Heavy Atom Analogues of 1,2,3-Dithiazolylium Salts: Preparation, Structures and Redox Chemistry
Maarit Risto; Abdeljalil Assoud; Stephen M. Winter; Raija Oilunkaniemi; Risto S. Laitinen; Richard T. Oakley; Inorganic Chemistry 47 (2008) 10100–10109; doi:10.1021/ic8013738

data_4306550
_publ_section_title
;
Heavy Atom Analogues of 1,2,3-Dithiazolylium Salts: Preparation, Structures
and Redox Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10100
_journal_page_last               10109
_journal_paper_doi               10.1021/ic8013738
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C6 H4 N S Se, Cl4 Ga'
_chemical_formula_sum            'C6 H4 Cl4 Ga N S Se'
_chemical_formula_weight         412.64
_chemical_name_systematic
; 
 ? 
;
_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                 94.4450(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4587(3)
_cell_length_b                   10.2322(4)
_cell_length_c                   17.0845(7)
_cell_measurement_reflns_used    3060
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.90
_cell_volume                     1299.95(9)
_computing_cell_refinement       'APEX II'
_computing_data_collection       'APEX II'
_computing_data_reduction        'APEX II'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega 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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12141
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.91
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    5.860
_exptl_absorpt_correction_T_max  0.7994
_exptl_absorpt_correction_T_min  0.4357
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'APEX II'
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    2.108
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         3755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0131P)^2^+1.2946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                2822
_reflns_number_total             3755
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8013738_si_002.cif
_cod_data_source_block           mr-2-49_0m
_cod_database_code               4306550