#------------------------------------------------------------------------------
#$Date: 2024-05-11 04:51:26 +0300 (Sat, 11 May 2024) $
#$Revision: 291818 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023123.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_2023123
loop_
_publ_author_name
'Guseinov, Firudin I.'
'\,Celikesir, Sevim T\"urktekin'
'Akkurt, Mehmet'
'Ovsyannikov, Viacheslav O.'
'Ugrak, Bogdan I.'
'Lavrova, Oksana M.'
'Samigullina, Aida I.'
'Bhattarai, Ajaya'
_publ_section_title
;
Synthesis, crystal structure and Hirshfeld surface analysis of
(3Z)-4-[(4-amino-1,2,5-oxadiazol-3-yl)amino]-3-bromo-1,1,1-trifluorobut-3-en-2-one
;
_journal_coeditor_code TX2085
_journal_issue 6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024004080
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C6 H4 Br F3 N4 O2'
_chemical_formula_moiety 'C6 H4 Br F3 N4 O2'
_chemical_formula_sum 'C6 H4 Br F3 N4 O2'
_chemical_formula_weight 301.04
_chemical_name_systematic
(3Z)-4-[(4-Amino-1,2,5-oxadiazol-3-yl)amino]-3-bromo-1,1,1-trifluorobut-3-en-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 difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 95.1372(6)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 4.95281(3)
_cell_length_b 14.05150(10)
_cell_length_c 13.52080(10)
_cell_measurement_reflns_used 17512
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 78.8320
_cell_measurement_theta_min 4.4520
_cell_volume 937.192(11)
_computing_cell_refinement
;
CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0303
_diffrn_reflns_av_unetI/netI 0.0137
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 24751
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 79.645
_diffrn_reflns_theta_min 4.548
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 6.460
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.490
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 2.134
_exptl_crystal_description block
_exptl_crystal_F_000 584
_exptl_crystal_size_max 0.210
_exptl_crystal_size_mid 0.040
_exptl_crystal_size_min 0.040
_refine_diff_density_max 0.725
_refine_diff_density_min -0.501
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.093
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 159
_refine_ls_number_reflns 2038
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.098
_refine_ls_R_factor_all 0.0278
_refine_ls_R_factor_gt 0.0275
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+2.0497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0649
_refine_ls_wR_factor_ref 0.0651
_reflns_number_gt 2010
_reflns_number_total 2038
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file tx2085.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2023123
_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 0.344
_shelx_estimated_absorpt_t_max 0.782
_shelx_hkl_file
;
0 0 -1 0.32 0.13
0 0 2 691.76 19.41
0 0 -2 762.76 19.14
0 0 -3 0.50 0.37
0 0 -4 12.84 1.37
0 0 -5 0.15 0.48
0 0 6 297.88 11.14
0 0 -6 266.35 9.96
0 0 7 0.36 0.31
0 0 7 0.57 0.58
0 0 7 0.23 0.31
0 0 8 592.92 20.91
0 0 8 579.46 16.13
0 0 9 0.32 0.43
0 0 9 -0.41 0.73
0 0 10 455.57 14.05
0 0 10 486.61 14.43
0 0 10 465.30 14.06
0 0 -10 466.81 13.77
0 0 10 463.70 14.08
0 0 10 505.51 20.03
0 0 10 473.80 14.12
0 0 10 475.30 14.09
0 0 11 0.27 0.54
0 0 11 1.23 0.67
0 0 -11 0.24 0.48
0 0 11 -0.42 0.50
0 0 11 1.11 1.14
0 0 11 -0.14 0.47
0 0 11 0.27 0.49
0 0 11 0.69 0.55
0 0 12 93.86 4.45
0 0 12 84.19 4.28
0 0 12 92.66 4.41
0 0 12 88.23 4.58
0 0 12 93.37 4.45
0 0 12 97.07 8.73
0 0 12 95.74 8.37
0 0 12 85.44 4.41
0 0 -12 83.14 4.07
0 0 13 -0.16 0.54
0 0 13 0.28 0.49
0 0 13 -0.68 0.98
0 0 13 0.28 0.61
0 0 13 0.16 0.45
0 0 13 -0.14 0.46
0 0 13 0.14 0.46
0 0 13 -0.13 0.46
0 0 13 0.63 1.12
0 0 13 0.66 0.68
0 0 14 44.93 2.99
0 0 14 54.83 3.01
0 0 14 49.12 2.85
0 0 14 51.41 2.96
0 0 15 0.34 0.36
0 0 15 0.12 0.42
0 0 15 0.10 0.33
0 0 15 0.09 0.35
0 0 -16 41.59 2.26
0 0 16 37.65 2.19
0 0 16 40.67 2.14
0 0 17 -0.08 0.17
0 0 -17 0.04 0.20
0 -1 0 0.30 0.18
0 1 0 0.44 0.15
0 1 1 1.01 0.26
0 -1 1 1.00 0.21
0 1 1 0.91 0.28
0 -1 -2 19.70 1.31
0 1 2 20.02 1.43
0 -1 -3 32.72 2.05
0 1 3 35.24 2.32
0 -1 -4 1688.50 44.88
0 1 4 1757.75 45.65
0 1 5 498.40 16.66
0 -1 -5 507.91 15.63
0 1 5 499.61 16.41
0 1 5 520.03 16.24
0 -1 -6 549.43 17.32
0 1 6 541.32 18.65
0 1 6 559.12 18.10
0 1 6 537.84 18.31
0 1 7 129.06 7.91
0 -1 -7 149.22 7.22
0 1 7 136.85 7.90
0 1 7 145.05 7.65
0 -1 7 153.53 4.97
0 1 7 148.80 4.98
0 -1 7 133.46 4.96
0 -1 -8 63.26 4.64
0 -1 8 60.19 5.22
0 1 8 64.83 5.53
0 1 8 65.87 5.28
0 -1 8 63.40 3.08
0 1 8 63.40 2.94
0 -1 8 60.60 2.88
0 1 9 94.57 7.01
0 -1 9 106.53 7.72
0 1 9 101.34 4.20
0 1 10 65.36 3.45
0 -1 10 63.82 3.39
0 -1 10 59.39 3.43
0 1 10 65.83 3.39
0 1 10 62.92 3.52
0 -1 10 62.73 3.36
0 -1 -10 61.31 3.25
0 1 10 60.36 3.35
0 -1 10 59.23 3.29
0 1 10 59.81 3.29
0 -1 10 67.27 3.49
0 1 10 72.54 3.53
0 1 10 75.00 6.56
0 -1 10 64.08 6.40
0 -1 11 219.93 13.02
0 -1 11 196.45 7.23
0 1 11 201.62 12.14
0 1 11 193.14 7.35
0 -1 11 189.39 7.27
0 -1 11 205.77 7.43
0 -1 11 195.16 7.59
0 1 11 196.75 7.30
0 1 11 197.02 7.63
0 -1 -11 195.05 7.17
0 -1 11 198.13 7.39
0 1 11 204.88 7.39
0 -1 11 197.83 7.35
0 1 11 201.67 7.43
0 -1 11 202.14 12.85
0 1 11 200.63 7.43
0 -1 12 223.78 8.04
0 1 12 238.47 13.94
0 -1 12 220.62 13.69
0 -1 12 216.12 8.10
0 1 12 236.95 8.36
0 -1 12 237.48 8.33
0 1 12 240.53 8.30
0 -1 12 212.45 8.34
0 1 12 238.42 8.69
0 -1 -12 219.36 8.02
0 -1 12 230.17 8.29
0 1 12 230.12 8.22
0 1 12 224.10 8.23
0 -1 12 216.04 8.10
0 -1 12 249.45 14.80
0 1 12 233.98 8.40
0 1 13 61.10 3.49
0 -1 13 57.73 3.25
0 1 13 66.77 6.94
0 1 13 61.26 3.42
0 1 13 54.11 3.23
0 1 13 57.30 3.30
0 1 13 60.46 3.64
0 -1 13 64.31 3.50
0 1 13 50.75 3.32
0 1 13 61.19 3.41
0 -1 13 65.72 3.56
0 -1 -13 54.70 3.18
0 -1 13 57.55 6.83
0 1 14 260.64 9.15
0 -1 -14 255.47 8.45
0 -1 14 277.46 8.96
0 1 14 273.51 8.85
0 1 14 276.96 8.91
0 -1 14 265.20 8.91
0 1 14 258.78 8.81
0 -1 14 249.25 8.50
0 -1 15 30.05 2.13
0 1 15 25.15 1.99
0 1 15 29.01 2.12
0 1 15 26.54 1.85
0 -1 15 24.24 1.63
0 -1 15 32.61 2.03
0 -1 15 30.62 1.98
0 1 16 27.82 1.79
0 1 16 29.94 1.86
0 -1 16 28.80 1.82
0 1 -16 30.23 1.85
0 1 16 22.92 1.37
0 -1 16 29.01 1.65
0 1 -16 29.44 1.71
0 1 16 27.50 1.73
0 -1 16 27.28 1.71
0 -1 17 0.13 0.18
0 1 17 0.08 0.19
0 -1 -17 -0.04 0.20
0 1 -17 0.13 0.22
0 2 0 20.49 1.25
0 2 0 20.96 1.21
0 -2 0 18.17 1.36
0 2 1 269.51 7.76
0 2 -1 259.64 7.66
0 -2 -1 277.25 8.12
0 -2 1 262.00 7.33
0 -2 -2 194.96 6.61
0 -2 2 202.66 5.97
0 2 2 208.52 6.86
0 2 3 1758.75 46.81
0 -2 -3 1815.20 46.40
0 2 4 18.97 1.99
0 -2 -4 17.93 1.79
0 -2 5 285.01 10.35
0 2 5 298.38 11.02
0 2 5 292.30 10.45
0 -2 -5 266.90 10.08
0 2 6 457.84 15.43
0 2 6 459.37 16.14
0 -2 6 475.80 15.62
0 -2 6 474.54 15.96
0 -2 -6 461.42 15.28
0 -2 6 430.13 12.43
0 2 6 447.31 12.34
0 2 7 552.62 18.62
0 2 7 546.13 19.28
0 -2 7 536.69 18.47
0 -2 7 540.21 18.86
0 -2 -7 515.99 17.91
0 2 7 488.59 19.13
0 -2 7 521.00 14.53
0 2 7 548.00 14.66
0 -2 7 521.87 14.76
0 2 8 113.63 7.16
0 -2 8 120.76 7.30
0 -2 8 107.47 7.18
0 2 8 101.50 7.27
0 -2 -8 95.22 6.23
0 2 8 120.46 8.00
0 -2 8 91.45 7.10
0 -2 8 101.11 4.30
0 -2 8 110.14 4.17
0 2 8 109.46 4.20
0 -2 9 542.69 19.97
0 2 9 516.52 20.79
0 -2 9 517.53 20.24
0 2 9 516.55 19.84
0 -2 9 495.86 14.78
0 2 9 488.04 14.51
0 -2 9 504.53 14.53
0 -2 9 476.98 20.47
0 -2 -9 504.38 18.61
0 2 9 545.51 21.46
0 -2 10 7.02 1.08
0 2 10 7.68 1.11
0 2 10 5.01 0.94
0 -2 10 5.48 0.96
0 2 10 5.87 0.97
0 -2 10 5.90 0.99
0 -2 10 4.86 0.95
0 2 10 5.91 2.02
0 -2 10 6.33 2.14
0 -2 -10 4.64 0.93
0 -2 10 5.07 0.91
0 2 10 4.38 1.67
0 -2 10 5.77 1.95
0 2 10 3.98 1.76
0 -2 10 8.16 2.15
0 -2 10 5.32 0.96
0 2 10 6.93 1.06
0 -2 10 5.86 0.97
0 2 10 5.63 0.95
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0 -2 11 359.77 11.65
0 -2 11 362.37 17.24
0 2 11 376.47 18.66
0 2 11 373.31 17.49
0 -2 11 366.05 17.80
0 -2 11 337.49 11.17
0 -2 11 345.71 11.45
0 2 11 364.69 11.61
0 2 11 366.58 11.49
0 -2 11 356.99 11.60
0 2 11 336.39 11.72
0 -2 -11 366.96 11.49
0 2 11 366.49 11.63
0 -2 11 343.27 11.43
0 -2 11 373.16 18.55
0 -2 11 364.36 11.54
0 2 11 372.29 11.64
0 -2 12 26.51 2.23
0 2 12 29.48 2.27
0 2 12 25.42 4.23
0 2 12 20.43 4.14
0 -2 12 34.00 4.80
0 -2 12 31.53 2.21
0 -2 12 38.15 5.27
0 2 12 25.80 2.17
0 2 12 27.48 2.20
0 -2 12 27.91 2.29
0 2 12 29.27 2.51
0 -2 -12 31.31 2.36
0 2 12 27.30 2.24
0 -2 12 24.17 4.47
0 -2 12 23.35 2.14
0 2 12 28.18 2.32
0 2 13 48.92 2.99
0 2 13 42.82 3.05
0 2 13 42.21 2.76
0 -2 13 50.57 3.04
0 -2 13 42.21 2.64
0 2 13 44.19 2.88
0 -2 -13 46.58 2.91
0 -2 13 47.71 2.99
0 2 13 46.21 2.89
0 -2 13 52.32 3.18
0 2 13 48.25 3.11
0 2 14 0.91 0.58
0 2 14 0.79 0.49
0 2 14 1.04 0.54
0 -2 14 0.37 0.48
0 2 14 0.57 0.45
0 -2 14 0.49 0.44
0 2 14 0.71 0.55
0 -2 -14 1.01 0.50
0 2 14 1.52 0.68
0 -2 14 0.47 0.41
0 -2 14 0.83 0.49
0 2 14 0.85 0.57
0 -2 15 3.09 0.71
0 -2 15 4.21 0.77
0 2 15 2.72 0.63
0 -2 -15 2.68 0.72
0 2 -15 2.57 0.72
0 -2 -15 4.36 0.69
0 2 15 3.75 0.80
0 -2 15 2.61 0.68
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0 2 15 3.35 0.75
0 -2 15 3.40 0.69
0 2 -16 4.41 0.70
0 2 16 3.66 0.64
0 -2 16 3.49 0.64
0 2 16 4.48 0.72
0 -2 16 3.27 0.59
0 -2 16 3.61 0.60
0 -2 -16 3.38 0.62
0 2 -16 3.24 0.64
0 -2 -16 4.39 0.72
0 2 16 4.20 0.59
0 -2 16 2.99 0.55
0 2 -17 14.86 0.91
0 2 -17 15.17 0.86
0 -2 17 12.87 0.80
0 -3 0 0.12 0.42
0 3 0 0.62 0.34
0 3 0 0.43 0.32
0 -3 1 335.59 10.93
0 -3 -1 339.44 10.85
0 3 1 359.62 10.43
0 3 -1 332.51 10.17
0 -3 1 348.24 9.21
0 3 1 351.96 9.14
0 3 2 1022.04 25.21
0 -3 2 979.60 25.26
0 3 2 959.76 26.07
0 -3 -2 991.43 26.71
0 -3 -3 86.16 4.22
0 -3 3 86.58 3.87
0 3 3 87.52 3.85
0 3 3 84.67 4.40
0 -3 -4 19.38 2.01
0 -3 4 19.08 2.19
0 3 4 20.61 1.92
0 3 4 20.67 2.27
0 -3 4 23.06 2.00
0 -3 -5 1076.59 31.21
0 -3 5 1085.58 32.17
0 -3 5 1133.51 31.02
0 3 5 1104.83 32.04
0 3 5 1101.71 31.04
0 -3 -6 72.68 4.82
0 -3 6 64.67 5.06
0 3 6 76.14 4.85
0 -3 6 68.21 4.58
0 3 6 73.22 5.23
0 3 6 71.66 2.81
0 -3 6 64.19 2.87
0 -3 6 67.51 2.72
0 -3 7 406.01 16.09
0 -3 -7 394.28 14.86
0 3 7 388.02 15.73
0 -3 7 416.97 15.58
0 -3 7 407.86 14.93
0 3 7 404.56 15.02
0 -3 7 385.79 11.17
0 -3 7 390.88 11.49
0 3 7 391.52 11.26
0 3 8 10.45 2.45
0 -3 8 15.47 2.82
0 -3 -8 10.53 2.06
0 -3 8 12.49 1.18
0 3 8 13.67 1.24
0 -3 8 13.56 1.35
0 3 8 15.21 2.81
0 -3 8 13.36 2.33
0 3 8 13.98 2.40
0 -3 8 12.37 2.37
0 3 9 260.12 13.91
0 -3 9 297.51 13.37
0 -3 9 266.33 13.37
0 3 9 270.10 12.97
0 3 9 266.44 8.80
0 -3 9 247.63 8.65
0 3 9 271.76 8.85
0 -3 9 259.18 8.74
0 -3 9 265.93 8.83
0 -3 9 273.68 8.92
0 -3 -9 265.55 8.67
0 -3 9 274.63 8.96
0 3 9 267.14 8.63
0 -3 9 263.74 8.56
0 -3 9 272.03 14.06
0 -3 -9 269.98 12.57
0 3 9 257.63 14.04
0 -3 10 54.15 2.84
0 3 10 48.42 5.86
0 -3 10 52.20 5.67
0 3 10 61.81 5.95
0 -3 10 62.94 5.94
0 3 10 59.32 3.26
0 3 10 56.08 3.18
0 -3 10 57.61 3.24
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0 3 10 55.62 3.15
0 -3 10 57.14 3.25
0 -3 -10 55.51 3.14
0 -3 -10 52.72 2.94
0 -3 10 61.94 3.43
0 -3 10 53.29 3.02
0 3 10 53.27 3.09
0 -3 -10 54.73 5.19
0 3 10 54.15 6.22
0 -3 10 57.31 6.28
0 -3 11 129.51 5.17
0 -3 11 135.51 9.63
0 -3 11 134.25 9.87
0 3 11 131.04 10.25
0 3 11 135.12 9.70
0 3 11 142.51 5.81
0 -3 11 133.72 5.70
0 3 11 138.90 5.63
0 -3 -11 130.39 5.59
0 3 11 141.47 5.69
0 -3 11 142.04 5.85
0 3 11 130.12 5.62
0 -3 11 135.12 10.38
0 3 11 152.82 11.14
0 -3 11 134.72 5.61
0 3 11 134.00 5.68
0 3 12 15.55 3.33
0 -3 12 18.87 3.66
0 3 12 13.09 3.34
0 -3 12 11.70 2.97
0 3 12 15.03 1.64
0 -3 12 12.52 1.53
0 3 12 11.95 1.43
0 -3 -12 16.31 1.70
0 3 12 15.21 1.65
0 3 12 11.96 1.42
0 -3 12 13.88 1.63
0 3 12 14.59 3.44
0 -3 12 10.38 1.40
0 3 12 11.37 1.48
0 3 13 145.97 5.85
0 3 13 148.51 5.80
0 -3 13 141.23 5.87
0 3 13 142.10 5.80
0 -3 -13 143.98 5.89
0 -3 13 130.14 5.77
0 3 13 146.97 6.07
0 3 13 145.19 5.80
0 -3 13 140.13 5.87
0 3 14 149.36 5.61
0 3 14 146.63 5.60
0 3 14 141.58 5.86
0 -3 14 146.65 5.86
0 -3 14 143.70 5.76
0 3 14 149.42 5.62
0 3 14 153.29 5.96
0 -3 -14 149.02 5.74
0 3 14 144.33 5.53
0 -3 14 151.43 5.82
0 -3 -15 185.73 6.32
0 -3 15 186.17 6.53
0 3 15 185.36 6.70
0 3 15 179.41 6.66
0 -3 15 196.28 6.77
0 -3 15 190.86 6.68
0 3 15 201.46 6.69
0 -3 -15 196.54 6.73
0 3 -15 203.11 6.78
0 -3 15 198.16 6.62
0 -3 15 203.29 6.64
0 -3 15 203.61 6.62
0 -3 16 14.26 1.07
0 3 16 16.82 1.15
0 3 -16 16.62 1.23
0 -3 16 15.71 1.10
0 4 0 2046.66 53.47
0 4 0 2108.11 53.26
0 -4 0 2067.66 54.40
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_shelx_res_file
;
TITL GG-23 in P2(1)/n
shelx.res
created by SHELXL-2018/3 at 17:52:13 on 05-Apr-2024
CELL 1.54184 4.95281 14.05150 13.52080 90.000 95.1372 90.000
ZERR 4.00 0.00003 0.00010 0.00010 0.000 0.0006 0.000
LATT 1
SYMM 1/2 - X, 1/2 + Y, 1/2 - Z
SFAC C H BR F N O
UNIT 24 16 4 12 16 8
MERG 2
EQIV $1 -x+1/2, y-1/2, -z+1/2
HTAB N6 O10_$1
EQIV $2 -x+2, -y, -z+1
HTAB N6 N1_$2
HTAB C8 F12
HTAB C8 F12A
SADI C11 F12 C11 F12A
SADI C11 F13 C11 F13A
SADI C11 F14 C11 F14A
EADP F12 F12A F13 F13A F14 F14A
FMAP 2 53
PLAN 3
SIZE 0.040 0.040 0.210
ACTA
BOND $H
CONF
L.S. 13
TEMP -173.00
WGHT 0.021200 2.049700
FVAR 0.36829 0.51528
BR9 3 0.191843 0.359281 0.196371 11.00000 0.02440 0.01774 =
0.02471 -0.00055 -0.00423 -0.00003
PART 1
F12 4 0.884481 0.544621 0.371091 21.00000 0.02916 0.01958 =
0.02821 -0.00046 -0.00160 -0.00029
F13 4 0.529462 0.581162 0.447263 21.00000 0.02916 0.01958 =
0.02821 -0.00046 -0.00160 -0.00029
F14 4 0.652147 0.669671 0.327517 21.00000 0.02916 0.01958 =
0.02821 -0.00046 -0.00160 -0.00029
PART 2
F12A 4 0.854868 0.545289 0.401831 -21.00000 0.02916 0.01958 =
0.02821 -0.00046 -0.00160 -0.00029
F14A 4 0.706154 0.663879 0.316290 -21.00000 0.02916 0.01958 =
0.02821 -0.00046 -0.00160 -0.00029
F13A 4 0.482503 0.612143 0.436369 -21.00000 0.02916 0.01958 =
0.02821 -0.00046 -0.00160 -0.00029
PART 0
O2 6 1.207367 0.207479 0.502217 11.00000 0.02638 0.01578 =
0.03171 0.00158 -0.01047 -0.00147
O10 6 0.278144 0.572891 0.233549 11.00000 0.02776 0.01936 =
0.02612 0.00323 -0.00620 0.00310
N1 5 1.096522 0.116618 0.487742 11.00000 0.02362 0.01564 =
0.02583 0.00031 -0.00308 0.00000
N3 5 1.044165 0.274727 0.451455 11.00000 0.02630 0.01713 =
0.03079 0.00231 -0.00899 0.00085
N6 5 0.713452 0.055152 0.394729 11.00000 0.02188 0.01651 =
0.04780 0.00463 -0.01425 -0.00133
H6A 2 0.568403 0.065007 0.372886 11.00000 0.02918
H6B 2 0.747867 0.000047 0.426580 11.00000 0.03308
N7 5 0.632868 0.272982 0.350669 11.00000 0.01896 0.01469 =
0.02378 0.00057 -0.00244 0.00038
H7 2 0.524947 0.240842 0.315618 11.00000 0.02408
C4 1 0.841710 0.227748 0.408556 11.00000 0.01985 0.01665 =
0.02155 0.00088 -0.00093 0.00122
C5 1 0.870807 0.127955 0.430033 11.00000 0.01942 0.01737 =
0.02183 0.00149 -0.00048 0.00188
C8 1 0.620881 0.368879 0.346906 11.00000 0.02157 0.01661 =
0.02099 -0.00092 0.00084 0.00085
H8 2 0.747974 0.399701 0.392641 11.00000 0.01858
C9 1 0.446792 0.421863 0.286855 11.00000 0.02039 0.01663 =
0.02015 -0.00066 -0.00017 -0.00178
C10 1 0.437609 0.524566 0.285645 11.00000 0.02086 0.01786 =
0.02089 0.00147 0.00055 -0.00038
C11 1 0.629330 0.582841 0.360477 11.00000 0.02563 0.01801 =
0.02269 0.00295 -0.00259 -0.00040
HKLF 4
REM GG-23 in P2(1)/n
REM wR2 = 0.0651, GooF = S = 1.093, Restrained GooF = 1.098 for all data
REM R1 = 0.0275 for 2010 Fo > 4sig(Fo) and 0.0278 for all 2038 data
REM 159 parameters refined using 3 restraints
END
WGHT 0.0212 2.0497
REM Highest difference peak 0.725, deepest hole -0.501, 1-sigma level 0.081
Q1 1 0.5794 0.5384 0.4618 11.00000 0.05 0.72
Q2 1 0.7767 0.5434 0.4400 11.00000 0.05 0.69
Q3 1 0.4142 0.6571 0.4173 11.00000 0.05 0.59
;
_shelx_res_checksum 51741
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
Br Br9 0.19184(5) 0.35928(2) 0.19637(2) 0.02267(9) Uani d 1 . .
F F12 0.8845(8) 0.5446(3) 0.3711(3) 0.0259(3) Uani d 0.515(6) A 1
F F13 0.5295(8) 0.5812(3) 0.4473(3) 0.0259(3) Uani d 0.515(6) A 1
F F14 0.6521(9) 0.6697(4) 0.3275(4) 0.0259(3) Uani d 0.515(6) A 1
F F12A 0.8549(8) 0.5453(3) 0.4018(3) 0.0259(3) Uani d 0.485(6) A 2
F F14A 0.7062(9) 0.6639(4) 0.3163(4) 0.0259(3) Uani d 0.485(6) A 2
F F13A 0.4825(8) 0.6121(3) 0.4364(3) 0.0259(3) Uani d 0.485(6) A 2
O O2 1.2074(4) 0.20748(12) 0.50222(14) 0.0254(4) Uani d 1 . .
O O10 0.2781(4) 0.57289(12) 0.23355(13) 0.0249(4) Uani d 1 . .
N N1 1.0965(4) 0.11662(14) 0.48774(16) 0.0220(4) Uani d 1 . .
N N3 1.0442(4) 0.27473(15) 0.45145(17) 0.0254(4) Uani d 1 . .
N N6 0.7135(5) 0.05515(16) 0.3947(2) 0.0298(5) Uani d 1 . .
H H6A 0.568(7) 0.065(2) 0.373(3) 0.029(9) Uiso d 1 . .
H H6B 0.748(7) 0.000(3) 0.427(3) 0.033(9) Uiso d 1 . .
N N7 0.6329(4) 0.27298(14) 0.35067(15) 0.0194(4) Uani d 1 . .
H H7 0.525(6) 0.241(2) 0.316(2) 0.024(8) Uiso d 1 . .
C C4 0.8417(5) 0.22775(16) 0.40856(17) 0.0195(4) Uani d 1 . .
C C5 0.8708(5) 0.12796(17) 0.43003(18) 0.0197(4) Uani d 1 . .
C C8 0.6209(5) 0.36888(17) 0.34691(18) 0.0198(5) Uani d 1 . .
H H8 0.748(6) 0.400(2) 0.393(2) 0.019(7) Uiso d 1 . .
C C9 0.4468(5) 0.42186(16) 0.28686(17) 0.0192(4) Uani d 1 . .
C C10 0.4376(5) 0.52457(17) 0.28565(17) 0.0199(5) Uani d 1 . .
C C11 0.6293(5) 0.58284(17) 0.36048(18) 0.0224(5) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Br9 0.02440(14) 0.01774(14) 0.02471(14) -0.00003(9) -0.00423(9) -0.00055(9)
F12 0.0292(8) 0.0196(6) 0.0282(7) -0.0003(6) -0.0016(6) -0.0005(7)
F13 0.0292(8) 0.0196(6) 0.0282(7) -0.0003(6) -0.0016(6) -0.0005(7)
F14 0.0292(8) 0.0196(6) 0.0282(7) -0.0003(6) -0.0016(6) -0.0005(7)
F12A 0.0292(8) 0.0196(6) 0.0282(7) -0.0003(6) -0.0016(6) -0.0005(7)
F14A 0.0292(8) 0.0196(6) 0.0282(7) -0.0003(6) -0.0016(6) -0.0005(7)
F13A 0.0292(8) 0.0196(6) 0.0282(7) -0.0003(6) -0.0016(6) -0.0005(7)
O2 0.0264(9) 0.0158(8) 0.0317(9) -0.0015(7) -0.0105(7) 0.0016(7)
O10 0.0278(9) 0.0194(8) 0.0261(9) 0.0031(7) -0.0062(7) 0.0032(7)
N1 0.0236(10) 0.0156(9) 0.0258(10) 0.0000(8) -0.0031(8) 0.0003(8)
N3 0.0263(10) 0.0171(10) 0.0308(11) 0.0009(8) -0.0090(9) 0.0023(8)
N6 0.0219(11) 0.0165(10) 0.0478(14) -0.0013(8) -0.0142(10) 0.0046(10)
N7 0.0190(9) 0.0147(9) 0.0238(10) 0.0004(8) -0.0024(8) 0.0006(8)
C4 0.0198(11) 0.0166(11) 0.0216(11) 0.0012(8) -0.0009(8) 0.0009(9)
C5 0.0194(10) 0.0174(11) 0.0218(11) 0.0019(8) -0.0005(9) 0.0015(9)
C8 0.0216(11) 0.0166(11) 0.0210(11) 0.0009(9) 0.0008(9) -0.0009(9)
C9 0.0204(11) 0.0166(11) 0.0202(11) -0.0018(9) -0.0002(8) -0.0007(8)
C10 0.0209(11) 0.0179(11) 0.0209(11) -0.0004(9) 0.0006(8) 0.0015(9)
C11 0.0256(12) 0.0180(11) 0.0227(11) -0.0004(9) -0.0026(9) 0.0029(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N3 O2 N1 . . 110.46(17) ?
C5 N1 O2 . . 105.97(18) ?
C4 N3 O2 . . 105.58(19) ?
C5 N6 H6A . . 120(3) ?
C5 N6 H6B . . 114(2) ?
H6A N6 H6B . . 118(3) ?
C8 N7 C4 . . 120.3(2) ?
C8 N7 H7 . . 120(2) ?
C4 N7 H7 . . 119(2) ?
N3 C4 N7 . . 121.7(2) ?
N3 C4 C5 . . 110.3(2) ?
N7 C4 C5 . . 127.9(2) ?
N1 C5 N6 . . 123.5(2) ?
N1 C5 C4 . . 107.6(2) ?
N6 C5 C4 . . 128.7(2) ?
N7 C8 C9 . . 126.5(2) ?
N7 C8 H8 . . 114.1(18) ?
C9 C8 H8 . . 119.4(18) ?
C8 C9 C10 . . 125.1(2) ?
C8 C9 Br9 . . 118.96(18) ?
C10 C9 Br9 . . 115.99(17) ?
O10 C10 C9 . . 125.6(2) ?
O10 C10 C11 . . 114.1(2) ?
C9 C10 C11 . . 120.1(2) ?
F14 C11 F13 . . 111.9(3) ?
F12A C11 F14A . . 105.3(3) ?
F14 C11 F12 . . 107.1(3) ?
F13 C11 F12 . . 108.5(3) ?
F12A C11 F13A . . 106.8(3) ?
F14A C11 F13A . . 105.4(3) ?
F14 C11 C10 . . 109.6(3) ?
F13 C11 C10 . . 108.3(2) ?
F12A C11 C10 . . 120.7(3) ?
F14A C11 C10 . . 109.5(3) ?
F12 C11 C10 . . 111.4(3) ?
F13A C11 C10 . . 108.1(2) ?
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
Br9 C9 . 1.894(2) ?
F12 C11 . 1.369(5) ?
F13 C11 . 1.314(4) ?
F14 C11 . 1.307(5) ?
F12A C11 . 1.314(5) ?
F14A C11 . 1.356(6) ?
F13A C11 . 1.373(5) ?
O2 N3 . 1.385(3) ?
O2 N1 . 1.397(3) ?
O10 C10 . 1.217(3) ?
N1 C5 . 1.314(3) ?
N3 C4 . 1.294(3) ?
N6 C5 . 1.347(3) ?
N6 H6A . 0.76(4) ?
N6 H6B . 0.89(4) ?
N7 C8 . 1.350(3) ?
N7 C4 . 1.393(3) ?
N7 H7 . 0.82(3) ?
C4 C5 . 1.437(3) ?
C8 C9 . 1.353(3) ?
C8 H8 . 0.95(3) ?
C9 C10 . 1.444(3) ?
C10 C11 . 1.557(3) ?
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
N6 H6A O10 2_545 0.77(4) 2.14(4) 2.871(3) 159(4) yes
N6 H6B N1 3_756 0.90(4) 2.11(4) 2.995(3) 169(3) yes
N7 H7 Br9 . 0.81(3) 2.76(3) 3.127(2) 109(2) yes
C8 H8 F12 . 0.95(3) 2.17(3) 2.799(5) 123(2) yes
C8 H8 F12A . 0.95(3) 2.11(3) 2.808(5) 129(2) yes
C8 H8 N3 . 0.95(3) 2.38(3) 2.759(3) 103.3(19) 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
N3 O2 N1 C5 . . . . -0.3(3) ?
N1 O2 N3 C4 . . . . 0.5(3) ?
O2 N3 C4 N7 . . . . 179.6(2) ?
O2 N3 C4 C5 . . . . -0.5(3) ?
C8 N7 C4 N3 . . . . -7.5(4) ?
C8 N7 C4 C5 . . . . 172.6(2) ?
O2 N1 C5 N6 . . . . 176.1(2) ?
O2 N1 C5 C4 . . . . 0.0(3) ?
N3 C4 C5 N1 . . . . 0.4(3) ?
N7 C4 C5 N1 . . . . -179.7(2) ?
N3 C4 C5 N6 . . . . -175.5(3) ?
N7 C4 C5 N6 . . . . 4.4(4) ?
C4 N7 C8 C9 . . . . 173.0(2) ?
N7 C8 C9 C10 . . . . 179.2(2) ?
N7 C8 C9 Br9 . . . . -0.7(4) ?
C8 C9 C10 O10 . . . . -178.3(2) ?
Br9 C9 C10 O10 . . . . 1.6(3) ?
C8 C9 C10 C11 . . . . -2.8(4) ?
Br9 C9 C10 C11 . . . . 177.15(17) ?
O10 C10 C11 F14 . . . . -24.2(4) ?
C9 C10 C11 F14 . . . . 159.8(3) ?
O10 C10 C11 F13 . . . . 98.1(3) ?
C9 C10 C11 F13 . . . . -77.9(3) ?
O10 C10 C11 F12A . . . . -161.5(3) ?
C9 C10 C11 F12A . . . . 22.5(4) ?
O10 C10 C11 F14A . . . . -39.1(4) ?
C9 C10 C11 F14A . . . . 144.9(3) ?
O10 C10 C11 F12 . . . . -142.7(3) ?
C9 C10 C11 F12 . . . . 41.4(3) ?
O10 C10 C11 F13A . . . . 75.2(3) ?
C9 C10 C11 F13A . . . . -100.8(3) ?