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_4321082
_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 Br4 F26 O5 Te5'
_chemical_formula_weight         1681.48
_space_group_IT_number           2
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                103.53(4)
_cell_angle_beta                 103.53(4)
_cell_angle_gamma                105.10(4)
_cell_formula_units_Z            4
_cell_length_a                   9.778(4)
_cell_length_b                   17.731(7)
_cell_length_c                   18.870(8)
_cell_measurement_temperature    90(2)
_cell_volume                     2915(2)
_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  0.0739
_diffrn_reflns_av_sigmaI/netI    0.0875
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33411
_diffrn_reflns_theta_max         25.91
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    12.863
_exptl_crystal_density_diffrn    3.831
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.533
_refine_diff_density_min         -2.120
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.920
_refine_ls_goodness_of_fit_obs   1.026
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         10391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_restrained_S_obs      1.026
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_obs          0.0368
_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^)+(0.0140P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0582
_refine_ls_wR_factor_obs         0.0513
_reflns_number_observed          7008
_reflns_number_total             10508
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000118g_3.cif
_cod_data_source_block           As2Br4F26O5Te5(-183C)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0140P)^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^)+(0.0140P)^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        2915.2(21)
_cod_database_code               4321082