Halogenated Carboxonium Salts: Preparation and Structural Analysis
Rolf Minkwitz; Stefan Reinemann; Oliver Blecher; Hans Hartl; Irene Brüdgam; Inorganic Chemistry 38 (1999) 844–847; doi:10.1021/ic981212o

data_4321810
_publ_contact_author
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 Prof. Dr. Rolf Minkwitz
 Fachbereich Chemie der Universit\"at Dortmund
 D-44221 Dortmund, Germany
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_publ_contact_author_email       minkwitz@citrin.chemie.uni-dortmund.de
_publ_contact_author_fax         '049 231 755-3797'
_publ_contact_author_phone       '049 231 755-3809'
_publ_section_title
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 Halogenated Carboxonium Salts: Preparation and Structural Analysis
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              844
_journal_page_last               847
_journal_paper_doi               10.1021/ic981212o
_journal_volume                  38
_journal_year                    1999
_chemical_formula_structural     'CH3OCHF+ SbF6-'
_chemical_formula_sum            'C2 H4 F7 O Sb'
_chemical_formula_weight         298.80
_chemical_name_systematic
; 
Methyl-fluoromethylidene-oxonium-hexafluoroantimonate  
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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(3)
_cell_angle_beta                 111.27(2)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            4
_cell_length_a                   9.942(2)
_cell_length_b                   7.454(2)
_cell_length_c                   10.297(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      15
_cell_volume                     711.1(3)
_computing_cell_refinement       'NONIUS EXPRESS'
_computing_data_collection       'NONIUS EXPRESS'
_computing_data_reduction        'NONIUS MOLEN'
_computing_molecular_graphics    'ORTEP, SHELXTL PLUS (1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_measurement_device       'NONIUS CAD4'
_diffrn_measurement_method       omega/2theta
_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  0.0591
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4209
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         3.46
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.959
_exptl_absorpt_correction_T_max  0.9976
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.791
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         3.731
_refine_diff_density_min         -3.648
_refine_diff_density_rms         0.296
_refine_ls_extinction_coef       0.0113(18)
_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_all   1.196
_refine_ls_goodness_of_fit_obs   1.218
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         2072
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.198
_refine_ls_restrained_S_obs      1.218
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_obs          0.0471
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1515
_refine_ls_wR_factor_obs         0.1446
_reflns_number_observed          1835
_reflns_number_total             2073
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981212o_1.cif
_cod_data_source_block           fleth_psi
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^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^)+(0.1000P)^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               4321810