Synthesis and crystal structure studies of 5-(tri-fluoro-meth-yl)-1,3,4-thia-diazol-2(3<i>H</i>)-one at 180 K.
Geetha, Doreswamy; Mohan Kumar, Thaluru M.; Anil Kumar, Haleyur G.; Shreenivas, Mellekatte T.; Basavaraju, Yeriyur B.; Yathirajan, Hemmige S.; Parkin, Sean; Acta crystallographica. Section E, Crystallographic communications 79 (2023) 557–561; doi:10.1107/S2056989023004267

data_2022769
_publ_section_title
;
 Synthesis and crystal structure studies of
 5-(tri-fluoro-meth-yl)-1,3,4-thia-diazol-2(3<i>H</i>)-one at
 180&#x2005;K.
;
_journal_coeditor_code           VM2283
_journal_issue                   'Pt 6'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              557
_journal_page_last               561
_journal_paper_doi               10.1107/S2056989023004267
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C3 H F3 N2 O S'
_chemical_formula_moiety         'C3 H F3 N2 O S'
_chemical_formula_sum            'C3 H F3 N2 O S'
_chemical_formula_weight         170.12
_chemical_name_systematic
;
5-(Trifluoromethyl)-1,3,4-thiadiazol-2(3<i>H</i>)-one
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2019/2 and CIFFIX'
_cell_angle_alpha                63.253(2)
_cell_angle_beta                 71.160(2)
_cell_angle_gamma                67.954(2)
_cell_formula_units_Z            12
_cell_length_a                   10.8996(7)
_cell_length_b                   13.9700(8)
_cell_length_c                   14.1351(9)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      33.09
_cell_measurement_theta_min      2.38
_cell_volume                     1750.38(19)
_computing_cell_refinement
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>XP</i> in <i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_publication_material
;
<i>SHELX</i> (Sheldrick, 2008) and <i>publCIF</i> (Westrip,
2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture dual source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            52212
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.052
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.280
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.313
_refine_ls_extinction_coef       0.0078(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL2019/2</i> (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         8021
_refine_ls_number_restraints     273
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0319P)^2^+1.2580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0899
_reflns_number_gt                6646
_reflns_number_total             8021
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2283sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2022769.cif.'
_cod_database_code               2022769
_cod_database_fobs_code          2022769
_shelx_estimated_absorpt_t_min   0.845
_shelx_estimated_absorpt_t_max   0.863
_shelx_hkl_checksum              66118
_shelx_res_checksum              48456