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_7115182
_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_sum            'C4 H7 As2 F11 N2 S'
_chemical_formula_weight         474.02
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.746(3)
_cell_length_b                   8.023(2)
_cell_length_c                   11.034(2)
_cell_measurement_reflns_used    'multiple data'
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      27.12
_cell_measurement_theta_min      2.31
_cell_volume                     1305.4(5)
_computing_cell_refinement       SAINT
_computing_data_collection       SAINT
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measurement_device       'Siemens P4/CCD'
_diffrn_measurement_method       /w
_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  0.0309
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13468
_diffrn_reflns_theta_max         27.12
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.402
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.413
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.412
_exptl_crystal_description       Sphere
_exptl_crystal_F_000             904
_exptl_crystal_size_rad          0.4
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.848
_refine_ls_extinction_coef       0.0044(4)
_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_obs   1.087
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1502
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0262
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0615
_reflns_number_observed          1367
_reflns_number_total             1502
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            904107i.txt
_cod_data_source_block           3
_cod_depositor_comments
;
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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7115182