#------------------------------------------------------------------------------
#$Date: 2020-11-25 07:11:19 +0200 (Wed, 25 Nov 2020) $
#$Revision: 259242 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/22/2022282.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_2022282
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(2,4,6-trifluorobenzoate)
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-I 2ya'
_space_group_name_H-M_alt 'I 1 2/a 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 112.62(3)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 23.308(10)
_cell_length_b 7.132(3)
_cell_length_c 27.253(9)
_cell_measurement_reflns_used 4856
_cell_measurement_temperature 193.4
_cell_measurement_theta_max 27.4479
_cell_measurement_theta_min 3.0091
_cell_volume 4182(3)
_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_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device
;
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 0.0440
_diffrn_reflns_av_unetI/netI 0.0337
_diffrn_reflns_limit_h_max 28
_diffrn_reflns_limit_h_min -30
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 35
_diffrn_reflns_limit_l_min -35
_diffrn_reflns_number 20765
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.448
_diffrn_reflns_theta_min 3.009
_exptl_absorpt_coefficient_mu 0.138
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.7965
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details DTABSCOR
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.526
_exptl_crystal_description prism
_exptl_crystal_F_000 1952
_exptl_crystal_size_max 0.238
_exptl_crystal_size_mid 0.116
_exptl_crystal_size_min 0.087
_refine_diff_density_max 0.220
_refine_diff_density_min -0.218
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.134
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 307
_refine_ls_number_reflns 4763
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.134
_refine_ls_R_factor_all 0.0620
_refine_ls_R_factor_gt 0.0464
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.5393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1131
_refine_ls_wR_factor_ref 0.1234
_reflns_number_gt 3880
_reflns_number_total 4763
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file op3007sup1.cif
_cod_data_source_block 9
_cod_database_code 2022282
_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
;
1 -1 0 2.22 0.65
1 1 0 5.99 1.45
-1 1 0 1.06 0.41
-1 -1 0 1.04 0.40
1 -1 0 -0.26 0.37
-1 1 0 0.78 0.34
-1 1 0 0.82 0.87
-1 1 0 1.45 0.43
-2 0 4 1455.80 7.42
2 0 -4 1436.74 6.63
-2 0 4 1469.70 6.75
0 0 4 1.64 0.37
0 0 -4 2.27 0.65
0 0 -4 1.43 0.21
0 0 -4 1.54 0.39
0 0 4 1.92 0.21
0 0 4 1.34 0.37
-3 0 -1 0.18 0.25
3 0 1 0.47 0.44
3 0 1 -0.04 0.18
-3 0 -1 0.23 0.33
-3 0 -1 0.34 0.41
-1 -1 2 4740.68 264.08
1 1 -2 4609.76 256.82
-1 -1 2 4716.93 262.79
-1 1 2 4677.01 260.56
1 -1 -2 4435.79 17.27
-1 1 2 4658.46 259.48
1 1 -2 4803.47 267.59
-2 -1 1 1839.40 9.44
2 1 -1 1854.16 9.42
2 1 -1 1793.81 9.20
2 -1 -1 1891.56 9.82
4 0 -2 165.09 5.35
-4 0 2 169.66 5.59
4 0 -2 170.13 5.58
-1 -1 -2 1704.73 7.55
-1 1 -2 1642.48 9.27
1 1 2 1631.38 8.78
1 -1 2 1653.11 8.98
1 1 2 1709.22 8.93
1 1 2 1674.71 7.48
2 1 1 167.36 5.64
-2 -1 -1 157.99 5.43
2 1 1 160.36 5.14
-2 -1 -1 168.92 5.45
-2 1 -1 168.45 5.78
2 -1 1 165.71 5.75
-2 1 -1 159.47 5.23
2 -1 1 175.00 5.82
2 1 1 179.09 6.06
2 1 1 163.08 5.64
2 -1 1 158.86 5.38
-2 1 -1 156.84 5.44
0 1 -3 0.29 0.64
0 -1 3 0.62 0.48
0 -1 -3 0.34 0.31
0 1 3 0.26 0.49
0 -1 3 0.72 0.59
0 1 -3 0.52 0.56
0 1 -3 0.63 0.38
0 1 3 0.64 0.30
0 1 -3 0.56 0.55
0 -1 -3 0.49 0.52
0 1 3 0.54 0.29
2 1 -3 1.38 0.77
-2 -1 3 3.52 0.75
-2 1 3 2.57 0.40
2 1 -3 2.81 0.62
-2 1 3 2.55 0.68
2 -1 -3 3.90 1.18
-2 1 3 2.45 0.52
-2 -1 3 2.41 0.66
2 1 -3 3.05 0.62
-2 -1 3 3.03 0.74
-2 1 3 2.20 0.69
-2 1 3 2.85 0.61
-1 0 5 0.28 0.35
-1 0 5 0.28 0.54
1 0 -5 0.84 0.63
4 0 0 6.36 1.46
-4 0 0 6.33 1.49
4 0 0 6.74 1.01
-4 0 0 12.33 1.02
-4 0 0 5.59 1.12
4 0 0 7.33 1.31
3 1 -2 356.02 4.13
-3 -1 2 373.78 3.90
-3 -1 2 380.32 4.25
-3 -1 2 365.26 4.20
3 -1 -2 358.50 3.99
-3 1 2 362.38 4.20
-3 1 2 366.22 2.26
-3 1 2 378.39 4.24
3 -1 -2 364.60 4.16
4 0 -4 1855.72 8.30
-4 0 4 1820.00 8.24
4 0 -4 1771.03 9.23
-4 0 4 1871.45 9.66
-3 0 5 0.17 0.27
3 0 -5 0.17 0.48
-3 0 5 -0.20 0.55
3 0 -5 0.09 0.20
3 0 -5 0.37 0.60
-3 0 5 1.02 0.57
3 1 0 0.68 0.50
-3 -1 0 0.59 0.59
-3 -1 0 0.43 0.53
3 1 0 1.71 1.20
3 1 0 0.63 0.65
-3 -1 0 0.52 0.55
-3 1 0 0.27 0.58
-3 1 0 0.20 0.43
-3 1 0 0.34 0.48
3 -1 0 0.42 0.50
3 -1 0 0.40 0.40
3 -1 0 0.81 1.03
-1 1 4 1331.10 6.89
-1 -1 4 1348.98 8.32
1 -1 -4 1367.54 8.05
1 1 -4 1329.41 8.59
1 1 -4 1370.62 7.49
-1 -1 4 1347.19 8.83
1 -1 -4 1351.15 7.10
-2 0 -4 176.73 5.72
-2 0 -4 189.10 6.43
2 0 4 185.67 6.02
2 0 4 174.58 5.62
-2 0 -4 173.89 5.53
3 0 3 0.55 0.47
-3 0 -3 0.51 0.42
3 0 3 0.22 0.76
-3 0 -3 0.51 0.74
5 0 -3 0.71 0.63
5 0 -3 0.67 0.56
-5 0 3 0.26 0.50
-5 0 3 0.22 0.40
-5 0 3 0.35 0.58
-3 -1 4 144.24 5.17
3 1 -4 162.79 5.77
3 1 -4 169.87 6.00
-3 -1 4 163.59 5.89
-3 1 4 154.31 4.79
3 -1 -4 146.90 5.10
-3 1 4 152.23 5.28
3 -1 -4 146.56 5.51
3 -1 -4 157.04 4.90
2 0 -6 2152.14 10.50
2 0 -6 2174.56 10.27
-5 0 1 0.11 0.31
-5 0 1 0.11 0.98
-5 0 1 -0.16 0.51
5 0 -1 0.48 0.45
5 0 -1 0.13 0.41
1 0 5 0.57 0.58
-1 0 -5 0.43 0.57
1 0 5 0.17 0.28
-1 0 -5 0.41 0.76
-1 0 -5 0.16 0.27
-4 -1 1 1.25 0.62
4 1 -1 0.88 0.70
-4 -1 1 0.85 0.57
4 1 -1 1.28 0.97
-4 1 1 1.55 0.66
4 -1 -1 1.46 0.42
4 -1 -1 1.11 1.11
-4 1 1 0.68 0.29
2 1 3 997.44 6.93
-2 1 -3 1031.47 7.03
-2 -1 -3 1032.55 7.50
2 -1 3 988.17 6.72
-2 1 -3 1025.09 6.81
2 -1 3 1021.54 7.78
4 1 -3 2.93 0.54
4 1 -3 2.37 0.75
-4 -1 3 2.51 0.71
4 1 -3 2.72 0.76
-4 -1 3 2.35 0.77
4 -1 -3 2.68 0.77
-4 1 3 3.26 0.86
-4 0 -2 6403.93 356.72
4 0 2 6834.82 380.48
-4 0 -2 6751.45 375.86
-1 1 -4 787.40 6.34
1 -1 4 802.96 5.83
-1 1 -4 804.21 5.62
-1 -1 -4 840.60 4.65
1 1 4 793.95 4.73
-1 -1 -4 841.25 6.42
1 1 4 817.40 6.00
2 1 -5 2.23 0.78
-2 1 5 1.77 0.39
2 -1 -5 1.90 0.59
-2 -1 5 2.02 0.63
2 -1 -5 2.76 0.83
-2 1 5 2.68 0.79
2 1 -5 1.87 0.50
-2 -1 5 1.48 0.73
-2 1 5 2.14 0.52
-3 -1 -2 1512.59 6.20
3 1 2 1523.05 6.11
-3 1 -2 1497.48 9.40
-3 1 -2 1538.89 8.43
0 0 -6 74.35 2.80
0 0 -6 77.66 2.65
0 0 6 78.90 2.67
0 0 6 78.44 3.00
5 0 -5 0.25 0.77
5 0 -5 0.82 0.69
-5 0 5 -0.14 0.51
-5 0 5 0.58 1.00
-5 0 5 0.24 0.59
0 -1 5 93.95 3.86
0 1 -5 97.65 3.56
0 1 -5 94.13 3.41
0 1 -5 99.02 3.86
0 -1 -5 100.42 3.76
0 1 5 92.30 4.00
0 -1 -5 99.28 3.68
0 1 5 92.46 3.59
0 -1 -5 102.58 5.07
0 1 5 92.05 3.84
-4 -1 -1 201.42 6.37
4 1 1 203.25 6.38
-4 -1 -1 209.44 7.12
-4 1 -1 225.34 12.88
4 -1 1 192.04 6.41
4 -1 1 204.94 7.04
-4 1 -1 215.34 7.48
5 0 1 0.43 0.48
-5 0 -1 0.33 0.48
-5 0 -1 0.06 0.57
-5 0 -1 0.05 9.88
4 1 -5 105.10 3.82
-4 -1 5 111.45 4.15
-4 -1 5 106.22 4.20
4 -1 -5 107.09 4.74
-4 1 5 103.99 3.85
4 -1 -5 106.39 3.41
-4 1 5 95.02 3.00
4 1 -5 106.35 4.24
4 -1 -5 97.80 3.74
5 1 -2 51.80 2.49
-5 -1 2 57.15 2.84
-5 1 2 57.57 2.82
-5 1 2 55.64 2.01
5 -1 -2 55.93 2.25
5 -1 -2 58.03 2.87
-5 -1 2 56.65 2.49
3 0 -7 0.27 0.58
-3 0 7 0.46 0.56
-3 0 7 0.07 0.11
-6 0 2 2905.88 13.98
-6 0 4 1.37 0.60
-6 0 4 2.32 0.65
-6 0 4 0.80 0.50
6 0 -4 0.43 0.55
1 0 -7 0.10 0.13
1 0 -7 0.24 0.59
-1 0 7 0.16 0.11
1 0 -7 0.42 0.66
-1 0 7 0.84 0.84
-1 -1 6 114.64 4.51
1 1 -6 108.43 3.97
1 1 -6 121.93 4.98
1 1 -6 113.28 3.95
-1 1 6 108.63 4.07
1 -1 -6 114.56 4.67
-1 1 6 109.11 3.88
1 -1 -6 124.40 4.96
-1 1 6 112.15 3.96
1 -1 -6 113.84 4.42
3 1 -6 1440.86 7.65
-3 -1 6 1448.78 7.99
3 -1 -6 1444.01 9.32
-3 1 6 1430.58 8.38
-5 1 4 378.42 4.60
5 -1 -4 378.75 4.96
-5 -1 4 395.89 4.83
-5 -1 4 390.74 5.15
5 1 -4 397.53 5.19
-5 -1 0 70.12 2.61
5 1 0 71.81 3.20
-5 1 0 72.83 2.79
5 -1 0 70.21 2.65
5 -1 0 73.45 3.75
-5 1 0 72.33 3.16
-5 -1 0 72.54 3.31
5 1 0 68.98 2.49
-6 0 0 9.41 1.89
-6 0 0 7.77 1.01
-6 0 0 9.49 1.58
6 0 0 8.45 1.53
0 -2 0 4.47 1.06
0 -2 0 3.70 1.37
0 2 0 3.12 0.72
3 0 5 6.69 0.99
-3 0 -5 13.01 2.75
3 0 5 11.67 2.53
1 -2 -1 33.66 2.10
-1 -2 1 36.85 2.25
1 -2 -1 36.36 2.71
-1 -2 1 36.82 2.62
-1 2 1 38.52 2.02
1 2 -1 38.33 2.49
-3 1 -4 4393.01 18.73
3 -1 4 4340.36 19.23
-3 -1 -4 4715.28 262.93
-5 0 7 -0.86 1.05
-5 0 7 0.52 0.28
5 0 -7 -0.07 1.55
5 0 -7 -0.10 0.33
-5 0 7 -0.22 0.54
2 -1 5 48.55 2.24
2 -1 5 53.89 2.72
-2 1 -5 49.09 2.28
-2 1 -5 49.92 2.54
-2 -1 -5 49.74 3.04
2 1 5 46.29 1.72
-6 0 6 9999.00 556.87
-6 0 6 9608.63 534.98
6 0 -6 9454.94 526.42
1 -2 1 3632.88 18.87
0 2 -2 2058.23 12.57
0 -2 2 2060.15 13.35
0 -2 2 1921.92 13.05
-4 1 -3 3873.04 16.92
-4 -1 -3 3769.85 18.57
-4 -1 -3 3815.91 17.58
-4 1 -3 3757.61 16.81
2 1 -7 7.81 0.74
-2 1 7 8.54 1.94
-2 -1 7 11.92 2.09
2 -1 -7 9.47 1.38
-2 -1 7 7.57 1.13
2 -1 -7 8.62 0.95
2 1 -7 8.66 1.27
-2 1 7 9.02 0.77
-6 -1 3 200.68 7.02
-6 -1 3 217.09 7.37
6 1 -3 197.57 6.99
-6 1 3 192.39 6.80
6 -1 -3 197.01 7.64
6 -1 -3 191.37 5.98
-6 1 3 161.23 5.12
-2 0 8 45.06 3.03
2 0 -8 41.88 2.20
-1 1 -6 1655.38 8.67
-1 1 -6 1728.58 11.68
1 1 6 1657.10 7.72
1 1 6 1707.11 8.01
1 1 6 1646.61 9.28
2 -2 0 127.38 5.14
-2 -2 0 129.64 5.55
-2 -2 0 136.27 5.64
-2 2 0 127.27 5.07
2 2 0 123.28 4.84
-2 2 0 129.89 4.74
-5 -1 6 10.40 1.89
-5 -1 6 7.98 1.20
5 -1 -6 10.91 2.64
5 1 -6 6.35 1.15
5 1 -6 7.83 1.55
-5 1 6 8.13 1.62
5 -1 -6 8.98 1.08
-5 1 6 7.85 0.78
-2 -2 2 628.76 7.37
2 -2 -2 605.87 5.31
-2 2 2 641.58 5.68
2 2 -2 640.42 7.18
-2 2 2 595.96 7.08
-2 -2 2 632.05 6.92
-1 0 -7 2.54 0.71
1 0 7 -0.26 0.50
1 0 7 1.23 0.77
-5 0 -3 3.07 6.15
7 0 -3 0.17 0.29
-7 0 3 0.48 0.68
-7 0 3 -0.32 0.87
7 0 -3 0.33 0.54
-6 1 1 10.55 0.87
6 -1 -1 9.83 0.84
6 1 -1 11.64 1.50
-6 -1 1 13.33 1.04
6 -1 -1 10.80 1.22
6 1 -1 11.00 0.88
-6 -1 1 12.43 1.28
-6 1 1 11.21 1.19
-1 2 3 354.18 4.34
1 2 -3 358.07 8.96
-1 -2 3 353.31 6.01
-1 -2 3 350.96 5.60
1 -2 -3 321.76 4.67
4 1 -7 627.76 6.55
4 -1 -7 609.62 4.30
4 -1 -7 612.36 5.50
-4 1 7 622.06 5.38
4 1 -7 620.25 5.12
-4 -1 7 613.25 5.10
-5 1 -2 2630.79 13.93
-6 -1 5 80.42 3.46
-6 -1 5 83.05 3.37
6 1 -5 83.55 3.66
6 -1 -5 100.91 6.37
-6 1 5 103.06 4.34
-3 -2 1 3.58 0.87
3 2 -1 4.76 1.38
-3 -2 1 4.02 1.18
3 -2 -1 4.92 0.99
3 -2 -1 4.14 0.71
-3 2 1 4.65 0.74
-3 2 1 3.79 1.11
-7 0 5 0.79 0.69
7 0 -5 0.18 0.48
-7 0 5 0.87 1.09
-7 0 5 0.45 0.58
0 -1 7 29.24 1.93
0 -1 7 29.93 1.56
0 1 -7 31.09 2.22
0 1 -7 29.39 1.91
0 1 7 31.16 1.89
0 1 7 28.90 1.74
0 -1 -7 31.54 2.15
0 1 7 30.05 1.97
0 -1 -7 32.13 1.75
7 0 -1 0.28 0.23
-7 0 1 -0.02 0.85
-7 0 1 0.30 0.56
1 -2 3 1670.88 12.90
-1 2 -3 1648.37 11.53
-1 2 -3 1656.16 11.03
1 2 3 1700.47 11.33
2 2 2 12.73 1.42
-2 2 -2 15.31 3.51
2 -2 2 17.62 4.04
2 2 2 11.90 2.69
-2 2 -2 12.10 1.25
-2 -2 -2 12.51 1.52
-2 -2 -2 11.64 1.24
-3 -2 3 39.14 3.91
-3 -2 3 41.95 3.14
3 2 -3 43.47 2.64
3 -2 -3 37.75 1.72
-3 2 3 38.79 2.46
-3 2 3 43.34 1.95
0 0 8 2.17 0.71
0 0 -8 2.92 0.67
0 0 8 2.72 0.38
0 0 -8 2.48 0.73
-6 0 -2 1194.57 6.99
-6 0 -2 1226.13 9.28
6 0 2 1223.72 6.93
-2 -2 4 30.08 5.08
2 2 -4 24.99 1.85
-2 -2 4 25.09 2.27
2 -2 -4 25.93 2.80
-2 2 4 28.03 1.57
2 -2 -4 25.86 1.74
0 2 4 3.44 0.95
0 2 -4 4.16 1.01
0 -2 -4 3.38 1.05
0 -2 4 4.86 1.52
3 -2 1 205.24 7.54
-3 -2 -1 185.51 6.44
-3 -2 -1 205.41 7.83
-3 2 -1 199.37 7.23
-3 2 -1 201.36 6.86
3 2 1 207.97 7.78
3 1 -8 27.76 1.35
3 -1 -8 27.63 1.54
-3 1 8 27.33 1.41
3 1 -8 30.74 2.27
-3 -1 8 30.18 2.80
-3 -1 8 29.83 2.48
-3 1 8 29.53 1.87
-3 1 8 26.26 1.66
-3 1 8 28.10 1.57
-6 -1 -1 324.76 3.03
-6 -1 -1 304.38 4.82
-6 -1 -1 340.99 5.90
6 -1 1 319.07 5.10
-4 -2 2 272.99 4.47
-4 -2 2 286.18 5.67
4 2 -2 263.72 4.83
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-24 -4 24 5.77 2.80
-20 2 -14 1.96 2.12
-20 -2 -14 1.83 2.16
-20 -2 -14 3.50 2.72
-20 2 -14 1.33 1.19
-28 -3 17 7.42 2.83
-28 -3 17 8.32 2.63
-28 3 17 6.02 3.02
-28 3 17 6.89 2.22
6 5 -29 0.90 1.60
-6 -5 29 -0.57 1.49
-20 2 32 21.96 12.19
-20 -2 32 30.44 7.68
10 -8 -16 36.00 17.20
10 8 -16 56.79 13.20
-10 8 16 52.55 11.92
-10 -8 16 56.79 12.97
-29 2 17 1.27 1.28
-29 -2 17 1.42 1.92
-29 2 17 2.36 2.00
-29 -2 17 3.43 2.43
7 -8 -17 1.60 1.53
-7 -8 17 4.99 3.31
-7 8 17 3.26 2.15
7 8 -17 6.06 2.84
-14 -2 34 1.18 1.44
-14 2 34 1.34 1.31
14 2 -34 0.90 1.64
-24 -3 27 14.16 5.20
-24 3 27 12.43 4.14
-26 -4 4 1.46 2.05
26 4 -4 3.80 2.74
26 -4 -4 1.94 2.01
-26 4 4 2.30 2.26
-29 2 9 5.69 2.21
-29 2 9 4.97 2.62
-29 -2 9 5.04 2.16
-18 -5 27 2.44 2.84
18 5 -27 1.78 2.16
-18 5 27 1.07 1.37
12 7 11 2.83 3.73
-12 -7 -11 0.82 2.50
12 -7 11 0.72 1.30
-12 7 -11 3.07 2.57
22 6 -4 4.63 2.86
-22 -6 4 0.74 1.74
-22 6 4 0.52 1.67
22 -6 -4 -0.25 1.20
-3 -7 22 1.40 1.92
3 7 -22 0.70 1.72
-10 0 -26 0.56 1.66
22 5 -23 1.63 1.66
-22 -5 23 1.87 2.38
-22 5 23 1.46 1.74
-17 0 -19 1.91 1.78
25 5 -14 10.94 4.11
-25 -5 14 16.53 4.73
-25 5 14 13.94 4.51
25 -5 -14 12.85 6.71
-13 0 35 -0.17 1.36
3 9 4 3.12 2.14
3 9 4 4.00 3.87
-3 9 -4 3.16 2.71
3 -9 4 3.75 3.35
-3 -9 -4 2.60 1.90
16 7 -19 4.53 3.13
16 -7 -19 4.63 2.55
-16 -7 19 5.93 3.47
2 -9 5 8.53 3.24
-2 -9 -5 3.53 2.03
2 9 5 5.83 2.86
-2 9 -5 3.38 1.50
2 9 5 7.65 4.11
-2 9 -5 5.92 3.46
-15 -7 20 4.11 4.47
15 7 -20 1.61 2.06
15 -7 -20 4.26 2.55
-15 7 20 3.67 2.35
2 -1 -33 32.70 7.81
2 1 -33 25.74 12.36
4 5 25 9.35 2.91
4 -5 25 5.27 2.43
-4 5 -25 3.27 2.35
-21 -3 30 1.02 1.75
-21 3 30 1.23 1.62
21 3 -30 1.22 1.68
-7 -4 -25 1.27 1.49
-7 4 -25 3.76 2.39
-18 0 34 2.32 2.22
-17 4 -15 1.05 1.51
-17 -4 -15 1.81 1.48
17 4 15 2.86 2.21
8 2 -34 13.04 4.18
-30 0 14 28.53 16.93
-30 0 14 22.36 11.09
5 -7 18 2.12 2.29
-5 7 -18 1.14 2.02
-5 -7 -18 2.24 2.73
-22 -6 16 19.25 5.55
-22 -6 16 15.02 7.10
22 6 -16 22.29 6.47
-22 6 16 11.12 3.96
22 -6 -16 14.80 7.80
-27 -4 13 12.73 4.49
27 4 -13 10.04 3.12
-27 4 13 11.00 4.04
-27 4 13 9.17 2.76
24 5 -19 8.70 3.29
-24 -5 19 6.68 3.08
-24 -5 19 5.64 2.88
-24 5 19 7.74 2.61
-24 5 19 7.41 3.04
15 4 -31 0.01 1.30
-15 -4 31 3.13 2.90
-15 4 31 1.77 1.50
-4 9 -3 2.81 3.24
4 9 3 1.70 1.93
-4 -9 -3 2.37 2.02
-4 -9 -3 0.79 1.75
4 -9 3 2.24 2.82
27 4 -11 1.33 1.79
-27 -4 11 2.69 2.33
-27 4 11 2.41 2.27
27 -4 -11 2.25 2.28
-25 -5 8 2.11 2.31
25 5 -8 0.54 1.93
-25 5 8 0.30 1.68
25 -5 -8 2.25 1.33
2 -9 -7 4.38 2.46
-2 -9 7 1.83 1.89
2 9 -7 0.49 0.93
2 9 -7 2.23 2.27
-2 9 7 2.45 2.48
5 1 -34 15.14 4.69
5 -1 -34 9.26 4.65
-6 -9 3 6.41 3.07
-6 -9 3 2.26 2.97
-6 9 3 2.53 2.29
6 -9 -3 4.57 2.67
6 9 -3 3.13 2.25
-1 9 -6 2.71 2.32
1 9 6 2.09 3.19
-1 9 -6 1.59 2.77
-1 -9 -6 2.82 2.35
1 -9 6 2.89 3.11
2 4 -30 0.68 1.58
2 -4 -30 0.09 0.87
-30 0 12 1.30 2.05
0 -7 21 2.78 2.81
0 7 -21 -0.49 1.76
-23 4 -5 5.75 2.59
-23 -4 -5 11.09 5.21
23 4 5 7.78 3.25
-19 -7 4 0.59 1.66
19 7 -4 0.04 2.19
19 -7 -4 2.47 1.72
-19 7 4 4.07 3.06
5 -9 -6 1.41 1.52
-5 -9 6 2.39 1.87
-5 9 6 2.48 3.60
5 9 -6 4.02 2.62
5 9 -6 2.77 2.68
-8 -3 33 4.66 2.60
8 3 -33 6.61 4.23
3 -6 23 3.79 2.50
-3 6 -23 3.67 2.54
3 6 23 4.02 2.24
-28 2 22 0.34 1.00
-28 -2 22 1.63 2.41
-28 2 22 3.50 2.12
3 8 -17 5.21 2.42
-3 -8 17 9.61 4.41
3 8 -17 6.53 2.65
-3 8 17 8.62 3.28
1 6 -25 8.65 3.95
-1 -6 25 6.27 4.15
19 6 5 0.08 2.84
-19 -6 -5 -0.04 1.79
-19 6 -5 1.08 1.67
19 -6 5 -0.06 1.27
-4 -6 26 1.99 2.10
4 6 -26 5.10 3.13
0 8 -16 1.47 1.60
0 8 -16 3.98 2.82
0 -8 16 1.10 2.73
0 8 16 3.14 2.42
12 8 4 8.10 4.15
-12 8 -4 8.02 3.00
-12 -8 -4 7.98 4.81
12 -8 4 4.57 2.73
-9 0 35 2.84 2.16
9 0 -35 -0.04 1.00
-22 0 32 2.10 2.81
6 -9 -1 3.75 2.50
-6 -9 1 6.66 2.93
-6 -9 1 1.84 3.34
6 9 -1 3.82 2.40
-6 9 1 5.35 3.04
-21 -6 19 26.79 6.67
-21 -6 19 19.11 6.68
21 6 -19 31.51 8.19
21 -6 -19 22.56 10.51
-21 6 19 24.63 6.30
-21 -4 -9 45.25 10.81
21 4 9 40.78 10.02
-21 4 -9 24.74 13.43
-18 -5 -11 7.83 3.48
18 5 11 4.07 2.91
-18 5 -11 2.46 1.82
-14 -3 33 1.16 2.05
14 3 -33 1.53 1.36
-26 0 28 6.87 2.79
-4 9 7 4.74 2.67
-4 -9 7 7.94 3.11
4 -9 -7 6.28 2.46
4 9 -7 3.59 2.22
4 9 -7 7.76 4.05
-17 -7 18 0.47 1.52
17 -7 -18 1.62 1.59
-17 -7 18 1.42 2.38
17 7 -18 1.25 2.19
-17 7 18 0.41 1.32
-7 8 -11 25.36 10.39
-7 8 -11 27.06 6.51
7 -8 11 42.63 10.33
7 8 11 33.56 8.11
-7 -8 -11 28.11 15.17
-27 1 26 2.60 2.33
-27 -1 26 0.90 1.16
-20 1 -15 0.30 1.71
-20 -1 -15 1.14 2.13
-20 1 -15 0.96 1.56
-20 -1 -15 2.01 1.88
14 7 -21 18.49 5.58
-14 -7 21 19.35 5.71
-14 7 21 14.16 8.28
14 -7 -21 18.07 6.66
-6 8 -12 11.10 5.44
6 -8 12 12.35 6.27
-6 8 -12 10.03 2.81
-6 -8 -12 9.94 4.72
-20 1 33 15.37 4.91
-20 -1 33 22.39 6.34
-30 0 16 6.43 3.69
-30 0 16 3.61 5.16
-14 -5 29 4.46 3.76
-14 5 29 4.28 2.16
14 5 -29 4.17 2.40
-5 -4 31 10.27 3.55
5 4 -31 18.41 5.80
-5 -9 -2 11.17 10.25
5 9 2 8.12 5.12
5 -9 2 17.54 5.28
-5 9 -2 9.62 6.31
-5 -9 -2 13.57 4.04
6 -9 -5 4.06 2.47
6 9 -5 2.82 2.70
-6 9 5 1.21 2.28
-6 -9 5 2.63 2.16
-5 2 -29 1.95 2.50
-5 -2 -29 0.99 1.72
-26 -4 20 0.30 1.39
-26 -4 20 1.10 1.60
26 4 -20 3.13 2.24
-26 4 20 0.95 1.14
-26 4 20 2.16 3.10
4 0 -34 2.59 1.73
-8 -8 -10 45.45 22.77
8 -8 10 65.79 14.43
-8 8 -10 40.42 16.45
8 8 10 52.85 12.02
-5 3 -28 2.47 2.90
-5 -3 -28 1.03 1.44
-18 -4 30 3.22 2.71
-18 4 30 0.67 1.29
18 4 -30 1.44 1.72
27 4 -15 0.00 0.98
-27 4 15 0.71 1.90
-27 4 15 3.28 2.39
-28 -3 7 3.17 2.40
28 3 -7 2.33 2.12
-28 3 7 3.65 2.07
-28 3 7 4.62 2.29
12 1 -35 3.36 2.07
-12 1 35 3.76 2.29
-16 -7 -5 1.45 1.84
16 7 5 1.31 1.99
-16 7 -5 2.41 2.24
16 -7 5 0.72 1.75
0 -9 7 10.04 4.00
0 9 -7 11.81 4.65
0 9 7 10.75 5.33
0 -9 -7 7.78 3.71
-3 0 -31 1.66 1.59
14 8 -12 10.13 3.79
-14 -8 12 12.24 6.77
-14 -8 12 8.89 3.44
-14 8 12 10.71 3.05
14 -8 -12 10.42 3.50
13 7 10 5.06 2.66
-13 -7 -10 2.81 2.51
-13 7 -10 1.81 1.59
13 -7 10 0.60 1.29
-25 -3 26 1.24 1.61
-25 3 26 0.04 1.62
5 -8 13 2.67 2.04
-5 8 -13 4.25 3.04
-5 -8 -13 7.68 3.81
5 8 13 7.00 3.10
27 -4 -9 3.88 1.70
-27 -4 9 1.58 2.14
27 4 -9 1.29 1.43
-27 4 9 0.48 1.29
-9 0 -27 0.27 1.64
-27 -3 22 2.39 2.24
-27 3 22 0.60 1.43
-27 3 22 2.28 2.12
-9 -8 17 1.35 1.98
9 -8 -17 2.15 1.77
9 8 -17 2.41 2.03
9 8 -17 3.18 2.80
-9 8 17 1.13 1.57
-18 0 -18 14.18 7.71
-15 -8 7 14.19 6.09
15 8 -7 12.60 4.84
15 -8 -7 19.84 7.19
-15 8 7 13.38 4.78
-6 1 -29 2.91 2.40
-6 -1 -29 2.53 2.29
-10 1 35 3.45 1.94
10 1 -35 2.85 2.06
19 7 -14 3.30 3.24
-19 -7 14 4.10 2.16
-19 -7 14 2.79 2.49
19 -7 -14 3.05 2.54
-19 7 14 3.21 2.21
-28 -1 1 -0.31 1.68
-28 1 1 0.50 1.51
28 1 -1 1.79 2.32
-15 0 35 1.69 2.35
26 3 1 15.68 5.66
-26 3 -1 6.81 3.76
-26 -3 -1 7.66 5.06
-30 0 10 2.06 2.55
-8 -7 23 45.63 11.20
8 7 -23 32.92 8.27
1 0 -33 1.60 2.24
-9 8 -9 20.61 6.07
9 -8 9 16.38 10.16
9 8 9 17.11 4.84
-9 -8 -9 17.27 9.22
-4 7 -19 -0.16 1.38
4 -7 19 1.34 2.27
4 7 19 3.61 2.19
-4 -7 -19 0.75 1.47
-25 0 -7 2.90 2.39
-30 1 13 17.68 4.92
-30 -1 13 22.10 5.67
-30 1 13 15.61 4.45
-15 8 5 17.38 5.55
15 8 -5 20.63 6.56
-15 -8 5 16.19 6.44
15 -8 -5 17.85 9.57
17 6 9 3.65 3.03
-17 -6 -9 4.77 2.86
17 -6 9 4.17 2.61
-17 6 -9 2.77 2.11
-27 -1 -2 4.86 2.75
27 1 2 2.00 1.89
-27 1 -2 3.10 1.81
-20 -3 -13 11.29 7.69
-20 3 -13 9.77 4.71
20 3 13 18.72 5.84
-20 3 -13 8.96 6.27
25 5 -16 3.08 2.31
-25 -5 16 0.18 0.98
-25 -5 16 0.95 1.51
-25 5 16 1.79 1.50
25 -5 -16 1.40 1.12
3 -3 -32 1.24 1.54
3 3 -32 0.33 1.49
-3 -3 32 0.39 1.21
-17 -5 28 1.62 2.67
17 5 -28 1.88 1.63
-17 5 28 1.72 1.71
3 2 -33 1.70 2.22
3 -2 -33 2.54 1.96
-20 -3 31 4.58 3.19
20 3 -31 1.58 1.41
-3 -9 8 1.31 2.55
3 -9 -8 1.22 2.11
3 9 -8 0.48 1.43
-3 9 8 2.03 2.97
3 9 -8 2.39 2.70
-30 -1 15 0.19 1.33
-30 1 15 -0.03 1.22
23 5 -22 2.94 2.22
-23 -5 22 2.24 2.19
-23 5 22 1.53 2.16
-21 -5 -6 6.20 3.56
21 -5 6 2.20 2.37
21 5 6 2.81 3.97
-21 5 -6 3.43 1.79
-6 9 -1 6.75 3.80
-6 -9 -1 15.41 7.73
-6 -9 -1 6.81 3.53
6 -9 1 18.02 5.25
-15 -8 9 0.80 1.49
-15 -8 9 1.17 1.48
-15 8 9 2.18 3.08
15 -8 -9 3.81 2.42
-6 -7 23 4.32 3.59
6 7 -23 0.23 1.74
-27 -3 2 2.75 2.55
-27 3 2 1.21 2.09
-14 -8 0 2.79 1.99
-14 8 0 5.95 2.97
14 -8 0 4.85 3.23
-4 8 -14 0.82 1.38
-4 8 -14 2.49 2.47
-4 -8 -14 0.53 1.45
-23 -6 11 10.65 3.42
23 -6 -11 8.76 3.39
-18 -4 -14 1.85 1.66
-23 -3 -8 15.60 5.07
23 3 8 11.70 5.66
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT2018 (Sheldrick, 2015a)'
;
_shelx_hkl_checksum 49983
_shelx_res_file
;
TITL shelx_trans_a.res in I2/a
shelx_trans.res
created by SHELXL-2018/3 at 15:12:22 on 20-Oct-2020
REM Old TITL RNR-2A
REM SHELXT solution in I2/a: R1 0.183, Rweak 0.379, Alpha 0.036
REM 0.999 for 354 systematic absences, Orientation as input
REM Formula found by SHELXT: C13 F6 O7
CELL 0.71075 23.3083 7.1321 27.2533 90 112.621 90
ZERR 8 0.0098 0.0027 0.0088 0 0.027 0
LATT 2
SYMM 0.5-X,+Y,-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 0.058200 0.539300
FVAR 0.25881
F6 3 -0.595381 -0.863401 -0.252295 11.00000 0.05313 0.03378 =
0.06321 -0.00358 0.03588 0.00337
F3 3 -0.699609 -0.656244 -0.394735 11.00000 0.04465 0.02920 =
0.07651 0.00054 0.00092 0.00441
F5 3 -0.736575 -1.008922 -0.174736 11.00000 0.06884 0.04198 =
0.07206 0.01022 0.04324 -0.00539
O1 4 -0.654447 -0.323404 -0.378652 11.00000 0.02926 0.03131 =
0.04017 -0.00861 0.00934 0.00004
O3 4 -0.597196 -0.510446 -0.280896 11.00000 0.04553 0.03615 =
0.03833 -0.00401 0.01977 -0.01096
F4 3 -0.679056 -0.385948 -0.180566 11.00000 0.10006 0.02978 =
0.09940 -0.00532 0.07375 0.00339
O4 4 -0.580175 -0.326473 -0.209717 11.00000 0.05953 0.03579 =
0.05123 -0.01204 0.02717 -0.01394
F2 3 -0.893139 -0.744036 -0.530195 11.00000 0.05968 0.06568 =
0.06981 -0.02062 0.00517 -0.02730
O2 4 -0.725124 -0.101410 -0.384621 11.00000 0.04157 0.03325 =
0.07468 -0.01365 0.01189 0.00546
F1 3 -0.823408 -0.138329 -0.479049 11.00000 0.06512 0.03393 =
0.11460 0.01936 -0.02141 -0.00129
C18 1 -0.601162 -0.467226 -0.234449 11.00000 0.03266 0.02991 =
0.03731 -0.00169 0.01279 0.00054
C11 1 -0.711935 -0.252808 -0.396752 11.00000 0.03362 0.02668 =
0.04124 0.00100 0.01471 0.00044
C19 1 -0.635208 -0.614329 -0.217844 11.00000 0.03236 0.02927 =
0.03479 0.00082 0.01204 0.00062
C12 1 -0.757729 -0.385786 -0.433689 11.00000 0.03305 0.02990 =
0.03587 0.00094 0.01389 -0.00326
C2 1 -0.563963 -0.381048 -0.301942 11.00000 0.03327 0.03106 =
0.03569 -0.00002 0.01247 -0.00598
AFIX 13
H2 2 -0.528538 -0.323624 -0.271892 11.00000 -1.20000
AFIX 0
C4 1 -0.514102 -0.379767 -0.368769 11.00000 0.02937 0.03901 =
0.03245 0.00153 0.00812 0.00112
C24 1 -0.632883 -0.805303 -0.227983 11.00000 0.03276 0.03281 =
0.03602 -0.00158 0.01483 0.00319
C1 1 -0.606872 -0.227518 -0.334424 11.00000 0.03216 0.02898 =
0.03842 -0.00906 0.01165 -0.00350
AFIX 13
H1 2 -0.626082 -0.159152 -0.312525 11.00000 -1.20000
AFIX 0
C3 1 -0.538963 -0.498497 -0.335580 11.00000 0.03542 0.03041 =
0.04100 0.00301 0.01421 0.00396
AFIX 23
H3A 2 -0.505325 -0.580416 -0.312073 11.00000 -1.20000
H3B 2 -0.572576 -0.580005 -0.359305 11.00000 -1.20000
AFIX 0
C5 1 -0.529625 -0.189952 -0.378659 11.00000 0.03139 0.03738 =
0.03683 0.00262 0.00834 -0.00205
C17 1 -0.751121 -0.579722 -0.430764 11.00000 0.03630 0.03265 =
0.04118 -0.00159 0.01368 -0.00066
C6 1 -0.570574 -0.092773 -0.354791 11.00000 0.03779 0.02864 =
0.04726 0.00004 0.01343 -0.00227
AFIX 23
H6A 2 -0.600234 -0.010341 -0.382039 11.00000 -1.20000
H6B 2 -0.544278 -0.012360 -0.325027 11.00000 -1.20000
AFIX 0
C20 1 -0.673210 -0.567492 -0.190761 11.00000 0.04964 0.02776 =
0.04578 0.00011 0.02334 0.00479
C22 1 -0.702684 -0.879754 -0.188043 11.00000 0.04058 0.03595 =
0.04130 0.00961 0.01683 -0.00121
C23 1 -0.665413 -0.939922 -0.213395 11.00000 0.04414 0.02845 =
0.04466 0.00110 0.01827 -0.00037
AFIX 43
H23 2 -0.662217 -1.069007 -0.220563 11.00000 -1.20000
AFIX 0
C21 1 -0.707778 -0.695193 -0.175806 11.00000 0.04794 0.03847 =
0.04580 0.00551 0.02630 0.00641
AFIX 43
H21 2 -0.733785 -0.657632 -0.157963 11.00000 -1.20000
AFIX 0
C13 1 -0.813664 -0.322749 -0.472036 11.00000 0.04110 0.03308 =
0.05162 0.00861 0.00981 -0.00386
C7 1 -0.476075 -0.463175 -0.391671 11.00000 0.04050 0.05241 =
0.04352 0.00290 0.01701 0.00816
AFIX 43
H7 2 -0.465397 -0.591903 -0.385128 11.00000 -1.20000
AFIX 0
C15 1 -0.848872 -0.626419 -0.498600 11.00000 0.04373 0.04899 =
0.04196 -0.01013 0.01411 -0.01765
C16 1 -0.795802 -0.702132 -0.462187 11.00000 0.04906 0.03390 =
0.05731 -0.01005 0.01692 -0.00722
AFIX 43
H16 2 -0.789935 -0.834012 -0.458670 11.00000 -1.20000
AFIX 0
C10 1 -0.506511 -0.089226 -0.410961 11.00000 0.04226 0.05091 =
0.04875 0.01388 0.01453 -0.00100
AFIX 43
H10 2 -0.516759 0.039693 -0.417708 11.00000 -1.20000
AFIX 0
C14 1 -0.859539 -0.438574 -0.504939 11.00000 0.03950 0.05252 =
0.04254 0.00591 0.00607 -0.00867
AFIX 43
H14 2 -0.896844 -0.389864 -0.530823 11.00000 -1.20000
AFIX 0
C9 1 -0.469041 -0.173513 -0.433274 11.00000 0.05464 0.08074 =
0.05540 0.02086 0.02941 0.00172
AFIX 43
H9 2 -0.453709 -0.102928 -0.455201 11.00000 -1.20000
AFIX 0
C8 1 -0.453842 -0.361308 -0.423617 11.00000 0.04964 0.08094 =
0.05373 0.00840 0.02944 0.00992
AFIX 43
H8 2 -0.428125 -0.419917 -0.438983 11.00000 -1.20000
AFIX 0
HKLF 4
REM shelx_trans_a.res in I2/a
REM wR2 = 0.1234, GooF = S = 1.134, Restrained GooF = 1.134 for all data
REM R1 = 0.0464 for 3880 Fo > 4sig(Fo) and 0.0620 for all 4763 data
REM 307 parameters refined using 0 restraints
END
WGHT 0.0582 0.5393
REM Highest difference peak 0.220, deepest hole -0.218, 1-sigma level 0.038
Q1 1 -0.8207 -0.1308 -0.4383 11.00000 0.05 0.22
Q2 1 -0.6338 -0.6989 -0.2234 11.00000 0.05 0.18
Q3 1 -0.8419 -0.3775 -0.4823 11.00000 0.05 0.16
Q4 1 -0.7981 -0.1542 -0.4804 11.00000 0.05 0.16
Q5 1 -0.5263 -0.2944 -0.3759 11.00000 0.05 0.14
;
_shelx_res_checksum 32059
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -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
F F6 -0.59538(4) -0.86340(12) -0.25229(4) 0.0460(3) Uani d 1 . .
F F3 -0.69961(5) -0.65624(13) -0.39473(4) 0.0569(3) Uani d 1 . .
F F5 -0.73657(5) -1.00892(14) -0.17474(4) 0.0561(3) Uani d 1 . .
O O1 -0.65445(5) -0.32340(14) -0.37865(4) 0.0348(3) Uani d 1 . .
O O3 -0.59720(5) -0.51045(15) -0.28090(4) 0.0389(3) Uani d 1 . .
F F4 -0.67906(6) -0.38595(14) -0.18057(5) 0.0658(3) Uani d 1 . .
O O4 -0.58017(6) -0.32647(15) -0.20972(5) 0.0471(3) Uani d 1 . .
F F2 -0.89314(5) -0.74404(17) -0.53019(5) 0.0710(4) Uani d 1 . .
O O2 -0.72512(5) -0.10141(16) -0.38462(5) 0.0530(3) Uani d 1 . .
F F1 -0.82341(6) -0.13833(14) -0.47905(6) 0.0881(5) Uani d 1 . .
C C18 -0.60116(7) -0.4672(2) -0.23445(6) 0.0335(3) Uani d 1 . .
C C11 -0.71193(7) -0.2528(2) -0.39675(6) 0.0338(3) Uani d 1 . .
C C19 -0.63521(7) -0.6143(2) -0.21784(6) 0.0324(3) Uani d 1 . .
C C12 -0.75773(7) -0.3858(2) -0.43369(6) 0.0327(3) Uani d 1 . .
C C2 -0.56396(7) -0.3810(2) -0.30194(6) 0.0336(3) Uani d 1 . .
H H2 -0.528538 -0.323624 -0.271892 0.040 Uiso calc 1 . .
C C4 -0.51410(7) -0.3798(2) -0.36877(6) 0.0347(3) Uani d 1 . .
C C24 -0.63288(7) -0.8053(2) -0.22798(6) 0.0334(3) Uani d 1 . .
C C1 -0.60687(7) -0.2275(2) -0.33442(6) 0.0338(3) Uani d 1 . .
H H1 -0.626082 -0.159152 -0.312525 0.041 Uiso calc 1 . .
C C3 -0.53896(7) -0.4985(2) -0.33558(6) 0.0358(3) Uani d 1 . .
H H3A -0.505325 -0.580416 -0.312073 0.043 Uiso calc 1 . .
H H3B -0.572576 -0.580005 -0.359305 0.043 Uiso calc 1 . .
C C5 -0.52963(7) -0.1900(2) -0.37866(6) 0.0366(4) Uani d 1 . .
C C17 -0.75112(7) -0.5797(2) -0.43076(6) 0.0371(4) Uani d 1 . .
C C6 -0.57057(7) -0.0928(2) -0.35479(7) 0.0388(4) Uani d 1 . .
H H6A -0.600234 -0.010341 -0.382039 0.047 Uiso calc 1 . .
H H6B -0.544278 -0.012360 -0.325027 0.047 Uiso calc 1 . .
C C20 -0.67321(8) -0.5675(2) -0.19076(6) 0.0396(4) Uani d 1 . .
C C22 -0.70268(7) -0.8798(2) -0.18804(6) 0.0389(4) Uani d 1 . .
C C23 -0.66541(7) -0.9399(2) -0.21340(6) 0.0387(4) Uani d 1 . .
H H23 -0.662217 -1.069007 -0.220563 0.046 Uiso calc 1 . .
C C21 -0.70778(8) -0.6952(2) -0.17581(7) 0.0416(4) Uani d 1 . .
H H21 -0.733785 -0.657632 -0.157963 0.050 Uiso calc 1 . .
C C13 -0.81366(8) -0.3227(2) -0.47204(7) 0.0443(4) Uani d 1 . .
C C7 -0.47607(8) -0.4632(3) -0.39167(7) 0.0452(4) Uani d 1 . .
H H7 -0.465397 -0.591903 -0.385128 0.054 Uiso calc 1 . .
C C15 -0.84887(8) -0.6264(2) -0.49860(7) 0.0456(4) Uani d 1 . .
C C16 -0.79580(8) -0.7021(2) -0.46219(7) 0.0478(4) Uani d 1 . .
H H16 -0.789935 -0.834012 -0.458670 0.057 Uiso calc 1 . .
C C10 -0.50651(8) -0.0892(3) -0.41096(7) 0.0482(4) Uani d 1 . .
H H10 -0.516759 0.039693 -0.417708 0.058 Uiso calc 1 . .
C C14 -0.85954(8) -0.4386(3) -0.50494(7) 0.0478(4) Uani d 1 . .
H H14 -0.896844 -0.389864 -0.530823 0.057 Uiso calc 1 . .
C C9 -0.46904(9) -0.1735(3) -0.43327(8) 0.0611(5) Uani d 1 . .
H H9 -0.453709 -0.102928 -0.455201 0.073 Uiso calc 1 . .
C C8 -0.45384(9) -0.3613(3) -0.42362(8) 0.0586(5) Uani d 1 . .
H H8 -0.428125 -0.419917 -0.438983 0.070 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
F6 0.0531(6) 0.0338(5) 0.0632(6) 0.0034(4) 0.0359(5) -0.0036(4)
F3 0.0447(6) 0.0292(5) 0.0765(8) 0.0044(4) 0.0009(5) 0.0005(5)
F5 0.0688(7) 0.0420(6) 0.0721(7) -0.0054(5) 0.0432(6) 0.0102(5)
O1 0.0293(5) 0.0313(5) 0.0402(6) 0.0000(4) 0.0093(5) -0.0086(4)
O3 0.0455(6) 0.0362(6) 0.0383(6) -0.0110(5) 0.0198(5) -0.0040(5)
F4 0.1001(9) 0.0298(5) 0.0994(9) 0.0034(5) 0.0737(8) -0.0053(5)
O4 0.0595(7) 0.0358(6) 0.0512(7) -0.0139(5) 0.0272(6) -0.0120(5)
F2 0.0597(7) 0.0657(8) 0.0698(8) -0.0273(6) 0.0052(6) -0.0206(6)
O2 0.0416(7) 0.0333(6) 0.0747(9) 0.0055(5) 0.0119(6) -0.0136(6)
F1 0.0651(8) 0.0339(6) 0.1146(11) -0.0013(5) -0.0214(7) 0.0194(6)
C18 0.0327(8) 0.0299(7) 0.0373(8) 0.0005(6) 0.0128(6) -0.0017(6)
C11 0.0336(8) 0.0267(7) 0.0412(9) 0.0004(6) 0.0147(7) 0.0010(6)
C19 0.0324(7) 0.0293(7) 0.0348(8) 0.0006(6) 0.0120(6) 0.0008(6)
C12 0.0330(7) 0.0299(7) 0.0359(8) -0.0033(6) 0.0139(6) 0.0009(6)
C2 0.0333(8) 0.0311(7) 0.0357(8) -0.0060(6) 0.0125(7) 0.0000(6)
C4 0.0294(7) 0.0390(8) 0.0325(8) 0.0011(6) 0.0081(6) 0.0015(6)
C24 0.0328(8) 0.0328(8) 0.0360(8) 0.0032(6) 0.0148(7) -0.0016(6)
C1 0.0322(7) 0.0290(7) 0.0384(8) -0.0035(6) 0.0116(7) -0.0091(6)
C3 0.0354(8) 0.0304(8) 0.0410(9) 0.0040(6) 0.0142(7) 0.0030(6)
C5 0.0314(8) 0.0374(8) 0.0368(9) -0.0021(6) 0.0083(7) 0.0026(6)
C17 0.0363(8) 0.0326(8) 0.0412(9) -0.0007(6) 0.0137(7) -0.0016(7)
C6 0.0378(8) 0.0286(7) 0.0473(9) -0.0023(6) 0.0134(7) 0.0000(7)
C20 0.0496(9) 0.0278(8) 0.0458(9) 0.0048(6) 0.0233(8) 0.0001(7)
C22 0.0406(9) 0.0359(8) 0.0413(9) -0.0012(7) 0.0168(7) 0.0096(7)
C23 0.0441(9) 0.0285(7) 0.0447(9) -0.0004(6) 0.0183(8) 0.0011(7)
C21 0.0479(9) 0.0385(9) 0.0458(10) 0.0064(7) 0.0263(8) 0.0055(7)
C13 0.0411(9) 0.0331(8) 0.0516(10) -0.0039(7) 0.0098(8) 0.0086(7)
C7 0.0405(9) 0.0524(10) 0.0435(10) 0.0082(7) 0.0170(8) 0.0029(8)
C15 0.0437(10) 0.0490(10) 0.0420(10) -0.0177(8) 0.0141(8) -0.0101(8)
C16 0.0491(10) 0.0339(8) 0.0573(11) -0.0072(7) 0.0169(9) -0.0100(8)
C10 0.0423(9) 0.0509(10) 0.0487(10) -0.0010(8) 0.0145(8) 0.0139(8)
C14 0.0395(9) 0.0525(10) 0.0425(10) -0.0087(8) 0.0061(8) 0.0059(8)
C9 0.0546(11) 0.0807(15) 0.0554(12) 0.0017(10) 0.0294(10) 0.0209(11)
C8 0.0496(11) 0.0809(15) 0.0537(12) 0.0099(10) 0.0294(10) 0.0084(10)
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 . . 117.70(11) ?
C18 O3 C2 . . 117.80(11) ?
O3 C18 C19 . . 111.34(12) ?
O4 C18 O3 . . 124.07(14) ?
O4 C18 C19 . . 124.59(14) ?
O1 C11 C12 . . 111.43(12) ?
O2 C11 O1 . . 124.25(14) ?
O2 C11 C12 . . 124.32(14) ?
C24 C19 C18 . . 124.24(13) ?
C20 C19 C18 . . 120.94(13) ?
C20 C19 C24 . . 114.82(14) ?
C17 C12 C11 . . 123.98(14) ?
C17 C12 C13 . . 114.49(14) ?
C13 C12 C11 . . 121.37(14) ?
O3 C2 H2 . . 109.5 ?
O3 C2 C1 . . 110.85(12) ?
O3 C2 C3 . . 105.94(11) ?
C1 C2 H2 . . 109.5 ?
C3 C2 H2 . . 109.5 ?
C3 C2 C1 . . 111.52(12) ?
C5 C4 C3 . . 121.86(14) ?
C7 C4 C3 . . 118.99(14) ?
C7 C4 C5 . . 119.12(15) ?
F6 C24 C19 . . 118.62(13) ?
F6 C24 C23 . . 117.48(13) ?
C23 C24 C19 . . 123.87(14) ?
O1 C1 C2 . . 105.38(11) ?
O1 C1 H1 . . 110.5 ?
O1 C1 C6 . . 110.38(12) ?
C2 C1 H1 . . 110.5 ?
C2 C1 C6 . . 109.57(12) ?
C6 C1 H1 . . 110.5 ?
C2 C3 H3A . . 109.2 ?
C2 C3 H3B . . 109.2 ?
C4 C3 C2 . . 112.25(12) ?
C4 C3 H3A . . 109.2 ?
C4 C3 H3B . . 109.2 ?
H3A C3 H3B . . 107.9 ?
C4 C5 C6 . . 121.25(14) ?
C10 C5 C4 . . 119.04(15) ?
C10 C5 C6 . . 119.72(15) ?
F3 C17 C12 . . 119.68(13) ?
F3 C17 C16 . . 116.60(14) ?
C16 C17 C12 . . 123.69(15) ?
C1 C6 H6A . . 108.9 ?
C1 C6 H6B . . 108.9 ?
C5 C6 C1 . . 113.52(13) ?
C5 C6 H6A . . 108.9 ?
C5 C6 H6B . . 108.9 ?
H6A C6 H6B . . 107.7 ?
F4 C20 C19 . . 118.46(14) ?
F4 C20 C21 . . 117.33(14) ?
C21 C20 C19 . . 124.14(15) ?
F5 C22 C23 . . 118.13(14) ?
F5 C22 C21 . . 118.30(14) ?
C23 C22 C21 . . 123.57(15) ?
C24 C23 H23 . . 121.5 ?
C22 C23 C24 . . 117.04(14) ?
C22 C23 H23 . . 121.5 ?
C20 C21 H21 . . 121.7 ?
C22 C21 C20 . . 116.52(15) ?
C22 C21 H21 . . 121.7 ?
F1 C13 C12 . . 118.88(14) ?
F1 C13 C14 . . 116.82(15) ?
C14 C13 C12 . . 124.26(16) ?
C4 C7 H7 . . 119.5 ?
C8 C7 C4 . . 120.96(17) ?
C8 C7 H7 . . 119.5 ?
F2 C15 C16 . . 118.30(16) ?
F2 C15 C14 . . 118.20(16) ?
C14 C15 C16 . . 123.50(16) ?
C17 C16 H16 . . 121.3 ?
C15 C16 C17 . . 117.31(16) ?
C15 C16 H16 . . 121.3 ?
C5 C10 H10 . . 119.4 ?
C9 C10 C5 . . 121.16(18) ?
C9 C10 H10 . . 119.4 ?
C13 C14 H14 . . 121.6 ?
C15 C14 C13 . . 116.74(16) ?
C15 C14 H14 . . 121.6 ?
C10 C9 H9 . . 120.1 ?
C10 C9 C8 . . 119.80(17) ?
C8 C9 H9 . . 120.1 ?
C7 C8 C9 . . 119.93(18) ?
C7 C8 H8 . . 120.0 ?
C9 C8 H8 . . 120.0 ?
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
F6 C24 . 1.3492(17) ?
F3 C17 . 1.3404(19) ?
F5 C22 . 1.3508(18) ?
O1 C11 . 1.3356(19) ?
O1 C1 . 1.4567(18) ?
O3 C18 . 1.3401(19) ?
O3 C2 . 1.4569(17) ?
F4 C20 . 1.3422(18) ?
O4 C18 . 1.2032(18) ?
F2 C15 . 1.3514(19) ?
O2 C11 . 1.2033(18) ?
F1 C13 . 1.3359(19) ?
C18 C19 . 1.487(2) ?
C11 C12 . 1.492(2) ?
C19 C24 . 1.395(2) ?
C19 C20 . 1.394(2) ?
C12 C17 . 1.391(2) ?
C12 C13 . 1.395(2) ?
C2 H2 . 1.0000 ?
C2 C1 . 1.517(2) ?
C2 C3 . 1.514(2) ?
C4 C3 . 1.508(2) ?
C4 C5 . 1.400(2) ?
C4 C7 . 1.398(2) ?
C24 C23 . 1.374(2) ?
C1 H1 . 1.0000 ?
C1 C6 . 1.519(2) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C5 C6 . 1.514(2) ?
C5 C10 . 1.395(2) ?
C17 C16 . 1.376(2) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C20 C21 . 1.377(2) ?
C22 C23 . 1.370(2) ?
C22 C21 . 1.374(2) ?
C23 H23 . 0.9500 ?
C21 H21 . 0.9500 ?
C13 C14 . 1.376(2) ?
C7 H7 . 0.9500 ?
C7 C8 . 1.379(3) ?
C15 C16 . 1.365(3) ?
C15 C14 . 1.361(3) ?
C16 H16 . 0.9500 ?
C10 H10 . 0.9500 ?
C10 C9 . 1.379(3) ?
C14 H14 . 0.9500 ?
C9 H9 . 0.9500 ?
C9 C8 . 1.385(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
F6 C24 C23 C22 . . . . 179.08(14) ?
F3 C17 C16 C15 . . . . 179.17(15) ?
F5 C22 C23 C24 . . . . 178.04(14) ?
F5 C22 C21 C20 . . . . -179.03(15) ?
O1 C11 C12 C17 . . . . 29.2(2) ?
O1 C11 C12 C13 . . . . -155.60(15) ?
O1 C1 C6 C5 . . . . -69.26(16) ?
O3 C18 C19 C24 . . . . 34.0(2) ?
O3 C18 C19 C20 . . . . -145.29(14) ?
O3 C2 C1 O1 . . . . -62.45(15) ?
O3 C2 C1 C6 . . . . 178.80(11) ?
O3 C2 C3 C4 . . . . 168.80(11) ?
F4 C20 C21 C22 . . . . 178.04(15) ?
O4 C18 C19 C24 . . . . -146.54(16) ?
O4 C18 C19 C20 . . . . 34.2(2) ?
F2 C15 C16 C17 . . . . 179.43(15) ?
F2 C15 C14 C13 . . . . 179.77(16) ?
O2 C11 C12 C17 . . . . -150.50(17) ?
O2 C11 C12 C13 . . . . 24.7(2) ?
F1 C13 C14 C15 . . . . 178.46(17) ?
C18 O3 C2 C1 . . . . -86.51(15) ?
C18 O3 C2 C3 . . . . 152.36(12) ?
C18 C19 C24 F6 . . . . 3.1(2) ?
C18 C19 C24 C23 . . . . -178.71(15) ?
C18 C19 C20 F4 . . . . 0.8(2) ?
C18 C19 C20 C21 . . . . 177.64(15) ?
C11 O1 C1 C2 . . . . 145.89(13) ?
C11 O1 C1 C6 . . . . -95.90(15) ?
C11 C12 C17 F3 . . . . -3.5(2) ?
C11 C12 C17 C16 . . . . 174.61(15) ?
C11 C12 C13 F1 . . . . 6.6(2) ?
C11 C12 C13 C14 . . . . -175.62(16) ?
C19 C24 C23 C22 . . . . 0.9(2) ?
C19 C20 C21 C22 . . . . 1.2(3) ?
C12 C17 C16 C15 . . . . 1.0(3) ?
C12 C13 C14 C15 . . . . 0.6(3) ?
C2 O3 C18 O4 . . . . 1.7(2) ?
C2 O3 C18 C19 . . . . -178.84(12) ?
C2 C1 C6 C5 . . . . 46.35(17) ?
C4 C5 C6 C1 . . . . -17.0(2) ?
C4 C5 C10 C9 . . . . 0.2(3) ?
C4 C7 C8 C9 . . . . 0.2(3) ?
C24 C19 C20 F4 . . . . -178.49(14) ?
C24 C19 C20 C21 . . . . -1.7(2) ?
C1 O1 C11 O2 . . . . 11.7(2) ?
C1 O1 C11 C12 . . . . -168.05(12) ?
C1 C2 C3 C4 . . . . 48.10(16) ?
C3 C2 C1 O1 . . . . 55.33(15) ?
C3 C2 C1 C6 . . . . -63.42(15) ?
C3 C4 C5 C6 . . . . 2.1(2) ?
C3 C4 C5 C10 . . . . -178.16(14) ?
C3 C4 C7 C8 . . . . 178.03(16) ?
C5 C4 C3 C2 . . . . -17.6(2) ?
C5 C4 C7 C8 . . . . 0.0(2) ?
C5 C10 C9 C8 . . . . 0.0(3) ?
C17 C12 C13 F1 . . . . -177.79(16) ?
C17 C12 C13 C14 . . . . 0.0(3) ?
C6 C5 C10 C9 . . . . 179.94(16) ?
C20 C19 C24 F6 . . . . -177.58(13) ?
C20 C19 C24 C23 . . . . 0.6(2) ?
C23 C22 C21 C20 . . . . 0.5(3) ?
C21 C22 C23 C24 . . . . -1.5(2) ?
C13 C12 C17 F3 . . . . -178.94(14) ?
C13 C12 C17 C16 . . . . -0.9(2) ?
C7 C4 C3 C2 . . . . 164.44(14) ?
C7 C4 C5 C6 . . . . -179.92(14) ?
C7 C4 C5 C10 . . . . -0.2(2) ?
C16 C15 C14 C13 . . . . -0.5(3) ?
C10 C5 C6 C1 . . . . 163.33(14) ?
C10 C9 C8 C7 . . . . -0.1(3) ?
C14 C15 C16 C17 . . . . -0.3(3) ?
_cod_database_fobs_code 2022282