Crystal and mol-ecular structure of 4-fluoro-1<i>H</i>-pyrazole at 150 K.
Ahmed, Basil M.; Zeller, Matthias; Mezei, Gellert; Acta crystallographica. Section E, Crystallographic communications 79 (2023) 428–431; doi:10.1107/S2056989023003055

data_2022737
_publ_section_title
;
 Crystal and mol-ecular structure of 4-fluoro-1<i>H</i>-pyrazole at
 150&#x2005;K.
;
_journal_coeditor_code           VM2280
_journal_issue                   'Pt 5'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              428
_journal_page_last               431
_journal_paper_doi               10.1107/S2056989023003055
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C3 H3 F N2'
_chemical_formula_moiety         'C3 H3 F N2'
_chemical_formula_sum            'C3 H3 F N2'
_chemical_formula_weight         86.07
_chemical_name_systematic
;
4-Fluoro-1<i>H</i>-pyrazole
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                71.689(2)
_cell_angle_beta                 87.731(2)
_cell_angle_gamma                84.968(2)
_cell_formula_units_Z            4
_cell_length_a                   5.6045(2)
_cell_length_b                   7.4315(3)
_cell_length_c                   9.5396(4)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.1425
_cell_measurement_theta_min      2.2489
_cell_volume                     375.72(3)
_computing_cell_refinement
;
SAINT V8.40B (Bruker, 2022)
;
_computing_data_collection
;
APEX4 v2022.1-1 (Bruker, 2022)
;
_computing_data_reduction
;
SAINT V8.40B (Bruker, 2022)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b),
<i>ShelXle</i> Rev1460 (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS D8 Quest'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15049
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.160
_diffrn_reflns_theta_min         2.249
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           30
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       block
_exptl_crystal_F_000             176
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.430
_exptl_crystal_size_min          0.380
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.257
_refine_ls_extinction_coef       0.040(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL2018/3</i> (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0579P)^2^+0.0788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                2635
_reflns_number_total             2875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2280sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2022737.cif.'
_cod_database_code               2022737
_cod_database_fobs_code          2022737
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.950
_shelx_hkl_checksum              63950
_shelx_res_checksum              69258