Tribromohydroxyphosphonium Hexafluorometalate: Synthesis, Spectroscopic Characterization, and Crystal Structure of Br3POH+AsF6-
Rolf Minkwitz; Markus Dzyk; Inorganic Chemistry 41 (2002) 1474–1477; doi:10.1021/ic0109039

data_4317701
_publ_contact_author_address
;
          Anorganische Chemie
          Universit\"at Dortmund
          Otto-Hahn-Str. 6
          44221 Dortmund
          Germany
;
_publ_contact_author_email       minkwitz@citrin.chemie.uni-dortmund.de
_publ_contact_author_fax         '049 231 755-3797'
_publ_contact_author_name        'Prof. Dr. Rolf Minkwitz'
_publ_contact_author_phone       '049 231 755-3809'
_publ_section_title
;
 Tribromohydroxyphosphonium Hexafluorometalate: Synthesis, Spectroscopic
 Characterization, and Crystal Structure of Br3POH+AsF6-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1474
_journal_page_last               1477
_journal_paper_doi               10.1021/ic0109039
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'As Br3 F6 H O P'
_chemical_formula_weight         476.63
_chemical_name_systematic
;
   Tribromohydroxyphosphonium hexafluoroarsenate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9250(10)
_cell_length_b                   8.7160(10)
_cell_length_c                   8.4850(10)
_cell_measurement_temperature    173(2)
_cell_volume                     955.87(17)
_computing_cell_refinement       'DENZO SCALEPACK'
_computing_data_collection       KappaCCD
_computing_data_reduction        'DENZO SCALEPACK'
_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-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'KappaCCD NONIUS'
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0821
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1300
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    16.309
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.312
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       0.0021(4)
_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   0.970
_refine_ls_goodness_of_fit_obs   0.939
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         907
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_restrained_S_obs      0.939
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_obs          0.0322
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.6562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0799
_refine_ls_wR_factor_obs         0.0646
_reflns_number_observed          653
_reflns_number_total             907
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0109039.cif
_cod_data_source_block           1324
_cod_depositor_comments
;
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.6562P] 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^)+(0.0000P)^2^+0.6562P] 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        955.9(2)
_cod_original_formula_sum        'H As Br3 F6 O P'
_cod_database_code               4317701