6 -7 1309.40 511.060 1
10 -4 -6 4605.50 839.046 2
-4 -6 -6 6036.39 1006.88 1
10 -4 -5 126.874 305.855 2
-4 -6 -5-52.1800 299.641 1
10 -4 -4-245.940 455.161 2
-4 -6 -4 113.834 299.661 1
10 -4 -3 275.940 307.087 2
-4 -6 -3 1011.67 464.767 1
-4 -6 -2 2960.45 706.479 1
10 -4 -2 2945.31 653.734 2
-4 -6 -1 6346.12 977.424 1
10 -4 -1 7991.98 1053.22 2
-4 -6 0 1064.84 475.047 1
10 -4 0 1144.05 478.516 2
10 -4 1 4091.45 770.959 2
-4 -6 1 3592.08 783.214 1
-4 -6 2 2131.84 560.163 1
10 -4 2 2750.35 658.164 2
-4 -6 3 2082.40 639.498 1
10 -4 3 1783.41 516.164 2
-4 -6 4 482.636 338.728 1
10 -4 4 927.468 398.987 2
10 -4 5 8601.71 1000.20 2
-4 -6 5 9804.68 1140.84 1
-4 -6 6 3378.97 712.772 1
10 -4 6 2934.51 623.295 2
-4 -6 7 6993.10 986.585 1
-4 -6 8 9769.30 1162.41 1
-4 -6 9 1633.59 529.325 1
-4 -6 10 1800.56 558.800 1
-4 -6 11 2483.26 644.468 1
-4 -6 12 3070.13 720.909 1
-3 -7 -13 892.921 564.054 1
10 -3 -12 4753.24 946.849 2
-3 -7 -12 2921.60 815.818 1
10 -3 -11 6142.93 1025.70 2
-3 -7 -11 5239.46 1067.35 1
10 -3 -10 2731.27 701.084 2
-3 -7 -10 2898.00 861.680 1
10 -3 -9 11158.1 1338.67 2
-3 -7 -9 13304.9 1569.28 1
10 -3 -8 3498.28 778.847 2
-3 -7 -8 3285.41 792.737 1
10 -3 -7 648.114 448.304 2
-3 -7 -7 1297.37 658.102 1
10 -3 -6 4695.46 852.191 2
-3 -7 -6 5436.26 987.665 1
-3 -7 -5 1296.78 543.666 1
10 -3 -5 2307.84 642.100 2
-3 -7 -4-202.344 340.297 1
10 -3 -4 738.534 468.679 2
-3 -7 -3 3325.06 770.580 1
10 -3 -3 2847.10 676.946 2
-3 -7 -2 8909.38 1191.78 1
10 -3 -2 10450.3 1220.50 2
-3 -7 -1 3288.15 766.190 1
10 -3 -1 4105.90 811.987 2
-3 -7 0 1331.31 573.692 1
10 -3 0 1699.58 580.486 2
-3 -7 1-262.261 424.258 1
10 -3 1 310.353 318.779 2
10 -3 2 1155.43 475.080 2
-3 -7 2 953.443 450.116 1
-3 -7 3-181.548 369.082 1
10 -3 3 404.632 326.332 2
-3 -7 4 5779.47 964.265 1
10 -3 4 6180.60 928.460 2
-3 -7 5 939.966 485.124 1
10 -3 5 1627.48 522.220 2
-3 -7 6 184.963 312.332 1
10 -3 6-153.984 240.751 2
-3 -7 7 3145.66 723.874 1
10 -3 7 2358.78 610.447 2
-3 -7 8 209.462 354.321 1
10 -3 8 147.856 239.359 2
-3 -7 9 1026.62 472.767 1
-3 -7 10 557.313 442.781 1
-3 -7 11 6755.63 1067.17 1
-3 -7 12 4606.77 886.111 1
-3 -7 13 1695.62 578.293 1
-2 -8 -11 5391.24 1157.86 1
-2 -8 -10 2368.73 732.462 1
10 -2 -10 3546.65 803.347 2
-2 -8 -9 1495.65 687.081 1
10 -2 -9 584.174 401.018 2
-2 -8 -8 2112.14 726.720 1
10 -2 -8 2840.35 721.775 2
-2 -8 -7 562.287 500.742 1
10 -2 -7 1107.81 560.773 2
10 -2 -6 4733.10 898.176 2
-2 -8 -6 5887.06 1060.15 1
-2 -8 -5 9804.53 1365.32 1
10 -2 -5 6935.83 1075.71 2
-2 -8 -4 2908.01 796.599 1
10 -2 -4 5101.83 911.333 2
-2 -8 -3 2786.98 786.800 1
10 -2 -3 2333.51 679.461 2
-2 -8 -2 3714.79 879.675 1
10 -2 -2 6583.01 1013.62 2
-2 -8 -1 580.831 462.804 1
10 -2 -1 2293.37 640.182 2
-2 -8 0-842.404 693.343 1
10 -2 0-531.140 364.221 2
-2 -8 1 3903.72 885.086 1
10 -2 1 3186.63 730.217 2
10 -2 2 7987.32 1095.16 2
-2 -8 2 7555.10 1171.37 1
10 -2 3 7133.96 1018.52 2
-2 -8 3 6449.65 1084.22 1
-2 -8 4 4757.37 917.186 1
10 -2 4 4269.24 826.165 2
-2 -8 5-410.814 441.960 1
10 -2 5 588.283 429.100 2
-2 -8 6 35.6299 385.661 1
10 -2 6 306.420 291.693 2
-2 -8 7 2308.46 707.446 1
10 -2 7 1547.49 521.023 2
-2 -8 8 7465.38 1105.39 1
10 -2 8 10200.3 1191.30 2
-2 -8 9 927.895 460.303 1
10 -2 9 959.968 467.974 2
-2 -8 10-241.453 346.773 1
10 -2 10 854.520 432.917 2
-2 -8 11 2613.38 727.472 1
-1 -9 -8-264.742 446.734 1
-1 -9 -7 3964.53 948.189 1
10 -1 -7 3357.37 799.025 2
-1 -9 -6 5308.50 1097.78 1
10 -1 -6 5543.39 1002.33 2
-1 -9 -5 342.120 353.737 1
10 -1 -5 1196.77 546.728 2
-1 -9 -4 1717.73 662.266 1
10 -1 -4 3043.84 735.423 2
-1 -9 -3 152.945 440.645 1
10 -1 -3-233.025 386.939 2
-1 -9 -2 1164.77 582.476 1
10 -1 -2 838.345 433.525 2
-1 -9 -1 12407.9 1494.86 1
10 -1 -1 8757.36 1185.32 2
-1 -9 0 6973.35 1137.24 1
10 -1 0 5490.45 941.740 2
10 -1 1 1416.64 547.482 2
-1 -9 1 1107.02 509.974 1
10 -1 2 5735.06 947.679 2
-1 -9 2 5376.49 1005.83 1
10 -1 3 321.288 249.034 2
-1 -9 3-151.487 386.446 1
-1 -9 4-321.458 408.960 1
10 -1 4 492.836 449.415 2
-1 -9 5 6373.98 1073.24 1
10 -1 5 4577.75 882.843 2
-1 -9 6 5539.18 1021.81 1
10 -1 6 4280.88 846.036 2
-1 -9 7 4243.55 903.866 1
10 -1 7 2454.70 675.383 2
-1 -9 8 4677.46 966.525 1
10 -1 8 6076.00 976.738 2
10 -1 9 606.860 396.323 2
10 -1 10 197.199 293.374 2
10 -1 11 816.077 448.373 2
0 -10 -2 3196.80 845.098 1
0 -10 -1-135.334 431.900 1
10 0 -1 1590.62 587.091 2
0 -10 0 353.764 343.925 1
10 0 0 760.990 458.492 2
10 0 1 320.061 341.442 2
0 -10 1-599.182 478.144 1
10 0 2-297.199 402.435 2
0 -10 2 242.633 364.940 1
10 0 3 5946.91 1004.30 2
10 0 4 3292.95 762.012 2
11 -8 -8 5464.55 944.033 2
11 -8 -7 7657.14 1087.02 2
11 -8 -6 1945.55 599.239 2
11 -8 -5 1126.59 461.720 2
11 -7 -9 2675.67 762.275 2
11 -7 -8 1455.59 591.001 2
11 -7 -7 2974.47 754.592 2
11 -7 -6-85.9340 337.057 2
11 -7 -5 3045.98 698.913 2
11 -7 -4 4025.92 802.943 2
11 -7 -3 6497.90 966.510 2
11 -7 -2 1104.46 493.018 2
11 -6 -9 441.936 429.119 2
11 -6 -8 169.340 463.765 2
11 -6 -7 595.436 448.581 2
11 -6 -6 225.572 324.750 2
11 -6 -5 3472.85 747.654 2
11 -6 -4-440.272 385.282 2
11 -6 -3-46.4971 230.393 2
11 -6 -2 469.118 374.457 2
11 -6 -1 2478.50 654.142 2
11 -6 0-26.0949 284.974 2
11 -5 -8 1537.62 569.151 2
11 -5 -7 5302.02 931.143 2
11 -5 -6 5962.90 976.178 2
11 -5 -5 2166.15 672.148 2
11 -5 -4-204.787 353.520 2
11 -5 -3 4784.61 869.047 2
11 -5 -2 3575.56 761.210 2
11 -5 -1 4019.70 831.017 2
11 -5 0 1988.95 594.974 2
11 -5 1 32.4764 293.303 2
11 -5 2 1851.93 590.975 2
11 -5 3-108.076 329.844 2
-4 -7 -10-1250.20 600.442 1
-4 -7 -9 842.950 475.476 1
-4 -7 -8 1301.69 649.700 1
11 -4 -7 3208.77 836.131 2
-4 -7 -7 1630.17 610.864 1
-4 -7 -6 7891.88 1207.55 1
11 -4 -6 7963.58 1165.82 2
-4 -7 -5 6133.23 1095.88 1
11 -4 -5 7155.31 1087.62 2
-4 -7 -4-543.987 626.380 1
11 -4 -4-174.657 331.950 2
-4 -7 -3 6754.20 1095.67 1
11 -4 -3 7651.65 1110.62 2
-4 -7 -2 2633.73 704.464 1
11 -4 -2 5409.93 934.173 2
-4 -7 -1 1316.75 572.116 1
11 -4 -1 2026.01 585.666 2
11 -4 0 1625.11 586.173 2
-4 -7 0 112.500 491.185 1
-4 -7 1 1463.40 624.419 1
11 -4 1 4857.51 851.716 2
-4 -7 2 2623.22 727.238 1
11 -4 2 4278.98 817.744 2
-4 -7 3 6919.00 1059.04 1
11 -4 3 7685.79 1054.83 2
-4 -7 4 5481.71 947.803 1
11 -4 4 5382.85 907.009 2
-4 -7 5 423.262 493.118 1
11 -4 5 619.376 364.484 2
-4 -7 6 906.314 517.638 1
-4 -7 7 847.048 396.725 1
-4 -7 8 2263.69 625.063 1
-4 -7 9 2575.00 697.599 1
-4 -7 10 429.651 441.151 1
-3 -8 -7 3334.75 899.982 1
-3 -8 -6 3403.34 875.602 1
-3 -8 -5 1205.56 592.598 1
11 -3 -5 793.672 488.466 2
-3 -8 -4 1041.90 579.302 1
11 -3 -4 1207.75 528.567 2
-3 -8 -3 21.8287 396.396 1
11 -3 -3 1166.32 489.146 2
-3 -8 -2 3736.08 833.260 1
11 -3 -2 4227.89 867.621 2
-3 -8 -1 2314.52 712.803 1
11 -3 -1 1807.43 559.059 2
11 -3 0 1764.38 590.185 2
-3 -8 0 1231.64 564.757 1
11 -3 1 2581.72 708.522 2
-3 -8 1 2638.72 731.372 1
-3 -8 2 1472.79 594.522 1
11 -3 2 1808.54 606.859 2
-3 -8 3-267.559 383.216 1
11 -3 3 557.703 459.863 2
-3 -8 4 1117.68 506.488 1
11 -3 4 1259.07 491.852 2
-3 -8 5 1581.30 617.815 1
11 -3 5 1688.23 564.602 2
-3 -8 6 514.766 470.353 1
11 -3 6 675.709 456.910 2
-3 -8 7 10409.3 1340.69 1
11 -3 7 7099.28 1036.46 2
-3 -8 8 4473.02 934.320 1
-2 -9 -2 347.772 513.797 1
-2 -9 -1 3718.21 921.722 1
11 -2 0 427.732 399.216 2
-2 -9 0 39.4225 407.383 1
11 -2 1 522.075 368.241 2
-2 -9 1-33.0510 379.084 1
11 -2 2 206.260 365.788 2
-2 -9 2 61.3175 334.155 1
11 -2 3 1212.09 516.934 2
11 -2 4 3323.93 766.499 2
11 -2 5 839.891 457.118 2
12 -6 -3 2970.78 736.871 2
12 -6 -2 1095.74 504.734 2
12 -6 -1 3541.94 779.200 2
12 -5 0 716.148 454.935 2
12 -5 1 3712.02 794.984 2
0 0 0 0.00 0.00 0
TITL xi095 in P3(1)
REM P3(1) (#144 in standard setting)
CELL 0.71073 8.082388 8.082388 18.334128 90.0000 90.0000 120.0000
ZERR 3.00 0.000296 0.000296 0.000763 0.0000 0.0000 0.0000
LATT -1
SYMM -y, x-y, z+1/3
SYMM -x+y,-x, z+2/3
SFAC C O F Cl Sb
UNIT 3.00 3.00 48.00 3.00 9.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 66261
_shelx_res_file
;
TITL shelxt_a.res in P3(1)
shelx.res
created by SHELXL-2019/3 at 09:14:14 on 28-Oct-2024
CELL 0.71073 8.0824 8.0824 18.3341 90.000 90.000 120.000
ZERR 3.00 0.0003 0.0003 0.0008 0.000 0.000 0.000
LATT -1
SYMM - Y, X - Y, 1/3 + Z
SYMM - X + Y, - X, 2/3 + Z
SFAC C O F CL SB
UNIT 3 3 48 3 9
MERG 2
TWIN -1.00 -1.00 0.00 0.00 1.00 0.00 0.00 0.00 -1.00 -4
SHEL1000 0.67
FMAP 2
PLAN 20
SIZE 0.106 0.136 0.190
ACTA
BOND
CONF
LIST 4
L.S. 10
TEMP -171.00
WGHT 0.026200
BASF -0.01219 0.06455 0.09269
FVAR 1.64048
SB2 5 0.633761 -0.035105 0.609350 11.00000 0.01968 0.01976 =
0.01591 0.00027 -0.00068 0.01207
SB3 5 0.618624 -0.003973 0.392940 11.00000 0.01728 0.01879 =
0.01464 -0.00022 0.00033 0.00828
SB1 5 0.362343 0.243975 0.580926 11.00000 0.02397 0.02209 =
0.01819 -0.00258 -0.00272 0.01622
CL1 4 0.066966 0.522097 0.481835 11.00000 0.03177 0.02677 =
0.02325 0.00216 -0.00196 0.01772
F6 3 0.492085 0.103776 0.627581 11.00000 0.02623 0.03323 =
0.01542 0.00033 0.00044 0.02211
F11 3 0.584060 -0.006089 0.505854 11.00000 0.03956 0.03346 =
0.01468 -0.00001 0.00118 0.02583
F14 3 0.354297 -0.121778 0.389619 11.00000 0.02099 0.03261 =
0.01941 -0.00532 -0.00364 0.01129
F12 3 0.875714 0.111183 0.417156 11.00000 0.02557 0.03752 =
0.02806 -0.00793 -0.00529 0.01499
F3 3 0.158168 0.090253 0.639291 11.00000 0.02588 0.03329 =
0.03019 0.00215 -0.00248 0.01675
F7 3 0.844019 0.203386 0.598360 11.00000 0.01864 0.01890 =
0.04648 -0.00092 0.00212 0.00409
F1 3 0.247899 0.367670 0.537009 11.00000 0.04905 0.04261 =
0.02766 -0.00179 -0.01141 0.03449
F15 3 0.652861 0.001479 0.293306 11.00000 0.03171 0.04247 =
0.01583 -0.00284 0.00216 0.01931
F13 3 0.634742 0.232524 0.397625 11.00000 0.04351 0.02287 =
0.02306 0.00213 0.00382 0.01918
F2 3 0.273736 0.051401 0.513152 11.00000 0.03551 0.03158 =
0.02746 -0.00877 -0.01240 0.02090
F9 3 0.659724 -0.050836 0.708282 11.00000 0.04684 0.04511 =
0.02065 0.00131 -0.00594 0.03092
F16 3 0.593749 -0.242014 0.409075 11.00000 0.03504 0.02283 =
0.03178 -0.00406 -0.00737 0.01692
F4 3 0.591987 0.380923 0.532623 11.00000 0.03597 0.02941 =
0.03148 0.00295 0.00716 0.01867
F8 3 0.396665 -0.248711 0.605002 11.00000 0.03245 0.02020 =
0.03667 0.00303 0.00840 0.00945
F5 3 0.461824 0.413791 0.658089 11.00000 0.03396 0.02759 =
0.02322 -0.00743 -0.00495 0.01895
F10 3 0.757150 -0.161675 0.579448 11.00000 0.04175 0.04301 =
0.03423 -0.00245 -0.00505 0.03183
O1 2 -0.088633 0.742413 0.459915 11.00000 0.05773 0.05575 =
0.04292 -0.00032 0.00337 0.04853
C1 1 9.970583 10.646600 10.467900 11.00000 0.04072 0.03747 =
0.01427 -0.00524 -0.00047 0.01901
HKLF 4
REM shelxt_a.res in P3(1)
REM wR2 = 0.0767, GooF = S = 1.032, Restrained GooF = 1.032 for all data
REM R1 = 0.0384 for 3029 Fo > 4sig(Fo) and 0.0462 for all 3334 data
REM 199 parameters refined using 0 restraints
END
WGHT 0.0262 0.0000
REM Highest difference peak 1.356, deepest hole -1.093, 1-sigma level 0.238
Q1 1 0.2614 0.1048 0.5843 11.00000 0.05 1.36
Q2 1 0.7071 -0.0886 0.6123 11.00000 0.05 1.15
Q3 1 0.6113 0.1034 0.4082 11.00000 0.05 1.12
Q4 1 0.5860 -0.1866 0.6088 11.00000 0.05 1.11
Q5 1 0.4926 -0.0209 0.3941 11.00000 0.05 1.10
Q6 1 0.6781 0.1157 0.4039 11.00000 0.05 1.09
Q7 1 0.6009 0.0636 0.6139 11.00000 0.05 1.08
Q8 1 0.3998 0.1388 0.5741 11.00000 0.05 1.05
Q9 1 0.2647 0.2676 0.5668 11.00000 0.05 1.05
Q10 1 0.5483 -0.1432 0.3886 11.00000 0.05 0.97
Q11 1 0.5941 0.0823 0.3068 11.00000 0.05 0.96
Q12 1 0.4782 0.3135 0.5571 11.00000 0.05 0.93
Q13 1 0.7718 -0.0166 0.6006 11.00000 0.05 0.92
Q14 1 0.9340 0.0707 0.6391 11.00000 0.05 0.90
Q15 1 0.4340 0.3882 0.5754 11.00000 0.05 0.89
Q16 1 0.6519 -0.1380 0.5814 11.00000 0.05 0.89
Q17 1 0.6804 -0.0965 0.3912 11.00000 0.05 0.88
Q18 1 0.7033 0.3289 0.6254 11.00000 0.05 0.86
Q19 1 -0.1618 0.6239 0.4622 11.00000 0.05 0.84
Q20 1 0.5166 0.3052 0.5858 11.00000 0.05 0.83
;
_shelx_res_checksum 8685
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
loop_
_atom_site_type_symbol
_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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb Sb2 0.63376(11) -0.03511(10) 0.6093(6) 0.01747(16) Uani d 1 . .
Sb Sb3 0.61862(11) -0.00397(11) 0.3929(6) 0.01723(15) Uani d 1 . .
Sb Sb1 0.36234(12) 0.24398(12) 0.5809(6) 0.01933(17) Uani d 1 . .
Cl Cl1 0.0670(5) 0.5221(5) 0.4818(6) 0.0259(6) Uani d 1 . .
F F6 0.4921(10) 0.1038(10) 0.6276(7) 0.0217(15) Uani d 1 . .
F F11 0.5841(11) -0.0061(11) 0.5059(7) 0.0259(16) Uani d 1 . .
F F14 0.3543(10) -0.1218(11) 0.3896(7) 0.0253(16) Uani d 1 . .
F F12 0.8757(10) 0.1112(12) 0.4172(7) 0.0307(18) Uani d 1 . .
F F3 0.1582(11) 0.0903(10) 0.6393(7) 0.0289(17) Uani d 1 . .
F F7 0.8440(10) 0.2034(10) 0.5984(8) 0.0304(18) Uani d 1 . .
F F1 0.2479(12) 0.3677(12) 0.5370(7) 0.035(2) Uani d 1 . .
F F15 0.6529(11) 0.0015(11) 0.2933(8) 0.0297(19) Uani d 1 . .
F F13 0.6347(12) 0.2325(11) 0.3976(7) 0.0287(18) Uani d 1 . .
F F2 0.2737(11) 0.0514(11) 0.5132(7) 0.0297(17) Uani d 1 . .
F F9 0.6597(12) -0.0508(12) 0.7083(8) 0.034(2) Uani d 1 . .
F F16 0.5937(11) -0.2420(10) 0.4091(7) 0.0288(17) Uani d 1 . .
F F4 0.5920(11) 0.3809(11) 0.5326(7) 0.0313(18) Uani d 1 . .
F F8 0.3967(11) -0.2487(11) 0.6050(7) 0.0314(18) Uani d 1 . .
F F5 0.4618(10) 0.4138(11) 0.6581(7) 0.0267(16) Uani d 1 . .
F F10 0.7572(12) -0.1617(12) 0.5794(7) 0.0349(19) Uani d 1 . .
O O1 -0.0886(17) 0.7424(16) 0.4599(8) 0.043(3) Uani d 1 . .
C C1 -0.029417 0.646600 0.467900 0.031(3) Uani d 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Sb2 0.0197(4) 0.0198(4) 0.0159(4) 0.0121(3) -0.0007(3) 0.0003(3)
Sb3 0.0173(4) 0.0188(4) 0.0146(4) 0.0083(3) 0.0003(3) -0.0002(3)
Sb1 0.0240(4) 0.0221(4) 0.0182(4) 0.0162(4) -0.0027(3) -0.0026(3)
Cl1 0.0318(17) 0.0268(16) 0.0233(15) 0.0177(14) -0.0020(13) 0.0022(13)
F6 0.026(4) 0.033(4) 0.015(3) 0.022(3) 0.000(3) 0.000(3)
F11 0.040(4) 0.033(4) 0.015(3) 0.026(4) 0.001(3) 0.000(3)
F14 0.021(4) 0.033(4) 0.019(4) 0.011(3) -0.004(3) -0.005(3)
F12 0.026(4) 0.038(5) 0.028(4) 0.015(4) -0.005(3) -0.008(3)
F3 0.026(4) 0.033(4) 0.030(4) 0.017(4) -0.002(3) 0.002(3)
F7 0.019(4) 0.019(4) 0.046(5) 0.004(3) 0.002(3) -0.001(3)
F1 0.049(5) 0.043(5) 0.028(4) 0.034(5) -0.011(4) -0.002(4)
F15 0.032(4) 0.042(5) 0.016(4) 0.019(4) 0.002(3) -0.003(3)
F13 0.044(5) 0.023(4) 0.023(4) 0.019(4) 0.004(3) 0.002(3)
F2 0.036(4) 0.032(4) 0.027(4) 0.021(4) -0.012(3) -0.009(3)
F9 0.047(5) 0.045(5) 0.021(5) 0.031(4) -0.006(4) 0.001(4)
F16 0.035(4) 0.023(4) 0.032(4) 0.017(3) -0.007(4) -0.004(3)
F4 0.036(4) 0.029(4) 0.031(4) 0.019(4) 0.007(4) 0.003(4)
F8 0.032(4) 0.020(4) 0.037(5) 0.009(3) 0.008(4) 0.003(3)
F5 0.034(4) 0.028(4) 0.023(4) 0.019(4) -0.005(3) -0.007(3)
F10 0.042(5) 0.043(5) 0.034(5) 0.032(4) -0.005(4) -0.002(4)
O1 0.058(7) 0.056(7) 0.043(7) 0.049(6) 0.003(6) 0.000(6)
C1 0.041(8) 0.037(8) 0.014(6) 0.019(7) 0.000(5) -0.005(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
F8 Sb2 F10 . . 93.8(4) ?
F8 Sb2 F7 . . 165.6(3) ?
F10 Sb2 F7 . . 94.4(4) ?
F8 Sb2 F9 . . 94.6(4) ?
F10 Sb2 F9 . . 98.3(3) ?
F7 Sb2 F9 . . 95.9(4) ?
F8 Sb2 F11 . . 83.8(4) ?
F10 Sb2 F11 . . 88.8(3) ?
F7 Sb2 F11 . . 84.6(4) ?
F9 Sb2 F11 . . 172.9(3) ?
F8 Sb2 F6 . . 85.0(3) ?
F10 Sb2 F6 . . 172.2(3) ?
F7 Sb2 F6 . . 85.3(3) ?
F9 Sb2 F6 . . 89.5(3) ?
F11 Sb2 F6 . . 83.5(3) ?
F15 Sb3 F13 . . 95.1(3) ?
F15 Sb3 F14 . . 95.8(3) ?
F13 Sb3 F14 . . 90.0(3) ?
F15 Sb3 F16 . . 96.9(4) ?
F13 Sb3 F16 . . 168.0(4) ?
F14 Sb3 F16 . . 88.5(3) ?
F15 Sb3 F12 . . 96.2(3) ?
F13 Sb3 F12 . . 89.3(4) ?
F14 Sb3 F12 . . 168.0(3) ?
F16 Sb3 F12 . . 89.7(4) ?
F15 Sb3 F11 . . 179.1(4) ?
F13 Sb3 F11 . . 84.4(3) ?
F14 Sb3 F11 . . 85.0(3) ?
F16 Sb3 F11 . . 83.6(3) ?
F12 Sb3 F11 . . 83.0(3) ?
F3 Sb1 F2 . . 89.0(3) ?
F3 Sb1 F4 . . 169.1(3) ?
F2 Sb1 F4 . . 91.9(4) ?
F3 Sb1 F1 . . 95.5(4) ?
F2 Sb1 F1 . . 94.3(4) ?
F4 Sb1 F1 . . 95.3(4) ?
F3 Sb1 F5 . . 88.1(3) ?
F2 Sb1 F5 . . 170.8(3) ?
F4 Sb1 F5 . . 89.3(4) ?
F1 Sb1 F5 . . 94.6(4) ?
F3 Sb1 F6 . . 85.3(3) ?
F2 Sb1 F6 . . 84.6(3) ?
F4 Sb1 F6 . . 83.9(3) ?
F1 Sb1 F6 . . 178.6(3) ?
F5 Sb1 F6 . . 86.5(3) ?
Sb2 F6 Sb1 . . 146.0(4) ?
Sb2 F11 Sb3 . . 156.6(4) ?
O1 C1 Cl1 . . 176.1(8) ?
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
Sb2 F8 . 1.831(8) ?
Sb2 F10 . 1.834(7) ?
Sb2 F7 . 1.835(7) ?
Sb2 F9 . 1.838(8) ?
Sb2 F11 . 1.978(8) ?
Sb2 F6 . 1.992(6) ?
Sb3 F15 . 1.845(8) ?
Sb3 F13 . 1.852(7) ?
Sb3 F14 . 1.855(7) ?
Sb3 F16 . 1.855(7) ?
Sb3 F12 . 1.857(7) ?
Sb3 F11 . 2.088(8) ?
Sb1 F3 . 1.833(8) ?
Sb1 F2 . 1.834(7) ?
Sb1 F4 . 1.844(8) ?
Sb1 F1 . 1.852(7) ?
Sb1 F5 . 1.852(7) ?
Sb1 F6 . 2.075(7) ?
Cl1 C1 . 1.571(3) ?
O1 C1 . 1.105(10) ?