#------------------------------------------------------------------------------
#$Date: 2020-11-25 07:11:19 +0200 (Wed, 25 Nov 2020) $
#$Revision: 259242 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/22/2022279.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_2022279
loop_
_publ_author_name
'Rutherford, Ryan Noboru'
'Ura, Shinji'
'Chan, Tak-Hang'
'Fukumoto, Kozo'
'Nishioka, Takanori'
'Renzetti, Andrea'
_publ_section_title
;
Dibenzoate esters of cis-tetralin-2,3-diol as analogs of
(--)-epigallocatechin gallate: synthesis and crystal structure of
anticancer drug candidates
;
_journal_coeditor_code OP3007
_journal_issue 12
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229620014916
_journal_volume 76
_journal_year 2020
_chemical_formula_iupac 'C24 H14 F6 O4'
_chemical_formula_moiety 'C24 H14 F6 O4'
_chemical_formula_sum 'C24 H14 F6 O4'
_chemical_formula_weight 480.35
_chemical_name_systematic
;
(2R,3S)-1,2,3,4-Tetrahydronaphthalene-2,3-diyl
bis(3,4,5-trifluorobenzoate)
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha 90
_cell_angle_beta 97.204(4)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 30.399(10)
_cell_length_b 9.176(3)
_cell_length_c 14.994(5)
_cell_measurement_reflns_used 4720
_cell_measurement_temperature 193.4
_cell_measurement_theta_max 27.4794
_cell_measurement_theta_min 3.0057
_cell_volume 4149(2)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2008)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2008)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2008)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 193.4
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method dtprofit.ref
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71075
_diffrn_reflns_av_R_equivalents 0.0360
_diffrn_reflns_av_unetI/netI 0.0291
_diffrn_reflns_limit_h_max 39
_diffrn_reflns_limit_h_min -39
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 20773
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.446
_diffrn_reflns_theta_min 3.006
_exptl_absorpt_coefficient_mu 0.140
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.7129
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details DTABSCOR
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.538
_exptl_crystal_description prism
_exptl_crystal_F_000 1952
_exptl_crystal_size_max 0.175
_exptl_crystal_size_mid 0.094
_exptl_crystal_size_min 0.092
_refine_diff_density_max 0.196
_refine_diff_density_min -0.278
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.006
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 307
_refine_ls_number_reflns 4718
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.006
_refine_ls_R_factor_all 0.0572
_refine_ls_R_factor_gt 0.0410
_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^)+(0.0689P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1111
_refine_ls_wR_factor_ref 0.1204
_reflns_number_gt 3317
_reflns_number_total 4718
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file op3007sup1.cif
_cod_data_source_block 6
_cod_original_cell_volume 4150(2)
_cod_database_code 2022279
_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_hkl_file
;
3 1 0 7013.48 17.93
-4 0 -1 0.04 0.36
4 0 1 0.46 0.71
-4 0 -1 -0.04 0.61
4 0 1 0.04 0.41
-4 0 -1 0.15 0.74
3 -1 -1 39.20 1.94
3 -1 -1 39.15 1.56
-3 -1 1 36.92 1.47
3 1 -1 39.16 1.56
3 1 -1 36.35 1.65
-3 -1 1 40.49 1.79
3 -1 -1 39.26 1.69
-3 1 1 38.03 1.60
-3 1 1 40.99 1.83
-3 1 1 35.18 1.47
-2 0 -2 134.32 1.40
2 0 2 142.93 1.72
-2 0 -2 144.97 1.75
-2 0 -2 156.36 2.76
2 0 2 159.77 2.62
3 1 1 1029.92 8.39
3 -1 1 1095.16 8.10
-3 1 -1 1120.44 8.36
3 -1 1 1041.95 8.37
3 1 1 1038.82 8.27
-3 1 -1 1126.16 8.86
-3 -1 -1 1122.42 7.15
1 -1 -2 67.56 2.36
-1 -1 2 59.48 2.28
1 1 -2 63.33 2.50
1 -1 -2 68.27 2.63
-1 -1 2 62.66 2.19
1 1 -2 63.48 2.20
1 -1 -2 61.14 2.17
-1 -1 2 70.32 2.77
1 1 -2 62.23 2.48
1 -1 -2 58.98 2.25
4 0 -2 226.87 3.24
4 0 -2 221.97 2.90
-1 -1 -2 899.18 7.53
1 -1 2 930.74 7.79
-1 -1 -2 896.76 6.00
1 1 2 846.94 7.11
-1 -1 -2 901.20 7.45
-1 1 -2 933.10 6.32
1 -1 2 867.17 7.57
3 -1 -2 0.38 0.99
3 1 -2 0.35 0.52
3 -1 -2 0.18 0.36
-3 -1 2 0.70 0.47
3 -1 -2 0.30 0.70
-3 1 2 0.34 0.53
3 1 -2 0.66 0.86
-3 -1 2 0.00 0.74
3 -1 -2 0.38 0.53
-3 -1 2 0.30 0.55
-3 1 2 0.20 0.46
3 1 -2 0.47 0.64
-5 -1 0 184.39 3.20
5 1 0 200.02 2.80
5 -1 0 185.81 2.83
-5 1 0 190.01 3.16
5 1 0 184.08 3.05
-5 -1 0 192.90 2.67
-5 1 0 173.30 3.06
5 -1 0 184.45 3.03
5 1 0 185.91 2.51
-5 -1 0 200.63 2.60
-5 1 0 187.20 2.96
6 0 0 4391.99 12.90
6 0 0 4513.41 11.39
-6 0 0 4473.69 11.38
-4 0 -2 1358.95 11.58
4 0 2 1334.79 11.05
4 0 2 1396.08 10.21
4 0 2 1402.31 9.87
0 0 3 0.06 0.18
0 0 3 0.70 0.97
0 0 -3 1.01 1.22
0 0 3 0.24 0.44
0 0 -3 0.03 0.20
0 0 -3 0.89 0.95
6 0 -1 0.24 0.57
-6 0 1 0.01 0.27
-6 0 1 0.08 0.61
6 0 -1 0.46 0.71
-6 0 1 0.58 1.27
6 0 -1 0.22 0.25
-2 0 3 0.58 0.83
2 0 -3 0.18 0.54
2 0 -3 0.05 0.15
2 0 -3 0.17 0.54
-2 0 3 0.35 0.52
2 0 -3 0.49 0.54
-3 1 -2 550.89 6.17
3 -1 2 553.24 4.58
-3 -1 -2 569.14 5.96
3 1 2 599.29 5.93
-3 1 -2 545.76 5.66
3 1 2 589.64 6.01
-5 -1 -1 0.85 0.37
5 1 1 0.62 0.28
5 -1 1 0.64 0.51
-5 1 -1 0.54 0.42
-5 1 -1 0.67 0.58
5 -1 1 0.70 0.51
-5 1 -1 0.84 0.60
5 1 1 1.40 0.71
5 1 1 1.09 0.59
-5 -1 -1 0.78 1.18
5 -1 1 0.37 0.40
-6 0 -1 0.13 0.54
6 0 1 0.14 0.83
6 0 1 0.74 0.98
-6 0 -1 1.44 1.83
-6 0 -1 0.20 0.76
6 0 1 -0.12 0.58
-2 0 -3 0.39 1.19
2 0 3 0.10 0.73
-2 0 -3 0.18 0.30
2 0 3 0.26 0.43
-2 0 -3 0.27 0.43
-6 0 2 4381.37 13.54
4 0 -3 -0.05 0.44
-4 0 3 0.25 0.98
4 0 -3 0.04 0.38
-4 0 3 0.39 0.78
-5 -1 2 47.75 2.59
-5 1 2 45.20 2.44
5 -1 -2 48.82 2.53
5 1 -2 49.66 2.24
-5 -1 2 53.43 2.60
5 1 -2 45.86 1.91
-5 1 2 43.64 1.77
-5 -1 2 45.68 1.77
5 -1 -2 47.78 1.87
2 2 0 25.78 1.67
-2 -2 0 23.25 1.38
-2 -2 0 25.56 1.74
-2 2 0 23.91 1.71
2 -2 0 25.56 1.60
2 2 0 24.28 1.54
-2 2 0 24.30 1.61
-1 -1 3 603.56 6.44
1 -1 -3 555.73 5.27
-1 -1 3 583.67 4.43
-1 1 3 559.01 5.91
-1 1 3 587.56 5.39
-1 -1 3 564.41 5.64
1 1 -3 541.34 5.57
1 -1 -3 560.79 5.33
-1 1 3 549.02 5.51
0 -2 -1 5314.53 16.43
0 -2 1 5158.15 15.78
-2 2 1 418.08 5.36
2 2 -1 384.96 4.98
2 -2 -1 408.47 4.67
-2 2 1 384.77 4.28
-2 -2 1 414.31 5.13
-2 -2 1 418.45 5.26
-1 -1 -3 4223.36 28.76
-1 -1 -3 4298.95 12.30
3 1 -3 76.72 3.31
3 -1 -3 77.40 2.78
-3 1 3 88.09 3.13
-3 1 3 75.48 3.19
3 -1 -3 76.20 2.97
-3 -1 3 73.25 2.74
3 -1 -3 75.74 2.91
-3 -1 3 80.89 3.09
3 1 -3 75.55 2.74
-3 1 3 76.02 4.00
2 2 1 242.08 2.94
-2 2 -1 249.77 4.27
-2 2 -1 246.79 3.67
2 -2 1 231.59 3.68
-2 -2 -1 249.75 4.38
-2 -2 -1 261.34 3.21
2 -2 1 250.21 4.59
2 2 1 239.44 4.06
6 0 2 99.35 3.51
-6 0 -2 104.06 3.55
6 0 2 105.94 3.88
-6 0 -2 109.77 4.07
-6 0 -2 119.09 4.52
-4 0 -3 0.13 0.56
4 0 3 -0.18 0.56
4 0 3 -0.01 0.37
-4 0 -3 0.00 0.52
-4 0 -3 1.39 1.81
4 2 0 1182.11 9.22
-4 -2 0 1244.74 11.33
-4 2 0 1247.80 11.84
4 2 0 1218.52 10.71
4 -2 0 1163.27 10.17
0 -2 -2 279.43 4.66
0 2 2 272.80 3.14
0 -2 -2 269.27 3.12
0 -2 2 294.20 4.51
0 -2 2 270.46 3.72
0 2 -2 262.08 4.31
7 1 0 339.85 3.95
-7 1 0 336.20 4.40
-7 -1 0 344.30 3.99
-7 -1 0 348.69 5.02
-7 1 0 367.82 5.27
-7 -1 0 353.99 4.16
7 1 0 340.89 4.07
7 1 -1 58.72 2.35
7 -1 -1 48.33 2.30
-7 -1 1 51.81 2.33
-7 -1 1 52.62 2.60
-7 1 1 52.26 2.71
7 -1 -1 46.27 2.06
-7 1 1 47.64 2.21
-7 -1 1 48.20 1.91
-4 2 1 115.01 4.28
-4 -2 1 110.18 4.41
-4 2 1 123.67 4.96
4 2 -1 120.47 4.37
-4 -2 1 117.59 4.60
4 -2 -1 107.25 3.98
3 -1 3 180.15 3.52
3 1 3 176.80 3.28
-3 1 -3 176.83 3.61
-3 1 -3 182.21 2.20
-3 -1 -3 180.88 3.11
3 1 3 178.55 3.08
3 1 3 175.70 1.76
-2 -2 2 318.48 4.37
2 2 -2 317.97 4.15
-2 -2 2 318.06 4.77
2 -2 -2 312.94 3.82
-2 2 2 307.14 3.74
-2 2 2 313.48 4.53
2 2 -2 340.10 5.59
-2 2 2 339.27 4.87
-6 0 3 0.11 0.38
-6 0 3 0.37 0.97
8 0 0 542.55 5.53
-8 0 0 564.67 6.65
-8 0 0 550.15 5.78
8 0 0 580.22 6.25
-8 0 1 0.47 1.61
8 0 -1 -0.09 0.34
-8 0 1 -0.04 0.53
5 1 -3 26.91 1.35
-5 -1 3 25.82 1.25
-5 1 3 25.59 1.83
-5 -1 3 25.67 1.73
-5 1 3 25.57 1.62
-5 -1 3 26.29 2.12
-5 1 3 24.30 1.16
5 -1 -3 24.23 1.13
5 1 -3 25.18 1.58
2 -2 2 39.94 1.82
2 2 2 39.33 2.11
2 2 2 42.83 1.60
-2 2 -2 40.36 3.38
-2 -2 -2 45.06 1.82
2 -2 2 44.31 3.14
-2 -2 -2 41.98 2.37
-2 2 -2 41.60 1.91
-7 -1 -1 3448.91 13.68
-7 1 -1 3537.82 13.48
7 1 1 3445.05 9.31
-7 1 -1 3506.64 12.65
7 1 -2 1945.32 6.30
-4 -2 2 1767.23 9.87
-4 2 2 1781.42 11.20
-4 -2 2 1675.03 8.90
-8 0 -1 0.76 1.08
8 0 1 0.63 0.98
-8 0 -1 1.50 1.73
-8 0 2 0.12 0.28
-8 0 2 -0.12 1.02
-8 0 2 0.11 0.49
-2 0 -4 1.40 0.41
2 0 4 2.23 0.72
-2 0 -4 1.61 0.62
-2 0 -4 2.08 1.22
2 0 4 2.56 0.65
1 -1 -4 230.66 3.54
-1 -1 4 253.69 2.27
-1 1 4 246.22 3.96
1 1 -4 268.51 4.04
-1 1 4 262.23 3.62
1 -1 -4 251.11 3.26
-1 1 4 266.10 3.54
1 1 -4 254.49 2.33
6 2 0 8064.45 16.72
-3 1 4 1327.12 10.91
3 1 -4 1348.89 10.56
-3 1 4 1264.66 11.64
3 1 -4 1325.90 9.79
-3 -1 4 1394.70 10.06
3 -1 -4 1342.90 10.70
-3 -1 4 1388.31 10.95
-3 1 4 1303.61 11.27
1 1 4 0.64 0.60
1 1 4 1.17 0.60
-1 -1 -4 0.68 0.41
1 -1 4 1.30 1.04
-1 -1 -4 3.64 0.48
-1 -1 -4 0.83 0.53
-1 1 -4 0.65 0.61
4 -2 2 9998.67 20.33
-4 2 -2 9999.00 25.14
0 2 3 0.63 0.31
0 2 3 0.64 0.51
0 -2 -3 0.67 0.63
0 -2 3 1.14 0.67
0 -2 3 0.75 0.41
0 2 -3 0.95 1.14
0 -2 -3 0.97 0.41
0 -2 3 0.84 0.86
6 -2 -1 481.44 6.14
-6 -2 1 501.45 6.15
-6 2 1 478.16 6.39
-6 2 1 492.34 6.19
6 2 -1 460.15 5.35
-5 -1 -3 952.47 6.34
5 1 3 957.28 10.40
-5 1 -3 985.21 10.21
-5 1 -3 1015.51 8.05
5 -1 3 960.98 7.80
-5 -1 -3 947.98 8.71
5 1 3 979.99 6.59
-2 -2 3 90.36 3.37
-2 2 3 98.76 3.96
2 -2 -3 98.85 3.56
2 2 -3 96.80 3.76
-2 2 3 101.15 3.84
-2 -2 3 105.95 4.24
2 2 -3 102.34 3.70
-2 2 3 91.60 3.32
6 0 3 0.19 0.55
-6 0 -3 -0.01 0.69
-6 0 -3 -0.06 1.00
-6 0 -3 0.21 0.44
6 0 3 0.24 0.47
-7 -1 -2 1113.24 10.57
-7 1 -2 1131.35 9.70
7 1 2 1208.27 10.93
7 1 2 1177.35 8.39
7 1 2 1144.86 8.23
-7 -1 3 344.32 5.24
-7 -1 3 311.75 4.59
-7 1 3 333.62 5.12
7 -1 -3 315.87 3.29
7 1 -3 353.25 3.38
-7 1 3 346.54 3.77
7 -1 -3 324.83 4.96
6 2 1 8742.22 35.73
6 2 1 8863.61 14.67
-2 2 -3 49.40 2.00
-2 2 -3 52.61 2.84
2 -2 3 49.07 2.00
-2 -2 -3 50.58 2.58
2 -2 3 48.66 2.66
2 2 3 49.37 2.54
-2 -2 -3 49.26 1.76
-8 0 -2 22.32 1.70
8 0 2 23.75 1.38
-8 0 -2 24.39 1.77
-8 0 -2 23.66 1.26
-8 0 3 0.12 0.63
-8 0 3 -0.12 1.03
-6 -2 2 64.72 3.37
-6 -2 2 55.04 2.64
-6 2 2 54.94 2.77
-6 2 2 62.72 2.69
6 2 -2 67.85 2.88
6 -2 -2 67.41 3.08
-4 0 -4 122.44 4.88
4 0 4 119.24 4.20
4 0 4 118.83 4.05
-4 0 -4 109.07 4.06
-4 0 -4 117.26 4.01
-4 2 3 368.18 4.84
4 2 -3 354.58 4.80
-4 -2 3 335.78 5.42
4 -2 -3 362.88 4.78
-9 -1 1 343.44 5.31
9 1 -1 347.00 4.26
-9 -1 1 337.62 4.32
-9 1 1 327.81 4.27
9 -1 -1 320.01 4.11
-9 1 1 342.43 5.37
-9 -1 1 341.04 4.70
9 -1 -1 345.94 5.20
-5 -1 4 2524.35 8.36
-5 1 4 2590.01 12.02
-5 -1 4 2617.68 10.09
3 -1 4 55.66 2.78
-3 -1 -4 51.53 1.89
3 1 4 55.95 2.08
-3 -1 -4 58.34 2.54
-3 1 -4 56.34 1.93
-3 1 -4 57.65 3.29
9 1 0 2078.44 9.35
-9 -1 0 2097.91 11.72
-1 -3 0 1908.73 10.60
-10 0 1 -0.26 0.56
-10 0 1 0.56 1.07
10 0 -1 -0.03 0.86
9 -1 -2 127.14 4.31
-9 -1 2 127.94 4.82
-9 1 2 124.91 4.95
-9 1 2 131.83 4.50
-9 -1 2 132.03 4.37
9 1 -2 126.02 4.25
9 -1 -2 117.23 4.55
-10 0 0 508.63 6.84
10 0 0 481.77 5.83
-9 1 -1 0.32 1.08
9 1 1 0.74 0.36
9 1 1 1.04 0.71
9 1 1 0.54 0.44
-9 1 -1 0.80 1.16
-9 -1 -1 0.08 1.13
9 -1 1 0.60 0.63
-2 0 5 0.33 0.83
2 0 -5 0.00 0.33
-2 0 5 0.10 0.32
2 0 -5 -0.27 0.71
-6 -2 -2 1805.25 11.48
6 2 2 1804.47 11.58
-6 2 -2 1751.21 11.35
-6 -2 -2 1772.80 4.90
-1 3 1 329.38 5.30
1 3 -1 318.80 5.41
-1 -3 1 342.05 5.85
1 -3 -1 352.62 6.49
-1 -3 1 312.18 4.86
1 -3 -1 356.26 5.04
-4 2 -3 2310.54 16.15
0 0 5 0.30 0.67
0 0 -5 0.10 0.19
0 0 -5 0.32 0.36
3 3 0 10.17 1.22
-3 3 0 9.63 1.42
-3 3 0 9.22 1.76
-3 -3 0 11.23 2.45
3 -3 0 9.98 1.34
-10 0 2 1023.79 7.88
-10 0 2 962.41 7.27
-10 0 2 1001.54 10.53
-10 0 2 948.41 9.84
-6 2 3 100.30 3.79
6 2 -3 101.18 3.84
-6 -2 3 98.37 3.91
-6 -2 3 93.77 4.05
6 -2 -3 103.03 4.20
8 2 0 1665.49 9.50
8 -2 0 1684.39 10.58
-8 2 1 260.59 4.49
8 -2 -1 259.18 4.77
-8 -2 1 265.42 4.16
8 2 -1 250.12 4.07
-8 2 1 260.63 5.20
7 1 3 7.36 3.67
-7 1 -3 5.11 1.01
-7 1 -3 5.29 1.00
-7 -1 -3 4.77 0.97
7 -1 3 5.54 0.89
-7 -1 -3 5.18 1.01
4 0 -5 -0.04 0.37
-4 0 5 -0.47 0.97
4 0 -5 0.24 0.63
-4 0 5 0.00 0.65
4 0 -5 -0.19 0.52
-3 3 1 84.52 3.73
3 3 -1 89.14 4.25
-3 -3 1 90.81 3.93
-3 -3 1 92.34 3.78
3 -3 -1 91.93 3.91
-2 2 4 1974.47 10.77
2 2 -4 1930.77 11.78
2 2 -4 1999.97 8.24
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-20 0 5 -0.07 0.90
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8 6 0 337.77 14.27
8 -6 0 318.89 12.78
3 -3 9 47.43 4.98
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0 -2 -10 20.91 5.08
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5 -5 -7 39.00 3.42
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2 0 -11 -0.01 0.35
2 0 -11 0.19 0.42
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18 -4 -2 2.61 0.96
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-20 -2 5 31.05 3.75
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-20 -2 5 25.49 2.08
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-13 -5 -3 -0.83 1.08
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-15 -5 2 0.41 0.95
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-15 5 2 0.45 0.47
-15 -5 2 0.14 1.21
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-6 -4 -8 59.07 4.93
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-18 4 0 305.80 13.13
-18 -4 0 287.60 12.57
18 -4 0 279.58 14.11
18 4 0 277.18 14.31
-18 -4 0 275.72 12.30
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-2 -10 -10 1.24 2.22
2 10 10 0.62 0.77
-13 -11 -2 0.83 1.82
13 11 2 0.16 1.82
13 -11 2 1.84 2.53
13 -11 2 1.01 2.69
-13 11 -2 0.65 1.69
-9 1 -18 3.00 3.09
-9 -1 -18 4.26 3.89
1 11 -7 2.40 2.15
-1 11 7 4.15 2.42
-1 -11 7 3.81 4.83
1 -11 -7 5.86 3.39
34 -4 -9 3.79 3.31
-34 4 9 0.72 1.85
-34 -4 9 0.27 1.46
-34 -4 9 1.61 2.07
34 2 -11 7.78 3.46
34 -2 -11 6.53 2.96
-34 -2 11 7.04 3.12
-34 2 11 4.32 4.68
18 -10 4 0.78 1.51
18 -10 4 0.22 2.18
18 10 4 0.67 1.48
-18 10 -4 1.05 1.35
-18 -10 -4 1.87 2.73
-30 2 -10 18.61 6.37
-30 -2 -10 18.78 4.76
-3 -11 7 1.15 2.18
3 11 -7 -0.01 1.91
-3 11 7 0.17 1.54
3 -11 -7 1.11 2.45
-28 -8 5 5.12 3.20
28 -8 -5 3.08 4.58
-28 8 5 3.33 2.90
-36 4 6 15.27 4.51
36 4 -6 15.75 3.80
-36 -4 6 16.43 4.23
36 -4 -6 14.67 7.22
-32 0 13 1.32 2.57
32 0 -13 0.40 2.17
-2 0 -19 0.16 1.44
36 2 -9 -0.04 1.58
36 -2 -9 2.24 2.27
-36 -2 9 0.73 1.48
-36 2 9 0.96 2.38
-39 1 2 0.61 1.55
-39 -1 2 0.51 0.98
39 -1 -2 0.06 1.46
39 1 -2 0.21 1.23
9 11 -6 2.36 2.27
-9 11 6 4.16 3.12
-9 -11 6 1.84 2.06
9 -11 -6 1.50 1.67
-9 -11 6 2.19 2.20
-35 -5 5 1.07 2.45
35 5 -5 0.71 1.22
-35 5 5 0.06 1.27
35 -5 -5 1.74 3.04
-23 -1 -14 1.99 1.85
-23 1 -14 1.61 2.42
-39 1 3 1.00 1.76
-39 -1 3 0.68 1.92
39 -1 -3 2.71 2.57
39 1 -3 0.70 1.31
-11 -1 19 0.73 1.02
-11 1 19 0.81 1.47
-23 -7 12 -0.02 1.39
23 -7 -12 1.68 2.13
-23 7 12 0.92 1.06
38 0 -7 0.59 2.38
-38 0 7 0.84 2.19
-31 7 -1 2.00 2.36
-31 7 -1 -0.03 1.54
-31 -7 -1 0.79 1.74
31 -7 1 0.26 1.60
28 -4 10 2.24 1.72
-28 -4 -10 2.30 2.05
-28 -4 -10 1.58 1.76
-28 4 -10 2.76 3.43
38 -2 1 11.86 11.51
-38 -2 -1 11.91 8.04
-38 2 -1 21.76 5.22
-29 -1 -11 0.58 1.85
-29 1 -11 1.30 1.41
-2 -2 19 -0.42 1.18
-25 -7 11 2.52 2.97
-25 7 11 0.90 1.76
25 -7 -11 2.46 2.02
-12 0 19 0.49 1.16
32 -4 7 0.20 1.25
-32 -4 -7 0.91 1.64
-32 -4 -7 1.67 1.73
-32 4 -7 1.61 1.81
-8 -2 -18 0.42 1.57
-8 2 -18 0.13 1.45
1 11 7 5.68 2.61
-1 11 -7 5.47 2.79
-1 -11 -7 6.56 3.48
1 -11 7 5.41 4.99
-10 -4 18 1.37 2.44
-15 -9 11 0.63 1.54
15 -9 -11 1.52 1.43
28 -6 -11 1.27 2.39
-28 -6 11 0.97 1.46
-28 6 11 -0.48 1.54
-28 -6 11 0.46 1.11
-9 -11 -5 0.78 2.15
9 11 5 0.75 1.74
9 -11 5 1.78 1.87
-9 11 -5 -0.15 1.08
-8 -2 19 1.93 1.81
8 -10 9 2.85 2.91
-8 10 -9 3.91 2.71
8 10 9 3.09 3.18
-8 -10 -9 2.74 3.24
17 -7 12 1.31 2.28
-17 7 -12 -0.19 2.01
-17 -7 -12 0.15 1.90
-17 -7 -12 0.99 0.95
-35 3 -5 4.74 2.78
-35 -3 -5 9.05 3.26
35 -3 5 5.19 6.21
-35 -3 -5 4.38 6.30
-31 7 5 0.31 1.20
31 -7 -5 0.78 2.25
-31 -7 5 0.51 1.91
-13 -5 17 6.09 3.05
-8 -10 10 0.50 1.70
-8 10 10 0.27 1.02
8 -10 -10 0.48 2.22
8 10 -10 0.80 1.42
-25 -9 4 3.03 2.85
25 -9 -4 4.22 3.03
-25 9 4 2.68 3.28
-25 9 4 2.19 1.99
-32 4 11 4.24 3.15
-32 -4 11 5.39 2.92
-32 -4 11 4.56 4.35
-2 -8 -14 0.44 1.45
2 8 14 0.57 1.04
-2 8 -14 0.83 1.71
2 -8 14 0.82 1.91
-27 -5 13 -0.04 0.91
27 -5 -13 0.52 1.59
-27 5 13 0.39 0.83
-29 -7 8 3.94 5.61
29 -7 -8 11.22 4.35
-29 -7 8 10.16 4.04
-29 7 8 6.46 4.93
13 11 -4 1.86 2.63
-13 11 4 2.74 3.55
13 -11 -4 2.38 2.15
13 -11 -4 2.59 3.32
-13 -11 4 3.26 2.39
-5 -11 7 1.52 2.25
-5 11 7 0.46 1.61
5 -11 -7 3.14 3.85
5 11 -7 3.49 3.28
-20 -8 -9 0.05 1.34
20 8 9 -0.06 1.40
-20 8 -9 1.12 1.36
20 -8 9 1.39 2.31
-39 -1 1 0.32 1.52
-39 1 1 0.09 1.55
39 1 -1 -0.02 1.12
39 -1 -1 1.82 2.49
-11 -11 -4 5.95 4.30
11 11 4 3.87 2.99
-11 11 -4 3.40 4.21
11 -11 4 3.46 2.67
11 -11 4 2.85 2.69
-23 -9 -4 2.33 2.15
23 -9 4 4.35 4.82
-23 9 -4 2.88 2.60
23 9 4 2.63 2.24
-15 -3 18 1.60 1.79
-26 0 16 1.06 1.96
26 -6 9 3.13 2.70
-26 -6 -9 1.57 2.67
-26 -6 -9 -0.01 1.72
-26 6 -9 1.50 1.35
-25 -9 -1 18.54 11.92
-25 9 -1 21.32 4.38
25 -9 1 25.46 5.50
-25 9 -1 21.79 8.46
-35 5 -1 -0.02 1.57
-35 -5 -1 0.60 1.77
35 -5 1 0.60 1.88
-20 10 -2 15.18 3.92
-20 -10 -2 11.68 6.83
20 -10 2 15.82 8.63
20 10 2 10.63 8.15
-5 7 -15 3.01 5.20
5 7 15 4.10 3.67
5 -7 15 3.34 2.40
-18 8 -10 1.35 2.11
18 -8 10 1.26 2.95
-18 -8 -10 2.61 2.20
18 8 10 1.82 2.19
-34 -4 -5 1.69 2.86
-34 -4 -5 0.55 0.82
34 -4 5 0.50 2.55
-34 4 -5 0.73 1.55
-39 1 4 3.15 2.41
-39 -1 4 3.56 3.39
39 -1 -4 1.86 2.18
39 1 -4 2.24 2.36
-25 7 -8 0.69 1.88
-25 -7 -8 1.24 2.43
-25 -7 -8 1.02 1.62
25 -7 8 0.81 2.02
-38 2 6 2.36 2.58
-38 -2 6 0.48 2.19
38 -2 -6 1.20 1.79
38 2 -6 0.32 1.44
-28 -8 -2 31.40 6.33
28 8 2 26.98 8.75
28 -8 2 33.35 6.50
-28 8 -2 30.61 6.31
37 -3 2 4.60 6.07
-37 -3 -2 10.14 3.97
-20 2 -15 2.54 2.98
-20 -2 -15 1.51 2.15
-11 -9 12 1.31 2.34
11 -9 -12 0.61 1.62
-11 9 12 1.12 1.60
-37 -1 -4 1.32 1.39
-37 1 -4 1.48 1.34
-37 -1 -4 1.96 2.23
-37 1 -4 0.50 0.97
-20 4 -14 42.97 8.18
-20 -4 -14 49.97 8.26
13 9 10 6.92 3.26
-13 -9 -10 4.18 2.23
13 -9 10 7.01 4.14
-34 -2 -7 0.18 1.24
-34 2 -7 0.82 1.32
-34 -2 -7 1.38 1.56
-22 6 14 1.41 2.00
-22 -6 14 0.62 1.49
22 -6 -14 1.57 2.18
-36 -4 -2 7.85 2.97
36 -4 2 9.37 3.73
5 -9 12 3.68 3.38
-5 -9 -12 3.03 2.29
-5 9 -12 1.94 2.63
5 9 12 2.58 4.09
-18 0 -16 4.66 2.91
-25 5 14 0.43 0.94
-25 -5 14 0.96 1.14
25 -5 -14 0.47 1.58
14 -6 -16 2.31 2.66
-14 -6 16 5.02 2.76
-10 0 -18 3.72 2.66
-23 -9 7 2.03 2.08
-23 -9 7 1.93 2.38
-23 9 7 3.60 3.22
-36 0 10 0.67 2.00
36 0 -10 0.90 2.80
-13 -7 15 10.22 4.28
13 -7 -15 7.39 4.01
-26 8 8 2.03 2.47
-26 -8 8 1.65 1.57
-26 -8 8 2.50 2.69
22 -2 -17 -0.03 1.58
-22 -2 17 1.61 2.53
7 -11 6 10.56 3.70
7 11 6 6.99 5.66
-7 11 -6 8.48 5.17
-7 -11 -6 6.27 3.61
10 -8 -14 4.75 7.08
-10 -8 14 6.68 9.14
-6 6 -16 4.80 4.74
-6 -6 -16 3.74 4.57
6 -6 16 6.67 3.96
29 -5 -12 1.44 2.49
-29 -5 12 1.32 1.47
-29 5 12 1.41 1.55
-29 -5 12 0.93 1.84
-21 -7 13 2.16 2.37
-21 7 13 2.06 1.57
5 -5 17 5.34 3.04
-5 -5 -17 8.66 4.17
-5 5 -17 6.07 4.10
-18 6 -13 2.26 2.54
-18 -6 -13 2.90 3.72
18 -6 13 1.46 1.65
-34 6 2 2.78 3.32
-34 -6 2 1.74 2.25
-2 -4 -18 0.85 1.49
0 -2 19 5.49 2.19
14 10 7 0.97 1.57
-14 -10 -7 0.03 1.80
14 -10 7 0.66 1.74
4 -10 10 0.99 2.74
4 10 10 1.88 2.08
-4 -10 -10 1.75 2.29
22 8 8 4.81 5.50
22 -8 8 4.77 3.16
-22 -8 -8 4.29 2.27
-19 -3 -15 9.87 3.84
-19 3 -15 5.29 8.18
21 -9 6 23.48 5.43
-21 -9 -6 18.90 5.13
21 9 6 15.18 12.30
3 11 7 1.65 1.79
-3 -11 -7 3.95 3.45
-3 11 -7 1.50 2.03
3 -11 7 4.47 3.36
-30 -6 -6 2.12 2.44
30 -6 6 4.47 3.39
-30 -6 -6 3.37 2.54
-30 6 -6 4.66 3.05
-15 -11 1 0.48 1.77
-15 11 1 0.43 1.86
15 11 -1 0.28 1.56
-19 5 16 2.00 2.21
-19 -5 16 1.90 2.62
-23 -1 17 4.39 3.38
-18 -4 17 0.52 1.58
18 -4 -17 0.77 1.75
-34 -6 3 3.08 2.72
-34 6 3 2.13 2.88
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT2018 (Sheldrick, 2015a)'
;
_shelx_hkl_checksum 13495
_shelx_res_file
;
TITL shelx_trans_a.res in C2/c
shelx_trans.res
created by SHELXL-2018/3 at 15:27:06 on 20-Oct-2020
REM Old TITL AR-51A
REM SHELXT solution in C2/c: R1 0.259, Rweak 0.306, Alpha 0.041
REM 0.483 for 268 systematic absences, Orientation as input
REM Formula found by SHELXT: C25 F1 O5
CELL 0.71075 30.3993 9.1762 14.9943 90 97.204 90
ZERR 8 0.0103 0.003 0.0049 0 0.004 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H F O
UNIT 192 112 48 32
L.S. 30
PLAN 5
TEMP -79.75
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM
REM
REM
WGHT 0.068900
FVAR 0.32840
O1 4 -0.421501 -0.244012 -0.298596 11.00000 0.04067 0.03720 =
0.05590 -0.00272 -0.00662 -0.00025
F5 3 -0.290142 -0.266962 -0.757968 11.00000 0.08930 0.07644 =
0.04998 -0.00393 -0.00087 0.01047
O3 4 -0.347759 -0.146829 -0.378572 11.00000 0.04449 0.05642 =
0.05126 -0.00668 -0.00038 -0.00977
O4 4 -0.282295 -0.028979 -0.361967 11.00000 0.04625 0.06857 =
0.06233 -0.01229 -0.00487 -0.01253
F4 3 -0.234414 -0.070777 -0.670275 11.00000 0.07964 0.09592 =
0.07303 -0.00081 0.02247 -0.01770
F6 3 -0.356909 -0.379076 -0.678858 11.00000 0.09324 0.09449 =
0.07306 -0.02870 -0.00509 -0.03329
O2 4 -0.484164 -0.140701 -0.364805 11.00000 0.05581 0.04654 =
0.12625 0.00051 -0.02821 0.00730
F1 3 -0.578258 -0.570512 -0.467554 11.00000 0.08664 0.14460 =
0.08366 -0.01499 0.00020 -0.07052
F3 3 -0.450070 -0.774370 -0.312621 11.00000 0.15481 0.04236 =
0.12436 0.01359 0.03573 0.00341
F2 3 -0.531101 -0.806125 -0.407464 11.00000 0.17726 0.07442 =
0.11911 -0.02332 0.04608 -0.07410
C19 1 -0.307128 -0.141806 -0.501933 11.00000 0.03969 0.04215 =
0.05148 -0.00043 -0.00710 0.00351
C18 1 -0.310379 -0.098022 -0.407605 11.00000 0.04012 0.04506 =
0.05535 -0.00134 -0.00317 -0.00080
C12 1 -0.479529 -0.398684 -0.356245 11.00000 0.04855 0.04546 =
0.03764 -0.00294 0.00607 -0.00677
C24 1 -0.335822 -0.242598 -0.546983 11.00000 0.04606 0.05479 =
0.06035 -0.00282 -0.00370 -0.00699
AFIX 43
H24 2 -0.359297 -0.283633 -0.518978 11.00000 -1.20000
AFIX 0
C5 1 -0.381708 -0.140367 -0.112680 11.00000 0.04983 0.04916 =
0.05548 -0.01399 -0.00090 -0.00473
C11 1 -0.462750 -0.247142 -0.341075 11.00000 0.04018 0.04336 =
0.05226 -0.00299 -0.00323 0.00182
C3 1 -0.331773 -0.231098 -0.224332 11.00000 0.04203 0.06732 =
0.05616 -0.00630 -0.00230 0.00745
AFIX 23
H3A 2 -0.340438 -0.327858 -0.249968 11.00000 -1.20000
H3B 2 -0.299146 -0.222529 -0.221040 11.00000 -1.20000
AFIX 0
C20 1 -0.272977 -0.082397 -0.543660 11.00000 0.04453 0.04660 =
0.05700 -0.00024 -0.00329 -0.00086
AFIX 43
H20 2 -0.253370 -0.013052 -0.513025 11.00000 -1.20000
AFIX 0
C2 1 -0.353276 -0.113846 -0.285857 11.00000 0.04404 0.05234 =
0.05156 -0.00941 -0.00067 -0.00625
AFIX 13
H2 2 -0.338585 -0.018539 -0.268980 11.00000 -1.20000
AFIX 0
C4 1 -0.344862 -0.221029 -0.130562 11.00000 0.04839 0.05748 =
0.05183 -0.01090 -0.00460 -0.00012
C6 1 -0.409109 -0.054032 -0.185507 11.00000 0.04660 0.04452 =
0.06760 -0.01326 0.00226 0.00017
AFIX 23
H6A 2 -0.401557 0.050513 -0.177655 11.00000 -1.20000
H6B 2 -0.440867 -0.065419 -0.178400 11.00000 -1.20000
AFIX 0
C23 1 -0.329597 -0.281810 -0.632848 11.00000 0.05632 0.05308 =
0.05551 -0.00822 -0.01125 -0.00343
C13 1 -0.521829 -0.414644 -0.403171 11.00000 0.05188 0.06559 =
0.04386 -0.00153 0.00352 -0.01451
AFIX 43
H13 2 -0.538970 -0.331635 -0.423176 11.00000 -1.20000
AFIX 0
C22 1 -0.295749 -0.224998 -0.674708 11.00000 0.05941 0.05277 =
0.04543 0.00045 -0.00576 0.01318
C1 1 -0.402154 -0.099924 -0.279586 11.00000 0.04378 0.03744 =
0.05903 -0.00417 -0.00264 -0.00222
AFIX 13
H1 2 -0.415907 -0.027404 -0.324470 11.00000 -1.20000
AFIX 0
C17 1 -0.454769 -0.519074 -0.325898 11.00000 0.06375 0.04312 =
0.04950 -0.00020 0.01251 -0.00255
AFIX 43
H17 2 -0.425934 -0.508165 -0.293956 11.00000 -1.20000
AFIX 0
C10 1 -0.392519 -0.137884 -0.024922 11.00000 0.06568 0.06518 =
0.06050 -0.02098 0.00805 -0.00417
AFIX 43
H10 2 -0.417454 -0.083226 -0.011767 11.00000 -1.20000
AFIX 0
C21 1 -0.267810 -0.124588 -0.629264 11.00000 0.04891 0.05374 =
0.05708 0.00678 0.00184 0.00363
C14 1 -0.538105 -0.551648 -0.419778 11.00000 0.07018 0.08760 =
0.04980 -0.00932 0.01177 -0.04111
C7 1 -0.320212 -0.295904 -0.061090 11.00000 0.06854 0.07905 =
0.05733 -0.00894 -0.00858 0.01620
AFIX 43
H7 2 -0.295142 -0.350722 -0.073316 11.00000 -1.20000
AFIX 0
C9 1 -0.367604 -0.213400 0.042775 11.00000 0.09864 0.07688 =
0.05088 -0.01486 0.00730 -0.00698
AFIX 43
H9 2 -0.375514 -0.210948 0.102072 11.00000 -1.20000
AFIX 0
C16 1 -0.472854 -0.655022 -0.343026 11.00000 0.10364 0.04090 =
0.06504 0.00382 0.02932 -0.00604
C15 1 -0.514324 -0.672638 -0.389974 11.00000 0.11030 0.05878 =
0.06319 -0.01323 0.03075 -0.04383
C8 1 -0.331189 -0.292651 0.024885 11.00000 0.09737 0.08456 =
0.05195 -0.00636 -0.00775 0.01370
AFIX 43
H8 2 -0.313866 -0.344500 0.071637 11.00000 -1.20000
AFIX 0
HKLF 4
REM shelx_trans_a.res in C2/c
REM wR2 = 0.1204, GooF = S = 1.006, Restrained GooF = 1.006 for all data
REM R1 = 0.0410 for 3317 Fo > 4sig(Fo) and 0.0572 for all 4718 data
REM 307 parameters refined using 0 restraints
END
WGHT 0.0689 0.0000
REM Highest difference peak 0.196, deepest hole -0.278, 1-sigma level 0.034
Q1 1 -0.2792 -0.1963 -0.6376 11.00000 0.05 0.16
Q2 1 -0.5187 -0.6270 -0.4087 11.00000 0.05 0.15
Q3 1 -0.3006 -0.1742 -0.5005 11.00000 0.05 0.14
Q4 1 -0.4813 -0.3666 -0.3440 11.00000 0.05 0.14
Q5 1 -0.4947 -0.4070 -0.3591 11.00000 0.05 0.14
;
_shelx_res_checksum 55265
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_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
O O1 -0.42150(3) -0.24401(9) -0.29860(6) 0.0457(2) Uani d 1 . .
F F5 -0.29014(3) -0.26696(10) -0.75797(6) 0.0727(3) Uani d 1 . .
O O3 -0.34776(3) -0.14683(10) -0.37857(6) 0.0513(2) Uani d 1 . .
O O4 -0.28229(3) -0.02898(12) -0.36197(7) 0.0600(3) Uani d 1 . .
F F4 -0.23441(3) -0.07078(12) -0.67027(6) 0.0818(3) Uani d 1 . .
F F6 -0.35691(3) -0.37908(12) -0.67886(6) 0.0882(3) Uani d 1 . .
O O2 -0.48416(3) -0.14070(12) -0.36481(9) 0.0796(4) Uani d 1 . .
F F1 -0.57826(4) -0.57051(14) -0.46755(7) 0.1059(4) Uani d 1 . .
F F3 -0.45007(4) -0.77437(11) -0.31262(8) 0.1056(4) Uani d 1 . .
F F2 -0.53110(5) -0.80613(12) -0.40746(8) 0.1213(5) Uani d 1 . .
C C19 -0.30713(4) -0.14181(14) -0.50193(9) 0.0455(3) Uani d 1 . .
C C18 -0.31038(4) -0.09802(15) -0.40761(9) 0.0476(3) Uani d 1 . .
C C12 -0.47953(4) -0.39868(14) -0.35625(8) 0.0438(3) Uani d 1 . .
C C24 -0.33582(5) -0.24260(15) -0.54698(10) 0.0546(4) Uani d 1 . .
H H24 -0.359297 -0.283633 -0.518978 0.066 Uiso calc 1 . .
C C5 -0.38171(4) -0.14037(15) -0.11268(9) 0.0521(3) Uani d 1 . .
C C11 -0.46275(4) -0.24714(14) -0.34107(9) 0.0460(3) Uani d 1 . .
C C3 -0.33177(4) -0.23110(17) -0.22433(9) 0.0559(4) Uani d 1 . .
H H3A -0.340438 -0.327858 -0.249968 0.067 Uiso calc 1 . .
H H3B -0.299146 -0.222529 -0.221040 0.067 Uiso calc 1 . .
C C20 -0.27298(4) -0.08240(15) -0.54366(9) 0.0502(3) Uani d 1 . .
H H20 -0.253370 -0.013052 -0.513025 0.060 Uiso calc 1 . .
C C2 -0.35328(4) -0.11385(15) -0.28586(9) 0.0499(3) Uani d 1 . .
H H2 -0.338585 -0.018539 -0.268980 0.060 Uiso calc 1 . .
C C4 -0.34486(4) -0.22103(16) -0.13056(9) 0.0535(4) Uani d 1 . .
C C6 -0.40911(4) -0.05403(15) -0.18551(10) 0.0533(4) Uani d 1 . .
H H6A -0.401557 0.050513 -0.177655 0.064 Uiso calc 1 . .
H H6B -0.440867 -0.065419 -0.178400 0.064 Uiso calc 1 . .
C C23 -0.32960(5) -0.28181(16) -0.63285(10) 0.0565(4) Uani d 1 . .
C C13 -0.52183(4) -0.41464(17) -0.40317(8) 0.0540(4) Uani d 1 . .
H H13 -0.538970 -0.331635 -0.423176 0.065 Uiso calc 1 . .
C C22 -0.29575(5) -0.22500(15) -0.67471(9) 0.0536(4) Uani d 1 . .
C C1 -0.40215(4) -0.09992(14) -0.27959(9) 0.0475(3) Uani d 1 . .
H H1 -0.415907 -0.027404 -0.324470 0.057 Uiso calc 1 . .
C C17 -0.45477(5) -0.51907(15) -0.32590(9) 0.0517(3) Uani d 1 . .
H H17 -0.425934 -0.508165 -0.293956 0.062 Uiso calc 1 . .
C C10 -0.39252(5) -0.13788(18) -0.02492(10) 0.0638(4) Uani d 1 . .
H H10 -0.417454 -0.083226 -0.011767 0.077 Uiso calc 1 . .
C C21 -0.26781(4) -0.12459(16) -0.62926(10) 0.0537(4) Uani d 1 . .
C C14 -0.53810(6) -0.5516(2) -0.41978(10) 0.0688(5) Uani d 1 . .
C C7 -0.32021(6) -0.29590(19) -0.06109(11) 0.0697(5) Uani d 1 . .
H H7 -0.295142 -0.350722 -0.073316 0.084 Uiso calc 1 . .
C C9 -0.36760(7) -0.21340(19) 0.04277(11) 0.0756(5) Uani d 1 . .
H H9 -0.375514 -0.210948 0.102072 0.091 Uiso calc 1 . .
C C16 -0.47285(7) -0.65502(16) -0.34303(11) 0.0683(5) Uani d 1 . .
C C15 -0.51432(7) -0.67264(19) -0.38997(11) 0.0757(5) Uani d 1 . .
C C8 -0.33119(7) -0.2927(2) 0.02488(12) 0.0794(5) Uani d 1 . .
H H8 -0.313866 -0.344500 0.071637 0.095 Uiso calc 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
O1 0.0407(5) 0.0372(5) 0.0559(6) -0.0003(4) -0.0066(4) -0.0027(4)
F5 0.0893(7) 0.0764(6) 0.0500(5) 0.0105(5) -0.0009(5) -0.0039(4)
O3 0.0445(5) 0.0564(6) 0.0513(6) -0.0098(4) -0.0004(4) -0.0067(4)
O4 0.0462(5) 0.0686(7) 0.0623(6) -0.0125(5) -0.0049(5) -0.0123(5)
F4 0.0796(7) 0.0959(8) 0.0730(6) -0.0177(5) 0.0225(5) -0.0008(5)
F6 0.0932(7) 0.0945(7) 0.0731(6) -0.0333(6) -0.0051(5) -0.0287(5)
O2 0.0558(6) 0.0465(6) 0.1262(10) 0.0073(5) -0.0282(6) 0.0005(6)
F1 0.0866(7) 0.1446(11) 0.0837(7) -0.0705(7) 0.0002(6) -0.0150(7)
F3 0.1548(11) 0.0424(5) 0.1244(9) 0.0034(6) 0.0357(8) 0.0136(5)
F2 0.1773(13) 0.0744(7) 0.1191(9) -0.0741(8) 0.0461(9) -0.0233(7)
C19 0.0397(7) 0.0421(7) 0.0515(8) 0.0035(5) -0.0071(6) -0.0004(6)
C18 0.0401(7) 0.0451(7) 0.0554(8) -0.0008(6) -0.0032(6) -0.0013(6)
C12 0.0486(7) 0.0455(7) 0.0376(7) -0.0068(6) 0.0061(5) -0.0029(5)
C24 0.0461(7) 0.0548(8) 0.0603(9) -0.0070(6) -0.0037(6) -0.0028(7)
C5 0.0498(8) 0.0492(8) 0.0555(9) -0.0047(6) -0.0009(6) -0.0140(6)
C11 0.0402(7) 0.0434(7) 0.0523(8) 0.0018(5) -0.0032(6) -0.0030(6)
C3 0.0420(7) 0.0673(9) 0.0562(9) 0.0075(7) -0.0023(6) -0.0063(7)
C20 0.0445(7) 0.0466(7) 0.0570(9) -0.0009(6) -0.0033(6) -0.0002(6)
C2 0.0440(7) 0.0523(8) 0.0516(8) -0.0062(6) -0.0007(6) -0.0094(6)
C4 0.0484(8) 0.0575(8) 0.0518(8) -0.0001(6) -0.0046(6) -0.0109(6)
C6 0.0466(7) 0.0445(7) 0.0676(9) 0.0002(6) 0.0023(7) -0.0133(6)
C23 0.0563(8) 0.0531(8) 0.0555(9) -0.0034(7) -0.0112(7) -0.0082(7)
C13 0.0519(8) 0.0656(9) 0.0439(8) -0.0145(7) 0.0035(6) -0.0015(7)
C22 0.0594(9) 0.0528(8) 0.0454(8) 0.0132(7) -0.0058(7) 0.0005(6)
C1 0.0438(7) 0.0374(7) 0.0590(8) -0.0022(5) -0.0026(6) -0.0042(6)
C17 0.0637(8) 0.0431(7) 0.0495(8) -0.0026(6) 0.0125(7) -0.0002(6)
C10 0.0657(9) 0.0652(10) 0.0605(10) -0.0042(8) 0.0080(8) -0.0210(8)
C21 0.0489(8) 0.0537(8) 0.0571(9) 0.0036(6) 0.0018(7) 0.0068(7)
C14 0.0702(10) 0.0876(13) 0.0498(9) -0.0411(9) 0.0118(8) -0.0093(8)
C7 0.0685(10) 0.0790(11) 0.0573(10) 0.0162(9) -0.0086(8) -0.0089(8)
C9 0.0986(13) 0.0769(12) 0.0509(9) -0.0070(10) 0.0073(9) -0.0149(8)
C16 0.1036(13) 0.0409(8) 0.0650(10) -0.0060(8) 0.0293(9) 0.0038(7)
C15 0.1103(15) 0.0588(10) 0.0632(10) -0.0438(10) 0.0307(10) -0.0132(8)
C8 0.0974(13) 0.0846(12) 0.0519(10) 0.0137(11) -0.0077(9) -0.0064(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_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
C11 O1 C1 . . 116.37(10) ?
C18 O3 C2 . . 116.38(9) ?
C24 C19 C18 . . 122.08(13) ?
C24 C19 C20 . . 120.14(13) ?
C20 C19 C18 . . 117.74(12) ?
O3 C18 C19 . . 112.23(11) ?
O4 C18 O3 . . 123.99(12) ?
O4 C18 C19 . . 123.77(12) ?
C13 C12 C11 . . 116.87(12) ?
C17 C12 C11 . . 122.32(12) ?
C17 C12 C13 . . 120.82(13) ?
C19 C24 H24 . . 120.7 ?
C23 C24 C19 . . 118.64(13) ?
C23 C24 H24 . . 120.7 ?
C4 C5 C6 . . 121.44(13) ?
C10 C5 C4 . . 118.62(13) ?
C10 C5 C6 . . 119.92(13) ?
O1 C11 C12 . . 112.13(11) ?
O2 C11 O1 . . 124.43(12) ?
O2 C11 C12 . . 123.44(12) ?
H3A C3 H3B . . 107.9 ?
C2 C3 H3A . . 109.1 ?
C2 C3 H3B . . 109.1 ?
C4 C3 H3A . . 109.1 ?
C4 C3 H3B . . 109.1 ?
C4 C3 C2 . . 112.34(11) ?
C19 C20 H20 . . 120.3 ?
C21 C20 C19 . . 119.45(13) ?
C21 C20 H20 . . 120.3 ?
O3 C2 C3 . . 110.04(11) ?
O3 C2 H2 . . 108.8 ?
O3 C2 C1 . . 108.10(10) ?
C3 C2 H2 . . 108.8 ?
C1 C2 C3 . . 112.14(12) ?
C1 C2 H2 . . 108.8 ?
C5 C4 C3 . . 121.48(12) ?
C7 C4 C5 . . 119.30(14) ?
C7 C4 C3 . . 119.21(13) ?
C5 C6 H6A . . 108.9 ?
C5 C6 H6B . . 108.9 ?
C5 C6 C1 . . 113.52(11) ?
H6A C6 H6B . . 107.7 ?
C1 C6 H6A . . 108.9 ?
C1 C6 H6B . . 108.9 ?
F6 C23 C24 . . 120.33(13) ?
F6 C23 C22 . . 117.77(13) ?
C24 C23 C22 . . 121.90(13) ?
C12 C13 H13 . . 120.7 ?
C14 C13 C12 . . 118.69(15) ?
C14 C13 H13 . . 120.7 ?
F5 C22 C23 . . 120.51(13) ?
F5 C22 C21 . . 120.83(14) ?
C23 C22 C21 . . 118.66(13) ?
O1 C1 C2 . . 106.70(10) ?
O1 C1 C6 . . 109.52(11) ?
O1 C1 H1 . . 110.3 ?
C2 C1 C6 . . 109.65(10) ?
C2 C1 H1 . . 110.3 ?
C6 C1 H1 . . 110.3 ?
C12 C17 H17 . . 120.8 ?
C16 C17 C12 . . 118.40(14) ?
C16 C17 H17 . . 120.8 ?
C5 C10 H10 . . 119.5 ?
C9 C10 C5 . . 120.97(15) ?
C9 C10 H10 . . 119.5 ?
F4 C21 C20 . . 120.46(13) ?
F4 C21 C22 . . 118.31(13) ?
C20 C21 C22 . . 121.21(14) ?
F1 C14 C13 . . 120.00(18) ?
F1 C14 C15 . . 118.41(15) ?
C13 C14 C15 . . 121.59(15) ?
C4 C7 H7 . . 119.2 ?
C8 C7 C4 . . 121.53(16) ?
C8 C7 H7 . . 119.2 ?
C10 C9 H9 . . 119.9 ?
C10 C9 C8 . . 120.23(16) ?
C8 C9 H9 . . 119.9 ?
F3 C16 C17 . . 119.93(17) ?
F3 C16 C15 . . 118.58(15) ?
C15 C16 C17 . . 121.48(16) ?
F2 C15 C14 . . 120.33(18) ?
F2 C15 C16 . . 120.66(19) ?
C14 C15 C16 . . 119.00(14) ?
C7 C8 C9 . . 119.35(16) ?
C7 C8 H8 . . 120.3 ?
C9 C8 H8 . . 120.3 ?
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
O1 C11 . 1.3336(16) ?
O1 C1 . 1.4606(15) ?
F5 C22 . 1.3376(16) ?
O3 C18 . 1.3437(16) ?
O3 C2 . 1.4529(16) ?
O4 C18 . 1.2050(15) ?
F4 C21 . 1.3451(17) ?
F6 C23 . 1.3484(16) ?
O2 C11 . 1.2026(16) ?
F1 C14 . 1.3468(19) ?
F3 C16 . 1.3445(19) ?
F2 C15 . 1.3401(18) ?
C19 C18 . 1.4855(19) ?
C19 C24 . 1.3874(18) ?
C19 C20 . 1.3890(19) ?
C12 C11 . 1.4888(18) ?
C12 C13 . 1.3940(17) ?
C12 C17 . 1.3813(19) ?
C24 H24 . 0.9500 ?
C24 C23 . 1.373(2) ?
C5 C4 . 1.3963(19) ?
C5 C6 . 1.512(2) ?
C5 C10 . 1.396(2) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C3 C2 . 1.512(2) ?
C3 C4 . 1.511(2) ?
C20 H20 . 0.9500 ?
C20 C21 . 1.368(2) ?
C2 H2 . 1.0000 ?
C2 C1 . 1.5060(18) ?
C4 C7 . 1.387(2) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C6 C1 . 1.512(2) ?
C23 C22 . 1.373(2) ?
C13 H13 . 0.9500 ?
C13 C14 . 1.362(2) ?
C22 C21 . 1.375(2) ?
C1 H1 . 1.0000 ?
C17 H17 . 0.9500 ?
C17 C16 . 1.374(2) ?
C10 H10 . 0.9500 ?
C10 C9 . 1.375(2) ?
C14 C15 . 1.369(3) ?
C7 H7 . 0.9500 ?
C7 C8 . 1.372(2) ?
C9 H9 . 0.9500 ?
C9 C8 . 1.379(3) ?
C16 C15 . 1.374(3) ?
C8 H8 . 0.9500 ?
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
F5 C22 C21 F4 . . . . -0.7(2) ?
F5 C22 C21 C20 . . . . -179.19(12) ?
O3 C2 C1 O1 . . . . 65.84(13) ?
O3 C2 C1 C6 . . . . -175.63(10) ?
F6 C23 C22 F5 . . . . -0.7(2) ?
F6 C23 C22 C21 . . . . 179.36(12) ?
F1 C14 C15 F2 . . . . -0.7(2) ?
F1 C14 C15 C16 . . . . 178.44(14) ?
F3 C16 C15 F2 . . . . -2.1(2) ?
F3 C16 C15 C14 . . . . 178.82(14) ?
C19 C24 C23 F6 . . . . -179.77(12) ?
C19 C24 C23 C22 . . . . 0.5(2) ?
C19 C20 C21 F4 . . . . -178.61(12) ?
C19 C20 C21 C22 . . . . -0.1(2) ?
C18 O3 C2 C3 . . . . -87.56(14) ?
C18 O3 C2 C1 . . . . 149.68(11) ?
C18 C19 C24 C23 . . . . -177.43(12) ?
C18 C19 C20 C21 . . . . 177.37(11) ?
C12 C13 C14 F1 . . . . -177.78(12) ?
C12 C13 C14 C15 . . . . 1.3(2) ?
C12 C17 C16 F3 . . . . -178.45(13) ?
C12 C17 C16 C15 . . . . 0.7(2) ?
C24 C19 C18 O3 . . . . -10.62(18) ?
C24 C19 C18 O4 . . . . 168.10(13) ?
C24 C19 C20 C21 . . . . -0.3(2) ?
C24 C23 C22 F5 . . . . 179.02(12) ?
C24 C23 C22 C21 . . . . -0.9(2) ?
C5 C4 C7 C8 . . . . 0.0(2) ?
C5 C6 C1 O1 . . . . 70.05(14) ?
C5 C6 C1 C2 . . . . -46.71(15) ?
C5 C10 C9 C8 . . . . 0.3(3) ?
C11 O1 C1 C2 . . . . -146.63(11) ?
C11 O1 C1 C6 . . . . 94.76(13) ?
C11 C12 C13 C14 . . . . 178.91(12) ?
C11 C12 C17 C16 . . . . -179.91(13) ?
C3 C2 C1 O1 . . . . -55.64(14) ?
C3 C2 C1 C6 . . . . 62.89(15) ?
C3 C4 C7 C8 . . . . -178.74(16) ?
C20 C19 C18 O3 . . . . 171.79(11) ?
C20 C19 C18 O4 . . . . -9.5(2) ?
C20 C19 C24 C23 . . . . 0.1(2) ?
C2 O3 C18 O4 . . . . -0.77(19) ?
C2 O3 C18 C19 . . . . 177.94(10) ?
C2 C3 C4 C5 . . . . 16.95(19) ?
C2 C3 C4 C7 . . . . -164.32(13) ?
C4 C5 C6 C1 . . . . 17.94(18) ?
C4 C5 C10 C9 . . . . -0.2(2) ?
C4 C3 C2 O3 . . . . -167.43(10) ?
C4 C3 C2 C1 . . . . -47.08(15) ?
C4 C7 C8 C9 . . . . 0.1(3) ?
C6 C5 C4 C3 . . . . -2.7(2) ?
C6 C5 C4 C7 . . . . 178.61(13) ?
C6 C5 C10 C9 . . . . -178.81(14) ?
C23 C22 C21 F4 . . . . 179.20(12) ?
C23 C22 C21 C20 . . . . 0.7(2) ?
C13 C12 C11 O1 . . . . -177.72(11) ?
C13 C12 C11 O2 . . . . 2.2(2) ?
C13 C12 C17 C16 . . . . -0.04(19) ?
C13 C14 C15 F2 . . . . -179.84(14) ?
C13 C14 C15 C16 . . . . -0.7(2) ?
C1 O1 C11 O2 . . . . 0.8(2) ?
C1 O1 C11 C12 . . . . -179.33(10) ?
C17 C12 C11 O1 . . . . 2.15(18) ?
C17 C12 C11 O2 . . . . -177.98(14) ?
C17 C12 C13 C14 . . . . -1.0(2) ?
C17 C16 C15 F2 . . . . 178.78(14) ?
C17 C16 C15 C14 . . . . -0.4(2) ?
C10 C5 C4 C3 . . . . 178.74(13) ?
C10 C5 C4 C7 . . . . 0.0(2) ?
C10 C5 C6 C1 . . . . -163.47(12) ?
C10 C9 C8 C7 . . . . -0.3(3) ?
_cod_database_fobs_code 2022279