#------------------------------------------------------------------------------
#$Date: 2024-10-01 05:27:30 +0300 (Tue, 01 Oct 2024) $
#$Revision: 294956 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/27/1572727.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_1572727
loop_
_publ_author_name
'Schwarzer, Anke'
'Stapf, Manuel'
_publ_section_title
;
2-Bromoacetamide
;
_journal_coeditor_code BH4089
_journal_issue 9
_journal_name_full IUCrData
_journal_paper_doi 10.1107/S2414314624008630
_journal_volume 9
_journal_year 2024
_chemical_formula_iupac 'C2 H4 Br N O'
_chemical_formula_moiety 'C2 H4 Br N O'
_chemical_formula_sum 'C2 H4 Br N O'
_chemical_formula_weight 137.97
_chemical_name_systematic
;
2-Bromoacetamide
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 99.94(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.373(4)
_cell_length_b 5.1899(14)
_cell_length_c 7.557(3)
_cell_measurement_reflns_used 1778
_cell_measurement_temperature 93(2)
_cell_measurement_theta_max 22.49
_cell_measurement_theta_min 1.74
_cell_volume 400.7(2)
_computing_cell_refinement
;
X-Area (Stoe & Cie, 2023)
;
_computing_data_collection
;
X-Area (Stoe & Cie, 2023)
;
_computing_data_reduction
;
X-Area (Stoe & Cie, 2023)
;
_computing_molecular_graphics
;
XP (Sheldrick, 2008)
;
_computing_publication_material
;
WinGX (Farrugia, 2012), publCIF (Westrip, 2010)
and
ShelXle (H\"ubschle et al., 2011)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 93(2)
_diffrn_detector 'Pilatus 300K'
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type 'Stoe Stadivari'
_diffrn_measurement_method 'rotation method, \w scans'
_diffrn_radiation_monochromator 'Graded multilayer mirror'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0358
_diffrn_reflns_av_unetI/netI 0.0299
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 4506
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.976
_diffrn_reflns_theta_min 1.993
_diffrn_source 'Primux 50 Mo'
_diffrn_source_current 0.830
_diffrn_source_power 0.050
_diffrn_source_voltage 60
_exptl_absorpt_coefficient_mu 10.060
_exptl_absorpt_correction_T_max 0.6679
_exptl_absorpt_correction_T_min 0.3296
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
[X-Red32 (Stoe & Cie, 2023; Koziskova et al., 2016]
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 2.287
_exptl_crystal_description plate
_exptl_crystal_F_000 264
_exptl_crystal_size_max 0.110
_exptl_crystal_size_mid 0.090
_exptl_crystal_size_min 0.040
_refine_diff_density_max 0.584
_refine_diff_density_min -0.506
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.044
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 52
_refine_ls_number_reflns 879
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.044
_refine_ls_R_factor_all 0.0362
_refine_ls_R_factor_gt 0.0275
_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^)+(0.0417P)^2^+0.0569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0654
_refine_ls_wR_factor_ref 0.0682
_reflns_number_gt 731
_reflns_number_total 879
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file bh4089.cif
_cod_data_source_block I
_cod_original_cell_volume 400.7(3)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1572727
_shelx_estimated_absorpt_t_min 0.404
_shelx_estimated_absorpt_t_max 0.689
_shelx_hkl_file
;
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5 1 3 122.56 7.21
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2 -3 5 231.51 17.99
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1 -3 4 33.96 8.87
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-3 -5 0 272.73 16.30
-3 3 2 -1.20 2.73
-2 -3 2 24.75 7.13
-2 2 2 27.70 2.20
-10 -1 8 127.65 16.71
-8 -2 7 90.95 15.71
-7 -3 6 19.64 12.90
-6 1 6 77.19 7.70
-5 -4 4 58.06 10.42
-4 -4 3 301.47 17.84
-4 -3 4 19.85 10.09
-3 -4 2 43.20 8.47
-3 -3 3 -2.53 7.83
-2 -1 3 82.30 6.64
-8 1 7 67.79 8.99
-7 -5 4 7.80 12.15
-6 -6 1 2.00 12.93
-5 -6 -1 34.67 12.46
-4 -5 1 37.55 12.32
-3 -1 4 435.58 13.52
-2 -4 0 24.68 8.06
-11 -1 8 179.28 19.18
-8 -1 7 77.97 13.63
-7 2 6 21.93 4.87
-6 -5 3 105.35 13.61
-6 -1 6 79.86 11.57
-5 -6 -2 189.82 16.86
0 -2 -6 67.83 4.39
-9 -2 7 264.86 21.04
-6 -6 0 32.23 14.12
-6 -3 5 98.99 14.86
-6 0 6 782.40 20.73
-5 -2 5 433.47 18.58
-3 -5 -2 400.72 16.82
-8 -4 5 24.15 14.43
-7 -2 6 36.25 12.95
-6 -4 4 70.37 11.73
-4 -5 0 37.33 11.07
-3 -5 -3 174.07 12.52
-3 -4 1 686.02 21.68
-7 -5 3 20.64 10.65
-6 -6 -1 6.05 12.12
-5 -4 3 8.73 8.60
-5 -3 4 17.98 10.64
-4 -4 2 186.91 14.85
-2 -4 -1 226.96 11.71
-2 -3 1 1561.67 26.14
1 0 -4 333.78 9.64
-10 -2 7 200.67 19.96
-9 -1 7 -3.13 11.11
-7 -6 0 -1.58 14.70
-5 -5 1 169.38 14.30
-2 -2 2 24.35 4.64
-7 -4 4 77.17 15.02
-7 -3 5 245.21 18.53
-7 -1 6 553.59 21.72
-5 1 5 194.81 8.64
-3 -3 2 2.73 5.64
-8 -2 6 19.32 10.10
-7 -6 -1 22.89 14.15
-2 -4 -2 209.45 10.67
-10 -1 7 25.78 10.08
-7 0 6 269.70 14.83
-7 1 6 516.99 15.70
-6 -5 1 541.65 24.89
-6 -4 3 281.38 17.26
-5 -5 0 53.71 12.96
-4 -5 -2 181.06 13.18
-4 -1 4 1300.03 24.07
1 -1 -5 28.85 4.13
1 -1 -4 689.80 9.83
-8 -4 4 1.71 9.89
-8 -3 5 742.06 28.78
-7 -6 -2 18.18 13.06
-6 -3 4 0.03 7.48
-5 -4 2 42.61 9.50
-4 -4 1 1209.17 28.84
-11 -1 7 22.77 14.47
-9 -2 6 263.75 18.17
-8 -5 2 4.98 14.90
-8 -1 6 532.26 22.47
-5 -2 4 6.17 8.23
-1 -1 1 238.50 6.82
1 1 -2 2580.06 24.53
-9 -4 4 -4.47 14.05
-9 -3 5 336.57 22.24
-7 -5 1 114.54 16.44
-7 -4 3 693.72 27.81
-7 -2 5 359.15 19.39
-6 -1 5 5.46 8.78
-3 -1 3 9.77 3.64
-2 -4 -4 -0.73 5.10
-2 -3 0 43.68 5.39
-1 -2 0 109.74 6.09
1 -1 -6 20.76 4.27
-7 -3 4 -7.15 11.26
-6 -5 0 304.61 19.01
-4 -3 2 5.11 7.77
-4 -2 3 366.17 14.90
-3 -4 -1 8.23 7.38
-3 -3 1 289.23 12.92
-2 -1 2 1456.61 19.34
1 0 -2 81.41 3.70
-10 -3 5 164.11 20.19
-9 -1 6 225.05 17.32
-8 0 6 2.70 9.51
-6 -4 2 61.21 10.59
-5 -5 -2 51.99 10.59
-11 -2 6 46.46 12.71
-8 -5 1 9.87 13.74
-8 -4 3 329.73 20.16
-8 1 6 534.83 17.82
-6 2 5 723.37 13.07
-5 -4 1 394.34 17.80
-2 -2 1 75.80 5.74
-7 -5 0 240.18 18.33
-6 -5 -1 95.23 13.49
-6 -3 3 339.02 18.43
-5 -5 -3 63.13 11.12
-5 -1 4 984.16 22.26
-10 -1 6 3.97 12.95
-9 -4 3 52.49 12.77
-9 0 6 613.11 23.40
-7 -1 5 113.22 10.95
-6 1 5 -1.11 6.28
-3 -4 -2 24.24 7.34
-1 -3 -3 250.35 7.99
-9 -3 4 31.05 14.81
-6 -5 -2 27.94 11.47
-6 -4 1 32.73 11.35
-5 -3 2 17.59 9.00
-2 3 2 27.71 3.27
-1 3 1 2239.87 23.32
-9 1 6 213.23 14.43
-8 -4 2 58.87 14.40
-7 -5 -1 358.02 20.45
-7 -3 3 202.21 16.12
-5 -2 3 9.27 7.21
-4 -4 -1 499.73 18.28
-12 -1 6 245.68 22.45
-10 -3 4 -4.96 14.52
-10 0 6 485.37 22.48
-9 -5 0 2.07 15.45
-8 -1 5 154.95 15.09
-7 -2 4 141.95 12.40
-6 -5 -3 23.09 10.56
-4 -3 1 -1.58 5.43
-3 -4 -3 240.87 11.67
-3 -3 0 44.25 7.10
-11 -2 5 272.79 23.18
-9 -4 2 -0.53 13.96
-8 -5 -1 95.01 15.68
-7 -5 -2 165.27 16.17
1 1 -1 233.76 6.68
2 0 -4 3826.37 31.01
-11 0 6 402.14 22.42
-8 -3 3 236.46 18.53
-7 -4 1 183.74 14.66
-6 -3 2 36.81 11.13
-6 -1 4 289.55 14.60
-5 0 4 34.44 6.20
-4 -2 2 248.42 12.05
-2 0 2 347.22 7.65
-1 -3 -4 25.11 4.17
-12 0 6 19.70 13.87
-10 -4 2 -12.15 11.23
-10 1 6 -0.29 8.80
-9 -5 -1 10.16 11.32
-9 -1 5 119.85 15.34
-8 -5 -2 118.23 16.34
-8 -2 4 57.20 10.66
-7 -5 -3 64.85 13.27
-4 -4 -2 65.74 9.49
-1 -2 -1 1910.51 19.40
-13 0 6 231.19 21.76
-9 -3 3 824.70 30.58
-8 -4 1 627.61 26.19
-5 -4 -1 919.16 24.59
-3 -2 1 1260.92 21.80
-3 1 3 7.69 2.56
-11 1 6 139.66 15.44
-10 -1 5 7.21 13.25
-9 -2 4 3.82 11.74
-8 -5 -3 202.57 17.69
-7 -3 2 1.56 10.28
-5 -3 1 855.66 22.94
-3 3 3 3.53 1.97
-2 -3 -2 0.60 4.56
-2 -2 0 276.47 9.52
-11 -3 3 201.39 21.40
-11 -1 5 10.34 14.81
-10 -2 4 262.20 20.55
-4 -4 -3 -7.68 7.18
-4 -3 0 3.40 6.56
-1 -3 -5 1194.86 14.00
0 -1 -1 42.95 2.00
-12 -1 5 29.96 16.50
-10 -4 1 84.43 13.63
-7 -2 3 869.05 26.32
-6 -4 -1 392.62 19.26
-5 -4 -2 37.27 9.72
-5 1 4 986.29 17.19
-2 4 2 107.99 7.16
0 -2 -3 134.22 3.77
-11 -2 4 93.58 14.49
-8 -3 2 4.65 10.95
-6 -3 1 942.92 26.38
-6 0 4 1445.96 25.90
-5 -2 2 285.78 13.28
2 1 -2 1511.38 19.76
-8 1 5 164.29 12.08
-4 -4 -4 24.00 7.62
-9 -3 2 -0.94 8.86
-7 -4 -1 35.78 12.20
-1 -1 0 1177.42 12.93
-11 -3 2 -3.33 15.43
-10 -3 2 22.07 10.83
-7 -3 1 447.35 21.20
-5 -4 -3 228.49 13.98
2 -1 -5 2.67 3.13
-9 -2 3 87.27 12.55
-8 -4 -1 73.33 12.04
-8 2 5 35.67 7.24
-6 -2 2 9.10 6.83
-6 -1 3 281.91 13.76
-5 2 4 5.14 3.72
-5 3 4 20.74 2.68
0 3 1 245.99 8.85
1 2 0 115.16 6.06
-10 -4 -1 241.59 21.35
-10 -2 3 62.98 14.90
-9 -4 -1 455.09 24.10
-7 -4 -2 22.84 12.12
-5 -4 -4 22.40 8.87
-4 -1 2 293.90 11.44
-3 -3 -2 30.98 6.09
-12 -2 3 250.53 20.73
-12 -1 4 133.33 19.80
-11 -1 4 24.33 12.02
-10 1 5 -1.07 10.94
-6 -4 -3 682.09 23.51
-13 1 5 58.18 15.98
-12 1 5 42.42 15.68
-11 1 5 27.49 12.79
-9 -3 1 130.59 14.29
-9 2 5 105.67 11.97
-8 -4 -2 31.18 12.37
-7 -2 2 960.23 26.44
-6 1 4 296.37 11.68
-5 -4 -5 4.66 8.06
-10 -4 -2 39.11 16.17
-9 -4 -2 28.15 10.77
-8 0 4 530.56 20.36
-7 -4 -3 268.80 17.98
-7 -1 3 -0.75 7.05
-6 -4 -4 24.80 10.32
-5 -2 1 466.18 17.03
-3 4 3 952.97 12.94
-2 -3 -4 5.48 5.10
-8 -4 -3 40.81 13.50
-8 -2 2 126.86 12.61
-7 -3 0 39.66 9.41
-2 -2 -1 268.41 8.83
-1 3 2 42.72 4.46
3 0 -4 885.33 16.03
-11 2 5 254.74 17.95
-9 -4 -3 32.27 14.24
-9 -2 2 88.52 14.87
-9 0 4 14.51 10.89
-8 -3 0 13.15 12.68
-8 -1 3 114.47 13.46
-7 -4 -4 61.82 12.76
-3 0 2 6274.08 37.06
-13 0 4 46.57 17.49
-12 -2 2 55.24 17.38
-12 0 4 394.03 25.09
-10 -2 2 28.43 10.64
-10 0 4 583.35 25.29
-9 -4 -4 16.00 13.44
-9 -3 0 14.75 13.42
-8 -4 -4 18.49 12.54
-7 -4 -5 314.50 19.10
-4 -3 -2 49.77 8.53
-3 -3 -3 988.13 20.00
-1 4 2 23.07 5.86
2 -1 -4 77.94 3.82
-11 -3 0 16.56 11.62
-11 -1 3 21.92 16.06
-10 -3 0 -10.16 9.58
-10 -1 3 121.13 16.99
-7 1 4 41.38 7.98
-6 -2 1 13.09 7.07
-4 1 3 197.04 7.52
2 1 -1 1281.01 16.91
-4 -2 0 1410.35 24.72
-2 -3 -5 229.08 9.32
-8 1 4 646.61 21.07
-7 -2 1 292.29 16.79
-5 -3 -2 -2.43 7.86
3 1 -2 161.14 8.35
-1 5 0 176.40 14.57
0 1 6 307.12 17.58
0 3 7 30.77 17.26
0 6 -1 29.58 11.18
1 -1 3 1.68 2.07
1 0 6 69.50 9.43
1 2 -4 59.21 3.64
1 3 8 -5.95 17.96
-1 1 3 722.31 17.53
-1 2 5 776.64 25.13
3 2 9 11.94 18.61
-1 1 2 2557.70 28.00
-1 3 -1 179.55 8.29
-1 3 5 87.90 15.35
0 5 -2 154.68 10.46
5 -3 2 -3.91 4.29
-1 2 4 61.26 10.68
-1 5 2 570.14 24.80
0 4 6 72.21 20.38
0 6 0 689.76 26.95
0 6 3 3.78 16.73
1 4 -4 84.01 4.15
1 7 1 7.54 17.06
2 -1 5 10.02 4.80
2 2 8 12.70 16.02
4 -1 7 13.42 7.57
-1 3 4 -1.42 10.82
0 1 5 341.06 16.03
0 3 6 0.13 15.93
0 6 1 44.81 15.60
1 2 7 72.85 17.56
1 4 7 51.14 22.92
2 3 8 15.43 21.40
-1 4 3 71.66 14.21
3 -1 6 6.25 6.51
3 1 8 271.80 21.52
-1 2 0 126.99 6.75
-1 2 3 81.21 8.20
-1 4 2 29.18 11.38
-1 2 2 91.10 8.68
0 5 -1 1.35 8.49
1 1 6 898.98 26.70
2 1 -5 6.05 4.92
2 1 7 104.60 14.61
3 2 8 -4.47 17.51
3 3 8 9.42 20.92
-1 2 1 257.76 9.99
-1 3 2 46.09 7.37
0 2 5 80.01 11.17
0 3 5 831.27 29.28
1 4 6 4.84 13.13
1 5 -3 443.57 14.03
1 6 -1 10.34 10.71
1 6 3 -1.96 17.91
2 0 6 231.75 13.21
2 4 7 -0.73 16.57
2 7 0 273.58 24.02
2 7 1 1.09 17.57
0 0 2 696.77 10.84
0 1 4 1708.13 28.94
0 4 -2 110.74 7.81
0 5 1 7.25 11.94
1 3 6 24.61 16.76
2 2 7 15.24 15.91
4 1 8 13.94 14.47
1 1 -4 663.38 12.13
1 6 1 65.81 15.56
0 3 4 26.75 11.72
0 4 3 87.61 14.51
1 -1 -1 221.89 7.01
1 4 5 25.45 16.36
1 5 4 135.51 17.27
4 2 8 25.14 17.84
0 2 4 10.71 6.15
2 4 6 5.77 13.02
2 5 5 38.07 21.77
3 1 7 16.60 13.34
4 -3 2 39.06 4.81
5 1 8 13.39 16.73
0 4 -1 1010.64 21.86
0 4 2 108.77 13.54
1 5 -2 518.97 17.84
1 5 3 0.07 15.30
2 6 -2 169.24 14.66
3 2 7 204.94 22.10
3 7 0 157.03 20.46
1 2 5 49.94 12.25
1 4 4 57.04 14.77
2 3 6 29.82 12.57
5 2 8 60.16 21.32
0 4 0 0.79 5.13
1 -1 2 -0.65 0.98
2 -1 4 -2.47 3.18
2 5 4 21.25 17.89
2 6 -1 2.51 11.06
2 6 1 3.05 15.19
3 4 6 4.34 18.98
4 -1 6 26.70 6.59
0 3 -2 24.91 3.82
1 5 -1 311.98 16.39
1 5 1 14.91 13.12
2 2 -6 87.11 6.18
2 6 0 7.79 9.62
3 5 5 47.81 16.31
3 6 3 12.71 20.60
4 1 7 10.15 13.85
4 3 7 6.83 19.89
6 1 8 134.21 20.00
6 2 8 41.56 22.06
1 5 0 168.10 13.41
3 -1 5 25.25 6.19
4 2 7 374.20 26.71
2 5 3 27.59 12.20
3 3 6 5.93 11.80
3 6 2 16.15 17.46
0 1 2 1433.54 20.47
0 2 2 60.50 7.77
0 3 1 223.19 11.99
1 1 4 959.79 21.95
1 2 4 48.95 10.57
1 4 -3 57.29 6.13
2 4 4 0.94 14.27
3 1 6 13.05 11.85
3 5 4 45.10 17.96
5 3 7 185.42 25.86
0 3 -1 243.69 9.50
1 4 2 -2.83 10.12
3 6 -2 360.13 19.95
5 1 7 26.70 15.37
5 2 7 135.16 22.17
2 5 -3 28.30 7.09
3 6 -1 30.58 12.86
4 3 6 -0.84 17.75
1 1 -5 32.24 4.71
2 5 1 275.26 20.06
3 5 3 167.88 21.12
4 5 4 278.41 26.35
4 6 2 43.92 18.87
5 -1 6 441.77 16.48
0 2 1 1747.63 24.56
2 3 4 5.10 12.61
2 4 3 1057.50 33.12
2 5 -2 246.12 14.68
2 5 0 540.69 22.82
3 3 5 48.73 15.58
4 4 5 160.18 21.57
6 1 7 152.12 19.44
6 2 7 6.96 18.68
0 1 1 36.47 4.36
1 2 3 948.02 23.78
1 4 -2 31.09 6.27
1 4 0 198.43 13.25
2 5 -1 622.92 22.60
3 4 4 159.82 16.90
4 1 6 24.91 13.61
4 6 1 5.62 16.08
0 0 -2 712.16 10.32
0 2 -2 54.28 3.01
1 3 2 -4.48 8.01
1 4 -1 170.69 11.20
5 5 4 166.96 24.94
1 1 3 2.40 4.01
2 2 4 545.65 21.55
4 5 3 404.21 24.78
4 6 -1 39.77 13.52
5 -2 5 -1.14 4.42
5 4 5 5.71 18.11
7 1 7 27.66 17.96
0 2 -1 1762.37 18.07
2 1 4 -0.01 7.03
3 5 1 601.83 27.56
4 3 5 409.69 24.10
4 4 4 35.41 16.45
4 6 -2 317.64 19.65
5 0 6 91.72 13.37
5 2 6 92.70 18.83
1 3 -4 6.45 2.41
2 3 3 93.54 11.51
3 -3 2 25.68 3.76
3 3 4 2.71 12.13
3 4 3 207.46 17.09
5 6 1 38.14 13.79
6 -1 6 458.90 19.06
6 4 5 112.25 21.59
8 1 7 1.24 19.08
1 3 1 162.67 10.23
2 4 1 239.14 16.68
3 5 0 262.71 19.05
5 5 3 81.69 18.89
5 6 0 331.38 24.20
7 3 6 -12.33 20.24
1 2 2 969.81 21.61
6 2 6 17.32 16.72
9 1 7 -11.97 19.05
3 4 2 30.49 13.24
3 5 -3 4.23 7.97
3 5 -2 16.69 11.16
3 5 -1 55.72 12.95
5 6 -1 21.52 15.31
1 3 0 20.66 6.61
2 4 0 36.41 10.45
3 2 4 256.21 16.14
4 3 4 30.99 15.10
4 4 3 2.68 10.76
4 5 1 78.33 16.57
5 5 2 43.04 17.81
5 6 -2 27.73 13.31
6 5 3 32.44 15.84
7 2 6 123.16 22.62
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 10210
_shelx_res_file
;
TITL MS_2BAA-01 in P2(1)/c
MS_2BAA-01_a.res
created by SHELXL-2019/3 at 13:58:13 on 11-Jun-2024
CELL 0.71073 10.3729 5.1899 7.5567 90.000 99.943 90.000
ZERR 4.000 0.0041 0.0014 0.0032 0.000 0.033 0.000
LATT 1
SYMM -X, 1/2+Y, 1/2-Z
SFAC C H BR N O
UNIT 8 16 4 4 4
L.S. 10
BOND $h
CONF
TEMP -180.15
SIZE 0.11 0.09 0.04
LIST 4
ACTA
OMIT -3 54
HTAB N1 Br1
EQIV $1 x, y+1, z
HTAB N1 O1_$1
EQIV $2 -x+2, -y+1, -z+1
HTAB N1 O1_$2
EQIV $3 x, y-1, z
HTAB C2 Br1_$3
EQIV $4 x, -y+1/2, z+1/2
HTAB C2 O1_$4
FMAP 2
PLAN 20
WGHT 0.041700 0.056900
FVAR 0.51563
BR1 3 0.611796 0.825817 0.686532 11.00000 0.01411 0.01458 =
0.01913 0.00064 0.00526 0.00213
O1 5 0.868087 0.294488 0.554135 11.00000 0.01687 0.01286 =
0.02596 -0.00054 0.00779 0.00024
N1 4 0.885488 0.727102 0.581343 11.00000 0.01352 0.01531 =
0.02509 -0.00236 0.00814 0.00081
H1N 2 0.853879 0.862972 0.607850 11.00000 -1.50000
H2N 2 0.950340 0.735010 0.550151 11.00000 -1.50000
C1 1 0.825731 0.506021 0.596164 11.00000 0.01139 0.01671 =
0.01349 0.00337 0.00126 0.00295
C2 1 0.699680 0.497440 0.670872 11.00000 0.01468 0.01279 =
0.02159 0.00065 0.00629 0.00119
AFIX 23
H2A 2 0.718682 0.421332 0.792727 11.00000 -1.20000
H2B 2 0.638276 0.380045 0.594915 11.00000 -1.20000
AFIX 0
HKLF 4
REM MS_2BAA-01 in P2(1)/c
REM wR2 = 0.0682, GooF = S = 1.044, Restrained GooF = 1.044 for all data
REM R1 = 0.0275 for 731 Fo > 4sig(Fo) and 0.0362 for all 879 data
REM 52 parameters refined using 0 restraints
END
WGHT 0.0417 0.0569
REM Highest difference peak 0.584, deepest hole -0.506, 1-sigma level 0.132
Q1 1 0.6260 0.9612 0.5424 11.00000 0.05 0.58
Q2 1 0.6203 0.9882 0.8116 11.00000 0.05 0.53
Q3 1 0.6022 0.6625 0.8174 11.00000 0.05 0.50
Q4 1 0.7021 0.8641 0.8418 11.00000 0.05 0.50
Q5 1 0.5806 0.1799 0.4790 11.00000 0.05 0.49
Q6 1 0.5070 0.6948 0.5619 11.00000 0.05 0.46
Q7 1 0.5231 0.8447 0.5191 11.00000 0.05 0.44
Q8 1 1.0350 0.8456 0.6580 11.00000 0.05 0.36
Q9 1 0.6278 1.0423 0.6566 11.00000 0.05 0.36
Q10 1 0.5170 0.2528 0.5869 11.00000 0.05 0.35
Q11 1 0.8265 0.4993 0.4097 11.00000 0.05 0.35
Q12 1 0.6523 0.6313 0.5957 11.00000 0.05 0.35
Q13 1 0.8842 1.0894 0.6876 11.00000 0.05 0.34
Q14 1 0.7159 0.5158 0.4538 11.00000 0.05 0.34
Q15 1 0.7959 0.8334 0.6958 11.00000 0.05 0.34
Q16 1 0.6376 0.5017 0.9080 11.00000 0.05 0.33
Q17 1 0.5497 0.6031 0.6801 11.00000 0.05 0.33
Q18 1 0.7479 0.5058 0.5979 11.00000 0.05 0.33
Q19 1 0.8072 0.1523 0.6473 11.00000 0.05 0.32
Q20 1 0.5789 0.3619 0.8300 11.00000 0.05 0.32
;
_shelx_res_checksum 79635
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.61180(3) 0.82582(6) 0.68653(4) 0.01566(15) Uani d 1 . .
O O1 0.8681(3) 0.2945(4) 0.5541(3) 0.0181(6) Uani d 1 . .
N N1 0.8855(3) 0.7271(6) 0.5813(4) 0.0174(7) Uani d 1 . .
H H1N 0.854(4) 0.863(7) 0.608(6) 0.026 Uiso d 1 . .
H H2N 0.950(5) 0.735(8) 0.550(6) 0.026 Uiso d 1 . .
C C1 0.8257(3) 0.5060(7) 0.5962(4) 0.0140(7) Uani d 1 . .
C C2 0.6997(3) 0.4974(6) 0.6709(5) 0.0160(7) Uani d 1 . .
H H2A 0.718682 0.421332 0.792727 0.019 Uiso calc 1 . .
H H2B 0.638276 0.380045 0.594915 0.019 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 0.0141(2) 0.0146(2) 0.0191(2) 0.00213(14) 0.00526(14) 0.00064(14)
O1 0.0169(14) 0.0129(12) 0.0260(15) 0.0002(10) 0.0078(12) -0.0005(10)
N1 0.0135(16) 0.0153(14) 0.0251(18) 0.0008(13) 0.0081(14) -0.0024(13)
C1 0.0114(18) 0.0167(16) 0.0135(16) 0.0029(14) 0.0013(13) 0.0034(14)
C2 0.0147(19) 0.0128(15) 0.0216(17) 0.0012(15) 0.0063(14) 0.0006(15)
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
30 17 10 0.0667
30 -4 3 0.0783
30 -14 -1 0.0910
30 4 -9 0.0943
14 8 -15 0.0979
-3 -2 15 0.1196
-30 1 4 0.0693
-30 2 -7 0.1064
-30 10 3 0.0666
-15 -1 8 0.1044
-1 -15 0 0.0554
7 6 -30 0.0877
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 H1N . . 121(3) ?
C1 N1 H2N . . 122(3) ?
H1N N1 H2N . . 117(5) ?
O1 C1 N1 . . 123.7(3) ?
O1 C1 C2 . . 115.8(3) ?
N1 C1 C2 . . 120.5(3) ?
C1 C2 Br1 . . 116.2(2) ?
C1 C2 H2A . . 108.2 ?
Br1 C2 H2A . . 108.2 ?
C1 C2 H2B . . 108.2 ?
Br1 C2 H2B . . 108.2 ?
H2A C2 H2B . . 107.4 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Br1 C2 . 1.946(3) ?
O1 C1 . 1.244(4) ?
N1 C1 . 1.318(5) ?
N1 H1N . 0.82(4) ?
N1 H2N . 0.75(5) ?
C1 C2 . 1.512(5) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
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 H1N Br1 . 0.82(4) 2.69(4) 3.120(3) 115(3) yes
N1 H1N O1 1_565 0.82(4) 2.29(4) 2.955(4) 140(4) yes
N1 H2N O1 3_766 0.75(5) 2.17(5) 2.915(5) 172(5) yes
C2 H2B Br1 1_545 0.99 2.98 3.610(3) 122 yes
C2 H2A O1 4_566 0.99 2.55 3.462(4) 153 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
O1 C1 C2 Br1 . . . . -166.7(2) no
N1 C1 C2 Br1 . . . . 14.4(4) no