#------------------------------------------------------------------------------
#$Date: 2024-08-09 04:46:27 +0300 (Fri, 09 Aug 2024) $
#$Revision: 294065 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/25/2312565.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_2312565
loop_
_publ_author_name
'Jaconelli, Harry S.'
'Kennedy, Alan R.'
_publ_section_title
;
Salt forms of amides: protonation of acetanilide.
;
_journal_coeditor_code EF3058
_journal_issue 9
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229624007332
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C8 H10 N1 O1 +, Br-, C8 H9 N1 O1'
_chemical_formula_moiety 'C8 H10 N1 O1 +, Br-, C8 H9 N1 O1'
_chemical_formula_sum 'C16 H19 Br N2 O2'
_chemical_formula_weight 351.24
_chemical_name_systematic
;
N-(1-Hydroxyethylidene)anilinium bromide--N-phenylacetamide
(1/1)
;
_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 mixed
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 104.385(3)
_cell_angle_beta 98.342(2)
_cell_angle_gamma 96.386(2)
_cell_formula_units_Z 3
_cell_length_a 7.8794(2)
_cell_length_b 9.7748(3)
_cell_length_c 16.2720(4)
_cell_measurement_reflns_used 12581
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 71.0150
_cell_measurement_theta_min 4.6690
_cell_volume 1186.86(6)
_computing_cell_refinement
;
Crysalis PRO (Rigaku OD, 2019)
;
_computing_data_collection
;
Crysalis PRO (Rigaku OD, 2019)
;
_computing_data_reduction
;
Crysalis PRO (Rigaku OD, 2019)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
SHELXL2018 in WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type 'Rigaku Synergy-i '
_diffrn_measurement_method 'omega scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_unetI/netI 0.0214
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 8381
_diffrn_reflns_theta_full 70.000
_diffrn_reflns_theta_max 71.496
_diffrn_reflns_theta_min 2.850
_diffrn_source 'microsource tube '
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 3.591
_exptl_absorpt_correction_T_max 0.890
_exptl_absorpt_correction_T_min 0.668
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Rigaku OD, 2023), based on expressions derived by
Clark & Reid (1995)]
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.474
_exptl_crystal_description brick
_exptl_crystal_F_000 540
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.04
_exptl_crystal_size_min 0.04
_refine_diff_density_max 0.728
_refine_diff_density_min -0.895
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.114
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 310
_refine_ls_number_reflns 8381
_refine_ls_number_restraints 5
_refine_ls_restrained_S_all 1.113
_refine_ls_R_factor_all 0.0614
_refine_ls_R_factor_gt 0.0544
_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^)+(0.1085P)^2^+0.3679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1558
_refine_ls_wR_factor_ref 0.1642
_reflns_number_gt 7175
_reflns_number_total 8381
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ef3058.cif
_cod_data_source_block ACTHBr
_cod_database_code 2312565
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 0 -1 3.92705 1.56267 1
0 0 2 32.7503 3.44716 1
0 0 3 4614.69 20.5803 1
0 0 4 567.585 10.0861 1
0 2 3 39.8414 11.3711 -2
0 0 -5 39.8414 11.3711 1
0 0 -6 61800.1 138.748 1
0 0 -7 108.658 14.1414 1
0 0 -8 106.985 42.2731 1
0 -3 -5 82.6988 28.0954 -2
0 0 8 82.6988 28.0954 1
0 0 9 7365.79 105.310 1
0 -4 -6 779.524 30.1403 -2
0 0 10 779.524 30.1403 1
0 0 -11 122.654 13.4880 1
0 0 -12 1807.25 36.8223 1
0 -5 -8 675.669 37.0987 -2
0 0 13 675.669 37.0987 1
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0 6 9 4586.54 106.686 -2
0 0 -15 4586.54 106.686 1
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0 7 11 4472.32 85.5184 -2
0 0 -18 4472.32 85.5184 1
0 8 10 652.394 62.5232 -2
0 1 -19 652.394 62.5232 1
0 1 -18 267.696 19.5617 1
0 1 -17 149.786 17.4501 1
0 1 -16 1160.47 38.8433 1
0 1 -15 3.88509 15.8606 1
0 6 7 675.206 35.3007 -2
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0 -3 -2 1705.62 64.3751 -2
0 -1 6 1705.62 64.3751 1
0 -1 5 167.564 10.6896 1
0 -1 4 25345.0 61.1670 1
0 -1 3 243.207 6.19887 1
0 -1 2 332.680 7.03697 1
0 1 -1 70932.6 157.797 1
0 1 -1 30246.0 81.3142 -2
0 1 -1 30246.0 81.3142 1
0 -1 0 190.518 4.71079 1
0 1 1-3.14871 3.82725 1
0 -1 -2 272.275 6.69603 1
0 1 3 1004.60 11.6622 1
0 1 4 484.706 17.0976 -2
0 -1 -4 484.706 17.0976 1
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0 1 6 12.5587 10.9696 1
0 -1 -7 107.317 39.0581 1
0 -2 -6 205.505 22.6784 -2
0 1 7 205.505 22.6784 1
0 1 8 5407.46 71.5738 1
0 3 7 231.374 24.2970 -2
0 -1 -9 231.374 24.2970 1
0 -1 -10 49.4938 17.4247 1
0 -3 -8 132.561 68.0777 -2
0 1 10 132.561 68.0777 1
0 -1 -11 2865.84 48.6777 1
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0 -1 -12 142.260 26.5694 1
0 1 13 379.804 29.2560 1
0 -1 -15 30.2526 22.5520 1
0 -1 -16 12.6046 19.0702 1
0 6 12 5411.42 101.519 -2
0 -1 -17 5411.42 101.519 1
0 -1 -18 6.79454 13.0352 1
0 2 -19 19.9726 14.2539 1
0 2 -18-13.4676 16.8862 1
0 2 -17 3551.87 67.0730 1
0 2 -16 118.079 20.8299 1
0 7 6 717.779 38.3032 -2
0 2 -15 717.779 38.3032 1
0 -2 14 5828.24 67.4493 1
0 2 -13 531.956 23.7029 1
0 6 4 1318.61 40.7447 -2
0 2 -12 1318.61 40.7447 1
0 2 -11 11924.8 81.9999 1
0 -2 10 147.907 44.8252 1
0 5 3 532.388 56.9399 -2
0 2 -10 532.388 56.9399 1
0 -2 9 845.672 36.1646 1
0 -2 8 25819.3 144.680 1
0 -4 -1 564.450 27.4632 -2
0 -2 7 564.450 27.4632 1
0 -2 6 828.513 21.8766 1
0 2 -5 54831.4 147.819 1
0 -2 4 474.255 12.1523 1
0 2 -3 652.696 14.0879 1
0 2 -2 140317. 334.325 -2
0 2 -2 140317. 334.325 1
0 -2 1 427.056 10.1270 1
0 -2 0 493.297 10.5236 1
0 -2 -1 21351.5 53.3971 1
0 2 2 5.41336 7.59361 1
0 0 5 34.9572 14.1685 -2
0 -2 -3 34.9572 14.1685 1
0 -2 -4 17072.3 65.7373 1
0 2 5 237.532 12.1517 1
0 -2 -6 46.6476 17.1696 1
0 -1 -7 137.194 20.2914 -2
0 2 6 137.194 20.2914 1
0 2 7 10199.2 84.7952 1
0 -2 -8 49.4129 21.8530 -2
0 2 8 49.4129 21.8530 1
0 -2 -9 2.62921 11.7589 1
0 -2 -9 18.2082 60.6150 -2
0 2 9 18.2082 60.6150 1
0 -2 -10 6186.43 72.9852 1
0 -3 -10 283.745 33.7130 -2
0 2 11 283.745 33.7130 1
0 -2 -12 568.952 28.9255 1
0 4 11 14134.3 295.736 -2
0 -2 -13 14134.3 295.736 1
0 -2 -14 370.158 28.5914 1
0 -2 -15 22.2097 18.7793 1
0 5 13 5332.84 125.062 -2
0 -2 -16 5332.84 125.062 1
0 -2 -17 0.14155 14.1681 1
0 3 -19 172.793 21.9384 1
0 3 -18 818.620 39.3825 1
0 3 -17 174.318 29.0712 1
0 8 5 772.095 43.3153 -2
0 3 -16 772.095 43.3153 1
0 3 -15 6203.08 78.9592 1
0 3 -14 444.851 30.0511 1
0 -3 13 638.096 86.6811 1
0 7 3 2079.64 99.3085 -2
0 3 -13 2079.64 99.3085 1
0 3 -12 12348.5 110.433 1
0 -3 11 768.672 56.4431 1
0 3 -10 1119.34 50.7338 1
0 3 -9 7197.02 115.157 1
0 -5 0 1310.82 86.1852 -2
0 -3 8 1310.82 86.1852 1
0 -3 7 2245.44 50.7271 1
0 -3 6 28348.1 126.297 1
0 -3 5 896.449 22.0548 1
0 3 -4 1143.75 19.1028 1
0 3 -3 19853.3 135.417 -2
0 3 -3 19853.3 135.417 1
0 3 -2 592.392 15.7301 1
0 -3 1 355.542 12.5573 1
0 -3 0 24805.7 74.4382 1
0 -3 -1 259.418 11.8976 1
0 1 -6 1545.11 97.9446 -2
0 3 2 1545.11 97.9446 1
0 -3 -3 143.148 12.6302 1
0 -3 -4 3.08106 10.9447 1
0 -3 -5-14.2428 25.2939 1
0 0 -8 90.0278 18.2931 -2
0 3 5 90.0278 18.2931 1
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0 -3 -7 288.356 22.8407 1
0 -3 -8 380.381 18.6666 1
0 -3 -9 2333.45 40.2487 1
0 2 11 230.205 26.7366 -2
0 -3 -10 230.205 26.7366 1
0 -3 -11 360.076 26.2711 1
0 3 12 1259.54 72.3286 -2
0 -3 -12 1259.54 72.3286 1
0 -3 -13 347.918 32.9891 1
0 3 14 19.2719 19.4291 1
0 4 14 15529.1 336.311 -2
0 -3 -15 15529.1 336.311 1
0 3 16 691.515 27.9169 1
0 5 15 72.2325 21.6520 -2
0 -3 -17 72.2325 21.6520 1
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0 4 -17 1623.88 72.8625 1
0 4 -16 7325.11 83.2169 1
0 4 -15 627.752 31.0945 1
0 4 -14 1525.24 59.8458 1
0 8 2 1899.76 98.9804 -2
0 4 -14 1899.76 98.9804 1
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0 -4 12 202.904 33.4740 1
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0 4 -10 3643.75 49.7760 1
0 6 -1 2017.34 113.550 -2
0 4 -9 2017.34 113.550 1
0 -4 8 1223.20 44.4027 1
0 -4 7 46794.4 249.229 1
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0 4 1 453.847 23.3010 1
0 -4 -2 693.536 20.2910 1
0 4 3 646.871 21.2279 1
0 -4 -4 884.913 60.6977 1
0 1 -9 1071.67 37.5717 -2
0 4 4 1071.67 37.5717 1
0 4 5 39064.6 157.965 1
0 0 10 657.273 26.3295 -2
0 -4 -6 657.273 26.3295 1
0 -4 -7 149.123 17.7086 1
0 4 8 2310.65 47.8249 1
0 1 12 156.295 25.0702 -2
0 -4 -9 156.295 25.0702 1
0 4 10 716.185 36.7612 1
0 2 13 15949.5 215.528 -2
0 -4 -11 15949.5 215.528 1
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0 -4 -13 348.735 27.4510 1
0 3 15 13307.7 211.771 -2
0 -4 -14 13307.7 211.771 1
0 -4 -15 1.99957 14.0715 1
0 4 16 30.3283 21.0102 -2
0 -4 -16 30.3283 21.0102 1
0 5 -19 642.243 27.9875 1
0 10 3 519.098 35.3778 -2
0 5 -18 519.098 35.3778 1
0 5 -17 6761.53 86.5504 1
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0 5 -15 655.527 36.7821 1
0 5 -14 412.819 27.1915 1
0 5 -13 2630.56 53.9539 1
0 5 -12 2731.59 56.0116 1
0 5 -11 214.681 21.3429 1
0 -7 2 1294.51 85.3567 -2
0 -5 10 1294.51 85.3567 1
0 5 -9 979.345 25.6301 1
0 -5 8 11689.7 132.403 1
0 5 -7 1090.03 42.6616 1
0 -5 6 1353.81 36.4164 1
0 -5 5 567.144 33.6971 -2
0 -5 5 567.144 33.6971 1
0 -5 4 147.364 19.7951 1
0 -5 3 396.219 23.1796 1
0 5 -2 17186.8 107.109 1
0 -5 1 283.673 19.0611 1
0 3 -8 1143.89 38.2305 -2
0 5 0 1143.89 38.2305 1
0 -5 -1 2282.79 39.6621 1
0 5 2 433.971 22.7562 1
0 -5 -3 722.356 30.6365 1
0 2 -10 788.290 69.1347 -2
0 5 3 788.290 69.1347 1
0 -5 -4 6247.88 56.9269 1
0 -5 -5 559.031 86.8923 1
0 1 -11 563.307 32.3632 -2
0 5 5 563.307 32.3632 1
0 -5 -6 228.350 22.5290 1
0 -5 -7 2986.91 52.2134 1
0 0 -13 839.048 38.7557 -2
0 5 8 839.048 38.7557 1
0 -5 -9 533.105 40.6806 1
0 1 14 7672.68 231.413 -2
0 -5 -10 7672.68 231.413 1
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0 1 15 583.613 85.5624 -2
0 -5 -11 583.613 85.5624 1
0 -5 -12 58.6795 18.1825 1
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0 -5 -14 223.618 18.5093 1
0 3 17 112.565 24.4959 -2
0 -5 -15 112.565 24.4959 1
0 6 -18 3043.02 50.4737 1
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0 6 -15 4467.91 67.8678 1
0 6 -14 45.6568 19.3727 1
0 6 -13 248.528 24.8364 1
0 -6 12 8945.81 100.764 1
0 8 -3 2258.46 89.7166 -2
0 6 -11 2258.46 89.7166 1
0 6 -10 651.842 25.4730 1
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0 6 -8 651.418 23.8264 1
0 -6 7 542.925 28.3010 1
0 6 -6 12219.7 194.482 -2
0 6 -6 12219.7 194.482 1
0 -6 5 321.374 22.8549 1
0 -6 4 456.888 24.8749 1
0 -6 3 917.013 31.9201 1
0 -6 2 477.597 25.3982 1
0 -4 9 2287.31 123.342 -2
0 -6 1 2287.31 123.342 1
0 -6 0 10462.8 77.1502 1
0 6 1 810.815 24.3305 1
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0 -6 -3 8271.80 71.5937 1
0 6 4 539.788 76.5051 1
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0 0 15 4729.48 91.0644 -2
0 -6 -9 4729.48 91.0644 1
0 -6 -10 122.669 36.4775 1
0 0 16 317.918 72.4404 -2
0 -6 -10 317.918 72.4404 1
0 6 11 252.311 26.4606 1
0 1 17 5441.55 104.804 -2
0 -6 -12 5441.55 104.804 1
0 -6 -13 85.4279 14.9406 1
0 7 -18 333.005 23.6038 1
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0 -7 7 4738.00 149.379 1
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0 -7 4 423.259 23.8820 1
0 -7 3 665.441 24.3654 1
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0 7 -2 2049.07 79.8329 1
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0 -7 -3 2179.67 95.7089 1
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0 -7 -11 4348.32 103.121 1
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0 8 -11 505.963 56.4427 1
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0 8 -9 965.704 72.3325 1
0 -8 8 17032.6 285.603 -2
0 -8 8 17032.6 285.603 1
0 -8 7 502.176 29.2960 1
0 8 -6 1030.44 34.1630 1
0 -8 5 213.330 21.8136 1
0 8 -4 544.414 26.2839 1
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0 8 -3 3006.27 110.253 1
0 -8 2 30164.6 148.681 1
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0 -5 13 4261.21 161.870 -2
0 -8 0 4261.21 161.870 1
0 8 1 336.109 35.5154 1
0 8 2 117.397 40.1914 1
0 -8 -3 1046.64 59.5935 1
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0 8 5 717.437 46.1029 1
0 8 6 1191.86 41.4826 1
0 -8 -7 1280.68 48.0875 1
0 8 8 149.276 25.6690 1
0 8 9 87.3868 21.7126 1
0 1 -19 370.666 29.8580 -2
0 8 10 370.666 29.8580 1
0 9 -16 398.040 21.7073 1
0 9 -15 1629.25 31.0060 1
0 11 -6 702.591 33.1125 -2
0 9 -14 702.591 33.1125 1
0 9 -13 498.550 32.3806 1
0 -9 12 1178.06 57.5160 1
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0 9 -9 801.425 66.1896 -2
0 9 -9 801.425 66.1896 1
0 -9 8 635.967 38.6899 1
0 -9 7 1892.23 59.1975 1
0 9 -6 361.168 37.5931 1
0 -9 5 702.371 43.7849 1
0 -7 12 2628.39 103.197 -2
0 -9 4 2628.39 103.197 1
0 -9 3 3215.23 75.0927 1
0 -9 2 1192.17 51.5554 1
0 9 -1 835.670 37.7634 1
0 -9 0 102.468 30.8902 1
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8 -5 6 573.634 20.1350 2
8 -5 8 204.728 29.1910 2
-8 4 10 69.8965 18.1762 2
-8 4 8 541.029 32.5572 2
-8 4 6 129.385 45.2629 2
8 -4 -5 2254.02 70.5202 2
8 -4 -3 280.799 35.6669 2
8 -4 -2 1419.73 82.3669 2
8 -4 0 376.516 37.4807 2
8 -4 2 355.597 29.3401 2
8 -4 3 55.4399 21.4207 2
8 -4 4 1305.31 85.6480 2
8 -4 5 242.174 20.0003 2
8 -4 7 231.320 16.9093 2
8 -4 8 191.607 16.1010 2
-8 3 11 79.5825 19.0901 2
-8 3 9 2545.53 56.1948 2
8 -3 -6 437.833 31.0392 2
8 -3 -4 33.2901 23.1522 2
8 -3 -3 1056.99 72.3498 2
8 -3 -1 81.5183 20.8893 2
8 -3 1 451.370 39.4550 2
8 -3 2 53.4755 28.3098 2
8 -3 4 797.982 36.5860 2
8 -3 6 459.434 29.2710 2
8 -3 7 280.919 23.3173 2
-8 2 12 3.16633 14.0309 2
-8 2 10 2776.57 51.3622 2
8 -2 -7 974.358 69.7841 2
8 -2 -5 455.011 28.0427 2
8 -2 -4 2849.57 110.903 2
8 -2 -2-20.3608 17.6808 2
8 -2 0 260.706 24.7146 2
8 -2 1 267.048 27.9434 2
8 -2 3 161.273 21.5851 2
8 -2 5 502.803 30.1432 2
8 -2 6 73.8931 18.0362 2
8 -2 8 954.573 46.9670 2
-8 1 13 48.1064 19.1372 2
-8 1 11 2612.73 48.3985 2
8 -1 -8 322.402 34.7095 2
8 -1 -6 40.7053 17.4571 2
8 -1 -5 1721.95 64.3112 2
8 -1 -4 207.026 46.8926 2
8 -1 -3 203.690 20.8811 2
8 -1 -1 274.202 23.9406 2
8 -1 0 37.2013 26.5387 2
8 -1 2 198.752 22.5543 2
8 -1 4 737.117 35.1909 2
8 -1 5 138.528 26.0245 2
8 -1 7 406.615 38.8886 2
-8 0 12 930.868 27.8171 2
8 0 -11 89.4486 32.1004 2
-8 0 10 73.8522 22.2807 2
-8 0 9 1111.90 37.6869 2
8 0 -7 26.5200 17.0355 2
8 0 -6 1311.95 58.0205 2
8 0 -5 167.627 42.4894 2
8 0 -4 17.6996 17.2715 2
8 0 -2 25.7149 17.4920 2
8 0 -1-8.20481 25.1963 2
8 0 1 12.4965 24.6193 2
8 0 3 1354.31 54.0357 2
8 0 4 892.350 43.0797 2
8 0 6 4337.94 76.2731 2
8 0 7 210.960 30.7572 2
-8 -1 13 526.456 23.4079 2
8 1 -12 8.52525 17.5442 2
-8 -1 11-11.6547 15.7681 2
-8 -1 10 835.056 34.4416 2
8 1 -8 71.8620 17.8913 2
8 1 -7 316.942 29.4076 2
8 1 -6 18.7943 28.1187 2
8 1 -5 177.127 22.1254 2
8 1 -3 35.6089 20.5007 2
8 1 -2 39.2698 24.4985 2
8 1 0 278.951 47.8874 2
8 1 2 754.523 43.1654 2
8 1 3 480.883 35.9414 2
8 1 5 1631.63 50.4215 2
8 1 6 91.4392 26.5026 2
8 2 -13 35.2507 14.3249 2
-8 -2 12 61.4232 17.5837 2
-8 -2 11 789.919 34.5871 2
8 2 -9 25.5835 21.2154 2
8 2 -8 360.155 27.8979 2
8 2 -7 60.6856 20.2426 2
8 2 -6-5.07206 18.5003 2
8 2 -4 219.521 20.1265 2
8 2 -3 30.8521 17.2964 2
8 2 -1 18.4772 16.8206 2
8 2 1 3116.61 77.9161 2
8 2 2 22.8580 21.9408 2
8 2 4 6205.12 90.3315 2
8 2 5 22.9915 23.1437 2
-8 -3 12 317.144 22.5730 2
8 3 -10 39.2062 19.1981 2
8 3 -9 684.214 31.0821 2
8 3 -8 13.7291 16.6310 2
8 3 -7-7.40215 14.2624 2
8 3 -5-7.73311 14.6901 2
8 3 -4-8.71903 14.3484 2
8 3 -2 191.146 22.7919 2
8 3 0 2426.68 70.8229 2
8 3 1-0.95275 20.3948 2
8 3 3 2148.34 55.2675 2
8 4 -11 82.0879 26.9854 2
8 4 -10 714.408 52.4015 2
8 4 -9-10.5269 13.8510 2
8 4 -8 24.0138 15.0254 2
8 4 -6 50.3695 17.4719 2
8 4 -5-1.06732 15.2869 2
8 4 -3 10.0630 14.5383 2
8 4 -1 2489.82 96.0565 2
8 4 0 143.052 32.5568 2
8 4 2 1427.31 66.0594 2
8 5 -9 200.616 20.3308 2
8 5 -7 18.7096 12.4443 2
8 5 -6 328.534 20.2709 2
8 5 -5 429.427 23.8509 2
8 5 -4 43.1084 16.0658 2
8 5 -2 2028.31 75.3827 2
8 5 -1 63.1696 23.0985 2
9 -5 -4 327.915 35.9645 2
9 -5 -2 26.9800 11.4817 2
9 -5 -1 291.213 26.7683 2
9 -5 1-12.3794 13.7893 2
9 -5 2-25.4578 21.1283 2
9 -4 -5 91.3808 19.9218 2
9 -4 -3 93.5401 36.2085 2
9 -4 -2 322.967 22.6355 2
9 -4 0 99.6856 15.0826 2
9 -4 1 164.023 39.4540 2
9 -4 2 145.935 14.4842 2
9 -4 3 361.567 19.0397 2
-9 3 8 51.9560 17.5090 2
9 -3 -6 1085.82 56.5452 2
9 -3 -3 58.9124 28.0378 2
9 -3 -1 160.136 17.7687 2
9 -3 0 743.949 63.2884 2
9 -3 1-9.45156 19.1635 2
9 -3 2 27.4414 12.9682 2
9 -3 4 187.541 20.9715 2
-9 2 9 13.0746 16.6224 2
-9 2 7 528.371 33.5714 2
9 -2 -5 83.6526 33.3464 2
9 -2 -4 323.598 41.4934 2
9 -2 -2 124.254 17.3069 2
9 -2 -1 855.837 66.8153 2
9 -2 0 261.351 43.1444 2
9 -2 1 3.80754 20.1324 2
9 -2 3 77.2140 20.1881 2
-9 1 8 1379.07 50.1723 2
9 -1 -6 42.3917 16.0511 2
9 -1 -5 207.903 25.3192 2
9 -1 -3 28.0763 15.5851 2
9 -1 -2 3243.91 102.214 2
9 -1 -1 66.0969 28.7796 2
9 -1 0 424.010 43.1031 2
9 -1 2 29.8112 23.8493 2
9 -1 3 51.1846 22.9237 2
9 -1 4 1855.36 61.0417 2
-9 0 9 550.946 26.7307 2
9 0 -8 48.6874 24.5910 2
9 0 -7-13.4460 13.7387 2
9 0 -6 1564.99 49.4414 2
9 0 -4 8.68295 15.1441 2
9 0 -3 439.876 46.2903 2
9 0 -2 462.216 45.3071 2
9 0 -1 24.5354 17.7577 2
9 0 1 13.7660 24.3053 2
9 0 2 31.1370 22.2291 2
9 0 3 745.238 45.4183 2
9 1 -9-18.7466 20.0066 2
9 1 -8-5.44253 14.3512 2
9 1 -7 1034.17 57.8054 2
9 1 -5 1.36358 17.1666 2
9 1 -4 1311.39 67.8291 2
9 1 -3 81.3555 28.8143 2
9 1 -2 127.184 21.1343 2
9 1 0 20.1525 23.2791 2
9 1 1 26.4555 23.4696 2
9 1 2 342.396 35.4755 2
9 2 -8 1018.26 51.1808 2
9 2 -6 4.56033 14.7604 2
9 2 -5 453.418 40.9520 2
9 2 -4 46.1917 16.7890 2
9 2 -3 6.19738 15.3600 2
9 2 -1 334.242 33.8907 2
9 2 0 36.1812 20.2511 2
0 0 0 0.00000 0.00000 0
TITL ACT_HBr_Big_TWINXXXXXXXX_twin1_hklf4 in P-1
REM P-1 (#2 in standard setting)
CELL 1.54184 7.883914 9.770463 16.262192 104.3747 98.3537 96.3926
ZERR 3.00 0.000177 0.000303 0.000423 0.0025 0.0020 0.0022
LATT 1
SFAC C H N O Br
UNIT 48.00 48.00 6.00 12.00 3.00
REM CrysAlisPro recorded range (K): Min=99.4; max=100.4; aver:99.9
TEMP -173
SIZE 0.04 0.04 0.18
TREF
HKLF 5
BASF 0.40606
END
;
_shelx_hkl_checksum 50750
_shelx_res_file
;
TITL shelxt_a.res in P-1
shelx.res
created by SHELXL-2018/3 at 11:09:33 on 01-May-2024
CELL 1.54184 7.8794 9.7748 16.2720 104.385 98.342 96.386
ZERR 3.00 0.0002 0.0003 0.0004 0.003 0.002 0.002
LATT 1
SFAC BR O N C H
UNIT 3 6 6 48 57
MERG 0
OMIT -3.00 180.00
OMIT 0 1 -1
dfix .88 .01 n1 h1n n2 h2n n3 h3n o1 h1h o3 h2h
HTAB N1 Br1
HTAB N2 Br2
HTAB N3 Br1
HTAB O1 O2
EQIV $1 -x-1, -y, -z
HTAB O3 O3_$1
FMAP 2
PLAN 20
ACTA 140.00
BOND $H
CONF
LIST 4
L.S. 10
TEMP -173.00
WGHT 0.108500 0.367900
BASF 0.39965
FVAR 2.36159
BR1 1 -0.006020 0.349654 0.331703 11.00000 0.02683 0.03423 =
0.02112 0.00647 -0.00316 0.00078
BR2 1 1.000000 1.000000 1.000000 10.50000 0.02680 0.04410 =
0.02067 0.00833 -0.00270 0.00076
O1 2 0.423537 0.526786 0.632949 11.00000 0.02678 0.02330 =
0.02327 0.00506 -0.00443 -0.00179
O2 2 0.566468 0.773375 0.701662 11.00000 0.02792 0.02371 =
0.02474 0.00400 -0.00428 -0.00172
O3 2 -0.438707 0.124513 0.033330 11.00000 0.02746 0.02260 =
0.02664 0.00519 -0.00629 -0.00147
N1 3 0.233750 0.390463 0.517227 11.00000 0.02510 0.02450 =
0.01796 0.00503 -0.00295 -0.00103
N2 3 0.747238 0.942572 0.809405 11.00000 0.02273 0.02369 =
0.01804 0.00526 -0.00309 -0.00119
N3 3 -0.264979 0.282436 0.146575 11.00000 0.02656 0.02343 =
0.01899 0.00559 -0.00404 -0.00168
C1 4 0.218203 0.262525 0.545609 11.00000 0.02251 0.02461 =
0.02408 0.00652 -0.00645 -0.00250
C2 4 0.158081 0.262190 0.621889 11.00000 0.02611 0.02615 =
0.02431 0.00388 0.00121 0.00371
AFIX 43
H2 5 0.131148 0.347421 0.656919 11.00000 -1.20000
AFIX 0
C3 4 0.138006 0.135630 0.646085 11.00000 0.02735 0.02951 =
0.02688 0.00716 0.00217 0.00087
AFIX 43
H3 5 0.098346 0.134591 0.698376 11.00000 -1.20000
AFIX 0
C4 4 0.175459 0.010326 0.594426 11.00000 0.02518 0.02730 =
0.03385 0.01025 -0.00135 0.00044
AFIX 43
H4 5 0.161757 -0.075893 0.611414 11.00000 -1.20000
AFIX 0
C5 4 0.233079 0.011908 0.517767 11.00000 0.02616 0.02458 =
0.03287 0.00469 -0.00100 0.00188
AFIX 43
H5 5 0.258480 -0.073577 0.482297 11.00000 -1.20000
AFIX 0
C6 4 0.253810 0.138663 0.492640 11.00000 0.02381 0.02498 =
0.02571 0.00588 -0.00140 0.00009
AFIX 43
H6 5 0.291790 0.139731 0.439966 11.00000 -1.20000
AFIX 0
C7 4 0.325317 0.514016 0.560646 11.00000 0.02021 0.02635 =
0.02284 0.00697 0.00000 0.00256
C8 4 0.316317 0.636640 0.521729 11.00000 0.02826 0.02341 =
0.02506 0.00631 0.00034 -0.00042
AFIX 137
H8A 5 0.267078 0.711502 0.558722 11.00000 -1.50000
H8B 5 0.242638 0.603984 0.464497 11.00000 -1.50000
H8C 5 0.433324 0.674983 0.516404 11.00000 -1.50000
AFIX 0
C9 4 0.738554 1.065322 0.777674 11.00000 0.02233 0.02366 =
0.02048 0.00454 0.00177 0.00193
C10 4 0.614868 1.072361 0.708732 11.00000 0.02660 0.02577 =
0.02506 0.00628 -0.00137 0.00033
AFIX 43
H10 5 0.528277 0.992407 0.679939 11.00000 -1.20000
AFIX 0
C11 4 0.619758 1.197595 0.682666 11.00000 0.03060 0.02731 =
0.02859 0.00739 0.00107 0.00503
AFIX 43
H11 5 0.534882 1.203047 0.636223 11.00000 -1.20000
AFIX 0
C12 4 0.746437 1.314660 0.723320 11.00000 0.03292 0.02504 =
0.02967 0.00853 0.00682 0.00374
AFIX 43
H12 5 0.750615 1.398643 0.703798 11.00000 -1.20000
AFIX 0
C13 4 0.867762 1.307918 0.793206 11.00000 0.02555 0.02463 =
0.03390 0.00158 0.00344 -0.00079
AFIX 43
H13 5 0.953099 1.388521 0.822479 11.00000 -1.20000
AFIX 0
C14 4 0.863957 1.184412 0.819838 11.00000 0.02350 0.02613 =
0.02483 0.00286 0.00015 0.00093
AFIX 43
H14 5 0.947293 1.180257 0.867250 11.00000 -1.20000
AFIX 0
C15 4 0.670881 0.807944 0.773056 11.00000 0.02123 0.02613 =
0.02173 0.00568 0.00036 0.00213
C16 4 0.711428 0.701597 0.821918 11.00000 0.02779 0.02591 =
0.02344 0.00627 0.00007 0.00084
AFIX 137
H16A 5 0.603436 0.654437 0.832463 11.00000 -1.50000
H16B 5 0.787250 0.750527 0.877147 11.00000 -1.50000
H16C 5 0.770231 0.629968 0.788241 11.00000 -1.50000
AFIX 0
C17 4 -0.277576 0.403625 0.112241 11.00000 0.01864 0.02293 =
0.02344 0.00550 -0.00489 -0.00259
C18 4 -0.232256 0.401170 0.032612 11.00000 0.02923 0.02638 =
0.02694 0.00680 0.00124 0.00051
AFIX 43
H18 5 -0.194259 0.319168 -0.000052 11.00000 -1.20000
AFIX 0
C19 4 -0.243369 0.520593 0.001463 11.00000 0.03205 0.02936 =
0.02933 0.00963 0.00379 -0.00095
AFIX 43
H19 5 -0.212383 0.520087 -0.052886 11.00000 -1.20000
AFIX 0
C20 4 -0.298991 0.640190 0.048614 11.00000 0.03300 0.02476 =
0.02934 0.00872 -0.00494 -0.00182
AFIX 43
H20 5 -0.307166 0.721000 0.026550 11.00000 -1.20000
AFIX 0
C21 4 -0.342809 0.641395 0.128403 11.00000 0.02946 0.02469 =
0.03283 0.00559 -0.00071 0.00070
AFIX 43
H21 5 -0.381078 0.723343 0.160965 11.00000 -1.20000
AFIX 0
C22 4 -0.330952 0.523085 0.160958 11.00000 0.02729 0.02616 =
0.02420 0.00628 -0.00029 -0.00150
AFIX 43
H22 5 -0.359168 0.524403 0.215935 11.00000 -1.20000
AFIX 0
C23 4 -0.340428 0.151201 0.106620 11.00000 0.02362 0.02429 =
0.02269 0.00471 0.00139 0.00267
C24 4 -0.309711 0.036328 0.150425 11.00000 0.02772 0.02175 =
0.02472 0.00656 0.00029 0.00103
AFIX 137
H24A 5 -0.421197 -0.019420 0.150223 11.00000 -1.50000
H24B 5 -0.250319 0.079760 0.210067 11.00000 -1.50000
H24C 5 -0.237484 -0.026649 0.119696 11.00000 -1.50000
AFIX 0
H1N 5 0.171959 0.382751 0.466252 11.00000 0.01984
H2N 5 0.817655 0.961745 0.859059 11.00000 0.02741
H3N 5 -0.202128 0.301130 0.198141 11.00000 0.02919
H1H 5 0.483008 0.612909 0.659279 11.00000 0.07094
PART -1
H2H 5 -0.486091 0.036538 0.005361 10.50000 0.05694
HKLF 5
REM shelxt_a.res in P-1
REM wR2 = 0.1642, GooF = S = 1.114, Restrained GooF = 1.113 for all data
REM R1 = 0.0544 for 7175 Fo > 4sig(Fo) and 0.0614 for all 8381 data
REM 310 parameters refined using 5 restraints
END
WGHT 0.1086 0.3684
REM Highest difference peak 0.728, deepest hole -0.895, 1-sigma level 0.094
Q1 1 -0.1026 0.3684 0.3816 11.00000 0.05 0.73
Q2 1 1.0839 0.9637 0.9457 11.00000 0.05 0.63
Q3 1 0.1129 0.2676 0.2800 11.00000 0.05 0.52
Q4 1 1.1138 0.9928 0.9553 11.00000 0.05 0.52
Q5 1 -0.1395 0.4176 0.3245 11.00000 0.05 0.45
Q6 1 -0.1015 0.2326 0.2764 11.00000 0.05 0.42
Q7 1 -0.0783 0.4183 0.2828 11.00000 0.05 0.40
Q8 1 0.1010 0.4660 0.3832 11.00000 0.05 0.38
Q9 1 0.1484 0.3021 0.3366 11.00000 0.05 0.38
Q10 1 0.1184 0.2735 0.3546 11.00000 0.05 0.38
Q11 1 0.2144 0.5973 0.5647 11.00000 0.05 0.35
Q12 1 1.1308 0.9159 1.0083 11.00000 0.05 0.35
Q13 1 0.1108 0.3681 0.3942 11.00000 0.05 0.34
Q14 1 -0.0599 0.4528 0.3800 11.00000 0.05 0.34
Q15 1 -0.1807 -0.0405 0.0741 11.00000 0.05 0.34
Q16 1 0.0677 0.3498 0.2801 11.00000 0.05 0.33
Q17 1 1.0630 0.9323 1.0605 11.00000 0.05 0.33
Q18 1 1.1074 1.1112 1.0438 11.00000 0.05 0.31
Q19 1 0.8318 0.6684 0.7520 11.00000 0.05 0.31
Q20 1 0.6535 0.7398 0.8757 11.00000 0.05 0.31
;
_shelx_res_checksum 18072
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
Br Br1 -0.00602(5) 0.34965(4) 0.33170(2) 0.02865(17) Uani d 1 . .
Br Br2 1.000000 1.000000 1.000000 0.03169(19) Uani d 1 . .
O O1 0.4235(4) 0.5268(3) 0.63295(18) 0.0260(6) Uani d 1 . .
O O2 0.5665(4) 0.7734(3) 0.70166(18) 0.0273(6) Uani d 1 . .
O O3 -0.4387(4) 0.1245(3) 0.03333(19) 0.0274(6) Uani d 1 . .
N N1 0.2337(4) 0.3905(3) 0.5172(2) 0.0237(7) Uani d 1 . .
N N2 0.7472(4) 0.9426(3) 0.8094(2) 0.0226(6) Uani d 1 . .
N N3 -0.2650(4) 0.2824(3) 0.1466(2) 0.0243(7) Uani d 1 . .
C C1 0.2182(5) 0.2625(4) 0.5456(2) 0.0253(8) Uani d 1 . .
C C2 0.1581(5) 0.2622(4) 0.6219(2) 0.0264(8) Uani d 1 . .
H H2 0.131148 0.347421 0.656919 0.032 Uiso calc 1 . .
C C3 0.1380(5) 0.1356(4) 0.6461(2) 0.0285(8) Uani d 1 . .
H H3 0.098346 0.134591 0.698376 0.034 Uiso calc 1 . .
C C4 0.1755(5) 0.0103(4) 0.5944(3) 0.0294(8) Uani d 1 . .
H H4 0.161757 -0.075893 0.611414 0.035 Uiso calc 1 . .
C C5 0.2331(5) 0.0119(4) 0.5178(3) 0.0292(8) Uani d 1 . .
H H5 0.258480 -0.073577 0.482297 0.035 Uiso calc 1 . .
C C6 0.2538(5) 0.1387(4) 0.4926(2) 0.0259(8) Uani d 1 . .
H H6 0.291790 0.139731 0.439966 0.031 Uiso calc 1 . .
C C7 0.3253(5) 0.5140(4) 0.5606(3) 0.0236(8) Uani d 1 . .
C C8 0.3163(5) 0.6366(4) 0.5217(3) 0.0264(8) Uani d 1 . .
H H8A 0.267078 0.711502 0.558722 0.040 Uiso calc 1 . .
H H8B 0.242638 0.603984 0.464497 0.040 Uiso calc 1 . .
H H8C 0.433324 0.674983 0.516404 0.040 Uiso calc 1 . .
C C9 0.7386(5) 1.0653(4) 0.7777(2) 0.0228(7) Uani d 1 . .
C C10 0.6149(5) 1.0724(4) 0.7087(2) 0.0268(8) Uani d 1 . .
H H10 0.528277 0.992407 0.679939 0.032 Uiso calc 1 . .
C C11 0.6198(5) 1.1976(4) 0.6827(2) 0.0293(8) Uani d 1 . .
H H11 0.534882 1.203047 0.636223 0.035 Uiso calc 1 . .
C C12 0.7464(5) 1.3147(4) 0.7233(3) 0.0289(8) Uani d 1 . .
H H12 0.750615 1.398643 0.703798 0.035 Uiso calc 1 . .
C C13 0.8678(5) 1.3079(4) 0.7932(3) 0.0297(8) Uani d 1 . .
H H13 0.953099 1.388521 0.822479 0.036 Uiso calc 1 . .
C C14 0.8640(5) 1.1844(4) 0.8198(2) 0.0262(8) Uani d 1 . .
H H14 0.947293 1.180257 0.867250 0.031 Uiso calc 1 . .
C C15 0.6709(5) 0.8079(4) 0.7731(3) 0.0237(8) Uani d 1 . .
C C16 0.7114(5) 0.7016(4) 0.8219(3) 0.0265(8) Uani d 1 . .
H H16A 0.603436 0.654437 0.832463 0.040 Uiso calc 1 . .
H H16B 0.787250 0.750527 0.877147 0.040 Uiso calc 1 . .
H H16C 0.770231 0.629968 0.788241 0.040 Uiso calc 1 . .
C C17 -0.2776(5) 0.4036(4) 0.1122(2) 0.0232(8) Uani d 1 . .
C C18 -0.2323(5) 0.4012(4) 0.0326(2) 0.0283(8) Uani d 1 . .
H H18 -0.194259 0.319168 -0.000052 0.034 Uiso calc 1 . .
C C19 -0.2434(5) 0.5206(4) 0.0015(3) 0.0306(8) Uani d 1 . .
H H19 -0.212383 0.520087 -0.052886 0.037 Uiso calc 1 . .
C C20 -0.2990(5) 0.6402(4) 0.0486(3) 0.0304(8) Uani d 1 . .
H H20 -0.307166 0.721000 0.026550 0.036 Uiso calc 1 . .
C C21 -0.3428(5) 0.6414(4) 0.1284(3) 0.0303(8) Uani d 1 . .
H H21 -0.381078 0.723343 0.160965 0.036 Uiso calc 1 . .
C C22 -0.3310(5) 0.5231(4) 0.1610(2) 0.0269(8) Uani d 1 . .
H H22 -0.359168 0.524403 0.215935 0.032 Uiso calc 1 . .
C C23 -0.3404(5) 0.1512(4) 0.1066(3) 0.0242(8) Uani d 1 . .
C C24 -0.3097(5) 0.0363(4) 0.1504(3) 0.0254(8) Uani d 1 . .
H H24A -0.421197 -0.019420 0.150223 0.038 Uiso calc 1 . .
H H24B -0.250319 0.079760 0.210067 0.038 Uiso calc 1 . .
H H24C -0.237484 -0.026649 0.119696 0.038 Uiso calc 1 . .
H H1N 0.172(5) 0.383(4) 0.4663(14) 0.020(10) Uiso d 1 . .
H H2N 0.818(5) 0.962(5) 0.8591(16) 0.027(12) Uiso d 1 . .
H H3N -0.202(5) 0.301(5) 0.1981(15) 0.029(12) Uiso d 1 . .
H H1H 0.483(7) 0.613(3) 0.659(3) 0.07(2) Uiso d 1 . .
H H2H -0.486(19) 0.037(6) 0.005(9) 0.06(3) Uiso d 0.5 A -1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Br1 0.0268(3) 0.0342(3) 0.0211(3) 0.00078(17) -0.00316(17) 0.00647(17)
Br2 0.0268(3) 0.0441(4) 0.0207(3) 0.0008(2) -0.0027(2) 0.0083(2)
O1 0.0268(14) 0.0233(13) 0.0233(14) -0.0018(10) -0.0044(11) 0.0051(10)
O2 0.0279(14) 0.0237(13) 0.0247(15) -0.0017(10) -0.0043(11) 0.0040(11)
O3 0.0275(14) 0.0226(13) 0.0266(15) -0.0015(11) -0.0063(12) 0.0052(11)
N1 0.0251(16) 0.0245(15) 0.0180(16) -0.0010(12) -0.0030(13) 0.0050(12)
N2 0.0227(16) 0.0237(15) 0.0180(16) -0.0012(12) -0.0031(12) 0.0053(12)
N3 0.0266(16) 0.0234(15) 0.0190(16) -0.0017(12) -0.0040(13) 0.0056(13)
C1 0.0225(18) 0.0246(18) 0.0241(19) -0.0025(14) -0.0064(15) 0.0065(15)
C2 0.0261(18) 0.0262(18) 0.0243(19) 0.0037(14) 0.0012(15) 0.0039(14)
C3 0.0273(19) 0.0295(19) 0.027(2) 0.0009(15) 0.0022(15) 0.0072(15)
C4 0.0252(19) 0.0273(18) 0.034(2) 0.0004(14) -0.0014(16) 0.0103(16)
C5 0.0262(19) 0.0246(18) 0.033(2) 0.0019(14) -0.0010(16) 0.0047(15)
C6 0.0238(18) 0.0250(18) 0.0257(19) 0.0001(14) -0.0014(15) 0.0059(14)
C7 0.0202(18) 0.0264(18) 0.0228(19) 0.0026(14) 0.0000(15) 0.0070(15)
C8 0.028(2) 0.0234(18) 0.025(2) -0.0004(14) 0.0003(16) 0.0063(15)
C9 0.0223(17) 0.0237(17) 0.0205(19) 0.0019(14) 0.0018(14) 0.0045(14)
C10 0.0266(18) 0.0258(18) 0.0251(19) 0.0003(14) -0.0014(15) 0.0063(14)
C11 0.031(2) 0.0273(19) 0.029(2) 0.0050(15) 0.0011(16) 0.0074(15)
C12 0.033(2) 0.0250(18) 0.030(2) 0.0037(15) 0.0068(16) 0.0085(15)
C13 0.0256(19) 0.0246(18) 0.034(2) -0.0008(14) 0.0034(16) 0.0016(15)
C14 0.0235(18) 0.0261(18) 0.0248(19) 0.0009(14) 0.0001(14) 0.0029(14)
C15 0.0212(18) 0.0261(18) 0.0217(19) 0.0021(14) 0.0004(15) 0.0057(15)
C16 0.0278(19) 0.0259(18) 0.023(2) 0.0008(15) 0.0001(15) 0.0063(15)
C17 0.0186(17) 0.0229(17) 0.0234(19) -0.0026(13) -0.0049(14) 0.0055(14)
C18 0.029(2) 0.0264(18) 0.027(2) 0.0005(15) 0.0012(15) 0.0068(15)
C19 0.032(2) 0.0294(19) 0.029(2) -0.0009(15) 0.0038(16) 0.0096(15)
C20 0.033(2) 0.0248(18) 0.029(2) -0.0018(15) -0.0049(16) 0.0087(15)
C21 0.029(2) 0.0247(18) 0.033(2) 0.0007(15) -0.0007(16) 0.0056(15)
C22 0.0273(19) 0.0262(18) 0.0242(19) -0.0015(14) -0.0003(15) 0.0063(14)
C23 0.0236(19) 0.0243(18) 0.023(2) 0.0027(14) 0.0014(15) 0.0047(15)
C24 0.0277(19) 0.0217(17) 0.025(2) 0.0010(14) 0.0003(16) 0.0066(15)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.6763 1.2805 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
C7 O1 H1H . . 116(4) ?
C23 O3 H2H . . 121(10) ?
C7 N1 C1 . . 126.2(3) ?
C7 N1 H1N . . 119(3) ?
C1 N1 H1N . . 115(3) ?
C15 N2 C9 . . 129.4(3) ?
C15 N2 H2N . . 118(3) ?
C9 N2 H2N . . 112(3) ?
C23 N3 C17 . . 124.8(3) ?
C23 N3 H3N . . 120(3) ?
C17 N3 H3N . . 115(3) ?
C6 C1 C2 . . 121.3(3) ?
C6 C1 N1 . . 118.3(3) ?
C2 C1 N1 . . 120.3(3) ?
C3 C2 C1 . . 119.1(3) ?
C3 C2 H2 . . 120.4 ?
C1 C2 H2 . . 120.4 ?
C2 C3 C4 . . 120.6(4) ?
C2 C3 H3 . . 119.7 ?
C4 C3 H3 . . 119.7 ?
C5 C4 C3 . . 119.7(4) ?
C5 C4 H4 . . 120.2 ?
C3 C4 H4 . . 120.2 ?
C4 C5 C6 . . 120.3(4) ?
C4 C5 H5 . . 119.8 ?
C6 C5 H5 . . 119.8 ?
C1 C6 C5 . . 119.0(4) ?
C1 C6 H6 . . 120.5 ?
C5 C6 H6 . . 120.5 ?
O1 C7 N1 . . 120.4(3) ?
O1 C7 C8 . . 121.6(3) ?
N1 C7 C8 . . 118.0(3) ?
C7 C8 H8A . . 109.5 ?
C7 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C7 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
C10 C9 C14 . . 119.6(3) ?
C10 C9 N2 . . 124.2(3) ?
C14 C9 N2 . . 116.2(3) ?
C11 C10 C9 . . 119.3(3) ?
C11 C10 H10 . . 120.4 ?
C9 C10 H10 . . 120.4 ?
C12 C11 C10 . . 121.1(4) ?
C12 C11 H11 . . 119.5 ?
C10 C11 H11 . . 119.5 ?
C11 C12 C13 . . 119.3(3) ?
C11 C12 H12 . . 120.3 ?
C13 C12 H12 . . 120.3 ?
C14 C13 C12 . . 120.1(3) ?
C14 C13 H13 . . 120.0 ?
C12 C13 H13 . . 120.0 ?
C13 C14 C9 . . 120.6(3) ?
C13 C14 H14 . . 119.7 ?
C9 C14 H14 . . 119.7 ?
O2 C15 N2 . . 121.5(3) ?
O2 C15 C16 . . 122.0(3) ?
N2 C15 C16 . . 116.5(3) ?
C15 C16 H16A . . 109.5 ?
C15 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
C15 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
C22 C17 C18 . . 121.1(3) ?
C22 C17 N3 . . 118.8(3) ?
C18 C17 N3 . . 120.1(3) ?
C17 C18 C19 . . 118.9(4) ?
C17 C18 H18 . . 120.5 ?
C19 C18 H18 . . 120.5 ?
C20 C19 C18 . . 120.8(4) ?
C20 C19 H19 . . 119.6 ?
C18 C19 H19 . . 119.6 ?
C19 C20 C21 . . 119.6(4) ?
C19 C20 H20 . . 120.2 ?
C21 C20 H20 . . 120.2 ?
C20 C21 C22 . . 120.4(4) ?
C20 C21 H21 . . 119.8 ?
C22 C21 H21 . . 119.8 ?
C17 C22 C21 . . 119.2(4) ?
C17 C22 H22 . . 120.4 ?
C21 C22 H22 . . 120.4 ?
O3 C23 N3 . . 120.3(3) ?
O3 C23 C24 . . 121.6(3) ?
N3 C23 C24 . . 118.0(3) ?
C23 C24 H24A . . 109.5 ?
C23 C24 H24B . . 109.5 ?
H24A C24 H24B . . 109.5 ?
C23 C24 H24C . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C7 . 1.281(5) ?
O1 H1H . 0.887(14) ?
O2 C15 . 1.267(5) ?
O3 C23 . 1.274(5) ?
O3 H2H . 0.878(14) ?
N1 C7 . 1.309(5) ?
N1 C1 . 1.436(5) ?
N1 H1N . 0.880(13) ?
N2 C15 . 1.333(5) ?
N2 C9 . 1.424(4) ?
N2 H2N . 0.876(14) ?
N3 C23 . 1.314(5) ?
N3 C17 . 1.437(4) ?
N3 H3N . 0.875(13) ?
C1 C6 . 1.384(5) ?
C1 C2 . 1.392(5) ?
C2 C3 . 1.388(5) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.391(5) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.391(6) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.398(5) ?
C5 H5 . 0.9500 ?
C6 H6 . 0.9500 ?
C7 C8 . 1.492(5) ?
C8 H8A . 0.9800 ?
C8 H8B . 0.9800 ?
C8 H8C . 0.9800 ?
C9 C10 . 1.396(5) ?
C9 C14 . 1.397(5) ?
C10 C11 . 1.390(5) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.386(5) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.395(6) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.379(5) ?
C13 H13 . 0.9500 ?
C14 H14 . 0.9500 ?
C15 C16 . 1.492(5) ?
C16 H16A . 0.9800 ?
C16 H16B . 0.9800 ?
C16 H16C . 0.9800 ?
C17 C22 . 1.384(5) ?
C17 C18 . 1.388(5) ?
C18 C19 . 1.390(5) ?
C18 H18 . 0.9500 ?
C19 C20 . 1.383(6) ?
C19 H19 . 0.9500 ?
C20 C21 . 1.389(6) ?
C20 H20 . 0.9500 ?
C21 C22 . 1.393(5) ?
C21 H21 . 0.9500 ?
C22 H22 . 0.9500 ?
C23 C24 . 1.495(5) ?
C24 H24A . 0.9800 ?
C24 H24B . 0.9800 ?
C24 H24C . 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1N Br1 . 0.880(13) 2.350(14) 3.228(3) 176(4) yes
N2 H2N Br2 . 0.876(14) 2.442(14) 3.316(3) 176(4) yes
N3 H3N Br1 . 0.875(13) 2.385(15) 3.256(3) 174(4) yes
O1 H1H O2 . 0.887(14) 1.572(17) 2.454(4) 172(6) yes
O3 H2H O3 2_455 0.878(14) 1.55(2) 2.428(5) 173(16) 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
C7 N1 C1 C6 . . . . -126.7(4) ?
C7 N1 C1 C2 . . . . 57.3(5) ?
C6 C1 C2 C3 . . . . 1.7(6) ?
N1 C1 C2 C3 . . . . 177.5(3) ?
C1 C2 C3 C4 . . . . -0.7(6) ?
C2 C3 C4 C5 . . . . -0.2(6) ?
C3 C4 C5 C6 . . . . 0.2(6) ?
C2 C1 C6 C5 . . . . -1.7(5) ?
N1 C1 C6 C5 . . . . -177.6(3) ?
C4 C5 C6 C1 . . . . 0.8(5) ?
C1 N1 C7 O1 . . . . 5.7(6) ?
C1 N1 C7 C8 . . . . -176.5(4) ?
C15 N2 C9 C10 . . . . 15.0(6) ?
C15 N2 C9 C14 . . . . -165.0(4) ?
C14 C9 C10 C11 . . . . 0.6(6) ?
N2 C9 C10 C11 . . . . -179.4(3) ?
C9 C10 C11 C12 . . . . 0.8(6) ?
C10 C11 C12 C13 . . . . -1.9(6) ?
C11 C12 C13 C14 . . . . 1.7(6) ?
C12 C13 C14 C9 . . . . -0.4(6) ?
C10 C9 C14 C13 . . . . -0.8(6) ?
N2 C9 C14 C13 . . . . 179.2(3) ?
C9 N2 C15 O2 . . . . -3.7(6) ?
C9 N2 C15 C16 . . . . 177.8(4) ?
C23 N3 C17 C22 . . . . 126.4(4) ?
C23 N3 C17 C18 . . . . -55.3(5) ?
C22 C17 C18 C19 . . . . -0.9(6) ?
N3 C17 C18 C19 . . . . -179.1(3) ?
C17 C18 C19 C20 . . . . -0.2(6) ?
C18 C19 C20 C21 . . . . 0.6(6) ?
C19 C20 C21 C22 . . . . 0.0(6) ?
C18 C17 C22 C21 . . . . 1.4(6) ?
N3 C17 C22 C21 . . . . 179.7(3) ?
C20 C21 C22 C17 . . . . -1.0(6) ?
C17 N3 C23 O3 . . . . -2.9(6) ?
C17 N3 C23 C24 . . . . 178.2(3) ?