#------------------------------------------------------------------------------
#$Date: 2024-06-01 05:13:04 +0300 (Sat, 01 Jun 2024) $
#$Revision: 292154 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023142.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_2023142
loop_
_publ_author_name
'Sow, Salif'
'Thiam, Mariama'
'Odame, Felix'
'Thiam, Elhadj Ibrahima'
'Diouf, Ousmane'
'Ellena, Javier'
'Gaye, Mohamed'
'Tshentu, Zenixole'
_publ_section_title
;
Crystal structure of 1-(1,3-benzothiazol-2-yl)-3-(4-bromobenzoyl)thiourea
;
_journal_coeditor_code PK2706
_journal_issue 6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 663
_journal_page_last 666
_journal_paper_doi 10.1107/S2056989024004742
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C15 H10 Br N3 O S2'
_chemical_formula_moiety 'C15 H10 Br N3 O S2'
_chemical_formula_sum 'C15 H10 Br N3 O S2'
_chemical_formula_weight 392.29
_chemical_name_systematic
;
1-(1,3-Benzothiazol-2-yl)-3-(4-bromobenzoyl)thiourea
;
_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
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha 90
_cell_angle_beta 103.606(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 13.5009(5)
_cell_length_b 6.4130(2)
_cell_length_c 17.9147(7)
_cell_measurement_reflns_used 9123
_cell_measurement_temperature 99.99(10)
_cell_measurement_theta_max 33.9080
_cell_measurement_theta_min 3.0900
_cell_volume 1507.55(10)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
Olex2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.00
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0414
_diffrn_reflns_av_unetI/netI 0.0299
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 18792
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.368
_diffrn_reflns_theta_min 3.105
_exptl_absorpt_coefficient_mu 3.007
_exptl_absorpt_correction_T_max 0.986
_exptl_absorpt_correction_T_min 0.804
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour 'light colourless'
_exptl_crystal_density_diffrn 1.728
_exptl_crystal_description block
_exptl_crystal_F_000 784
_exptl_crystal_size_max 0.102
_exptl_crystal_size_mid 0.061
_exptl_crystal_size_min 0.057
_refine_diff_density_max 0.345
_refine_diff_density_min -0.298
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.026
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 199
_refine_ls_number_reflns 3074
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.026
_refine_ls_R_factor_all 0.0334
_refine_ls_R_factor_gt 0.0240
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+1.3729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0541
_refine_ls_wR_factor_ref 0.0570
_reflns_number_gt 2581
_reflns_number_total 3074
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file pk2706.cif
_cod_data_source_block I
_cod_original_cell_volume 1507.54(10)
_cod_database_code 2023142
_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 0.749
_shelx_estimated_absorpt_t_max 0.847
_shelx_hkl_file
;
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0 0 -4 1096.55 47.0524 3
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0 0 4 1043.95 47.2194 8
0 0 -5 1.91464 2.72992 1
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0 0 -5 2.73209 2.97625 8
0 0 -6 2654.99 110.613 8
0 0 -6 2407.66 110.463 1
0 0 -6 2594.65 108.206 7
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0 0 -8 318.754 18.4937 1
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0 0 -8 348.427 18.5647 8
0 0 -9 4.40626 4.29846 1
0 0 -9-2.25975 4.83901 3
0 0 -9 0.80101 4.92940 8
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0 0 13 13.1485 8.49935 1
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0 0 -14 134.850 13.6828 1
0 0 14 121.975 13.1996 1
0 0 -14 142.725 13.4983 3
0 0 14 132.618 14.1207 2
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0 0 -20 393.404 30.4385 1
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0 1 -3 141.540 7.40572 1
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0 -1 3 133.428 7.29172 10
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0 -1 -4 4494.18 186.319 7
0 1 -4 4580.03 185.241 10
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0 1 -6 792.222 35.4725 1
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18 1 -11 101.526 14.5193 10
18 -1 -10-4.92084 13.3794 10
-18 1 10-23.3199 18.0555 2
18 1 -10 2.71130 12.3182 10
18 -1 -9 36.1978 14.8840 10
-18 1 9 15.4304 18.9857 2
18 1 -9 14.5738 12.8773 10
-18 1 8-7.70765 19.1971 2
18 -1 -8-1.80881 14.8589 10
18 1 -8 10.9364 13.1084 10
18 1 -7 448.136 30.2226 10
18 -1 -7 446.050 31.5381 10
-18 1 7 388.858 34.0020 2
-18 1 6-5.15050 20.1413 2
18 1 -6-5.27869 14.2447 10
18 -1 -6 11.7444 15.7285 10
18 1 -5 437.668 31.0634 10
18 -1 -5 430.659 31.8267 10
-18 1 5 426.542 35.0099 2
-18 1 4-10.3487 19.2617 2
18 1 -4 19.3573 15.9193 10
18 -1 -4 44.2302 17.5652 10
-18 1 3 20.6280 19.2026 2
18 1 -3 30.2307 16.3998 10
18 -1 -3 13.0781 16.5210 10
-18 1 2 10.3733 18.2496 2
18 1 -2-6.30598 16.2436 10
18 -1 -2-11.2681 18.1093 10
-18 1 1 23.6006 18.9447 2
18 1 -1 21.8503 16.9351 10
18 -1 -1 51.1088 18.9908 10
-18 1 0-2.65547 20.6861 2
18 1 0 9.06322 16.7076 10
18 -1 0-4.80109 17.7800 10
18 1 1 581.574 39.9732 10
-18 1 -1 661.317 42.7516 2
-18 1 -2 13.5862 20.4199 2
18 1 2 33.8640 20.7384 10
18 -1 2 30.5322 19.6112 10
-18 1 -3 124.621 24.6523 2
18 1 3 169.125 24.0398 10
18 -1 3 127.879 23.9441 10
18 1 4 79.2467 22.4899 10
-18 -2 13 18.4271 19.6196 2
-18 2 13 39.5730 20.5858 2
-18 -2 12 345.225 31.9061 2
-18 2 12 335.904 32.3053 2
18 -2 -11 3.52761 14.4450 10
-18 -2 11-7.74838 18.2703 2
-18 2 11-33.7305 21.5485 2
18 -2 -10 12.9069 14.8735 10
-18 -2 10 2.55462 18.2407 2
-18 2 10 7.69485 18.5742 2
18 2 -10 1.28588 12.1557 10
18 -2 -9 1.92329 15.0423 10
-18 -2 9 10.1968 18.5438 2
-18 2 9-5.11007 18.1550 2
18 2 -9-4.21738 12.5054 10
18 -2 -8-3.99242 15.3018 10
-18 -2 8-17.8597 18.7310 2
-18 2 8-12.7961 18.9569 2
18 2 -8 1.51345 13.0887 10
-18 -2 7 12.7606 18.9583 2
-18 2 7 17.8949 18.3095 2
18 -2 -7 43.2915 17.5931 10
18 2 -7 54.7308 15.3242 10
-18 -2 6 30.6650 19.2662 2
-18 2 6 53.7210 19.6133 2
18 -2 -6 23.4545 16.0395 10
18 2 -6 70.2176 16.2488 10
-18 -2 5-28.2656 19.3682 2
-18 2 5-7.70268 17.9812 2
18 -2 -5 11.0258 17.0426 10
18 2 -5-1.81018 15.0324 10
-18 -2 4 120.503 22.6273 2
-18 2 4 120.157 21.5595 2
18 -2 -4 136.012 22.0599 10
18 2 -4 146.603 19.7705 10
-18 -2 3 30.8003 19.3257 2
-18 2 3 33.2027 19.4774 2
18 -2 -3 46.6243 18.1713 10
-18 -2 2-18.1467 19.8742 2
-18 2 2-23.1722 19.2433 2
18 -2 -2 4.79541 16.7959 10
-18 -2 1-5.24211 19.4159 2
-18 2 1 25.9844 20.4057 2
18 -2 -1 4.91628 17.4695 10
-18 -2 0 116.701 22.9805 2
-18 2 0 141.751 23.3411 2
18 -2 0 179.267 24.1686 10
-18 -2 -1 26.8102 19.5093 2
-18 2 -1 18.5444 20.2267 2
18 -2 1-7.77958 19.2136 10
-18 -2 -2 32.8199 20.8182 2
-18 2 -2 24.2797 20.4493 2
18 -2 2 23.8895 20.3750 10
-18 -3 12 179.317 25.2435 2
-18 3 12 174.428 25.5260 2
-18 -3 11 22.7923 19.0947 2
-18 3 11 5.07166 19.6831 2
-18 -3 10 5.04853 18.6279 2
-18 3 10 35.3202 21.1067 2
18 -3 -9 51.7204 18.2418 10
-18 -3 9 27.7666 19.2796 2
-18 3 9 37.8161 19.4152 2
18 3 -9 55.2254 13.9032 10
18 -3 -8 24.3264 18.6369 10
-18 3 8 27.7102 20.4105 2
-18 -3 8 2.52046 18.8509 2
18 3 -8 23.9628 13.8293 10
18 -3 -7 553.118 38.8276 10
18 3 -7 537.056 34.7016 10
-18 -3 7 544.946 39.2776 2
-18 3 7 578.955 41.0584 2
-18 -3 6 20.2777 20.2661 2
-18 3 6 15.1044 19.9749 2
18 -3 -6 67.8663 19.6209 10
-18 -3 5 75.8096 21.7635 2
-18 3 5 70.2839 21.8332 2
18 -3 -5 98.5461 20.4552 10
-18 -3 4-17.6698 20.4407 2
-18 3 4-27.4707 20.6671 2
18 -3 -4 14.7766 18.7246 10
-18 -3 3 33.0891 20.4576 2
-18 3 3-15.0820 19.1911 2
18 -3 -3 20.1298 18.8064 10
-18 -3 2-15.4217 19.2916 2
-18 3 2-5.06268 19.4044 2
18 -3 -2-5.15874 18.7668 10
-18 -3 1 26.0024 19.0305 2
-18 3 1 25.5713 19.9474 2
18 -3 -1 23.7944 19.2605 10
-18 -3 0 15.7423 19.0195 2
-18 3 0 15.4425 19.2518 2
18 -3 0 35.1133 20.2893 10
-18 -3 -1 88.0721 23.0774 2
-18 3 -1 44.4120 20.2779 2
-18 -4 10 64.3374 20.5870 2
-18 4 10 68.6170 20.8861 2
-18 -4 9-12.3348 20.0708 2
-18 4 9-34.1730 20.9235 2
-18 -4 8 61.7524 20.9136 2
-18 4 8 73.1097 20.9159 2
-18 -4 7 22.2610 18.9590 2
-18 4 7 4.87177 18.5939 2
18 -4 -7-7.57301 20.7381 10
-18 -4 6 39.3932 20.4573 2
-18 4 6 21.7565 18.6968 2
18 -4 -6-2.57933 19.3720 10
-18 -4 5 2.45930 18.8490 2
-18 4 5 12.0454 19.4307 2
18 -4 -5-13.1444 20.0653 10
-18 -4 4 113.911 23.1346 2
-18 4 4 140.311 24.1511 2
18 -4 -4 158.466 25.4650 10
-18 -4 3 17.4865 20.8452 2
-18 4 3 21.9117 20.1752 2
18 -4 -3 43.7834 21.0041 10
-18 -4 2-30.2291 22.5012 2
-18 4 2-19.6013 20.5120 2
-18 -4 1 71.1028 22.3396 2
-18 4 1 32.0457 21.2102 2
-19 0 10-5.43729 20.7510 2
19 0 -10-3.13859 13.1676 10
-19 0 9 220.627 27.1665 2
19 0 -9 216.672 22.0088 10
-19 0 8-24.5326 21.5767 2
19 0 -8-1.75891 14.3001 10
-19 0 7 65.3358 20.9846 2
19 0 -7 74.0772 17.6062 10
-19 0 6-16.3892 20.1496 2
19 0 -6-11.6324 16.2758 10
-19 0 5 32.8154 20.9071 2
19 0 -5 26.2809 17.5781 10
-19 0 4-21.8164 20.3869 2
19 0 -4-10.5600 17.1105 10
-19 0 3 120.023 23.1741 2
19 0 -3 147.353 22.0649 10
-19 0 2-16.4958 19.7281 2
19 0 -2-6.84782 17.9999 10
19 0 -1 80.3231 21.2160 10
19 0 0-4.88105 18.3944 10
19 0 1 143.681 24.3745 10
19 -1 -11 13.0654 14.2685 10
19 -1 -10 8.66531 14.4425 10
-19 -1 10 2.70647 19.9588 2
19 -1 -9 3.63604 14.6647 10
-19 1 9 29.8929 19.6785 2
19 1 -9-4.65156 14.2929 10
-19 1 8 38.1238 20.9187 2
19 -1 -8 30.5842 16.0446 10
19 1 -8 34.6830 14.9378 10
-19 1 7-5.43748 20.8460 2
19 -1 -7 19.9125 16.1911 10
19 1 -7 24.6185 16.2656 10
-19 1 6 60.0151 22.8494 2
19 1 -6 85.3746 17.7117 10
19 -1 -6 105.557 20.1434 10
-19 1 5 16.3605 19.8355 2
19 1 -5 11.7308 16.9599 10
19 -1 -5-21.4484 17.2994 10
-19 1 4 59.7655 20.9394 2
19 1 -4 57.5461 18.4171 10
19 -1 -4 44.5253 18.2257 10
-19 1 3 59.8541 22.5031 2
19 1 -3 98.3605 19.4453 10
19 -1 -3 108.131 21.7727 10
-19 1 2 164.467 27.1833 2
19 1 -2 210.870 24.7888 10
19 1 -1 9.18718 18.5940 10
19 -1 -1-12.2638 19.1070 10
19 1 0 40.3018 19.4780 10
19 -1 0-17.6500 19.8797 10
19 1 1-2.44856 19.2265 10
19 -2 -11 29.5248 16.6607 10
19 -2 -10 7.70424 15.9386 10
19 -2 -9 241.621 24.4775 10
19 -2 -8 18.8228 16.8690 10
-19 -2 8-13.4439 21.7677 2
-19 2 8-16.1937 22.3303 2
19 2 -8 12.8164 14.6825 10
19 -2 -7 216.659 24.9223 10
-19 -2 7 215.556 27.8155 2
-19 2 7 264.310 29.7401 2
19 2 -7 251.217 23.0709 10
19 -2 -6 2.23381 17.4017 10
-19 -2 6 2.70269 20.2821 2
-19 2 6-27.0588 21.4965 2
19 2 -6 21.6378 15.1289 10
19 -2 -5 34.7370 18.7944 10
-19 -2 5 37.7156 20.7748 2
-19 2 5-13.4714 22.4093 2
19 2 -5 66.5569 18.5968 10
-19 -2 4 37.6536 22.2730 2
-19 2 4 5.37112 20.9428 2
19 -2 -4 19.0686 18.5188 10
19 2 -4 29.9651 17.0177 10
19 -2 -3 88.3228 21.4667 10
19 2 -3 140.059 21.6825 10
19 -2 -2 22.6571 19.7437 10
19 2 -2 87.0760 19.7338 10
19 -2 -1 105.916 22.3828 10
19 2 -1 99.5071 21.7972 10
19 2 0 7.02830 18.9684 10
19 -3 -9-4.47372 18.6385 10
19 -3 -8 46.0002 19.2592 10
19 -3 -7-2.37467 18.7222 10
19 3 -7-11.7472 14.7940 10
19 -3 -6-17.0432 18.8200 10
19 3 -6 35.7181 16.5614 10
19 -3 -5 12.5256 19.3684 10
19 3 -5 17.0356 16.4846 10
19 -3 -4 128.486 24.0835 10
20 0 -9-1.75407 14.7676 10
20 0 -8 40.6942 16.4408 10
20 0 -7 31.0964 17.4427 10
20 0 -6 2.03667 17.3801 10
20 0 -5-10.6359 17.4797 10
20 0 -4 223.307 25.7510 10
20 0 -3-11.4905 20.1327 10
20 0 -2 50.1436 20.0043 10
20 -1 -9 104.829 19.0512 10
20 -1 -8 15.9875 16.7112 10
20 1 -8-1.73872 15.9825 10
20 -1 -7-10.4457 17.2313 10
20 1 -7-14.7236 16.6295 10
20 -1 -6-8.67268 17.4951 10
20 1 -6-15.5849 17.1773 10
20 -1 -5 67.4384 19.7090 10
20 1 -5 49.0812 18.2938 10
20 1 -4 51.2820 19.0875 10
20 -1 -4 83.8012 21.3848 10
20 1 -3 73.7350 20.8400 10
20 -1 -3 79.5369 21.5453 10
20 1 -2 4.65711 19.1293 10
20 -2 -9 14.6391 17.9750 10
20 -2 -8 13.0473 19.1129 10
20 -2 -7-31.6106 19.4968 10
20 2 -7-26.7647 16.0632 10
20 -2 -6 53.6377 19.7264 10
20 2 -6 3.78806 16.4076 10
20 -2 -5 14.4351 18.6915 10
20 2 -5 31.7874 18.2852 10
20 2 -4 186.663 24.7749 10
20 2 -3 21.6805 18.3374 10
20 -3 -9 110.448 22.4011 10
20 -3 -8 11.8668 19.9188 10
20 3 -5 29.2145 18.1965 10
21 0 -7 2.02228 17.3720 10
21 0 -6-16.9495 18.5104 10
21 -1 -7-32.5414 18.7461 10
21 1 -6 8.05652 17.5873 10
0 0 0 0.00 0.00 0
TITL 20220919597CdCl2_auto in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 0.71073 13.500882 6.412968 17.914732 90.0000 103.6060 90.0000
ZERR 3.00 0.000542 0.000202 0.000693 0.0000 0.0038 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N O S Cl Br Cd
UNIT 45.00 30.00 9.00 3.00 6.00 6.00 3.00 3.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
SIZE 0.06 0.06 0.10
TREF
HKLF 4
END
;
_shelx_hkl_checksum 1491
_shelx_res_file
;
TITL 20220919597cdcl2_auto_a.res in P2(1)/n
20220919597cdcl2_auto.res
created by SHELXL-2018/3 at 22:00:00 on 05-Apr-2024
REM Old TITL 20220919597CdCl2_auto in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.079, Rweak 0.001, Alpha 0.031
REM 0.331 for 229 systematic absences, Orientation as input
REM Formula found by SHELXT: C5 N2 O S2 Cl Br
CELL 0.71073 13.500882 6.412968 17.914732 90 103.606 90
ZERR 4 0.000542 0.000202 0.000693 0 0.0038 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Br N O S
UNIT 60 40 4 12 4 8
EQIV $1 -X,1-Y,1-Z
EQIV $2 -X,-Y,1-Z
EQIV $3 0.5-X,0.5+Y,1.5-Z
EQIV $4 1-X,2-Y,1-Z
L.S. 15
PLAN 5
SIZE 0.057 0.061 0.102
TEMP -173.15
CONF
HTAB N3 S2_$1
HTAB N2 O1
HTAB C14 S2_$2
HTAB C2 S1_$3
HTAB C5 N1_$4
MORE -1
BOND $H
HTAB
fmap 2
acta
SHEL 10 0.8
REM
REM
REM
WGHT 0.019100 1.372900
FVAR 0.49986
BR1 3 0.072978 -0.507174 0.270337 11.00000 0.02144 0.01489 =
0.01875 -0.00376 0.00297 -0.00221
S1 6 0.248692 0.987721 0.634474 11.00000 0.01901 0.01636 =
0.01678 -0.00332 0.00898 -0.00372
S2 6 0.107180 0.618093 0.594458 11.00000 0.02033 0.02271 =
0.02626 -0.00728 0.01266 -0.00675
O1 5 0.296830 0.391806 0.432245 11.00000 0.01632 0.01718 =
0.02226 -0.00159 0.00705 -0.00172
N3 4 0.163409 0.389716 0.489867 11.00000 0.01636 0.01604 =
0.02119 -0.00483 0.00868 -0.00642
AFIX 43
H3 2 0.106967 0.322341 0.490909 11.00000 -1.20000
AFIX 0
N1 4 0.379996 0.946081 0.548992 11.00000 0.01486 0.01635 =
0.01541 0.00039 0.00362 -0.00141
N2 4 0.263971 0.677361 0.529232 11.00000 0.01590 0.01465 =
0.01577 -0.00384 0.00735 -0.00210
AFIX 43
H2 2 0.298111 0.627829 0.496902 11.00000 -1.20000
AFIX 0
C10 1 0.183227 0.103496 0.404974 11.00000 0.01615 0.01153 =
0.01500 0.00175 0.00197 -0.00018
C11 1 0.244009 0.007119 0.362280 11.00000 0.01741 0.01872 =
0.01995 -0.00059 0.00696 -0.00355
AFIX 43
H11 2 0.307296 0.068130 0.359855 11.00000 -1.20000
AFIX 0
C8 1 0.183014 0.565735 0.535916 11.00000 0.01734 0.01652 =
0.01600 0.00015 0.00349 -0.00083
C9 1 0.220534 0.305652 0.442511 11.00000 0.01501 0.01609 =
0.01360 0.00343 0.00142 0.00124
C13 1 0.120629 -0.263069 0.327038 11.00000 0.02043 0.01138 =
0.01474 -0.00077 -0.00025 -0.00116
C6 1 0.405040 1.129787 0.590489 11.00000 0.01387 0.01410 =
0.01234 0.00027 0.00043 0.00064
C4 1 0.499934 1.441091 0.629912 11.00000 0.01823 0.01889 =
0.02313 0.00077 0.00036 -0.00497
AFIX 43
H4 2 0.553913 1.533414 0.626970 11.00000 -1.20000
AFIX 0
C12 1 0.213053 -0.177290 0.323207 11.00000 0.02094 0.01948 =
0.02103 -0.00241 0.00859 0.00055
AFIX 43
H12 2 0.254784 -0.243387 0.294303 11.00000 -1.20000
AFIX 0
C14 1 0.059560 -0.173140 0.370253 11.00000 0.01468 0.01660 =
0.02328 0.00030 0.00656 -0.00200
AFIX 43
H14 2 -0.003263 -0.235813 0.372947 11.00000 -1.20000
AFIX 0
C3 1 0.436523 1.487199 0.679713 11.00000 0.02306 0.01511 =
0.01847 -0.00371 -0.00162 -0.00184
AFIX 43
H3A 2 0.448160 1.611081 0.709576 11.00000 -1.20000
AFIX 0
C2 1 0.357971 1.356974 0.686195 11.00000 0.02193 0.01975 =
0.01609 -0.00211 0.00262 0.00019
AFIX 43
H2A 2 0.315825 1.387679 0.720416 11.00000 -1.20000
AFIX 0
C1 1 0.342600 1.178159 0.640595 11.00000 0.01583 0.01706 =
0.01416 0.00106 0.00293 -0.00093
C7 1 0.301660 0.861201 0.566405 11.00000 0.01554 0.01515 =
0.01237 0.00126 0.00307 -0.00015
C15 1 0.091652 0.010041 0.409557 11.00000 0.01872 0.01752 =
0.02099 -0.00182 0.00809 -0.00017
AFIX 43
H15 2 0.050806 0.072576 0.439944 11.00000 -1.20000
AFIX 0
C5 1 0.484741 1.263326 0.585230 11.00000 0.01548 0.01837 =
0.01969 -0.00078 0.00372 -0.00239
AFIX 43
H5 2 0.527660 1.232504 0.551582 11.00000 -1.20000
AFIX 0
HKLF 4
REM 20220919597cdcl2_auto_a.res in P2(1)/n
REM wR2 = 0.0570, GooF = S = 1.026, Restrained GooF = 1.026 for all data
REM R1 = 0.0240 for 2581 Fo > 4sig(Fo) and 0.0334 for all 3074 data
REM 199 parameters refined using 0 restraints
END
WGHT 0.0191 1.3729
REM Instructions for potential hydrogen bonds
HTAB N3 S2_$1
HTAB N2 O1
HTAB C14 S2_$2
HTAB C2 S1_$3
HTAB C5 N1_$4
REM Highest difference peak 0.345, deepest hole -0.298, 1-sigma level 0.065
Q1 1 0.1982 0.1982 0.4226 11.00000 0.05 0.34
Q2 1 0.3646 1.1575 0.6063 11.00000 0.05 0.30
Q3 1 0.0793 -0.0642 0.3749 11.00000 0.05 0.30
Q4 1 0.1785 -0.2138 0.3374 11.00000 0.05 0.28
Q5 1 0.4590 1.4408 0.6498 11.00000 0.05 0.28
;
_shelx_res_checksum 13537
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
Br Br1 0.07298(2) -0.50717(3) 0.27034(2) 0.01865(7) Uani d 1 . .
S S1 0.24869(4) 0.98772(8) 0.63447(3) 0.01659(12) Uani d 1 . .
S S2 0.10718(4) 0.61809(8) 0.59446(3) 0.02191(13) Uani d 1 . .
O O1 0.29683(11) 0.3918(2) 0.43225(8) 0.0182(3) Uani d 1 . .
N N3 0.16341(14) 0.3897(3) 0.48987(10) 0.0172(4) Uani d 1 . .
H H3 0.106967 0.322341 0.490909 0.021 Uiso calc 1 . .
N N1 0.38000(13) 0.9461(3) 0.54899(10) 0.0155(4) Uani d 1 . .
N N2 0.26397(13) 0.6774(3) 0.52923(10) 0.0148(4) Uani d 1 . .
H H2 0.298111 0.627829 0.496902 0.018 Uiso calc 1 . .
C C10 0.18323(16) 0.1035(3) 0.40497(12) 0.0145(4) Uani d 1 . .
C C11 0.24401(17) 0.0071(3) 0.36228(12) 0.0183(4) Uani d 1 . .
H H11 0.307296 0.068130 0.359855 0.022 Uiso calc 1 . .
C C8 0.18301(16) 0.5657(3) 0.53592(12) 0.0167(4) Uani d 1 . .
C C9 0.22053(16) 0.3057(3) 0.44251(12) 0.0152(4) Uani d 1 . .
C C13 0.12063(17) -0.2631(3) 0.32704(12) 0.0162(4) Uani d 1 . .
C C6 0.40504(15) 1.1298(3) 0.59049(11) 0.0139(4) Uani d 1 . .
C C4 0.49993(17) 1.4411(3) 0.62991(13) 0.0208(5) Uani d 1 . .
H H4 0.553913 1.533414 0.626970 0.025 Uiso calc 1 . .
C C12 0.21305(17) -0.1773(3) 0.32321(13) 0.0199(5) Uani d 1 . .
H H12 0.254784 -0.243387 0.294303 0.024 Uiso calc 1 . .
C C14 0.05956(16) -0.1731(3) 0.37025(13) 0.0178(4) Uani d 1 . .
H H14 -0.003263 -0.235813 0.372947 0.021 Uiso calc 1 . .
C C3 0.43652(17) 1.4872(3) 0.67971(13) 0.0200(5) Uani d 1 . .
H H3A 0.448160 1.611081 0.709576 0.024 Uiso calc 1 . .
C C2 0.35797(17) 1.3570(3) 0.68620(12) 0.0196(5) Uani d 1 . .
H H2A 0.315825 1.387679 0.720416 0.023 Uiso calc 1 . .
C C1 0.34260(16) 1.1782(3) 0.64059(12) 0.0158(4) Uani d 1 . .
C C7 0.30166(16) 0.8612(3) 0.56641(12) 0.0144(4) Uani d 1 . .
C C15 0.09165(17) 0.0100(3) 0.40956(13) 0.0185(4) Uani d 1 . .
H H15 0.050806 0.072576 0.439944 0.022 Uiso calc 1 . .
C C5 0.48474(16) 1.2633(3) 0.58523(12) 0.0179(4) Uani d 1 . .
H H5 0.527660 1.232504 0.551582 0.021 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
Br1 0.02144(12) 0.01489(11) 0.01875(12) -0.00221(8) 0.00297(8) -0.00376(8)
S1 0.0190(3) 0.0164(2) 0.0168(3) -0.0037(2) 0.0090(2) -0.0033(2)
S2 0.0203(3) 0.0227(3) 0.0263(3) -0.0068(2) 0.0127(2) -0.0073(2)
O1 0.0163(8) 0.0172(7) 0.0223(8) -0.0017(6) 0.0071(6) -0.0016(6)
N3 0.0164(9) 0.0160(9) 0.0212(10) -0.0064(7) 0.0087(8) -0.0048(7)
N1 0.0149(9) 0.0163(8) 0.0154(9) -0.0014(7) 0.0036(7) 0.0004(7)
N2 0.0159(9) 0.0147(8) 0.0158(9) -0.0021(7) 0.0074(7) -0.0038(7)
C10 0.0162(11) 0.0115(10) 0.0150(11) -0.0002(8) 0.0020(9) 0.0018(8)
C11 0.0174(11) 0.0187(11) 0.0199(11) -0.0035(9) 0.0070(9) -0.0006(9)
C8 0.0173(11) 0.0165(10) 0.0160(11) -0.0008(8) 0.0035(9) 0.0001(8)
C9 0.0150(11) 0.0161(10) 0.0136(11) 0.0012(8) 0.0014(9) 0.0034(8)
C13 0.0204(12) 0.0114(9) 0.0147(11) -0.0012(8) -0.0002(9) -0.0008(8)
C6 0.0139(11) 0.0141(10) 0.0123(10) 0.0006(8) 0.0004(8) 0.0003(8)
C4 0.0182(12) 0.0189(11) 0.0231(12) -0.0050(9) 0.0004(9) 0.0008(8)
C12 0.0209(12) 0.0195(11) 0.0210(12) 0.0005(9) 0.0086(10) -0.0024(9)
C14 0.0147(11) 0.0166(10) 0.0233(12) -0.0020(8) 0.0066(9) 0.0003(8)
C3 0.0231(12) 0.0151(10) 0.0185(11) -0.0018(9) -0.0016(9) -0.0037(8)
C2 0.0219(12) 0.0198(11) 0.0161(11) 0.0002(9) 0.0026(9) -0.0021(8)
C1 0.0158(11) 0.0171(10) 0.0142(11) -0.0009(8) 0.0029(9) 0.0011(8)
C7 0.0155(11) 0.0152(10) 0.0124(10) -0.0002(8) 0.0031(8) 0.0013(8)
C15 0.0187(11) 0.0175(10) 0.0210(12) -0.0002(9) 0.0081(9) -0.0018(9)
C5 0.0155(11) 0.0184(10) 0.0197(11) -0.0024(8) 0.0037(9) -0.0008(8)
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'
Br Br -0.2901 2.4595 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0518
0 1 0 0.0505
1 0 -1 0.0256
-2 -1 2 0.0440
2 -1 -2 0.0513
0 0 1 0.0265
0 0 -1 0.0307
-1 0 -1 0.0328
-2 0 1 0.0289
-1 -2 0 0.0456
-1 -1 1 0.0438
2 0 1 0.0265
8 -2 19 0.0268
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
C1 S1 C7 . . 87.61(9) ?
C8 N3 H3 . . 115.6 ?
C9 N3 H3 . . 115.6 ?
C9 N3 C8 . . 128.78(18) ?
C7 N1 C6 . . 109.74(17) ?
C8 N2 H2 . . 115.6 ?
C8 N2 C7 . . 128.81(17) ?
C7 N2 H2 . . 115.6 ?
C11 C10 C9 . . 116.96(18) ?
C11 C10 C15 . . 119.18(19) ?
C15 C10 C9 . . 123.85(18) ?
C10 C11 H11 . . 119.7 ?
C12 C11 C10 . . 120.6(2) ?
C12 C11 H11 . . 119.7 ?
N3 C8 S2 . . 118.68(15) ?
N2 C8 S2 . . 125.92(16) ?
N2 C8 N3 . . 115.40(17) ?
O1 C9 N3 . . 121.88(19) ?
O1 C9 C10 . . 122.19(18) ?
N3 C9 C10 . . 115.92(18) ?
C12 C13 Br1 . . 119.98(16) ?
C12 C13 C14 . . 121.79(19) ?
C14 C13 Br1 . . 118.22(16) ?
N1 C6 C1 . . 114.95(18) ?
N1 C6 C5 . . 125.29(18) ?
C5 C6 C1 . . 119.76(18) ?
C3 C4 H4 . . 119.6 ?
C5 C4 H4 . . 119.6 ?
C5 C4 C3 . . 120.8(2) ?
C11 C12 H12 . . 120.6 ?
C13 C12 C11 . . 118.89(19) ?
C13 C12 H12 . . 120.6 ?
C13 C14 H14 . . 120.6 ?
C13 C14 C15 . . 118.80(19) ?
C15 C14 H14 . . 120.6 ?
C4 C3 H3A . . 119.3 ?
C2 C3 C4 . . 121.5(2) ?
C2 C3 H3A . . 119.3 ?
C3 C2 H2A . . 121.3 ?
C3 C2 C1 . . 117.4(2) ?
C1 C2 H2A . . 121.3 ?
C6 C1 S1 . . 110.00(15) ?
C2 C1 S1 . . 128.16(16) ?
C2 C1 C6 . . 121.83(19) ?
N1 C7 S1 . . 117.69(15) ?
N1 C7 N2 . . 118.04(18) ?
N2 C7 S1 . . 124.26(15) ?
C10 C15 H15 . . 119.7 ?
C14 C15 C10 . . 120.69(19) ?
C14 C15 H15 . . 119.7 ?
C6 C5 H5 . . 120.7 ?
C4 C5 C6 . . 118.65(19) ?
C4 C5 H5 . . 120.7 ?
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
Br1 C13 . 1.894(2) ?
S1 C1 . 1.745(2) ?
S1 C7 . 1.751(2) ?
S2 C8 . 1.663(2) ?
O1 C9 . 1.220(2) ?
N3 H3 . 0.8800 ?
N3 C8 . 1.386(3) ?
N3 C9 . 1.383(3) ?
N1 C6 . 1.392(3) ?
N1 C7 . 1.291(3) ?
N2 H2 . 0.8800 ?
N2 C8 . 1.335(3) ?
N2 C7 . 1.390(3) ?
C10 C11 . 1.391(3) ?
C10 C9 . 1.492(3) ?
C10 C15 . 1.394(3) ?
C11 H11 . 0.9500 ?
C11 C12 . 1.388(3) ?
C13 C12 . 1.380(3) ?
C13 C14 . 1.383(3) ?
C6 C1 . 1.403(3) ?
C6 C5 . 1.396(3) ?
C4 H4 . 0.9500 ?
C4 C3 . 1.406(3) ?
C4 C5 . 1.380(3) ?
C12 H12 . 0.9500 ?
C14 H14 . 0.9500 ?
C14 C15 . 1.386(3) ?
C3 H3A . 0.9500 ?
C3 C2 . 1.376(3) ?
C2 H2A . 0.9500 ?
C2 C1 . 1.395(3) ?
C15 H15 . 0.9500 ?
C5 H5 . 0.9500 ?
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
N3 H3 S2 3_566 0.88 2.96 3.6102(19) 132.1 yes
N2 H2 O1 . 0.88 1.90 2.633(2) 139.1 yes
C14 H14 S2 3_556 0.95 2.95 3.779(2) 146.4 yes
C2 H2A S1 2_556 0.95 3.00 3.908(2) 160.7 yes
C5 H5 N1 3_676 0.95 2.68 3.604(3) 165.0 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
Br1 C13 C12 C11 . . . . 176.90(16) ?
Br1 C13 C14 C15 . . . . -177.46(16) ?
N1 C6 C1 S1 . . . . -0.6(2) ?
N1 C6 C1 C2 . . . . 179.95(19) ?
N1 C6 C5 C4 . . . . 179.7(2) ?
C10 C11 C12 C13 . . . . 0.4(3) ?
C11 C10 C9 O1 . . . . 5.2(3) ?
C11 C10 C9 N3 . . . . -174.74(18) ?
C11 C10 C15 C14 . . . . -2.0(3) ?
C8 N3 C9 O1 . . . . -4.8(3) ?
C8 N3 C9 C10 . . . . 175.1(2) ?
C8 N2 C7 S1 . . . . 1.2(3) ?
C8 N2 C7 N1 . . . . -177.8(2) ?
C9 N3 C8 S2 . . . . -173.64(17) ?
C9 N3 C8 N2 . . . . 5.5(3) ?
C9 C10 C11 C12 . . . . -177.60(19) ?
C9 C10 C15 C14 . . . . 177.0(2) ?
C13 C14 C15 C10 . . . . 0.7(3) ?
C6 N1 C7 S1 . . . . -0.4(2) ?
C6 N1 C7 N2 . . . . 178.69(17) ?
C4 C3 C2 C1 . . . . -0.8(3) ?
C12 C13 C14 C15 . . . . 1.1(3) ?
C14 C13 C12 C11 . . . . -1.7(3) ?
C3 C4 C5 C6 . . . . 0.0(3) ?
C3 C2 C1 S1 . . . . -178.55(17) ?
C3 C2 C1 C6 . . . . 0.8(3) ?
C1 S1 C7 N1 . . . . 0.05(18) ?
C1 S1 C7 N2 . . . . -178.98(19) ?
C1 C6 C5 C4 . . . . 0.0(3) ?
C7 S1 C1 C6 . . . . 0.32(16) ?
C7 S1 C1 C2 . . . . 179.7(2) ?
C7 N1 C6 C1 . . . . 0.7(3) ?
C7 N1 C6 C5 . . . . -179.1(2) ?
C7 N2 C8 S2 . . . . -2.1(3) ?
C7 N2 C8 N3 . . . . 178.90(19) ?
C15 C10 C11 C12 . . . . 1.5(3) ?
C15 C10 C9 O1 . . . . -173.8(2) ?
C15 C10 C9 N3 . . . . 6.2(3) ?
C5 C6 C1 S1 . . . . 179.10(16) ?
C5 C6 C1 C2 . . . . -0.3(3) ?
C5 C4 C3 C2 . . . . 0.5(3) ?