Tetrachloro- and Tetrabromoarsonium(V) Cations: Raman and 75As, 19F NMR Spectroscopic Characterization and X-ray Crystal Structures of [AsCl4][As(OTeF5)6] and [AsBr4][AsF(OTeF5)5]
Michael Gerken; Peter Kolb; Andreas Wegner; Hélène P. A. Mercier; Horst Borrmann; David A. Dixon; Gary J. Schrobilgen; Inorganic Chemistry 39 (2000) 2813–2824; doi:10.1021/ic000118g

data_4321080
_publ_section_title
;
 Tetrachloro- and Tetrabromoarsonium(V) Cations: Raman and 75As, 19F NMR
 Spectroscopic Characterization and X-ray Crystal Structures of
 [AsCl4][As(OTeF5)6] and [AsBr4][AsF(OTeF5)5]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2813
_journal_page_last               2824
_journal_paper_doi               10.1021/ic000118g
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'As2 Cl4 F30 O6 Te6'
_chemical_formula_weight         1723.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            24
_cell_length_a                   19.688(3)
_cell_length_b                   19.688(3)
_cell_length_c                   55.264(11)
_cell_measurement_temperature    90(2)
_cell_volume                     18551(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_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  0.1722
_diffrn_reflns_av_sigmaI/netI    0.0845
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       75
_diffrn_reflns_limit_l_min       -73
_diffrn_reflns_number            47032
_diffrn_reflns_theta_max         29.19
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    8.260
_exptl_crystal_density_diffrn    3.702
_exptl_crystal_F_000             18336
_refine_diff_density_max         10.901
_refine_diff_density_min         -3.980
_refine_diff_density_rms         1.151
_refine_ls_extinction_coef       0.00086(7)
_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   1.714
_refine_ls_goodness_of_fit_obs   1.806
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         11009
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.718
_refine_ls_restrained_S_obs      1.805
_refine_ls_R_factor_all          0.1436
_refine_ls_R_factor_obs          0.1341
_refine_ls_shift/esd_max         2.342
_refine_ls_shift/esd_mean        0.143
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2253P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.4505
_refine_ls_wR_factor_obs         0.4246
_reflns_number_observed          8839
_reflns_number_total             11012
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000118g_1.cif
_cod_data_source_block           As2Cl4F30O6Te6(-183C)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.2253P)^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^)+(0.2253P)^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_original_cell_volume        18551.6(53)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4321080