Synthesis and Characterization of the First Examples of Perfluoroalkyl-Substituted Trialkyloxonium Salts, [(CH3)2OCF3]+[Sb2F11]- and [(CH3)2OCF(CF3)2]+[Sb2F11]-
Rolf Minkwitz; Stefan Reinemann; Raphael Seelbinder; Detlef Konikowski; Hans Hartl; Irene Brüdgam; Joachim Hegge; Berthold Hoge; Jeffrey A. Sheehy; Karl O. Christe; Inorganic Chemistry 40 (2001) 4404–4408; doi:10.1021/ic010239w

data_4320093
_publ_section_title
;
 Synthesis and Characterization of the First Examples of
 Perfluoroalkyl-Substituted Trialkyloxonium Salts, [(CH3)2OCF3]+[Sb2F11]-
 and [(CH3)2OCF(CF3)2]+[Sb2F11]-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4404
_journal_page_last               4408
_journal_paper_doi               10.1021/ic010239w
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C3 H6 F14 O Sb2'
_chemical_formula_weight         567.58
_chemical_melting_point          233.15
_chemical_name_common            'methylated trifluoromethyl-methyl ether'
_chemical_name_systematic
;
trifluoromethyl-dimethyl-oxonium
undecafluorodiantimonate
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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            4
_cell_length_a                   9.293(6)
_cell_length_b                   12.456(7)
_cell_length_c                   11.548(8)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    171(2)
_cell_measurement_theta_max      14.59
_cell_measurement_theta_min      7.54
_cell_volume                     1336.7(15)
_computing_cell_refinement       'Nicolet R3m/V'
_computing_data_collection       'Nicolet R3m/V'
_computing_data_reduction        'Nicolet R3m/V'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material
;SHELXL-93 (Sheldrick, 1993), Parst
(Nardelli, 1983), Platon (Spek, 1982) & Missym (Le Page, 1987)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      171(2)
_diffrn_measured_fraction_theta_full 0.841
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measurement_device_type  'Nicolet R3m/V'
_diffrn_measurement_method       \w--2\q
_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  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1659
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         2.73
_diffrn_standards_decay_%        <5
_diffrn_standards_interval_count 300
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    4.199
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.621
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.820
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(6)
_refine_ls_extinction_coef       0.0023(3)
_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   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         907
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+0.2991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0624
_reflns_number_gt                885
_reflns_number_total             907
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010239w.cif
_cod_data_source_block           nic346
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '-40' was changed to '233.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

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

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not determined' 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_database_code               4320093