#------------------------------------------------------------------------------
#$Date: 2024-04-27 04:58:22 +0300 (Sat, 27 Apr 2024) $
#$Revision: 291385 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023112.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_2023112
loop_
_publ_author_name
'Stewart, John W.'
'Irons, Elena M.'
'Osorio Abanto, Giovanna'
'Zeller, Matthias'
'Zaleski, Curtis M.'
'Predecki, Daniel P.'
_publ_section_title
;
Synthesis and crystal structures of N,2,4,6-tetramethylanilinium
trifluoromethanesulfonate and
N-isopropylidene-N,2,4,6-tetramethylanilinium trifluoromethanesulfonate
;
_journal_issue 5
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024003438
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C13 H20 N +, C F3 O3 S -'
_chemical_formula_moiety 'C13 H20 N +, C F3 O3 S -'
_chemical_formula_sum 'C14 H20 F3 N O3 S'
_chemical_formula_weight 339.37
_chemical_name_systematic
;
N-Isopropylidene-N,2,4,6-tetramethylanilinium
trifluoromethanesulfonate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 102.024(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 6.8580(4)
_cell_length_b 19.4619(12)
_cell_length_c 12.6131(7)
_cell_measurement_reflns_used 9901
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 33.1254
_cell_measurement_theta_min 2.6659
_cell_volume 1646.53(17)
_computing_cell_refinement
;
SAINT V8.40B (Bruker, 2022)
;
_computing_data_collection
;
APEX4 v2022.10-0 (Bruker, 2022)
;
_computing_data_reduction
;
SAINT V8.40B (Bruker, 2022)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b),
ShelXle Rev1541 (H\"ubschle et al., 2011)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device 'three circle diffractometer'
_diffrn_measurement_device_type 'Bruker AXS D8 Quest'
_diffrn_measurement_method 'omega and phi scans'
_diffrn_radiation_monochromator 'Triumph curved graphite crystal'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0402
_diffrn_reflns_av_unetI/netI 0.0283
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 28
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 35093
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 33.176
_diffrn_reflns_theta_min 1.955
_diffrn_source 'fine focus sealed tube X-ray source'
_diffrn_source_current 30
_diffrn_source_voltage 50
_exptl_absorpt_coefficient_mu 0.237
_exptl_absorpt_correction_T_max 0.7465
_exptl_absorpt_correction_T_min 0.6620
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.369
_exptl_crystal_description block
_exptl_crystal_F_000 712
_exptl_crystal_size_max 0.450
_exptl_crystal_size_mid 0.430
_exptl_crystal_size_min 0.320
_refine_diff_density_max 0.626
_refine_diff_density_min -0.413
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.044
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 205
_refine_ls_number_reflns 6151
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.044
_refine_ls_R_factor_all 0.0649
_refine_ls_R_factor_gt 0.0454
_refine_ls_shift/su_max 0.036
_refine_ls_shift/su_mean 0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+0.6525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1250
_refine_ls_wR_factor_ref 0.1356
_reflns_number_gt 4836
_reflns_number_total 6151
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ej2004.cif
_cod_data_source_block 2
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2023112
_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 0.901
_shelx_estimated_absorpt_t_max 0.928
_shelx_hkl_file
;
-1 0 0 9.09149 0.41151 3
-1 0 0 8.14195 0.85980 1
-2 0 0 9276.82 242.543 2
2 0 0 7342.99 233.875 2
3 0 0 0.81150 0.40258 3
3 0 0 2.49280 1.20151 1
-3 0 0 -0.2536 1.25125 1
-3 0 0 0.84032 0.43758 3
4 0 0 47.5894 3.73557 1
-4 0 0 43.3448 4.02370 1
-4 0 0 48.8856 1.88857 3
4 0 0 47.4671 1.75018 3
4 0 0 47.4558 1.71541 3
5 0 0 -0.0052 0.49230 3
-5 0 0 0.44016 0.65334 3
-5 0 0 -2.0151 2.16142 1
5 0 0 1.01273 1.86166 1
5 0 0 0.76972 0.57162 3
6 0 0 509.341 17.1581 1
-6 0 0 468.597 17.5443 1
-6 0 0 478.783 13.1608 3
6 0 0 481.288 12.7756 3
6 0 0 508.923 12.8434 3
-7 0 0 -0.6701 0.82819 3
7 0 0 -0.2782 2.99102 1
-7 0 0 -4.3404 2.99262 1
7 0 0 -0.3972 0.62978 3
-8 0 0 0.82622 1.00285 3
-8 0 0 -8.7219 4.46277 1
8 0 0 -3.2737 3.73171 1
8 0 0 0.35915 0.59786 3
-9 0 0 -0.1804 6.61396 1
-9 0 0 -1.2246 1.00330 3
-1 -1 0 1067.03 26.5578 1
-1 1 0 1010.69 26.7039 1
-2 -1 0 39.0422 1.31552 3
-2 -1 0 37.4814 2.46858 1
-2 1 0 41.9502 2.62124 1
2 1 0 41.3057 2.36106 1
2 1 0 40.5348 1.28678 3
-2 1 0 38.5550 1.37388 3
2 1 0 39.2885 1.26378 3
3 -1 0 38.4622 1.45924 3
-3 -1 0 35.5521 1.43597 3
-3 -1 0 41.1796 2.99727 1
3 1 0 38.4035 2.93480 1
3 1 0 37.4178 1.34931 3
-3 1 0 35.5303 3.10957 1
-3 1 0 34.5742 1.49199 3
3 1 0 40.1800 1.39665 3
4 -1 0 47.2286 3.86066 1
-4 -1 0 42.0804 1.76374 3
4 -1 0 42.2502 1.70668 3
-4 -1 0 43.3827 3.85525 1
4 1 0 47.7030 3.72083 1
4 1 0 42.6439 1.61974 3
4 1 0 46.2980 1.61295 3
-4 1 0 43.7169 1.84022 3
-4 1 0 35.2176 3.64671 1
-5 -1 0 2.55460 2.25805 1
5 -1 0 -0.0623 0.52171 3
5 -1 0 -2.0291 1.73912 1
-5 -1 0 0.96984 0.69817 3
5 -1 0 0.48733 0.59327 3
5 1 0 0.33782 0.48950 3
-5 1 0 -2.4668 1.75060 1
5 1 0 0.04122 0.54006 3
-5 1 0 -0.8831 0.61487 3
5 1 0 -0.3651 1.97264 1
6 -1 0 2.96434 0.82062 3
-6 -1 0 2.57753 2.75171 1
-6 -1 0 1.65396 0.85815 3
6 -1 0 2.90022 2.56990 1
6 -1 0 2.09043 0.69677 3
6 1 0 0.60966 2.40419 1
-6 1 0 2.80793 0.96250 3
-6 1 0 1.87578 2.97231 1
6 1 0 2.78830 0.72497 3
6 1 0 1.46374 0.58964 3
7 -1 0 -6.1981 2.79768 1
-7 -1 0 0.13324 0.88118 3
7 -1 0 -0.2760 0.66205 3
-7 -1 0 -1.9388 2.96898 1
7 1 0 1.39868 3.18459 1
-7 1 0 4.73047 3.69875 1
-7 1 0 1.10852 0.90368 3
7 1 0 0.34493 0.59450 3
8 -1 0 19.5435 1.41967 3
8 -1 0 19.8524 4.90005 1
-8 -1 0 25.0396 2.11283 3
-8 -1 0 28.5015 5.93431 1
8 1 0 19.3533 1.16101 3
-8 1 0 14.8776 5.73744 1
8 1 0 19.5622 4.58844 1
-8 1 0 20.4614 2.14090 3
-9 -1 0 -0.4533 1.09742 3
9 -1 0 3.65657 5.70042 1
-9 -1 0 -0.6652 6.27820 1
-9 1 0 12.6823 6.94233 1
1 -2 0 6922.23 194.557 2
-1 -2 0 6611.39 186.538 2
-1 2 0 7052.09 195.813 2
1 2 0 6748.71 186.149 2
-2 -2 0 3925.00 123.172 2
2 -2 0 3252.19 125.598 2
2 2 0 3772.59 120.342 2
-2 2 0 3892.99 130.458 2
-3 -2 0 25.8938 2.76854 1
-3 -2 0 23.5288 1.12246 3
3 2 0 22.0822 0.98116 3
-3 2 0 21.0134 2.61455 1
3 2 0 21.5972 2.39286 1
-3 2 0 22.2335 1.22569 3
3 2 0 21.4005 0.99728 3
4 -2 0 476.469 12.3174 3
-4 -2 0 487.027 15.2045 1
-4 -2 0 467.812 12.3209 3
4 2 0 460.522 14.7516 1
-4 2 0 463.090 12.4188 3
-4 2 0 490.016 15.6680 1
4 2 0 469.215 12.1520 3
4 2 0 477.426 12.1484 3
-5 -2 0 495.052 13.4409 3
-5 -2 0 497.670 16.9241 1
5 -2 0 517.196 13.3870 3
5 -2 0 528.225 17.2151 1
-5 2 0 503.558 13.5552 3
5 2 0 515.133 13.1747 3
5 2 0 530.798 16.6733 1
-5 2 0 500.217 17.4365 1
5 2 0 516.318 13.1809 3
6 -2 0 90.6200 3.17358 3
-6 -2 0 88.1529 3.32482 3
6 -2 0 89.2605 3.07857 3
-6 -2 0 87.5364 6.60156 1
6 -2 0 100.712 6.83563 1
-6 2 0 87.1073 3.40095 3
6 2 0 91.0406 2.91652 3
6 2 0 90.3764 6.24414 1
-6 2 0 95.4942 7.31095 1
6 2 0 88.7409 2.87275 3
-7 -2 0 2.51785 1.00525 3
-7 -2 0 4.55550 3.89855 1
7 -2 0 3.25200 3.20634 1
7 -2 0 3.91833 0.88620 3
7 2 0 6.20818 3.11708 1
-7 2 0 4.44206 1.15315 3
-7 2 0 -1.3102 3.49986 1
7 2 0 4.24812 0.72092 3
7 2 0 4.15288 0.69065 3
-8 -2 0 24.1510 5.46806 1
8 -2 0 26.3056 1.67074 3
8 -2 0 21.0189 5.11395 1
-8 -2 0 27.4407 2.22038 3
-8 2 0 15.7365 5.23566 1
-8 2 0 27.5494 2.31173 3
8 2 0 24.6723 1.16095 3
-9 -2 0 11.6411 6.41787 1
-9 -2 0 5.09272 1.34040 3
9 -2 0 14.1413 6.19021 1
-9 2 0 5.77320 1.36829 3
-9 2 0 8.70785 6.92541 1
0 -3 0 0.06281 0.18059 3
0 -3 0 0.74551 0.59103 1
0 3 0 0.53357 0.20731 3
0 3 0 2.02655 0.64265 1
-1 -3 0 659.027 16.6084 3
1 -3 0 649.531 18.0451 1
-1 -3 0 677.644 17.6489 1
-1 3 0 677.942 16.7035 3
1 3 0 660.781 16.5885 3
-1 3 0 660.866 18.0937 1
-2 -3 0 9056.18 265.212 2
2 -3 0 9999.99 279.602 2
2 3 0 9222.54 263.581 2
-2 3 0 9513.91 278.422 2
2 3 0 9229.37 263.143 2
-3 -3 0 248.102 8.73345 1
-3 -3 0 255.308 6.75769 3
3 3 0 259.066 6.64540 3
-3 3 0 251.377 6.89244 3
-3 3 0 249.676 9.22787 1
3 3 0 261.177 8.66576 1
3 3 0 255.543 6.64157 3
4 -3 0 719.490 18.1067 3
-4 -3 0 708.121 21.0009 1
-4 -3 0 675.636 18.0237 3
4 3 0 716.432 17.8600 3
4 3 0 723.429 20.6628 1
4 3 0 718.535 17.8592 3
-4 3 0 691.177 21.4606 1
-4 3 0 690.497 18.1843 3
5 -3 0 1.56653 0.79710 3
-5 -3 0 1.08789 0.76095 3
5 -3 0 4.33196 2.18298 1
-5 -3 0 3.70413 2.46856 1
5 3 0 -0.7095 1.92803 1
-5 3 0 3.07675 1.00330 3
5 3 0 0.80787 0.52221 3
-5 3 0 0.22842 2.13732 1
-6 -3 0 57.2725 5.95823 1
6 -3 0 64.5557 6.15390 1
6 -3 0 59.2217 2.52855 3
-6 -3 0 56.4144 2.59177 3
6 3 0 58.5128 2.10784 3
-6 3 0 57.4947 2.77591 3
-6 3 0 66.2767 6.25044 1
6 3 0 55.7909 2.05679 3
-7 -3 0 72.5146 3.14074 3
7 -3 0 75.0365 2.91011 3
7 -3 0 85.7708 7.38829 1
-7 -3 0 73.7976 7.64360 1
7 3 0 75.7542 2.39143 3
7 3 0 71.4366 2.37015 3
-7 3 0 77.1739 8.15632 1
-7 3 0 71.5525 3.28425 3
8 -3 0 87.1051 9.10202 1
-8 -3 0 76.6107 9.01144 1
8 -3 0 72.3790 2.90014 3
-8 -3 0 77.1411 3.43647 3
-8 3 0 87.0059 10.1533 1
-8 3 0 76.9585 3.56118 3
-9 -3 0 18.4094 1.86330 3
-9 -3 0 15.8199 6.68330 1
9 -3 0 13.2194 6.38537 1
9 -3 0 17.3083 1.87270 3
-9 3 0 12.9512 1.73424 3
-9 3 0 28.7173 7.57002 1
10 -3 0 26.6903 14.9922 1
0 -4 0 1572.09 40.4282 1
0 4 0 1573.00 40.4235 1
-1 -4 0 573.621 15.7351 1
1 -4 0 577.568 14.5618 3
1 -4 0 598.131 16.2841 1
-1 -4 0 588.926 14.4682 3
-1 4 0 565.341 14.5472 3
1 4 0 566.874 14.4320 3
1 4 0 575.954 15.6556 1
-1 4 0 571.343 16.2136 1
1 4 0 558.947 14.4262 3
2 -4 0 3586.10 91.1364 1
-2 -4 0 3523.09 90.4710 1
-2 4 0 3637.70 91.3348 1
-3 -4 0 519.577 15.2861 1
-3 -4 0 501.930 12.9693 3
-3 -4 0 503.966 12.9688 3
3 -4 0 490.027 15.8636 1
3 4 0 513.847 12.8449 3
-3 4 0 503.429 15.9203 1
3 4 0 506.486 12.8488 3
-3 4 0 508.193 13.1598 3
-4 -4 0 454.277 11.7297 3
-4 -4 0 439.511 14.5183 1
-4 4 0 449.497 11.9097 3
-4 4 0 470.800 15.4869 1
4 4 0 440.718 11.4830 3
4 4 0 439.810 11.4910 3
5 -4 0 1680.25 42.4963 3
-5 -4 0 1660.08 42.4638 3
-5 -4 0 1718.82 46.4354 1
5 4 0 1711.99 42.1257 3
5 4 0 1663.26 42.1158 3
-5 4 0 1686.17 47.2357 1
-5 4 0 1690.78 42.6740 3
-6 -4 0 178.684 5.60051 3
-6 -4 0 187.988 9.65388 1
6 -4 0 188.471 5.60515 3
6 -4 0 180.249 9.83303 1
6 4 0 181.362 5.03991 3
-6 4 0 190.033 10.1212 1
6 4 0 182.585 5.04304 3
-6 4 0 179.826 5.82639 3
-7 -4 0 25.9067 4.86591 1
7 -4 0 29.1634 1.95827 3
-7 -4 0 29.6401 2.10178 3
7 -4 0 32.8385 5.25203 1
7 4 0 30.3463 1.20357 3
-7 4 0 20.0317 5.17583 1
-7 4 0 32.0421 2.33123 3
7 4 0 30.7422 1.25348 3
-8 -4 0 0.23698 4.52335 1
8 -4 0 4.59658 4.23745 1
-8 -4 0 -0.6822 0.90567 3
8 -4 0 0.02662 0.78990 3
-8 4 0 -1.1857 4.60099 1
-8 4 0 -1.5525 0.99274 3
9 -4 0 0.90933 6.02151 1
-9 -4 0 2.69297 6.55269 1
-9 4 0 -0.4739 1.09970 3
-9 4 0 5.86683 7.46028 1
0 -5 0 -0.0608 0.84730 1
0 -5 0 0.51813 0.34679 3
0 5 0 -0.0226 0.81812 1
0 5 0 0.60764 0.32897 3
-1 -5 0 4669.06 117.181 1
2 -5 0 471.742 14.8844 1
2 -5 0 503.720 12.6690 3
-2 -5 0 483.389 12.4814 3
-2 -5 0 469.230 14.1962 1
-2 -5 0 485.767 12.4890 3
2 5 0 489.970 12.4028 3
2 5 0 498.076 12.4231 3
-2 5 0 491.113 12.6597 3
-2 5 0 519.350 15.3321 1
-3 -5 0 2447.53 64.7102 1
3 -5 0 2485.02 65.6155 1
-3 5 0 2579.35 65.9632 1
4 -5 0 148.137 7.54689 1
-4 -5 0 153.441 4.42699 3
-4 -5 0 139.873 6.88171 1
-4 -5 0 148.863 4.39843 3
4 5 0 147.971 4.14556 3
-4 5 0 152.543 4.67187 3
4 5 0 151.749 4.15368 3
-4 5 0 157.566 7.80965 1
-5 -5 0 553.387 18.2571 1
-5 -5 0 538.075 14.4977 3
5 -5 0 563.496 14.6305 3
-5 5 0 574.520 19.3345 1
5 5 0 555.653 14.1247 3
-5 5 0 543.643 14.7470 3
5 5 0 551.622 14.1179 3
-6 -5 0 222.279 10.5403 1
-6 -5 0 206.411 6.33429 3
6 -5 0 211.365 6.36647 3
6 -5 0 218.625 10.4739 1
6 5 0 211.532 5.71501 3
-6 5 0 214.748 6.65766 3
-6 5 0 218.567 11.5926 1
6 5 0 212.107 5.71907 3
7 -5 0 72.5302 7.41582 1
-7 -5 0 54.8250 6.24745 1
-7 -5 0 64.7528 2.98442 3
7 -5 0 71.8664 2.93576 3
-7 5 0 66.3073 3.25741 3
-7 5 0 74.4688 7.81492 1
8 -5 0 -0.9652 0.83022 3
8 -5 0 -1.0896 4.34008 1
-8 -5 0 -0.3852 0.94651 3
-8 -5 0 3.04727 4.76224 1
-8 5 0 9.48083 5.78248 1
-8 5 0 0.51993 1.23088 3
-9 -5 0 10.8791 6.93036 1
9 -5 0 16.8161 6.80128 1
-9 -5 0 16.8089 1.81200 3
9 -5 0 18.1000 1.67460 3
-9 5 0 9.90403 8.22212 1
-9 5 0 21.4307 2.16502 3
0 -6 0 462.346 11.9572 3
0 -6 0 477.447 13.9041 1
0 6 0 464.718 13.8641 1
0 6 0 464.386 11.9394 3
1 -6 0 1123.19 30.7515 1
-1 -6 0 1104.24 30.1909 1
1 -6 0 1159.94 28.5079 3
-1 -6 0 1113.97 28.3880 3
1 6 0 1163.92 30.2372 1
-1 6 0 1170.21 30.9073 1
-1 6 0 1108.15 28.4672 3
1 6 0 1129.02 28.3494 3
-2 -6 0 2013.29 54.1880 1
2 -6 0 2136.34 55.1694 1
-2 6 0 2138.80 55.4125 1
-3 -6 0 592.154 15.4473 3
-3 -6 0 594.477 15.4546 3
-3 -6 0 606.791 17.9789 1
3 -6 0 588.237 18.7098 1
3 -6 0 604.396 15.6580 3
-3 6 0 609.210 19.0534 1
3 6 0 621.277 15.2978 3
-3 6 0 608.841 15.7045 3
3 6 0 613.931 15.3154 3
-4 -6 0 5.40581 0.79519 3
4 -6 0 7.39633 0.88180 3
4 -6 0 4.27402 2.34029 1
-4 -6 0 4.86425 0.74730 3
-4 -6 0 3.90825 2.02764 1
-4 6 0 6.04546 2.57410 1
4 6 0 5.15889 0.56797 3
-4 6 0 4.41891 0.88628 3
-5 -6 0 134.189 4.24022 3
5 -6 0 116.915 7.89545 1
-5 -6 0 133.639 7.43988 1
-5 6 0 129.831 8.25608 1
-5 6 0 137.137 4.55270 3
5 6 0 138.070 3.78478 3
5 6 0 136.360 3.78940 3
-6 -6 0 10.6565 3.45141 1
-6 -6 0 13.9699 1.38087 3
6 -6 0 17.2236 1.57383 3
6 6 0 15.5022 0.96255 3
-6 6 0 8.99860 4.21043 1
-6 6 0 12.4406 1.53385 3
6 6 0 16.2131 0.96653 3
-7 -6 0 3.97092 3.98889 1
7 -6 0 12.3535 4.16388 1
-7 -6 0 8.78517 1.29239 3
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0 12 -17 18.6320 2.32413 3
4 -13 -17 19.7918 2.44092 3
4 13 -17 15.5465 2.50427 3
3 -13 -17 -1.1941 1.40809 3
-3 13 17 -7.1778 8.39189 1
3 13 -17 4.04506 1.81254 3
2 -13 -17 10.7634 1.75176 3
2 13 -17 10.1659 2.12186 3
1 -13 -17 19.3120 1.92633 3
1 13 -17 19.9813 2.50559 3
0 -13 -17 6.95224 1.33669 3
0 -13 -17 4.46215 1.10897 3
0 13 -17 2.63668 1.67704 3
3 -14 -17 5.68125 1.59384 3
3 14 -17 2.37057 2.07839 3
-3 14 17 4.21033 8.57020 1
2 -14 -17 1.36097 1.31718 3
2 14 -17 1.23689 1.71204 3
1 -14 -17 -0.4622 1.06551 3
1 14 -17 -1.0601 1.74399 3
5 0 -18 0.71237 1.50594 3
4 0 -18 47.1451 3.58983 3
-4 0 18 36.0687 11.1941 1
-3 0 18 -3.5090 8.61893 1
3 0 -18 -3.9407 1.28009 3
-2 0 18 2.73403 7.23726 1
2 0 -18 4.64135 1.60456 3
2 0 -18 4.53122 1.61133 3
-1 0 18 0.72230 4.84645 1
1 0 -18 2.11412 1.30142 3
0 0 -18 390.765 11.4188 3
0 0 -18 373.042 11.2564 3
-1 0 -18 0.26510 1.21212 3
-1 0 -18 1.20965 1.25237 3
5 -1 -18 -2.0611 1.24492 3
5 1 -18 0.91235 1.64181 3
-4 -1 18 -0.4860 10.1053 1
4 -1 -18 0.49827 1.43810 3
-4 1 18 -1.8507 10.1353 1
4 1 -18 2.22735 1.69787 3
3 -1 -18 0.85434 1.50199 3
-3 -1 18 -5.4669 8.90324 1
3 1 -18 1.62924 1.58847 3
-3 1 18 -5.6672 8.15714 1
2 -1 -18 12.5729 1.86738 3
-2 -1 18 18.8085 7.90253 1
2 -1 -18 9.66480 1.76221 3
2 1 -18 14.7509 2.12438 3
2 1 -18 13.4667 2.19561 3
-2 1 18 6.30353 7.17910 1
1 -1 -18 8.41922 1.78758 3
-1 -1 18 -1.5341 5.79105 1
1 -1 -18 8.00721 1.67283 3
-1 1 18 8.64377 4.32769 1
1 1 -18 6.56264 1.51911 3
1 1 -18 6.20385 1.69913 3
0 -1 -18 2.10031 1.31028 3
0 -1 -18 0.18140 1.42213 3
0 1 -18 1.23225 1.57855 3
0 1 -18 -0.5294 1.28537 3
-1 -1 -18 1.09415 1.21090 3
-1 -1 -18 0.61396 1.20811 3
-1 1 -18 2.01432 1.33740 3
-1 1 -18 1.02886 1.29506 3
5 -2 -18 19.4632 2.24854 3
5 2 -18 20.8172 2.44735 3
-4 -2 18 26.8514 11.9249 1
4 -2 -18 42.7273 3.36683 3
4 2 -18 41.4174 3.50407 3
-4 2 18 46.2367 10.9729 1
-3 -2 18 25.0502 9.86569 1
3 -2 -18 28.1438 2.96443 3
3 2 -18 23.6962 2.59964 3
-3 2 18 5.54842 8.25055 1
-2 -2 18 28.3046 8.31847 1
2 -2 -18 20.3377 2.25114 3
2 -2 -18 16.7811 2.00631 3
2 2 -18 26.3163 2.57995 3
-2 2 18 19.1086 7.15916 1
1 -2 -18 25.1057 2.45742 3
1 -2 -18 24.7415 2.62876 3
-1 -2 18 17.3168 6.67853 1
1 2 -18 16.6036 2.07169 3
1 2 -18 23.4493 2.45123 3
0 -2 -18 -1.0742 0.96315 3
0 -2 -18 0.04606 1.18026 3
0 2 -18 3.70396 1.53210 3
0 2 -18 1.20020 1.42538 3
-1 -2 -18 65.1342 3.24879 3
-1 -2 -18 61.3389 3.17830 3
-1 2 -18 63.6986 5.20045 3
-1 2 -18 58.7718 3.49732 3
5 -3 -18 2.55860 1.64773 3
5 3 -18 0.23883 1.79769 3
-4 -3 18 -5.4730 12.2200 1
4 -3 -18 2.90286 1.49917 3
4 3 -18 2.29326 1.63155 3
-4 3 18 -3.3384 9.67778 1
3 -3 -18 6.26402 1.70197 3
-3 -3 18 12.9207 9.41477 1
-3 3 18 1.07690 8.52919 1
3 3 -18 5.64934 1.81905 3
2 -3 -18 79.7531 4.12877 3
2 -3 -18 80.3866 4.00183 3
-2 -3 18 81.6525 10.5409 1
2 3 -18 86.4831 4.49451 3
-2 3 18 68.5323 8.44409 1
1 -3 -18 0.72056 1.27619 3
-1 -3 18 6.68116 6.88262 1
1 -3 -18 1.37469 1.21513 3
1 3 -18 2.44906 1.53411 3
1 3 -18 1.76218 2.08617 3
0 -3 -18 7.51267 1.42970 3
0 -3 -18 3.03366 1.21336 3
0 3 -18 3.20365 2.50288 3
0 3 -18 2.61844 1.35019 3
-1 -3 -18 -0.8218 1.01870 3
-1 -3 -18 -1.3469 0.98608 3
-1 3 -18 0.89694 1.24467 3
5 -4 -18 28.5764 3.12053 3
5 4 -18 21.4946 2.54999 3
4 -4 -18 11.2529 1.96163 3
-4 4 18 17.1151 10.6016 1
3 -4 -18 13.5663 2.02708 3
-3 -4 18 8.73067 9.73743 1
3 4 -18 13.2750 2.17583 3
-3 4 18 14.6105 8.69054 1
-2 -4 18 14.4096 8.92685 1
2 -4 -18 20.1598 2.12927 3
2 -4 -18 27.3134 2.77941 3
-2 4 18 17.7021 6.36492 1
2 4 -18 20.9214 2.32627 3
-1 -4 18 13.3123 7.57133 1
1 -4 -18 4.26904 1.43107 3
1 -4 -18 4.57593 1.33973 3
1 4 -18 2.85365 1.51952 3
0 -4 18 -3.0666 5.04599 1
0 -4 -18 0.47159 0.96681 3
0 -4 -18 -1.3733 1.00093 3
0 4 -18 -0.3189 1.24927 3
-1 -4 -18 5.19630 1.22338 3
-1 -4 -18 2.38871 1.09226 3
-1 4 -18 7.35739 1.48786 3
5 -5 -18 -0.4431 1.47726 3
5 5 -18 1.79121 1.72748 3
4 -5 -18 5.23480 1.82060 3
-4 5 18 15.3356 11.8124 1
4 5 -18 2.25423 1.73989 3
-3 -5 18 29.4130 11.4086 1
3 -5 -18 59.5644 3.63459 3
-3 5 18 55.5217 9.91136 1
3 5 -18 56.0086 3.93600 3
2 -5 -18 0.73852 1.24441 3
2 -5 -18 -1.1285 1.28111 3
-2 -5 18 -0.5334 9.15798 1
-2 5 18 -7.3647 5.71880 1
2 5 -18 4.94553 1.83868 3
1 -5 -18 52.1881 3.04535 3
1 -5 -18 58.3060 3.28263 3
-1 -5 18 38.8737 8.77818 1
1 5 -18 57.7562 3.67794 3
0 -5 -18 -1.4368 0.94776 3
0 -5 18 -2.4541 6.32301 1
0 -5 -18 1.29972 1.06159 3
0 5 -18 -0.9057 1.29936 3
-1 -5 -18 4.53856 1.07517 3
-1 -5 -18 2.79145 1.09891 3
-1 5 -18 1.54930 1.31911 3
5 -6 -18 20.4239 2.45756 3
5 6 -18 27.7242 2.94925 3
4 -6 -18 2.41362 1.53068 3
4 6 -18 1.56113 1.60743 3
3 -6 -18 1.21626 1.35395 3
-3 -6 18 -6.2979 11.6987 1
-3 6 18 -5.9189 8.27292 1
3 6 -18 -0.8860 1.63154 3
2 -6 -18 -0.2834 1.47515 3
-2 -6 18 3.63867 9.70868 1
2 -6 -18 2.18033 1.27145 3
2 6 -18 0.44704 1.50924 3
-2 6 18 -9.1293 5.21626 1
1 -6 -18 8.56089 1.48210 3
-1 -6 18 7.82907 8.78455 1
1 -6 -18 10.5801 1.46681 3
1 6 -18 10.9723 1.97031 3
0 -6 -18 5.84399 1.25645 3
0 -6 -18 6.77389 1.29216 3
0 -6 18 13.7582 7.55460 1
0 6 -18 5.31700 1.53337 3
-1 -6 -18 4.30032 1.10247 3
-1 -6 -18 4.93069 1.09755 3
-1 6 -18 1.66984 1.43137 3
5 -7 -18 7.49655 1.92166 3
5 7 -18 10.2448 2.21574 3
4 -7 -18 1.77895 1.46506 3
4 7 -18 -0.4193 1.59791 3
3 -7 -18 5.71347 1.58233 3
3 7 -18 3.70707 1.70977 3
-3 7 18 13.4704 8.47045 1
-2 -7 18 24.3018 11.1638 1
2 -7 -18 17.6977 2.00703 3
-2 7 18 19.3047 6.00771 1
2 7 -18 18.1433 2.33767 3
-1 -7 18 18.5913 9.43330 1
1 -7 -18 26.6754 2.40926 3
1 -7 -18 23.6098 2.26053 3
1 7 -18 27.5678 3.03755 3
0 -7 -18 0.67552 0.92897 3
0 -7 -18 1.61331 1.00737 3
0 -7 18 1.74537 8.39852 1
0 7 -18 -1.9531 1.28252 3
-1 -7 -18 9.50167 1.30802 3
4 -8 -18 31.0263 2.98369 3
4 8 -18 28.3556 3.06606 3
3 -8 -18 6.67247 1.72153 3
3 8 -18 8.61822 1.91836 3
-3 8 18 16.8063 8.60080 1
2 -8 -18 -0.5479 1.11128 3
2 8 -18 -0.0272 1.61701 3
-1 -8 18 -11.435 13.6073 1
1 -8 -18 -0.3769 0.99699 3
1 -8 -18 0.52602 1.10380 3
1 8 -18 -0.1389 1.45379 3
0 -8 18 -5.5382 9.25947 1
0 -8 -18 1.82788 0.98137 3
0 -8 -18 2.71027 0.97939 3
0 8 -18 0.81376 1.44316 3
4 -9 -18 1.89375 1.49313 3
4 9 -18 0.16592 1.85589 3
3 -9 -18 4.12010 1.54368 3
-3 9 18 2.83885 8.48978 1
3 9 -18 3.78060 1.81670 3
2 -9 -18 41.0615 3.01030 3
2 9 -18 41.9104 3.67135 3
1 -9 -18 1.81947 1.18097 3
1 9 -18 -0.0716 1.46898 3
0 -9 -18 2.00342 1.06044 3
0 -9 -18 4.27666 1.10467 3
0 9 -18 4.25851 1.68093 3
3 -10 -18 -0.1591 1.37352 3
3 10 -18 0.07251 1.63108 3
-3 10 18 -16.081 8.33526 1
2 -10 -18 0.59824 1.21881 3
2 10 -18 -0.9365 1.68062 3
1 -10 -18 -0.7546 1.07931 3
1 10 -18 1.01519 1.65011 3
2 -11 -18 41.0392 2.98379 3
2 11 -18 40.2173 3.60162 3
4 0 -19 -1.0512 1.50378 3
3 0 -19 0.12607 1.38577 3
2 0 -19 1.14866 1.48221 3
-2 0 19 -1.3347 8.50394 1
1 0 -19 31.7761 2.96516 3
4 -1 -19 0.24030 1.50572 3
4 1 -19 1.63792 1.58737 3
3 -1 -19 15.2055 2.10197 3
3 1 -19 11.3996 1.92333 3
-2 -1 19 -14.682 9.06775 1
2 -1 -19 0.45185 1.41741 3
2 1 -19 2.46855 1.67890 3
-2 1 19 -12.260 8.13145 1
1 -1 -19 2.86922 1.46018 3
1 1 -19 1.11875 1.49128 3
4 -2 -19 0.52929 1.54752 3
4 2 -19 -1.2277 1.45078 3
3 -2 -19 9.25707 1.78364 3
3 2 -19 11.7968 1.94279 3
2 -2 -19 44.5395 3.37912 3
-2 -2 19 46.4876 10.7910 1
2 2 -19 50.4518 3.63372 3
-2 2 19 41.9843 8.34425 1
1 -2 -19 67.2677 3.77841 3
-1 -2 19 63.8496 10.8564 1
1 2 -19 71.3906 4.05487 3
4 -3 -19 17.6547 2.34653 3
3 -3 -19 3.06309 1.56382 3
3 3 -19 3.13254 1.80918 3
2 -3 -19 4.62896 1.64119 3
-2 3 19 9.50316 7.15186 1
2 3 -19 3.94028 1.69461 3
1 -3 -19 4.72134 1.48563 3
-1 -3 19 -6.3681 7.93146 1
1 3 -19 2.78348 1.57461 3
3 -4 -19 -1.3872 1.34333 3
3 4 -19 -1.3596 1.41762 3
2 -4 -19 31.1412 2.94141 3
2 4 -19 39.3527 3.38999 3
-1 -4 19 -4.3302 8.80521 1
1 -4 -19 1.93726 1.28337 3
1 4 -19 2.79348 1.62369 3
3 -5 -19 5.39545 1.58376 3
3 5 -19 8.68397 2.06518 3
2 -5 -19 8.45487 1.68054 3
2 5 -19 12.4830 2.18236 3
1 -5 -19 1.33127 1.20063 3
1 5 -19 -1.3972 1.33572 3
2 -6 -19 13.8796 1.89839 3
2 6 -19 16.1975 2.26844 3
0 0 0 0.00 0.00 0
_exptl_absorpt_process_details
)
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
J. Appl. Cryst. 48 (2015) 3-10
)
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_max 0.7465
_exptl_absorpt_correction_T_min 0.6620
_exptl_special_details
)
The following wavelength and cell were deduced by SADABS from the
direction cosines etc. They are given here for emergency use only:
CELL 0.71081 6.857 19.460 12.619 89.997 102.048 90.001
)
;
_shelx_hkl_checksum 13954
_shelx_res_file
;
TITL GO_1_0m_a.res in P2(1)/n
2.res
created by SHELXL-2018/3 at 10:25:05 on 31-Jan-2024
REM Old TITL GO_1_0m in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.150, Rweak 0.007, Alpha 0.028
REM 0.958 for 110 systematic absences, Orientation as input
REM Formula found by SHELXT: C14 N O3 F3 S
CELL 0.71073 6.8580 19.4619 12.6131 90.000 102.024 90.000
ZERR 4.000 0.0004 0.0012 0.0007 0.000 0.002 0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C H N O F S
UNIT 56 80 4 12 12 4
TEMP -123.150
SIZE 0.45 0.43 0.32
L.S. 1
BOND $H
ACTA
CONF
LIST 4
FMAP 2
PLAN 20
HTAB
EQIV $1 x+1, y, z
EQIV $2 x+1/2, -y+3/2, z+1/2
HTAB C11 O1_$1
REM HTAB C11 O3_$1
EQIV $3 x+3/2, -y+3/2, z+1/2
REM HTAB C11 F3_$2
REM HTAB C11 O2_$2
EQIV $4 -x+3/2, y-1/2, -z+3/2
HTAB C12 F2_$4
REM HTAB C12 O2_$3
REM HTAB C12 O3_$1
HTAB C13 O1_$1
HTAB C13 O2_$2
HTAB C13 O3
MPLA C1 N1 C10 C11 C12 C13
MPLA 7 N1 C1 C2 C3 C4 C5 C6 C7 C8 C9
WGHT 0.064700 0.652500
FVAR 0.75029
S1 6 0.154786 0.797801 0.613914 11.00000 0.02328 0.02674 =
0.02618 -0.00088 0.00446 -0.00154
F1 5 0.376060 0.862871 0.775615 11.00000 0.12447 0.08827 =
0.03210 -0.00966 -0.00771 -0.05453
F2 5 0.252980 0.927438 0.641881 11.00000 0.09691 0.02803 =
0.07955 -0.00498 0.03036 -0.01204
F3 5 0.495016 0.861457 0.631584 11.00000 0.04313 0.08754 =
0.09411 -0.03371 0.02484 -0.03452
O1 4 -0.021069 0.813551 0.653532 11.00000 0.03960 0.04687 =
0.06950 -0.00240 0.02913 -0.00095
O2 4 0.134079 0.804378 0.498946 11.00000 0.06120 0.06163 =
0.02825 -0.00462 0.00678 -0.01983
O3 4 0.256153 0.736566 0.660544 11.00000 0.04054 0.03087 =
0.07076 0.00160 -0.00360 0.00428
N1 3 0.865353 0.641444 0.770995 11.00000 0.02319 0.01958 =
0.02657 0.00095 0.00425 0.00165
C1 1 0.812043 0.575680 0.717315 11.00000 0.02206 0.01913 =
0.02860 0.00113 0.00359 -0.00061
C2 1 0.739191 0.523577 0.774983 11.00000 0.02348 0.02353 =
0.03242 0.00632 0.00500 0.00095
C3 1 0.682164 0.462174 0.720579 11.00000 0.02588 0.02058 =
0.04607 0.00710 0.00632 -0.00125
AFIX 43
H3 2 0.631492 0.426053 0.757740 11.00000 -1.20000
AFIX 0
C4 1 0.697272 0.452263 0.613609 11.00000 0.02646 0.02044 =
0.04656 -0.00264 0.00316 -0.00254
C5 1 0.769584 0.505694 0.559463 11.00000 0.03507 0.02687 =
0.03353 -0.00460 0.00622 -0.00431
AFIX 43
H5 2 0.779749 0.499239 0.486153 11.00000 -1.20000
AFIX 0
C6 1 0.827524 0.568362 0.609485 11.00000 0.02935 0.02279 =
0.02878 0.00025 0.00686 -0.00322
C7 1 0.727495 0.532169 0.892153 11.00000 0.04012 0.03875 =
0.03348 0.00989 0.01100 0.00109
AFIX 137
H7A 2 0.675490 0.577958 0.903002 11.00000 -1.50000
H7B 2 0.860854 0.526986 0.937972 11.00000 -1.50000
H7C 2 0.638530 0.497155 0.911733 11.00000 -1.50000
AFIX 0
C8 1 0.637682 0.384450 0.558175 11.00000 0.04039 0.02474 =
0.06811 -0.01146 0.00728 -0.00768
AFIX 137
H8A 2 0.613907 0.390669 0.479424 11.00000 -1.50000
H8B 2 0.515577 0.367745 0.578344 11.00000 -1.50000
H8C 2 0.744876 0.350912 0.580769 11.00000 -1.50000
AFIX 0
C9 1 0.904738 0.625689 0.549630 11.00000 0.04962 0.02976 =
0.03279 0.00056 0.01454 -0.01069
AFIX 137
H9A 2 0.898812 0.611766 0.474357 11.00000 -1.50000
H9B 2 1.043117 0.635892 0.584635 11.00000 -1.50000
H9C 2 0.822601 0.666766 0.550892 11.00000 -1.50000
AFIX 0
C10 1 1.039052 0.652571 0.831806 11.00000 0.02571 0.02372 =
0.03105 0.00158 0.00216 -0.00040
C11 1 1.081853 0.718410 0.891988 11.00000 0.04047 0.02996 =
0.03670 -0.00645 0.00036 -0.00561
AFIX 137
H11A 2 1.071297 0.756521 0.840322 11.00000 -1.50000
H11B 2 1.217001 0.717058 0.936743 11.00000 -1.50000
H11C 2 0.985468 0.725038 0.938559 11.00000 -1.50000
AFIX 0
C12 1 1.200418 0.600564 0.843441 11.00000 0.02564 0.03165 =
0.06038 0.00329 -0.00417 0.00394
AFIX 137
H12A 2 1.148345 0.558503 0.805015 11.00000 -1.50000
H12B 2 1.249569 0.590234 0.920420 11.00000 -1.50000
H12C 2 1.309884 0.618616 0.812571 11.00000 -1.50000
AFIX 0
C13 1 0.706362 0.694615 0.753336 11.00000 0.02660 0.02531 =
0.03600 0.00236 0.00658 0.00755
AFIX 137
H13A 2 0.758175 0.737207 0.728243 11.00000 -1.50000
H13B 2 0.663458 0.703278 0.821535 11.00000 -1.50000
H13C 2 0.592598 0.678426 0.698583 11.00000 -1.50000
AFIX 0
C14 1 0.330020 0.865522 0.669495 11.00000 0.04786 0.03447 =
0.03440 -0.00671 0.01015 -0.01320
HKLF 4
REM GO_1_0m_a.res in P2(1)/n
REM wR2 = 0.1356, GooF = S = 1.044, Restrained GooF = 1.044 for all data
REM R1 = 0.0454 for 4836 Fo > 4sig(Fo) and 0.0649 for all 6151 data
REM 205 parameters refined using 0 restraints
END
WGHT 0.0647 0.6554
REM Instructions for potential hydrogen bonds
HTAB C11 O1_$1
HTAB C13 O1_$1
HTAB C13 O2_$2
HTAB C13 O3
REM Highest difference peak 0.626, deepest hole -0.413, 1-sigma level 0.061
Q1 1 0.2846 0.7490 0.5951 11.00000 0.05 0.63
Q2 1 0.0621 0.7920 0.6983 11.00000 0.05 0.57
Q3 1 0.2758 0.9224 0.7220 11.00000 0.05 0.57
Q4 1 0.0733 0.8396 0.5159 11.00000 0.05 0.54
Q5 1 0.5046 0.8530 0.7006 11.00000 0.05 0.44
Q6 1 0.4707 0.8299 0.7510 11.00000 0.05 0.34
Q7 1 0.8221 0.5718 0.6593 11.00000 0.05 0.32
Q8 1 0.2355 0.7992 0.5236 11.00000 0.05 0.30
Q9 1 0.7627 0.5495 0.7419 11.00000 0.05 0.30
Q10 1 0.7212 0.5296 0.8365 11.00000 0.05 0.28
Q11 1 0.7047 0.4932 0.7447 11.00000 0.05 0.28
Q12 1 1.1121 0.6274 0.8356 11.00000 0.05 0.26
Q13 1 0.4616 0.8954 0.6217 11.00000 0.05 0.25
Q14 1 0.9484 0.6491 0.8039 11.00000 0.05 0.25
Q15 1 0.7024 0.4590 0.6659 11.00000 0.05 0.24
Q16 1 1.0344 0.6884 0.8637 11.00000 0.05 0.24
Q17 1 0.8539 0.5965 0.5823 11.00000 0.05 0.24
Q18 1 1.0656 0.7177 0.9447 11.00000 0.05 0.23
Q19 1 0.6937 0.4278 0.5967 11.00000 0.05 0.22
Q20 1 0.7684 0.4719 0.5960 11.00000 0.05 0.22
;
_shelx_res_checksum 2745
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
S S1 0.15479(4) 0.79780(2) 0.61391(2) 0.02550(8) Uani d 1 . .
F F1 0.3761(3) 0.86287(8) 0.77561(9) 0.0851(5) Uani d 1 . .
F F2 0.2530(2) 0.92744(5) 0.64188(11) 0.0664(3) Uani d 1 . .
F F3 0.49502(18) 0.86146(8) 0.63158(12) 0.0734(4) Uani d 1 . .
O O1 -0.02107(18) 0.81355(7) 0.65353(12) 0.0494(3) Uani d 1 . .
O O2 0.1341(2) 0.80438(7) 0.49895(9) 0.0507(3) Uani d 1 . .
O O3 0.25615(18) 0.73657(6) 0.66054(11) 0.0496(3) Uani d 1 . .
N N1 0.86535(15) 0.64144(5) 0.77099(8) 0.02325(18) Uani d 1 . .
C C1 0.81204(17) 0.57568(6) 0.71732(9) 0.0235(2) Uani d 1 . .
C C2 0.73919(18) 0.52358(6) 0.77498(10) 0.0266(2) Uani d 1 . .
C C3 0.68216(19) 0.46217(6) 0.72058(12) 0.0310(3) Uani d 1 . .
H H3 0.631492 0.426053 0.757740 0.037 Uiso calc 1 . .
C C4 0.69727(19) 0.45226(7) 0.61361(12) 0.0318(3) Uani d 1 . .
C C5 0.7696(2) 0.50569(7) 0.55946(11) 0.0320(3) Uani d 1 . .
H H5 0.779749 0.499239 0.486153 0.038 Uiso calc 1 . .
C C6 0.82752(19) 0.56836(6) 0.60949(10) 0.0269(2) Uani d 1 . .
C C7 0.7275(2) 0.53217(8) 0.89215(12) 0.0370(3) Uani d 1 . .
H H7A 0.675490 0.577958 0.903002 0.055 Uiso calc 1 . .
H H7B 0.860854 0.526986 0.937972 0.055 Uiso calc 1 . .
H H7C 0.638530 0.497155 0.911733 0.055 Uiso calc 1 . .
C C8 0.6377(2) 0.38445(8) 0.55818(16) 0.0450(4) Uani d 1 . .
H H8A 0.613907 0.390669 0.479424 0.067 Uiso calc 1 . .
H H8B 0.515577 0.367745 0.578344 0.067 Uiso calc 1 . .
H H8C 0.744876 0.350912 0.580769 0.067 Uiso calc 1 . .
C C9 0.9047(2) 0.62569(7) 0.54963(12) 0.0365(3) Uani d 1 . .
H H9A 0.898812 0.611766 0.474357 0.055 Uiso calc 1 . .
H H9B 1.043117 0.635892 0.584635 0.055 Uiso calc 1 . .
H H9C 0.822601 0.666766 0.550892 0.055 Uiso calc 1 . .
C C10 1.03905(18) 0.65257(6) 0.83181(10) 0.0274(2) Uani d 1 . .
C C11 1.0819(2) 0.71841(7) 0.89199(12) 0.0368(3) Uani d 1 . .
H H11A 1.071297 0.756521 0.840322 0.055 Uiso calc 1 . .
H H11B 1.217001 0.717058 0.936743 0.055 Uiso calc 1 . .
H H11C 0.985468 0.725038 0.938559 0.055 Uiso calc 1 . .
C C12 1.2004(2) 0.60056(8) 0.84344(15) 0.0411(3) Uani d 1 . .
H H12A 1.148345 0.558503 0.805015 0.062 Uiso calc 1 . .
H H12B 1.249569 0.590234 0.920420 0.062 Uiso calc 1 . .
H H12C 1.309884 0.618616 0.812571 0.062 Uiso calc 1 . .
C C13 0.70636(19) 0.69461(6) 0.75334(11) 0.0293(2) Uani d 1 . .
H H13A 0.758175 0.737207 0.728243 0.044 Uiso calc 1 . .
H H13B 0.663458 0.703278 0.821535 0.044 Uiso calc 1 . .
H H13C 0.592598 0.678426 0.698583 0.044 Uiso calc 1 . .
C C14 0.3300(3) 0.86552(8) 0.66949(12) 0.0387(3) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
S1 0.02328(14) 0.02674(14) 0.02618(14) -0.00154(10) 0.00446(10) -0.00088(10)
F1 0.1245(13) 0.0883(10) 0.0321(5) -0.0545(9) -0.0077(6) -0.0097(6)
F2 0.0969(10) 0.0280(5) 0.0795(8) -0.0120(5) 0.0304(7) -0.0050(5)
F3 0.0431(6) 0.0875(9) 0.0941(10) -0.0345(6) 0.0248(6) -0.0337(8)
O1 0.0396(6) 0.0469(6) 0.0695(8) -0.0009(5) 0.0291(6) -0.0024(6)
O2 0.0612(8) 0.0616(8) 0.0282(5) -0.0198(6) 0.0068(5) -0.0046(5)
O3 0.0405(6) 0.0309(5) 0.0708(8) 0.0043(4) -0.0036(6) 0.0016(5)
N1 0.0232(4) 0.0196(4) 0.0266(4) 0.0017(3) 0.0043(3) 0.0010(3)
C1 0.0221(5) 0.0191(4) 0.0286(5) -0.0006(4) 0.0036(4) 0.0011(4)
C2 0.0235(5) 0.0235(5) 0.0324(5) 0.0009(4) 0.0050(4) 0.0063(4)
C3 0.0259(6) 0.0206(5) 0.0461(7) -0.0013(4) 0.0063(5) 0.0071(5)
C4 0.0265(6) 0.0204(5) 0.0466(7) -0.0025(4) 0.0032(5) -0.0026(5)
C5 0.0351(6) 0.0269(6) 0.0335(6) -0.0043(5) 0.0062(5) -0.0046(5)
C6 0.0293(6) 0.0228(5) 0.0288(5) -0.0032(4) 0.0069(4) 0.0002(4)
C7 0.0401(7) 0.0387(7) 0.0335(6) 0.0011(6) 0.0110(5) 0.0099(5)
C8 0.0404(8) 0.0247(6) 0.0681(11) -0.0077(5) 0.0073(7) -0.0115(6)
C9 0.0496(8) 0.0298(6) 0.0328(6) -0.0107(6) 0.0145(6) 0.0006(5)
C10 0.0257(5) 0.0237(5) 0.0310(5) -0.0004(4) 0.0022(4) 0.0016(4)
C11 0.0405(7) 0.0300(6) 0.0367(6) -0.0056(5) 0.0004(5) -0.0065(5)
C12 0.0256(6) 0.0317(7) 0.0604(9) 0.0039(5) -0.0042(6) 0.0033(6)
C13 0.0266(6) 0.0253(5) 0.0360(6) 0.0076(4) 0.0066(5) 0.0024(4)
C14 0.0479(8) 0.0345(7) 0.0344(6) -0.0132(6) 0.0101(6) -0.0067(5)
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'
N N 0.0061 0.0033 '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
O1 S1 O2 . . 114.90(9) ?
O1 S1 O3 . . 113.84(8) ?
O2 S1 O3 . . 115.11(8) ?
O1 S1 C14 . . 104.29(8) ?
O2 S1 C14 . . 104.07(7) ?
O3 S1 C14 . . 102.57(8) ?
C10 N1 C1 . . 122.21(10) ?
C10 N1 C13 . . 121.91(11) ?
C1 N1 C13 . . 115.87(10) ?
C6 C1 C2 . . 122.77(11) ?
C6 C1 N1 . . 118.69(10) ?
C2 C1 N1 . . 118.47(11) ?
C3 C2 C1 . . 117.36(12) ?
C3 C2 C7 . . 120.79(12) ?
C1 C2 C7 . . 121.83(12) ?
C4 C3 C2 . . 121.87(12) ?
C4 C3 H3 . . 119.1 ?
C2 C3 H3 . . 119.1 ?
C3 C4 C5 . . 118.67(12) ?
C3 C4 C8 . . 120.26(13) ?
C5 C4 C8 . . 121.06(14) ?
C4 C5 C6 . . 121.98(12) ?
C4 C5 H5 . . 119.0 ?
C6 C5 H5 . . 119.0 ?
C5 C6 C1 . . 117.34(11) ?
C5 C6 C9 . . 121.29(12) ?
C1 C6 C9 . . 121.37(11) ?
C2 C7 H7A . . 109.5 ?
C2 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
C2 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
C4 C8 H8A . . 109.5 ?
C4 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C4 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
C6 C9 H9A . . 109.5 ?
C6 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
C6 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
N1 C10 C12 . . 121.33(12) ?
N1 C10 C11 . . 120.42(12) ?
C12 C10 C11 . . 118.25(12) ?
C10 C11 H11A . . 109.5 ?
C10 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C10 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C10 C12 H12A . . 109.5 ?
C10 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C10 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
N1 C13 H13A . . 109.5 ?
N1 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
N1 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
F1 C14 F3 . . 108.99(16) ?
F1 C14 F2 . . 107.49(14) ?
F3 C14 F2 . . 106.43(14) ?
F1 C14 S1 . . 111.32(11) ?
F3 C14 S1 . . 111.33(11) ?
F2 C14 S1 . . 111.08(12) ?
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 O1 . 1.4315(12) ?
S1 O2 . 1.4330(12) ?
S1 O3 . 1.4419(12) ?
S1 C14 . 1.8226(15) ?
F1 C14 . 1.3107(18) ?
F2 C14 . 1.333(2) ?
F3 C14 . 1.319(2) ?
N1 C10 . 1.2937(16) ?
N1 C1 . 1.4584(15) ?
N1 C13 . 1.4860(15) ?
C1 C6 . 1.3934(17) ?
C1 C2 . 1.3994(16) ?
C2 C3 . 1.3929(18) ?
C2 C7 . 1.5060(19) ?
C3 C4 . 1.388(2) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.3910(19) ?
C4 C8 . 1.5095(19) ?
C5 C6 . 1.3925(17) ?
C5 H5 . 0.9500 ?
C6 C9 . 1.5039(18) ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
C8 H8A . 0.9800 ?
C8 H8B . 0.9800 ?
C8 H8C . 0.9800 ?
C9 H9A . 0.9800 ?
C9 H9B . 0.9800 ?
C9 H9C . 0.9800 ?
C10 C12 . 1.4843(18) ?
C10 C11 . 1.4871(18) ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
C11 H11C . 0.9800 ?
C12 H12A . 0.9800 ?
C12 H12B . 0.9800 ?
C12 H12C . 0.9800 ?
C13 H13A . 0.9800 ?
C13 H13B . 0.9800 ?
C13 H13C . 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C11 H11A O1 1_655 0.98 2.56 3.477(2) 155.4 yes
C12 H12A F2 2_646 0.98 2.69 3.3859(18) 128.5 yes
C13 H13A O1 1_655 0.98 2.45 3.3789(18) 159.0 yes
C13 H13B O2 4_676 0.98 2.29 3.2377(18) 161.6 yes
C13 H13C O3 . 0.98 2.52 3.1723(17) 123.5 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
C10 N1 C1 C6 . . . . -97.12(14) ?
C13 N1 C1 C6 . . . . 84.04(14) ?
C10 N1 C1 C2 . . . . 85.64(15) ?
C13 N1 C1 C2 . . . . -93.20(13) ?
C6 C1 C2 C3 . . . . 0.47(18) ?
N1 C1 C2 C3 . . . . 177.60(10) ?
C6 C1 C2 C7 . . . . 178.81(12) ?
N1 C1 C2 C7 . . . . -4.06(18) ?
C1 C2 C3 C4 . . . . 0.35(19) ?
C7 C2 C3 C4 . . . . -178.00(12) ?
C2 C3 C4 C5 . . . . -0.7(2) ?
C2 C3 C4 C8 . . . . 178.79(13) ?
C3 C4 C5 C6 . . . . 0.2(2) ?
C8 C4 C5 C6 . . . . -179.25(13) ?
C4 C5 C6 C1 . . . . 0.5(2) ?
C4 C5 C6 C9 . . . . -179.79(14) ?
C2 C1 C6 C5 . . . . -0.90(19) ?
N1 C1 C6 C5 . . . . -178.02(11) ?
C2 C1 C6 C9 . . . . 179.42(13) ?
N1 C1 C6 C9 . . . . 2.30(18) ?
C1 N1 C10 C12 . . . . 4.98(19) ?
C13 N1 C10 C12 . . . . -176.25(13) ?
C1 N1 C10 C11 . . . . -175.12(12) ?
C13 N1 C10 C11 . . . . 3.65(19) ?
O1 S1 C14 F1 . . . . 63.94(16) ?
O2 S1 C14 F1 . . . . -175.28(14) ?
O3 S1 C14 F1 . . . . -55.02(16) ?
O1 S1 C14 F3 . . . . -174.22(13) ?
O2 S1 C14 F3 . . . . -53.45(15) ?
O3 S1 C14 F3 . . . . 66.82(14) ?
O1 S1 C14 F2 . . . . -55.81(13) ?
O2 S1 C14 F2 . . . . 64.97(13) ?
O3 S1 C14 F2 . . . . -174.77(11) ?