Preparation and Crystal Structure of Tetraphenylphosphonium Triiodotetrabromide [PPh4][I3Br4]
Rolf Minkwitz; Michael Berkei; Ralf Ludwig; Inorganic Chemistry 40 (2001) 25–28; doi:10.1021/ic000257y

data_4319100
_publ_section_title
;
 Preparation and Crystal Structure of Tetraphenylphosphonium
 Triiodotetrabromide [PPh4][I3Br4]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              25
_journal_page_last               28
_journal_paper_doi               10.1021/ic000257y
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C24 H20 Br4 I3 P'
_chemical_formula_weight         1039.71
_chemical_name_common            'tetraphenylphosphonium triiodotetrabromide'
_space_group_IT_number           2
_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                66.800(10)
_cell_angle_beta                 77.210(10)
_cell_angle_gamma                85.730(10)
_cell_formula_units_Z            2
_cell_length_a                   10.9470(10)
_cell_length_b                   11.9450(10)
_cell_length_c                   12.8960(10)
_cell_measurement_temperature    173(2)
_cell_volume                     1511.3(3)
_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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0807
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10073
_diffrn_reflns_theta_max         25.63
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    8.455
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.285
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       0.0034(2)
_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   0.850
_refine_ls_goodness_of_fit_obs   0.898
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.850
_refine_ls_restrained_S_obs      0.898
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_obs          0.0362
_refine_ls_shift/su_max          -0.337
_refine_ls_shift/su_mean         0.036
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1207
_refine_ls_wR_factor_obs         0.0944
_reflns_number_observed          3138
_reflns_number_total             5530
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000257y.cif
_cod_data_source_block           C24H20Br4I3P
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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^)+(0.0705P)^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^)+(0.0705P)^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        1511.3(2)
_cod_database_code               4319100