Unsymmetrical 1λ3-1,2,4,6-Thiatriazinyls with Aryl and Trifluoromethyl Substituents: Synthesis, Crystal Structures, EPR Spectroscopy, and Voltammetry
René T. Boeré; Tracey L. Roemmele; Xin Yu; Inorganic Chemistry 50 (2011) 5123–5136; doi:10.1021/ic2003996

data_4325254
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of Lethbridge
Lethbridge, AB Canada
T1K 3M4
;
_publ_contact_author_email       boere@uleth.ca
_publ_contact_author_fax         +1-403-329-2057
_publ_contact_author_name        'R.T. Boer\'e'
_publ_contact_author_phone       +1-403-329-2045
_publ_section_title
;
 Unsymmetrical 1\l3-1,2,4,6-Thiatriazinyls with Aryl and Trifluoromethyl
 Substituents: Synthesis, Crystal Structures, EPR Spectroscopy, and
 Voltammetry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5123
_journal_page_last               5136
_journal_paper_doi               10.1021/ic2003996
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C10 H4 F6 N3 S, C10 H4 F6 N3 S'
_chemical_formula_sum            'C20 H8 F12 N6 S2'
_chemical_formula_weight         624.44
_chemical_name_common            '4-CF3/CF3 TTA dimer'
_chemical_name_systematic
; 
 3-(4-trifluoromethylphenyl)-5-(4-trifluoromethyl)-1-thia-2,4,6-triazinyl
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                94.0420(10)
_cell_angle_beta                 107.4760(10)
_cell_angle_gamma                96.1190(10)
_cell_formula_units_Z            4
_cell_length_a                   10.7943(6)
_cell_length_b                   13.3162(8)
_cell_length_c                   16.7910(10)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.87
_cell_measurement_theta_min      3.69
_cell_volume                     2275.6(2)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2006)'
_computing_publication_material  'publCIF (Westrip, 2007)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type
;
Bruker ApexII CCD area-detector diffractometer
;
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26627
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_min         1.90
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker D8'
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS (Bruker, 2006)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_recrystallization_method sublimation
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         10697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0627P)^2^+0.3309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1260
_reflns_number_gt                7403
_reflns_number_total             10697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2003996_si_001_12.cif
_cod_data_source_block           5e_4-CF3-C6H4C(CF3C)N3S
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4325254