#------------------------------------------------------------------------------
#$Date: 2024-09-11 04:38:19 +0300 (Wed, 11 Sep 2024) $
#$Revision: 294713 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023248.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_2023248
loop_
_publ_author_name
'Yan, Ran'
'Dai, Zhaohua'
'Shlian, Daniel G.'
'Mitchell, Trinit'y D.'
'Loo, Aaron'
'Mulosmani, Kaltrina'
'Upmacis, Rita K.'
_publ_section_title
;
Molecular structure of tris[(6-bromopyridin-2-yl)methyl]amine
;
_journal_coeditor_code EV2008
_journal_issue 10
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024008685
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C18 H15 Br3 N4'
_chemical_formula_moiety 'C18 H15 Br3 N4'
_chemical_formula_sum 'C18 H15 Br3 N4'
_chemical_formula_weight 527.07
_chemical_name_systematic
;
Tris[(6-bromopyridin-2-yl)methyl]amine
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method SHELXL-2019/1
_cell_angle_alpha 79.168(2)
_cell_angle_beta 88.671(2)
_cell_angle_gamma 78.962(2)
_cell_formula_units_Z 2
_cell_length_a 6.2445(8)
_cell_length_b 13.2335(16)
_cell_length_c 13.4984(16)
_cell_measurement_reflns_used 3031
_cell_measurement_temperature 180(2)
_cell_measurement_theta_max 23.83
_cell_measurement_theta_min 3.07
_cell_volume 1075.2(2)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX4 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2019/1 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick 2015a)
;
_diffrn_ambient_temperature 180(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0701
_diffrn_reflns_av_unetI/netI 0.0795
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 11638
_diffrn_reflns_theta_full 25.000
_diffrn_reflns_theta_max 25.026
_diffrn_reflns_theta_min 1.536
_exptl_absorpt_coefficient_mu 5.635
_exptl_absorpt_correction_T_max 0.7461
_exptl_absorpt_correction_T_min 0.5352
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.628
_exptl_crystal_description plate
_exptl_crystal_F_000 512
_exptl_crystal_size_max 0.150
_exptl_crystal_size_mid 0.130
_exptl_crystal_size_min 0.040
_refine_diff_density_max 0.469
_refine_diff_density_min -0.672
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.016
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 226
_refine_ls_number_reflns 3813
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.016
_refine_ls_R_factor_all 0.0884
_refine_ls_R_factor_gt 0.0452
_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^)+(0.0464P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0984
_refine_ls_wR_factor_ref 0.1139
_reflns_number_gt 2434
_reflns_number_total 3813
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ev2008.cif
_cod_data_source_block I
_cod_database_code 2023248
_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 0.485
_shelx_estimated_absorpt_t_max 0.806
_shelx_hkl_file
;
-1 0 0 17.20 3.90
1 0 0 17.30 4.50
1 0 0 12.20 3.00
-2 0 0 638.54 32.80
2 0 0 599.44 33.50
2 0 0 618.44 30.90
-3 0 0 242.68 19.40
3 0 0 240.78 16.80
3 0 0 231.08 20.90
-4 0 0 237.68 22.10
4 0 0 242.28 25.10
4 0 0 225.38 18.80
-5 0 0 1.40 10.60
5 0 0 -4.10 13.20
5 0 0 -10.10 8.20
-6 0 0 196.98 30.80
6 0 0 218.28 34.70
6 0 0 202.08 25.00
-7 0 0 258.47 41.00
7 0 0 277.57 43.10
7 0 0 246.68 35.00
-8 0 0 -4.50 27.00
8 0 0 -11.70 23.70
8 0 0 37.00 29.50
8 -1 0 3.50 30.80
8 -1 0 -31.00 22.40
-8 1 0 3.10 28.40
7 -1 0 -11.80 22.40
7 -1 0 1.50 18.50
-7 1 0 -23.50 20.60
6 -1 0 47.60 24.30
6 -1 0 54.99 17.50
-6 1 0 48.50 18.80
5 -1 0 526.95 42.90
5 -1 0 551.24 35.20
-5 1 0 532.25 38.90
4 -1 0 23.50 9.10
4 -1 0 23.20 12.80
-4 1 0 20.00 10.20
3 -1 0 643.14 40.50
3 -1 0 702.63 35.70
-3 1 0 664.83 37.90
2 -1 0 347.57 20.00
2 -1 0 372.36 23.90
-2 1 0 357.86 21.60
1 -1 0 432.56 23.60
1 -1 0 463.55 21.60
-1 1 0 429.66 22.20
0 -1 0 101.89 6.00
0 1 0 80.39 5.80
0 1 0 92.29 5.70
-1 -1 0 891.41 41.00
1 1 0 847.22 39.80
1 1 0 901.51 40.10
2 1 0 1278.27 59.69
2 1 0 1316.67 61.49
-3 -1 0 1641.44 78.99
3 1 0 1602.24 79.59
3 1 0 1650.83 76.39
-4 -1 0 464.55 32.00
4 1 0 431.66 32.70
4 1 0 466.05 28.70
-5 -1 0 89.09 17.60
5 1 0 95.79 16.30
5 1 0 99.19 22.80
-6 -1 0 -4.80 12.90
6 1 0 16.70 18.00
6 1 0 -1.90 12.00
-7 -1 0 36.80 24.10
7 1 0 40.60 26.00
7 1 0 39.60 20.40
-8 -1 0 -13.60 25.80
8 1 0 13.10 23.60
8 1 0 -3.40 28.90
8 -2 0 162.18 32.90
8 -2 0 104.49 39.10
-8 2 0 47.10 31.50
7 -2 0 20.60 25.70
7 -2 0 32.30 21.00
-7 2 0 23.10 24.00
6 -2 0 85.49 27.50
6 -2 0 50.09 17.60
-6 2 0 40.10 19.40
5 -2 0 242.28 31.90
5 -2 0 259.57 24.40
-5 2 0 304.97 29.30
4 -2 0 116.69 21.70
4 -2 0 58.69 11.50
-4 2 0 77.39 14.40
3 -2 0 397.36 24.30
3 -2 0 392.26 29.90
-3 2 0 415.66 26.80
2 -2 0 1402.56 64.69
2 -2 0 1358.86 68.89
-2 2 0 1418.86 66.09
1 -2 0 8637.84 380.66
1 -2 0 8772.12 383.26
-1 2 0 8978.70 381.16
-1 2 0 8936.71 380.86
0 -2 0 137.09 9.80
0 -2 0 122.69 8.50
0 2 0 150.48 10.10
0 2 0 141.89 9.40
-1 -2 0 22.50 5.30
1 2 0 19.20 3.00
1 2 0 27.20 4.50
1 2 0 20.80 4.30
-2 -2 0 532.75 29.40
-2 -2 0 512.85 26.10
2 2 0 539.65 27.40
2 2 0 530.55 27.70
-3 -2 0 133.09 15.30
3 2 0 135.89 15.10
3 2 0 153.38 13.30
-4 -2 0 138.49 17.90
4 2 0 109.49 14.40
4 2 0 150.78 21.30
-5 -2 0 492.65 37.20
5 2 0 505.75 38.60
5 2 0 517.35 34.20
-6 -2 0 182.78 27.60
6 2 0 198.28 25.30
6 2 0 174.38 29.70
-7 -2 0 26.60 21.40
7 2 0 -31.80 16.10
7 2 0 13.70 21.30
-8 -2 0 -38.80 20.30
8 2 0 7.70 26.50
8 2 0 41.40 25.10
8 -3 0 26.40 33.90
-8 3 0 33.40 28.10
-8 3 0 37.30 28.10
7 -3 0 85.49 32.90
7 -3 0 12.70 21.00
-7 3 0 22.80 24.80
6 -3 0 207.38 35.80
6 -3 0 115.39 21.90
-6 3 0 196.98 30.70
5 -3 0 4.40 16.60
5 -3 0 -6.30 10.30
-5 3 0 -9.70 11.90
4 -3 0 103.39 15.00
4 -3 0 119.69 21.90
-4 3 0 105.39 17.00
3 -3 0 56.69 10.20
3 -3 0 41.50 14.40
-3 3 0 70.79 11.90
2 -3 0 1456.75 70.39
-2 3 0 1359.76 65.39
-2 3 0 1375.96 66.09
1 -3 0 2016.80 94.69
1 -3 0 2056.49 92.59
-1 3 0 2040.90 91.89
-1 3 0 2116.09 92.29
0 -3 0 2046.50 91.39
0 -3 0 2029.90 92.89
0 3 0 1981.70 92.39
0 3 0 2182.98 93.39
-1 -3 0 317.57 19.40
1 3 0 341.27 18.10
1 3 0 309.17 17.50
-2 -3 0 659.73 33.30
-2 -3 0 614.94 30.90
2 3 0 544.05 29.40
2 3 0 604.34 30.70
-3 -3 0 753.32 35.90
-3 -3 0 752.32 41.30
3 3 0 668.83 38.60
3 3 0 724.03 38.10
-4 -3 0 45.80 12.30
4 3 0 56.79 11.50
4 3 0 48.40 12.40
-5 -3 0 384.76 32.10
5 3 0 402.56 32.70
5 3 0 370.06 28.50
-6 -3 0 175.78 27.20
6 3 0 172.88 28.50
6 3 0 225.98 26.60
-7 -3 0 6.80 19.30
7 3 0 18.20 19.30
7 3 0 -18.60 17.60
-8 -3 0 27.40 27.50
8 3 0 51.49 25.80
8 -4 0 70.69 38.10
-8 4 0 9.50 26.90
-8 4 0 -18.20 28.70
7 -4 0 67.39 32.30
-7 4 0 42.80 23.30
-7 4 0 56.19 25.40
6 -4 0 114.99 30.60
-6 4 0 58.09 21.60
-6 4 0 69.29 20.90
5 -4 0 11.40 19.00
-5 4 0 38.40 15.20
-5 4 0 25.80 15.10
4 -4 0 -3.50 14.20
-4 4 0 26.80 12.00
-4 4 0 -3.20 9.40
3 -4 0 393.26 32.30
-3 4 0 398.56 27.00
-3 4 0 421.96 28.00
2 -4 0 2513.65 112.89
2 -4 0 2411.66 118.29
-2 4 0 2574.64 114.59
-2 4 0 2512.35 113.69
1 -4 0 229.78 16.50
1 -4 0 233.78 18.80
-1 4 0 225.28 14.90
-1 4 0 223.98 15.20
0 -4 0 54.89 9.90
0 -4 0 64.89 8.90
0 4 0 77.49 10.90
0 4 0 68.39 9.90
-1 -4 0 1759.32 83.79
1 4 0 1854.41 82.09
1 4 0 1793.62 81.79
-2 -4 0 68.89 10.40
2 4 0 54.09 9.10
2 4 0 58.99 6.50
2 4 0 58.79 8.70
-3 -4 0 193.08 18.50
-3 -4 0 166.78 14.10
3 4 0 168.58 15.10
3 4 0 165.78 14.30
-4 -4 0 236.38 23.70
4 4 0 269.87 21.10
4 4 0 269.67 22.20
-5 -4 0 256.57 27.00
5 4 0 250.57 25.50
5 4 0 290.27 25.40
-6 -4 0 22.70 14.20
6 4 0 57.59 17.00
6 4 0 27.20 16.30
-7 -4 0 30.00 20.50
7 4 0 53.99 21.20
7 4 0 -15.00 16.20
-8 -4 0 -3.80 24.70
8 4 0 -15.10 22.70
8 -5 0 14.70 33.50
-8 5 0 1.10 28.80
-8 5 0 -25.10 32.50
7 -5 0 40.80 33.30
-7 5 0 18.00 20.40
-7 5 0 2.60 22.90
6 -5 0 -2.00 22.40
-6 5 0 47.80 20.10
-6 5 0 -12.80 18.00
5 -5 0 178.68 31.30
-5 5 0 167.88 27.10
-5 5 0 152.98 23.60
4 -5 0 85.39 22.30
-4 5 0 72.39 16.20
-4 5 0 97.39 17.30
3 -5 0 937.31 56.09
-3 5 0 870.91 48.80
-3 5 0 947.51 50.39
2 -5 0 1001.70 50.49
2 -5 0 998.40 55.69
-2 5 0 946.61 50.39
-2 5 0 1089.99 51.79
1 -5 0 24.90 8.60
1 -5 0 34.70 11.10
-1 5 0 37.10 8.10
-1 5 0 23.50 7.30
0 -5 0 35.00 9.80
0 -5 0 29.10 8.00
0 5 0 28.20 8.20
0 5 0 34.70 9.00
-1 -5 0 889.81 46.60
1 5 0 855.91 44.00
1 5 0 932.51 44.70
-2 -5 0 315.77 23.30
2 5 0 362.96 22.80
2 5 0 368.76 22.20
-3 -5 0 17.40 8.50
-3 -5 0 14.20 8.90
3 5 0 12.20 5.90
3 5 0 15.90 6.80
-4 -5 0 1040.30 52.79
-4 -5 0 1030.50 59.19
4 5 0 1088.69 54.49
4 5 0 1057.29 55.09
-5 -5 0 568.94 42.00
5 5 0 638.14 39.00
5 5 0 608.34 39.40
-6 -5 0 -13.80 11.30
6 5 0 20.00 14.00
6 5 0 21.10 13.70
-7 -5 0 -13.00 17.00
7 5 0 -13.80 15.80
-8 -5 0 57.59 30.10
8 5 0 77.49 28.10
7 -6 0 78.99 34.90
-7 6 0 26.00 25.40
-7 6 0 31.90 26.30
6 -6 0 14.00 24.80
-6 6 0 8.50 18.40
-6 6 0 13.20 20.00
5 -6 0 6.10 20.10
-5 6 0 4.50 16.30
-5 6 0 13.10 15.10
4 -6 0 206.08 31.30
-4 6 0 249.48 27.10
-4 6 0 234.08 25.60
3 -6 0 84.29 19.90
3 -6 0 68.59 13.50
-3 6 0 66.49 14.00
-3 6 0 78.09 14.90
2 -6 0 12.60 11.70
2 -6 0 2.90 8.20
-2 6 0 7.00 7.90
-2 6 0 -0.90 6.90
1 -6 0 1695.53 82.99
1 -6 0 1741.73 82.09
-1 6 0 1732.93 81.49
-1 6 0 1633.44 80.99
0 -6 0 447.06 29.80
0 -6 0 433.76 26.70
0 6 0 532.65 30.40
0 6 0 477.05 29.10
-1 -6 0 20.80 9.10
1 6 0 8.60 6.90
1 6 0 7.70 7.50
-2 -6 0 126.49 16.30
2 6 0 151.58 14.90
2 6 0 175.18 16.40
-3 -6 0 80.19 14.10
3 6 0 69.89 12.40
3 6 0 61.59 12.40
-4 -6 0 4.50 9.70
-4 -6 0 21.30 10.10
4 6 0 0.20 7.20
4 6 0 1.20 8.40
-5 -6 0 5.90 9.90
-5 -6 0 15.60 12.30
5 6 0 27.10 11.90
-6 -6 0 97.59 21.00
6 6 0 104.69 21.00
-7 -6 0 11.80 17.20
7 6 0 1.80 17.40
-8 -6 0 37.00 28.70
8 6 0 31.80 25.50
7 -7 0 -2.60 34.00
-7 7 0 12.30 26.40
-7 7 0 2.10 27.90
6 -7 0 -4.70 28.70
-6 7 0 -4.50 21.20
-6 7 0 13.90 21.10
5 -7 0 -22.50 20.30
-5 7 0 11.60 18.10
-5 7 0 -2.50 17.50
4 -7 0 769.52 56.29
-4 7 0 737.53 48.20
-4 7 0 752.52 49.20
3 -7 0 419.26 37.10
3 -7 0 428.36 30.00
-3 7 0 426.36 32.20
-3 7 0 423.26 31.10
2 -7 0 10.00 13.30
2 -7 0 29.50 11.70
-2 7 0 27.30 10.60
-2 7 0 15.20 9.10
1 -7 0 163.58 18.70
1 -7 0 140.29 18.30
-1 7 0 173.38 19.00
-1 7 0 143.29 18.70
0 -7 0 821.92 45.30
0 -7 0 886.51 49.40
0 7 0 948.31 48.70
0 7 0 920.41 48.70
-1 -7 0 76.49 8.00
-1 -7 0 89.79 15.50
1 7 0 88.39 14.00
1 7 0 107.79 15.10
-2 -7 0 33.70 12.50
2 7 0 34.50 11.40
2 7 0 19.30 9.10
-3 -7 0 1881.11 92.79
3 7 0 1905.31 90.59
3 7 0 1858.11 91.19
-4 -7 0 1132.49 63.39
-4 -7 0 1133.79 59.09
4 7 0 1038.00 57.89
-5 -7 0 8.00 12.70
-5 -7 0 47.10 13.80
5 7 0 24.20 12.60
-6 -7 0 11.10 14.80
6 7 0 1.10 13.30
-7 -7 0 20.20 18.00
7 7 0 23.90 20.40
-8 -7 0 -16.40 24.70
8 7 0 -18.30 24.10
7 -8 0 -4.70 36.40
-7 8 0 12.30 29.10
6 -8 0 5.60 31.40
-6 8 0 36.90 23.70
-6 8 0 2.50 22.90
5 -8 0 11.40 26.20
-5 8 0 16.90 19.60
-5 8 0 45.50 20.80
4 -8 0 -33.70 17.80
-4 8 0 -10.30 15.40
-4 8 0 15.50 16.30
3 -8 0 65.69 20.00
3 -8 0 26.20 15.00
-3 8 0 67.09 16.80
-3 8 0 64.69 16.70
2 -8 0 427.46 30.90
2 -8 0 400.56 34.00
-2 8 0 347.27 29.60
-2 8 0 427.26 30.60
1 -8 0 170.88 20.50
1 -8 0 136.29 19.50
-1 8 0 120.99 17.90
-1 8 0 74.19 17.60
0 -8 0 161.78 20.70
0 -8 0 167.38 17.70
0 8 0 181.38 20.50
0 8 0 155.78 20.30
-1 -8 0 22.90 6.20
-1 -8 0 37.30 13.40
1 8 0 23.40 11.10
1 8 0 18.00 10.60
-2 -8 0 -15.60 9.30
2 8 0 -3.40 9.40
2 8 0 -2.40 9.20
-3 -8 0 186.38 23.00
3 8 0 196.88 21.10
3 8 0 177.98 21.90
-4 -8 0 126.69 21.90
-4 -8 0 115.59 19.50
4 8 0 83.99 15.00
-5 -8 0 18.20 16.50
-5 -8 0 51.39 14.90
5 8 0 28.30 13.50
-6 -8 0 -6.00 14.00
6 8 0 -7.80 13.00
-7 -8 0 33.40 21.20
7 8 0 89.49 26.80
-8 -8 0 32.80 26.40
8 8 0 -6.00 24.20
6 -9 0 -22.20 32.00
-6 9 0 3.70 26.30
-6 9 0 -18.20 30.50
5 -9 0 160.48 37.80
-5 9 0 162.28 28.60
-5 9 0 139.19 29.80
4 -9 0 135.79 32.00
-4 9 0 94.99 24.40
-4 9 0 208.48 28.90
3 -9 0 17.30 15.10
3 -9 0 8.00 18.20
-3 9 0 42.20 17.70
-3 9 0 23.70 16.10
2 -9 0 220.68 26.00
2 -9 0 223.18 28.50
-2 9 0 194.58 25.50
-2 9 0 162.88 25.60
1 -9 0 269.37 25.90
1 -9 0 247.88 26.70
-1 9 0 311.47 27.80
-1 9 0 246.08 28.20
0 -9 0 2.90 10.20
0 -9 0 5.00 12.50
0 9 0 21.80 12.00
0 9 0 2.60 12.00
-1 -9 0 143.19 22.80
-1 -9 0 106.39 11.50
1 9 0 107.59 18.50
1 9 0 113.29 18.30
-2 -9 0 707.33 43.60
2 9 0 611.24 40.70
2 9 0 595.24 39.30
-3 -9 0 417.26 34.90
3 9 0 437.86 32.70
3 9 0 400.66 33.00
-4 -9 0 72.29 17.30
-4 -9 0 93.99 20.00
4 9 0 73.49 16.00
-5 -9 0 73.29 19.50
-5 -9 0 55.99 20.00
5 9 0 73.99 17.90
-6 -9 0 23.00 17.00
6 9 0 1.30 15.20
-7 -9 0 -18.40 18.00
7 9 0 0.50 19.60
-8 -9 0 30.20 26.90
8 9 0 -13.00 24.10
6 -10 0 8.60 35.90
5 -10 0 2.60 31.00
-5 10 0 -8.60 21.80
-5 10 0 -5.50 24.10
4 -10 0 -15.50 24.40
-4 10 0 3.00 21.20
-4 10 0 -8.40 19.80
3 -10 0 124.59 28.00
3 -10 0 107.59 22.00
-3 10 0 89.89 23.50
-3 10 0 111.49 24.90
2 -10 0 13.60 15.80
2 -10 0 32.20 19.30
-2 10 0 2.70 16.80
-2 10 0 -0.70 15.20
1 -10 0 46.00 17.60
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2 -1 17 -5.20 27.30
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3 -4 -17 -0.60 22.60
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3 -5 -17 24.90 23.80
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3 -6 -17 71.29 35.60
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3 -7 -17 6.80 35.60
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2 -1 -18 -32.40 23.30
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1 -1 -18 32.70 28.90
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0 -1 -18 11.50 29.10
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0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 3045
_shelx_res_file
;
TITL TPABr3
tpa821_sq.res
created by SHELXL-2019/1 at 16:08:33 on 21-Aug-2024
CELL 0.71073 6.2445 13.2335 13.4984 79.168 88.671 78.962
ZERR 2.000 0.0008 0.0016 0.0016 0.002 0.002 0.002
LATT 1
SFAC C H N BR
UNIT 36 30 8 6
TEMP -93.16
SIZE 0.04 0.13 0.15
L.S. 5 0 26
BOND
FMAP 2
WPDB -1
SHEL 999 0.84
OMIT 0 1 0
OMIT 0 -1 1
PLAN 20
CONF
ABIN
ACTA 50
REM EXTI 0.000000
WGHT 0.046400
FVAR 0.48501
N1 3 0.201917 0.356643 0.533685 11.00000 0.03110 0.04164 =
0.03814 -0.01292 0.00060 -0.00822
N2 3 0.296205 0.099183 0.219064 11.00000 0.02417 0.02865 =
0.04760 -0.01315 0.00234 -0.00589
N3 3 0.147758 0.575699 0.091142 11.00000 0.02669 0.03720 =
0.02639 -0.00720 -0.00260 -0.00758
N4 3 0.281419 0.348452 0.280549 11.00000 0.02649 0.03386 =
0.02654 -0.00903 -0.00252 -0.00272
C1 1 0.188765 0.416018 0.351693 11.00000 0.03211 0.04557 =
0.02574 -0.00848 -0.00036 -0.01013
AFIX 23
H1B 2 0.033813 0.410977 0.363630 11.00000 -1.20000
H1C 2 0.195167 0.489831 0.322584 11.00000 -1.20000
AFIX 0
C2 1 0.233764 0.243521 0.309996 11.00000 0.03463 0.03407 =
0.04556 -0.00704 0.00754 -0.01217
AFIX 23
H2B 2 0.082095 0.244305 0.289608 11.00000 -1.20000
H2C 2 0.245189 0.222326 0.384317 11.00000 -1.20000
AFIX 0
C3 1 0.201453 0.394805 0.177418 11.00000 0.02135 0.04612 =
0.04172 -0.01237 0.00013 -0.01084
AFIX 23
H3B 2 0.040155 0.413243 0.177665 11.00000 -1.20000
H3C 2 0.242935 0.342154 0.133650 11.00000 -1.20000
AFIX 0
C11 1 0.314896 0.383101 0.450801 11.00000 0.02736 0.04745 =
0.03940 -0.01986 0.00405 -0.00987
C12 1 0.539273 0.379837 0.453469 11.00000 0.03709 0.08118 =
0.04650 -0.02014 0.00429 -0.02550
AFIX 43
H12A 2 0.615838 0.397766 0.393057 11.00000 -1.20000
AFIX 0
C13 1 0.648122 0.350273 0.544861 11.00000 0.02235 0.10896 =
0.06157 -0.02203 -0.00178 -0.02413
AFIX 43
H13A 2 0.800619 0.348382 0.548534 11.00000 -1.20000
AFIX 0
C14 1 0.533021 0.323449 0.630982 11.00000 0.03179 0.07754 =
0.04378 -0.01711 -0.00844 -0.00748
AFIX 43
H14A 2 0.602337 0.302168 0.695444 11.00000 -1.20000
AFIX 0
C15 1 0.314257 0.328990 0.619020 11.00000 0.03938 0.05145 =
0.04219 -0.01668 0.00205 -0.01395
C21 1 0.388090 0.164286 0.262189 11.00000 0.02865 0.03299 =
0.03015 -0.00496 0.00086 -0.00437
C22 1 0.611132 0.158542 0.263515 11.00000 0.02877 0.04952 =
0.04757 -0.01233 0.00235 -0.02070
AFIX 43
H22A 2 0.671672 0.206481 0.293351 11.00000 -1.20000
AFIX 0
C23 1 0.746102 0.082644 0.221192 11.00000 0.02329 0.05001 =
0.06068 -0.00995 0.00406 -0.00815
AFIX 43
H23A 2 0.899873 0.077695 0.221881 11.00000 -1.20000
AFIX 0
C24 1 0.654052 0.014336 0.178020 11.00000 0.02039 0.04913 =
0.06352 -0.01680 0.00293 -0.00065
AFIX 43
H24A 2 0.740674 -0.039675 0.149128 11.00000 -1.20000
AFIX 0
C25 1 0.431074 0.028510 0.179015 11.00000 0.03331 0.03691 =
0.05152 -0.00337 -0.00728 -0.00979
C31 1 0.291421 0.491574 0.133982 11.00000 0.02822 0.03726 =
0.01949 -0.00920 0.00051 -0.00881
C32 1 0.514160 0.491727 0.138182 11.00000 0.02243 0.04157 =
0.03822 -0.00765 -0.00020 -0.00701
AFIX 43
H32A 2 0.612525 0.430920 0.170020 11.00000 -1.20000
AFIX 0
C33 1 0.589424 0.580209 0.096048 11.00000 0.02424 0.04353 =
0.04380 -0.01654 0.00297 -0.01116
AFIX 43
H33A 2 0.740996 0.581301 0.097381 11.00000 -1.20000
AFIX 0
C34 1 0.442068 0.668646 0.051195 11.00000 0.03281 0.04728 =
0.03741 -0.01680 0.00939 -0.01829
AFIX 43
H34A 2 0.488557 0.731787 0.021853 11.00000 -1.20000
AFIX 0
C35 1 0.225317 0.660515 0.051250 11.00000 0.02856 0.04044 =
0.03256 -0.01583 0.00112 -0.00971
BR1 4 0.147826 0.288522 0.736193 11.00000 0.04573 0.08903 =
0.03828 -0.00857 0.00411 -0.00836
BR2 4 0.292230 -0.062065 0.117337 11.00000 0.04283 0.05829 =
0.08893 -0.04104 -0.00460 -0.00872
BR3 4 0.011777 0.777915 -0.008584 11.00000 0.03434 0.04234 =
0.05741 -0.00092 -0.00853 -0.00949
HKLF 4
REM TPABr3
REM wR2 = 0.1139, GooF = S = 1.016, Restrained GooF = 1.016 for all data
REM R1 = 0.0452 for 2434 Fo > 4sig(Fo) and 0.0884 for all 3813 data
REM 226 parameters refined using 0 restraints
END
WGHT 0.0463 0.0000
REM Highest difference peak 0.469, deepest hole -0.672, 1-sigma level 0.101
Q1 1 0.1416 0.1985 0.7171 11.00000 0.05 0.47
Q2 1 0.2772 -0.1710 0.1250 11.00000 0.05 0.41
Q3 1 0.1665 0.3805 0.7368 11.00000 0.05 0.39
Q4 1 0.4486 -0.1422 0.1155 11.00000 0.05 0.38
Q5 1 0.3599 0.0344 0.1357 11.00000 0.05 0.38
Q6 1 0.0677 0.2343 0.6976 11.00000 0.05 0.38
Q7 1 0.0807 0.7834 0.0656 11.00000 0.05 0.37
Q8 1 -0.0355 0.7566 -0.1031 11.00000 0.05 0.36
Q9 1 0.0391 0.2580 0.6877 11.00000 0.05 0.36
Q10 1 0.2379 0.3379 0.6594 11.00000 0.05 0.35
Q11 1 0.2272 -0.0868 0.2006 11.00000 0.05 0.35
Q12 1 0.1985 0.5867 0.0421 11.00000 0.05 0.35
Q13 1 0.1590 0.2038 0.8200 11.00000 0.05 0.35
Q14 1 0.7356 0.2814 0.4365 11.00000 0.05 0.34
Q15 1 0.0908 0.5787 0.0572 11.00000 0.05 0.34
Q16 1 0.3577 0.2456 0.7968 11.00000 0.05 0.33
Q17 1 0.7765 0.0987 0.1137 11.00000 0.05 0.33
Q18 1 0.5636 0.4525 0.1792 11.00000 0.05 0.33
Q19 1 0.1206 0.0340 0.0724 11.00000 0.05 0.33
Q20 1 0.0389 0.7157 -0.0081 11.00000 0.05 0.32
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_shelx_res_checksum 59807
_shelx_fab_file
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2 0 0 7.47 0.00
3 0 0 -1.03 0.00
4 0 0 0.22 0.00
5 0 0 0.16 0.00
6 0 0 -0.59 0.00
7 0 0 -1.51 0.00
8 0 0 -0.49 0.00
-8 1 0 -0.51 0.00
-7 1 0 -0.03 0.00
-6 1 0 -0.74 0.00
-5 1 0 0.23 0.00
-4 1 0 -0.10 0.00
-3 1 0 -1.51 0.00
-2 1 0 4.44 0.00
-1 1 0 -1.86 0.00
0 1 0 51.20 0.00
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2 1 0 7.26 0.00
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7 1 0 -1.78 0.00
8 1 0 -1.08 0.00
-8 2 0 -0.76 0.00
-7 2 0 1.56 0.00
-6 2 0 -0.39 0.00
-5 2 0 0.16 0.00
-4 2 0 -0.50 0.00
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0 6 19 -2.37 0.00
1 6 19 -0.55 0.00
0 7 19 -1.63 0.00
1 7 19 -0.13 0.00
3 -14 1 1.63 0.00
6 9 11 -0.36 0.00
0 0 0 0.00 0.00
# SQUEEZE RESULTS (Version = 100117)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.030 0.000 0.500 167 47 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details
)
TITL i1_a.res in P-1
CELL 6.2445 13.2335 13.4984 79.17 88.67 78.96
SPGR P-1
# Solvent Accessible Volume = 168
# Electrons Found in S.A.V. = 47
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.469 0.941 0.450 ! 3.79 eA-3
C102 0.096 0.906 0.416 ! 3.24 eA-3
C103 0.625 0.087 0.529 ! 2.85 eA-3
C104 0.206 0.913 0.450 ! 2.71 eA-3
C105 0.500 1.000 0.500 ! 2.40 eA-3
C106 0.963 0.095 0.520 ! 2.19 eA-3
C107 0.948 0.970 0.488 ! 2.17 eA-3
C108 0.092 1.003 0.483 ! 2.08 eA-3
C109 0.937 0.939 0.453 ! 1.94 eA-3
C110 0.037 0.957 0.439 ! 1.87 eA-3
C111 0.243 0.968 0.490 ! 1.83 eA-3
Q112 0.910 0.233 0.053 ! 1.83 eA-3
C113 0.278 0.020 0.506 ! 1.81 eA-3
Q114 0.625 0.079 0.346 ! 1.65 eA-3
C115 0.573 0.928 0.405 ! 1.55 eA-3
C116 0.819 0.914 0.482 ! 1.52 eA-3
Q117 0.566 0.609 0.067 ! 1.52 eA-3
Q118 0.066 0.784 0.033 ! 1.51 eA-3
Q119 0.277 0.626 0.200 ! 1.48 eA-3
Q120 0.063 0.237 0.035 ! 1.47 eA-3
Q121 0.350 0.888 0.123 ! 1.46 eA-3
Q122 0.881 0.393 0.920 ! 1.44 eA-3
C123 0.600 1.006 0.457 ! 1.42 eA-3
Q124 0.289 0.403 0.258 ! 1.41 eA-3
Q125 0.315 0.685 0.065 ! 1.39 eA-3
Q126 0.806 0.048 0.438 ! 1.39 eA-3
Q127 0.604 0.627 0.108 ! 1.37 eA-3
Q128 0.192 0.236 0.343 ! 1.36 eA-3
Q129 0.281 0.357 0.434 ! 1.35 eA-3
Q130 0.557 0.473 0.156 ! 1.35 eA-3
Q131 0.027 0.171 0.017 ! 1.33 eA-3
Q132 0.438 0.075 0.076 ! 1.31 eA-3
Q133 0.373 0.940 0.143 ! 1.30 eA-3
Q134 0.902 0.749 0.296 ! 1.30 eA-3
Q135 0.885 1.004 0.401 ! 1.30 eA-3
Q136 0.873 0.627 0.073 ! 1.29 eA-3
C137 0.750 0.905 0.418 ! 1.29 eA-3
Q138 1.005 0.566 0.362 ! 1.29 eA-3
Q139 0.225 0.359 0.173 ! 1.29 eA-3
Q140 0.475 0.185 0.260 ! 1.27 eA-3
Q141 0.968 0.302 0.062 ! 1.27 eA-3
Q142 0.158 0.862 0.377 ! 1.27 eA-3
Q143 0.250 0.966 0.137 ! 1.26 eA-3
Q144 0.448 0.640 0.287 ! 1.25 eA-3
Q145 0.720 0.498 0.217 ! 1.24 eA-3
Q146 0.498 0.450 0.180 ! 1.23 eA-3
Q147 0.943 0.330-0.005 ! 1.23 eA-3
Q148 0.336 0.745 0.171 ! 1.22 eA-3
Q149 0.777 0.075 0.905 ! 1.22 eA-3
Q150 0.092 0.922 0.295 ! 1.22 eA-3
Q151 0.787 0.043 0.373 ! 1.21 eA-3
C152 0.067 0.063 0.434 ! 1.20 eA-3
Q153 0.247 0.955 0.373 ! 1.20 eA-3
Q154 0.105 0.621 0.200 ! 1.20 eA-3
Q155 0.908 0.216 0.235 ! 1.20 eA-3
Q156 0.818 0.859 0.982 ! 1.19 eA-3
Q157 0.794 0.317 0.033 ! 1.19 eA-3
Q158 0.244 0.871 0.404 ! 1.19 eA-3
Q159 0.470 0.581 0.284 ! 1.17 eA-3
Q160 0.082 0.216 0.977 ! 1.17 eA-3
Q161 0.560 0.508 0.315 ! 1.16 eA-3
Q162 0.476 0.177 0.435 ! 1.16 eA-3
Q163 0.134 0.542 0.081 ! 1.16 eA-3
Q164 0.730 0.467 0.156 ! 1.16 eA-3
Q165 0.842 0.810 0.283 ! 1.16 eA-3
Q166 0.474 0.286 0.267 ! 1.15 eA-3
Q167 0.531 0.357 0.281 ! 1.13 eA-3
Q168 0.655 0.069 0.467 ! 1.13 eA-3
Q169 0.908 0.784 0.489 ! 1.13 eA-3
Q170 0.367 0.811 0.120 ! 1.13 eA-3
Q171 0.625 0.054 0.981 ! 1.13 eA-3
Q172 0.754 0.310 0.441 ! 1.13 eA-3
Q173 0.182 0.637 0.159 ! 1.12 eA-3
Q174 0.259 0.146 0.954 ! 1.12 eA-3
Q175 0.939 0.776 0.142 ! 1.11 eA-3
Q176 0.159 0.725 0.052 ! 1.10 eA-3
Q177 0.773 0.173 0.453 ! 1.10 eA-3
Q178 1.006 0.642 0.244 ! 1.10 eA-3
Q179 0.308 0.827 0.173 ! 1.10 eA-3
Q180 0.378 0.028 0.255 ! 1.10 eA-3
Q181 0.217 0.593 0.408 ! 1.10 eA-3
Q182 0.182 0.955 0.743 ! 1.10 eA-3
Q183 0.825 0.562 0.154 ! 1.09 eA-3
Q184 0.842 0.374 0.316 ! 1.09 eA-3
Q185 0.528 0.134 0.059 ! 1.09 eA-3
Q186 0.252 0.404 0.207 ! 1.08 eA-3
Q187 0.131 0.987 0.282 ! 1.08 eA-3
Q188 0.953 0.201 0.385 ! 1.08 eA-3
Q189 0.065 0.576 0.035 ! 1.08 eA-3
Q190 0.280 0.498 0.167 ! 1.08 eA-3
Q191 0.831 0.828 0.218 ! 1.08 eA-3
Q192 0.713 0.691 0.250 ! 1.08 eA-3
Q193 0.371 0.186 0.860 ! 1.08 eA-3
Q194 0.913 0.343 0.090 ! 1.08 eA-3
Q195 0.712 0.172 0.374 ! 1.08 eA-3
Q196 0.502 0.403 0.916 ! 1.08 eA-3
Q197 0.344 0.804 0.283 ! 1.07 eA-3
Q198 0.757 0.419 0.264 ! 1.07 eA-3
Q199 0.225 0.284 0.699 ! 1.07 eA-3
)
;
_shelx_fab_checksum 17474
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
N N1 0.2019(7) 0.3566(4) 0.5337(3) 0.0361(12) Uani d 1 . .
N N2 0.2962(7) 0.0992(3) 0.2191(3) 0.0326(11) Uani d 1 . .
N N3 0.1478(7) 0.5757(4) 0.0911(3) 0.0297(11) Uani d 1 . .
N N4 0.2814(7) 0.3485(3) 0.2805(3) 0.0289(11) Uani d 1 . .
C C1 0.1888(9) 0.4160(5) 0.3517(4) 0.0339(14) Uani d 1 . .
H H1B 0.033813 0.410977 0.363630 0.041 Uiso calc 1 . .
H H1C 0.195167 0.489831 0.322584 0.041 Uiso calc 1 . .
C C2 0.2338(9) 0.2435(4) 0.3100(4) 0.0375(14) Uani d 1 . .
H H2B 0.082095 0.244305 0.289608 0.045 Uiso calc 1 . .
H H2C 0.245189 0.222326 0.384317 0.045 Uiso calc 1 . .
C C3 0.2015(8) 0.3948(4) 0.1774(4) 0.0352(14) Uani d 1 . .
H H3B 0.040155 0.413243 0.177665 0.042 Uiso calc 1 . .
H H3C 0.242935 0.342154 0.133650 0.042 Uiso calc 1 . .
C C11 0.3149(9) 0.3831(5) 0.4508(4) 0.0362(14) Uani d 1 . .
C C12 0.5393(10) 0.3798(5) 0.4535(5) 0.0520(18) Uani d 1 . .
H H12A 0.615838 0.397766 0.393057 0.062 Uiso calc 1 . .
C C13 0.6481(10) 0.3503(6) 0.5449(5) 0.062(2) Uani d 1 . .
H H13A 0.800619 0.348382 0.548534 0.074 Uiso calc 1 . .
C C14 0.5330(9) 0.3234(5) 0.6310(5) 0.0505(18) Uani d 1 . .
H H14A 0.602337 0.302168 0.695444 0.061 Uiso calc 1 . .
C C15 0.3143(10) 0.3290(5) 0.6190(4) 0.0426(15) Uani d 1 . .
C C21 0.3881(8) 0.1643(4) 0.2622(4) 0.0309(13) Uani d 1 . .
C C22 0.6111(9) 0.1585(5) 0.2635(4) 0.0398(15) Uani d 1 . .
H H22A 0.671672 0.206481 0.293351 0.048 Uiso calc 1 . .
C C23 0.7461(9) 0.0826(5) 0.2212(4) 0.0446(16) Uani d 1 . .
H H23A 0.899873 0.077695 0.221881 0.054 Uiso calc 1 . .
C C24 0.6541(9) 0.0143(5) 0.1780(5) 0.0444(16) Uani d 1 . .
H H24A 0.740674 -0.039675 0.149128 0.053 Uiso calc 1 . .
C C25 0.4311(9) 0.0285(5) 0.1790(5) 0.0407(15) Uani d 1 . .
C C31 0.2914(8) 0.4916(4) 0.1340(4) 0.0275(13) Uani d 1 . .
C C32 0.5142(8) 0.4917(5) 0.1382(4) 0.0339(14) Uani d 1 . .
H H32A 0.612525 0.430920 0.170020 0.041 Uiso calc 1 . .
C C33 0.5894(9) 0.5802(4) 0.0960(4) 0.0355(14) Uani d 1 . .
H H33A 0.740996 0.581301 0.097381 0.043 Uiso calc 1 . .
C C34 0.4421(9) 0.6686(5) 0.0512(4) 0.0367(15) Uani d 1 . .
H H34A 0.488557 0.731787 0.021853 0.044 Uiso calc 1 . .
C C35 0.2253(8) 0.6605(5) 0.0512(4) 0.0322(14) Uani d 1 . .
Br Br1 0.14783(11) 0.28852(6) 0.73619(5) 0.0588(2) Uani d 1 . .
Br Br2 0.29223(11) -0.06206(6) 0.11734(6) 0.0598(2) Uani d 1 . .
Br Br3 0.01178(10) 0.77792(5) -0.00858(5) 0.0454(2) Uani d 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
N1 0.031(3) 0.042(3) 0.038(3) -0.008(2) 0.001(2) -0.013(2)
N2 0.024(2) 0.029(3) 0.048(3) -0.006(2) 0.002(2) -0.013(2)
N3 0.027(3) 0.037(3) 0.026(2) -0.008(2) -0.003(2) -0.007(2)
N4 0.026(2) 0.034(3) 0.027(3) -0.003(2) -0.0025(19) -0.009(2)
C1 0.032(3) 0.046(4) 0.026(3) -0.010(3) 0.000(2) -0.008(3)
C2 0.035(3) 0.034(4) 0.046(4) -0.012(3) 0.008(3) -0.007(3)
C3 0.021(3) 0.046(4) 0.042(4) -0.011(3) 0.000(2) -0.012(3)
C11 0.027(3) 0.047(4) 0.039(4) -0.010(3) 0.004(3) -0.020(3)
C12 0.037(4) 0.081(5) 0.047(4) -0.026(4) 0.004(3) -0.020(4)
C13 0.022(3) 0.109(6) 0.062(5) -0.024(4) -0.002(3) -0.022(4)
C14 0.032(4) 0.078(5) 0.044(4) -0.007(3) -0.008(3) -0.017(4)
C15 0.039(4) 0.051(4) 0.042(4) -0.014(3) 0.002(3) -0.017(3)
C21 0.029(3) 0.033(3) 0.030(3) -0.004(3) 0.001(2) -0.005(3)
C22 0.029(3) 0.050(4) 0.048(4) -0.021(3) 0.002(3) -0.012(3)
C23 0.023(3) 0.050(4) 0.061(4) -0.008(3) 0.004(3) -0.010(4)
C24 0.020(3) 0.049(4) 0.064(4) -0.001(3) 0.003(3) -0.017(3)
C25 0.033(3) 0.037(4) 0.052(4) -0.010(3) -0.007(3) -0.003(3)
C31 0.028(3) 0.037(4) 0.019(3) -0.009(3) 0.001(2) -0.009(3)
C32 0.022(3) 0.042(4) 0.038(3) -0.007(3) 0.000(2) -0.008(3)
C33 0.024(3) 0.044(4) 0.044(4) -0.011(3) 0.003(3) -0.017(3)
C34 0.033(3) 0.047(4) 0.037(3) -0.018(3) 0.009(3) -0.017(3)
C35 0.029(3) 0.040(4) 0.033(3) -0.010(3) 0.001(2) -0.016(3)
Br1 0.0457(4) 0.0890(6) 0.0383(4) -0.0084(4) 0.0041(3) -0.0086(4)
Br2 0.0428(4) 0.0583(5) 0.0889(6) -0.0087(3) -0.0046(4) -0.0410(4)
Br3 0.0343(4) 0.0423(4) 0.0574(4) -0.0095(3) -0.0085(3) -0.0009(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
N N 0.0061 0.0033 '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'
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
C15 N1 C11 . . 116.0(5) ?
C25 N2 C21 . . 116.3(5) ?
C35 N3 C31 . . 117.2(4) ?
C2 N4 C1 . . 111.4(4) ?
C2 N4 C3 . . 110.4(4) ?
C1 N4 C3 . . 110.9(4) ?
N4 C1 C11 . . 110.2(4) ?
N4 C2 C21 . . 111.9(4) ?
N4 C3 C31 . . 112.6(4) ?
N1 C11 C12 . . 122.4(5) ?
N1 C11 C1 . . 117.0(5) ?
C12 C11 C1 . . 120.6(5) ?
C13 C12 C11 . . 119.0(6) ?
C12 C13 C14 . . 119.1(6) ?
C15 C14 C13 . . 116.6(6) ?
N1 C15 C14 . . 126.8(6) ?
N1 C15 Br1 . . 114.9(4) ?
C14 C15 Br1 . . 118.3(5) ?
N2 C21 C22 . . 121.9(5) ?
N2 C21 C2 . . 116.2(5) ?
C22 C21 C2 . . 121.9(5) ?
C21 C22 C23 . . 119.7(5) ?
C24 C23 C22 . . 119.0(5) ?
C25 C24 C23 . . 116.4(6) ?
N2 C25 C24 . . 126.7(5) ?
N2 C25 Br2 . . 114.8(4) ?
C24 C25 Br2 . . 118.5(5) ?
N3 C31 C32 . . 122.2(5) ?
N3 C31 C3 . . 116.7(4) ?
C32 C31 C3 . . 121.1(5) ?
C33 C32 C31 . . 119.3(5) ?
C32 C33 C34 . . 119.3(5) ?
C35 C34 C33 . . 116.9(5) ?
N3 C35 C34 . . 125.1(5) ?
N3 C35 Br3 . . 115.1(4) ?
C34 C35 Br3 . . 119.8(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
N1 C15 . 1.317(7) ?
N1 C11 . 1.335(7) ?
N2 C25 . 1.320(7) ?
N2 C21 . 1.343(6) ?
N3 C35 . 1.324(6) ?
N3 C31 . 1.334(6) ?
N4 C2 . 1.456(6) ?
N4 C1 . 1.468(6) ?
N4 C3 . 1.469(6) ?
C1 C11 . 1.516(7) ?
C2 C21 . 1.511(7) ?
C3 C31 . 1.509(7) ?
C11 C12 . 1.395(8) ?
C12 C13 . 1.376(8) ?
C13 C14 . 1.378(8) ?
C14 C15 . 1.366(8) ?
C15 Br1 . 1.920(6) ?
C21 C22 . 1.381(7) ?
C22 C23 . 1.384(8) ?
C23 C24 . 1.378(8) ?
C24 C25 . 1.369(7) ?
C25 Br2 . 1.920(6) ?
C31 C32 . 1.394(7) ?
C32 C33 . 1.365(7) ?
C33 C34 . 1.389(8) ?
C34 C35 . 1.378(7) ?
C35 Br3 . 1.905(6) ?
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
C2 N4 C1 C11 . . . . 71.5(5) ?
C3 N4 C1 C11 . . . . -165.2(4) ?
C1 N4 C2 C21 . . . . -159.9(4) ?
C3 N4 C2 C21 . . . . 76.5(5) ?
C2 N4 C3 C31 . . . . -166.5(4) ?
C1 N4 C3 C31 . . . . 69.6(5) ?
C15 N1 C11 C12 . . . . 1.3(9) ?
C15 N1 C11 C1 . . . . -179.6(5) ?
N4 C1 C11 N1 . . . . -122.2(5) ?
N4 C1 C11 C12 . . . . 57.0(7) ?
N1 C11 C12 C13 . . . . -1.3(10) ?
C1 C11 C12 C13 . . . . 179.6(6) ?
C11 C12 C13 C14 . . . . 0.8(11) ?
C12 C13 C14 C15 . . . . -0.4(10) ?
C11 N1 C15 C14 . . . . -0.9(9) ?
C11 N1 C15 Br1 . . . . -178.7(4) ?
C13 C14 C15 N1 . . . . 0.5(10) ?
C13 C14 C15 Br1 . . . . 178.2(5) ?
C25 N2 C21 C22 . . . . 0.8(8) ?
C25 N2 C21 C2 . . . . -178.7(5) ?
N4 C2 C21 N2 . . . . -132.6(5) ?
N4 C2 C21 C22 . . . . 47.9(7) ?
N2 C21 C22 C23 . . . . -1.3(9) ?
C2 C21 C22 C23 . . . . 178.2(5) ?
C21 C22 C23 C24 . . . . 0.3(9) ?
C22 C23 C24 C25 . . . . 1.1(9) ?
C21 N2 C25 C24 . . . . 0.7(9) ?
C21 N2 C25 Br2 . . . . -179.5(4) ?
C23 C24 C25 N2 . . . . -1.7(10) ?
C23 C24 C25 Br2 . . . . 178.6(5) ?
C35 N3 C31 C32 . . . . 0.6(7) ?
C35 N3 C31 C3 . . . . -178.9(4) ?
N4 C3 C31 N3 . . . . -131.2(5) ?
N4 C3 C31 C32 . . . . 49.3(7) ?
N3 C31 C32 C33 . . . . -0.9(8) ?
C3 C31 C32 C33 . . . . 178.6(5) ?
C31 C32 C33 C34 . . . . 0.9(8) ?
C32 C33 C34 C35 . . . . -0.7(8) ?
C31 N3 C35 C34 . . . . -0.4(8) ?
C31 N3 C35 Br3 . . . . -179.9(4) ?
C33 C34 C35 N3 . . . . 0.5(8) ?
C33 C34 C35 Br3 . . . . 180.0(4) ?