Oxidation of methyl groups in the reaction of sulfur homopolyatomic cations with acetonitrile: formation and crystal structure of the novel trithietanylium ring
Stanley Cameron, T.; Decken, Andreas; Fang, Min; Passmore, Jack; Wood, Dale J.; Parsons, Simon; Chemical Communications  (1999) 1801–; doi:10.1039/a904107i

data_7115180
_publ_section_title
;
 Oxidation of methyl groups in the reaction of sulfur homopolyatomic
 cations with acetonitrile: formation and crystal structure of the novel
 trithietanylium ring
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              1801
_journal_paper_doi               10.1039/a904107i
_journal_year                    1999
_chemical_formula_moiety         '[MeCSNC(Me)NH]+[AsF6]-'
_chemical_formula_sum            'C4 H7 As F6 N2 S'
_chemical_formula_weight         304.10
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     Patterson
_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            8
_cell_length_a                   11.874(3)
_cell_length_b                   12.617(3)
_cell_length_c                   13.005(3)
_cell_measurement_reflns_used    69
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     1948.3(8)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
Stoe Stadi-4 diffractometer equipped with an Oxford Cryosystems lt device.
;
_diffrn_measurement_method       'Omega-theta with profile-fitting (Clegg)'
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3649
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.83
_diffrn_standards_decay_%        -3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.757
_exptl_absorpt_correction_T_max  0.407
_exptl_absorpt_correction_T_min  0.354
_exptl_absorpt_correction_type   'Optimised numerical'
_exptl_absorpt_process_details
;
The face indices and distances were refined against a set of psi-scan
data, and then used to perform an absorption correction by Gaussian
integration (Stoe X-shape; Shelxtl Xprep). 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.073
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.00045(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    'Rotating group (Me)/ Refall (NH)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         1725
_refine_ls_number_restraints     352
_refine_ls_restrained_S_all      1.518
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0060P)^2^+6.4612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                1222
_reflns_number_total             1725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            904107i.txt
_cod_data_source_block           1s41sn
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'Difference map' was changed
to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7115180