Synthesis and properties of the 3-tert-butyl-7-trifluoromethyl-1,4-dihydro-1-phenyl-1,2,4-benzotriazin-4-yl radical
Takahashi, Yusuke; Miura, Youhei; Yoshioka, Naoki; New J. Chem. 39 (2015) 4783–; doi:10.1039/C5NJ00393H

data_7054838
_publ_section_title
;
 Synthesis and properties of the
 3-tert-butyl-7-trifluoromethyl-1,4-dihydro-1-phenyl-1,2,4-benzotriazin-4-yl
 radical
;
_journal_issue                   6
_journal_name_full               'New J. Chem.'
_journal_page_first              4783
_journal_paper_doi               10.1039/C5NJ00393H
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C18 H17 F3 N3'
_chemical_formula_sum            'C18 H17 F3 N3'
_chemical_formula_weight         332.34
_chemical_name_systematic
;
3-tert-butyl-7-trifluoromethyl-1,4-dihydro-1-phenyl-1,2,4-benzotriazin-4-yl
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2015-03-24 deposited with the CCDC.
2015-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.487(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.592(2)
_cell_length_b                   18.904(7)
_cell_length_c                   15.882(5)
_cell_measurement_reflns_used    1622
_cell_measurement_temperature    296.(2)
_cell_measurement_theta_max      22.2728
_cell_measurement_theta_min      2.5082
_cell_volume                     1677.3(10)
_computing_cell_refinement       'APEX2 v2013.4-1 (Bruker AXS)'
_computing_data_collection
;
Bruker Instrument Service V3.0.28 (Bruker AXS Inc., 2013)
;
_computing_data_reduction        'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XSHELL V 6.3.1(Bruker AXS Inc., 2004)'
_computing_publication_material
;
Generate Report (Bruker AXS Inc., 2013)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_diffrn_ambient_temperature      296.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4642
_diffrn_reflns_theta_full        27.35
_diffrn_reflns_theta_max         27.35
_diffrn_reflns_theta_min         2.15
_diffrn_source                   'micro focus sealed tube'
_diffrn_source_type              'INCOATEC I\mS'
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            black-red
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.780
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.264
_refine_ls_abs_structure_details
;
Flack x determined using 614 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   2.0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2871
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0662
_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^)+(0.1000P)^2^+0.4543P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1736
_refine_ls_wR_factor_ref         0.2069
_reflns_number_gt                1725
_reflns_number_total             2871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00393h2.cif
_cod_data_source_block           1Ph3tBu7CF3BT
_cod_depositor_comments
'Adding full bibliography for 7054837--7054838.cif.'
_cod_original_cell_volume        1677.3(11)
_cod_database_code               7054838