#------------------------------------------------------------------------------
#$Date: 2020-12-05 07:25:49 +0200 (Sat, 05 Dec 2020) $
#$Revision: 259552 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/22/2022290.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_2022290
loop_
_publ_author_name
'Rosiak, Damian'
'Okuniewski, Andrzej'
'Chojnacki, Jaros\/law'
_publ_section_title
;
The influence of the type of halogen substituent and its position on the
molecular conformation, intermolecular interactions and crystal packing
for a series of 1-benzoyl-3-(halogenophenyl)thioureas
;
_journal_coeditor_code WP3011
_journal_issue 1
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229620015594
_journal_volume 77
_journal_year 2021
_chemical_absolute_configuration ad
_chemical_formula_iupac 'C14 H11 Br N2 O S'
_chemical_formula_moiety 'C14 H11 Br N2 O S'
_chemical_formula_sum 'C14 H11 Br N2 O S'
_chemical_formula_weight 335.22
_chemical_name_common 1-Benzoyl-3-m-bromophenylthiourea
_chemical_name_systematic
;
1-Benzoyl-3-(3-bromophenyl)thiourea
;
_space_group_crystal_system monoclinic
_space_group_IT_number 7
_space_group_name_Hall 'P -2yc'
_space_group_name_H-M_alt 'P 1 c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 90
_cell_angle_beta 91.052(12)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 4.6404(7)
_cell_length_b 15.017(2)
_cell_length_c 19.074(3)
_cell_measurement_reflns_used 6776
_cell_measurement_temperature 125
_cell_measurement_theta_max 29.42
_cell_measurement_theta_min 2.53
_cell_volume 1328.9(3)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2009)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2009)
;
_computing_data_reduction
;
X-RED32 (Stoe & Cie, 2009)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 125
_diffrn_detector 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device '2-circle goniometer'
_diffrn_measurement_device_type 'Stoe IPDS 2T'
_diffrn_measurement_method 'rotation method, \w scans'
_diffrn_radiation_monochromator 'parabolic x-ray mirror'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0872
_diffrn_reflns_av_unetI/netI 0.0669
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 15213
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.997
_diffrn_reflns_theta_min 2.530
_diffrn_source 'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_source_current 1.000
_diffrn_source_power 0.050
_diffrn_source_voltage 50
_exptl_absorpt_coefficient_mu 3.241
_exptl_absorpt_correction_T_max 0.8747
_exptl_absorpt_correction_T_min 0.3544
_exptl_absorpt_correction_type integration
_exptl_absorpt_process_details
;
[X-RED32 (Stoe & Cie, 2009), by Gaussian integration,
analogous to Coppens (1970)]
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.675
_exptl_crystal_description needle
_exptl_crystal_F_000 672
_exptl_crystal_size_max 0.678
_exptl_crystal_size_mid 0.052
_exptl_crystal_size_min 0.04
_refine_diff_density_max 1.967
_refine_diff_density_min -0.654
_refine_ls_abs_structure_details
;
Flack (1983), 2288 Friedel pairs
;
_refine_ls_abs_structure_Flack 0.01(2)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.021
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 343
_refine_ls_number_reflns 4909
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.021
_refine_ls_R_factor_all 0.0761
_refine_ls_R_factor_gt 0.0656
_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^)+(0.1436P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1674
_refine_ls_wR_factor_ref 0.1832
_reflns_number_gt 4294
_reflns_number_total 4537
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wp3011sup1.cif
_cod_data_source_block 5
_cod_original_cell_volume 1329.0(3)
_cod_database_code 2022290
_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 0.217
_shelx_estimated_absorpt_t_max 0.881
_shelx_hkl_file
;
-3 -12 17 4.41 9.65
-3 -11 -5 0.26 9.13
-3 -11 16 29.74 9.70
-3 -10 15 11.08 7.71
-3 -9 13 18.44 7.90
-3 -8 9 59.34 8.99
-2 -14 -13 -1.53 8.58
-2 -12 -12 2.24 6.76
-2 -8 19 78.48 8.53
-2 -7 18 14.03 5.85
-2 -6 16 0.27 7.36
-2 -4 2 368.42 14.58
-2 -4 10 19.29 4.66
-1 -13 -16 1.15 8.74
-1 -10 -14 54.90 5.41
-1 -7 22 49.39 9.14
-1 -6 -10 352.23 8.69
-1 -6 21 4.56 8.17
-1 -4 18 23.33 5.26
0 -9 -16 7.55 7.58
0 -8 -15 239.75 6.65
0 -7 -14 40.25 5.10
0 -6 24 -7.28 6.55
0 -5 -12 18.20 6.01
0 -4 21 9.48 7.70
0 -1 -4 762.90 13.94
0 0 11 -0.08 4.55
1 -7 -16 130.37 7.75
1 -6 -15 133.54 7.21
1 -4 23 -2.49 8.16
1 -3 -11 230.50 7.35
1 -2 20 5.66 5.33
1 -1 18 58.99 5.43
1 0 15 -3.77 6.97
1 1 11 62.26 6.63
2 -10 -19 5.04 7.22
2 -4 24 -3.88 7.16
2 -1 19 6.65 6.02
2 0 -6 1206.49 13.74
2 1 -3 757.98 14.23
2 1 13 7.55 5.67
3 -10 -19 0.39 7.44
3 -6 -16 44.04 5.49
3 -3 -12 59.01 5.60
3 -2 21 9.18 6.42
3 1 -3 107.06 6.88
3 1 13 0.11 6.53
4 -6 -15 4.13 6.28
5 -5 -12 -3.59 6.75
5 -2 -7 54.90 6.64
5 -1 14 0.64 7.43
6 -4 -7 -3.14 7.54
6 -3 -5 3.04 7.68
-3 -16 -9 7.15 12.11
-3 -10 -4 77.33 11.71
-3 -10 14 88.45 8.23
-3 -9 12 34.39 7.87
-3 -8 8 100.89 8.99
-2 -13 -13 53.17 7.79
-2 -10 21 38.50 7.63
-2 -9 20 54.81 6.55
-2 -7 -7 105.74 8.99
-2 -7 17 43.97 7.74
-2 -6 -5 71.62 7.75
-2 -6 15 23.19 6.67
-2 -5 13 12.52 5.39
-1 -15 -17 5.55 9.81
-1 -12 -16 -0.94 7.51
-1 -8 23 14.64 7.12
-1 -5 -9 50.28 6.32
-1 -5 19 9.05 6.67
-1 -4 17 1.15 7.09
-1 -3 15 131.36 5.75
0 -14 -19 -3.64 9.53
0 -12 -18 0.22 6.09
0 -10 -17 2.06 7.42
0 -5 22 8.42 7.51
0 -2 -7 83.48 7.04
0 0 10 969.56 11.46
1 -11 -19 5.50 6.66
1 -9 -18 66.11 8.17
1 -8 -17 74.37 6.18
1 -5 -14 141.94 5.51
1 -5 24 -5.20 6.78
1 -4 -13 494.01 8.46
1 -3 21 9.48 7.84
1 -2 19 57.36 7.48
1 1 10 22.02 6.28
2 -6 -16 5.89 4.72
2 -3 22 3.50 6.34
2 -1 -9 190.99 7.00
2 0 16 54.56 5.90
3 -8 -18 93.88 7.30
3 -7 -17 10.13 4.63
3 -5 -15 46.01 4.03
3 -4 -14 73.98 6.02
3 -3 22 6.46 6.15
3 -2 -11 13.58 5.34
3 -2 20 -0.74 8.08
3 -1 -9 68.50 5.17
3 -1 18 1.60 7.39
3 0 16 25.75 5.39
4 -2 -10 19.91 4.51
4 -2 19 5.16 7.33
4 -1 17 3.63 6.91
4 0 -5 -2.46 5.60
4 0 14 89.25 8.39
4 1 -1 45.66 9.01
5 -6 -14 6.96 6.86
5 -4 -11 -0.54 5.95
5 0 9 -1.84 7.67
6 -2 -2 -2.14 7.87
-3 -15 -9 1.20 10.23
-3 -12 16 -2.86 8.92
-3 -11 15 -2.08 7.26
-3 -10 13 41.18 7.62
-3 -8 3 89.06 10.31
-3 -8 6 11.78 8.72
-3 -8 7 122.63 8.03
-2 -15 -14 3.49 9.62
-2 -11 -12 1.29 8.40
-2 -10 -11 56.89 7.41
-2 -10 20 29.14 8.57
-2 -9 -10 54.33 7.21
-2 -9 19 37.81 7.87
-2 -8 18 30.91 7.22
-2 -5 12 86.76 7.44
-2 -4 3 10.36 7.94
-1 -14 -17 4.00 6.50
-1 -10 -15 12.41 7.00
-1 -9 -14 26.53 6.86
-1 -9 23 12.49 9.42
-1 -8 -13 9.11 6.73
-1 -8 22 -6.32 8.67
-1 -7 -12 42.07 6.60
-1 -7 21 33.88 7.93
-1 -6 20 8.56 5.30
-1 -5 18 0.72 6.82
-1 -3 -5 383.80 11.01
-1 -3 14 28.23 6.50
0 -13 -19 7.92 8.79
0 -11 -18 16.98 7.99
0 -8 -16 9.71 6.30
0 -7 24 4.63 6.07
0 -6 23 13.76 5.99
0 -4 -11 304.83 6.57
0 -4 20 136.25 7.53
0 0 9 3.87 5.79
1 -12 -20 27.79 7.12
1 -10 -19 23.60 8.38
1 -4 22 2.79 6.85
1 0 -5 5.82 6.59
1 0 14 137.69 5.96
1 1 9 436.22 9.81
2 -10 -20 25.08 6.80
2 -9 -19 38.76 5.37
2 -4 23 -4.78 5.41
2 -3 -13 8.63 6.20
2 -2 -11 143.26 5.97
2 -2 20 6.88 4.27
2 -1 18 12.60 4.60
2 0 15 -0.72 5.64
2 1 12 84.13 5.81
3 -9 -19 2.32 5.23
3 -3 -13 132.22 6.19
3 0 -7 3.13 3.95
3 0 15 2.85 6.03
3 1 12 59.85 6.25
4 -7 -17 -0.88 6.52
4 -6 -16 18.56 6.36
4 -5 -15 57.17 5.85
4 -3 -12 4.73 5.26
4 -1 -8 5.51 4.64
4 -1 16 -1.98 7.36
4 1 9 33.20 6.67
5 -5 -13 7.92 6.95
5 -3 -10 17.89 5.85
5 -2 -8 4.94 6.52
5 -1 -5 41.18 6.05
5 -1 13 8.64 7.87
5 0 -1 1.24 8.22
5 0 8 61.80 9.94
6 -3 -6 11.60 7.55
-3 -13 -8 48.98 9.12
-3 -13 16 1.02 8.93
-3 -12 -7 87.78 9.87
-3 -12 15 145.43 9.67
-3 -11 14 1.12 7.72
-3 -8 4 350.22 11.80
-3 -8 5 23.20 7.96
-2 -14 -14 41.74 8.90
-2 -12 -13 47.67 7.43
-2 -8 -9 185.06 7.84
-2 -8 17 0.63 6.99
-2 -7 16 72.90 6.10
-2 -6 14 32.65 6.37
-2 -5 -3 152.44 12.08
-2 -5 11 216.50 7.68
-2 -4 4 163.86 8.15
-1 -13 -17 11.25 8.61
-1 -11 -16 49.25 8.11
-1 -6 -11 28.81 6.37
-1 -6 19 78.51 7.37
-1 -4 16 23.49 4.81
-1 -2 10 33.05 4.39
0 -12 -19 0.51 7.69
0 -10 -18 20.47 6.99
0 -9 -17 106.10 7.64
0 -8 24 17.27 8.38
0 -6 -14 6.94 4.65
0 -6 22 11.63 7.28
0 -5 -13 68.88 6.36
0 -5 21 3.80 6.42
0 -3 18 143.58 6.07
0 0 8 32.52 6.46
1 -11 -20 15.45 8.63
1 -8 -18 -0.91 7.05
1 -7 -17 22.45 6.92
1 -6 -16 46.52 7.13
1 -6 24 14.98 6.04
1 -5 -15 80.97 6.31
1 -5 23 6.02 6.10
1 -3 -12 197.24 5.33
1 -3 20 3.74 6.62
1 -2 18 1.08 6.63
1 -1 -8 87.13 5.10
1 -1 16 16.17 5.93
1 0 13 -5.29 6.37
1 1 8 606.71 11.17
2 -8 -19 82.21 6.68
2 -7 -18 16.19 6.77
2 -6 -17 55.03 6.92
2 -3 21 28.33 4.89
2 -2 19 13.85 5.87
2 0 -7 -1.32 5.46
2 1 11 110.44 6.02
3 -8 -19 23.65 6.60
3 -7 -18 16.38 6.29
3 -6 -17 55.17 6.50
3 -5 -16 11.58 5.75
3 -4 22 1.64 8.19
3 -3 21 1.54 5.89
3 1 -4 79.63 6.82
3 1 11 19.51 5.60
4 -4 -14 20.32 5.68
4 -2 18 5.19 7.04
4 0 13 2.04 7.03
4 1 8 26.68 7.78
5 -4 -12 36.70 6.23
5 -2 15 2.83 8.34
6 -2 -3 10.94 7.47
-3 -16 -10 -0.96 10.25
-3 -14 -9 1.79 9.36
-3 -11 -6 8.16 8.54
-3 -11 13 20.87 8.83
-3 -10 12 23.23 6.49
-3 -9 9 17.86 8.31
-2 -15 -15 2.06 7.75
-2 -13 -14 9.37 8.35
-2 -11 20 3.90 7.86
-2 -10 19 -6.66 7.79
-2 -9 18 32.74 7.67
-2 -7 15 135.98 7.54
-2 -6 13 59.98 6.75
-2 -5 10 161.52 7.35
-1 -14 -18 -6.98 9.42
-1 -12 -17 49.40 8.70
-1 -9 22 1.07 8.18
-1 -8 -14 112.42 6.60
-1 -8 21 15.63 8.04
-1 -7 20 20.22 7.12
-1 -5 17 75.67 7.33
-1 -4 -8 908.98 11.78
-1 -4 15 81.79 6.55
-1 -3 13 11.67 4.35
-1 -2 9 1105.78 11.97
0 -13 -20 13.26 8.78
0 -11 -19 -0.30 6.59
0 -7 23 13.89 6.18
0 -4 19 6.06 5.87
0 -3 -10 195.20 7.02
0 -2 -8 10.94 6.20
0 -1 -5 487.92 10.86
0 0 7 3.79 5.73
1 -10 -20 12.34 7.20
1 -9 -19 89.84 6.10
1 -5 22 -2.20 7.33
1 -4 -14 48.70 6.09
1 -4 21 -2.91 6.45
2 -9 -20 38.19 7.44
2 -5 23 25.29 7.41
2 -4 -15 41.47 7.07
2 -4 22 26.09 5.28
2 -2 -12 8.10 6.69
2 -1 -10 -0.10 5.21
2 0 14 90.41 6.06
2 1 -4 327.98 8.99
3 -9 -20 7.84 5.36
3 -4 -15 1.46 4.01
3 -2 -12 24.70 5.59
3 -1 -10 53.93 5.21
4 -7 -18 1.63 5.83
4 -6 -17 7.94 5.61
4 -3 -13 -1.26 5.34
4 -3 19 -7.43 7.25
4 -2 -11 81.02 5.43
4 -1 -9 4.02 4.54
4 -1 15 15.07 6.80
4 0 -6 188.75 6.82
4 1 -2 31.36 7.25
5 -5 -14 10.19 6.56
5 -3 -11 38.65 5.49
5 -1 -6 69.88 6.22
5 -1 12 10.29 7.12
5 0 -2 88.95 8.90
5 0 7 -0.89 7.62
6 -3 -7 1.90 7.29
-3 -13 15 -3.60 8.55
-3 -12 14 2.66 7.93
-2 -14 -15 1.02 9.48
-2 -10 -12 56.11 7.29
-2 -9 -11 0.69 6.26
-2 -8 16 75.39 7.22
-2 -6 -6 41.92 6.43
-1 -13 -18 13.26 8.36
-1 -10 -16 51.38 7.48
-1 -9 -15 35.18 4.94
-1 -7 -13 143.49 7.35
-1 -6 18 139.59 7.61
-1 -5 -10 217.41 5.83
-1 -2 8 1090.94 12.30
0 -9 -18 11.88 6.62
0 -8 -17 169.45 7.67
0 -8 23 4.15 7.57
0 -7 -16 103.56 7.04
0 -7 22 32.68 7.43
0 -6 21 12.51 6.90
0 -5 20 5.49 5.06
0 -4 -12 89.23 4.78
0 0 6 1556.29 15.85
1 -11 -21 7.76 7.80
1 -7 -18 57.99 7.07
1 -7 24 6.52 6.23
1 -6 -17 22.33 6.35
1 -6 23 2.26 5.78
1 -3 19 12.26 5.00
1 -2 -11 908.73 9.95
1 -2 17 183.88 7.28
1 -1 15 46.35 4.77
1 0 -6 1770.98 16.06
1 0 12 753.43 9.88
1 1 7 424.78 10.04
2 -10 -21 13.51 5.70
2 -7 -19 33.56 6.36
2 -6 -18 44.81 6.27
2 -3 -14 -3.54 6.15
2 -3 20 1.32 4.44
2 -2 18 4.28 6.04
2 0 -8 171.03 6.34
2 1 10 41.81 5.36
3 -8 -20 6.08 5.87
3 -7 -19 4.35 6.46
3 -6 -18 -3.77 6.05
3 -5 -17 22.11 6.15
3 -3 -14 38.91 4.23
3 -3 20 -5.56 5.90
3 -2 18 -3.15 6.84
3 0 -8 222.50 6.31
3 1 10 171.58 7.29
4 -4 -15 0.17 4.91
4 0 12 51.32 6.69
4 1 7 7.58 6.91
5 -4 -13 13.68 6.38
5 -2 -9 10.22 5.60
6 -2 -4 1.32 7.15
-3 -15 -10 -4.02 8.24
-3 -13 14 -3.42 7.78
-3 -12 13 -8.72 7.61
-3 -11 12 90.96 7.37
-3 -10 -5 24.39 9.58
-2 -12 -14 8.83 7.09
-2 -11 19 12.29 6.10
-2 -10 18 20.60 6.84
-2 -9 17 40.17 5.31
-2 -8 -10 78.18 6.14
-2 -7 14 130.54 6.78
-2 -6 12 9.53 5.82
-2 -5 9 140.02 6.76
-1 -11 -17 8.23 5.52
-1 -10 22 6.97 6.44
-1 -9 21 15.52 7.57
-1 -8 20 19.31 7.40
-1 -7 19 34.32 5.37
-1 -5 16 202.58 7.16
-1 -4 14 26.91 6.38
-1 -3 -6 154.91 7.21
-1 -2 -2 1592.90 29.30
-1 -2 7 140.62 6.89
0 -10 -19 0.98 7.19
0 -5 -14 276.65 7.43
0 -4 18 262.70 6.22
0 -1 11 3.59 3.67
0 0 5 -0.11 6.32
1 -8 -19 18.55 5.25
1 -5 -16 207.40 5.70
1 -5 21 9.02 7.01
1 -4 -15 85.67 5.64
1 -4 20 5.84 5.05
1 -1 -9 30.50 4.35
1 -1 14 87.20 6.34
1 0 11 -2.05 5.49
1 1 6 61.69 6.50
2 -9 -21 14.28 7.07
2 -8 -20 55.76 5.57
2 -6 23 8.03 7.32
2 -5 22 10.17 6.93
2 -4 -16 248.66 7.36
2 -4 21 4.15 4.60
2 0 13 2.31 4.90
3 -4 -16 17.20 5.54
3 -4 21 -0.01 5.45
3 -2 -13 282.12 6.76
3 -1 -11 20.40 5.10
3 0 13 -3.41 5.41
3 1 -5 68.08 6.13
4 -6 -18 13.97 5.64
4 -3 -14 13.55 4.69
4 -2 -12 41.45 4.86
4 -1 -10 16.93 4.22
4 -1 14 0.18 7.53
4 0 -7 -0.51 5.01
5 -5 -15 -0.58 6.60
5 -3 -12 15.05 5.07
5 -2 14 5.20 6.14
5 -1 -7 49.22 5.70
5 -1 11 3.39 7.29
6 -3 -8 1.61 7.19
-3 -14 -10 9.65 9.03
-3 -13 -9 11.69 8.69
-3 -12 -8 53.51 8.65
-3 -9 7 220.64 8.83
-2 -13 -15 21.28 7.69
-2 -12 19 6.79 8.02
-2 -11 18 49.58 7.75
-2 -9 16 87.57 6.88
-2 -8 15 173.88 7.03
-2 -7 13 82.50 6.67
-2 -6 11 122.29 6.52
-1 -12 -18 8.19 5.81
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1 -13 2 70.66 4.35
1 -13 3 32.67 4.07
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1 -2 20 2.85 4.40
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1 3 19 21.07 4.30
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1 -8 -8 66.09 4.11
1 -5 19 17.82 5.42
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1 -5 -11 202.02 4.14
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1 9 3 107.39 4.24
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1 4 14 283.00 4.35
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-1 4 -8 903.13 6.72
-1 6 -14 275.65 3.69
0 -20 2 24.01 4.39
0 -18 3 11.72 3.75
0 -16 4 5.36 2.70
0 -7 4 521.67 5.29
0 8 -24 7.18 3.02
0 8 -16 4.16 3.34
0 8 -15 233.05 4.02
1 -19 4 33.62 2.86
1 -16 5 54.26 3.52
1 -4 4 811.79 7.04
1 4 -3 83.53 3.78
1 9 -17 65.40 3.04
1 9 -16 16.76 3.58
2 -18 5 33.79 2.92
2 -12 6 99.20 3.65
2 -10 6 106.97 3.46
2 -3 4 82.30 2.91
2 1 1 177.62 7.40
2 8 -10 11.96 2.74
2 9 -14 27.09 2.38
3 -17 5 7.73 3.95
3 -13 6 19.55 2.59
3 -12 6 22.17 3.09
3 -11 6 1.69 2.87
3 -10 6 33.37 2.38
3 -6 5 219.55 4.00
3 9 -14 5.68 3.41
4 -14 5 0.03 3.34
4 -13 5 34.36 3.76
4 -12 5 16.45 3.65
4 -11 5 0.27 3.21
4 -10 5 75.91 3.73
4 -9 5 41.96 3.40
4 6 -7 18.24 3.54
5 -7 3 48.17 3.73
5 6 -10 0.69 3.64
5 7 -13 7.62 4.07
6 -6 0 1.37 4.11
6 -4 -1 2.38 4.73
-4 -7 -15 17.23 6.01
-4 -6 -17 7.59 5.52
-3 -17 -7 18.28 5.09
-3 -12 -5 36.73 4.78
-3 -11 -5 6.09 4.65
-3 -2 -10 49.36 3.84
-3 0 -14 117.91 4.12
-3 1 -22 -1.41 3.24
-3 1 -19 1.83 2.74
-3 1 -18 7.50 3.85
-3 1 -17 8.97 3.69
-2 -2 -4 518.59 9.35
-2 -1 -5 187.60 5.30
-2 2 -9 11.32 2.78
-2 3 -11 104.15 3.59
-2 4 -14 51.74 3.36
-1 -19 0 51.25 4.01
-1 -15 2 31.67 3.19
-1 -3 0 488.68 10.60
-1 3 -6 166.68 4.51
-1 5 -10 235.53 3.54
-1 6 -13 198.78 3.29
-1 7 -24 9.28 4.20
-1 7 -23 9.85 3.95
-1 7 -22 7.51 3.04
-1 7 -21 6.34 2.89
-1 7 -20 5.71 2.96
-1 7 -18 32.03 3.31
0 -15 4 91.89 3.09
0 -14 4 65.20 3.77
0 -8 4 345.53 4.72
0 2 -2 175.72 4.98
0 7 -11 156.45 3.08
1 -20 3 -0.46 3.03
1 -18 4 3.72 3.15
1 -15 5 71.95 3.19
1 -7 5 76.16 2.45
1 6 -6 27.03 3.11
1 7 -8 242.45 4.22
1 8 -11 54.74 2.74
1 9 -15 63.17 2.91
1 9 -14 178.78 3.85
2 -19 4 2.97 3.59
2 -16 5 71.20 3.40
2 -11 6 23.98 2.35
2 -6 5 56.41 3.18
2 7 -7 45.55 2.58
2 9 -13 47.96 2.34
2 10 -21 28.76 3.71
2 10 -20 21.52 3.32
2 10 -19 4.45 3.20
2 10 -18 29.32 3.03
3 -16 5 80.19 3.89
3 -4 4 141.54 3.53
3 -2 3 26.90 3.05
3 8 -10 28.45 3.43
3 9 -13 21.23 3.45
3 10 -19 2.15 3.71
4 -6 4 1.91 3.02
4 -2 2 64.45 4.03
4 5 -5 109.86 5.66
4 7 -9 77.33 3.61
4 8 -12 7.12 3.68
4 9 -17 50.27 4.10
4 9 -16 3.11 3.62
5 -9 3 0.62 3.21
5 -8 3 4.47 3.08
5 -5 2 3.93 3.36
5 -3 1 2.22 3.13
-4 -6 -16 10.74 5.24
-4 -5 -18 -0.81 4.97
-3 -15 -6 -0.16 4.26
-3 -1 -11 29.65 3.24
-3 0 -13 2.25 3.24
-3 1 -16 30.05 3.61
-2 0 -6 1924.08 11.68
-2 4 -13 118.00 3.63
-2 5 -23 23.11 4.01
-2 5 -22 15.98 3.10
-2 5 -21 0.95 2.78
-2 5 -20 32.30 2.81
-2 5 -19 16.51 3.64
-2 5 -18 2.64 3.40
-2 5 -17 41.65 3.31
-1 -14 2 5.84 2.40
-1 -13 2 48.87 3.41
-1 -8 2 525.41 5.79
-1 6 -12 86.15 3.51
-1 7 -16 17.37 3.33
0 -19 2 56.92 3.00
0 -17 3 52.14 2.88
0 -13 4 24.52 3.09
0 -12 4 15.97 3.31
0 -11 4 378.42 4.79
0 -3 2 82.80 4.22
0 3 -3 126.21 4.37
0 5 -6 319.06 4.27
0 7 -10 127.11 3.62
0 9 -23 2.56 3.92
0 9 -22 15.09 3.72
0 9 -21 47.10 4.00
0 9 -20 15.07 3.53
0 9 -19 1.63 3.35
1 -19 3 39.92 3.73
1 -17 4 3.54 3.13
1 -14 5 25.99 2.22
1 -1 2 751.92 9.29
1 8 -10 74.67 3.46
1 9 -13 371.27 4.42
1 10 -22 3.63 3.67
1 10 -21 -1.43 3.77
1 10 -20 14.06 3.47
2 -18 4 107.24 3.96
2 -15 5 37.26 3.23
2 6 -5 75.94 3.13
2 8 -9 511.93 4.76
2 9 -12 67.87 3.03
2 10 -17 9.71 2.90
2 10 -16 104.39 2.97
3 -17 4 -1.98 3.69
3 -15 5 7.91 2.56
3 -14 5 5.08 3.53
3 -8 5 15.13 3.00
3 -7 5 73.42 2.55
3 7 -7 27.71 3.65
3 10 -18 2.05 3.95
3 10 -17 5.58 3.69
4 -15 4 3.24 3.27
4 -14 4 -3.55 3.43
4 -7 4 65.18 3.18
4 9 -15 22.67 3.66
5 -12 3 1.89 2.78
5 -11 3 11.55 3.27
5 -10 3 7.86 3.23
5 -6 2 31.12 3.72
5 7 -12 4.09 3.93
6 -3 -2 16.59 4.34
-4 -5 -17 14.35 5.05
-3 1 -15 33.39 3.39
-3 2 -22 2.08 4.26
-3 2 -21 15.51 4.20
-3 2 -20 1.32 3.85
-3 2 -19 44.96 4.02
-3 2 -18 2.97 3.45
-2 -13 -1 108.48 3.92
-2 -12 -1 87.22 4.31
-2 1 -7 368.12 5.32
-2 3 -10 92.39 3.44
-2 5 -16 130.91 3.81
-1 -18 0 14.37 3.67
-1 -16 1 51.13 3.67
-1 -12 2 35.55 3.15
-1 -11 2 186.24 4.00
-1 -10 2 12.98 2.92
-1 4 -7 140.82 3.72
-1 5 -9 45.34 2.30
-1 6 -11 31.69 3.03
-1 7 -15 73.62 2.63
-1 7 -14 54.57 3.01
0 -20 1 6.16 2.95
0 -18 2 247.17 4.54
0 -16 3 247.41 3.70
0 8 -12 5.84 2.79
0 9 -18 8.64 2.48
0 9 -17 116.22 3.84
1 -20 2 -0.03 3.50
1 -18 3 16.77 3.34
1 -16 4 19.01 3.17
1 -5 4 432.57 4.65
1 5 -4 260.84 4.62
1 10 -19 22.55 2.81
1 10 -18 90.38 3.99
1 10 -17 8.92 3.46
2 -17 4 -0.01 3.15
2 -14 5 2.67 2.71
2 -13 5 372.75 4.33
2 -8 5 292.32 4.21
2 -7 5 177.26 3.27
2 -4 4 496.42 5.46
2 -2 3 135.83 3.99
2 9 -11 11.05 2.53
2 10 -15 13.01 2.70
3 -16 4 4.12 3.61
3 -13 5 22.24 2.49
3 -12 5 34.58 3.35
3 -11 5 11.32 3.08
3 -10 5 29.52 3.11
3 -9 5 53.24 3.05
3 8 -9 50.75 3.37
3 9 -12 31.70 3.46
4 -13 4 10.94 3.30
4 -9 4 19.22 3.28
4 -8 4 26.60 3.01
4 8 -11 12.02 3.33
5 -4 1 10.18 3.71
5 -2 0 19.71 3.17
6 -5 -1 17.59 3.58
-4 -4 -19 1.37 4.56
-3 -16 -7 31.74 4.35
-3 -2 -9 257.08 5.32
-3 1 -14 23.20 3.26
-3 2 -17 55.83 3.82
-2 -11 -1 37.57 3.35
-2 -10 -1 25.59 3.24
-2 2 -8 620.89 5.96
-2 4 -12 246.90 4.36
-2 5 -15 2.91 3.16
-2 6 -23 6.29 3.57
-2 6 -22 10.45 3.61
-2 6 -21 21.34 3.50
-2 6 -20 0.38 3.42
-1 -19 -1 18.04 3.71
-1 -15 1 4.61 3.10
-1 8 -23 4.64 2.91
-1 8 -21 25.32 2.85
-1 8 -20 21.32 2.64
-1 8 -18 25.73 3.40
0 -17 2 5.20 3.42
0 -15 3 24.03 2.58
0 -6 3 74.46 3.69
0 6 -7 52.48 3.13
0 7 -9 83.51 3.35
0 9 -16 8.88 2.28
0 9 -15 29.92 3.56
1 -15 4 64.09 2.94
1 -3 3 633.70 6.61
1 7 -7 78.15 3.24
1 8 -9 199.70 3.90
1 9 -12 233.54 3.97
1 10 -16 -2.66 3.19
2 -18 3 8.30 3.41
2 -16 4 15.32 3.04
2 -12 5 272.85 3.88
2 -11 5 54.28 2.92
2 -10 5 37.27 2.99
2 -9 5 130.20 3.57
2 10 -14 118.47 3.36
3 -15 4 49.72 3.64
3 -5 4 136.91 2.86
3 -1 2 56.28 3.35
3 6 -5 112.93 4.03
3 9 -11 124.16 3.83
3 10 -15 22.16 3.38
4 -15 3 4.57 3.64
4 -11 4 4.68 2.31
4 -10 4 13.60 2.43
4 -5 3 34.42 3.05
5 -12 2 4.15 3.54
5 -8 2 17.43 3.26
5 -7 2 3.68 2.86
6 -6 -1 0.80 3.65
-2 5 -14 15.15 2.31
-2 6 -19 8.54 2.73
-1 -17 0 55.90 3.14
-1 8 -17 19.84 2.38
0 -14 3 25.18 2.43
1 -19 2 65.79 2.93
1 -17 3 14.47 2.42
1 -14 4 14.30 2.11
1 -6 4 153.05 2.99
1 10 -15 41.65 2.52
2 11 -20 7.88 2.62
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 34412
_shelx_res_file
;
TITL g73_a.res in Pc
g73.res
created by SHELXL-2018/1 at 13:24:59 on 10-Jul-2020
REM Old TITL G73 LIGAND
REM SHELXT solution in Pc
REM R1 0.116, Rweak 0.020, Alpha 0.006, Orientation as input
REM Flack x = 0.104 ( 0.028 ) from Parsons' quotients
REM Formula found by SHELXT: C28 Br2 N4 O2 S2
CELL 0.71073 4.6404 15.0174 19.074 90 91.052 90
ZERR 4 0.0007 0.0024 0.0025 0 0.012 0
LATT -1
SYMM +X,-Y,0.5+Z
SFAC C H Br N O S
UNIT 56 44 4 8 4 4
EQIV $1 -1+X,-1+Y,+Z
EQIV $2 1+X,1+Y,+Z
L.S. 10
PLAN 2
SIZE 0.04 0.052 0.678
TEMP -148.15
HTAB N2 O1
HTAB N2A O1A
HTAB N1 S1A_$1
HTAB N1A S1_$2
list 4
BOND $H
MERG
MORE -1
HTAB
fmap 2 53
acta
OMIT -2 52
OMIT 1 5 11
OMIT 0 5 11
REM
REM
REM
WGHT 0.143600
FVAR 0.34070
BR1A 3 0.121563 0.360146 0.600488 11.00000 0.04155 0.02330 =
0.03703 0.00175 0.00632 -0.00426
BR1 3 0.847177 0.397776 0.388041 11.00000 0.04737 0.02154 =
0.04043 0.00022 0.00915 -0.00661
S1 6 0.219299 -0.051819 0.423204 11.00000 0.04761 0.01932 =
0.03285 -0.00335 0.01469 -0.00212
S1A 6 0.835627 0.799206 0.587133 11.00000 0.05496 0.02259 =
0.03475 -0.00720 0.02018 -0.00133
O1A 5 1.111416 0.570501 0.449073 11.00000 0.03723 0.02158 =
0.02894 -0.00095 0.00494 -0.00663
O1 5 -0.122882 0.182588 0.546079 11.00000 0.03689 0.02016 =
0.02950 0.00089 0.00588 -0.00122
N2 4 0.201099 0.126684 0.446058 11.00000 0.02979 0.02110 =
0.02062 -0.00459 0.00546 -0.00092
AFIX 43
H2 2 0.116675 0.168717 0.470412 11.00000 -1.20000
AFIX 0
N2A 4 0.814232 0.624670 0.554828 11.00000 0.02924 0.02396 =
0.02769 -0.00392 0.00592 -0.00068
AFIX 43
H2A 2 0.886318 0.584080 0.526870 11.00000 -1.20000
AFIX 0
N1A 4 1.130364 0.711459 0.493640 11.00000 0.02875 0.01995 =
0.02864 -0.00223 0.00756 -0.00490
AFIX 43
H1A 2 1.221915 0.762601 0.490681 11.00000 -1.20000
AFIX 0
N1 4 -0.098513 0.038217 0.510796 11.00000 0.02669 0.01930 =
0.03025 0.00163 0.00606 -0.00298
AFIX 43
H1 2 -0.172561 -0.015048 0.517202 11.00000 -1.20000
AFIX 0
C12 1 -0.483748 0.144453 0.655878 11.00000 0.03319 0.02624 =
0.03016 -0.00384 0.00546 0.00695
AFIX 43
H12 2 -0.404248 0.202517 0.652126 11.00000 -1.20000
AFIX 0
C10 1 -0.204048 0.104555 0.552791 11.00000 0.01986 0.02177 =
0.02415 -0.00036 -0.00027 -0.00291
C1 1 0.110936 0.044145 0.459236 11.00000 0.03002 0.02480 =
0.02305 0.00078 0.00253 0.00135
C22A 1 0.527379 0.634555 0.663336 11.00000 0.03273 0.02872 =
0.01953 -0.00298 0.00668 -0.00387
AFIX 43
H22A 2 0.609316 0.690436 0.675859 11.00000 -1.20000
AFIX 0
C24 1 0.806103 0.236286 0.309912 11.00000 0.03374 0.02809 =
0.02684 0.00594 0.00643 -0.00597
AFIX 43
H24 2 0.940707 0.263197 0.279534 11.00000 -1.20000
AFIX 0
C11A 1 1.418072 0.672291 0.392588 11.00000 0.02422 0.01968 =
0.02296 -0.00147 0.00201 0.00322
C23A 1 0.330572 0.594100 0.705780 11.00000 0.03647 0.03604 =
0.02592 -0.00353 -0.00288 0.00640
AFIX 43
H23A 2 0.278747 0.622390 0.748276 11.00000 -1.20000
AFIX 0
C26 1 0.510334 0.244592 0.411880 11.00000 0.02864 0.01809 =
0.02798 0.00142 0.00218 0.00901
AFIX 43
H26 2 0.441157 0.277844 0.450456 11.00000 -1.20000
AFIX 0
C21 1 0.410202 0.156886 0.399261 11.00000 0.03118 0.02561 =
0.02587 0.00218 -0.00083 0.00253
C25 1 0.707068 0.280703 0.368028 11.00000 0.03557 0.02428 =
0.02843 -0.00421 -0.00071 0.00835
C26A 1 0.484523 0.509283 0.582899 11.00000 0.02999 0.02840 =
0.01988 -0.00250 0.00388 0.00698
AFIX 43
H26A 2 0.539187 0.479402 0.541306 11.00000 -1.20000
AFIX 0
C13A 1 1.635058 0.632493 0.284126 11.00000 0.03080 0.02398 =
0.02877 -0.00525 0.00726 0.00131
AFIX 43
H13A 2 1.656135 0.591839 0.246407 11.00000 -1.20000
AFIX 0
C11 1 -0.412565 0.078956 0.607268 11.00000 0.01906 0.02174 =
0.02922 -0.00064 -0.00267 0.00242
C23 1 0.702491 0.150992 0.297329 11.00000 0.03971 0.02838 =
0.02467 0.00018 0.00465 -0.00341
AFIX 43
H23 2 0.768490 0.119194 0.257672 11.00000 -1.20000
AFIX 0
C13 1 -0.667480 0.125118 0.708785 11.00000 0.03038 0.03337 =
0.02962 -0.00938 0.00430 0.00078
AFIX 43
H13 2 -0.711529 0.169799 0.742179 11.00000 -1.20000
AFIX 0
C21A 1 0.605551 0.591420 0.600686 11.00000 0.02722 0.02319 =
0.02322 0.00010 0.00147 0.00532
C10A 1 1.206051 0.646170 0.446622 11.00000 0.02789 0.02340 =
0.01952 -0.00365 0.00364 0.00128
C16 1 -0.534842 -0.005357 0.613207 11.00000 0.03315 0.02360 =
0.02574 -0.00120 0.00426 -0.00040
AFIX 43
H16 2 -0.488645 -0.050385 0.580284 11.00000 -1.20000
AFIX 0
C1A 1 0.921720 0.704524 0.545805 11.00000 0.02631 0.02298 =
0.02697 -0.00181 -0.00207 -0.00156
C24A 1 0.204613 0.512500 0.688143 11.00000 0.02676 0.02737 =
0.03021 0.00964 0.00355 -0.00002
AFIX 43
H24A 2 0.067460 0.485458 0.717769 11.00000 -1.20000
AFIX 0
C14A 1 1.791965 0.710235 0.284871 11.00000 0.02759 0.04143 =
0.03289 -0.00190 0.00118 0.00014
AFIX 43
H14A 2 1.921841 0.722651 0.248208 11.00000 -1.20000
AFIX 0
C22 1 0.503982 0.110596 0.341311 11.00000 0.03578 0.02162 =
0.03261 -0.00295 -0.00119 -0.00042
AFIX 43
H22 2 0.434508 0.052300 0.331595 11.00000 -1.20000
AFIX 0
C25A 1 0.284788 0.472287 0.626568 11.00000 0.03319 0.01660 =
0.02980 0.00023 -0.00273 0.00298
C12A 1 1.447046 0.612489 0.337374 11.00000 0.02814 0.02263 =
0.03087 -0.00343 0.00849 -0.00847
AFIX 43
H12A 2 1.339264 0.558708 0.336270 11.00000 -1.20000
AFIX 0
C14 1 -0.789935 0.042266 0.714667 11.00000 0.02349 0.03277 =
0.02422 0.00220 0.00310 0.00024
AFIX 43
H14 2 -0.919974 0.030087 0.751344 11.00000 -1.20000
AFIX 0
C15 1 -0.721807 -0.023916 0.666322 11.00000 0.03578 0.02560 =
0.03024 0.00331 0.00305 -0.00406
AFIX 43
H15 2 -0.804361 -0.081564 0.670121 11.00000 -1.20000
AFIX 0
C15A 1 1.759605 0.770935 0.339801 11.00000 0.03408 0.02565 =
0.03365 0.00168 0.00266 -0.00754
AFIX 43
H15A 2 1.865168 0.825140 0.340197 11.00000 -1.20000
AFIX 0
C16A 1 1.574425 0.751850 0.393222 11.00000 0.03054 0.02171 =
0.03562 -0.00558 0.00133 0.00526
AFIX 43
H16A 2 1.552695 0.792864 0.430674 11.00000 -1.20000
AFIX 0
HKLF 4
REM g73_a.res in Pc
REM R1 = 0.0656 for 4294 Fo > 4sig(Fo) and 0.0761 for all 4909 data
REM 343 parameters refined using 2 restraints
END
WGHT 0.1436 0.0000
REM Instructions for potential hydrogen bonds
HTAB N2 O1
HTAB N2A O1A
HTAB C22A S1A
HTAB C22 S1
REM Highest difference peak 1.967, deepest hole -0.654, 1-sigma level 0.151
Q1 1 1.1210 0.8561 0.6025 11.00000 0.05 1.97
Q2 1 1.8543 0.8926 0.3878 11.00000 0.05 1.68
;
_shelx_res_checksum 25907
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, 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 Br1A 0.1216(2) 0.36015(7) 0.60049(6) 0.0339(3) Uani d 1 . .
Br Br1 0.8472(2) 0.39778(7) 0.38804(7) 0.0363(3) Uani d 1 . .
S S1 0.2193(7) -0.05182(18) 0.42320(16) 0.0331(6) Uani d 1 . .
S S1A 0.8356(7) 0.7992(2) 0.58713(17) 0.0372(7) Uani d 1 . .
O O1A 1.1114(18) 0.5705(5) 0.4491(4) 0.0292(17) Uani d 1 . .
O O1 -0.1229(18) 0.1826(5) 0.5461(4) 0.0288(17) Uani d 1 . .
N N2 0.201(2) 0.1267(7) 0.4461(5) 0.0238(19) Uani d 1 . .
H H2 0.116675 0.168717 0.470412 0.029 Uiso calc 1 . .
N N2A 0.814(2) 0.6247(7) 0.5548(5) 0.027(2) Uani d 1 . .
H H2A 0.886318 0.584080 0.526870 0.032 Uiso calc 1 . .
N N1A 1.130(2) 0.7115(6) 0.4936(5) 0.0257(18) Uani d 1 . .
H H1A 1.221915 0.762601 0.490681 0.031 Uiso calc 1 . .
N N1 -0.099(2) 0.0382(6) 0.5108(5) 0.0253(18) Uani d 1 . .
H H1 -0.172561 -0.015048 0.517202 0.030 Uiso calc 1 . .
C C12 -0.484(3) 0.1445(8) 0.6559(7) 0.030(3) Uani d 1 . .
H H12 -0.404248 0.202517 0.652126 0.036 Uiso calc 1 . .
C C10 -0.204(2) 0.1046(7) 0.5528(6) 0.022(2) Uani d 1 . .
C C1 0.111(2) 0.0441(7) 0.4592(6) 0.026(2) Uani d 1 . .
C C22A 0.527(3) 0.6346(8) 0.6633(6) 0.027(2) Uani d 1 . .
H H22A 0.609316 0.690436 0.675859 0.032 Uiso calc 1 . .
C C24 0.806(3) 0.2363(8) 0.3099(6) 0.029(2) Uani d 1 . .
H H24 0.940707 0.263197 0.279534 0.035 Uiso calc 1 . .
C C11A 1.418(2) 0.6723(7) 0.3926(5) 0.022(2) Uani d 1 . .
C C23A 0.331(3) 0.5941(9) 0.7058(6) 0.033(3) Uani d 1 . .
H H23A 0.278747 0.622390 0.748276 0.039 Uiso calc 1 . .
C C26 0.510(2) 0.2446(7) 0.4119(6) 0.025(2) Uani d 1 . .
H H26 0.441157 0.277844 0.450456 0.030 Uiso calc 1 . .
C C21 0.410(3) 0.1569(8) 0.3993(6) 0.028(2) Uani d 1 . .
C C25 0.707(3) 0.2807(8) 0.3680(6) 0.029(2) Uani d 1 . .
C C26A 0.485(2) 0.5093(8) 0.5829(6) 0.026(2) Uani d 1 . .
H H26A 0.539187 0.479402 0.541306 0.031 Uiso calc 1 . .
C C13A 1.635(3) 0.6325(7) 0.2841(6) 0.028(2) Uani d 1 . .
H H13A 1.656135 0.591839 0.246407 0.033 Uiso calc 1 . .
C C11 -0.413(2) 0.0790(7) 0.6073(6) 0.023(2) Uani d 1 . .
C C23 0.702(3) 0.1510(8) 0.2973(6) 0.031(2) Uani d 1 . .
H H23 0.768490 0.119194 0.257672 0.037 Uiso calc 1 . .
C C13 -0.667(3) 0.1251(9) 0.7088(6) 0.031(2) Uani d 1 . .
H H13 -0.711529 0.169799 0.742179 0.037 Uiso calc 1 . .
C C21A 0.606(3) 0.5914(7) 0.6007(6) 0.025(2) Uani d 1 . .
C C10A 1.206(3) 0.6462(7) 0.4466(6) 0.024(2) Uani d 1 . .
C C16 -0.535(3) -0.0054(8) 0.6132(6) 0.027(2) Uani d 1 . .
H H16 -0.488645 -0.050385 0.580284 0.033 Uiso calc 1 . .
C C1A 0.922(2) 0.7045(7) 0.5458(6) 0.025(2) Uani d 1 . .
C C24A 0.205(2) 0.5125(8) 0.6881(6) 0.028(2) Uani d 1 . .
H H24A 0.067460 0.485458 0.717769 0.034 Uiso calc 1 . .
C C14A 1.792(3) 0.7102(9) 0.2849(7) 0.034(3) Uani d 1 . .
H H14A 1.921841 0.722651 0.248208 0.041 Uiso calc 1 . .
C C22 0.504(3) 0.1106(8) 0.3413(7) 0.030(3) Uani d 1 . .
H H22 0.434508 0.052300 0.331595 0.036 Uiso calc 1 . .
C C25A 0.285(2) 0.4723(7) 0.6266(6) 0.027(2) Uani d 1 . .
C C12A 1.447(3) 0.6125(8) 0.3374(7) 0.027(2) Uani d 1 . .
H H12A 1.339264 0.558708 0.336270 0.033 Uiso calc 1 . .
C C14 -0.790(2) 0.0423(8) 0.7147(6) 0.027(2) Uani d 1 . .
H H14 -0.919974 0.030087 0.751344 0.032 Uiso calc 1 . .
C C15 -0.722(3) -0.0239(8) 0.6663(6) 0.031(2) Uani d 1 . .
H H15 -0.804361 -0.081564 0.670121 0.037 Uiso calc 1 . .
C C15A 1.760(3) 0.7709(8) 0.3398(6) 0.031(2) Uani d 1 . .
H H15A 1.865168 0.825140 0.340197 0.037 Uiso calc 1 . .
C C16A 1.574(3) 0.7518(8) 0.3932(6) 0.029(2) Uani d 1 . .
H H16A 1.552695 0.792864 0.430674 0.035 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
Br1A 0.0415(6) 0.0233(6) 0.0370(6) -0.0043(5) 0.0063(4) 0.0017(5)
Br1 0.0474(7) 0.0215(6) 0.0404(6) -0.0066(5) 0.0091(5) 0.0002(5)
S1 0.0476(17) 0.0193(12) 0.0329(14) -0.0021(11) 0.0147(12) -0.0033(10)
S1A 0.0550(19) 0.0226(13) 0.0347(14) -0.0013(13) 0.0202(13) -0.0072(11)
O1A 0.037(4) 0.022(4) 0.029(4) -0.007(3) 0.005(3) -0.001(3)
O1 0.037(4) 0.020(4) 0.029(4) -0.001(3) 0.006(3) 0.001(3)
N2 0.030(5) 0.021(4) 0.021(4) -0.001(4) 0.005(4) -0.005(4)
N2A 0.029(5) 0.024(4) 0.028(5) -0.001(4) 0.006(4) -0.004(4)
N1A 0.029(5) 0.020(4) 0.029(4) -0.005(4) 0.008(4) -0.002(4)
N1 0.027(4) 0.019(4) 0.030(5) -0.003(4) 0.006(4) 0.002(4)
C12 0.033(6) 0.026(6) 0.030(6) 0.007(5) 0.005(5) -0.004(5)
C10 0.020(5) 0.022(6) 0.024(5) -0.003(4) 0.000(4) 0.000(4)
C1 0.030(5) 0.025(5) 0.023(5) 0.001(4) 0.003(4) 0.001(4)
C22A 0.033(6) 0.029(6) 0.020(5) -0.004(4) 0.007(4) -0.003(4)
C24 0.034(6) 0.028(6) 0.027(5) -0.006(5) 0.006(4) 0.006(4)
C11A 0.024(5) 0.020(5) 0.023(5) 0.003(4) 0.002(4) -0.001(4)
C23A 0.036(6) 0.036(7) 0.026(6) 0.006(5) -0.003(5) -0.004(4)
C26 0.029(5) 0.018(5) 0.028(5) 0.009(4) 0.002(4) 0.001(4)
C21 0.031(6) 0.026(5) 0.026(5) 0.003(4) -0.001(4) 0.002(4)
C25 0.036(6) 0.024(5) 0.028(5) 0.008(5) -0.001(5) -0.004(4)
C26A 0.030(6) 0.028(5) 0.020(5) 0.007(4) 0.004(4) -0.003(4)
C13A 0.031(6) 0.024(5) 0.029(6) 0.001(4) 0.007(5) -0.005(4)
C11 0.019(5) 0.022(4) 0.029(5) 0.002(4) -0.003(4) -0.001(4)
C23 0.040(7) 0.028(6) 0.025(5) -0.003(5) 0.005(5) 0.000(4)
C13 0.030(6) 0.033(6) 0.030(6) 0.001(5) 0.004(5) -0.009(5)
C21A 0.027(5) 0.023(5) 0.023(5) 0.005(5) 0.001(4) 0.000(4)
C10A 0.028(5) 0.023(6) 0.020(5) 0.001(4) 0.004(4) -0.004(4)
C16 0.033(6) 0.024(5) 0.026(5) 0.000(4) 0.004(4) -0.001(4)
C1A 0.026(5) 0.023(5) 0.027(5) -0.002(4) -0.002(4) -0.002(4)
C24A 0.027(5) 0.027(5) 0.030(6) 0.000(4) 0.004(4) 0.010(4)
C14A 0.028(6) 0.041(7) 0.033(6) 0.000(5) 0.001(4) -0.002(5)
C22 0.036(7) 0.022(6) 0.033(6) 0.000(4) -0.001(5) -0.003(4)
C25A 0.033(6) 0.017(5) 0.030(6) 0.003(4) -0.003(5) 0.000(4)
C12A 0.028(6) 0.023(6) 0.031(6) -0.008(4) 0.008(4) -0.003(5)
C14 0.023(5) 0.033(6) 0.024(5) 0.000(4) 0.003(4) 0.002(4)
C15 0.036(6) 0.026(5) 0.030(6) -0.004(4) 0.003(5) 0.003(4)
C15A 0.034(6) 0.026(5) 0.034(6) -0.008(4) 0.003(5) 0.002(5)
C16A 0.031(6) 0.022(5) 0.036(6) 0.005(4) 0.001(5) -0.006(4)
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_
_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 N2 H2 . . 115.0 ?
C1 N2 C21 . . 130.0(11) ?
C21 N2 H2 . . 115.0 ?
C21A N2A H2A . . 113.8 ?
C1A N2A H2A . . 113.8 ?
C1A N2A C21A . . 132.3(10) ?
C10A N1A H1A . . 116.7 ?
C10A N1A C1A . . 126.5(9) ?
C1A N1A H1A . . 116.7 ?
C10 N1 H1 . . 115.7 ?
C10 N1 C1 . . 128.6(9) ?
C1 N1 H1 . . 115.7 ?
C11 C12 H12 . . 120.0 ?
C13 C12 H12 . . 120.0 ?
C13 C12 C11 . . 120.0(12) ?
O1 C10 N1 . . 120.9(11) ?
O1 C10 C11 . . 121.4(10) ?
N1 C10 C11 . . 117.7(9) ?
N2 C1 S1 . . 128.6(10) ?
N2 C1 N1 . . 114.6(10) ?
N1 C1 S1 . . 116.8(8) ?
C23A C22A H22A . . 120.7 ?
C23A C22A C21A . . 118.7(11) ?
C21A C22A H22A . . 120.7 ?
C25 C24 H24 . . 121.1 ?
C25 C24 C23 . . 117.8(11) ?
C23 C24 H24 . . 121.1 ?
C12A C11A C10A . . 115.3(10) ?
C12A C11A C16A . . 120.0(11) ?
C16A C11A C10A . . 124.6(10) ?
C22A C23A H23A . . 119.1 ?
C22A C23A C24A . . 121.8(12) ?
C24A C23A H23A . . 119.1 ?
C21 C26 H26 . . 120.4 ?
C25 C26 H26 . . 120.4 ?
C25 C26 C21 . . 119.2(11) ?
N2 C21 C26 . . 114.9(10) ?
C22 C21 N2 . . 125.2(11) ?
C22 C21 C26 . . 119.8(12) ?
C24 C25 Br1 . . 119.2(9) ?
C26 C25 Br1 . . 118.2(9) ?
C26 C25 C24 . . 122.5(11) ?
C21A C26A H26A . . 120.6 ?
C25A C26A H26A . . 120.6 ?
C25A C26A C21A . . 118.9(10) ?
C14A C13A H13A . . 119.4 ?
C14A C13A C12A . . 121.1(11) ?
C12A C13A H13A . . 119.4 ?
C12 C11 C10 . . 116.6(11) ?
C16 C11 C12 . . 119.0(12) ?
C16 C11 C10 . . 124.4(10) ?
C24 C23 H23 . . 119.1 ?
C24 C23 C22 . . 121.8(12) ?
C22 C23 H23 . . 119.1 ?
C12 C13 H13 . . 119.4 ?
C12 C13 C14 . . 121.2(11) ?
C14 C13 H13 . . 119.4 ?
N2A C21A C22A . . 123.6(10) ?
C26A C21A N2A . . 116.2(10) ?
C26A C21A C22A . . 120.2(12) ?
O1A C10A N1A . . 122.8(11) ?
O1A C10A C11A . . 121.0(10) ?
N1A C10A C11A . . 116.2(9) ?
C11 C16 H16 . . 119.7 ?
C15 C16 C11 . . 120.5(11) ?
C15 C16 H16 . . 119.7 ?
N2A C1A S1A . . 128.2(10) ?
N2A C1A N1A . . 115.4(10) ?
N1A C1A S1A . . 116.3(8) ?
C23A C24A H24A . . 120.9 ?
C25A C24A C23A . . 118.1(11) ?
C25A C24A H24A . . 120.9 ?
C13A C14A H14A . . 120.1 ?
C13A C14A C15A . . 119.8(12) ?
C15A C14A H14A . . 120.1 ?
C21 C22 C23 . . 118.9(11) ?
C21 C22 H22 . . 120.6 ?
C23 C22 H22 . . 120.6 ?
C26A C25A Br1A . . 117.9(8) ?
C26A C25A C24A . . 122.3(11) ?
C24A C25A Br1A . . 119.8(9) ?
C11A C12A H12A . . 120.5 ?
C13A C12A C11A . . 119.1(11) ?
C13A C12A H12A . . 120.5 ?
C13 C14 H14 . . 120.3 ?
C13 C14 C15 . . 119.5(11) ?
C15 C14 H14 . . 120.3 ?
C16 C15 C14 . . 119.7(11) ?
C16 C15 H15 . . 120.1 ?
C14 C15 H15 . . 120.1 ?
C14A C15A H15A . . 120.1 ?
C16A C15A C14A . . 119.8(11) ?
C16A C15A H15A . . 120.1 ?
C11A C16A H16A . . 119.9 ?
C15A C16A C11A . . 120.2(10) ?
C15A C16A H16A . . 119.9 ?
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
Br1A C25A . 1.909(11) ?
Br1 C25 . 1.911(12) ?
S1 C1 . 1.678(12) ?
S1A C1A . 1.678(11) ?
O1A C10A . 1.219(14) ?
O1 C10 . 1.238(14) ?
N2 H2 . 0.8800 ?
N2 C1 . 1.334(15) ?
N2 C21 . 1.406(17) ?
N2A H2A . 0.8800 ?
N2A C21A . 1.408(17) ?
N2A C1A . 1.311(15) ?
N1A H1A . 0.8800 ?
N1A C10A . 1.379(14) ?
N1A C1A . 1.405(15) ?
N1 H1 . 0.8800 ?
N1 C10 . 1.374(15) ?
N1 C1 . 1.398(15) ?
C12 H12 . 0.9500 ?
C12 C11 . 1.396(16) ?
C12 C13 . 1.36(2) ?
C10 C11 . 1.483(17) ?
C22A H22A . 0.9500 ?
C22A C23A . 1.37(2) ?
C22A C21A . 1.412(17) ?
C24 H24 . 0.9500 ?
C24 C25 . 1.380(17) ?
C24 C23 . 1.388(17) ?
C11A C10A . 1.490(16) ?
C11A C12A . 1.392(17) ?
C11A C16A . 1.398(16) ?
C23A H23A . 0.9500 ?
C23A C24A . 1.396(18) ?
C26 H26 . 0.9500 ?
C26 C21 . 1.416(16) ?
C26 C25 . 1.362(18) ?
C21 C22 . 1.383(19) ?
C26A H26A . 0.9500 ?
C26A C21A . 1.395(16) ?
C26A C25A . 1.375(17) ?
C13A H13A . 0.9500 ?
C13A C14A . 1.376(17) ?
C13A C12A . 1.384(18) ?
C11 C16 . 1.393(16) ?
C23 H23 . 0.9500 ?
C23 C22 . 1.40(2) ?
C13 H13 . 0.9500 ?
C13 C14 . 1.373(18) ?
C16 H16 . 0.9500 ?
C16 C15 . 1.374(17) ?
C24A H24A . 0.9500 ?
C24A C25A . 1.378(17) ?
C14A H14A . 0.9500 ?
C14A C15A . 1.399(18) ?
C22 H22 . 0.9500 ?
C12A H12A . 0.9500 ?
C14 H14 . 0.9500 ?
C14 C15 . 1.396(17) ?
C15 H15 . 0.9500 ?
C15A H15A . 0.9500 ?
C15A C16A . 1.375(18) ?
C16A H16A . 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
N2 H2 O1 . 0.88 1.85 2.590(13) 140.6 yes
N2A H2A O1A . 0.88 1.84 2.595(14) 142.4 yes
N1A H1A S1 1_665 0.88 3.07 3.825(9) 145.2 yes
N1 H1 S1A 1_445 0.88 3.09 3.888(10) 151.4 yes
_cod_database_fobs_code 2022290