Interaction of 1,3,2,4-Benzodithiadiazines and Their 1-Se Congeners with Ph3P and Some Properties of the Iminophosphorane Products
Alexander Yu. Makarov; Vladimir V. Zhivonitko; Arkady G. Makarov; Samat B. Zikirin; Irina Yu. Bagryanskaya; Victor A. Bagryansky; Yuri V. Gatilov; Irina G. Irtegova; Makhmut M. Shakirov; Andrey V. Zibarev; Inorganic Chemistry 50 (2011) 3017–3027; doi:10.1021/ic102565x

data_4324787
_publ_contact_author_email       bagryan@nioch.nsc.ru
_publ_contact_author_name        'Dr. I. Yu. Bagryanskaya'
_publ_section_title
;
 Interaction of 1,3,2,4-Benzodithiadiazines and Their 1-Se Congeners with
 Ph3P and Some Properties of the Iminophosphorane Products
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3017
_journal_page_last               3027
_journal_paper_doi               10.1021/ic102565x
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C6 H F3 N2 S Se'
_chemical_formula_sum            'C6 H F3 N2 S Se'
_chemical_formula_weight         269.11
_chemical_melting_point          346
_chemical_name_systematic
; 
 5,6,8-trifluoro-3\l^4^\s^2^,1,2,4-benzothiaselenadiazine 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   25.520(3)
_cell_length_b                   3.8358(5)
_cell_length_c                   31.309(4)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.84
_cell_measurement_theta_min      2.52
_cell_volume                     3064.8(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.1159
_diffrn_reflns_av_sigmaI/netI    0.0863
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            27424
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    5.171
_exptl_absorpt_correction_T_max  0.6473
_exptl_absorpt_correction_T_min  0.3964
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS-2008/1 - Bruker AXS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.333
_exptl_crystal_description       needle
_exptl_crystal_F_000             2048
_exptl_crystal_recrystallization_method MeCN
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         7988
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                5915
_reflns_number_total             7988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102565x_si_001_5.cif
_cod_data_source_block           h7se_compound_5
_cod_database_code               4324787