Synthesis and characterization of the heteroaromatic MF6− (M = As, Sb) salts of the 1,2,4-trithiolanylium dication [PhCSSC(Ph)S]2+
Cameron, T. Stanley; Decken, Andreas; Fang, Min; Passmore, Jack; Chemical Communications  (2001) 1370–; doi:10.1039/b100001m

data_7114730
_publ_section_title
;
 Synthesis and characterization of the heteroaromatic MF6&#x2212; (M = As,
 Sb) salts of the 1,2,4-trithiolanylium dication
 [Ph&#xE010;CSSC(Ph)S&#xE011;]2+
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1370
_journal_paper_doi               10.1039/b100001m
_journal_year                    2001
_chemical_formula_sum            'C14 H10 F12 S3 Sb2'
_chemical_formula_weight         745.89
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 104.56(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.359(5)
_cell_length_b                   15.148(2)
_cell_length_c                   15.762(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      19.9
_cell_measurement_theta_min      18.8
_cell_volume                     2162.8(12)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
SHELXS86 (Sheldrick, 1985)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.00991
_diffrn_orient_matrix_UB_12      0.06211
_diffrn_orient_matrix_UB_13      0.02220
_diffrn_orient_matrix_UB_21      -0.01147
_diffrn_orient_matrix_UB_22      0.02212
_diffrn_orient_matrix_UB_23      -0.06113
_diffrn_orient_matrix_UB_31      -0.10935
_diffrn_orient_matrix_UB_32      0.00331
_diffrn_orient_matrix_UB_33      -0.00821
_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  0.06174
_diffrn_reflns_av_sigmaI/netI    0.130
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6923
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        -1.66
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.885
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.291
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1408.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.38
_refine_diff_density_min         -1.08
_refine_ls_extinction_coef       0.00000024(2)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   2.910
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     281
_refine_ls_number_reflns         2263
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.2080
_refine_ls_wR_factor_ref         0.2020
_reflns_number_gt                2263
_reflns_number_total             6564
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            b100001m.txt
_cod_data_source_block           pass7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2162.8(9)
_cod_original_sg_symbol_H-M      'P 21/n     '
_cod_original_formula_sum        'C14 H10 F12 S3 Sb2 '
_cod_database_code               7114730