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_4321811
_publ_contact_author
;
 Prof. Dr. Rolf Minkwitz
 Fachbereich Chemie der Universit\"at Dortmund
 D-44221 Dortmund, Germany
;
_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
;
 Halogenated Carboxonium Salts: Preparation and Structural Analysis
;
_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     'CH3OHCl+ SbF6-'
_chemical_formula_sum            'C2 H4 Cl F6 O Sb'
_chemical_formula_weight         319.25
_chemical_name_systematic
; 
 Methyl-chloromethylidene-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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 92.59(3)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            4
_cell_length_a                   5.970(3)
_cell_length_b                   12.019(5)
_cell_length_c                   10.994(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      15
_cell_volume                     788.1(6)
_computing_cell_refinement       'NONIUS EXPRESS'
_computing_data_collection       'NONIUS EXPRESS'
_computing_data_reduction        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  0.0983
_diffrn_reflns_av_sigmaI/netI    0.0897
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1774
_diffrn_reflns_theta_max         25.86
_diffrn_reflns_theta_min         3.39
_diffrn_standards_decay_%        5
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.891
_exptl_absorpt_correction_T_max  1.169
_exptl_absorpt_correction_T_min  0.624
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.657
_exptl_crystal_description       plate
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       0.0035(16)
_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   1.141
_refine_ls_goodness_of_fit_obs   1.146
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_restrained_S_obs      1.146
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_obs          0.0419
_refine_ls_shift/esd_max         -0.007
_refine_ls_shift/esd_mean        0.001
_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         0.1372
_refine_ls_wR_factor_obs         0.1344
_reflns_number_observed          999
_reflns_number_total             1045
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981212o_2.cif
_cod_data_source_block           chloreth
_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 
;
_cod_database_code               4321811