"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_4026880
_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            'C5 H2 F6 N2'
_chemical_formula_weight         204.09
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.568(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            24
_cell_length_a                   16.4630(5)
_cell_length_b                   12.5288(3)
_cell_length_c                   21.5826(6)
_cell_measurement_temperature    100(2)
_cell_volume                     4140.0(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0576
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            37673
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_T_max  0.9768
_exptl_absorpt_correction_T_min  0.9543
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         11951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1201
_reflns_number_gt                6968
_reflns_number_total             11951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo202305c_si_002.cif
_cod_data_source_block           tolm105
_cod_database_code               4026880