"Reported, but Still Unknown." A Closer Look into 3,4-Bis- and 3,4,5-Tris(trifluoromethyl)pyrazoles
Igor I. Gerus; Roman X. Mironetz; Ivan S. Kondratov; Andrei V. Bezdudny; Yurii V. Dmytriv; Oleg V. Shishkin; Viktoriia S. Starova; Olga A. Zaporozhets; Andrey A. Tolmachev; Pavel K. Mykhailiuk; Journal of Organic Chemistry 77 (2012) 47–56; doi:10.1021/jo202305c

data_4026879
_publ_section_title
;
 "Reported, but Still Unknown." A Closer Look into 3,4-Bis- and
 3,4,5-Tris(trifluoromethyl)pyrazoles
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              47
_journal_page_last               56
_journal_paper_doi               10.1021/jo202305c
_journal_volume                  77
_journal_year                    2012
_chemical_formula_sum            'C6 H2 F9 N2 O0.5'
_chemical_formula_weight         281.09
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.914(5)
_cell_angle_beta                 101.077(5)
_cell_angle_gamma                108.534(5)
_cell_formula_units_Z            4
_cell_length_a                   9.0544(5)
_cell_length_b                   9.4420(6)
_cell_length_c                   11.9252(8)
_cell_measurement_temperature    100(2)
_cell_volume                     941.73(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10975
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.250
_exptl_absorpt_correction_T_max  0.9754
_exptl_absorpt_correction_T_min  0.9517
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.814
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.814
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                2953
_reflns_number_total             5457
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo202305c_si_001.cif
_cod_data_source_block           tolm78
_cod_depositor_comments
;

2025-10-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C12 H4 F18 N4 O'
_cod_original_formula_weight         562.19
_cod_original_formula_units_Z            2
_cod_original_cell_volume        941.73(10)
_cod_database_code               4026879