#------------------------------------------------------------------------------
#$Date: 2024-12-10 04:51:12 +0200 (Tue, 10 Dec 2024) $
#$Revision: 296811 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312734.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_2312734
loop_
_publ_author_name
'Hollenwäger, Dirk'
'Bockmair, Valentin'
'Kornath, Andreas J.'
_publ_section_title
;
The crystal structures of methyl prop-2-ynoate, dimethyl fumarate and
their protonated species.
;
_journal_coeditor_code OJ3025
_journal_issue 1
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229624011653
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac '0.5C6 H10 O4 2+, Sb2 F11 -'
_chemical_formula_moiety '0.5(C6 H10 O4 2+), F11 Sb2 -'
_chemical_formula_sum 'C3 H5 F11 O2 Sb2'
_chemical_formula_weight 525.57
_chemical_name_systematic
;
Hemi{[1,4-dimethoxy-4-oxidaniumylidenebut-2-en-1-ylidene]oxidanium}
undecafluorodiarsenate
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 61
_space_group_name_Hall '-P 2ac 2ab'
_space_group_name_H-M_alt 'P b c a'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 7.8461(6)
_cell_length_b 15.1531(11)
_cell_length_c 19.5536(17)
_cell_measurement_reflns_used 3099
_cell_measurement_temperature 101(2)
_cell_measurement_theta_max 31.4330
_cell_measurement_theta_min 3.0730
_cell_volume 2324.8(3)
_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
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 101(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.923
_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 0.0526
_diffrn_reflns_av_unetI/netI 0.0541
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 13316
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 32.201
_diffrn_reflns_theta_min 2.883
_diffrn_source_current 40
_diffrn_source_voltage 50
_exptl_absorpt_coefficient_mu 4.786
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.80661
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2020)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 3.003
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle
_exptl_crystal_F_000 1920
_exptl_crystal_size_max 0.247
_exptl_crystal_size_mid 0.109
_exptl_crystal_size_min 0.049
_refine_diff_density_max 1.088
_refine_diff_density_min -1.007
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.040
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 169
_refine_ls_number_reflns 3784
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.040
_refine_ls_R_factor_all 0.0568
_refine_ls_R_factor_gt 0.0362
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0210P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0633
_refine_ls_wR_factor_ref 0.0706
_reflns_number_gt 2878
_reflns_number_total 3784
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file oj3025.cif
_cod_data_source_block VII
_cod_database_code 2312734
_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 0.384
_shelx_estimated_absorpt_t_max 0.799
_shelx_hkl_file
;
0 0 2-3.24914 8.14350 2
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0 0 4 100499. 2115.53 2
0 0 5-6.59546 25.2271 2
0 0 6 2351.82 124.911 2
0 0 7 20.9187 26.6705 2
0 0 8 1318.97 104.253 2
0 0 9 41.2277 32.7877 2
0 0 10 10.6519 38.3645 2
0 0 11 129.667 51.4060 2
0 0 12 5030.92 252.244 2
0 0 13 805.497 116.520 2
0 0 14 19241.9 625.500 2
0 0 15 600.223 109.166 2
0 0 16 10943.8 458.153 2
0 0 17 795.087 129.948 2
0 0 18 13559.7 551.426 2
0 0 19 346.447 90.6320 2
0 0 20 3095.04 252.377 2
0 0 21 229.927 79.8517 2
0 0 22 3872.95 296.113 2
0 0 23 46.1766 58.0174 2
0 0 24 117.264 69.8485 2
0 0 25 39.4006 58.0354 2
0 0 26 35.1087 47.9961 2
0 0 27 91.2162 57.0850 2
0 0 28 68.7480 61.5276 2
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0 -1 1 6.74374 5.49197 1
0 1 2-2.92573 11.5361 2
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0 -1 3 3.50619 11.8812 2
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0 -1 5 20.3717 19.7881 2
0 1 5 1.49135 30.6596 2
0 -1 6-5.35964 24.7215 2
0 1 6-9.19938 29.8717 2
0 -1 7 65.3727 32.1722 2
0 1 7 56.6282 38.8523 2
0 1 8 26.0221 34.6728 2
0 -1 8 12.0153 32.3225 2
0 1 9 10.9146 30.8544 2
0 -1 9 21.9506 30.0949 2
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0 1 10-3.68522 31.1909 2
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0 -1 12 28.1313 33.4208 2
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0 1 17 4.16097 41.0252 2
0 -1 17 11.4983 40.4000 2
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0 1 18 53.1780 41.5656 2
0 -1 19-82.5326 54.5786 2
0 1 19-18.7469 45.0644 2
0 -1 20 10.3928 56.5618 2
0 1 20 3.44706 43.1721 2
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0 1 21 68.2211 58.6656 2
0 1 22 14.4641 51.1763 2
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0 1 23-39.4948 55.2136 2
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0 -1 24 70.4829 61.8883 2
0 1 24-69.1245 53.4613 2
0 -1 25 263.937 98.2987 2
0 1 25 89.4772 67.5385 2
0 -1 26-9.73380 41.0073 2
0 1 26 42.2516 58.9010 2
0 1 27-2.65477 48.6873 2
0 -1 27-133.562 72.1527 2
0 1 28 25.6328 60.6844 2
0 1 29-15.3542 70.4654 2
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0 2 1 16.4466 14.6117 2
0 2 1 5.49333 9.76280 3
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0 -2 2 3693.33 114.056 1
0 2 2 3736.31 128.255 2
0 -2 3 17770.6 426.789 1
0 2 3 16468.0 444.022 2
0 -2 3 19056.1 399.955 2
0 2 4 9500.81 291.550 2
0 -2 4 10192.3 249.598 2
0 2 5 19260.0 497.235 2
0 -2 5 18213.7 443.516 2
0 2 6 2265.48 142.033 2
0 -2 6 2577.08 114.016 2
0 -2 7 4100.69 165.037 2
0 2 7 4509.60 201.183 2
0 -2 8 345.811 52.7383 2
0 2 8 266.001 64.6095 2
0 -2 9 21560.5 579.286 2
0 2 9 21982.2 619.551 2
0 2 10 13950.8 464.759 2
0 -2 10 13641.9 420.741 2
0 -2 11 267.315 55.9653 2
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0 -2 13 20751.5 622.442 2
0 -2 14 15523.5 528.504 2
0 2 14 16695.6 578.248 2
0 2 15 868.640 124.236 2
0 -2 15 892.676 112.901 2
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0 -2 16 1532.63 147.488 2
0 2 17 344.690 97.5359 2
0 -2 17 449.479 95.9187 2
0 2 18 1888.02 194.428 2
0 -2 18 2263.00 194.487 2
0 -2 19 466.136 104.464 2
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0 2 21 4273.26 318.566 2
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0 -2 23 315.191 104.473 2
0 2 23 367.290 113.761 2
0 2 24 3625.41 315.200 2
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0 -2 25 5170.74 353.561 2
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0 3 3 8.62606 27.7727 2
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0 3 4-14.6748 32.4655 2
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0 -3 6-6.19568 16.0597 2
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0 3 7 30.3230 37.9216 2
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0 3 8 9.53617 34.8567 2
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0 6 -2 115.658 17.1340 2
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0 6 3 11320.4 343.519 2
0 -6 4 21.3371 23.4939 1
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0 6 5 5227.77 224.937 2
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0 -7 3-41.5048 30.2553 1
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0 7 8 41.4887 39.2647 2
0 -7 8 10.5809 9.58059 2
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0 -7 13-10.3071 23.0227 2
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0 7 26-15.1213 86.5099 2
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0 8 0 11200.0 314.438 2
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0 -8 1 455.737 59.8430 1
0 -8 -1 470.775 66.3085 1
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10 1 4 243.754 90.5551 3
-10 1 4 243.630 79.8789 2
10 -1 5 23.1216 47.2835 3
10 1 5-29.5351 63.9931 3
-10 -1 5 178.324 66.8012 2
-10 1 5 79.1947 60.2679 2
-10 -1 6 2401.46 226.149 2
10 -1 6 2393.06 238.913 3
10 1 6 2212.64 237.703 3
-10 1 6 2764.86 244.402 2
10 -1 7 168.148 63.4849 3
10 1 7 271.872 89.8761 3
-10 -1 7 263.644 80.1707 2
-10 1 7 342.176 89.7978 2
10 -1 8 674.883 132.146 3
10 1 8 658.562 135.200 3
-10 -1 8 654.075 119.435 2
-10 1 8 658.909 125.116 2
10 -1 9 176.700 77.0408 3
10 1 9 159.933 78.4419 3
-10 -1 9 185.934 68.5119 2
-10 1 9 154.918 71.7493 2
10 -1 10 2850.52 271.030 3
10 1 10 2433.50 261.467 3
-10 -1 10 2301.39 224.132 2
-10 1 10 2410.36 234.504 2
10 1 11 192.112 81.6497 3
10 -1 11 135.637 74.0126 3
-10 -1 11 224.707 90.8938 2
-10 1 11 396.350 114.761 2
10 -1 12 284.156 87.2273 3
10 1 12 336.326 117.084 3
-10 -1 12 206.618 75.0629 2
-10 1 12 304.377 89.1623 2
10 -1 13 45.1664 46.8329 3
10 1 13 119.847 87.0030 3
-10 -1 13 239.955 84.1192 2
-10 1 13 131.944 84.0105 2
10 -1 14 1112.30 176.557 3
10 1 14 993.103 177.197 3
-10 -1 14 882.734 146.573 2
10 -1 15 605.604 139.464 3
10 2 0 293.282 97.3810 3
10 -2 0 243.177 82.5049 3
10 2 1 115.868 74.7859 3
10 -2 1 47.3476 39.8141 3
10 2 -1 117.760 68.3296 3
10 -2 -1-105.010 72.6730 3
10 2 -2-36.8943 57.0537 3
10 -2 -2-51.5461 61.8702 3
10 2 2 30.3002 46.4692 3
10 -2 2-67.3740 57.4660 3
10 2 -3 443.772 121.946 3
10 -2 3 337.677 97.0343 3
10 2 3 531.150 128.702 3
10 -2 -3 166.823 67.6688 3
-10 2 3 365.609 98.5873 2
10 -2 -4 349.262 102.790 3
10 -2 4 549.618 116.360 3
10 2 4 392.215 105.154 3
10 2 -4 363.892 97.8709 3
-10 2 4 414.666 99.4082 2
10 -2 5-71.3439 58.8670 3
10 2 5 14.3737 48.3042 3
-10 2 5 79.3292 67.7639 2
10 -2 6-32.0864 47.6990 3
10 2 6 94.7362 73.7529 3
-10 -2 6-10.8374 39.1557 2
-10 2 6 41.2463 53.5373 2
10 -2 7 252.116 84.4318 3
10 2 7 314.972 101.328 3
-10 -2 7 293.305 81.1791 2
-10 2 7 294.056 91.4123 2
10 -2 8 18.2562 49.7995 3
10 2 8 86.2997 66.8289 3
-10 -2 8 137.733 73.7563 2
-10 2 8 64.1878 56.4742 2
10 -2 9 55.8975 40.1006 3
10 2 9 110.425 57.7354 3
-10 -2 9 140.921 73.0731 2
-10 2 9 82.8366 63.8251 2
10 -2 10 61.6153 61.9464 3
10 2 10 49.6150 67.4243 3
-10 -2 10 117.204 64.0422 2
-10 2 10-2.03699 42.3766 2
10 2 11-21.8728 66.9586 3
10 -2 11-97.9428 76.6025 3
-10 -2 11 94.5064 62.3051 2
-10 2 11 78.6498 64.3655 2
10 -2 12-22.7795 47.7752 3
10 2 12 18.8899 56.4026 3
-10 -2 12 73.9702 37.1201 2
-10 2 12-47.6275 53.2550 2
10 -2 13 121.593 72.6387 3
10 2 13 5.00585 54.2323 3
-10 -2 13 66.4732 62.7306 2
-10 2 13-7.80420 51.6900 2
-10 -2 14 61.5065 52.1999 2
-10 -2 15 90.0555 60.6131 2
10 3 0 2942.47 270.661 3
10 -3 0 2694.89 243.885 3
10 3 1 1322.56 181.734 3
10 -3 1 1165.17 159.742 3
10 3 -1 1372.83 189.141 3
10 -3 -1 1190.43 159.862 3
10 3 -2-16.6530 48.8289 3
10 -3 -2-26.7218 46.8457 3
10 3 2-39.0792 49.0088 3
10 -3 2-56.7320 69.5944 3
-10 3 2-6.78675 47.4890 2
10 -3 3 1568.10 187.499 3
10 3 -3 1196.84 179.280 3
10 3 3 1742.38 214.005 3
10 -3 -3 1404.86 181.553 3
-10 3 3 1506.53 185.001 2
10 -3 -4 1672.77 213.304 3
10 -3 4 2015.41 210.015 3
10 3 4 1825.51 218.412 3
-10 3 4 1878.63 205.833 2
10 3 -4 2315.07 249.391 3
10 3 -5 315.780 99.0045 3
10 -3 5 279.622 92.3128 3
10 3 5 464.487 112.577 3
-10 3 5 325.224 83.5223 2
10 -3 6 61.9973 67.3363 3
10 3 6 169.815 91.9406 3
-10 3 6 16.6489 39.6639 2
10 -3 7 71.1890 53.3315 3
10 3 7 152.998 80.8447 3
-10 3 7 140.474 59.5510 2
10 -3 8 36.0736 43.3954 3
10 3 8 6.00128 57.4569 3
-10 -3 8-26.7063 43.8884 2
-10 3 8-14.4171 58.7633 2
10 -3 9-173.231 71.2296 3
10 3 9 17.2236 49.9237 3
-10 -3 9-13.4739 36.1075 2
-10 3 9-123.203 71.0813 2
10 -3 10 35.3234 50.3542 3
10 3 10-121.043 84.2920 3
-10 -3 10 23.4493 45.0655 2
-10 3 10 66.4305 57.1944 2
10 3 11 431.178 115.040 3
-10 -3 11 468.029 101.002 2
-10 3 11 270.660 87.1937 2
10 3 12 482.866 126.826 3
-10 -3 12 211.218 69.4635 2
-10 3 12 484.475 118.676 2
-10 -3 13 24.4263 40.5921 2
10 4 0 795.769 143.723 3
10 -4 0 1036.84 153.255 3
10 -4 1 16.2788 38.8975 3
10 4 -1-13.2021 49.6066 3
10 -4 -1 25.7712 41.1044 3
10 4 1 81.6453 74.0275 3
-10 4 1 42.5879 50.8080 2
10 4 -2 90.1264 64.5222 3
10 -4 -2 260.111 82.6730 3
10 4 2 39.0134 51.5976 3
10 -4 2 123.284 56.3613 3
-10 4 2 87.9757 63.5353 2
10 4 -3-5.34632 52.0136 3
10 -4 3-43.3642 43.7819 3
10 4 3 104.337 75.6198 3
10 -4 -3-32.5740 50.9150 3
-10 4 3 19.8308 58.7643 2
10 -4 -4 296.850 110.462 3
10 -4 4 96.5715 59.8032 3
10 4 4 104.101 74.2345 3
10 4 -4 209.836 77.5983 3
-10 4 4 177.354 61.5507 2
10 4 -5 9.54844 60.6976 3
10 -4 5 235.933 81.6988 3
10 4 5 173.631 79.8985 3
-10 4 5 96.1828 71.4426 2
10 4 6 151.429 76.8993 3
-10 4 6 137.554 71.9020 2
10 4 7-5.38825 47.0037 3
-10 4 7 7.31703 49.7583 2
10 4 8-44.7506 58.9069 3
-10 4 8 14.4365 52.0077 2
10 4 9 368.021 110.104 3
-10 -4 9 211.458 74.6587 2
-10 4 9 158.512 79.2970 2
10 4 10 12.8991 53.4626 3
-10 -4 10 3.07300 33.0554 2
-10 4 10 2.31246 44.6434 2
10 4 11 69.9626 58.2272 3
-10 -4 11-33.6637 35.4544 2
-10 4 11-68.8759 82.5863 2
10 4 12 229.361 87.0800 3
-10 -4 12 158.066 77.3899 2
10 5 0 972.377 161.447 3
10 -5 0 753.294 124.199 3
10 5 -1 120.017 69.4485 3
10 -5 -1 101.079 57.6871 3
10 5 1 200.287 89.5764 3
-10 5 1 288.976 97.6249 2
10 5 -2 30.8381 53.3865 3
10 -5 -2 10.6112 48.8238 3
10 5 2 89.5025 57.4324 3
-10 5 2 72.3983 66.1289 2
10 5 -3 49.5119 65.0276 3
10 5 3 219.107 94.6971 3
10 -5 -3 198.129 74.5653 3
-10 5 3 167.470 73.5171 2
10 -5 -4 221.845 88.1182 3
10 5 4 422.317 105.198 3
10 5 -4 319.058 110.128 3
-10 5 4 197.789 79.6404 2
10 5 5 1491.93 204.623 3
10 5 -5 1881.32 229.195 3
-10 5 5 1789.47 205.413 2
10 5 -6 74.6514 63.1944 3
10 5 6 168.502 76.4491 3
-10 5 6 117.120 59.5850 2
10 5 7 307.243 112.485 3
-10 5 7 389.405 112.392 2
10 5 8 83.3724 73.6736 3
-10 5 8-45.7060 47.4167 2
-10 5 9 3448.18 304.010 2
10 5 9 3843.38 331.872 3
10 5 10 164.991 94.4634 3
-10 5 10 243.582 100.883 2
10 5 11 257.092 93.2978 3
10 6 0 39.7849 74.3702 3
10 6 1-39.0512 67.8015 3
-10 6 1 56.9614 56.0348 2
10 6 -2-31.3628 61.5189 3
10 6 2 4.48902 55.2125 3
-10 6 2 81.6016 61.1380 2
10 6 -3 424.660 102.996 3
10 6 3 374.890 106.307 3
-10 6 3 417.600 102.575 2
10 6 4 31.9745 61.8365 3
10 6 -4 80.4996 84.7239 3
-10 6 4 41.5885 48.5937 2
10 6 5 458.581 114.710 3
10 6 -5 534.971 128.412 3
-10 6 5 549.945 116.973 2
10 6 6 107.009 79.2205 3
10 6 -6 103.779 82.5256 3
-10 6 6-61.6105 47.3457 2
10 6 7 347.829 111.795 3
-10 6 7 263.320 92.9063 2
10 6 8 44.3808 74.5126 3
-10 6 8-23.6320 57.5836 2
10 6 9 1168.14 189.887 3
-10 6 9 949.015 165.338 2
-10 7 0 2861.57 266.703 2
10 7 0 3120.90 292.808 3
10 7 -1 391.119 101.581 3
10 7 1 384.921 105.400 3
-10 7 1 361.764 103.871 2
10 7 -2 383.622 112.100 3
10 7 2 218.348 85.3671 3
-10 7 2 100.924 89.2325 2
10 7 -3 126.694 77.8365 3
10 7 3 116.434 73.3589 3
-10 7 3 76.6090 61.1139 2
10 7 -4 1128.41 174.998 3
10 7 4 864.884 161.056 3
-10 7 4 988.238 160.288 2
10 7 5 1554.63 210.790 3
10 7 -5 1378.74 193.156 3
-10 7 5 1069.33 166.736 2
10 7 6 246.113 103.759 3
10 7 -6 275.544 101.460 3
-10 7 6 39.4451 60.9752 2
10 7 -7 226.331 70.0516 3
10 7 7 174.265 78.1131 3
-10 7 7 353.371 99.5748 2
10 7 8 44.3055 99.4604 3
-10 7 8 23.8977 57.8985 2
10 8 0 668.416 137.644 3
-10 8 0 433.269 116.374 2
10 8 1 173.846 102.541 3
10 8 -1 234.468 85.3188 3
-10 8 1 140.557 76.8367 2
10 8 -2-21.2025 54.6034 3
10 8 2-90.3197 53.2034 3
-10 8 2 15.7607 53.5135 2
10 8 -3 17.4052 49.7184 3
10 8 3 145.428 78.1747 3
-10 8 3 86.2308 63.9168 2
10 8 -4 195.198 95.7286 3
10 8 4 64.5997 57.7982 3
-10 8 4 192.315 89.9560 2
10 8 5 21.2107 75.3079 3
10 8 -5 63.0934 75.6743 3
-10 8 5-82.2016 52.4148 2
10 8 6 219.382 107.092 3
10 8 -6 28.6011 53.0446 3
-10 8 6 86.2561 77.6161 2
10 8 -7 41.8558 53.6741 3
-10 8 7 59.2739 52.4801 2
10 9 0 1874.49 232.054 3
-10 9 0 1225.16 176.888 2
10 9 1 1006.94 170.818 3
10 9 -1 828.837 151.978 3
-10 9 1 709.543 137.338 2
10 9 -2 82.4463 86.3305 3
10 9 2 119.864 76.3476 3
-10 9 2 79.2997 74.0723 2
10 9 -3 1077.23 172.070 3
10 9 3 1252.10 193.529 3
-10 9 3 1152.39 170.940 2
10 9 -4 1246.00 189.502 3
10 9 4 1290.80 195.513 3
-10 9 4 1263.44 182.855 2
10 9 -5-78.1580 83.3186 3
-10 9 5 131.795 83.3259 2
-10 10 0 153.898 60.3201 2
-10 10 1 148.340 86.7390 2
-10 10 2-45.0499 59.2895 2
-10 10 3 306.292 101.514 2
11 0 0-48.4888 66.9855 3
11 0 -1 15.4677 51.4618 3
11 0 1 140.525 72.9844 3
11 0 2 2593.66 266.562 3
11 0 -2 3259.31 297.766 3
11 0 -3 39.7504 76.7304 3
11 0 3-97.8454 76.3133 3
11 0 4-86.9665 69.4037 3
11 0 -4 59.1480 60.5756 3
11 0 5-89.8279 74.3253 3
11 0 -5 18.7403 60.2513 3
11 0 -6 911.379 171.169 3
11 0 6 1199.97 180.436 3
11 0 7 23.1440 46.5220 3
-11 0 7-2.90516 53.2400 2
11 0 8 115.448 72.5022 3
11 0 9-16.8316 61.0696 3
11 1 0-9.70624 53.6701 3
11 -1 0 56.2351 49.3581 3
11 1 -1 310.669 100.762 3
11 -1 -1 206.292 86.2210 3
11 1 1 192.850 80.7727 3
11 -1 1 68.9488 55.0944 3
11 1 -2 89.3455 79.2971 3
11 -1 -2 22.0817 49.2104 3
11 -1 2 39.5374 54.1340 3
11 1 2 69.3923 50.9847 3
11 1 -3 83.8739 64.0704 3
11 -1 -3 15.5442 51.1298 3
11 -1 3-41.9671 64.3104 3
11 1 3 131.976 87.2938 3
11 -1 4 336.019 99.2464 3
11 1 4 477.668 121.823 3
11 1 -4 369.065 114.692 3
11 -1 -4 287.817 87.5281 3
11 -1 5 172.021 82.7135 3
11 1 5 150.098 66.1982 3
11 1 -5 152.795 86.9123 3
11 -1 -5 256.398 86.2421 3
11 1 -6 32.7171 56.3567 3
11 -1 -6 73.2278 61.4949 3
11 -1 6 82.8824 58.3744 3
11 1 6-22.8507 79.9490 3
-11 1 6-16.2233 47.3952 2
11 -1 7 2.90565 51.0351 3
11 1 7 53.2314 53.3141 3
11 -1 8 792.581 153.262 3
11 1 8 840.073 166.456 3
11 -1 9 63.2372 72.3705 3
11 -2 0 39.3375 69.6976 3
11 2 0-31.8316 59.1940 3
11 2 -1 278.873 106.695 3
11 -2 -1 157.220 78.1984 3
11 2 1 29.1962 53.3418 3
11 -2 1 29.6573 47.8049 3
11 2 -2 636.380 137.497 3
11 -2 -2 593.641 126.353 3
11 -2 2 403.835 114.839 3
11 2 2 576.428 136.836 3
11 2 -3 46.5362 54.6600 3
11 -2 -3 76.7860 75.4145 3
11 -2 3-28.9766 55.5059 3
11 2 3 43.9470 62.2662 3
11 -2 4-6.52431 64.0827 3
11 2 4 151.523 76.7047 3
11 2 -4 90.8440 75.4547 3
11 -2 -4 187.314 78.3118 3
11 -2 5 500.561 117.252 3
11 2 5 350.502 99.4254 3
11 2 -5 546.732 130.871 3
11 -2 -5 363.752 116.916 3
-11 2 5 375.949 100.313 2
11 -2 -6 218.138 99.9517 3
11 -2 6 261.111 81.0963 3
11 2 6 282.082 84.4846 3
11 -2 7 1048.53 167.237 3
11 2 7 840.223 152.296 3
11 -2 8 480.488 105.379 3
11 -2 9 113.091 69.1182 3
11 3 0-140.442 87.9585 3
11 -3 0 58.2211 71.3993 3
11 3 -1 343.783 108.875 3
11 -3 -1 173.315 76.5562 3
11 3 1 447.384 124.357 3
11 -3 1 309.529 93.3544 3
11 3 -2 367.768 96.6356 3
11 -3 -2 331.461 96.7295 3
11 -3 2 351.766 102.218 3
11 3 2 182.519 78.3141 3
11 3 -3 284.988 93.5536 3
11 -3 -3 251.081 92.6338 3
11 -3 3 256.627 87.6125 3
11 3 3 123.440 66.3823 3
11 -3 4 132.144 65.9465 3
11 3 -4 212.033 100.168 3
11 3 4 53.2944 49.0871 3
11 -3 -4 1.46328 53.8463 3
11 -3 5 470.061 110.912 3
11 3 5 536.153 131.612 3
11 -3 -5 403.746 117.201 3
11 -3 -6 85.0850 55.5012 3
11 4 0 15.1195 58.3650 3
11 -4 0 56.3202 58.0890 3
11 4 -1 297.878 110.381 3
11 -4 -1 165.903 75.3992 3
11 4 1 381.779 118.445 3
11 4 -2 14.1389 49.8073 3
11 -4 -2 31.8869 54.9813 3
11 4 2-10.4645 54.9485 3
11 -4 -3 426.183 110.239 3
11 4 3 773.282 164.463 3
11 -4 -4 581.033 130.674 3
11 -4 -5-28.6394 51.1347 3
11 -4 -6 182.099 83.0624 3
0 0 0 0.00 0.00 0
TITL xi082 in Pbca
REM Pbca (#61 in standard setting)
CELL 0.71073 7.846147 15.153072 19.553578 90.0000 90.0000 90.0000
ZERR 1.00 0.000649 0.001065 0.001719 0.0000 0.0000 0.0000
LATT 1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H O F Sb
UNIT 24.00 32.00 24.00 80.00 16.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 46381
_shelx_res_file
;
TITL shelxt_a.res in Pbca
shelx.res
created by SHELXL-2018/3 at 09:18:30 on 17-Nov-2021
CELL 0.71073 7.8461 15.1531 19.5536 90.000 90.000 90.000
ZERR 8.00 0.0006 0.0011 0.0017 0.000 0.000 0.000
LATT 1
SYMM 1/2 - X, - Y, 1/2 + Z
SYMM - X, 1/2 + Y, 1/2 - Z
SYMM 1/2 + X, 1/2 - Y, - Z
SFAC C H O F SB
UNIT 24 40 16 88 16
MERG 2
OMIT 0 0 2
OMIT 0 2 0
HTAB O1 F1
EQIV $2 -x+3/2, y+1/2, z
HTAB C3 F9_$2
HTAB C3 F8
EQIV $3 x-1/2, -y+1/2, -z+1
HTAB C2 F10_$3
FMAP 2
PLAN 20
SIZE 0.049 0.109 0.247
ACTA
HTAB 2.00000
BOND
CONF
LIST 6
L.S. 10
TEMP -172.00
WGHT 0.021000
FVAR 0.46183
SB1 5 0.532887 0.119508 0.588836 11.00000 0.02181 0.01431 =
0.01902 0.00006 -0.00136 -0.00328
SB2 5 0.879798 0.294346 0.645181 11.00000 0.02106 0.01545 =
0.02066 0.00125 -0.00279 -0.00268
F6 4 0.687801 0.201733 0.641869 11.00000 0.03613 0.02505 =
0.02584 -0.00143 -0.00115 -0.01643
F4 4 0.380740 0.046181 0.543526 11.00000 0.02744 0.02273 =
0.02604 -0.00626 -0.00331 -0.00477
F11 4 1.050074 0.379492 0.647440 11.00000 0.02207 0.02753 =
0.04793 0.00295 -0.00487 -0.00795
F7 4 0.763056 0.342552 0.571014 11.00000 0.03085 0.02778 =
0.02133 0.00617 -0.00237 0.00273
F1 4 0.412053 0.222817 0.565548 11.00000 0.03598 0.01941 =
0.03111 -0.00224 -0.00331 0.00617
F8 4 0.735721 0.356279 0.703739 11.00000 0.03392 0.03169 =
0.02827 -0.01016 0.00507 -0.00492
F2 4 0.409561 0.112946 0.669851 11.00000 0.03890 0.04158 =
0.01892 0.00128 0.00488 -0.01564
F3 4 0.672340 0.139573 0.513226 11.00000 0.03045 0.02823 =
0.02469 -0.00255 0.00937 -0.00346
O2 3 0.452137 0.521553 0.624368 11.00000 0.02778 0.01783 =
0.01689 -0.00288 0.00217 -0.00136
F5 4 0.678931 0.031136 0.618910 11.00000 0.03305 0.02406 =
0.05090 0.01029 -0.01424 -0.00107
F10 4 0.995819 0.219393 0.585518 11.00000 0.03335 0.02540 =
0.04572 -0.00706 0.00455 0.00474
F9 4 0.962324 0.230035 0.718615 11.00000 0.04905 0.03521 =
0.03983 0.01445 -0.01710 -0.00766
O1 3 0.406524 0.379408 0.615806 11.00000 0.02526 0.01608 =
0.02633 -0.00020 0.00404 0.00052
AFIX 147
H1 2 0.400397 0.339397 0.586174 11.00000 -1.50000
AFIX 0
C1 1 0.447040 0.452136 0.587052 11.00000 0.01613 0.01578 =
0.02059 -0.00223 -0.00151 0.00451
C3 1 0.420356 0.513630 0.699204 11.00000 0.04067 0.02728 =
0.01706 -0.00385 0.00066 0.00220
AFIX 137
H4 2 0.312992 0.482094 0.706860 11.00000 -1.50000
H5 2 0.413086 0.572665 0.719463 11.00000 -1.50000
H3 2 0.514077 0.480919 0.720535 11.00000 -1.50000
AFIX 0
C2 1 0.488803 0.460432 0.514251 11.00000 0.01748 0.01856 =
0.02059 -0.00203 0.00062 0.00074
H2 2 0.498060 0.410428 0.487649 11.00000 0.00601
HKLF 4
REM shelxt_a.res in Pbca
REM wR2 = 0.0706, GooF = S = 1.040, Restrained GooF = 1.040 for all data
REM R1 = 0.0362 for 2878 Fo > 4sig(Fo) and 0.0568 for all 3784 data
REM 169 parameters refined using 0 restraints
END
WGHT 0.0211 0.0000
REM Instructions for potential hydrogen bonds
HTAB O1 F1
HTAB C3 F9_$2
HTAB C3 F8
HTAB C2 F10_$3
REM Highest difference peak 1.088, deepest hole -1.007, 1-sigma level 0.202
Q1 1 0.4184 0.1184 0.5897 11.00000 0.05 1.09
Q2 1 0.8656 0.3334 0.6748 11.00000 0.05 0.97
Q3 1 0.5223 0.1445 0.6213 11.00000 0.05 0.96
Q4 1 0.9918 0.2912 0.6427 11.00000 0.05 0.92
Q5 1 0.8799 0.2930 0.5302 11.00000 0.05 0.90
Q6 1 0.9156 0.3010 0.5918 11.00000 0.05 0.88
Q7 1 1.0449 0.3028 0.6468 11.00000 0.05 0.84
Q8 1 0.5330 0.0833 0.6191 11.00000 0.05 0.83
Q9 1 0.5388 0.1546 0.5590 11.00000 0.05 0.80
Q10 1 0.3048 0.4990 0.6781 11.00000 0.05 0.77
Q11 1 0.6269 -0.0244 0.6440 11.00000 0.05 0.76
Q12 1 0.9325 0.3631 0.6501 11.00000 0.05 0.76
Q13 1 0.4655 0.1803 0.5842 11.00000 0.05 0.74
Q14 1 0.4615 0.0824 0.5333 11.00000 0.05 0.74
Q15 1 0.9104 0.2442 0.6081 11.00000 0.05 0.73
Q16 1 0.3694 0.3702 0.5541 11.00000 0.05 0.73
Q17 1 0.5689 0.0954 0.5390 11.00000 0.05 0.72
Q18 1 0.8181 0.3349 0.6061 11.00000 0.05 0.71
Q19 1 0.6012 0.0530 0.5869 11.00000 0.05 0.71
Q20 1 0.7782 0.0890 0.5282 11.00000 0.05 0.69
;
_shelx_res_checksum 56029
loop_
_space_group_symop_operation_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_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 Sb1 0.53289(3) 0.11951(2) 0.58884(2) 0.01838(7) Uani d 1 . .
Sb Sb2 0.87980(3) 0.29435(2) 0.64518(2) 0.01906(8) Uani d 1 . .
F F6 0.6878(3) 0.20173(15) 0.64187(14) 0.0290(6) Uani d 1 . .
F F4 0.3807(3) 0.04618(14) 0.54353(14) 0.0254(6) Uani d 1 . .
F F11 1.0501(3) 0.37949(16) 0.64744(16) 0.0325(7) Uani d 1 . .
F F7 0.7631(3) 0.34255(15) 0.57101(14) 0.0267(6) Uani d 1 . .
F F1 0.4121(3) 0.22282(15) 0.56555(15) 0.0288(6) Uani d 1 . .
F F8 0.7357(3) 0.35628(15) 0.70374(15) 0.0313(6) Uani d 1 . .
F F2 0.4096(4) 0.11295(17) 0.66985(15) 0.0331(6) Uani d 1 . .
F F3 0.6723(3) 0.13957(15) 0.51323(14) 0.0278(6) Uani d 1 . .
O O2 0.4521(4) 0.52155(17) 0.62437(16) 0.0208(6) Uani d 1 . .
F F5 0.6789(3) 0.03114(16) 0.61891(17) 0.0360(7) Uani d 1 . .
F F10 0.9958(3) 0.21939(16) 0.58552(17) 0.0348(7) Uani d 1 . .
F F9 0.9623(4) 0.23004(17) 0.71862(17) 0.0414(8) Uani d 1 . .
O O1 0.4065(4) 0.37941(18) 0.61581(18) 0.0226(6) Uani d 1 . .
H H1 0.400397 0.339397 0.586174 0.034 Uiso calc 1 . .
C C1 0.4470(5) 0.4521(2) 0.5871(2) 0.0175(8) Uani d 1 . .
C C3 0.4204(6) 0.5136(3) 0.6992(3) 0.0283(10) Uani d 1 . .
H H4 0.312992 0.482094 0.706860 0.043 Uiso calc 1 . .
H H5 0.413086 0.572665 0.719463 0.043 Uiso calc 1 . .
H H3 0.514077 0.480919 0.720535 0.043 Uiso calc 1 . .
C C2 0.4888(5) 0.4604(3) 0.5143(2) 0.0189(9) Uani d 1 . .
H H2 0.498(5) 0.410(3) 0.488(2) 0.006(10) Uiso 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
Sb1 0.02181(13) 0.01431(12) 0.01902(15) -0.00328(10) -0.00136(11) 0.00006(12)
Sb2 0.02106(13) 0.01545(12) 0.02066(16) -0.00268(10) -0.00279(11) 0.00125(12)
F6 0.0361(14) 0.0251(12) 0.0258(16) -0.0164(10) -0.0012(12) -0.0014(12)
F4 0.0274(13) 0.0227(11) 0.0260(15) -0.0048(9) -0.0033(11) -0.0063(12)
F11 0.0221(13) 0.0275(13) 0.048(2) -0.0080(10) -0.0049(13) 0.0029(13)
F7 0.0308(14) 0.0278(12) 0.0213(15) 0.0027(10) -0.0024(11) 0.0062(12)
F1 0.0360(15) 0.0194(12) 0.0311(17) 0.0062(10) -0.0033(12) -0.0022(12)
F8 0.0339(15) 0.0317(12) 0.0283(16) -0.0049(11) 0.0051(12) -0.0102(13)
F2 0.0389(16) 0.0416(15) 0.0189(15) -0.0156(12) 0.0049(12) 0.0013(13)
F3 0.0304(14) 0.0282(12) 0.0247(15) -0.0035(10) 0.0094(11) -0.0026(12)
O2 0.0278(15) 0.0178(13) 0.0169(16) -0.0014(11) 0.0022(13) -0.0029(13)
F5 0.0330(14) 0.0241(12) 0.051(2) -0.0011(10) -0.0142(15) 0.0103(14)
F10 0.0333(15) 0.0254(13) 0.046(2) 0.0047(10) 0.0046(13) -0.0071(13)
F9 0.0490(18) 0.0352(15) 0.040(2) -0.0077(13) -0.0171(15) 0.0145(15)
O1 0.0253(15) 0.0161(13) 0.0263(18) 0.0005(11) 0.0040(13) -0.0002(13)
C1 0.0161(18) 0.0158(17) 0.021(2) 0.0045(14) -0.0015(16) -0.0022(18)
C3 0.041(3) 0.027(2) 0.017(2) 0.0022(18) 0.001(2) -0.004(2)
C2 0.0175(19) 0.0186(18) 0.021(2) 0.0007(14) 0.0006(16) -0.0020(18)
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'
H H 0.0000 0.0000 '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'
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
F4 Sb1 F5 . . 96.68(11) ?
F4 Sb1 F2 . . 92.29(12) ?
F5 Sb1 F2 . . 90.73(14) ?
F4 Sb1 F3 . . 95.54(11) ?
F5 Sb1 F3 . . 90.38(13) ?
F2 Sb1 F3 . . 171.91(11) ?
F4 Sb1 F1 . . 93.34(11) ?
F5 Sb1 F1 . . 169.97(12) ?
F2 Sb1 F1 . . 89.34(12) ?
F3 Sb1 F1 . . 88.18(12) ?
F4 Sb1 F6 . . 176.70(11) ?
F5 Sb1 F6 . . 84.91(11) ?
F2 Sb1 F6 . . 84.78(11) ?
F3 Sb1 F6 . . 87.33(11) ?
F1 Sb1 F6 . . 85.11(11) ?
F9 Sb2 F11 . . 95.48(12) ?
F9 Sb2 F8 . . 90.04(14) ?
F11 Sb2 F8 . . 94.12(12) ?
F9 Sb2 F7 . . 168.79(11) ?
F11 Sb2 F7 . . 95.72(12) ?
F8 Sb2 F7 . . 89.00(12) ?
F9 Sb2 F10 . . 89.65(14) ?
F11 Sb2 F10 . . 94.98(12) ?
F8 Sb2 F10 . . 170.88(11) ?
F7 Sb2 F10 . . 89.53(13) ?
F9 Sb2 F6 . . 85.50(11) ?
F11 Sb2 F6 . . 178.88(11) ?
F8 Sb2 F6 . . 85.34(11) ?
F7 Sb2 F6 . . 83.29(11) ?
F10 Sb2 F6 . . 85.55(11) ?
Sb1 F6 Sb2 . . 150.90(15) ?
C1 O2 C3 . . 119.2(3) ?
O1 C1 O2 . . 117.7(4) ?
O1 C1 C2 . . 123.8(4) ?
O2 C1 C2 . . 118.4(4) ?
C2 C2 C1 5_666 . 120.8(5) ?
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
Sb1 F4 . 1.856(2) ?
Sb1 F5 . 1.858(2) ?
Sb1 F2 . 1.859(3) ?
Sb1 F3 . 1.864(3) ?
Sb1 F1 . 1.886(2) ?
Sb1 F6 . 2.026(2) ?
Sb2 F9 . 1.852(3) ?
Sb2 F11 . 1.858(2) ?
Sb2 F8 . 1.863(3) ?
Sb2 F7 . 1.864(3) ?
Sb2 F10 . 1.865(3) ?
Sb2 F6 . 2.060(2) ?
O2 C1 . 1.281(5) ?
O2 C3 . 1.489(6) ?
O1 C1 . 1.277(5) ?
C1 C2 . 1.466(6) ?
C2 C2 5_666 1.334(8) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1 F1 . 0.84 1.81 2.569(4) 148.6 yes
C3 H5 F9 8_765 0.98 2.58 3.427(5) 145.1 yes
C3 H3 F8 . 0.98 2.59 3.437(5) 145.0 yes
C2 H2 F10 4_456 0.92(4) 2.43(4) 3.352(5) 175(3) yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C3 O2 C1 O1 . . . . 3.3(5) ?
C3 O2 C1 C2 . . . . -176.4(4) ?
O1 C1 C2 C2 . . . 5_666 172.3(5) ?
O2 C1 C2 C2 . . . 5_666 -8.1(7) ?