#------------------------------------------------------------------------------
#$Date: 2024-06-19 04:56:42 +0300 (Wed, 19 Jun 2024) $
#$Revision: 292463 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023173.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_2023173
loop_
_publ_author_name
'Semenikhin, Oleksandr A.'
'Shova, Sergiu'
'Golenya, Irina A.'
'Naumova, Dina D.'
'Gural'skiy, Il'ya A.'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of 2-bromoethylammonium
bromide -- a possible side product upon synthesis of hybrid perovskites
;
_journal_coeditor_code WM5723
_journal_issue 7
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024005619
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C2 H7 Br N +, Br -'
_chemical_formula_moiety 'C2 H7 Br N +, Br -'
_chemical_formula_sum 'C2 H7 Br2 N'
_chemical_formula_weight 204.91
_chemical_name_systematic
;
2-Bromoethylammonium bromide
;
_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 geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 90
_cell_angle_beta 100.546(5)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.8966(4)
_cell_length_b 8.3394(4)
_cell_length_c 9.0089(4)
_cell_measurement_reflns_used 2526
_cell_measurement_temperature 200.00(10)
_cell_measurement_theta_max 30.0180
_cell_measurement_theta_min 2.6320
_cell_volume 583.24(5)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2024)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2024)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2024)
;
_computing_molecular_graphics
;
Olex2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 200.00(10)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0239
_diffrn_reflns_av_unetI/netI 0.0293
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 4504
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 30.251
_diffrn_reflns_theta_min 2.624
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 13.749
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.45125
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2024)
;
_exptl_crystal_colour 'clear intense colourless'
_exptl_crystal_density_diffrn 2.334
_exptl_crystal_description plate
_exptl_crystal_F_000 384
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.02
_refine_diff_density_max 0.560
_refine_diff_density_min -0.469
_refine_ls_extinction_coef 0.0055(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.037
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 49
_refine_ls_number_reflns 1453
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.037
_refine_ls_R_factor_all 0.0305
_refine_ls_R_factor_gt 0.0236
_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^)+(0.0280P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0525
_refine_ls_wR_factor_ref 0.0541
_reflns_number_gt 1242
_reflns_number_total 1453
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wm5723.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2023173
_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 0.232
_shelx_estimated_absorpt_t_max 0.771
_shelx_hkl_file
;
0 0 -1 0.54 0.66
0 0 -1 0.88 0.45
0 0 -2 4.54 1.04
0 0 -2 3.70 1.34
0 0 2 5.53 1.09
0 0 -3 -0.15 1.37
0 0 -3 -0.78 2.08
0 0 3 -1.06 1.93
0 0 3 -0.94 1.46
0 0 -4 1315.80 42.27
0 0 -4 1394.31 40.84
0 0 4 1377.91 42.60
0 0 4 1377.39 41.61
0 0 5 4.69 3.31
0 0 -5 1.23 3.24
0 0 -5 -0.77 2.22
0 0 5 -1.00 2.51
0 0 -6 1722.76 52.71
0 0 6 1762.75 54.05
0 0 6 1837.70 55.37
0 0 -6 1713.46 54.38
0 0 -7 -1.00 3.93
0 0 -7 -0.31 2.97
0 0 -7 1.07 3.58
0 0 7 -0.97 3.81
0 0 -8 16.25 2.53
0 0 -8 19.07 3.88
0 0 -8 17.20 5.13
0 0 -8 26.23 4.64
0 0 8 22.78 5.35
0 0 9 0.65 5.24
0 0 -9 2.37 4.64
0 0 -10 3.14 5.02
0 0 10 -0.73 6.16
0 0 11 -0.81 7.17
0 -1 0 0.32 0.54
0 1 1 14.67 1.27
0 1 -1 14.27 1.20
0 1 -1 14.53 1.00
0 1 1 10.39 0.96
0 -1 -1 14.18 1.23
0 1 -1 14.53 0.98
0 -1 -2 3600.87 100.78
0 -1 -2 3627.83 100.98
0 1 2 3521.60 99.77
0 1 -2 3557.50 100.61
0 1 2 3602.75 100.69
0 1 -2 3453.03 100.70
0 -1 -3 2449.70 70.83
0 -1 3 2422.76 71.65
0 1 -3 2511.70 70.67
0 -1 -3 2371.99 71.14
0 1 3 2504.17 70.85
0 -1 -3 2472.57 70.60
0 1 -3 2391.51 70.63
0 -1 -4 31.94 3.82
0 1 -4 35.87 2.77
0 1 4 36.99 3.49
0 1 4 32.77 3.19
0 -1 -4 31.79 3.29
0 -1 4 37.25 4.26
0 1 -4 37.94 3.28
0 -1 -4 31.91 3.10
0 1 -4 36.27 3.28
0 1 -5 366.39 13.37
0 -1 -5 341.34 14.58
0 1 -5 362.51 12.49
0 1 5 324.41 13.45
0 -1 5 344.65 15.23
0 1 5 357.79 13.09
0 -1 -5 322.06 12.60
0 -1 -5 332.93 13.12
0 1 -5 363.35 13.36
0 -1 -6 1331.85 40.32
0 1 -6 1341.48 41.06
0 1 -6 1407.64 79.88
0 1 6 1276.82 41.51
0 -1 6 1260.74 43.31
0 -1 -6 1275.53 42.78
0 -1 -6 1307.26 40.75
0 -1 7 5.87 5.02
0 -1 -7 13.56 3.66
0 1 7 10.35 4.04
0 -1 -7 3.61 4.93
0 1 -7 16.91 4.15
0 1 -7 10.34 3.47
0 -1 -7 14.99 4.14
0 1 -8 890.77 29.53
0 -1 -8 918.77 31.46
0 1 -8 927.03 31.55
0 -1 8 924.49 33.96
0 1 -8 927.81 30.34
0 -1 -8 908.84 33.59
0 1 8 1001.39 33.27
0 1 9 74.10 8.39
0 -1 -9 81.24 7.45
0 1 -9 86.52 6.92
0 -1 9 104.17 9.78
0 1 10 188.17 13.09
0 -1 -10 193.61 11.77
0 1 -10 205.02 11.16
0 1 11 44.38 8.68
0 -2 0 1105.83 32.51
0 2 -1 1119.75 32.20
0 2 1 1152.22 33.29
0 2 1 1113.87 32.24
0 2 1 1138.86 33.34
0 -2 1 1124.77 32.52
0 -2 1 1117.53 32.24
0 -2 -1 1157.49 32.96
0 2 -2 5880.29 163.18
0 -2 -2 5755.70 163.16
0 2 2 5695.81 163.30
0 -2 2 5853.48 163.24
0 2 -2 5714.96 162.92
0 2 -2 5863.39 163.75
0 2 2 5898.97 164.04
0 -2 -2 5723.11 163.88
0 -2 -3 385.11 13.19
0 2 -3 377.71 12.93
0 -2 3 356.85 12.77
0 -2 3 384.95 13.42
0 -2 -3 375.41 12.72
0 2 3 366.51 12.86
0 -2 -3 390.42 13.59
0 2 -3 377.47 12.70
0 -2 -4 583.06 19.28
0 -2 4 573.43 20.09
0 -2 -4 565.37 18.93
0 -2 -4 577.63 19.74
0 2 4 564.60 19.23
0 2 -4 558.10 18.88
0 2 4 582.75 17.83
0 2 -4 576.51 18.95
0 -2 4 574.14 19.15
0 2 -5 1471.24 44.14
0 -2 5 1469.32 46.30
0 -2 -5 1385.71 45.00
0 -2 -5 1455.33 44.13
0 2 -5 1452.32 42.84
0 2 5 1456.65 44.41
0 2 5 1466.35 44.61
0 2 -5 1424.43 43.90
0 -2 5 1426.78 44.34
0 -2 -5 1422.12 44.71
0 2 6 311.75 13.61
0 2 6 325.84 13.19
0 -2 6 283.10 15.10
0 2 -6 332.15 12.00
0 -2 -6 316.66 13.56
0 -2 -6 317.57 14.47
0 2 -6 329.63 12.97
0 -2 -6 304.96 12.75
0 -2 6 308.53 13.28
0 2 -6 322.21 13.18
0 2 -7 197.62 8.87
0 2 -7 198.92 9.92
0 -2 -7 185.16 11.72
0 -2 7 197.40 10.63
0 2 7 205.32 10.92
0 -2 7 187.91 12.83
0 -2 -7 192.25 10.47
0 -2 -8 80.69 7.46
0 2 8 76.42 7.80
0 2 -8 67.93 5.69
0 -2 8 68.54 9.37
0 -2 8 72.10 7.33
0 2 -8 73.55 5.79
0 -2 9 335.33 18.91
0 2 9 356.32 16.93
0 -2 9 341.57 16.44
0 2 -9 326.45 13.77
0 -2 10 3.64 6.25
0 -2 10 8.22 7.95
0 2 10 7.54 6.62
0 2 -10 2.14 4.59
0 2 11 63.41 9.63
0 -2 11 53.24 8.95
0 -3 0 1.17 1.55
0 3 0 -0.32 1.46
0 3 1 821.30 23.72
0 3 -1 823.98 23.66
0 -3 1 804.03 25.53
0 3 1 827.01 25.42
0 3 1 826.60 25.50
0 -3 -1 824.25 23.67
0 -3 -1 822.64 25.21
0 -3 2 383.36 12.53
0 -3 2 385.28 12.28
0 3 2 386.16 13.64
0 3 2 398.70 13.66
0 3 -2 377.34 13.39
0 3 -2 387.84 12.25
0 3 2 376.59 12.30
0 -3 -3 2069.64 61.08
0 3 -3 2002.02 60.78
0 3 -3 2082.44 59.52
0 -3 3 2053.73 61.20
0 3 3 2110.02 60.29
0 -3 3 2058.90 60.20
0 3 3 2104.13 61.34
0 -3 4 2905.30 86.97
0 -3 -4 3058.28 86.65
0 -3 4 2918.15 85.99
0 3 -4 2990.12 86.26
0 3 4 3010.09 86.19
0 3 -4 2929.79 85.05
0 3 -5 -0.61 2.60
0 3 -5 -0.31 2.67
0 -3 5 2.31 2.71
0 -3 -5 3.05 3.02
0 3 5 2.23 2.91
0 -3 -5 2.45 2.79
0 3 5 4.09 2.93
0 -3 5 0.88 3.42
0 3 -5 -0.62 2.75
0 3 5 0.35 1.92
0 3 6 157.05 8.82
0 -3 -6 148.31 8.36
0 3 -6 152.47 7.14
0 -3 -6 162.47 8.59
0 -3 6 187.01 11.22
0 -3 -6 146.01 9.14
0 3 6 153.27 8.87
0 3 -6 170.56 8.46
0 3 -6 161.50 8.34
0 3 -6 158.35 8.52
0 -3 6 165.72 8.98
0 3 -7 31.44 3.94
0 -3 7 38.13 5.43
0 3 -7 31.62 4.41
0 -3 -7 34.15 5.89
0 -3 7 34.41 7.32
0 3 7 33.57 5.24
0 3 -7 32.18 4.70
0 -3 8 220.40 12.10
0 -3 8 226.62 15.12
0 3 -8 225.42 9.90
0 3 8 207.98 12.16
0 3 -9 66.19 5.83
0 3 9 56.75 7.90
0 -3 9 70.79 11.07
0 -3 9 63.65 7.37
0 3 10 493.28 22.13
0 -3 10 487.62 24.87
0 -3 10 474.18 21.50
0 -3 11 25.49 9.99
0 -3 12 45.77 10.95
0 4 0 73.31 4.40
0 -4 0 79.32 4.82
0 -4 -1 196.27 6.08
0 4 1 198.81 8.40
0 4 1 199.63 8.45
0 -4 -1 201.29 8.40
0 4 -1 197.84 6.09
0 4 2 2432.57 70.22
0 -4 -2 2483.31 70.14
0 -4 2 2495.75 70.98
0 4 2 2470.38 72.46
0 4 -2 2455.65 70.10
0 4 2 2442.83 72.31
0 -4 -2 2446.82 71.61
0 -4 -3 637.63 19.43
0 -4 3 600.74 19.41
0 -4 3 621.84 21.08
0 4 3 598.12 20.98
0 4 -3 617.98 19.39
0 4 -3 631.22 20.96
0 -4 -3 604.22 19.94
0 4 3 604.25 19.50
0 4 -4 1165.70 36.46
0 4 4 1127.56 35.49
0 -4 4 1141.22 36.84
0 4 4 1156.11 36.87
0 -4 4 1167.04 35.50
0 4 -4 1165.97 35.29
0 -4 -4 1169.26 35.32
0 -4 -4 1151.10 36.56
0 4 -5 67.85 5.13
0 4 5 67.06 5.40
0 4 -5 65.22 4.02
0 -4 5 71.78 6.05
0 4 -5 69.73 5.60
0 -4 -5 70.66 5.22
0 -4 5 67.88 5.11
0 -4 -5 73.53 5.86
0 4 6 98.34 5.44
0 -4 -6 108.10 6.89
0 -4 6 101.90 8.28
0 4 6 96.50 7.06
0 4 -6 107.45 6.93
0 4 -6 106.95 5.66
0 4 -6 95.73 6.89
0 -4 6 107.06 7.04
0 4 7 728.01 26.75
0 -4 7 745.13 26.61
0 4 -7 745.51 24.41
0 4 -7 752.01 24.06
0 -4 7 801.24 29.97
0 -4 8 328.93 18.22
0 4 -8 302.74 12.41
0 4 8 286.08 14.74
0 4 -8 307.09 11.87
0 -4 8 302.45 14.75
0 4 9 96.43 9.25
0 -4 9 112.58 9.51
0 -4 9 106.09 12.97
0 -4 10 18.93 10.53
0 -4 11 166.00 16.64
0 5 0 1.34 2.31
0 -5 0 0.33 2.79
0 5 1 3048.46 89.03
0 -5 -1 3020.92 89.04
0 5 1 3073.86 89.08
0 5 2 31.93 4.20
0 5 -2 44.35 4.46
0 5 -2 41.77 2.35
0 -5 -2 44.60 4.16
0 5 2 37.83 4.23
0 -5 -2 38.04 2.31
0 -5 2 39.09 3.40
0 -5 -3 8.14 2.01
0 5 3 5.15 3.53
0 5 3 13.07 3.34
0 5 -3 8.12 2.02
0 -5 -3 6.84 3.01
0 5 -3 5.03 3.22
0 -5 3 5.80 3.60
0 5 -4 326.72 11.87
0 -5 -4 325.91 11.85
0 -5 -4 355.71 12.68
0 5 4 304.37 11.95
0 5 -4 317.28 13.44
0 -5 4 321.98 13.96
0 5 5 1272.54 40.24
0 5 -5 1319.21 40.05
0 -5 5 1307.78 42.18
0 -5 5 1272.12 40.18
0 -5 -5 1275.84 39.57
0 -5 -5 1343.18 40.00
0 -5 6 131.17 7.92
0 -5 -6 138.13 6.87
0 5 6 138.62 6.70
0 -5 6 145.85 9.47
0 -5 -6 143.25 7.79
0 5 -6 135.45 7.84
0 5 6 119.41 7.83
0 5 -7 69.71 4.72
0 5 7 69.48 6.76
0 -5 -7 72.51 4.88
0 -5 7 67.89 8.40
0 -5 7 77.08 6.77
0 -5 8 67.56 10.37
0 5 8 65.37 7.44
0 -5 9 39.56 9.98
0 -5 10 118.19 14.42
0 -5 11 10.28 11.13
0 6 0 810.00 26.11
0 -6 0 780.30 26.66
0 6 0 759.78 25.71
0 6 1 1529.32 46.19
0 6 1 1492.25 46.10
0 -6 -1 1460.18 46.14
0 6 -1 1463.18 45.09
0 6 2 11.79 3.93
0 6 2 8.47 3.91
0 -6 2 11.17 2.93
0 -6 -2 6.17 3.34
0 -6 3 22.02 3.57
0 -6 3 31.89 5.18
0 6 -3 26.64 2.50
0 -6 -3 27.18 2.54
0 -6 -3 24.20 4.02
0 6 3 28.56 5.00
0 -6 4 76.91 7.02
0 -6 -4 82.38 4.81
0 6 -4 72.98 4.51
0 -6 -4 83.92 6.05
0 -6 5 151.99 9.87
0 -6 -5 160.25 8.39
0 6 -5 160.77 7.93
0 -6 -5 174.08 8.06
0 -6 6 182.52 11.36
0 -6 -6 189.76 9.02
0 -6 -6 177.33 9.06
0 6 -6 193.94 9.35
0 -6 -7 796.07 25.87
0 -6 7 802.13 30.41
0 -6 8 16.69 8.05
0 -6 9 187.37 15.30
0 -6 10 -10.57 9.79
0 7 0 0.76 3.52
0 7 0 1.16 3.58
0 7 -1 1060.59 34.04
0 7 1 1108.23 35.19
0 -7 -1 1045.49 35.23
0 7 1 1061.26 35.05
0 7 -2 343.11 13.45
0 7 2 339.13 15.03
0 -7 -2 364.19 14.95
0 -7 2 351.43 13.44
0 -7 -3 476.81 18.24
0 -7 3 489.90 17.60
0 -7 3 490.95 19.79
0 7 -3 479.47 17.00
0 -7 -4 415.05 16.20
0 -7 4 404.35 17.67
0 7 -4 406.80 13.90
0 -7 -4 415.16 13.91
0 -7 -5 320.60 13.67
0 -7 5 357.51 16.34
0 -7 6 81.32 8.55
0 7 -6 75.56 5.89
0 -7 -6 90.86 6.48
0 -7 7 85.58 9.14
0 -7 8 33.53 8.79
0 -7 9 -1.03 8.84
0 8 0 79.57 7.13
0 8 -1 186.61 9.72
0 8 1 176.58 10.30
0 8 -1 205.48 10.09
0 -8 2 75.39 6.13
0 8 -2 84.00 6.24
0 8 2 76.06 7.44
0 8 -2 87.20 6.31
0 -8 3 304.31 13.15
0 -8 -3 311.44 14.19
0 -8 3 315.73 15.47
0 8 -3 314.65 12.70
0 -8 4 42.27 7.38
0 8 -4 43.38 4.77
0 -8 -4 50.34 5.94
0 -8 -5 339.07 14.77
0 -8 5 347.36 17.28
0 -8 6 114.11 10.42
0 -8 7 136.99 11.83
0 -8 8 32.37 9.42
0 9 0 -1.94 4.37
0 9 -1 149.11 9.50
0 9 1 155.32 10.26
0 9 -2 10.48 4.43
0 -9 3 1095.75 39.21
0 9 -3 1119.90 35.85
0 -9 4 9.17 6.60
0 -9 5 15.14 6.89
0 -9 6 56.14 9.34
0 10 0 286.20 14.13
0 10 -1 28.37 6.13
0 -10 2 16.41 6.76
0 -10 3 33.01 8.06
1 0 -12 2.61 6.17
1 0 -11 2.43 5.75
1 0 -10 386.03 16.97
1 0 -9 4.18 3.66
1 0 -9 -0.88 3.91
1 0 -9 10.00 4.71
-1 0 8 587.59 23.22
1 0 -8 614.29 19.46
1 0 -8 609.76 21.01
1 0 -8 618.97 22.12
1 0 -8 649.62 22.80
1 0 -7 2.24 3.43
1 0 -7 1.98 3.38
1 0 -7 0.27 2.57
-1 0 7 0.46 3.94
1 0 -7 -1.59 1.83
-1 0 6 293.42 13.15
1 0 -6 296.62 12.88
1 0 -6 331.36 13.16
1 0 -6 321.21 12.97
1 0 -6 334.09 12.87
1 0 -6 321.89 11.80
1 0 -6 323.47 10.66
1 0 -5 -0.22 1.27
1 0 -5 -1.75 2.54
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-8 1 1 419.26 21.32
-8 -1 1 368.65 15.72
-8 1 1 397.71 16.40
8 -1 0 52.06 6.87
-8 -1 0 48.12 7.85
-8 1 0 69.55 8.90
-8 1 -1 6.98 8.14
8 -1 1 3.82 5.83
-8 1 -1 3.10 6.43
-8 1 -2 -1.03 7.98
8 -1 2 2.12 6.19
-8 1 -2 -2.40 6.67
-8 -1 -2 15.74 8.90
-8 1 -3 26.20 9.11
8 -1 3 26.90 7.47
-8 -1 -3 24.72 8.63
8 -1 4 285.02 16.86
-8 1 -4 308.88 19.59
-8 1 -5 77.49 12.40
-8 2 9 22.30 7.11
8 -2 -8 -1.78 7.53
-8 2 8 -6.38 8.08
-8 -2 8 1.87 8.12
-8 2 8 3.79 6.29
-8 2 7 274.24 17.08
-8 -2 7 305.38 17.88
-8 -2 7 275.72 13.84
-8 2 6 108.74 11.60
-8 -2 6 135.26 12.55
-8 2 5 81.57 10.83
-8 -2 5 79.53 10.60
-8 2 5 92.38 9.88
-8 2 4 64.10 9.85
-8 -2 4 63.14 10.13
-8 2 4 71.72 8.89
-8 -2 3 121.25 9.52
8 -2 -3 131.23 7.50
-8 2 3 132.70 11.83
-8 -2 2 345.15 16.40
8 -2 -2 330.29 14.33
-8 -2 2 338.91 13.67
-8 2 2 308.19 18.09
-8 -2 1 252.30 13.86
-8 2 1 266.86 16.08
8 -2 -1 248.09 12.69
-8 -2 1 223.71 11.77
-8 2 1 265.97 16.64
-8 2 0 481.46 22.43
8 -2 0 467.41 19.87
-8 2 -1 461.22 22.02
8 -2 1 445.18 20.24
-8 2 -1 472.23 24.38
8 -2 2 130.02 10.88
-8 2 -2 142.47 14.23
-8 2 -3 38.20 10.09
8 -2 3 35.22 8.10
-8 2 -3 40.50 8.61
-8 2 -4 162.84 13.68
8 -2 4 154.51 12.95
-8 2 -4 173.42 15.86
-8 2 -5 -12.56 9.85
-8 3 9 8.49 7.31
-8 3 8 226.51 14.14
-8 -3 7 8.78 5.77
8 -3 -7 -2.57 7.22
-8 3 7 8.85 7.27
-8 -3 7 6.37 8.03
8 -3 -6 123.72 11.72
-8 3 6 135.91 12.20
-8 -3 6 159.31 13.10
-8 3 6 149.14 11.40
-8 3 5 75.62 9.54
8 -3 -5 58.74 8.78
-8 3 5 96.12 11.00
-8 -3 5 81.67 10.65
-8 3 4 7.24 7.28
-8 -3 4 4.58 5.06
-8 3 4 7.35 8.02
-8 -3 4 1.89 7.89
-8 3 3 6.10 7.04
8 -3 -3 -2.90 4.27
-8 -3 3 -1.57 5.20
8 -3 -2 610.84 23.33
-8 -3 2 581.90 22.31
-8 3 2 633.25 28.42
-8 3 1 397.99 20.94
8 -3 -1 364.65 17.21
-8 3 1 424.35 22.39
-8 3 0 55.85 10.85
8 -3 0 59.15 7.55
-8 3 0 58.02 9.67
8 -3 1 160.04 11.76
8 -3 2 80.03 9.63
-8 3 -2 81.95 12.13
-8 3 -2 81.42 10.81
8 -3 3 2.47 6.83
-8 3 -3 -10.65 10.15
-8 3 -3 3.65 8.19
8 -3 4 32.83 8.57
-8 3 -4 30.17 11.36
-8 3 -4 37.43 9.00
-8 -4 8 9.12 6.16
-8 4 8 8.61 7.63
-8 -4 7 31.13 7.13
8 -4 -7 33.86 9.05
-8 4 7 40.41 8.74
-8 -4 7 38.44 9.56
-8 4 7 45.60 7.90
8 -4 -6 236.21 15.78
-8 4 6 305.45 17.29
-8 -4 6 272.80 16.98
-8 -4 6 268.02 15.45
-8 4 6 317.54 16.42
8 -4 -5 202.50 13.86
-8 4 5 200.33 14.65
-8 -4 5 195.27 14.50
-8 4 5 211.12 13.96
-8 4 4 -1.74 7.02
-8 4 4 0.90 7.45
8 -4 -4 5.67 6.19
-8 -4 4 -3.63 7.49
-8 -4 4 0.82 4.69
-8 4 3 39.70 9.01
8 -4 -3 36.53 7.31
-8 -4 3 50.77 6.51
-8 4 3 30.16 8.62
-8 4 2 39.99 9.50
8 -4 -2 43.18 6.27
8 -4 -2 34.64 6.62
8 -4 -1 -2.40 5.75
8 -4 -1 3.09 4.97
8 -4 0 610.88 22.56
8 -4 0 628.36 25.24
8 -4 1 14.04 6.50
8 -4 1 12.09 4.50
-8 4 -1 7.59 8.52
8 -4 2 0.81 6.80
-8 4 -2 3.73 8.08
8 -4 3 74.18 10.28
-8 4 -3 72.76 10.77
8 -4 4 90.75 11.53
-8 -5 8 96.83 9.95
-8 -5 7 10.85 6.95
-8 5 7 -0.84 7.94
-8 -5 7 3.36 7.66
-8 -5 6 29.29 8.45
-8 5 6 37.83 8.57
-8 -5 6 18.42 7.63
8 -5 -6 28.48 8.37
-8 5 6 30.30 8.36
-8 5 5 2.56 7.40
-8 5 5 0.84 7.59
-8 -5 5 8.37 7.38
8 -5 -5 10.16 6.95
-8 5 4 -2.82 8.14
8 -5 -4 1.44 6.14
-8 5 4 -5.24 7.74
-8 -5 4 0.86 7.61
-8 5 3 598.04 27.20
-8 -5 3 556.32 26.55
8 -5 -3 604.15 24.81
-8 -5 3 658.68 22.87
8 -5 -2 39.28 6.96
8 -5 -2 23.78 6.62
8 -5 -1 -0.62 5.88
8 -5 -1 0.49 4.70
8 -5 0 -2.77 6.76
8 -5 1 207.89 13.81
8 -5 2 4.17 7.35
-8 5 -2 11.24 9.01
8 -5 3 287.48 17.57
-8 -6 7 13.52 7.95
-8 6 7 16.20 8.35
-8 6 6 20.52 8.37
-8 -6 6 9.95 7.82
8 -6 -6 14.64 8.61
-8 6 6 11.23 7.20
-8 -6 6 7.95 7.49
8 -6 -5 386.09 19.88
-8 6 5 375.76 19.71
-8 -6 5 364.44 19.43
-8 -6 5 399.37 20.95
-8 -6 4 63.55 9.63
8 -6 -4 79.72 9.79
-8 6 3 34.44 9.08
-8 -6 3 17.97 7.56
8 -6 -3 13.12 6.55
8 -6 -2 7.62 5.70
-8 6 2 6.19 8.37
8 -6 -2 17.68 6.51
8 -6 -1 21.15 6.83
8 -6 0 9.35 6.91
8 -6 1 95.46 10.48
8 -6 2 103.78 11.33
-8 7 6 13.53 7.85
8 -7 -5 28.21 8.31
-8 7 5 29.62 8.11
-8 7 4 48.98 8.72
8 -7 -4 41.28 8.61
8 -7 -3 157.98 11.73
-8 7 3 134.03 12.38
-8 7 2 152.68 13.04
8 -7 -1 149.79 11.73
8 -7 0 52.83 8.78
-9 0 6 335.44 21.17
-9 0 5 -1.13 9.48
-9 0 4 -3.38 8.91
-9 0 3 1.50 7.32
-9 0 2 807.79 31.34
-9 0 1 0.78 7.12
-9 0 1 -1.98 7.67
-9 0 0 109.40 10.69
-9 0 -1 2.43 7.10
-9 0 -1 1.04 8.17
-9 0 -2 12.82 7.44
-9 0 -2 9.53 8.92
-9 0 -3 13.93 9.45
-9 -1 6 15.91 10.51
-9 -1 5 130.20 14.14
-9 -1 4 -4.56 9.77
-9 -1 3 8.16 6.66
-9 1 3 10.73 7.99
-9 -1 2 -2.81 6.85
-9 1 2 -1.65 7.33
-9 1 2 8.51 8.38
-9 -1 1 59.10 8.90
-9 1 1 71.26 9.57
-9 1 1 69.15 11.40
-9 -1 0 397.22 19.68
-9 1 0 374.02 19.87
-9 -1 -1 172.06 13.02
-9 1 -1 138.90 12.42
-9 1 -1 186.18 15.87
-9 1 -2 18.95 9.62
-9 1 -2 12.85 8.21
-9 2 8 65.91 9.47
-9 2 6 126.59 14.07
-9 -2 6 171.73 15.42
-9 -2 5 89.45 12.47
-9 2 5 80.68 12.03
-9 2 4 227.22 17.51
-9 -2 4 216.07 17.37
-9 -2 3 347.16 17.16
-9 2 3 410.45 20.97
-9 2 2 130.54 12.89
-9 -2 2 118.12 10.26
-9 2 1 54.84 10.43
-9 -2 1 83.53 9.62
-9 2 1 69.74 10.73
9 -2 -1 77.82 7.93
-9 2 0 118.34 13.51
-9 -2 0 127.94 11.51
-9 2 0 114.73 11.42
9 -2 0 135.18 10.32
-9 2 -1 1.13 8.83
9 -2 1 2.09 6.67
-9 2 -1 0.88 7.57
-9 2 -2 86.96 13.05
9 -2 2 104.68 10.37
9 -2 3 214.93 14.92
-9 3 8 3.22 8.27
-9 -3 7 -0.69 6.81
9 -3 -6 132.05 12.66
-9 3 6 166.65 14.48
-9 -3 6 172.10 15.36
-9 -3 5 152.29 14.88
-9 3 5 149.71 14.46
-9 3 5 170.56 12.98
-9 3 4 37.36 8.84
-9 3 4 11.69 9.06
-9 -3 4 15.36 9.07
-9 -3 4 22.81 6.21
-9 3 3 99.30 11.86
-9 -3 3 99.80 9.12
-9 -3 2 147.52 11.12
-9 3 2 147.69 13.94
-9 3 1 -1.10 9.01
9 -3 -1 -4.15 5.61
-9 -3 1 6.88 6.99
-9 3 0 59.57 11.56
9 -3 0 52.56 7.86
-9 3 0 47.69 9.89
-9 3 -1 168.58 13.95
9 -3 1 173.22 12.54
9 -3 2 365.77 18.89
9 -3 3 1.70 7.06
-9 -4 7 0.75 7.77
9 -4 -6 8.93 8.20
-9 4 6 24.37 8.16
-9 4 5 0.86 7.63
9 -4 -5 7.43 7.51
-9 4 5 9.39 9.48
-9 -4 5 4.19 8.74
9 -4 -4 379.22 19.54
-9 4 4 391.60 22.41
-9 -4 4 379.32 22.14
-9 4 4 455.30 22.37
-9 4 3 19.47 9.09
-9 4 3 25.95 9.56
9 -4 -3 13.41 6.89
-9 -4 3 11.23 5.62
-9 4 2 2.26 9.68
9 -4 -2 8.87 6.31
-9 -4 2 15.99 6.48
-9 4 1 91.26 12.64
9 -4 -1 95.43 9.41
9 -4 -1 68.80 8.13
-9 4 0 79.19 12.92
9 -4 0 75.66 9.50
9 -4 1 24.38 8.25
9 -4 2 119.36 12.03
-9 -5 7 300.82 17.61
-9 5 6 16.60 8.39
-9 -5 6 12.21 7.90
-9 5 5 7.26 7.57
-9 5 5 5.08 8.92
-9 -5 5 -3.96 8.50
9 -5 -5 7.55 8.00
-9 5 4 -5.10 9.53
-9 -5 4 -7.95 9.33
9 -5 -4 4.65 6.90
-9 5 4 9.29 9.26
9 -5 -3 104.26 10.36
-9 5 3 86.75 12.12
-9 -5 3 90.79 12.66
-9 5 2 22.69 10.37
9 -5 -2 27.18 6.88
-9 -5 2 31.82 6.92
9 -5 0 0.76 6.98
9 -5 1 7.42 7.37
-9 6 5 11.85 9.12
9 -6 -5 10.16 8.25
-9 6 4 17.46 10.32
9 -6 -4 0.77 7.40
-9 6 4 3.99 8.95
-9 -6 4 4.66 8.79
-9 6 3 43.30 10.61
-9 -6 3 45.76 9.85
-9 6 2 97.90 12.59
9 -6 0 -1.56 7.38
-10 0 2 64.39 9.59
-10 0 1 -1.62 7.58
-10 0 0 258.76 16.49
-10 -1 3 184.15 13.10
-10 -1 2 35.86 8.57
-10 1 2 53.28 10.09
-10 1 2 50.85 9.95
-10 -1 1 11.14 7.70
-10 1 1 7.73 7.81
-10 -1 0 98.35 11.36
-10 2 4 49.92 9.95
-10 -2 3 -0.67 6.73
-10 2 3 -2.93 8.06
-10 -2 2 90.62 10.06
-10 -2 1 315.41 17.28
-10 -2 0 30.27 8.76
-10 3 5 6.99 7.95
-10 3 4 12.39 8.81
-10 -3 3 80.61 8.94
-10 -3 2 264.71 15.15
-10 -3 1 2.94 7.07
-10 -3 0 128.85 12.38
10 -4 -4 22.23 8.28
10 -4 -3 27.67 7.66
-10 -4 2 99.33 9.87
-10 -4 1 51.93 9.23
10 -5 -4 11.96 7.80
0 0 0 0.00 0.00
TITL shS_505_IlGu_auto in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 7.896597 8.339368 9.008899 90.0000 100.5455 90.0000
ZERR 4.00 0.000388 0.000362 0.000398 0.0000 0.0045 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N Cu Br
UNIT 8.00 28.00 4.00 4.00 16.00
REM CrysAlisPro recorded range (K): Min=200.0; max=200.0; aver:200.0
TEMP -73
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 93166
_shelx_res_file
;
TITL shs_505_ilgu_auto_a.res in P2(1)/c
shs_505_ilgu_auto.res
created by SHELXL-2018/3 at 16:00:29 on 01-May-2024
REM Old TITL shS_505_IlGu_auto in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.085, Rweak 0.005, Alpha 0.012
REM 0.401 for 89 systematic absences, Orientation as input
REM Formula found by SHELXT: C1 N Br1
CELL 0.71073 7.896597 8.339368 9.008899 90 100.5455 90
ZERR 4 0.000388 0.000362 0.000398 0 0.0045 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Br N
UNIT 8 28 8 4
EQIV $1 1-X,0.5+Y,1.5-Z
EQIV $2 1-X,1-Y,1-Z
EQIV $3 +X,0.5-Y,0.5+Z
L.S. 4
PLAN 5
SIZE 0.02 0.05 0.15
TEMP -73
CONF
HTAB N1 Br2
HTAB N1 Br2_$1
HTAB N1 Br2_$2
HTAB N1 Br2_$3
BOND
MORE -1
BOND $H
fmap 2
acta
REM
REM
REM
WGHT 0.028000
EXTI 0.005491
FVAR 0.54272
BR2 3 0.622879 0.216580 0.526106 11.00000 0.03128 0.02218 =
0.02435 -0.00179 0.00574 0.00045
BR1 3 0.802866 0.890020 0.821385 11.00000 0.02685 0.03231 =
0.05264 -0.00512 0.00868 -0.00574
N1 4 0.613038 0.541386 0.733780 11.00000 0.02891 0.02274 =
0.02382 0.00007 0.00481 0.00080
AFIX 138
H1A 2 0.582498 0.457891 0.681856 11.00000 -1.20000
H1B 2 0.574677 0.623917 0.683487 11.00000 -1.20000
H1C 2 0.572782 0.537967 0.814867 11.00000 -1.20000
AFIX 0
C2 1 0.803363 0.549027 0.770619 11.00000 0.02350 0.02861 =
0.02858 0.00590 0.00765 0.00672
AFIX 23
H2A 2 0.848456 0.575438 0.678011 11.00000 -1.20000
H2B 2 0.848904 0.442408 0.806124 11.00000 -1.20000
AFIX 0
C1 1 0.866974 0.672694 0.890757 11.00000 0.02564 0.04198 =
0.02943 0.00710 -0.00229 -0.00195
AFIX 23
H1D 2 0.993935 0.665423 0.918954 11.00000 -1.20000
H1E 2 0.817760 0.649328 0.981906 11.00000 -1.20000
AFIX 0
HKLF 4
REM shs_505_ilgu_auto_a.res in P2(1)/c
REM wR2 = 0.0541, GooF = S = 1.037, Restrained GooF = 1.037 for all data
REM R1 = 0.0236 for 1242 Fo > 4sig(Fo) and 0.0305 for all 1453 data
REM 49 parameters refined using 0 restraints
END
WGHT 0.0280 0.0000
REM Highest difference peak 0.560, deepest hole -0.469, 1-sigma level 0.102
Q1 1 0.7497 0.2207 0.5357 11.00000 0.05 0.56
Q2 1 0.5158 0.2226 0.5143 11.00000 0.05 0.54
Q3 1 0.8989 0.8690 0.8348 11.00000 0.05 0.47
Q4 1 0.6248 0.3312 0.5614 11.00000 0.05 0.43
Q5 1 0.6841 0.8666 0.8161 11.00000 0.05 0.42
;
_shelx_res_checksum 21198
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 Br2 0.62288(3) 0.21658(3) 0.52611(2) 0.02586(10) Uani d 1 . .
Br Br1 0.80287(4) 0.89002(3) 0.82138(3) 0.03709(11) Uani d 1 . .
N N1 0.6130(3) 0.5414(2) 0.7338(2) 0.0252(4) Uani d 1 . .
H H1A 0.5825(5) 0.4579(15) 0.6819(15) 0.030 Uiso calc 1 . .
H H1B 0.5747(6) 0.6239(14) 0.6835(16) 0.030 Uiso calc 1 . .
H H1C 0.5728(7) 0.5380(17) 0.8149(12) 0.030 Uiso calc 1 . .
C C2 0.8034(3) 0.5490(3) 0.7706(3) 0.0265(5) Uani d 1 . .
H H2A 0.848456 0.575438 0.678011 0.032 Uiso calc 1 . .
H H2B 0.848904 0.442408 0.806124 0.032 Uiso calc 1 . .
C C1 0.8670(4) 0.6727(3) 0.8908(3) 0.0333(6) Uani d 1 . .
H H1D 0.993935 0.665423 0.918954 0.040 Uiso calc 1 . .
H H1E 0.817760 0.649328 0.981906 0.040 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
Br2 0.03128(17) 0.02218(16) 0.02435(15) 0.00045(10) 0.00574(11) -0.00179(9)
Br1 0.02685(18) 0.03231(18) 0.0526(2) -0.00574(11) 0.00868(13) -0.00512(11)
N1 0.0289(12) 0.0227(10) 0.0238(10) 0.0008(9) 0.0048(9) 0.0001(8)
C2 0.0235(14) 0.0286(13) 0.0286(12) 0.0067(11) 0.0076(10) 0.0059(10)
C1 0.0256(15) 0.0420(15) 0.0294(13) -0.0019(13) -0.0023(11) 0.0071(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'
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
H1A N1 H1B . . 109.5 ?
H1A N1 H1C . . 109.5 ?
H1B N1 H1C . . 109.5 ?
C2 N1 H1A . . 109.5 ?
C2 N1 H1B . . 109.5 ?
C2 N1 H1C . . 109.5 ?
N1 C2 H2A . . 109.1 ?
N1 C2 H2B . . 109.1 ?
N1 C2 C1 . . 112.4(2) ?
H2A C2 H2B . . 107.9 ?
C1 C2 H2A . . 109.1 ?
C1 C2 H2B . . 109.1 ?
Br1 C1 H1D . . 109.3 ?
Br1 C1 H1E . . 109.3 ?
C2 C1 Br1 . . 111.77(17) ?
C2 C1 H1D . . 109.3 ?
C2 C1 H1E . . 109.3 ?
H1D C1 H1E . . 107.9 ?
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
Br1 C1 . 1.953(3) ?
N1 H1A . 0.849(12) ?
N1 H1B . 0.849(12) ?
N1 H1C . 0.849(12) ?
N1 C2 . 1.480(3) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C2 C1 . 1.513(4) ?
C1 H1D . 0.9900 ?
C1 H1E . 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 H1A Br2 . 0.85 2.51 3.3010(19) 156.1 yes
N1 H1B Br2 3_666 0.85 2.59 3.381(2) 156.2 yes
N1 H1C Br2 4_566 0.85 2.83 3.3904(19) 125.1 yes
N1 H1C Br2 2_656 0.85 2.73 3.4292(18) 140.3 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
N1 C2 C1 Br1 . . . . -64.8(2) ?