#------------------------------------------------------------------------------
#$Date: 2022-11-08 19:22:49 +0000 (Tue, 08 Nov 2022) $
#$Revision: 279107 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/42/2244206.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_2244206
loop_
_publ_author_name
'Priyanka, Prabhakar'
'Jayanna, Bidarur K.'
'Kiran Kumar, Haruvegowda'
Vinaya
'Divakara, Thayamma R.'
'Yathirajan, Hemmige S.'
'Glidewell, Christopher'
'Parkin, Sean'
_publ_section_title
;
Synthesis and crystal structure of topiramate azidosulfate at 90K and
298K
;
_journal_coeditor_code VM2271
_journal_issue 10
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 984
_journal_page_last 988
_journal_paper_doi 10.1107/S2056989022008799
_journal_volume 78
_journal_year 2022
_chemical_absolute_configuration ad
_chemical_formula_moiety 'C12 H19 N3 O8 S'
_chemical_formula_sum 'C12 H19 N3 O8 S'
_chemical_formula_weight 365.36
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method 'SHELXL-2019/2 and CIFFIX'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.0717(8)
_cell_length_b 9.1135(12)
_cell_length_c 22.506(3)
_cell_measurement_reflns_used 9504
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 27.49
_cell_measurement_theta_min 3.37
_cell_volume 1655.6(4)
_computing_cell_refinement
;
APEX3 (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
APEX3 (Bruker, 2016)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and publCIF (Westrip,
2010)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Bruker D8 Venture dual source'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0666
_diffrn_reflns_av_unetI/netI 0.0425
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 22913
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.501
_diffrn_reflns_theta_min 2.411
_diffrn_source microsource
_exptl_absorpt_coefficient_mu 0.242
_exptl_absorpt_correction_T_max 0.959
_exptl_absorpt_correction_T_min 0.815
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.466
_exptl_crystal_description 'cut block'
_exptl_crystal_F_000 768
_exptl_crystal_size_max 0.240
_exptl_crystal_size_mid 0.220
_exptl_crystal_size_min 0.140
_refine_diff_density_max 0.203
_refine_diff_density_min -0.270
_refine_ls_abs_structure_details
;
Flack x determined using 1388 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.07(5)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 221
_refine_ls_number_reflns 3786
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.036
_refine_ls_R_factor_all 0.0386
_refine_ls_R_factor_gt 0.0357
_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^)+(0.0574P)^2^+0.1732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0960
_refine_ls_wR_factor_ref 0.0987
_reflns_number_gt 3523
_reflns_number_total 3786
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vm2271sup1.cif
_cod_data_source_block I-298K
_cod_original_cell_volume 1655.6(3)
_cod_database_code 2244206
_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 0.944
_shelx_estimated_absorpt_t_max 0.967
_shelx_hkl_file
;
1 0 0 0.37672 0.23840 2
1 0 0 0.29275 0.20469 3
-1 0 0 0.20112 0.23380 2
-1 0 0 0.89932 0.25574 3
-3 0 0 0.83844 0.56056 3
3 0 0 0.26901 0.62169 2
-3 0 0 0.61043 0.53449 2
-4 0 0 112.054 10.5093 3
-4 0 0 131.059 10.6383 2
4 0 0 120.860 10.6730 2
-4 0 0 118.608 10.4977 4
5 0 0 12.0731 2.02814 2
-5 0 0 14.4827 1.79350 4
-6 0 0 170.238 13.9692 3
-6 0 0 143.644 13.8791 2
-6 0 0 162.207 13.8368 4
-7 0 0 28.0095 3.67707 3
-7 0 0 30.8004 3.45144 4
-8 0 0 74.3061 7.17821 3
-8 0 0 73.5139 7.08280 2
-8 0 0 71.1456 6.81138 4
-9 0 0 -0.4281 1.15947 2
-9 0 0 2.99617 1.48984 3
-9 0 0 1.97899 1.02309 4
-9 0 0 3.03200 1.14129 4
-10 0 0 14.8415 2.73476 3
0 1 0 -0.1915 0.24361 3
0 -1 0 0.01782 0.25972 4
0 -1 0 0.29592 0.31041 5
0 -1 0 -0.2017 0.22910 3
0 1 0 0.55941 0.28584 5
0 1 0 -0.0806 0.24958 4
1 -1 0 347.054 25.8082 3
-1 -1 0 329.710 25.9511 3
-1 -1 0 267.954 25.8210 5
1 1 0 290.728 25.7951 5
-1 1 0 302.771 25.7962 3
1 1 0 265.113 25.8951 3
-1 -1 0 317.319 25.7955 4
1 1 0 319.949 25.7871 4
1 -1 0 270.210 25.9262 4
1 1 0 333.761 25.8875 2
-1 1 0 345.601 25.9966 4
2 1 0 871.193 75.5611 3
-2 1 0 861.997 75.5873 4
-2 -1 0 929.251 75.5969 3
-2 1 0 949.791 75.6662 2
-3 1 0 744.122 58.6617 2
-3 -1 0 714.039 58.5812 3
3 1 0 704.291 58.4513 2
-3 1 0 661.857 58.5559 4
3 1 0 731.575 58.5515 3
-3 -1 0 630.841 58.2162 4
4 1 0 258.257 22.4715 2
4 1 0 243.283 22.4727 3
-4 1 0 260.482 22.6381 2
-4 1 0 255.374 22.5799 4
-4 -1 0 288.635 22.2172 4
-4 1 0 282.338 22.3505 3
-4 -1 0 261.805 22.5959 3
-4 -1 0 257.372 22.4055 2
5 1 0 29.2519 3.43421 2
-5 -1 0 30.0346 3.27459 2
-5 -1 0 30.9588 3.07528 4
-5 1 0 34.3907 3.24943 3
-5 -1 0 31.1892 3.50006 3
-5 1 0 31.2724 3.47754 4
-5 1 0 32.8494 3.62468 2
-5 -1 0 35.1623 3.03027 4
-6 1 0 0.45195 0.98147 3
-6 -1 0 0.62343 0.95159 2
-6 -1 0 1.16811 0.80534 4
-6 1 0 0.25722 1.25196 2
-6 -1 0 1.66816 0.74805 4
6 1 0 1.57019 1.26359 2
-6 1 0 2.18735 1.27724 4
-6 -1 0 1.71002 1.36793 3
-7 -1 0 496.735 42.2967 3
-7 -1 0 490.064 41.6954 4
-7 -1 0 500.547 42.0346 2
7 1 0 492.421 42.1760 2
-7 1 0 513.308 42.0096 3
-7 1 0 476.529 42.2899 2
-7 -1 0 501.512 41.6251 4
-7 1 0 494.825 42.2161 4
-8 1 0 0.15937 1.29139 3
-8 -1 0 3.58674 0.87479 4
-8 1 0 3.34271 1.82487 2
-8 -1 0 1.22549 1.66625 3
-8 -1 0 3.16626 0.84823 4
-9 1 0 5.88061 1.83852 3
-9 1 0 7.06865 1.88509 4
-9 1 0 5.64110 1.91197 2
-9 -1 0 6.49468 1.27401 5
-10 -1 0 21.2609 2.65574 5
-10 -1 0 26.1074 3.57738 3
-1 -2 0 371.116 30.5998 4
1 -2 0 348.511 30.7542 4
-1 -2 0 379.461 30.7376 3
-1 2 0 371.586 30.5766 3
1 2 0 306.792 30.5800 5
-1 2 0 419.627 30.8545 4
1 -2 0 388.595 30.5772 3
-1 2 0 352.695 30.6021 5
-1 -2 0 351.283 30.6595 5
1 2 0 409.995 30.7660 3
1 2 0 305.173 30.5356 4
-2 2 0 51.2447 4.78888 4
2 2 0 48.3758 4.40127 5
-2 -2 0 47.9762 4.69649 3
-2 -2 0 48.9367 4.56607 5
2 2 0 54.2098 4.78119 3
-2 -2 0 53.0973 4.42895 4
2 -2 0 43.4297 4.69348 4
-2 2 0 49.4265 4.43083 3
-3 -2 0 219.212 19.4465 3
-3 2 0 229.499 19.0927 3
-3 2 0 195.488 19.4329 4
3 2 0 262.246 19.3135 2
3 2 0 227.895 19.4496 3
-3 -2 0 206.264 19.0006 4
-3 2 0 212.716 19.5448 2
-3 -2 0 247.986 19.2203 5
3 2 0 227.208 18.9959 4
-4 -2 0 87.6171 8.21023 4
4 2 0 99.5620 8.80468 3
4 2 0 110.229 8.66112 2
-4 2 0 90.2604 8.83773 4
-4 -2 0 101.354 8.42757 5
-4 2 0 99.4163 8.37800 3
-4 -2 0 91.7866 8.79593 3
-4 2 0 88.8856 8.89046 2
5 2 0 110.549 9.79450 3
-5 2 0 104.882 9.91018 4
-5 -2 0 121.788 9.14436 4
5 2 0 108.321 9.64750 2
-5 2 0 94.8055 9.86987 2
-5 -2 0 115.216 9.57609 2
-5 2 0 93.7482 9.27500 3
-5 -2 0 103.920 9.30967 5
-6 2 0 976.494 76.7512 3
-6 -2 0 879.167 76.8778 2
-6 -2 0 891.668 76.6523 5
-6 2 0 870.906 77.2523 4
-6 2 0 944.366 77.3805 2
-6 -2 0 910.501 77.2820 3
6 2 0 935.307 77.0017 2
-7 2 0 5.46510 1.99114 4
7 2 0 2.58369 1.58965 2
-7 -2 0 5.82053 2.07547 3
-7 2 0 1.10400 1.74464 2
-7 -2 0 4.03175 1.16836 5
-7 2 0 1.35419 1.13302 3
-7 -2 0 4.41789 1.39413 2
-8 -2 0 364.533 31.0150 5
-8 -2 0 361.679 31.7359 3
-8 2 0 358.978 30.9833 3
-8 2 0 370.533 31.7729 2
8 2 0 359.912 31.2909 2
-8 2 0 375.797 31.6827 4
-9 2 0 3.10184 1.12843 3
-9 2 0 3.81776 1.86866 2
-9 -2 0 2.43167 1.90975 3
-9 2 0 2.12160 1.59636 4
-9 2 0 1.11259 0.96380 3
-10 -2 0 3.89883 1.91864 3
-10 -2 0 0.17622 1.31828 5
-10 2 0 0.96880 1.61257 4
-10 2 0 1.64038 0.79578 3
0 -3 0 2.27639 0.87613 3
0 3 0 0.12956 0.66284 5
0 3 0 0.00383 0.60102 3
0 -3 0 0.16734 0.70105 4
0 -3 0 0.76107 0.75604 5
0 3 0 0.02826 0.64113 4
-1 -3 0 5.11053 1.25974 5
1 3 0 6.07516 1.34896 3
-1 -3 0 8.87321 1.63234 3
1 -3 0 9.41202 1.28611 3
-1 3 0 9.47075 1.50235 4
1 3 0 10.2834 1.45362 5
-1 3 0 7.64778 1.38923 5
1 -3 0 8.00928 1.63665 4
-1 -3 0 6.07582 1.23408 4
1 3 0 6.51786 1.31435 4
-1 3 0 6.64911 1.21273 3
-2 3 0 979.829 85.6440 4
-2 -3 0 1046.85 85.3362 4
2 -3 0 1017.39 85.2820 3
-2 3 0 1044.77 85.3070 3
-2 -3 0 1020.35 85.6002 3
2 3 0 1055.69 85.3041 4
2 3 0 919.621 85.3026 5
-2 3 0 1050.28 85.3863 5
-2 -3 0 1072.88 85.5308 5
2 3 0 973.289 85.4778 2
2 -3 0 1030.01 86.0256 4
-3 -3 0 872.863 75.8380 3
-3 3 0 954.912 75.4200 3
3 3 0 826.644 75.5817 2
-3 -3 0 843.580 75.6120 5
3 3 0 915.296 75.8379 3
3 3 0 911.472 75.3052 5
-3 3 0 911.539 75.9467 4
3 3 0 964.167 75.3640 4
4 3 0 53.2817 4.75950 2
-4 3 0 46.5709 4.36990 3
-4 -3 0 51.8393 4.73758 5
4 3 0 37.0431 4.76922 3
-4 3 0 49.4282 5.22469 2
-4 -3 0 38.4165 4.94666 3
-5 3 0 2.94707 1.74857 4
-5 -3 0 5.05844 1.41285 5
5 3 0 4.08127 1.70054 3
-5 -3 0 3.75080 0.80734 4
-5 3 0 6.96400 2.09361 2
-5 -3 0 6.10189 1.87254 3
-5 3 0 4.92866 1.08504 3
5 3 0 3.68872 1.38694 2
-6 -3 0 42.1750 4.52025 5
6 3 0 41.5696 4.88432 3
-6 3 0 42.3399 4.14637 3
-6 3 0 45.0501 5.17567 4
6 3 0 40.4240 4.64439 2
-6 3 0 46.3920 5.27157 2
-6 3 0 39.1512 4.07912 3
-6 -3 0 39.2843 5.05652 3
-7 3 0 964.651 84.2307 2
7 3 0 983.287 83.6604 2
-7 3 0 1004.24 83.2447 3
-7 3 0 944.610 83.2365 3
-7 -3 0 956.496 84.1217 3
-7 -3 0 1131.81 83.7788 5
-7 3 0 973.666 84.1597 4
-8 -3 0 3.18318 1.57539 5
-8 3 0 1.49581 0.86806 3
-8 -3 0 3.35023 2.20795 3
-8 3 0 1.76611 1.73956 2
8 3 0 0.44220 1.47906 2
-8 3 0 0.47393 1.77249 4
-8 3 0 1.58959 0.99338 3
-9 3 0 19.0552 3.32494 4
-9 -3 0 18.0133 3.07236 5
-9 -3 0 23.7491 3.74193 3
-9 3 0 15.5870 3.57185 2
-10 3 0 15.5288 3.05786 4
-10 -3 0 10.6140 2.46245 5
-10 -3 0 5.71939 2.55610 3
0 4 0 1680.38 143.961 5
0 -4 0 1758.74 143.978 5
-1 4 0 339.513 31.0498 5
-1 -4 0 386.671 31.1764 3
-1 -4 0 331.782 31.0130 4
1 -4 0 334.037 30.9452 5
1 -4 0 421.675 31.0480 3
1 4 0 369.676 31.0521 4
1 4 0 330.273 31.0182 5
-1 -4 0 395.287 31.2324 5
1 4 0 363.013 31.1278 3
-1 4 0 390.408 31.0382 3
-1 4 0 345.696 31.1935 4
1 -4 0 364.755 31.2531 4
2 4 0 947.393 82.7162 3
-2 -4 0 983.556 82.6816 5
2 -4 0 1098.51 82.9896 4
-2 4 0 1101.50 82.4876 3
2 4 0 962.262 82.5053 5
2 4 0 882.857 82.3859 4
-2 4 0 854.872 83.3152 5
-2 -4 0 1048.05 82.5422 4
2 -4 0 961.952 82.4010 3
3 -4 0 387.613 32.5419 3
-3 -4 0 428.873 32.6786 4
-3 -4 0 382.077 33.0615 3
3 4 0 383.111 32.5259 4
-3 4 0 380.463 32.7056 5
3 4 0 332.808 32.9072 3
3 4 0 398.087 32.5667 5
-3 4 0 376.960 33.1345 4
-4 4 0 41.1781 4.48410 4
4 4 0 29.6409 3.47429 4
-4 4 0 40.7199 3.82182 5
4 4 0 38.7595 3.32450 5
-4 4 0 39.2014 3.62754 3
-4 -4 0 33.6760 4.28478 3
4 4 0 35.6379 3.29280 5
-4 -4 0 33.0291 3.98411 5
-4 -4 0 29.3169 3.49070 4
4 4 0 34.3984 4.16492 3
4 4 0 39.2539 4.12519 2
5 4 0 68.7262 6.87894 2
-5 -4 0 81.6998 7.07254 5
-5 4 0 73.2816 7.39918 4
-5 4 0 65.1051 6.33813 3
-5 4 0 67.5444 7.47392 2
-5 -4 0 70.5691 6.30338 4
-5 -4 0 66.0500 7.27151 3
5 4 0 65.4296 7.04536 3
-6 -4 0 308.431 26.7837 3
6 4 0 319.063 26.6881 3
-6 -4 0 306.464 26.3531 5
6 4 0 305.794 26.2410 2
-6 4 0 298.032 26.8072 4
-6 4 0 274.496 25.7012 3
-6 4 0 318.770 27.0358 2
-7 -4 0 28.1168 4.04651 5
-7 4 0 34.8602 4.59312 4
7 4 0 34.5982 4.07185 2
-7 -4 0 30.9953 4.50552 3
-7 4 0 28.3132 3.14093 3
-7 4 0 30.9500 3.09215 3
7 4 0 28.9776 4.58805 3
-8 4 0 160.328 14.5243 4
-8 4 0 136.211 14.5274 2
-8 4 0 153.902 12.9797 3
8 4 0 147.824 13.7963 2
-8 4 0 157.639 13.3696 5
-8 -4 0 157.007 14.0397 5
-9 -4 0 4.75180 2.47031 3
-9 4 0 6.57764 2.43915 4
9 4 0 5.19598 1.84164 2
-9 4 0 4.98192 1.43086 5
-9 -4 0 5.13903 2.06143 5
0 -5 0 9.37943 2.13856 3
0 5 0 13.0734 2.30440 5
0 -5 0 16.3407 2.46948 5
0 -5 0 17.7117 2.38879 4
1 -5 0 2673.20 213.386 4
1 5 0 2215.80 213.044 3
-1 -5 0 2347.12 213.109 3
1 5 0 2693.40 213.181 5
-1 5 0 2575.59 213.163 5
-1 -5 0 2753.07 213.222 4
-1 5 0 2577.35 213.032 3
-2 5 0 105.420 9.78342 5
-2 5 0 91.9935 9.50800 3
-2 -5 0 99.8756 9.65869 4
-2 5 0 101.875 9.97030 4
-2 -5 0 96.1608 9.85281 5
2 5 0 99.1424 9.88503 3
2 -5 0 124.364 10.2761 4
-2 -5 0 89.7044 9.76036 3
2 5 0 115.378 9.78743 5
2 -5 0 113.541 9.64111 3
2 5 0 123.553 9.79759 4
3 5 0 17.4512 2.55139 5
3 -5 0 20.0507 3.00975 4
-3 5 0 16.6556 2.69382 3
3 5 0 16.4121 2.84499 3
-3 -5 0 22.5845 3.08758 5
-3 5 0 15.9949 2.73723 5
3 -5 0 20.5382 2.52253 3
-3 -5 0 27.8229 3.46835 3
-3 5 0 18.9864 3.04634 4
-4 -5 0 60.1034 5.91331 4
-4 5 0 59.4972 6.67555 4
-4 5 0 57.4314 5.79042 3
4 5 0 50.6144 6.59259 3
-4 -5 0 60.7056 6.38247 5
4 5 0 71.0604 5.87487 4
-4 -5 0 54.0783 6.52741 3
-4 5 0 67.3032 6.22060 5
5 5 0 8.81029 2.50462 3
-5 -5 0 3.89002 2.08965 3
5 5 0 7.07044 1.52546 4
-5 5 0 6.13009 1.79374 5
-5 5 0 4.37258 1.42598 3
-5 -5 0 9.82770 1.80435 4
-5 5 0 8.93982 2.78396 4
-5 -5 0 9.48789 2.44882 5
-5 5 0 6.20106 4.08470 2
5 5 0 1.97844 2.07991 2
-6 5 0 84.2883 9.71301 2
-6 5 0 93.1510 8.29296 3
-6 -5 0 83.1869 9.04520 5
-6 -5 0 98.7766 9.62743 3
-6 5 0 91.4950 9.52685 4
-6 5 0 97.8904 8.72300 5
6 5 0 93.9399 8.92384 2
-7 -5 0 54.0187 6.08996 5
-7 5 0 63.3196 5.61260 5
-7 5 0 50.3500 4.93176 3
-7 5 0 40.4365 7.14737 2
7 5 0 53.8460 5.84718 2
-7 5 0 47.8483 6.35308 4
-7 -5 0 59.7233 6.99037 3
8 5 0 1.53430 1.69672 2
-8 5 0 3.30066 1.53905 5
-8 5 0 3.07952 2.34974 4
-8 -5 0 1.51901 1.84289 5
-8 -5 0 1.19376 2.20590 3
-9 -5 0 10.1660 2.94646 5
-9 5 0 14.8807 3.54278 4
-9 -5 0 9.87917 3.18164 3
0 -6 0 587.993 48.0344 3
0 6 0 564.399 48.1124 4
0 -6 0 499.863 47.9183 5
0 6 0 654.161 48.1839 3
0 6 0 513.871 47.9745 5
1 6 0 164.150 16.0757 5
-1 6 0 187.118 16.1128 3
-1 -6 0 164.794 16.1656 5
1 6 0 167.743 16.1660 3
1 6 0 187.029 16.2061 4
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3 2 -26 0.64811 2.05491 5
-3 -2 -26 1.37276 2.51890 2
-3 -2 -26 0.03824 2.73590 3
-3 2 -26 4.11685 2.73956 2
3 -2 -26 -2.3472 2.04872 5
3 -2 -26 1.19642 3.71271 2
-4 -2 -26 7.87322 3.34386 5
4 2 -26 6.84017 2.69973 5
4 2 -26 3.70094 3.60922 2
-4 -2 -26 8.93256 3.47815 3
4 -2 -26 1.48055 3.82306 2
4 -2 -26 4.53214 2.50065 5
-4 2 -26 7.18653 3.06993 2
-4 2 -26 4.93129 2.97827 5
0 -3 -26 76.3972 8.11635 3
0 -3 -26 80.6326 9.28629 2
0 3 -26 54.3589 8.43923 2
0 3 -26 70.3472 8.14615 5
-1 -3 -26 -2.2413 2.60791 2
-1 -3 -26 -0.0914 2.45474 5
-1 -3 -26 1.25135 2.61860 3
1 3 -26 1.07134 2.34546 5
1 3 -26 0.51129 2.48596 2
1 -3 -26 6.77088 3.58450 2
-1 3 -26 0.38195 2.62457 2
1 -3 -26 0.18198 2.62580 5
-1 3 -26 5.16326 2.65467 5
1 -3 -26 0.20372 2.13761 3
-2 -3 -26 2.44709 3.84450 5
-2 -3 -26 2.56147 2.96801 3
2 3 -26 -0.5728 3.04441 2
-2 -3 -26 -0.8319 2.38111 2
2 3 -26 0.89817 2.33764 5
-2 3 -26 0.36595 2.54335 2
-2 3 -26 -0.2567 3.35125 5
2 -3 -26 -0.8871 1.99025 3
2 -3 -26 -0.6487 3.16895 2
2 -3 -26 -1.1657 2.11702 5
3 3 -26 14.2388 3.54902 5
3 3 -26 9.22469 4.55284 2
-3 -3 -26 16.1091 4.17265 5
-3 3 -26 16.1664 3.90082 5
-3 3 -26 12.6843 3.97745 2
3 -3 -26 17.7518 3.73983 3
3 -3 -26 23.1981 4.43042 5
3 -3 -26 20.1057 7.40981 2
0 4 -26 20.5354 5.13135 2
0 -4 -26 16.8066 4.06848 5
0 -4 -26 15.7183 4.00883 3
0 -4 -26 15.0290 4.90534 2
0 4 -26 30.7106 5.17299 5
1 4 -26 5.44853 2.69766 5
1 4 -26 4.95788 3.39305 2
-1 -4 -26 8.80235 3.56695 3
1 -4 -26 6.52950 2.80539 3
-1 4 -26 1.05129 4.22290 5
1 -4 -26 4.33686 3.85374 2
-1 4 -26 9.52564 3.69078 2
1 -4 -26 5.33825 2.98445 5
-2 -4 -26 7.36966 3.35193 5
2 4 -26 7.37385 4.45709 2
2 4 -26 13.6249 3.65831 5
-2 -4 -26 16.0233 4.25365 3
2 -4 -26 18.0278 3.71032 3
-2 4 -26 15.5545 4.28644 2
-2 4 -26 15.1461 4.05671 4
-2 4 -26 14.9769 3.63829 5
2 -4 -26 11.9652 3.57832 5
2 -4 -26 14.5561 5.30254 2
3 4 -26 5.12044 2.78025 5
-3 -4 -26 0.02045 2.70849 5
-3 -4 -26 4.36674 3.56827 3
3 4 -26 4.22912 3.57502 2
3 -4 -26 2.13007 2.54511 5
3 -4 -26 3.96625 4.02608 2
-3 4 -26 2.03326 2.61069 5
3 -4 -26 3.93200 2.46646 3
-3 4 -26 4.55907 3.03180 2
0 -5 -26 110.435 11.2619 3
0 5 -26 80.5142 11.0374 4
0 5 -26 114.459 11.0569 5
-1 -5 -26 2.00017 3.16166 5
-1 -5 -26 -2.0203 2.70454 3
1 5 -26 3.26889 4.87396 5
1 5 -26 4.55578 3.58434 2
-1 5 -26 6.26728 3.46494 2
1 -5 -26 5.32333 2.91623 3
-1 5 -26 11.8706 3.96510 4
-1 5 -26 3.58715 2.63858 5
1 -5 -26 -0.9027 2.82536 5
0 0 -27 -0.0991 2.65418 2
0 0 -27 4.93241 2.95312 5
1 0 -27 6.89813 3.09318 5
-1 0 -27 7.26557 3.18190 5
1 0 -27 4.56251 3.81084 2
-1 0 -27 6.73401 3.57267 2
2 0 -27 -3.3052 2.18487 5
-2 0 -27 -0.8441 2.30735 2
-2 0 -27 1.25012 3.91947 5
2 0 -27 0.42475 3.39692 2
3 0 -27 7.76718 7.20343 2
-3 0 -27 6.14333 3.09033 2
-3 0 -27 8.20760 3.16161 5
3 0 -27 8.72384 3.24872 5
-4 0 -27 2.48573 2.37835 2
4 0 -27 -0.6634 3.25771 2
0 -1 -27 93.9115 11.8182 2
0 -1 -27 108.620 11.2643 5
0 1 -27 109.979 11.2135 5
0 1 -27 113.126 12.0904 2
-1 -1 -27 18.4599 4.29946 5
1 1 -27 15.9591 3.85325 5
-1 -1 -27 15.1563 4.51453 2
1 1 -27 23.9000 5.28535 2
-1 1 -27 17.4020 4.50878 2
1 -1 -27 12.5255 4.53984 2
-1 1 -27 14.6493 3.67323 5
1 -1 -27 14.5697 3.88620 5
2 1 -27 0.38716 2.32806 5
-2 -1 -27 -1.4855 2.56472 2
2 1 -27 1.60051 3.35075 2
2 -1 -27 3.07764 3.45573 2
2 -1 -27 3.07292 2.79967 5
-2 1 -27 2.22874 2.77122 2
-3 -1 -27 9.27031 3.37197 2
3 1 -27 8.89266 3.12455 5
3 1 -27 11.9795 4.63865 2
-3 -1 -27 3.63489 3.23012 5
3 -1 -27 3.50252 5.03881 2
-3 1 -27 9.31344 3.55481 2
3 -1 -27 10.9815 3.15798 5
-3 1 -27 11.4099 3.61731 5
0 2 -27 -1.0736 2.63802 2
0 -2 -27 3.55523 3.06737 5
0 -2 -27 0.60886 2.85376 2
0 2 -27 3.36222 2.55379 5
1 2 -27 1.44924 2.96862 2
-1 -2 -27 3.18188 2.83618 5
1 2 -27 1.96430 2.36157 5
-1 -2 -27 5.57825 3.40642 2
1 -2 -27 2.29233 2.70073 5
-1 2 -27 4.90960 2.70862 5
1 -2 -27 -1.5016 3.11066 2
-1 2 -27 2.00468 2.87166 2
-2 -2 -27 5.20504 3.21915 2
2 2 -27 4.44848 4.07921 2
-2 -2 -27 3.30753 3.49229 5
2 2 -27 2.22010 2.60273 5
-2 2 -27 1.27451 2.72850 5
-2 2 -27 1.56727 2.68263 2
2 -2 -27 3.17789 3.58833 2
2 -2 -27 -1.7449 2.22340 5
3 2 -27 22.6519 4.37095 5
-3 -2 -27 22.8785 4.78555 2
-3 -2 -27 18.3393 4.54392 3
-3 -2 -27 19.8498 4.55064 5
3 2 -27 12.8670 4.97790 2
3 -2 -27 15.6159 3.81315 5
-3 2 -27 23.9605 4.82519 2
3 -2 -27 13.5602 5.03506 2
-3 2 -27 24.5777 4.69108 5
0 -3 -27 42.4125 7.58694 2
0 -3 -27 42.2414 6.30268 3
0 3 -27 44.7192 7.18040 2
0 -3 -27 53.4132 6.81029 5
0 3 -27 39.3332 6.60002 5
-1 -3 -27 16.7156 4.94201 2
1 3 -27 25.8514 5.98874 2
1 3 -27 12.8470 3.51468 5
-1 -3 -27 27.1739 4.57296 3
-1 3 -27 13.8715 4.37772 2
1 -3 -27 23.2424 4.44983 3
-1 3 -27 22.8818 5.17953 5
1 -3 -27 26.7153 4.85089 5
1 -3 -27 21.4092 5.63349 2
-2 -3 -27 11.4489 3.70879 2
2 3 -27 8.02691 3.11065 5
-2 -3 -27 6.92467 3.28701 5
2 3 -27 7.81037 3.96361 2
-2 3 -27 13.3644 3.59999 5
2 -3 -27 4.46728 2.45789 3
-2 3 -27 9.71965 3.49851 2
2 -3 -27 9.47343 3.27983 5
3 3 -27 1.55662 3.35775 2
-3 3 -27 -1.6613 2.56260 2
3 -3 -27 7.00746 4.54424 2
0 -4 -27 2.66668 2.81847 3
0 -4 -27 7.50304 3.84081 2
0 4 -27 2.55562 3.59390 2
0 4 -27 0.57845 2.57676 5
1 4 -27 8.45845 4.22480 2
-1 -4 -27 9.48383 3.72338 3
-1 -4 -27 13.4963 3.84142 5
-1 4 -27 13.8211 3.83268 5
-1 4 -27 5.23238 3.57294 2
1 -4 -27 21.9554 5.75788 2
1 -4 -27 15.2958 3.70269 3
1 -4 -27 17.8016 4.24352 5
0 0 -28 6.94759 3.05599 5
0 0 -28 11.1936 4.27781 2
-1 0 -28 40.0923 6.35173 2
1 0 -28 38.5191 6.97057 2
-1 0 -28 24.0276 6.18254 5
1 0 -28 33.9605 5.72416 5
-2 0 -28 24.5168 5.10526 5
-2 0 -28 30.0725 5.47813 2
2 0 -28 25.6268 4.92586 5
-3 0 -28 15.8529 4.20408 2
3 0 -28 20.5257 5.67324 2
0 1 -28 8.48967 3.77699 5
0 -1 -28 -1.3279 3.18437 2
0 -1 -28 8.96758 3.42304 5
0 1 -28 10.2218 4.11376 2
-1 -1 -28 15.6663 4.46200 5
1 1 -28 8.33874 3.30869 5
1 1 -28 3.10828 3.49632 2
-1 -1 -28 10.5194 4.15313 2
-1 1 -28 7.36623 3.50496 2
1 -1 -28 12.4317 3.74427 5
1 -1 -28 8.78819 4.21079 2
-1 1 -28 9.27710 3.28430 5
-2 -1 -28 2.13668 2.51527 5
-2 -1 -28 6.73815 3.30354 2
2 1 -28 1.30831 3.72220 2
2 1 -28 2.91546 2.70129 5
-2 1 -28 3.51579 2.91339 5
-2 1 -28 2.35959 2.68547 2
2 -1 -28 1.38878 2.83169 5
0 -2 -28 17.4385 5.36621 2
0 2 -28 31.1466 6.23892 2
0 2 -28 24.9020 7.22807 5
1 2 -28 -1.8862 3.32496 2
-1 -2 -28 2.35682 2.73763 5
1 2 -28 1.97506 2.64386 5
-1 -2 -28 0.13482 3.18752 2
1 -2 -28 -1.3902 3.13335 2
-1 2 -28 6.09533 2.86043 5
1 -2 -28 0.70905 2.69275 5
-1 2 -28 0.70927 2.95914 2
2 2 -28 4.30670 4.14469 2
-2 -2 -28 11.3746 3.79585 2
-2 -2 -28 6.52582 3.21285 3
-2 -2 -28 9.78804 3.47515 5
2 2 -28 5.79332 3.01639 5
2 -2 -28 19.1110 5.17433 2
2 -2 -28 8.08987 3.39235 5
-2 2 -28 12.9182 3.69330 5
-2 2 -28 9.35886 3.88046 2
0 3 -28 2.55553 3.27896 2
0 -3 -28 -1.2109 3.32405 2
0 -3 -28 2.23855 2.36340 3
0 -3 -28 3.82935 2.96463 5
0 3 -28 -1.2890 2.45698 5
-1 -3 -28 6.16165 4.83393 3
-1 -3 -28 4.83841 3.58585 2
1 3 -28 3.96739 3.78231 5
1 3 -28 1.74814 3.18832 2
-1 -3 -28 9.65744 3.70324 5
1 -3 -28 5.46908 4.18492 2
1 -3 -28 5.21990 3.03770 5
1 -3 -28 7.03238 3.06060 3
-1 3 -28 5.31056 3.50843 2
-1 3 -28 5.06703 3.06641 5
0 0 -29 -1.6971 2.33661 5
0 0 -29 0.59981 2.94030 2
-1 0 -29 23.9100 5.76112 2
-1 0 -29 19.7631 4.66032 5
0 -1 -29 -2.7686 3.04444 2
0 -1 -29 3.40574 3.08586 5
0 1 -29 -0.5300 3.05650 2
0 1 -29 -2.4557 2.30639 5
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 60331
_shelx_res_file
;
TITL m22221 : space group P212121
m22221.res
created by SHELXL-2019/2 at 13:39:46 on 19-Aug-2022
CELL 0.71073 8.0717 9.1135 22.5064 90.000 90.000 90.000
ZERR 4 0.0008 0.0012 0.0028 0.000 0.000 0.000
LATT -1
SYMM 1/2-X, -Y, 1/2+Z
SYMM -X, 1/2+Y, 1/2-Z
SYMM 1/2+X, 1/2-Y, -Z
SFAC C H N O S
UNIT 48 76 12 32 4
TEMP 25
SIZE 0.24 0.22 0.14
REM FORM cut block
REM COLR colourless
L.S. 10
BOND $H
LIST 4
ACTA
CONF
FMAP 2
REM Instructions for potential hydrogen bonds
EQIV $1 x-1, y, z
HTAB C7 O1_$1
HTAB C7 O5_$1
REM These have the wrong geometry to be considered H-bonds, but tabulate
REM them anyway:
EQIV $2 x, y-1, z
HTAB C5 O8_$2
EQIV $3 -x+1, y+1/2, -z+1/2
HTAB C12 O4_$3
REM Various ring plane statistics:
MPLA O1 C1 C2 C3 C4 C5
MPLA C2 C1 O5 C9 O4
MPLA O2 O3 C3 C4 C6
MPLA 4 C2 C1 O5 C9 O4
MPLA 4 O2 O3 C3 C4 C6
MPLA 3 O3 C4 C6 O2 C3
REM Specific torsion angles:
RTAB tors C2 C1 C12 O6
RTAB tors C1 C12 O6 S1
RTAB tors C12 O6 S1 N1
RTAB tors O6 S1 N1 N2
PLAN 5
REM EXTI 0.006692 not significant.
WGHT 0.057400 0.173200
FVAR 0.86157
S1 5 0.749348 0.790399 0.395494 11.00000 0.06016 0.03026 =
0.05982 -0.00738 0.00564 -0.00492
O1 4 0.686747 0.397745 0.389589 11.00000 0.03646 0.03107 =
0.03262 0.00114 -0.00519 -0.00142
O2 4 0.375981 0.301500 0.443100 11.00000 0.03551 0.05649 =
0.03331 -0.00076 -0.00098 0.00883
O3 4 0.297609 0.401948 0.356387 11.00000 0.03733 0.05799 =
0.03775 0.00715 0.00454 0.01363
O4 4 0.611459 0.220060 0.270622 11.00000 0.03819 0.04182 =
0.04162 -0.01481 0.00715 -0.00601
O5 4 0.816319 0.375315 0.298582 11.00000 0.03118 0.04510 =
0.04554 -0.01334 0.00418 -0.00253
O6 4 0.790040 0.657976 0.354613 11.00000 0.04408 0.03266 =
0.05047 -0.00460 0.00481 -0.00361
O7 4 0.903033 0.832438 0.420183 11.00000 0.07100 0.06585 =
0.08481 -0.02558 0.00401 -0.02657
O8 4 0.646915 0.891017 0.365619 11.00000 0.10997 0.03465 =
0.09830 0.00373 -0.00073 0.01395
N1 3 0.624738 0.720840 0.446950 11.00000 0.05849 0.05917 =
0.05827 -0.00791 0.01301 0.00146
N2 3 0.699789 0.636640 0.483010 11.00000 0.07744 0.06305 =
0.05700 -0.00312 0.00889 -0.00659
N3 3 0.751794 0.563869 0.516566 11.00000 0.12706 0.10544 =
0.07685 0.02581 0.00027 0.00311
C1 1 0.673036 0.424223 0.328739 11.00000 0.03124 0.03238 =
0.03151 -0.00165 -0.00068 0.00093
C2 1 0.531188 0.341251 0.297762 11.00000 0.03234 0.04200 =
0.02923 -0.00454 -0.00050 0.00055
AFIX 13
H2 2 0.479985 0.403642 0.267422 11.00000 -1.20000
AFIX 0
C3 1 0.399819 0.282259 0.339720 11.00000 0.02764 0.04388 =
0.03529 -0.00580 -0.00022 -0.00188
AFIX 13
H3 2 0.333367 0.207389 0.319499 11.00000 -1.20000
AFIX 0
C4 1 0.466168 0.221081 0.398917 11.00000 0.03324 0.03333 =
0.03822 0.00090 0.00280 0.00125
AFIX 13
H4 2 0.442711 0.115874 0.402132 11.00000 -1.20000
AFIX 0
C5 1 0.648747 0.249871 0.406613 11.00000 0.03382 0.03052 =
0.04174 0.00611 -0.00165 0.00410
AFIX 23
H5A 2 0.679702 0.234428 0.447786 11.00000 -1.20000
H5B 2 0.711710 0.181983 0.382284 11.00000 -1.20000
AFIX 0
C6 1 0.238721 0.368687 0.414817 11.00000 0.03435 0.05437 =
0.03541 0.00254 0.00285 0.00969
C7 1 0.092871 0.265038 0.412200 11.00000 0.03463 0.09080 =
0.04889 0.00625 0.00140 -0.00552
AFIX 137
H7A 2 0.005298 0.309049 0.389497 11.00000 -1.50000
H7B 2 0.054350 0.245317 0.451757 11.00000 -1.50000
H7C 2 0.126270 0.174873 0.393681 11.00000 -1.50000
AFIX 0
C8 1 0.201401 0.511523 0.445672 11.00000 0.07514 0.06195 =
0.06398 -0.00469 0.02063 0.02208
AFIX 137
H8A 2 0.299085 0.571603 0.446096 11.00000 -1.50000
H8B 2 0.166869 0.492278 0.485738 11.00000 -1.50000
H8C 2 0.114454 0.561748 0.424853 11.00000 -1.50000
AFIX 0
C9 1 0.773439 0.268418 0.254109 11.00000 0.03729 0.04721 =
0.04163 -0.01302 0.00721 -0.00221
C10 1 0.890510 0.140597 0.258164 11.00000 0.05263 0.05664 =
0.07217 -0.01837 0.01135 0.01164
AFIX 137
H10A 2 0.860101 0.067868 0.229299 11.00000 -1.50000
H10B 2 0.884762 0.098732 0.297250 11.00000 -1.50000
H10C 2 1.001458 0.173537 0.250531 11.00000 -1.50000
AFIX 0
C11 1 0.771035 0.339639 0.193148 11.00000 0.06003 0.07877 =
0.04489 -0.00523 0.01055 -0.00948
AFIX 137
H11A 2 0.742453 0.267603 0.163763 11.00000 -1.50000
H11B 2 0.878574 0.379166 0.184444 11.00000 -1.50000
H11C 2 0.690558 0.417191 0.192682 11.00000 -1.50000
AFIX 0
C12 1 0.653626 0.588359 0.322986 11.00000 0.04502 0.03313 =
0.04150 0.00197 -0.00492 0.00213
AFIX 23
H12A 2 0.655642 0.616531 0.281430 11.00000 -1.20000
H12B 2 0.548641 0.619096 0.339866 11.00000 -1.20000
AFIX 0
HKLF 4
REM m22221 : space group P212121
REM wR2 = 0.0987, GooF = S = 1.036, Restrained GooF = 1.036 for all data
REM R1 = 0.0357 for 3523 Fo > 4sig(Fo) and 0.0386 for all 3786 data
REM 221 parameters refined using 0 restraints
END
WGHT 0.0574 0.1732
REM Highest difference peak 0.203, deepest hole -0.270, 1-sigma level 0.042
Q1 1 0.6026 0.3747 0.3190 11.00000 0.05 0.20
Q2 1 0.7549 0.4102 0.3125 11.00000 0.05 0.16
Q3 1 0.6757 0.7825 0.4252 11.00000 0.05 0.16
Q4 1 0.5917 0.4266 0.4096 11.00000 0.05 0.15
Q5 1 0.2969 0.3226 0.4342 11.00000 0.05 0.15
;
_shelx_res_checksum 35970
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
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 0.74935(9) 0.79040(6) 0.39549(3) 0.05008(19) Uani d 1 . .
O O1 0.68675(18) 0.39774(16) 0.38959(6) 0.0334(3) Uani d 1 . .
O O2 0.3760(2) 0.3015(2) 0.44310(7) 0.0418(4) Uani d 1 . .
O O3 0.29761(19) 0.4019(2) 0.35639(7) 0.0444(4) Uani d 1 . .
O O4 0.6115(2) 0.22006(19) 0.27062(7) 0.0405(4) Uani d 1 . .
O O5 0.81632(19) 0.37532(19) 0.29858(8) 0.0406(4) Uani d 1 . .
O O6 0.7900(2) 0.65798(18) 0.35461(8) 0.0424(4) Uani d 1 . .
O O7 0.9030(3) 0.8324(3) 0.42018(11) 0.0739(7) Uani d 1 . .
O O8 0.6469(4) 0.8910(2) 0.36562(13) 0.0810(7) Uani d 1 . .
N N1 0.6247(3) 0.7208(3) 0.44695(12) 0.0586(6) Uani d 1 . .
N N2 0.6998(4) 0.6366(3) 0.48301(13) 0.0658(7) Uani d 1 . .
N N3 0.7518(6) 0.5639(5) 0.51657(17) 0.1031(12) Uani d 1 . .
C C1 0.6730(3) 0.4242(2) 0.32874(9) 0.0317(4) Uani d 1 . .
C C2 0.5312(3) 0.3413(3) 0.29776(9) 0.0345(4) Uani d 1 . .
H H2 0.479985 0.403642 0.267422 0.041 Uiso calc 1 . .
C C3 0.3998(2) 0.2823(3) 0.33972(9) 0.0356(4) Uani d 1 . .
H H3 0.333367 0.207389 0.319499 0.043 Uiso calc 1 . .
C C4 0.4662(3) 0.2211(2) 0.39892(10) 0.0349(4) Uani d 1 . .
H H4 0.442711 0.115874 0.402132 0.042 Uiso calc 1 . .
C C5 0.6487(3) 0.2499(2) 0.40661(10) 0.0354(5) Uani d 1 . .
H H5A 0.679702 0.234428 0.447786 0.042 Uiso calc 1 . .
H H5B 0.711710 0.181983 0.382284 0.042 Uiso calc 1 . .
C C6 0.2387(3) 0.3687(3) 0.41482(10) 0.0414(5) Uani d 1 . .
C C7 0.0929(3) 0.2650(4) 0.41220(13) 0.0581(8) Uani d 1 . .
H H7A 0.005298 0.309049 0.389497 0.087 Uiso calc 1 . .
H H7B 0.054350 0.245317 0.451757 0.087 Uiso calc 1 . .
H H7C 0.126270 0.174873 0.393681 0.087 Uiso calc 1 . .
C C8 0.2014(4) 0.5115(4) 0.44567(16) 0.0670(9) Uani d 1 . .
H H8A 0.299085 0.571603 0.446096 0.101 Uiso calc 1 . .
H H8B 0.166869 0.492278 0.485738 0.101 Uiso calc 1 . .
H H8C 0.114454 0.561748 0.424853 0.101 Uiso calc 1 . .
C C9 0.7734(3) 0.2684(3) 0.25411(10) 0.0420(5) Uani d 1 . .
C C10 0.8905(4) 0.1406(3) 0.25816(15) 0.0605(7) Uani d 1 . .
H H10A 0.860101 0.067868 0.229299 0.091 Uiso calc 1 . .
H H10B 0.884762 0.098732 0.297250 0.091 Uiso calc 1 . .
H H10C 1.001458 0.173537 0.250531 0.091 Uiso calc 1 . .
C C11 0.7710(4) 0.3396(4) 0.19315(12) 0.0612(7) Uani d 1 . .
H H11A 0.742453 0.267603 0.163763 0.092 Uiso calc 1 . .
H H11B 0.878574 0.379166 0.184444 0.092 Uiso calc 1 . .
H H11C 0.690558 0.417191 0.192682 0.092 Uiso calc 1 . .
C C12 0.6536(3) 0.5884(2) 0.32299(11) 0.0399(5) Uani d 1 . .
H H12A 0.655642 0.616531 0.281430 0.048 Uiso calc 1 . .
H H12B 0.548641 0.619096 0.339866 0.048 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
S1 0.0602(4) 0.0303(3) 0.0598(4) -0.0049(3) 0.0056(3) -0.0074(2)
O1 0.0365(7) 0.0311(7) 0.0326(7) -0.0014(6) -0.0052(6) 0.0011(6)
O2 0.0355(7) 0.0565(10) 0.0333(7) 0.0088(8) -0.0010(6) -0.0008(7)
O3 0.0373(8) 0.0580(10) 0.0377(8) 0.0136(7) 0.0045(7) 0.0071(7)
O4 0.0382(7) 0.0418(8) 0.0416(8) -0.0060(7) 0.0071(7) -0.0148(7)
O5 0.0312(7) 0.0451(9) 0.0455(9) -0.0025(7) 0.0042(6) -0.0133(7)
O6 0.0441(9) 0.0327(8) 0.0505(9) -0.0036(6) 0.0048(7) -0.0046(7)
O7 0.0710(14) 0.0659(14) 0.0848(16) -0.0266(12) 0.0040(12) -0.0256(12)
O8 0.110(2) 0.0347(10) 0.0983(17) 0.0140(12) -0.0007(16) 0.0037(11)
N1 0.0585(13) 0.0592(14) 0.0583(13) 0.0015(12) 0.0130(11) -0.0079(12)
N2 0.0774(18) 0.0630(16) 0.0570(15) -0.0066(14) 0.0089(14) -0.0031(13)
N3 0.127(3) 0.105(3) 0.077(2) 0.003(3) 0.000(3) 0.026(2)
C1 0.0312(9) 0.0324(10) 0.0315(10) 0.0009(8) -0.0007(8) -0.0017(8)
C2 0.0323(10) 0.0420(11) 0.0292(10) 0.0006(8) -0.0005(8) -0.0045(9)
C3 0.0276(8) 0.0439(11) 0.0353(10) -0.0019(9) -0.0002(8) -0.0058(9)
C4 0.0332(9) 0.0333(10) 0.0382(11) 0.0012(8) 0.0028(8) 0.0009(9)
C5 0.0338(10) 0.0305(10) 0.0417(11) 0.0041(8) -0.0017(8) 0.0061(8)
C6 0.0343(10) 0.0544(13) 0.0354(11) 0.0097(11) 0.0028(9) 0.0025(9)
C7 0.0346(11) 0.091(2) 0.0489(14) -0.0055(13) 0.0014(10) 0.0063(15)
C8 0.075(2) 0.0620(18) 0.0640(18) 0.0221(16) 0.0206(16) -0.0047(15)
C9 0.0373(11) 0.0472(12) 0.0416(11) -0.0022(10) 0.0072(9) -0.0130(10)
C10 0.0526(15) 0.0566(15) 0.0722(18) 0.0116(14) 0.0114(14) -0.0184(14)
C11 0.0600(16) 0.0788(19) 0.0449(14) -0.0095(16) 0.0106(13) -0.0052(13)
C12 0.0450(12) 0.0331(11) 0.0415(12) 0.0021(9) -0.0049(9) 0.0020(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
O8 S1 O7 . . 121.86(16) ?
O8 S1 O6 . . 110.36(14) ?
O7 S1 O6 . . 104.96(12) ?
O8 S1 N1 . . 103.09(17) ?
O7 S1 N1 . . 111.19(15) ?
O6 S1 N1 . . 104.17(11) ?
C1 O1 C5 . . 114.07(16) ?
C6 O2 C4 . . 107.84(16) ?
C3 O3 C6 . . 105.87(17) ?
C2 O4 C9 . . 106.84(16) ?
C1 O5 C9 . . 110.53(16) ?
C12 O6 S1 . . 117.92(14) ?
N2 N1 S1 . . 112.8(2) ?
N3 N2 N1 . . 173.9(4) ?
O1 C1 O5 . . 110.61(17) ?
O1 C1 C12 . . 105.30(17) ?
O5 C1 C12 . . 110.87(19) ?
O1 C1 C2 . . 114.75(18) ?
O5 C1 C2 . . 103.67(16) ?
C12 C1 C2 . . 111.76(18) ?
O4 C2 C3 . . 108.12(18) ?
O4 C2 C1 . . 103.75(16) ?
C3 C2 C1 . . 114.32(17) ?
O4 C2 H2 . . 110.1 ?
C3 C2 H2 . . 110.1 ?
C1 C2 H2 . . 110.1 ?
O3 C3 C2 . . 107.36(18) ?
O3 C3 C4 . . 104.59(17) ?
C2 C3 C4 . . 115.04(17) ?
O3 C3 H3 . . 109.9 ?
C2 C3 H3 . . 109.9 ?
C4 C3 H3 . . 109.9 ?
O2 C4 C5 . . 109.14(18) ?
O2 C4 C3 . . 103.79(16) ?
C5 C4 C3 . . 112.11(18) ?
O2 C4 H4 . . 110.5 ?
C5 C4 H4 . . 110.5 ?
C3 C4 H4 . . 110.5 ?
O1 C5 C4 . . 110.00(17) ?
O1 C5 H5A . . 109.7 ?
C4 C5 H5A . . 109.7 ?
O1 C5 H5B . . 109.7 ?
C4 C5 H5B . . 109.7 ?
H5A C5 H5B . . 108.2 ?
O2 C6 O3 . . 104.16(17) ?
O2 C6 C8 . . 108.8(2) ?
O3 C6 C8 . . 107.9(2) ?
O2 C6 C7 . . 110.9(2) ?
O3 C6 C7 . . 110.8(2) ?
C8 C6 C7 . . 113.7(2) ?
C6 C7 H7A . . 109.5 ?
C6 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
C6 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
C6 C8 H8A . . 109.5 ?
C6 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C6 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
O4 C9 O5 . . 104.36(16) ?
O4 C9 C10 . . 108.7(2) ?
O5 C9 C10 . . 109.3(2) ?
O4 C9 C11 . . 110.8(2) ?
O5 C9 C11 . . 110.0(2) ?
C10 C9 C11 . . 113.2(2) ?
C9 C10 H10A . . 109.5 ?
C9 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C9 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C9 C11 H11A . . 109.5 ?
C9 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C9 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
O6 C12 C1 . . 108.13(18) ?
O6 C12 H12A . . 110.1 ?
C1 C12 H12A . . 110.1 ?
O6 C12 H12B . . 110.1 ?
C1 C12 H12B . . 110.1 ?
H12A C12 H12B . . 108.4 ?
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 O8 . 1.406(3) ?
S1 O7 . 1.412(2) ?
S1 O6 . 1.5527(17) ?
S1 N1 . 1.660(3) ?
O1 C1 . 1.395(3) ?
O1 C5 . 1.434(3) ?
O2 C6 . 1.417(3) ?
O2 C4 . 1.434(3) ?
O3 C3 . 1.418(3) ?
O3 C6 . 1.431(3) ?
O4 C2 . 1.419(3) ?
O4 C9 . 1.429(3) ?
O5 C1 . 1.413(3) ?
O5 C9 . 1.439(3) ?
O6 C12 . 1.457(3) ?
N1 N2 . 1.271(4) ?
N2 N3 . 1.089(5) ?
C1 C12 . 1.510(3) ?
C1 C2 . 1.539(3) ?
C2 C3 . 1.518(3) ?
C2 H2 . 0.9800 ?
C3 C4 . 1.540(3) ?
C3 H3 . 0.9800 ?
C4 C5 . 1.507(3) ?
C4 H4 . 0.9800 ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C6 C8 . 1.506(4) ?
C6 C7 . 1.511(4) ?
C7 H7A . 0.9600 ?
C7 H7B . 0.9600 ?
C7 H7C . 0.9600 ?
C8 H8A . 0.9600 ?
C8 H8B . 0.9600 ?
C8 H8C . 0.9600 ?
C9 C10 . 1.503(4) ?
C9 C11 . 1.518(4) ?
C10 H10A . 0.9600 ?
C10 H10B . 0.9600 ?
C10 H10C . 0.9600 ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C11 H11C . 0.9600 ?
C12 H12A . 0.9700 ?
C12 H12B . 0.9700 ?
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
C7 H7A O1 1_455 0.96 2.70 3.531(3) 145.8 no
C7 H7A O5 1_455 0.96 2.62 3.540(3) 160.0 no
C5 H5B O8 1_545 0.97 2.73 3.398(3) 126.7 no
C12 H12A O4 3_655 0.97 2.63 3.234(3) 120.7 no
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
O8 S1 O6 C12 . . . . -47.7(2) ?
O7 S1 O6 C12 . . . . 179.27(18) ?
N1 S1 O6 C12 . . . . 62.31(19) ?
O8 S1 N1 N2 . . . . -173.4(2) ?
O7 S1 N1 N2 . . . . -41.2(3) ?
O6 S1 N1 N2 . . . . 71.3(2) ?
C5 O1 C1 O5 . . . . -80.8(2) ?
C5 O1 C1 C12 . . . . 159.36(17) ?
C5 O1 C1 C2 . . . . 36.0(2) ?
C9 O5 C1 O1 . . . . 121.76(19) ?
C9 O5 C1 C12 . . . . -121.8(2) ?
C9 O5 C1 C2 . . . . -1.7(2) ?
C9 O4 C2 C3 . . . . -154.34(17) ?
C9 O4 C2 C1 . . . . -32.6(2) ?
O1 C1 C2 O4 . . . . -99.94(19) ?
O5 C1 C2 O4 . . . . 20.8(2) ?
C12 C1 C2 O4 . . . . 140.27(19) ?
O1 C1 C2 C3 . . . . 17.6(3) ?
O5 C1 C2 C3 . . . . 138.32(19) ?
C12 C1 C2 C3 . . . . -102.2(2) ?
C6 O3 C3 C2 . . . . -150.25(18) ?
C6 O3 C3 C4 . . . . -27.6(2) ?
O4 C2 C3 O3 . . . . -167.48(17) ?
C1 C2 C3 O3 . . . . 77.5(2) ?
O4 C2 C3 C4 . . . . 76.6(2) ?
C1 C2 C3 C4 . . . . -38.4(3) ?
C6 O2 C4 C5 . . . . 135.43(19) ?
C6 O2 C4 C3 . . . . 15.7(2) ?
O3 C3 C4 O2 . . . . 7.4(2) ?
C2 C3 C4 O2 . . . . 124.95(19) ?
O3 C3 C4 C5 . . . . -110.21(19) ?
C2 C3 C4 C5 . . . . 7.3(3) ?
C1 O1 C5 C4 . . . . -69.5(2) ?
O2 C4 C5 O1 . . . . -70.3(2) ?
C3 C4 C5 O1 . . . . 44.1(2) ?
C4 O2 C6 O3 . . . . -33.2(2) ?
C4 O2 C6 C8 . . . . -148.0(2) ?
C4 O2 C6 C7 . . . . 86.1(2) ?
C3 O3 C6 O2 . . . . 38.0(2) ?
C3 O3 C6 C8 . . . . 153.5(2) ?
C3 O3 C6 C7 . . . . -81.4(2) ?
C2 O4 C9 O5 . . . . 31.7(2) ?
C2 O4 C9 C10 . . . . 148.3(2) ?
C2 O4 C9 C11 . . . . -86.6(2) ?
C1 O5 C9 O4 . . . . -17.9(2) ?
C1 O5 C9 C10 . . . . -134.0(2) ?
C1 O5 C9 C11 . . . . 101.1(2) ?
S1 O6 C12 C1 . . . . -135.17(17) ?
O1 C1 C12 O6 . . . . 53.4(2) ?
O5 C1 C12 O6 . . . . -66.3(2) ?
C2 C1 C12 O6 . . . . 178.62(17) ?