#------------------------------------------------------------------------------
#$Date: 2024-08-07 01:02:56 +0300 (Wed, 07 Aug 2024) $
#$Revision: 293983 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/25/2312522.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_2312522
loop_
_publ_author_name
'Pickl, Thomas'
'Zuber, Julian'
'Stephan, Johannes'
'Pöthig, Alexander'
_publ_section_title
;
Crystal structure elucidation of a geminal and vicinal
bis(trifluoromethanesulfonate) ester.
;
_journal_coeditor_code OJ3019
_journal_issue 'Pt 7'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first 278
_journal_page_last 283
_journal_paper_doi 10.1107/S2053229624005230
_journal_volume 80
_journal_year 2024
_chemical_absolute_configuration unk
_chemical_formula_iupac 'C3 H2 F6 O6 S2'
_chemical_formula_moiety 'C3 H2 F6 O6 S2'
_chemical_formula_sum 'C3 H2 F6 O6 S2'
_chemical_formula_weight 312.17
_chemical_melting_point 289
_chemical_name_common 'Methylene bis(triflate)'
_chemical_name_systematic
;
Methanediyl bis(trifluoromethanesulfonate)
;
_space_group_crystal_system monoclinic
_space_group_IT_number 4
_space_group_name_Hall 'P 2yb'
_space_group_name_H-M_alt 'P 1 21 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90
_cell_angle_beta 102.406(5)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 8.9822(12)
_cell_length_b 4.9413(6)
_cell_length_c 10.9400(14)
_cell_measurement_reflns_used 5142
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.242
_cell_measurement_theta_min 2.325
_cell_volume 474.22(11)
_computing_cell_refinement
;
SAINT (Bruker, 2019)
;
_computing_data_collection
;
APEX4 (Bruker, 2022)
;
_computing_data_reduction
;
SAINT (Bruker, 2019)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020)
;
_computing_publication_material
;
PLATON (Spek, 2020), enCIFer (Allen et al., 2004) and
FinalCif (Kratzert, 2023)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b) and ShelXle (H\"ubschle et al.,
2011)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector CPAD
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device 'three-angle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 VENTURE'
_diffrn_measurement_method '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator 'Helios optic'
_diffrn_radiation_probe x-ray
_diffrn_radiation_source 'TXS rotating anode'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0438
_diffrn_reflns_av_unetI/netI 0.0283
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 2295
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.290
_diffrn_reflns_theta_min 2.322
_diffrn_source 'TXS rotating anode'
_diffrn_source_current 50.0
_diffrn_source_voltage 50.0
_exptl_absorpt_coefficient_mu 0.676
_exptl_absorpt_correction_T_max 0.745686
_exptl_absorpt_correction_T_min 0.54003
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(TWINABS; Bruker, 2012)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 2.186
_exptl_crystal_description plate
_exptl_crystal_F_000 308
_exptl_crystal_size_max 0.349
_exptl_crystal_size_mid 0.320
_exptl_crystal_size_min 0.062
_refine_diff_density_max 0.410
_refine_diff_density_min -0.470
_refine_ls_abs_structure_details
;
Flack x determined using 959 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.12(4)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.054
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 155
_refine_ls_number_reflns 2295
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.053
_refine_ls_R_factor_all 0.0289
_refine_ls_R_factor_gt 0.0271
_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^)+(0.0318P)^2^+0.3843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0690
_refine_ls_wR_factor_ref 0.0719
_reflns_number_gt 2254
_reflns_number_total 2295
_reflns_threshold_expression 'I > 2\s(I)'
_twin_individual_id 2
_twin_individual_twin_matrix_11 0.00348
_twin_individual_twin_matrix_12 -0.0005
_twin_individual_twin_matrix_13 -1.00013
_twin_individual_twin_matrix_21 -1.0
_twin_individual_twin_matrix_22 0.00071
_twin_individual_twin_matrix_23 -0.00087
_twin_individual_twin_matrix_31 0.00242
_twin_individual_twin_matrix_32 1.00013
_twin_individual_twin_matrix_33 0.52089
_iucr_refine_instructions_details
;
TITL PicTh28_0m_4_a.res in P2(1)
PicTh28_fine.res
created by SHELXL-2019/2 at 11:36:10 on 11-Aug-2023
CELL 0.71073 8.9822 4.9413 10.9400 90.000 102.406 90.000
ZERR 2.00 0.0012 0.0006 0.0014 0.000 0.005 0.000
LATT -1
SYMM -x, y+1/2, -z
SFAC C H O F S
UNIT 6 4 12 12 4
OMIT -1 4 10 ! affected by cryo stream shadow
OMIT 3 4 9 ! affected by cryo stream shadow
OMIT 9 3 4 ! affected by cryo stream shadow
OMIT 3 5 3 ! affected by cryo stream shadow
LIST 4
TEMP -173.150
SIZE 0.062 0.320 0.349
ACTA
L.S. 4
FMAP 2
PLAN -10
HTAB
BOND $H
CONF
WGHT 0.031800 0.384300
BASF 0.29332
FVAR 1.05585
S1 5 0.965948 0.489799 0.319721 11.00000 0.01122 0.02095 =
0.02018 -0.00237 0.00330 0.00073
S2 5 0.440528 0.478883 0.321702 11.00000 0.01147 0.01848 =
0.01861 0.00152 0.00380 0.00112
F1 4 0.789566 0.173884 0.161328 11.00000 0.02810 0.03591 =
0.03339 -0.01311 0.00852 -0.01311
F2 4 1.006931 0.257369 0.118308 11.00000 0.02788 0.05097 =
0.03449 -0.01508 0.01555 0.00121
F3 4 0.831785 0.563430 0.087971 11.00000 0.04356 0.03384 =
0.02180 0.00417 -0.00006 0.00168
F4 4 0.451390 0.448049 0.086786 11.00000 0.04542 0.04653 =
0.02058 -0.00417 0.00833 0.00849
F5 4 0.528734 0.826003 0.173763 11.00000 0.02858 0.03196 =
0.03356 0.01218 0.01028 -0.00484
F6 4 0.289600 0.733917 0.129337 11.00000 0.02208 0.04254 =
0.02892 0.01054 0.00081 0.00927
O1 3 0.816915 0.625839 0.344605 11.00000 0.01166 0.02138 =
0.02291 -0.00065 0.00656 0.00227
O2 3 1.008735 0.265946 0.399504 11.00000 0.02457 0.02687 =
0.02657 0.00467 0.00428 0.01077
O3 3 1.067926 0.701538 0.308972 11.00000 0.01879 0.03058 =
0.03306 -0.01066 0.01037 -0.00833
O4 3 0.605690 0.356211 0.343513 11.00000 0.01217 0.02202 =
0.02246 0.00205 0.00466 0.00082
O5 3 0.338110 0.259630 0.304714 11.00000 0.01401 0.02697 =
0.03634 0.00392 0.00361 -0.00207
O6 3 0.434515 0.691729 0.407011 11.00000 0.02119 0.02488 =
0.02277 0.00000 0.00492 0.00648
C1 1 0.730323 0.493218 0.423089 11.00000 0.01207 0.03873 =
0.01819 -0.00018 0.00356 -0.00469
AFIX 23
H1 2 0.795251 0.361855 0.478791 11.00000 -1.20000
H2 2 0.691600 0.627764 0.475688 11.00000 -1.20000
AFIX 0
C2 1 0.893222 0.361773 0.160892 11.00000 0.02103 0.02610 =
0.02205 -0.00536 0.00569 -0.00218
C3 1 0.426985 0.630924 0.166627 11.00000 0.02264 0.02754 =
0.01731 0.00385 0.00182 0.00270
HKLF 5 1 1 0 0 0 1 0 0 0 1
REM PicTh28_0m_4_a.res in P2(1)
REM wR2 = 0.0719, GooF = S = 1.054, Restrained GooF = 1.053 for all data
REM R1 = 0.0271 for 2254 Fo > 4sig(Fo) and 0.0289 for all 2295 data
REM 155 parameters refined using 1 restraints
END
WGHT 0.0318 0.3842
REM Instructions for potential hydrogen bonds
EQIV $1 -x+2, y-1/2, -z+1
HTAB C1 O3_$1
EQIV $2 -x+1, y+1/2, -z+1
HTAB C1 O5_$2
HTAB C1 O6
REM Highest difference peak 0.410, deepest hole -0.470, 1-sigma level 0.077
Q1 1 0.9319 0.4368 0.2392 11.00000 0.05 0.41
Q2 1 0.4400 0.5350 0.2277 11.00000 0.05 0.38
Q3 1 1.0190 0.4721 -0.0133 11.00000 0.05 0.31
Q4 1 1.0182 0.8052 0.1587 11.00000 0.05 0.28
Q5 1 0.4272 0.4832 0.0166 11.00000 0.05 0.28
Q6 1 0.3272 0.4709 -0.0240 11.00000 0.05 0.27
Q7 1 0.4763 0.4936 0.4088 11.00000 0.05 0.26
Q8 1 0.4900 0.4725 0.4700 11.00000 0.05 0.26
Q9 1 0.6769 0.6599 0.0202 11.00000 0.05 0.24
Q10 1 0.9321 0.4641 0.0206 11.00000 0.05 0.24
;
_cod_data_source_file oj3019.cif
_cod_data_source_block 1
_cod_depositor_comments
'Adding full bibliography for 2312521--2312522.cif.'
_cod_original_sg_symbol_H-M 'P 21'
_cod_database_code 2312522
_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 0.798
_shelx_estimated_absorpt_t_max 0.959
_shelx_hkl_file
;
1 0 0 37.7210 1.04674 1
-2 0 1 6150.10 244.815 -2
2 0 0 6150.10 244.815 1
3 0 0 18.1854 0.37909 1
-4 0 2 1349.78 46.0225 -2
4 0 0 1349.78 46.0225 1
5 0 0 969.901 25.7869 1
-6 0 3 51.7906 1.22892 -2
6 0 0 51.7906 1.22892 1
-7 0 4 758.357 19.1786 -2
7 0 0 758.357 19.1786 1
-8 0 4 772.063 12.8154 -2
8 0 0 772.063 12.8154 1
-9 0 5 102.978 2.48413 -2
9 0 0 102.978 2.48413 1
-10 0 5 91.4487 2.29101 -2
10 0 0 91.4487 2.29101 1
-11 0 6 53.5120 1.95187 -2
11 0 0 53.5120 1.95187 1
0 1 0 1.25108 0.33186 -2
0 -1 0 1.25108 0.33186 1
0 -1 0 0.51290 0.33282 -2
0 1 0 0.51290 0.33282 1
-1 -1 0 513.550 13.5279 1
1 1 0 542.663 21.9790 1
-2 1 1 2878.18 88.4458 -2
-2 -1 0 2878.18 88.4458 1
2 -1 -1 3018.70 122.051 -2
2 1 0 3018.70 122.051 1
-3 -1 0 499.447 13.4317 1
3 1 0 512.822 13.4734 1
-4 1 2 1610.13 68.7156 -2
-4 -1 0 1610.13 68.7156 1
4 -1 -2 1672.84 54.1565 -2
4 1 0 1672.84 54.1565 1
-5 -1 0 730.999 21.6846 1
5 1 0 756.297 25.7413 1
-6 1 3 1286.48 55.7057 -2
-6 -1 0 1286.48 55.7057 1
6 -1 -3 1298.40 56.3884 -2
6 1 0 1298.40 56.3884 1
-7 1 4 435.029 6.49192 -2
-7 -1 0 435.029 6.49192 1
7 -1 -4 444.434 6.78853 -2
7 1 0 444.434 6.78853 1
-8 1 4 693.501 11.1584 -2
-8 -1 0 693.501 11.1584 1
8 -1 -4 673.882 10.2317 -2
8 1 0 673.882 10.2317 1
-9 1 5 279.069 5.26103 -2
-9 -1 0 279.069 5.26103 1
9 -1 -5 283.310 5.62457 -2
9 1 0 283.310 5.62457 1
-10 1 5 16.9839 1.26129 -2
-10 -1 0 16.9839 1.26129 1
10 -1 -5 16.3179 1.05638 -2
10 1 0 16.3179 1.05638 1
-11 1 6 244.262 7.97348 -2
-11 -1 0 244.262 7.97348 1
11 -1 -6 244.473 5.76451 -2
11 1 0 244.473 5.76451 1
0 2 0 241.228 7.82553 -2
0 -2 0 241.228 7.82553 1
0 -2 0 236.634 11.2376 -2
0 2 0 236.634 11.2376 1
-1 -2 0 481.964 39.9668 1
1 2 0 479.284 20.4712 1
-2 2 1 1348.84 35.9670 -2
-2 -2 0 1348.84 35.9670 1
2 -2 -1 1252.57 32.3804 -2
2 2 0 1252.57 32.3804 1
-3 -2 0 729.264 16.8026 1
3 2 0 706.497 20.5295 1
-4 2 2 14.8057 0.48752 -2
-4 -2 0 14.8057 0.48752 1
4 -2 -2 16.1460 0.52863 -2
4 2 0 16.1460 0.52863 1
-5 2 3 209.536 9.76915 -2
-5 -2 0 209.536 9.76915 1
5 -2 -3 210.147 9.38577 -2
5 2 0 210.147 9.38577 1
-6 2 3 149.675 2.05517 -2
-6 -2 0 149.675 2.05517 1
6 -2 -3 144.169 2.44412 -2
6 2 0 144.169 2.44412 1
-7 2 4 123.590 3.31936 -2
-7 -2 0 123.590 3.31936 1
7 -2 -4 113.078 4.32938 -2
7 2 0 113.078 4.32938 1
-8 2 4 259.666 4.87192 -2
-8 -2 0 259.666 4.87192 1
8 -2 -4 256.764 4.44770 -2
8 2 0 256.764 4.44770 1
-9 2 5 19.8175 0.93527 -2
-9 -2 0 19.8175 0.93527 1
9 -2 -5 21.3618 0.85420 -2
9 2 0 21.3618 0.85420 1
-10 2 5 253.337 7.59757 -2
-10 -2 0 253.337 7.59757 1
10 -2 -5 263.845 6.50269 -2
10 2 0 263.845 6.50269 1
11 -2 -6 5.07807 2.91295 -2
11 2 0 5.07807 2.91295 1
0 3 0 0.11751 0.46091 -2
0 -3 0 0.11751 0.46091 1
0 -3 0 -0.1955 0.76158 -2
0 3 0 -0.1955 0.76158 1
-1 -3 0 215.725 3.40619 1
1 3 0 215.892 4.92194 1
-2 3 1 304.861 6.40427 -2
-2 -3 0 304.861 6.40427 1
2 -3 -1 303.062 8.08577 -2
2 3 0 303.062 8.08577 1
-3 3 2 107.570 6.34637 -2
-3 -3 0 107.570 6.34637 1
3 3 0 34.7517 1.00171 1
-4 3 2 741.974 18.9162 -2
-4 -3 0 741.974 18.9162 1
4 -3 -2 762.292 26.1420 -2
4 3 0 762.292 26.1420 1
-5 3 3 356.555 6.48566 -2
-5 -3 0 356.555 6.48566 1
5 -3 -3 323.862 10.7477 -2
5 3 0 323.862 10.7477 1
-6 3 3 410.584 6.12244 -2
-6 -3 0 410.584 6.12244 1
6 -3 -3 396.093 5.98395 -2
6 3 0 396.093 5.98395 1
-7 3 4 213.909 3.78017 -2
-7 -3 0 213.909 3.78017 1
7 -3 -4 212.225 6.97666 -2
7 3 0 212.225 6.97666 1
-8 3 4 128.136 2.57401 -2
-8 -3 0 128.136 2.57401 1
8 -3 -4 127.113 3.99432 -2
8 3 0 127.113 3.99432 1
-9 3 5 187.211 4.86336 -2
-9 -3 0 187.211 4.86336 1
9 -3 -5 195.280 6.97031 -2
9 3 0 195.280 6.97031 1
-10 3 5 53.5064 10.0513 -2
-10 -3 0 53.5064 10.0513 1
10 -3 -5 27.1638 2.38510 -2
10 3 0 27.1638 2.38510 1
-1 -4 0 77.3242 1.85498 1
1 4 0 76.4373 1.81030 1
-2 4 1 556.719 11.5677 -2
-2 -4 0 556.719 11.5677 1
2 -4 -1 563.424 11.3474 -2
2 4 0 563.424 11.3474 1
-3 4 2 538.300 29.5656 -2
-3 -4 0 538.300 29.5656 1
3 -4 -2 549.991 24.6506 -2
3 4 0 549.991 24.6506 1
-4 4 2 507.334 10.7306 -2
-4 -4 0 507.334 10.7306 1
4 -4 -2 520.385 11.6381 -2
4 4 0 520.385 11.6381 1
-5 4 3 16.6256 1.01395 -2
-5 -4 0 16.6256 1.01395 1
5 -4 -3 16.3185 1.36798 -2
5 4 0 16.3185 1.36798 1
-6 4 3 152.403 2.78367 -2
-6 -4 0 152.403 2.78367 1
6 -4 -3 141.957 3.27557 -2
6 4 0 141.957 3.27557 1
-7 4 4 155.718 4.41862 -2
-7 -4 0 155.718 4.41862 1
7 -4 -4 150.579 5.65044 -2
7 4 0 150.579 5.65044 1
-8 4 4 123.835 3.81685 -2
-8 -4 0 123.835 3.81685 1
8 -4 -4 111.575 4.47009 -2
8 4 0 111.575 4.47009 1
-9 4 5 53.7894 2.22352 -2
-9 -4 0 53.7894 2.22352 1
9 -4 -5 51.1602 3.05726 -2
9 4 0 51.1602 3.05726 1
0 5 0 -0.2377 1.10616 -2
0 -5 0 -0.2377 1.10616 1
0 -5 0 0.70109 1.09280 -2
0 5 0 0.70109 1.09280 1
-1 -5 0 116.178 2.63996 1
1 5 0 109.605 3.69250 1
-2 5 1 107.354 3.74944 -2
-2 -5 0 107.354 3.74944 1
2 -5 -1 99.3446 3.41202 -2
2 5 0 99.3446 3.41202 1
-3 5 2 177.061 9.49784 -2
-3 -5 0 177.061 9.49784 1
3 5 0 109.972 6.47019 1
-4 5 2 388.188 9.82033 -2
-4 -5 0 388.188 9.82033 1
4 -5 -2 394.318 13.8445 -2
4 5 0 394.318 13.8445 1
-5 5 3 5.67309 0.85045 -2
-5 -5 0 5.67309 0.85045 1
5 -5 -3 7.10600 2.59109 -2
5 5 0 7.10600 2.59109 1
-6 5 3 136.488 4.07182 -2
-6 -5 0 136.488 4.07182 1
-7 5 4 8.00490 1.15710 -2
-7 -5 0 8.00490 1.15710 1
7 -5 -4 10.3886 2.82319 -2
7 5 0 10.3886 2.82319 1
0 6 0 205.220 10.9325 -2
0 -6 0 205.220 10.9325 1
0 -6 0 196.201 10.6369 -2
0 6 0 196.201 10.6369 1
-1 6 1 30.9424 3.20561 -2
-1 -6 0 30.9424 3.20561 1
1 6 0 12.8296 1.35570 1
-2 6 1 126.683 3.78461 -2
-2 -6 0 126.683 3.78461 1
2 -6 -1 106.337 6.90228 -2
2 6 0 106.337 6.90228 1
-3 6 2 9.99299 1.38597 -2
-3 -6 0 9.99299 1.38597 1
3 6 0 6.83356 1.28867 1
-4 6 2 36.0893 1.73138 -2
-4 -6 0 36.0893 1.73138 1
-11 0 5 460.702 9.50573 -2
-11 0 1 460.702 9.50573 1
-10 0 4 169.596 3.31379 -2
-10 0 1 169.596 3.31379 1
-9 0 4 143.832 2.89584 -2
-9 0 1 143.832 2.89584 1
-8 0 3 93.0890 2.42116 -2
-8 0 1 93.0890 2.42116 1
-7 0 3 49.0192 1.18553 -2
-7 0 1 49.0192 1.18553 1
-6 0 2 574.254 24.4435 -2
-6 0 1 574.254 24.4435 1
-5 0 1 2.11740 0.24701 1
-4 0 1 172.609 3.37512 -2
-4 0 1 172.609 3.37512 1
-3 0 1 6.33735 0.21658 1
2 0 0 6481.50 181.351 -2
-2 0 1 6481.50 181.351 1
-1 0 1 95.5798 2.82960 1
1 0 1 46.9732 0.75589 1
-2 0 2 2036.42 59.9717 -2
2 0 1 2036.42 59.9717 1
3 0 1 1826.54 40.4152 1
-4 0 3 124.870 2.01802 -2
4 0 1 124.870 2.01802 1
5 0 1 500.809 14.8062 1
-7 0 5 3.24548 0.68812 -2
7 0 1 3.24548 0.68812 1
-8 0 5 233.814 3.95713 -2
8 0 1 233.814 3.95713 1
-9 0 6 176.949 4.36621 -2
9 0 1 176.949 4.36621 1
-10 0 6 5.22710 1.08371 -2
10 0 1 5.22710 1.08371 1
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-2 -2 -10 52.4787 1.40752 -2
-2 2 11 52.4787 1.40752 1
1 -2 -11 31.2442 0.93163 1
-1 2 11 31.3145 0.92743 1
0 2 11 38.1148 1.18649 -2
0 -2 -11 38.1148 1.18649 1
0 -2 -11 41.0363 1.15889 -2
0 2 11 41.0363 1.15889 1
-1 -2 -11 14.9863 0.66545 1
1 2 11 15.2401 0.83846 1
-2 2 12 247.052 9.35497 -2
-2 -2 -11 247.052 9.35497 1
2 -2 -12 254.531 6.64454 -2
2 2 11 254.531 6.64454 1
-3 2 13 42.1373 2.88390 -2
-3 -2 -11 42.1373 2.88390 1
3 -2 -13 47.2356 2.79555 -2
3 2 11 47.2356 2.79555 1
-4 2 13 29.0235 2.23812 -2
-4 -2 -11 29.0235 2.23812 1
4 -2 -13 38.4536 1.79973 -2
4 2 11 38.4536 1.79973 1
7 -3 -11 8.29641 8.73109 1
-7 -3 -7 39.6413 2.66717 -2
-7 3 11 39.6413 2.66717 1
6 3 8 200.597 6.10470 -2
6 -3 -11 200.597 6.10470 1
-6 -3 -8 215.617 5.99585 -2
-6 3 11 215.617 5.99585 1
5 3 8 25.5886 1.77348 -2
5 -3 -11 25.5886 1.77348 1
-5 -3 -8 28.4061 2.37146 -2
-5 3 11 28.4061 2.37146 1
4 3 9 595.138 14.8549 -2
4 -3 -11 595.138 14.8549 1
-4 -3 -9 628.474 13.4633 -2
-4 3 11 628.474 13.4633 1
3 3 9 39.1335 2.39334 -2
3 -3 -11 39.1335 2.39334 1
-3 -3 -9 41.2779 2.19197 -2
-3 3 11 41.2779 2.19197 1
2 3 10 127.678 2.93140 -2
2 -3 -11 127.678 2.93140 1
-2 -3 -10 137.106 2.96994 -2
-2 3 11 137.106 2.96994 1
1 3 10 13.1845 3.33587 -2
1 -3 -11 13.1845 3.33587 1
-1 -3 -10 7.61125 2.29674 -2
-1 3 11 7.61125 2.29674 1
0 3 11 24.9892 1.15432 -2
0 -3 -11 24.9892 1.15432 1
0 -3 -11 27.4008 1.09026 -2
0 3 11 27.4008 1.09026 1
-1 -3 -11 1.80250 0.55986 1
1 3 11 0.96111 0.55928 1
-2 3 12 32.6820 1.34406 -2
-2 -3 -11 32.6820 1.34406 1
2 -3 -12 39.6048 2.27841 -2
2 3 11 39.6048 2.27841 1
-3 -3 -11 13.0283 2.38649 1
3 3 11 19.3419 1.57203 1
3 -4 -11 33.2592 1.48887 1
-3 4 11 30.8842 2.09039 1
2 4 10 181.790 3.90468 -2
2 -4 -11 181.790 3.90468 1
-2 -4 -10 192.546 10.6651 -2
-2 4 11 192.546 10.6651 1
1 -4 -11 3.66347 0.52643 1
-1 4 11 5.04883 1.98441 1
-1 -4 -11 0.89348 1.29869 1
1 -4 -11 0.23863 0.50706 -2
1 4 11 0.23863 0.50706 1
8 0 8 16.0394 3.52894 -2
-8 0 12 16.0394 3.52894 1
7 0 8 37.5824 2.71028 -2
-7 0 12 37.5824 2.71028 1
6 0 9 14.7177 1.23022 -2
-6 0 12 14.7177 1.23022 1
5 0 9 62.2132 2.02988 -2
-5 0 12 62.2132 2.02988 1
4 0 10 240.181 4.55974 -2
-4 0 12 240.181 4.55974 1
3 0 10 273.653 8.88070 -2
-3 0 12 273.653 8.88070 1
2 0 11 443.475 6.71676 -2
-2 0 12 443.475 6.71676 1
-1 0 12 185.423 3.24913 1
0 0 12 730.486 13.3146 -2
0 0 12 730.486 13.3146 1
1 0 12 -0.0608 0.52484 1
-2 0 13 5.66293 1.04061 -2
2 0 12 5.66293 1.04061 1
-3 0 14 31.2172 11.4704 -2
3 0 12 31.2172 11.4704 1
-4 0 14 77.7196 3.84342 -2
4 0 12 77.7196 3.84342 1
8 1 8 220.031 10.1903 -2
8 -1 -12 220.031 10.1903 1
-8 -1 -8 249.954 6.33504 -2
-8 1 12 249.954 6.33504 1
7 1 8 47.6339 3.33645 -2
7 -1 -12 47.6339 3.33645 1
-7 -1 -8 58.1522 2.54322 -2
-7 1 12 58.1522 2.54322 1
6 1 9 155.186 8.39556 -2
6 -1 -12 155.186 8.39556 1
-6 -1 -9 167.372 3.99684 -2
-6 1 12 167.372 3.99684 1
5 1 9 66.6994 3.09290 -2
5 -1 -12 66.6994 3.09290 1
-5 -1 -9 65.2988 2.48078 -2
-5 1 12 65.2988 2.48078 1
4 1 10 52.3130 1.69058 -2
4 -1 -12 52.3130 1.69058 1
-4 -1 -10 58.6663 1.51317 -2
-4 1 12 58.6663 1.51317 1
3 1 10 137.976 5.04980 -2
3 -1 -12 137.976 5.04980 1
-3 -1 -10 146.312 4.60652 -2
-3 1 12 146.312 4.60652 1
2 1 11 17.9952 0.98399 -2
2 -1 -12 17.9952 0.98399 1
-2 -1 -11 21.1940 1.08267 -2
-2 1 12 21.1940 1.08267 1
1 -1 -12 2.62898 0.40445 1
-1 1 12 2.30457 0.40498 1
0 1 12 132.737 3.02663 -2
0 -1 -12 132.737 3.02663 1
0 -1 -12 138.379 3.02857 -2
0 1 12 138.379 3.02857 1
-1 -1 -12 13.5388 0.80347 1
1 1 12 13.4000 0.78452 1
-2 1 13 579.266 19.7486 -2
-2 -1 -12 579.266 19.7486 1
2 -1 -13 539.612 12.4713 -2
2 1 12 539.612 12.4713 1
-3 1 14 12.4035 3.06385 -2
-3 -1 -12 12.4035 3.06385 1
3 -1 -14 13.1440 2.73795 -2
3 1 12 13.1440 2.73795 1
-4 1 14 180.541 7.11957 -2
-4 -1 -12 180.541 7.11957 1
4 -1 -14 181.481 6.13577 -2
4 1 12 181.481 6.13577 1
7 2 8 160.787 11.2452 -2
7 -2 -12 160.787 11.2452 1
-7 -2 -8 179.128 8.37578 -2
-7 2 12 179.128 8.37578 1
6 2 9 130.954 3.52382 -2
6 -2 -12 130.954 3.52382 1
-6 -2 -9 136.457 5.39834 -2
-6 2 12 136.457 5.39834 1
5 -2 -12 28.3309 1.68069 1
-5 2 12 27.5269 2.08789 1
4 2 10 378.229 14.7178 -2
4 -2 -12 378.229 14.7178 1
-4 -2 -10 380.041 6.94075 -2
-4 2 12 380.041 6.94075 1
3 2 10 78.0330 4.39420 -2
3 -2 -12 78.0330 4.39420 1
-3 -2 -10 82.4483 4.78449 -2
-3 2 12 82.4483 4.78449 1
2 2 11 249.204 6.35080 -2
2 -2 -12 249.204 6.35080 1
-2 -2 -11 242.104 4.85312 -2
-2 2 12 242.104 4.85312 1
1 -2 -12 2.36675 0.46255 1
-1 2 12 2.67530 0.49114 1
0 2 12 218.685 8.74521 -2
0 -2 -12 218.685 8.74521 1
0 -2 -12 226.320 6.08542 -2
0 2 12 226.320 6.08542 1
-1 -2 -12 4.32706 0.55193 1
1 -2 -13 7.36171 2.54678 -2
1 2 12 7.36171 2.54678 1
-2 2 13 -0.3131 0.66958 -2
-2 -2 -12 -0.3131 0.66958 1
2 -2 -13 0.42618 0.86624 -2
2 2 12 0.42618 0.86624 1
-3 -2 -12 4.38419 1.40059 1
3 2 12 7.15246 0.85069 1
-6 3 12 -0.0277 0.20720 1
5 3 9 24.6050 5.56867 -2
5 -3 -12 24.6050 5.56867 1
-5 -3 -9 34.7457 1.59859 -2
-5 3 12 34.7457 1.59859 1
4 3 10 27.6832 1.89539 -2
4 -3 -12 27.6832 1.89539 1
-4 -3 -10 34.8399 1.80282 -2
-4 3 12 34.8399 1.80282 1
3 3 10 63.3260 5.38898 -2
3 -3 -12 63.3260 5.38898 1
-3 3 12 32.4253 2.13827 1
2 3 11 25.3173 1.09359 -2
2 -3 -12 25.3173 1.09359 1
-2 -3 -11 26.2533 1.74196 -2
-2 3 12 26.2533 1.74196 1
1 -3 -12 1.79516 0.41834 1
-1 3 12 1.83376 0.57208 1
0 3 12 104.379 2.79838 -2
0 -3 -12 104.379 2.79838 1
0 -3 -12 116.755 3.34533 -2
0 3 12 116.755 3.34533 1
-1 -3 -12 1.83118 0.79751 1
1 3 12 2.96373 0.65410 1
7 0 9 23.7849 2.48332 -2
-7 0 13 23.7849 2.48332 1
6 0 10 185.021 5.99554 -2
-6 0 13 185.021 5.99554 1
5 0 10 18.3282 2.22732 -2
-5 0 13 18.3282 2.22732 1
4 0 11 211.799 6.80490 -2
-4 0 13 211.799 6.80490 1
3 0 11 85.6518 4.25765 -2
-3 0 13 85.6518 4.25765 1
2 0 12 9.76192 1.08669 -2
-2 0 13 9.76192 1.08669 1
-1 0 13 0.53877 0.42118 1
0 0 13 85.0494 2.32942 -2
0 0 13 85.0494 2.32942 1
1 0 13 16.4809 0.91985 1
-2 0 14 476.617 11.5322 -2
2 0 13 476.617 11.5322 1
7 -1 -13 64.2792 11.2195 1
-7 -1 -9 130.151 4.17785 -2
-7 1 13 130.151 4.17785 1
6 1 10 20.9192 2.11107 -2
6 -1 -13 20.9192 2.11107 1
-6 -1 -10 25.8805 1.71688 -2
-6 1 13 25.8805 1.71688 1
5 -1 -13 5.58291 0.96140 1
-5 -1 -10 26.1679 2.30834 -2
-5 1 13 26.1679 2.30834 1
4 1 11 170.085 5.34271 -2
4 -1 -13 170.085 5.34271 1
-4 -1 -11 165.168 3.94815 -2
-4 1 13 165.168 3.94815 1
3 -1 -13 7.48407 0.99493 1
-3 -1 -11 14.0893 1.89438 -2
-3 1 13 14.0893 1.89438 1
2 1 12 490.021 14.6634 -2
2 -1 -13 490.021 14.6634 1
-2 -1 -12 494.467 8.27491 -2
-2 1 13 494.467 8.27491 1
1 -1 -13 30.8239 1.17082 1
-1 1 13 34.1685 1.13925 1
0 1 13 352.049 8.18894 -2
0 -1 -13 352.049 8.18894 1
0 -1 -13 346.479 7.34178 -2
0 1 13 346.479 7.34178 1
-1 1 14 16.9903 13.7039 -2
-1 -1 -13 16.9903 13.7039 1
1 1 13 15.0752 1.20764 1
-2 1 14 94.6301 10.9556 -2
-2 -1 -13 94.6301 10.9556 1
2 -1 -14 83.7379 6.17461 -2
2 1 13 83.7379 6.17461 1
6 -2 -13 80.4091 21.1682 1
-6 2 13 83.6076 2.72975 1
5 -2 -13 41.0709 2.36893 1
-5 -2 -10 74.3939 2.87572 -2
-5 2 13 74.3939 2.87572 1
4 2 11 33.4096 2.85550 -2
4 -2 -13 33.4096 2.85550 1
-4 -2 -11 43.6884 1.37598 -2
-4 2 13 43.6884 1.37598 1
3 2 11 34.4612 3.73995 -2
3 -2 -13 34.4612 3.73995 1
-3 -2 -11 43.6558 2.13012 -2
-3 2 13 43.6558 2.13012 1
2 2 12 0.02594 0.79064 -2
2 -2 -13 0.02594 0.79064 1
-2 -2 -12 1.47582 0.70863 -2
-2 2 13 1.47582 0.70863 1
1 -2 -13 5.04926 0.54003 1
-1 2 13 5.17698 0.67770 1
0 2 13 36.0614 4.14889 -2
0 -2 -13 36.0614 4.14889 1
0 -2 -13 36.4535 1.31967 -2
0 2 13 36.4535 1.31967 1
-1 -2 -13 -0.6038 1.14821 1
1 2 13 0.86449 0.18422 1
5 0 11 34.8955 4.05882 -2
-5 0 14 34.8955 4.05882 1
4 0 12 66.2309 2.80600 -2
-4 0 14 66.2309 2.80600 1
-3 0 14 0.48025 0.53847 1
2 0 13 536.943 9.47309 -2
-2 0 14 536.943 9.47309 1
-1 0 14 1.64299 0.57631 1
0 0 14 205.721 5.17344 -2
0 0 14 205.721 5.17344 1
5 -1 -14 2.36140 1.61855 1
-5 -1 -11 14.0288 2.08475 -2
-5 1 14 14.0288 2.08475 1
4 1 12 154.238 15.7225 -2
4 -1 -14 154.238 15.7225 1
-4 -1 -12 160.778 5.67220 -2
-4 1 14 160.778 5.67220 1
3 -1 -14 9.95370 1.28596 1
-3 1 14 3.89348 0.90401 1
2 1 13 80.7109 7.67273 -2
2 -1 -14 80.7109 7.67273 1
-2 -1 -13 76.5805 2.70500 -2
-2 1 14 76.5805 2.70500 1
1 -1 -14 15.8344 5.26301 1
-1 1 14 22.1510 1.24122 1
0 1 14 -3.1675 9.23919 -2
0 -1 -14 -3.1675 9.23919 1
0 -1 -14 6.66261 1.03064 -2
0 1 14 6.66261 1.03064 1
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 83096
_shelx_res_file
;
TITL PicTh28_0m_4_a.res in P2(1)
PicTh28_fine.res
created by SHELXL-2019/2 at 11:36:10 on 11-Aug-2023
CELL 0.71073 8.9822 4.9413 10.9400 90.000 102.406 90.000
ZERR 2.00 0.0012 0.0006 0.0014 0.000 0.005 0.000
LATT -1
SYMM -x, y+1/2, -z
SFAC C H O F S
UNIT 6 4 12 12 4
OMIT -1 4 10 ! affected by cryo stream shadow
OMIT 3 4 9 ! affected by cryo stream shadow
OMIT 9 3 4 ! affected by cryo stream shadow
OMIT 3 5 3 ! affected by cryo stream shadow
LIST 4
TEMP -173.150
SIZE 0.062 0.320 0.349
ACTA
L.S. 4
FMAP 2
PLAN -10
HTAB
BOND $H
CONF
WGHT 0.031800 0.384300
BASF 0.29332
FVAR 1.05585
S1 5 0.965948 0.489799 0.319721 11.00000 0.01122 0.02095 =
0.02018 -0.00237 0.00330 0.00073
S2 5 0.440528 0.478883 0.321702 11.00000 0.01147 0.01848 =
0.01861 0.00152 0.00380 0.00112
F1 4 0.789566 0.173884 0.161328 11.00000 0.02810 0.03591 =
0.03339 -0.01311 0.00852 -0.01311
F2 4 1.006931 0.257369 0.118308 11.00000 0.02788 0.05097 =
0.03449 -0.01508 0.01555 0.00121
F3 4 0.831785 0.563430 0.087971 11.00000 0.04356 0.03384 =
0.02180 0.00417 -0.00006 0.00168
F4 4 0.451390 0.448049 0.086786 11.00000 0.04542 0.04653 =
0.02058 -0.00417 0.00833 0.00849
F5 4 0.528734 0.826003 0.173763 11.00000 0.02858 0.03196 =
0.03356 0.01218 0.01028 -0.00484
F6 4 0.289600 0.733917 0.129337 11.00000 0.02208 0.04254 =
0.02892 0.01054 0.00081 0.00927
O1 3 0.816915 0.625839 0.344605 11.00000 0.01166 0.02138 =
0.02291 -0.00065 0.00656 0.00227
O2 3 1.008735 0.265946 0.399504 11.00000 0.02457 0.02687 =
0.02657 0.00467 0.00428 0.01077
O3 3 1.067926 0.701538 0.308972 11.00000 0.01879 0.03058 =
0.03306 -0.01066 0.01037 -0.00833
O4 3 0.605690 0.356211 0.343513 11.00000 0.01217 0.02202 =
0.02246 0.00205 0.00466 0.00082
O5 3 0.338110 0.259630 0.304714 11.00000 0.01401 0.02697 =
0.03634 0.00392 0.00361 -0.00207
O6 3 0.434515 0.691729 0.407011 11.00000 0.02119 0.02488 =
0.02277 0.00000 0.00492 0.00648
C1 1 0.730323 0.493218 0.423089 11.00000 0.01207 0.03873 =
0.01819 -0.00018 0.00356 -0.00469
AFIX 23
H1 2 0.795251 0.361855 0.478791 11.00000 -1.20000
H2 2 0.691600 0.627764 0.475688 11.00000 -1.20000
AFIX 0
C2 1 0.893222 0.361773 0.160892 11.00000 0.02103 0.02610 =
0.02205 -0.00536 0.00569 -0.00218
C3 1 0.426985 0.630924 0.166627 11.00000 0.02264 0.02754 =
0.01731 0.00385 0.00182 0.00270
HKLF 5 1 1 0 0 0 1 0 0 0 1
REM PicTh28_0m_4_a.res in P2(1)
REM wR2 = 0.0719, GooF = S = 1.054, Restrained GooF = 1.053 for all data
REM R1 = 0.0271 for 2254 Fo > 4sig(Fo) and 0.0289 for all 2295 data
REM 155 parameters refined using 1 restraints
END
WGHT 0.0318 0.3842
REM Instructions for potential hydrogen bonds
EQIV $1 -x+2, y-1/2, -z+1
HTAB C1 O3_$1
EQIV $2 -x+1, y+1/2, -z+1
HTAB C1 O5_$2
HTAB C1 O6
REM Highest difference peak 0.410, deepest hole -0.470, 1-sigma level 0.077
Q1 1 0.9319 0.4368 0.2392 11.00000 0.05 0.41
Q2 1 0.4400 0.5350 0.2277 11.00000 0.05 0.38
Q3 1 1.0190 0.4721 -0.0133 11.00000 0.05 0.31
Q4 1 1.0182 0.8052 0.1587 11.00000 0.05 0.28
Q5 1 0.4272 0.4832 0.0166 11.00000 0.05 0.28
Q6 1 0.3272 0.4709 -0.0240 11.00000 0.05 0.27
Q7 1 0.4763 0.4936 0.4088 11.00000 0.05 0.26
Q8 1 0.4900 0.4725 0.4700 11.00000 0.05 0.26
Q9 1 0.6769 0.6599 0.0202 11.00000 0.05 0.24
Q10 1 0.9321 0.4641 0.0206 11.00000 0.05 0.24
;
_shelx_res_checksum 37891
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, 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
S S1 0.96595(10) 0.4898(2) 0.31972(8) 0.0175(2) Uani d 1 . .
S S2 0.44053(10) 0.4789(2) 0.32170(8) 0.01610(19) Uani d 1 . .
F F1 0.7896(3) 0.1739(6) 0.1613(3) 0.0322(7) Uani d 1 . .
F F2 1.0069(3) 0.2574(7) 0.1183(3) 0.0364(7) Uani d 1 . .
F F3 0.8318(4) 0.5634(7) 0.0880(3) 0.0341(7) Uani d 1 . .
F F4 0.4514(4) 0.4480(7) 0.0868(2) 0.0373(7) Uani d 1 . .
F F5 0.5287(3) 0.8260(6) 0.1738(2) 0.0308(7) Uani d 1 . .
F F6 0.2896(3) 0.7339(7) 0.1293(3) 0.0319(6) Uani d 1 . .
O O1 0.8169(3) 0.6258(6) 0.3446(3) 0.0182(6) Uani d 1 . .
O O2 1.0087(4) 0.2659(7) 0.3995(3) 0.0262(7) Uani d 1 . .
O O3 1.0679(3) 0.7015(7) 0.3090(3) 0.0268(7) Uani d 1 . .
O O4 0.6057(3) 0.3562(6) 0.3435(3) 0.0187(6) Uani d 1 . .
O O5 0.3381(3) 0.2596(7) 0.3047(3) 0.0260(7) Uani d 1 . .
O O6 0.4345(4) 0.6917(7) 0.4070(3) 0.0229(6) Uani d 1 . .
C C1 0.7303(5) 0.4932(13) 0.4231(3) 0.0230(6) Uani d 1 . .
H H1 0.795251 0.361855 0.478791 0.028 Uiso calc 1 . .
H H2 0.691600 0.627764 0.475688 0.028 Uiso calc 1 . .
C C2 0.8932(5) 0.3618(10) 0.1609(4) 0.0229(9) Uani d 1 . .
C C3 0.4270(5) 0.6309(9) 0.1666(4) 0.0229(8) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
S1 0.0112(4) 0.0210(4) 0.0202(4) 0.0007(4) 0.0033(4) -0.0024(5)
S2 0.0115(4) 0.0185(4) 0.0186(4) 0.0011(5) 0.0038(3) 0.0015(5)
F1 0.0281(15) 0.0359(16) 0.0334(13) -0.0131(12) 0.0085(12) -0.0131(12)
F2 0.0279(15) 0.051(2) 0.0345(14) 0.0012(14) 0.0156(12) -0.0151(14)
F3 0.0436(17) 0.0338(14) 0.0218(12) 0.0017(13) -0.0001(12) 0.0042(10)
F4 0.0454(17) 0.0465(19) 0.0206(11) 0.0085(17) 0.0083(11) -0.0042(13)
F5 0.0286(15) 0.0320(15) 0.0336(14) -0.0048(11) 0.0103(12) 0.0122(11)
F6 0.0221(13) 0.0425(16) 0.0289(13) 0.0093(13) 0.0008(11) 0.0105(13)
O1 0.0117(13) 0.0214(14) 0.0229(14) 0.0023(11) 0.0066(11) -0.0006(11)
O2 0.0246(16) 0.0269(17) 0.0266(15) 0.0108(14) 0.0043(13) 0.0047(13)
O3 0.0188(15) 0.0306(17) 0.0331(16) -0.0083(13) 0.0104(14) -0.0107(14)
O4 0.0122(13) 0.0220(13) 0.0225(14) 0.0008(12) 0.0047(12) 0.0020(12)
O5 0.0140(14) 0.0270(17) 0.0363(16) -0.0021(12) 0.0036(13) 0.0039(14)
O6 0.0212(15) 0.0249(15) 0.0228(14) 0.0065(13) 0.0049(12) 0.0000(13)
C1 0.0121(13) 0.0387(19) 0.0182(13) -0.0047(17) 0.0036(16) 0.000(2)
C2 0.021(2) 0.026(2) 0.0221(19) -0.0022(17) 0.0057(16) -0.0054(17)
C3 0.023(2) 0.028(2) 0.0173(17) 0.0027(19) 0.0018(17) 0.0039(17)
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'
S S 0.1246 0.1234 '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
O2 S1 O3 . . 122.5(2) ?
O2 S1 O1 . . 110.91(17) ?
O3 S1 O1 . . 106.8(2) ?
O2 S1 C2 . . 108.1(2) ?
O3 S1 C2 . . 106.4(2) ?
O1 S1 C2 . . 99.69(19) ?
O5 S2 O6 . . 122.87(19) ?
O5 S2 O4 . . 106.97(19) ?
O6 S2 O4 . . 110.79(18) ?
O5 S2 C3 . . 106.3(2) ?
O6 S2 C3 . . 107.5(2) ?
O4 S2 C3 . . 99.85(19) ?
C1 O1 S1 . . 120.0(3) ?
C1 O4 S2 . . 119.9(3) ?
O4 C1 O1 . . 107.8(2) ?
O4 C1 H1 . . 110.1 ?
O1 C1 H1 . . 110.1 ?
O4 C1 H2 . . 110.1 ?
O1 C1 H2 . . 110.1 ?
H1 C1 H2 . . 108.5 ?
F1 C2 F2 . . 109.2(4) ?
F1 C2 F3 . . 109.3(4) ?
F2 C2 F3 . . 109.7(4) ?
F1 C2 S1 . . 110.4(3) ?
F2 C2 S1 . . 109.0(3) ?
F3 C2 S1 . . 109.3(3) ?
F4 C3 F6 . . 109.9(4) ?
F4 C3 F5 . . 109.3(4) ?
F6 C3 F5 . . 109.1(4) ?
F4 C3 S2 . . 110.3(3) ?
F6 C3 S2 . . 108.4(3) ?
F5 C3 S2 . . 109.7(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
S1 O2 . 1.410(4) ?
S1 O3 . 1.412(4) ?
S1 O1 . 1.573(3) ?
S1 C2 . 1.833(4) ?
S2 O5 . 1.408(3) ?
S2 O6 . 1.415(3) ?
S2 O4 . 1.573(3) ?
S2 C3 . 1.835(4) ?
F1 C2 . 1.316(5) ?
F2 C2 . 1.316(5) ?
F3 C2 . 1.321(6) ?
F4 C3 . 1.308(5) ?
F5 C3 . 1.319(5) ?
F6 C3 . 1.316(5) ?
O1 C1 . 1.435(5) ?
O4 C1 . 1.432(5) ?
C1 H1 . 0.9900 ?
C1 H2 . 0.9900 ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
F3 F6 2.894(5) 1_555 2_645 yes
F1 F5 2.933(4) 1_555 1_545 yes
F4 F5 2.957(3) 1_555 2_645 yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_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
C1 H1 O2 1_555 1_555 1_555 0.99 2.317 2.803(6) 109.23 yes
C1 H2 O6 1_555 1_555 1_555 0.99 2.292 2.802(6) 110.91 yes
C1 H1 O3 1_555 1_555 2_746 0.99 2.510 3.416(5) 151.98 yes
C1 H2 O5 1_555 1_555 2_646 0.99 2.558 3.430(5) 146.87 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
O2 S1 O1 C1 . . . . -10.4(4) ?
O3 S1 O1 C1 . . . . -146.1(3) ?
C2 S1 O1 C1 . . . . 103.3(3) ?
O5 S2 O4 C1 . . . . -147.9(3) ?
O6 S2 O4 C1 . . . . -11.6(4) ?
C3 S2 O4 C1 . . . . 101.6(3) ?
S2 O4 C1 O1 . . . . -103.7(4) ?
S1 O1 C1 O4 . . . . -98.6(4) ?
O2 S1 C2 F1 . . . . 50.7(4) ?
O3 S1 C2 F1 . . . . -176.1(3) ?
O1 S1 C2 F1 . . . . -65.2(4) ?
O2 S1 C2 F2 . . . . -69.3(4) ?
O3 S1 C2 F2 . . . . 64.0(4) ?
O1 S1 C2 F2 . . . . 174.9(3) ?
O2 S1 C2 F3 . . . . 170.9(3) ?
O3 S1 C2 F3 . . . . -55.9(4) ?
O1 S1 C2 F3 . . . . 55.0(3) ?
O5 S2 C3 F4 . . . . -54.8(4) ?
O6 S2 C3 F4 . . . . 171.9(3) ?
O4 S2 C3 F4 . . . . 56.3(4) ?
O5 S2 C3 F6 . . . . 65.7(3) ?
O6 S2 C3 F6 . . . . -67.6(4) ?
O4 S2 C3 F6 . . . . 176.7(3) ?
O5 S2 C3 F5 . . . . -175.3(3) ?
O6 S2 C3 F5 . . . . 51.4(4) ?
O4 S2 C3 F5 . . . . -64.2(3) ?