#------------------------------------------------------------------------------
#$Date: 2024-07-20 04:58:36 +0300 (Sat, 20 Jul 2024) $
#$Revision: 293488 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023203.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_2023203
loop_
_publ_author_name
'Novikov, Egor M.'
'Guillen Campos, Jesus'
'Read de Alaniz, Javier'
'Fonari, Marina S.'
'Timofeeva, Tatiana V.'
_publ_section_title
;
Synthesis, molecular and crystal structures of
4-amino-3,5-difluorobenzonitrile, ethyl 4-amino-3,5-difluorobenzoate, and
diethyl 4,4′-(diazene-1,2-diyl)bis(3,5-difluorobenzoate)
;
_journal_coeditor_code JQ2034
_journal_issue 8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024006819
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C7 H4 F2 N2'
_chemical_formula_moiety 'C7 H4 F2 N2'
_chemical_formula_sum 'C7 H4 F2 N2'
_chemical_formula_weight 154.12
_chemical_name_systematic
;
4-Amino-3,5-difluorobenzonitrile
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha 90
_cell_angle_beta 94.604(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 3.7283(4)
_cell_length_b 10.5275(12)
_cell_length_c 16.9073(19)
_cell_measurement_reflns_used 4913
_cell_measurement_temperature 100.15
_cell_measurement_theta_max 31.206
_cell_measurement_theta_min 2.281
_cell_volume 661.46(13)
_computing_cell_refinement
;
SAINT-Plus V8.40b (Bruker, 2019)
;
_computing_data_collection
;
APEX2 Ver. 2019.11-0. (Bruker, 2019)
;
_computing_data_reduction
;
SAINT-Plus V8.40b (Bruker, 2019)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.15
_diffrn_detector 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \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 0.0292
_diffrn_reflns_av_unetI/netI 0.0203
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 11242
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 31.650
_diffrn_reflns_theta_min 2.281
_diffrn_source 'sealed X-ray tube'
_diffrn_source_current 43.0
_diffrn_source_power 1.634
_diffrn_source_voltage 38.0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.136
_exptl_absorpt_correction_T_max 0.7462
_exptl_absorpt_correction_T_min 0.6606
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_density_diffrn 1.548
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 312
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.12
_refine_diff_density_max 0.458
_refine_diff_density_min -0.228
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.086
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 108
_refine_ls_number_reflns 2140
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.086
_refine_ls_R_factor_all 0.0578
_refine_ls_R_factor_gt 0.0467
_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^)+(0.0659P)^2^+0.2291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1233
_refine_ls_wR_factor_ref 0.1303
_reflns_number_gt 1775
_reflns_number_total 2140
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jq2034.cif
_cod_data_source_block I
_cod_database_code 2023203
_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 0.953
_shelx_estimated_absorpt_t_max 0.984
_shelx_hkl_file
;
1 0 0 0.60 0.10
1 0 0 0.90 0.50
1 0 0 0.80 0.40
-2 0 0 598.14 14.90
-2 0 0 599.04 14.90
2 0 0 619.34 15.10
2 0 0 599.34 15.10
2 0 0 581.54 15.00
2 0 0 610.94 15.10
-3 0 0 1.60 0.90
-3 0 0 2.30 0.90
3 0 0 1.20 1.00
3 0 0 0.70 0.90
-4 0 0 280.77 8.10
-4 0 0 272.97 8.10
4 0 0 254.87 8.30
-5 0 0 -0.80 1.40
-5 0 0 -0.20 1.90
5 0 0 0.40 2.00
5 -1 0 2.10 2.10
-5 1 0 0.50 1.80
-5 1 0 1.30 1.50
4 -1 0 10.10 1.80
4 -1 0 6.40 1.60
-4 1 0 10.20 1.80
-4 1 0 7.80 1.70
3 -1 0 24.10 1.80
3 -1 0 19.00 1.80
-3 1 0 16.40 1.60
-3 1 0 17.40 1.50
2 -1 0 353.16 9.20
2 -1 0 362.16 9.50
2 -1 0 359.26 9.40
1 -1 0 3.00 0.60
0 -1 0 0.50 0.10
0 -1 0 0.50 0.10
0 -1 0 0.40 0.10
0 1 0 0.60 0.10
0 1 0 0.50 0.20
0 1 0 0.60 0.10
0 1 0 0.50 0.10
-1 -1 0 2.30 0.40
-1 -1 0 0.70 0.40
1 1 0 4.60 0.70
1 1 0 1.70 0.50
-2 -1 0 343.07 8.90
-2 -1 0 351.16 9.00
2 1 0 351.16 9.20
2 1 0 358.36 9.40
-3 -1 0 16.80 1.50
-3 -1 0 15.80 1.50
3 1 0 20.00 1.80
3 1 0 20.20 1.80
-4 -1 0 6.20 1.60
4 1 0 9.10 1.80
4 1 0 10.60 1.90
-5 -1 0 -0.60 1.80
-5 -1 0 1.50 1.80
5 1 0 3.40 2.00
-5 2 0 19.50 2.50
-5 2 0 19.80 2.50
4 -2 0 21.00 2.30
4 -2 0 20.30 2.20
4 -2 0 15.80 2.30
-4 2 0 18.60 2.10
-4 2 0 21.00 2.20
-4 2 0 24.80 2.40
3 -2 0 113.09 3.90
3 -2 0 113.59 3.90
3 -2 0 107.39 4.10
-3 2 0 109.59 4.10
-3 2 0 116.49 4.00
2 -2 0 716.13 18.10
2 -2 0 745.13 17.90
2 -2 0 725.93 17.70
-2 2 0 682.73 17.60
1 -2 0 9321.47 248.08
1 -2 0 9961.70 230.38
1 -2 0 9999.00 231.78
-1 2 0 9345.37 259.47
0 -2 0 900.81 21.50
0 -2 0 891.21 21.50
0 -2 0 890.01 21.80
0 -2 0 910.21 21.50
0 2 0 898.81 21.60
0 2 0 866.21 21.80
-1 -2 0 9198.18 229.98
-1 -2 0 9816.32 223.68
-1 -2 0 9077.69 228.78
1 2 0 9211.28 260.07
1 2 0 9695.53 225.88
-2 -2 0 703.23 17.60
-2 -2 0 724.53 17.40
2 2 0 737.33 18.20
2 2 0 702.23 17.90
-3 -2 0 111.49 3.60
-3 -2 0 108.79 3.80
3 2 0 110.79 4.30
3 2 0 106.29 4.00
-4 -2 0 22.80 2.40
4 2 0 22.60 2.50
4 2 0 25.50 2.70
-5 -2 0 21.20 2.70
-5 -2 0 19.60 2.60
5 2 0 20.40 3.00
-5 3 0 7.60 2.20
4 -3 0 -3.60 1.40
4 -3 0 0.80 0.80
-4 3 0 0.00 1.10
-4 3 0 -0.10 1.30
-4 3 0 0.80 1.50
3 -3 0 27.80 2.20
3 -3 0 28.20 2.30
3 -3 0 28.90 1.90
-3 3 0 25.00 1.90
-3 3 0 29.50 2.30
2 -3 0 1943.51 47.60
2 -3 0 2018.10 48.40
2 -3 0 2028.80 48.00
-2 3 0 2012.40 47.80
1 -3 0 20.20 1.10
1 -3 0 18.20 1.20
1 -3 0 18.70 0.70
-1 3 0 17.90 1.00
0 -3 0 0.20 0.20
0 -3 0 -0.20 0.30
-1 -3 0 17.90 0.90
-1 -3 0 15.90 0.50
1 3 0 17.90 1.30
1 3 0 18.50 0.50
1 3 0 16.60 1.00
-2 -3 0 2046.20 47.40
-2 -3 0 1904.71 47.70
2 3 0 1963.60 47.70
2 3 0 2020.20 48.10
-3 -3 0 27.10 2.00
-3 -3 0 20.20 1.60
3 3 0 28.70 2.50
3 3 0 25.50 2.00
-4 -3 0 -0.40 1.40
-4 -3 0 -2.00 1.20
4 3 0 -0.40 1.30
4 3 0 1.60 1.50
-5 -3 0 10.40 2.30
-5 -3 0 9.90 2.30
5 3 0 18.20 3.20
-5 4 0 4.10 2.10
-5 4 0 4.70 2.50
4 -4 0 16.50 2.30
-4 4 0 18.20 2.50
3 -4 0 325.87 9.50
3 -4 0 346.87 9.00
3 -4 0 326.77 10.00
-3 4 0 327.57 9.20
-3 4 0 337.07 9.70
2 -4 0 229.38 6.20
2 -4 0 243.08 7.10
2 -4 0 242.48 6.80
-2 4 0 229.78 6.50
1 -4 0 626.14 15.10
1 -4 0 580.44 15.20
1 -4 0 621.94 14.40
-1 4 0 621.34 14.90
-1 4 0 573.24 14.40
0 -4 0 339.67 8.60
0 -4 0 345.77 8.20
0 -4 0 334.67 8.50
0 4 0 330.57 8.70
-1 -4 0 599.44 14.90
-1 -4 0 579.54 14.30
1 4 0 604.24 14.90
1 4 0 622.64 14.40
1 4 0 610.94 15.30
-2 -4 0 229.18 6.40
2 4 0 243.88 6.80
2 4 0 230.98 7.10
-3 -4 0 312.07 8.70
3 4 0 321.57 9.20
3 4 0 313.17 9.60
-4 -4 0 12.80 2.00
-4 -4 0 10.00 1.80
4 4 0 14.80 2.30
4 4 0 17.00 2.70
-5 -4 0 3.40 2.00
-5 -4 0 4.50 1.80
5 4 0 7.50 2.40
5 -5 0 -1.20 2.50
-5 5 0 1.70 1.80
-5 5 0 4.60 2.50
4 -5 0 321.67 9.90
-4 5 0 308.27 9.80
3 -5 0 447.16 12.20
3 -5 0 443.76 12.80
3 -5 0 433.06 11.30
-3 5 0 421.46 12.20
-3 5 0 449.16 11.70
2 -5 0 27.10 1.20
2 -5 0 25.40 1.90
2 -5 0 26.50 1.80
-2 5 0 24.30 1.50
1 -5 0 1881.61 46.00
1 -5 0 1963.50 45.20
1 -5 0 2005.30 45.80
-1 5 0 1800.52 45.10
-1 5 0 1882.31 45.60
0 -5 0 -0.10 0.20
0 -5 0 -0.40 0.40
0 -5 0 -0.40 0.40
0 5 0 1.10 0.80
-1 -5 0 1974.20 44.80
-1 -5 0 1886.01 44.90
-1 -5 0 1867.21 45.20
1 5 0 1785.22 44.80
1 5 0 1877.41 45.50
-2 -5 0 25.20 1.50
2 5 0 24.30 2.10
2 5 0 24.90 1.70
-3 -5 0 435.46 11.60
-3 -5 0 426.06 11.40
3 5 0 425.46 11.80
3 5 0 410.26 12.30
-4 -5 0 318.17 9.50
-4 -5 0 320.87 9.40
4 5 0 324.97 10.00
4 5 0 303.07 10.30
-5 -5 0 3.10 1.90
5 5 0 7.90 2.60
-5 6 0 4.40 2.10
-5 6 0 8.20 2.90
4 -6 0 90.49 4.80
-4 6 0 90.09 4.60
3 -6 0 41.40 2.90
3 -6 0 35.70 3.00
-3 6 0 39.50 2.30
-3 6 0 37.90 2.80
2 -6 0 0.00 1.00
2 -6 0 0.30 0.80
2 -6 0 0.60 0.40
-2 6 0 0.10 0.70
1 -6 0 117.29 2.80
1 -6 0 117.79 3.80
1 -6 0 111.29 4.00
-1 6 0 109.89 3.60
-1 6 0 108.79 2.80
0 -6 0 100.69 3.40
0 -6 0 104.59 2.90
0 -6 0 103.79 3.40
0 6 0 107.19 3.60
-1 -6 0 110.99 3.10
-1 -6 0 109.39 3.50
1 6 0 106.89 4.00
-2 -6 0 -0.30 0.60
-2 -6 0 -0.50 0.60
2 6 0 0.30 1.10
2 6 0 -1.10 0.70
-3 -6 0 37.40 2.30
-3 -6 0 35.80 2.20
3 6 0 37.90 2.60
3 6 0 34.30 3.00
-4 -6 0 93.59 4.20
-4 -6 0 93.29 4.10
4 6 0 90.49 5.00
-5 -6 0 7.20 2.00
4 -7 0 56.99 4.20
-4 7 0 62.69 4.00
3 -7 0 83.19 4.00
3 -7 0 90.49 4.60
-3 7 0 87.59 3.70
-3 7 0 93.79 4.30
2 -7 0 29.20 2.10
2 -7 0 33.70 2.60
-2 7 0 28.70 1.90
1 -7 0 83.79 3.30
1 -7 0 85.29 3.40
-1 7 0 88.19 3.30
0 -7 0 -0.40 0.30
0 -7 0 0.10 0.60
0 -7 0 0.10 0.60
0 7 0 0.60 0.90
-1 -7 0 86.29 2.70
-1 -7 0 86.79 2.90
-1 -7 0 86.89 3.20
1 7 0 90.79 3.80
-2 -7 0 29.80 1.90
-2 -7 0 25.40 1.80
2 7 0 31.00 2.60
-3 -7 0 82.59 3.50
-3 -7 0 80.59 3.50
3 7 0 79.69 4.40
-4 -7 0 60.29 3.50
-4 -7 0 58.49 3.30
4 7 0 56.39 4.50
4 -8 0 6.70 2.40
-4 8 0 9.10 2.60
3 -8 0 14.80 2.30
3 -8 0 18.00 2.80
-3 8 0 18.10 2.50
2 -8 0 35.30 2.70
2 -8 0 32.30 2.40
-2 8 0 32.20 2.20
1 -8 0 206.28 6.70
1 -8 0 216.38 6.60
-1 8 0 218.48 6.50
0 -8 0 0.60 0.70
0 -8 0 1.30 0.80
0 -8 0 0.70 0.40
0 8 0 1.30 1.20
-1 -8 0 213.38 6.00
-1 -8 0 223.18 5.90
-1 -8 0 213.98 6.40
1 8 0 209.38 7.00
-2 -8 0 30.50 2.00
-2 -8 0 29.40 1.90
2 8 0 33.60 2.90
-3 -8 0 16.20 1.90
-3 -8 0 15.60 1.90
3 8 0 12.50 2.50
-4 -8 0 9.20 2.00
-4 -8 0 8.50 2.00
4 8 0 8.20 2.80
4 -9 0 2.50 2.20
-4 9 0 5.30 2.30
3 -9 0 29.80 3.60
3 -9 0 22.40 2.70
-3 9 0 27.60 2.90
2 -9 0 77.29 4.10
2 -9 0 78.69 3.80
-2 9 0 78.79 3.60
1 -9 0 43.40 2.70
1 -9 0 47.40 2.60
-1 9 0 42.70 2.70
0 -9 0 -1.20 0.80
0 -9 0 0.60 0.80
0 9 0 0.50 1.30
-1 -9 0 45.20 2.00
-1 -9 0 44.00 2.40
1 9 0 44.40 3.10
-2 -9 0 76.89 3.40
-2 -9 0 75.19 3.10
2 9 0 77.79 4.30
-3 -9 0 27.00 2.50
-3 -9 0 23.10 2.40
3 9 0 22.90 3.20
-4 -9 0 3.30 1.60
-4 -9 0 5.30 1.90
4 9 0 5.00 2.60
4 -10 0 0.00 2.20
3 -10 0 12.20 2.30
3 -10 0 12.80 2.90
-3 10 0 15.20 2.60
2 -10 0 41.60 3.50
2 -10 0 43.00 3.00
-2 10 0 38.10 2.80
-2 10 0 43.20 3.00
1 -10 0 155.88 5.60
1 -10 0 163.88 6.00
-1 10 0 159.98 5.80
0 -10 0 -1.30 0.80
0 -10 0 0.00 1.00
0 10 0 1.30 1.70
-1 -10 0 152.08 5.30
-1 -10 0 149.09 4.60
1 10 0 156.18 6.10
-2 -10 0 38.20 2.60
-2 -10 0 37.10 2.30
2 10 0 35.70 3.30
-3 -10 0 10.70 1.90
-3 -10 0 9.20 1.80
3 10 0 10.70 2.90
-4 -10 0 5.90 1.90
3 -11 0 0.10 1.80
-3 11 0 8.90 2.50
2 -11 0 2.90 1.60
2 -11 0 1.20 1.80
-2 11 0 3.10 1.70
1 -11 0 -0.50 1.20
1 -11 0 0.80 1.20
-1 11 0 1.50 1.80
0 -11 0 0.40 1.10
0 -11 0 -1.30 1.10
0 11 0 -1.40 1.50
-1 -11 0 1.30 1.20
1 11 0 2.00 1.80
-2 -11 0 1.90 1.30
-2 -11 0 1.00 1.00
2 11 0 1.10 2.00
-3 -11 0 7.30 2.00
-3 -11 0 6.30 1.80
3 11 0 8.10 2.60
3 -12 0 39.40 3.80
-3 12 0 46.60 4.10
2 -12 0 1.30 1.70
2 -12 0 -1.60 1.80
-2 12 0 2.30 2.10
1 -12 0 28.70 2.70
1 -12 0 28.40 2.80
-1 12 0 31.60 3.40
-1 12 0 34.30 3.00
0 -12 0 56.19 3.40
0 12 0 56.29 3.90
-1 -12 0 32.40 2.70
1 12 0 32.30 3.70
-2 -12 0 0.30 1.40
2 12 0 -0.40 2.30
-3 -12 0 42.80 3.60
3 12 0 42.50 5.40
2 -13 0 -0.30 1.70
-2 13 0 3.10 2.10
1 -13 0 2.00 1.90
1 -13 0 4.40 1.80
-1 13 0 -0.10 2.10
-1 13 0 6.90 1.90
0 -13 0 0.90 1.40
0 13 0 -4.10 2.10
-1 -13 0 5.50 1.80
1 13 0 5.00 2.40
-2 -13 0 1.30 1.60
2 13 0 2.30 2.50
1 -14 0 3.00 1.80
0 -14 0 1.00 1.60
0 14 0 -3.10 2.30
-1 -14 0 1.10 1.90
1 14 0 1.10 2.40
0 15 0 -4.80 2.20
0 15 -1 3.10 2.80
1 14 -1 6.30 3.00
-1 -14 1 7.70 2.40
0 14 -1 -0.30 2.20
0 -14 1 3.20 1.70
1 -14 1 26.00 3.20
-2 14 -1 107.39 5.90
2 13 -1 8.60 3.10
-2 -13 1 11.70 2.30
1 13 -1 7.40 2.60
-1 -13 1 8.60 2.20
0 13 -1 4.50 2.50
0 -13 1 7.30 2.00
-1 13 -1 35.20 3.30
-1 13 -1 25.90 4.60
1 -13 1 31.60 3.10
-2 13 -1 7.00 2.40
2 -13 1 4.10 2.00
3 12 -1 9.20 3.40
-3 -12 1 7.00 2.10
-3 -12 1 4.00 3.00
2 12 -1 3.10 2.30
-2 -12 1 1.90 1.60
1 12 -1 19.10 3.00
-1 -12 1 21.90 2.60
0 12 -1 97.99 4.90
0 -12 1 95.39 4.40
-1 12 -1 22.60 3.00
-1 12 -1 30.00 2.90
1 -12 1 23.60 2.70
-2 12 -1 17.60 2.90
2 -12 1 14.10 2.50
-3 12 -1 56.59 4.50
3 -12 1 45.20 4.00
3 11 -1 3.90 2.40
-3 -11 1 4.80 1.70
-3 -11 1 3.90 1.60
2 11 -1 3.00 2.30
-2 -11 1 -0.20 0.60
-2 -11 1 0.30 1.30
1 11 -1 23.90 3.20
-1 -11 1 28.40 2.40
0 11 -1 3.90 1.80
0 11 -1 8.90 1.50
0 -11 1 4.00 1.40
-1 11 -1 6.50 2.00
-1 11 -1 6.30 1.70
1 -11 1 3.90 1.50
1 -11 1 4.90 1.80
-2 11 -1 10.10 2.30
2 -11 1 7.20 2.30
2 -11 1 9.00 2.10
-3 11 -1 2.70 2.20
3 -11 1 0.50 1.80
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1 3 23 7.60 3.90
-1 4 23 -1.10 2.30
0 4 23 5.40 1.90
-1 5 23 2.80 2.10
-1 0 24 -0.90 1.50
-1 1 24 -0.70 1.70
0 1 24 17.00 3.90
-1 2 24 1.00 1.80
0 2 24 -0.30 1.50
-1 3 24 2.10 1.90
0 3 24 0.70 1.90
0 4 24 2.70 2.10
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 70618
_shelx_res_file
;
TITL en_106_13_a.res in P2(1)/n
en_106_13.res
created by SHELXL-2019/1 at 10:29:21 on 13-Nov-2023
REM Old TITL EN_106_13 in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.103, Rweak 0.004, Alpha 0.016, Orientation as input
REM Formula found by SHELXT: C7 N2 F2
CELL 0.71073 3.7283 10.5275 16.9073 90 94.604 90
ZERR 4 0.0004 0.0012 0.0019 0 0.002 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H F N
UNIT 28 16 8 8
L.S. 60
PLAN 10
SIZE 0.22 0.36 0.12
TEMP -173
CONF
BOND $H
list 4
MORE -1
fmap 2 53
acta
REM
REM
REM
WGHT 0.065900 0.229100
FVAR 0.98060
F1 3 0.833731 0.476538 0.399266 11.00000 0.04037 0.02210 =
0.03092 0.00499 0.00347 0.00748
F2 3 0.365128 0.804808 0.234928 11.00000 0.04656 0.02716 =
0.01992 0.00565 -0.00081 0.00215
N2 4 0.676203 0.567700 0.249995 11.00000 0.03838 0.02440 =
0.02076 -0.00205 0.00648 0.00149
N1 4 0.251777 0.893598 0.574541 11.00000 0.04247 0.04257 =
0.02987 -0.00949 0.00989 -0.00564
C6 1 0.437905 0.757259 0.309252 11.00000 0.02271 0.02038 =
0.01851 0.00325 0.00084 -0.00358
C4 1 0.674094 0.592518 0.391894 11.00000 0.02144 0.01734 =
0.02356 0.00219 0.00254 -0.00076
C5 1 0.600307 0.637318 0.314446 11.00000 0.01900 0.01923 =
0.02017 -0.00006 0.00343 -0.00450
C2 1 0.431677 0.776845 0.449231 11.00000 0.02015 0.02397 =
0.02130 -0.00314 0.00397 -0.00490
C7 1 0.351808 0.827913 0.373567 11.00000 0.02075 0.01853 =
0.02516 -0.00084 0.00230 -0.00114
AFIX 43
H7 2 0.241446 0.908931 0.366727 11.00000 -1.20000
AFIX 0
C3 1 0.595991 0.657800 0.458660 11.00000 0.02311 0.02559 =
0.01866 0.00294 0.00174 -0.00366
AFIX 43
H3 2 0.652163 0.622977 0.509999 11.00000 -1.20000
AFIX 0
C1 1 0.333694 0.843847 0.518488 11.00000 0.02672 0.02857 =
0.02533 -0.00342 0.00456 -0.00562
H2A 2 0.670660 0.601952 0.206587 11.00000 0.04662
H2B 2 0.814160 0.500212 0.255968 11.00000 0.03631
HKLF 4
REM en_106_13_a.res in P2(1)/n
REM wR2 = 0.1303, GooF = S = 1.086, Restrained GooF = 1.086 for all data
REM R1 = 0.0467 for 1775 Fo > 4sig(Fo) and 0.0578 for all 2140 data
REM 108 parameters refined using 0 restraints
END
WGHT 0.0659 0.2291
REM Highest difference peak 0.458, deepest hole -0.228, 1-sigma level 0.056
Q1 1 0.6373 0.6210 0.3545 11.00000 0.05 0.46
Q2 1 0.6475 0.6375 0.4214 11.00000 0.05 0.41
Q3 1 0.4142 0.8002 0.3426 11.00000 0.05 0.40
Q4 1 0.4163 0.8054 0.4123 11.00000 0.05 0.37
Q5 1 0.4766 0.6932 0.3136 11.00000 0.05 0.35
Q6 1 0.5507 0.7268 0.4533 11.00000 0.05 0.32
Q7 1 0.4197 0.8082 0.4837 11.00000 0.05 0.27
Q8 1 0.3685 0.8394 0.5630 11.00000 0.05 0.25
Q9 1 0.4070 0.7843 0.2757 11.00000 0.05 0.23
Q10 1 0.2185 0.8993 0.5280 11.00000 0.05 0.22
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_shelx_res_checksum 46252
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
F F1 0.8337(2) 0.47654(7) 0.39927(5) 0.0311(2) Uani d 1 . .
F F2 0.3651(2) 0.80481(8) 0.23493(4) 0.0314(2) Uani d 1 . .
N N2 0.6762(3) 0.56770(11) 0.24999(7) 0.0276(3) Uani d 1 . .
N N1 0.2518(4) 0.89360(14) 0.57454(7) 0.0379(3) Uani d 1 . .
C C6 0.4379(3) 0.75726(11) 0.30925(7) 0.0206(2) Uani d 1 . .
C C4 0.6741(3) 0.59252(11) 0.39189(7) 0.0207(2) Uani d 1 . .
C C5 0.6003(3) 0.63732(11) 0.31445(6) 0.0194(2) Uani d 1 . .
C C2 0.4317(3) 0.77685(12) 0.44923(7) 0.0217(2) Uani d 1 . .
C C7 0.3518(3) 0.82791(11) 0.37357(7) 0.0215(2) Uani d 1 . .
H H7 0.241446 0.908931 0.366727 0.026 Uiso calc 1 . .
C C3 0.5960(3) 0.65780(12) 0.45866(7) 0.0224(2) Uani d 1 . .
H H3 0.652163 0.622977 0.509999 0.027 Uiso calc 1 . .
C C1 0.3337(4) 0.84385(13) 0.51849(8) 0.0267(3) Uani d 1 . .
H H2A 0.671(6) 0.602(2) 0.2066(14) 0.047(6) Uiso d 1 . .
H H2B 0.814(5) 0.500(2) 0.2560(12) 0.036(5) 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
F1 0.0404(5) 0.0221(4) 0.0309(4) 0.0075(3) 0.0035(3) 0.0050(3)
F2 0.0466(5) 0.0272(4) 0.0199(4) 0.0021(3) -0.0008(3) 0.0057(3)
N2 0.0384(6) 0.0244(5) 0.0208(5) 0.0015(5) 0.0065(4) -0.0020(4)
N1 0.0425(7) 0.0426(7) 0.0299(6) -0.0056(6) 0.0099(5) -0.0095(5)
C6 0.0227(5) 0.0204(5) 0.0185(5) -0.0036(4) 0.0008(4) 0.0032(4)
C4 0.0214(5) 0.0173(5) 0.0236(5) -0.0008(4) 0.0025(4) 0.0022(4)
C5 0.0190(5) 0.0192(5) 0.0202(5) -0.0045(4) 0.0034(4) -0.0001(4)
C2 0.0201(5) 0.0240(6) 0.0213(5) -0.0049(4) 0.0040(4) -0.0031(4)
C7 0.0208(5) 0.0185(5) 0.0252(5) -0.0011(4) 0.0023(4) -0.0008(4)
C3 0.0231(5) 0.0256(6) 0.0187(5) -0.0037(4) 0.0017(4) 0.0029(4)
C1 0.0267(6) 0.0286(6) 0.0253(6) -0.0056(5) 0.0046(4) -0.0034(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C5 N2 H2A . . 119.3(15) ?
C5 N2 H2B . . 120.1(13) ?
H2A N2 H2B . . 115.7(19) ?
F2 C6 C5 . . 116.31(10) ?
F2 C6 C7 . . 119.29(11) ?
C7 C6 C5 . . 124.39(11) ?
F1 C4 C5 . . 116.14(10) ?
F1 C4 C3 . . 119.63(10) ?
C3 C4 C5 . . 124.23(11) ?
N2 C5 C6 . . 123.49(11) ?
N2 C5 C4 . . 122.01(11) ?
C4 C5 C6 . . 114.49(10) ?
C7 C2 C3 . . 120.55(11) ?
C7 C2 C1 . . 120.46(11) ?
C3 C2 C1 . . 118.95(11) ?
C6 C7 C2 . . 117.98(11) ?
C6 C7 H7 . . 121.0 ?
C2 C7 H7 . . 121.0 ?
C4 C3 C2 . . 118.35(10) ?
C4 C3 H3 . . 120.8 ?
C2 C3 H3 . . 120.8 ?
N1 C1 C2 . . 177.81(15) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
F1 C4 . 1.3596(14) ?
F2 C6 . 1.3596(13) ?
N2 C5 . 1.3617(15) ?
N2 H2A . 0.82(2) ?
N2 H2B . 0.88(2) ?
N1 C1 . 1.1455(18) ?
C6 C5 . 1.4000(16) ?
C6 C7 . 1.3765(16) ?
C4 C5 . 1.3982(16) ?
C4 C3 . 1.3726(16) ?
C2 C7 . 1.3975(17) ?
C2 C3 . 1.3984(17) ?
C2 C1 . 1.4390(17) ?
C7 H7 . 0.9500 ?
C3 H3 . 0.9500 ?
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
N2 H2A N1 4_675 0.82(2) 2.28(2) 3.0297(17) 153(2)
N2 H2B F2 2_645 0.88(2) 2.38(2) 3.2526(15) 173.9(19)
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
F1 C4 C5 N2 . . . . 1.45(17) ?
F1 C4 C5 C6 . . . . -179.65(10) ?
F1 C4 C3 C2 . . . . -179.98(10) ?
F2 C6 C5 N2 . . . . -1.79(17) ?
F2 C6 C5 C4 . . . . 179.34(10) ?
F2 C6 C7 C2 . . . . -179.65(10) ?
C5 C6 C7 C2 . . . . 0.04(18) ?
C5 C4 C3 C2 . . . . 0.06(18) ?
C7 C6 C5 N2 . . . . 178.51(12) ?
C7 C6 C5 C4 . . . . -0.36(17) ?
C7 C2 C3 C4 . . . . -0.41(17) ?
C3 C4 C5 N2 . . . . -178.59(12) ?
C3 C4 C5 C6 . . . . 0.31(17) ?
C3 C2 C7 C6 . . . . 0.36(17) ?
C1 C2 C7 C6 . . . . -177.28(11) ?
C1 C2 C3 C4 . . . . 177.26(11) ?