#------------------------------------------------------------------------------
#$Date: 2024-11-09 03:46:40 +0100 (Sat, 09 Nov 2024) $
#$Revision: 295853 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/33/2023313.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_2023313
loop_
_publ_author_name
'Mahadevaiah, Harish Kumar'
'Shivanna, Harishkumar'
'Hanumaiah, Anil Kumar'
'Hirehalli Chikkegowda, Devarajegowda'
'Bandrehalli Siddagangaiah, Palakshamurthy'
_publ_section_title
;
Crystal structure, Hirshfeld surface analysis, DFT and molecular docking
studies of ethyl 5-amino-2-bromoisonicotinate
;
_journal_coeditor_code OI2013
_journal_issue 12
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024010594
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C8 H9 Br N2 O2'
_chemical_formula_moiety 'C8 H9 Br N2 O2'
_chemical_formula_sum 'C8 H9 Br N2 O2'
_chemical_formula_weight 245.08
_chemical_name_common
;
Ethyl 5-amino-2-bromoisonicotinate
;
_chemical_name_systematic
;
Ethyl 5-amino-2-bromopyridine-4-carboxylate
;
_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 mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 92.468(7)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 4.1538(9)
_cell_length_b 8.9978(16)
_cell_length_c 25.487(5)
_cell_measurement_reflns_used 2367
_cell_measurement_temperature 567(2)
_cell_measurement_theta_max 29.0
_cell_measurement_theta_min 2.5
_cell_volume 951.7(3)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 567(2)
_diffrn_detector_area_resol_mean 0.97
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type 'Bruker SMART APEXII CCD'
_diffrn_measurement_method '\f and \W scans'
_diffrn_radiation_monochromator Graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0367
_diffrn_reflns_av_unetI/netI 0.0191
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_limit_l_min -33
_diffrn_reflns_number 21643
_diffrn_reflns_theta_full 25.000
_diffrn_reflns_theta_max 28.259
_diffrn_reflns_theta_min 2.772
_diffrn_source 'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu 4.288
_exptl_absorpt_correction_T_max 0.401
_exptl_absorpt_correction_T_min 0.225
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour 'pale yellow'
_exptl_crystal_density_diffrn 1.710
_exptl_crystal_description Prism
_exptl_crystal_F_000 488
_exptl_crystal_size_max 0.320
_exptl_crystal_size_mid 0.270
_exptl_crystal_size_min 0.210
_refine_diff_density_max 0.532
_refine_diff_density_min -0.447
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_constraints 0.12
_refine_ls_number_parameters 126
_refine_ls_number_reflns 2353
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.036
_refine_ls_R_factor_all 0.0433
_refine_ls_R_factor_gt 0.0316
_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^)+(0.0216P)^2^+0.6676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0649
_refine_ls_wR_factor_ref 0.0689
_reflns_number_gt 1910
_reflns_number_total 2353
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file oi2013.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2023313
_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 0.341
_shelx_estimated_absorpt_t_max 0.466
_shelx_hkl_file
;
2 0 0 7012.00 177.68
2 0 0 7097.19 178.78
2 0 0 6917.81 177.08
2 0 0 7037.00 175.48
-2 0 0 7192.88 175.38
-2 0 0 7036.10 177.38
-2 0 0 7008.30 178.28
-2 0 0 6890.91 177.58
-3 0 0 2375.26 65.19
-3 0 0 2417.26 68.79
-3 0 0 2340.87 69.69
3 0 0 2397.96 70.89
3 0 0 2325.77 65.59
-3 0 0 2413.86 69.29
3 0 0 2383.26 68.69
-4 0 0 346.47 18.60
4 0 0 364.36 24.40
4 0 0 329.87 18.90
-4 0 0 331.87 21.60
-4 0 0 370.76 23.60
-5 0 0 43.60 12.00
5 0 0 38.00 15.60
-5 0 0 10.10 9.80
-5 0 0 47.00 16.00
-1 -1 0 22.70 3.10
-1 -1 0 27.20 2.40
1 -1 0 25.80 3.50
1 -1 0 25.90 4.20
1 -1 0 22.60 3.60
-1 -1 0 30.20 4.00
-1 -1 0 28.20 3.70
-1 1 0 22.00 3.20
-1 1 0 30.90 4.10
1 1 0 32.50 2.50
-1 1 0 24.30 3.90
-1 1 0 25.10 3.30
1 1 0 17.80 2.90
1 1 0 26.50 3.30
2 -1 0 -2.70 4.30
-2 -1 0 7.20 4.50
2 -1 0 -2.20 4.10
-2 -1 0 5.20 4.70
2 -1 0 5.40 3.40
-2 -1 0 2.10 3.00
2 -1 0 1.20 4.30
-2 -1 0 6.70 4.70
2 1 0 5.10 3.90
-2 1 0 1.30 4.10
-2 1 0 2.80 4.60
2 1 0 6.40 4.20
-2 1 0 0.00 4.50
2 1 0 4.10 4.20
-2 1 0 2.80 4.00
3 -1 0 314.37 19.10
3 -1 0 290.27 16.80
-3 -1 0 271.07 16.30
-3 -1 0 300.87 17.60
-3 -1 0 313.47 13.50
-3 -1 0 309.87 17.40
3 1 0 285.67 16.60
-3 1 0 275.47 16.90
3 1 0 288.17 13.80
3 1 0 295.27 18.40
-3 1 0 298.97 16.00
-3 1 0 312.47 17.80
-3 1 0 311.67 17.80
-4 -1 0 101.29 14.90
-4 -1 0 98.49 14.40
-4 -1 0 91.19 10.70
4 -1 0 68.79 14.60
4 1 0 98.89 18.70
4 1 0 106.19 11.40
-4 1 0 60.99 11.20
4 1 0 70.69 12.20
-4 1 0 77.59 12.00
-4 1 0 122.49 15.80
5 -1 0 8.20 12.20
-5 -1 0 14.80 8.60
-5 -1 0 -2.30 11.50
-5 -1 0 -7.70 13.40
-5 1 0 -2.20 11.30
-5 1 0 24.30 11.60
-5 1 0 2.60 12.60
5 1 0 20.00 12.50
1 -2 0 6153.68 155.98
1 -2 0 6288.37 154.58
1 -2 0 6427.76 155.58
-1 -2 0 6263.97 153.48
-1 -2 0 6285.47 155.98
1 -2 0 6246.98 155.78
-1 -2 0 6244.77 155.48
1 2 0 5998.80 155.28
-1 2 0 6297.67 156.08
1 2 0 6189.78 151.88
-1 2 0 6113.49 155.68
1 2 0 6207.08 156.08
1 2 0 6297.57 153.48
-1 2 0 6053.99 154.38
1 2 0 6082.59 151.78
2 -2 0 3478.65 91.89
-2 -2 0 3447.46 92.39
2 -2 0 3657.03 92.99
-2 -2 0 3521.65 87.19
-2 -2 0 3454.15 93.09
2 -2 0 3442.26 92.09
-2 -2 0 3482.25 90.99
2 -2 0 3525.15 93.59
-2 2 0 3416.66 92.59
2 2 0 3447.66 87.49
-2 2 0 3510.35 94.09
2 2 0 3426.06 90.79
-2 2 0 3511.85 92.49
-2 2 0 3437.56 91.89
2 2 0 3491.95 93.79
3 -2 0 945.21 35.80
3 -2 0 918.11 33.10
-3 -2 0 895.61 34.30
-3 -2 0 955.20 34.20
-3 -2 0 972.10 27.80
-3 -2 0 952.00 33.30
3 -2 0 971.40 34.00
3 2 0 897.81 35.30
3 2 0 977.40 34.30
-3 2 0 952.50 33.60
-3 2 0 913.31 34.60
-3 2 0 931.31 33.80
-3 2 0 933.91 34.30
3 2 0 939.21 28.40
3 2 0 887.81 33.00
-4 -2 0 375.76 23.30
-4 -2 0 332.47 15.50
-4 -2 0 345.47 22.10
4 -2 0 369.26 25.20
4 2 0 326.87 16.40
-4 2 0 354.26 21.60
-4 2 0 377.76 23.60
-4 2 0 345.67 22.70
4 2 0 369.76 25.30
4 2 0 336.37 22.00
-4 2 0 308.97 21.90
-5 -2 0 53.29 10.30
5 -2 0 50.09 15.20
-5 -2 0 91.69 18.40
5 2 0 42.00 15.70
-5 2 0 44.80 13.10
-5 2 0 45.80 14.20
-5 2 0 41.90 16.40
0 -3 0 0.20 2.50
0 -3 0 3.80 3.20
0 3 0 1.60 2.80
0 3 0 3.20 3.90
0 3 0 4.20 1.10
1 -3 0 57.99 5.80
-1 -3 0 48.60 4.00
-1 -3 0 47.80 5.80
1 -3 0 73.19 7.70
-1 -3 0 55.39 5.80
-1 -3 0 64.59 3.80
1 -3 0 57.89 5.30
1 -3 0 56.09 6.40
1 3 0 61.19 6.20
-1 3 0 56.09 6.30
1 3 0 61.89 4.40
1 3 0 47.80 6.00
-1 3 0 48.80 6.00
-1 3 0 56.29 5.40
-1 3 0 55.79 6.90
1 3 0 63.89 4.10
-2 -3 0 77.19 11.40
2 -3 0 77.09 9.70
2 -3 0 84.79 9.30
2 -3 0 65.09 8.60
-2 -3 0 70.99 7.70
2 -3 0 84.79 10.20
-2 3 0 52.39 7.70
2 3 0 76.69 7.80
-2 3 0 61.09 7.60
2 3 0 62.89 4.20
2 3 0 68.99 4.60
2 3 0 74.29 9.80
-2 3 0 48.10 8.70
-3 -3 0 -5.90 7.30
-3 -3 0 -0.40 6.50
3 -3 0 4.20 5.70
-3 -3 0 6.70 7.20
3 -3 0 -1.60 6.80
-3 3 0 -8.80 7.00
-3 3 0 6.80 7.70
3 3 0 11.80 8.60
3 3 0 2.60 3.50
3 3 0 -0.30 5.90
-3 3 0 -4.00 7.50
3 3 0 -1.10 7.10
-3 3 0 2.70 7.10
3 3 0 4.90 6.00
-4 -3 0 88.39 14.90
-4 -3 0 77.99 13.20
4 -3 0 66.19 15.00
-4 3 0 91.89 15.70
-4 3 0 100.49 16.10
4 3 0 79.49 8.00
4 3 0 79.09 8.30
-4 3 0 99.59 15.90
4 3 0 85.09 15.50
-4 3 0 95.69 16.20
4 3 0 61.79 10.90
-5 -3 0 8.60 10.40
5 -3 0 -4.10 12.60
-5 -3 0 12.40 13.80
-5 3 0 8.40 12.70
-5 3 0 14.50 13.30
5 3 0 -15.90 13.70
5 3 0 2.50 5.90
-5 3 0 10.10 13.90
0 -4 0 9588.44 236.68
0 -4 0 9606.24 232.98
0 -4 0 9620.14 236.28
0 4 0 9405.06 227.68
0 4 0 9058.29 237.68
0 4 0 9530.15 228.18
0 4 0 9258.37 232.58
0 4 0 8839.52 236.78
-1 -4 0 8022.80 198.58
1 -4 0 8005.70 203.08
-1 -4 0 7876.81 203.88
-1 -4 0 8301.47 203.48
1 -4 0 7819.42 203.68
1 -4 0 7982.60 199.58
1 -4 0 7890.41 203.28
-1 4 0 8312.37 204.78
-1 4 0 7812.32 203.88
1 4 0 7743.33 204.48
1 4 0 8125.59 204.18
-1 4 0 8216.88 203.48
1 4 0 8308.07 197.48
1 4 0 8183.88 198.68
-1 4 0 8090.19 199.48
2 -4 0 1672.93 50.79
-2 -4 0 1541.75 47.20
2 -4 0 1497.25 47.60
-2 -4 0 1572.14 43.60
-2 -4 0 1591.84 54.49
2 -4 0 1531.95 45.40
-2 4 0 1562.74 48.20
2 4 0 1537.55 39.80
2 4 0 1566.34 49.00
-2 4 0 1542.75 45.60
2 4 0 1497.45 39.70
2 4 0 1488.05 47.50
2 4 0 1511.85 43.20
3 -4 0 1140.49 43.00
-3 -4 0 1202.48 39.00
-3 -4 0 1183.78 41.40
-3 4 0 1200.18 43.10
-3 4 0 1243.48 43.10
3 4 0 1152.58 41.70
3 4 0 1213.58 44.60
3 4 0 1316.17 32.60
3 4 0 1185.08 31.70
3 4 0 1166.38 38.40
-3 4 0 1177.88 42.70
-3 4 0 1157.48 40.90
4 -4 0 378.06 27.60
-4 -4 0 335.67 23.00
-4 -4 0 344.87 22.20
4 4 0 359.56 24.10
4 4 0 376.26 12.20
-4 4 0 393.36 25.10
-4 4 0 383.86 23.90
-4 4 0 376.16 25.20
-4 4 0 374.76 25.90
4 4 0 395.26 27.70
-5 -4 0 37.00 13.80
-5 -4 0 12.70 12.20
5 -4 0 5.90 14.00
-5 4 0 44.80 17.30
-5 4 0 30.20 16.30
-5 4 0 14.10 13.10
5 4 0 13.70 13.50
0 -5 0 -3.10 4.60
0 -5 0 -0.20 4.30
0 -5 0 -0.40 4.30
0 5 0 7.40 6.00
0 5 0 -2.70 4.70
0 5 0 2.60 5.50
-1 -5 0 83.09 9.90
1 -5 0 83.89 12.10
1 -5 0 70.69 6.20
1 -5 0 91.49 10.60
-1 -5 0 89.29 10.70
-1 -5 0 73.69 4.10
1 -5 0 85.39 10.40
-1 -5 0 86.29 6.90
1 5 0 107.19 12.40
-1 5 0 70.29 6.50
1 5 0 120.49 13.00
1 5 0 80.39 4.00
-1 5 0 70.09 9.50
1 5 0 75.69 7.00
-2 -5 0 9.60 5.50
-2 -5 0 -1.20 4.30
2 -5 0 -2.10 5.30
-2 -5 0 3.40 6.30
2 -5 0 4.10 5.30
2 -5 0 -0.80 5.10
2 5 0 8.60 3.20
2 5 0 6.20 7.90
2 5 0 12.40 4.90
-2 5 0 17.60 8.60
-2 5 0 3.10 4.80
-2 5 0 10.30 6.80
2 5 0 10.30 5.30
-2 5 0 14.80 6.60
-3 -5 0 -2.10 6.50
-3 -5 0 12.10 6.10
3 -5 0 12.90 9.50
-3 5 0 -10.00 7.20
3 5 0 2.50 10.80
-3 5 0 0.10 8.20
3 5 0 1.70 6.30
-3 5 0 -4.60 9.40
-3 5 0 -7.80 7.10
3 5 0 -2.50 6.60
4 -5 0 55.19 15.10
-4 -5 0 32.00 10.00
-4 -5 0 47.40 11.60
-4 5 0 61.59 13.30
-4 5 0 29.10 11.30
-4 5 0 31.50 20.40
4 5 0 35.00 14.90
-4 5 0 27.10 14.00
4 5 0 59.89 11.90
-5 -5 0 9.40 12.10
-5 5 0 -3.80 14.90
5 5 0 -5.10 16.00
-5 5 0 14.30 14.00
-5 5 0 21.20 13.40
0 -6 0 3406.06 95.09
0 -6 0 3431.56 91.99
0 -6 0 3487.05 95.89
0 6 0 3375.06 97.19
0 6 0 3379.96 97.69
0 6 0 3490.45 91.99
-1 -6 0 2820.62 76.09
-1 -6 0 2871.81 82.19
1 -6 0 2730.73 82.59
1 -6 0 2888.61 81.79
1 -6 0 2776.42 80.49
1 -6 0 2996.20 74.79
-1 -6 0 2785.72 81.89
-1 6 0 2735.23 83.29
-1 6 0 3063.19 81.29
1 6 0 2978.00 76.09
1 6 0 2823.42 84.79
1 6 0 2952.20 85.39
-1 6 0 2854.01 84.79
-1 6 0 2921.61 74.39
2 -6 0 1348.07 45.70
2 -6 0 1396.96 45.00
-2 -6 0 1335.07 37.10
-2 -6 0 1318.87 44.40
-2 6 0 1228.08 45.80
2 6 0 1300.77 45.40
2 6 0 1273.57 35.40
-2 6 0 1321.77 46.40
2 6 0 1324.27 36.50
2 6 0 1302.47 47.00
-2 6 0 1277.07 45.60
-2 6 0 1330.17 40.30
2 6 0 1274.97 36.60
-3 -6 0 370.66 21.30
3 -6 0 336.67 23.10
-3 -6 0 351.66 17.70
3 6 0 346.37 17.00
-3 6 0 371.56 23.80
-3 6 0 333.77 22.80
-3 6 0 315.67 23.00
3 6 0 349.47 22.40
-3 6 0 329.67 19.30
3 6 0 391.46 26.40
-4 -6 0 66.89 12.80
4 -6 0 74.29 16.00
-4 -6 0 87.79 15.80
4 6 0 102.69 18.30
-4 6 0 93.49 18.90
-4 6 0 99.19 20.20
-4 6 0 71.19 14.80
4 6 0 57.59 17.60
-4 6 0 92.89 16.20
0 -7 0 -2.10 6.40
0 -7 0 -1.90 5.60
0 7 0 -0.70 6.90
0 7 0 6.00 7.60
0 7 0 -10.20 6.50
-1 -7 0 186.68 12.00
1 -7 0 164.98 14.60
1 -7 0 187.38 9.30
-1 -7 0 174.08 14.90
-1 7 0 143.09 14.90
1 7 0 137.59 15.80
-1 7 0 153.68 17.50
1 7 0 173.78 11.70
1 7 0 179.88 17.40
-1 7 0 190.08 15.70
-1 7 0 170.48 9.20
-2 -7 0 29.90 8.90
-2 -7 0 19.20 5.40
2 -7 0 7.50 6.40
-2 -7 0 16.60 4.40
2 -7 0 35.70 10.20
-2 7 0 27.10 10.20
-2 7 0 20.40 11.30
2 7 0 18.10 9.90
2 7 0 16.20 9.80
2 7 0 13.40 5.30
-2 7 0 10.80 7.10
2 7 0 12.70 4.10
-2 7 0 15.10 10.00
-3 -7 0 6.20 6.30
-3 -7 0 17.50 8.80
3 7 0 -7.40 7.10
-3 7 0 -2.60 8.50
-3 7 0 9.10 9.60
3 7 0 -0.20 10.10
-3 7 0 2.60 9.90
3 7 0 -3.60 9.50
4 -7 0 1.80 12.10
-4 -7 0 10.90 9.80
-4 -7 0 13.50 9.40
-4 7 0 16.70 12.90
4 7 0 6.90 14.80
-4 7 0 29.80 22.10
-4 7 0 2.10 13.80
0 -8 0 708.23 30.60
0 8 0 742.43 29.80
0 8 0 803.92 35.00
0 8 0 760.22 34.10
-1 -8 0 164.98 15.40
-1 -8 0 137.09 14.10
1 -8 0 181.08 15.80
1 -8 0 176.88 9.00
1 8 0 216.18 19.90
-1 8 0 161.08 16.50
1 8 0 161.58 17.90
-1 8 0 202.48 22.00
-1 8 0 207.48 18.00
1 8 0 179.88 13.20
-1 8 0 170.38 8.90
2 -8 0 314.27 21.50
2 -8 0 303.57 15.90
-2 -8 0 313.57 14.60
-2 8 0 323.07 26.50
2 8 0 369.46 26.70
2 8 0 313.27 13.90
-2 8 0 361.16 23.40
-2 8 0 320.57 23.50
-2 8 0 311.87 16.30
2 8 0 310.07 24.30
-3 -8 0 185.78 12.00
3 -8 0 185.18 19.40
-3 -8 0 186.68 19.10
-3 8 0 213.08 23.60
-3 8 0 180.18 21.80
-3 8 0 221.58 22.10
-3 8 0 234.48 18.20
3 8 0 182.38 12.10
3 8 0 204.48 22.80
3 8 0 193.28 24.00
-4 -8 0 49.10 10.80
-4 8 0 46.40 19.30
-4 8 0 46.00 17.30
4 8 0 48.90 17.30
-4 8 0 44.60 14.30
0 -9 0 3.90 6.70
0 9 0 -7.30 8.60
0 9 0 9.00 10.30
0 9 0 -6.50 8.10
-1 -9 0 15.70 7.50
1 -9 0 9.50 7.90
-1 -9 0 4.10 8.10
-1 9 0 11.40 11.10
1 9 0 7.50 8.20
-1 9 0 -2.90 10.90
-1 9 0 12.70 8.60
-1 9 0 5.60 3.00
-1 9 0 0.40 3.40
1 9 0 3.00 11.30
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3 1 -10 286.77 19.50
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2 -3 -10 949.80 33.30
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_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 2376
_shelx_res_file
;
TITL BSPM_1_0m_a.res in P2(1)/c
shelx.res
created by SHELXL-2019/3 at 21:15:29 on 07-Oct-2024
CELL 0.71073 4.1538 8.9978 25.4873 90.000 92.468 90.000
ZERR 4.00 0.0009 0.0016 0.0051 0.000 0.007 0.000
LATT 1
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H BR N O
UNIT 32 36 4 8 8
MERG 2
EQIV $1 x,y,z
HTAB N2 O2_$1
EQIV $3 -x,+y+1/2,-z+1/2
HTAB N2 N1_$3
FMAP 2
PLAN 20
SIZE 0.210 0.270 0.320
ACTA 50.00
TEMP 294
BOND $H
CONF
LIST 4
L.S. 10
WGHT 0.021600 0.667600
FVAR 0.96271
BR1 3 0.509815 0.236684 0.332907 11.00000 0.07039 0.04411 =
0.07136 -0.01644 -0.01747 0.00444
O1 5 0.675612 0.719531 0.447889 11.00000 0.07177 0.04209 =
0.03991 -0.00751 -0.01997 0.00062
O2 5 0.424491 0.916069 0.411762 11.00000 0.10442 0.03961 =
0.05720 -0.00683 -0.02245 0.00779
N2 4 0.081097 0.870531 0.318667 11.00000 0.10207 0.04667 =
0.05185 0.00908 -0.03130 0.00561
C1 1 0.390951 0.682002 0.367797 11.00000 0.04749 0.03817 =
0.03044 0.00146 -0.00479 -0.00557
C2 1 0.194901 0.730328 0.324863 11.00000 0.05590 0.04262 =
0.03591 0.00833 -0.00729 -0.00576
C3 1 0.110585 0.622017 0.286775 11.00000 0.06255 0.05599 =
0.03344 0.00504 -0.01391 -0.00746
AFIX 43
H3 2 -0.019460 0.651860 0.258076 11.00000 -1.20000
AFIX 0
N1 4 0.201617 0.481693 0.288639 11.00000 0.05694 0.05129 =
0.03493 -0.00410 -0.00896 -0.00855
C4 1 0.386665 0.440300 0.329810 11.00000 0.04602 0.03985 =
0.03942 -0.00425 -0.00261 -0.00558
C5 1 0.486972 0.533643 0.369598 11.00000 0.04880 0.04138 =
0.03308 0.00050 -0.00897 -0.00330
AFIX 43
H5 2 0.617469 0.498569 0.397470 11.00000 -1.20000
AFIX 0
C6 1 0.494730 0.786346 0.410301 11.00000 0.05887 0.04013 =
0.03674 -0.00055 -0.00690 -0.00361
C7 1 0.791673 0.811160 0.491739 11.00000 0.06833 0.05567 =
0.04184 -0.01672 -0.01590 -0.00521
AFIX 23
H7A 2 0.612483 0.860208 0.507725 11.00000 -1.20000
H7B 2 0.938171 0.886598 0.479721 11.00000 -1.20000
AFIX 0
C8 1 0.960099 0.712119 0.530180 11.00000 0.07986 0.09135 =
0.04780 -0.00651 -0.02035 -0.00322
AFIX 33
H8A 2 1.039906 0.769478 0.559719 11.00000 -1.50000
H8B 2 0.812758 0.638136 0.541835 11.00000 -1.50000
H8C 2 1.137029 0.664411 0.513954 11.00000 -1.50000
AFIX 0
H2A 2 -0.018322 0.889177 0.291118 11.00000 0.06367
H2B 2 0.140763 0.933784 0.343239 11.00000 0.06744
HKLF 4
REM BSPM_1_0m_a.res in P2(1)/c
REM wR2 = 0.0689, GooF = S = 1.036, Restrained GooF = 1.036 for all data
REM R1 = 0.0316 for 1910 Fo > 4sig(Fo) and 0.0433 for all 2353 data
REM 126 parameters refined using 0 restraints
END
WGHT 0.0216 0.6651
REM Highest difference peak 0.532, deepest hole -0.447, 1-sigma level 0.048
Q1 1 0.5169 0.2932 0.3092 11.00000 0.05 0.53
Q2 1 0.3871 0.2545 0.3611 11.00000 0.05 0.27
Q3 1 0.4155 0.7243 0.3896 11.00000 0.05 0.23
Q4 1 0.4775 0.6160 0.3607 11.00000 0.05 0.21
Q5 1 0.2875 0.7185 0.3504 11.00000 0.05 0.20
Q6 1 0.2057 0.6702 0.3023 11.00000 0.05 0.20
Q7 1 0.5314 0.1658 0.3141 11.00000 0.05 0.19
Q8 1 0.4644 0.4837 0.3472 11.00000 0.05 0.19
Q9 1 0.8642 0.7454 0.5032 11.00000 0.05 0.19
Q10 1 0.2507 0.5555 0.2817 11.00000 0.05 0.18
Q11 1 0.3032 0.4748 0.3054 11.00000 0.05 0.17
Q12 1 0.7064 0.7777 0.4725 11.00000 0.05 0.16
Q13 1 0.7067 0.2599 0.3438 11.00000 0.05 0.15
Q14 1 0.7810 0.7602 0.4283 11.00000 0.05 0.15
Q15 1 0.3016 0.9173 0.4054 11.00000 0.05 0.15
Q16 1 0.6720 0.7995 0.4837 11.00000 0.05 0.15
Q17 1 1.1347 0.6275 0.5298 11.00000 0.05 0.14
Q18 1 0.6901 0.9329 0.4923 11.00000 0.05 0.14
Q19 1 0.1787 0.4205 0.2655 11.00000 0.05 0.14
Q20 1 0.1123 0.5379 0.3006 11.00000 0.05 0.14
;
_shelx_res_checksum 90287
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 Br1 0.50981(7) 0.23668(3) 0.33291(2) 0.06255(12) Uani d 1 . .
O O1 0.6756(4) 0.71953(17) 0.44789(6) 0.0519(4) Uani d 1 . .
O O2 0.4245(5) 0.91607(19) 0.41176(7) 0.0678(5) Uani d 1 . .
N N2 0.0811(7) 0.8705(3) 0.31867(10) 0.0679(7) Uani d 1 . .
C C1 0.3910(5) 0.6820(2) 0.36780(8) 0.0389(4) Uani d 1 . .
C C2 0.1949(6) 0.7303(2) 0.32486(8) 0.0451(5) Uani d 1 . .
C C3 0.1106(6) 0.6220(3) 0.28677(9) 0.0511(6) Uani d 1 . .
H H3 -0.019460 0.651860 0.258076 0.061 Uiso calc 1 . .
N N1 0.2016(5) 0.4817(2) 0.28864(7) 0.0480(5) Uani d 1 . .
C C4 0.3867(5) 0.4403(2) 0.32981(8) 0.0419(5) Uani d 1 . .
C C5 0.4870(5) 0.5336(2) 0.36960(8) 0.0414(5) Uani d 1 . .
H H5 0.617469 0.498569 0.397470 0.050 Uiso calc 1 . .
C C6 0.4947(6) 0.7863(3) 0.41030(8) 0.0455(5) Uani d 1 . .
C C7 0.7917(7) 0.8112(3) 0.49174(9) 0.0558(6) Uani d 1 . .
H H7A 0.612483 0.860208 0.507725 0.067 Uiso calc 1 . .
H H7B 0.938171 0.886598 0.479721 0.067 Uiso calc 1 . .
C C8 0.9601(8) 0.7121(4) 0.53018(11) 0.0737(8) Uani d 1 . .
H H8A 1.039906 0.769478 0.559719 0.111 Uiso calc 1 . .
H H8B 0.812758 0.638136 0.541835 0.111 Uiso calc 1 . .
H H8C 1.137029 0.664411 0.513954 0.111 Uiso calc 1 . .
H H2A -0.018(6) 0.889(3) 0.2911(12) 0.064(8) Uiso d 1 . .
H H2B 0.141(7) 0.934(3) 0.3432(12) 0.067(9) 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
Br1 0.07039(19) 0.04411(15) 0.0714(2) 0.00444(12) -0.01747(13) -0.01644(12)
O1 0.0718(11) 0.0421(8) 0.0399(8) 0.0006(7) -0.0200(7) -0.0075(7)
O2 0.1044(15) 0.0396(9) 0.0572(11) 0.0078(9) -0.0225(10) -0.0068(8)
N2 0.102(2) 0.0467(12) 0.0519(14) 0.0056(12) -0.0313(13) 0.0091(10)
C1 0.0475(12) 0.0382(10) 0.0304(10) -0.0056(9) -0.0048(9) 0.0015(8)
C2 0.0559(13) 0.0426(11) 0.0359(11) -0.0058(10) -0.0073(9) 0.0083(9)
C3 0.0625(15) 0.0560(14) 0.0334(11) -0.0075(11) -0.0139(10) 0.0050(10)
N1 0.0569(12) 0.0513(11) 0.0349(9) -0.0085(9) -0.0090(8) -0.0041(8)
C4 0.0460(12) 0.0399(11) 0.0394(11) -0.0056(9) -0.0026(9) -0.0042(9)
C5 0.0488(12) 0.0414(11) 0.0331(10) -0.0033(9) -0.0090(9) 0.0005(8)
C6 0.0589(14) 0.0401(11) 0.0367(11) -0.0036(10) -0.0069(10) -0.0005(8)
C7 0.0683(16) 0.0557(14) 0.0418(12) -0.0052(12) -0.0159(11) -0.0167(11)
C8 0.080(2) 0.091(2) 0.0478(15) -0.0032(17) -0.0203(14) -0.0065(14)
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'
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
C6 O1 C7 . . 117.00(18) ?
C2 N2 H2A . . 117(2) ?
C2 N2 H2B . . 115.9(19) ?
H2A N2 H2B . . 127(3) ?
C5 C1 C2 . . 118.54(19) ?
C5 C1 C6 . . 120.56(19) ?
C2 C1 C6 . . 120.9(2) ?
N2 C2 C1 . . 124.5(2) ?
N2 C2 C3 . . 119.3(2) ?
C1 C2 C3 . . 116.2(2) ?
N1 C3 C2 . . 125.1(2) ?
N1 C3 H3 . . 117.4 ?
C2 C3 H3 . . 117.4 ?
C3 N1 C4 . . 116.92(19) ?
N1 C4 C5 . . 124.2(2) ?
N1 C4 Br1 . . 116.65(15) ?
C5 C4 Br1 . . 119.19(16) ?
C4 C5 C1 . . 119.1(2) ?
C4 C5 H5 . . 120.5 ?
C1 C5 H5 . . 120.5 ?
O2 C6 O1 1 . 123.0(2) ?
O2 C6 O1 . . 123.0(2) ?
O2 C6 C1 1 . 125.0(2) ?
O2 C6 C1 . . 125.0(2) ?
O1 C6 C1 . . 112.08(19) ?
O1 C7 C8 . . 107.4(2) ?
O1 C7 H7A . . 110.2 ?
C8 C7 H7A . . 110.2 ?
O1 C7 H7B . . 110.2 ?
C8 C7 H7B . . 110.2 ?
H7A C7 H7B . . 108.5 ?
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 ?
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
Br1 C4 . 1.903(2) ?
O1 C6 . 1.335(3) ?
O1 C7 . 1.454(2) ?
O2 C6 . 1.204(3) ?
N2 C2 . 1.354(3) ?
N2 H2A . 0.82(3) ?
N2 H2B . 0.87(3) ?
C1 C5 . 1.393(3) ?
C1 C2 . 1.405(3) ?
C1 C6 . 1.483(3) ?
C2 C3 . 1.409(3) ?
C3 N1 . 1.318(3) ?
C3 H3 . 0.9300 ?
N1 C4 . 1.327(3) ?
C4 C5 . 1.368(3) ?
C5 H5 . 0.9300 ?
C7 C8 . 1.478(4) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C8 H8A . 0.9600 ?
C8 H8B . 0.9600 ?
C8 H8C . 0.9600 ?
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
N2 H2B O2 1 0.87(3) 2.07(3) 2.746(3) 133(2) yes
C5 H5 O1 1 0.93 2.3700 2.694(3) 99.88(3) y
N2 H2A N1 2 0.82(3) 2.30(3) 3.096(3) 166(3) 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
C5 C1 C2 N2 . . . . 179.0(2) ?
C6 C1 C2 N2 . . . . -1.2(4) ?
C5 C1 C2 C3 . . . . 0.2(3) ?
C6 C1 C2 C3 . . . . -180.0(2) ?
N2 C2 C3 N1 . . . . -179.0(3) ?
C1 C2 C3 N1 . . . . -0.1(4) ?
C2 C3 N1 C4 . . . . 0.1(4) ?
C3 N1 C4 C5 . . . . -0.2(3) ?
C3 N1 C4 Br1 . . . . 178.77(18) ?
N1 C4 C5 C1 . . . . 0.3(4) ?
Br1 C4 C5 C1 . . . . -178.67(16) ?
C2 C1 C5 C4 . . . . -0.2(3) ?
C6 C1 C5 C4 . . . . 179.9(2) ?
C7 O1 C6 O2 . . . 1 -0.6(4) ?
C7 O1 C6 O2 . . . . -0.6(4) ?
C7 O1 C6 C1 . . . . 180.0(2) ?
C5 C1 C6 O2 . . . 1 179.6(2) ?
C2 C1 C6 O2 . . . 1 -0.2(4) ?
C5 C1 C6 O2 . . . . 179.6(2) ?
C2 C1 C6 O2 . . . . -0.2(4) ?
C5 C1 C6 O1 . . . . -1.0(3) ?
C2 C1 C6 O1 . . . . 179.1(2) ?
C6 O1 C7 C8 . . . . 175.2(2) ?