Tris(dimethylamino)oxosulfonium Difluorotrimethylsilicate, (Me2N)3SO+Me3SiF2- (TAOS Fluoride)
Jens Wessel; Ulrich Behrens; Enno Lork; Tobias Borrmann; Wolf-Dieter Stohrer; Rüdiger Mews; Inorganic Chemistry 41 (2002) 4715–4721; doi:10.1021/ic0201755

data_4318438
_publ_contact_author
;
       R\"udiger Mews
       Institut f\"ur Anorganische und Physikalische Chemie
       der Universit\"at
       Postfach 330 440
       28334 Bremen
       Bundesrepublik Deutschland
;
_publ_contact_author_email       mews@chemie.uni-bremen.de
_publ_contact_author_fax         '049 421 2184267'
_publ_contact_author_phone       '049 421 2183354'
_publ_section_title
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 Tris(dimethylamino)oxosulfonium Difluorotrimethylsilicate,
 (Me2N)3SO+Me3SiF2- (TAOS Fluoride)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4715
_journal_page_last               4721
_journal_paper_doi               10.1021/ic0201755
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C9 H27 F2 N3 O S Si'
_chemical_formula_weight         291.49
_chemical_melting_point          330.6(5)
_chemical_name_common            TAOS-Fluoride
_chemical_name_systematic
;
Tris(dimethylamino)oxosulfonium-trimethyldifluorosilicate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0730(10)
_cell_length_b                   8.583(2)
_cell_length_c                   11.1480(10)
_cell_measurement_reflns_used    43
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      16.1
_cell_measurement_theta_min      5.2
_cell_volume                     770.2(2)
_computing_cell_refinement       'Siemens XSCAnS'
_computing_data_collection       'Siemens XSCAnS'
_computing_data_reduction        XPREP
_computing_molecular_graphics    'SHELXTL XPW'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1071
_diffrn_reflns_av_sigmaI/netI    0.0708
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4363
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        'random variation +/-2.0'
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       blocks
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.016
_refine_ls_goodness_of_fit_obs   1.043
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3532
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.015
_refine_ls_restrained_S_obs      1.043
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_obs          0.0455
_refine_ls_shift/esd_max         -0.044
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1145
_refine_ls_wR_factor_obs         0.1132
_reflns_number_observed          3281
_reflns_number_total             3532
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0201755_1.cif
_cod_data_source_block           jw21
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '57-58 deg. C' was changed to
'330.6(5)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+0.0000P] 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^)+(0.0814P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4318438