#------------------------------------------------------------------------------
#$Date: 2021-02-05 16:53:19 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261799 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/22/2022289.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_2022289
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 11
_journal_page_last 19
_journal_paper_doi 10.1107/S2053229620015594
_journal_volume 77
_journal_year 2021
_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 335.23
_chemical_name_common 1-Benzoyl-3-o-bromophenylthiourea
_chemical_name_systematic
;
1-Benzoyl-3-(2-bromophenyl)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 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 90
_cell_angle_beta 95.183(8)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 3.9592(4)
_cell_length_b 15.142(2)
_cell_length_c 22.250(2)
_cell_measurement_reflns_used 7760
_cell_measurement_temperature 120
_cell_measurement_theta_max 29.66
_cell_measurement_theta_min 2.69
_cell_volume 1328.4(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 120
_diffrn_detector 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_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 0.0569
_diffrn_reflns_av_unetI/netI 0.0541
_diffrn_reflns_limit_h_max 4
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_number 7908
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.996
_diffrn_reflns_theta_min 2.690
_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 3.243
_exptl_absorpt_correction_T_max 0.8920
_exptl_absorpt_correction_T_min 0.3786
_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 1.676
_exptl_crystal_description needle
_exptl_crystal_F_000 672
_exptl_crystal_size_max 0.76
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.034
_refine_diff_density_max 1.061
_refine_diff_density_min -1.475
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.069
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 172
_refine_ls_number_reflns 3530
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.069
_refine_ls_R_factor_all 0.0626
_refine_ls_R_factor_gt 0.0492
_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^)+(0.0967P)^2^+0.6126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1270
_refine_ls_wR_factor_ref 0.1450
_reflns_number_gt 2917
_reflns_number_total 3566
_reflns_threshold_expression I>=2u(I)
_cod_data_source_file wp3011sup1.cif
_cod_data_source_block 4
_cod_depositor_comments
'Adding full bibliography for 2022286--2022290.cif.'
_cod_database_code 2022289
_cod_database_fobs_code 2022289
_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 0.192
_shelx_estimated_absorpt_t_max 0.898
_shelx_hkl_file
;
-4 4 -2 170.54 15.24
-4 4 -1 54.76 15.48
-4 4 0 120.28 16.29
-4 4 6 25.58 18.62
-4 4 7 2.98 18.62
-4 5 -6 9.85 17.35
-4 5 12 9.67 25.95
-4 6 -9 7.61 11.92
-4 7 -12 -1.53 18.02
-3 2 -3 147.17 19.29
-3 3 -8 182.41 20.36
-3 3 13 25.71 22.13
-3 4 -11 114.56 13.57
-3 5 -14 38.16 16.79
-3 7 -17 2.57 11.54
-3 8 -19 49.85 15.76
-2 1 -6 1090.58 22.80
-2 2 -10 336.03 17.64
-2 3 -13 64.13 18.06
-2 7 24 9.68 42.34
-1 0 -3 652.73 30.48
-1 1 -9 1370.21 28.80
-1 3 -15 19.94 16.35
-1 5 -19 54.71 19.71
-1 7 -22 24.16 20.77
-1 9 27 24.04 28.60
0 2 14 46.22 19.86
0 4 19 5.99 20.07
0 8 25 347.73 28.41
0 9 26 9.56 27.37
1 1 4 3097.57 43.49
1 2 10 60.12 18.92
1 4 16 173.79 18.57
1 6 20 508.86 24.99
1 8 23 -0.22 20.55
1 9 24 59.09 27.86
3 6 6 366.58 20.99
3 10 16 20.91 17.75
4 10 -3 6.89 23.95
4 10 -2 -2.24 21.97
4 10 -1 8.79 22.23
4 10 0 267.67 24.49
4 10 2 141.45 21.18
4 10 3 39.78 17.62
4 11 -8 316.37 26.06
4 11 6 -0.72 21.38
4 12 -11 10.75 22.61
-5 7 1 -3.27 19.01
-5 7 4 5.87 20.97
-5 7 5 0.28 21.68
-4 4 -3 18.02 15.63
-4 5 -8 -24.78 17.67
-4 5 -7 15.06 11.80
-3 2 -5 25.02 19.79
-3 2 -4 462.70 17.76
-3 2 9 61.02 19.40
-3 3 -9 162.77 23.50
-3 4 -12 483.49 21.50
-3 6 -16 17.63 12.54
-2 1 10 16.16 24.64
-2 2 14 14.28 34.24
-2 4 -16 1067.54 23.93
-2 5 -18 21.06 18.81
-2 8 -22 7.86 19.21
-1 2 -13 84.55 18.49
0 1 -9 284.86 29.13
0 1 10 590.66 27.42
0 6 22 363.14 23.65
1 1 2 775.70 31.03
1 1 3 2295.32 40.67
1 3 13 351.96 21.96
1 5 18 43.32 15.86
1 7 21 13.41 22.73
2 3 4 44.09 18.16
2 6 15 117.27 18.48
2 7 17 1.74 13.67
2 11 22 119.88 28.37
3 6 4 40.66 18.45
3 6 5 195.37 14.88
3 7 9 21.07 14.32
3 8 11 5.44 20.55
3 9 -15 0.04 26.00
3 9 13 4.39 21.77
3 11 16 -5.26 26.91
4 11 -7 3.30 24.67
4 11 3 -5.71 24.88
4 12 7 46.21 23.57
-4 4 -5 205.94 18.38
-4 4 -4 32.20 16.04
-4 5 -9 16.10 16.49
-3 2 -6 280.68 20.45
-3 3 -10 73.99 20.36
-3 4 -13 522.69 21.32
-3 5 -15 12.29 17.11
-3 6 -17 83.68 16.93
-3 8 -20 23.66 18.36
-2 1 -7 135.71 12.16
-2 2 -11 428.46 14.29
-2 3 -14 36.85 16.89
-1 0 -4 0.87 15.71
-1 0 6 -2.24 29.50
-1 1 -10 1139.03 26.66
-1 3 -16 26.41 16.47
-1 4 -18 47.75 17.57
-1 5 -20 6.12 17.61
-1 8 -24 256.23 24.06
0 2 -13 181.63 22.94
0 3 16 121.34 20.39
0 4 -18 306.10 24.97
0 5 20 28.56 20.93
0 8 -24 126.66 23.17
0 9 -25 33.42 24.06
0 10 -26 200.17 26.89
1 1 0 3597.75 53.88
1 1 1 3464.66 53.42
1 2 9 41.49 19.73
1 4 15 171.88 19.67
1 5 -18 10.30 23.81
1 6 19 620.83 25.17
1 8 22 293.22 24.39
1 9 23 31.59 25.40
2 3 2 86.19 19.18
2 3 3 154.96 18.73
2 4 -10 845.68 32.55
2 5 12 -0.60 13.10
2 6 14 105.54 19.92
2 7 16 87.40 19.91
2 8 18 15.21 15.59
3 6 -5 113.45 20.33
3 6 1 24.44 18.31
3 6 2 225.38 19.47
3 6 3 -13.02 13.75
3 7 -10 2.64 20.03
3 7 7 80.82 21.19
3 7 8 4.33 14.73
3 10 14 6.60 23.64
4 11 -3 16.29 24.68
4 11 -2 109.43 24.83
4 11 -1 5.40 23.10
4 12 -9 -10.81 24.87
4 12 4 37.00 25.32
4 12 5 -0.68 26.04
-4 3 0 -3.48 17.85
-4 3 1 810.09 23.06
-4 4 -6 93.90 17.23
-4 5 -10 113.33 17.36
-4 5 14 -1.96 30.02
-4 6 -12 102.83 13.85
-4 7 -14 70.13 14.66
-3 2 -7 22.45 19.47
-3 2 10 166.73 22.33
-3 3 -11 30.09 19.67
-3 5 -16 -3.97 15.96
-3 7 -19 -11.65 17.80
-2 0 0 725.46 23.46
-2 0 1 -13.32 17.97
-2 0 2 550.34 22.27
-2 1 -8 224.27 12.50
-2 2 -12 167.54 15.99
-2 3 -15 -2.11 16.03
-2 4 -17 106.21 17.51
-2 5 -19 9.87 19.34
-2 8 -23 229.80 23.41
-1 0 -5 918.27 28.48
-1 3 17 5.49 24.35
-1 5 21 59.06 24.23
-1 7 -23 27.78 22.23
-1 7 24 3.51 25.29
-1 8 25 47.79 29.44
0 2 13 184.12 21.19
0 3 -16 94.34 25.58
0 4 18 328.79 23.85
0 5 -20 25.12 18.88
0 7 -23 -5.07 21.18
0 8 24 156.42 25.11
1 2 8 939.57 27.59
1 3 12 800.59 24.16
1 4 -16 221.87 30.65
1 5 17 75.16 13.47
1 6 -20 1.70 29.02
1 9 -24 222.07 32.53
1 10 -25 50.11 33.01
2 3 -3 991.83 27.99
2 3 -1 1925.95 33.33
2 3 0 468.22 22.80
2 3 1 1355.11 28.00
2 5 -13 12.43 25.58
2 8 17 666.61 23.26
3 6 -3 6.56 12.44
3 6 -2 183.59 17.58
3 6 -1 63.26 16.77
3 7 6 523.08 21.98
3 8 -12 277.55 27.87
3 8 9 31.81 20.34
3 9 11 0.57 21.64
3 11 15 114.22 19.09
3 12 16 186.29 24.58
4 12 -7 44.23 26.73
4 13 5 109.22 28.21
-5 6 -2 17.81 17.99
-5 6 0 26.59 18.82
-5 6 3 14.54 15.04
-5 6 4 2.88 20.95
-4 3 -3 86.26 15.70
-4 3 -2 14.86 17.02
-4 3 -1 233.84 14.72
-4 4 -8 73.62 17.53
-4 4 -7 195.49 13.92
-4 5 -11 14.07 16.93
-4 6 -13 44.33 13.75
-4 6 17 19.30 36.49
-3 1 -2 381.61 18.33
-3 1 1 391.52 14.56
-3 1 3 564.22 18.97
-3 2 -8 609.87 22.89
-3 3 -12 296.55 19.84
-3 4 -14 457.31 17.97
-3 6 -18 3.09 13.04
-3 7 -20 209.43 16.94
-2 0 -2 45.19 17.52
-2 0 -1 -6.14 12.26
-2 0 3 -2.88 15.75
-2 0 4 18.65 16.96
-2 1 -9 612.67 18.78
-2 6 -21 18.50 21.51
-1 0 -6 -10.97 20.31
-1 1 -11 893.29 24.24
-1 2 -14 152.12 14.03
-1 4 -19 222.08 18.14
-1 4 19 49.14 21.64
-1 6 -22 130.44 20.37
-1 9 26 7.20 27.50
0 6 -22 346.46 25.75
0 6 21 171.27 20.64
1 4 14 215.66 19.81
1 8 -23 21.01 27.81
1 11 24 15.30 26.52
2 7 15 32.98 18.04
2 9 18 12.44 21.86
2 11 20 31.39 25.22
3 7 4 621.63 21.76
3 9 -14 22.67 23.46
3 9 10 -8.60 20.49
4 12 1 42.78 18.54
4 13 -9 126.59 25.21
4 13 4 23.86 23.23
-5 6 7 5.12 19.97
-5 6 8 10.83 20.31
-4 3 -5 118.61 17.31
-4 3 -4 56.22 17.93
-4 3 8 54.83 25.58
-4 4 -9 19.64 17.57
-4 4 12 192.28 27.02
-4 7 19 31.42 38.96
-3 1 -4 17.29 15.44
-3 1 -3 477.62 18.58
-3 1 6 36.98 13.54
-3 2 -9 271.13 21.87
-3 4 -15 121.24 20.10
-3 6 -19 58.25 17.88
-2 0 -4 525.65 19.57
-2 0 -3 -5.26 11.27
-2 0 5 0.71 16.35
-2 1 -10 136.59 15.41
-2 2 -13 324.63 14.19
-2 3 -16 10.57 16.54
-2 4 -18 276.02 19.71
-2 5 -20 16.05 18.67
-2 7 -23 262.96 20.78
-2 8 -24 16.45 22.69
-1 1 11 1181.13 57.20
-1 3 -17 -0.86 16.81
-1 5 -21 9.14 19.63
-1 7 -24 16.12 18.76
-1 8 -25 7.75 22.38
-1 9 -26 29.48 25.85
0 1 -10 586.30 26.36
0 3 15 1328.87 30.18
0 5 19 11.07 23.49
0 7 22 9.19 21.77
1 2 7 143.47 20.91
1 3 11 -2.24 18.49
1 5 16 5.19 16.31
1 9 22 17.67 16.90
1 10 23 112.16 19.39
2 4 -9 334.00 25.58
2 6 12 288.47 18.40
3 7 2 260.13 19.81
3 7 3 137.78 18.82
3 8 -11 70.91 21.15
3 11 -17 70.09 28.00
3 12 14 71.31 24.91
4 13 -7 332.89 26.35
4 13 -6 38.53 25.78
4 13 -4 19.54 27.44
4 13 0 11.31 23.75
4 13 1 101.01 27.24
-5 5 1 34.43 16.93
-5 5 3 39.65 17.31
-5 6 9 12.83 20.28
-4 3 -6 -11.10 18.47
-4 3 9 194.63 27.13
-4 4 -10 84.51 17.25
-4 6 -15 -0.26 18.32
-3 1 -5 349.63 17.89
-3 2 -10 453.73 21.87
-3 3 -13 89.32 14.87
-3 4 -16 24.02 18.04
-3 5 -18 0.59 16.69
-2 0 -5 6.95 15.64
-2 1 11 36.92 24.60
-2 2 -14 170.21 16.44
-2 6 22 29.51 29.51
-1 0 -7 20.22 14.33
-1 1 -12 76.17 17.23
-1 2 -15 20.62 16.45
-1 6 -23 271.40 20.87
-1 6 22 116.20 22.32
0 2 -14 47.02 17.82
0 2 12 187.18 19.72
0 4 -19 14.81 19.48
0 4 17 -0.46 18.87
0 8 -25 429.18 24.80
0 8 23 390.07 25.03
0 9 24 11.02 23.42
0 10 25 12.47 27.67
1 4 13 240.28 20.53
2 9 17 2.69 16.20
2 12 20 28.74 24.87
3 7 -6 371.78 20.35
3 7 -4 117.43 19.44
3 7 -2 436.28 20.30
3 7 -1 389.66 20.06
3 7 0 1022.78 23.34
3 7 1 244.78 19.17
3 8 -10 459.77 25.29
3 8 5 99.48 18.39
3 9 -13 28.01 24.93
3 10 10 24.06 21.46
3 11 12 -4.12 22.50
4 13 -3 210.77 20.67
4 13 -2 2.45 18.55
-5 5 -2 15.82 19.12
-5 5 -1 6.45 14.45
-5 5 6 1.58 17.12
-4 2 0 21.84 20.59
-4 3 -8 15.92 18.28
-4 3 -7 1.90 13.66
-4 4 -11 54.37 17.45
-4 4 13 36.02 23.97
-4 5 -14 25.47 17.41
-4 6 -16 24.96 18.47
-3 1 -7 106.39 16.41
-3 1 -6 16.73 11.51
-3 2 -11 206.83 19.73
-3 2 12 1336.12 36.78
-3 3 -14 82.73 20.27
-3 6 -20 77.64 19.39
-2 0 -6 19.32 11.27
-2 0 6 761.04 26.40
-2 1 -11 129.09 11.64
-2 3 -17 -4.11 16.03
-2 4 -19 325.86 19.30
-2 5 -21 32.31 18.97
-2 7 -24 5.71 20.23
-1 0 -8 -13.99 18.28
-1 2 14 76.82 24.38
-1 3 -18 -5.27 16.24
-1 4 -20 525.73 21.24
-1 7 23 21.97 24.49
-1 10 26 -6.48 30.71
0 1 8 2175.97 45.64
0 3 -17 109.04 19.26
0 5 -21 10.69 18.24
0 6 20 189.70 20.04
0 7 -24 12.95 20.40
1 2 6 4.16 12.56
1 3 10 291.09 18.53
1 5 15 575.65 21.35
1 6 17 419.30 17.46
1 7 -22 274.41 30.37
1 10 22 -10.82 19.90
1 11 23 18.48 19.35
2 4 -8 1041.82 29.26
2 4 3 6.78 16.84
2 4 4 38.08 12.08
2 7 13 83.78 16.98
2 8 -19 3.80 33.52
2 9 16 11.08 20.64
3 10 9 215.68 21.44
3 11 11 8.13 21.84
4 14 -3 7.13 23.31
-5 5 -6 11.93 16.88
-5 5 -5 2.96 18.81
-5 5 -4 3.05 13.62
-4 2 -3 314.77 21.48
-4 3 -9 -13.12 18.56
-4 3 10 96.91 23.71
-4 5 16 7.47 28.88
-4 6 18 109.86 38.81
-3 1 -8 365.61 18.36
-3 2 -12 311.53 19.69
-3 3 -15 26.13 20.65
-3 4 -17 148.61 14.65
-2 0 -7 0.70 10.45
-2 1 -12 482.27 17.55
-2 2 -15 208.58 13.28
-2 6 -23 9.45 20.87
-1 2 -16 1456.37 24.65
-1 5 -22 6.92 18.91
-1 5 20 180.61 22.81
-1 7 -25 39.32 20.93
-1 8 -26 56.26 23.53
-1 8 24 343.48 25.91
-1 9 25 13.34 24.29
0 0 -3 -1.67 26.86
0 1 -11 1068.24 30.74
0 3 14 251.52 22.89
0 5 18 451.01 25.95
0 6 -23 12.18 24.35
1 2 5 124.38 19.40
1 4 12 7.72 17.49
1 12 23 137.36 27.17
2 4 2 127.32 18.00
2 5 -12 805.37 31.33
2 7 12 172.92 19.87
2 10 17 60.13 16.30
2 12 19 73.95 18.02
3 9 -12 7.97 19.93
3 10 8 -12.06 19.91
3 11 -16 77.50 27.57
-5 4 2 4.45 15.82
-5 5 9 80.04 30.13
-4 2 -6 45.57 20.15
-4 3 -10 19.08 18.21
-4 4 -13 144.18 14.40
-4 4 14 70.19 27.21
-4 5 -16 222.12 17.40
-3 0 -1 36.15 13.49
-3 0 0 6.49 13.19
-3 0 1 84.33 14.44
-3 1 -9 94.00 17.27
-3 2 -13 -5.76 19.39
-3 3 -16 72.72 17.26
-3 4 -18 44.08 19.48
-3 5 -20 -8.06 18.68
-2 0 -8 722.33 16.27
-2 0 7 3.42 16.41
-2 1 -13 113.18 15.16
-2 2 -16 177.31 17.07
-2 3 -18 17.43 12.63
-2 4 -20 80.77 13.66
-2 5 -22 6.55 19.88
-2 7 23 92.77 30.21
-1 0 -9 566.81 18.50
-1 3 -19 84.24 17.58
-1 4 -21 136.11 18.41
-1 4 18 10.03 21.99
-1 6 -24 55.39 21.45
0 0 -4 3393.87 70.94
0 2 -15 41.99 17.86
0 4 16 50.76 19.05
0 8 22 19.61 21.01
0 9 23 107.48 23.26
0 10 24 52.41 23.62
1 3 9 90.59 13.78
1 5 14 61.56 17.23
1 6 16 85.82 12.91
1 10 21 504.64 26.05
2 4 0 37.10 17.53
2 4 1 4.74 16.58
2 12 18 121.72 21.89
3 8 -7 -4.07 18.43
3 8 -6 684.14 23.61
3 8 -1 5.02 17.71
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4 -6 -13 72.19 5.13
4 -5 -16 1.87 5.37
4 -5 -15 36.19 4.86
4 -4 -19 56.79 5.99
-5 -6 -5 168.33 5.11
-4 -10 4 1.67 5.18
-4 -7 2 341.76 6.72
-4 -6 1 123.77 5.36
-4 -5 0 466.31 6.93
-4 -2 -4 122.49 4.34
-4 0 -9 -5.06 4.72
-4 1 -13 9.79 4.60
-4 1 -12 35.11 3.47
-3 0 -3 8.66 4.14
-3 3 -11 44.26 3.96
-3 4 -22 8.06 3.21
-3 4 -20 48.04 3.90
-3 4 -19 17.42 3.86
-3 4 -18 53.93 3.31
-3 4 -17 141.51 3.81
-2 1 -2 210.23 5.51
-2 2 -4 312.98 5.41
-2 4 -10 709.55 6.35
-2 5 -26 82.29 4.90
-2 5 -25 58.64 4.93
-2 5 -15 55.74 4.21
-1 1 -1 3426.06 18.57
-1 3 -5 2.54 3.23
-1 4 -8 280.10 5.76
-1 6 -23 260.94 5.28
-1 6 -21 289.47 5.46
-1 6 -20 544.47 6.40
1 -16 8 23.28 4.82
1 -8 6 140.94 4.85
2 -16 5 38.44 5.06
2 -15 5 63.86 5.13
2 -10 4 565.60 6.50
2 -8 3 529.19 6.30
3 -12 0 33.56 3.91
3 -11 0 15.72 4.69
3 -8 -2 55.18 3.49
3 -4 -6 79.02 4.70
4 -13 -6 27.76 5.07
4 -12 -7 48.02 4.39
4 -11 -7 3.71 5.41
4 -10 -8 39.41 4.96
4 -9 -9 60.74 4.02
4 -8 -10 2.26 3.51
4 -7 -11 121.65 5.78
4 -6 -12 486.37 6.85
4 -5 -14 6.70 4.88
4 -4 -18 326.96 6.92
-4 1 -14 196.85 4.41
-2 5 -16 32.57 2.85
-1 2 -3 1831.97 12.82
1 -4 3 639.87 7.50
2 -18 5 51.63 4.27
3 -17 1 45.87 4.24
3 -16 1 45.48 4.47
3 -15 1 618.27 6.75
3 -14 1 9.62 4.05
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 8728
_shelx_res_file
;
TITL g72_a.res in P2(1)/n
g72.res
created by SHELXL-2018/1 at 12:26:47 on 09-Jul-2020
REM Old TITL G72 LIGAND
REM SHELXT solution in P2(1)/n
REM R1 0.077, Rweak 0.005, Alpha 0.028, Orientation as input
REM Formula found by SHELXT: C14 Br N2 O S
CELL 0.71073 3.9592 15.1421 22.2497 90 95.183 90
ZERR 4 0.0004 0.0021 0.0022 0 0.008 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Br N O S
UNIT 56 44 4 8 4 4
EQIV $1 1-X,1-Y,1-Z
L.S. 20
PLAN 5
SIZE 0.034 0.05 0.76
TEMP -153.15
HTAB N2 O1
HTAB N1 S1_$1
BOND $H
list 4
MORE -1
fmap 2
acta
MERG 2
OMIT -2 58
OMIT -5 3 2
OMIT 1 17 14
REM
REM
REM
WGHT 0.096700 0.612600
FVAR 0.43008
BR1 3 0.833620 0.344330 0.770916 11.00000 0.02142 0.01716 =
0.01984 0.00192 0.00254 0.00371
S1 6 0.625920 0.549608 0.586435 11.00000 0.02045 0.01486 =
0.01472 0.00159 0.00201 -0.00404
O1 5 0.270650 0.274190 0.628561 11.00000 0.05525 0.01629 =
0.01788 0.00271 0.00431 -0.00787
N1 4 0.356236 0.391298 0.566528 11.00000 0.02256 0.01298 =
0.01293 0.00087 0.00181 -0.00177
AFIX 43
H1 2 0.353938 0.406926 0.528399 11.00000 -1.20000
AFIX 0
N2 4 0.407961 0.435706 0.666601 11.00000 0.02440 0.01391 =
0.01368 0.00136 0.00297 -0.00346
AFIX 43
H2 2 0.329777 0.382603 0.673484 11.00000 -1.20000
AFIX 0
C26 1 0.661584 0.461422 0.768824 11.00000 0.01362 0.01629 =
0.01879 0.00224 0.00211 -0.00091
C21 1 0.474750 0.492245 0.717078 11.00000 0.01627 0.01590 =
0.01470 0.00267 0.00503 -0.00127
C23 1 0.393370 0.630141 0.768534 11.00000 0.02034 0.01408 =
0.02320 -0.00031 0.00723 -0.00318
AFIX 43
H23 2 0.297239 0.687607 0.768823 11.00000 -1.20000
AFIX 0
C25 1 0.722968 0.514556 0.819928 11.00000 0.01850 0.02288 =
0.01513 -0.00228 -0.00055 -0.00170
AFIX 43
H25 2 0.853494 0.492943 0.854762 11.00000 -1.20000
AFIX 0
C22 1 0.335187 0.577361 0.717319 11.00000 0.01868 0.01575 =
0.01831 0.00067 0.00340 -0.00278
AFIX 43
H22 2 0.201802 0.598914 0.682784 11.00000 -1.20000
AFIX 0
C1 1 0.453635 0.456184 0.609403 11.00000 0.01408 0.01416 =
0.01358 -0.00054 -0.00016 0.00035
C11 1 0.154574 0.251673 0.522899 11.00000 0.02007 0.01344 =
0.01517 0.00067 0.00470 -0.00392
C14 1 -0.050994 0.146569 0.424032 11.00000 0.02315 0.02329 =
0.02040 -0.00737 0.00529 -0.00731
AFIX 43
H14 2 -0.119601 0.110393 0.390232 11.00000 -1.20000
AFIX 0
C24 1 0.589801 0.599791 0.819047 11.00000 0.02255 0.01867 =
0.01974 -0.00481 0.00572 -0.00287
AFIX 43
H24 2 0.633754 0.637177 0.853146 11.00000 -1.20000
AFIX 0
C16 1 -0.031302 0.288566 0.472801 11.00000 0.01565 0.01704 =
0.01884 -0.00066 0.00240 -0.00235
AFIX 43
H16 2 -0.084947 0.349728 0.472294 11.00000 -1.20000
AFIX 0
C12 1 0.234441 0.161781 0.524232 11.00000 0.02200 0.01549 =
0.01965 0.00097 0.00011 0.00031
AFIX 43
H12 2 0.353727 0.136073 0.558862 11.00000 -1.20000
AFIX 0
C10 1 0.263319 0.305340 0.577665 11.00000 0.02511 0.01331 =
0.01729 0.00191 0.00231 -0.00188
C13 1 0.134961 0.110608 0.473520 11.00000 0.02618 0.01583 =
0.02685 -0.00289 0.00578 -0.00195
AFIX 43
H13 2 0.196328 0.049976 0.473065 11.00000 -1.20000
AFIX 0
C15 1 -0.138267 0.235427 0.423433 11.00000 0.02069 0.02293 =
0.01640 -0.00060 0.00032 -0.00302
AFIX 43
H15 2 -0.269855 0.259882 0.389659 11.00000 -1.20000
AFIX 0
HKLF 4
REM g72_a.res in P2(1)/n
REM R1 = 0.0492 for 2917 Fo > 4sig(Fo) and 0.0626 for all 3530 data
REM 172 parameters refined using 0 restraints
END
WGHT 0.0967 0.6126
REM Highest difference peak 1.061, deepest hole -1.475, 1-sigma level 0.177
Q1 1 0.5502 0.3225 0.7595 11.00000 0.05 1.06
Q2 1 0.5843 0.3805 0.7492 11.00000 0.05 0.99
Q3 1 1.1395 0.3395 0.7808 11.00000 0.05 0.97
Q4 1 1.0604 0.3839 0.7981 11.00000 0.05 0.97
Q5 1 0.9585 0.2983 0.7379 11.00000 0.05 0.87
;
_shelx_res_checksum 56368
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 0.83362(8) 0.34433(2) 0.77092(2) 0.01943(14) Uani d 1 . .
S S1 0.6259(2) 0.54961(5) 0.58644(4) 0.01665(18) Uani d 1 . .
O O1 0.2706(9) 0.27419(16) 0.62856(12) 0.0297(6) Uani d 1 . .
N N1 0.3562(7) 0.39130(16) 0.56653(12) 0.0161(5) Uani d 1 . .
H H1 0.353938 0.406926 0.528399 0.019 Uiso calc 1 . .
N N2 0.4080(8) 0.43571(16) 0.66660(13) 0.0173(5) Uani d 1 . .
H H2 0.329777 0.382603 0.673484 0.021 Uiso calc 1 . .
C C26 0.6616(8) 0.46142(19) 0.76882(15) 0.0162(6) Uani d 1 . .
C C21 0.4747(8) 0.49224(19) 0.71708(14) 0.0154(6) Uani d 1 . .
C C23 0.3934(9) 0.6301(2) 0.76853(16) 0.0189(6) Uani d 1 . .
H H23 0.297239 0.687607 0.768823 0.023 Uiso calc 1 . .
C C25 0.7230(8) 0.5146(2) 0.81993(15) 0.0190(6) Uani d 1 . .
H H25 0.853494 0.492943 0.854762 0.023 Uiso calc 1 . .
C C22 0.3352(8) 0.5774(2) 0.71732(15) 0.0175(6) Uani d 1 . .
H H22 0.201802 0.598914 0.682784 0.021 Uiso calc 1 . .
C C1 0.4536(8) 0.45618(19) 0.60940(14) 0.0140(5) Uani d 1 . .
C C11 0.1546(8) 0.25167(18) 0.52290(14) 0.0160(6) Uani d 1 . .
C C14 -0.0510(9) 0.1466(2) 0.42403(17) 0.0221(7) Uani d 1 . .
H H14 -0.119601 0.110393 0.390232 0.026 Uiso calc 1 . .
C C24 0.5898(9) 0.5998(2) 0.81905(16) 0.0201(6) Uani d 1 . .
H H24 0.633754 0.637177 0.853146 0.024 Uiso calc 1 . .
C C16 -0.0313(8) 0.2886(2) 0.47280(15) 0.0171(6) Uani d 1 . .
H H16 -0.084947 0.349728 0.472294 0.021 Uiso calc 1 . .
C C12 0.2344(9) 0.16178(19) 0.52423(16) 0.0192(6) Uani d 1 . .
H H12 0.353727 0.136073 0.558862 0.023 Uiso calc 1 . .
C C10 0.2633(9) 0.30534(19) 0.57767(15) 0.0185(6) Uani d 1 . .
C C13 0.1350(9) 0.1106(2) 0.47352(17) 0.0227(7) Uani d 1 . .
H H13 0.196328 0.049976 0.473065 0.027 Uiso calc 1 . .
C C15 -0.1383(9) 0.2354(2) 0.42343(15) 0.0201(6) Uani d 1 . .
H H15 -0.269855 0.259882 0.389659 0.024 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 0.0214(2) 0.01716(18) 0.0198(2) 0.00371(10) 0.00254(13) 0.00192(10)
S1 0.0205(4) 0.0149(3) 0.0147(4) -0.0040(2) 0.0020(3) 0.0016(2)
O1 0.0553(19) 0.0163(11) 0.0179(12) -0.0079(11) 0.0043(12) 0.0027(9)
N1 0.0226(13) 0.0130(10) 0.0129(12) -0.0018(9) 0.0018(10) 0.0009(9)
N2 0.0244(13) 0.0139(10) 0.0137(12) -0.0035(9) 0.0030(11) 0.0014(9)
C26 0.0136(12) 0.0163(12) 0.0188(15) -0.0009(10) 0.0021(12) 0.0022(11)
C21 0.0163(13) 0.0159(12) 0.0147(14) -0.0013(10) 0.0050(11) 0.0027(10)
C23 0.0203(14) 0.0141(13) 0.0232(16) -0.0032(11) 0.0072(13) -0.0003(11)
C25 0.0185(14) 0.0229(14) 0.0151(14) -0.0017(11) -0.0005(12) -0.0023(11)
C22 0.0187(14) 0.0157(12) 0.0183(14) -0.0028(10) 0.0034(12) 0.0007(11)
C1 0.0141(12) 0.0142(12) 0.0136(13) 0.0004(9) -0.0002(11) -0.0005(10)
C11 0.0201(13) 0.0134(12) 0.0152(14) -0.0039(10) 0.0047(12) 0.0007(10)
C14 0.0232(16) 0.0233(15) 0.0204(16) -0.0073(12) 0.0053(14) -0.0074(12)
C24 0.0225(15) 0.0187(13) 0.0197(15) -0.0029(11) 0.0057(13) -0.0048(11)
C16 0.0157(13) 0.0170(12) 0.0188(15) -0.0023(10) 0.0024(12) -0.0007(11)
C12 0.0220(15) 0.0155(13) 0.0197(16) 0.0003(10) 0.0001(13) 0.0010(11)
C10 0.0251(15) 0.0133(13) 0.0173(15) -0.0019(10) 0.0023(13) 0.0019(10)
C13 0.0262(16) 0.0158(13) 0.0268(17) -0.0019(12) 0.0058(14) -0.0029(12)
C15 0.0207(15) 0.0229(14) 0.0164(15) -0.0030(11) 0.0003(12) -0.0006(11)
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 N1 H1 . . 116.5 ?
C10 N1 H1 . . 116.5 ?
C10 N1 C1 . . 126.9(3) ?
C21 N2 H2 . . 117.2 ?
C1 N2 H2 . . 117.2 ?
C1 N2 C21 . . 125.6(3) ?
C21 C26 Br1 . . 119.8(2) ?
C21 C26 C25 . . 121.4(3) ?
C25 C26 Br1 . . 118.9(2) ?
C26 C21 N2 . . 120.0(3) ?
C26 C21 C22 . . 119.0(3) ?
C22 C21 N2 . . 120.8(3) ?
C22 C23 H23 . . 119.6 ?
C24 C23 H23 . . 119.6 ?
C24 C23 C22 . . 120.8(3) ?
C26 C25 H25 . . 120.5 ?
C24 C25 C26 . . 119.0(3) ?
C24 C25 H25 . . 120.5 ?
C21 C22 H22 . . 120.2 ?
C23 C22 C21 . . 119.6(3) ?
C23 C22 H22 . . 120.2 ?
N1 C1 S1 . . 118.8(2) ?
N2 C1 S1 . . 125.5(2) ?
N2 C1 N1 . . 115.7(3) ?
C16 C11 C12 . . 120.6(3) ?
C16 C11 C10 . . 121.7(3) ?
C12 C11 C10 . . 117.7(3) ?
C13 C14 H14 . . 119.9 ?
C13 C14 C15 . . 120.3(3) ?
C15 C14 H14 . . 119.9 ?
C23 C24 C25 . . 120.2(3) ?
C23 C24 H24 . . 119.9 ?
C25 C24 H24 . . 119.9 ?
C11 C16 H16 . . 120.1 ?
C11 C16 C15 . . 119.9(3) ?
C15 C16 H16 . . 120.1 ?
C11 C12 H12 . . 120.8 ?
C13 C12 C11 . . 118.5(3) ?
C13 C12 H12 . . 120.8 ?
O1 C10 N1 . . 123.0(3) ?
O1 C10 C11 . . 121.7(3) ?
N1 C10 C11 . . 115.3(3) ?
C14 C13 C12 . . 121.1(3) ?
C14 C13 H13 . . 119.4 ?
C12 C13 H13 . . 119.4 ?
C14 C15 C16 . . 119.6(3) ?
C14 C15 H15 . . 120.2 ?
C16 C15 H15 . . 120.2 ?
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 C26 . 1.898(3) ?
S1 C1 . 1.671(3) ?
O1 C10 . 1.225(4) ?
N1 H1 . 0.8800 ?
N1 C1 . 1.399(4) ?
N1 C10 . 1.381(4) ?
N2 H2 . 0.8800 ?
N2 C21 . 1.418(4) ?
N2 C1 . 1.338(4) ?
C26 C21 . 1.392(5) ?
C26 C25 . 1.396(4) ?
C21 C22 . 1.402(4) ?
C23 H23 . 0.9500 ?
C23 C22 . 1.394(5) ?
C23 C24 . 1.386(5) ?
C25 H25 . 0.9500 ?
C25 C24 . 1.394(5) ?
C22 H22 . 0.9500 ?
C11 C16 . 1.396(5) ?
C11 C12 . 1.397(4) ?
C11 C10 . 1.495(4) ?
C14 H14 . 0.9500 ?
C14 C13 . 1.380(6) ?
C14 C15 . 1.389(5) ?
C24 H24 . 0.9500 ?
C16 H16 . 0.9500 ?
C16 C15 . 1.396(5) ?
C12 H12 . 0.9500 ?
C12 C13 . 1.396(5) ?
C13 H13 . 0.9500 ?
C15 H15 . 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
N1 H1 S1 3_666 0.88 2.65 3.526(3) 177.4 yes
N2 H2 O1 . 0.88 1.93 2.629(4) 135.8 yes