Convenient Preparation and Full Characterization of a Synthetically Useful Salt of the Dithianitronium Cation, SNSSbF6, from Readily Available Starting Materials
T. Stanley Cameron; Aaron Mailman; Jack Passmore; Konstantin V. Shuvaev; Inorganic Chemistry 44 (2005) 6524–6528; doi:10.1021/ic0483139

data_4309554
_publ_section_title
;
Convenient Preparation and Full Characterization of a Synthetically Useful
Salt of the Dithianitronium Cation, SNSSbF6, from Readily Available
Starting Materials
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6524
_journal_page_last               6528
_journal_paper_doi               10.1021/ic0483139
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'F6 N S2 Sb'
_chemical_formula_weight         313.87
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_cell_angle_alpha                90
_cell_angle_beta                 90.58(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.740(2)
_cell_length_b                   6.644(2)
_cell_length_c                   5.334(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      19.6
_cell_volume                     345.16(14)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction
'teXsan for Windows version 1.06 (MSC, 1997-1999)'
_computing_publication_material
'teXsan for Windows version 1.06 (MSC, 1997-1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
SHELX97 (Sheldrick, 1997)
;
_diffrn_ambient_temperature      183.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.01125
_diffrn_orient_matrix_UB_12      0.13900
_diffrn_orient_matrix_UB_13      0.06910
_diffrn_orient_matrix_UB_21      0.00625
_diffrn_orient_matrix_UB_22      0.05461
_diffrn_orient_matrix_UB_23      -0.17420
_diffrn_orient_matrix_UB_31      -0.10187
_diffrn_orient_matrix_UB_32      0.01870
_diffrn_orient_matrix_UB_33      -0.00498
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.01840
_diffrn_reflns_av_sigmaI/netI    0.018
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            576
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         3.71
_diffrn_standards_decay_%        0.09
_diffrn_standards_interval_count 1
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.636
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    3.019
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             288.00
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.66
_refine_diff_density_min         -1.07
_refine_ls_extinction_coef       0.0000000(1)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   1.930
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     31
_refine_ls_number_reflns         546
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0190
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0006
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     unit
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0190
_refine_ls_wR_factor_ref         0.0480
_reflns_number_gt                546
_reflns_number_total             546
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ic0483139si20050222_123349.cif
_cod_data_source_block           '_afc5r.xtl_Cu_radiation___'
_cod_original_cell_volume        345.2(1)
_cod_original_sg_symbol_H-M      'C 2/m '
_cod_original_formula_sum        'F6 N S2 Sb '
_cod_database_code               4309554