#------------------------------------------------------------------------------
#$Date: 2020-12-05 07:32:57 +0200 (Sat, 05 Dec 2020) $
#$Revision: 259555 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/22/2022294.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_2022294
loop_
_publ_author_name
'Mulrooney, David Z. T.'
'M\"uller-Bunz, Helge'
'Keene, Tony D.'
_publ_section_title
;
Crystal structure and halogen--hydrogen bonding of a Del\'epine reaction
intermediate
;
_journal_coeditor_code HB7951
_journal_issue 1
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 1
_journal_page_last 4
_journal_paper_doi 10.1107/S2056989020015601
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac 'C11 H22 Br N4 +, Br -'
_chemical_formula_moiety 'C11 H22 Br N4 +, Br -'
_chemical_formula_sum 'C11 H22 Br2 N4'
_chemical_formula_weight 370.14
_chemical_name_common '5-Bromourotropinium bromide'
_chemical_name_systematic
;
1-(5-Bromopentyl)-3,5,7-triaza-1-azoniatricyclo[3.3.1.1^3,7^]decane bromide
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha 90
_cell_angle_beta 101.742(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.7897(2)
_cell_length_b 14.8937(3)
_cell_length_c 11.1294(2)
_cell_measurement_reflns_used 10133
_cell_measurement_temperature 100
_cell_measurement_theta_max 76.7010
_cell_measurement_theta_min 5.0240
_cell_volume 1426.47(5)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Berndt, 1999)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
ShelXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.15
_diffrn_detector_area_resol_mean 10.3196
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0403
_diffrn_reflns_av_unetI/netI 0.0210
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 22370
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 76.926
_diffrn_reflns_theta_min 5.029
_exptl_absorpt_coefficient_mu 7.093
_exptl_absorpt_correction_T_max 0.788
_exptl_absorpt_correction_T_min 0.698
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.724
_exptl_crystal_description block
_exptl_crystal_F_000 744
_exptl_crystal_size_max 0.081
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.048
_refine_diff_density_max 0.532
_refine_diff_density_min -0.641
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.038
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 154
_refine_ls_number_reflns 2992
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.038
_refine_ls_R_factor_all 0.0310
_refine_ls_R_factor_gt 0.0254
_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^)+(0.0253P)^2^+1.7861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0593
_refine_ls_wR_factor_ref 0.0625
_reflns_number_gt 2652
_reflns_number_total 2992
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb7951sup1.cif
_cod_data_source_block I
_cod_database_code 2022294
_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 0.597
_shelx_estimated_absorpt_t_max 0.727
_shelx_hkl_file
;
0 0 1 0.10 1.65
0 0 2 1772.28 19.66
0 0 2 1825.03 29.97
0 0 3 -8.84 6.21
0 0 3 -0.40 2.42
0 0 3 4.89 8.77
0 0 4 117.15 16.46
0 0 4 116.78 6.95
0 0 5 -12.37 10.27
0 0 6 3707.10 96.27
0 0 7 3.51 6.63
0 0 7 -4.11 14.22
0 0 8 12.26 6.07
0 0 8 25.44 8.95
0 0 8 19.68 4.50
0 0 8 9.55 7.93
0 0 8 2.73 6.61
0 0 8 19.53 5.35
0 0 9 5.68 5.89
0 0 9 4.29 5.91
0 0 9 -16.28 6.88
0 0 9 -5.87 4.97
0 0 9 -7.45 6.80
0 0 9 -11.83 3.27
0 0 10 224.83 13.98
0 0 10 238.74 18.42
0 0 10 247.37 15.77
0 0 10 231.54 17.52
0 0 -11 10.12 5.42
0 0 11 -4.88 6.40
0 0 11 -10.37 6.36
0 0 11 -8.66 7.49
0 0 12 126.23 12.21
0 0 12 139.90 11.99
0 0 12 130.00 9.89
0 0 13 1.02 4.02
0 0 13 0.58 3.14
0 0 13 2.54 3.40
0 1 -1 48.42 3.74
0 -1 -1 49.49 2.95
0 1 1 45.63 4.25
0 -1 1 45.00 4.02
0 -1 1 40.82 4.08
0 1 1 50.21 3.00
0 1 2 107.22 8.79
0 -1 2 109.54 7.34
0 1 2 85.21 3.66
0 -1 2 104.80 8.48
0 1 -2 96.38 7.01
0 -1 3 3720.12 65.69
0 1 3 3880.24 67.42
0 1 3 3706.15 65.97
0 -1 3 4061.25 57.27
0 -1 3 3835.96 44.39
0 -1 4 1374.72 28.90
0 1 4 1480.65 48.92
0 -1 4 1327.75 38.87
0 -1 4 1424.16 47.16
0 -1 5 25.31 4.63
0 1 5 23.44 13.15
0 -1 5 27.02 11.89
0 1 6 281.04 30.26
0 -1 6 330.30 32.46
0 -1 7 85.25 20.25
0 1 7 67.44 17.71
0 -1 7 95.89 15.89
0 1 8 33.57 20.11
0 -1 8 51.69 11.91
0 -1 8 44.83 7.26
0 1 8 43.40 7.21
0 1 8 49.78 8.07
0 -1 8 41.04 5.91
0 1 8 33.70 8.46
0 1 8 41.48 10.47
0 -1 8 36.99 6.56
0 -1 8 34.07 8.19
0 1 8 34.69 7.86
0 -1 8 54.72 10.08
0 1 8 30.46 9.57
0 -1 8 29.47 18.16
0 1 8 33.80 7.11
0 -1 9 240.57 14.83
0 1 9 261.96 33.99
0 -1 9 242.10 17.70
0 1 9 193.33 19.30
0 1 9 271.07 29.90
0 -1 9 239.84 15.29
0 -1 9 217.33 25.88
0 1 9 207.74 18.21
0 1 9 242.36 15.57
0 -1 9 235.72 15.02
0 1 9 226.23 16.99
0 -1 9 217.86 16.43
0 1 9 241.74 17.91
0 -1 9 279.21 37.51
0 -1 -9 240.53 15.70
0 -1 10 497.99 24.67
0 -1 10 490.71 21.44
0 1 10 457.24 23.84
0 1 10 500.93 25.33
0 1 10 532.66 22.87
0 -1 10 487.35 24.89
0 -1 -10 523.59 23.09
0 -1 10 496.16 21.71
0 1 10 504.94 26.37
0 -1 11 33.60 8.21
0 -1 11 22.04 4.52
0 1 11 20.04 7.00
0 1 -11 18.23 6.47
0 -1 11 22.56 8.52
0 1 11 20.45 7.09
0 -1 11 34.64 7.40
0 1 11 34.29 8.78
0 -1 -11 35.03 5.49
0 -1 12 11.40 7.34
0 -1 12 11.84 5.69
0 1 12 13.67 7.75
0 1 12 18.79 5.88
0 1 -12 6.54 4.39
0 1 12 12.92 6.69
0 -1 12 19.41 7.80
0 -1 13 65.90 7.43
0 1 13 59.32 6.43
0 -1 13 66.41 7.07
0 1 13 78.57 7.74
0 -1 13 69.76 6.03
0 1 13 68.33 6.04
0 -2 0 5.14 2.21
0 2 0 5.50 1.30
0 -2 0 6.02 1.64
0 -2 0 5.73 3.65
0 -2 -1 322.34 10.83
0 -2 1 324.50 11.05
0 2 -1 290.78 9.96
0 -2 1 306.37 13.01
0 2 1 312.85 11.68
0 -2 1 318.55 9.32
0 2 1 313.41 12.68
0 -2 2 297.69 14.12
0 2 2 283.34 16.00
0 -2 2 301.71 13.88
0 -2 -2 277.43 9.18
0 2 2 290.89 14.05
0 2 -2 287.86 12.17
0 -2 3 988.80 29.48
0 -2 3 1018.79 27.56
0 2 3 1025.99 30.77
0 2 3 1046.78 36.79
0 -2 3 1026.71 35.85
0 2 3 982.29 34.92
0 -2 4 250.37 17.91
0 2 4 234.00 21.49
0 -2 4 224.35 21.93
0 2 4 221.78 21.13
0 -2 4 232.20 14.54
0 -2 5 59.05 8.22
0 -2 5 64.88 15.77
0 2 5 48.73 14.90
0 -2 5 38.04 10.35
0 2 6 172.64 23.05
0 -2 6 173.37 18.22
0 -2 6 160.64 22.57
0 2 7 3300.22 105.38
0 -2 7 3292.34 82.17
0 -2 7 3350.59 101.90
0 -2 8 -4.39 5.39
0 2 8 5.56 7.14
0 2 8 3.70 4.29
0 -2 8 7.51 3.93
0 2 8 17.23 11.32
0 2 8 1.99 4.72
0 -2 8 24.41 8.55
0 2 8 7.24 6.48
0 2 8 4.72 7.83
0 -2 8 11.15 5.01
0 -2 8 2.83 1.73
0 2 8 1.41 9.48
0 2 8 -8.45 3.37
0 -2 8 -11.56 12.81
0 -2 8 4.29 2.24
0 -2 9 447.16 20.41
0 -2 9 442.92 19.99
0 -2 9 452.61 23.51
0 -2 9 421.25 20.54
0 -2 9 446.74 37.11
0 2 9 502.54 27.47
0 -2 9 470.39 24.32
0 2 9 446.02 38.10
0 2 9 462.64 24.12
0 -2 9 443.10 44.91
0 2 9 484.34 22.03
0 2 9 544.30 30.11
0 2 9 476.73 25.85
0 -2 -9 489.15 22.67
0 2 9 420.43 45.24
0 2 9 444.38 23.00
0 2 10 39.34 9.66
0 -2 10 40.46 7.69
0 -2 -10 27.02 7.85
0 -2 10 36.27 5.79
0 2 10 26.93 12.05
0 2 10 30.66 8.70
0 2 10 29.09 9.01
0 -2 10 28.51 7.25
0 -2 10 33.92 7.56
0 -2 10 40.66 8.51
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0 2 -11 -1.85 4.15
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0 2 11 10.31 6.28
0 -2 -11 11.26 5.63
0 2 11 3.18 6.38
0 -2 11 -4.82 6.79
0 -2 11 2.75 4.85
0 2 -12 4.49 3.92
0 -2 -12 8.28 3.19
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0 2 12 0.38 4.48
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0 2 12 2.47 4.74
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0 -2 12 5.62 6.19
0 -2 13 490.82 15.92
0 2 13 451.02 14.45
0 2 13 481.86 14.23
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0 -3 0 1.15 2.30
0 -3 0 -0.07 4.67
0 -3 0 2.20 2.74
0 3 0 -0.04 3.48
0 3 1 2045.93 34.33
0 3 -1 2053.17 31.92
0 -3 1 1963.86 30.29
0 -3 1 2095.51 39.15
0 -3 1 2028.86 24.73
0 3 1 2042.22 35.97
0 -3 -1 2050.54 33.96
0 -3 -2 506.08 16.03
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0 -3 2 485.28 20.71
0 -3 2 493.86 18.52
0 3 -2 500.60 17.22
0 3 2 480.89 21.38
0 -3 2 484.88 16.07
0 -3 3 6535.41 69.90
0 -3 3 6484.92 78.94
0 3 3 6602.04 78.87
0 -3 3 6447.53 91.58
0 3 -3 6482.29 68.79
0 -3 3 6515.92 77.09
0 3 3 6687.67 90.93
0 3 3 6599.26 97.31
0 -3 4 1563.81 52.73
0 -3 4 1601.67 41.80
0 3 4 1570.35 53.96
0 -3 4 1637.45 45.28
0 -3 4 1636.09 40.84
0 3 4 1668.21 53.01
0 3 5 5.70 9.84
0 -3 5 13.95 6.19
0 3 5 3.27 9.08
0 -3 5 5.95 12.23
0 -3 5 2.32 5.06
0 -3 5 0.75 6.57
0 -3 6 828.94 47.61
0 3 6 832.48 49.50
0 -3 6 833.34 37.45
0 -3 7 167.07 19.45
0 3 7 219.73 29.67
0 -3 7 175.71 25.87
0 -3 8 8.80 4.83
0 3 8 -8.26 13.23
0 3 8 -0.42 2.06
0 3 8 -3.98 7.00
0 -3 8 12.12 5.28
0 -3 8 -27.09 13.04
0 -3 8 -6.87 4.48
0 -3 8 -0.12 5.50
0 3 8 8.57 10.56
0 -3 8 14.69 3.90
0 3 8 -2.45 4.66
0 3 8 -1.18 3.57
0 3 8 6.19 7.57
0 3 8 12.11 9.13
0 -3 8 2.35 4.02
0 -3 8 -3.52 4.67
0 3 9 292.25 19.68
0 -3 9 331.64 17.69
0 -3 9 301.64 18.58
0 -3 9 295.51 19.14
0 3 9 338.12 24.85
0 3 9 316.86 22.41
0 -3 9 310.12 19.79
0 -3 -9 309.38 18.86
0 3 9 301.52 40.67
0 3 9 321.08 18.13
0 -3 9 313.98 17.57
0 3 9 308.18 19.87
0 3 9 313.92 22.78
0 3 9 324.14 32.56
0 -3 9 304.20 30.15
0 -3 9 310.02 16.42
0 3 10 1458.19 40.93
0 3 10 1417.83 48.15
0 -3 10 1520.19 36.24
0 3 10 1504.28 45.63
0 3 10 1528.56 42.94
0 -3 10 1491.14 36.62
0 -3 -10 1510.34 40.27
0 -3 10 1474.29 37.90
0 -3 10 1518.60 42.27
0 -3 10 1421.24 33.12
0 3 10 1547.79 38.81
0 -3 10 1463.18 41.12
0 -3 11 31.16 7.24
0 -3 11 29.17 9.09
0 -3 11 48.44 9.27
0 3 -11 32.71 6.63
0 3 11 29.76 7.75
0 3 11 39.81 11.31
0 -3 11 29.18 7.01
0 -3 -11 31.05 8.00
0 3 11 36.78 8.35
0 3 11 40.62 8.56
0 3 12 102.04 9.55
0 -3 12 105.32 8.56
0 3 -12 88.93 9.46
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0 3 12 97.91 9.65
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0 3 13 65.04 6.75
0 3 13 62.74 5.67
0 -4 0 8428.03 50.32
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0 4 1 134.67 10.95
0 -4 -1 124.46 8.22
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0 4 1 139.22 11.60
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0 -4 1 142.64 12.99
0 -4 1 126.26 7.14
0 4 -2 22.56 5.63
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0 -4 -2 23.51 6.07
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0 -4 2 26.91 5.10
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0 -4 2 16.44 7.54
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0 -4 3 440.61 21.49
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0 -4 3 427.14 18.72
0 -4 3 415.02 22.92
0 -4 -3 411.52 16.31
0 4 3 454.05 29.01
0 -4 4 173.78 16.44
0 -4 4 206.74 17.44
0 4 4 182.31 19.40
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0 4 4 198.12 21.23
0 -4 5 10.24 6.33
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0 -4 6 1554.48 49.56
0 4 6 1607.43 71.11
0 -4 6 1504.61 51.23
0 -4 7 595.34 35.68
0 4 7 597.34 48.02
0 -4 8 93.47 10.74
0 4 8 76.64 9.46
0 4 8 102.91 18.58
0 -4 8 84.15 11.25
0 4 8 82.19 9.94
0 -4 8 96.64 17.15
0 4 8 93.53 21.35
0 4 8 69.76 12.12
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0 4 9 109.18 16.63
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0 -4 9 113.90 12.84
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0 4 10 168.59 13.96
0 -4 -10 171.33 15.08
0 -4 10 135.50 11.91
0 -4 10 163.84 15.18
0 4 10 176.47 17.62
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0 4 11 58.96 9.85
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0 4 -13 49.81 4.86
0 4 -13 38.84 3.96
0 -4 13 48.00 5.45
0 5 0 0.09 6.12
0 -5 0 3.55 7.48
0 5 0 -2.07 5.22
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0 -5 0 -0.62 3.18
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0 -5 1 5.44 4.38
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0 -5 -1 6.74 6.30
0 -5 1 1.39 2.27
0 5 1 -1.71 5.16
0 -5 2 140.04 9.35
0 -5 2 129.02 15.24
0 5 2 136.04 17.11
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0 -5 2 131.86 11.80
0 5 -2 140.12 11.85
0 5 2 141.05 12.97
0 -5 -2 140.59 12.63
0 5 3 2563.47 62.49
0 5 3 2631.23 55.66
0 5 3 2583.20 71.81
0 -5 -3 2634.30 47.25
0 -5 3 2623.87 54.46
0 -5 3 2640.15 62.16
0 5 -3 2787.39 52.61
0 -5 3 2603.71 46.70
0 5 4 271.88 20.28
0 -5 4 252.21 17.36
0 5 -4 262.59 16.72
0 5 4 284.93 27.47
0 5 4 241.21 22.97
0 -5 4 240.16 21.13
0 -5 4 255.56 20.13
0 -5 5 128.31 15.56
0 -5 5 143.64 16.16
0 -5 5 116.14 14.05
0 5 5 127.63 18.80
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0 -5 6 1.56 4.03
0 -5 6 10.57 6.77
0 -5 6 3.70 4.82
0 -5 7 4.86 3.06
0 -5 7 21.30 7.76
0 5 7 10.79 5.95
0 -5 7 12.89 5.04
0 -5 7 1.09 1.70
0 5 7 18.97 16.93
0 -5 7 12.68 4.91
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10 -1 -4 222.89 12.62
10 1 -4 219.48 13.04
10 -1 -4 212.86 12.88
10 1 -4 210.40 13.63
10 -1 -3 10.95 5.27
10 1 -3 8.43 5.50
10 -1 -3 9.52 8.23
10 -1 -3 10.48 5.60
10 1 -3 8.73 5.04
10 1 -3 7.10 2.53
10 -1 -2 5.54 6.00
10 1 -2 6.82 6.49
10 -1 -2 7.96 9.53
10 -1 -2 -2.18 4.23
10 1 -2 -0.23 5.26
10 -1 -2 3.75 5.08
10 1 -2 5.81 3.12
10 -1 -1 23.24 6.26
10 1 -1 21.48 7.75
10 -1 -1 23.87 5.97
10 1 -1 13.92 5.64
10 -1 -1 22.24 5.70
10 1 -1 21.25 5.80
10 -1 -1 20.69 3.84
10 1 -1 24.05 5.27
10 -1 0 283.27 13.89
10 1 0 282.67 13.49
10 -1 0 279.42 12.14
10 1 0 283.49 13.03
10 -1 0 287.24 12.71
10 1 0 275.95 11.94
10 -1 0 295.74 12.46
10 1 1 73.96 6.71
10 -1 1 67.52 6.18
10 1 1 61.60 6.67
10 -1 1 63.95 5.57
10 -1 1 61.31 6.46
10 1 1 64.18 6.67
10 -1 2 5.95 2.55
10 1 2 3.64 3.13
10 -1 2 6.76 3.10
10 1 2 1.79 3.47
10 -1 3 268.80 8.96
10 1 3 259.04 9.38
10 -1 3 254.28 9.21
10 1 3 266.76 9.85
10 2 -8 -3.97 2.38
10 -2 -8 -1.00 2.35
10 -2 -7 225.75 10.51
10 2 -7 239.43 10.36
10 2 -7 227.96 11.08
10 -2 -6 1.94 2.41
10 2 -6 4.52 3.83
10 -2 -6 11.23 5.44
10 -2 -6 7.25 4.24
10 -2 -6 2.82 2.47
10 2 -6 5.99 3.62
10 -2 -6 8.72 3.96
10 -2 -5 24.04 5.11
10 2 -5 25.16 5.76
10 -2 -5 28.03 8.19
10 -2 -5 23.56 4.20
10 2 -5 27.36 5.28
10 -2 -5 24.90 5.30
10 -2 -4 4.31 3.76
10 2 -4 3.59 4.79
10 -2 -4 8.87 8.13
10 -2 -4 5.76 3.98
10 2 -4 5.07 5.27
10 -2 -4 5.28 3.93
10 2 -4 4.10 1.59
10 -2 -3 547.31 26.56
10 -2 -3 611.01 19.85
10 2 -3 590.34 20.29
10 2 -3 613.04 18.13
10 -2 -3 597.69 19.78
10 -2 -3 591.79 20.93
10 2 -3 561.96 21.49
10 -2 -2 3.96 5.26
10 2 -2 -8.46 6.15
10 -2 -2 6.97 7.64
10 -2 -2 0.65 4.69
10 2 -2 6.27 5.29
10 -2 -2 4.74 5.07
10 2 -2 -0.36 3.68
10 -2 -1 270.74 13.63
10 2 -1 258.28 13.43
10 2 -1 247.39 12.58
10 -2 -1 244.85 12.90
10 2 -1 242.79 12.00
10 2 -1 242.71 14.37
10 2 0 10.49 4.43
10 -2 0 16.71 5.02
10 2 0 9.71 4.98
10 -2 0 12.46 4.39
10 2 0 14.93 3.78
10 -2 0 5.80 1.56
10 2 0 15.87 4.24
10 -2 0 2.45 2.03
10 2 1 4.33 3.88
10 2 1 13.00 4.37
10 -2 1 13.28 3.61
10 -2 1 12.04 2.77
10 2 1 14.55 4.12
10 -2 1 14.20 3.65
10 -2 2 10.91 2.65
10 2 2 11.15 3.87
10 -2 2 8.17 2.60
10 2 2 9.30 3.34
10 2 3 428.97 11.68
10 2 3 396.51 11.57
10 3 -8 7.31 2.32
10 -3 -7 129.87 7.52
10 3 -7 137.10 7.66
10 3 -7 150.16 9.02
10 -3 -6 278.59 15.25
10 3 -6 302.50 12.72
10 -3 -6 274.02 10.73
10 3 -6 297.63 13.87
10 -3 -5 4.47 1.99
10 3 -5 3.48 5.67
10 -3 -5 0.46 7.02
10 -3 -5 -2.85 2.35
10 3 -5 -2.31 4.18
10 -3 -5 2.82 2.73
10 -3 -4 293.09 18.53
10 -3 -4 328.44 13.51
10 3 -4 349.98 15.51
10 3 -4 335.41 12.36
10 -3 -4 300.37 13.61
10 -3 -4 324.46 14.22
10 3 -4 316.09 15.97
10 -3 -3 19.88 4.65
10 3 -3 19.93 6.50
10 -3 -3 19.95 9.25
10 3 -3 7.82 4.46
10 -3 -3 24.57 5.27
10 3 -3 27.91 6.60
10 -3 -3 12.16 5.01
10 3 -3 16.37 4.25
10 3 -2 5.10 5.88
10 -3 -2 4.73 8.30
10 3 -2 5.27 5.36
10 -3 -2 2.81 4.43
10 3 -2 5.18 5.41
10 -3 -2 6.88 5.33
10 3 -2 -0.84 3.35
10 -3 -1 93.72 11.31
10 -3 -1 104.35 8.71
10 3 -1 99.31 8.50
10 3 -1 104.77 9.56
10 3 -1 109.89 8.76
10 -3 -1 93.92 8.36
10 3 -1 101.17 7.73
10 3 -1 102.58 9.66
10 -3 0 411.39 15.30
10 3 0 422.28 14.74
10 3 0 370.10 15.70
10 3 0 398.45 15.40
10 -3 0 401.34 14.48
10 3 0 360.29 11.51
10 3 1 0.15 4.33
10 -3 1 -3.07 2.60
10 -3 1 0.94 1.38
10 -3 1 -2.55 0.98
10 3 2 67.12 5.87
10 -3 2 54.63 4.57
10 3 2 57.72 5.39
10 -4 -7 83.12 7.37
10 4 -7 99.52 6.66
10 4 -7 101.41 7.29
10 4 -6 7.44 3.65
10 -4 -6 7.58 5.50
10 4 -6 7.19 3.85
10 -4 -6 6.02 1.36
10 4 -5 13.45 5.10
10 -4 -5 7.48 6.83
10 -4 -5 8.93 2.56
10 4 -5 10.61 4.80
10 -4 -5 9.38 3.52
10 4 -5 2.31 1.77
10 -4 -4 150.58 14.15
10 -4 -4 188.19 9.36
10 4 -4 166.33 10.51
10 4 -4 158.96 9.04
10 -4 -4 164.72 10.10
10 4 -4 161.73 10.98
10 -4 -3 48.43 10.80
10 -4 -3 62.68 6.07
10 4 -3 56.36 7.26
10 4 -3 52.62 7.29
10 4 -3 56.42 6.11
10 -4 -3 53.02 6.61
10 4 -3 67.99 8.50
10 4 -2 36.94 6.59
10 -4 -2 30.95 9.34
10 4 -2 45.61 6.63
10 4 -2 25.39 5.73
10 -4 -2 38.90 5.53
10 4 -2 45.93 6.25
10 -4 -2 39.74 6.31
10 -4 -1 44.73 9.43
10 -4 -1 56.63 6.49
10 4 -1 66.93 6.74
10 4 -1 46.34 7.69
10 4 -1 53.54 6.65
10 -4 -1 57.93 6.86
10 4 -1 51.18 5.34
10 4 -1 57.83 7.26
10 4 0 176.61 8.70
10 4 0 174.02 11.48
10 4 0 180.35 10.30
10 -4 0 174.56 9.53
10 4 1 25.96 5.40
10 -4 1 14.84 3.43
10 4 1 27.01 4.60
10 -4 2 8.57 2.15
10 4 2 13.42 3.78
10 4 2 4.21 3.29
10 5 -7 403.01 11.44
10 5 -7 418.42 12.30
10 5 -6 19.17 4.66
10 -5 -6 23.75 5.78
10 5 -6 21.65 4.16
10 5 -5 -2.72 3.82
10 -5 -5 7.67 5.54
10 5 -5 -5.66 4.14
10 5 -5 0.35 3.69
10 -5 -5 -0.64 1.92
10 5 -5 -3.90 1.59
10 5 -4 6.11 4.43
10 -5 -4 3.68 6.45
10 5 -4 -2.45 4.81
10 -5 -4 -0.40 1.30
10 5 -4 0.64 3.85
10 -5 -4 0.84 3.08
10 5 -4 3.73 2.47
10 -5 -3 81.36 10.95
10 -5 -3 88.03 6.54
10 5 -3 89.05 7.27
10 5 -3 83.98 8.53
10 5 -3 90.94 7.39
10 -5 -3 85.15 7.21
10 5 -3 93.67 8.19
10 -5 -2 51.81 8.98
10 5 -2 59.85 6.23
10 5 -2 64.52 8.45
10 5 -2 48.85 6.22
10 -5 -2 63.25 6.95
10 5 -2 65.72 7.31
10 5 -1 24.89 6.27
10 5 -1 27.84 4.28
10 -5 -1 36.74 5.50
10 5 -1 25.73 3.56
10 5 -1 30.77 5.49
10 5 0 40.36 6.88
10 -5 0 40.05 5.14
10 5 0 38.47 5.08
10 5 1 71.52 7.00
10 5 1 89.06 6.89
10 -5 1 82.53 5.72
10 5 2 15.56 3.15
10 5 2 14.87 2.94
10 6 -6 0.69 1.48
10 -6 -6 5.92 3.80
10 6 -6 -0.53 2.36
10 -6 -5 89.05 9.01
10 6 -5 83.18 6.32
10 6 -5 80.32 6.61
10 6 -5 69.04 4.65
10 6 -5 82.38 6.52
10 6 -4 -1.52 3.34
10 -6 -4 -3.10 5.02
10 6 -4 2.03 4.23
10 6 -4 0.86 2.78
10 -6 -4 0.54 2.03
10 6 -4 3.24 1.30
10 -6 -3 212.74 13.41
10 6 -3 215.75 9.65
10 6 -3 213.67 12.31
10 6 -3 221.13 10.30
10 -6 -3 229.73 9.98
10 6 -3 207.89 10.06
10 6 -2 32.54 4.79
10 -6 -2 28.26 6.45
10 6 -2 35.50 6.50
10 6 -2 33.13 4.24
10 -6 -2 38.54 4.76
10 6 -2 37.99 5.11
10 6 -1 135.74 10.08
10 6 -1 126.31 8.11
10 -6 -1 147.48 8.09
10 6 0 40.69 6.09
10 6 0 51.98 5.14
10 -6 0 52.21 5.09
10 6 1 45.25 5.32
10 6 1 46.45 4.78
10 -6 1 44.18 3.97
10 -7 -5 -5.05 3.56
10 -7 -4 295.87 13.36
10 7 -4 300.76 12.12
10 7 -4 315.77 10.49
10 -7 -3 9.14 4.29
10 7 -3 6.18 3.97
10 -7 -3 -1.54 1.94
10 7 -3 2.92 2.01
10 -7 -2 4.02 3.35
10 7 -2 -2.35 4.05
10 -7 -2 2.17 1.88
10 7 -2 -0.17 2.05
10 7 -1 73.45 7.19
10 7 -1 88.68 6.50
10 -7 -1 80.93 5.71
10 7 0 191.50 9.64
10 -7 0 187.24 7.58
10 8 -3 184.11 7.57
10 8 -2 1.55 3.67
10 8 -2 1.94 1.60
11 0 -4 0.90 1.33
11 0 -4 1.58 1.72
11 0 -3 10.99 2.39
11 0 -3 7.98 2.56
11 0 -2 -3.63 2.48
11 0 -2 -1.44 1.89
11 1 -4 21.47 3.14
11 1 -4 20.43 3.20
11 -1 -4 19.94 2.78
11 1 -4 17.33 2.83
11 -1 -3 130.87 6.31
11 1 -3 123.77 6.52
11 -1 -3 133.73 6.45
11 1 -3 130.94 6.43
11 -1 -2 256.45 8.87
11 1 -2 250.90 8.79
11 2 -3 1.15 2.08
11 -2 -3 3.21 1.68
0 0 0 0.00 0.00
TITL kee24 in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 1.54184 8.789729 14.893684 11.129405 90.0000 101.7421 90.0000
ZERR 4.00 0.000137 0.000277 0.000187 0.0000 0.0016 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N Br
UNIT 44.00 88.00 16.00 8.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 87887
_shelx_res_file
;
TITL kee24_a.res in P2(1)/n
kee24.res
created by SHELXL-2018/3 at 14:29:49 on 01-Jul-2020
REM Old TITL kee24 in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.105, Rweak 0.042, Alpha 0.017
REM 0.474 for 125 systematic absences, Orientation as input
REM Formula found by SHELXT: C12 N3 Br2
CELL 1.54184 8.7897 14.8937 11.1294 90 101.742 90
ZERR 4 0.0002 0.0003 0.0002 0 0.002 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Br N
UNIT 44 88 8 16
L.S. 10
PLAN 5
SIZE 0.048 0.06 0.081
TEMP -173
CONF
BOND
list 4
fmap 2
acta
MORE -1
BOND $H
REM
REM
REM
WGHT 0.025300 1.786100
FVAR 0.45620
BR17 3 0.262073 0.119596 0.166584 11.00000 0.02347 0.02523 =
0.02747 -0.00790 0.00593 -0.00279
BR1 3 0.834011 0.600493 0.025663 11.00000 0.02808 0.04267 =
0.03123 0.00965 0.00409 -0.00985
N14 4 0.048396 0.326896 0.356990 11.00000 0.01764 0.02372 =
0.02443 0.00006 0.00378 -0.00135
N9 4 0.181725 0.392616 0.550949 11.00000 0.02136 0.02155 =
0.02052 -0.00006 0.00596 0.00160
N7 4 0.332008 0.326446 0.411478 11.00000 0.01693 0.01729 =
0.02132 -0.00054 0.00388 0.00073
N11 4 0.180713 0.230443 0.522730 11.00000 0.02571 0.01933 =
0.02639 0.00135 0.00921 -0.00078
C13 1 0.187544 0.335031 0.307588 11.00000 0.01690 0.02370 =
0.01972 -0.00017 0.00179 -0.00025
AFIX 23
H13A 2 0.188486 0.393964 0.266600 11.00000 -1.20000
H13B 2 0.189079 0.287431 0.245757 11.00000 -1.20000
AFIX 0
C8 1 0.323295 0.400580 0.504918 11.00000 0.02118 0.01674 =
0.02201 -0.00262 0.00452 -0.00048
AFIX 23
H8A 2 0.413960 0.396114 0.573916 11.00000 -1.20000
H8B 2 0.326628 0.459996 0.465655 11.00000 -1.20000
AFIX 0
C12 1 0.322199 0.236544 0.476063 11.00000 0.02331 0.01671 =
0.02692 0.00130 0.00618 0.00192
AFIX 23
H12A 2 0.325576 0.186875 0.417548 11.00000 -1.20000
H12B 2 0.412836 0.230205 0.544750 11.00000 -1.20000
AFIX 0
C4 1 0.658534 0.420727 0.263111 11.00000 0.01909 0.02306 =
0.02682 -0.00243 0.00635 0.00026
AFIX 23
H4A 2 0.723264 0.440004 0.342377 11.00000 -1.20000
H4B 2 0.700757 0.363271 0.239322 11.00000 -1.20000
AFIX 0
C3 1 0.666101 0.491421 0.165607 11.00000 0.02176 0.02739 =
0.02640 0.00110 0.00604 -0.00188
AFIX 23
H3A 2 0.601900 0.471674 0.086368 11.00000 -1.20000
H3B 2 0.622209 0.548478 0.189060 11.00000 -1.20000
AFIX 0
C6 1 0.480705 0.329391 0.364983 11.00000 0.01784 0.02329 =
0.02476 -0.00233 0.00688 0.00099
AFIX 23
H6A 2 0.491918 0.272273 0.322120 11.00000 -1.20000
H6B 2 0.568745 0.333678 0.436101 11.00000 -1.20000
AFIX 0
C2 1 0.831237 0.507357 0.149935 11.00000 0.02477 0.02929 =
0.02637 0.00369 0.00628 -0.00193
AFIX 23
H2A 2 0.874916 0.450893 0.124359 11.00000 -1.20000
H2B 2 0.896396 0.526437 0.229127 11.00000 -1.20000
AFIX 0
C16 1 0.047769 0.239657 0.419211 11.00000 0.02325 0.02457 =
0.03080 -0.00149 0.00622 -0.00669
AFIX 23
H16A 2 -0.049980 0.233470 0.449665 11.00000 -1.20000
H16B 2 0.051124 0.190783 0.359514 11.00000 -1.20000
AFIX 0
C5 1 0.491464 0.406882 0.278003 11.00000 0.01850 0.02728 =
0.02664 0.00191 0.00500 -0.00092
AFIX 23
H5A 2 0.453165 0.462523 0.310466 11.00000 -1.20000
H5B 2 0.424587 0.394188 0.196898 11.00000 -1.20000
AFIX 0
C15 1 0.046748 0.398876 0.447310 11.00000 0.01993 0.02387 =
0.02503 0.00119 0.00542 0.00486
AFIX 23
H15A 2 -0.050356 0.394968 0.479113 11.00000 -1.20000
H15B 2 0.048158 0.457856 0.406527 11.00000 -1.20000
AFIX 0
C10 1 0.176269 0.304392 0.609530 11.00000 0.02687 0.02239 =
0.02296 0.00211 0.00768 0.00121
AFIX 23
H10A 2 0.265689 0.298837 0.679369 11.00000 -1.20000
H10B 2 0.079868 0.299928 0.642209 11.00000 -1.20000
AFIX 0
HKLF 4
REM kee24_a.res in P2(1)/n
REM wR2 = 0.0625, GooF = S = 1.038, Restrained GooF = 1.038 for all data
REM R1 = 0.0254 for 2652 Fo > 4sig(Fo) and 0.0310 for all 2992 data
REM 154 parameters refined using 0 restraints
END
WGHT 0.0253 1.7862
REM Highest difference peak 0.532, deepest hole -0.641, 1-sigma level 0.076
Q1 1 0.2265 0.1568 0.1257 11.00000 0.05 0.53
Q2 1 0.0471 0.2856 0.3839 11.00000 0.05 0.34
Q3 1 -0.0124 0.3333 0.3215 11.00000 0.05 0.31
Q4 1 0.7434 0.5045 0.1569 11.00000 0.05 0.30
Q5 1 0.3145 0.1209 0.0614 11.00000 0.05 0.30
;
_shelx_res_checksum 6349
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 Br17 0.26207(3) 0.11960(2) 0.16658(2) 0.02528(8) Uani d 1 . .
Br Br1 0.83401(3) 0.60049(2) 0.02566(3) 0.03427(9) Uani d 1 . .
N N14 0.0484(2) 0.32690(14) 0.35699(18) 0.0220(4) Uani d 1 . .
N N9 0.1817(2) 0.39262(14) 0.55095(18) 0.0209(4) Uani d 1 . .
N N7 0.3320(2) 0.32645(13) 0.41148(17) 0.0185(4) Uani d 1 . .
N N11 0.1807(2) 0.23044(14) 0.52273(19) 0.0233(4) Uani d 1 . .
C C13 0.1875(3) 0.33503(16) 0.3076(2) 0.0204(4) Uani d 1 . .
H H13A 0.188486 0.393964 0.266600 0.024 Uiso calc 1 . .
H H13B 0.189079 0.287431 0.245757 0.024 Uiso calc 1 . .
C C8 0.3233(3) 0.40058(15) 0.5049(2) 0.0200(4) Uani d 1 . .
H H8A 0.413960 0.396114 0.573916 0.024 Uiso calc 1 . .
H H8B 0.326628 0.459996 0.465655 0.024 Uiso calc 1 . .
C C12 0.3222(3) 0.23654(16) 0.4761(2) 0.0222(5) Uani d 1 . .
H H12A 0.325576 0.186875 0.417548 0.027 Uiso calc 1 . .
H H12B 0.412836 0.230205 0.544750 0.027 Uiso calc 1 . .
C C4 0.6585(3) 0.42073(17) 0.2631(2) 0.0228(5) Uani d 1 . .
H H4A 0.723264 0.440004 0.342377 0.027 Uiso calc 1 . .
H H4B 0.700757 0.363271 0.239322 0.027 Uiso calc 1 . .
C C3 0.6661(3) 0.49142(17) 0.1656(2) 0.0250(5) Uani d 1 . .
H H3A 0.601900 0.471674 0.086368 0.030 Uiso calc 1 . .
H H3B 0.622209 0.548478 0.189060 0.030 Uiso calc 1 . .
C C6 0.4807(3) 0.32939(16) 0.3650(2) 0.0216(5) Uani d 1 . .
H H6A 0.491918 0.272273 0.322120 0.026 Uiso calc 1 . .
H H6B 0.568745 0.333678 0.436101 0.026 Uiso calc 1 . .
C C2 0.8312(3) 0.50736(18) 0.1499(2) 0.0267(5) Uani d 1 . .
H H2A 0.874916 0.450893 0.124359 0.032 Uiso calc 1 . .
H H2B 0.896396 0.526437 0.229127 0.032 Uiso calc 1 . .
C C16 0.0478(3) 0.23966(17) 0.4192(2) 0.0261(5) Uani d 1 . .
H H16A -0.049980 0.233470 0.449665 0.031 Uiso calc 1 . .
H H16B 0.051124 0.190783 0.359514 0.031 Uiso calc 1 . .
C C5 0.4915(3) 0.40688(17) 0.2780(2) 0.0241(5) Uani d 1 . .
H H5A 0.453165 0.462523 0.310466 0.029 Uiso calc 1 . .
H H5B 0.424587 0.394188 0.196898 0.029 Uiso calc 1 . .
C C15 0.0467(3) 0.39888(16) 0.4473(2) 0.0228(5) Uani d 1 . .
H H15A -0.050356 0.394968 0.479113 0.027 Uiso calc 1 . .
H H15B 0.048158 0.457856 0.406527 0.027 Uiso calc 1 . .
C C10 0.1763(3) 0.30439(16) 0.6095(2) 0.0237(5) Uani d 1 . .
H H10A 0.265689 0.298837 0.679369 0.028 Uiso calc 1 . .
H H10B 0.079868 0.299928 0.642209 0.028 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
Br17 0.02347(13) 0.02523(14) 0.02747(13) -0.00279(9) 0.00593(9) -0.00790(9)
Br1 0.02808(14) 0.04267(18) 0.03123(15) -0.00985(11) 0.00409(11) 0.00965(11)
N14 0.0176(9) 0.0237(11) 0.0244(10) -0.0014(7) 0.0038(7) 0.0001(8)
N9 0.0214(9) 0.0215(10) 0.0205(9) 0.0016(7) 0.0060(7) -0.0001(7)
N7 0.0169(9) 0.0173(9) 0.0213(9) 0.0007(7) 0.0039(7) -0.0005(7)
N11 0.0257(10) 0.0193(10) 0.0264(10) -0.0008(8) 0.0092(8) 0.0013(8)
C13 0.0169(10) 0.0237(12) 0.0197(10) -0.0002(8) 0.0018(8) -0.0002(9)
C8 0.0212(11) 0.0167(11) 0.0220(10) -0.0005(8) 0.0045(8) -0.0026(8)
C12 0.0233(11) 0.0167(11) 0.0269(12) 0.0019(8) 0.0062(9) 0.0013(9)
C4 0.0191(11) 0.0231(12) 0.0268(11) 0.0003(9) 0.0063(9) -0.0024(9)
C3 0.0218(11) 0.0274(13) 0.0264(12) -0.0019(9) 0.0060(9) 0.0011(10)
C6 0.0178(10) 0.0233(12) 0.0248(11) 0.0010(8) 0.0069(8) -0.0023(9)
C2 0.0248(12) 0.0293(13) 0.0264(12) -0.0019(10) 0.0063(9) 0.0037(10)
C16 0.0233(12) 0.0246(13) 0.0308(13) -0.0067(9) 0.0062(10) -0.0015(10)
C5 0.0185(11) 0.0273(13) 0.0266(12) -0.0009(9) 0.0050(9) 0.0019(9)
C15 0.0199(11) 0.0239(12) 0.0250(11) 0.0049(9) 0.0054(9) 0.0012(9)
C10 0.0269(12) 0.0224(12) 0.0230(11) 0.0012(9) 0.0077(9) 0.0021(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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
-3 -3 -5 0.0262
-1 -6 6 0.0210
1 0 -1 0.0219
3 -7 3 0.0323
-2 -8 4 0.0348
-3 8 -2 0.0228
3 -8 -2 0.0426
-4 -4 5 0.0270
-3 8 3 0.0198
-3 1 7 0.0248
2 5 5 0.0290
-5 2 5 0.0220
-4 -3 -3 0.0230
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
C13 N14 C16 . . 109.72(19) ?
C13 N14 C15 . . 109.01(18) ?
C15 N14 C16 . . 108.66(19) ?
C8 N9 C15 . . 109.30(18) ?
C8 N9 C10 . . 109.79(18) ?
C10 N9 C15 . . 107.96(19) ?
C8 N7 C13 . . 107.64(17) ?
C8 N7 C12 . . 107.27(17) ?
C12 N7 C13 . . 107.99(17) ?
C6 N7 C13 . . 112.44(17) ?
C6 N7 C8 . . 112.39(17) ?
C6 N7 C12 . . 108.89(17) ?
C12 N11 C16 . . 108.50(19) ?
C12 N11 C10 . . 109.20(19) ?
C10 N11 C16 . . 108.76(19) ?
N14 C13 N7 . . 109.89(18) ?
N14 C13 H13A . . 109.7 ?
N14 C13 H13B . . 109.7 ?
N7 C13 H13A . . 109.7 ?
N7 C13 H13B . . 109.7 ?
H13A C13 H13B . . 108.2 ?
N9 C8 N7 . . 110.37(18) ?
N9 C8 H8A . . 109.6 ?
N9 C8 H8B . . 109.6 ?
N7 C8 H8A . . 109.6 ?
N7 C8 H8B . . 109.6 ?
H8A C8 H8B . . 108.1 ?
N7 C12 H12A . . 109.4 ?
N7 C12 H12B . . 109.4 ?
N11 C12 N7 . . 111.02(18) ?
N11 C12 H12A . . 109.4 ?
N11 C12 H12B . . 109.4 ?
H12A C12 H12B . . 108.0 ?
H4A C4 H4B . . 108.1 ?
C3 C4 H4A . . 109.5 ?
C3 C4 H4B . . 109.5 ?
C3 C4 C5 . . 110.7(2) ?
C5 C4 H4A . . 109.5 ?
C5 C4 H4B . . 109.5 ?
C4 C3 H3A . . 109.2 ?
C4 C3 H3B . . 109.2 ?
H3A C3 H3B . . 107.9 ?
C2 C3 C4 . . 111.8(2) ?
C2 C3 H3A . . 109.2 ?
C2 C3 H3B . . 109.2 ?
N7 C6 H6A . . 108.7 ?
N7 C6 H6B . . 108.7 ?
N7 C6 C5 . . 114.37(19) ?
H6A C6 H6B . . 107.6 ?
C5 C6 H6A . . 108.7 ?
C5 C6 H6B . . 108.7 ?
Br1 C2 H2A . . 109.7 ?
Br1 C2 H2B . . 109.7 ?
C3 C2 Br1 . . 109.96(17) ?
C3 C2 H2A . . 109.7 ?
C3 C2 H2B . . 109.7 ?
H2A C2 H2B . . 108.2 ?
N14 C16 H16A . . 109.2 ?
N14 C16 H16B . . 109.2 ?
N11 C16 N14 . . 111.85(19) ?
N11 C16 H16A . . 109.2 ?
N11 C16 H16B . . 109.2 ?
H16A C16 H16B . . 107.9 ?
C4 C5 H5A . . 109.4 ?
C4 C5 H5B . . 109.4 ?
C6 C5 C4 . . 111.0(2) ?
C6 C5 H5A . . 109.4 ?
C6 C5 H5B . . 109.4 ?
H5A C5 H5B . . 108.0 ?
N14 C15 N9 . . 111.64(19) ?
N14 C15 H15A . . 109.3 ?
N14 C15 H15B . . 109.3 ?
N9 C15 H15A . . 109.3 ?
N9 C15 H15B . . 109.3 ?
H15A C15 H15B . . 108.0 ?
N9 C10 H10A . . 109.3 ?
N9 C10 H10B . . 109.3 ?
N11 C10 N9 . . 111.71(19) ?
N11 C10 H10A . . 109.3 ?
N11 C10 H10B . . 109.3 ?
H10A C10 H10B . . 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 C2 . 1.962(3) ?
N14 C13 . 1.444(3) ?
N14 C16 . 1.473(3) ?
N14 C15 . 1.472(3) ?
N9 C8 . 1.444(3) ?
N9 C15 . 1.480(3) ?
N9 C10 . 1.472(3) ?
N7 C13 . 1.539(3) ?
N7 C8 . 1.529(3) ?
N7 C12 . 1.530(3) ?
N7 C6 . 1.501(3) ?
N11 C12 . 1.445(3) ?
N11 C16 . 1.471(3) ?
N11 C10 . 1.471(3) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C4 C3 . 1.523(3) ?
C4 C5 . 1.525(3) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C3 C2 . 1.515(3) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C6 C5 . 1.522(3) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C15 H15A . 0.9900 ?
C15 H15B . 0.9900 ?
C10 H10A . 0.9900 ?
C10 H10B . 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_D
_geom_hbond_site_symmetry_H
_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
C12 H12A Br17 . . . 0.99 2.91 3.800(2) 150 y
C13 H13B Br17 . . . 0.99 2.77 3.689(2) 155 y
C15 H15A Br17 . . 4_566 0.99 2.92 3.844(3) 156 y
C8 H8B Br17 . . 2_555 0.99 2.82 3.777(2) 162 y
C6 H6B Br17 . . 4_666 0.99 2.86 3.819(2) 163 y
C5 H5B Br1 . . 3_665 0.99 3.00 3.960(3) 163 y
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
N7 C6 C5 C4 . . . . 164.35(19) ?
C13 N14 C16 N11 . . . . 61.4(3) ?
C13 N14 C15 N9 . . . . -61.1(2) ?
C13 N7 C8 N9 . . . . 58.2(2) ?
C13 N7 C12 N11 . . . . -57.7(2) ?
C13 N7 C6 C5 . . . . 49.2(3) ?
C8 N9 C15 N14 . . . . 60.4(2) ?
C8 N9 C10 N11 . . . . -60.0(2) ?
C8 N7 C13 N14 . . . . -58.8(2) ?
C8 N7 C12 N11 . . . . 58.1(2) ?
C8 N7 C6 C5 . . . . -72.4(2) ?
C12 N7 C13 N14 . . . . 56.8(2) ?
C12 N7 C8 N9 . . . . -57.8(2) ?
C12 N7 C6 C5 . . . . 168.85(19) ?
C12 N11 C16 N14 . . . . -60.9(3) ?
C12 N11 C10 N9 . . . . 59.5(2) ?
C4 C3 C2 Br1 . . . . -178.93(17) ?
C3 C4 C5 C6 . . . . 173.8(2) ?
C6 N7 C13 N14 . . . . 176.92(19) ?
C6 N7 C8 N9 . . . . -177.46(18) ?
C6 N7 C12 N11 . . . . 179.94(19) ?
C16 N14 C13 N7 . . . . -58.7(2) ?
C16 N14 C15 N9 . . . . 58.4(2) ?
C16 N11 C12 N7 . . . . 59.3(2) ?
C16 N11 C10 N9 . . . . -58.7(2) ?
C5 C4 C3 C2 . . . . 179.3(2) ?
C15 N14 C13 N7 . . . . 60.2(2) ?
C15 N14 C16 N11 . . . . -57.7(2) ?
C15 N9 C8 N7 . . . . -58.9(2) ?
C15 N9 C10 N11 . . . . 59.0(2) ?
C10 N9 C8 N7 . . . . 59.3(2) ?
C10 N9 C15 N14 . . . . -59.0(2) ?
C10 N11 C12 N7 . . . . -59.1(2) ?
C10 N11 C16 N14 . . . . 57.8(2) ?
_cod_database_fobs_code 2022294