#------------------------------------------------------------------------------
#$Date: 2021-02-19 08:01:46 +0200 (Fri, 19 Feb 2021) $
#$Revision: 262087 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/23/2022327.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_2022327
loop_
_publ_author_name
'Medviediev, Volodymyr'
'Daszkiewicz, Marek'
_publ_section_title
;
Structural and theoretical analysis of 2-chloro-4-nitroaniline and
2-methyl-6-nitroaniline salts
;
_journal_coeditor_code DV3005
_journal_issue 3
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi 10.1107/S2053229621001455
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac 'C7 H9 N2 O2 +, Br -'
_chemical_formula_moiety 'C7 H9 N2 O2 +, Br -'
_chemical_formula_sum 'C7 H9 Br N2 O2'
_chemical_formula_weight 233.07
_chemical_name_systematic
;
2-Methyl-6-nitroanilinium bromide
;
_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
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha 76.646(3)
_cell_angle_beta 73.897(2)
_cell_angle_gamma 76.045(2)
_cell_formula_units_Z 2
_cell_length_a 6.8920(2)
_cell_length_b 7.7281(3)
_cell_length_c 8.9210(2)
_cell_measurement_reflns_used 6602
_cell_measurement_temperature 295.0(10)
_cell_measurement_theta_max 29.1490
_cell_measurement_theta_min 2.8080
_cell_volume 436.12(2)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2008) and OLEX2 (Dolomanov et al.,
2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 295.0(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Rigaku Xcalibur Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0273
_diffrn_reflns_av_unetI/netI 0.0187
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 15285
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.980
_diffrn_reflns_theta_min 3.133
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 4.673
_exptl_absorpt_correction_T_max 0.973
_exptl_absorpt_correction_T_min 0.947
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
{CrysAlis PRO (Rigaku OD, 2015), based on expressions derived by
Clark & Reid (1995)]
;
_exptl_crystal_colour 'clear yellowish colourless'
_exptl_crystal_density_diffrn 1.775
_exptl_crystal_description block
_exptl_crystal_F_000 232
_exptl_crystal_size_max 0.461
_exptl_crystal_size_mid 0.334
_exptl_crystal_size_min 0.184
_refine_diff_density_max 0.331
_refine_diff_density_min -0.387
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.109
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 122
_refine_ls_number_reflns 2299
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.109
_refine_ls_R_factor_all 0.0342
_refine_ls_R_factor_gt 0.0262
_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^)+(0.0284P)^2^+0.0941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0585
_refine_ls_wR_factor_ref 0.0608
_reflns_number_gt 1986
_reflns_number_total 2299
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file dv3005sup1.cif
_cod_data_source_block 3
_cod_database_code 2022327
_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 -2 25.36 2.16
0 0 -2 27.61 2.02
0 0 2 26.22 1.27
0 0 2 25.97 1.97
0 0 -2 26.55 1.87
0 0 -2 24.97 1.89
0 0 2 25.64 1.94
0 0 2 24.73 1.67
0 0 -2 24.38 1.17
0 0 2 28.77 2.29
0 0 2 26.32 1.92
0 0 -2 23.49 1.64
0 0 -2 26.04 2.00
0 0 2 25.80 1.96
0 0 -2 24.44 2.02
0 0 2 25.20 1.95
0 0 -3 3570.11 52.71
0 0 3 3354.32 54.04
0 0 -3 3454.15 53.95
0 0 -3 3495.30 54.32
0 0 -3 3395.78 53.87
0 0 3 3597.55 52.62
0 0 -3 3468.21 55.08
0 0 3 3364.82 53.28
0 0 -3 3397.31 53.60
0 0 -3 3390.08 53.50
0 0 3 3325.19 54.82
0 0 -3 3494.62 49.93
0 0 -3 3379.02 53.14
0 0 -3 3146.31 48.97
0 0 3 3484.19 54.05
0 0 3 3398.44 54.13
0 0 3 3388.90 53.24
0 0 -3 3368.36 53.87
0 0 3 3472.61 50.33
0 0 4 64.84 4.40
0 0 -4 63.49 4.43
0 0 -4 53.33 3.47
0 0 4 52.30 4.42
0 0 4 59.29 3.59
0 0 -4 60.89 4.37
0 0 -4 51.27 3.80
0 0 -4 57.79 4.51
0 0 -4 58.06 4.14
0 0 4 58.45 4.03
0 0 -4 51.93 3.83
0 0 -4 52.06 3.75
0 0 -4 56.79 4.01
0 0 4 55.23 3.81
0 0 -4 55.28 3.76
0 0 -4 57.80 1.97
0 0 4 56.08 2.70
0 0 -4 58.77 2.48
0 0 5 15.38 2.46
0 0 -5 17.92 2.83
0 0 -5 12.58 2.42
0 0 -5 12.22 2.66
0 0 -5 12.09 0.92
0 0 5 11.13 2.73
0 0 5 17.03 2.73
0 0 -5 14.35 2.62
0 0 -5 15.36 2.57
0 0 -5 12.05 2.69
0 0 -5 15.51 2.54
0 0 -5 14.22 2.49
0 0 5 11.62 2.39
0 0 -5 15.95 2.62
0 0 -5 13.00 1.40
0 0 -5 14.25 2.62
0 0 -5 10.82 2.01
0 0 5 22.67 3.44
0 0 6 754.04 19.71
0 0 6 744.24 22.06
0 0 6 774.12 18.95
0 0 -6 780.08 19.66
0 0 -6 778.85 14.58
0 0 -6 758.67 21.31
0 0 -6 739.75 20.44
0 0 6 764.28 20.80
0 0 -6 782.13 19.22
0 0 6 732.14 20.08
0 0 7 510.13 19.20
0 0 7 513.94 17.64
0 0 7 492.46 17.02
0 0 7 512.28 15.69
0 0 -7 528.50 18.49
0 0 7 513.49 16.44
0 0 -7 509.28 10.98
0 0 8 4.41 3.54
0 0 8 3.25 3.83
0 0 -8 -0.21 3.61
0 0 8 3.15 2.47
0 0 8 5.79 3.23
0 0 -8 4.24 1.17
0 0 9 11.32 3.52
0 0 9 20.50 3.90
0 0 9 11.42 4.44
0 0 -9 19.34 5.03
0 0 9 23.76 5.32
0 0 -10 71.85 9.15
0 0 10 65.31 7.17
0 0 10 71.88 7.28
0 0 10 69.91 8.19
0 0 10 84.91 10.18
0 0 11 11.69 4.38
0 0 11 13.54 5.40
0 0 11 10.80 4.29
0 0 -11 11.24 4.48
0 0 -11 13.33 5.79
0 1 -11 5.70 4.87
0 -1 11 1.47 3.31
0 1 -11 6.33 4.51
0 -1 10 62.96 8.06
0 1 -10 71.60 7.77
0 -1 10 81.68 7.75
0 1 -10 74.94 9.27
0 -1 10 67.22 6.97
0 -1 9 94.18 7.53
0 1 -9 105.87 8.80
0 -1 9 87.71 7.37
0 1 -9 78.99 8.64
0 -1 9 103.64 9.34
0 -1 8 57.15 6.58
0 -1 8 49.74 7.06
0 -1 8 51.35 5.32
0 1 -8 54.24 3.80
0 1 -8 54.51 6.78
0 -1 8 58.51 5.71
0 1 -7 164.67 6.46
0 1 -7 173.89 5.56
0 1 -7 179.64 10.38
0 -1 7 165.62 9.91
0 -1 7 180.20 8.91
0 -1 7 174.19 8.76
0 -1 7 150.99 10.53
0 -1 6 530.54 15.13
0 1 -6 520.55 15.94
0 1 -6 531.44 17.18
0 1 -6 541.40 11.72
0 -1 6 508.61 18.17
0 1 -6 526.51 12.67
0 -1 6 548.45 17.39
0 -1 6 542.62 15.28
0 1 -5 143.44 5.18
0 1 -5 145.59 7.58
0 1 -5 139.91 7.55
0 1 -5 151.19 5.67
0 -1 5 148.07 6.73
0 -1 5 142.72 7.91
0 -1 5 150.71 7.59
0 1 -5 146.03 7.91
0 1 -5 156.24 7.23
0 1 -5 153.20 7.40
0 1 -5 146.45 6.66
0 -1 5 142.89 8.31
0 -1 5 147.09 6.63
0 -1 5 132.21 7.45
0 1 -4 128.83 6.46
0 1 -4 119.55 4.84
0 1 -4 127.09 6.47
0 1 -4 128.75 6.60
0 1 -4 127.58 6.07
0 1 -4 121.27 6.32
0 -1 4 109.78 6.25
0 1 -4 131.10 5.57
0 -1 4 128.68 6.48
0 -1 4 123.96 6.89
0 1 -4 125.57 5.61
0 -1 4 126.83 5.60
0 -1 4 133.57 5.60
0 1 -4 124.98 4.70
0 1 -4 117.31 5.82
0 1 -4 118.55 6.21
0 1 -4 125.39 6.97
0 1 -4 124.61 6.18
0 -1 4 122.33 6.08
0 1 -3 2423.05 39.59
0 -1 3 2419.14 42.04
0 1 -3 2450.63 40.80
0 -1 3 2505.84 41.63
0 -1 3 2431.97 40.68
0 1 -3 2415.15 41.76
0 1 -3 2458.57 40.36
0 1 -3 2477.60 41.96
0 1 -3 2453.52 39.41
0 -1 3 2412.42 39.02
0 1 -3 2436.39 41.46
0 1 -3 2318.54 38.92
0 -1 3 2491.09 40.59
0 1 -3 2504.16 42.76
0 1 -3 2468.32 40.76
0 1 -3 2449.42 41.26
0 1 -3 2451.35 38.92
0 -1 3 2465.78 42.54
0 -1 3 2438.92 41.71
0 -1 3 2510.73 39.85
0 1 -3 2443.82 41.59
0 1 -2 3676.84 55.51
0 1 -2 3491.90 56.83
0 1 -2 3556.85 55.63
0 1 -2 3716.02 57.35
0 -1 2 3822.40 57.69
0 -1 2 3736.08 57.00
0 -1 2 3604.81 54.59
0 -1 2 3544.43 56.92
0 -1 2 3697.83 56.81
0 -1 2 3628.27 57.20
0 1 -2 3670.33 54.80
0 1 -2 3651.05 55.76
0 -1 2 3608.88 55.75
0 -1 2 3747.47 57.70
0 -1 2 3628.89 56.25
0 1 -2 3887.42 57.92
0 1 -2 3609.66 56.69
0 1 -2 3689.90 56.88
0 1 -2 3647.46 56.26
0 -1 2 3714.88 55.63
0 1 -2 3860.64 57.79
0 1 -1 13.12 1.30
0 1 -1 13.11 0.94
0 -1 1 15.58 1.57
0 1 -1 15.17 1.30
0 -1 1 14.69 1.52
0 1 -1 13.38 1.31
0 1 -1 12.18 1.39
0 1 -1 13.13 1.41
0 -1 1 11.42 1.23
0 -1 1 13.54 1.14
0 1 -1 13.46 1.39
0 1 -1 13.10 1.27
0 -1 1 13.45 1.37
0 1 -1 14.07 1.18
0 -1 1 16.27 1.57
0 1 -1 11.11 1.40
0 1 -1 11.54 1.43
0 1 -1 13.01 1.41
0 -1 1 13.58 1.46
0 1 -1 10.18 1.22
0 1 0 0.93 0.66
0 -1 0 10.53 1.09
0 -1 -1 2444.82 37.40
0 1 1 2404.56 38.57
0 -1 -1 2567.92 39.21
0 -1 -1 2537.53 38.71
0 -1 -1 2485.47 38.83
0 1 1 2565.91 39.18
0 1 2 1195.07 21.15
0 1 2 1178.02 18.97
0 1 2 1235.12 20.84
0 1 2 1184.03 21.65
0 -1 -2 1191.31 21.52
0 1 2 1151.17 20.58
0 1 2 1151.18 21.40
0 -1 -2 1181.84 20.51
0 -1 -2 1219.09 20.89
0 -1 -2 1200.91 21.70
0 -1 -3 1758.90 31.90
0 1 3 1742.18 31.67
0 1 3 1791.75 26.93
0 -1 -3 1807.93 31.76
0 1 3 1733.60 28.96
0 1 3 1783.66 31.38
0 1 3 1780.51 31.82
0 -1 -3 1780.20 31.16
0 -1 -3 1807.68 30.53
0 1 3 1809.55 31.32
0 -1 -3 1809.02 31.44
0 -1 -3 1783.80 31.98
0 -1 -3 1748.00 28.81
0 1 3 1853.43 30.56
0 -1 -4 2724.68 47.24
0 -1 -4 2810.70 45.48
0 -1 -4 2670.86 43.70
0 1 4 2702.77 47.11
0 1 4 2719.93 40.40
0 -1 -4 2660.99 47.27
0 1 4 2806.80 45.37
0 -1 -4 2788.16 47.70
0 -1 -4 2722.38 46.83
0 1 4 2742.96 46.94
0 1 4 2691.67 47.26
0 1 4 2636.54 44.06
0 -1 -4 2761.86 46.93
0 1 4 2808.44 46.75
0 -1 -5 384.26 13.06
0 -1 -5 373.39 11.39
0 -1 -5 378.88 10.59
0 -1 -5 383.79 11.57
0 1 5 350.29 12.34
0 1 5 350.04 7.41
0 1 5 358.57 12.15
0 -1 -5 398.72 12.81
0 1 5 366.59 12.27
0 -1 -5 380.64 12.74
0 -1 -5 371.87 12.54
0 1 5 373.54 11.30
0 1 5 363.76 10.87
0 1 5 349.64 12.64
0 -1 -5 365.22 12.76
0 -1 -6 139.22 6.80
0 -1 -6 133.38 7.32
0 1 6 127.01 8.17
0 1 6 128.51 4.04
0 1 6 135.45 7.92
0 1 6 138.97 7.11
0 -1 -6 154.67 8.95
0 1 6 134.72 7.86
0 1 6 142.55 7.22
0 -1 -7 180.98 10.66
0 -1 -7 182.44 8.50
0 1 7 176.28 9.69
0 1 7 185.75 10.04
0 1 7 167.28 10.42
0 1 7 164.60 8.68
0 1 7 184.30 9.00
0 1 8 282.89 12.73
0 1 8 273.40 11.96
0 -1 -8 263.65 14.10
0 1 8 272.43 12.99
0 1 8 293.54 13.86
0 1 8 277.45 14.60
0 1 9 9.59 4.49
0 -1 -9 5.07 3.97
0 1 9 1.34 3.39
0 1 9 5.76 3.53
0 1 9 4.16 3.34
0 1 10 57.20 7.90
0 -1 -10 63.54 8.94
0 1 10 61.53 8.51
0 1 10 65.82 7.55
0 1 10 59.62 6.84
0 1 11 24.32 5.72
0 -1 -11 29.26 6.89
0 1 11 28.43 5.31
0 1 11 29.85 6.01
0 1 12 -0.88 3.56
0 1 12 6.81 4.89
0 2 -11 5.86 4.89
0 2 -11 16.90 5.72
0 2 -10 13.16 5.04
0 -2 10 1.29 4.33
0 2 -10 8.36 4.34
0 -2 10 4.97 3.38
0 -2 9 186.64 12.81
0 -2 9 168.48 10.35
0 2 -9 160.34 11.98
0 2 -9 182.73 12.20
0 -2 9 190.15 10.38
0 -2 8 68.47 5.91
0 2 -8 59.86 7.01
0 2 -8 71.45 7.38
0 -2 8 68.43 6.41
0 -2 8 71.93 7.78
0 2 -8 58.78 4.63
0 2 -7 -1.31 2.74
0 -2 7 -2.50 3.51
0 2 -7 1.11 1.48
0 2 -7 0.12 1.66
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0 2 -7 2.98 2.58
0 -2 7 0.16 1.92
0 -2 6 507.59 18.70
0 -2 6 514.27 16.84
0 2 -6 501.35 14.08
0 2 -6 555.64 17.69
0 -2 6 528.60 14.66
0 2 -6 493.29 15.14
0 2 -6 516.76 13.82
0 -2 6 540.80 18.06
0 2 -6 507.04 16.79
0 -2 6 517.36 15.57
0 -2 5 1262.12 30.12
0 2 -5 1286.58 27.10
0 2 -5 1321.68 28.85
0 2 -5 1201.71 25.25
0 -2 5 1268.37 26.43
0 2 -5 1222.68 25.08
0 2 -5 1236.43 27.51
0 -2 5 1280.02 28.99
0 -2 5 1275.68 24.92
0 2 -5 1189.97 25.20
0 -2 5 1252.95 27.34
0 2 -5 1205.02 25.86
0 -2 4 386.59 10.22
0 2 -4 377.79 11.18
0 2 -4 391.46 13.65
0 2 -4 399.64 11.69
0 2 -4 387.31 12.16
0 -2 4 376.54 13.31
0 -2 4 393.78 11.63
0 -2 4 377.75 11.67
0 2 -4 374.11 11.27
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0 2 -4 383.37 11.70
0 2 -4 397.39 12.95
0 2 -4 392.10 12.64
0 2 -4 403.98 13.30
0 2 -4 368.16 11.19
0 2 -4 393.69 13.31
0 2 -4 368.37 10.29
0 2 -4 389.87 12.87
0 2 -3 1176.68 25.51
0 2 -3 1233.71 23.43
0 2 -3 1202.26 21.77
0 2 -3 1223.03 25.54
0 -2 3 1197.62 25.61
0 -2 3 1226.82 23.75
0 2 -3 1242.19 24.37
0 2 -3 1200.79 24.91
0 -2 3 1199.82 24.89
0 2 -3 1232.76 25.58
0 -2 3 1189.80 25.66
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0 -2 3 1219.01 25.40
0 -2 3 1225.06 23.50
0 -2 3 1184.19 24.12
0 2 -2 1563.48 29.63
0 -2 2 1518.28 28.35
0 2 -2 1576.66 29.06
0 2 -2 1536.98 27.58
0 2 -2 1579.03 29.00
0 -2 2 1552.31 29.25
0 2 -2 1545.46 28.93
0 2 -2 1566.15 28.02
0 -2 2 1532.98 26.75
0 -2 2 1471.46 27.65
0 2 -2 1565.11 29.30
0 2 -2 1529.49 25.35
0 2 -2 1521.16 29.68
0 2 -2 1593.07 28.65
0 -2 2 1544.36 29.18
0 2 -2 1553.82 29.26
0 2 -2 1546.22 27.98
0 2 -2 1587.80 27.12
0 2 -1 1002.43 19.28
0 -2 1 950.90 18.98
0 2 -1 998.89 20.30
0 -2 1 974.90 20.22
0 2 -1 972.56 20.56
0 2 -1 985.73 19.48
0 2 -1 968.03 18.79
0 -2 1 962.33 20.37
0 -2 1 956.19 19.60
0 -2 1 997.42 19.48
0 2 -1 992.55 19.93
0 2 -1 977.54 20.30
0 2 -1 965.65 17.96
0 -2 1 1056.41 18.41
0 2 -1 1018.93 19.38
0 -2 1 976.26 18.98
0 -2 0 131.54 5.08
0 -2 0 145.24 5.40
0 -2 0 125.00 5.98
0 2 0 126.75 5.76
0 -2 0 138.84 6.46
0 -2 0 120.12 5.78
0 2 0 132.37 4.81
0 -2 0 126.89 5.77
0 2 0 134.28 4.85
0 -2 0 126.33 5.86
0 -2 0 134.34 4.94
0 2 0 138.42 5.38
0 2 1 4551.15 68.92
0 2 1 4454.15 68.14
0 -2 -1 4492.64 66.81
0 -2 -1 4455.97 68.35
0 -2 -1 4405.70 69.07
0 -2 -1 4415.56 68.82
0 -2 -2 2710.26 42.71
0 2 2 2762.76 42.62
0 2 2 2728.49 45.11
0 2 2 2741.00 45.96
0 2 2 2747.33 45.35
0 -2 -2 2705.62 45.12
0 -2 -2 2835.70 46.00
0 2 3 502.95 13.01
0 -2 -3 521.40 13.74
0 2 3 504.72 13.54
0 -2 -3 522.66 14.12
0 -2 -3 525.67 13.24
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-7 -6 -3 116.15 12.32
-7 -6 -3 131.37 12.46
7 6 3 121.42 10.21
-7 -6 -4 42.36 8.52
-7 -6 -4 37.97 8.09
7 6 4 26.65 5.61
7 6 5 26.41 4.52
-7 -6 -5 38.59 7.87
7 6 5 24.61 4.91
-7 -6 -5 46.33 8.83
7 6 6 66.67 6.82
7 6 6 67.32 11.47
7 6 6 60.68 6.85
-7 -6 -6 77.32 10.75
7 6 7 2.09 3.04
7 6 7 2.64 5.41
7 6 7 7.84 3.70
7 6 7 7.36 5.65
7 6 7 -4.97 5.30
-7 -6 -7 6.00 5.56
7 6 8 14.08 4.33
-7 -6 -8 9.82 5.83
7 6 8 2.61 5.63
7 6 8 -1.23 5.73
7 6 8 9.83 4.78
-7 -6 -8 12.07 6.84
7 6 9 17.65 4.96
-7 -6 -9 21.50 7.41
7 6 9 6.88 5.50
-7 -6 -9 15.11 6.68
-7 -7 2 -3.93 5.67
-7 -7 1 29.41 7.20
-7 -7 0 48.93 8.99
-7 -7 0 40.33 7.78
7 7 0 49.44 8.13
-7 -7 -1 5.30 5.10
7 7 1 16.02 5.62
-7 -7 -2 5.81 6.06
-7 -7 -2 9.11 5.77
7 7 2 -3.90 4.33
-7 -7 -3 54.64 9.27
-7 -7 -3 82.34 10.68
7 7 3 73.24 8.67
-7 -7 -4 0.66 5.71
-7 -7 -4 -6.34 6.46
7 7 4 3.15 4.02
-7 -7 -5 4.41 5.54
7 7 5 -0.74 3.48
-7 -7 -5 -0.28 5.53
7 7 6 52.68 6.55
7 7 6 40.17 9.83
7 7 6 42.22 6.39
7 7 6 53.78 9.78
-7 -7 -6 68.72 10.93
7 7 7 5.99 3.64
7 7 7 11.97 5.56
7 7 7 4.71 3.66
7 7 7 7.25 6.07
-7 -7 -7 7.43 6.03
7 7 8 -3.83 4.29
7 7 9 -2.63 4.24
-7 -8 0 71.96 10.36
-7 -8 -1 0.14 5.26
-7 -8 -2 30.80 7.64
7 8 2 31.46 7.23
-7 -8 -3 7.93 6.45
-7 -8 -3 10.86 5.98
7 8 3 3.56 4.29
-7 -8 -4 18.78 7.06
-7 -8 -4 25.33 8.07
7 8 4 16.61 5.05
-7 -8 -5 -8.34 5.69
7 8 5 -1.44 4.30
-7 -8 -6 -1.53 5.58
7 8 6 -0.35 6.07
7 8 6 -0.67 4.03
7 8 7 1.55 3.53
7 8 8 1.86 4.21
7 9 5 -6.44 5.29
7 9 6 6.87 4.81
-8 3 1 10.98 5.20
8 -3 -1 13.43 6.14
8 -3 0 8.90 7.12
8 -3 0 0.74 5.59
8 -3 1 22.59 8.15
8 -3 1 27.24 7.61
8 -3 2 43.18 9.10
8 -3 2 37.46 8.00
8 -3 3 -0.17 4.54
8 -3 3 16.20 7.06
8 -3 4 25.52 7.36
8 -3 4 38.59 9.04
8 -3 5 31.75 6.12
-8 2 2 9.11 4.21
8 -2 -2 8.50 6.19
8 -2 -2 1.38 4.85
-8 2 1 34.19 6.37
8 -2 -1 32.55 8.71
8 -2 -1 45.30 8.32
-8 2 0 7.43 3.87
8 -2 0 13.59 5.80
8 -2 0 8.59 5.37
-8 2 -1 11.58 4.57
8 -2 1 9.17 6.07
8 -2 1 15.64 5.97
8 -2 1 -0.71 4.55
-8 2 -2 56.95 8.26
8 -2 2 64.75 9.76
8 -2 2 63.15 8.64
8 -2 2 69.88 10.72
-8 2 -3 32.10 6.44
8 -2 3 23.55 6.73
8 -2 3 28.33 6.34
8 -2 3 39.50 8.00
8 -2 3 39.46 5.95
8 -2 4 3.59 5.10
8 -2 4 -3.80 5.29
8 -2 4 3.38 4.52
8 -2 4 -0.57 3.31
-8 2 -5 50.25 7.05
8 -2 5 45.54 7.65
8 -2 5 49.24 8.69
8 -2 5 43.37 6.65
-8 2 -6 41.71 6.90
8 -2 6 33.06 7.45
8 -2 6 30.58 7.14
8 -2 6 23.51 5.82
-8 1 3 30.40 6.19
8 -1 -3 24.90 6.00
-8 1 2 1.53 3.49
-8 1 2 4.34 4.01
8 -1 -2 5.94 3.52
-8 1 1 17.60 4.99
8 -1 -1 26.50 5.30
8 -1 -1 25.31 7.13
8 -1 -1 25.75 6.66
-8 1 0 28.74 5.80
8 -1 0 25.42 7.60
8 -1 0 33.18 6.75
-8 1 -1 17.16 4.92
8 -1 1 23.23 7.38
8 -1 1 14.21 5.79
8 -1 1 16.75 5.21
-8 1 -2 20.55 5.12
8 -1 2 23.02 5.23
8 -1 2 27.51 6.28
8 -1 2 26.43 5.70
8 -1 2 27.29 6.82
8 -1 2 24.76 4.66
-8 1 -3 80.01 8.95
8 -1 3 96.49 8.60
8 -1 3 84.45 9.04
8 -1 3 78.47 9.74
8 -1 3 87.78 8.12
8 -1 3 94.97 11.34
-8 1 -4 82.83 9.42
8 -1 4 102.64 11.94
8 -1 4 89.95 8.34
8 -1 4 72.06 8.45
8 -1 4 85.46 10.05
8 -1 4 106.52 9.36
-8 1 -5 47.20 7.29
8 -1 5 38.82 6.20
8 -1 5 34.86 6.22
8 -1 5 38.91 7.39
8 -1 5 41.17 6.76
8 -1 5 31.94 7.03
8 -1 6 112.48 10.05
8 -1 6 104.14 12.50
8 -1 6 106.42 10.50
8 -1 6 110.02 10.48
8 -1 6 89.68 10.26
8 -1 7 17.14 7.17
8 -1 7 19.82 5.34
-8 1 -7 9.59 6.22
8 -1 7 12.97 4.77
8 -1 7 23.25 6.19
8 -1 8 0.19 3.82
8 -1 8 0.17 4.22
-8 0 3 19.36 5.89
8 0 -3 9.35 5.00
-8 0 2 11.20 4.34
-8 0 2 11.92 4.33
-8 0 1 -0.10 3.60
-8 0 1 4.99 3.72
8 0 -1 1.14 5.00
-8 0 0 73.36 8.21
8 0 0 76.69 10.12
-8 0 0 97.97 8.40
-8 0 -1 18.44 4.97
-8 0 -1 12.51 3.74
8 0 1 7.49 5.07
8 0 1 7.12 3.38
8 0 1 18.29 4.19
8 0 2 5.11 4.73
-8 0 -2 -1.26 3.82
8 0 2 9.01 4.59
8 0 2 2.67 4.34
8 0 2 4.78 3.21
8 0 2 2.89 3.34
-8 0 -3 80.03 8.69
8 0 3 94.97 9.16
8 0 3 98.99 11.59
8 0 3 93.13 8.40
8 0 3 79.08 8.61
8 0 3 94.11 8.30
-8 0 -4 58.16 7.72
8 0 4 53.16 7.01
8 0 4 41.94 5.87
8 0 4 46.44 8.71
8 0 4 43.66 6.73
8 0 4 52.40 6.81
-8 0 -5 46.00 7.04
8 0 5 37.31 8.08
8 0 5 43.97 6.58
8 0 5 45.60 6.35
8 0 5 41.29 6.49
8 0 5 49.86 7.02
-8 0 -6 31.62 6.38
8 0 6 37.39 6.64
8 0 6 47.16 9.16
8 0 6 34.66 5.69
8 0 6 22.58 5.37
8 0 6 41.73 6.86
-8 0 -7 79.57 9.24
8 0 7 78.49 9.13
8 0 7 97.40 12.21
-8 0 -7 79.89 10.46
8 0 7 82.96 8.71
8 0 7 77.83 8.61
8 0 7 73.50 9.19
8 0 8 26.08 8.27
8 0 8 22.46 5.62
-8 0 -8 11.24 5.43
8 0 8 13.40 5.01
8 0 8 17.38 5.37
8 0 9 15.14 5.56
-8 -1 3 22.72 6.03
-8 -1 2 42.92 6.77
-8 -1 2 36.46 6.80
8 1 -2 28.25 6.04
-8 -1 1 14.52 4.94
-8 -1 1 6.37 3.83
8 1 -1 6.46 3.98
8 1 -1 11.03 5.00
-8 -1 0 81.75 8.45
-8 -1 0 69.64 7.75
8 1 0 75.17 8.66
8 1 0 75.80 9.08
8 1 0 75.24 6.98
-8 -1 -1 66.71 7.81
-8 -1 -1 66.83 7.04
8 1 1 75.26 8.75
8 1 1 80.75 8.70
8 1 1 63.49 6.61
-8 -1 -2 45.57 5.88
-8 -1 -2 45.18 6.78
8 1 2 38.55 6.07
8 1 2 43.44 6.23
-8 -1 -3 33.77 5.11
-8 -1 -3 31.96 5.73
8 1 3 28.10 6.24
8 1 3 29.04 7.07
8 1 3 41.27 5.82
8 1 3 30.07 5.37
-8 -1 -4 35.75 6.47
8 1 4 40.60 7.95
8 1 4 42.83 6.94
8 1 4 33.77 4.88
8 1 4 41.22 5.57
8 1 4 41.17 6.20
-8 -1 -5 98.21 9.58
8 1 5 94.87 9.96
8 1 5 98.62 11.43
8 1 5 85.19 7.67
8 1 5 93.02 7.64
8 1 5 99.28 9.44
-8 -1 -6 2.87 3.93
8 1 6 8.18 4.76
-8 -1 -6 -6.19 5.61
8 1 6 -0.88 3.15
8 1 6 0.90 5.47
8 1 6 3.50 2.93
8 1 6 8.66 4.38
-8 -1 -7 56.55 7.81
8 1 7 55.21 8.10
8 1 7 48.99 7.57
-8 -1 -7 49.12 8.20
8 1 7 57.04 9.31
8 1 7 64.68 7.24
8 1 7 61.47 7.05
8 1 7 51.55 7.73
-8 -1 -8 58.34 8.20
8 1 8 54.91 9.61
8 1 8 71.78 8.92
8 1 8 66.23 8.81
-8 -1 -8 58.32 8.79
8 1 8 69.51 7.87
-8 -1 -9 -3.87 4.33
-8 -2 2 43.06 7.39
8 2 -2 44.47 6.99
-8 -2 1 37.68 6.19
-8 -2 1 23.40 5.67
8 2 -1 27.25 5.80
-8 -2 0 37.64 6.34
-8 -2 0 40.06 6.58
8 2 0 35.87 6.49
8 2 1 139.80 11.16
-8 -2 -1 131.95 10.41
8 2 1 140.44 10.22
-8 -2 -1 120.72 10.10
-8 -2 -2 66.74 7.39
-8 -2 -2 70.86 7.78
8 2 2 71.27 7.85
8 2 2 59.02 7.09
-8 -2 -3 29.73 5.29
-8 -2 -3 18.60 4.85
8 2 3 22.50 4.71
8 2 3 27.12 5.58
8 2 4 123.09 11.89
8 2 4 89.48 10.36
8 2 4 86.78 8.42
-8 -2 -4 114.04 9.12
8 2 4 93.74 9.12
-8 -2 -4 118.43 10.11
-8 -2 -5 85.69 9.13
8 2 5 74.72 7.62
8 2 5 110.96 11.34
-8 -2 -5 92.06 8.25
8 2 5 87.26 10.39
8 2 5 105.15 9.95
8 2 6 17.72 5.55
-8 -2 -6 33.42 6.41
8 2 6 22.03 4.88
8 2 6 25.43 6.28
8 2 6 25.44 6.10
-8 -2 -7 1.71 3.81
8 2 7 -2.83 3.98
8 2 7 -2.31 4.17
-8 -2 -7 1.82 3.72
8 2 7 1.47 4.66
8 2 7 -5.19 5.04
8 2 7 -0.68 4.15
-8 -2 -8 78.64 8.74
8 2 8 72.92 8.74
8 2 8 84.10 10.29
-8 -2 -8 80.69 9.51
-8 -2 -9 26.20 6.60
-8 -3 2 21.83 6.15
8 3 -2 5.95 4.86
-8 -3 1 34.23 6.59
8 3 -1 39.08 6.63
-8 -3 0 2.07 4.05
8 3 0 0.02 4.20
-8 -3 -1 5.65 4.20
-8 -3 -1 -2.70 4.04
8 3 1 0.70 4.32
8 3 2 86.56 8.80
-8 -3 -2 108.25 9.96
-8 -3 -2 104.86 9.55
-8 -3 -3 61.78 7.54
-8 -3 -3 70.43 8.28
8 3 3 57.18 7.25
8 3 3 62.50 7.95
-8 -3 -4 0.17 3.15
-8 -3 -4 6.60 4.72
8 3 4 5.27 3.39
8 3 4 8.74 5.61
8 3 4 9.70 4.56
8 3 4 3.50 3.95
8 3 4 6.04 4.70
-8 -3 -5 66.30 7.94
-8 -3 -5 70.07 8.22
8 3 5 65.46 9.01
8 3 5 57.63 6.40
8 3 5 63.61 9.70
8 3 5 62.99 7.33
8 3 5 40.33 6.79
-8 -3 -6 74.79 8.29
-8 -3 -6 69.91 8.23
8 3 6 63.84 7.29
8 3 6 59.80 8.72
8 3 6 70.33 9.96
8 3 6 71.31 8.81
-8 -3 -7 3.95 3.95
8 3 7 1.75 3.59
8 3 7 5.68 5.48
8 3 7 -0.66 5.37
8 3 7 5.88 5.23
-8 -3 -7 5.70 3.88
-8 -3 -8 -2.18 3.58
8 3 8 2.64 3.39
8 3 8 2.50 4.81
8 3 8 2.31 4.78
8 3 8 5.31 5.07
-8 -3 -9 61.61 8.56
8 3 9 57.55 8.24
-8 -4 1 55.01 8.67
8 4 -1 55.07 7.76
-8 -4 0 51.46 8.11
8 4 0 45.25 7.04
-8 -4 -1 6.99 4.44
8 4 1 3.84 4.17
-8 -4 -2 31.89 6.38
8 4 2 28.37 5.59
-8 -4 -3 85.17 9.46
-8 -4 -3 88.91 9.29
8 4 3 83.13 8.67
-8 -4 -4 8.64 3.87
-8 -4 -4 22.00 5.34
8 4 4 16.87 4.90
-8 -4 -5 -1.24 3.97
-8 -4 -5 6.97 4.84
8 4 5 2.11 2.67
8 4 5 -2.21 5.64
8 4 5 1.37 3.69
8 4 5 3.02 4.33
8 4 5 7.07 4.51
-8 -4 -6 90.54 9.76
-8 -4 -6 99.02 9.68
8 4 6 101.26 8.77
8 4 6 102.00 12.48
8 4 6 92.29 8.67
8 4 6 103.76 10.81
-8 -4 -7 1.86 3.93
8 4 7 6.73 4.13
8 4 7 11.66 6.35
8 4 7 2.85 3.10
8 4 7 -7.95 6.44
8 4 7 -2.92 4.94
-8 -4 -7 6.13 4.80
-8 -4 -8 1.25 4.17
8 4 8 1.80 3.53
8 4 8 -0.57 5.69
-8 -4 -8 0.24 4.24
-8 -4 -9 19.09 5.75
8 4 9 17.59 5.53
8 4 9 16.11 6.80
-8 -4 -9 24.44 6.50
-8 -5 0 29.44 6.90
8 5 0 42.22 7.56
-8 -5 -1 23.20 6.55
8 5 1 22.18 5.96
-8 -5 -2 5.05 5.14
8 5 2 -0.20 4.12
-8 -5 -3 12.56 5.67
-8 -5 -3 14.01 5.06
8 5 3 13.40 5.01
-8 -5 -4 98.39 11.00
-8 -5 -4 108.02 10.91
8 5 4 116.07 10.06
-8 -5 -5 5.94 5.22
-8 -5 -5 2.68 4.52
8 5 5 10.30 6.56
8 5 5 7.38 4.21
8 5 6 7.45 3.42
8 5 6 16.97 6.82
8 5 6 9.44 4.00
8 5 6 18.85 7.00
-8 -5 -6 15.01 5.58
8 5 7 114.83 9.54
8 5 7 125.85 13.92
8 5 7 117.97 9.67
8 5 7 127.80 13.77
8 5 7 115.63 11.79
-8 -5 -7 114.82 12.01
8 5 8 1.83 3.46
8 5 8 -0.63 6.09
-8 -5 -8 7.79 5.33
8 5 9 -1.63 3.99
-8 -5 -9 5.69 6.05
-8 -6 -1 77.93 11.03
8 6 1 57.22 8.18
-8 -6 -2 2.77 5.85
-8 -6 -2 4.73 4.21
8 6 2 7.60 4.73
-8 -6 -3 3.82 4.45
8 6 3 -0.73 3.62
-8 -6 -4 27.00 7.26
-8 -6 -4 10.23 5.20
8 6 4 13.51 5.02
-8 -6 -5 15.52 6.74
-8 -6 -5 31.34 7.81
8 6 5 20.06 7.78
8 6 5 15.11 4.87
-8 -6 -6 4.16 4.84
8 6 6 0.12 5.86
8 6 6 1.51 3.75
8 6 6 -0.30 5.24
-8 -6 -6 10.99 5.98
8 6 7 -2.80 3.52
8 6 7 -0.47 5.59
-8 -6 -7 0.62 5.32
8 6 8 40.31 6.66
-8 -6 -8 52.48 9.05
-8 -7 -1 14.10 6.05
-8 -7 -2 37.09 7.34
-8 -7 -3 9.03 5.71
8 7 3 -4.42 5.09
-8 -7 -4 10.00 5.70
8 7 4 3.88 4.84
-8 -7 -5 17.04 6.61
8 7 5 15.05 5.32
-8 -7 -6 3.55 5.48
8 7 6 -0.12 4.04
-8 -8 -3 -2.68 6.06
-8 -8 -4 1.99 5.48
8 8 5 16.18 5.82
8 8 6 5.20 4.78
9 -1 0 8.52 6.11
9 -1 1 36.85 8.18
9 -1 2 8.98 4.97
9 -1 3 5.17 4.76
9 -1 4 26.03 6.80
9 -1 4 17.03 4.55
9 -1 5 2.13 4.43
9 -1 5 10.43 5.02
9 0 3 26.27 5.36
9 0 4 2.84 3.86
9 0 4 2.66 5.87
9 0 4 3.77 3.61
9 0 5 50.07 7.39
9 0 5 41.28 6.87
9 0 6 11.70 5.24
-9 -1 1 15.01 5.10
-9 -1 1 8.75 4.65
-9 -1 0 30.04 6.40
-9 -1 0 31.76 6.11
-9 -1 -1 -5.49 5.13
-9 -1 -2 17.41 5.34
9 1 2 24.11 6.54
9 1 2 23.82 5.28
9 1 3 55.09 9.88
9 1 3 56.20 8.67
9 1 3 47.71 6.82
9 1 4 27.57 7.84
9 1 4 21.29 5.95
9 1 4 24.20 5.42
9 1 5 6.57 4.36
9 1 5 6.72 5.39
9 1 5 3.35 4.64
9 1 6 38.28 7.71
9 1 6 31.32 8.19
9 1 7 19.18 7.98
-9 -2 1 20.83 5.66
-9 -2 1 27.92 6.13
-9 -2 0 34.80 6.74
-9 -2 0 23.13 5.98
-9 -2 -1 12.17 5.05
-9 -2 -1 30.63 6.38
9 2 1 31.12 5.66
-9 -2 -2 -0.94 4.10
-9 -2 -2 0.84 3.62
9 2 2 -2.60 3.78
9 2 2 -2.69 3.65
-9 -2 -3 15.33 4.47
-9 -2 -3 19.59 5.94
9 2 3 27.51 6.78
9 2 3 19.21 5.07
9 2 4 62.89 9.40
9 2 4 56.85 9.15
9 2 4 52.05 7.58
9 2 5 -4.00 4.89
9 2 5 4.18 5.06
9 2 5 -6.09 4.88
9 2 6 11.88 6.68
9 2 6 18.04 6.07
-9 -3 0 62.09 8.77
-9 -3 -1 41.31 7.13
-9 -3 -1 47.92 7.68
-9 -3 -2 18.44 5.70
-9 -3 -2 7.46 4.21
9 3 2 12.23 4.88
9 3 2 11.94 4.95
-9 -3 -3 13.52 4.67
-9 -3 -3 6.13 4.31
9 3 3 7.07 4.73
9 3 3 15.64 5.49
-9 -3 -4 31.22 6.14
9 3 4 18.02 6.13
9 3 4 31.82 6.69
9 3 4 39.57 8.44
9 3 4 28.36 6.67
-9 -3 -5 19.90 5.26
9 3 5 14.68 6.63
9 3 5 6.48 4.56
9 3 5 21.87 7.00
9 3 7 18.80 5.38
9 3 8 8.10 4.13
-9 -4 -1 37.41 7.92
-9 -4 -2 28.61 6.33
-9 -4 -3 10.92 4.84
9 4 3 -2.95 4.67
9 4 3 3.30 4.65
-9 -4 -4 19.98 5.69
9 4 4 10.21 7.28
9 4 4 17.45 5.88
9 4 4 17.50 5.91
-9 -4 -5 38.63 7.12
9 4 5 43.35 7.07
-9 -4 -6 10.81 5.18
9 4 6 12.16 5.07
-9 -5 -3 12.54 6.35
-9 -5 -4 10.62 6.05
9 5 4 9.33 5.40
-9 -5 -5 32.82 6.88
9 5 5 16.63 5.24
-9 -5 -6 2.31 4.99
9 5 6 7.37 4.93
-9 -5 -7 8.92 5.81
9 6 5 0.05 4.41
9 6 6 51.90 7.93
0 0 0 0.00 0.00
TITL V323_10_ABS in P-1
REM P-1 (#2 in standard setting)
CELL 0.71073 6.892045 7.728117 8.920985 76.6458 73.8972 76.0445
ZERR 2.00 0.000179 0.000253 0.000244 0.0026 0.0023 0.0025
LATT 1
SFAC C H N O
UNIT 22.00 20.00 2.00 2.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 87814
_shelx_res_file
;
TITL v323_10_abs_a.res in P-1
v323_10_abs.res
created by SHELXL-2018/3 at 14:19:28 on 09-Jul-2020
REM Old TITL V323_10_ABS in P-1
REM SHELXT solution in P-1: R1 0.149, Rweak 0.013, Alpha 0.049
REM 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C8 N O2 Br
rem EQIV $2 1-X,-Y,1-Z
rem EQIV $3 1-X,1-Y,1-Z
rem HTAB N1 O2_$2
rem HTAB C5 Br1_$3
CELL 0.71073 6.892 7.7281 8.921 76.646 73.897 76.045
ZERR 2 0.0002 0.0003 0.0002 0.003 0.002 0.002
LATT 1
SFAC C H Br N O
UNIT 14 18 2 4 4
EQIV $1 1-X,-Y,2-Z
L.S. 8 0 0
PLAN 1
TEMP 21.9(10)
CONF
HTAB N1 O1
HTAB N1 Br1
HTAB N1 Br1_$1
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
OMIT 0 58
OMIT 0 1 0
REM
REM
REM
WGHT 0.028400 0.094100
FVAR 0.96608
BR1 3 0.816002 0.100381 0.851824 11.00000 0.04293 0.05194 =
0.04204 0.01167 -0.01413 -0.01063
O1 5 0.290259 0.058423 0.535013 11.00000 0.06878 0.04040 =
0.05181 -0.00939 -0.01581 -0.01710
N1 4 0.360498 0.124311 0.796944 11.00000 0.04291 0.02956 =
0.03179 0.00078 -0.01098 -0.00520
H1A 2 0.359266 0.044053 0.739309 11.00000 0.06196
H1B 2 0.281396 0.094558 0.888874 11.00000 0.05658
H1C 2 0.492208 0.108130 0.810724 11.00000 0.05163
C1 1 0.293735 0.310053 0.721272 11.00000 0.02508 0.02851 =
0.03214 0.00042 -0.00493 -0.00792
O2 5 0.370436 0.252049 0.323718 11.00000 0.08692 0.07727 =
0.03237 -0.00736 -0.01516 -0.02595
N2 4 0.315828 0.211642 0.467763 11.00000 0.03716 0.04958 =
0.03639 -0.00783 -0.01273 -0.01093
C2 1 0.256836 0.447453 0.807836 11.00000 0.02963 0.03515 =
0.04009 -0.00779 -0.00230 -0.00938
C3 1 0.199302 0.625148 0.731925 11.00000 0.03717 0.03123 =
0.06731 -0.01158 -0.00448 -0.00993
AFIX 43
H3 2 0.168936 0.719362 0.788371 11.00000 -1.20000
AFIX 0
C4 1 0.186348 0.664540 0.575305 11.00000 0.04067 0.03102 =
0.06895 0.01081 -0.01857 -0.01031
AFIX 43
H4 2 0.148182 0.784148 0.528182 11.00000 -1.20000
AFIX 0
C5 1 0.229126 0.529291 0.489229 11.00000 0.03553 0.03965 =
0.04630 0.01164 -0.01675 -0.01401
AFIX 43
H5 2 0.224223 0.555655 0.383067 11.00000 -1.20000
AFIX 0
C6 1 0.279916 0.352185 0.563563 11.00000 0.02703 0.03268 =
0.03533 0.00053 -0.00986 -0.00945
C7 1 0.279644 0.406124 0.976472 11.00000 0.05711 0.05525 =
0.04016 -0.01765 -0.00648 -0.01217
AFIX 137
H7A 2 0.195481 0.320174 1.038442 11.00000 -1.50000
H7B 2 0.237042 0.515587 1.020032 11.00000 -1.50000
H7C 2 0.420924 0.356305 0.978274 11.00000 -1.50000
AFIX 0
HKLF 4
REM v323_10_abs_a.res in P-1
REM wR2 = 0.0608, GooF = S = 1.109, Restrained GooF = 1.109 for all data
REM R1 = 0.0262 for 1986 Fo > 4sig(Fo) and 0.0342 for all 2299 data
REM 122 parameters refined using 0 restraints
END
WGHT 0.0284 0.0941
REM Highest difference peak 0.331, deepest hole -0.387, 1-sigma level 0.072
Q1 1 0.2865 0.3565 0.3324 11.00000 0.05 0.33
;
_shelx_res_checksum 40154
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 0.81600(3) 0.10038(3) 0.85182(2) 0.04788(9) Uani d 1 . .
O O1 0.2903(3) 0.0584(2) 0.53501(18) 0.0519(4) Uani d 1 . .
N N1 0.3605(3) 0.1243(2) 0.7969(2) 0.0356(3) Uani d 1 . .
H H1A 0.359(4) 0.044(4) 0.739(3) 0.062(7) Uiso d 1 . .
H H1B 0.281(4) 0.095(3) 0.889(3) 0.057(7) Uiso d 1 . .
H H1C 0.492(4) 0.108(3) 0.811(3) 0.052(6) Uiso d 1 . .
C C1 0.2937(2) 0.3101(2) 0.7213(2) 0.0294(3) Uani d 1 . .
O O2 0.3704(3) 0.2520(2) 0.32372(17) 0.0638(5) Uani d 1 . .
N N2 0.3158(2) 0.2116(2) 0.46776(19) 0.0397(4) Uani d 1 . .
C C2 0.2568(3) 0.4475(2) 0.8078(2) 0.0354(4) Uani d 1 . .
C C3 0.1993(3) 0.6251(3) 0.7319(3) 0.0457(5) Uani d 1 . .
H H3 0.168936 0.719362 0.788371 0.055 Uiso calc 1 . .
C C4 0.1863(3) 0.6645(3) 0.5753(3) 0.0484(5) Uani d 1 . .
H H4 0.148182 0.784148 0.528182 0.058 Uiso calc 1 . .
C C5 0.2291(3) 0.5293(3) 0.4892(2) 0.0411(4) Uani d 1 . .
H H5 0.224223 0.555655 0.383067 0.049 Uiso calc 1 . .
C C6 0.2799(2) 0.3522(2) 0.5636(2) 0.0316(3) Uani d 1 . .
C C7 0.2796(4) 0.4061(3) 0.9765(2) 0.0500(5) Uani d 1 . .
H H7A 0.195481 0.320174 1.038442 0.075 Uiso calc 1 . .
H H7B 0.237042 0.515587 1.020032 0.075 Uiso calc 1 . .
H H7C 0.420924 0.356305 0.978274 0.075 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Br1 0.04293(13) 0.05194(14) 0.04204(12) -0.01063(9) -0.01413(9) 0.01167(9)
O1 0.0688(10) 0.0404(8) 0.0518(8) -0.0171(7) -0.0158(7) -0.0094(7)
N1 0.0429(9) 0.0296(8) 0.0318(8) -0.0052(7) -0.0110(7) 0.0008(6)
C1 0.0251(7) 0.0285(8) 0.0321(8) -0.0079(6) -0.0049(6) 0.0004(6)
O2 0.0869(12) 0.0773(12) 0.0324(7) -0.0260(10) -0.0152(8) -0.0074(8)
N2 0.0372(8) 0.0496(10) 0.0364(8) -0.0109(7) -0.0127(6) -0.0078(7)
C2 0.0296(8) 0.0352(9) 0.0401(9) -0.0094(7) -0.0023(7) -0.0078(7)
C3 0.0372(10) 0.0312(9) 0.0673(14) -0.0099(8) -0.0045(9) -0.0116(9)
C4 0.0407(10) 0.0310(9) 0.0690(14) -0.0103(8) -0.0186(10) 0.0108(9)
C5 0.0355(9) 0.0397(10) 0.0463(10) -0.0140(8) -0.0167(8) 0.0116(8)
C6 0.0270(8) 0.0327(8) 0.0353(9) -0.0094(7) -0.0099(7) 0.0005(7)
C7 0.0571(13) 0.0552(13) 0.0402(10) -0.0122(10) -0.0065(9) -0.0177(10)
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -4 5 0.1593
-5 -3 -2 0.1427
5 2 4 0.1656
-3 0 -5 0.1601
3 5 -5 0.1521
-1 5 1 0.0920
1 -5 -1 0.0920
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
H1A N1 H1B . . 105(2) ?
H1A N1 H1C . . 108(2) ?
H1B N1 H1C . . 108(2) ?
C1 N1 H1A . . 111.5(17) ?
C1 N1 H1B . . 112.9(17) ?
C1 N1 H1C . . 110.7(15) ?
C2 C1 N1 . . 118.04(15) ?
C2 C1 C6 . . 120.05(16) ?
C6 C1 N1 . . 121.77(16) ?
O1 N2 C6 . . 118.93(15) ?
O2 N2 O1 . . 122.57(17) ?
O2 N2 C6 . . 118.50(17) ?
C1 C2 C3 . . 117.32(17) ?
C1 C2 C7 . . 121.11(17) ?
C3 C2 C7 . . 121.57(18) ?
C2 C3 H3 . . 119.1 ?
C4 C3 C2 . . 121.83(19) ?
C4 C3 H3 . . 119.1 ?
C3 C4 H4 . . 119.7 ?
C5 C4 C3 . . 120.57(18) ?
C5 C4 H4 . . 119.7 ?
C4 C5 H5 . . 120.8 ?
C4 C5 C6 . . 118.49(18) ?
C6 C5 H5 . . 120.8 ?
C1 C6 N2 . . 122.02(15) ?
C5 C6 C1 . . 121.68(17) ?
C5 C6 N2 . . 116.30(16) ?
C2 C7 H7A . . 109.5 ?
C2 C7 H7B . . 109.5 ?
C2 C7 H7C . . 109.5 ?
H7A C7 H7B . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 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 N2 . 1.228(2) ?
N1 H1A . 0.90(3) ?
N1 H1B . 0.86(3) ?
N1 H1C . 0.92(3) ?
N1 C1 . 1.461(2) ?
C1 C2 . 1.389(3) ?
C1 C6 . 1.394(2) ?
O2 N2 . 1.222(2) ?
N2 C6 . 1.467(2) ?
C2 C3 . 1.399(3) ?
C2 C7 . 1.508(3) ?
C3 H3 . 0.9300 ?
C3 C4 . 1.383(3) ?
C4 H4 . 0.9300 ?
C4 C5 . 1.366(3) ?
C5 H5 . 0.9300 ?
C5 C6 . 1.383(2) ?
C7 H7A . 0.9600 ?
C7 H7B . 0.9600 ?
C7 H7C . 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
N1 H1A O1 . 0.90(3) 1.98(3) 2.693(2) 135(2) yes
N1 H1B Br1 2_657 0.86(3) 2.47(3) 3.2717(17) 155(2) yes
N1 H1C Br1 . 0.92(3) 2.34(3) 3.2650(18) 174(2) 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
O1 N2 C6 C1 . . . . 24.5(2) ?
O1 N2 C6 C5 . . . . -154.82(17) ?
N1 C1 C2 C3 . . . . 178.02(16) ?
N1 C1 C2 C7 . . . . -1.5(3) ?
N1 C1 C6 N2 . . . . 4.9(2) ?
N1 C1 C6 C5 . . . . -175.88(16) ?
C1 C2 C3 C4 . . . . -2.3(3) ?
O2 N2 C6 C1 . . . . -155.44(18) ?
O2 N2 C6 C5 . . . . 25.3(2) ?
C2 C1 C6 N2 . . . . -179.47(15) ?
C2 C1 C6 C5 . . . . -0.2(3) ?
C2 C3 C4 C5 . . . . 0.3(3) ?
C3 C4 C5 C6 . . . . 1.8(3) ?
C4 C5 C6 C1 . . . . -1.8(3) ?
C4 C5 C6 N2 . . . . 177.48(16) ?
C6 C1 C2 C3 . . . . 2.2(2) ?
C6 C1 C2 C7 . . . . -177.35(17) ?
C7 C2 C3 C4 . . . . 177.29(19) ?
_cod_database_fobs_code 2022327