#------------------------------------------------------------------------------
#$Date: 2024-06-26 04:47:00 +0300 (Wed, 26 Jun 2024) $
#$Revision: 292598 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023179.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_2023179
loop_
_publ_author_name
'Pronina, Anastasia A.'
'Podrezova, Alexandra G.'
'Grigoriev, Mikhail S.'
'Hasanov, Khudayar I.'
'Sadikhova, Nurlana D.'
'Akkurt, Mehmet'
'Bhattarai, Ajaya'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of
1-[6-bromo-2-(4-fluorophenyl)-1,2,3,4-tetrahydroquinolin-4-yl]pyrrolidin-2-one
;
_journal_coeditor_code EX2084
_journal_issue 7
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024005826
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C19 H18 Br F N2 O'
_chemical_formula_moiety 'C19 H18 Br F N2 O'
_chemical_formula_sum 'C19 H18 Br F N2 O'
_chemical_formula_weight 389.26
_chemical_name_systematic
1-[6-Bromo-2-(4-fluorophenyl)-1,2,3,4-tetrahydroquinolin-4-yl]pyrrolidin-2-one
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 101.518(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 9.2092(6)
_cell_length_b 9.0576(6)
_cell_length_c 20.4085(13)
_cell_measurement_reflns_used 5298
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 27.06
_cell_measurement_theta_min 3.03
_cell_volume 1668.06(19)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Bruker Kappa APEXII area-detector diffractometer'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0571
_diffrn_reflns_av_unetI/netI 0.0486
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 28015
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 30.140
_diffrn_reflns_theta_min 3.795
_exptl_absorpt_coefficient_mu 2.483
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.7522
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.550
_exptl_crystal_description bulk
_exptl_crystal_F_000 792
_exptl_crystal_size_max 0.400
_exptl_crystal_size_mid 0.360
_exptl_crystal_size_min 0.340
_refine_diff_density_max 0.445
_refine_diff_density_min -0.405
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.019
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 221
_refine_ls_number_reflns 4882
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.019
_refine_ls_R_factor_all 0.0574
_refine_ls_R_factor_gt 0.0345
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+0.8068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0659
_refine_ls_wR_factor_ref 0.0723
_reflns_number_gt 3713
_reflns_number_total 4882
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ex2084.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2023179
_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 0.437
_shelx_estimated_absorpt_t_max 0.486
_shelx_hkl_file
;
1 0 0 -0.6746 0.27633 8
1 0 0 0.15209 0.31493 12
1 0 0 -0.2487 0.40028 13
1 0 0 -0.2163 0.21343 6
1 0 0 0.33399 0.32361 1
1 0 0 0.20463 0.31348 1
2 0 0 2819.33 92.0768 1
2 0 0 2889.42 92.6688 13
2 0 0 2944.92 92.0129 8
2 0 0 2834.62 90.7764 11
2 0 0 2874.22 91.7409 12
2 0 0 2839.14 92.5113 1
2 0 0 2847.08 91.2487 6
-2 0 0 2671.63 95.3715 10
3 0 0 -0.0932 2.75100 12
3 0 0 1.33464 1.62619 11
-3 0 0 -4.9897 3.83303 10
3 0 0 -0.5926 2.41574 1
3 0 0 -5.7708 2.54906 1
3 0 0 3.40751 2.25369 6
3 0 0 2.52639 2.62684 8
4 0 0 73.9710 4.74263 11
4 0 0 63.8830 6.26359 12
4 0 0 75.6065 7.57295 1
4 0 0 66.9786 5.42563 6
4 0 0 68.0246 11.3348 9
-4 0 0 75.1911 9.82148 10
4 0 0 72.6618 6.87775 1
5 0 0 5.34547 8.56061 9
5 0 0 -6.0114 3.21409 6
5 0 0 1.98537 4.13552 1
-5 0 0 18.6107 7.76347 10
5 0 0 -1.0958 2.61763 11
5 0 0 -3.1106 4.16452 12
5 0 0 1.34727 5.02768 1
6 0 0 883.126 34.3509 12
6 0 0 886.637 35.8495 1
6 0 0 847.432 45.2911 9
6 0 0 919.779 31.2129 11
-6 0 0 886.223 40.7885 10
6 0 0 876.577 32.7158 6
6 0 0 899.934 36.4825 1
7 0 0 0.94042 3.30848 11
7 0 0 9.27726 7.66845 1
7 0 0 2.03090 11.4702 9
7 0 0 -6.4959 5.56831 1
7 0 0 -7.1736 4.89652 6
7 0 0 4.89454 5.45357 12
-7 0 0 2.60818 10.9312 10
8 0 0 329.436 29.6172 9
8 0 0 369.725 17.4860 6
8 0 0 330.069 19.6921 12
8 0 0 306.201 21.3891 1
9 0 0 -8.5900 7.18738 12
9 0 0 6.29403 15.3971 9
9 0 0 -1.6147 9.43940 1
9 0 0 4.30566 6.45191 6
10 0 0 413.534 27.6484 1
10 0 0 458.850 42.0083 9
11 0 0 3.45418 12.6566 1
11 0 0 21.2179 20.0258 9
12 0 0 -4.5649 13.5470 1
12 0 0 3.58961 22.5378 9
0 -1 0 1.31114 0.59619 1
0 -1 0 -0.2403 0.24060 6
0 -1 0 0.64311 0.54498 9
0 -1 0 0.17305 0.28913 5
0 -1 0 -0.2217 0.23205 3
0 -1 0 -0.1698 0.29609 12
0 1 0 -0.0756 0.30975 8
0 1 0 0.35668 0.58185 7
0 1 0 -0.3367 0.20336 13
0 1 0 0.06022 0.41934 1
1 -1 0 684.292 23.6158 1
1 1 0 688.131 24.4350 7
2 -1 0 1346.25 48.6505 9
2 -1 0 1366.33 44.5600 12
2 -1 0 1391.15 46.6082 8
2 -1 0 1344.49 46.4316 1
2 -1 0 1381.89 46.1871 1
2 1 0 1391.58 46.6526 4
2 1 0 1352.87 44.7798 14
-2 1 0 1388.04 46.5533 4
2 1 0 1364.13 45.8128 1
2 1 0 1381.55 46.2325 1
2 1 0 1368.25 46.4332 12
2 1 0 1400.57 46.0923 6
3 -1 0 182.951 12.4559 9
3 -1 0 168.890 6.58503 6
3 -1 0 171.123 9.71957 1
3 -1 0 168.156 7.62158 12
3 -1 0 161.829 9.16014 1
3 1 0 176.522 9.58386 12
3 1 0 170.100 9.31914 1
3 1 0 164.043 8.77595 6
-3 1 0 184.550 10.3529 4
3 1 0 159.291 9.14843 1
3 1 0 174.344 7.87553 8
4 -1 0 752.492 26.4407 12
4 -1 0 754.033 33.0019 9
4 -1 0 729.563 25.0981 6
4 -1 0 731.154 28.8628 1
4 -1 0 736.615 28.1962 1
-4 1 0 720.970 29.2925 4
4 1 0 728.604 28.3083 12
4 1 0 768.045 29.2544 1
4 1 0 708.891 28.5456 1
4 1 0 747.467 27.5258 6
4 1 0 738.176 26.6823 8
5 -1 0 385.753 23.4785 9
5 -1 0 376.581 14.5475 6
5 -1 0 382.966 16.0962 12
5 -1 0 377.817 18.9635 1
5 -1 0 389.818 18.1699 1
-5 -1 0 392.353 22.9962 10
-5 1 0 378.550 20.0079 4
5 1 0 368.817 15.7690 11
5 1 0 371.663 18.4557 1
5 1 0 369.376 17.2083 6
5 1 0 362.044 17.8163 12
6 -1 0 90.0014 10.1875 1
-6 -1 0 88.2981 14.5893 10
6 -1 0 104.314 15.4914 9
6 -1 0 95.1286 6.98770 6
6 -1 0 92.9354 8.55081 12
6 -1 0 107.366 11.4521 1
6 1 0 86.7089 9.81561 12
6 1 0 93.0354 11.1270 1
6 1 0 106.915 9.95069 6
-6 1 0 102.347 13.1162 4
6 1 0 105.102 11.0749 1
7 -1 0 51.1075 6.28123 6
-7 -1 0 35.7483 12.9017 10
7 -1 0 55.4044 10.8374 1
7 -1 0 50.7814 14.7341 9
7 -1 0 50.0568 7.73307 12
7 1 0 51.9886 9.86495 1
-7 1 0 48.0120 12.2668 4
7 1 0 43.9056 9.53038 12
7 1 0 45.0348 10.3039 1
7 1 0 46.2893 8.14532 6
8 -1 0 620.583 23.8968 6
8 -1 0 560.322 26.5229 12
8 -1 0 587.694 38.0057 9
8 -1 0 602.882 30.3451 1
-8 -1 0 579.996 36.7325 10
8 1 0 616.516 30.4158 1
8 1 0 581.133 26.7320 6
8 1 0 636.114 28.9740 12
-8 1 0 545.946 32.0164 4
-9 -1 0 429.371 35.3792 10
9 -1 0 356.469 34.8434 9
9 -1 0 368.343 21.4938 12
9 -1 0 388.150 25.3808 1
9 1 0 429.572 23.6324 12
-9 1 0 342.040 28.8889 4
9 1 0 377.663 21.0037 6
9 1 0 356.613 24.6170 1
10 -1 0 -14.437 16.3490 9
10 -1 0 4.23176 11.1016 1
10 1 0 7.14498 10.8305 12
10 1 0 13.8825 11.5273 1
-10 1 0 -18.145 13.9322 4
11 -1 0 62.8968 15.3751 1
11 -1 0 23.0698 22.1413 9
11 1 0 40.6521 14.4903 1
11 1 0 31.7184 25.0054 9
-11 1 0 48.7612 18.9624 4
12 -1 0 16.4674 14.5073 1
12 -1 0 -5.7860 21.7619 9
12 1 0 33.0865 14.7808 1
12 1 0 0.78038 22.0537 9
-12 1 0 -16.977 17.6272 4
0 -2 0 6879.39 227.162 9
0 -2 0 6966.26 224.938 5
0 -2 0 7096.45 226.091 3
0 -2 0 7067.50 225.496 12
0 -2 0 7092.49 225.472 6
0 -2 0 7364.43 226.148 1
0 2 0 7217.18 224.590 13
0 2 0 6957.53 226.721 7
0 2 0 7268.00 226.240 1
0 2 0 6747.86 225.243 8
1 -2 0 2358.61 76.1021 5
1 -2 0 2271.24 79.4676 9
1 -2 0 2425.03 78.2110 1
-1 -2 0 2392.80 78.1017 3
-1 -2 0 2333.09 77.8025 6
-1 -2 0 2338.30 78.0021 12
1 2 0 2384.78 79.3842 7
1 2 0 2395.57 76.0063 8
1 2 0 2334.93 77.6505 1
1 2 0 2442.55 77.7975 1
-1 2 0 2347.78 77.6684 13
-1 2 0 2395.61 78.3833 7
-1 2 0 2360.58 78.1925 1
-1 2 0 2375.36 78.0134 8
2 -2 0 94.6047 9.28020 9
-2 -2 0 102.133 6.92688 3
2 -2 0 102.322 7.05858 1
2 -2 0 100.130 5.08869 5
2 2 0 109.634 6.79628 1
2 2 0 110.430 4.25342 8
-2 2 0 113.398 7.15282 4
2 2 0 104.900 5.54261 14
2 2 0 92.0433 6.76752 12
2 2 0 117.911 6.86103 1
2 2 0 116.447 6.95848 6
-2 2 0 94.6000 7.91275 13
3 -2 0 2488.08 82.9897 1
-3 -2 0 2385.14 83.4311 3
3 -2 0 2475.68 86.8583 9
3 -2 0 2443.94 83.2137 1
3 2 0 2456.91 82.2775 1
3 2 0 2538.04 83.4490 12
-3 2 0 2412.65 83.9592 13
3 2 0 2488.80 82.8696 6
3 2 0 2566.72 82.6520 1
-3 2 0 2506.02 83.2635 4
3 2 0 2457.46 80.0268 14
4 -2 0 95.6731 11.9472 9
4 -2 0 113.861 9.66338 1
-4 -2 0 82.7349 13.5694 3
4 -2 0 99.9287 8.78436 1
4 2 0 98.3597 8.92375 6
4 2 0 99.2536 5.86381 8
4 2 0 98.6788 8.43128 1
4 2 0 82.3506 8.91133 12
4 2 0 111.230 8.86841 1
-4 2 0 98.0211 9.84219 4
4 2 0 96.2977 5.59212 14
5 -2 0 0.58185 3.25701 12
5 -2 0 6.30304 8.40893 9
5 -2 0 -0.2494 5.45092 1
5 2 0 -2.4670 5.68597 12
5 2 0 0.91252 4.91985 1
5 2 0 4.02983 4.53559 1
5 2 0 4.30310 2.60433 14
5 2 0 19.9528 5.94953 6
-5 2 0 9.49563 6.97759 4
5 2 0 0.74549 3.20101 8
6 -2 0 6.61271 10.1900 9
6 -2 0 15.3341 7.39013 1
6 -2 0 16.1494 4.72308 12
6 2 0 29.0055 7.83258 12
6 2 0 2.67718 7.01854 1
6 2 0 13.8673 3.56121 14
-6 2 0 17.4728 7.37144 4
6 2 0 14.9034 6.28717 1
6 2 0 7.29278 6.03671 6
7 -2 0 1331.15 47.3889 12
7 -2 0 1230.54 59.3182 9
7 -2 0 1380.63 52.7822 1
7 2 0 1276.61 51.3540 12
7 2 0 1333.30 45.3763 14
-7 2 0 1299.63 53.9801 4
7 2 0 1386.26 50.3619 6
7 2 0 1317.02 52.6327 1
8 -2 0 3.56770 13.1908 9
8 -2 0 38.0764 7.51023 12
-8 -2 0 15.5557 13.9461 10
8 -2 0 7.21504 9.40110 1
8 2 0 11.5196 3.68574 14
8 2 0 24.9543 9.41730 12
8 2 0 9.00155 9.45522 1
8 2 0 22.9140 7.89240 6
-8 2 0 21.3841 12.1420 4
-9 -2 0 23.0578 16.6974 10
9 -2 0 22.9275 11.6996 1
9 -2 0 8.51140 13.2904 9
9 2 0 10.0895 9.51015 12
-9 2 0 7.73704 13.3450 4
9 2 0 12.5247 10.9356 1
9 2 0 27.5228 10.0239 6
10 -2 0 17.4058 19.3565 9
-10 -2 0 48.9804 19.6139 10
10 -2 0 24.2327 12.8606 1
10 2 0 30.9785 13.4692 12
-10 2 0 16.0351 14.9246 4
10 2 0 39.3473 13.1919 1
10 2 0 26.9341 11.2650 6
-11 -2 0 36.8046 21.9361 10
11 -2 0 26.5336 14.6806 1
11 -2 0 15.2050 22.3489 9
11 2 0 37.2421 14.0838 1
-11 2 0 25.4961 17.4837 4
12 -2 0 42.2677 16.7004 1
12 -2 0 34.9420 26.4065 9
-12 2 0 31.4613 20.2293 4
12 2 0 22.0998 14.6457 1
0 -3 0 2.91412 2.72814 12
0 -3 0 -0.2487 2.69575 5
0 -3 0 -2.8237 4.26756 9
0 -3 0 -1.3048 3.25677 3
0 -3 0 -1.6709 2.46976 6
0 3 0 1.29399 2.51375 8
0 3 0 5.56164 3.71390 7
0 3 0 -1.0309 3.05425 1
0 3 0 0.20255 2.03450 13
1 -3 0 1784.79 58.1920 5
-1 -3 0 1833.08 60.7344 3
-1 -3 0 1771.72 60.4299 12
1 -3 0 1759.65 62.6677 9
1 3 0 1787.30 58.2706 8
1 3 0 1702.78 60.2551 1
-1 3 0 1738.61 59.5962 13
-1 3 0 1761.94 60.3268 8
1 3 0 1830.20 60.5021 1
-2 -3 0 641.348 26.3720 12
-2 -3 0 678.092 26.5909 3
2 -3 0 664.292 23.0823 5
2 -3 0 663.283 28.7320 9
2 3 0 658.130 22.4077 8
2 3 0 689.978 25.9153 1
2 3 0 662.903 25.6965 1
-2 3 0 714.768 26.7675 8
-2 3 0 688.507 26.3278 13
-3 -3 0 393.159 18.5359 3
3 -3 0 380.265 14.1568 5
3 -3 0 388.695 20.7358 9
3 3 0 401.638 18.1890 6
3 3 0 365.310 16.9646 1
3 3 0 378.460 12.4170 8
-3 3 0 370.557 17.8537 13
3 3 0 394.500 17.1032 1
-3 3 0 367.621 17.3510 4
3 3 0 347.868 18.0862 12
4 -3 0 872.814 35.4832 1
-4 -3 0 878.788 35.6687 3
4 -3 0 886.363 39.3982 9
4 3 0 860.912 29.3371 8
4 3 0 878.226 28.8756 8
-4 3 0 879.347 34.8406 4
4 3 0 910.520 34.8365 6
4 3 0 891.731 35.1260 12
4 3 0 848.065 33.4638 1
-4 3 0 882.193 36.0073 13
4 3 0 906.002 34.0731 1
5 -3 0 217.039 15.5159 1
-5 -3 0 236.208 17.0453 3
5 -3 0 226.260 21.1549 9
5 3 0 227.483 13.9428 1
5 3 0 252.670 15.2204 12
-5 3 0 231.019 14.8763 4
-5 3 0 228.126 16.9594 13
5 3 0 237.471 9.80601 14
5 3 0 217.701 14.4298 1
5 3 0 238.209 15.1678 6
5 3 0 232.546 9.74158 8
6 -3 0 299.341 19.4230 1
6 -3 0 265.816 25.3617 9
6 3 0 254.518 17.2040 6
6 3 0 268.132 17.5292 1
6 3 0 244.375 17.8645 12
-6 3 0 289.806 19.4742 4
6 3 0 286.934 12.2593 8
6 3 0 257.632 16.5297 1
6 3 0 274.843 10.5358 14
7 -3 0 78.3456 12.5391 1
7 -3 0 72.8915 17.8322 9
7 3 0 66.5515 11.8520 12
-7 3 0 79.9031 13.8474 4
7 3 0 67.1688 12.0995 1
7 3 0 74.5203 11.6178 6
8 -3 0 255.454 21.3064 1
8 -3 0 251.172 28.5495 9
8 3 0 248.122 19.3162 6
8 3 0 239.216 20.3763 12
-8 3 0 252.442 23.4542 4
9 -3 0 259.675 31.4645 9
9 -3 0 209.650 21.6602 1
-9 3 0 261.342 25.1426 4
9 3 0 306.446 20.8306 6
9 3 0 245.218 22.8326 12
9 3 0 257.308 22.9300 1
10 -3 0 33.0122 21.2041 9
10 -3 0 64.5311 15.8084 1
-10 -3 0 49.7868 24.9382 10
10 3 0 102.297 17.1157 1
-10 3 0 41.2943 14.4689 4
10 3 0 64.8129 15.0211 12
10 3 0 65.8788 13.5328 6
11 -3 0 10.0284 14.7787 1
11 -3 0 22.3263 25.3772 9
-11 -3 0 15.5746 20.7767 10
-11 3 0 5.74728 18.1025 4
11 3 0 12.4429 15.3125 12
11 3 0 12.2515 13.6465 1
12 -3 0 126.845 32.9847 9
12 -3 0 129.328 23.0648 1
-12 -3 0 96.0225 27.1974 10
12 3 0 135.921 20.8798 1
-12 3 0 149.126 27.6206 4
0 -4 0 119.858 9.85810 3
0 -4 0 124.211 8.80154 12
0 -4 0 117.066 7.56252 5
0 -4 0 111.917 11.4653 9
0 4 0 118.583 6.78597 13
0 4 0 122.961 8.31306 8
1 -4 0 118.551 11.9406 9
1 -4 0 112.700 6.80040 5
-1 -4 0 105.355 8.95114 12
-1 -4 0 117.117 9.66256 3
1 4 0 107.724 6.83813 8
-1 4 0 98.8169 8.65754 8
1 4 0 112.074 4.81397 13
-1 4 0 113.552 7.68163 13
2 -4 0 572.917 20.7704 5
2 -4 0 567.351 27.3116 9
-2 -4 0 577.351 24.6056 12
-2 -4 0 641.155 25.2224 3
2 4 0 565.797 20.3090 8
-2 4 0 565.561 24.4313 8
-2 4 0 551.283 23.7785 13
2 4 0 569.161 24.2696 1
-3 -4 0 -0.4070 6.18831 12
3 -4 0 4.46523 7.47707 9
3 -4 0 2.59755 2.59600 5
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1 2 27 54.9023 21.8250 11
5 -3 -27 3.99755 16.2418 1
-5 -3 27 -18.647 19.0660 11
-5 3 27 11.4253 21.7978 2
5 3 -27 -24.883 18.0036 8
5 3 -27 -6.0772 13.7502 1
-4 -3 27 234.229 32.6996 11
4 -3 -27 198.148 26.5271 1
4 3 -27 208.985 29.7866 8
4 3 -27 190.859 25.1900 1
-4 3 27 225.095 35.8401 2
-3 -3 27 8.78401 20.7328 11
3 -3 -27 37.7272 20.1237 1
-3 3 27 68.7666 24.6685 11
-3 3 27 59.8722 25.6260 2
3 3 -27 51.9145 19.1309 1
3 3 -27 10.0029 14.6103 8
2 -3 -27 55.4522 21.2585 1
-2 -3 27 12.7666 20.2692 11
-2 3 27 32.3525 22.5633 11
2 3 -27 8.21847 16.0352 1
-2 3 27 40.4701 21.2272 2
-1 -3 27 60.6275 22.2551 11
1 -3 -27 76.0937 22.1447 1
1 3 -27 73.9972 21.7040 1
-1 3 27 78.7800 23.5390 2
-1 3 27 46.2949 24.2279 11
0 -3 27 25.3285 22.3948 11
0 3 27 42.5938 23.1257 11
0 3 -27 -0.5982 19.8726 1
-4 -4 27 1.52067 21.4830 11
4 -4 -27 8.98464 15.9119 1
4 4 -27 -4.2896 19.4653 8
-4 4 27 19.1726 22.8548 2
4 4 -27 26.6107 16.4999 1
3 -4 -27 92.9610 22.3233 1
-3 -4 27 24.2323 21.4357 11
3 4 -27 37.5512 21.2054 8
-3 4 27 104.028 26.2747 2
-3 4 27 45.4757 26.8438 11
3 4 -27 69.3959 20.4992 1
-2 -4 27 -25.107 18.2712 11
2 -4 -27 13.7351 18.5116 1
-2 4 27 23.1956 22.4639 2
-2 4 27 5.86118 21.7976 11
2 4 -27 6.44649 17.4773 1
2 4 -27 12.7720 19.1701 8
-1 -4 27 111.824 24.9407 11
1 4 -27 78.1817 22.3085 1
-1 4 27 61.9239 25.6477 11
-1 4 27 72.5559 23.3116 2
5 0 -28 35.4728 15.8706 1
-5 0 28 2.85052 22.7309 2
-4 0 28 12.3193 21.0623 11
4 0 -28 1.56544 15.8632 1
-3 0 28 -19.559 18.5793 11
3 0 -28 14.9560 15.6987 1
-2 0 28 99.5395 25.5462 11
2 0 -28 129.205 24.7708 1
-1 0 28 -36.311 17.1212 11
1 0 -28 4.48540 17.9243 1
0 0 -28 49.5791 21.6838 1
0 0 28 70.8041 23.2467 11
5 -1 -28 34.4381 17.0627 1
5 1 -28 17.2831 14.8651 1
-5 1 28 80.6801 28.1859 2
5 1 -28 30.8554 22.8890 8
4 -1 -28 57.3484 18.5678 1
-4 -1 28 59.7479 24.6596 11
-4 1 28 70.4262 24.8640 11
-4 1 28 50.2171 27.8602 2
4 1 -28 79.0083 19.1608 1
3 -1 -28 3.81474 17.0120 1
-3 -1 28 51.8391 23.1012 11
3 1 -28 26.5851 16.5126 1
-3 1 28 7.07982 20.9007 11
-2 -1 28 10.9508 20.4856 11
2 -1 -28 48.7720 19.3113 1
-2 1 28 12.5926 20.5039 11
2 1 -28 28.8433 18.3122 1
-1 -1 28 41.3158 21.8547 11
1 -1 -28 39.5675 20.9281 1
1 1 -28 45.8201 20.3830 1
-1 1 28 28.2169 21.6857 11
0 -1 28 39.4933 20.6574 11
0 1 28 28.4083 23.4854 11
0 1 -28 49.0381 21.7511 1
4 -2 -28 26.9315 18.8162 1
-4 -2 28 73.5721 24.5078 11
4 2 -28 52.1485 24.5172 8
4 2 -28 59.1634 17.5509 1
-4 2 28 37.0649 27.3641 2
-3 -2 28 51.4431 23.6267 11
3 -2 -28 55.7818 19.8659 1
-3 2 28 78.1690 25.3582 11
3 2 -28 54.6514 19.0678 1
-3 2 28 22.1838 24.6078 2
-2 -2 28 12.2744 19.5215 11
2 -2 -28 12.8752 19.3192 1
2 2 -28 10.6349 17.1697 1
-2 2 28 11.6906 19.8913 2
-2 2 28 46.3067 23.3662 11
-1 -2 28 50.3131 22.1850 11
1 -2 -28 23.7785 20.6942 1
-1 2 28 64.5456 24.0677 11
1 2 -28 90.2729 23.0965 1
3 -3 -28 30.3064 19.7762 1
3 3 -28 2.75852 17.1775 1
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 64296
_shelx_res_file
;
TITL PA-117 in P2(1)/n
shelx.res
created by SHELXL-2018/3 at 11:15:30 on 04-Apr-2024
CELL 0.71073 9.2092 9.0576 20.4085 90.000 101.518 90.000
ZERR 4.00 0.0006 0.0006 0.0013 0.000 0.002 0.000
LATT 1
SYMM 1/2 - X, 1/2 + Y, 1/2 - Z
SFAC C H BR F N O
UNIT 76 72 4 4 8 4
MERG 2
SHEL 5.5 0.5
EQIV $1 -x+1, -y, -z+1
HTAB N1 O1_$1
EQIV $2 x-1/2, -y+1/2, z+1/2
HTAB C5 F1_$2
EQIV $3 -x+2, -y, -z+1
HTAB C23 O1_$3
HTAB N1 O1_$1
HTAB C5 F1_$2
EQIV $4 x+1, y, z
HTAB C15 Br1_$4
HTAB C23 O1_$3
FMAP 2
PLAN 5
SIZE 0.340 0.360 0.400
ACTA
BOND $H
CONF
L.S. 13
TEMP -173.00
WGHT 0.026700 0.806800
FVAR 0.44588
C2 1 0.648971 0.125024 0.428630 11.00000 0.01220 0.01256 =
0.00937 0.00069 0.00270 -0.00008
AFIX 13
H2A 2 0.664204 0.021487 0.445624 11.00000 -1.20000
AFIX 0
C3 1 0.709403 0.231122 0.485625 11.00000 0.01210 0.01169 =
0.01057 -0.00036 0.00293 -0.00166
AFIX 23
H3A 2 0.695266 0.334338 0.469667 11.00000 -1.20000
H3B 2 0.816813 0.213924 0.501577 11.00000 -1.20000
AFIX 0
C4 1 0.627220 0.205789 0.542731 11.00000 0.01235 0.00901 =
0.00841 -0.00069 0.00274 -0.00132
AFIX 13
H4A 2 0.639259 0.099050 0.555148 11.00000 -1.20000
AFIX 0
C4A 1 0.463444 0.231956 0.517030 11.00000 0.01282 0.00712 =
0.00938 0.00160 0.00288 -0.00222
C5 1 0.372157 0.285480 0.558356 11.00000 0.01595 0.01140 =
0.01063 -0.00049 0.00369 -0.00218
AFIX 43
H5A 2 0.413562 0.314242 0.602937 11.00000 -1.20000
AFIX 0
C6 1 0.220995 0.296772 0.534451 11.00000 0.01316 0.01108 =
0.01708 -0.00063 0.00724 0.00055
C7 1 0.156921 0.250282 0.470722 11.00000 0.01039 0.01249 =
0.02030 0.00111 0.00304 -0.00083
AFIX 43
H7A 2 0.052477 0.253929 0.455694 11.00000 -1.20000
AFIX 0
C8 1 0.247201 0.198366 0.429162 11.00000 0.01371 0.01054 =
0.01306 -0.00108 0.00072 -0.00287
AFIX 43
H8A 2 0.204136 0.166365 0.385250 11.00000 -1.20000
AFIX 0
C8A 1 0.401472 0.192342 0.450990 11.00000 0.01356 0.00693 =
0.01293 0.00111 0.00393 -0.00160
C12 1 0.742022 0.223598 0.661423 11.00000 0.00941 0.01635 =
0.01016 0.00111 0.00384 0.00236
C13 1 0.811585 0.341244 0.709948 11.00000 0.01768 0.02072 =
0.01130 -0.00185 -0.00007 -0.00108
AFIX 23
H13A 2 0.921011 0.333787 0.718707 11.00000 -1.20000
H13B 2 0.777820 0.331985 0.752877 11.00000 -1.20000
AFIX 0
C14 1 0.760084 0.487188 0.675780 11.00000 0.04111 0.01609 =
0.01484 -0.00306 0.00049 -0.00471
AFIX 23
H14A 2 0.677041 0.529078 0.693974 11.00000 -1.20000
H14B 2 0.842211 0.559631 0.682281 11.00000 -1.20000
AFIX 0
C15 1 0.710070 0.449268 0.601915 11.00000 0.01833 0.01061 =
0.01472 -0.00115 0.00268 -0.00244
AFIX 23
H15A 2 0.617049 0.501351 0.582257 11.00000 -1.20000
H15B 2 0.787199 0.475484 0.576387 11.00000 -1.20000
AFIX 0
C21 1 0.729952 0.144883 0.371543 11.00000 0.01262 0.01362 =
0.00714 -0.00212 0.00084 -0.00104
C22 1 0.845263 0.049345 0.366157 11.00000 0.01529 0.01380 =
0.01403 -0.00118 0.00251 0.00037
AFIX 43
H22A 2 0.866503 -0.031520 0.396188 11.00000 -1.20000
AFIX 0
C23 1 0.930007 0.070008 0.317636 11.00000 0.01157 0.02196 =
0.01665 -0.00692 0.00163 -0.00037
AFIX 43
H23A 2 1.008962 0.004965 0.314036 11.00000 -1.20000
AFIX 0
C24 1 0.895498 0.187288 0.275353 11.00000 0.01396 0.03557 =
0.01034 -0.00169 0.00535 -0.00185
C25 1 0.782863 0.284931 0.278489 11.00000 0.02182 0.03630 =
0.01885 0.01382 0.00802 0.00658
AFIX 43
H25A 2 0.762472 0.365242 0.248101 11.00000 -1.20000
AFIX 0
C26 1 0.699907 0.262719 0.327319 11.00000 0.01617 0.02331 =
0.01714 0.00744 0.00642 0.00699
AFIX 43
H26A 2 0.621590 0.328838 0.330588 11.00000 -1.20000
AFIX 0
BR1 3 0.100627 0.377062 0.591524 11.00000 0.01630 0.02401 =
0.02408 -0.00610 0.00963 0.00192
F1 4 0.977795 0.209877 0.227406 11.00000 0.02342 0.05551 =
0.01863 0.00602 0.01413 0.00115
N1 5 0.489563 0.150975 0.405984 11.00000 0.01156 0.01730 =
0.00956 -0.00365 0.00264 -0.00315
N11 5 0.687198 0.289873 0.602273 11.00000 0.01367 0.00841 =
0.00794 -0.00018 0.00128 -0.00020
O1 6 0.736762 0.090594 0.672145 11.00000 0.02283 0.01256 =
0.01178 0.00310 0.00251 0.00420
H1 2 0.445667 0.093942 0.375288 11.00000 0.02221
HKLF 4
REM PA-117 in P2(1)/n
REM wR2 = 0.0723, GooF = S = 1.019, Restrained GooF = 1.019 for all data
REM R1 = 0.0345 for 3713 Fo > 4sig(Fo) and 0.0574 for all 4882 data
REM 221 parameters refined using 0 restraints
END
WGHT 0.0267 0.8068
REM Highest difference peak 0.445, deepest hole -0.405, 1-sigma level 0.083
Q1 1 0.6786 0.2232 0.5210 11.00000 0.05 0.44
Q2 1 0.7937 0.1031 0.3672 11.00000 0.05 0.43
Q3 1 0.8658 0.0420 0.3304 11.00000 0.05 0.40
Q4 1 0.3297 0.2263 0.4427 11.00000 0.05 0.39
Q5 1 0.6243 0.4862 0.6760 11.00000 0.05 0.38
;
_shelx_res_checksum 6533
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C2 0.64897(19) 0.1250(2) 0.42863(9) 0.0113(3) Uani d 1 . .
H H2A 0.664204 0.021487 0.445624 0.014 Uiso calc 1 . .
C C3 0.7094(2) 0.2311(2) 0.48563(9) 0.0114(4) Uani d 1 . .
H H3A 0.695266 0.334338 0.469667 0.014 Uiso calc 1 . .
H H3B 0.816813 0.213924 0.501577 0.014 Uiso calc 1 . .
C C4 0.62722(19) 0.2058(2) 0.54273(9) 0.0098(3) Uani d 1 . .
H H4A 0.639259 0.099050 0.555148 0.012 Uiso calc 1 . .
C C4A 0.46344(19) 0.23196(19) 0.51703(9) 0.0097(3) Uani d 1 . .
C C5 0.3722(2) 0.2855(2) 0.55836(9) 0.0125(4) Uani d 1 . .
H H5A 0.413562 0.314242 0.602937 0.015 Uiso calc 1 . .
C C6 0.2210(2) 0.2968(2) 0.53445(10) 0.0132(4) Uani d 1 . .
C C7 0.1569(2) 0.2503(2) 0.47072(10) 0.0144(4) Uani d 1 . .
H H7A 0.052477 0.253929 0.455694 0.017 Uiso calc 1 . .
C C8 0.2472(2) 0.1984(2) 0.42916(10) 0.0127(4) Uani d 1 . .
H H8A 0.204136 0.166365 0.385250 0.015 Uiso calc 1 . .
C C8A 0.4015(2) 0.19234(19) 0.45099(9) 0.0110(4) Uani d 1 . .
C C12 0.74202(19) 0.2236(2) 0.66142(9) 0.0117(4) Uani d 1 . .
C C13 0.8116(2) 0.3412(2) 0.70995(10) 0.0170(4) Uani d 1 . .
H H13A 0.921011 0.333787 0.718707 0.020 Uiso calc 1 . .
H H13B 0.777820 0.331985 0.752877 0.020 Uiso calc 1 . .
C C14 0.7601(3) 0.4872(2) 0.67578(10) 0.0247(5) Uani d 1 . .
H H14A 0.677041 0.529078 0.693974 0.030 Uiso calc 1 . .
H H14B 0.842211 0.559631 0.682281 0.030 Uiso calc 1 . .
C C15 0.7101(2) 0.4493(2) 0.60191(10) 0.0146(4) Uani d 1 . .
H H15A 0.617049 0.501351 0.582257 0.018 Uiso calc 1 . .
H H15B 0.787199 0.475484 0.576387 0.018 Uiso calc 1 . .
C C21 0.7300(2) 0.1449(2) 0.37154(9) 0.0113(4) Uani d 1 . .
C C22 0.8453(2) 0.0493(2) 0.36616(10) 0.0144(4) Uani d 1 . .
H H22A 0.866503 -0.031520 0.396188 0.017 Uiso calc 1 . .
C C23 0.9300(2) 0.0700(2) 0.31764(10) 0.0169(4) Uani d 1 . .
H H23A 1.008962 0.004965 0.314036 0.020 Uiso calc 1 . .
C C24 0.8955(2) 0.1873(3) 0.27535(10) 0.0195(4) Uani d 1 . .
C C25 0.7829(2) 0.2849(3) 0.27849(11) 0.0251(5) Uani d 1 . .
H H25A 0.762472 0.365242 0.248101 0.030 Uiso calc 1 . .
C C26 0.6999(2) 0.2627(2) 0.32732(10) 0.0184(4) Uani d 1 . .
H H26A 0.621590 0.328838 0.330588 0.022 Uiso calc 1 . .
Br Br1 0.10063(2) 0.37706(2) 0.59152(2) 0.02069(7) Uani d 1 . .
F F1 0.97779(13) 0.20988(16) 0.22741(6) 0.0311(3) Uani d 1 . .
N N1 0.48956(17) 0.15098(18) 0.40598(8) 0.0127(3) Uani d 1 . .
N N11 0.68720(16) 0.28987(17) 0.60227(7) 0.0101(3) Uani d 1 . .
O O1 0.73676(15) 0.09059(14) 0.67215(7) 0.0159(3) Uani d 1 . .
H H1 0.446(3) 0.094(3) 0.3753(12) 0.022(6) Uiso 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
C2 0.0122(8) 0.0126(9) 0.0094(9) -0.0001(7) 0.0027(7) 0.0007(7)
C3 0.0121(8) 0.0117(9) 0.0106(9) -0.0017(7) 0.0029(7) -0.0004(7)
C4 0.0124(8) 0.0090(9) 0.0084(9) -0.0013(7) 0.0027(7) -0.0007(7)
C4A 0.0128(8) 0.0071(8) 0.0094(9) -0.0022(7) 0.0029(7) 0.0016(7)
C5 0.0159(9) 0.0114(9) 0.0106(9) -0.0022(7) 0.0037(7) -0.0005(7)
C6 0.0132(9) 0.0111(9) 0.0171(10) 0.0006(7) 0.0072(8) -0.0006(7)
C7 0.0104(8) 0.0125(9) 0.0203(10) -0.0008(7) 0.0030(8) 0.0011(8)
C8 0.0137(9) 0.0105(9) 0.0131(9) -0.0029(7) 0.0007(7) -0.0011(7)
C8A 0.0136(9) 0.0069(9) 0.0129(9) -0.0016(7) 0.0039(7) 0.0011(7)
C12 0.0094(8) 0.0164(10) 0.0102(9) 0.0024(7) 0.0038(7) 0.0011(7)
C13 0.0177(10) 0.0207(11) 0.0113(10) -0.0011(8) -0.0001(8) -0.0019(8)
C14 0.0411(13) 0.0161(11) 0.0148(11) -0.0047(9) 0.0005(10) -0.0031(8)
C15 0.0183(9) 0.0106(9) 0.0147(10) -0.0024(7) 0.0027(8) -0.0012(7)
C21 0.0126(8) 0.0136(10) 0.0071(8) -0.0010(7) 0.0008(7) -0.0021(7)
C22 0.0153(9) 0.0138(10) 0.0140(10) 0.0004(7) 0.0025(8) -0.0012(8)
C23 0.0116(9) 0.0220(11) 0.0167(10) -0.0004(8) 0.0016(8) -0.0069(8)
C24 0.0140(9) 0.0356(12) 0.0103(10) -0.0018(9) 0.0053(8) -0.0017(9)
C25 0.0218(11) 0.0363(13) 0.0188(11) 0.0066(9) 0.0080(9) 0.0138(10)
C26 0.0162(9) 0.0233(11) 0.0171(10) 0.0070(8) 0.0064(8) 0.0074(8)
Br1 0.01630(10) 0.02401(11) 0.02408(12) 0.00192(9) 0.00963(8) -0.00610(10)
F1 0.0234(7) 0.0555(9) 0.0186(7) 0.0011(6) 0.0141(5) 0.0060(6)
N1 0.0116(7) 0.0173(9) 0.0096(8) -0.0032(6) 0.0026(6) -0.0037(6)
N11 0.0137(7) 0.0084(7) 0.0079(7) -0.0002(6) 0.0013(6) -0.0002(6)
O1 0.0228(7) 0.0126(7) 0.0118(7) 0.0042(5) 0.0025(6) 0.0031(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 '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
N1 C2 C21 . . 110.74(14) ?
N1 C2 C3 . . 109.20(15) ?
C21 C2 C3 . . 110.55(14) ?
N1 C2 H2A . . 108.8 ?
C21 C2 H2A . . 108.8 ?
C3 C2 H2A . . 108.8 ?
C2 C3 C4 . . 109.03(14) ?
C2 C3 H3A . . 109.9 ?
C4 C3 H3A . . 109.9 ?
C2 C3 H3B . . 109.9 ?
C4 C3 H3B . . 109.9 ?
H3A C3 H3B . . 108.3 ?
N11 C4 C4A . . 113.30(14) ?
N11 C4 C3 . . 113.41(14) ?
C4A C4 C3 . . 108.86(15) ?
N11 C4 H4A . . 107.0 ?
C4A C4 H4A . . 107.0 ?
C3 C4 H4A . . 107.0 ?
C5 C4A C8A . . 119.53(17) ?
C5 C4A C4 . . 121.70(16) ?
C8A C4A C4 . . 118.66(15) ?
C6 C5 C4A . . 119.94(18) ?
C6 C5 H5A . . 120.0 ?
C4A C5 H5A . . 120.0 ?
C7 C6 C5 . . 121.30(17) ?
C7 C6 Br1 . . 120.02(14) ?
C5 C6 Br1 . . 118.67(14) ?
C6 C7 C8 . . 118.99(17) ?
C6 C7 H7A . . 120.5 ?
C8 C7 H7A . . 120.5 ?
C7 C8 C8A . . 120.88(18) ?
C7 C8 H8A . . 119.6 ?
C8A C8 H8A . . 119.6 ?
N1 C8A C4A . . 121.61(16) ?
N1 C8A C8 . . 119.18(17) ?
C4A C8A C8 . . 119.19(16) ?
O1 C12 N11 . . 125.02(18) ?
O1 C12 C13 . . 127.12(17) ?
N11 C12 C13 . . 107.85(16) ?
C12 C13 C14 . . 105.05(16) ?
C12 C13 H13A . . 110.7 ?
C14 C13 H13A . . 110.7 ?
C12 C13 H13B . . 110.7 ?
C14 C13 H13B . . 110.7 ?
H13A C13 H13B . . 108.8 ?
C15 C14 C13 . . 105.17(17) ?
C15 C14 H14A . . 110.7 ?
C13 C14 H14A . . 110.7 ?
C15 C14 H14B . . 110.7 ?
C13 C14 H14B . . 110.7 ?
H14A C14 H14B . . 108.8 ?
N11 C15 C14 . . 103.49(16) ?
N11 C15 H15A . . 111.1 ?
C14 C15 H15A . . 111.1 ?
N11 C15 H15B . . 111.1 ?
C14 C15 H15B . . 111.1 ?
H15A C15 H15B . . 109.0 ?
C26 C21 C22 . . 118.86(17) ?
C26 C21 C2 . . 121.75(16) ?
C22 C21 C2 . . 119.20(16) ?
C23 C22 C21 . . 121.23(18) ?
C23 C22 H22A . . 119.4 ?
C21 C22 H22A . . 119.4 ?
C24 C23 C22 . . 117.51(18) ?
C24 C23 H23A . . 121.2 ?
C22 C23 H23A . . 121.2 ?
C23 C24 F1 . . 118.44(18) ?
C23 C24 C25 . . 123.63(18) ?
F1 C24 C25 . . 117.93(19) ?
C24 C25 C26 . . 118.0(2) ?
C24 C25 H25A . . 121.0 ?
C26 C25 H25A . . 121.0 ?
C25 C26 C21 . . 120.77(18) ?
C25 C26 H26A . . 119.6 ?
C21 C26 H26A . . 119.6 ?
C8A N1 C2 . . 120.88(16) ?
C8A N1 H1 . . 113.3(15) ?
C2 N1 H1 . . 115.7(15) ?
C12 N11 C4 . . 121.86(16) ?
C12 N11 C15 . . 114.52(16) ?
C4 N11 C15 . . 123.22(15) ?
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
C2 N1 . 1.467(2) ?
C2 C21 . 1.514(2) ?
C2 C3 . 1.526(2) ?
C2 H2A . 1.0000 ?
C3 C4 . 1.528(2) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 N11 . 1.447(2) ?
C4 C4A . 1.513(2) ?
C4 H4A . 1.0000 ?
C4A C5 . 1.391(2) ?
C4A C8A . 1.401(3) ?
C5 C6 . 1.384(3) ?
C5 H5A . 0.9500 ?
C6 C7 . 1.382(3) ?
C6 Br1 . 1.9053(18) ?
C7 C8 . 1.383(3) ?
C7 H7A . 0.9500 ?
C8 C8A . 1.403(3) ?
C8 H8A . 0.9500 ?
C8A N1 . 1.393(2) ?
C12 O1 . 1.227(2) ?
C12 N11 . 1.352(2) ?
C12 C13 . 1.508(3) ?
C13 C14 . 1.525(3) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C14 C15 . 1.525(3) ?
C14 H14A . 0.9900 ?
C14 H14B . 0.9900 ?
C15 N11 . 1.459(2) ?
C15 H15A . 0.9900 ?
C15 H15B . 0.9900 ?
C21 C26 . 1.389(3) ?
C21 C22 . 1.391(3) ?
C22 C23 . 1.390(3) ?
C22 H22A . 0.9500 ?
C23 C24 . 1.365(3) ?
C23 H23A . 0.9500 ?
C24 F1 . 1.367(2) ?
C24 C25 . 1.374(3) ?
C25 C26 . 1.386(3) ?
C25 H25A . 0.9500 ?
C26 H26A . 0.9500 ?
N1 H1 . 0.85(2) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1 O1 3_656 0.85(2) 2.43(2) 3.217(2) 154(2) yes
C5 H5A F1 4_566 0.95 2.50 3.393(2) 156.6 yes
C23 H23A O1 3_756 0.95 2.46 3.365(2) 159.3 yes
C15 H15B Br1 1_655 0.99 2.98 3.703(2) 131.0 yes
C2 H2A Cg3 3_656 1.00 2.68 3.676(2) 172 yes
C15 H15A Cg3 3_666 0.99 2.94 3.386(2) 109 yes
C15 H15B Cg3 3_666 0.99 2.97 3.386(2) 106 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 C2 C3 C4 . . . . 59.01(19) ?
C21 C2 C3 C4 . . . . -178.91(15) ?
C2 C3 C4 N11 . . . . 173.65(15) ?
C2 C3 C4 C4A . . . . -59.24(19) ?
N11 C4 C4A C5 . . . . -22.0(2) ?
C3 C4 C4A C5 . . . . -149.14(17) ?
N11 C4 C4A C8A . . . . 162.03(16) ?
C3 C4 C4A C8A . . . . 34.9(2) ?
C8A C4A C5 C6 . . . . 1.1(3) ?
C4 C4A C5 C6 . . . . -174.83(17) ?
C4A C5 C6 C7 . . . . 2.6(3) ?
C4A C5 C6 Br1 . . . . -177.82(14) ?
C5 C6 C7 C8 . . . . -3.2(3) ?
Br1 C6 C7 C8 . . . . 177.20(14) ?
C6 C7 C8 C8A . . . . 0.1(3) ?
C5 C4A C8A N1 . . . . 174.11(16) ?
C4 C4A C8A N1 . . . . -9.8(3) ?
C5 C4A C8A C8 . . . . -4.1(3) ?
C4 C4A C8A C8 . . . . 171.96(16) ?
C7 C8 C8A N1 . . . . -174.75(17) ?
C7 C8 C8A C4A . . . . 3.5(3) ?
O1 C12 C13 C14 . . . . -169.00(18) ?
N11 C12 C13 C14 . . . . 12.1(2) ?
C12 C13 C14 C15 . . . . -19.0(2) ?
C13 C14 C15 N11 . . . . 18.7(2) ?
N1 C2 C21 C26 . . . . 44.1(2) ?
C3 C2 C21 C26 . . . . -77.1(2) ?
N1 C2 C21 C22 . . . . -140.90(18) ?
C3 C2 C21 C22 . . . . 97.9(2) ?
C26 C21 C22 C23 . . . . 0.0(3) ?
C2 C21 C22 C23 . . . . -175.11(17) ?
C21 C22 C23 C24 . . . . -0.2(3) ?
C22 C23 C24 F1 . . . . 179.79(18) ?
C22 C23 C24 C25 . . . . 0.2(3) ?
C23 C24 C25 C26 . . . . 0.0(3) ?
F1 C24 C25 C26 . . . . -179.62(19) ?
C24 C25 C26 C21 . . . . -0.2(3) ?
C22 C21 C26 C25 . . . . 0.2(3) ?
C2 C21 C26 C25 . . . . 175.16(19) ?
C4A C8A N1 C2 . . . . 9.6(3) ?
C8 C8A N1 C2 . . . . -172.17(17) ?
C21 C2 N1 C8A . . . . -156.30(16) ?
C3 C2 N1 C8A . . . . -34.3(2) ?
O1 C12 N11 C4 . . . . -5.8(3) ?
C13 C12 N11 C4 . . . . 173.15(15) ?
O1 C12 N11 C15 . . . . -178.77(17) ?
C13 C12 N11 C15 . . . . 0.2(2) ?
C4A C4 N11 C12 . . . . 115.73(18) ?
C3 C4 N11 C12 . . . . -119.53(17) ?
C4A C4 N11 C15 . . . . -71.9(2) ?
C3 C4 N11 C15 . . . . 52.8(2) ?
C14 C15 N11 C12 . . . . -12.3(2) ?
C14 C15 N11 C4 . . . . 174.87(16) ?