#------------------------------------------------------------------------------
#$Date: 2024-08-01 05:14:56 +0300 (Thu, 01 Aug 2024) $
#$Revision: 293618 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023213.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_2023213
loop_
_publ_author_name
'Hakimov, Muminjon'
'Khozhimatova, Shakhnoza'
'Ortikov, Ilkhomjon'
'Abdugafurov, Ibragimdjan'
'Tojiboev, Akmaljon'
_publ_section_title
;
Synthesis, crystal structure and Hirshfeld surface analysis of
[1-(4-bromophenyl)-1H-1,2,3-triazol-4-yl]methyl 2-(4-nitrophenoxy)acetate
;
_journal_coeditor_code ZV2035
_journal_issue 8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 910
_journal_page_last 912
_journal_paper_doi 10.1107/S2056989024007436
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C17 H13 Br N4 O5'
_chemical_formula_moiety 'C17 H13 Br N4 O5'
_chemical_formula_sum 'C17 H13 Br N4 O5'
_chemical_formula_weight 433.22
_chemical_melting_point 419
_chemical_name_systematic
;
[1-(4-Bromophenyl)-1H-1,2,3-triazol-4-yl]methyl
2-(4-nitrophenoxy)acetate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 99.4243(16)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 17.3468(3)
_cell_length_b 10.40583(19)
_cell_length_c 9.87841(16)
_cell_measurement_reflns_used 5570
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 70.8300
_cell_measurement_theta_min 2.5800
_cell_volume 1759.06(5)
_computing_cell_refinement
;
CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/1 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0444
_diffrn_reflns_av_unetI/netI 0.0317
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 16655
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 71.635
_diffrn_reflns_theta_min 2.582
_exptl_absorpt_coefficient_mu 3.536
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.65350
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2020)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.636
_exptl_crystal_description prism
_exptl_crystal_F_000 872
_exptl_crystal_size_max 0.6
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.2
_refine_diff_density_max 0.268
_refine_diff_density_min -0.526
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.061
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 244
_refine_ls_number_reflns 3401
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.061
_refine_ls_R_factor_all 0.0439
_refine_ls_R_factor_gt 0.0352
_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^)+(0.0412P)^2^+0.3925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0878
_refine_ls_wR_factor_ref 0.0939
_reflns_number_gt 2758
_reflns_number_total 3401
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file zv2035.cif
_cod_data_source_block I
_cod_original_cell_volume 1759.07(5)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2023213
_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 0.225
_shelx_estimated_absorpt_t_max 0.538
_shelx_hkl_file
;
1 0 0 402.658 31.2333 3
-1 0 0 322.336 30.5393 4
1 0 0 371.480 31.4406 54
2 0 0 23512.4 675.018 3
-2 0 0 23220.4 684.555 4
-2 0 0 24720.2 710.464 5
2 0 0 23425.2 684.277 54
-2 0 0 24255.6 645.268 23
-3 0 0 36117.8 1049.36 4
3 0 0 36234.4 1040.00 3
-3 0 0 36624.3 1082.10 5
3 0 0 35762.2 1050.61 54
-3 0 0 37816.7 990.847 23
-4 0 0 46390.2 1359.14 5
-4 0 0 44827.0 1313.75 4
4 0 0 44165.3 1299.18 3
4 0 0 44310.1 1317.11 54
-4 0 0 47004.0 1232.87 23
5 0 0 39793.8 1244.14 54
-5 0 0 41625.6 1245.29 4
5 0 0 42040.0 1235.00 3
-6 0 0 5947.28 320.702 4
6 0 0 5470.56 302.884 3
-7 0 0 29577.4 1012.38 4
7 0 0 29317.8 998.289 3
8 0 0 599.128 117.998 3
-8 0 0 535.082 93.1156 62
-9 0 0 17375.5 781.963 8
9 0 0 17350.4 744.272 3
-9 0 0 17228.3 700.153 62
-10 0 0 972.970 179.236 8
10 0 0 943.244 156.873 3
-10 0 0 913.548 138.954 62
11 0 0 43029.3 1569.08 3
-11 0 0 47606.6 1551.38 62
12 0 0 6926.84 499.506 3
-12 0 0 7077.28 476.504 62
-12 0 0 8385.36 516.669 46
-13 0 0 3333.59 335.131 62
-13 0 0 3338.75 336.629 46
-14 0 0 1089.75 206.465 46
15 0 0 8468.93 640.130 34
16 0 0 12904.8 797.142 34
17 0 0 47.8698 83.9599 34
18 0 0 433.060 152.360 40
18 0 0 512.441 154.849 34
19 0 0 2003.12 260.044 40
19 0 0 1854.75 243.076 34
20 0 0 28.2138 42.8506 40
20 0 0-27.5834 54.0840 34
21 0 0 338.979 79.6545 34
0 1 0-3.42376 9.95793 53
0 -1 0 6.68531 24.1706 21
0 -1 0-19.7682 13.2398 57
0 -1 0-4.18025 14.1971 9
0 1 0 4.73286 8.03758 7
0 1 0-3.73554 10.3590 1
-1 -1 0 29696.4 786.384 61
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1 1 0 29932.1 770.919 10
-1 -1 0 28985.8 829.807 9
-1 1 0 29627.4 807.387 6
-1 -1 0 30408.5 828.588 8
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1 -1 0 29939.8 848.350 21
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-2 -1 0 9148.03 330.434 8
-2 -1 0 9190.23 316.940 4
-2 1 0 9077.52 325.630 2
-2 -1 0 9401.49 307.679 62
2 -1 0 9241.82 322.088 21
-2 -1 0 9466.89 322.118 21
3 1 0 24658.9 729.727 3
3 -1 0 25822.2 762.480 3
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-3 -1 0 25055.4 781.674 8
-3 1 0 24270.1 776.426 2
-3 -1 0 26642.5 728.651 21
3 -1 0 25186.0 724.283 21
-4 -1 0 149.040 53.5256 8
-4 1 0 232.651 79.5667 5
-4 -1 0 276.067 60.0403 4
4 1 0 244.765 50.6902 3
-5 1 0 4736.79 296.395 5
5 -1 0 4595.50 257.914 3
-5 -1 0 4593.38 255.848 4
-5 1 0 4594.17 270.974 4
5 1 0 4142.41 231.477 3
-5 -1 0 4076.43 262.648 8
5 1 0 5036.25 264.473 54
-5 -1 0 4507.58 233.938 23
-6 1 0 9196.46 450.521 4
-6 -1 0 9547.10 433.617 4
6 -1 0 9059.32 427.573 3
-6 -1 0 9897.31 468.643 8
6 1 0 9624.42 419.781 3
-6 1 0 9576.45 487.015 5
-6 -1 0 10386.2 427.130 62
-7 1 0 43745.2 1421.87 4
7 -1 0 43488.9 1388.54 3
7 1 0 44885.0 1373.86 3
-7 -1 0 43142.6 1381.89 4
-7 1 0 44750.3 1482.34 5
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-7 -1 0 44733.6 1360.83 62
-8 -1 0 12777.4 610.331 8
-8 1 0 11373.4 573.904 4
8 1 0 11239.0 538.357 3
8 -1 0 12032.0 564.750 3
-8 1 0 12472.2 643.058 5
-8 -1 0 12477.5 541.533 62
-9 -1 0 14508.5 703.760 8
9 1 0 14405.2 649.749 3
9 -1 0 13951.2 654.727 3
-9 1 0 14269.3 606.226 62
-9 -1 0 14250.5 628.904 62
10 -1 0 30487.9 1171.11 3
-10 -1 0 31121.2 1222.24 8
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-10 -1 0 32880.8 1148.27 62
11 -1 0 3215.66 321.619 3
-11 -1 0 3683.79 310.074 46
-11 -1 0 3477.16 312.411 62
12 -1 0 32301.3 1336.13 3
-12 -1 0 35898.8 1309.46 46
-12 -1 0 34265.2 1313.53 62
-12 1 0 36105.3 1305.79 59
13 -1 0 6477.13 522.665 3
-13 1 0 7513.08 501.449 59
-13 -1 0 7213.27 510.832 62
-13 -1 0 7360.28 504.949 46
-13 1 0 6874.23 504.637 46
-14 -1 0 5374.77 462.463 62
-14 1 0 5571.22 447.542 59
-14 1 0 5640.69 473.700 46
15 1 0 3927.43 419.819 34
15 -1 0 3286.49 387.484 34
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16 1 0 16926.9 910.131 34
16 -1 0 15126.1 872.444 34
-16 1 0 14233.8 786.859 59
-17 1 0 312.046 118.843 59
17 1 0 609.757 164.776 34
17 -1 0 515.933 164.771 34
17 1 0 238.409 111.007 40
18 -1 0 41.6417 73.0291 34
18 1 0-41.7211 89.6124 34
18 1 0 128.749 92.1793 40
19 1 0 243.412 101.809 34
19 -1 0 587.257 139.307 34
19 -1 0 765.303 158.935 40
19 1 0 542.866 145.901 40
-20 -1 0 1625.23 203.737 20
20 -1 0 1827.32 213.344 40
20 1 0 1852.18 218.762 41
20 1 0 1490.20 197.269 40
20 -1 0 1773.95 208.182 34
20 1 0 1683.03 203.335 34
0 2 0 141490. 3697.29 53
0 -2 0 136417. 3785.54 21
0 -2 0 143579. 3715.76 9
0 2 0 140844. 3704.95 1
0 2 0 145288. 3658.43 7
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1 -2 0 91464.4 2397.65 47
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1 2 0 92058.3 2479.12 1
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2 -2 0 3268.30 204.272 21
-3 -2 0 7736.50 264.353 46
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3 -2 0 7023.78 305.192 3
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3 -2 0 7536.66 338.166 21
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-4 -2 0 44470.3 1237.37 46
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-4 2 0 43333.5 1342.27 2
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4 -2 0 46407.4 1314.23 3
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-4 -2 0 43317.2 1282.49 62
-5 -2 0 3440.73 228.484 4
5 -2 0 3383.23 225.702 3
-5 2 0 3596.23 279.389 5
-5 -2 0 3632.57 252.427 8
-5 2 0 3505.25 255.218 2
-5 -2 0 3990.33 229.872 62
-6 2 0 3003.37 280.527 5
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6 -2 0 3480.00 248.251 3
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-6 -2 0 3984.39 245.900 62
-7 -2 0 746.250 134.680 8
-7 -2 0 749.222 120.992 4
7 -2 0 608.068 114.064 3
-7 2 0 601.548 139.954 5
-7 2 0 701.762 132.979 4
-7 -2 0 830.001 118.317 62
-8 -2 0 88.3267 63.2595 8
-8 2 0 30.9037 54.2214 4
-8 2 0 144.892 89.8539 5
8 -2 0 175.923 76.3571 3
-8 -2 0 21.7628 42.7023 62
-9 -2 0 1594.92 218.110 8
9 -2 0 1066.13 168.321 3
-9 2 0 973.068 182.711 4
-9 2 0 1428.14 231.018 5
-9 -2 0 1099.02 157.692 62
10 -2 0-32.8062 57.5357 3
-10 -2 0-37.0877 72.7210 8
-10 -2 0 28.5795 43.4088 62
11 -2 0 3677.29 348.891 3
-11 2 0 3641.51 320.742 59
-11 -2 0 4199.63 353.543 62
12 -2 0 2077.85 279.580 3
-12 -2 0 1949.87 252.740 62
-12 2 0 1920.77 243.852 59
13 -2 0-45.7630 69.5056 3
-13 2 0 37.9291 57.6079 59
-13 -2 0 163.878 107.776 62
-13 2 0 198.886 92.2837 46
-14 2 0 1780.22 257.965 46
-14 -2 0 980.617 202.564 62
-14 2 0 1639.30 249.018 59
14 2 0 1666.55 266.544 34
14 -2 0 1426.74 254.145 3
15 2 0 48.3603 103.873 34
15 -2 0-49.1124 74.5913 34
-15 2 0 42.7777 75.0212 59
16 2 0 97.2745 95.3740 40
16 2 0 188.931 124.258 34
16 -2 0 47.8765 83.9731 34
-16 2 0-42.7319 99.1457 59
17 2 0 915.821 202.257 40
17 2 0 1098.15 215.855 34
17 -2 0 932.640 200.081 34
-17 2 0 964.487 197.729 59
-18 -2 0 681.769 184.201 20
-18 2 0 741.892 159.297 59
18 2 0 1143.61 209.846 40
18 2 0 848.281 180.091 34
18 -2 0 775.570 181.107 34
-19 2 0 1208.82 180.202 59
-19 -2 0 1635.45 231.082 20
19 2 0 1488.16 208.950 34
19 -2 0 1138.08 189.323 34
19 2 0 1707.43 236.555 40
19 -2 0 1378.79 203.174 40
19 2 0 1580.27 220.113 41
-20 -2 0 586.458 120.971 20
20 -2 0 367.335 92.9925 40
20 2 0 654.300 126.242 40
20 2 0 422.246 106.688 41
20 2 0 638.816 125.028 34
20 -2 0 329.326 90.6676 34
0 -3 0 20.6434 54.3048 21
0 -3 0 10.1275 28.0831 57
0 3 0-22.8631 37.5066 53
0 -3 0 38.9939 42.6459 9
0 3 0-12.0204 31.6214 1
-1 -3 0 56885.5 1700.16 21
1 -3 0 55421.8 1698.43 21
-1 -3 0 55378.5 1542.09 61
-1 -3 0 57411.7 1563.64 57
1 -3 0 54452.4 1561.93 57
-1 3 0 56292.1 1586.58 53
-1 -3 0 56698.9 1609.58 9
1 3 0 54717.1 1577.25 1
-1 3 0 54238.7 1585.30 1
2 -3 0 9816.18 473.545 21
-2 -3 0 10563.0 480.648 21
2 -3 0 9540.04 393.786 57
-2 3 0 9855.82 408.764 53
2 3 0 9720.94 403.469 1
-2 -3 0 10157.3 430.863 9
-3 -3 0 4182.12 216.247 62
-3 -3 0 4295.24 269.429 9
-3 3 0 3688.82 244.704 2
3 -3 0 4520.71 287.777 21
-3 -3 0 3998.10 269.345 21
-4 -3 0 4466.45 250.839 62
-4 3 0 4802.11 295.153 2
-4 -3 0 5194.83 316.188 9
4 -3 0 4618.86 264.310 3
4 -3 0 4457.14 286.620 21
-4 -3 0 5286.91 305.278 21
-5 -3 0 15023.5 566.534 62
-5 3 0 14693.6 631.665 2
5 -3 0 13913.2 576.861 3
-5 -3 0 14685.9 630.663 8
-5 -3 0 13477.6 619.206 9
-6 -3 0 314.883 71.2916 62
-6 3 0 458.611 113.757 2
-6 -3 0 457.120 101.789 4
-6 -3 0 217.024 82.8288 9
-6 -3 0 433.754 102.870 8
6 -3 0 268.868 77.3984 3
-7 -3 0 4785.55 314.128 62
7 -3 0 4834.23 329.146 3
-7 3 0 5140.86 411.594 5
-7 -3 0 4794.43 359.102 8
-7 -3 0 4561.50 365.396 9
-7 -3 0 4256.51 329.746 23
-8 3 0 7099.51 514.949 5
8 -3 0 5657.97 387.377 3
-8 -3 0 5794.96 439.981 9
-8 -3 0 6061.98 441.838 8
-8 -3 0 6554.57 395.217 62
9 -3 0 1254.77 189.781 3
-9 3 0 1123.63 205.119 4
-9 -3 0 1767.30 246.222 8
-9 -3 0 1504.50 190.856 62
10 -3 0 603.114 141.214 39
-10 -3 0 243.910 107.346 8
10 -3 0 390.196 116.757 3
-10 -3 0 346.000 103.623 62
11 -3 0 992.163 195.395 3
11 -3 0 706.296 158.351 39
-11 -3 0 1116.99 207.873 19
-11 3 0 1150.27 190.098 58
-11 -3 0 1128.90 187.314 62
-11 3 0 1060.35 183.202 59
-12 -3 0 274.351 103.845 62
-12 3 0 477.882 137.318 59
-12 3 0 829.105 172.161 58
12 -3 0 658.376 168.220 3
-12 -3 0 599.591 167.213 19
-13 3 0 203.022 100.947 46
13 -3 0 286.482 118.626 3
-13 -3 0 300.039 112.971 62
-13 3 0 361.176 131.852 59
-14 3 0 42.7018 83.7352 59
14 3 0 47.6478 83.5700 40
-15 3 0 43.8072 76.8417 59
15 3 0 95.6125 110.920 40
-16 3 0-42.8671 65.1104 59
16 3 0 46.1404 80.9220 40
-16 -3 0 97.9933 74.4192 20
17 3 0 7189.27 539.074 40
-17 -3 0 6781.31 535.141 20
-17 3 0 7249.79 519.156 59
18 3 0 37.1632 72.8792 40
18 3 0 38.0298 74.5781 41
-18 -3 0 39.3011 68.9362 20
-18 3 0 103.158 73.8685 59
19 3 0 546.021 131.115 40
19 3 0 779.512 152.919 41
-19 -3 0 660.973 141.475 20
-19 3 0 441.961 109.288 59
-20 3 0 20.0049 39.2257 59
20 3 0 22.1593 47.5966 40
20 3 0-22.9915 34.9204 41
-20 -3 0-48.2116 47.2662 17
0 -4 0 101318. 2994.79 21
0 -4 0 100614. 2797.28 57
0 -4 0 104319. 2812.00 61
0 -4 0 105938. 2870.43 9
0 4 0 100473. 2842.83 1
1 -4 0 7622.92 460.183 21
-1 -4 0 7962.77 468.380 21
-1 -4 0 8184.01 366.627 57
1 -4 0 7774.23 363.191 57
-1 4 0 7669.72 382.167 53
1 4 0 7657.80 377.890 1
-1 -4 0 7898.41 396.430 9
2 -4 0 555.316 133.822 21
-2 -4 0 348.740 105.791 21
2 -4 0 349.110 74.4734 57
-2 4 0 460.736 93.8998 53
2 4 0 555.579 95.7292 1
-2 -4 0 500.284 102.927 9
3 -4 0 725.520 142.426 21
-3 -4 0 595.822 131.630 21
3 -4 0 780.630 108.939 57
-3 4 0 577.211 106.768 53
-3 4 0 697.090 122.039 2
-3 -4 0 697.739 122.150 9
3 4 0 725.864 113.212 1
4 -4 0 19495.3 811.260 21
-4 -4 0 19149.6 803.422 21
4 -4 0 19782.4 750.650 57
-4 -4 0 20890.7 808.805 9
-4 4 0 19168.8 788.228 2
4 -4 0 20391.3 733.719 3
4 4 0 21049.0 775.804 1
5 -4 0 9415.66 463.498 3
-5 4 0 9920.05 518.413 2
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-3 -6 10 1842.15 255.142 26
-2 -6 10 37.9478 66.5523 26
2 -6 -10-27.7117 54.3376 36
-2 6 10 35.4580 53.8552 52
-2 -6 10 33.6756 51.1482 52
-1 -6 10 569.898 150.985 26
1 -6 -10 648.719 141.188 36
-1 6 10 763.440 152.425 52
-1 -6 10 805.782 161.000 52
-1 -6 10 1074.62 172.687 12
0 -6 -10 222.671 88.0607 36
0 6 10 59.2141 58.1440 52
0 -6 10 217.517 98.2975 12
-1 -6 -10 807.611 153.588 42
-1 -6 -10 1088.32 169.508 36
1 -6 10 954.891 170.333 12
-2 -6 -10 243.339 85.5046 36
-2 -6 -10 268.977 94.4825 42
2 6 10 122.124 75.8954 55
2 -6 10 173.036 94.7594 12
2 -6 10 238.991 87.2747 13
-3 -6 -10 552.510 109.564 36
-3 -6 -10 725.334 129.728 42
3 -6 10 558.214 120.642 12
3 -6 10 495.850 111.744 13
3 6 10 505.869 115.239 55
-5 7 10 820.019 130.338 52
5 -7 -10 717.331 118.578 35
-4 -7 10 181.863 82.1519 26
-4 7 10 24.7053 43.3496 52
4 -7 -10 108.327 60.0929 35
-3 -7 10 54.5723 75.6943 26
-3 7 10 77.8309 55.7677 52
3 -7 -10 128.750 67.8784 35
-2 -7 10 80.8417 66.8336 26
2 -7 -10-20.4958 40.1870 36
2 -7 -10 40.8708 43.8929 35
-2 7 10-25.5737 31.7135 52
1 -7 -10 790.987 127.861 36
-1 7 10 708.485 129.046 52
-11 0 11-24.6410 48.3187 30
-10 0 11-28.1697 42.7896 30
-9 0 11 31.1360 47.2955 30
-8 0 11-33.4017 58.5840 30
-7 0 11-32.3982 80.3570 52
-6 0 11-35.8691 83.2206 52
-5 0 11 38.8161 58.9614 52
-4 0 11-40.9834 62.2535 52
-3 0 11-42.0118 63.8157 52
-2 0 11-41.6358 81.6439 52
-1 0 11-39.8196 69.8405 52
0 0 11-41.3281 72.4829 55
0 0 11-36.7481 64.4514 52
0 0 11-25.4466 49.9003 50
1 0 11 40.9836 88.0365 55
1 0 11 50.6438 49.6646 50
2 0 11-39.1212 76.7080 55
2 0 11 24.9032 48.8309 50
3 0 11 36.0173 54.7032 55
3 0 11-23.9593 29.7127 50
4 0 11 22.2416 43.6136 50
5 0 11-19.5164 34.2303 50
-11 -1 11 355.903 91.2687 30
-11 1 11 484.579 110.873 30
-10 -1 11-27.0828 47.4965 30
-10 1 11 167.745 73.5457 30
-9 -1 11 89.5296 64.1411 30
-9 1 11 93.3043 66.8419 30
-8 -1 11 95.5015 68.4476 30
-8 1 11 168.391 83.5867 30
-7 1 11 884.776 173.671 30
-7 1 11 918.484 165.233 52
-7 -1 11 450.311 130.431 52
-6 -1 11 1250.54 169.940 50
-6 1 11 953.206 180.165 52
-6 -1 11 1242.80 203.844 52
-5 -1 11 26.0842 51.1641 50
-5 1 11 76.8137 82.5058 52
-5 -1 11 114.958 82.3180 52
-4 -1 11 105.725 69.5307 50
-4 1 11-40.6872 61.7953 52
-4 -1 11 161.423 93.6248 52
-3 -1 11 213.186 81.1126 50
-3 1 11 166.972 96.9822 52
-3 -1 11 247.886 114.679 52
-2 1 11-41.2854 72.4060 52
-2 -1 11-40.9656 62.2204 52
-2 -1 11 26.7328 40.6052 50
-1 1 11 39.2927 68.9094 52
-1 -1 11-39.2646 76.9878 52
-1 -1 11 26.6900 40.5366 50
0 1 11 379.095 128.476 55
0 1 11 396.097 122.842 52
0 -1 11 509.168 132.004 52
0 -1 11 557.558 119.281 50
1 1 11 206.169 108.661 55
1 -1 11 288.490 89.2994 50
2 1 11 622.332 153.706 55
2 -1 11 869.587 144.851 50
3 1 11 35.4361 62.1465 55
3 -1 11-24.4366 52.4879 50
4 1 11 1183.03 180.505 55
4 -1 11 788.432 128.586 50
5 1 11 235.045 82.7605 55
5 -1 11 216.314 64.7647 50
-11 2 11 44.7812 51.9461 30
-11 -2 11-21.4247 37.5740 30
-10 -2 11 739.805 134.636 30
-10 2 11 763.821 137.941 30
-9 -2 11-27.2222 53.3778 30
-9 2 11 29.7109 52.1073 30
-9 -2 11-21.9392 33.3243 50
-8 2 11 423.236 121.873 30
-8 -2 11 646.838 119.603 50
-7 2 11 1314.77 208.474 30
-7 -2 11 1237.02 171.880 50
-7 2 11 1466.86 199.267 52
-7 -2 11 1326.14 196.005 52
-6 -2 11 234.372 85.7317 50
-6 2 11 371.399 114.882 52
-6 -2 11 273.261 103.996 52
-5 -2 11 1456.52 185.751 50
-5 2 11 1518.25 227.333 52
-5 -2 11 995.590 185.810 52
-4 -2 11 453.638 113.193 50
-4 2 11 827.230 176.752 52
-4 -2 11 659.631 152.882 52
-3 -2 11 828.199 143.807 50
-3 2 11 646.609 155.675 52
-3 -2 11 833.265 175.042 52
-2 2 11 238.812 104.870 52
-2 -2 11 393.140 129.123 52
-2 -2 11 186.223 70.2321 50
-1 -2 11 2162.48 228.383 50
-1 -2 11 1770.75 248.794 52
0 2 11 41.1069 72.0987 55
0 2 11 34.0714 66.8138 52
0 -2 11 34.8742 52.9771 52
0 -2 11 51.9805 45.5926 50
1 2 11 1585.40 238.121 55
1 -2 11 1218.07 168.439 50
2 2 11 184.342 91.6290 55
2 -2 11 268.918 77.5159 50
3 2 11 4807.50 382.352 55
3 -2 11 4252.21 307.739 50
4 2 11 516.938 118.772 55
4 -2 11 478.368 100.666 50
-5 2 -11 1400.34 148.540 59
5 2 11 1321.49 170.373 55
5 -2 11 1382.38 150.631 50
-10 3 11 1182.89 160.332 30
-9 3 11 26.8337 40.7762 30
-9 -3 11 104.204 57.8047 50
-8 3 11 239.325 87.2640 30
-8 -3 11 297.407 87.7028 50
-7 3 11 548.244 130.817 30
-7 3 11 649.099 128.958 52
-7 -3 11 674.320 131.587 52
-6 -3 11 1072.89 158.456 50
-6 3 11 994.006 169.965 52
-6 -3 11 1070.94 174.491 52
-5 -3 11 303.734 94.5708 50
-5 3 11 585.998 142.044 52
-5 -3 11 273.586 104.248 52
-4 -3 11 736.459 135.420 50
-4 3 11 1032.51 184.241 52
-4 -3 11 973.533 177.415 52
-3 -3 11 328.569 91.6553 50
-3 3 11 189.057 99.7213 52
-3 -3 11 331.758 112.197 52
-2 -3 11 149.938 66.0153 50
-2 3 11 370.043 117.149 52
-2 -3 11 400.978 119.751 52
-1 3 11 38.6518 47.9438 55
-1 3 11-69.1123 74.2307 52
-1 -3 11-69.5971 86.3131 52
-1 -3 11-24.5425 43.0551 50
0 3 11 1376.80 217.250 55
0 3 11 1327.00 192.275 52
0 -3 11 1279.17 195.053 52
0 -3 11 1194.75 160.228 50
0 -3 -11 1431.84 190.900 36
1 3 11 906.780 172.078 55
1 -3 11 529.343 108.070 50
-1 -3 -11 709.966 135.466 36
2 3 11 1725.79 225.801 55
2 -3 11 1716.73 181.910 50
-2 -3 -11 1701.79 198.198 36
3 3 11 381.031 106.692 55
3 -3 11 537.624 98.0028 50
-3 -3 -11 554.071 110.633 36
4 -3 11 814.903 113.254 50
-4 -3 -11 1019.31 136.749 36
-8 4 11-25.4599 44.6533 30
-8 -4 11-19.8161 45.9760 50
-7 4 11 112.084 69.4969 30
-7 -4 11 21.2791 45.7056 50
-7 4 11-22.7040 39.8175 52
-6 4 11 206.528 85.9737 30
-6 -4 11 243.508 80.2157 50
-6 4 11 188.055 78.3153 52
-6 -4 11 216.622 78.9326 52
-5 -4 11 743.276 124.222 50
-5 4 11 515.838 122.822 52
-5 -4 11 506.904 120.726 52
-4 -4 11 180.545 71.4786 50
-4 4 11 163.720 90.8959 52
-4 -4 11 158.243 83.3643 52
-3 4 11 1477.58 215.773 52
-3 -4 11 1654.56 184.776 50
-3 -4 11 1392.71 206.410 52
-2 -4 11 570.344 109.840 50
-2 4 11 489.243 125.564 52
-2 -4 11 797.638 151.405 52
-1 4 11 1474.87 217.728 55
-1 -4 11 1255.76 157.981 50
-1 4 11 1441.13 196.722 52
-1 -4 11 1388.02 195.898 52
1 -4 -11 1603.27 188.327 36
0 -4 11 122.393 53.8304 50
0 4 11 367.873 117.378 55
0 4 11 157.350 65.1821 52
0 -4 11 272.436 86.2389 52
0 -4 -11 117.610 74.4895 36
1 -4 11 919.167 125.237 50
1 4 11 904.071 160.830 55
-1 -4 -11 745.516 127.105 36
2 -4 11-17.4160 34.1495 50
2 4 11 27.9122 48.9517 55
-2 -4 -11-20.7674 36.4217 36
-6 -5 11 51.8329 45.4695 50
-5 -5 11 53.6012 38.3798 50
-5 5 11 48.2743 59.8663 52
-5 -5 11 23.3605 35.4832 52
5 -5 -11-19.9040 42.7546 35
-4 -5 11 18.0108 38.6909 50
-4 5 11 52.8931 61.3592 52
-4 -5 11 25.1643 38.2251 52
-3 -5 11 195.731 64.5867 50
-3 5 11 299.266 101.375 52
-3 -5 11 232.528 84.9617 52
-2 -5 11 120.665 50.1985 50
-2 5 11 104.837 65.0547 52
-2 -5 11 75.8167 58.6880 52
-1 5 11 164.572 72.2609 55
-1 5 11 141.807 62.2972 52
-1 -5 11 164.046 65.1018 52
-5 0 12 263.366 78.8334 52
-4 0 12 204.886 81.1354 52
-3 0 12 338.101 102.344 52
-2 0 12 224.745 79.1534 52
-5 1 12-23.3383 35.4471 52
-5 -1 12 23.3007 35.3900 52
-4 1 12 475.510 108.173 52
-4 -1 12 474.032 105.598 52
-3 1 12 2485.79 239.306 52
-3 -1 12 2130.90 223.286 52
-2 1 12 2154.53 218.058 52
-2 -1 12 1829.51 203.418 52
0 0 0 0.00 0.00 0
TITL exp_537_TSh-22 in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 1.54184 17.346848 10.405827 9.878413 90.0000 99.4243 90.0000
ZERR 8.00 0.000320 0.000191 0.000164 0.0000 0.0016 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N O
UNIT 88.00 80.00 8.00 8.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 1375
_shelx_res_file
;
TITL 1.res in P2(1)/c
1.res
created by SHELXL-2018/3 at 10:15:29 on 19-Jul-2024
REM Old TITL exp_537_tsh-22_a.res in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.116, Rweak 0.008, Alpha 0.034
REM 0.242 for 87 systematic absences, Orientation as input
REM Formula found by SHELXT: C20 N2 O4 Br
REM #####
CELL 1.54184 17.346848 10.405827 9.878413 90 99.4243 90
ZERR 4 0.00032 0.000191 0.000164 0 0.0016 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O Br
UNIT 68 52 16 20 4
EQIV $1 +X,0.5-Y,-0.5+Z
EQIV $2 2-X,1-Y,2-Z
EQIV $3 1-X,0.5+Y,1.5-Z
EQIV $4 2-X,1-Y,1-Z
L.S. 12
PLAN 5
SIZE 0.2 0.4 0.6
CONF
MPLA 10 O7 C1 C2 C3 C4 C5 C6 N13 O14 O15
HTAB C8 O16_$1
HTAB C2 O16_$2
HTAB C26 N17_$3
HTAB C20 N18_$3
HTAB C5 O7_$1
HTAB C5 O16_$1
HTAB C8 O14_$4
HTAB C4 O7_$1
BOND
list 4
MORE -1
BOND $H
fmap 2
acta
REM
REM
REM
WGHT 0.041200 0.392500
FVAR 2.73095
BR27 5 0.233148 0.340832 0.137471 11.00000 0.05937 0.06126 =
0.05047 -0.00058 -0.00636 -0.00121
C25 1 0.334900 0.406786 0.382419 11.00000 0.04357 0.03556 =
0.05040 0.00153 0.00486 0.00321
AFIX 43
H25 2 0.312633 0.487975 0.368205 11.00000 -1.20000
AFIX 0
O10 4 0.719280 0.305386 0.810147 11.00000 0.03244 0.05943 =
0.03992 0.00410 0.00200 -0.00271
O7 4 0.922803 0.358857 0.855185 11.00000 0.03608 0.07975 =
0.03719 -0.00452 0.00340 -0.00977
O16 4 0.804632 0.334281 1.004221 11.00000 0.04709 0.07382 =
0.03517 0.00100 0.00192 -0.00194
N19 3 0.487792 0.242752 0.624087 11.00000 0.03481 0.03228 =
0.05062 0.00474 0.00675 0.00241
O14 4 1.150991 0.420904 0.431662 11.00000 0.06518 0.10004 =
0.05627 0.00739 0.02392 0.00446
O15 4 1.213453 0.526036 0.604461 11.00000 0.05805 0.06667 =
0.09882 -0.00420 0.03067 -0.01617
N18 3 0.503032 0.123002 0.674704 11.00000 0.05948 0.03572 =
0.07729 0.01136 -0.00995 -0.00086
N13 3 1.158597 0.459368 0.550629 11.00000 0.04632 0.05148 =
0.06425 0.01109 0.01713 0.00709
N17 3 0.562802 0.132774 0.773906 11.00000 0.05871 0.04649 =
0.07660 0.01501 -0.00932 0.00074
C24 1 0.310060 0.308023 0.292770 11.00000 0.03852 0.04720 =
0.04140 0.00022 0.00699 -0.00271
C21 1 0.426022 0.263903 0.511987 11.00000 0.03314 0.03792 =
0.04295 0.00156 0.00901 -0.00161
C26 1 0.392534 0.384885 0.492579 11.00000 0.04020 0.03468 =
0.04845 -0.00337 0.00573 -0.00082
AFIX 43
H26 2 0.409094 0.450859 0.554001 11.00000 -1.20000
AFIX 0
C9 1 0.790738 0.322986 0.882771 11.00000 0.03502 0.03778 =
0.04030 0.00573 0.00135 0.00088
C3 1 1.098524 0.424312 0.632164 11.00000 0.03894 0.04485 =
0.05194 0.00374 0.01040 0.00517
C6 1 0.979955 0.374646 0.776663 11.00000 0.03489 0.05212 =
0.04000 0.00041 0.00585 0.00019
C20 1 0.537754 0.327125 0.694245 11.00000 0.03539 0.03619 =
0.05666 0.00292 0.00582 -0.00283
AFIX 43
H20 2 0.538958 0.415583 0.681321 11.00000 -1.20000
AFIX 0
C12 1 0.585865 0.257001 0.787405 11.00000 0.03327 0.04809 =
0.04959 0.00326 0.00941 0.00012
C5 1 0.974087 0.332667 0.642024 11.00000 0.03844 0.05577 =
0.04302 -0.00573 0.00199 -0.00451
AFIX 43
H5 2 0.930095 0.287661 0.600952 11.00000 -1.20000
AFIX 0
C8 1 0.848173 0.321954 0.784792 11.00000 0.03653 0.05623 =
0.03770 -0.00238 0.00072 -0.00579
AFIX 23
H8A 2 0.850981 0.236529 0.746602 11.00000 -1.20000
H8B 2 0.831325 0.381126 0.709912 11.00000 -1.20000
AFIX 0
C22 1 0.400852 0.164825 0.422642 11.00000 0.04460 0.03586 =
0.05292 -0.00364 0.01145 0.00338
AFIX 43
H22 2 0.423542 0.083905 0.436396 11.00000 -1.20000
AFIX 0
C23 1 0.341845 0.186095 0.312655 11.00000 0.05194 0.04247 =
0.04547 -0.00928 0.00839 -0.00448
AFIX 43
H23 2 0.323799 0.119527 0.252980 11.00000 -1.20000
AFIX 0
C11 1 0.655197 0.296616 0.887495 11.00000 0.03803 0.06929 =
0.04484 0.00381 0.00858 0.00066
AFIX 23
H11A 2 0.646112 0.379063 0.927913 11.00000 -1.20000
H11B 2 0.666662 0.233527 0.960297 11.00000 -1.20000
AFIX 0
C2 1 1.106969 0.461395 0.768001 11.00000 0.03684 0.05528 =
0.05758 -0.00668 0.00402 -0.00711
AFIX 43
H2 2 1.152186 0.502689 0.809906 11.00000 -1.20000
AFIX 0
C4 1 1.033770 0.358026 0.569576 11.00000 0.04414 0.05472 =
0.04223 -0.00540 0.00710 0.00146
AFIX 43
H4 2 1.030331 0.330596 0.479185 11.00000 -1.20000
AFIX 0
C1 1 1.047530 0.436242 0.839877 11.00000 0.04378 0.06917 =
0.04299 -0.00978 0.00610 -0.00451
AFIX 43
H1 2 1.052372 0.460485 0.931496 11.00000 -1.20000
AFIX 0
HKLF 4
REM 1.res in P2(1)/c
REM wR2 = 0.0939, GooF = S = 1.061, Restrained GooF = 1.061 for all data
REM R1 = 0.0352 for 2758 Fo > 4sig(Fo) and 0.0439 for all 3401 data
REM 244 parameters refined using 0 restraints
END
WGHT 0.0412 0.3923
REM Highest difference peak 0.268, deepest hole -0.526, 1-sigma level 0.053
Q1 1 0.2069 0.3366 0.2063 11.00000 0.05 0.27
Q2 1 1.0840 0.3702 0.6135 11.00000 0.05 0.19
Q3 1 0.3152 0.3632 0.3308 11.00000 0.05 0.18
Q4 1 1.0979 0.3193 0.7597 11.00000 0.05 0.17
Q5 1 0.2905 0.1388 0.1094 11.00000 0.05 0.17
;
_shelx_res_checksum 32252
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br27 0.23315(2) 0.34083(3) 0.13747(3) 0.05876(13) Uani d 1 . .
C C25 0.33490(14) 0.4068(2) 0.3824(3) 0.0435(5) Uani d 1 . .
H H25 0.312633 0.487975 0.368205 0.052 Uiso calc 1 . .
O O10 0.71928(9) 0.30539(17) 0.81015(16) 0.0444(4) Uani d 1 . .
O O7 0.92280(10) 0.35886(19) 0.85518(17) 0.0513(5) Uani d 1 . .
O O16 0.80463(11) 0.33428(18) 1.00422(17) 0.0526(5) Uani d 1 . .
N N19 0.48779(11) 0.24275(18) 0.6241(2) 0.0393(4) Uani d 1 . .
O O14 1.15099(13) 0.4209(2) 0.4317(2) 0.0723(6) Uani d 1 . .
O O15 1.21345(13) 0.5260(2) 0.6045(3) 0.0725(6) Uani d 1 . .
N N18 0.50303(15) 0.1230(2) 0.6747(3) 0.0599(6) Uani d 1 . .
N N13 1.15860(13) 0.4594(2) 0.5506(3) 0.0531(6) Uani d 1 . .
N N17 0.56280(15) 0.1328(2) 0.7739(3) 0.0629(7) Uani d 1 . .
C C24 0.31006(14) 0.3080(2) 0.2928(2) 0.0423(5) Uani d 1 . .
C C21 0.42602(13) 0.2639(2) 0.5120(2) 0.0377(5) Uani d 1 . .
C C26 0.39253(14) 0.3849(2) 0.4926(3) 0.0413(5) Uani d 1 . .
H H26 0.409094 0.450859 0.554001 0.050 Uiso calc 1 . .
C C9 0.79074(14) 0.3230(2) 0.8828(2) 0.0382(5) Uani d 1 . .
C C3 1.09852(14) 0.4243(2) 0.6322(3) 0.0449(6) Uani d 1 . .
C C6 0.97995(14) 0.3746(2) 0.7767(2) 0.0424(5) Uani d 1 . .
C C20 0.53775(14) 0.3271(2) 0.6942(3) 0.0429(5) Uani d 1 . .
H H20 0.538958 0.415583 0.681321 0.052 Uiso calc 1 . .
C C12 0.58587(14) 0.2570(2) 0.7874(3) 0.0434(6) Uani d 1 . .
C C5 0.97409(15) 0.3327(3) 0.6420(3) 0.0463(6) Uani d 1 . .
H H5 0.930095 0.287661 0.600952 0.056 Uiso calc 1 . .
C C8 0.84817(14) 0.3220(3) 0.7848(2) 0.0441(6) Uani d 1 . .
H H8A 0.850981 0.236529 0.746602 0.053 Uiso calc 1 . .
H H8B 0.831325 0.381126 0.709912 0.053 Uiso calc 1 . .
C C22 0.40085(15) 0.1648(2) 0.4226(3) 0.0441(6) Uani d 1 . .
H H22 0.423542 0.083905 0.436396 0.053 Uiso calc 1 . .
C C23 0.34185(16) 0.1861(2) 0.3127(3) 0.0466(6) Uani d 1 . .
H H23 0.323799 0.119527 0.252980 0.056 Uiso calc 1 . .
C C11 0.65520(15) 0.2966(3) 0.8875(3) 0.0505(6) Uani d 1 . .
H H11A 0.646112 0.379063 0.927913 0.061 Uiso calc 1 . .
H H11B 0.666662 0.233527 0.960297 0.061 Uiso calc 1 . .
C C2 1.10697(15) 0.4614(3) 0.7680(3) 0.0503(6) Uani d 1 . .
H H2 1.152186 0.502689 0.809906 0.060 Uiso calc 1 . .
C C4 1.03377(15) 0.3580(2) 0.5696(3) 0.0470(6) Uani d 1 . .
H H4 1.030331 0.330596 0.479185 0.056 Uiso calc 1 . .
C C1 1.04753(15) 0.4362(3) 0.8399(3) 0.0521(7) Uani d 1 . .
H H1 1.052372 0.460485 0.931496 0.063 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
Br27 0.0594(2) 0.0613(2) 0.05047(19) -0.00121(14) -0.00636(14) -0.00058(13)
C25 0.0436(13) 0.0356(12) 0.0504(14) 0.0032(10) 0.0049(11) 0.0015(11)
O10 0.0324(8) 0.0594(11) 0.0399(9) -0.0027(7) 0.0020(7) 0.0041(8)
O7 0.0361(9) 0.0798(13) 0.0372(9) -0.0098(8) 0.0034(7) -0.0045(8)
O16 0.0471(10) 0.0738(13) 0.0352(9) -0.0019(9) 0.0019(8) 0.0010(8)
N19 0.0348(10) 0.0323(10) 0.0506(11) 0.0024(8) 0.0067(9) 0.0047(9)
O14 0.0652(14) 0.1000(18) 0.0563(13) 0.0045(12) 0.0239(11) 0.0074(12)
O15 0.0580(13) 0.0667(14) 0.0988(16) -0.0162(11) 0.0307(12) -0.0042(12)
N18 0.0595(15) 0.0357(11) 0.0773(17) -0.0009(10) -0.0099(12) 0.0114(11)
N13 0.0463(13) 0.0515(13) 0.0643(15) 0.0071(10) 0.0171(11) 0.0111(11)
N17 0.0587(15) 0.0465(13) 0.0766(17) 0.0007(11) -0.0093(13) 0.0150(12)
C24 0.0385(13) 0.0472(14) 0.0414(13) -0.0027(10) 0.0070(10) 0.0002(11)
C21 0.0331(12) 0.0379(12) 0.0429(13) -0.0016(9) 0.0090(10) 0.0016(10)
C26 0.0402(13) 0.0347(12) 0.0484(14) -0.0008(10) 0.0057(10) -0.0034(10)
C9 0.0350(12) 0.0378(12) 0.0403(13) 0.0009(9) 0.0014(10) 0.0057(10)
C3 0.0389(13) 0.0449(14) 0.0519(14) 0.0052(11) 0.0104(11) 0.0037(11)
C6 0.0349(12) 0.0521(14) 0.0400(13) 0.0002(10) 0.0059(10) 0.0004(11)
C20 0.0354(12) 0.0362(12) 0.0567(15) -0.0028(10) 0.0058(11) 0.0029(11)
C12 0.0333(12) 0.0481(14) 0.0496(14) 0.0001(10) 0.0094(10) 0.0033(11)
C5 0.0384(13) 0.0558(16) 0.0430(13) -0.0045(11) 0.0020(10) -0.0057(11)
C8 0.0365(13) 0.0562(15) 0.0377(12) -0.0058(11) 0.0007(10) -0.0024(11)
C22 0.0446(13) 0.0359(13) 0.0529(14) 0.0034(10) 0.0115(11) -0.0036(11)
C23 0.0519(15) 0.0425(14) 0.0455(14) -0.0045(11) 0.0084(12) -0.0093(11)
C11 0.0380(13) 0.0693(17) 0.0448(14) 0.0007(12) 0.0086(11) 0.0038(13)
C2 0.0368(13) 0.0553(16) 0.0576(16) -0.0071(11) 0.0040(11) -0.0067(13)
C4 0.0441(14) 0.0547(16) 0.0422(13) 0.0015(12) 0.0071(11) -0.0054(11)
C1 0.0438(14) 0.0692(18) 0.0430(14) -0.0045(13) 0.0061(11) -0.0098(13)
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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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'
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
C24 C25 H25 . . 120.1 ?
C26 C25 H25 . . 120.1 ?
C26 C25 C24 . . 119.8(2) ?
C9 O10 C11 . . 116.63(19) ?
C6 O7 C8 . . 116.33(18) ?
N18 N19 C21 . . 120.4(2) ?
C20 N19 N18 . . 109.9(2) ?
C20 N19 C21 . . 129.7(2) ?
N17 N18 N19 . . 106.7(2) ?
O14 N13 C3 . . 118.1(2) ?
O15 N13 O14 . . 123.6(2) ?
O15 N13 C3 . . 118.3(2) ?
N18 N17 C12 . . 109.5(2) ?
C25 C24 Br27 . . 119.41(19) ?
C25 C24 C23 . . 121.1(2) ?
C23 C24 Br27 . . 119.47(19) ?
C26 C21 N19 . . 119.5(2) ?
C22 C21 N19 . . 120.0(2) ?
C22 C21 C26 . . 120.5(2) ?
C25 C26 C21 . . 119.7(2) ?
C25 C26 H26 . . 120.2 ?
C21 C26 H26 . . 120.2 ?
O10 C9 C8 . . 107.9(2) ?
O16 C9 O10 . . 124.8(2) ?
O16 C9 C8 . . 127.3(2) ?
C2 C3 N13 . . 119.6(2) ?
C4 C3 N13 . . 118.7(2) ?
C4 C3 C2 . . 121.7(2) ?
O7 C6 C5 . . 124.1(2) ?
O7 C6 C1 . . 115.9(2) ?
C5 C6 C1 . . 120.0(2) ?
N19 C20 H20 . . 127.1 ?
N19 C20 C12 . . 105.8(2) ?
C12 C20 H20 . . 127.1 ?
N17 C12 C11 . . 121.7(2) ?
C20 C12 N17 . . 108.0(2) ?
C20 C12 C11 . . 130.3(2) ?
C6 C5 H5 . . 120.2 ?
C4 C5 C6 . . 119.6(2) ?
C4 C5 H5 . . 120.2 ?
O7 C8 C9 . . 109.35(19) ?
O7 C8 H8A . . 109.8 ?
O7 C8 H8B . . 109.8 ?
C9 C8 H8A . . 109.8 ?
C9 C8 H8B . . 109.8 ?
H8A C8 H8B . . 108.3 ?
C21 C22 H22 . . 120.0 ?
C21 C22 C23 . . 119.9(2) ?
C23 C22 H22 . . 120.0 ?
C24 C23 H23 . . 120.5 ?
C22 C23 C24 . . 119.0(2) ?
C22 C23 H23 . . 120.5 ?
O10 C11 C12 . . 105.9(2) ?
O10 C11 H11A . . 110.6 ?
O10 C11 H11B . . 110.6 ?
C12 C11 H11A . . 110.6 ?
C12 C11 H11B . . 110.6 ?
H11A C11 H11B . . 108.7 ?
C3 C2 H2 . . 120.6 ?
C1 C2 C3 . . 118.8(2) ?
C1 C2 H2 . . 120.6 ?
C3 C4 C5 . . 119.4(2) ?
C3 C4 H4 . . 120.3 ?
C5 C4 H4 . . 120.3 ?
C6 C1 H1 . . 119.8 ?
C2 C1 C6 . . 120.4(2) ?
C2 C1 H1 . . 119.8 ?
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
Br27 C24 . 1.892(2) ?
C25 H25 . 0.9300 ?
C25 C24 . 1.379(3) ?
C25 C26 . 1.371(3) ?
O10 C9 . 1.339(3) ?
O10 C11 . 1.451(3) ?
O7 C6 . 1.365(3) ?
O7 C8 . 1.418(3) ?
O16 C9 . 1.190(3) ?
N19 N18 . 1.353(3) ?
N19 C21 . 1.426(3) ?
N19 C20 . 1.344(3) ?
O14 N13 . 1.228(3) ?
O15 N13 . 1.226(3) ?
N18 N17 . 1.309(3) ?
N13 C3 . 1.464(3) ?
N17 C12 . 1.353(3) ?
C24 C23 . 1.385(4) ?
C21 C26 . 1.387(3) ?
C21 C22 . 1.381(3) ?
C26 H26 . 0.9300 ?
C9 C8 . 1.498(3) ?
C3 C2 . 1.381(4) ?
C3 C4 . 1.376(4) ?
C6 C5 . 1.388(3) ?
C6 C1 . 1.391(3) ?
C20 H20 . 0.9300 ?
C20 C12 . 1.351(3) ?
C12 C11 . 1.485(4) ?
C5 H5 . 0.9300 ?
C5 C4 . 1.377(4) ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C22 H22 . 0.9300 ?
C22 C23 . 1.383(4) ?
C23 H23 . 0.9300 ?
C11 H11A . 0.9700 ?
C11 H11B . 0.9700 ?
C2 H2 . 0.9300 ?
C2 C1 . 1.370(3) ?
C4 H4 . 0.9300 ?
C1 H1 . 0.9300 ?
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
C26 H26 N17 2_656 0.93 2.54 3.463(3) 173.1 yes
C5 H5 O16 4_565 0.93 2.56 3.493(3) 175.7 yes
C8 H8A O16 4_565 0.97 2.51 3.195(3) 127.7 yes
C8 H8B O14 3_766 0.97 2.54 3.427(3) 152.6 yes
C2 H2 O16 3_767 0.93 2.52 3.287(3) 139.7 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
Br27 C24 C23 C22 . . . . 176.72(19) ?
C25 C24 C23 C22 . . . . -1.7(4) ?
O10 C9 C8 O7 . . . . 171.6(2) ?
O7 C6 C5 C4 . . . . 177.3(2) ?
O7 C6 C1 C2 . . . . -177.3(2) ?
O16 C9 C8 O7 . . . . -10.0(4) ?
N19 N18 N17 C12 . . . . 0.1(3) ?
N19 C21 C26 C25 . . . . 177.9(2) ?
N19 C21 C22 C23 . . . . -178.9(2) ?
N19 C20 C12 N17 . . . . -1.5(3) ?
N19 C20 C12 C11 . . . . 176.0(2) ?
O14 N13 C3 C2 . . . . 177.3(3) ?
O14 N13 C3 C4 . . . . -4.5(4) ?
O15 N13 C3 C2 . . . . -3.1(4) ?
O15 N13 C3 C4 . . . . 175.0(2) ?
N18 N19 C21 C26 . . . . 156.9(2) ?
N18 N19 C21 C22 . . . . -24.1(3) ?
N18 N19 C20 C12 . . . . 1.6(3) ?
N18 N17 C12 C20 . . . . 0.9(3) ?
N18 N17 C12 C11 . . . . -176.8(2) ?
N13 C3 C2 C1 . . . . 175.2(2) ?
N13 C3 C4 C5 . . . . -175.2(2) ?
N17 C12 C11 O10 . . . . 97.3(3) ?
C24 C25 C26 C21 . . . . 0.8(4) ?
C21 N19 N18 N17 . . . . 178.9(2) ?
C21 N19 C20 C12 . . . . -178.4(2) ?
C21 C22 C23 C24 . . . . 1.3(4) ?
C26 C25 C24 Br27 . . . . -177.75(18) ?
C26 C25 C24 C23 . . . . 0.6(4) ?
C26 C21 C22 C23 . . . . 0.1(4) ?
C9 O10 C11 C12 . . . . -171.2(2) ?
C3 C2 C1 C6 . . . . -0.1(4) ?
C6 O7 C8 C9 . . . . -173.9(2) ?
C6 C5 C4 C3 . . . . 0.2(4) ?
C20 N19 N18 N17 . . . . -1.0(3) ?
C20 N19 C21 C26 . . . . -23.2(4) ?
C20 N19 C21 C22 . . . . 155.8(2) ?
C20 C12 C11 O10 . . . . -79.9(3) ?
C5 C6 C1 C2 . . . . 3.2(4) ?
C8 O7 C6 C5 . . . . -13.6(4) ?
C8 O7 C6 C1 . . . . 166.9(2) ?
C22 C21 C26 C25 . . . . -1.1(3) ?
C11 O10 C9 O16 . . . . -1.6(4) ?
C11 O10 C9 C8 . . . . 176.9(2) ?
C2 C3 C4 C5 . . . . 2.9(4) ?
C4 C3 C2 C1 . . . . -3.0(4) ?
C1 C6 C5 C4 . . . . -3.2(4) ?