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_4324790
_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_formula_moiety         'C12 H2 F8 N2 S4'
_chemical_formula_sum            'C12 H2 F8 N2 S4'
_chemical_formula_weight         454.40
_chemical_melting_point          479
_chemical_name_systematic
; 
 1,2,3,4,8,9,10,11-octafluoro-7',14'-
 dibenzo[d,i][1,2,6,7,3,8]tetrathiadiazecine
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.166(3)
_cell_length_b                   5.3890(10)
_cell_length_c                   12.325(3)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.767
_cell_measurement_theta_min      22.538
_cell_volume                     752.7(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker XSCANS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            1799
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        -3.17
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  0.9579
_exptl_absorpt_correction_T_min  0.5038
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_description       plate-needle
_exptl_crystal_F_000             448
_exptl_crystal_recrystallization_method chloroform
_exptl_crystal_size_max          1.1
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.066
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0580
_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^)+(0.0609P)^2^+0.0831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                1313
_reflns_number_total             1722
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102565x_si_001_8.cif
_cod_data_source_block           zvota_compound_10
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4324790