#------------------------------------------------------------------------------
#$Date: 2025-02-08 05:10:10 +0200 (Sat, 08 Feb 2025) $
#$Revision: 297642 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573866.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_1573866
loop_
_publ_author_name
'Albert, Daniel R.'
'Gau, Michael'
'Rajaseelan, Edward'
_publ_section_title
;
4-(4-tert-Butylbenzyl)-1-neopentyl-1,2,4-triazolium bromide
;
_journal_coeditor_code HB4505
_journal_issue 2
_journal_name_full IUCrData
_journal_paper_doi 10.1107/S2414314625000926
_journal_volume 10
_journal_year 2025
_chemical_formula_iupac 'C18 H28 N3 +, Br -'
_chemical_formula_moiety 'C18 H28 N3 +, Br -'
_chemical_formula_sum 'C18 H28 Br N3'
_chemical_formula_weight 366.34
_chemical_name_systematic
;
4-(4-tert-Butylbenzyl)-1-neopentyl-1,2,4-triazolium bromide
;
_space_group_crystal_system monoclinic
_space_group_IT_number 7
_space_group_name_Hall 'P -2yc'
_space_group_name_H-M_alt 'P 1 c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha 90
_cell_angle_beta 90.4350(10)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 14.9741(2)
_cell_length_b 6.38420(10)
_cell_length_c 10.07410(10)
_cell_measurement_reflns_used 11602
_cell_measurement_temperature 100
_cell_measurement_theta_max 74.3920
_cell_measurement_theta_min 2.9120
_cell_volume 963.03(2)
_computing_cell_refinement
;
CrysAlisPro 1.171.43.134a (Rigaku OD, 2024)
;
_computing_data_collection
;
CrysAlisPro 1.171.43.134a (Rigaku OD, 2024)
;
_computing_data_reduction
;
CrysAlisPro 1.171.43.134a (Rigaku OD, 2024)
;
_computing_molecular_graphics
;
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_publication_material
;
PublCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device '\k-geometry diffractometer'
_diffrn_measurement_device_type 'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0665
_diffrn_reflns_av_unetI/netI 0.0437
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 14617
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 74.473
_diffrn_reflns_theta_min 2.951
_exptl_absorpt_coefficient_mu 2.898
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.67545
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
[SCALE3 ABSPACK in CrysAlis PRO (Rigaku OD, 2024)]
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.263
_exptl_crystal_description needle
_exptl_crystal_F_000 384
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.01
_refine_diff_density_max 0.766
_refine_diff_density_min -0.869
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack 0.31(4)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.147
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 206
_refine_ls_number_reflns 3683
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.147
_refine_ls_R_factor_all 0.0454
_refine_ls_R_factor_gt 0.0428
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0959P)^2^+0.2583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1149
_refine_ls_wR_factor_ref 0.1354
_reflns_number_gt 3564
_reflns_number_total 3683
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb4505.cif
_cod_data_source_block I
_cod_database_code 1573866
_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_hkl_file
;
-18 0 -3 1.17 2.09
-18 0 -2 87.92 6.30
-18 0 -2 90.63 6.38
-18 0 -1 1.09 2.97
-18 0 -1 -0.14 2.79
-18 0 0 42.96 5.03
-18 0 0 31.81 4.48
-18 0 1 -0.72 3.35
-18 0 1 -1.44 3.13
-18 0 1 0.87 2.81
-18 0 2 104.70 7.19
-18 0 2 89.80 6.87
-18 0 2 102.51 7.17
-18 0 3 0.44 2.75
-18 0 3 0.45 2.23
-18 0 3 -0.92 2.54
-18 1 -2 32.25 3.07
-18 -1 -2 38.15 4.16
-18 1 -2 35.86 4.02
-18 -1 -2 32.67 3.17
-18 1 -2 28.44 3.54
-18 1 -1 15.32 3.19
-18 -1 -1 16.21 2.89
-18 1 -1 17.25 3.49
-18 1 -1 20.69 3.20
-18 -1 -1 14.17 3.55
-18 1 0 80.00 5.69
-18 -1 0 90.16 6.67
-18 1 0 84.23 6.49
-18 -1 0 72.51 5.44
-18 1 0 64.12 5.88
-18 1 1 6.47 2.76
-18 1 1 6.79 3.11
-18 -1 1 5.12 2.44
-18 1 1 2.46 2.65
-18 1 2 58.96 5.25
-18 1 2 72.62 5.64
-18 1 2 77.22 5.16
-18 1 2 72.57 5.20
-18 1 3 23.80 3.29
-18 1 3 28.48 3.10
-18 1 3 33.59 3.52
-18 1 3 29.02 3.76
-18 -2 -1 3.74 2.32
-18 2 -1 5.68 2.03
-18 -2 0 19.70 2.98
-18 2 0 16.07 2.86
-18 2 1 103.07 6.28
-18 -2 1 103.72 6.17
-17 0 -4 80.16 9.02
-17 0 -3 -0.16 3.55
-17 0 -3 -2.33 2.41
-17 0 -2 48.63 5.50
-17 0 -2 36.33 8.14
-17 0 -1 0.19 3.21
-17 0 -1 1.24 4.43
-17 0 -1 -1.47 4.47
-17 0 -1 5.33 6.03
-17 0 0 45.24 5.99
-17 0 0 62.60 7.25
-17 0 0 72.05 7.44
-17 0 0 70.64 7.17
-17 0 1 -0.19 3.39
-17 0 1 0.44 4.01
-17 0 1 5.99 4.91
-17 0 1 1.08 4.59
-17 0 2 70.53 7.48
-17 0 2 77.76 7.72
-17 0 2 83.60 7.85
-17 0 3 -2.20 4.27
-17 0 3 1.95 3.76
-17 0 3 3.03 4.17
-17 0 4 139.54 9.28
-17 0 4 146.34 9.56
-17 0 4 150.07 9.50
-17 0 5 1.22 2.85
-17 0 5 -1.93 2.58
-17 0 5 2.81 2.64
-17 -1 -4 65.99 4.99
-17 1 -4 74.84 5.71
-17 1 -4 59.00 5.28
-17 1 -3 21.16 4.25
-17 1 -3 34.15 4.15
-17 -1 -3 29.66 4.82
-17 1 -3 25.26 4.39
-17 -1 -3 33.84 4.12
-17 -1 -3 21.45 6.58
-17 1 -2 118.71 8.97
-17 -1 -2 143.08 9.41
-17 1 -2 143.50 8.61
-17 1 -2 136.24 9.22
-17 -1 -2 90.64 11.44
-17 -1 -2 151.44 8.89
-17 -1 -2 71.84 7.91
-17 1 -1 36.52 5.32
-17 1 -1 29.17 5.22
-17 -1 -1 25.14 7.31
-17 1 -1 31.85 5.38
-17 -1 -1 36.61 4.89
-17 -1 -1 42.30 6.04
-17 1 0 80.63 7.84
-17 1 0 90.71 8.22
-17 -1 0 83.50 7.30
-17 1 0 93.59 7.66
-17 1 0 97.58 8.16
-17 1 1 12.10 4.38
-17 1 1 12.60 4.53
-17 -1 1 10.96 4.04
-17 1 1 9.44 4.27
-17 1 1 13.55 4.73
-17 1 2 78.02 7.13
-17 1 2 85.60 7.41
-17 -1 2 68.01 6.67
-17 1 2 68.62 7.48
-17 1 3 157.95 9.60
-17 1 3 150.46 9.59
-17 1 3 137.20 9.92
-17 -1 3 143.93 9.17
-17 1 4 141.93 8.48
-17 -1 4 124.08 8.08
-17 1 4 140.06 9.26
-17 1 4 155.85 8.98
-17 -1 4 158.06 9.17
-17 1 5 23.67 3.62
-17 -1 5 21.95 3.46
-17 1 5 24.22 3.44
-17 -1 5 26.15 3.41
-17 2 -4 59.11 4.25
-17 2 -3 15.37 3.14
-17 -2 -3 9.36 2.71
-17 -2 -3 19.39 3.63
-17 -2 -2 55.12 4.94
-17 2 -2 77.77 6.77
-17 -2 -2 88.35 6.75
-17 2 -2 81.20 6.30
-17 -2 -2 70.03 8.49
-17 -2 -2 62.08 6.84
-17 2 -1 44.06 5.63
-17 -2 -1 29.61 4.08
-17 -2 -1 49.64 5.33
-17 2 -1 42.28 5.19
-17 -2 -1 27.77 6.36
-17 -2 0 35.95 4.66
-17 -2 0 52.32 5.52
-17 -2 0 44.61 5.45
-17 2 0 56.54 5.84
-17 2 0 45.61 5.87
-17 2 1 109.62 8.72
-17 2 1 113.86 7.01
-17 -2 1 119.66 8.25
-17 2 1 125.72 8.57
-17 -2 1 124.15 8.47
-17 -2 2 62.71 6.06
-17 2 2 60.93 6.37
-17 -2 2 75.56 6.16
-17 2 2 69.48 5.11
-17 2 2 63.69 6.30
-17 -2 3 60.05 5.41
-17 2 3 59.31 5.74
-17 2 3 56.72 4.43
-17 -2 3 63.52 5.25
-17 -2 4 10.51 2.75
-17 2 4 9.65 2.87
-17 -2 4 12.24 2.07
-17 3 -2 16.08 2.86
-17 -3 -2 13.13 2.36
-17 -3 -2 13.65 3.24
-17 -3 -1 70.43 5.39
-17 -3 -1 73.16 6.84
-17 3 -1 82.69 6.06
-17 3 0 38.93 4.46
-17 -3 0 32.90 3.82
-17 -3 1 13.32 2.87
-17 3 1 15.58 3.36
-17 -3 2 10.95 2.65
-17 3 2 11.31 2.88
-16 0 -5 -1.19 2.52
-16 0 -4 90.59 7.54
-16 0 -4 111.29 8.45
-16 0 -3 -1.15 4.50
-16 0 -3 -0.86 3.44
-16 0 -2 8.93 4.58
-16 0 -2 10.45 5.46
-16 0 -2 17.84 6.04
-16 0 -1 -1.56 4.14
-16 0 -1 -0.81 5.17
-16 0 -1 0.81 5.33
-16 0 0 464.82 21.82
-16 0 0 440.10 21.49
-16 0 1 -1.41 5.49
-16 0 1 5.83 5.72
-16 0 2 221.41 14.93
-16 0 2 232.14 15.09
-16 0 2 224.15 15.07
-16 0 3 0.52 5.03
-16 0 3 -0.51 5.27
-16 0 3 0.27 4.87
-16 0 4 317.19 17.16
-16 0 4 284.76 16.83
-16 0 4 302.77 16.85
-16 0 5 -1.77 4.13
-16 0 5 -1.13 4.07
-16 0 5 2.20 3.72
-16 0 6 205.07 11.01
-16 0 6 188.23 10.52
-16 0 6 174.69 10.60
-16 1 -6 54.13 4.51
-16 1 -6 47.14 4.17
-16 -1 -5 43.67 4.48
-16 1 -5 37.28 4.77
-16 1 -5 36.68 4.68
-16 1 -4 80.98 7.34
-16 -1 -4 93.94 7.86
-16 1 -4 96.15 6.97
-16 1 -4 81.01 7.42
-16 -1 -4 83.34 6.95
-16 1 -3 11.71 4.59
-16 -1 -3 9.43 4.87
-16 1 -3 15.09 4.50
-16 -1 -3 10.14 4.25
-16 1 -3 18.25 4.94
-16 -1 -3 12.42 8.02
-16 1 -2 137.51 10.00
-16 -1 -2 146.57 11.08
-16 1 -2 139.37 10.81
-16 -1 -2 140.75 10.20
-16 1 -2 111.03 10.20
-16 -1 -1 54.57 6.30
-16 1 -1 68.48 8.24
-16 1 -1 63.64 8.21
-16 -1 -1 66.84 7.56
-16 1 -1 74.37 8.44
-16 -1 -1 75.23 8.61
-16 1 -1 74.50 7.87
-16 1 0 61.00 7.73
-16 -1 0 59.58 7.32
-16 1 0 65.74 8.45
-16 -1 0 48.03 9.61
-16 1 0 67.08 8.15
-16 1 1 12.23 5.50
-16 -1 1 19.70 5.34
-16 1 1 13.27 5.79
-16 1 1 11.07 5.80
-16 1 2 184.62 12.54
-16 1 2 170.61 12.49
-16 1 2 183.98 13.19
-16 -1 2 165.89 12.05
-16 1 3 9.30 5.40
-16 1 3 11.98 5.25
-16 1 3 13.53 5.15
-16 -1 3 11.91 4.73
-16 -1 4 96.99 8.54
-16 1 4 102.66 8.91
-16 1 4 91.89 8.88
-16 -1 4 84.60 7.88
-16 1 4 103.59 8.59
-16 1 5 82.55 7.35
-16 -1 5 90.07 7.45
-16 -1 5 78.57 7.35
-16 1 5 75.94 6.70
-16 1 5 79.43 7.54
-16 -1 5 70.56 6.50
-16 1 6 74.70 4.60
-16 -1 6 80.47 5.96
-16 1 6 78.74 5.85
-16 -1 6 89.61 5.64
-16 2 -5 14.58 2.95
-16 2 -5 16.63 3.35
-16 2 -4 40.69 5.22
-16 2 -4 42.96 4.91
-16 -2 -4 25.87 4.55
-16 -2 -3 175.30 11.13
-16 2 -3 216.90 12.93
-16 -2 -3 232.64 12.56
-16 2 -3 210.80 12.07
-16 -2 -3 174.53 15.63
-16 -2 -3 185.27 13.32
-16 2 -2 66.18 7.66
-16 -2 -2 61.47 6.61
-16 -2 -2 85.25 7.92
-16 2 -2 86.18 7.56
-16 -2 -2 57.56 10.23
-16 2 -1 78.09 8.32
-16 -2 -1 68.83 7.23
-16 2 -1 88.19 6.97
-16 -2 -1 90.74 8.49
-16 -2 -1 79.27 7.69
-16 2 -1 83.73 8.12
-16 -2 -1 57.54 10.04
-16 2 0 79.83 8.38
-16 -2 0 78.39 7.79
-16 -2 0 81.01 8.06
-16 2 0 83.42 7.14
-16 -2 0 49.74 9.47
-16 2 0 71.30 7.88
-16 2 1 87.24 7.72
-16 -2 1 81.69 8.12
-16 -2 1 95.53 8.57
-16 2 1 85.58 7.50
-16 -2 1 64.78 8.95
-16 2 1 85.55 8.54
-16 2 2 44.98 5.78
-16 2 2 45.51 5.81
-16 -2 2 55.31 6.72
-16 2 2 41.30 6.34
-16 -2 2 46.36 6.31
-16 2 3 45.86 5.24
-16 -2 3 49.33 6.12
-16 2 3 48.05 5.79
-16 2 3 55.27 6.76
-16 -2 3 43.38 6.24
-16 2 4 58.88 5.73
-16 -2 4 53.18 5.78
-16 2 4 55.75 6.41
-16 -2 4 52.09 5.97
-16 -2 5 52.87 4.45
-16 2 5 67.04 5.13
-16 2 5 48.93 5.46
-16 -2 5 55.45 5.49
-16 -3 -4 31.28 4.01
-16 -3 -4 25.47 4.14
-16 3 -4 34.46 3.74
-16 3 -3 44.14 5.06
-16 -3 -3 35.18 4.45
-16 -3 -3 41.86 6.70
-16 3 -3 39.35 3.61
-16 -3 -3 45.92 5.98
-16 3 -2 33.99 5.32
-16 -3 -2 36.30 4.77
-16 -3 -2 34.85 7.20
-16 -3 -2 38.82 4.66
-16 3 -2 37.92 4.23
-16 -3 -2 48.51 6.98
-16 -3 -1 67.95 6.74
-16 -3 -1 88.73 6.61
-16 -3 -1 77.58 9.11
-16 3 -1 65.30 5.92
-16 3 -1 75.02 7.24
-16 -3 0 16.22 5.75
-16 -3 0 21.22 4.04
-16 3 0 18.65 3.79
-16 -3 0 21.33 4.45
-16 3 0 21.49 5.13
-16 3 1 136.15 8.78
-16 3 1 133.66 9.93
-16 3 2 5.18 2.95
-16 3 2 4.30 3.63
-16 3 3 133.34 8.00
-16 3 4 7.66 2.18
-16 -4 -1 35.43 5.04
-16 -4 -1 43.90 4.23
-16 4 0 19.85 2.80
-16 -4 0 32.54 3.76
-16 4 1 52.34 4.14
-16 -4 1 75.54 5.46
-15 0 -7 0.15 2.11
-15 0 -6 87.45 6.71
-15 0 -5 2.38 4.33
-15 0 -5 2.46 3.37
-15 0 -4 145.51 11.10
-15 0 -4 179.39 12.26
-15 0 -3 0.29 5.33
-15 0 -3 -2.80 4.22
-15 0 -2 281.60 17.08
-15 0 -2 255.42 16.53
-15 0 -1 -3.20 6.34
-15 0 -1 1.28 5.82
-15 0 -1 -2.53 4.52
-15 0 0 525.04 27.54
-15 0 0 540.91 27.73
-15 0 1 -2.31 6.62
-15 0 1 0.67 5.93
-15 0 2 57.92 9.03
-15 0 2 52.58 8.88
-15 0 3 -1.59 6.04
-15 0 3 -2.25 6.11
-15 0 4 127.41 11.69
-15 0 4 109.85 10.96
-15 0 4 139.56 11.87
-15 0 5 -5.77 5.67
-15 0 5 2.43 4.75
-15 0 5 -0.81 5.44
-15 0 6 227.11 13.48
-15 0 6 193.45 13.06
-15 0 6 224.58 13.78
-15 0 7 1.10 3.34
-15 0 7 6.04 3.57
-15 -1 -7 14.73 3.84
-15 1 -7 18.39 2.99
-15 1 -6 51.73 5.48
-15 1 -6 49.97 5.53
-15 -1 -6 54.14 5.11
-15 1 -5 5.16 4.02
-15 -1 -5 5.74 4.70
-15 -1 -5 8.14 3.86
-15 1 -5 5.38 4.03
-15 1 -4 87.52 8.00
-15 -1 -4 93.73 9.14
-15 -1 -4 85.52 8.27
-15 1 -4 93.69 8.88
-15 1 -4 84.26 8.73
-15 -1 -3 27.06 5.73
-15 1 -3 21.02 5.91
-15 -1 -3 25.59 6.49
-15 1 -3 27.13 5.84
-15 -1 -3 17.80 4.00
-15 1 -3 25.51 6.04
-15 -1 -3 19.69 4.47
-15 -1 -2 160.33 11.50
-15 1 -2 159.31 12.94
-15 -1 -2 131.34 10.77
-15 -1 -2 196.51 13.58
-15 1 -2 194.80 13.64
-15 1 -2 190.74 12.91
-15 -1 -2 182.85 13.51
-15 1 -2 147.14 12.72
-15 -1 -2 168.57 12.54
-15 1 -1 55.95 8.55
-15 1 -1 60.91 8.50
-15 -1 -1 55.82 8.47
-15 -1 -1 47.63 6.56
-15 -1 -1 64.59 8.87
-15 1 -1 57.00 7.88
-15 -1 -1 47.66 7.63
-15 1 -1 57.08 8.55
-15 1 0 125.48 11.06
-15 1 0 108.58 10.51
-15 -1 0 102.06 10.16
-15 1 0 100.81 10.85
-15 -1 0 83.38 8.65
-15 1 1 20.83 6.84
-15 -1 1 23.62 8.56
-15 -1 1 29.29 6.51
-15 1 1 33.22 7.56
-15 1 1 25.33 7.33
-15 1 2 277.36 17.73
-15 -1 2 271.30 17.32
-15 1 2 303.89 18.04
-15 1 2 256.55 17.87
-15 1 3 77.95 9.20
-15 1 3 82.47 9.46
-15 -1 3 79.29 9.01
-15 1 3 83.00 9.85
-15 -1 4 142.33 11.86
-15 1 4 149.84 11.98
-15 1 4 135.21 11.84
-15 -1 4 120.77 10.63
-15 1 4 134.75 11.11
-15 1 5 46.55 7.29
-15 -1 5 40.70 6.72
-15 1 5 45.56 6.70
-15 -1 5 35.91 6.00
-15 1 5 38.66 6.77
-15 -1 5 35.21 6.89
-15 -1 6 126.29 9.27
-15 1 6 126.34 9.53
-15 -1 6 96.58 8.19
-15 -1 6 106.89 9.12
-15 1 6 128.87 8.81
-15 1 6 120.87 9.54
-15 1 7 6.18 3.55
-15 -1 7 6.05 3.09
-15 1 7 6.56 2.74
-15 -1 7 3.20 2.01
-15 -1 7 1.58 3.23
-15 1 7 2.32 3.30
-15 2 -6 46.79 4.51
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10 -3 -8 69.46 9.15
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10 -4 -4 38.73 9.12
10 -4 -4 29.45 10.04
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10 -4 -4 35.95 10.96
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10 -4 -3 234.71 21.14
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10 -4 -2 149.14 14.60
10 -4 -2 145.16 16.94
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10 -4 1 357.90 21.27
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10 -4 2 66.88 10.71
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10 -5 1 186.12 16.88
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13 -1 6 272.35 20.44
13 1 6 236.97 19.22
13 -1 7 19.66 8.03
13 1 7 26.43 7.84
13 -1 8 22.29 6.08
13 1 8 25.38 5.63
13 2 -7 108.24 13.02
13 2 -6 100.00 14.60
13 2 -5 72.83 14.05
13 -2 -5 102.86 12.08
13 2 -4 329.53 19.63
13 -2 -4 378.79 24.15
13 2 -3 147.76 12.35
13 -2 -3 183.43 17.44
13 2 -3 137.37 17.46
13 -2 -2 138.51 13.78
13 2 -2 184.58 13.59
13 2 -2 158.29 17.62
13 2 -1 295.05 18.26
13 2 -1 251.23 21.58
13 -2 0 350.78 24.27
13 2 0 250.37 20.90
13 -2 1 663.86 34.92
13 2 1 566.21 30.68
13 -2 2 5.34 8.12
13 -2 3 94.39 13.27
13 -2 4 194.45 17.72
13 -2 5 93.48 12.60
13 -2 6 17.22 8.30
13 2 6 12.22 7.80
13 2 7 25.19 6.55
13 -2 8 133.99 10.07
13 -3 -7 192.02 11.28
13 3 -7 215.06 15.50
13 -3 -6 8.76 4.26
13 -3 -6 9.24 6.87
13 3 -6 4.93 3.38
13 3 -6 0.86 7.44
13 -3 -5 165.41 12.20
13 3 -5 175.87 16.91
13 -3 -5 209.62 16.64
13 3 -5 231.86 13.90
13 -3 -4 16.51 5.50
13 3 -4 13.92 9.01
13 3 -4 27.17 5.81
13 -3 -4 20.49 8.84
13 -3 -4 23.73 6.97
13 -3 -3 344.65 20.62
13 3 -3 451.97 22.93
13 -3 -3 479.44 24.97
13 3 -3 360.44 25.54
13 -3 -3 389.15 24.79
13 -3 -3 391.88 23.71
13 3 -2 194.59 13.87
13 -3 -2 160.50 15.24
13 -3 -2 172.59 15.20
13 -3 -2 222.14 17.03
13 3 -2 143.11 15.23
13 -3 -1 121.77 13.05
13 -3 -1 125.78 13.91
13 3 -1 144.14 14.31
13 -3 2 195.42 14.48
13 -3 3 167.79 14.33
13 -3 4 4.19 6.99
13 -3 5 206.50 15.67
13 -3 6 22.98 6.99
13 3 6 21.01 6.03
13 -3 7 112.53 9.27
13 4 -6 6.77 3.71
13 -4 -6 0.94 4.77
13 -4 -6 2.75 2.81
13 -4 -5 162.50 10.47
13 4 -5 154.97 11.64
13 -4 -5 187.52 15.64
13 4 -5 173.85 10.73
13 -4 -5 184.92 13.72
13 -4 -5 155.89 11.40
13 -4 -4 3.74 4.45
13 4 -4 1.67 4.92
13 4 -4 1.43 2.83
13 -4 -4 5.82 6.87
13 -4 -4 -2.69 5.79
13 4 -3 131.50 10.11
13 -4 -3 131.99 12.49
13 -4 -3 123.09 12.81
13 -4 -3 114.76 9.97
13 4 -2 86.98 8.48
13 -4 -2 91.46 11.18
13 -4 -2 72.73 10.44
13 -4 -2 71.92 8.24
13 -4 -1 235.44 16.91
13 4 -1 234.39 14.85
13 -4 -1 209.16 13.99
13 -4 0 31.42 7.59
13 4 0 22.43 5.10
13 -4 0 36.47 13.08
13 -4 1 92.66 14.86
13 -4 2 40.25 11.45
13 -4 5 39.80 8.15
13 -5 -4 97.69 8.31
13 -5 -4 107.36 9.99
13 -5 -4 83.64 6.31
13 -5 -3 152.46 11.43
13 -5 -3 145.49 9.30
13 -5 -2 26.50 6.06
13 5 -2 14.50 3.40
13 -5 -2 8.60 9.67
13 -5 -1 128.67 11.07
13 -5 -1 156.51 13.63
13 5 -1 123.55 8.96
13 -5 -1 155.32 15.87
13 -5 0 208.23 13.31
13 5 0 182.79 11.60
13 5 1 100.29 7.81
13 -5 1 125.54 13.78
13 -5 2 7.73 8.17
13 5 2 12.97 3.22
13 -5 2 17.31 8.08
13 -5 3 62.04 9.68
13 -5 4 32.75 6.58
14 0 -8 13.11 3.74
14 0 -7 3.09 3.47
14 0 -7 -1.43 6.87
14 0 -6 159.57 11.61
14 0 -6 139.76 14.92
14 0 -5 -1.40 3.57
14 0 -5 0.58 8.67
14 0 -4 456.92 23.31
14 0 -3 -0.83 3.58
14 0 -2 125.86 9.98
14 0 -2 115.94 16.04
14 0 -1 0.26 3.02
14 0 -1 -3.16 8.46
14 0 0 445.39 22.84
14 0 0 560.63 32.05
14 0 1 -3.97 8.64
14 0 2 160.15 16.20
14 0 3 -5.50 7.92
14 0 5 -0.97 9.21
14 0 6 49.67 10.24
14 0 7 1.50 6.39
14 0 8 101.15 8.22
14 1 -8 169.66 11.46
14 1 -7 88.01 8.32
14 1 -6 197.95 13.19
14 -1 -6 206.75 15.99
14 1 -5 81.17 8.25
14 1 -5 69.10 13.00
14 -1 -5 72.08 11.90
14 1 -4 199.15 13.70
14 -1 -4 215.05 19.23
14 1 -4 180.17 18.74
14 1 -3 14.07 4.71
14 1 -3 7.07 9.56
14 -1 -3 14.54 9.39
14 1 -2 221.39 14.95
14 1 -2 209.56 20.59
14 1 -1 534.67 26.69
14 1 -1 530.02 33.13
14 1 0 211.48 14.28
14 -1 0 252.38 20.87
14 1 0 237.55 19.65
14 -1 1 112.71 14.50
14 1 1 120.95 14.20
14 -1 2 440.11 27.08
14 1 2 385.88 24.28
14 -1 3 56.89 11.76
14 1 3 78.70 10.72
14 -1 4 70.88 12.36
14 1 5 51.25 11.04
14 1 6 193.83 15.68
14 -1 7 35.48 7.46
14 1 7 42.24 7.10
14 -1 8 17.26 4.56
14 1 8 16.49 3.49
14 2 -7 59.55 6.25
14 2 -7 46.55 8.10
14 2 -6 97.64 8.38
14 2 -6 98.98 12.06
14 2 -5 85.32 8.29
14 2 -5 62.94 11.57
14 -2 -5 80.26 9.27
14 2 -4 49.08 6.81
14 2 -4 55.07 11.68
14 -2 -4 61.94 9.89
14 2 -3 331.19 19.30
14 2 -3 286.27 23.42
14 -2 -2 221.39 17.16
14 2 -2 280.83 17.04
14 2 -2 233.66 20.34
14 2 -1 185.96 13.50
14 -2 -1 206.50 18.05
14 2 -1 184.09 17.18
14 2 0 92.24 9.37
14 -2 0 126.08 14.56
14 2 0 99.93 12.41
14 -2 1 47.89 8.34
14 2 1 72.65 9.98
14 -2 2 173.27 15.45
14 -2 3 11.38 8.19
14 -2 4 128.44 13.60
14 -2 5 93.14 11.45
14 2 5 73.61 10.91
14 -2 6 36.07 7.81
14 2 6 30.96 7.68
14 2 7 55.08 6.20
14 -3 -6 10.81 5.72
14 3 -6 16.72 3.65
14 3 -6 24.22 6.31
14 -3 -5 206.02 14.82
14 3 -5 205.75 12.57
14 3 -5 190.03 15.07
14 -3 -4 6.03 6.47
14 3 -4 11.00 4.18
14 3 -4 6.91 6.68
14 -3 -3 142.84 13.13
14 3 -3 145.58 13.97
14 -3 -2 23.38 7.32
14 -3 -2 21.30 7.47
14 3 -2 15.25 6.65
14 -3 -1 47.19 8.26
14 3 -1 49.92 8.34
14 -3 2 6.51 8.96
14 -3 4 31.89 6.84
14 -3 5 157.95 11.45
14 3 5 119.08 11.19
14 -3 6 0.19 4.23
14 3 6 5.12 3.65
14 -4 -5 263.37 14.68
14 -4 -4 6.37 5.10
14 4 -4 5.13 2.71
14 -4 -4 -1.45 9.03
14 -4 -3 145.60 11.94
14 4 -3 159.19 10.33
14 -4 -2 37.21 7.28
14 4 -2 32.16 5.00
14 -4 -1 285.78 17.01
14 4 -1 285.29 16.20
14 -4 -1 325.14 23.41
14 4 0 4.54 3.50
14 -4 0 10.55 10.23
14 4 1 77.59 7.54
14 -4 1 99.48 13.35
14 -4 2 18.30 8.55
14 -4 5 44.17 5.76
14 -5 -2 16.89 3.72
14 -5 -2 17.42 7.26
14 -5 -1 64.51 5.08
14 -5 -1 97.56 10.64
14 -5 0 124.29 10.93
14 -5 0 104.11 11.45
14 -5 1 77.26 9.42
14 -5 1 58.67 8.24
14 -5 2 4.98 5.59
15 0 -7 1.10 4.17
15 0 -6 260.47 17.74
15 0 -5 1.94 2.01
15 0 -5 -6.28 7.80
15 0 -4 121.86 8.80
15 0 -3 1.81 2.58
15 0 -3 -4.49 8.86
15 0 -2 43.13 5.35
15 0 -2 63.27 12.61
15 0 -1 1.13 7.99
15 0 0 574.22 33.39
15 0 1 1.55 7.49
15 0 2 282.24 20.76
15 0 3 0.49 8.62
15 0 6 94.63 10.29
15 0 7 2.24 4.29
15 1 -7 4.56 4.40
15 1 -6 137.46 9.66
15 -1 -6 143.16 11.18
15 1 -5 40.69 5.50
15 1 -5 62.72 10.36
15 -1 -5 49.36 8.93
15 1 -4 135.79 10.39
15 -1 -4 167.86 15.43
15 1 -4 155.06 15.82
15 1 -3 81.76 8.06
15 -1 -3 106.42 13.25
15 1 -3 92.49 12.82
15 1 -2 286.64 16.86
15 -1 -2 323.45 23.12
15 1 -2 296.78 22.37
15 1 -1 18.66 4.77
15 1 -1 32.33 9.41
15 1 0 111.98 9.25
15 -1 0 146.82 15.43
15 1 0 143.82 14.37
15 -1 1 45.46 9.28
15 1 1 49.96 6.04
15 -1 1 68.62 11.40
15 1 1 55.02 10.00
15 -1 2 147.35 14.75
15 1 2 148.44 10.83
15 -1 2 216.40 17.81
15 1 2 207.56 15.92
15 -1 3 28.26 9.49
15 -1 4 76.18 11.17
15 -1 5 8.24 7.59
15 1 5 4.87 7.18
15 1 6 46.12 7.91
15 -1 7 19.09 5.14
15 1 7 22.25 4.71
15 -2 -6 19.94 5.39
15 2 -6 22.79 6.28
15 -2 -5 48.44 7.37
15 2 -5 56.68 6.17
15 2 -5 48.52 8.84
15 -2 -4 53.18 8.04
15 2 -4 61.86 6.68
15 -2 -4 69.47 9.21
15 2 -4 55.38 9.97
15 2 -3 325.17 17.63
15 -2 -3 366.49 21.54
15 2 -3 320.75 21.57
15 2 -2 135.03 10.79
15 2 -2 143.48 14.39
15 2 -1 153.12 11.67
15 2 -1 167.68 15.05
15 2 0 127.07 10.45
15 -2 0 163.02 15.50
15 2 0 148.88 13.31
15 2 1 114.71 9.45
15 2 1 117.86 11.47
15 -2 2 66.24 8.53
15 -2 3 239.06 16.74
15 -2 4 43.26 8.16
15 -2 5 52.48 7.97
15 2 5 43.34 8.34
15 -2 6 52.98 6.79
15 2 6 39.48 6.36
15 -3 -5 65.39 6.97
15 3 -5 81.36 7.81
15 -3 -4 55.84 7.33
15 3 -4 66.38 8.04
15 -3 -3 80.91 8.61
15 3 -3 95.36 9.64
15 -3 -2 10.26 4.97
15 3 -2 15.43 5.47
15 3 -1 385.91 20.03
15 3 0 59.94 6.76
15 3 1 274.93 15.60
15 -3 1 284.53 20.41
15 3 2 8.76 3.36
15 3 5 65.25 6.82
15 -4 -4 -0.85 2.64
15 -4 -4 6.20 5.62
15 -4 -3 29.48 4.54
15 -4 -2 13.46 3.81
15 4 -2 10.15 2.83
15 -4 -2 10.29 8.23
15 4 -1 130.14 8.97
15 -4 -1 157.92 14.33
15 4 0 3.46 2.52
15 -4 0 5.11 7.84
15 4 1 62.97 5.90
15 -4 1 77.06 9.93
15 -4 4 23.30 5.02
16 0 -6 228.13 13.72
16 0 -5 1.61 5.63
16 0 -3 2.19 7.28
16 0 -2 280.37 20.58
16 0 -1 0.47 7.01
16 0 0 491.35 28.43
16 0 1 -2.15 6.69
16 0 2 15.33 8.07
16 0 3 -0.77 6.87
16 0 4 101.01 11.43
16 0 6 42.39 6.31
16 -1 -5 113.80 9.38
16 1 -5 93.68 9.74
16 1 -4 81.83 7.04
16 -1 -4 114.35 10.90
16 1 -4 96.01 11.02
16 1 -3 10.43 3.47
16 -1 -3 17.69 7.55
16 1 -3 16.16 7.50
16 1 -2 142.74 10.02
16 1 -2 184.31 15.43
16 1 -1 9.96 3.30
16 1 -1 15.45 7.72
16 1 0 47.31 5.58
16 -1 0 77.57 11.13
16 1 0 66.33 10.05
16 -1 1 31.33 6.48
16 1 1 21.75 3.71
16 -1 2 119.21 11.90
16 -1 3 12.90 6.65
16 -1 4 84.62 9.82
16 -1 5 35.76 6.78
16 1 5 41.39 7.22
16 1 6 56.59 6.21
16 -2 -5 40.06 4.65
16 2 -5 61.45 7.26
16 2 -4 61.87 5.52
16 2 -4 68.81 8.38
16 2 -3 54.51 5.84
16 -2 -3 66.49 8.74
16 2 -3 63.37 8.53
16 2 -2 43.73 5.32
16 -2 -2 58.20 9.09
16 2 -2 43.99 8.08
16 2 -1 78.47 7.37
16 -2 -1 104.08 11.42
16 2 -1 106.26 10.43
16 2 0 57.19 6.35
16 2 0 91.04 9.20
16 2 1 69.30 6.67
16 2 1 83.56 8.16
16 2 2 46.05 5.34
16 2 3 145.68 9.17
16 -2 4 8.88 4.35
16 2 4 51.53 7.81
16 -2 5 13.42 4.10
16 2 5 13.46 4.85
16 3 -4 11.96 3.16
16 3 -3 149.52 9.26
16 3 -3 151.84 9.48
16 3 -2 4.44 2.44
16 3 -1 135.33 9.15
16 3 0 18.00 3.70
16 -3 0 21.20 8.31
16 3 1 53.70 5.57
16 -3 1 74.09 8.86
16 3 2 35.60 4.32
16 3 4 34.41 5.31
16 -4 -1 73.21 8.10
16 -4 0 33.06 5.90
17 0 -5 -2.27 3.78
17 0 -3 -1.58 5.60
17 0 -2 98.63 10.59
17 0 -1 3.87 5.84
17 0 0 68.82 9.42
17 0 1 3.28 5.50
17 0 1 -3.60 6.05
17 0 2 48.38 8.00
17 0 3 0.27 5.38
17 0 4 115.02 9.64
17 -1 -5 32.61 3.72
17 1 -5 30.09 4.88
17 -1 -4 194.60 12.01
17 1 -4 163.19 12.03
17 -1 -3 186.69 13.17
17 1 -3 190.33 13.54
17 1 -2 95.68 10.00
17 1 -1 15.21 6.15
17 -1 0 107.39 11.06
17 1 0 104.49 10.18
17 1 1 34.41 6.56
17 1 2 122.60 11.21
17 -1 3 32.72 5.52
17 1 3 32.41 6.83
17 -1 4 56.95 6.35
17 2 -4 13.09 3.63
17 2 -3 80.53 7.36
17 2 -2 70.83 7.33
17 2 -1 131.09 9.63
17 2 0 50.95 6.01
17 2 3 11.45 5.33
17 2 4 70.10 6.42
17 -3 -2 9.47 5.48
17 -3 -1 21.17 5.92
17 -3 0 43.48 5.85
18 0 -3 2.82 3.56
18 0 -2 119.20 9.47
18 0 -1 2.35 4.12
18 0 3 -2.42 3.05
18 -1 -3 46.26 5.15
18 1 -3 45.17 5.18
18 1 -2 91.97 7.56
18 1 -1 5.70 4.04
18 1 1 8.97 4.12
18 1 2 36.14 5.43
18 2 0 17.11 3.73
18 2 1 2.75 3.49
0 0 0 0.00 0.00
TITL 99718 in Pc
REM Pc (#7 in standard setting)
CELL 1.54184 14.974081 6.384199 10.074134 90.0000 90.4354 90.0000
ZERR 3.00 0.000214 0.000085 0.000136 0.0000 0.0013 0.0000
LATT -1
SYMM x,-y, z+1/2
SFAC C H N Br
UNIT 54.00 84.00 9.00 3.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 28799
_shelx_res_file
;
TITL 99718_a.res in Pc
99718.res
created by SHELXL-2018/3 at 10:58:09 on 15-Jan-2025
REM Old TITL 99718 in Pc
REM SHELXT solution in Pc: R1 0.104, Rweak 0.023, Alpha 0.007
REM 0.415 for 183 systematic absences, Orientation as input
REM Flack x = 0.294 ( 0.026 ) from 1607 Parsons' quotients
REM Formula found by SHELXT: C18 N3 Br
CELL 1.54184 14.9741 6.3842 10.0741 90 90.435 90
ZERR 2 0.0002 0.0001 0.0001 0 0.001 0
LATT -1
SYMM +X,-Y,0.5+Z
SFAC C H Br N
UNIT 36 56 2 6
EQIV $1 +X,-Y,-0.5+Z
EQIV $2 +X,1+Y,+Z
EQIV $3 +X,1-Y,-0.5+Z
L.S. 4 0 0
PLAN 7
TEMP -173
CONF
HTAB C1 Br1_$1
HTAB C2 Br1_$2
HTAB C3 Br1_$3
list 4
WPDB -2
MORE -1
BOND $H
fmap 2 53
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
REM
REM
REM
WGHT 0.095900 0.258300
BASF 0.30905
FVAR 0.89193
BR1 3 0.546560 0.069086 0.654930 11.00000 0.04248 0.02038 =
0.02436 0.00186 0.00457 0.00679
N1 4 0.550000 0.463690 0.378279 11.00000 0.02209 0.02107 =
0.01884 0.00243 0.00196 0.00009
N2 4 0.678294 0.371302 0.453900 11.00000 0.01950 0.02597 =
0.02144 0.00030 -0.00041 0.00453
N3 4 0.661995 0.566623 0.506179 11.00000 0.02296 0.02546 =
0.03375 -0.01127 -0.00729 0.00243
C1 1 0.610149 0.309267 0.380633 11.00000 0.02179 0.02544 =
0.02086 -0.00064 0.00112 0.00079
AFIX 43
H1 2 0.604702 0.177837 0.337098 11.00000 -1.20000
AFIX 0
C2 1 0.584896 0.617629 0.457593 11.00000 0.02567 0.01699 =
0.03690 -0.00681 0.00038 0.00216
AFIX 43
H2 2 0.555844 0.746944 0.474936 11.00000 -1.20000
AFIX 0
C3 1 0.464719 0.459030 0.307031 11.00000 0.02054 0.01599 =
0.02414 -0.00379 -0.00204 -0.00343
AFIX 23
H3A 2 0.454105 0.316252 0.271962 11.00000 -1.20000
H3B 2 0.467148 0.556569 0.230747 11.00000 -1.20000
AFIX 0
C4 1 0.388305 0.520586 0.396565 11.00000 0.02224 0.02242 =
0.01899 0.00045 -0.00285 -0.00329
C5 1 0.352828 0.374055 0.485017 11.00000 0.03162 0.01517 =
0.03087 -0.00005 0.00297 0.00267
AFIX 43
H5 2 0.378248 0.238097 0.491755 11.00000 -1.20000
AFIX 0
C6 1 0.280174 0.428440 0.563011 11.00000 0.02535 0.03089 =
0.02581 0.00636 -0.00075 -0.00184
AFIX 43
H6 2 0.256577 0.327384 0.622421 11.00000 -1.20000
AFIX 0
C7 1 0.240724 0.626363 0.557025 11.00000 0.02018 0.02385 =
0.02252 -0.00012 0.00192 -0.00098
C8 1 0.279831 0.772546 0.472192 11.00000 0.03168 0.02477 =
0.03583 0.00774 0.01002 0.00729
AFIX 43
H8 2 0.256487 0.910800 0.468385 11.00000 -1.20000
AFIX 0
C9 1 0.352695 0.719565 0.392680 11.00000 0.03156 0.01901 =
0.03596 0.01171 0.00386 0.00407
AFIX 43
H9 2 0.377835 0.821754 0.335496 11.00000 -1.20000
AFIX 0
C10 1 0.158664 0.684920 0.639538 11.00000 0.02042 0.03842 =
0.02243 -0.00110 0.00126 0.00464
C11 1 0.122790 0.500401 0.717666 11.00000 0.05454 0.05407 =
0.09379 0.01260 0.05260 0.00676
AFIX 137
H11A 2 0.171894 0.432843 0.766215 11.00000 -1.50000
H11B 2 0.095357 0.399365 0.656521 11.00000 -1.50000
H11C 2 0.077949 0.549817 0.780724 11.00000 -1.50000
AFIX 0
C12 1 0.086153 0.773436 0.550455 11.00000 0.03272 0.14050 =
0.03730 0.01715 0.00649 0.03765
AFIX 137
H12A 2 0.110278 0.890299 0.498836 11.00000 -1.50000
H12B 2 0.036538 0.823367 0.604882 11.00000 -1.50000
H12C 2 0.064673 0.663981 0.489943 11.00000 -1.50000
AFIX 0
C13 1 0.186813 0.853098 0.739684 11.00000 0.04138 0.07584 =
0.05343 -0.02478 0.01297 0.00310
AFIX 137
H13A 2 0.236811 0.801050 0.793659 11.00000 -1.50000
H13B 2 0.136364 0.886337 0.797395 11.00000 -1.50000
H13C 2 0.205292 0.979608 0.692129 11.00000 -1.50000
AFIX 0
C14 1 0.757996 0.254072 0.489958 11.00000 0.02283 0.02739 =
0.02546 0.00272 -0.00048 0.00573
AFIX 23
H14A 2 0.742071 0.103995 0.496963 11.00000 -1.20000
H14B 2 0.778492 0.300990 0.578763 11.00000 -1.20000
AFIX 0
C15 1 0.835610 0.276070 0.392720 11.00000 0.02709 0.02771 =
0.03102 0.00807 0.00092 0.00872
C16 1 0.810111 0.179065 0.260290 11.00000 0.04051 0.05794 =
0.02789 -0.00616 -0.00107 0.01450
AFIX 137
H16A 2 0.792902 0.032522 0.273682 11.00000 -1.50000
H16B 2 0.861192 0.185658 0.200193 11.00000 -1.50000
H16C 2 0.759767 0.256349 0.221446 11.00000 -1.50000
AFIX 0
C17 1 0.859014 0.508702 0.376364 11.00000 0.02741 0.04563 =
0.06540 0.01458 0.00725 0.00195
AFIX 137
H17A 2 0.807805 0.583173 0.337805 11.00000 -1.50000
H17B 2 0.910499 0.522528 0.317528 11.00000 -1.50000
H17C 2 0.873678 0.568915 0.463317 11.00000 -1.50000
AFIX 0
C18 1 0.913941 0.156130 0.453428 11.00000 0.02600 0.04580 =
0.04049 0.00558 -0.00242 0.00842
AFIX 137
H18A 2 0.928094 0.213916 0.541221 11.00000 -1.50000
H18B 2 0.966108 0.169448 0.395882 11.00000 -1.50000
H18C 2 0.897962 0.007942 0.462197 11.00000 -1.50000
AFIX 0
HKLF 4
REM 99718_a.res in Pc
REM wR2 = 0.1354, GooF = S = 1.147, Restrained GooF = 1.147 for all data
REM R1 = 0.0428 for 3564 Fo > 4sig(Fo) and 0.0454 for all 3683 data
REM 206 parameters refined using 2 restraints
END
WGHT 0.0959 0.2583
REM Highest difference peak 0.766, deepest hole -0.869, 1-sigma level 0.082
Q1 1 0.4813 0.1596 0.6402 11.00000 0.05 0.77
Q2 1 0.4821 -0.0148 0.6386 11.00000 0.05 0.72
Q3 1 0.4854 0.0389 0.6569 11.00000 0.05 0.70
Q4 1 0.6123 -0.0226 0.6746 11.00000 0.05 0.69
Q5 1 0.6127 0.1400 0.6651 11.00000 0.05 0.66
Q6 1 0.6037 0.0466 0.6474 11.00000 0.05 0.65
Q7 1 0.5636 0.0629 0.7608 11.00000 0.05 0.43
;
_shelx_res_checksum 91963
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br1 0.54656(4) 0.06909(7) 0.65493(5) 0.0291(2) Uani d 1 . .
N N1 0.5500(4) 0.4637(8) 0.3783(5) 0.0207(10) Uani d 1 . .
N N2 0.6783(3) 0.3713(9) 0.4539(5) 0.0223(9) Uani d 1 . .
N N3 0.6620(4) 0.5666(8) 0.5062(7) 0.0274(14) Uani d 1 . .
C C1 0.6101(3) 0.3093(10) 0.3806(6) 0.0227(11) Uani d 1 . .
H H1 0.604702 0.177837 0.337098 0.027 Uiso calc 1 . .
C C2 0.5849(4) 0.6176(10) 0.4576(7) 0.0265(12) Uani d 1 . .
H H2 0.555844 0.746944 0.474936 0.032 Uiso calc 1 . .
C C3 0.4647(5) 0.4590(10) 0.3070(7) 0.0202(12) Uani d 1 . .
H H3A 0.454105 0.316252 0.271962 0.024 Uiso calc 1 . .
H H3B 0.467148 0.556569 0.230747 0.024 Uiso calc 1 . .
C C4 0.3883(4) 0.5206(10) 0.3966(6) 0.0212(11) Uani d 1 . .
C C5 0.3528(4) 0.3741(10) 0.4850(7) 0.0259(11) Uani d 1 . .
H H5 0.378248 0.238097 0.491755 0.031 Uiso calc 1 . .
C C6 0.2802(4) 0.4284(9) 0.5630(7) 0.0274(14) Uani d 1 . .
H H6 0.256577 0.327384 0.622421 0.033 Uiso calc 1 . .
C C7 0.2407(4) 0.6264(10) 0.5570(6) 0.0222(10) Uani d 1 . .
C C8 0.2798(4) 0.7725(11) 0.4722(8) 0.0307(13) Uani d 1 . .
H H8 0.256487 0.910800 0.468385 0.037 Uiso calc 1 . .
C C9 0.3527(4) 0.7196(9) 0.3927(7) 0.0288(13) Uani d 1 . .
H H9 0.377835 0.821754 0.335496 0.035 Uiso calc 1 . .
C C10 0.1587(4) 0.6849(11) 0.6395(6) 0.0271(12) Uani d 1 . .
C C11 0.1228(7) 0.5004(18) 0.7177(13) 0.067(3) Uani d 1 . .
H H11A 0.171894 0.432843 0.766215 0.101 Uiso calc 1 . .
H H11B 0.095357 0.399365 0.656521 0.101 Uiso calc 1 . .
H H11C 0.077949 0.549817 0.780724 0.101 Uiso calc 1 . .
C C12 0.0862(5) 0.773(2) 0.5505(9) 0.070(3) Uani d 1 . .
H H12A 0.110278 0.890299 0.498836 0.105 Uiso calc 1 . .
H H12B 0.036538 0.823367 0.604882 0.105 Uiso calc 1 . .
H H12C 0.064673 0.663981 0.489943 0.105 Uiso calc 1 . .
C C13 0.1868(6) 0.8531(18) 0.7397(10) 0.057(2) Uani d 1 . .
H H13A 0.236811 0.801050 0.793659 0.085 Uiso calc 1 . .
H H13B 0.136364 0.886337 0.797395 0.085 Uiso calc 1 . .
H H13C 0.205292 0.979608 0.692129 0.085 Uiso calc 1 . .
C C14 0.7580(4) 0.2541(10) 0.4900(6) 0.0252(11) Uani d 1 . .
H H14A 0.742071 0.103995 0.496963 0.030 Uiso calc 1 . .
H H14B 0.778492 0.300990 0.578763 0.030 Uiso calc 1 . .
C C15 0.8356(4) 0.2761(11) 0.3927(7) 0.0286(13) Uani d 1 . .
C C16 0.8101(5) 0.1791(14) 0.2603(8) 0.0421(17) Uani d 1 . .
H H16A 0.792902 0.032522 0.273682 0.063 Uiso calc 1 . .
H H16B 0.861192 0.185658 0.200193 0.063 Uiso calc 1 . .
H H16C 0.759767 0.256349 0.221446 0.063 Uiso calc 1 . .
C C17 0.8590(5) 0.5087(15) 0.3764(10) 0.0461(18) Uani d 1 . .
H H17A 0.807805 0.583173 0.337805 0.069 Uiso calc 1 . .
H H17B 0.910499 0.522528 0.317528 0.069 Uiso calc 1 . .
H H17C 0.873678 0.568915 0.463317 0.069 Uiso calc 1 . .
C C18 0.9139(4) 0.1561(13) 0.4534(8) 0.0374(15) Uani d 1 . .
H H18A 0.928094 0.213916 0.541221 0.056 Uiso calc 1 . .
H H18B 0.966108 0.169448 0.395882 0.056 Uiso calc 1 . .
H H18C 0.897962 0.007942 0.462197 0.056 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 0.0425(3) 0.0204(3) 0.0244(3) 0.0068(3) 0.0046(2) 0.0019(3)
N1 0.022(2) 0.021(3) 0.019(3) 0.0001(19) 0.002(2) 0.0024(19)
N2 0.019(2) 0.026(2) 0.021(2) 0.005(2) -0.0004(17) 0.000(2)
N3 0.023(3) 0.025(3) 0.034(3) 0.0024(18) -0.007(3) -0.011(2)
C1 0.022(2) 0.025(3) 0.021(3) 0.001(2) 0.0011(19) -0.001(2)
C2 0.026(3) 0.017(2) 0.037(3) 0.002(3) 0.000(2) -0.007(3)
C3 0.021(3) 0.016(2) 0.024(3) -0.003(2) -0.002(2) -0.004(2)
C4 0.022(2) 0.022(3) 0.019(3) -0.003(2) -0.003(2) 0.000(2)
C5 0.032(3) 0.015(2) 0.031(3) 0.003(2) 0.003(2) 0.000(2)
C6 0.025(3) 0.031(4) 0.026(3) -0.002(2) -0.001(2) 0.006(2)
C7 0.020(2) 0.024(3) 0.023(3) -0.001(2) 0.0019(19) 0.000(2)
C8 0.032(3) 0.025(3) 0.036(4) 0.007(2) 0.010(3) 0.008(3)
C9 0.032(3) 0.019(3) 0.036(3) 0.004(2) 0.004(2) 0.012(3)
C10 0.020(2) 0.038(3) 0.022(3) 0.005(2) 0.001(2) -0.001(2)
C11 0.055(5) 0.054(5) 0.094(8) 0.007(4) 0.053(5) 0.013(6)
C12 0.033(3) 0.141(10) 0.037(4) 0.038(5) 0.006(3) 0.017(5)
C13 0.041(4) 0.076(6) 0.053(5) 0.003(4) 0.013(3) -0.025(5)
C14 0.023(2) 0.027(3) 0.025(3) 0.006(2) 0.000(2) 0.003(2)
C15 0.027(3) 0.028(3) 0.031(3) 0.009(2) 0.001(2) 0.008(3)
C16 0.041(3) 0.058(5) 0.028(4) 0.015(3) -0.001(3) -0.006(3)
C17 0.027(3) 0.046(4) 0.065(5) 0.002(3) 0.007(3) 0.015(4)
C18 0.026(3) 0.046(4) 0.040(4) 0.008(3) -0.002(3) 0.006(3)
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_
_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 C2 . . 105.4(5) ?
C1 N1 C3 . . 125.5(5) ?
C2 N1 C3 . . 129.1(5) ?
N3 N2 C14 . . 121.3(5) ?
C1 N2 N3 . . 110.4(5) ?
C1 N2 C14 . . 128.1(6) ?
C2 N3 N2 . . 104.1(5) ?
N1 C1 H1 . . 126.0 ?
N2 C1 N1 . . 107.9(5) ?
N2 C1 H1 . . 126.0 ?
N1 C2 H2 . . 123.9 ?
N3 C2 N1 . . 112.1(6) ?
N3 C2 H2 . . 123.9 ?
N1 C3 H3A . . 109.4 ?
N1 C3 H3B . . 109.4 ?
N1 C3 C4 . . 111.3(5) ?
H3A C3 H3B . . 108.0 ?
C4 C3 H3A . . 109.4 ?
C4 C3 H3B . . 109.4 ?
C5 C4 C3 . . 119.9(6) ?
C9 C4 C3 . . 121.1(6) ?
C9 C4 C5 . . 119.1(6) ?
C4 C5 H5 . . 120.2 ?
C6 C5 C4 . . 119.7(6) ?
C6 C5 H5 . . 120.2 ?
C5 C6 H6 . . 118.9 ?
C5 C6 C7 . . 122.3(6) ?
C7 C6 H6 . . 118.9 ?
C6 C7 C8 . . 116.9(5) ?
C6 C7 C10 . . 122.5(6) ?
C8 C7 C10 . . 120.6(6) ?
C7 C8 H8 . . 119.3 ?
C7 C8 C9 . . 121.4(6) ?
C9 C8 H8 . . 119.3 ?
C4 C9 C8 . . 120.6(6) ?
C4 C9 H9 . . 119.7 ?
C8 C9 H9 . . 119.7 ?
C11 C10 C7 . . 112.3(6) ?
C11 C10 C13 . . 107.4(8) ?
C12 C10 C7 . . 110.1(5) ?
C12 C10 C11 . . 110.0(8) ?
C12 C10 C13 . . 108.8(8) ?
C13 C10 C7 . . 108.1(5) ?
C10 C11 H11A . . 109.5 ?
C10 C11 H11B . . 109.5 ?
C10 C11 H11C . . 109.5 ?
H11A C11 H11B . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C10 C12 H12A . . 109.5 ?
C10 C12 H12B . . 109.5 ?
C10 C12 H12C . . 109.5 ?
H12A C12 H12B . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C10 C13 H13A . . 109.5 ?
C10 C13 H13B . . 109.5 ?
C10 C13 H13C . . 109.5 ?
H13A C13 H13B . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
N2 C14 H14A . . 108.6 ?
N2 C14 H14B . . 108.6 ?
N2 C14 C15 . . 114.8(5) ?
H14A C14 H14B . . 107.6 ?
C15 C14 H14A . . 108.6 ?
C15 C14 H14B . . 108.6 ?
C14 C15 C17 . . 109.4(6) ?
C16 C15 C14 . . 109.7(6) ?
C16 C15 C17 . . 110.9(7) ?
C16 C15 C18 . . 109.6(6) ?
C18 C15 C14 . . 106.4(5) ?
C18 C15 C17 . . 110.7(6) ?
C15 C16 H16A . . 109.5 ?
C15 C16 H16B . . 109.5 ?
C15 C16 H16C . . 109.5 ?
H16A C16 H16B . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
C15 C17 H17A . . 109.5 ?
C15 C17 H17B . . 109.5 ?
C15 C17 H17C . . 109.5 ?
H17A C17 H17B . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
C15 C18 H18A . . 109.5 ?
C15 C18 H18B . . 109.5 ?
C15 C18 H18C . . 109.5 ?
H18A C18 H18B . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
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
N1 C1 . 1.335(7) ?
N1 C2 . 1.368(9) ?
N1 C3 . 1.460(8) ?
N2 N3 . 1.376(8) ?
N2 C1 . 1.316(8) ?
N2 C14 . 1.453(7) ?
N3 C2 . 1.292(9) ?
C1 H1 . 0.9500 ?
C2 H2 . 0.9500 ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C3 C4 . 1.514(9) ?
C4 C5 . 1.399(9) ?
C4 C9 . 1.378(8) ?
C5 H5 . 0.9500 ?
C5 C6 . 1.391(9) ?
C6 H6 . 0.9500 ?
C6 C7 . 1.396(9) ?
C7 C8 . 1.397(9) ?
C7 C10 . 1.535(7) ?
C8 H8 . 0.9500 ?
C8 C9 . 1.400(9) ?
C9 H9 . 0.9500 ?
C10 C11 . 1.517(12) ?
C10 C12 . 1.513(10) ?
C10 C13 . 1.530(11) ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
C11 H11C . 0.9800 ?
C12 H12A . 0.9800 ?
C12 H12B . 0.9800 ?
C12 H12C . 0.9800 ?
C13 H13A . 0.9800 ?
C13 H13B . 0.9800 ?
C13 H13C . 0.9800 ?
C14 H14A . 0.9900 ?
C14 H14B . 0.9900 ?
C14 C15 . 1.532(8) ?
C15 C16 . 1.517(11) ?
C15 C17 . 1.535(11) ?
C15 C18 . 1.525(8) ?
C16 H16A . 0.9800 ?
C16 H16B . 0.9800 ?
C16 H16C . 0.9800 ?
C17 H17A . 0.9800 ?
C17 H17B . 0.9800 ?
C17 H17C . 0.9800 ?
C18 H18A . 0.9800 ?
C18 H18B . 0.9800 ?
C18 H18C . 0.9800 ?
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
C1 H1 Br1 2_554 0.95 2.57 3.446(6) 154 yes
C2 H2 Br1 1_565 0.95 2.75 3.550(6) 143 yes
C3 H3B Br1 2_564 0.99 2.78 3.599(7) 141 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 C3 C4 C5 . . . . -79.6(7) ?
N1 C3 C4 C9 . . . . 100.4(7) ?
N2 N3 C2 N1 . . . . 1.0(8) ?
N2 C14 C15 C16 . . . . -65.7(7) ?
N2 C14 C15 C17 . . . . 56.2(8) ?
N2 C14 C15 C18 . . . . 175.8(6) ?
N3 N2 C1 N1 . . . . 2.6(7) ?
N3 N2 C14 C15 . . . . -96.1(7) ?
C1 N1 C2 N3 . . . . 0.6(8) ?
C1 N1 C3 C4 . . . . 129.5(6) ?
C1 N2 N3 C2 . . . . -2.2(8) ?
C1 N2 C14 C15 . . . . 89.9(8) ?
C2 N1 C1 N2 . . . . -1.9(7) ?
C2 N1 C3 C4 . . . . -48.7(9) ?
C3 N1 C1 N2 . . . . 179.5(6) ?
C3 N1 C2 N3 . . . . 179.1(7) ?
C3 C4 C5 C6 . . . . -177.3(6) ?
C3 C4 C9 C8 . . . . 177.5(7) ?
C4 C5 C6 C7 . . . . -0.2(10) ?
C5 C4 C9 C8 . . . . -2.5(10) ?
C5 C6 C7 C8 . . . . -2.5(10) ?
C5 C6 C7 C10 . . . . 178.0(6) ?
C6 C7 C8 C9 . . . . 2.8(10) ?
C6 C7 C10 C11 . . . . -4.4(10) ?
C6 C7 C10 C12 . . . . -127.4(8) ?
C6 C7 C10 C13 . . . . 114.0(8) ?
C7 C8 C9 C4 . . . . -0.3(12) ?
C8 C7 C10 C11 . . . . 176.1(8) ?
C8 C7 C10 C12 . . . . 53.1(10) ?
C8 C7 C10 C13 . . . . -65.6(8) ?
C9 C4 C5 C6 . . . . 2.7(9) ?
C10 C7 C8 C9 . . . . -177.7(6) ?
C14 N2 N3 C2 . . . . -177.2(6) ?
C14 N2 C1 N1 . . . . 177.2(6) ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.69(4)
2 0.31(4)